data_6274 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H20 P)+, (C42 H30 Re S6)-, (C3 H7 N O)' _chemical_formula_sum 'C69 H57 N O P Re S6' _chemical_formula_weight 1325.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.220(2) _cell_length_b 31.379(3) _cell_length_c 14.747(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.663(8) _cell_angle_gamma 90.00 _cell_volume 5880.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque parallelepiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 2.352 _exptl_absorpt_correction_type 'Gaussian' _exptl_absorpt_correction_T_min 0.6137 _exptl_absorpt_correction_T_max 0.7342 _exptl_absorpt_process_details 'SADABS 2008/1, Bruker AXS (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '3106 images at 0.5 deg. stepwise rotation in omega and phi, 15 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 149706 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17126 _reflns_number_gt 15194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+14.9211P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17126 _refine_ls_number_parameters 816 _refine_ls_number_restraints 169 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.198709(8) -0.138197(3) 0.250121(7) 0.01747(3) Uani 1 1 d D . . S1 S 0.32043(5) -0.08280(2) 0.29768(5) 0.02459(13) Uani 1 1 d . A . C2 C 0.4446(2) -0.10163(9) 0.3824(2) 0.0236(5) Uani 1 1 d . . . C3 C 0.4580(2) -0.14329(9) 0.4074(2) 0.0224(5) Uani 1 1 d . A . S4 S 0.34998(5) -0.17758(2) 0.35059(5) 0.02103(12) Uani 1 1 d . A . C5 C 0.5245(2) -0.06734(10) 0.4245(2) 0.0276(6) Uani 1 1 d . A . C6 C 0.5479(3) -0.04244(11) 0.3603(3) 0.0370(7) Uani 1 1 d . . . H6 H 0.5180 -0.0492 0.2901 0.044 Uiso 1 1 calc R A . C7 C 0.6149(3) -0.00747(12) 0.3973(3) 0.0435(8) Uani 1 1 d . A . H7 H 0.6316 0.0093 0.3529 0.052 Uiso 1 1 calc R . . C8 C 0.6567(3) 0.00268(11) 0.4993(3) 0.0413(8) Uani 1 1 d . . . H8 H 0.7018 0.0267 0.5247 0.050 Uiso 1 1 calc R A . C9 C 0.6334(3) -0.02190(11) 0.5645(3) 0.0357(7) Uani 1 1 d . A . H9 H 0.6618 -0.0146 0.6343 0.043 Uiso 1 1 calc R . . C10 C 0.5687(2) -0.05714(10) 0.5280(2) 0.0308(6) Uani 1 1 d . . . H10 H 0.5542 -0.0744 0.5730 0.037 Uiso 1 1 calc R A . C11 C 0.5579(2) -0.16362(9) 0.4821(2) 0.0235(5) Uani 1 1 d . . . C12 C 0.6516(2) -0.15895(11) 0.4747(3) 0.0325(7) Uani 1 1 d . A . H12 H 0.6528 -0.1425 0.4212 0.039 Uiso 1 1 calc R . . C13 C 0.7438(3) -0.17834(12) 0.5454(3) 0.0409(8) Uani 1 1 d . . . H13 H 0.8072 -0.1750 0.5395 0.049 Uiso 1 1 calc R A . C14 C 0.7434(3) -0.20225(12) 0.6239(3) 0.0391(8) Uani 1 1 d . A . H14 H 0.8065 -0.2152 0.6721 0.047 Uiso 1 1 calc R . . C15 C 0.6507(3) -0.20722(10) 0.6320(3) 0.0338(7) Uani 1 1 d . . . H15 H 0.6501 -0.2235 0.6860 0.041 Uiso 1 1 calc R A . C16 C 0.5583(2) -0.18826(10) 0.5610(2) 0.0285(6) Uani 1 1 d . A . H16 H 0.4947 -0.1922 0.5664 0.034 Uiso 1 1 calc R . . S21 S 0.09863(6) -0.09111(2) 0.11920(5) 0.02482(13) Uani 1 1 d . A . C22 C 0.0726(2) -0.11396(10) 0.0026(2) 0.0269(6) Uani 1 1 d . . . C23 C 0.1099(2) -0.15345(10) 0.0003(2) 0.0240(5) Uani 1 1 d . A . S24 S 0.18530(5) -0.18000(2) 0.11416(5) 0.02088(12) Uani 1 1 d . A . C25 C 0.0067(3) -0.08698(11) -0.0862(2) 0.0338(7) Uani 1 1 d . A . C26 C 0.0304(3) -0.04359(13) -0.0870(3) 0.0455(9) Uani 1 1 d . . . H26 H 0.0874 -0.0314 -0.0297 0.055 Uiso 1 1 calc R A . C27 C -0.0290(3) -0.01840(15) -0.1708(3) 0.0520(10) Uani 1 1 d . A . H27 H -0.0117 0.0108 -0.1711 0.062 Uiso 1 1 calc R . . C28 C -0.1130(3) -0.03563(14) -0.2536(3) 0.0469(9) Uani 1 1 d . . . H28 H -0.1528 -0.0184 -0.3113 0.056 Uiso 1 1 calc R A . C29 C -0.1392(3) -0.07804(14) -0.2525(3) 0.0431(9) Uani 1 1 d . A . H29 H -0.1980 -0.0897 -0.3091 0.052 Uiso 1 1 calc R . . C30 C -0.0799(3) -0.10398(13) -0.1690(2) 0.0365(7) Uani 1 1 d . . . H30 H -0.0986 -0.1330 -0.1688 0.044 Uiso 1 1 calc R A . C31 C 0.0931(2) -0.17668(12) -0.0940(2) 0.0317(7) Uani 1 1 d . . . C32 C 0.0555(3) -0.21868(12) -0.1104(3) 0.0376(8) Uani 1 1 d . A . H32 H 0.0448 -0.2331 -0.0591 0.045 Uiso 1 1 calc R . . C33 C 0.0336(3) -0.23934(17) -0.2012(3) 0.0565(12) Uani 1 1 d . . . H33 H 0.0065 -0.2676 -0.2124 0.068 Uiso 1 1 calc R A . C34 C 0.0510(4) -0.2191(2) -0.2744(3) 0.0698(16) Uani 1 1 d . A . H34 H 0.0346 -0.2331 -0.3368 0.084 Uiso 1 1 calc R . . C35 C 0.0922(5) -0.1786(2) -0.2584(3) 0.0740(17) Uani 1 1 d . . . H35 H 0.1059 -0.1652 -0.3090 0.089 Uiso 1 1 calc R A . C36 C 0.1141(4) -0.15669(16) -0.1672(3) 0.0511(10) Uani 1 1 d . A . H36 H 0.1428 -0.1287 -0.1561 0.061 Uiso 1 1 calc R . . S41 S 0.1239(4) -0.10133(9) 0.3408(4) 0.0297(5) Uani 0.628(3) 1 d PD A 1 S44 S 0.1078(10) -0.19582(13) 0.2774(10) 0.0211(3) Uani 0.628(3) 1 d PD A 1 C42 C 0.0329(4) -0.13523(18) 0.3553(4) 0.0270(12) Uani 0.628(3) 1 d PD A 1 C43 C 0.0330(6) -0.17702(18) 0.3354(6) 0.0242(10) Uani 0.628(3) 1 d PD A 1 C45 C -0.0344(4) -0.11650(19) 0.3995(4) 0.0340(11) Uani 0.628(3) 1 d PD A 1 C46 C -0.1350(5) -0.1046(4) 0.3386(6) 0.085(3) Uani 0.628(3) 1 d PD A 1 H46 H -0.1619 -0.1079 0.2673 0.102 Uiso 0.628(3) 1 calc PR A 1 C47 C -0.2003(6) -0.0877(4) 0.3771(8) 0.103(4) Uani 0.628(3) 1 d PD A 1 H47 H -0.2691 -0.0781 0.3325 0.124 Uiso 0.628(3) 1 calc PR A 1 C48 C -0.1637(7) -0.0849(3) 0.4804(7) 0.067(2) Uani 0.628(3) 1 d PD A 1 H48 H -0.2059 -0.0725 0.5083 0.080 Uiso 0.628(3) 1 calc PR A 1 C49 C -0.0705(14) -0.0996(6) 0.5393(9) 0.071(3) Uani 0.628(3) 1 d PD A 1 H49 H -0.0439 -0.0983 0.6110 0.086 Uiso 0.628(3) 1 calc PR A 1 C50 C -0.0101(8) -0.1174(3) 0.4966(5) 0.061(3) Uani 0.628(3) 1 d PD A 1 H50 H 0.0535 -0.1311 0.5409 0.073 Uiso 0.628(3) 1 calc PR A 1 C51 C -0.0370(4) -0.20713(17) 0.3538(3) 0.0229(11) Uani 0.628(3) 1 d PD A 1 C52 C -0.0025(5) -0.2296(4) 0.4448(10) 0.0348(18) Uani 0.628(3) 1 d PD A 1 H52 H 0.0680 -0.2269 0.4959 0.042 Uiso 0.628(3) 1 calc PR A 1 C53 C -0.0740(6) -0.2563(7) 0.4598(16) 0.0432(15) Uani 0.628(3) 1 d PD A 1 H53 H -0.0502 -0.2739 0.5183 0.052 Uiso 0.628(3) 1 calc PR A 1 C54 C -0.1787(5) -0.25685(19) 0.3892(6) 0.0387(17) Uani 0.628(3) 1 d PD A 1 H54 H -0.2276 -0.2732 0.4021 0.046 Uiso 0.628(3) 1 calc PR A 1 C55 C -0.2126(5) -0.2341(3) 0.3009(7) 0.059(3) Uani 0.628(3) 1 d PD A 1 H55 H -0.2842 -0.2355 0.2517 0.071 Uiso 0.628(3) 1 calc PR A 1 C56 C -0.1429(4) -0.2091(3) 0.2835(6) 0.051(2) Uani 0.628(3) 1 d PD A 1 H56 H -0.1672 -0.1930 0.2227 0.061 Uiso 0.628(3) 1 calc PR A 1 S41X S 0.1363(10) -0.0926(2) 0.3394(10) 0.0297(5) Uani 0.218(3) 1 d PD A 2 S44X S 0.1034(9) -0.1886(2) 0.2885(10) 0.0211(3) Uani 0.218(3) 1 d PD A 2 C42X C 0.0553(11) -0.1231(3) 0.3771(12) 0.0270(12) Uani 0.218(3) 1 d PD A 2 C43X C 0.0384(13) -0.1644(3) 0.3508(15) 0.0242(10) Uani 0.218(3) 1 d PD A 2 C45X C -0.0023(10) -0.0989(4) 0.4245(10) 0.0340(11) Uani 0.218(3) 1 d PD A 2 C46X C -0.0714(14) -0.0675(6) 0.3739(12) 0.085(3) Uani 0.218(3) 1 d PD A 2 H46X H -0.0699 -0.0553 0.3156 0.102 Uiso 0.218(3) 1 calc PR A 2 C47X C -0.1446(15) -0.0525(8) 0.4050(16) 0.103(4) Uani 0.218(3) 1 d PD A 2 H47X H -0.2025 -0.0355 0.3611 0.124 Uiso 0.218(3) 1 calc PR A 2 C48X C -0.1310(17) -0.0629(7) 0.5007(17) 0.067(2) Uani 0.218(3) 1 d PD A 2 H48X H -0.1670 -0.0477 0.5315 0.080 Uiso 0.218(3) 1 calc PR A 2 C49X C -0.068(4) -0.0941(17) 0.548(2) 0.071(3) Uani 0.218(3) 1 d PD A 2 H49X H -0.0702 -0.1073 0.6049 0.086 Uiso 0.218(3) 1 calc PR A 2 C50X C 0.004(2) -0.1077(11) 0.5142(15) 0.061(3) Uani 0.218(3) 1 d PD A 2 H50X H 0.0620 -0.1245 0.5591 0.073 Uiso 0.218(3) 1 calc PR A 2 C51X C -0.0319(9) -0.1927(4) 0.3735(10) 0.0229(11) Uani 0.218(3) 1 d PD A 2 C52X C 0.0087(11) -0.2285(12) 0.436(3) 0.0348(18) Uani 0.218(3) 1 d PD A 2 H52X H 0.0807 -0.2361 0.4605 0.042 Uiso 0.218(3) 1 calc PR A 2 C53X C -0.0592(15) -0.253(2) 0.461(5) 0.0432(15) Uani 0.218(3) 1 d PD A 2 H53X H -0.0316 -0.2740 0.5127 0.052 Uiso 0.218(3) 1 calc PR A 2 C54X C -0.1665(15) -0.2460(6) 0.4101(18) 0.0387(17) Uani 0.218(3) 1 d PD A 2 H54X H -0.2126 -0.2621 0.4276 0.046 Uiso 0.218(3) 1 calc PR A 2 C55X C -0.2069(10) -0.2161(7) 0.335(2) 0.059(3) Uani 0.218(3) 1 d PD A 2 H55X H -0.2809 -0.2135 0.2955 0.071 Uiso 0.218(3) 1 calc PR A 2 C56X C -0.1406(10) -0.1897(7) 0.3154(16) 0.051(2) Uani 0.218(3) 1 d PD A 2 H56X H -0.1691 -0.1693 0.2623 0.061 Uiso 0.218(3) 1 calc PR A 2 S41Y S 0.1146(16) -0.0973(3) 0.3268(15) 0.0297(5) Uani 0.154(3) 1 d PD A 3 S44Y S 0.105(4) -0.1932(5) 0.284(4) 0.0211(3) Uani 0.154(3) 1 d PD A 3 C42Y C 0.0594(17) -0.1321(4) 0.3845(14) 0.0270(12) Uani 0.154(3) 1 d PD A 3 C43Y C 0.0407(19) -0.1727(4) 0.3519(19) 0.0242(10) Uani 0.154(3) 1 d PD A 3 C45Y C 0.0329(12) -0.1128(6) 0.4632(12) 0.0340(11) Uani 0.154(3) 1 d PD A 3 C46Y C -0.0653(15) -0.1156(13) 0.456(2) 0.085(3) Uani 0.154(3) 1 d PD A 3 H46Y H -0.1154 -0.1333 0.4051 0.102 Uiso 0.154(3) 1 calc PR A 3 C47Y C -0.096(2) -0.0935(19) 0.520(4) 0.103(4) Uani 0.154(3) 1 d PD A 3 H47Y H -0.1673 -0.0940 0.5090 0.124 Uiso 0.154(3) 1 calc PR A 3 C48Y C -0.0217(19) -0.0710(9) 0.600(2) 0.067(2) Uani 0.154(3) 1 d PD A 3 H48Y H -0.0392 -0.0577 0.6487 0.080 Uiso 0.154(3) 1 calc PR A 3 C49Y C 0.0732(17) -0.0683(8) 0.6087(15) 0.071(3) Uani 0.154(3) 1 d PD A 3 H49Y H 0.1259 -0.0529 0.6634 0.086 Uiso 0.154(3) 1 calc PR A 3 C50Y C 0.0968(13) -0.0880(7) 0.5372(14) 0.061(3) Uani 0.154(3) 1 d PD A 3 H50Y H 0.1649 -0.0833 0.5421 0.073 Uiso 0.154(3) 1 calc PR A 3 C51Y C -0.0173(13) -0.2039(5) 0.3836(13) 0.0229(11) Uani 0.154(3) 1 d PD A 3 C52Y C 0.0363(12) -0.2354(8) 0.4558(19) 0.0348(18) Uani 0.154(3) 1 d PD A 3 H52Y H 0.1103 -0.2387 0.4814 0.042 Uiso 0.154(3) 1 calc PR A 3 C53Y C -0.0209(18) -0.2621(7) 0.4899(17) 0.0432(15) Uani 0.154(3) 1 d PD A 3 H53Y H 0.0151 -0.2816 0.5436 0.052 Uiso 0.154(3) 1 calc PR A 3 C54Y C -0.1296(18) -0.2598(7) 0.445(2) 0.0387(17) Uani 0.154(3) 1 d PD A 3 H54Y H -0.1680 -0.2773 0.4691 0.046 Uiso 0.154(3) 1 calc PR A 3 C55Y C -0.1819(13) -0.2323(10) 0.366(3) 0.059(3) Uani 0.154(3) 1 d PD A 3 H55Y H -0.2565 -0.2307 0.3358 0.071 Uiso 0.154(3) 1 calc PR A 3 C56Y C -0.1265(13) -0.2071(9) 0.330(2) 0.051(2) Uani 0.154(3) 1 d PD A 3 H56Y H -0.1631 -0.1918 0.2688 0.061 Uiso 0.154(3) 1 calc PR A 3 P60 P 0.42637(5) 0.12204(2) 0.10146(5) 0.02223(13) Uani 1 1 d . . . C61 C 0.3093(2) 0.15376(10) 0.0633(2) 0.0231(5) Uani 1 1 d . . . C62 C 0.3140(2) 0.19460(11) 0.1008(2) 0.0330(7) Uani 1 1 d . . . H62 H 0.3782 0.2053 0.1525 0.040 Uiso 1 1 calc R . . C63 C 0.2235(3) 0.21984(12) 0.0618(3) 0.0408(8) Uani 1 1 d . . . H63 H 0.2263 0.2479 0.0873 0.049 Uiso 1 1 calc R . . C64 C 0.1296(2) 0.20438(12) -0.0137(3) 0.0355(7) Uani 1 1 d . . . H64 H 0.0687 0.2219 -0.0405 0.043 Uiso 1 1 calc R . . C65 C 0.1247(2) 0.16346(12) -0.0500(3) 0.0345(7) Uani 1 1 d . . . H65 H 0.0602 0.1528 -0.1012 0.041 Uiso 1 1 calc R . . C66 C 0.2135(2) 0.13807(10) -0.0121(2) 0.0296(6) Uani 1 1 d . . . H66 H 0.2098 0.1099 -0.0371 0.035 Uiso 1 1 calc R . . C71 C 0.4756(2) 0.13022(10) 0.0090(2) 0.0264(6) Uani 1 1 d . . . C72 C 0.4060(3) 0.14191(14) -0.0900(2) 0.0422(9) Uani 1 1 d . . . H72 H 0.3336 0.1462 -0.1082 0.051 Uiso 1 1 calc R . . C73 C 0.4432(4) 0.14732(16) -0.1621(3) 0.0533(11) Uani 1 1 d . . . H73 H 0.3960 0.1554 -0.2294 0.064 Uiso 1 1 calc R . . C74 C 0.5486(3) 0.14098(13) -0.1361(3) 0.0438(9) Uani 1 1 d . . . H74 H 0.5733 0.1443 -0.1858 0.053 Uiso 1 1 calc R . . C75 C 0.6181(3) 0.12981(11) -0.0373(3) 0.0361(7) Uani 1 1 d . . . H75 H 0.6906 0.1259 -0.0195 0.043 Uiso 1 1 calc R . . C76 C 0.5822(2) 0.12433(11) 0.0357(2) 0.0295(6) Uani 1 1 d . . . H76 H 0.6300 0.1166 0.1031 0.035 Uiso 1 1 calc R . . C81 C 0.5274(2) 0.13603(9) 0.2259(2) 0.0234(5) Uani 1 1 d . . . C82 C 0.5524(3) 0.10838(10) 0.3079(2) 0.0299(6) Uani 1 1 d . . . H82 H 0.5155 0.0823 0.2987 0.036 Uiso 1 1 calc R . . C83 C 0.6315(3) 0.11931(12) 0.4029(2) 0.0362(7) Uani 1 1 d . . . H83 H 0.6482 0.1006 0.4586 0.043 Uiso 1 1 calc R . . C84 C 0.6860(3) 0.15691(12) 0.4170(2) 0.0350(7) Uani 1 1 d . . . H84 H 0.7405 0.1639 0.4821 0.042 Uiso 1 1 calc R . . C85 C 0.6612(3) 0.18476(12) 0.3357(2) 0.0348(7) Uani 1 1 d . . . H85 H 0.6982 0.2109 0.3456 0.042 Uiso 1 1 calc R . . C86 C 0.5823(2) 0.17430(10) 0.2403(2) 0.0292(6) Uani 1 1 d . . . H86 H 0.5658 0.1932 0.1849 0.035 Uiso 1 1 calc R . . C91 C 0.3911(3) 0.06730(10) 0.1024(2) 0.0317(6) Uani 1 1 d . . . C92 C 0.4455(5) 0.03571(15) 0.0807(4) 0.0710(16) Uani 1 1 d . . . H92 H 0.5012 0.0429 0.0648 0.085 Uiso 1 1 calc R . . C93 C 0.4180(6) -0.00697(15) 0.0825(5) 0.091(2) Uani 1 1 d . . . H93 H 0.4553 -0.0289 0.0680 0.109 Uiso 1 1 calc R . . C94 C 0.3358(4) -0.01716(14) 0.1054(3) 0.0579(12) Uani 1 1 d . . . H94 H 0.3139 -0.0460 0.1016 0.069 Uiso 1 1 calc R . . C95 C 0.2864(3) 0.01359(12) 0.1333(3) 0.0419(8) Uani 1 1 d . . . H95 H 0.2333 0.0061 0.1528 0.050 Uiso 1 1 calc R . . C96 C 0.3142(3) 0.05581(11) 0.1327(3) 0.0367(7) Uani 1 1 d . . . H96 H 0.2806 0.0773 0.1532 0.044 Uiso 1 1 calc R . . O100 O 0.2886(9) -0.0517(4) 0.8133(9) 0.152(4) Uiso 0.628(3) 1 d PDU A 1 C101 C 0.2095(15) -0.0464(7) 0.7368(14) 0.206(10) Uiso 0.628(3) 1 d PDU A 1 H101 H 0.1797 -0.0666 0.6833 0.247 Uiso 0.628(3) 1 calc PR A 1 N102 N 0.1681(7) -0.0072(4) 0.7376(7) 0.112(3) Uiso 0.628(3) 1 d PDU A 1 C103 C 0.0659(9) 0.0005(4) 0.6398(8) 0.095(3) Uiso 0.628(3) 1 d PDU A 1 H10A H 0.0382 0.0289 0.6423 0.143 Uiso 0.628(3) 1 calc PR A 1 H10B H 0.0137 -0.0211 0.6338 0.143 Uiso 0.628(3) 1 calc PR A 1 H10C H 0.0805 -0.0013 0.5810 0.143 Uiso 0.628(3) 1 calc PR A 1 C104 C 0.2101(12) 0.0268(5) 0.8193(11) 0.134(5) Uiso 0.628(3) 1 d PD A 1 H10D H 0.1632 0.0516 0.7979 0.201 Uiso 0.628(3) 1 calc PR A 1 H10E H 0.2807 0.0354 0.8303 0.201 Uiso 0.628(3) 1 calc PR A 1 H10F H 0.2136 0.0154 0.8827 0.201 Uiso 0.628(3) 1 calc PR A 1 O110 O 0.156(2) -0.0448(10) 0.6025(19) 0.152(4) Uiso 0.218(3) 1 d PD A 2 C111 C 0.158(2) -0.0203(10) 0.666(3) 0.206(10) Uiso 0.218(3) 1 d PD A 2 H111 H 0.1293 0.0076 0.6513 0.247 Uiso 0.218(3) 1 calc PR A 2 N112 N 0.2073(17) -0.0372(8) 0.7614(19) 0.112(3) Uiso 0.218(3) 1 d PD A 2 C113 C 0.243(3) -0.0827(9) 0.755(2) 0.095(3) Uiso 0.218(3) 1 d PD A 2 H11A H 0.2773 -0.0952 0.8234 0.143 Uiso 0.218(3) 1 calc PR A 2 H11B H 0.2935 -0.0821 0.7265 0.143 Uiso 0.218(3) 1 calc PR A 2 H11C H 0.1823 -0.1001 0.7118 0.143 Uiso 0.218(3) 1 calc PR A 2 C114 C 0.230(3) -0.0195(12) 0.864(2) 0.134(5) Uiso 0.218(3) 1 d PD A 2 H11D H 0.2642 -0.0415 0.9159 0.201 Uiso 0.218(3) 1 calc PR A 2 H11E H 0.1643 -0.0107 0.8645 0.201 Uiso 0.218(3) 1 calc PR A 2 H11F H 0.2772 0.0051 0.8790 0.201 Uiso 0.218(3) 1 calc PR A 2 O120 O 0.311(3) -0.0055(14) 0.820(3) 0.152(4) Uiso 0.154(3) 1 d PD A 3 C121 C 0.256(3) 0.0207(12) 0.831(3) 0.206(10) Uiso 0.154(3) 1 d PD A 3 H121 H 0.2603 0.0504 0.8207 0.247 Uiso 0.154(3) 1 calc PR A 3 N122 N 0.187(2) 0.0025(10) 0.8607(19) 0.112(3) Uiso 0.154(3) 1 d PD A 3 C123 C 0.116(3) 0.0360(12) 0.875(3) 0.095(3) Uiso 0.154(3) 1 d PD A 3 H12A H 0.0692 0.0220 0.8979 0.143 Uiso 0.154(3) 1 calc PR A 3 H12B H 0.0748 0.0506 0.8105 0.143 Uiso 0.154(3) 1 calc PR A 3 H12C H 0.1603 0.0568 0.9260 0.143 Uiso 0.154(3) 1 calc PR A 3 C124 C 0.173(4) -0.0440(11) 0.880(4) 0.134(5) Uiso 0.154(3) 1 d PD A 3 H12D H 0.1176 -0.0468 0.9010 0.201 Uiso 0.154(3) 1 calc PR A 3 H12E H 0.2395 -0.0551 0.9329 0.201 Uiso 0.154(3) 1 calc PR A 3 H12F H 0.1541 -0.0603 0.8170 0.201 Uiso 0.154(3) 1 calc PR A 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01637(5) 0.02204(5) 0.01343(5) -0.00054(4) 0.00617(3) 0.00144(4) S1 0.0231(3) 0.0199(3) 0.0229(3) -0.0004(2) 0.0034(2) -0.0001(2) C2 0.0218(12) 0.0230(13) 0.0201(12) -0.0026(10) 0.0042(10) -0.0006(10) C3 0.0187(12) 0.0255(13) 0.0191(12) -0.0033(10) 0.0049(10) -0.0008(10) S4 0.0162(3) 0.0215(3) 0.0223(3) -0.0012(2) 0.0059(2) -0.0001(2) C5 0.0230(13) 0.0243(14) 0.0271(14) -0.0008(11) 0.0037(11) -0.0024(11) C6 0.0374(17) 0.0385(18) 0.0284(15) 0.0047(13) 0.0089(13) -0.0074(14) C7 0.0419(19) 0.0381(19) 0.043(2) 0.0089(16) 0.0128(16) -0.0084(15) C8 0.0342(17) 0.0246(15) 0.047(2) -0.0004(14) 0.0021(15) -0.0047(13) C9 0.0275(15) 0.0330(17) 0.0351(17) -0.0075(13) 0.0038(13) 0.0005(13) C10 0.0266(14) 0.0315(16) 0.0294(15) -0.0011(12) 0.0081(12) -0.0031(12) C11 0.0215(12) 0.0198(12) 0.0252(13) -0.0028(10) 0.0068(10) 0.0006(10) C12 0.0222(14) 0.0374(17) 0.0339(16) 0.0035(13) 0.0090(12) -0.0023(12) C13 0.0197(14) 0.047(2) 0.051(2) 0.0050(17) 0.0111(14) 0.0016(14) C14 0.0266(15) 0.0370(18) 0.0393(18) 0.0052(14) 0.0019(13) 0.0068(13) C15 0.0337(16) 0.0285(15) 0.0329(16) 0.0052(12) 0.0094(13) 0.0072(13) C16 0.0260(14) 0.0272(14) 0.0300(14) 0.0011(12) 0.0106(12) 0.0039(11) S21 0.0275(3) 0.0234(3) 0.0176(3) 0.0012(2) 0.0048(3) 0.0009(3) C22 0.0301(14) 0.0318(15) 0.0170(12) 0.0023(11) 0.0090(11) -0.0036(12) C23 0.0247(13) 0.0319(14) 0.0159(11) 0.0000(10) 0.0098(10) -0.0026(11) S24 0.0228(3) 0.0240(3) 0.0168(3) -0.0022(2) 0.0098(2) -0.0012(2) C25 0.0381(17) 0.0407(18) 0.0197(13) 0.0051(12) 0.0103(12) 0.0048(14) C26 0.051(2) 0.045(2) 0.0303(17) 0.0101(15) 0.0082(16) -0.0055(17) C27 0.053(2) 0.055(2) 0.038(2) 0.0190(18) 0.0120(18) -0.0007(19) C28 0.0376(19) 0.063(3) 0.0334(18) 0.0161(17) 0.0096(15) 0.0087(18) C29 0.0315(17) 0.070(3) 0.0227(15) 0.0022(16) 0.0073(13) 0.0033(17) C30 0.0327(16) 0.051(2) 0.0220(14) -0.0006(14) 0.0092(12) 0.0041(15) C31 0.0288(15) 0.0473(19) 0.0169(12) -0.0034(12) 0.0084(11) 0.0035(13) C32 0.0276(15) 0.053(2) 0.0294(15) -0.0187(15) 0.0098(13) -0.0021(14) C33 0.039(2) 0.081(3) 0.038(2) -0.033(2) 0.0072(16) 0.002(2) C34 0.074(3) 0.097(4) 0.0253(18) -0.020(2) 0.011(2) 0.022(3) C35 0.097(4) 0.106(5) 0.029(2) 0.020(2) 0.038(2) 0.036(3) C36 0.067(3) 0.067(3) 0.0280(17) 0.0122(17) 0.0289(18) 0.019(2) S41 0.0434(11) 0.0252(10) 0.0307(11) 0.0057(10) 0.0258(10) 0.0119(9) S44 0.0192(8) 0.0289(8) 0.0212(18) 0.0000(9) 0.0145(5) 0.0030(10) C42 0.020(3) 0.045(3) 0.016(3) -0.001(2) 0.008(2) 0.008(2) C43 0.0208(16) 0.038(3) 0.019(3) 0.003(2) 0.013(2) 0.008(2) C45 0.033(3) 0.038(3) 0.040(3) -0.006(2) 0.025(2) 0.008(2) C46 0.035(3) 0.145(8) 0.068(5) -0.050(5) 0.017(3) 0.020(4) C47 0.037(4) 0.150(10) 0.123(8) -0.073(7) 0.036(5) 0.010(4) C48 0.079(5) 0.052(4) 0.113(6) -0.018(4) 0.082(5) -0.001(4) C49 0.125(6) 0.059(6) 0.080(5) 0.021(4) 0.090(5) 0.034(4) C50 0.105(6) 0.055(6) 0.051(4) 0.012(4) 0.059(4) 0.040(5) C51 0.0245(19) 0.033(3) 0.017(3) -0.004(2) 0.015(2) 0.0044(19) C52 0.047(3) 0.039(2) 0.018(3) -0.0019(17) 0.014(3) -0.006(3) C53 0.077(5) 0.034(4) 0.028(3) -0.008(3) 0.032(4) -0.014(4) C54 0.047(3) 0.033(3) 0.057(4) -0.005(3) 0.041(3) 0.000(3) C55 0.028(3) 0.061(5) 0.096(7) 0.029(5) 0.033(4) 0.010(3) C56 0.024(2) 0.061(4) 0.062(5) 0.032(4) 0.015(3) 0.007(3) S41X 0.0434(11) 0.0252(10) 0.0307(11) 0.0057(10) 0.0258(10) 0.0119(9) S44X 0.0192(8) 0.0289(8) 0.0212(18) 0.0000(9) 0.0145(5) 0.0030(10) C42X 0.020(3) 0.045(3) 0.016(3) -0.001(2) 0.008(2) 0.008(2) C43X 0.0208(16) 0.038(3) 0.019(3) 0.003(2) 0.013(2) 0.008(2) C45X 0.033(3) 0.038(3) 0.040(3) -0.006(2) 0.025(2) 0.008(2) C46X 0.035(3) 0.145(8) 0.068(5) -0.050(5) 0.017(3) 0.020(4) C47X 0.037(4) 0.150(10) 0.123(8) -0.073(7) 0.036(5) 0.010(4) C48X 0.079(5) 0.052(4) 0.113(6) -0.018(4) 0.082(5) -0.001(4) C49X 0.125(6) 0.059(6) 0.080(5) 0.021(4) 0.090(5) 0.034(4) C50X 0.105(6) 0.055(6) 0.051(4) 0.012(4) 0.059(4) 0.040(5) C51X 0.0245(19) 0.033(3) 0.017(3) -0.004(2) 0.015(2) 0.0044(19) C52X 0.047(3) 0.039(2) 0.018(3) -0.0019(17) 0.014(3) -0.006(3) C53X 0.077(5) 0.034(4) 0.028(3) -0.008(3) 0.032(4) -0.014(4) C54X 0.047(3) 0.033(3) 0.057(4) -0.005(3) 0.041(3) 0.000(3) C55X 0.028(3) 0.061(5) 0.096(7) 0.029(5) 0.033(4) 0.010(3) C56X 0.024(2) 0.061(4) 0.062(5) 0.032(4) 0.015(3) 0.007(3) S41Y 0.0434(11) 0.0252(10) 0.0307(11) 0.0057(10) 0.0258(10) 0.0119(9) S44Y 0.0192(8) 0.0289(8) 0.0212(18) 0.0000(9) 0.0145(5) 0.0030(10) C42Y 0.020(3) 0.045(3) 0.016(3) -0.001(2) 0.008(2) 0.008(2) C43Y 0.0208(16) 0.038(3) 0.019(3) 0.003(2) 0.013(2) 0.008(2) C45Y 0.033(3) 0.038(3) 0.040(3) -0.006(2) 0.025(2) 0.008(2) C46Y 0.035(3) 0.145(8) 0.068(5) -0.050(5) 0.017(3) 0.020(4) C47Y 0.037(4) 0.150(10) 0.123(8) -0.073(7) 0.036(5) 0.010(4) C48Y 0.079(5) 0.052(4) 0.113(6) -0.018(4) 0.082(5) -0.001(4) C49Y 0.125(6) 0.059(6) 0.080(5) 0.021(4) 0.090(5) 0.034(4) C50Y 0.105(6) 0.055(6) 0.051(4) 0.012(4) 0.059(4) 0.040(5) C51Y 0.0245(19) 0.033(3) 0.017(3) -0.004(2) 0.015(2) 0.0044(19) C52Y 0.047(3) 0.039(2) 0.018(3) -0.0019(17) 0.014(3) -0.006(3) C53Y 0.077(5) 0.034(4) 0.028(3) -0.008(3) 0.032(4) -0.014(4) C54Y 0.047(3) 0.033(3) 0.057(4) -0.005(3) 0.041(3) 0.000(3) C55Y 0.028(3) 0.061(5) 0.096(7) 0.029(5) 0.033(4) 0.010(3) C56Y 0.024(2) 0.061(4) 0.062(5) 0.032(4) 0.015(3) 0.007(3) P60 0.0191(3) 0.0280(4) 0.0206(3) 0.0037(3) 0.0098(3) 0.0009(3) C61 0.0178(12) 0.0300(14) 0.0219(12) 0.0026(11) 0.0095(10) 0.0000(10) C62 0.0200(13) 0.0437(18) 0.0313(15) -0.0086(13) 0.0079(12) 0.0018(12) C63 0.0279(16) 0.043(2) 0.046(2) -0.0130(16) 0.0113(14) 0.0056(14) C64 0.0198(13) 0.047(2) 0.0386(17) 0.0044(15) 0.0117(13) 0.0072(13) C65 0.0199(13) 0.0429(18) 0.0332(16) 0.0055(14) 0.0051(12) -0.0055(13) C66 0.0236(13) 0.0293(15) 0.0308(15) 0.0026(12) 0.0078(12) -0.0028(11) C71 0.0258(13) 0.0338(16) 0.0230(13) -0.0004(11) 0.0139(11) 0.0003(11) C72 0.0297(16) 0.074(3) 0.0224(14) 0.0061(16) 0.0113(13) 0.0044(17) C73 0.053(2) 0.088(3) 0.0234(16) 0.0053(18) 0.0210(16) 0.000(2) C74 0.056(2) 0.055(2) 0.0358(18) -0.0035(16) 0.0335(18) -0.0059(18) C75 0.0357(17) 0.0395(18) 0.0456(19) -0.0030(14) 0.0294(16) -0.0024(14) C76 0.0272(14) 0.0336(15) 0.0318(15) 0.0031(12) 0.0168(12) 0.0020(12) C81 0.0212(12) 0.0292(14) 0.0204(12) 0.0055(10) 0.0098(10) 0.0037(10) C82 0.0336(15) 0.0303(15) 0.0255(14) 0.0088(12) 0.0131(12) 0.0062(12) C83 0.0406(18) 0.0433(19) 0.0209(14) 0.0090(13) 0.0104(13) 0.0120(15) C84 0.0283(15) 0.048(2) 0.0224(14) 0.0004(13) 0.0055(12) 0.0081(14) C85 0.0282(15) 0.0418(19) 0.0291(15) 0.0025(13) 0.0082(12) -0.0017(13) C86 0.0255(14) 0.0351(16) 0.0242(13) 0.0085(12) 0.0087(11) -0.0008(12) C91 0.0367(16) 0.0296(15) 0.0310(15) 0.0012(12) 0.0172(13) -0.0018(13) C92 0.119(5) 0.042(2) 0.103(4) -0.003(2) 0.095(4) 0.000(3) C93 0.177(7) 0.036(2) 0.125(5) -0.007(3) 0.126(5) -0.001(3) C94 0.101(4) 0.038(2) 0.050(2) -0.0040(17) 0.047(3) -0.013(2) C95 0.0409(19) 0.0391(19) 0.0410(19) 0.0089(15) 0.0141(16) -0.0059(15) C96 0.0321(16) 0.0326(17) 0.0457(19) 0.0090(14) 0.0177(15) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 S44X 2.312(6) . ? Re1 S1 2.3282(7) . ? Re1 S24 2.3311(6) . ? Re1 S21 2.3389(7) . ? Re1 S4 2.3428(7) . ? Re1 S41 2.353(2) . ? Re1 S41Y 2.360(7) . ? Re1 S44 2.360(2) . ? Re1 S44Y 2.369(7) . ? Re1 S41X 2.369(6) . ? S1 C2 1.746(3) . ? C2 C3 1.348(4) . ? C2 C5 1.483(4) . ? C3 C11 1.494(4) . ? C3 S4 1.750(3) . ? C5 C6 1.378(4) . ? C5 C10 1.402(4) . ? C6 C7 1.394(5) . ? C7 C8 1.383(5) . ? C8 C9 1.384(5) . ? C9 C10 1.384(4) . ? C11 C12 1.392(4) . ? C11 C16 1.395(4) . ? C12 C13 1.396(5) . ? C13 C14 1.381(5) . ? C14 C15 1.386(5) . ? C15 C16 1.393(4) . ? S21 C22 1.742(3) . ? C22 C23 1.354(4) . ? C22 C25 1.486(4) . ? C23 C31 1.491(4) . ? C23 S24 1.746(3) . ? C25 C30 1.394(5) . ? C25 C26 1.404(5) . ? C26 C27 1.389(5) . ? C27 C28 1.379(6) . ? C28 C29 1.384(6) . ? C29 C30 1.399(5) . ? C31 C36 1.392(5) . ? C31 C32 1.402(5) . ? C32 C33 1.392(5) . ? C33 C34 1.366(7) . ? C34 C35 1.375(8) . ? C35 C36 1.414(6) . ? S41 C42 1.761(5) . ? S44 C43 1.739(4) . ? C42 C43 1.344(6) . ? C42 C45 1.498(5) . ? C43 C51 1.482(5) . ? C45 C50 1.314(7) . ? C45 C46 1.357(8) . ? C46 C47 1.392(9) . ? C47 C48 1.373(12) . ? C48 C49 1.301(13) . ? C49 C50 1.388(7) . ? C51 C56 1.395(6) . ? C51 C52 1.396(7) . ? C52 C53 1.408(7) . ? C53 C54 1.382(10) . ? C54 C55 1.369(8) . ? C55 C56 1.375(7) . ? S41X C42X 1.768(6) . ? S44X C43X 1.742(5) . ? C42X C43X 1.342(7) . ? C42X C45X 1.499(6) . ? C43X C51X 1.484(6) . ? C45X C50X 1.314(8) . ? C45X C46X 1.356(9) . ? C46X C47X 1.394(10) . ? C47X C48X 1.376(13) . ? C48X C49X 1.303(14) . ? C49X C50X 1.390(8) . ? C51X C56X 1.394(7) . ? C51X C52X 1.400(9) . ? C52X C53X 1.409(8) . ? C53X C54X 1.382(10) . ? C54X C55X 1.369(9) . ? C55X C56X 1.376(8) . ? S41Y C42Y 1.770(6) . ? S44Y C43Y 1.750(5) . ? C42Y C43Y 1.345(7) . ? C42Y C45Y 1.499(6) . ? C43Y C51Y 1.484(6) . ? C45Y C50Y 1.315(8) . ? C45Y C46Y 1.356(9) . ? C46Y C47Y 1.392(10) . ? C47Y C48Y 1.375(13) . ? C48Y C49Y 1.301(14) . ? C49Y C50Y 1.388(8) . ? C51Y C56Y 1.394(7) . ? C51Y C52Y 1.401(8) . ? C52Y C53Y 1.409(8) . ? C53Y C54Y 1.383(11) . ? C54Y C55Y 1.370(9) . ? C55Y C56Y 1.377(8) . ? P60 C91 1.791(3) . ? P60 C61 1.799(3) . ? P60 C81 1.804(3) . ? P60 C71 1.808(3) . ? C61 C62 1.385(4) . ? C61 C66 1.406(4) . ? C62 C63 1.396(5) . ? C63 C64 1.388(5) . ? C64 C65 1.381(5) . ? C65 C66 1.381(4) . ? C71 C72 1.396(4) . ? C71 C76 1.398(4) . ? C72 C73 1.394(5) . ? C73 C74 1.385(6) . ? C74 C75 1.389(5) . ? C75 C76 1.394(4) . ? C81 C86 1.396(4) . ? C81 C82 1.398(4) . ? C82 C83 1.390(5) . ? C83 C84 1.375(5) . ? C84 C85 1.395(5) . ? C85 C86 1.388(4) . ? C91 C92 1.380(5) . ? C91 C96 1.402(4) . ? C92 C93 1.398(7) . ? C93 C94 1.393(7) . ? C94 C95 1.361(6) . ? C95 C96 1.383(5) . ? O100 C101 1.19(2) . ? C101 N102 1.37(2) . ? N102 C104 1.518(16) . ? N102 C103 1.540(13) . ? O110 C111 1.20(2) . ? C111 N112 1.37(2) . ? N112 C114 1.505(18) . ? N112 C113 1.535(16) . ? O120 C121 1.20(2) . ? C121 N122 1.37(2) . ? N122 C124 1.516(18) . ? N122 C123 1.532(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S44X Re1 S1 151.1(3) . . ? S44X Re1 S24 89.7(2) . . ? S1 Re1 S24 116.24(2) . . ? S44X Re1 S21 115.3(3) . . ? S1 Re1 S21 82.63(2) . . ? S24 Re1 S21 82.00(2) . . ? S44X Re1 S4 87.6(3) . . ? S1 Re1 S4 81.71(2) . . ? S24 Re1 S4 86.82(2) . . ? S21 Re1 S4 154.31(3) . . ? S44X Re1 S41 74.49(16) . . ? S1 Re1 S41 85.78(9) . . ? S24 Re1 S41 151.91(14) . . ? S21 Re1 S41 84.01(14) . . ? S4 Re1 S41 114.90(15) . . ? S1 Re1 S41Y 85.3(3) . . ? S24 Re1 S41Y 148.7(5) . . ? S21 Re1 S41Y 78.5(5) . . ? S4 Re1 S41Y 120.2(5) . . ? S1 Re1 S44 155.6(3) . . ? S24 Re1 S44 82.87(17) . . ? S21 Re1 S44 116.6(4) . . ? S4 Re1 S44 84.6(3) . . ? S41 Re1 S44 81.81(8) . . ? S41Y Re1 S44 84.3(3) . . ? S1 Re1 S44Y 153.3(13) . . ? S24 Re1 S44Y 86.3(7) . . ? S21 Re1 S44Y 116.3(15) . . ? S4 Re1 S44Y 85.8(14) . . ? S41 Re1 S44Y 78.2(3) . . ? S41Y Re1 S44Y 80.8(3) . . ? S44X Re1 S41X 82.50(19) . . ? S1 Re1 S41X 78.19(19) . . ? S24 Re1 S41X 155.7(3) . . ? S21 Re1 S41X 80.6(3) . . ? S4 Re1 S41X 115.7(4) . . ? S44 Re1 S41X 89.82(17) . . ? C2 S1 Re1 109.84(10) . . ? C3 C2 C5 127.0(3) . . ? C3 C2 S1 119.8(2) . . ? C5 C2 S1 113.1(2) . . ? C2 C3 C11 125.9(3) . . ? C2 C3 S4 118.6(2) . . ? C11 C3 S4 115.5(2) . . ? C3 S4 Re1 109.76(10) . . ? C6 C5 C10 119.3(3) . . ? C6 C5 C2 119.9(3) . . ? C10 C5 C2 120.4(3) . . ? C5 C6 C7 120.7(3) . . ? C8 C7 C6 119.5(3) . . ? C7 C8 C9 120.4(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C5 120.1(3) . . ? C12 C11 C16 118.5(3) . . ? C12 C11 C3 121.6(3) . . ? C16 C11 C3 119.9(3) . . ? C11 C12 C13 120.5(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 119.7(3) . . ? C14 C15 C16 120.0(3) . . ? C15 C16 C11 120.9(3) . . ? C22 S21 Re1 109.61(11) . . ? C23 C22 C25 126.7(3) . . ? C23 C22 S21 119.3(2) . . ? C25 C22 S21 114.0(2) . . ? C22 C23 C31 124.8(3) . . ? C22 C23 S24 119.4(2) . . ? C31 C23 S24 115.8(2) . . ? C23 S24 Re1 109.67(10) . . ? C30 C25 C26 119.0(3) . . ? C30 C25 C22 120.9(3) . . ? C26 C25 C22 120.1(3) . . ? C27 C26 C25 120.4(4) . . ? C28 C27 C26 120.3(4) . . ? C27 C28 C29 119.8(3) . . ? C28 C29 C30 120.7(3) . . ? C25 C30 C29 119.7(4) . . ? C36 C31 C32 119.2(3) . . ? C36 C31 C23 120.2(3) . . ? C32 C31 C23 120.6(3) . . ? C33 C32 C31 120.4(4) . . ? C34 C33 C32 120.1(5) . . ? C33 C34 C35 120.6(4) . . ? C34 C35 C36 120.5(4) . . ? C31 C36 C35 119.1(5) . . ? C42 S41 Re1 108.46(18) . . ? C43 S44 Re1 109.06(18) . . ? C43 C42 C45 122.8(4) . . ? C43 C42 S41 119.3(3) . . ? C45 C42 S41 117.6(4) . . ? C42 C43 C51 121.0(3) . . ? C42 C43 S44 120.0(3) . . ? C51 C43 S44 118.8(3) . . ? C50 C45 C46 114.2(5) . . ? C50 C45 C42 124.0(5) . . ? C46 C45 C42 120.7(5) . . ? C45 C46 C47 122.2(7) . . ? C48 C47 C46 119.1(8) . . ? C49 C48 C47 118.9(6) . . ? C48 C49 C50 119.4(9) . . ? C45 C50 C49 124.9(7) . . ? C56 C51 C52 119.2(4) . . ? C56 C51 C43 118.8(4) . . ? C52 C51 C43 121.5(5) . . ? C51 C52 C53 119.0(7) . . ? C54 C53 C52 119.9(6) . . ? C55 C54 C53 120.7(5) . . ? C54 C55 C56 120.0(6) . . ? C55 C56 C51 121.0(5) . . ? C42X S41X Re1 107.9(3) . . ? C43X S44X Re1 109.8(3) . . ? C43X C42X C45X 124.0(7) . . ? C43X C42X S41X 119.2(5) . . ? C45X C42X S41X 116.2(6) . . ? C42X C43X C51X 124.3(6) . . ? C42X C43X S44X 120.3(5) . . ? C51X C43X S44X 115.4(5) . . ? C50X C45X C46X 114.4(7) . . ? C50X C45X C42X 123.8(8) . . ? C46X C45X C42X 121.7(8) . . ? C45X C46X C47X 121.9(10) . . ? C48X C47X C46X 118.5(10) . . ? C49X C48X C47X 118.2(8) . . ? C48X C49X C50X 118.8(13) . . ? C45X C50X C49X 124.6(9) . . ? C56X C51X C52X 118.4(7) . . ? C56X C51X C43X 119.6(7) . . ? C52X C51X C43X 120.4(7) . . ? C51X C52X C53X 118.7(12) . . ? C54X C53X C52X 119.4(7) . . ? C55X C54X C53X 120.5(7) . . ? C54X C55X C56X 120.2(8) . . ? C55X C56X C51X 120.3(7) . . ? C42Y S41Y Re1 108.9(4) . . ? C43Y S44Y Re1 110.0(4) . . ? C43Y C42Y C45Y 125.5(7) . . ? C43Y C42Y S41Y 118.2(5) . . ? C45Y C42Y S41Y 116.3(6) . . ? C42Y C43Y C51Y 124.2(7) . . ? C42Y C43Y S44Y 118.8(6) . . ? C51Y C43Y S44Y 116.3(6) . . ? C50Y C45Y C46Y 114.0(7) . . ? C50Y C45Y C42Y 124.1(7) . . ? C46Y C45Y C42Y 121.5(8) . . ? C45Y C46Y C47Y 122.8(10) . . ? C48Y C47Y C46Y 119.0(10) . . ? C49Y C48Y C47Y 118.7(8) . . ? C48Y C49Y C50Y 119.6(10) . . ? C45Y C50Y C49Y 125.5(9) . . ? C56Y C51Y C52Y 117.7(7) . . ? C56Y C51Y C43Y 120.4(7) . . ? C52Y C51Y C43Y 121.0(7) . . ? C51Y C52Y C53Y 119.1(9) . . ? C54Y C53Y C52Y 119.9(8) . . ? C55Y C54Y C53Y 120.2(7) . . ? C54Y C55Y C56Y 120.1(8) . . ? C55Y C56Y C51Y 120.7(9) . . ? C91 P60 C61 108.06(15) . . ? C91 P60 C81 108.86(14) . . ? C61 P60 C81 112.69(13) . . ? C91 P60 C71 110.26(15) . . ? C61 P60 C71 107.61(13) . . ? C81 P60 C71 109.34(13) . . ? C62 C61 C66 119.7(3) . . ? C62 C61 P60 121.0(2) . . ? C66 C61 P60 119.1(2) . . ? C61 C62 C63 119.3(3) . . ? C64 C63 C62 120.6(3) . . ? C65 C64 C63 119.9(3) . . ? C64 C65 C66 120.1(3) . . ? C65 C66 C61 120.2(3) . . ? C72 C71 C76 119.9(3) . . ? C72 C71 P60 119.6(2) . . ? C76 C71 P60 120.5(2) . . ? C73 C72 C71 119.8(3) . . ? C74 C73 C72 120.3(4) . . ? C73 C74 C75 120.0(3) . . ? C74 C75 C76 120.4(3) . . ? C75 C76 C71 119.6(3) . . ? C86 C81 C82 119.6(3) . . ? C86 C81 P60 120.0(2) . . ? C82 C81 P60 120.4(2) . . ? C83 C82 C81 119.7(3) . . ? C84 C83 C82 120.7(3) . . ? C83 C84 C85 119.9(3) . . ? C86 C85 C84 120.1(3) . . ? C85 C86 C81 120.0(3) . . ? C92 C91 C96 119.2(3) . . ? C92 C91 P60 120.0(3) . . ? C96 C91 P60 120.7(3) . . ? C91 C92 C93 119.6(4) . . ? C94 C93 C92 119.7(5) . . ? C95 C94 C93 120.9(4) . . ? C94 C95 C96 119.3(4) . . ? C95 C96 C91 120.9(3) . . ? O100 C101 N102 110.1(17) . . ? C101 N102 C104 128.5(12) . . ? C101 N102 C103 111.3(11) . . ? C104 N102 C103 120.2(10) . . ? O110 C111 N112 112.2(19) . . ? C111 N112 C114 132.4(16) . . ? C111 N112 C113 109.2(13) . . ? C114 N112 C113 118.4(15) . . ? O120 C121 N122 111(2) . . ? C121 N122 C124 129.1(17) . . ? C121 N122 C123 111.6(15) . . ? C124 N122 C123 119.3(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.203 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.101 #===END data_6321 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H20 P)+, (C42 H30 Re S6)-, (C4 H9 N O)' _chemical_formula_sum 'C70 H59 N O P Re S6' _chemical_formula_weight 1339.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1730(10) _cell_length_b 31.364(3) _cell_length_c 14.7187(12) _cell_angle_alpha 90.00 _cell_angle_beta 116.539(4) _cell_angle_gamma 90.00 _cell_volume 5853.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque parallelepiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 2.364 _exptl_absorpt_correction_type 'Gaussian' _exptl_absorpt_correction_T_min 0.8712 _exptl_absorpt_correction_T_max 0.9114 _exptl_absorpt_process_details 'SADABS 2008/1, Bruker AXS (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '3634 images at 0.5 deg. stepwise rotation in omega and phi, 5 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 304224 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 32.50 _reflns_number_total 21162 _reflns_number_gt 19747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.1882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21162 _refine_ls_number_parameters 745 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.325 _refine_ls_restrained_S_all 1.327 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.701187(7) 0.861679(3) 0.750689(7) 0.01500(2) Uani 1 1 d . . . S1 S 0.60779(5) 0.80645(2) 0.78115(5) 0.02145(13) Uani 1 1 d . . . C2 C 0.5369(2) 0.82709(12) 0.8418(2) 0.0294(7) Uani 1 1 d . A . C3 C 0.5455(2) 0.86851(14) 0.8659(3) 0.0412(8) Uani 1 1 d . . . S4 S 0.63041(6) 0.90122(3) 0.84081(6) 0.03173(16) Uani 1 1 d . A . C5 C 0.4665(2) 0.79715(13) 0.8602(2) 0.0325(7) Uani 1 1 d . . . C6 C 0.5029(3) 0.77019(12) 0.9418(3) 0.0394(9) Uani 1 1 d . A . H6 H 0.5762 0.7690 0.9867 0.047 Uiso 1 1 calc R . . C7 C 0.4323(4) 0.74439(13) 0.9592(3) 0.0502(10) Uani 1 1 d . . . H7 H 0.4573 0.7257 1.0160 0.060 Uiso 1 1 calc R A . C8 C 0.3263(3) 0.74615(14) 0.8937(3) 0.0504(9) Uani 1 1 d . A . H8 H 0.2778 0.7294 0.9068 0.060 Uiso 1 1 calc R . . C9 C 0.2909(3) 0.7715(2) 0.8109(5) 0.0793(17) Uani 1 1 d . . . H9 H 0.2179 0.7718 0.7648 0.095 Uiso 1 1 calc R A . C10 C 0.3592(3) 0.7968(2) 0.7933(4) 0.0752(17) Uani 1 1 d . A . H10 H 0.3333 0.8143 0.7346 0.090 Uiso 1 1 calc R . . C11 C 0.4732(6) 0.8939(3) 0.8970(6) 0.0293(13) Uani 0.23 1 d PG A 1 C12 C 0.4713(9) 0.8789(4) 0.9851(7) 0.0444(15) Uani 0.23 1 d PG A 1 H12 H 0.5146 0.8555 1.0208 0.053 Uiso 0.23 1 calc PR A 1 C13 C 0.4062(12) 0.8982(5) 1.0210(9) 0.0457(16) Uani 0.23 1 d PG A 1 H13 H 0.4049 0.8880 1.0812 0.055 Uiso 0.23 1 calc PR A 1 C14 C 0.3429(11) 0.9324(5) 0.9688(12) 0.070(2) Uani 0.23 1 d PG A 1 H14 H 0.2984 0.9456 0.9933 0.084 Uiso 0.23 1 calc PR A 1 C15 C 0.3448(9) 0.9474(4) 0.8807(11) 0.0525(19) Uani 0.23 1 d PG A 1 H15 H 0.3016 0.9708 0.8450 0.063 Uiso 0.23 1 calc PR A 1 C16 C 0.4099(7) 0.9281(3) 0.8448(8) 0.0453(17) Uani 0.23 1 d PG A 1 H16 H 0.4112 0.9383 0.7846 0.054 Uiso 0.23 1 calc PR A 1 C11X C 0.4644(3) 0.88114(17) 0.9019(4) 0.0293(13) Uani 0.36 1 d PG A 2 C12X C 0.5015(5) 0.8860(2) 1.0061(4) 0.0444(15) Uani 0.36 1 d PG A 2 H12X H 0.5710 0.8771 1.0511 0.053 Uiso 0.36 1 calc PR A 2 C13X C 0.4370(7) 0.9039(3) 1.0445(5) 0.0457(16) Uani 0.36 1 d PG A 2 H13X H 0.4624 0.9072 1.1158 0.055 Uiso 0.36 1 calc PR A 2 C14X C 0.3354(6) 0.9169(3) 0.9788(7) 0.070(2) Uani 0.36 1 d PG A 2 H14X H 0.2913 0.9291 1.0050 0.084 Uiso 0.36 1 calc PR A 2 C15X C 0.2982(4) 0.9120(3) 0.8745(6) 0.0525(19) Uani 0.36 1 d PG A 2 H15X H 0.2288 0.9209 0.8296 0.063 Uiso 0.36 1 calc PR A 2 C16X C 0.3627(4) 0.8941(2) 0.8361(4) 0.0453(17) Uani 0.36 1 d PG A 2 H16X H 0.3373 0.8908 0.7649 0.054 Uiso 0.36 1 calc PR A 2 C11Y C 0.4932(7) 0.8994(3) 0.9173(7) 0.0293(13) Uani 0.22 1 d PG A 3 C12Y C 0.4628(10) 0.8776(4) 0.9821(10) 0.0444(15) Uani 0.22 1 d PG A 3 H12Y H 0.4822 0.8486 0.9983 0.053 Uiso 0.22 1 calc PR A 3 C13Y C 0.4039(13) 0.8982(5) 1.0232(12) 0.0457(16) Uani 0.22 1 d PG A 3 H13Y H 0.3831 0.8833 1.0675 0.055 Uiso 0.22 1 calc PR A 3 C14Y C 0.3754(13) 0.9407(5) 0.9995(13) 0.070(2) Uani 0.22 1 d PG A 3 H14Y H 0.3352 0.9548 1.0276 0.084 Uiso 0.22 1 calc PR A 3 C15Y C 0.4058(11) 0.9625(3) 0.9347(13) 0.0525(19) Uani 0.22 1 d PG A 3 H15Y H 0.3864 0.9915 0.9185 0.063 Uiso 0.22 1 calc PR A 3 C16Y C 0.4647(9) 0.9419(3) 0.8936(10) 0.0453(17) Uani 0.22 1 d PG A 3 H16Y H 0.4855 0.9568 0.8493 0.054 Uiso 0.22 1 calc PR A 3 C11Z C 0.5229(7) 0.8878(3) 0.9526(7) 0.0293(13) Uani 0.19 1 d PG A 4 C12Z C 0.5977(8) 0.9092(4) 1.0367(8) 0.0444(15) Uani 0.19 1 d PG A 4 H12Z H 0.6690 0.9103 1.0478 0.053 Uiso 0.19 1 calc PR A 4 C13Z C 0.5681(12) 0.9290(5) 1.1045(9) 0.0457(16) Uani 0.19 1 d PG A 4 H13Z H 0.6192 0.9436 1.1619 0.055 Uiso 0.19 1 calc PR A 4 C14Z C 0.4637(13) 0.9274(6) 1.0882(12) 0.070(2) Uani 0.19 1 d PG A 4 H14Z H 0.4434 0.9409 1.1346 0.084 Uiso 0.19 1 calc PR A 4 C15Z C 0.3889(10) 0.9060(6) 1.0041(13) 0.0525(19) Uani 0.19 1 d PG A 4 H15Z H 0.3176 0.9049 0.9930 0.063 Uiso 0.19 1 calc PR A 4 C16Z C 0.4185(7) 0.8862(4) 0.9363(10) 0.0453(17) Uani 0.19 1 d PG A 4 H16Z H 0.3674 0.8716 0.8789 0.054 Uiso 0.19 1 calc PR A 4 S21 S 0.85225(5) 0.82226(2) 0.85022(5) 0.01711(12) Uani 1 1 d . . . C22 C 0.95995(19) 0.85637(8) 0.90711(18) 0.0173(5) Uani 1 1 d . . . C23 C 0.94754(19) 0.89829(9) 0.88208(19) 0.0188(5) Uani 1 1 d . . . S24 S 0.82326(5) 0.91710(2) 0.79818(5) 0.01930(13) Uani 1 1 d . . . C25 C 1.05953(19) 0.83635(9) 0.98125(19) 0.0187(5) Uani 1 1 d . . . C26 C 1.1533(2) 0.84084(11) 0.9735(2) 0.0269(6) Uani 1 1 d . . . H26 H 1.1548 0.8573 0.9200 0.032 Uiso 1 1 calc R . . C27 C 1.2454(2) 0.82109(12) 1.0443(3) 0.0359(8) Uani 1 1 d . . . H27 H 1.3090 0.8241 1.0383 0.043 Uiso 1 1 calc R . . C28 C 1.2447(3) 0.79747(12) 1.1223(3) 0.0345(8) Uani 1 1 d . . . H28 H 1.3078 0.7844 1.1703 0.041 Uiso 1 1 calc R . . C29 C 1.1522(2) 0.79277(10) 1.1310(2) 0.0281(7) Uani 1 1 d . . . H29 H 1.1516 0.7765 1.1852 0.034 Uiso 1 1 calc R . . C30 C 1.0598(2) 0.81184(9) 1.0602(2) 0.0216(6) Uani 1 1 d . . . H30 H 0.9961 0.8081 1.0658 0.026 Uiso 1 1 calc R . . C31 C 1.0266(2) 0.93263(9) 0.9244(2) 0.0237(6) Uani 1 1 d . . . C32 C 1.0500(3) 0.95787(11) 0.8604(2) 0.0314(7) Uani 1 1 d . . . H32 H 1.0203 0.9513 0.7900 0.038 Uiso 1 1 calc R . . C33 C 1.1167(3) 0.99284(12) 0.8980(3) 0.0395(9) Uani 1 1 d . . . H33 H 1.1342 1.0098 0.8542 0.047 Uiso 1 1 calc R . . C34 C 1.1574(3) 1.00252(12) 1.0006(3) 0.0379(9) Uani 1 1 d . . . H34 H 1.2018 1.0267 1.0267 0.045 Uiso 1 1 calc R . . C35 C 1.1348(3) 0.97812(11) 1.0644(3) 0.0330(8) Uani 1 1 d . . . H35 H 1.1635 0.9852 1.1344 0.040 Uiso 1 1 calc R . . C36 C 1.0701(2) 0.94295(11) 1.0278(2) 0.0274(7) Uani 1 1 d . . . H36 H 1.0550 0.9257 1.0728 0.033 Uiso 1 1 calc R . . S41 S 0.68754(5) 0.81974(2) 0.61500(4) 0.01637(11) Uani 1 1 d . . . C42 C 0.61120(19) 0.84596(9) 0.50132(18) 0.0179(5) Uani 1 1 d . . . C43 C 0.5742(2) 0.88569(9) 0.50361(19) 0.0205(5) Uani 1 1 d . . . S44 S 0.60127(5) 0.90857(2) 0.62004(5) 0.02026(13) Uani 1 1 d . . . C45 C 0.5931(2) 0.82269(9) 0.40721(19) 0.0206(5) Uani 1 1 d . . . C46 C 0.5565(2) 0.78073(10) 0.3917(2) 0.0243(6) Uani 1 1 d . . . H46 H 0.5467 0.7663 0.4436 0.029 Uiso 1 1 calc R . . C47 C 0.5341(3) 0.75984(12) 0.3010(2) 0.0322(7) Uani 1 1 d . . . H47 H 0.5085 0.7314 0.2909 0.039 Uiso 1 1 calc R . . C48 C 0.5491(3) 0.78037(14) 0.2259(2) 0.0396(9) Uani 1 1 d . . . H48 H 0.5317 0.7664 0.1632 0.048 Uiso 1 1 calc R . . C49 C 0.5893(3) 0.82124(14) 0.2414(2) 0.0410(9) Uani 1 1 d . . . H49 H 0.6018 0.8349 0.1902 0.049 Uiso 1 1 calc R . . C50 C 0.6116(3) 0.84255(11) 0.3318(2) 0.0313(7) Uani 1 1 d . . . H50 H 0.6395 0.8707 0.3422 0.038 Uiso 1 1 calc R . . C51 C 0.5083(2) 0.91252(11) 0.4145(2) 0.0275(6) Uani 1 1 d . . . C52 C 0.5329(3) 0.95555(12) 0.4136(3) 0.0388(9) Uani 1 1 d . . . H52 H 0.5910 0.9676 0.4702 0.047 Uiso 1 1 calc R . . C53 C 0.4724(3) 0.98091(14) 0.3299(3) 0.0441(10) Uani 1 1 d . . . H53 H 0.4896 1.0102 0.3295 0.053 Uiso 1 1 calc R . . C54 C 0.3878(3) 0.96359(15) 0.2478(3) 0.0443(10) Uani 1 1 d . . . H54 H 0.3476 0.9808 0.1903 0.053 Uiso 1 1 calc R . . C55 C 0.3612(3) 0.92113(15) 0.2487(2) 0.0388(9) Uani 1 1 d . . . H55 H 0.3020 0.9095 0.1923 0.047 Uiso 1 1 calc R . . C56 C 0.4213(2) 0.89520(13) 0.3325(2) 0.0312(7) Uani 1 1 d . . . H56 H 0.4028 0.8661 0.3334 0.037 Uiso 1 1 calc R . . P60 P 0.57400(5) 0.62205(3) 0.89665(5) 0.02118(14) Uani 1 1 d . . . C61 C 0.69095(19) 0.65364(10) 0.9354(2) 0.0217(5) Uani 1 1 d . . . C62 C 0.6876(2) 0.69457(12) 0.8980(2) 0.0292(7) Uani 1 1 d . . . H62 H 0.6239 0.7053 0.8454 0.035 Uiso 1 1 calc R . . C63 C 0.7775(3) 0.71971(12) 0.9374(3) 0.0360(8) Uani 1 1 d . . . H63 H 0.7752 0.7477 0.9120 0.043 Uiso 1 1 calc R . . C64 C 0.8706(2) 0.70417(12) 1.0138(3) 0.0310(7) Uani 1 1 d . . . H64 H 0.9317 0.7217 1.0410 0.037 Uiso 1 1 calc R . . C65 C 0.8749(2) 0.66347(11) 1.0506(2) 0.0290(7) Uani 1 1 d . . . H65 H 0.9391 0.6529 1.1027 0.035 Uiso 1 1 calc R . . C66 C 0.7862(2) 0.63793(10) 1.0119(2) 0.0253(6) Uani 1 1 d . . . H66 H 0.7895 0.6098 1.0370 0.030 Uiso 1 1 calc R . . C71 C 0.4738(2) 0.63640(10) 0.77293(19) 0.0222(5) Uani 1 1 d . . . C72 C 0.4184(2) 0.67454(11) 0.7583(2) 0.0289(7) Uani 1 1 d . . . H72 H 0.4346 0.6935 0.8136 0.035 Uiso 1 1 calc R . . C73 C 0.3398(3) 0.68463(12) 0.6629(2) 0.0331(8) Uani 1 1 d . . . H73 H 0.3021 0.7107 0.6529 0.040 Uiso 1 1 calc R . . C74 C 0.3155(2) 0.65693(11) 0.5816(2) 0.0292(7) Uani 1 1 d . . . H74 H 0.2607 0.6638 0.5165 0.035 Uiso 1 1 calc R . . C75 C 0.3715(2) 0.61941(11) 0.5961(2) 0.0282(7) Uani 1 1 d . . . H75 H 0.3559 0.6008 0.5403 0.034 Uiso 1 1 calc R . . C76 C 0.4502(2) 0.60856(10) 0.6912(2) 0.0244(6) Uani 1 1 d . . . H76 H 0.4876 0.5825 0.7008 0.029 Uiso 1 1 calc R . . C81 C 0.5234(2) 0.63009(11) 0.9879(2) 0.0253(6) Uani 1 1 d . . . C82 C 0.5916(3) 0.64245(17) 1.0868(3) 0.0465(11) Uani 1 1 d . . . H82 H 0.6642 0.6472 1.1054 0.056 Uiso 1 1 calc R . . C83 C 0.5532(3) 0.64793(19) 1.1587(3) 0.0550(13) Uani 1 1 d . . . H83 H 0.5996 0.6566 1.2259 0.066 Uiso 1 1 calc R . . C84 C 0.4482(3) 0.64083(14) 1.1321(3) 0.0392(8) Uani 1 1 d . . . H84 H 0.4222 0.6441 1.1811 0.047 Uiso 1 1 calc R . . C85 C 0.3811(2) 0.62896(11) 1.0345(2) 0.0306(7) Uani 1 1 d . . . H85 H 0.3086 0.6244 1.0162 0.037 Uiso 1 1 calc R . . C86 C 0.4179(2) 0.62358(11) 0.9622(2) 0.0275(6) Uani 1 1 d . . . H86 H 0.3705 0.6154 0.8949 0.033 Uiso 1 1 calc R . . C91 C 0.6090(2) 0.56730(10) 0.8952(2) 0.0253(6) Uani 1 1 d . . . C92 C 0.5515(3) 0.53556(12) 0.9144(2) 0.0335(7) Uani 1 1 d . . . H92 H 0.4946 0.5428 0.9289 0.040 Uiso 1 1 calc R . . C93 C 0.5786(3) 0.49311(13) 0.9120(3) 0.0423(9) Uani 1 1 d . . . H93 H 0.5403 0.4712 0.9255 0.051 Uiso 1 1 calc R . . C94 C 0.6611(3) 0.48252(12) 0.8900(3) 0.0382(8) Uani 1 1 d . . . H94 H 0.6803 0.4535 0.8908 0.046 Uiso 1 1 calc R . . C95 C 0.7153(3) 0.51369(12) 0.8671(3) 0.0352(8) Uani 1 1 d . . . H95 H 0.7702 0.5061 0.8497 0.042 Uiso 1 1 calc R . . C96 C 0.6896(2) 0.55611(12) 0.8693(3) 0.0326(7) Uani 1 1 d . . . H96 H 0.7267 0.5777 0.8533 0.039 Uiso 1 1 calc R . . O101 O 0.80821(17) 0.96234(15) 0.3438(2) 0.143(3) Uani 0.78 1 d PDU B 1 C102 C 0.72753(14) 0.96599(10) 0.27044(17) 0.111(3) Uani 0.78 1 d PDU B 1 C103 C 0.6805(4) 0.93125(16) 0.1849(4) 0.113(4) Uani 0.78 1 d PDU B 1 H10A H 0.6126 0.9411 0.1318 0.170 Uiso 0.78 1 calc PR B 1 H10B H 0.6702 0.9046 0.2141 0.170 Uiso 0.78 1 calc PR B 1 H10C H 0.7293 0.9263 0.1554 0.170 Uiso 0.78 1 calc PR B 1 N104 N 0.6678(3) 1.00174(13) 0.2549(3) 0.130(3) Uani 0.78 1 d PDU B 1 C105 C 0.5615(4) 1.0029(3) 0.1531(4) 0.131(4) Uani 0.78 1 d PDU B 1 H10D H 0.5241 1.0296 0.1498 0.196 Uiso 0.78 1 calc PR B 1 H10E H 0.5172 0.9787 0.1516 0.196 Uiso 0.78 1 calc PR B 1 H10F H 0.5774 1.0012 0.0949 0.196 Uiso 0.78 1 calc PR B 1 C106 C 0.7110(6) 1.03295(18) 0.3325(4) 0.138(4) Uani 0.78 1 d PDU B 1 H10G H 0.6627 1.0573 0.3159 0.208 Uiso 0.78 1 calc PR B 1 H10H H 0.7792 1.0426 0.3380 0.208 Uiso 0.78 1 calc PR B 1 H10I H 0.7211 1.0206 0.3974 0.208 Uiso 0.78 1 calc PR B 1 O111 O 0.8015(2) 0.94570(10) 0.2510(5) 0.143(3) Uani 0.22 1 d PD C 2 C112 C 0.72185(18) 0.96232(8) 0.1963(3) 0.111(3) Uani 0.22 1 d PD C 2 C113 C 0.6694(6) 0.9591(3) 0.0772(4) 0.113(4) Uani 0.22 1 d PD C 2 H11A H 0.6023 0.9747 0.0485 0.170 Uiso 0.22 1 calc PR C 2 H11B H 0.6565 0.9291 0.0568 0.170 Uiso 0.22 1 calc PR C 2 H11C H 0.7166 0.9717 0.0520 0.170 Uiso 0.22 1 calc PR C 2 N114 N 0.6675(4) 0.98632(18) 0.2341(4) 0.130(3) Uani 0.22 1 d PD C 2 C115 C 0.5618(5) 1.0071(3) 0.1526(8) 0.131(4) Uani 0.22 1 d PD C 2 H11D H 0.5296 1.0240 0.1873 0.196 Uiso 0.22 1 calc PR C 2 H11E H 0.5130 0.9845 0.1129 0.196 Uiso 0.22 1 calc PR C 2 H11F H 0.5774 1.0255 0.1073 0.196 Uiso 0.22 1 calc PR C 2 C116 C 0.7148(9) 0.9893(4) 0.3416(5) 0.138(4) Uani 0.22 1 d PD C 2 H11G H 0.6709 1.0072 0.3621 0.208 Uiso 0.22 1 calc PR C 2 H11H H 0.7850 1.0022 0.3660 0.208 Uiso 0.22 1 calc PR C 2 H11I H 0.7213 0.9608 0.3708 0.208 Uiso 0.22 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01390(3) 0.01951(4) 0.01174(3) 0.00029(3) 0.00584(2) 0.00241(3) S1 0.0158(2) 0.0300(3) 0.0223(2) 0.0034(2) 0.01182(18) 0.0005(2) C2 0.0185(9) 0.0501(18) 0.0253(10) 0.0104(11) 0.0148(8) 0.0084(11) C3 0.0403(11) 0.057(2) 0.0460(13) 0.0130(13) 0.0366(10) 0.0201(14) S4 0.0457(3) 0.0305(4) 0.0310(3) 0.0001(3) 0.0280(2) 0.0093(3) C5 0.0273(10) 0.0499(19) 0.0292(11) 0.0009(12) 0.0206(9) -0.0003(12) C6 0.0527(18) 0.0363(17) 0.0264(13) -0.0061(12) 0.0152(13) -0.0167(15) C7 0.092(2) 0.0351(17) 0.0343(14) -0.0143(12) 0.0376(15) -0.0232(18) C8 0.0573(14) 0.047(2) 0.0763(18) -0.0093(16) 0.0562(12) -0.0107(16) C9 0.0313(15) 0.091(4) 0.121(4) 0.043(3) 0.0394(19) 0.001(2) C10 0.0257(15) 0.108(4) 0.087(3) 0.048(3) 0.0213(18) -0.001(2) C11 0.0390(18) 0.019(3) 0.047(2) 0.007(2) 0.0351(15) 0.005(2) C12 0.061(3) 0.053(3) 0.0289(19) -0.010(2) 0.0283(18) 0.010(3) C13 0.044(3) 0.068(4) 0.033(2) -0.015(2) 0.0247(19) -0.002(3) C14 0.094(3) 0.060(6) 0.104(4) 0.014(4) 0.088(2) 0.029(4) C15 0.038(2) 0.048(4) 0.094(4) -0.023(3) 0.049(2) -0.004(3) C16 0.038(2) 0.042(4) 0.073(4) -0.018(3) 0.040(2) -0.004(3) C11X 0.0390(18) 0.019(3) 0.047(2) 0.007(2) 0.0351(15) 0.005(2) C12X 0.061(3) 0.053(3) 0.0289(19) -0.010(2) 0.0283(18) 0.010(3) C13X 0.044(3) 0.068(4) 0.033(2) -0.015(2) 0.0247(19) -0.002(3) C14X 0.094(3) 0.060(6) 0.104(4) 0.014(4) 0.088(2) 0.029(4) C15X 0.038(2) 0.048(4) 0.094(4) -0.023(3) 0.049(2) -0.004(3) C16X 0.038(2) 0.042(4) 0.073(4) -0.018(3) 0.040(2) -0.004(3) C11Y 0.0390(18) 0.019(3) 0.047(2) 0.007(2) 0.0351(15) 0.005(2) C12Y 0.061(3) 0.053(3) 0.0289(19) -0.010(2) 0.0283(18) 0.010(3) C13Y 0.044(3) 0.068(4) 0.033(2) -0.015(2) 0.0247(19) -0.002(3) C14Y 0.094(3) 0.060(6) 0.104(4) 0.014(4) 0.088(2) 0.029(4) C15Y 0.038(2) 0.048(4) 0.094(4) -0.023(3) 0.049(2) -0.004(3) C16Y 0.038(2) 0.042(4) 0.073(4) -0.018(3) 0.040(2) -0.004(3) C11Z 0.0390(18) 0.019(3) 0.047(2) 0.007(2) 0.0351(15) 0.005(2) C12Z 0.061(3) 0.053(3) 0.0289(19) -0.010(2) 0.0283(18) 0.010(3) C13Z 0.044(3) 0.068(4) 0.033(2) -0.015(2) 0.0247(19) -0.002(3) C14Z 0.094(3) 0.060(6) 0.104(4) 0.014(4) 0.088(2) 0.029(4) C15Z 0.038(2) 0.048(4) 0.094(4) -0.023(3) 0.049(2) -0.004(3) C16Z 0.038(2) 0.042(4) 0.073(4) -0.018(3) 0.040(2) -0.004(3) S21 0.0139(2) 0.0177(3) 0.0178(2) 0.00069(19) 0.00530(18) 0.00049(19) C22 0.0153(8) 0.0197(11) 0.0149(9) 0.0003(8) 0.0048(7) -0.0001(8) C23 0.0139(9) 0.0222(11) 0.0151(9) 0.0009(8) 0.0019(7) 0.0027(8) S24 0.0186(2) 0.0178(3) 0.0161(2) 0.0010(2) 0.00293(19) 0.0018(2) C25 0.0143(9) 0.0192(11) 0.0184(10) 0.0003(8) 0.0036(8) 0.0012(8) C26 0.0174(10) 0.0317(14) 0.0301(12) 0.0068(11) 0.0092(9) 0.0002(10) C27 0.0176(11) 0.0421(18) 0.0449(17) 0.0077(14) 0.0112(11) 0.0049(12) C28 0.0217(12) 0.0344(16) 0.0360(16) 0.0051(13) 0.0026(12) 0.0091(12) C29 0.0315(13) 0.0241(13) 0.0247(12) 0.0050(10) 0.0090(10) 0.0064(11) C30 0.0194(9) 0.0220(12) 0.0211(10) 0.0014(9) 0.0070(8) 0.0024(9) C31 0.0185(10) 0.0216(12) 0.0225(11) 0.0037(9) 0.0014(9) 0.0008(9) C32 0.0284(13) 0.0353(16) 0.0244(12) 0.0062(11) 0.0063(10) -0.0054(12) C33 0.0341(15) 0.0338(16) 0.0414(17) 0.0118(14) 0.0088(13) -0.0077(13) C34 0.0263(14) 0.0315(16) 0.0403(18) 0.0003(14) 0.0010(13) 0.0017(13) C35 0.0253(13) 0.0307(15) 0.0340(15) -0.0062(12) 0.0052(11) 0.0022(12) C36 0.0228(11) 0.0300(14) 0.0252(12) -0.0046(11) 0.0070(9) -0.0006(11) S41 0.0179(2) 0.0186(3) 0.0137(2) -0.00001(18) 0.00807(17) 0.0017(2) C42 0.0162(8) 0.0242(11) 0.0120(8) 0.0019(8) 0.0050(7) 0.0008(8) C43 0.0204(9) 0.0257(12) 0.0140(9) 0.0019(8) 0.0064(8) 0.0034(9) S44 0.0219(2) 0.0206(3) 0.0145(2) 0.0006(2) 0.00486(19) 0.0050(2) C45 0.0197(9) 0.0277(12) 0.0136(9) 0.0000(8) 0.0069(7) 0.0033(9) C46 0.0217(10) 0.0318(14) 0.0193(10) -0.0058(10) 0.0091(8) -0.0009(10) C47 0.0291(12) 0.0403(17) 0.0250(12) -0.0123(12) 0.0101(10) -0.0017(12) C48 0.0452(16) 0.053(2) 0.0171(11) -0.0081(12) 0.0109(11) 0.0107(16) C49 0.0571(17) 0.052(2) 0.0214(11) 0.0069(12) 0.0244(11) 0.0138(16) C50 0.0429(13) 0.0344(16) 0.0226(11) 0.0035(10) 0.0200(10) 0.0057(13) C51 0.0278(12) 0.0343(15) 0.0173(10) 0.0050(10) 0.0073(9) 0.0095(11) C52 0.0443(18) 0.0340(17) 0.0269(14) 0.0072(13) 0.0058(13) 0.0074(15) C53 0.0499(19) 0.0425(19) 0.0348(16) 0.0125(14) 0.0142(14) 0.0160(16) C54 0.0382(15) 0.062(2) 0.0302(14) 0.0180(15) 0.0133(12) 0.0238(16) C55 0.0263(12) 0.066(2) 0.0208(12) 0.0047(14) 0.0073(10) 0.0131(15) C56 0.0222(11) 0.0498(19) 0.0182(11) 0.0008(12) 0.0060(9) 0.0083(12) P60 0.0157(2) 0.0312(3) 0.0172(2) -0.0056(2) 0.00781(19) -0.0022(2) C61 0.0150(8) 0.0317(13) 0.0191(9) -0.0028(9) 0.0083(7) -0.0005(9) C62 0.0199(10) 0.0421(17) 0.0242(11) 0.0062(11) 0.0086(9) -0.0025(11) C63 0.0265(12) 0.0393(17) 0.0404(15) 0.0102(13) 0.0134(11) -0.0057(12) C64 0.0199(10) 0.0383(16) 0.0339(14) -0.0022(12) 0.0112(10) -0.0059(11) C65 0.0154(10) 0.0386(16) 0.0268(12) -0.0053(12) 0.0041(9) 0.0002(11) C66 0.0159(9) 0.0283(13) 0.0262(12) -0.0042(10) 0.0045(9) -0.0001(10) C71 0.0177(9) 0.0323(13) 0.0177(9) -0.0074(9) 0.0088(7) -0.0036(10) C72 0.0236(11) 0.0378(16) 0.0217(11) -0.0102(11) 0.0067(9) 0.0036(11) C73 0.0288(13) 0.0387(17) 0.0268(13) -0.0032(12) 0.0081(11) 0.0066(13) C74 0.0261(12) 0.0382(16) 0.0200(11) -0.0023(11) 0.0073(9) -0.0037(12) C75 0.0311(12) 0.0358(15) 0.0171(10) -0.0075(10) 0.0102(9) -0.0077(12) C76 0.0253(10) 0.0297(13) 0.0190(10) -0.0076(9) 0.0108(8) -0.0037(10) C81 0.0199(9) 0.0372(15) 0.0208(10) -0.0075(10) 0.0110(8) -0.0056(10) C82 0.0281(12) 0.090(3) 0.0243(12) -0.0167(16) 0.0146(10) -0.0139(17) C83 0.0468(17) 0.101(4) 0.0239(12) -0.0172(17) 0.0214(12) -0.009(2) C84 0.0408(13) 0.055(2) 0.0337(12) -0.0024(14) 0.0277(10) -0.0001(15) C85 0.0258(10) 0.0367(16) 0.0383(13) 0.0010(11) 0.0224(9) 0.0024(11) C86 0.0216(10) 0.0353(15) 0.0278(11) -0.0067(11) 0.0129(9) -0.0026(11) C91 0.0241(10) 0.0310(14) 0.0215(10) -0.0046(10) 0.0108(9) -0.0033(10) C92 0.0408(13) 0.0375(17) 0.0287(12) -0.0026(11) 0.0214(10) -0.0051(13) C93 0.0637(19) 0.0361(18) 0.0368(14) -0.0020(13) 0.0311(13) -0.0082(16) C94 0.0544(18) 0.0339(17) 0.0256(13) -0.0029(12) 0.0174(12) 0.0041(15) C95 0.0343(14) 0.0390(17) 0.0325(14) -0.0085(13) 0.0151(11) 0.0024(13) C96 0.0303(12) 0.0351(16) 0.0369(14) -0.0085(12) 0.0191(10) -0.0044(12) O101 0.081(4) 0.127(5) 0.138(5) -0.033(4) -0.027(4) 0.028(4) C102 0.084(4) 0.100(4) 0.115(4) 0.004(4) 0.013(4) 0.024(3) C103 0.099(6) 0.092(6) 0.120(7) -0.011(5) 0.023(5) -0.007(5) N104 0.106(4) 0.115(4) 0.124(4) 0.006(4) 0.011(4) 0.015(4) C105 0.103(5) 0.137(6) 0.122(6) 0.044(5) 0.024(5) 0.027(5) C106 0.144(7) 0.100(6) 0.079(5) -0.018(5) -0.032(5) 0.003(6) O111 0.081(4) 0.127(5) 0.138(5) -0.033(4) -0.027(4) 0.028(4) C112 0.084(4) 0.100(4) 0.115(4) 0.004(4) 0.013(4) 0.024(3) C113 0.099(6) 0.092(6) 0.120(7) -0.011(5) 0.023(5) -0.007(5) N114 0.106(4) 0.115(4) 0.124(4) 0.006(4) 0.011(4) 0.015(4) C115 0.103(5) 0.137(6) 0.122(6) 0.044(5) 0.024(5) 0.027(5) C116 0.144(7) 0.100(6) 0.079(5) -0.018(5) -0.032(5) 0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 S41 2.3261(6) . ? Re1 S24 2.3287(7) . ? Re1 S44 2.3308(6) . ? Re1 S21 2.3357(6) . ? Re1 S1 2.3419(7) . ? Re1 S4 2.3438(8) . ? S1 C2 1.740(3) . ? C2 C3 1.338(6) . ? C2 C5 1.480(5) . ? C3 C11X 1.519(6) . ? C3 C11 1.521(9) . ? C3 C11Z 1.570(10) . ? C3 C11Y 1.601(10) . ? C3 S4 1.741(4) . ? C5 C6 1.368(5) . ? C5 C10 1.395(5) . ? C6 C7 1.397(6) . ? C7 C8 1.377(6) . ? C8 C9 1.349(7) . ? C9 C10 1.363(7) . ? C11 C12 1.3900 . ? C11 C16 1.3901 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C11X C12X 1.3900 . ? C11X C16X 1.3900 . ? C12X C13X 1.3900 . ? C13X C14X 1.3900 . ? C14X C15X 1.3900 . ? C15X C16X 1.3900 . ? C11Y C12Y 1.3900 . ? C11Y C16Y 1.3900 . ? C12Y C13Y 1.3900 . ? C13Y C14Y 1.3900 . ? C14Y C15Y 1.3900 . ? C15Y C16Y 1.3900 . ? C11Z C12Z 1.3900 . ? C11Z C16Z 1.3900 . ? C12Z C13Z 1.3900 . ? C13Z C14Z 1.3900 . ? C14Z C15Z 1.3900 . ? C15Z C16Z 1.3900 . ? S21 C22 1.742(3) . ? C22 C23 1.356(4) . ? C22 C25 1.483(3) . ? C23 C31 1.476(4) . ? C23 S24 1.741(2) . ? C25 C26 1.391(4) . ? C25 C30 1.392(4) . ? C26 C27 1.399(4) . ? C27 C28 1.369(6) . ? C28 C29 1.381(5) . ? C29 C30 1.393(4) . ? C31 C32 1.380(5) . ? C31 C36 1.401(4) . ? C32 C33 1.391(5) . ? C33 C34 1.389(6) . ? C34 C35 1.355(6) . ? C35 C36 1.381(5) . ? S41 C42 1.740(2) . ? C42 C43 1.358(4) . ? C42 C45 1.483(4) . ? C43 C51 1.485(4) . ? C43 S44 1.735(3) . ? C45 C46 1.396(4) . ? C45 C50 1.396(4) . ? C46 C47 1.391(4) . ? C47 C48 1.375(5) . ? C48 C49 1.380(6) . ? C49 C50 1.394(5) . ? C51 C56 1.394(4) . ? C51 C52 1.395(5) . ? C52 C53 1.393(5) . ? C53 C54 1.378(5) . ? C54 C55 1.386(6) . ? C55 C56 1.404(5) . ? P60 C91 1.790(3) . ? P60 C61 1.792(3) . ? P60 C71 1.795(3) . ? P60 C81 1.801(3) . ? C61 C62 1.390(5) . ? C61 C66 1.405(4) . ? C62 C63 1.386(5) . ? C63 C64 1.385(4) . ? C64 C65 1.377(5) . ? C65 C66 1.381(4) . ? C71 C72 1.394(4) . ? C71 C76 1.400(4) . ? C72 C73 1.384(4) . ? C73 C74 1.392(5) . ? C74 C75 1.382(5) . ? C75 C76 1.387(4) . ? C81 C86 1.385(4) . ? C81 C82 1.395(4) . ? C82 C83 1.400(6) . ? C83 C84 1.378(5) . ? C84 C85 1.373(5) . ? C85 C86 1.388(5) . ? C91 C92 1.393(5) . ? C91 C96 1.400(5) . ? C92 C93 1.390(6) . ? C93 C94 1.385(6) . ? C94 C95 1.376(6) . ? C95 C96 1.384(5) . ? O101 C102 1.176(3) . ? C102 N104 1.361(5) . ? C102 C103 1.571(5) . ? N104 C106 1.419(6) . ? N104 C105 1.581(6) . ? O111 C112 1.176(3) . ? C112 N114 1.361(6) . ? C112 C113 1.571(6) . ? N114 C116 1.419(7) . ? N114 C115 1.581(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S41 Re1 S24 116.45(3) . . ? S41 Re1 S44 82.05(2) . . ? S24 Re1 S44 82.69(2) . . ? S41 Re1 S21 86.59(2) . . ? S24 Re1 S21 81.78(2) . . ? S44 Re1 S21 154.18(3) . . ? S41 Re1 S1 84.77(3) . . ? S24 Re1 S1 154.47(2) . . ? S44 Re1 S1 115.95(2) . . ? S21 Re1 S1 85.78(2) . . ? S41 Re1 S4 153.22(3) . . ? S24 Re1 S4 83.32(3) . . ? S44 Re1 S4 82.95(3) . . ? S21 Re1 S4 115.42(3) . . ? S1 Re1 S4 82.04(3) . . ? C2 S1 Re1 109.17(13) . . ? C3 C2 C5 123.9(3) . . ? C3 C2 S1 119.5(3) . . ? C5 C2 S1 116.6(3) . . ? C2 C3 C11X 110.6(4) . . ? C2 C3 C11 126.4(4) . . ? C2 C3 C11Z 124.2(5) . . ? C2 C3 C11Y 134.9(5) . . ? C2 C3 S4 120.4(3) . . ? C11X C3 S4 128.5(3) . . ? C11 C3 S4 112.2(4) . . ? C11Z C3 S4 110.9(5) . . ? C11Y C3 S4 104.7(4) . . ? C3 S4 Re1 108.61(14) . . ? C6 C5 C10 118.6(4) . . ? C6 C5 C2 122.2(3) . . ? C10 C5 C2 119.2(4) . . ? C5 C6 C7 119.9(4) . . ? C8 C7 C6 119.7(4) . . ? C9 C8 C7 120.4(4) . . ? C8 C9 C10 120.3(4) . . ? C9 C10 C5 120.9(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 C3 113.7(5) . . ? C16 C11 C3 126.3(5) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C12X C11X C16X 120.0 . . ? C12X C11X C3 116.2(3) . . ? C16X C11X C3 123.0(3) . . ? C13X C12X C11X 120.0 . . ? C12X C13X C14X 120.0 . . ? C15X C14X C13X 120.0 . . ? C14X C15X C16X 120.0 . . ? C15X C16X C11X 120.0 . . ? C12Y C11Y C16Y 120.0 . . ? C12Y C11Y C3 112.2(6) . . ? C16Y C11Y C3 127.3(6) . . ? C11Y C12Y C13Y 120.0 . . ? C14Y C13Y C12Y 120.0 . . ? C13Y C14Y C15Y 120.0 . . ? C14Y C15Y C16Y 120.0 . . ? C15Y C16Y C11Y 120.0 . . ? C12Z C11Z C16Z 120.0 . . ? C12Z C11Z C3 124.0(6) . . ? C16Z C11Z C3 115.7(6) . . ? C11Z C12Z C13Z 120.0 . . ? C14Z C13Z C12Z 120.0 . . ? C13Z C14Z C15Z 120.0 . . ? C14Z C15Z C16Z 120.0 . . ? C15Z C16Z C11Z 120.0 . . ? C22 S21 Re1 109.71(9) . . ? C23 C22 C25 125.2(2) . . ? C23 C22 S21 119.06(18) . . ? C25 C22 S21 115.78(19) . . ? C22 C23 C31 127.7(2) . . ? C22 C23 S24 119.25(19) . . ? C31 C23 S24 112.9(2) . . ? C23 S24 Re1 109.91(10) . . ? C26 C25 C30 118.6(2) . . ? C26 C25 C22 121.8(3) . . ? C30 C25 C22 119.6(2) . . ? C25 C26 C27 120.1(3) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C29 119.8(3) . . ? C28 C29 C30 120.0(3) . . ? C25 C30 C29 120.8(3) . . ? C32 C31 C36 119.0(3) . . ? C32 C31 C23 119.9(3) . . ? C36 C31 C23 120.7(3) . . ? C31 C32 C33 120.6(3) . . ? C34 C33 C32 118.9(4) . . ? C35 C34 C33 121.2(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 120.1(3) . . ? C42 S41 Re1 109.62(10) . . ? C43 C42 C45 124.5(2) . . ? C43 C42 S41 119.4(2) . . ? C45 C42 S41 116.1(2) . . ? C42 C43 C51 126.6(3) . . ? C42 C43 S44 119.10(19) . . ? C51 C43 S44 114.3(2) . . ? C43 S44 Re1 109.79(10) . . ? C46 C45 C50 118.6(3) . . ? C46 C45 C42 120.9(3) . . ? C50 C45 C42 120.5(3) . . ? C47 C46 C45 120.7(3) . . ? C48 C47 C46 120.0(3) . . ? C47 C48 C49 120.2(3) . . ? C48 C49 C50 120.3(3) . . ? C49 C50 C45 120.1(3) . . ? C56 C51 C52 119.8(3) . . ? C56 C51 C43 120.5(3) . . ? C52 C51 C43 119.7(3) . . ? C53 C52 C51 120.2(3) . . ? C54 C53 C52 120.0(4) . . ? C53 C54 C55 120.3(3) . . ? C54 C55 C56 120.3(3) . . ? C51 C56 C55 119.3(4) . . ? C91 P60 C61 108.20(14) . . ? C91 P60 C71 109.03(14) . . ? C61 P60 C71 112.60(14) . . ? C91 P60 C81 110.38(16) . . ? C61 P60 C81 107.73(13) . . ? C71 P60 C81 108.89(13) . . ? C62 C61 C66 119.5(3) . . ? C62 C61 P60 121.5(2) . . ? C66 C61 P60 118.8(2) . . ? C63 C62 C61 119.8(3) . . ? C64 C63 C62 120.3(3) . . ? C65 C64 C63 120.3(3) . . ? C64 C65 C66 120.2(3) . . ? C65 C66 C61 119.9(3) . . ? C72 C71 C76 120.0(2) . . ? C72 C71 P60 120.5(2) . . ? C76 C71 P60 119.5(2) . . ? C73 C72 C71 119.7(3) . . ? C72 C73 C74 120.5(3) . . ? C75 C74 C73 119.6(3) . . ? C74 C75 C76 120.8(3) . . ? C75 C76 C71 119.3(3) . . ? C86 C81 C82 119.1(3) . . ? C86 C81 P60 121.1(2) . . ? C82 C81 P60 119.8(2) . . ? C81 C82 C83 120.0(3) . . ? C84 C83 C82 120.1(3) . . ? C85 C84 C83 119.7(3) . . ? C84 C85 C86 120.9(3) . . ? C81 C86 C85 120.1(3) . . ? C92 C91 C96 119.9(3) . . ? C92 C91 P60 119.5(3) . . ? C96 C91 P60 120.5(3) . . ? C93 C92 C91 119.1(4) . . ? C94 C93 C92 120.5(4) . . ? C95 C94 C93 120.6(4) . . ? C94 C95 C96 119.7(4) . . ? C95 C96 C91 120.2(3) . . ? O101 C102 N104 120.7(3) . . ? O101 C102 C103 124.0(4) . . ? N104 C102 C103 115.3(3) . . ? C102 N104 C106 114.9(4) . . ? C102 N104 C105 115.9(4) . . ? C106 N104 C105 129.2(5) . . ? O111 C112 N114 120.7(5) . . ? O111 C112 C113 124.6(5) . . ? N114 C112 C113 114.8(4) . . ? C112 N114 C116 114.9(6) . . ? C112 N114 C115 115.8(5) . . ? C116 N114 C115 129.3(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.634 _refine_diff_density_min -6.382 _refine_diff_density_rms 0.149 #===END data_6281 _audit_creation_date 2008-07-02 _audit_block_code WGT-SS-086-01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source dichloromethane/pentane _chemical_melting_point ? _chemical_formula_moiety '2(C24 H20 P), C12 N6 Re S6' _chemical_formula_sum 'C60 H40 N6 P2 Re S6' _chemical_formula_weight 1285.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-p 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.032(8) _cell_length_b 15.316(6) _cell_length_c 18.062(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5542(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9718 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 37.53 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.102 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method none _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 2.522 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7034 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (G. M. Sheldrick, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 We acknowledge the ANKA Angstroemquelle Karlsruhe for the provision of beamtime and we would like to thank Dr. Gernot Buth for assistance using beamline SCD/PX ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.8 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ANKA synchrotron source, Karlsruhe' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type 'Bruker-AXS Smart APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 18.18 _diffrn_reflns_number 197019 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 33.13 _reflns_number_total 7224 _reflns_number_gt 6030 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.6536P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7220 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C12 C 0.61289(15) 0.76912(19) 0.14918(19) 0.0273(6) Uani 1 1 d . . . C15 C 0.64948(16) 0.7978(2) 0.08530(19) 0.0306(7) Uani 1 1 d . . . C2 C 0.47728(18) 0.4572(2) 0.2223(2) 0.0350(7) Uani 1 1 d . . . C5 C 0.4538(2) 0.3782(3) 0.1893(2) 0.0463(9) Uani 1 1 d . . . N16 N 0.67844(17) 0.8192(2) 0.03364(19) 0.0425(7) Uani 1 1 d . . . N6 N 0.4346(2) 0.3147(2) 0.1622(3) 0.0658(11) Uani 1 1 d . . . Re1 Re 0.5000 0.667616(11) 0.2500 0.02746(6) Uani 1 2 d S . . S11 S 0.55171(4) 0.69127(5) 0.13391(4) 0.02862(16) Uani 1 1 d . . . S1 S 0.44567(4) 0.55427(5) 0.18675(5) 0.03123(17) Uani 1 1 d . . . C13 C 0.62649(16) 0.8009(2) 0.21801(19) 0.0282(6) Uani 1 1 d . . . C17 C 0.67947(18) 0.8620(2) 0.2286(2) 0.0332(7) Uani 1 1 d . . . N18 N 0.72183(19) 0.9115(2) 0.2359(2) 0.0507(9) Uani 1 1 d . . . S14 S 0.58273(4) 0.76564(5) 0.29508(5) 0.02825(16) Uani 1 1 d . . . P20 P 0.63337(4) 0.16515(5) 0.09565(4) 0.02461(16) Uani 1 1 d . . . C21 C 0.55829(15) 0.1013(2) 0.10379(18) 0.0269(6) Uani 1 1 d . . . C22 C 0.56157(17) 0.0221(2) 0.1425(2) 0.0338(7) Uani 1 1 d . . . H22 H 0.6017 0.0057 0.1668 0.041 Uiso 1 1 calc R . . C23 C 0.50659(17) -0.0322(2) 0.1453(2) 0.0385(8) Uani 1 1 d . . . H23 H 0.5089 -0.0859 0.1716 0.046 Uiso 1 1 calc R . . C24 C 0.44825(17) -0.0082(2) 0.1099(2) 0.0363(8) Uani 1 1 d . . . H24 H 0.4105 -0.0457 0.1117 0.044 Uiso 1 1 calc R . . C25 C 0.44454(18) 0.0695(2) 0.0722(2) 0.0388(8) Uani 1 1 d . . . H25 H 0.4042 0.0854 0.0481 0.047 Uiso 1 1 calc R . . C26 C 0.49940(17) 0.1250(2) 0.0689(2) 0.0348(7) Uani 1 1 d . . . H26 H 0.4965 0.1788 0.0430 0.042 Uiso 1 1 calc R . . C31 C 0.61732(16) 0.2797(2) 0.08306(18) 0.0277(6) Uani 1 1 d . . . C32 C 0.58300(19) 0.3097(2) 0.0207(2) 0.0356(8) Uani 1 1 d . . . H32 H 0.5676 0.2698 -0.0157 0.043 Uiso 1 1 calc R . . C33 C 0.5716(2) 0.3989(2) 0.0126(2) 0.0418(8) Uani 1 1 d . . . H33 H 0.5473 0.4198 -0.0290 0.050 Uiso 1 1 calc R . . C34 C 0.59546(19) 0.4572(2) 0.0645(2) 0.0406(9) Uani 1 1 d . . . H34 H 0.5879 0.5180 0.0583 0.049 Uiso 1 1 calc R . . C35 C 0.6301(2) 0.4277(2) 0.1251(2) 0.0386(8) Uani 1 1 d . . . H35 H 0.6467 0.4683 0.1604 0.046 Uiso 1 1 calc R . . C36 C 0.64129(17) 0.3386(2) 0.13537(19) 0.0320(7) Uani 1 1 d . . . H36 H 0.6650 0.3184 0.1776 0.038 Uiso 1 1 calc R . . C41 C 0.68127(16) 0.1502(2) 0.17848(17) 0.0266(6) Uani 1 1 d . . . C42 C 0.65066(19) 0.1614(2) 0.24748(19) 0.0343(7) Uani 1 1 d . . . H42 H 0.6042 0.1730 0.2506 0.041 Uiso 1 1 calc R . . C43 C 0.6890(2) 0.1553(2) 0.3112(2) 0.0377(8) Uani 1 1 d . . . H43 H 0.6689 0.1634 0.3584 0.045 Uiso 1 1 calc R . . C44 C 0.75658(19) 0.1374(2) 0.30607(19) 0.0361(8) Uani 1 1 d . . . H44 H 0.7827 0.1339 0.3498 0.043 Uiso 1 1 calc R . . C45 C 0.78632(18) 0.1246(2) 0.23826(19) 0.0331(7) Uani 1 1 d . . . H45 H 0.8325 0.1110 0.2355 0.040 Uiso 1 1 calc R . . C46 C 0.74902(16) 0.13151(19) 0.17405(18) 0.0267(6) Uani 1 1 d . . . H46 H 0.7696 0.1235 0.1272 0.032 Uiso 1 1 calc R . . C51 C 0.68279(16) 0.1254(2) 0.01997(17) 0.0271(6) Uani 1 1 d . . . C52 C 0.69660(17) 0.0360(2) 0.01741(19) 0.0317(7) Uani 1 1 d . . . H52 H 0.6759 -0.0024 0.0517 0.038 Uiso 1 1 calc R . . C53 C 0.74040(19) 0.0036(2) -0.03497(19) 0.0365(8) Uani 1 1 d . . . H53 H 0.7501 -0.0571 -0.0364 0.044 Uiso 1 1 calc R . . C54 C 0.7700(2) 0.0595(3) -0.0852(2) 0.0449(9) Uani 1 1 d . . . H54 H 0.8002 0.0372 -0.1211 0.054 Uiso 1 1 calc R . . C55 C 0.7560(2) 0.1476(3) -0.0833(2) 0.0500(10) Uani 1 1 d . . . H55 H 0.7761 0.1856 -0.1184 0.060 Uiso 1 1 calc R . . C56 C 0.7128(2) 0.1811(2) -0.0305(2) 0.0395(8) Uani 1 1 d . . . H56 H 0.7038 0.2420 -0.0289 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C12 0.0227(15) 0.0198(14) 0.0394(17) 0.0024(12) 0.0019(13) 0.0007(11) C15 0.0290(16) 0.0226(15) 0.0403(18) 0.0043(13) 0.0022(14) 0.0005(12) C2 0.0362(18) 0.0266(16) 0.0423(19) -0.0026(14) 0.0163(15) -0.0034(14) C5 0.048(2) 0.034(2) 0.057(2) -0.0016(17) 0.0151(19) -0.0068(17) N16 0.0427(18) 0.0349(16) 0.0499(19) 0.0080(14) 0.0118(15) 0.0001(14) N6 0.076(3) 0.042(2) 0.078(3) -0.0140(19) 0.015(2) -0.016(2) Re1 0.02375(9) 0.02713(10) 0.03150(10) 0.000 0.00321(7) 0.000 S11 0.0259(4) 0.0289(4) 0.0310(4) -0.0027(3) 0.0047(3) -0.0053(3) S1 0.0284(4) 0.0292(4) 0.0360(4) -0.0019(3) 0.0051(3) -0.0054(3) C13 0.0273(16) 0.0195(14) 0.0378(17) 0.0003(12) 0.0002(13) 0.0025(12) C17 0.0351(18) 0.0242(15) 0.0404(18) 0.0002(13) 0.0008(14) -0.0017(14) N18 0.055(2) 0.0419(19) 0.056(2) -0.0035(15) -0.0016(17) -0.0195(16) S14 0.0260(4) 0.0259(4) 0.0329(4) -0.0042(3) 0.0027(3) -0.0003(3) P20 0.0241(4) 0.0210(4) 0.0287(4) -0.0001(3) -0.0030(3) -0.0017(3) C21 0.0248(15) 0.0238(14) 0.0320(16) -0.0029(12) 0.0001(12) -0.0012(12) C22 0.0281(16) 0.0288(16) 0.0444(19) 0.0069(14) -0.0043(14) -0.0024(13) C23 0.0321(18) 0.0326(17) 0.051(2) 0.0074(16) -0.0003(16) -0.0048(14) C24 0.0264(16) 0.0385(19) 0.0441(19) -0.0015(15) 0.0017(14) -0.0060(15) C25 0.0256(16) 0.042(2) 0.049(2) 0.0011(16) -0.0049(15) 0.0020(15) C26 0.0298(16) 0.0321(17) 0.0426(19) 0.0051(14) -0.0054(15) -0.0001(14) C31 0.0285(16) 0.0213(14) 0.0332(16) -0.0002(12) 0.0015(13) 0.0004(12) C32 0.043(2) 0.0298(17) 0.0343(18) 0.0008(14) -0.0068(15) -0.0008(15) C33 0.049(2) 0.0354(19) 0.041(2) 0.0089(16) -0.0016(17) 0.0047(16) C34 0.046(2) 0.0236(16) 0.052(2) 0.0033(15) 0.0106(17) 0.0046(15) C35 0.049(2) 0.0252(16) 0.0411(19) -0.0058(14) 0.0059(16) -0.0050(15) C36 0.0345(18) 0.0279(16) 0.0336(17) -0.0003(13) 0.0007(14) -0.0035(13) C41 0.0283(16) 0.0222(14) 0.0295(15) -0.0009(12) -0.0028(12) -0.0037(12) C42 0.0322(17) 0.0365(18) 0.0344(17) 0.0006(14) 0.0009(14) -0.0036(14) C43 0.046(2) 0.0366(19) 0.0309(17) 0.0018(14) 0.0025(15) -0.0096(16) C44 0.048(2) 0.0284(17) 0.0321(17) 0.0063(13) -0.0107(15) -0.0099(15) C45 0.0308(17) 0.0265(16) 0.0420(19) 0.0012(13) -0.0082(14) -0.0011(13) C46 0.0265(15) 0.0230(14) 0.0307(15) -0.0022(12) -0.0025(12) -0.0032(12) C51 0.0274(16) 0.0266(15) 0.0273(15) -0.0026(12) -0.0030(12) -0.0031(12) C52 0.0371(18) 0.0254(15) 0.0326(16) 0.0007(13) 0.0024(14) -0.0039(13) C53 0.046(2) 0.0265(16) 0.0370(18) -0.0051(14) 0.0058(16) -0.0026(15) C54 0.057(2) 0.0380(19) 0.040(2) -0.0054(16) 0.0156(18) -0.0041(18) C55 0.071(3) 0.0341(19) 0.045(2) 0.0038(17) 0.022(2) -0.0092(19) C56 0.052(2) 0.0265(17) 0.0404(19) 0.0033(14) 0.0086(17) -0.0026(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C12 C13 1.363(5) . ? C12 C15 1.436(5) . ? C12 S11 1.732(3) . ? C15 N16 1.147(4) . ? C2 C2 1.352(8) 3_655 ? C2 C5 1.428(5) . ? C2 S1 1.739(4) . ? C5 N6 1.155(5) . ? Re1 S1 2.3459(10) . ? Re1 S1 2.3459(10) 3_655 ? Re1 S11 2.3667(11) . ? Re1 S11 2.3667(11) 3_655 ? Re1 S14 2.3797(10) . ? Re1 S14 2.3798(10) 3_655 ? C13 C17 1.428(5) . ? C13 S14 1.732(3) . ? C17 N18 1.145(5) . ? P20 C41 1.792(3) . ? P20 C51 1.794(3) . ? P20 C31 1.798(3) . ? P20 C21 1.800(3) . ? C21 C26 1.386(4) . ? C21 C22 1.401(4) . ? C22 C23 1.381(5) . ? C23 C24 1.382(5) . ? C24 C25 1.373(5) . ? C25 C26 1.391(5) . ? C31 C36 1.392(4) . ? C31 C32 1.397(5) . ? C32 C33 1.393(5) . ? C33 C34 1.380(5) . ? C34 C35 1.373(5) . ? C35 C36 1.395(5) . ? C41 C46 1.390(4) . ? C41 C42 1.399(5) . ? C42 C43 1.387(5) . ? C43 C44 1.385(5) . ? C44 C45 1.376(5) . ? C45 C46 1.384(4) . ? C51 C56 1.385(5) . ? C51 C52 1.397(4) . ? C52 C53 1.383(5) . ? C53 C54 1.382(5) . ? C54 C55 1.378(5) . ? C55 C56 1.387(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 C12 C15 121.5(3) . . ? C13 C12 S11 122.2(3) . . ? C15 C12 S11 116.3(3) . . ? N16 C15 C12 178.7(4) . . ? C2 C2 C5 122.0(2) 3_655 . ? C2 C2 S1 121.21(13) 3_655 . ? C5 C2 S1 116.7(3) . . ? N6 C5 C2 179.4(6) . . ? S1 Re1 S1 84.53(5) . 3_655 ? S1 Re1 S11 83.39(3) . . ? S1 Re1 S11 109.98(3) 3_655 . ? S1 Re1 S11 109.98(3) . 3_655 ? S1 Re1 S11 83.39(3) 3_655 3_655 ? S11 Re1 S11 162.39(4) . 3_655 ? S1 Re1 S14 163.04(3) . . ? S1 Re1 S14 88.69(4) 3_655 . ? S11 Re1 S14 84.36(3) . . ? S11 Re1 S14 84.56(3) 3_655 . ? S1 Re1 S14 88.69(4) . 3_655 ? S1 Re1 S14 163.04(3) 3_655 3_655 ? S11 Re1 S14 84.56(3) . 3_655 ? S11 Re1 S14 84.36(3) 3_655 3_655 ? S14 Re1 S14 101.77(5) . 3_655 ? C12 S11 Re1 105.90(12) . . ? C2 S1 Re1 106.50(13) . . ? C12 C13 C17 120.4(3) . . ? C12 C13 S14 121.4(2) . . ? C17 C13 S14 118.2(3) . . ? N18 C17 C13 178.8(4) . . ? C13 S14 Re1 105.93(12) . . ? C41 P20 C51 107.30(15) . . ? C41 P20 C31 109.01(15) . . ? C51 P20 C31 109.48(15) . . ? C41 P20 C21 108.05(15) . . ? C51 P20 C21 109.80(14) . . ? C31 P20 C21 113.03(15) . . ? C26 C21 C22 119.6(3) . . ? C26 C21 P20 122.1(3) . . ? C22 C21 P20 118.2(2) . . ? C23 C22 C21 120.2(3) . . ? C22 C23 C24 119.8(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 120.5(3) . . ? C21 C26 C25 119.6(3) . . ? C36 C31 C32 120.2(3) . . ? C36 C31 P20 119.0(3) . . ? C32 C31 P20 120.7(2) . . ? C33 C32 C31 119.3(3) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 120.3(3) . . ? C34 C35 C36 120.6(3) . . ? C31 C36 C35 119.3(3) . . ? C46 C41 C42 120.3(3) . . ? C46 C41 P20 120.1(2) . . ? C42 C41 P20 119.6(3) . . ? C43 C42 C41 119.3(3) . . ? C44 C43 C42 119.9(3) . . ? C45 C44 C43 120.8(3) . . ? C44 C45 C46 120.1(3) . . ? C45 C46 C41 119.7(3) . . ? C56 C51 C52 119.7(3) . . ? C56 C51 P20 122.1(3) . . ? C52 C51 P20 117.8(2) . . ? C53 C52 C51 120.0(3) . . ? C54 C53 C52 120.0(3) . . ? C55 C54 C53 120.2(4) . . ? C54 C55 C56 120.4(3) . . ? C51 C56 C55 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 33.13 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.652 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.101 #===END