Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Jitendra K. Bera' ; Department of Chemistry Texas A&M University P.O. Box 30012 College Station, TX 77842-3012 ; 'Bradley W. Smucker' ; Department of Chemistry Texas A&M University P.O. Box 30012 College Station, TX 77842-3012 ; 'Richard A. Walton' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Kim R. Dunbar' ; Department of Chemistry Texas A&M University P.O. Box 30012 College Station, TX 77842-3012 ; _publ_requested_journal 'Chemical Communications' # 1. SUBMISSION DETAILS _publ_contact_author_name 'Kim R. Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A&M University P.O. Box 30012 College Station, TX 77842-3012 USA ; _publ_contact_author_email 'dunbar@mail.chem.tamu.edu' _publ_contact_author_fax '1(979)8457177' _publ_contact_author_phone '1(979)8455235' _publ_requested_journal ? _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; A New "Hybrid" Molecular Square Composed of Alternating Multiply-Bonded Dinuclear and Mononuclear Corners ; data_Compound_1 _database_code_CSD 166127 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C66 H64 Cl2 N2 O6 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1548.46 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 28.2880(16) _cell_length_b 10.1028(3) _cell_length_c 23.7579(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.1577(18) _cell_angle_gamma 90.00 _cell_volume 6195.1(10) _cell_measurement_reflns_used 22927 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.66 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.198 _cell_measurement_temperature 295 _exptl_crystal_F_000 3064 # 6. DATA COLLECTION _diffrn_ambient_temperature 295 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.2680 _exptl_absorpt_correction_T_max 0.4319 _diffrn_reflns_number 22927 _reflns_number_total 7023 _reflns_number_gt 5803 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_max 27 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.120 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6642 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 2.48 _refine_diff_density_min -3.16 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re 0.003335(9) 0.22926(2) 0.202784(10) 0.03278(10) Uani ? Cl 0.00368(8) 0.28458(17) 0.09965(8) 0.0525(7) Uani ? P(1) 0.07899(6) 0.09287(16) 0.23256(7) 0.0357(6) Uani ? P(2) -0.05417(6) 0.04731(15) 0.15695(7) 0.0345(5) Uani ? O(10) 0.05207(18) 0.4040(4) 0.23296(19) 0.0420(15) Uani ? O(11) -0.05731(17) 0.3744(4) 0.17162(18) 0.0409(15) Uani ? O(901) 0.2121(3) 0.3742(9) 0.0614(4) 0.112(4) Uani ? N(14) 0.1984(3) 0.7040(7) 0.3684(4) 0.068(3) Uani ? C(10) 0.0712(2) 0.4301(6) 0.2905(3) 0.040(2) Uani ? C(11) 0.1137(3) 0.5298(6) 0.3162(3) 0.044(2) Uani ? C(12) 0.1350(3) 0.5916(7) 0.2805(4) 0.058(3) Uani ? C(13) 0.1761(3) 0.6780(8) 0.3081(4) 0.069(4) Uani ? C(15) 0.1777(3) 0.6421(8) 0.4034(4) 0.060(3) Uani ? C(16) 0.1364(3) 0.5569(7) 0.3790(3) 0.049(2) Uani ? C(1B) -0.0754(2) -0.0300(6) 0.2128(3) 0.036(2) Uani ? C(111) 0.1433(3) 0.1720(7) 0.2695(3) 0.046(2) Uani ? C(112) 0.1836(3) 0.1195(9) 0.3203(4) 0.066(3) Uani ? C(113) 0.2325(3) 0.1763(13) 0.3411(5) 0.091(4) Uani ? C(114) 0.2413(4) 0.2832(12) 0.3122(6) 0.093(5) Uani ? C(115) 0.2012(4) 0.3369(10) 0.2608(5) 0.081(4) Uani ? C(116) 0.1522(3) 0.2824(7) 0.2404(4) 0.061(3) Uani ? C(121) 0.0928(2) -0.0054(7) 0.1753(3) 0.039(2) Uani ? C(122) 0.1003(3) 0.0586(8) 0.1277(3) 0.051(3) Uani ? C(123) 0.1139(3) -0.0153(9) 0.0869(3) 0.060(3) Uani ? C(124) 0.1181(3) -0.1508(9) 0.0920(3) 0.064(3) Uani ? C(125) 0.1097(4) -0.2134(8) 0.1381(4) 0.064(3) Uani ? C(126) 0.0966(3) -0.1410(7) 0.1789(3) 0.051(3) Uani ? C(211) -0.0338(2) -0.0982(6) 0.1262(3) 0.037(2) Uani ? C(212) -0.0262(3) -0.0795(7) 0.0723(3) 0.046(2) Uani ? C(213) -0.0158(3) -0.1835(8) 0.0422(3) 0.054(3) Uani ? C(214) -0.0109(3) -0.3111(8) 0.0664(4) 0.062(3) Uani ? C(215) -0.0172(3) -0.3328(7) 0.1203(4) 0.056(3) Uani ? C(216) -0.0286(3) -0.2226(7) 0.1496(4) 0.049(3) Uani ? C(221) -0.1157(2) 0.0771(6) 0.0894(3) 0.038(2) Uani ? C(222) -0.1478(3) -0.0292(8) 0.0622(3) 0.054(3) Uani ? C(223) -0.1945(3) -0.0102(9) 0.0120(3) 0.067(3) Uani ? C(224) -0.2093(3) 0.1151(9) -0.0118(3) 0.065(3) Uani ? C(225) -0.1776(3) 0.2207(8) 0.0150(4) 0.060(3) Uani ? C(226) -0.1309(3) 0.2028(7) 0.0648(3) 0.050(2) Uani ? C(901) 0.1687(6) 0.3335(15) 0.0726(9) 0.149(9) Uani ? C(902) 0.1330(5) 0.4365(15) 0.0671(7) 0.143(8) Uani ? H(12) 0.1220 0.5755 0.2383 0.0750 Uiso calc H(13) 0.1890 0.7210 0.2828 0.0890 Uiso calc H(15) 0.1921 0.6577 0.4457 0.0790 Uiso calc H(16) 0.1234 0.5167 0.4050 0.0640 Uiso calc H(112) 0.1779 0.0465 0.3406 0.0850 Uiso calc H(113) 0.2596 0.1405 0.3752 0.1190 Uiso calc H(114) 0.2741 0.3207 0.3268 0.1210 Uiso calc H(115) 0.2074 0.4090 0.2404 0.1050 Uiso calc H(116) 0.1251 0.3199 0.2070 0.0790 Uiso calc H(122) 0.0963 0.1499 0.1231 0.0670 Uiso calc H(123) 0.1202 0.0276 0.0559 0.0790 Uiso calc H(124) 0.1267 -0.1996 0.0643 0.0830 Uiso calc H(125) 0.1128 -0.3049 0.1420 0.0830 Uiso calc H(126) 0.0902 -0.1849 0.2095 0.0670 Uiso calc H(1B1) -0.1091 -0.0703 0.1911 0.0470 Uiso calc H(1B2) -0.0512 -0.0992 0.2351 0.0470 Uiso calc H(212) -0.0281 0.0056 0.0566 0.0600 Uiso calc H(213) -0.0120 -0.1691 0.0056 0.0700 Uiso calc H(214) -0.0034 -0.3816 0.0462 0.0810 Uiso calc H(215) -0.0140 -0.4174 0.1370 0.0730 Uiso calc H(216) -0.0327 -0.2361 0.1861 0.0640 Uiso calc H(222) -0.1379 -0.1141 0.0778 0.0700 Uiso calc H(223) -0.2159 -0.0821 -0.0058 0.0860 Uiso calc H(224) -0.2406 0.1278 -0.0457 0.0840 Uiso calc H(225) -0.1878 0.3054 -0.0006 0.0780 Uiso calc H(226) -0.1094 0.2750 0.0820 0.0640 Uiso calc H(901) 0.2334 0.3141 0.0705 0.1460 Uiso calc H(90A) 0.1810 0.2966 0.1138 0.1930 Uiso calc H(90B) 0.1508 0.2637 0.0437 0.1930 Uiso calc H(90C) 0.1481 0.4969 0.1010 0.1860 Uiso calc H(90D) 0.1019 0.3993 0.0677 0.1860 Uiso calc H(90E) 0.1247 0.4830 0.0290 0.1860 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re 0.04111(17) 0.03668(18) 0.02359(15) -0.00001(9) 0.01633(11) 0.00130(8) Cl 0.0720(12) 0.0607(11) 0.0345(9) 0.0043(8) 0.0318(9) 0.0074(7) P(1) 0.0441(10) 0.0408(9) 0.0266(8) 0.0012(6) 0.0189(7) 0.0010(6) P(2) 0.0423(9) 0.0402(9) 0.0232(7) -0.0026(6) 0.0157(7) -0.0002(6) O(10) 0.057(3) 0.039(2) 0.035(2) -0.0058(19) 0.024(2) 0.0021(17) O(11) 0.052(3) 0.040(2) 0.030(2) 0.0088(19) 0.016(2) 0.0007(17) O(901) 0.090(6) 0.133(7) 0.125(7) 0.020(5) 0.056(5) 0.029(6) N(14) 0.055(4) 0.071(5) 0.070(5) -0.009(3) 0.016(4) 0.000(4) C(10) 0.043(4) 0.032(3) 0.044(4) -0.001(2) 0.016(3) -0.005(3) C(11) 0.046(4) 0.040(4) 0.045(4) -0.001(3) 0.018(3) 0.001(3) C(12) 0.062(5) 0.051(4) 0.057(5) -0.012(3) 0.021(4) -0.001(3) C(13) 0.073(6) 0.062(5) 0.076(6) -0.013(4) 0.036(5) 0.008(4) C(15) 0.059(5) 0.056(5) 0.055(5) -0.005(3) 0.012(4) -0.010(4) C(16) 0.053(4) 0.047(4) 0.046(4) -0.001(3) 0.019(3) -0.003(3) C(1B) 0.046(4) 0.039(3) 0.027(3) -0.003(2) 0.018(3) 0.000(2) C(111) 0.047(4) 0.053(4) 0.041(4) 0.004(3) 0.021(3) -0.008(3) C(112) 0.054(5) 0.093(6) 0.047(4) -0.004(4) 0.017(4) -0.001(4) C(113) 0.044(5) 0.151(10) 0.067(6) -0.001(6) 0.010(5) -0.021(6) C(114) 0.050(6) 0.125(10) 0.106(9) -0.022(6) 0.034(6) -0.030(7) C(115) 0.063(6) 0.087(7) 0.099(8) -0.014(5) 0.040(6) -0.011(5) C(116) 0.056(5) 0.055(5) 0.076(6) -0.012(3) 0.031(4) -0.008(4) C(121) 0.038(3) 0.061(4) 0.021(3) 0.008(3) 0.014(3) -0.001(3) C(122) 0.059(5) 0.065(5) 0.040(4) 0.002(3) 0.030(3) 0.002(3) C(123) 0.065(5) 0.087(6) 0.044(4) -0.003(4) 0.038(4) 0.000(4) C(124) 0.062(5) 0.096(7) 0.043(4) 0.011(4) 0.031(4) -0.016(4) C(125) 0.083(6) 0.061(5) 0.058(5) 0.012(4) 0.040(5) -0.005(4) C(126) 0.068(5) 0.058(4) 0.033(4) 0.009(3) 0.027(3) 0.000(3) C(211) 0.047(4) 0.037(3) 0.032(3) -0.001(2) 0.020(3) -0.006(2) C(212) 0.060(4) 0.056(4) 0.033(3) 0.001(3) 0.029(3) 0.000(3) C(213) 0.067(5) 0.064(5) 0.040(4) -0.003(4) 0.031(4) -0.012(3) C(214) 0.067(5) 0.064(5) 0.063(5) 0.000(4) 0.034(4) -0.022(4) C(215) 0.072(5) 0.044(4) 0.063(5) -0.002(3) 0.039(4) -0.004(3) C(216) 0.057(5) 0.048(4) 0.048(4) -0.002(3) 0.027(4) -0.006(3) C(221) 0.039(3) 0.051(4) 0.025(3) -0.003(3) 0.013(3) 0.000(2) C(222) 0.055(4) 0.066(5) 0.037(4) -0.007(3) 0.016(3) -0.002(3) C(223) 0.044(4) 0.100(7) 0.044(4) -0.015(4) 0.006(3) -0.007(4) C(224) 0.047(5) 0.103(7) 0.037(4) 0.006(4) 0.010(4) 0.002(4) C(225) 0.059(5) 0.074(6) 0.042(4) 0.014(4) 0.016(4) 0.006(3) C(226) 0.054(4) 0.058(4) 0.033(4) 0.007(3) 0.014(3) 0.002(3) C(901) 0.141(13) 0.126(11) 0.232(18) 0.022(10) 0.130(13) 0.060(12) C(902) 0.110(11) 0.144(13) 0.179(15) 0.012(9) 0.063(10) -0.009(11) # 10. MOLECULAR GEOMETRY _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_publ_flag Re O(11) 2.145(4) ? Re O(10) 2.173(4) ? Re Re 2.3271(4) ? Re P(1) 2.3958(16) ? Re P(2) 2.4001(16) ? Re Cl 2.5170(16) ? P(1) C(1B) 1.828(6) ? P(1) C(111) 1.847(7) ? P(1) C(121) 1.851(6) ? P(2) C(211) 1.836(6) ? P(2) C(1B) 1.840(6) ? P(2) C(221) 1.846(6) ? O(10) C(10) 1.275(7) ? O(11) C(10) 1.254(7) ? O(901) C(901) 1.419(13) ? N(14) C(13) 1.334(11) ? N(14) C(15) 1.350(10) ? C(10) O(11) 1.254(7) ? C(10) C(11) 1.492(8) ? C(11) C(12) 1.375(9) ? C(11) C(16) 1.390(9) ? C(12) C(13) 1.385(11) ? C(15) C(16) 1.375(10) ? C(1B) P(1) 1.828(6) ? C(111) C(112) 1.382(10) ? C(111) C(116) 1.388(10) ? C(112) C(113) 1.389(12) ? C(113) C(114) 1.355(15) ? C(114) C(115) 1.392(15) ? C(115) C(116) 1.382(11) ? C(121) C(126) 1.374(10) ? C(121) C(122) 1.392(9) ? C(122) C(123) 1.397(9) ? C(123) C(124) 1.376(12) ? C(124) C(125) 1.369(11) ? C(125) C(126) 1.379(9) ? C(211) C(216) 1.358(9) ? C(211) C(212) 1.396(8) ? C(212) C(213) 1.370(9) ? C(213) C(214) 1.395(11) ? C(214) C(215) 1.381(11) ? C(215) C(216) 1.419(10) ? C(221) C(222) 1.384(9) ? C(221) C(226) 1.390(9) ? C(222) C(223) 1.384(10) ? C(223) C(224) 1.380(11) ? C(224) C(225) 1.371(11) ? C(225) C(226) 1.379(10) ? C(901) C(902) 1.420(16) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(11) Re O(10) 82.43(17) ? O(11) Re Re 87.93(11) ? O(10) Re Re 88.44(11) ? O(11) Re P(1) 170.61(12) ? O(10) Re P(1) 90.02(12) ? Re Re P(1) 97.49(4) ? O(11) Re P(2) 93.97(13) ? O(10) Re P(2) 172.98(11) ? Re Re P(2) 97.48(4) ? P(1) Re P(2) 92.93(5) ? O(11) Re Cl 80.41(12) ? O(10) Re Cl 83.46(11) ? Re Re Cl 166.56(4) ? P(1) Re Cl 93.23(6) ? P(2) Re Cl 90.02(6) ? C(1B) P(1) C(111) 106.7(3) ? C(1B) P(1) C(121) 104.3(3) ? C(111) P(1) C(121) 96.7(3) ? C(1B) P(1) Re 107.3(2) ? C(111) P(1) Re 118.6(2) ? C(121) P(1) Re 121.5(2) ? C(211) P(2) C(1B) 101.2(3) ? C(211) P(2) C(221) 97.0(3) ? C(1B) P(2) C(221) 103.1(3) ? C(211) P(2) Re 122.0(2) ? C(1B) P(2) Re 111.0(2) ? C(221) P(2) Re 119.5(2) ? C(10) O(10) Re 117.1(4) ? C(10) O(11) Re 120.1(4) ? C(13) N(14) C(15) 115.9(7) ? O(11) C(10) O(10) 123.8(6) ? O(11) C(10) C(11) 116.4(6) ? O(10) C(10) C(11) 119.8(6) ? C(12) C(11) C(16) 116.5(7) ? C(12) C(11) C(10) 122.5(6) ? C(16) C(11) C(10) 120.9(6) ? C(11) C(12) C(13) 119.3(7) ? N(14) C(13) C(12) 124.6(8) ? N(14) C(15) C(16) 122.6(7) ? C(15) C(16) C(11) 121.0(7) ? P(1) C(1B) P(2) 110.7(3) ? C(112) C(111) C(116) 119.4(7) ? C(112) C(111) P(1) 123.2(6) ? C(116) C(111) P(1) 117.1(6) ? C(111) C(112) C(113) 119.8(9) ? C(114) C(113) C(112) 120.7(10) ? C(113) C(114) C(115) 120.2(9) ? C(116) C(115) C(114) 119.4(10) ? C(115) C(116) C(111) 120.4(9) ? C(126) C(121) C(122) 118.7(6) ? C(126) C(121) P(1) 121.5(5) ? C(122) C(121) P(1) 119.8(5) ? C(121) C(122) C(123) 119.5(7) ? C(124) C(123) C(122) 120.6(7) ? C(125) C(124) C(123) 119.5(7) ? C(124) C(125) C(126) 120.2(8) ? C(121) C(126) C(125) 121.4(7) ? C(216) C(211) C(212) 118.0(6) ? C(216) C(211) P(2) 125.3(5) ? C(212) C(211) P(2) 116.6(5) ? C(213) C(212) C(211) 121.5(6) ? C(212) C(213) C(214) 120.0(7) ? C(215) C(214) C(213) 120.0(7) ? C(214) C(215) C(216) 118.2(7) ? C(211) C(216) C(215) 122.3(7) ? C(222) C(221) C(226) 118.8(6) ? C(222) C(221) P(2) 118.9(5) ? C(226) C(221) P(2) 122.3(5) ? C(221) C(222) C(223) 120.5(7) ? C(224) C(223) C(222) 120.3(8) ? C(225) C(224) C(223) 119.4(7) ? C(224) C(225) C(226) 120.8(7) ? C(225) C(226) C(221) 120.3(7) ? O(901) C(901) C(902) 114.2(12) ? #===END data_Compound_3 _database_code_CSD 166128 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85.18 H78.36 Cl2.37 F12 N4 O16.59 P4 Pt Re2 S4' _chemical_formula_weight 2555.00 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Pt' 'Pt' -1.7033 8.3905 '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' 'F' 'F' 0.0171 0.0103 '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 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.218(4) _cell_length_b 28.529(6) _cell_length_c 20.218(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.78(3) _cell_angle_gamma 90.00 _cell_volume 11525(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5002 _exptl_absorpt_coefficient_mu 3.562 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70586 _diffrn_reflns_av_R_equivalents 0.2771 _diffrn_reflns_av_sigmaI/netI 0.4704 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 24.90 _reflns_number_total 19136 _reflns_number_gt 5748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1659P)^2^+15.1260P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00315(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 19136 _refine_ls_number_parameters 1138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2920 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.3292 _refine_ls_wR_factor_gt 0.2230 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_restrained_S_all 0.870 _refine_ls_shift/su_max 2.459 _refine_ls_shift/su_mean 0.101 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.28375(6) 0.53178(4) -0.46014(6) 0.0503(4) Uani 1 1 d . . . Re1 Re 0.05501(6) 0.38983(4) -0.20599(5) 0.0437(4) Uani 1 1 d . . . Re2 Re 0.02339(6) 0.32531(4) -0.26994(5) 0.0446(4) Uani 1 1 d . . . S2 S -0.0347(4) 0.2741(2) -0.4354(3) 0.0412(19) Uani 1 1 d . . . S1 S 0.0698(5) 0.5128(2) -0.1986(4) 0.054(2) Uani 1 1 d . . . P1 P 0.1588(4) 0.3594(2) -0.1503(4) 0.048(2) Uani 1 1 d . . . P2 P 0.1058(4) 0.2708(3) -0.2212(4) 0.056(2) Uani 1 1 d . . . P3 P -0.0593(4) 0.2987(2) -0.2035(4) 0.050(2) Uani 1 1 d . . . P4 P -0.0063(4) 0.3773(2) -0.1142(4) 0.051(2) Uani 1 1 d . . . S3 S -0.3019(6) 0.7941(4) 0.0436(6) 0.091(3) Uani 1 1 d . . . S4 S 0.3484(5) 0.5490(3) 0.6322(4) 0.068(2) Uani 1 1 d . . . O4 O 0.0842(9) 0.3472(6) -0.3410(8) 0.045(5) Uani 1 1 d . . . O2 O -0.0206(9) 0.4296(5) -0.2614(9) 0.046(5) Uani 1 1 d . . . O3 O 0.1073(10) 0.4138(5) -0.2815(9) 0.054(5) Uani 1 1 d . . . N4 N -0.2321(13) 0.5575(8) -0.5288(13) 0.060(7) Uani 1 1 d . . . O11 O 0.0002(11) 0.5268(6) -0.2019(9) 0.063(6) Uani 1 1 d . . . O42 O 0.2982(11) 0.5668(6) 0.5788(10) 0.068(6) Uani 1 1 d . . . O1 O -0.0449(9) 0.3685(5) -0.3314(8) 0.049(5) Uani 1 1 d . . . N3 N -0.3349(13) 0.5123(7) -0.3867(12) 0.054(7) Uani 1 1 d . . . O41 O 0.3512(12) 0.4987(6) 0.6365(10) 0.078(7) Uani 1 1 d . . . N1 N -0.2036(12) 0.4946(8) -0.4220(10) 0.047(6) Uani 1 1 d . . . C13 C -0.4904(16) 0.6094(8) -0.5229(14) 0.051(8) Uani 1 1 d . . . F42 F 0.3513(11) 0.5515(8) 0.7606(10) 0.113(7) Uani 1 1 d . . . F43 F 0.3106(13) 0.6131(9) 0.7121(13) 0.133(10) Uani 1 1 d . . . C29 C 0.1141(15) 0.3890(10) -0.3325(12) 0.047(8) Uani 1 1 d . . . O12 O 0.1011(12) 0.5207(6) -0.2534(11) 0.083(7) Uani 1 1 d . . . O21 O -0.0186(11) 0.2739(6) -0.3566(10) 0.069(6) Uani 1 1 d . . . N2 N -0.3673(12) 0.5650(8) -0.4924(11) 0.049(6) Uani 1 1 d . . . C12 C -0.4438(16) 0.6109(10) -0.5658(14) 0.051(8) Uani 1 1 d . . . H12A H -0.4534 0.6263 -0.6067 0.061 Uiso 1 1 calc R . . C2B C -0.0327(14) 0.3164(8) -0.1170(11) 0.042(7) Uani 1 1 d . . . H2BA H -0.0694 0.3125 -0.0917 0.050 Uiso 1 1 calc R . . H2BB H 0.0041 0.2967 -0.0969 0.050 Uiso 1 1 calc R . . O13 O 0.0814(9) 0.4648(5) -0.1682(9) 0.056(5) Uani 1 1 d . . . C11 C -0.3826(16) 0.5894(10) -0.5475(15) 0.053(8) Uani 1 1 d . . . H11A H -0.3506 0.5923 -0.5758 0.064 Uiso 1 1 calc R . . C16 C -0.3966(15) 0.5309(9) -0.3875(13) 0.045(7) Uani 1 1 d . . . F41 F 0.2545(11) 0.5488(9) 0.7089(11) 0.106(8) Uani 1 1 d . . . C33 C -0.1673(14) 0.5471(10) -0.6203(13) 0.047(8) Uani 1 1 d . . . H33A H -0.1498 0.5269 -0.6493 0.057 Uiso 1 1 calc R . . O43 O 0.4116(11) 0.5719(8) 0.6379(12) 0.090(7) Uani 1 1 d . . . O32 O -0.3130(16) 0.8390(9) 0.0642(14) 0.124(10) Uani 1 1 d . . . C17 C -0.4355(15) 0.5244(10) -0.3380(14) 0.056(8) Uani 1 1 d . . . H17A H -0.4777 0.5378 -0.3405 0.068 Uiso 1 1 calc R . . O22 O -0.0720(15) 0.3175(9) -0.4571(11) 0.121(10) Uani 1 1 d . . . C2 C -0.1011(13) 0.4415(9) -0.3571(13) 0.039(7) Uani 1 1 d . . . C34 C -0.2109(16) 0.5308(11) -0.5767(13) 0.058(8) Uani 1 1 d . . . H34A H -0.2259 0.5000 -0.5813 0.069 Uiso 1 1 calc R . . C27 C -0.510(2) 0.4576(18) -0.257(2) 0.14(2) Uani 1 1 d . . . H27A H -0.4941 0.4277 -0.2694 0.205 Uiso 1 1 calc R . . H27B H -0.5332 0.4731 -0.2956 0.205 Uiso 1 1 calc R . . H27C H -0.5400 0.4531 -0.2247 0.205 Uiso 1 1 calc R . . C3 C -0.1053(16) 0.4872(9) -0.3374(15) 0.053(8) Uani 1 1 d . . . H3A H -0.0759 0.4995 -0.3018 0.064 Uiso 1 1 calc R . . C20 C -0.3132(17) 0.4852(10) -0.3327(14) 0.063(9) Uani 1 1 d . . . H20A H -0.2718 0.4707 -0.3312 0.075 Uiso 1 1 calc R . . C31 C -0.1734(15) 0.6221(10) -0.5717(14) 0.053(8) Uani 1 1 d . . . H31A H -0.1625 0.6538 -0.5695 0.063 Uiso 1 1 calc R . . C19 C -0.3465(18) 0.4777(11) -0.2812(16) 0.063(9) Uani 1 1 d . . . H19A H -0.3275 0.4597 -0.2448 0.076 Uiso 1 1 calc R . . C14 C -0.4766(18) 0.5829(10) -0.4656(16) 0.066(10) Uani 1 1 d . . . H14A H -0.5076 0.5795 -0.4363 0.080 Uiso 1 1 calc R . . C21 C -0.5580(17) 0.6327(10) -0.5364(15) 0.061(9) Uani 1 1 d . . . C28 C -0.4510(19) 0.4875(15) -0.2257(18) 0.089(12) Uani 1 1 d . . . C4 C -0.1558(16) 0.5143(10) -0.3732(15) 0.055(8) Uani 1 1 d . . . H4A H -0.1575 0.5462 -0.3642 0.066 Uiso 1 1 calc R . . F32 F -0.3601(19) 0.7261(12) -0.023(2) 0.27(2) Uani 1 1 d . . . O33 O -0.2431(18) 0.7793(11) 0.0242(17) 0.166(15) Uani 1 1 d . . . C32 C -0.2128(15) 0.6018(11) -0.5270(14) 0.059(9) Uani 1 1 d . . . H32A H -0.2259 0.6210 -0.4941 0.071 Uiso 1 1 calc R . . F33 F -0.4242(16) 0.7770(10) 0.011(2) 0.203(16) Uani 1 1 d . . . C15 C -0.413(2) 0.5610(10) -0.4534(13) 0.060(10) Uani 1 1 d . . . C18 C -0.408(2) 0.4963(13) -0.2828(17) 0.085(12) Uani 1 1 d . . . C25 C -0.4104(19) 0.4657(17) -0.1652(16) 0.14(2) Uani 1 1 d . . . H25A H -0.3930 0.4362 -0.1773 0.207 Uiso 1 1 calc R . . H25B H -0.4382 0.4610 -0.1313 0.207 Uiso 1 1 calc R . . H25C H -0.3740 0.4862 -0.1484 0.207 Uiso 1 1 calc R . . C30 C 0.1521(15) 0.4063(9) -0.3823(12) 0.047(8) Uani 1 1 d . . . C22 C -0.5612(15) 0.6634(12) -0.599(2) 0.098(14) Uani 1 1 d . . . H22K H -0.5272 0.6871 -0.5918 0.147 Uiso 1 1 calc R . . H22L H -0.6044 0.6779 -0.6087 0.147 Uiso 1 1 calc R . . H22M H -0.5539 0.6443 -0.6365 0.147 Uiso 1 1 calc R . . F31 F -0.354(2) 0.8007(11) -0.065(2) 0.25(2) Uani 1 1 d . . . C26 C -0.479(2) 0.5403(19) -0.2033(16) 0.16(2) Uani 1 1 d . . . H26A H -0.5061 0.5360 -0.1683 0.233 Uiso 1 1 calc R . . H26B H -0.5063 0.5545 -0.2414 0.233 Uiso 1 1 calc R . . H26C H -0.4422 0.5603 -0.1877 0.233 Uiso 1 1 calc R . . C6 C -0.1430(14) 0.4217(9) -0.4100(13) 0.045(7) Uani 1 1 d . . . H6A H -0.1361 0.3912 -0.4235 0.054 Uiso 1 1 calc R . . C1 C -0.0505(17) 0.4111(11) -0.3140(18) 0.062(10) Uani 1 1 d . . . C23 C -0.6139(15) 0.5951(10) -0.5507(16) 0.069(9) Uani 1 1 d . . . H23A H -0.6132 0.5754 -0.5122 0.104 Uiso 1 1 calc R . . H23B H -0.6064 0.5764 -0.5884 0.104 Uiso 1 1 calc R . . H23C H -0.6566 0.6103 -0.5605 0.104 Uiso 1 1 calc R . . C5 C -0.1963(15) 0.4486(9) -0.4430(14) 0.060(9) Uani 1 1 d . . . H5A H -0.2261 0.4359 -0.4781 0.072 Uiso 1 1 calc R . . C24 C -0.5738(18) 0.6623(12) -0.4792(19) 0.098(13) Uani 1 1 d . . . H24A H -0.5716 0.6433 -0.4398 0.147 Uiso 1 1 calc R . . H24B H -0.6179 0.6752 -0.4903 0.147 Uiso 1 1 calc R . . H24C H -0.5418 0.6873 -0.4710 0.147 Uiso 1 1 calc R . . O31 O -0.319(4) 0.7593(14) 0.101(2) 0.32(4) Uani 1 1 d . . . F11 F 0.0984(12) 0.5372(6) -0.0762(11) 0.105(8) Uani 1 1 d . . . F22 F -0.1297(13) 0.2249(9) -0.5085(11) 0.140(9) Uani 1 1 d . . . F12 F 0.1778(12) 0.5382(8) -0.1260(12) 0.111(8) Uani 1 1 d . . . F13 F 0.1041(11) 0.5925(6) -0.1449(10) 0.108(7) Uani 1 1 d . . . C326 C -0.1894(17) 0.3266(10) -0.1782(15) 0.055(8) Uani 1 1 d . . . H32B H -0.1741 0.3197 -0.1336 0.066 Uiso 1 1 calc R . . F21 F -0.1553(17) 0.2436(10) -0.4140(12) 0.157(11) Uani 1 1 d . . . C412 C -0.1098(15) 0.4426(8) -0.1588(15) 0.049(8) Uani 1 1 d . . . H41A H -0.0844 0.4533 -0.1904 0.058 Uiso 1 1 calc R . . F23 F -0.0805(15) 0.1903(8) -0.4161(12) 0.148(10) Uani 1 1 d . . . C111 C 0.1959(16) 0.3796(10) -0.0697(15) 0.064(9) Uani 1 1 d . . . C411 C -0.0851(15) 0.4070(11) -0.1137(15) 0.056(8) Uani 1 1 d . . . C322 C -0.1684(17) 0.3317(11) -0.2915(17) 0.063(9) Uani 1 1 d . . . H32C H -0.1398 0.3277 -0.3229 0.075 Uiso 1 1 calc R . . C416 C -0.1187(19) 0.3982(10) -0.0598(16) 0.068(10) Uani 1 1 d . . . H41B H -0.0960 0.3807 -0.0246 0.082 Uiso 1 1 calc R . . C325 C -0.254(2) 0.3403(10) -0.1968(18) 0.071(10) Uani 1 1 d . . . H32D H -0.2832 0.3439 -0.1660 0.085 Uiso 1 1 calc R . . C414 C -0.2078(16) 0.4503(10) -0.1037(17) 0.066(10) Uani 1 1 d . . . H41C H -0.2472 0.4664 -0.1001 0.079 Uiso 1 1 calc R . . C321 C -0.1454(15) 0.3225(10) -0.2259(15) 0.056(8) Uani 1 1 d . . . C311 C -0.0825(16) 0.2375(9) -0.1954(15) 0.058(9) Uani 1 1 d . . . C415 C -0.185(2) 0.4134(13) -0.0536(18) 0.090(12) Uani 1 1 d . . . H41D H -0.2102 0.4018 -0.0224 0.108 Uiso 1 1 calc R . . C426 C 0.091(2) 0.4071(14) 0.1040(17) 0.101(15) Uani 1 1 d . . . H42A H 0.1111 0.4136 0.1476 0.121 Uiso 1 1 calc R . . C324 C -0.230(2) 0.3460(13) -0.3116(18) 0.084(12) Uani 1 1 d . . . H32E H -0.2434 0.3540 -0.3562 0.101 Uiso 1 1 calc R . . C413 C -0.1731(18) 0.4619(11) -0.1558(17) 0.071(10) Uani 1 1 d . . . H41E H -0.1919 0.4827 -0.1889 0.085 Uiso 1 1 calc R . . C211 C 0.080(2) 0.2123(10) -0.195(2) 0.094(13) Uani 1 1 d . . . C312 C -0.1170(18) 0.2170(11) -0.2492(17) 0.077(10) Uani 1 1 d . . . H31B H -0.1258 0.2332 -0.2895 0.093 Uiso 1 1 calc R . . C425 C 0.0679(18) 0.4424(15) 0.0647(19) 0.094(13) Uani 1 1 d . . . H42B H 0.0692 0.4730 0.0809 0.113 Uiso 1 1 calc R . . C113 C 0.2211(18) 0.4405(13) 0.012(2) 0.093(13) Uani 1 1 d . . . H11C H 0.2153 0.4716 0.0238 0.112 Uiso 1 1 calc R . . C421 C 0.0331(14) 0.3873(11) -0.0278(16) 0.063(9) Uani 1 1 d . . . C215 C 0.030(2) 0.1364(12) -0.234(2) 0.091(13) Uani 1 1 d . . . H21A H 0.0019 0.1195 -0.2660 0.110 Uiso 1 1 calc R . . C423 C 0.0553(16) 0.3525(10) 0.0145(16) 0.069(10) Uani 1 1 d . . . H42C H 0.0505 0.3215 0.0001 0.083 Uiso 1 1 calc R . . C314 C -0.126(2) 0.1436(11) -0.185(2) 0.089(13) Uani 1 1 d . . . H31C H -0.1385 0.1125 -0.1805 0.107 Uiso 1 1 calc R . . C216 C 0.0495(15) 0.1823(10) -0.2441(15) 0.061(9) Uani 1 1 d . . . H21B H 0.0413 0.1937 -0.2877 0.073 Uiso 1 1 calc R . . C1TF C 0.116(3) 0.5490(12) -0.1355(19) 0.104(17) Uani 1 1 d . . . C313 C -0.1409(17) 0.1688(12) -0.245(2) 0.099(15) Uani 1 1 d . . . H31D H -0.1662 0.1548 -0.2816 0.119 Uiso 1 1 calc R . . C214 C 0.055(2) 0.1185(11) -0.175(3) 0.114(17) Uani 1 1 d . . . H21C H 0.0483 0.0867 -0.1677 0.137 Uiso 1 1 calc R . . C323 C -0.273(2) 0.3490(11) -0.266(3) 0.095(14) Uani 1 1 d . . . H32F H -0.3174 0.3571 -0.2817 0.114 Uiso 1 1 calc R . . C212 C 0.105(2) 0.1916(13) -0.1319(19) 0.110(15) Uani 1 1 d . . . H21D H 0.1303 0.2089 -0.0984 0.133 Uiso 1 1 calc R . . C422 C 0.0403(17) 0.4322(10) -0.0043(17) 0.082(11) Uani 1 1 d . . . H42D H 0.0272 0.4569 -0.0333 0.098 Uiso 1 1 calc R . . C116 C 0.234(3) 0.3506(15) -0.0238(19) 0.14(2) Uani 1 1 d . . . H11D H 0.2359 0.3185 -0.0317 0.174 Uiso 1 1 calc R . . C114 C 0.257(2) 0.4126(16) 0.0527(17) 0.095(13) Uani 1 1 d . . . H11E H 0.2754 0.4225 0.0954 0.114 Uiso 1 1 calc R . . C315 C -0.091(2) 0.1691(14) -0.1318(19) 0.099(13) Uani 1 1 d . . . H31E H -0.0804 0.1544 -0.0905 0.118 Uiso 1 1 calc R . . C424 C 0.0871(19) 0.3627(13) 0.0838(15) 0.091(13) Uani 1 1 d . . . H42E H 0.1040 0.3386 0.1126 0.110 Uiso 1 1 calc R . . C316 C -0.070(2) 0.2127(11) -0.1370(16) 0.092(13) Uani 1 1 d . . . H31F H -0.0472 0.2272 -0.0992 0.110 Uiso 1 1 calc R . . C4TF C 0.311(3) 0.5694(17) 0.705(2) 0.103(14) Uani 1 1 d . . . C115 C 0.268(3) 0.3693(16) 0.032(3) 0.15(2) Uani 1 1 d . . . H11F H 0.3002 0.3511 0.0582 0.184 Uiso 1 1 calc R . . C213 C 0.089(3) 0.1447(12) -0.122(3) 0.17(3) Uani 1 1 d . . . H21E H 0.1025 0.1309 -0.0804 0.198 Uiso 1 1 calc R . . C121 C 0.2299(16) 0.3720(11) -0.1965(13) 0.050(8) Uani 1 1 d . . . C122 C 0.2395(19) 0.4150(13) -0.214(2) 0.101(14) Uani 1 1 d . . . H12B H 0.2105 0.4387 -0.2047 0.122 Uiso 1 1 calc R . . C123 C 0.295(2) 0.4253(14) -0.2466(19) 0.097(13) Uani 1 1 d . . . H12C H 0.3037 0.4560 -0.2581 0.116 Uiso 1 1 calc R . . O23 O 0.0019(14) 0.2640(9) -0.4620(14) 0.103(9) Uiso 1 1 d . . . C126 C 0.267(3) 0.338(2) -0.213(4) 0.22(4) Uani 1 1 d . . . H12D H 0.2536 0.3075 -0.2100 0.260 Uiso 1 1 calc R . . C125 C 0.323(4) 0.3473(18) -0.235(5) 0.31(6) Uani 1 1 d . . . H12E H 0.3564 0.3249 -0.2337 0.374 Uiso 1 1 calc R . . C124 C 0.330(2) 0.3939(18) -0.260(2) 0.113(15) Uiso 1 1 d . . . H12F H 0.3629 0.3998 -0.2863 0.136 Uiso 1 1 calc R . . C221 C 0.1665(16) 0.2569(8) -0.2794(14) 0.097(15) Uani 1 1 d G . . C222 C 0.1497(13) 0.2597(8) -0.3471(14) 0.093(12) Uani 1 1 d G . . H22A H 0.1078 0.2709 -0.3657 0.111 Uiso 1 1 calc R . . C223 C 0.1943(18) 0.2462(10) -0.3875(14) 0.151(17) Uani 1 1 d G . . H22B H 0.1829 0.2481 -0.4337 0.181 Uiso 1 1 calc R . . C224 C 0.2557(17) 0.2298(10) -0.360(2) 0.20(2) Uani 1 1 d G . . H22C H 0.2862 0.2206 -0.3877 0.241 Uiso 1 1 calc R . . C225 C 0.2725(16) 0.2270(12) -0.292(2) 0.23(2) Uani 1 1 d G . . H22D H 0.3144 0.2158 -0.2738 0.271 Uiso 1 1 calc R . . C226 C 0.2279(19) 0.2405(11) -0.2521(16) 0.22(3) Uani 1 1 d G . . H22E H 0.2394 0.2386 -0.2058 0.259 Uiso 1 1 calc R . . C3TF C -0.364(4) 0.776(3) -0.019(3) 0.17(2) Uiso 1 1 d . . . Cl1 Cl -0.2199(13) 0.5811(9) -0.2483(14) 0.165(11) Uiso 0.574(17) 1 d P . . Cl2 Cl -0.3443(18) 0.6230(12) -0.2618(18) 0.224(15) Uiso 0.574(17) 1 d P . . Cl3 Cl -0.2399(12) 0.3213(8) -0.5024(12) 0.141(9) Uiso 0.574(17) 1 d P . . Cl4 Cl -0.2814(18) 0.2721(12) -0.6228(18) 0.229(16) Uiso 0.574(17) 1 d P . . O1S O 0.007(3) 0.4341(17) -0.500(3) 0.128(19) Uiso 0.574(17) 1 d P . . C2S C -0.234(9) 0.298(6) -0.568(8) 0.47(9) Uiso 0.574(17) 1 d P . . H2SA H -0.1981 0.2756 -0.5561 0.569 Uiso 0.574(17) 1 calc PR . . H2SB H -0.2151 0.3223 -0.5929 0.569 Uiso 0.574(17) 1 calc PR . . C1S C -0.260(5) 0.619(3) -0.303(5) 0.16(4) Uiso 0.574(17) 1 d P . . H1SA H -0.2681 0.6074 -0.3480 0.195 Uiso 0.574(17) 1 calc PR . . H1SB H -0.2373 0.6494 -0.3016 0.195 Uiso 0.574(17) 1 calc PR . . C2TF C -0.101(2) 0.2330(17) -0.443(2) 0.102(14) Uiso 1 1 d . . . C1B C 0.1507(13) 0.2946(7) -0.1428(14) 0.049(7) Uani 1 1 d . . . H1BA H 0.1948 0.2805 -0.1333 0.059 Uiso 1 1 calc R . . H1BB H 0.1265 0.2872 -0.1062 0.059 Uiso 1 1 calc R . . C112 C 0.1909(19) 0.4239(14) -0.050(2) 0.077(12) Uiso 1 1 d . . . H11B H 0.1661 0.4447 -0.0794 0.093 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 Pt1 0.0640(9) 0.0418(7) 0.0427(8) 0.0082(5) 0.0000(6) 0.0017(6) Re1 0.0672(9) 0.0281(6) 0.0333(7) -0.0027(5) -0.0006(6) 0.0020(6) Re2 0.0681(9) 0.0290(6) 0.0350(7) -0.0035(5) 0.0028(6) -0.0002(6) S2 0.075(6) 0.018(3) 0.025(4) -0.011(3) -0.011(4) 0.003(4) S1 0.091(7) 0.023(4) 0.047(5) 0.001(3) 0.003(5) 0.006(4) P1 0.069(6) 0.033(4) 0.041(5) 0.001(3) 0.003(4) 0.004(4) P2 0.062(6) 0.037(4) 0.067(6) -0.005(4) -0.004(5) -0.005(4) P3 0.075(6) 0.033(4) 0.038(5) 0.001(3) -0.004(4) 0.002(4) P4 0.068(6) 0.039(4) 0.043(5) -0.008(4) 0.001(4) -0.001(4) S3 0.099(9) 0.070(7) 0.105(9) 0.004(6) 0.016(7) 0.021(6) S4 0.079(7) 0.062(6) 0.060(6) -0.002(5) 0.004(5) -0.005(5) O4 0.055(13) 0.029(10) 0.053(12) -0.007(9) 0.017(10) -0.005(9) O2 0.079(15) 0.007(9) 0.045(12) 0.002(8) -0.009(11) -0.006(9) O3 0.097(16) 0.025(10) 0.042(12) -0.019(9) 0.017(11) -0.006(10) N4 0.08(2) 0.028(14) 0.076(19) -0.014(13) 0.019(15) 0.002(13) O11 0.101(18) 0.026(10) 0.057(13) -0.012(9) -0.007(12) 0.013(11) O42 0.085(16) 0.051(12) 0.063(15) 0.018(11) -0.006(12) 0.006(12) O1 0.080(15) 0.016(9) 0.046(11) -0.018(8) -0.005(10) 0.013(9) N3 0.057(18) 0.031(13) 0.077(19) 0.013(13) 0.023(14) 0.014(13) O41 0.11(2) 0.040(13) 0.077(16) 0.002(11) 0.009(14) 0.006(12) N1 0.058(17) 0.061(17) 0.027(14) 0.019(12) 0.025(12) -0.004(14) C13 0.08(2) 0.020(14) 0.042(18) -0.002(14) -0.006(17) -0.004(16) F42 0.121(19) 0.15(2) 0.068(15) -0.024(14) 0.006(13) -0.006(16) F43 0.15(2) 0.093(18) 0.16(2) -0.051(16) 0.004(18) 0.023(17) C29 0.07(2) 0.053(19) 0.017(15) 0.006(14) 0.005(14) -0.008(17) O12 0.13(2) 0.042(13) 0.090(18) -0.004(12) 0.041(16) -0.003(13) O21 0.103(18) 0.027(10) 0.083(16) -0.017(10) 0.031(13) -0.008(11) N2 0.076(19) 0.050(15) 0.017(13) 0.017(11) -0.003(13) 0.004(13) C12 0.06(2) 0.058(19) 0.036(17) -0.022(15) 0.008(16) -0.023(19) C2B 0.056(19) 0.051(17) 0.017(14) -0.014(12) -0.001(13) -0.017(15) O13 0.073(14) 0.022(10) 0.073(14) -0.031(9) 0.010(11) 0.019(9) C11 0.05(2) 0.054(19) 0.06(2) -0.007(17) 0.012(16) -0.002(17) C16 0.06(2) 0.033(15) 0.037(17) -0.007(13) 0.003(15) 0.001(16) F41 0.063(14) 0.15(2) 0.116(19) -0.022(15) 0.035(13) -0.008(15) C33 0.06(2) 0.055(19) 0.027(16) -0.022(14) -0.001(15) -0.014(16) O43 0.060(16) 0.110(19) 0.093(18) 0.015(15) -0.011(13) -0.020(15) O32 0.18(3) 0.078(19) 0.12(2) -0.045(16) 0.04(2) -0.018(19) C17 0.04(2) 0.08(2) 0.042(19) 0.010(17) -0.004(16) -0.017(18) O22 0.18(3) 0.10(2) 0.059(16) -0.042(14) -0.042(17) 0.041(19) C2 0.034(17) 0.042(17) 0.043(17) -0.026(14) 0.013(14) -0.022(14) C34 0.08(2) 0.06(2) 0.031(17) -0.006(16) 0.001(17) 0.005(19) C27 0.08(3) 0.24(6) 0.08(3) 0.08(4) -0.01(2) -0.03(4) C3 0.08(2) 0.023(15) 0.07(2) -0.002(15) 0.033(18) 0.019(16) C20 0.09(3) 0.06(2) 0.035(18) 0.026(16) 0.018(19) 0.008(19) C31 0.08(2) 0.041(17) 0.039(18) 0.017(15) 0.005(17) -0.002(16) C19 0.07(3) 0.07(2) 0.05(2) 0.008(17) 0.007(19) 0.02(2) C14 0.09(3) 0.040(18) 0.07(2) 0.009(17) 0.00(2) 0.016(18) C21 0.08(3) 0.046(19) 0.05(2) 0.005(16) -0.005(18) 0.03(2) C28 0.07(3) 0.13(3) 0.07(3) 0.01(2) 0.00(2) 0.01(3) C4 0.07(2) 0.032(16) 0.06(2) -0.003(16) 0.016(19) 0.005(17) F32 0.22(4) 0.12(3) 0.43(7) -0.01(3) -0.08(4) 0.00(3) O33 0.17(3) 0.15(3) 0.15(3) -0.08(2) -0.06(2) 0.11(3) C32 0.06(2) 0.07(2) 0.041(19) -0.044(17) -0.001(16) 0.000(19) F33 0.13(2) 0.13(2) 0.35(5) -0.05(3) 0.02(3) -0.01(2) C15 0.12(3) 0.041(18) 0.014(16) 0.021(13) -0.016(18) -0.01(2) C18 0.12(4) 0.09(3) 0.05(2) 0.00(2) 0.02(2) -0.03(3) C25 0.09(3) 0.27(6) 0.05(2) 0.08(3) 0.00(2) 0.03(4) C30 0.08(2) 0.032(16) 0.026(16) -0.006(13) 0.017(15) -0.004(16) C22 0.03(2) 0.08(3) 0.17(4) -0.03(3) -0.03(2) -0.007(19) F31 0.36(5) 0.16(3) 0.29(4) 0.11(3) 0.21(4) 0.14(3) C26 0.18(5) 0.27(7) 0.02(2) 0.04(3) 0.03(3) 0.07(5) C6 0.07(2) 0.030(15) 0.039(17) 0.000(13) 0.019(16) 0.005(15) C1 0.06(2) 0.05(2) 0.08(3) 0.01(2) 0.05(2) 0.037(19) C23 0.06(2) 0.06(2) 0.08(3) -0.003(18) 0.008(19) -0.018(19) C5 0.07(2) 0.041(17) 0.06(2) -0.021(16) -0.037(17) 0.025(16) C24 0.08(3) 0.09(3) 0.13(4) 0.03(3) 0.02(2) 0.05(2) O31 0.62(11) 0.15(3) 0.13(3) 0.00(3) -0.10(5) 0.18(5) F11 0.17(2) 0.051(12) 0.075(15) -0.030(11) -0.037(14) 0.006(13) F22 0.17(2) 0.16(2) 0.073(16) -0.048(15) -0.016(15) -0.032(19) F12 0.114(19) 0.080(15) 0.13(2) -0.017(13) -0.011(16) 0.029(15) F13 0.16(2) 0.040(11) 0.111(17) -0.004(11) -0.016(14) 0.013(12) C326 0.06(2) 0.051(18) 0.05(2) -0.013(16) -0.008(18) 0.003(18) F21 0.22(3) 0.16(2) 0.100(19) -0.011(17) 0.05(2) -0.01(2) C412 0.05(2) 0.014(14) 0.08(2) -0.029(15) 0.006(17) -0.003(14) F23 0.21(3) 0.091(17) 0.13(2) -0.042(15) -0.004(19) -0.044(18) C111 0.09(2) 0.032(19) 0.06(2) 0.010(16) 0.011(18) -0.001(17) C411 0.06(2) 0.07(2) 0.042(19) -0.027(17) 0.008(17) -0.012(18) C322 0.05(2) 0.07(2) 0.07(2) -0.001(18) 0.004(18) 0.023(19) C416 0.10(3) 0.046(19) 0.05(2) -0.032(16) 0.00(2) 0.02(2) C325 0.09(3) 0.045(19) 0.07(3) -0.013(17) -0.01(2) 0.003(19) C414 0.06(2) 0.038(18) 0.08(3) -0.024(18) -0.04(2) 0.023(16) C321 0.06(2) 0.058(19) 0.042(19) -0.014(16) -0.030(17) 0.006(17) C311 0.08(2) 0.040(18) 0.05(2) -0.011(16) -0.007(17) -0.023(17) C415 0.09(3) 0.10(3) 0.07(3) -0.02(2) -0.01(2) -0.01(3) C426 0.19(5) 0.07(3) 0.04(2) 0.01(2) -0.01(2) -0.03(3) C324 0.12(4) 0.08(3) 0.05(2) 0.02(2) 0.02(3) 0.00(3) C413 0.08(3) 0.07(2) 0.06(2) -0.029(19) 0.03(2) -0.01(2) C211 0.14(4) 0.035(19) 0.11(3) -0.04(2) 0.03(3) 0.01(2) C312 0.11(3) 0.06(2) 0.07(2) -0.016(18) 0.01(2) 0.00(2) C425 0.10(3) 0.11(3) 0.08(3) -0.08(3) 0.01(2) -0.03(3) C113 0.08(3) 0.08(2) 0.11(3) -0.05(3) -0.03(2) 0.03(2) C421 0.05(2) 0.06(2) 0.08(2) -0.03(2) 0.000(17) -0.006(17) C215 0.12(4) 0.05(2) 0.12(4) -0.01(2) 0.05(3) -0.01(2) C423 0.08(3) 0.039(18) 0.07(2) 0.015(18) -0.02(2) -0.013(18) C314 0.14(4) 0.027(18) 0.11(3) 0.03(2) 0.04(3) 0.01(2) C216 0.07(2) 0.05(2) 0.06(2) -0.015(17) 0.011(17) -0.014(18) C1TF 0.20(5) 0.05(2) 0.05(3) 0.004(18) -0.02(3) 0.08(3) C313 0.06(3) 0.05(2) 0.18(5) -0.05(3) -0.02(3) -0.004(19) C214 0.17(4) 0.017(19) 0.14(4) 0.00(2) -0.04(3) -0.04(2) C323 0.07(3) 0.05(2) 0.14(4) -0.01(3) -0.05(3) 0.00(2) C212 0.13(4) 0.09(3) 0.08(3) 0.02(2) -0.06(3) -0.05(3) C422 0.11(3) 0.039(19) 0.09(3) -0.024(18) -0.02(2) 0.010(19) C116 0.26(6) 0.09(3) 0.05(3) 0.04(2) -0.08(3) -0.01(4) C114 0.12(4) 0.10(3) 0.05(2) -0.03(2) -0.03(2) 0.04(3) C315 0.16(4) 0.07(3) 0.07(3) -0.01(2) 0.01(3) -0.01(3) C424 0.14(4) 0.09(3) 0.04(2) 0.019(19) -0.01(2) -0.06(3) C316 0.18(4) 0.03(2) 0.05(2) 0.013(17) 0.00(2) 0.00(2) C4TF 0.13(4) 0.10(4) 0.07(3) 0.02(3) -0.03(3) 0.00(3) C115 0.23(6) 0.07(3) 0.13(5) 0.03(3) -0.07(4) -0.01(4) C213 0.20(5) 0.02(2) 0.23(6) 0.05(3) -0.11(4) 0.00(3) C121 0.07(2) 0.048(19) 0.030(17) 0.007(14) 0.012(15) -0.008(17) C122 0.07(3) 0.08(3) 0.16(4) 0.07(3) 0.02(3) 0.02(2) C123 0.10(3) 0.09(3) 0.09(3) 0.05(2) -0.02(3) 0.01(3) C126 0.21(7) 0.13(5) 0.38(10) 0.04(5) 0.23(7) 0.03(5) C125 0.32(9) 0.10(4) 0.61(15) -0.13(6) 0.36(11) -0.09(5) C221 0.07(3) 0.035(18) 0.18(5) -0.01(2) 0.03(3) -0.015(18) C222 0.15(3) 0.09(3) 0.05(2) -0.004(18) 0.08(2) 0.01(2) C223 0.14(4) 0.08(3) 0.25(5) -0.03(3) 0.07(4) -0.02(3) C224 0.21(6) 0.18(5) 0.25(6) -0.16(4) 0.14(5) -0.09(5) C225 0.13(5) 0.26(5) 0.29(6) -0.16(5) 0.02(5) 0.08(4) C226 0.11(5) 0.31(6) 0.24(5) -0.21(5) 0.06(5) -0.05(5) C1B 0.039(18) 0.007(13) 0.10(2) 0.015(13) 0.002(15) -0.013(12) _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 Pt1 N2 1.96(2) . ? Pt1 N1 1.99(2) . ? Pt1 N4 2.00(2) . ? Pt1 N3 2.01(2) . ? Re1 O2 2.086(17) . ? Re1 O3 2.099(17) . ? Re1 Re2 2.2839(15) . ? Re1 O13 2.306(15) . ? Re1 P1 2.387(8) . ? Re1 P4 2.410(8) . ? Re2 O1 2.109(17) . ? Re2 O4 2.122(16) . ? Re2 O21 2.342(19) . ? Re2 P2 2.379(8) . ? Re2 P3 2.421(8) . ? S2 O23 1.02(3) . ? S2 O22 1.48(2) . ? S2 O21 1.58(2) . ? S2 C2TF 1.77(5) . ? S1 O12 1.38(2) . ? S1 O11 1.45(2) . ? S1 O13 1.506(18) . ? S1 C1TF 1.79(4) . ? P1 C111 1.78(3) . ? P1 C1B 1.87(2) . ? P1 C121 1.87(3) . ? P2 C1B 1.83(3) . ? P2 C211 1.85(3) . ? P2 C221 1.87(3) . ? P3 C2B 1.82(2) . ? P3 C311 1.82(3) . ? P3 C321 1.86(3) . ? P4 C411 1.81(3) . ? P4 C2B 1.82(2) . ? P4 C421 1.83(3) . ? S3 O32 1.38(2) . ? S3 O33 1.37(3) . ? S3 O31 1.61(5) . ? S3 C3TF 1.72(7) . ? S4 O43 1.43(2) . ? S4 O41 1.439(19) . ? S4 O42 1.46(2) . ? S4 C4TF 1.85(5) . ? O4 C29 1.34(3) . ? O2 C1 1.26(4) . ? O3 C29 1.27(3) . ? N4 C32 1.32(3) . ? N4 C34 1.35(3) . ? O1 C1 1.27(3) . ? N3 C16 1.35(3) . ? N3 C20 1.35(3) . ? N1 C4 1.39(3) . ? N1 C5 1.39(3) . ? C13 C12 1.38(4) . ? C13 C14 1.38(4) . ? C13 C21 1.51(4) . ? F42 C4TF 1.38(4) . ? F43 C4TF 1.25(4) . ? C29 C30 1.44(3) . ? N2 C15 1.31(4) . ? N2 C11 1.31(3) . ? C12 C11 1.38(4) . ? C16 C17 1.38(4) . ? C16 C15 1.58(3) . ? F41 C4TF 1.29(5) . ? C33 C30 1.36(3) 3_564 ? C33 C34 1.42(4) . ? C17 C18 1.42(4) . ? C2 C3 1.37(3) . ? C2 C6 1.38(3) . ? C2 C1 1.51(4) . ? C27 C28 1.52(5) . ? C3 C4 1.39(4) . ? C20 C19 1.34(4) . ? C31 C30 1.35(3) 3_564 ? C31 C32 1.42(4) . ? C19 C18 1.34(4) . ? C14 C15 1.41(4) . ? C21 C24 1.50(4) . ? C21 C22 1.54(4) . ? C21 C23 1.55(4) . ? C28 C25 1.50(4) . ? C28 C18 1.57(5) . ? C28 C26 1.70(6) . ? F32 C3TF 1.42(7) . ? F33 C3TF 1.45(7) . ? C30 C31 1.35(3) 3_564 ? C30 C33 1.36(3) 3_564 ? F31 C3TF 1.21(7) . ? C6 C5 1.41(3) . ? F11 C1TF 1.35(4) . ? F22 C2TF 1.39(5) . ? F12 C1TF 1.27(5) . ? F13 C1TF 1.27(3) . ? C326 C325 1.35(4) . ? C326 C321 1.41(4) . ? F21 C2TF 1.35(4) . ? C412 C413 1.40(4) . ? C412 C411 1.41(4) . ? F23 C2TF 1.37(5) . ? C111 C112 1.33(4) . ? C111 C116 1.38(4) . ? C411 C416 1.39(4) . ? C322 C324 1.31(5) . ? C322 C321 1.36(4) . ? C416 C415 1.43(4) . ? C325 C323 1.42(5) . ? C414 C413 1.39(4) . ? C414 C415 1.48(4) . ? C311 C312 1.33(4) . ? C311 C316 1.37(4) . ? C426 C424 1.33(5) . ? C426 C425 1.32(5) . ? C324 C323 1.36(5) . ? C211 C216 1.38(4) . ? C211 C212 1.43(5) . ? C312 C313 1.47(4) . ? C425 C422 1.45(4) . ? C113 C114 1.29(5) . ? C113 C112 1.39(5) . ? C421 C423 1.34(4) . ? C421 C422 1.36(4) . ? C215 C214 1.32(5) . ? C215 C216 1.39(4) . ? C423 C424 1.48(4) . ? C314 C315 1.40(5) . ? C314 C313 1.40(5) . ? C214 C213 1.40(5) . ? C212 C213 1.39(5) . ? C116 C115 1.34(5) . ? C114 C115 1.33(5) . ? C315 C316 1.32(4) . ? C121 C126 1.30(5) . ? C121 C122 1.30(4) . ? C122 C123 1.42(5) . ? C123 C124 1.20(5) . ? C126 C125 1.29(6) . ? C125 C124 1.44(7) . ? C221 C222 1.361(16) . ? C221 C226 1.362(16) . ? C222 C223 1.361(16) . ? C223 C224 1.361(16) . ? C224 C225 1.361(16) . ? C225 C226 1.361(16) . ? Cl1 C1S 1.67(9) . ? Cl2 C1S 2.00(9) . ? Cl3 C2S 1.51(16) . ? Cl4 C2S 1.54(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 N2 Pt1 N1 174.7(9) . . ? N2 Pt1 N4 96.2(10) . . ? N1 Pt1 N4 89.0(9) . . ? N2 Pt1 N3 82.2(10) . . ? N1 Pt1 N3 92.7(9) . . ? N4 Pt1 N3 174.3(9) . . ? O2 Re1 O3 80.9(7) . . ? O2 Re1 Re2 90.9(5) . . ? O3 Re1 Re2 88.8(4) . . ? O2 Re1 O13 77.8(6) . . ? O3 Re1 O13 79.8(6) . . ? Re2 Re1 O13 165.0(5) . . ? O2 Re1 P1 165.8(5) . . ? O3 Re1 P1 87.6(6) . . ? Re2 Re1 P1 97.11(17) . . ? O13 Re1 P1 92.2(5) . . ? O2 Re1 P4 94.2(6) . . ? O3 Re1 P4 169.5(5) . . ? Re2 Re1 P4 100.56(18) . . ? O13 Re1 P4 90.2(5) . . ? P1 Re1 P4 95.8(3) . . ? O1 Re2 O4 79.8(7) . . ? O1 Re2 Re1 87.9(4) . . ? O4 Re2 Re1 90.3(4) . . ? O1 Re2 O21 78.2(6) . . ? O4 Re2 O21 81.9(6) . . ? Re1 Re2 O21 165.1(5) . . ? O1 Re2 P2 168.6(5) . . ? O4 Re2 P2 91.8(5) . . ? Re1 Re2 P2 100.03(19) . . ? O21 Re2 P2 93.0(5) . . ? O1 Re2 P3 93.7(5) . . ? O4 Re2 P3 171.2(5) . . ? Re1 Re2 P3 95.50(17) . . ? O21 Re2 P3 90.9(5) . . ? P2 Re2 P3 93.7(3) . . ? O23 S2 O22 117(2) . . ? O23 S2 O21 118.4(19) . . ? O22 S2 O21 108.7(11) . . ? O23 S2 C2TF 112(2) . . ? O22 S2 C2TF 101(2) . . ? O21 S2 C2TF 96.7(17) . . ? O12 S1 O11 118.6(14) . . ? O12 S1 O13 114.6(12) . . ? O11 S1 O13 111.0(12) . . ? O12 S1 C1TF 103(2) . . ? O11 S1 C1TF 105.8(18) . . ? O13 S1 C1TF 101.6(13) . . ? C111 P1 C1B 106.0(13) . . ? C111 P1 C121 98.4(13) . . ? C1B P1 C121 108.4(13) . . ? C111 P1 Re1 122.1(11) . . ? C1B P1 Re1 108.5(9) . . ? C121 P1 Re1 112.5(10) . . ? C1B P2 C211 102.2(15) . . ? C1B P2 C221 109.7(13) . . ? C211 P2 C221 103.2(13) . . ? C1B P2 Re2 109.9(8) . . ? C211 P2 Re2 119.8(14) . . ? C221 P2 Re2 111.4(10) . . ? C2B P3 C311 102.8(13) . . ? C2B P3 C321 105.2(13) . . ? C311 P3 C321 97.3(14) . . ? C2B P3 Re2 108.6(9) . . ? C311 P3 Re2 124.0(10) . . ? C321 P3 Re2 116.7(11) . . ? C411 P4 C2B 101.2(14) . . ? C411 P4 C421 100.2(13) . . ? C2B P4 C421 105.3(13) . . ? C411 P4 Re1 119.5(11) . . ? C2B P4 Re1 107.6(8) . . ? C421 P4 Re1 120.8(10) . . ? O32 S3 O33 124(2) . . ? O32 S3 O31 107(2) . . ? O33 S3 O31 108(3) . . ? O32 S3 C3TF 112(3) . . ? O33 S3 C3TF 105(3) . . ? O31 S3 C3TF 98(3) . . ? O43 S4 O41 115.1(16) . . ? O43 S4 O42 114.5(13) . . ? O41 S4 O42 114.2(13) . . ? O43 S4 C4TF 105(2) . . ? O41 S4 C4TF 106.5(18) . . ? O42 S4 C4TF 99.0(17) . . ? C29 O4 Re2 118.3(15) . . ? C1 O2 Re1 116.5(17) . . ? C29 O3 Re1 122.5(16) . . ? C32 N4 C34 116(3) . . ? C32 N4 Pt1 121(2) . . ? C34 N4 Pt1 123(2) . . ? C1 O1 Re2 118(2) . . ? C16 N3 C20 115(2) . . ? C16 N3 Pt1 117.3(19) . . ? C20 N3 Pt1 128(2) . . ? C4 N1 C5 120(2) . . ? C4 N1 Pt1 119.8(19) . . ? C5 N1 Pt1 120(2) . . ? C12 C13 C14 119(3) . . ? C12 C13 C21 124(3) . . ? C14 C13 C21 117(3) . . ? O3 C29 O4 120(2) . . ? O3 C29 C30 121(3) . . ? O4 C29 C30 120(2) . . ? S2 O21 Re2 138.5(10) . . ? C15 N2 C11 117(3) . . ? C15 N2 Pt1 114(2) . . ? C11 N2 Pt1 128(2) . . ? C13 C12 C11 119(3) . . ? P4 C2B P3 109.7(13) . . ? S1 O13 Re1 134.0(11) . . ? N2 C11 C12 123(3) . . ? N3 C16 C17 124(3) . . ? N3 C16 C15 107(3) . . ? C17 C16 C15 128(3) . . ? C30 C33 C34 117(3) 3_564 . ? C16 C17 C18 117(3) . . ? C3 C2 C6 124(3) . . ? C3 C2 C1 116(3) . . ? C6 C2 C1 120(3) . . ? N4 C34 C33 124(3) . . ? C2 C3 C4 117(3) . . ? C19 C20 N3 125(3) . . ? C30 C31 C32 118(3) 3_564 . ? C20 C19 C18 119(3) . . ? C13 C14 C15 117(3) . . ? C13 C21 C24 114(3) . . ? C13 C21 C22 109(3) . . ? C24 C21 C22 109(3) . . ? C13 C21 C23 110(2) . . ? C24 C21 C23 107(3) . . ? C22 C21 C23 108(2) . . ? C25 C28 C27 114(4) . . ? C25 C28 C18 112(3) . . ? C27 C28 C18 106(3) . . ? C25 C28 C26 108(3) . . ? C27 C28 C26 109(3) . . ? C18 C28 C26 108(3) . . ? N1 C4 C3 121(3) . . ? N4 C32 C31 124(3) . . ? N2 C15 C14 124(2) . . ? N2 C15 C16 118(3) . . ? C14 C15 C16 117(3) . . ? C19 C18 C17 120(3) . . ? C19 C18 C28 122(4) . . ? C17 C18 C28 118(4) . . ? C31 C30 C33 121(3) 3_564 3_564 ? C31 C30 C29 122(3) 3_564 . ? C33 C30 C29 117(2) 3_564 . ? C2 C6 C5 119(2) . . ? O2 C1 O1 126(3) . . ? O2 C1 C2 116(2) . . ? O1 C1 C2 118(3) . . ? N1 C5 C6 118(2) . . ? C325 C326 C321 121(3) . . ? C413 C412 C411 120(3) . . ? C112 C111 C116 115(4) . . ? C112 C111 P1 122(3) . . ? C116 C111 P1 122(3) . . ? C416 C411 C412 118(3) . . ? C416 C411 P4 117(3) . . ? C412 C411 P4 124(2) . . ? C324 C322 C321 122(3) . . ? C411 C416 C415 126(3) . . ? C326 C325 C323 116(4) . . ? C413 C414 C415 123(3) . . ? C322 C321 C326 119(3) . . ? C322 C321 P3 118(3) . . ? C326 C321 P3 122(2) . . ? C312 C311 C316 119(3) . . ? C312 C311 P3 117(2) . . ? C316 C311 P3 124(2) . . ? C416 C415 C414 111(3) . . ? C424 C426 C425 123(4) . . ? C322 C324 C323 119(4) . . ? C414 C413 C412 120(3) . . ? C216 C211 C212 116(3) . . ? C216 C211 P2 118(3) . . ? C212 C211 P2 124(3) . . ? C311 C312 C313 120(3) . . ? C426 C425 C422 118(3) . . ? C114 C113 C112 120(3) . . ? C423 C421 C422 118(3) . . ? C423 C421 P4 123(2) . . ? C422 C421 P4 119(3) . . ? C214 C215 C216 115(4) . . ? C421 C423 C424 121(3) . . ? C315 C314 C313 114(3) . . ? C211 C216 C215 125(4) . . ? F12 C1TF F13 115(5) . . ? F12 C1TF F11 101(3) . . ? F13 C1TF F11 108(3) . . ? F12 C1TF S1 111(3) . . ? F13 C1TF S1 113(3) . . ? F11 C1TF S1 108(3) . . ? C314 C313 C312 120(3) . . ? C215 C214 C213 124(3) . . ? C324 C323 C325 123(4) . . ? C213 C212 C211 118(3) . . ? C421 C422 C425 122(3) . . ? C115 C116 C111 119(4) . . ? C113 C114 C115 119(4) . . ? C316 C315 C314 124(4) . . ? C426 C424 C423 118(3) . . ? C315 C316 C311 123(3) . . ? F43 C4TF F41 115(5) . . ? F43 C4TF F42 107(4) . . ? F41 C4TF F42 101(3) . . ? F43 C4TF S4 114(3) . . ? F41 C4TF S4 112(3) . . ? F42 C4TF S4 105(3) . . ? C114 C115 C116 123(5) . . ? C214 C213 C212 120(4) . . ? C126 C121 C122 121(4) . . ? C126 C121 P1 121(3) . . ? C122 C121 P1 118(3) . . ? C121 C122 C123 119(4) . . ? C124 C123 C122 119(4) . . ? C125 C126 C121 121(5) . . ? C126 C125 C124 116(6) . . ? C123 C124 C125 121(5) . . ? C222 C221 C226 120.0 . . ? C222 C221 P2 122(2) . . ? C226 C221 P2 118(2) . . ? C221 C222 C223 120.0 . . ? C222 C223 C224 120.0 . . ? C223 C224 C225 120.0 . . ? C226 C225 C224 120.0 . . ? C225 C226 C221 120.0 . . ? F31 C3TF F32 122(6) . . ? F31 C3TF F33 124(7) . . ? F32 C3TF F33 96(5) . . ? F31 C3TF S3 101(6) . . ? F32 C3TF S3 108(5) . . ? F33 C3TF S3 104(4) . . ? Cl3 C2S Cl4 136(10) . . ? Cl1 C1S Cl2 97(5) . . ? F21 C2TF F23 105(4) . . ? F21 C2TF F22 102(4) . . ? F23 C2TF F22 106(4) . . ? F21 C2TF S2 118(3) . . ? F23 C2TF S2 112(3) . . ? F22 C2TF S2 113(3) . . ? P2 C1B P1 109.5(13) . . ? C111 C112 C113 123(4) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.637 _refine_diff_density_min -1.703 _refine_diff_density_rms 0.364