# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1385 data_global #======================================================================= # 1. SUBMISSION DETAILS _publ_contact_author ; Dr N.C. Norman, School of Chemistry, Cantocks Close, University of Bristol. Bristol. BS8 1TS. ; _publ_contact_author_phone '0117 928 7577' _publ_contact_author_fax '0117 929 0509' _publ_contact_author_email N.C.Norman@bris.ac.uk _publ_requested_journal 'Journal Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #======================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Phosphine Exchange Reactions Involving cis-[Pt(PPh~3~)(Bcat)~2~] (cat = 1,2- O~2~C~6~H~4~) and the Oxidative Addition of 1,2-B~2~Cl~2~(NMe~2~)~2~ to Pt(0). ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Curtis, David' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Lesley, M.J. Gerald' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Norman, Nicholas C.' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Orpen, A. Guy' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; 'Starbuck, Jonathan' ; School of Chemistry University of Bristol Cantocks Close BS8 1TS. Bristol, UK ; #======================================================================= # 4. TEXT # # # N.C. NORMAN # data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C81 H69 B2 Cl2 O4 P5 Pt2' _chemical_formula_weight 1743.91 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz '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, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.493(13) _cell_length_b 12.601(3) _cell_length_c 24.635(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.442(14) _cell_angle_gamma 90.00 _cell_volume 14650.7(65) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method ? _exptl_crystal_F_000 6880 _exptl_absorpt_coefficient_mu 4.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.607799 _exptl_absorpt_correction_T_max 0.862085 _exptl_special_details ; SADABS (Sheldrick, 1996)s ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33762 _diffrn_reflns_av_R_equivalents 0.1854 _diffrn_reflns_av_sigmaI/netI 0.2351 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.00 _reflns_number_total 11470 _reflns_number_observed 5148 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 95 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] 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 'see text' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11375 _refine_ls_number_parameters 901 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.2074 _refine_ls_R_factor_obs 0.0823 _refine_ls_wR_factor_all 0.1812 _refine_ls_wR_factor_obs 0.1354 _refine_ls_goodness_of_fit_all 1.003 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.186 _refine_ls_shift/esd_max 0.088 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.14235(2) 0.78733(6) 0.14120(3) 0.0281(2) Uani 1 d . . Pt2 Pt 0.11177(2) 0.80242(7) 0.03883(3) 0.0305(2) Uani 1 d . . B1 B 0.1477(4) 0.6734(21) 0.0801(10) 0.038(7) Uani 1 d . . B2 B 0.0882(5) 0.8258(18) -0.0346(9) 0.033(6) Uani 1 d . . O1 O 0.1344(2) 0.5719(10) 0.0744(5) 0.034(3) Uani 1 d . . O2 O 0.1721(3) 0.6685(9) 0.0523(5) 0.035(3) Uani 1 d . . O3 O 0.0953(3) 0.7768(11) -0.0853(5) 0.053(4) Uani 1 d . . O4 O 0.0637(3) 0.8814(11) -0.0475(6) 0.060(4) Uani 1 d . . P1 P 0.14173(11) 0.9312(4) 0.0142(2) 0.0358(14) Uani 1 d . . P2 P 0.14290(11) 0.9702(4) 0.1354(2) 0.0347(13) Uani 1 d . . P3 P 0.07660(10) 0.6921(5) 0.0630(2) 0.0345(14) Uani 1 d . . P4 P 0.10742(10) 0.6977(4) 0.1826(2) 0.0334(13) Uani 1 d . . P5 P 0.18613(10) 0.7484(4) 0.1861(2) 0.0293(13) Uani 1 d . . C1 C 0.1500(5) 0.5099(19) 0.0427(8) 0.048(6) Uani 1 d . . C2 C 0.1441(5) 0.4045(18) 0.0254(9) 0.065(7) Uani 1 d . . H2 H 0.1281(5) 0.3660(18) 0.0347(9) 0.078 Uiso 1 calc R . C3 C 0.1637(6) 0.3623(20) -0.0067(12) 0.095(11) Uani 1 d . . H3A H 0.1610(6) 0.2922(20) -0.0204(12) 0.114 Uiso 1 calc R . C4 C 0.1864(6) 0.4181(24) -0.0188(12) 0.098(10) Uani 1 d U . H4A H 0.1995(6) 0.3843(24) -0.0394(12) 0.118 Uiso 1 calc R . C5 C 0.1917(5) 0.5276(19) -0.0017(10) 0.067(7) Uani 1 d . . H5 H 0.2072(5) 0.5675(19) -0.0121(10) 0.080 Uiso 1 calc R . C6 C 0.1726(4) 0.5684(17) 0.0304(9) 0.041(6) Uani 1 d . . C7 C 0.0728(5) 0.7974(18) -0.1237(8) 0.058(7) Uani 1 d D . C8 C 0.0676(6) 0.7678(18) -0.1779(8) 0.080(9) Uani 1 d D . H8 H 0.0813(6) 0.7262(18) -0.1933(8) 0.096 Uiso 1 calc R . C9 C 0.0432(6) 0.7958(29) -0.2107(13) 0.143(19) Uani 1 d D . H9A H 0.0394(6) 0.7782(29) -0.2483(13) 0.171 Uiso 1 calc R . C10 C 0.0251(7) 0.8529(24) -0.1817(9) 0.136(18) Uani 1 d D . H10A H 0.0071(7) 0.8665(24) -0.2015(9) 0.163 Uiso 1 calc R . C11 C 0.0280(5) 0.8941(20) -0.1293(10) 0.087(10) Uani 1 d D . H11 H 0.0143(5) 0.9367(20) -0.1143(10) 0.105 Uiso 1 calc R . C12 C 0.0541(4) 0.8641(16) -0.1013(10) 0.062(8) Uani 1 d D . C13 C 0.1710(4) 0.8883(15) -0.0219(8) 0.036(5) Uani 1 d . . C14 C 0.1937(4) 0.9562(19) -0.0244(8) 0.051(6) Uani 1 d . . H14A H 0.1946(4) 1.0230(19) -0.0064(8) 0.061 Uiso 1 calc R . C15 C 0.2161(5) 0.9219(22) -0.0552(8) 0.056(7) Uani 1 d . . H15A H 0.2319(5) 0.9666(22) -0.0579(8) 0.067 Uiso 1 calc R . C16 C 0.2145(5) 0.8269(22) -0.0801(9) 0.056(7) Uani 1 d . . H16A H 0.2299(5) 0.8045(22) -0.0990(9) 0.068 Uiso 1 calc R . C17 C 0.1913(5) 0.7606(18) -0.0790(8) 0.059(7) Uani 1 d . . H17A H 0.1902(5) 0.6947(18) -0.0979(8) 0.071 Uiso 1 calc R . C18 C 0.1699(5) 0.7941(18) -0.0493(9) 0.055(6) Uani 1 d . . H18A H 0.1538(5) 0.7498(18) -0.0479(9) 0.066 Uiso 1 calc R . C19 C 0.1252(4) 1.0306(17) -0.0322(8) 0.039(6) Uani 1 d . . C20 C 0.1249(5) 1.0230(23) -0.0857(11) 0.092(10) Uani 1 d . . H20A H 0.1352(5) 0.9663(23) -0.0996(11) 0.111 Uiso 1 calc R . C21 C 0.1102(6) 1.0951(24) -0.1243(10) 0.081(9) Uani 1 d . . H21A H 0.1088(6) 1.0846(24) -0.1626(10) 0.098 Uiso 1 calc R . C22 C 0.0976(6) 1.1842(21) -0.0997(14) 0.089(10) Uani 1 d . . H22A H 0.0908(6) 1.2417(21) -0.1225(14) 0.107 Uiso 1 calc R . C23 C 0.0950(6) 1.1897(23) -0.0457(11) 0.083(9) Uani 1 d . . H23A H 0.0837(6) 1.2421(23) -0.0310(11) 0.100 Uiso 1 calc R . C24 C 0.1099(6) 1.1143(19) -0.0131(10) 0.075(8) Uani 1 d . . H24A H 0.1097(6) 1.1202(19) 0.0253(10) 0.090 Uiso 1 calc R . C25 C 0.1586(4) 1.0093(17) 0.0729(8) 0.050(6) Uani 1 d . . H25A H 0.1793(4) 0.9957(17) 0.0777(8) 0.060 Uiso 1 calc R . H25B H 0.1556(4) 1.0860(17) 0.0658(8) 0.060 Uiso 1 calc R . C26 C 0.1108(4) 1.0524(18) 0.1258(8) 0.042(6) Uani 1 d . . C27 C 0.0850(4) 1.0086(18) 0.1091(9) 0.058(7) Uani 1 d . . H27A H 0.0838(4) 0.9336(18) 0.1057(9) 0.069 Uiso 1 calc R . C28 C 0.0601(5) 1.0679(19) 0.0965(9) 0.060(7) Uani 1 d U . H28A H 0.0424(5) 1.0347(19) 0.0856(9) 0.072 Uiso 1 calc R . C29 C 0.0627(6) 1.1780(21) 0.1007(12) 0.106(12) Uani 1 d . . H29A H 0.0464(6) 1.2208(21) 0.0910(12) 0.128 Uiso 1 calc R . C30 C 0.0877(5) 1.2263(18) 0.1184(10) 0.074(9) Uani 1 d . . H30A H 0.0888(5) 1.3013(18) 0.1215(10) 0.089 Uiso 1 calc R . C31 C 0.1112(5) 1.1649(16) 0.1314(8) 0.049(6) Uani 1 d . . H31A H 0.1285(5) 1.1985(16) 0.1448(8) 0.059 Uiso 1 calc R . C32 C 0.1640(4) 1.0520(14) 0.1888(8) 0.032(5) Uani 1 d . . C33 C 0.1531(5) 1.0841(15) 0.2355(9) 0.046(6) Uani 1 d . . H33A H 0.1341(5) 1.0643(15) 0.2394(9) 0.055 Uiso 1 calc R . C34 C 0.1670(4) 1.1414(15) 0.2760(8) 0.042(6) Uani 1 d . . H34A H 0.1584(4) 1.1626(15) 0.3072(8) 0.051 Uiso 1 calc R . C35 C 0.1949(4) 1.1677(16) 0.2695(10) 0.051(7) Uani 1 d . . H35A H 0.2058(4) 1.2076(16) 0.2972(10) 0.061 Uiso 1 calc R . C36 C 0.2070(4) 1.1381(16) 0.2250(9) 0.045(6) Uani 1 d . . H36A H 0.2263(4) 1.1537(16) 0.2224(9) 0.055 Uiso 1 calc R . C37 C 0.1911(4) 1.0846(15) 0.1825(8) 0.041(6) Uani 1 d . . H37A H 0.1989(4) 1.0707(15) 0.1494(8) 0.049 Uiso 1 calc R . C38 C 0.0423(4) 0.7564(16) 0.0626(9) 0.041(6) Uani 1 d . . C39 C 0.0333(4) 0.7963(20) 0.1070(10) 0.067(7) Uani 1 d . . H39A H 0.0452(4) 0.7901(20) 0.1405(10) 0.080 Uiso 1 calc R . C40 C 0.0069(5) 0.8478(20) 0.1074(11) 0.072(8) Uani 1 d . . H40A H 0.0010(5) 0.8746(20) 0.1404(11) 0.086 Uiso 1 calc R . C41 C -0.0097(5) 0.8578(18) 0.0593(13) 0.071(9) Uani 1 d . . H41A H -0.0275(5) 0.8924(18) 0.0583(13) 0.085 Uiso 1 calc R . C42 C -0.0012(5) 0.8188(20) 0.0128(13) 0.084(9) Uani 1 d . . H42A H -0.0129(5) 0.8252(20) -0.0210(13) 0.100 Uiso 1 calc R . C43 C 0.0249(4) 0.7694(17) 0.0151(10) 0.061(7) Uani 1 d . . H43A H 0.0310(4) 0.7433(17) -0.0178(10) 0.074 Uiso 1 calc R . C44 C 0.0675(4) 0.5787(16) 0.0177(8) 0.037(5) Uani 1 d . . C45 C 0.0446(4) 0.5187(17) 0.0279(10) 0.059(7) Uani 1 d . . H45A H 0.0350(4) 0.5326(17) 0.0589(10) 0.071 Uiso 1 calc R . C46 C 0.0359(4) 0.4375(21) -0.0080(11) 0.067(8) Uani 1 d . . H46A H 0.0196(4) 0.3969(21) -0.0025(11) 0.080 Uiso 1 calc R . C47 C 0.0506(5) 0.4153(18) -0.0511(11) 0.065(8) Uani 1 d . . H47A H 0.0442(5) 0.3582(18) -0.0746(11) 0.078 Uiso 1 calc R . C48 C 0.0745(5) 0.4722(18) -0.0628(10) 0.066(8) Uani 1 d . . H48 H 0.0845(5) 0.4564(18) -0.0931(10) 0.079 Uiso 1 calc R . C49 C 0.0825(4) 0.5549(15) -0.0255(8) 0.034(5) Uani 1 d . . H49A H 0.0989(4) 0.5957(15) -0.0304(8) 0.040 Uiso 1 calc R . C50 C 0.0833(4) 0.6259(15) 0.1296(8) 0.041(6) Uani 1 d . . H50A H 0.0914(4) 0.5551(15) 0.1240(8) 0.050 Uiso 1 calc R . H50B H 0.0649(4) 0.6149(15) 0.1441(8) 0.050 Uiso 1 calc R . C51 C 0.1168(4) 0.5890(19) 0.2315(11) 0.052(7) Uani 1 d . . C52 C 0.1160(5) 0.4806(19) 0.2192(9) 0.061(7) Uani 1 d . . H52A H 0.1096(5) 0.4583(19) 0.1831(9) 0.073 Uiso 1 calc R . C53 C 0.1246(6) 0.4043(22) 0.2590(12) 0.084(10) Uani 1 d . . H53A H 0.1219(6) 0.3311(22) 0.2508(12) 0.101 Uiso 1 calc R . C54 C 0.1359(8) 0.4326(25) 0.3063(14) 0.124(15) Uani 1 d . . H54A H 0.1428(8) 0.3795(25) 0.3317(14) 0.149 Uiso 1 calc R . C55 C 0.1383(5) 0.5396(25) 0.3220(11) 0.083(9) Uani 1 d . . H55 H 0.1469(5) 0.5604(25) 0.3571(11) 0.099 Uiso 1 calc R . C56 C 0.1277(5) 0.6120(20) 0.2839(11) 0.069(8) Uani 1 d . . H56A H 0.1278(5) 0.6844(20) 0.2947(11) 0.083 Uiso 1 calc R . C57 C 0.0819(4) 0.7670(15) 0.2229(8) 0.037(5) Uani 1 d . . C58 C 0.0842(4) 0.8746(18) 0.2261(9) 0.046(6) Uani 1 d . . H58A H 0.0993(4) 0.9096(18) 0.2112(9) 0.055 Uiso 1 calc R . C59 C 0.0645(5) 0.9336(20) 0.2510(10) 0.072(8) Uani 1 d . . H59A H 0.0656(5) 1.0088(20) 0.2526(10) 0.087 Uiso 1 calc R . C60 C 0.0427(5) 0.8775(25) 0.2739(9) 0.071(9) Uani 1 d . . H60A H 0.0293(5) 0.9158(25) 0.2922(9) 0.085 Uiso 1 calc R . C61 C 0.0406(5) 0.7667(24) 0.2700(11) 0.079(9) Uani 1 d . . H61A H 0.0254(5) 0.7309(24) 0.2841(11) 0.095 Uiso 1 calc R . C62 C 0.0602(4) 0.7106(21) 0.2461(9) 0.059(7) Uani 1 d . . H62A H 0.0595(4) 0.6352(21) 0.2448(9) 0.070 Uiso 1 calc R . C63 C 0.1918(4) 0.7617(15) 0.2613(8) 0.036(5) Uani 1 d . . C64 C 0.2092(6) 0.6917(19) 0.2929(8) 0.091(11) Uani 1 d . . H64A H 0.2178(6) 0.6326(19) 0.2773(8) 0.109 Uiso 1 calc R . C65 C 0.2135(6) 0.7130(25) 0.3498(11) 0.099(10) Uani 1 d . . H65A H 0.2269(6) 0.6724(25) 0.3726(11) 0.119 Uiso 1 calc R . C66 C 0.1980(7) 0.7948(23) 0.3727(11) 0.094(11) Uani 1 d . . H66A H 0.1984(7) 0.8011(23) 0.4112(11) 0.113 Uiso 1 calc R . C67 C 0.1827(5) 0.8633(20) 0.3392(10) 0.070(8) Uani 1 d . . H67A H 0.1745(5) 0.9247(20) 0.3534(10) 0.084 Uiso 1 calc R . C68 C 0.1792(5) 0.8432(16) 0.2853(9) 0.053(7) Uani 1 d . . H68A H 0.1672(5) 0.8890(16) 0.2626(9) 0.063 Uiso 1 calc R . C69 C 0.2006(3) 0.6153(13) 0.1756(7) 0.021(4) Uani 1 d . . C70 C 0.2289(4) 0.5922(15) 0.1724(7) 0.025(5) Uani 1 d . . H70A H 0.2425(4) 0.6475(15) 0.1767(7) 0.030 Uiso 1 calc R . C71 C 0.2373(4) 0.4910(19) 0.1631(9) 0.052(7) Uani 1 d . . H71A H 0.2565(4) 0.4791(19) 0.1571(9) 0.062 Uiso 1 calc R . C72 C 0.2194(5) 0.4057(17) 0.1621(9) 0.053(7) Uani 1 d . . H72A H 0.2260(5) 0.3359(17) 0.1562(9) 0.064 Uiso 1 calc R . C73 C 0.1912(5) 0.4236(19) 0.1699(8) 0.054(7) Uani 1 d . . H73A H 0.1784(5) 0.3658(19) 0.1701(8) 0.065 Uiso 1 calc R . C74 C 0.1817(4) 0.5289(17) 0.1775(8) 0.043(6) Uani 1 d . . H74A H 0.1627(4) 0.5413(17) 0.1839(8) 0.051 Uiso 1 calc R . C75 C 0.2164(4) 0.8280(16) 0.1674(8) 0.043(6) Uani 1 d . . C76 C 0.2193(4) 0.8433(16) 0.1123(8) 0.040(6) Uani 1 d . . H76A H 0.2053(4) 0.8160(16) 0.0853(8) 0.048 Uiso 1 calc R . C77 C 0.2427(4) 0.8988(17) 0.0963(9) 0.050(6) Uani 1 d . . H77A H 0.2446(4) 0.9077(17) 0.0586(9) 0.060 Uiso 1 calc R . C78 C 0.2632(4) 0.9412(16) 0.1356(8) 0.041(6) Uani 1 d . . H78A H 0.2787(4) 0.9819(16) 0.1257(8) 0.050 Uiso 1 calc R . C79 C 0.2599(4) 0.9210(15) 0.1894(8) 0.038(5) Uani 1 d . . H79A H 0.2740(4) 0.9468(15) 0.2165(8) 0.046 Uiso 1 calc R . C80 C 0.2381(4) 0.8672(15) 0.2059(7) 0.028(5) Uani 1 d . . H80A H 0.2372(4) 0.8555(15) 0.2437(7) 0.034 Uiso 1 calc R . C81 C -0.0059(4) 1.4496(13) 0.1368(7) 0.086(17) Uani 0.50 d PDU . Cl1 Cl 0.0243(4) 1.3691(15) 0.1565(8) 0.211(12) Uani 0.50 d PD . Cl2 Cl -0.0212(5) 1.4933(20) 0.1956(10) 0.105(13) Uani 0.22 d PD 1 Cl2' Cl -0.0009(5) 1.5786(13) 0.1657(10) 0.110(11) Uani 0.28 d PD 2 C82 C 0.2598(7) 0.8130(14) 0.4526(10) 0.092(19) Uani 0.50 d PD . Cl3 Cl 0.2723(4) 0.6812(13) 0.4451(8) 0.134(7) Uani 0.50 d PD . Cl4 Cl 0.2432(3) 0.8225(12) 0.5137(6) 0.083(4) Uani 0.50 d PD . 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 0.0249(4) 0.0311(5) 0.0280(5) -0.0015(4) 0.0010(4) 0.0003(4) Pt2 0.0291(5) 0.0329(5) 0.0283(5) 0.0003(4) -0.0014(4) -0.0013(4) B1 0.018(12) 0.055(19) 0.039(16) -0.007(13) -0.006(11) 0.015(13) B2 0.026(13) 0.041(16) 0.029(15) -0.010(12) -0.008(11) -0.002(12) O1 0.019(7) 0.043(9) 0.038(9) 0.000(7) 0.002(6) 0.009(7) O2 0.046(8) 0.029(9) 0.032(8) -0.002(6) 0.013(7) 0.005(7) O3 0.075(10) 0.056(11) 0.026(9) 0.005(8) -0.005(8) -0.017(9) O4 0.063(11) 0.042(10) 0.070(13) 0.009(9) -0.013(9) 0.012(9) P1 0.040(3) 0.038(4) 0.029(3) 0.004(3) 0.001(3) 0.000(3) P2 0.028(3) 0.037(3) 0.038(4) -0.004(3) -0.002(2) 0.002(3) P3 0.026(3) 0.040(4) 0.037(3) 0.001(3) 0.000(2) 0.000(3) P4 0.032(3) 0.035(3) 0.035(3) -0.002(3) 0.006(2) -0.004(3) P5 0.030(3) 0.031(3) 0.027(3) 0.001(2) 0.002(2) 0.005(2) C1 0.062(16) 0.059(17) 0.026(13) -0.003(12) 0.022(12) 0.026(14) C2 0.100(21) 0.039(16) 0.064(18) -0.005(13) 0.045(16) 0.005(15) C3 0.108(22) 0.051(18) 0.141(29) -0.052(18) 0.074(21) -0.019(17) C4 0.107(13) 0.094(13) 0.099(13) -0.018(9) 0.033(9) 0.012(9) C5 0.068(17) 0.058(18) 0.076(20) -0.016(15) 0.018(15) -0.003(15) C6 0.040(13) 0.037(14) 0.051(15) -0.007(12) 0.027(12) 0.025(11) C7 0.088(19) 0.042(15) 0.036(15) 0.011(13) -0.026(14) -0.015(16) C8 0.164(30) 0.041(17) 0.035(17) -0.002(13) 0.011(18) -0.022(18) C9 0.251(52) 0.136(35) 0.028(21) -0.029(21) -0.043(25) -0.050(34) C10 0.228(42) 0.123(32) 0.037(21) 0.048(19) -0.075(25) -0.118(31) C11 0.085(20) 0.076(20) 0.085(22) 0.005(17) -0.063(17) 0.025(16) C12 0.078(18) 0.020(14) 0.076(20) 0.003(13) -0.049(16) 0.018(13) C13 0.050(14) 0.018(12) 0.039(14) 0.002(10) 0.004(11) -0.011(11) C14 0.050(14) 0.081(18) 0.025(13) 0.002(12) 0.018(11) -0.024(14) C15 0.050(15) 0.096(22) 0.021(14) 0.025(14) 0.003(12) -0.005(15) C16 0.045(15) 0.081(21) 0.046(16) 0.019(15) 0.017(12) 0.015(15) C17 0.097(19) 0.058(17) 0.027(14) -0.016(11) 0.026(14) -0.018(15) C18 0.074(16) 0.043(15) 0.051(16) 0.028(14) 0.019(13) 0.007(15) C19 0.059(15) 0.033(14) 0.025(14) 0.006(10) 0.006(11) -0.003(12) C20 0.091(21) 0.136(28) 0.049(19) 0.033(19) 0.008(16) 0.052(20) C21 0.111(24) 0.094(24) 0.037(17) 0.024(16) 0.000(16) -0.007(20) C22 0.106(24) 0.037(18) 0.122(29) 0.032(19) 0.003(21) -0.004(17) C23 0.102(21) 0.095(23) 0.049(18) 0.030(18) -0.009(16) 0.012(19) C24 0.122(24) 0.047(17) 0.047(17) 0.018(14) -0.027(16) 0.008(17) C25 0.038(13) 0.057(16) 0.054(16) 0.021(12) 0.000(12) -0.006(12) C26 0.045(14) 0.057(16) 0.026(13) 0.005(11) 0.007(11) 0.002(13) C27 0.024(12) 0.060(17) 0.084(19) -0.019(14) -0.017(12) 0.023(12) C28 0.053(10) 0.065(10) 0.058(10) -0.007(8) -0.015(8) -0.005(8) C29 0.092(22) 0.057(20) 0.150(29) -0.032(18) -0.076(20) 0.030(17) C30 0.064(16) 0.035(16) 0.108(22) -0.020(14) -0.053(16) 0.012(14) C31 0.052(14) 0.029(14) 0.057(16) 0.001(11) -0.029(12) 0.005(12) C32 0.027(11) 0.017(11) 0.049(15) -0.018(10) -0.012(10) 0.002(10) C33 0.056(15) 0.027(13) 0.055(16) -0.020(12) 0.009(13) 0.008(11) C34 0.063(15) 0.041(14) 0.025(13) -0.017(11) 0.013(11) 0.004(12) C35 0.031(12) 0.037(14) 0.077(19) 0.006(12) -0.028(12) -0.012(11) C36 0.050(14) 0.049(15) 0.043(15) 0.008(12) 0.030(13) 0.012(12) C37 0.057(15) 0.029(13) 0.035(14) -0.007(10) -0.005(12) 0.011(12) C38 0.035(12) 0.053(15) 0.032(14) -0.006(11) -0.011(11) 0.003(11) C39 0.043(14) 0.082(20) 0.070(19) -0.010(17) -0.020(13) 0.015(15) C40 0.042(15) 0.093(22) 0.078(21) -0.018(16) -0.002(15) 0.012(15) C41 0.039(15) 0.049(17) 0.121(27) -0.027(17) -0.013(17) 0.015(13) C42 0.055(17) 0.061(20) 0.127(28) -0.035(18) -0.022(17) 0.007(15) C43 0.041(14) 0.058(18) 0.084(21) 0.010(14) 0.000(14) 0.029(13) C44 0.037(13) 0.044(14) 0.027(13) -0.002(11) -0.006(10) 0.014(11) C45 0.049(15) 0.032(14) 0.097(21) -0.031(14) 0.009(14) -0.016(13) C46 0.022(13) 0.089(22) 0.090(23) -0.003(18) 0.009(14) -0.003(14) C47 0.056(16) 0.045(17) 0.085(22) -0.029(15) -0.027(16) -0.018(14) C48 0.085(20) 0.043(16) 0.065(18) -0.032(14) -0.012(15) 0.029(15) C49 0.037(12) 0.039(14) 0.023(12) 0.006(10) -0.001(10) -0.002(11) C50 0.065(15) 0.020(12) 0.044(14) 0.007(10) 0.027(12) 0.003(11) C51 0.022(12) 0.049(17) 0.087(21) 0.038(15) 0.015(13) 0.017(12) C52 0.095(20) 0.047(17) 0.044(16) 0.001(13) 0.019(14) -0.016(15) C53 0.094(22) 0.076(21) 0.080(23) 0.059(19) 0.003(18) -0.031(18) C54 0.186(38) 0.063(23) 0.107(30) 0.056(22) -0.055(27) -0.036(24) C55 0.081(20) 0.102(25) 0.059(20) 0.021(18) -0.019(16) 0.017(20) C56 0.071(18) 0.057(18) 0.074(21) 0.020(16) -0.018(16) 0.027(15) C57 0.056(14) 0.022(13) 0.033(13) 0.005(10) 0.002(11) -0.005(11) C58 0.017(11) 0.057(16) 0.064(17) -0.027(13) 0.011(11) -0.012(11) C59 0.086(20) 0.073(20) 0.065(19) -0.007(15) 0.041(16) 0.020(16) C60 0.040(15) 0.133(27) 0.045(17) -0.033(18) 0.031(12) 0.008(18) C61 0.043(15) 0.111(26) 0.089(22) -0.037(19) 0.031(14) -0.011(17) C62 0.039(13) 0.080(18) 0.060(16) 0.010(16) 0.018(12) 0.015(15) C63 0.036(12) 0.034(13) 0.037(14) 0.004(11) -0.001(10) -0.008(10) C64 0.214(32) 0.045(16) 0.005(12) -0.003(11) -0.022(16) 0.033(19) C65 0.142(28) 0.088(24) 0.059(21) 0.037(19) -0.026(19) 0.005(23) C66 0.201(36) 0.050(19) 0.034(17) 0.015(16) 0.020(20) -0.039(23) C67 0.110(22) 0.051(18) 0.053(19) -0.024(15) 0.026(17) 0.005(16) C68 0.078(17) 0.039(15) 0.037(15) -0.025(12) -0.014(13) 0.026(13) C69 0.026(10) 0.015(10) 0.023(11) -0.008(8) 0.013(9) -0.014(9) C70 0.024(11) 0.026(12) 0.025(12) -0.005(9) 0.006(9) 0.001(9) C71 0.024(12) 0.075(19) 0.059(17) 0.032(14) 0.017(11) 0.021(13) C72 0.068(17) 0.030(15) 0.062(18) 0.012(12) 0.009(14) 0.018(13) C73 0.069(18) 0.062(18) 0.028(14) 0.010(12) -0.007(13) -0.017(15) C74 0.040(13) 0.055(16) 0.034(14) 0.004(12) 0.011(11) 0.000(13) C75 0.047(13) 0.045(15) 0.031(13) 0.009(11) -0.015(11) -0.009(11) C76 0.035(12) 0.057(15) 0.031(14) 0.015(11) 0.012(10) 0.008(11) C77 0.041(14) 0.059(17) 0.055(17) 0.015(13) 0.032(13) 0.012(12) C78 0.045(14) 0.048(15) 0.034(14) -0.008(11) 0.014(11) -0.014(12) C79 0.036(13) 0.040(14) 0.034(14) 0.004(11) -0.011(11) 0.007(11) C80 0.030(11) 0.046(13) 0.010(11) 0.015(9) 0.007(9) 0.009(10) C81 0.080(19) 0.090(19) 0.087(19) 0.003(10) 0.009(10) 0.006(10) Cl1 0.214(23) 0.273(29) 0.171(22) 0.122(21) 0.133(19) 0.078(21) Cl2 0.231(43) 0.037(18) 0.048(19) -0.024(16) 0.011(24) 0.005(24) Cl2' 0.135(25) 0.141(27) 0.048(17) -0.015(16) -0.025(17) -0.067(21) C82 0.162(54) 0.079(42) 0.029(30) -0.033(29) -0.014(32) 0.009(40) Cl3 0.159(17) 0.109(15) 0.143(18) -0.021(13) 0.058(14) 0.044(13) Cl4 0.072(9) 0.094(12) 0.077(11) -0.009(9) -0.014(8) 0.011(9) _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 B1 2.12(2) . ? Pt1 P5 2.297(5) . ? Pt1 P2 2.309(5) . ? Pt1 P4 2.334(5) . ? Pt1 Pt2 2.7719(13) . ? Pt2 B2 2.04(2) . ? Pt2 P1 2.284(5) . ? Pt2 P3 2.303(5) . ? Pt2 B1 2.49(2) . ? B1 O2 1.41(2) . ? B1 O1 1.43(3) . ? B2 O4 1.36(2) . ? B2 O3 1.47(2) . ? O1 C1 1.38(2) . ? O2 C6 1.37(2) . ? O3 C7 1.37(2) . ? O4 C12 1.37(2) . ? P1 C19 1.81(2) . ? P1 C13 1.82(2) . ? P1 C25 1.85(2) . ? P2 C26 1.84(2) . ? P2 C25 1.85(2) . ? P2 C32 1.87(2) . ? P3 C38 1.82(2) . ? P3 C44 1.83(2) . ? P3 C50 1.84(2) . ? P4 C51 1.85(2) . ? P4 C57 1.87(2) . ? P4 C50 1.87(2) . ? P5 C69 1.84(2) . ? P5 C63 1.85(2) . ? P5 C75 1.85(2) . ? C1 C6 1.36(3) . ? C1 C2 1.41(3) . ? C2 C3 1.39(3) . ? C3 C4 1.35(3) . ? C4 C5 1.46(3) . ? C5 C6 1.37(3) . ? C7 C8 1.382(15) . ? C7 C12 1.382(15) . ? C8 C9 1.38(2) . ? C9 C10 1.38(2) . ? C10 C11 1.38(2) . ? C11 C12 1.399(15) . ? C13 C18 1.36(3) . ? C13 C14 1.38(2) . ? C14 C15 1.44(3) . ? C15 C16 1.34(3) . ? C16 C17 1.39(3) . ? C17 C18 1.39(3) . ? C19 C20 1.32(3) . ? C19 C24 1.39(3) . ? C20 C21 1.44(3) . ? C21 C22 1.44(3) . ? C22 C23 1.35(3) . ? C23 C24 1.39(3) . ? C26 C27 1.36(3) . ? C26 C31 1.42(3) . ? C27 C28 1.40(3) . ? C28 C29 1.40(3) . ? C29 C30 1.36(3) . ? C30 C31 1.37(3) . ? C32 C33 1.37(2) . ? C32 C37 1.38(2) . ? C33 C34 1.34(2) . ? C34 C35 1.39(3) . ? C35 C36 1.35(3) . ? C36 C37 1.39(3) . ? C38 C39 1.32(3) . ? C38 C43 1.36(3) . ? C39 C40 1.41(3) . ? C40 C41 1.36(3) . ? C41 C42 1.35(3) . ? C42 C43 1.38(3) . ? C44 C45 1.37(3) . ? C44 C49 1.38(2) . ? C45 C46 1.39(3) . ? C46 C47 1.36(3) . ? C47 C48 1.40(3) . ? C48 C49 1.41(3) . ? C51 C56 1.37(3) . ? C51 C52 1.40(3) . ? C52 C53 1.40(3) . ? C53 C54 1.28(3) . ? C54 C55 1.40(4) . ? C55 C56 1.36(3) . ? C57 C58 1.36(3) . ? C57 C62 1.42(3) . ? C58 C59 1.39(3) . ? C59 C60 1.42(3) . ? C60 C61 1.40(3) . ? C61 C62 1.36(3) . ? C63 C68 1.36(2) . ? C63 C64 1.39(3) . ? C64 C65 1.42(3) . ? C65 C66 1.42(4) . ? C66 C67 1.35(3) . ? C67 C68 1.34(3) . ? C69 C70 1.39(2) . ? C69 C74 1.41(2) . ? C70 C71 1.36(3) . ? C71 C72 1.37(3) . ? C72 C73 1.39(3) . ? C73 C74 1.42(3) . ? C75 C76 1.39(2) . ? C75 C80 1.41(2) . ? C76 C77 1.41(2) . ? C77 C78 1.40(3) . ? C78 C79 1.37(2) . ? C79 C80 1.34(2) . ? C81 Cl2 1.7798(11) . ? C81 Cl1 1.7798(11) . ? C81 Cl2' 1.7801(11) . ? C82 Cl4 1.7800(11) . ? C82 Cl3 1.7800(11) . ? C82 Cl4 1.91(3) 7_566 ? Cl3 Cl4 1.32(2) 7_566 ? Cl4 Cl3 1.32(2) 7_566 ? Cl4 C82 1.91(3) 7_566 ? Cl4 Cl4 2.07(3) 7_566 ? 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 B1 Pt1 P5 91.4(6) . . ? B1 Pt1 P2 129.1(7) . . ? P5 Pt1 P2 103.1(2) . . ? B1 Pt1 P4 97.5(7) . . ? P5 Pt1 P4 109.6(2) . . ? P2 Pt1 P4 121.6(2) . . ? B1 Pt1 Pt2 59.4(6) . . ? P5 Pt1 Pt2 143.79(13) . . ? P2 Pt1 Pt2 83.32(14) . . ? P4 Pt1 Pt2 96.04(13) . . ? B2 Pt2 P1 87.6(6) . . ? B2 Pt2 P3 88.5(6) . . ? P1 Pt2 P3 171.5(2) . . ? B2 Pt2 B1 137.7(9) . . ? P1 Pt2 B1 98.8(6) . . ? P3 Pt2 B1 89.1(6) . . ? B2 Pt2 Pt1 175.2(7) . . ? P1 Pt2 Pt1 90.67(13) . . ? P3 Pt2 Pt1 92.56(13) . . ? B1 Pt2 Pt1 47.1(5) . . ? O2 B1 O1 107.0(17) . . ? O2 B1 Pt1 123.0(16) . . ? O1 B1 Pt1 126.2(16) . . ? O2 B1 Pt2 113.1(15) . . ? O1 B1 Pt2 105.7(12) . . ? Pt1 B1 Pt2 73.5(7) . . ? O4 B2 O3 106.9(17) . . ? O4 B2 Pt2 130.5(17) . . ? O3 B2 Pt2 122.5(15) . . ? C1 O1 B1 107.6(16) . . ? C6 O2 B1 106.4(16) . . ? C7 O3 B2 105.7(16) . . ? B2 O4 C12 109.0(16) . . ? C19 P1 C13 101.3(9) . . ? C19 P1 C25 104.1(9) . . ? C13 P1 C25 104.6(9) . . ? C19 P1 Pt2 114.8(7) . . ? C13 P1 Pt2 116.9(6) . . ? C25 P1 Pt2 113.5(6) . . ? C26 P2 C25 98.6(9) . . ? C26 P2 C32 98.7(9) . . ? C25 P2 C32 101.8(9) . . ? C26 P2 Pt1 123.7(7) . . ? C25 P2 Pt1 109.0(7) . . ? C32 P2 Pt1 121.0(6) . . ? C38 P3 C44 101.3(9) . . ? C38 P3 C50 105.8(10) . . ? C44 P3 C50 101.3(9) . . ? C38 P3 Pt2 113.8(7) . . ? C44 P3 Pt2 116.1(7) . . ? C50 P3 Pt2 116.6(7) . . ? C51 P4 C57 97.1(9) . . ? C51 P4 C50 100.5(11) . . ? C57 P4 C50 102.3(9) . . ? C51 P4 Pt1 120.8(6) . . ? C57 P4 Pt1 122.7(7) . . ? C50 P4 Pt1 109.9(6) . . ? C69 P5 C63 102.1(8) . . ? C69 P5 C75 98.4(8) . . ? C63 P5 C75 99.9(9) . . ? C69 P5 Pt1 117.2(6) . . ? C63 P5 Pt1 119.1(6) . . ? C75 P5 Pt1 116.7(6) . . ? C6 C1 O1 107.8(19) . . ? C6 C1 C2 125.2(20) . . ? O1 C1 C2 126.9(21) . . ? C3 C2 C1 114.0(22) . . ? C4 C3 C2 121.9(24) . . ? C3 C4 C5 123.2(26) . . ? C6 C5 C4 114.7(23) . . ? C1 C6 C5 120.9(21) . . ? C1 C6 O2 111.0(17) . . ? C5 C6 O2 128.0(21) . . ? O3 C7 C8 131.2(22) . . ? O3 C7 C12 109.1(16) . . ? C8 C7 C12 119.6(23) . . ? C7 C8 C9 123.1(25) . . ? C10 C9 C8 111.1(28) . . ? C9 C10 C11 132.4(28) . . ? C10 C11 C12 110.4(22) . . ? O4 C12 C7 108.8(16) . . ? O4 C12 C11 127.8(22) . . ? C7 C12 C11 122.8(22) . . ? C18 C13 C14 120.3(21) . . ? C18 C13 P1 120.7(16) . . ? C14 C13 P1 118.8(16) . . ? C13 C14 C15 117.6(21) . . ? C16 C15 C14 120.3(23) . . ? C15 C16 C17 122.0(22) . . ? C16 C17 C18 117.4(21) . . ? C13 C18 C17 122.4(22) . . ? C20 C19 C24 116.4(22) . . ? C20 C19 P1 122.4(19) . . ? C24 C19 P1 121.0(17) . . ? C19 C20 C21 124.3(27) . . ? C22 C21 C20 114.2(26) . . ? C23 C22 C21 122.8(27) . . ? C22 C23 C24 116.0(29) . . ? C23 C24 C19 125.1(25) . . ? P2 C25 P1 109.1(10) . . ? C27 C26 C31 115.8(20) . . ? C27 C26 P2 121.1(17) . . ? C31 C26 P2 123.0(16) . . ? C26 C27 C28 123.8(22) . . ? C29 C28 C27 116.7(22) . . ? C30 C29 C28 122.3(23) . . ? C29 C30 C31 118.9(21) . . ? C30 C31 C26 122.5(20) . . ? C33 C32 C37 116.8(18) . . ? C33 C32 P2 121.9(15) . . ? C37 C32 P2 121.3(16) . . ? C34 C33 C32 125.4(21) . . ? C33 C34 C35 116.0(20) . . ? C36 C35 C34 121.6(20) . . ? C35 C36 C37 120.2(20) . . ? C32 C37 C36 119.7(20) . . ? C39 C38 C43 116.4(20) . . ? C39 C38 P3 122.6(17) . . ? C43 C38 P3 120.9(18) . . ? C38 C39 C40 123.5(22) . . ? C41 C40 C39 117.9(24) . . ? C42 C41 C40 120.5(24) . . ? C41 C42 C43 118.8(26) . . ? C38 C43 C42 123.0(25) . . ? C45 C44 C49 120.8(20) . . ? C45 C44 P3 117.0(17) . . ? C49 C44 P3 122.2(16) . . ? C44 C45 C46 118.4(23) . . ? C47 C46 C45 120.4(22) . . ? C46 C47 C48 123.5(22) . . ? C47 C48 C49 114.3(22) . . ? C44 C49 C48 122.4(20) . . ? P3 C50 P4 115.8(10) . . ? C56 C51 C52 114.2(21) . . ? C56 C51 P4 119.8(20) . . ? C52 C51 P4 125.8(21) . . ? C53 C52 C51 121.3(24) . . ? C54 C53 C52 120.4(29) . . ? C53 C54 C55 122.1(29) . . ? C56 C55 C54 116.1(26) . . ? C55 C56 C51 125.4(26) . . ? C58 C57 C62 122.0(21) . . ? C58 C57 P4 116.5(16) . . ? C62 C57 P4 121.5(16) . . ? C57 C58 C59 120.4(21) . . ? C58 C59 C60 117.8(23) . . ? C61 C60 C59 121.1(22) . . ? C62 C61 C60 120.1(24) . . ? C61 C62 C57 118.6(24) . . ? C68 C63 C64 120.1(20) . . ? C68 C63 P5 118.9(16) . . ? C64 C63 P5 121.0(16) . . ? C63 C64 C65 116.4(23) . . ? C64 C65 C66 120.4(26) . . ? C67 C66 C65 119.1(25) . . ? C68 C67 C66 118.9(24) . . ? C67 C68 C63 124.2(22) . . ? C70 C69 C74 117.5(17) . . ? C70 C69 P5 125.3(13) . . ? C74 C69 P5 116.7(14) . . ? C71 C70 C69 120.8(18) . . ? C70 C71 C72 122.8(18) . . ? C71 C72 C73 118.4(21) . . ? C72 C73 C74 119.5(21) . . ? C69 C74 C73 120.3(19) . . ? C76 C75 C80 117.7(18) . . ? C76 C75 P5 118.7(15) . . ? C80 C75 P5 123.4(15) . . ? C75 C76 C77 120.5(20) . . ? C78 C77 C76 120.4(21) . . ? C79 C78 C77 116.8(19) . . ? C80 C79 C78 124.2(19) . . ? C79 C80 C75 120.3(18) . . ? Cl2 C81 Cl1 110.24(9) . . ? Cl1 C81 Cl2' 110.19(9) . . ? Cl4 C82 Cl3 109.5(14) . . ? Cl4 C82 Cl4 68.3(12) . 7_566 ? Cl3 C82 Cl4 41.7(7) . 7_566 ? Cl4 Cl3 C82 74.5(12) 7_566 . ? Cl3 Cl4 C82 170.4(18) 7_566 . ? Cl3 Cl4 C82 63.8(10) 7_566 7_566 ? C82 Cl4 C82 111.7(12) . 7_566 ? Cl3 Cl4 Cl4 116.0(15) 7_566 7_566 ? C82 Cl4 Cl4 58.9(11) . 7_566 ? C82 Cl4 Cl4 52.8(6) 7_566 7_566 ? _refine_diff_density_max 1.300 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.207 #=END data_7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C88.61 H77.54 B2 Cl1.38 O4 P6 Pt2' _chemical_formula_weight 1853.14 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/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 22.880(4) _cell_length_b 14.210(2) _cell_length_c 26.731(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.248(10) _cell_angle_gamma 90.00 _cell_volume 7924.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 222 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method ? _exptl_crystal_F_000 3683 _exptl_absorpt_coefficient_mu 3.746 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.553515 _exptl_absorpt_correction_T_max 0.765128 _exptl_special_details ; SADABS (Sheldrick, 1996)s ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60301 _diffrn_reflns_av_R_equivalents 0.1562 _diffrn_reflns_av_sigmaI/netI 0.1168 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 24.00 _reflns_number_total 12447 _reflns_number_observed 7765 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 87 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+72.6086P] 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 'see text' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12360 _refine_ls_number_parameters 952 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_obs 0.0656 _refine_ls_wR_factor_all 0.1418 _refine_ls_wR_factor_obs 0.1171 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.078 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.27724(2) 1.93471(3) 0.81142(2) 0.02232(15) Uani 1 d . . Pt2 Pt 0.31426(2) 1.74921(4) 0.81135(2) 0.02201(14) Uani 1 d . . B1 B 0.2594(8) 1.8333(11) 0.8626(7) 0.034(4) Uani 1 d . . B2 B 0.3428(7) 1.6134(11) 0.8057(6) 0.026(4) Uani 1 d . . O1 O 0.1968(4) 1.7940(6) 0.8473(4) 0.030(2) Uani 1 d . . O2 O 0.2961(4) 1.8165(6) 0.9183(3) 0.026(2) Uani 1 d . . O3 O 0.3841(4) 1.5854(5) 0.7822(4) 0.031(2) Uani 1 d . . O4 O 0.3199(5) 1.5335(6) 0.8230(4) 0.048(3) Uani 1 d . . P1 P 0.40780(15) 1.7703(2) 0.88697(14) 0.0237(8) Uani 1 d . . P2 P 0.3749(2) 1.9856(2) 0.87574(14) 0.0243(8) Uani 1 d . . P3 P 0.2285(2) 1.7281(2) 0.72892(14) 0.0260(8) Uani 1 d . . P4 P 0.25804(15) 1.9313(2) 0.71982(13) 0.0246(8) Uani 1 d . . P5 P 0.1906(2) 2.0211(2) 0.80804(14) 0.0262(8) Uani 1 d . . P6 P 0.1269(2) 2.2166(3) 0.8063(2) 0.0576(13) Uani 1 d . . C1 C 0.1969(6) 1.7558(9) 0.8940(5) 0.029(3) Uani 1 d . . C2 C 0.1496(7) 1.7094(10) 0.9019(7) 0.045(4) Uani 1 d . . H2A H 0.1088(7) 1.7002(10) 0.8726(7) 0.053 Uiso 1 calc R . C3 C 0.1628(8) 1.6753(12) 0.9547(7) 0.056(5) Uani 1 d . . H3A H 0.1303(8) 1.6435(12) 0.9615(7) 0.068 Uiso 1 calc R . C4 C 0.2220(8) 1.6873(12) 0.9965(7) 0.055(5) Uani 1 d . . H4A H 0.2299(8) 1.6628(12) 1.0318(7) 0.066 Uiso 1 calc R . C5 C 0.2710(7) 1.7345(10) 0.9886(6) 0.044(4) Uani 1 d . . H5A H 0.3122(7) 1.7432(10) 1.0175(6) 0.052 Uiso 1 calc R . C6 C 0.2560(6) 1.7677(9) 0.9365(6) 0.034(3) Uani 1 d . . C7 C 0.3884(6) 1.4880(9) 0.7862(5) 0.027(3) Uani 1 d . . C8 C 0.4234(6) 1.4255(10) 0.7697(6) 0.044(4) Uani 1 d . . H8A H 0.4508(6) 1.4463(10) 0.7533(6) 0.053 Uiso 1 calc R . C9 C 0.4164(7) 1.3316(9) 0.7784(6) 0.038(4) Uani 1 d . . H9A H 0.4411(7) 1.2869(9) 0.7690(6) 0.045 Uiso 1 calc R . C10 C 0.3749(9) 1.2995(11) 0.8003(6) 0.058(5) Uani 1 d . . H10A H 0.3706(9) 1.2337(11) 0.8041(6) 0.070 Uiso 1 calc R . C11 C 0.3387(9) 1.3624(10) 0.8172(7) 0.061(5) Uani 1 d . . H11A H 0.3102(9) 1.3421(10) 0.8327(7) 0.073 Uiso 1 calc R . C12 C 0.3487(7) 1.4573(9) 0.8091(6) 0.038(4) Uani 1 d . . C13 C 0.4246(7) 1.6924(10) 0.9472(6) 0.038(4) Uani 1 d . . C14 C 0.4801(7) 1.7074(10) 0.9936(6) 0.046(4) Uani 1 d . . H14A H 0.5086(7) 1.7564(10) 0.9941(6) 0.055 Uiso 1 calc R . C15 C 0.4944(7) 1.6516(12) 1.0390(6) 0.050(4) Uani 1 d . . H15A H 0.5323(7) 1.6623(12) 1.0712(6) 0.059 Uiso 1 calc R . C16 C 0.4529(8) 1.5794(13) 1.0374(6) 0.060(5) Uani 1 d . . H16A H 0.4624(8) 1.5403(13) 1.0686(6) 0.072 Uiso 1 calc R . C17 C 0.3982(8) 1.5641(11) 0.9910(7) 0.053(4) Uani 1 d . . H17A H 0.3705(8) 1.5137(11) 0.9901(7) 0.064 Uiso 1 calc R . C18 C 0.3830(6) 1.6211(9) 0.9459(5) 0.029(3) Uani 1 d . . H18A H 0.3443(6) 1.6116(9) 0.9142(5) 0.034 Uiso 1 calc R . C19 C 0.4792(5) 1.7490(9) 0.8728(5) 0.026(3) Uani 1 d . . C20 C 0.5028(7) 1.6575(10) 0.8786(6) 0.037(4) Uani 1 d . . H20A H 0.4829(7) 1.6083(10) 0.8900(6) 0.045 Uiso 1 calc R . C21 C 0.5562(7) 1.6392(10) 0.8673(6) 0.045(4) Uani 1 d . . H21A H 0.5721(7) 1.5768(10) 0.8702(6) 0.054 Uiso 1 calc R . C22 C 0.5856(7) 1.7105(11) 0.8522(6) 0.045(4) Uani 1 d . . H22A H 0.6228(7) 1.6981(11) 0.8459(6) 0.053 Uiso 1 calc R . C23 C 0.5613(6) 1.8002(11) 0.8463(6) 0.036(4) Uani 1 d . . H23A H 0.5812(6) 1.8494(11) 0.8349(6) 0.043 Uiso 1 calc R . C24 C 0.5086(6) 1.8193(10) 0.8566(5) 0.035(3) Uani 1 d . . H24A H 0.4924(6) 1.8817(10) 0.8525(5) 0.042 Uiso 1 calc R . C25 C 0.4219(5) 1.8871(8) 0.9195(5) 0.023(3) Uani 1 d . . H25A H 0.4680(5) 1.9022(8) 0.9322(5) 0.027 Uiso 1 calc R . H25B H 0.4123(5) 1.8836(8) 0.9523(5) 0.027 Uiso 1 calc R . C26 C 0.4373(6) 2.0417(8) 0.8583(5) 0.025(3) Uani 1 d . . C27 C 0.4290(6) 2.0453(9) 0.8036(6) 0.030(3) Uani 1 d . . H27A H 0.3893(6) 2.0260(9) 0.7755(6) 0.036 Uiso 1 calc R . C28 C 0.4773(6) 2.0764(9) 0.7899(6) 0.035(3) Uani 1 d . . H28A H 0.4704(6) 2.0794(9) 0.7524(6) 0.042 Uiso 1 calc R . C29 C 0.5352(7) 2.1030(9) 0.8296(6) 0.039(4) Uani 1 d . . H29A H 0.5696(7) 2.1200(9) 0.8201(6) 0.047 Uiso 1 calc R . C30 C 0.5431(6) 2.1048(10) 0.8834(7) 0.045(4) Uani 1 d . . H30A H 0.5820(6) 2.1273(10) 0.9112(7) 0.054 Uiso 1 calc R . C31 C 0.4945(6) 2.0740(10) 0.8972(6) 0.036(4) Uani 1 d . . H31A H 0.5006(6) 2.0753(10) 0.9346(6) 0.043 Uiso 1 calc R . C32 C 0.3772(5) 2.0684(9) 0.9301(5) 0.025(3) Uani 1 d . . C33 C 0.3605(6) 2.1618(9) 0.9147(5) 0.031(3) Uani 1 d . . H33A H 0.3543(6) 2.1809(9) 0.8788(5) 0.037 Uiso 1 calc R . C34 C 0.3528(7) 2.2267(9) 0.9489(6) 0.042(4) Uani 1 d . . H34A H 0.3427(7) 2.2900(9) 0.9371(6) 0.051 Uiso 1 calc R . C35 C 0.3597(6) 2.2003(11) 1.0013(6) 0.044(4) Uani 1 d . . H35A H 0.3526(6) 2.2445(11) 1.0248(6) 0.053 Uiso 1 calc R . C36 C 0.3771(6) 2.1088(10) 1.0183(5) 0.034(4) Uani 1 d . . H36A H 0.3840(6) 2.0900(10) 1.0544(5) 0.041 Uiso 1 calc R . C37 C 0.3845(6) 2.0440(10) 0.9819(5) 0.035(4) Uani 1 d . . H37A H 0.3950(6) 1.9807(10) 0.9935(5) 0.042 Uiso 1 calc R . C38 C 0.2435(6) 1.6478(9) 0.6813(6) 0.034(4) Uani 1 d . . C39 C 0.2655(6) 1.6787(11) 0.6432(5) 0.036(4) Uani 1 d . . H39A H 0.2700(6) 1.7442(11) 0.6386(5) 0.043 Uiso 1 calc R . C40 C 0.2815(7) 1.6134(12) 0.6110(6) 0.049(4) Uani 1 d . . H40A H 0.2933(7) 1.6346(12) 0.5827(6) 0.059 Uiso 1 calc R . C41 C 0.2799(8) 1.5186(12) 0.6211(6) 0.052(4) Uani 1 d . . H41A H 0.2942(8) 1.4747(12) 0.6017(6) 0.063 Uiso 1 calc R . C42 C 0.2580(7) 1.4868(11) 0.6581(7) 0.050(4) Uani 1 d . . H42A H 0.2558(7) 1.4211(11) 0.6638(7) 0.059 Uiso 1 calc R . C43 C 0.2391(6) 1.5506(10) 0.6876(6) 0.039(4) Uani 1 d . . H43A H 0.2227(6) 1.5280(10) 0.7127(6) 0.047 Uiso 1 calc R . C44 C 0.1584(7) 1.6736(9) 0.7329(6) 0.034(3) Uani 1 d . . C45 C 0.1634(6) 1.6222(9) 0.7777(6) 0.033(3) Uani 1 d . . H45A H 0.2041(6) 1.6145(9) 0.8074(6) 0.039 Uiso 1 calc R . C46 C 0.1093(7) 1.5810(10) 0.7800(6) 0.042(4) Uani 1 d . . H46A H 0.1135(7) 1.5464(10) 0.8117(6) 0.050 Uiso 1 calc R . C47 C 0.0505(7) 1.5893(12) 0.7376(7) 0.054(5) Uani 1 d . . H47A H 0.0138(7) 1.5612(12) 0.7395(7) 0.064 Uiso 1 calc R . C48 C 0.0458(7) 1.6382(13) 0.6931(8) 0.063(5) Uani 1 d . . H48A H 0.0050(7) 1.6442(13) 0.6632(8) 0.075 Uiso 1 calc R . C49 C 0.0991(7) 1.6807(10) 0.6891(7) 0.045(4) Uani 1 d . . H49A H 0.0945(7) 1.7139(10) 0.6569(7) 0.054 Uiso 1 calc R . C50 C 0.2001(6) 1.8345(9) 0.6881(5) 0.030(3) Uani 1 d . . H50A H 0.1575(6) 1.8521(9) 0.6865(5) 0.036 Uiso 1 calc R . H50B H 0.1959(6) 1.8232(9) 0.6503(5) 0.036 Uiso 1 calc R . C51 C 0.3189(6) 1.9017(8) 0.6936(5) 0.021(3) Uani 1 d . . C52 C 0.3716(6) 1.8498(9) 0.7250(6) 0.031(3) Uani 1 d . . H52A H 0.3771(6) 1.8321(9) 0.7609(6) 0.038 Uiso 1 calc R . C53 C 0.4168(6) 1.8221(9) 0.7067(5) 0.030(3) Uani 1 d . . H53A H 0.4529(6) 1.7866(9) 0.7301(5) 0.036 Uiso 1 calc R . C54 C 0.4100(6) 1.8455(9) 0.6545(6) 0.036(4) Uani 1 d . . H54A H 0.4409(6) 1.8258(9) 0.6414(6) 0.044 Uiso 1 calc R . C55 C 0.3582(6) 1.8973(9) 0.6220(6) 0.032(3) Uani 1 d . . H55A H 0.3527(6) 1.9138(9) 0.5859(6) 0.039 Uiso 1 calc R . C56 C 0.3135(6) 1.9261(9) 0.6413(5) 0.031(3) Uani 1 d . . H56A H 0.2782(6) 1.9634(9) 0.6184(5) 0.037 Uiso 1 calc R . C57 C 0.2204(7) 2.0309(10) 0.6748(6) 0.033(3) Uani 1 d . . C58 C 0.2542(8) 2.1166(11) 0.6911(8) 0.065(5) Uani 1 d . . H58A H 0.2925(8) 2.1181(11) 0.7237(8) 0.079 Uiso 1 calc R . C59 C 0.2335(11) 2.1976(13) 0.6614(9) 0.085(7) Uani 1 d . . H59A H 0.2548(11) 2.2555(13) 0.6752(9) 0.102 Uiso 1 calc R . C60 C 0.1828(12) 2.1946(14) 0.6126(9) 0.081(7) Uani 1 d . . H60A H 0.1716(12) 2.2483(14) 0.5894(9) 0.097 Uiso 1 calc R . C61 C 0.1480(12) 2.1153(18) 0.5967(8) 0.110(9) Uani 1 d . . H61A H 0.1092(12) 2.1160(18) 0.5645(8) 0.132 Uiso 1 calc R . C62 C 0.1680(8) 2.0304(11) 0.6272(7) 0.067(6) Uani 1 d . . H62A H 0.1446(8) 1.9739(11) 0.6141(7) 0.080 Uiso 1 calc R . C63 C 0.1137(6) 1.9988(9) 0.7488(5) 0.028(3) Uani 1 d . . C64 C 0.0871(8) 2.0625(11) 0.7068(6) 0.056(5) Uani 1 d . . H64A H 0.1077(8) 2.1214(11) 0.7090(6) 0.067 Uiso 1 calc R . C65 C 0.0308(8) 2.0427(13) 0.6612(7) 0.075(6) Uani 1 d . . H65A H 0.0146(8) 2.0860(13) 0.6316(7) 0.090 Uiso 1 calc R . C66 C -0.0014(7) 1.9598(13) 0.6593(7) 0.060(5) Uani 1 d . . H66A H -0.0417(7) 1.9485(13) 0.6297(7) 0.072 Uiso 1 calc R . C67 C 0.0245(7) 1.8931(11) 0.6999(6) 0.044(4) Uani 1 d . . H67A H 0.0032(7) 1.8347(11) 0.6975(6) 0.053 Uiso 1 calc R . C68 C 0.0831(6) 1.9123(9) 0.7453(6) 0.035(4) Uani 1 d . . H68A H 0.1016(6) 1.8665(9) 0.7733(6) 0.042 Uiso 1 calc R . C69 C 0.1711(6) 2.0096(9) 0.8683(6) 0.032(3) Uani 1 d . . C70 C 0.1101(7) 2.0031(10) 0.8666(6) 0.044(4) Uani 1 d . . H70A H 0.0741(7) 1.9996(10) 0.8323(6) 0.053 Uiso 1 calc R . C71 C 0.1014(8) 2.0018(11) 0.9156(7) 0.051(4) Uani 1 d . . H71A H 0.0593(8) 1.9981(11) 0.9144(7) 0.061 Uiso 1 calc R . C72 C 0.1522(8) 2.0058(12) 0.9641(6) 0.055(5) Uani 1 d . . H72A H 0.1459(8) 2.0045(12) 0.9970(6) 0.066 Uiso 1 calc R . C73 C 0.2136(7) 2.0118(13) 0.9666(6) 0.058(5) Uani 1 d . . H73A H 0.2497(7) 2.0148(13) 1.0009(6) 0.069 Uiso 1 calc R . C74 C 0.2210(7) 2.0132(11) 0.9196(6) 0.045(4) Uani 1 d . . H74A H 0.2633(7) 2.0170(11) 0.9216(6) 0.054 Uiso 1 calc R . C75 C 0.1968(6) 2.1518(9) 0.8064(6) 0.032(3) Uani 1 d . . H75A H 0.2353(6) 2.1720(9) 0.8387(6) 0.039 Uiso 1 calc R . H75B H 0.2031(6) 2.1697(9) 0.7732(6) 0.039 Uiso 1 calc R . C76 C 0.1021(9) 2.2895(13) 0.7432(8) 0.067(5) Uani 1 d . . C77 C 0.0347(8) 2.2952(14) 0.7066(9) 0.074(6) Uani 1 d . . H77A H 0.0042(8) 2.2700(14) 0.7186(9) 0.088 Uiso 1 calc R . C78 C 0.0153(8) 2.3312(13) 0.6608(8) 0.065(6) Uani 1 d . . H78A H -0.0294(8) 2.3277(13) 0.6384(8) 0.078 Uiso 1 calc R . C79 C 0.0549(9) 2.3781(15) 0.6385(11) 0.106(9) Uani 1 d . . H79A H 0.0383(9) 2.4068(15) 0.6033(11) 0.127 Uiso 1 calc R . C80 C 0.1161(10) 2.3778(12) 0.6713(9) 0.075(6) Uani 1 d . . H80A H 0.1444(10) 2.4098(12) 0.6592(9) 0.089 Uiso 1 calc R . C81 C 0.1448(9) 2.3308(12) 0.7263(8) 0.069(5) Uani 1 d . . H81A H 0.1897(9) 2.3297(12) 0.7480(8) 0.083 Uiso 1 calc R . C82 C 0.1657(8) 2.2999(13) 0.8601(11) 0.088(7) Uani 1 d . . C83 C 0.1915(9) 2.3863(13) 0.8591(9) 0.072(6) Uani 1 d . . H83A H 0.1885(9) 2.4097(13) 0.8248(9) 0.087 Uiso 1 calc R . C84 C 0.2244(11) 2.4464(13) 0.9092(10) 0.095(7) Uani 1 d . . H84A H 0.2450(11) 2.5032(13) 0.9069(10) 0.114 Uiso 1 calc R . C85 C 0.2242(10) 2.4177(14) 0.9595(10) 0.082(6) Uani 1 d . . H85A H 0.2389(10) 2.4587(14) 0.9903(10) 0.098 Uiso 1 calc R . C86 C 0.2021(10) 2.3275(19) 0.9633(9) 0.102(8) Uani 1 d . . H86A H 0.2069(10) 2.3043(19) 0.9982(9) 0.123 Uiso 1 calc R . C87 C 0.1728(12) 2.2704(17) 0.9169(10) 0.114(9) Uani 1 d . . H87A H 0.1566(12) 2.2107(17) 0.9211(10) 0.136 Uiso 1 calc R . Cl1 Cl -0.0409(12) 2.1082(14) 0.9655(7) 0.313(15) Uani 0.693(12) d PD 1 Cl2 Cl -0.0558(7) 2.3017(12) 0.9678(5) 0.188(7) Uani 0.693(12) d PD 1 C88 C -0.0918(12) 2.1941(13) 0.9732(16) 0.134(15) Uani 0.693(12) d PD 1 H88A H -0.0938(12) 2.1885(13) 1.0093(16) 0.161 Uiso 0.693(12) calc PR 1 H88B H -0.1356(12) 2.1885(13) 0.9439(16) 0.161 Uiso 0.693(12) calc PR 1 C89 C 0.0236(37) 2.2569(35) 0.9676(32) 0.119(28) Uiso 0.307(12) d PD 2 H89A H 0.0655(90) 2.2360(79) 0.9699(234) 0.178 Uiso 0.307(12) calc PR 2 H89B H -0.0093(191) 2.2432(56) 0.9309(94) 0.178 Uiso 0.307(12) calc PR 2 H89C H 0.0134(270) 2.2236(43) 0.9951(142) 0.178 Uiso 0.307(12) calc PR 2 C90 C 0.0256(24) 2.3637(31) 0.9782(22) 0.058(16) Uiso 0.307(12) d PD 2 H90A H 0.0698(24) 2.3704(31) 1.0067(22) 0.070 Uiso 0.307(12) calc PR 2 H90B H 0.0279(24) 2.3878(31) 0.9444(22) 0.070 Uiso 0.307(12) calc PR 2 C91 C -0.0067(28) 2.4472(16) 0.9928(29) 0.093(23) Uiso 0.307(12) d PD 2 H91A H -0.0144(28) 2.4227(16) 1.0242(29) 0.111 Uiso 0.307(12) calc PR 2 H91B H -0.0495(28) 2.4486(16) 0.9618(29) 0.111 Uiso 0.307(12) calc PR 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 Pt1 0.0232(3) 0.0191(3) 0.0271(3) 0.0002(2) 0.0128(2) 0.0016(2) Pt2 0.0214(3) 0.0177(2) 0.0296(3) -0.0001(2) 0.0131(2) 0.0006(2) B1 0.035(10) 0.037(10) 0.034(10) 0.001(8) 0.018(9) 0.004(8) B2 0.043(10) 0.035(9) 0.014(8) 0.007(7) 0.024(7) 0.006(8) O1 0.025(5) 0.025(5) 0.043(6) 0.006(4) 0.018(5) 0.005(4) O2 0.027(5) 0.026(5) 0.036(6) 0.011(4) 0.022(4) 0.003(4) O3 0.040(5) 0.017(5) 0.046(6) -0.002(4) 0.027(5) 0.002(4) O4 0.077(8) 0.024(5) 0.071(8) 0.001(5) 0.058(7) 0.002(5) P1 0.023(2) 0.019(2) 0.030(2) 0.0029(15) 0.012(2) 0.0034(14) P2 0.023(2) 0.020(2) 0.033(2) -0.003(2) 0.014(2) -0.0009(14) P3 0.022(2) 0.026(2) 0.031(2) -0.002(2) 0.011(2) -0.0019(14) P4 0.024(2) 0.022(2) 0.031(2) 0.000(2) 0.013(2) 0.003(2) P5 0.022(2) 0.026(2) 0.032(2) 0.001(2) 0.013(2) 0.0043(15) P6 0.060(3) 0.046(3) 0.077(3) -0.003(2) 0.039(3) 0.002(2) C1 0.034(8) 0.020(7) 0.044(8) 0.013(7) 0.028(7) 0.006(7) C2 0.039(9) 0.048(10) 0.059(11) 0.002(8) 0.032(8) -0.007(7) C3 0.046(11) 0.066(12) 0.070(13) 0.015(10) 0.037(10) -0.012(9) C4 0.067(12) 0.064(12) 0.055(11) 0.020(9) 0.045(10) -0.001(10) C5 0.052(10) 0.042(10) 0.039(9) 0.007(8) 0.019(8) 0.007(8) C6 0.035(8) 0.026(8) 0.051(10) -0.002(7) 0.026(8) -0.002(6) C7 0.030(8) 0.025(7) 0.032(8) -0.001(6) 0.020(7) -0.006(6) C8 0.041(9) 0.032(9) 0.077(11) -0.008(9) 0.041(9) -0.013(7) C9 0.051(10) 0.023(8) 0.051(10) -0.007(7) 0.034(8) 0.012(7) C10 0.112(15) 0.024(8) 0.061(11) 0.007(8) 0.058(11) 0.021(9) C11 0.120(15) 0.028(9) 0.077(12) 0.029(9) 0.084(12) 0.024(9) C12 0.055(10) 0.016(8) 0.049(9) 0.002(7) 0.029(8) 0.011(7) C13 0.048(10) 0.029(8) 0.043(9) -0.010(7) 0.024(8) 0.016(7) C14 0.048(10) 0.039(9) 0.052(10) 0.021(8) 0.023(9) -0.001(8) C15 0.033(9) 0.067(12) 0.048(10) 0.018(9) 0.017(8) 0.006(8) C16 0.062(12) 0.087(15) 0.032(9) 0.023(10) 0.021(9) 0.042(11) C17 0.072(12) 0.039(9) 0.070(12) 0.024(10) 0.051(10) 0.007(9) C18 0.020(7) 0.032(8) 0.038(9) -0.005(7) 0.016(6) 0.009(6) C19 0.013(6) 0.031(7) 0.031(7) -0.006(7) 0.005(5) -0.004(6) C20 0.039(9) 0.028(8) 0.044(9) -0.010(7) 0.016(8) 0.003(6) C21 0.040(9) 0.025(8) 0.075(12) 0.000(8) 0.028(9) 0.007(7) C22 0.033(9) 0.055(10) 0.059(11) -0.015(9) 0.032(8) 0.006(8) C23 0.034(8) 0.045(9) 0.042(9) -0.005(8) 0.028(7) -0.009(7) C24 0.048(9) 0.032(8) 0.033(8) 0.000(7) 0.025(8) -0.003(7) C25 0.020(7) 0.018(7) 0.034(8) 0.005(6) 0.015(6) 0.007(5) C26 0.026(7) 0.020(7) 0.037(8) 0.001(6) 0.021(7) 0.001(6) C27 0.027(7) 0.025(8) 0.041(9) -0.011(6) 0.016(7) 0.007(6) C28 0.037(8) 0.028(8) 0.051(9) 0.004(7) 0.028(8) 0.008(7) C29 0.036(9) 0.036(9) 0.059(11) 0.000(8) 0.034(8) -0.008(7) C30 0.026(8) 0.031(9) 0.071(12) 0.003(8) 0.014(8) -0.004(6) C31 0.022(7) 0.050(9) 0.044(9) -0.004(8) 0.021(7) -0.012(7) C32 0.027(7) 0.021(7) 0.035(8) 0.004(7) 0.021(6) 0.002(6) C33 0.045(9) 0.031(8) 0.030(8) 0.003(7) 0.028(7) 0.003(6) C34 0.055(10) 0.017(8) 0.053(10) -0.011(7) 0.020(8) 0.000(7) C35 0.040(9) 0.044(10) 0.050(11) -0.014(8) 0.019(8) -0.003(8) C36 0.028(8) 0.048(10) 0.027(8) -0.024(7) 0.011(7) -0.012(7) C37 0.039(9) 0.030(8) 0.036(9) 0.008(7) 0.014(7) -0.001(6) C38 0.032(8) 0.029(8) 0.041(9) -0.006(7) 0.016(7) -0.002(6) C39 0.029(8) 0.047(9) 0.029(8) -0.018(7) 0.010(7) -0.001(7) C40 0.062(11) 0.051(11) 0.041(10) -0.013(9) 0.027(9) 0.003(9) C41 0.067(12) 0.051(11) 0.044(10) -0.024(9) 0.028(9) 0.005(9) C42 0.062(11) 0.031(9) 0.058(11) -0.019(8) 0.027(9) 0.001(8) C43 0.050(10) 0.031(9) 0.040(9) -0.002(7) 0.024(8) 0.002(7) C44 0.039(9) 0.027(8) 0.046(9) -0.004(7) 0.027(8) -0.003(7) C45 0.019(7) 0.033(8) 0.041(9) -0.009(7) 0.007(7) 0.009(6) C46 0.048(10) 0.042(10) 0.044(9) -0.009(8) 0.028(8) -0.025(8) C47 0.036(10) 0.063(12) 0.072(12) -0.009(10) 0.033(10) -0.023(8) C48 0.021(9) 0.079(14) 0.075(13) 0.002(11) 0.006(9) -0.014(9) C49 0.045(10) 0.027(9) 0.063(11) 0.000(8) 0.022(9) -0.001(7) C50 0.027(8) 0.031(8) 0.034(8) -0.004(6) 0.016(7) 0.001(6) C51 0.025(7) 0.018(7) 0.021(7) -0.011(6) 0.010(6) -0.003(5) C52 0.034(8) 0.027(8) 0.039(9) 0.004(7) 0.022(7) -0.007(6) C53 0.030(8) 0.031(8) 0.032(8) 0.005(7) 0.016(7) -0.001(6) C54 0.033(9) 0.032(8) 0.054(10) -0.017(8) 0.028(8) -0.006(7) C55 0.036(8) 0.037(9) 0.037(8) -0.008(7) 0.028(7) -0.006(7) C56 0.030(8) 0.029(8) 0.039(8) 0.003(7) 0.020(7) 0.006(6) C57 0.041(9) 0.036(9) 0.034(9) 0.010(7) 0.028(8) 0.012(7) C58 0.056(11) 0.036(10) 0.093(14) 0.039(10) 0.019(10) 0.008(8) C59 0.137(20) 0.033(11) 0.082(16) 0.009(11) 0.043(15) 0.002(12) C60 0.153(22) 0.043(12) 0.059(14) 0.031(11) 0.056(15) 0.025(13) C61 0.135(22) 0.097(19) 0.055(14) 0.024(14) -0.003(14) 0.046(17) C62 0.080(13) 0.033(10) 0.053(11) 0.001(8) -0.009(10) 0.002(9) C63 0.028(8) 0.029(8) 0.035(8) -0.001(7) 0.022(7) 0.010(6) C64 0.069(12) 0.033(9) 0.049(10) 0.009(9) 0.006(9) 0.006(9) C65 0.048(11) 0.070(14) 0.064(13) 0.018(10) -0.019(10) 0.002(10) C66 0.034(10) 0.082(15) 0.051(11) -0.012(10) 0.004(9) -0.001(9) C67 0.036(9) 0.045(10) 0.050(10) -0.014(8) 0.016(8) -0.002(7) C68 0.033(8) 0.031(9) 0.038(9) 0.003(7) 0.012(7) 0.004(6) C69 0.031(8) 0.027(8) 0.041(9) -0.002(7) 0.020(7) 0.007(6) C70 0.030(8) 0.058(11) 0.056(10) -0.016(8) 0.029(8) -0.004(7) C71 0.045(10) 0.064(12) 0.062(12) -0.011(9) 0.039(10) -0.009(8) C72 0.071(12) 0.078(13) 0.035(10) -0.001(9) 0.040(10) -0.013(10) C73 0.042(10) 0.105(15) 0.026(9) -0.006(9) 0.013(8) -0.006(10) C74 0.028(9) 0.059(11) 0.046(10) -0.011(9) 0.014(8) -0.012(7) C75 0.036(8) 0.024(8) 0.037(8) -0.005(6) 0.014(7) 0.007(6) C76 0.074(13) 0.058(12) 0.090(15) 0.008(11) 0.056(12) 0.009(10) C77 0.032(11) 0.076(14) 0.117(18) -0.018(14) 0.036(12) -0.013(9) C78 0.030(10) 0.071(13) 0.085(15) 0.045(11) 0.014(10) 0.011(9) C79 0.047(13) 0.081(16) 0.184(26) 0.030(17) 0.041(15) 0.037(12) C80 0.093(16) 0.048(12) 0.112(17) 0.006(12) 0.072(14) -0.006(11) C81 0.065(13) 0.062(13) 0.089(15) 0.006(11) 0.041(12) 0.008(10) C82 0.044(11) 0.039(11) 0.162(23) -0.002(13) 0.023(13) 0.016(9) C83 0.084(14) 0.045(12) 0.099(16) 0.011(12) 0.049(12) 0.007(10) C84 0.131(20) 0.034(12) 0.124(20) -0.012(13) 0.058(17) 0.019(12) C85 0.118(18) 0.054(14) 0.100(18) -0.012(13) 0.072(15) -0.013(12) C86 0.103(19) 0.145(25) 0.061(14) -0.036(16) 0.037(14) -0.011(16) C87 0.170(26) 0.090(19) 0.083(17) 0.028(15) 0.054(18) 0.010(17) Cl1 0.527(35) 0.275(23) 0.203(16) 0.083(15) 0.218(20) 0.234(24) Cl2 0.216(15) 0.235(17) 0.134(10) 0.022(10) 0.096(10) 0.040(12) C88 0.098(29) 0.176(43) 0.125(33) 0.019(30) 0.042(25) -0.024(28) _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 B1 2.14(2) . ? Pt1 P5 2.303(3) . ? Pt1 P4 2.304(3) . ? Pt1 P2 2.305(3) . ? Pt1 Pt2 2.7690(8) . ? Pt2 B2 2.06(2) . ? Pt2 P1 2.281(3) . ? Pt2 P3 2.290(3) . ? Pt2 B1 2.51(2) . ? B1 O2 1.40(2) . ? B1 O1 1.43(2) . ? B2 O3 1.39(2) . ? B2 O4 1.40(2) . ? O1 C1 1.359(14) . ? O2 C6 1.389(14) . ? O3 C7 1.389(14) . ? O4 C12 1.395(15) . ? P1 C25 1.840(12) . ? P1 C19 1.847(12) . ? P1 C13 1.860(15) . ? P2 C32 1.854(13) . ? P2 C26 1.855(12) . ? P2 C25 1.857(11) . ? P3 C50 1.820(13) . ? P3 C44 1.824(14) . ? P3 C38 1.844(14) . ? P4 C57 1.828(13) . ? P4 C51 1.845(12) . ? P4 C50 1.856(13) . ? P5 C69 1.847(14) . ? P5 C63 1.847(13) . ? P5 C75 1.864(13) . ? P6 C82 1.79(2) . ? P6 C75 1.842(13) . ? P6 C76 1.86(2) . ? C1 C2 1.36(2) . ? C1 C6 1.37(2) . ? C2 C3 1.40(2) . ? C3 C4 1.37(2) . ? C4 C5 1.40(2) . ? C5 C6 1.37(2) . ? C7 C12 1.36(2) . ? C7 C8 1.38(2) . ? C8 C9 1.38(2) . ? C9 C10 1.38(2) . ? C10 C11 1.41(2) . ? C11 C12 1.40(2) . ? C13 C14 1.38(2) . ? C13 C18 1.38(2) . ? C14 C15 1.37(2) . ? C15 C16 1.39(2) . ? C16 C17 1.37(2) . ? C17 C18 1.37(2) . ? C19 C24 1.37(2) . ? C19 C20 1.39(2) . ? C20 C21 1.40(2) . ? C21 C22 1.37(2) . ? C22 C23 1.37(2) . ? C23 C24 1.37(2) . ? C26 C31 1.37(2) . ? C26 C27 1.40(2) . ? C27 C28 1.37(2) . ? C28 C29 1.37(2) . ? C29 C30 1.38(2) . ? C30 C31 1.38(2) . ? C32 C37 1.37(2) . ? C32 C33 1.40(2) . ? C33 C34 1.36(2) . ? C34 C35 1.39(2) . ? C35 C36 1.38(2) . ? C36 C37 1.40(2) . ? C38 C39 1.38(2) . ? C38 C43 1.40(2) . ? C39 C40 1.41(2) . ? C40 C41 1.38(2) . ? C41 C42 1.36(2) . ? C42 C43 1.38(2) . ? C44 C45 1.36(2) . ? C44 C49 1.39(2) . ? C45 C46 1.39(2) . ? C46 C47 1.36(2) . ? C47 C48 1.34(2) . ? C48 C49 1.40(2) . ? C51 C52 1.37(2) . ? C51 C56 1.40(2) . ? C52 C53 1.37(2) . ? C53 C54 1.38(2) . ? C54 C55 1.36(2) . ? C55 C56 1.38(2) . ? C57 C62 1.34(2) . ? C57 C58 1.41(2) . ? C58 C59 1.37(2) . ? C59 C60 1.35(3) . ? C60 C61 1.34(3) . ? C61 C62 1.42(2) . ? C63 C64 1.37(2) . ? C63 C68 1.40(2) . ? C64 C65 1.39(2) . ? C65 C66 1.38(2) . ? C66 C67 1.38(2) . ? C67 C68 1.42(2) . ? C69 C74 1.38(2) . ? C69 C70 1.38(2) . ? C70 C71 1.40(2) . ? C71 C72 1.34(2) . ? C72 C73 1.38(2) . ? C73 C74 1.33(2) . ? C76 C81 1.37(2) . ? C76 C77 1.45(2) . ? C77 C78 1.23(2) . ? C78 C79 1.44(3) . ? C79 C80 1.31(2) . ? C80 C81 1.50(2) . ? C82 C83 1.37(2) . ? C82 C87 1.52(3) . ? C83 C84 1.50(3) . ? C84 C85 1.41(3) . ? C85 C86 1.40(3) . ? C86 C87 1.40(3) . ? Cl1 C88 1.755(10) . ? Cl2 C88 1.771(10) . ? C89 C90 1.54(3) . ? C90 C91 1.53(3) . ? C91 C91 1.55(3) . ? 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 B1 Pt1 P5 89.8(4) . . ? B1 Pt1 P4 131.5(4) . . ? P5 Pt1 P4 100.63(12) . . ? B1 Pt1 P2 96.6(4) . . ? P5 Pt1 P2 114.66(12) . . ? P4 Pt1 P2 120.18(12) . . ? B1 Pt1 Pt2 59.9(4) . . ? P5 Pt1 Pt2 140.02(9) . . ? P4 Pt1 Pt2 84.49(9) . . ? P2 Pt1 Pt2 95.51(8) . . ? B2 Pt2 P1 88.7(4) . . ? B2 Pt2 P3 88.8(4) . . ? P1 Pt2 P3 172.43(12) . . ? B2 Pt2 B1 136.9(5) . . ? P1 Pt2 B1 87.2(4) . . ? P3 Pt2 B1 99.4(4) . . ? B2 Pt2 Pt1 175.5(4) . . ? P1 Pt2 Pt1 92.89(8) . . ? P3 Pt2 Pt1 89.06(8) . . ? B1 Pt2 Pt1 47.5(4) . . ? O2 B1 O1 109.3(12) . . ? O2 B1 Pt1 127.4(11) . . ? O1 B1 Pt1 120.8(10) . . ? O2 B1 Pt2 106.4(9) . . ? O1 B1 Pt2 109.0(9) . . ? Pt1 B1 Pt2 72.7(5) . . ? O3 B2 O4 109.4(12) . . ? O3 B2 Pt2 126.5(10) . . ? O4 B2 Pt2 124.1(9) . . ? C1 O1 B1 105.6(10) . . ? C6 O2 B1 105.3(11) . . ? C7 O3 B2 106.8(10) . . ? C12 O4 B2 105.0(10) . . ? C25 P1 C19 104.2(6) . . ? C25 P1 C13 101.2(6) . . ? C19 P1 C13 101.3(6) . . ? C25 P1 Pt2 117.1(4) . . ? C19 P1 Pt2 112.6(4) . . ? C13 P1 Pt2 118.3(5) . . ? C32 P2 C26 98.4(6) . . ? C32 P2 C25 99.3(6) . . ? C26 P2 C25 100.1(5) . . ? C32 P2 Pt1 119.4(4) . . ? C26 P2 Pt1 123.9(4) . . ? C25 P2 Pt1 111.5(4) . . ? C50 P3 C44 106.4(6) . . ? C50 P3 C38 102.8(6) . . ? C44 P3 C38 101.2(6) . . ? C50 P3 Pt2 114.9(4) . . ? C44 P3 Pt2 115.2(5) . . ? C38 P3 Pt2 114.6(4) . . ? C57 P4 C51 98.7(6) . . ? C57 P4 C50 102.6(6) . . ? C51 P4 C50 99.6(6) . . ? C57 P4 Pt1 121.1(4) . . ? C51 P4 Pt1 124.3(4) . . ? C50 P4 Pt1 106.8(4) . . ? C69 P5 C63 104.3(6) . . ? C69 P5 C75 99.0(6) . . ? C63 P5 C75 101.9(6) . . ? C69 P5 Pt1 115.5(4) . . ? C63 P5 Pt1 116.3(4) . . ? C75 P5 Pt1 117.4(4) . . ? C82 P6 C75 100.7(7) . . ? C82 P6 C76 103.1(10) . . ? C75 P6 C76 102.8(7) . . ? C2 C1 O1 129.5(13) . . ? C2 C1 C6 120.5(13) . . ? O1 C1 C6 110.0(11) . . ? C1 C2 C3 118.0(14) . . ? C4 C3 C2 120.8(14) . . ? C3 C4 C5 121.6(15) . . ? C6 C5 C4 115.8(14) . . ? C5 C6 C1 123.3(13) . . ? C5 C6 O2 126.8(13) . . ? C1 C6 O2 109.8(12) . . ? C12 C7 C8 121.2(12) . . ? C12 C7 O3 108.4(11) . . ? C8 C7 O3 130.4(12) . . ? C9 C8 C7 116.5(13) . . ? C8 C9 C10 122.7(13) . . ? C9 C10 C11 121.5(14) . . ? C12 C11 C10 113.9(14) . . ? C7 C12 O4 110.3(11) . . ? C7 C12 C11 124.2(13) . . ? O4 C12 C11 125.5(13) . . ? C14 C13 C18 120.5(14) . . ? C14 C13 P1 118.2(11) . . ? C18 C13 P1 121.3(11) . . ? C15 C14 C13 120.2(14) . . ? C14 C15 C16 119.3(15) . . ? C17 C16 C15 120.3(15) . . ? C16 C17 C18 120.6(15) . . ? C17 C18 C13 119.1(14) . . ? C24 C19 C20 119.9(12) . . ? C24 C19 P1 122.4(10) . . ? C20 C19 P1 117.7(10) . . ? C19 C20 C21 118.9(13) . . ? C22 C21 C20 120.4(13) . . ? C21 C22 C23 119.8(13) . . ? C24 C23 C22 120.6(13) . . ? C23 C24 C19 120.4(13) . . ? P1 C25 P2 116.1(6) . . ? C31 C26 C27 117.4(11) . . ? C31 C26 P2 123.0(10) . . ? C27 C26 P2 119.4(10) . . ? C28 C27 C26 120.9(13) . . ? C29 C28 C27 120.8(13) . . ? C28 C29 C30 119.0(13) . . ? C29 C30 C31 120.1(14) . . ? C26 C31 C30 121.6(13) . . ? C37 C32 C33 116.4(12) . . ? C37 C32 P2 125.7(10) . . ? C33 C32 P2 117.1(10) . . ? C34 C33 C32 122.8(13) . . ? C33 C34 C35 120.0(13) . . ? C36 C35 C34 118.9(14) . . ? C35 C36 C37 119.4(14) . . ? C32 C37 C36 122.5(13) . . ? C39 C38 C43 117.9(13) . . ? C39 C38 P3 122.7(11) . . ? C43 C38 P3 119.0(11) . . ? C38 C39 C40 120.3(14) . . ? C41 C40 C39 119.3(15) . . ? C42 C41 C40 121.0(15) . . ? C41 C42 C43 119.5(15) . . ? C42 C43 C38 121.6(14) . . ? C45 C44 C49 118.8(13) . . ? C45 C44 P3 121.3(11) . . ? C49 C44 P3 119.9(11) . . ? C44 C45 C46 120.5(13) . . ? C47 C46 C45 121.2(14) . . ? C48 C47 C46 118.3(14) . . ? C47 C48 C49 122.2(15) . . ? C44 C49 C48 119.0(15) . . ? P3 C50 P4 109.3(7) . . ? C52 C51 C56 116.1(11) . . ? C52 C51 P4 120.2(10) . . ? C56 C51 P4 123.6(9) . . ? C51 C52 C53 122.8(13) . . ? C52 C53 C54 120.2(13) . . ? C55 C54 C53 118.7(13) . . ? C54 C55 C56 120.4(13) . . ? C55 C56 C51 121.7(12) . . ? C62 C57 C58 117.4(14) . . ? C62 C57 P4 128.0(12) . . ? C58 C57 P4 114.5(11) . . ? C59 C58 C57 122.1(17) . . ? C60 C59 C58 119.5(19) . . ? C61 C60 C59 119.7(18) . . ? C60 C61 C62 121.4(19) . . ? C57 C62 C61 119.4(17) . . ? C64 C63 C68 118.9(13) . . ? C64 C63 P5 122.2(11) . . ? C68 C63 P5 118.9(10) . . ? C63 C64 C65 121.5(16) . . ? C66 C65 C64 119.6(16) . . ? C65 C66 C67 120.5(15) . . ? C66 C67 C68 119.4(14) . . ? C63 C68 C67 119.9(13) . . ? C74 C69 C70 116.6(13) . . ? C74 C69 P5 117.8(10) . . ? C70 C69 P5 125.5(11) . . ? C69 C70 C71 120.0(14) . . ? C72 C71 C70 120.1(14) . . ? C71 C72 C73 120.8(14) . . ? C74 C73 C72 118.3(15) . . ? C73 C74 C69 124.2(14) . . ? P6 C75 P5 115.0(7) . . ? C81 C76 C77 117.4(18) . . ? C81 C76 P6 123.1(15) . . ? C77 C76 P6 119.2(15) . . ? C78 C77 C76 123.0(19) . . ? C77 C78 C79 125.0(19) . . ? C80 C79 C78 113.8(22) . . ? C79 C80 C81 125.0(19) . . ? C76 C81 C80 115.6(18) . . ? C83 C82 C87 113.5(21) . . ? C83 C82 P6 130.8(21) . . ? C87 C82 P6 115.7(16) . . ? C82 C83 C84 123.7(21) . . ? C85 C84 C83 119.4(20) . . ? C86 C85 C84 118.6(21) . . ? C85 C86 C87 121.5(23) . . ? C86 C87 C82 122.8(22) . . ? Cl1 C88 Cl2 103.8(13) . . ? C91 C90 C89 146.2(49) . . ? C90 C91 C91 138.5(62) . . ? _refine_diff_density_max 1.627 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.190 #=END data_15 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H56 B2 O4 P2 Pt' _chemical_formula_weight 975.58 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 16.752(3) _cell_length_b 12.174(2) _cell_length_c 22.850(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.428(10) _cell_angle_gamma 90.00 _cell_volume 4337.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method ? _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 3.352 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.593986 _exptl_absorpt_correction_T_max 0.781329 _exptl_special_details ; SADABS (Sheldrick, 1996)s ; _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27083 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9917 _reflns_number_observed 7258 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+0.0000P] 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 'see text' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00020(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9916 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_obs 0.0356 _refine_ls_wR_factor_all 0.0608 _refine_ls_wR_factor_obs 0.0530 _refine_ls_goodness_of_fit_all 0.987 _refine_ls_goodness_of_fit_obs 1.034 _refine_ls_restrained_S_all 1.004 _refine_ls_restrained_S_obs 1.034 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.399110(10) 0.152550(12) 0.145160(7) 0.01971(5) Uani 1 d . . B1 B 0.4544(3) 0.0066(3) 0.1831(2) 0.0209(10) Uani 1 d . . B2 B 0.3671(3) 0.0415(3) 0.0728(2) 0.0230(10) Uani 1 d . . O1 O 0.5270(2) -0.0449(2) 0.17720(12) 0.0271(6) Uani 1 d . . O2 O 0.4268(2) -0.0590(2) 0.22262(12) 0.0237(6) Uani 1 d . . O3 O 0.4053(2) 0.0420(2) 0.02666(12) 0.0282(6) Uani 1 d . . O4 O 0.3089(2) -0.0473(2) 0.05929(13) 0.0343(7) Uani 1 d . . P1 P 0.31499(7) 0.29068(8) 0.07616(5) 0.0208(2) Uani 1 d . . P2 P 0.46367(7) 0.23822(8) 0.24316(5) 0.0207(2) Uani 1 d . . C1 C 0.5428(3) -0.1380(3) 0.2144(2) 0.0266(9) Uani 1 d . . C2 C 0.6080(3) -0.2136(3) 0.2258(2) 0.0374(11) Uani 1 d . . H2A H 0.6480(3) -0.2093(3) 0.2064(2) 0.045 Uiso 1 calc R . C3 C 0.6105(3) -0.2974(3) 0.2686(2) 0.0461(13) Uani 1 d . . H3A H 0.6530(3) -0.3507(3) 0.2777(2) 0.055 Uiso 1 calc R . C4 C 0.5514(3) -0.3028(3) 0.2977(2) 0.0434(13) Uani 1 d . . H4A H 0.5559(3) -0.3586(3) 0.3266(2) 0.052 Uiso 1 calc R . C5 C 0.4855(3) -0.2268(3) 0.2848(2) 0.0341(11) Uani 1 d . . H5A H 0.4451(3) -0.2306(3) 0.3038(2) 0.041 Uiso 1 calc R . C6 C 0.4829(3) -0.1455(3) 0.2424(2) 0.0247(9) Uani 1 d . . C7 C 0.3668(3) -0.0408(3) -0.0153(2) 0.0282(10) Uani 1 d . . C8 C 0.3802(3) -0.0703(4) -0.0693(2) 0.0387(11) Uani 1 d . . H8A H 0.4202(3) -0.0344(4) -0.0820(2) 0.046 Uiso 1 calc R . C9 C 0.3309(3) -0.1564(4) -0.1038(2) 0.0493(13) Uani 1 d . . H9A H 0.3377(3) -0.1788(4) -0.1406(2) 0.059 Uiso 1 calc R . C10 C 0.2721(4) -0.2094(4) -0.0847(2) 0.0536(15) Uani 1 d . . H10A H 0.2405(4) -0.2673(4) -0.1088(2) 0.064 Uiso 1 calc R . C11 C 0.2583(3) -0.1789(3) -0.0303(2) 0.0474(13) Uani 1 d . . H11A H 0.2179(3) -0.2137(3) -0.0176(2) 0.057 Uiso 1 calc R . C12 C 0.3085(3) -0.0935(3) 0.0036(2) 0.0328(10) Uani 1 d . . C13 C 0.3486(3) 0.3004(3) 0.0074(2) 0.0230(9) Uani 1 d . . H13A H 0.3315(3) 0.2292(3) -0.0134(2) 0.028 Uiso 1 calc R . C14 C 0.4453(3) 0.3023(3) 0.0239(2) 0.0300(10) Uani 1 d . . H14A H 0.4684(3) 0.3699(3) 0.0462(2) 0.036 Uiso 1 calc R . H14B H 0.4710(3) 0.2415(3) 0.0520(2) 0.036 Uiso 1 calc R . C15 C 0.4696(3) 0.2942(4) -0.0329(2) 0.0387(11) Uani 1 d . . H15A H 0.4583(3) 0.2202(4) -0.0496(2) 0.046 Uiso 1 calc R . H15B H 0.5307(3) 0.3075(4) -0.0205(2) 0.046 Uiso 1 calc R . C16 C 0.4219(3) 0.3742(4) -0.0837(2) 0.0420(12) Uani 1 d . . H16A H 0.4352(3) 0.3592(4) -0.1208(2) 0.050 Uiso 1 calc R . H16B H 0.4414(3) 0.4480(4) -0.0697(2) 0.050 Uiso 1 calc R . C17 C 0.3263(3) 0.3686(4) -0.1009(2) 0.0388(11) Uani 1 d . . H17A H 0.3053(3) 0.2985(4) -0.1207(2) 0.047 Uiso 1 calc R . H17B H 0.2991(3) 0.4261(4) -0.1310(2) 0.047 Uiso 1 calc R . C18 C 0.3022(3) 0.3818(3) -0.0436(2) 0.0340(11) Uani 1 d . . H18A H 0.3161(3) 0.4558(3) -0.0272(2) 0.041 Uiso 1 calc R . H18B H 0.2408(3) 0.3717(3) -0.0557(2) 0.041 Uiso 1 calc R . C19 C 0.3109(3) 0.4336(3) 0.1053(2) 0.0218(9) Uani 1 d . . H19A H 0.3036(3) 0.4233(3) 0.1456(2) 0.026 Uiso 1 calc R . C20 C 0.3948(3) 0.4922(3) 0.1221(2) 0.0339(11) Uani 1 d . . H20A H 0.4066(3) 0.5049(3) 0.0841(2) 0.041 Uiso 1 calc R . H20B H 0.4400(3) 0.4456(3) 0.1495(2) 0.041 Uiso 1 calc R . C21 C 0.3962(3) 0.6027(3) 0.1550(2) 0.0337(11) Uani 1 d . . H21A H 0.3931(3) 0.5894(3) 0.1960(2) 0.040 Uiso 1 calc R . H21B H 0.4498(3) 0.6401(3) 0.1613(2) 0.040 Uiso 1 calc R . C22 C 0.3235(3) 0.6744(3) 0.1177(2) 0.0367(11) Uani 1 d . . H22A H 0.3316(3) 0.6974(3) 0.0796(2) 0.044 Uiso 1 calc R . H22B H 0.3231(3) 0.7398(3) 0.1419(2) 0.044 Uiso 1 calc R . C23 C 0.2387(3) 0.6170(3) 0.1005(2) 0.0372(11) Uani 1 d . . H23A H 0.1940(3) 0.6644(3) 0.0732(2) 0.045 Uiso 1 calc R . H23B H 0.2266(3) 0.6043(3) 0.1384(2) 0.045 Uiso 1 calc R . C24 C 0.2360(3) 0.5075(3) 0.0675(2) 0.0308(10) Uani 1 d . . H24A H 0.2382(3) 0.5207(3) 0.0262(2) 0.037 Uiso 1 calc R . H24B H 0.1823(3) 0.4705(3) 0.0617(2) 0.037 Uiso 1 calc R . C25 C 0.1997(3) 0.2571(3) 0.0403(2) 0.0244(9) Uani 1 d . . H25A H 0.1738(3) 0.3185(3) 0.0120(2) 0.029 Uiso 1 calc R . C26 C 0.1546(3) 0.2554(3) 0.0873(2) 0.0293(10) Uani 1 d . . H26A H 0.1784(3) 0.1966(3) 0.1173(2) 0.035 Uiso 1 calc R . H26B H 0.1658(3) 0.3241(3) 0.1104(2) 0.035 Uiso 1 calc R . C27 C 0.0599(3) 0.2395(4) 0.0569(2) 0.0379(11) Uani 1 d . . H27A H 0.0360(3) 0.2316(4) 0.0895(2) 0.045 Uiso 1 calc R . H27B H 0.0349(3) 0.3047(4) 0.0328(2) 0.045 Uiso 1 calc R . C28 C 0.0349(3) 0.1419(4) 0.0145(2) 0.0407(11) Uani 1 d . . H28A H -0.0266(3) 0.1430(4) -0.0083(2) 0.049 Uiso 1 calc R . H28B H 0.0488(3) 0.0755(4) 0.0397(2) 0.049 Uiso 1 calc R . C29 C 0.0801(3) 0.1398(3) -0.0320(2) 0.0356(10) Uani 1 d . . H29A H 0.0568(3) 0.1976(3) -0.0628(2) 0.043 Uiso 1 calc R . H29B H 0.0687(3) 0.0701(3) -0.0540(2) 0.043 Uiso 1 calc R . C30 C 0.1762(3) 0.1554(3) -0.0008(2) 0.0318(9) Uani 1 d . . H30A H 0.2009(3) 0.1609(3) -0.0330(2) 0.038 Uiso 1 calc R . H30B H 0.2007(3) 0.0914(3) 0.0247(2) 0.038 Uiso 1 calc R . C31 C 0.5024(2) 0.1432(3) 0.3104(2) 0.0232(8) Uani 1 d . . C32 C 0.4584(3) 0.1234(3) 0.3504(2) 0.0359(11) Uani 1 d . . H32A H 0.4090(3) 0.1632(3) 0.3456(2) 0.043 Uiso 1 calc R . C33 C 0.4873(3) 0.0449(4) 0.3976(2) 0.0471(13) Uani 1 d . . H33A H 0.4580(3) 0.0332(4) 0.4247(2) 0.057 Uiso 1 calc R . C34 C 0.5590(3) -0.0152(4) 0.4040(2) 0.0438(13) Uani 1 d . . H34A H 0.5773(3) -0.0693(4) 0.4348(2) 0.053 Uiso 1 calc R . C35 C 0.6043(3) 0.0033(3) 0.3655(2) 0.0373(11) Uani 1 d . . H35A H 0.6538(3) -0.0367(3) 0.3710(2) 0.045 Uiso 1 calc R . C36 C 0.5760(3) 0.0821(3) 0.3186(2) 0.0293(10) Uani 1 d . . H36A H 0.6064(3) 0.0942(3) 0.2923(2) 0.035 Uiso 1 calc R . C37 C 0.5621(3) 0.3141(3) 0.2543(2) 0.0227(9) Uani 1 d . . C38 C 0.6152(3) 0.3527(3) 0.3138(2) 0.0297(9) Uani 1 d . . H38A H 0.6009(3) 0.3383(3) 0.3487(2) 0.036 Uiso 1 calc R . C39 C 0.6887(3) 0.4122(3) 0.3208(2) 0.0342(11) Uani 1 d . . H39A H 0.7229(3) 0.4389(3) 0.3601(2) 0.041 Uiso 1 calc R . C40 C 0.7109(3) 0.4315(3) 0.2693(2) 0.0377(11) Uani 1 d . . H40A H 0.7600(3) 0.4719(3) 0.2739(2) 0.045 Uiso 1 calc R . C41 C 0.6607(3) 0.3912(3) 0.2109(2) 0.0343(11) Uani 1 d . . H41A H 0.6767(3) 0.4033(3) 0.1766(2) 0.041 Uiso 1 calc R . C42 C 0.5870(3) 0.3332(3) 0.2034(2) 0.0276(9) Uani 1 d . . H42A H 0.5536(3) 0.3065(3) 0.1639(2) 0.033 Uiso 1 calc R . C43 C 0.3944(3) 0.3309(3) 0.2666(2) 0.0221(9) Uani 1 d . . C44 C 0.3117(3) 0.2955(3) 0.2551(2) 0.0318(10) Uani 1 d . . H44A H 0.2934(3) 0.2281(3) 0.2357(2) 0.038 Uiso 1 calc R . C45 C 0.2555(3) 0.3603(4) 0.2723(2) 0.0390(11) Uani 1 d . . H45A H 0.2002(3) 0.3354(4) 0.2648(2) 0.047 Uiso 1 calc R . C46 C 0.2811(3) 0.4611(4) 0.3005(2) 0.0421(12) Uani 1 d . . H46A H 0.2435(3) 0.5041(4) 0.3123(2) 0.050 Uiso 1 calc R . C47 C 0.3626(3) 0.4970(3) 0.3110(2) 0.0428(12) Uani 1 d . . H47A H 0.3799(3) 0.5652(3) 0.3295(2) 0.051 Uiso 1 calc R . C48 C 0.4199(3) 0.4329(3) 0.2944(2) 0.0317(10) Uani 1 d . . H48A H 0.4751(3) 0.4584(3) 0.3018(2) 0.038 Uiso 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 0.02374(8) 0.01644(7) 0.01818(8) -0.00041(8) 0.00673(6) 0.00041(8) B1 0.021(3) 0.021(2) 0.019(2) -0.003(2) 0.005(2) -0.004(2) B2 0.022(3) 0.019(2) 0.022(2) 0.005(2) 0.000(2) 0.002(2) O1 0.028(2) 0.0238(14) 0.033(2) -0.0002(13) 0.0141(14) 0.0024(12) O2 0.028(2) 0.0194(13) 0.025(2) 0.0027(12) 0.0109(13) 0.0013(11) O3 0.032(2) 0.0252(14) 0.025(2) -0.0075(12) 0.0084(13) -0.0004(12) O4 0.045(2) 0.0282(15) 0.026(2) -0.0039(14) 0.0088(14) -0.0113(14) P1 0.0243(6) 0.0173(5) 0.0203(6) 0.0004(4) 0.0076(5) -0.0003(4) P2 0.0226(6) 0.0193(5) 0.0196(5) -0.0004(4) 0.0070(5) -0.0006(4) C1 0.029(2) 0.022(2) 0.025(2) -0.004(2) 0.006(2) 0.000(2) C2 0.026(3) 0.030(2) 0.047(3) -0.011(2) 0.003(2) 0.006(2) C3 0.039(3) 0.023(2) 0.054(3) -0.005(2) -0.010(3) 0.008(2) C4 0.051(4) 0.018(2) 0.041(3) 0.004(2) -0.007(3) -0.007(2) C5 0.044(3) 0.026(2) 0.028(2) 0.001(2) 0.008(2) -0.010(2) C6 0.030(2) 0.015(2) 0.022(2) -0.001(2) 0.001(2) -0.001(2) C7 0.030(3) 0.023(2) 0.021(2) -0.006(2) -0.003(2) 0.008(2) C8 0.033(3) 0.045(3) 0.033(3) -0.011(2) 0.006(2) 0.015(2) C9 0.056(4) 0.048(3) 0.028(3) -0.015(3) -0.003(2) 0.018(3) C10 0.067(4) 0.033(3) 0.037(3) -0.013(2) -0.009(3) -0.002(3) C11 0.059(4) 0.035(3) 0.034(3) -0.003(2) -0.001(2) -0.009(2) C12 0.042(3) 0.024(2) 0.025(2) -0.002(2) 0.003(2) -0.001(2) C13 0.030(3) 0.019(2) 0.021(2) 0.006(2) 0.010(2) 0.003(2) C14 0.031(3) 0.032(2) 0.030(2) 0.000(2) 0.015(2) 0.003(2) C15 0.035(3) 0.045(3) 0.040(3) -0.006(2) 0.019(2) -0.003(2) C16 0.048(3) 0.051(3) 0.035(3) -0.003(2) 0.024(2) -0.010(2) C17 0.045(3) 0.041(3) 0.032(3) 0.007(2) 0.016(2) -0.005(2) C18 0.035(3) 0.037(2) 0.033(3) 0.005(2) 0.015(2) 0.001(2) C19 0.027(2) 0.020(2) 0.016(2) -0.003(2) 0.005(2) -0.001(2) C20 0.036(3) 0.023(2) 0.041(3) -0.003(2) 0.011(2) -0.002(2) C21 0.040(3) 0.027(2) 0.036(3) -0.006(2) 0.016(2) -0.007(2) C22 0.047(3) 0.023(2) 0.041(3) -0.007(2) 0.018(2) 0.003(2) C23 0.039(3) 0.025(2) 0.049(3) 0.000(2) 0.016(2) 0.007(2) C24 0.026(3) 0.028(2) 0.037(3) -0.002(2) 0.010(2) 0.000(2) C25 0.030(3) 0.019(2) 0.026(2) 0.000(2) 0.012(2) -0.002(2) C26 0.033(3) 0.034(2) 0.023(2) -0.003(2) 0.012(2) -0.004(2) C27 0.033(3) 0.051(3) 0.034(3) -0.005(2) 0.017(2) -0.010(2) C28 0.031(3) 0.055(3) 0.035(3) -0.011(2) 0.011(2) -0.012(2) C29 0.036(3) 0.036(2) 0.033(2) -0.004(2) 0.009(2) -0.006(2) C30 0.029(3) 0.036(2) 0.028(2) -0.004(2) 0.007(2) 0.001(2) C31 0.030(2) 0.017(2) 0.019(2) -0.005(2) 0.004(2) -0.006(2) C32 0.041(3) 0.036(3) 0.030(3) 0.005(2) 0.013(2) -0.002(2) C33 0.059(4) 0.049(3) 0.031(3) 0.016(2) 0.014(3) -0.003(3) C34 0.049(4) 0.032(3) 0.034(3) 0.012(2) -0.004(2) -0.010(2) C35 0.028(3) 0.028(2) 0.040(3) 0.003(2) -0.006(2) -0.002(2) C36 0.028(3) 0.025(2) 0.030(2) -0.001(2) 0.005(2) -0.003(2) C37 0.022(2) 0.016(2) 0.029(2) 0.001(2) 0.008(2) 0.0018(15) C38 0.029(2) 0.031(2) 0.028(2) 0.002(2) 0.009(2) 0.001(2) C39 0.028(3) 0.027(2) 0.039(3) -0.003(2) 0.002(2) -0.003(2) C40 0.028(3) 0.023(2) 0.066(3) 0.005(2) 0.021(3) 0.000(2) C41 0.037(3) 0.030(2) 0.044(3) 0.000(2) 0.024(2) -0.003(2) C42 0.031(3) 0.025(2) 0.029(2) 0.003(2) 0.013(2) 0.008(2) C43 0.027(2) 0.022(2) 0.019(2) -0.001(2) 0.010(2) 0.003(2) C44 0.028(3) 0.034(2) 0.033(3) -0.007(2) 0.009(2) -0.003(2) C45 0.030(3) 0.042(3) 0.049(3) -0.003(2) 0.021(2) 0.000(2) C46 0.046(3) 0.040(3) 0.050(3) -0.005(2) 0.029(3) 0.006(2) C47 0.051(4) 0.033(2) 0.051(3) -0.018(2) 0.027(3) -0.001(2) C48 0.033(3) 0.030(2) 0.033(3) -0.007(2) 0.015(2) -0.005(2) _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 B1 2.044(4) . ? Pt1 B2 2.050(4) . ? Pt1 P2 2.3456(10) . ? Pt1 P1 2.3824(11) . ? B1 O2 1.405(4) . ? B1 O1 1.417(5) . ? B2 O4 1.412(5) . ? B2 O3 1.419(5) . ? O1 C1 1.383(4) . ? O2 C6 1.374(4) . ? O3 C7 1.378(4) . ? O4 C12 1.389(4) . ? P1 C25 1.847(4) . ? P1 C13 1.856(4) . ? P1 C19 1.873(4) . ? P2 C37 1.825(4) . ? P2 C43 1.833(4) . ? P2 C31 1.841(4) . ? C1 C6 1.375(5) . ? C1 C2 1.379(5) . ? C2 C3 1.404(6) . ? C3 C4 1.380(7) . ? C4 C5 1.388(6) . ? C5 C6 1.374(5) . ? C7 C12 1.365(6) . ? C7 C8 1.380(5) . ? C8 C9 1.388(6) . ? C9 C10 1.375(7) . ? C10 C11 1.396(6) . ? C11 C12 1.382(6) . ? C13 C18 1.510(5) . ? C13 C14 1.524(5) . ? C14 C15 1.500(5) . ? C15 C16 1.502(6) . ? C16 C17 1.504(6) . ? C17 C18 1.514(5) . ? C19 C20 1.496(5) . ? C19 C24 1.530(5) . ? C20 C21 1.538(5) . ? C21 C22 1.488(6) . ? C22 C23 1.502(6) . ? C23 C24 1.524(5) . ? C25 C30 1.516(5) . ? C25 C26 1.523(5) . ? C26 C27 1.495(6) . ? C27 C28 1.493(6) . ? C28 C29 1.513(5) . ? C29 C30 1.515(5) . ? C31 C32 1.390(5) . ? C31 C36 1.392(5) . ? C32 C33 1.389(6) . ? C33 C34 1.367(6) . ? C34 C35 1.375(6) . ? C35 C36 1.386(5) . ? C37 C42 1.392(5) . ? C37 C38 1.405(5) . ? C38 C39 1.386(5) . ? C39 C40 1.378(6) . ? C40 C41 1.382(6) . ? C41 C42 1.377(6) . ? C43 C44 1.382(5) . ? C43 C48 1.389(5) . ? C44 C45 1.390(5) . ? C45 C46 1.380(6) . ? C46 C47 1.368(6) . ? C47 C48 1.394(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 B1 Pt1 B2 73.3(2) . . ? B1 Pt1 P2 90.13(12) . . ? B2 Pt1 P2 163.10(12) . . ? B1 Pt1 P1 163.91(12) . . ? B2 Pt1 P1 90.84(12) . . ? P2 Pt1 P1 105.84(4) . . ? O2 B1 O1 107.8(3) . . ? O2 B1 Pt1 124.2(3) . . ? O1 B1 Pt1 128.0(3) . . ? O4 B2 O3 107.7(3) . . ? O4 B2 Pt1 129.6(3) . . ? O3 B2 Pt1 122.7(3) . . ? C1 O1 B1 106.4(3) . . ? C6 O2 B1 107.5(3) . . ? C7 O3 B2 106.9(3) . . ? C12 O4 B2 106.4(3) . . ? C25 P1 C13 103.2(2) . . ? C25 P1 C19 101.3(2) . . ? C13 P1 C19 107.7(2) . . ? C25 P1 Pt1 114.04(12) . . ? C13 P1 Pt1 108.43(12) . . ? C19 P1 Pt1 120.67(13) . . ? C37 P2 C43 106.5(2) . . ? C37 P2 C31 100.1(2) . . ? C43 P2 C31 102.2(2) . . ? C37 P2 Pt1 115.88(13) . . ? C43 P2 Pt1 115.63(13) . . ? C31 P2 Pt1 114.60(12) . . ? C6 C1 C2 121.9(4) . . ? C6 C1 O1 109.4(3) . . ? C2 C1 O1 128.6(4) . . ? C1 C2 C3 115.9(4) . . ? C4 C3 C2 121.8(4) . . ? C3 C4 C5 121.3(4) . . ? C6 C5 C4 116.6(4) . . ? C5 C6 O2 128.7(4) . . ? C5 C6 C1 122.4(4) . . ? O2 C6 C1 108.9(3) . . ? C12 C7 O3 109.4(3) . . ? C12 C7 C8 122.0(4) . . ? O3 C7 C8 128.7(4) . . ? C7 C8 C9 116.5(5) . . ? C10 C9 C8 121.4(4) . . ? C9 C10 C11 121.9(4) . . ? C12 C11 C10 115.7(5) . . ? C7 C12 C11 122.4(4) . . ? C7 C12 O4 109.5(3) . . ? C11 C12 O4 128.0(4) . . ? C18 C13 C14 112.5(3) . . ? C18 C13 P1 117.7(3) . . ? C14 C13 P1 114.5(3) . . ? C15 C14 C13 112.6(3) . . ? C14 C15 C16 113.0(4) . . ? C15 C16 C17 112.8(3) . . ? C16 C17 C18 111.3(4) . . ? C13 C18 C17 111.9(3) . . ? C20 C19 C24 111.4(3) . . ? C20 C19 P1 112.4(3) . . ? C24 C19 P1 118.3(3) . . ? C19 C20 C21 112.7(3) . . ? C22 C21 C20 111.7(4) . . ? C21 C22 C23 112.0(3) . . ? C22 C23 C24 113.0(3) . . ? C23 C24 C19 111.4(3) . . ? C30 C25 C26 110.0(3) . . ? C30 C25 P1 116.7(3) . . ? C26 C25 P1 113.4(3) . . ? C27 C26 C25 112.9(3) . . ? C28 C27 C26 113.8(4) . . ? C27 C28 C29 112.0(4) . . ? C28 C29 C30 112.7(3) . . ? C29 C30 C25 112.6(3) . . ? C32 C31 C36 118.3(4) . . ? C32 C31 P2 123.2(3) . . ? C36 C31 P2 118.3(3) . . ? C33 C32 C31 120.8(4) . . ? C34 C33 C32 119.6(4) . . ? C33 C34 C35 120.8(4) . . ? C34 C35 C36 119.7(4) . . ? C35 C36 C31 120.7(4) . . ? C42 C37 C38 118.4(4) . . ? C42 C37 P2 119.9(3) . . ? C38 C37 P2 121.7(3) . . ? C39 C38 C37 120.6(4) . . ? C40 C39 C38 119.7(4) . . ? C39 C40 C41 120.3(4) . . ? C42 C41 C40 120.4(4) . . ? C41 C42 C37 120.6(4) . . ? C44 C43 C48 119.0(4) . . ? C44 C43 P2 116.8(3) . . ? C48 C43 P2 124.2(3) . . ? C43 C44 C45 120.3(4) . . ? C46 C45 C44 120.7(4) . . ? C47 C46 C45 119.0(4) . . ? C46 C47 C48 121.2(4) . . ? C43 C48 C47 119.8(4) . . ? _refine_diff_density_max 0.925 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.118 #=END data_16 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C43.50 H45.50 B2 Cl2 N2 P2 Pt' _chemical_formula_weight 945.87 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2268(10) _cell_length_b 12.0715(14) _cell_length_c 17.349(3) _cell_angle_alpha 85.897(8) _cell_angle_beta 72.861(10) _cell_angle_gamma 69.461(8) _cell_volume 2102.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 209 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method ? _exptl_crystal_F_000 945 _exptl_absorpt_coefficient_mu 3.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.478259 _exptl_absorpt_correction_T_max 0.769015 _exptl_special_details ; SADABS (Sheldrick, 1996)s ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21868 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9499 _reflns_number_observed 8089 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXTL (Siemens, 1995a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+0.0000P] 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 'see text' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00051(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9499 _refine_ls_number_parameters 484 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_obs 0.0240 _refine_ls_wR_factor_all 0.0464 _refine_ls_wR_factor_obs 0.0446 _refine_ls_goodness_of_fit_all 0.943 _refine_ls_goodness_of_fit_obs 0.987 _refine_ls_restrained_S_all 0.943 _refine_ls_restrained_S_obs 0.986 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt -0.251791(11) 0.268270(9) 0.258834(7) 0.01889(4) Uani 1 d . . B1 B -0.2046(4) 0.4095(3) 0.2875(2) 0.0281(8) Uani 1 d . . B2 B -0.1669(4) 0.2097(3) 0.3523(2) 0.0367(9) Uani 1 d . . N1 N -0.2850(3) 0.5070(2) 0.33767(15) 0.0323(6) Uani 1 d . . N2 N -0.0355(3) 0.1466(2) 0.3463(2) 0.0450(8) Uani 1 d . . P1 P -0.33836(7) 0.37156(6) 0.15657(4) 0.0194(2) Uani 1 d . . P2 P -0.27980(7) 0.08781(6) 0.24713(4) 0.0200(2) Uani 1 d . . Cl1 Cl -0.03476(8) 0.41093(7) 0.23505(5) 0.0380(2) Uani 1 d . . Cl2 Cl -0.27923(11) 0.23845(8) 0.45686(5) 0.0545(3) Uani 1 d . . C1 C -0.2529(4) 0.6109(3) 0.3521(2) 0.0487(10) Uani 1 d . . H1A H -0.1580(6) 0.5958(8) 0.3269(12) 0.073 Uiso 1 calc R . H1B H -0.2745(22) 0.6254(13) 0.4103(2) 0.073 Uiso 1 calc R . H1C H -0.3050(17) 0.6805(5) 0.3285(12) 0.073 Uiso 1 calc R . C2 C -0.4244(4) 0.5202(3) 0.3788(2) 0.0483(10) Uani 1 d . . H2A H -0.4396(7) 0.4475(8) 0.3702(11) 0.073 Uiso 1 calc R . H2B H -0.4830(4) 0.5870(12) 0.3568(9) 0.073 Uiso 1 calc R . H2C H -0.4433(7) 0.5348(19) 0.4368(3) 0.073 Uiso 1 calc R . C3 C 0.0622(3) 0.1090(3) 0.2655(2) 0.0498(10) Uani 1 d . . H3A H 0.0188(6) 0.1424(17) 0.2235(2) 0.075 Uiso 1 calc R . H3B H 0.0964(17) 0.0224(3) 0.2599(6) 0.075 Uiso 1 calc R . H3C H 0.1360(11) 0.1375(17) 0.2599(6) 0.075 Uiso 1 calc R . C4 C 0.0249(5) 0.1024(4) 0.4122(3) 0.0731(14) Uani 1 d . . H4A H -0.0428(7) 0.1287(21) 0.4642(3) 0.110 Uiso 1 calc R . H4B H 0.0964(18) 0.1335(20) 0.4076(10) 0.110 Uiso 1 calc R . H4C H 0.0613(25) 0.0157(4) 0.4087(10) 0.110 Uiso 1 calc R . C5 C -0.2085(3) 0.3689(2) 0.0632(2) 0.0215(6) Uani 1 d . . C6 C -0.0767(3) 0.3027(2) 0.0580(2) 0.0252(6) Uani 1 d . . H6A H -0.0562(3) 0.2550(2) 0.1016(2) 0.030 Uiso 1 calc R . C7 C 0.0254(3) 0.3053(3) -0.0100(2) 0.0314(7) Uani 1 d . . H7A H 0.1149(3) 0.2589(3) -0.0133(2) 0.038 Uiso 1 calc R . C8 C -0.0039(3) 0.3757(3) -0.0729(2) 0.0334(7) Uani 1 d . . H8A H 0.0656(3) 0.3779(3) -0.1194(2) 0.040 Uiso 1 calc R . C9 C -0.1346(3) 0.4434(3) -0.0684(2) 0.0326(7) Uani 1 d . . H9A H -0.1542(3) 0.4922(3) -0.1117(2) 0.039 Uiso 1 calc R . C10 C -0.2359(3) 0.4399(2) -0.0012(2) 0.0272(7) Uani 1 d . . H10A H -0.3252(3) 0.4862(2) 0.0015(2) 0.033 Uiso 1 calc R . C11 C -0.4226(3) 0.5330(2) 0.1728(2) 0.0222(6) Uani 1 d . . C12 C -0.3432(3) 0.6009(2) 0.1698(2) 0.0263(7) Uani 1 d . . H12A H -0.2499(3) 0.5627(2) 0.1590(2) 0.032 Uiso 1 calc R . C13 C -0.3973(3) 0.7225(2) 0.1824(2) 0.0308(7) Uani 1 d . . H13A H -0.3415(3) 0.7674(2) 0.1793(2) 0.037 Uiso 1 calc R . C14 C -0.5321(3) 0.7777(3) 0.1993(2) 0.0402(9) Uani 1 d . . H14A H -0.5701(3) 0.8610(3) 0.2090(2) 0.048 Uiso 1 calc R . C15 C -0.6128(3) 0.7130(3) 0.2022(2) 0.0464(10) Uani 1 d . . H15A H -0.7061(3) 0.7519(3) 0.2135(2) 0.056 Uiso 1 calc R . C16 C -0.5582(3) 0.5909(3) 0.1886(2) 0.0354(8) Uani 1 d . . H16A H -0.6144(3) 0.5469(3) 0.1902(2) 0.042 Uiso 1 calc R . C17 C -0.4631(3) 0.3287(2) 0.1300(2) 0.0230(6) Uani 1 d . . C18 C -0.4605(3) 0.3049(2) 0.0522(2) 0.0263(7) Uani 1 d . . H18A H -0.3892(3) 0.3092(2) 0.0075(2) 0.032 Uiso 1 calc R . C19 C -0.5620(3) 0.2747(2) 0.0396(2) 0.0349(8) Uani 1 d . . H19A H -0.5597(3) 0.2586(2) -0.0137(2) 0.042 Uiso 1 calc R . C20 C -0.6658(3) 0.2679(2) 0.1037(2) 0.0390(9) Uani 1 d . . H20A H -0.7357(3) 0.2488(2) 0.0943(2) 0.047 Uiso 1 calc R . C21 C -0.6690(3) 0.2884(2) 0.1815(2) 0.0356(8) Uani 1 d . . H21A H -0.7400(3) 0.2826(2) 0.2258(2) 0.043 Uiso 1 calc R . C22 C -0.5674(3) 0.3177(2) 0.1942(2) 0.0280(7) Uani 1 d . . H22A H -0.5687(3) 0.3306(2) 0.2478(2) 0.034 Uiso 1 calc R . C23 C -0.4267(3) 0.0714(2) 0.3211(2) 0.0218(6) Uani 1 d . . C24 C -0.4454(3) -0.0384(2) 0.3306(2) 0.0306(7) Uani 1 d . . H24A H -0.3830(3) -0.1043(2) 0.2967(2) 0.037 Uiso 1 calc R . C25 C -0.5531(3) -0.0515(3) 0.3883(2) 0.0375(8) Uani 1 d . . H25A H -0.5655(3) -0.1259(3) 0.3937(2) 0.045 Uiso 1 calc R . C26 C -0.6430(3) 0.0432(3) 0.4383(2) 0.0408(8) Uani 1 d . . H26A H -0.7178(3) 0.0342(3) 0.4779(2) 0.049 Uiso 1 calc R . C27 C -0.6249(3) 0.1516(3) 0.4312(2) 0.0394(8) Uani 1 d . . H27A H -0.6863(3) 0.2164(3) 0.4664(2) 0.047 Uiso 1 calc R . C28 C -0.5166(3) 0.1654(2) 0.3724(2) 0.0286(7) Uani 1 d . . H28A H -0.5044(3) 0.2399(2) 0.3675(2) 0.034 Uiso 1 calc R . C29 C -0.2863(3) 0.0494(2) 0.1480(2) 0.0200(6) Uani 1 d . . C30 C -0.3832(3) 0.0116(2) 0.1361(2) 0.0243(6) Uani 1 d . . H30A H -0.4524(3) 0.0044(2) 0.1811(2) 0.029 Uiso 1 calc R . C31 C -0.3799(3) -0.0157(2) 0.0589(2) 0.0310(7) Uani 1 d . . H31A H -0.4460(3) -0.0427(2) 0.0517(2) 0.037 Uiso 1 calc R . C32 C -0.2809(3) -0.0040(2) -0.0075(2) 0.0328(7) Uani 1 d . . H32A H -0.2789(3) -0.0227(2) -0.0602(2) 0.039 Uiso 1 calc R . C33 C -0.1852(3) 0.0351(2) 0.0033(2) 0.0313(7) Uani 1 d . . H33A H -0.1174(3) 0.0438(2) -0.0421(2) 0.038 Uiso 1 calc R . C34 C -0.1875(3) 0.0620(2) 0.0805(2) 0.0257(7) Uani 1 d . . H34A H -0.1213(3) 0.0891(2) 0.0873(2) 0.031 Uiso 1 calc R . C35 C -0.1522(3) -0.0474(2) 0.2675(2) 0.0230(6) Uani 1 d . . C36 C -0.0626(3) -0.1332(2) 0.2092(2) 0.0301(7) Uani 1 d . . H36A H -0.0636(3) -0.1239(2) 0.1545(2) 0.036 Uiso 1 calc R . C37 C 0.0286(3) -0.2328(3) 0.2310(2) 0.0414(9) Uani 1 d . . H37A H 0.0907(3) -0.2905(3) 0.1906(2) 0.050 Uiso 1 calc R . C38 C 0.0301(3) -0.2489(3) 0.3098(2) 0.0436(9) Uani 1 d . . H38A H 0.0925(3) -0.3176(3) 0.3239(2) 0.052 Uiso 1 calc R . C39 C -0.0594(3) -0.1652(3) 0.3684(2) 0.0405(8) Uani 1 d . . H39A H -0.0596(3) -0.1765(3) 0.4232(2) 0.049 Uiso 1 calc R . C40 C -0.1493(3) -0.0642(3) 0.3473(2) 0.0335(8) Uani 1 d . . H40A H -0.2096(3) -0.0059(3) 0.3878(2) 0.040 Uiso 1 calc R . C41 C 0.2371(11) 0.5081(9) 0.4284(7) 0.095(4) Uani 0.50 d P . H41A H 0.2657(29) 0.4760(56) 0.3731(14) 0.143 Uiso 0.50 calc PR . H41B H 0.2987(17) 0.4595(51) 0.4577(24) 0.143 Uiso 0.50 calc PR . H41C H 0.2366(18) 0.5896(12) 0.4273(38) 0.143 Uiso 0.50 calc PR . C42 C 0.1239(5) 0.5073(5) 0.4628(4) 0.101(2) Uani 1 d D . C43 C 0.0782(7) 0.4391(5) 0.4263(4) 0.115(2) Uani 1 d D . H43A H 0.1298(7) 0.3987(5) 0.3758(4) 0.138 Uiso 1 calc R . C44 C -0.0448(8) 0.4316(5) 0.4654(4) 0.100(2) Uani 1 d D . H44A H -0.0762(8) 0.3825(5) 0.4421(4) 0.120 Uiso 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 0.02401(6) 0.01890(6) 0.01761(6) 0.00201(4) -0.00640(4) -0.01198(4) B1 0.039(2) 0.029(2) 0.024(2) 0.0084(15) -0.016(2) -0.016(2) B2 0.060(3) 0.034(2) 0.032(2) 0.009(2) -0.017(2) -0.033(2) N1 0.051(2) 0.0276(13) 0.0276(14) 0.0001(11) -0.0155(13) -0.0206(13) N2 0.055(2) 0.049(2) 0.056(2) 0.0254(15) -0.040(2) -0.032(2) P1 0.0217(4) 0.0179(3) 0.0206(4) 0.0020(3) -0.0061(3) -0.0093(3) P2 0.0238(4) 0.0185(3) 0.0198(4) 0.0014(3) -0.0058(3) -0.0104(3) Cl1 0.0395(5) 0.0445(4) 0.0437(5) 0.0137(4) -0.0176(4) -0.0287(4) Cl2 0.0951(8) 0.0572(6) 0.0239(4) 0.0078(4) -0.0147(5) -0.0445(6) C1 0.081(3) 0.028(2) 0.051(2) -0.002(2) -0.031(2) -0.026(2) C2 0.053(2) 0.046(2) 0.031(2) -0.010(2) 0.001(2) -0.008(2) C3 0.027(2) 0.042(2) 0.087(3) 0.010(2) -0.023(2) -0.016(2) C4 0.098(4) 0.074(3) 0.088(3) 0.041(2) -0.076(3) -0.045(3) C5 0.027(2) 0.0175(13) 0.0213(15) 0.0002(11) -0.0062(12) -0.0104(12) C6 0.028(2) 0.0233(14) 0.027(2) 0.0042(12) -0.0099(13) -0.0106(13) C7 0.024(2) 0.034(2) 0.033(2) 0.0020(14) -0.0050(14) -0.0091(14) C8 0.033(2) 0.035(2) 0.028(2) 0.0009(14) 0.0017(14) -0.0154(15) C9 0.043(2) 0.029(2) 0.024(2) 0.0084(13) -0.0070(15) -0.0140(15) C10 0.031(2) 0.0209(14) 0.026(2) 0.0058(12) -0.0083(13) -0.0056(13) C11 0.029(2) 0.0195(14) 0.0203(14) 0.0014(11) -0.0056(12) -0.0118(12) C12 0.030(2) 0.0232(15) 0.027(2) 0.0007(13) -0.0095(13) -0.0094(13) C13 0.040(2) 0.0213(15) 0.036(2) 0.0016(13) -0.0127(15) -0.0141(14) C14 0.045(2) 0.021(2) 0.049(2) -0.0031(15) -0.007(2) -0.009(2) C15 0.027(2) 0.025(2) 0.077(3) -0.005(2) -0.005(2) -0.0033(15) C16 0.029(2) 0.026(2) 0.051(2) -0.0010(15) -0.008(2) -0.0121(14) C17 0.026(2) 0.0158(13) 0.028(2) 0.0013(12) -0.0110(13) -0.0062(12) C18 0.034(2) 0.0167(14) 0.031(2) 0.0020(12) -0.0155(14) -0.0074(13) C19 0.047(2) 0.0215(15) 0.046(2) -0.0002(14) -0.032(2) -0.0078(15) C20 0.032(2) 0.025(2) 0.072(3) -0.001(2) -0.030(2) -0.0095(14) C21 0.026(2) 0.026(2) 0.058(2) 0.002(2) -0.012(2) -0.0117(14) C22 0.028(2) 0.0249(15) 0.035(2) 0.0028(13) -0.0128(14) -0.0108(13) C23 0.024(2) 0.0236(14) 0.0185(14) 0.0020(12) -0.0052(12) -0.0105(12) C24 0.036(2) 0.027(2) 0.029(2) 0.0030(13) -0.0055(14) -0.0144(14) C25 0.043(2) 0.041(2) 0.035(2) 0.012(2) -0.009(2) -0.027(2) C26 0.033(2) 0.058(2) 0.030(2) 0.014(2) -0.0031(15) -0.022(2) C27 0.034(2) 0.045(2) 0.027(2) -0.0039(15) 0.0013(15) -0.005(2) C28 0.031(2) 0.027(2) 0.027(2) 0.0027(13) -0.0077(14) -0.0098(13) C29 0.0237(15) 0.0118(12) 0.0224(15) 0.0009(11) -0.0069(12) -0.0037(11) C30 0.028(2) 0.0201(14) 0.028(2) 0.0048(12) -0.0112(13) -0.0112(12) C31 0.040(2) 0.027(2) 0.037(2) 0.0039(14) -0.022(2) -0.0156(14) C32 0.043(2) 0.025(2) 0.027(2) -0.0024(13) -0.017(2) -0.0028(14) C33 0.033(2) 0.030(2) 0.023(2) 0.0001(13) -0.0023(14) -0.0069(14) C34 0.026(2) 0.0208(14) 0.028(2) 0.0001(12) -0.0052(13) -0.0081(12) C35 0.024(2) 0.0238(14) 0.027(2) 0.0037(12) -0.0100(13) -0.0131(12) C36 0.031(2) 0.031(2) 0.028(2) -0.0013(13) -0.0119(14) -0.0066(14) C37 0.038(2) 0.036(2) 0.043(2) -0.012(2) -0.017(2) 0.004(2) C38 0.040(2) 0.034(2) 0.056(2) 0.005(2) -0.024(2) -0.004(2) C39 0.045(2) 0.041(2) 0.034(2) 0.009(2) -0.018(2) -0.010(2) C40 0.038(2) 0.032(2) 0.025(2) 0.0007(14) -0.0053(15) -0.0090(15) C41 0.080(8) 0.098(8) 0.099(9) 0.051(6) -0.037(7) -0.020(7) C42 0.128(6) 0.076(4) 0.114(5) 0.039(4) -0.084(5) -0.019(4) C43 0.179(8) 0.073(4) 0.114(5) 0.013(4) -0.110(6) -0.015(4) C44 0.166(7) 0.056(3) 0.104(5) 0.006(3) -0.099(5) -0.020(4) _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 B2 2.076(4) . ? Pt1 B1 2.084(3) . ? Pt1 P2 2.3382(7) . ? Pt1 P1 2.3445(8) . ? B1 N1 1.378(4) . ? B1 Cl1 1.861(4) . ? B2 N2 1.379(5) . ? B2 Cl2 1.854(4) . ? N1 C2 1.472(4) . ? N1 C1 1.476(4) . ? N2 C4 1.472(4) . ? N2 C3 1.486(5) . ? P1 C5 1.826(3) . ? P1 C17 1.833(3) . ? P1 C11 1.844(3) . ? P2 C23 1.831(3) . ? P2 C29 1.840(3) . ? P2 C35 1.848(3) . ? C5 C6 1.392(4) . ? C5 C10 1.399(4) . ? C6 C7 1.389(4) . ? C7 C8 1.379(4) . ? C8 C9 1.388(4) . ? C9 C10 1.379(4) . ? C11 C16 1.384(4) . ? C11 C12 1.396(4) . ? C12 C13 1.383(4) . ? C13 C14 1.371(4) . ? C14 C15 1.377(4) . ? C15 C16 1.391(4) . ? C17 C18 1.392(4) . ? C17 C22 1.395(4) . ? C18 C19 1.388(4) . ? C19 C20 1.376(5) . ? C20 C21 1.376(5) . ? C21 C22 1.385(4) . ? C23 C28 1.382(4) . ? C23 C24 1.404(4) . ? C24 C25 1.374(4) . ? C25 C26 1.377(4) . ? C26 C27 1.384(4) . ? C27 C28 1.390(4) . ? C29 C30 1.388(4) . ? C29 C34 1.398(4) . ? C30 C31 1.389(4) . ? C31 C32 1.384(4) . ? C32 C33 1.378(4) . ? C33 C34 1.390(4) . ? C35 C36 1.388(4) . ? C35 C40 1.393(4) . ? C36 C37 1.392(4) . ? C37 C38 1.372(4) . ? C38 C39 1.377(4) . ? C39 C40 1.389(4) . ? C41 C42 1.238(10) . ? C42 C44 1.3797(10) 2_566 ? C42 C43 1.3797(10) . ? C43 C44 1.3798(10) . ? C44 C42 1.3798(10) 2_566 ? 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 B2 Pt1 B1 75.15(13) . . ? B2 Pt1 P2 92.23(9) . . ? B1 Pt1 P2 167.31(9) . . ? B2 Pt1 P1 167.63(9) . . ? B1 Pt1 P1 92.48(9) . . ? P2 Pt1 P1 100.13(3) . . ? N1 B1 Cl1 114.3(2) . . ? N1 B1 Pt1 128.7(3) . . ? Cl1 B1 Pt1 117.0(2) . . ? N2 B2 Cl2 114.8(3) . . ? N2 B2 Pt1 127.6(3) . . ? Cl2 B2 Pt1 117.5(2) . . ? B1 N1 C2 119.6(3) . . ? B1 N1 C1 127.8(3) . . ? C2 N1 C1 112.4(3) . . ? B2 N2 C4 128.0(3) . . ? B2 N2 C3 119.8(3) . . ? C4 N2 C3 112.1(3) . . ? C5 P1 C17 107.31(13) . . ? C5 P1 C11 99.32(12) . . ? C17 P1 C11 101.27(12) . . ? C5 P1 Pt1 112.34(9) . . ? C17 P1 Pt1 117.51(9) . . ? C11 P1 Pt1 117.00(9) . . ? C23 P2 C29 106.03(13) . . ? C23 P2 C35 98.92(12) . . ? C29 P2 C35 101.72(12) . . ? C23 P2 Pt1 114.20(9) . . ? C29 P2 Pt1 116.61(9) . . ? C35 P2 Pt1 117.12(9) . . ? C6 C5 C10 118.5(3) . . ? C6 C5 P1 119.5(2) . . ? C10 C5 P1 121.8(2) . . ? C7 C6 C5 120.9(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 C9 120.3(3) . . ? C10 C9 C8 120.0(3) . . ? C9 C10 C5 120.6(3) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 P1 124.8(2) . . ? C12 C11 P1 117.1(2) . . ? C13 C12 C11 121.5(3) . . ? C14 C13 C12 119.4(3) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 C16 120.2(3) . . ? C11 C16 C15 120.4(3) . . ? C18 C17 C22 118.1(3) . . ? C18 C17 P1 125.5(2) . . ? C22 C17 P1 116.4(2) . . ? C19 C18 C17 120.1(3) . . ? C20 C19 C18 120.6(3) . . ? C19 C20 C21 120.4(3) . . ? C20 C21 C22 119.1(3) . . ? C21 C22 C17 121.6(3) . . ? C28 C23 C24 118.8(3) . . ? C28 C23 P2 120.2(2) . . ? C24 C23 P2 120.9(2) . . ? C25 C24 C23 120.7(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C27 120.3(3) . . ? C26 C27 C28 119.9(3) . . ? C23 C28 C27 120.3(3) . . ? C30 C29 C34 118.4(3) . . ? C30 C29 P2 124.7(2) . . ? C34 C29 P2 116.9(2) . . ? C29 C30 C31 120.7(3) . . ? C32 C31 C30 120.4(3) . . ? C33 C32 C31 119.6(3) . . ? C32 C33 C34 120.3(3) . . ? C33 C34 C29 120.6(3) . . ? C36 C35 C40 118.7(3) . . ? C36 C35 P2 124.3(2) . . ? C40 C35 P2 117.0(2) . . ? C35 C36 C37 119.9(3) . . ? C38 C37 C36 121.0(3) . . ? C37 C38 C39 119.7(3) . . ? C38 C39 C40 119.9(3) . . ? C39 C40 C35 120.8(3) . . ? C41 C42 C44 123.6(9) . 2_566 ? C41 C42 C43 116.6(9) . . ? C44 C42 C43 119.8(5) 2_566 . ? C42 C43 C44 117.8(6) . . ? C42 C44 C43 122.4(5) 2_566 . ? _refine_diff_density_max 0.705 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.087 #=END data_17 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H36 B Cl2 N P2 Pt' _chemical_formula_weight 845.42 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.865(5) _cell_length_b 12.093(6) _cell_length_c 14.228(5) _cell_angle_alpha 95.819(6) _cell_angle_beta 92.523(10) _cell_angle_gamma 105.637(6) _cell_volume 1786.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 271 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method ? _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 4.195 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.302755 _exptl_absorpt_correction_T_max 0.547751 _exptl_special_details ; SADABS (Sheldrick, 1996)s ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14303 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5583 _reflns_number_observed 4722 _reflns_observed_criterion >2sigma(I) _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.0000P] 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 'see text' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5577 _refine_ls_number_parameters 456 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_obs 0.0307 _refine_ls_wR_factor_all 0.0616 _refine_ls_wR_factor_obs 0.0585 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_obs 1.047 _refine_ls_restrained_S_all 1.003 _refine_ls_restrained_S_obs 1.045 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt -0.18855(2) 0.04151(2) 0.228970(14) 0.02292(7) Uani 1 d D . Cl1 Cl 0.03256(13) 0.06405(11) 0.18266(10) 0.0370(4) Uani 1 d . . B1 B -0.3688(9) 0.0313(7) 0.2762(6) 0.024(2) Uani 0.749(6) d PD 1 N1 N -0.4847(6) -0.0052(5) 0.2220(4) 0.028(2) Uani 0.749(6) d PD 1 Cl2 Cl -0.3733(4) 0.0740(3) 0.4018(2) 0.0335(8) Uani 0.749(6) d PD 1 C1 C -0.6114(8) -0.0143(11) 0.2561(8) 0.047(3) Uani 0.749(6) d PD 1 H1A H -0.6035(11) 0.0044(58) 0.3251(9) 0.070 Uiso 0.749(6) calc PR 1 H1B H -0.6662(20) -0.0934(14) 0.2390(39) 0.070 Uiso 0.749(6) calc PR 1 H1C H -0.6496(26) 0.0399(35) 0.2270(35) 0.070 Uiso 0.749(6) calc PR 1 C2 C -0.4943(18) -0.0415(19) 0.1223(10) 0.038(5) Uani 0.749(6) d PD 1 H2A H -0.5330(47) 0.0088(32) 0.0883(10) 0.057 Uiso 0.749(6) calc PR 1 H2B H -0.5479(45) -0.1215(23) 0.1093(11) 0.057 Uiso 0.749(6) calc PR 1 H2C H -0.4086(19) -0.0366(48) 0.1011(12) 0.057 Uiso 0.749(6) calc PR 1 B1' B -0.3831(19) -0.0008(21) 0.2188(15) 0.026(6) Uani 0.251(6) d PDU 2 N1' N -0.4549(19) 0.0200(17) 0.2906(16) 0.041(6) Uani 0.251(6) d PD 2 Cl2' Cl -0.4610(15) -0.0528(17) 0.1040(9) 0.044(3) Uani 0.251(6) d PD 2 C1' C -0.5915(23) 0.0062(30) 0.2895(19) 0.028(8) Uani 0.251(6) d PDU 2 H1'A H -0.6299(33) -0.0164(140) 0.2244(23) 0.042 Uiso 0.251(6) calc PR 2 H1'B H -0.6070(23) 0.0794(44) 0.3144(106) 0.042 Uiso 0.251(6) calc PR 2 H1'C H -0.6302(32) -0.0539(94) 0.3291(90) 0.042 Uiso 0.251(6) calc PR 2 C2' C -0.4001(39) 0.0707(36) 0.3837(22) 0.017(11) Uani 0.251(6) d PDU 2 H2'A H -0.3075(43) 0.0802(89) 0.3870(31) 0.025 Uiso 0.251(6) calc PR 2 H2'B H -0.4391(83) 0.0201(55) 0.4303(24) 0.025 Uiso 0.251(6) calc PR 2 H2'C H -0.4163(90) 0.1464(52) 0.3975(35) 0.025 Uiso 0.251(6) calc PR 2 P1 P -0.16276(13) 0.23084(11) 0.20563(8) 0.0214(3) Uani 1 d . . P2 P -0.21133(13) -0.14630(11) 0.25525(9) 0.0217(3) Uani 1 d . . C3 C -0.1516(5) 0.2596(4) 0.0829(3) 0.0231(11) Uani 1 d . . C4 C -0.1603(5) 0.3652(4) 0.0566(3) 0.0349(14) Uani 1 d . . H4 H -0.1718(5) 0.4231(4) 0.1030(3) 0.042 Uiso 1 calc R . C5 C -0.1521(6) 0.3859(5) -0.0373(4) 0.046(2) Uani 1 d . . H5 H -0.1584(6) 0.4580(5) -0.0550(4) 0.056 Uiso 1 calc R . C6 C -0.1349(6) 0.3030(5) -0.1049(4) 0.047(2) Uani 1 d . . H6 H -0.1291(6) 0.3181(5) -0.1690(4) 0.057 Uiso 1 calc R . C7 C -0.1259(5) 0.1984(5) -0.0802(4) 0.0407(15) Uani 1 d . . H7 H -0.1138(5) 0.1412(5) -0.1271(4) 0.049 Uiso 1 calc R . C8 C -0.1345(5) 0.1765(4) 0.0131(3) 0.0298(13) Uani 1 d . . H8 H -0.1287(5) 0.1040(4) 0.0299(3) 0.036 Uiso 1 calc R . C9 C -0.0144(5) 0.3158(4) 0.2696(3) 0.0212(11) Uani 1 d . . C10 C 0.0830(5) 0.3909(4) 0.2282(3) 0.0277(12) Uani 1 d . . H10 H 0.0724(5) 0.4006(4) 0.1632(3) 0.033 Uiso 1 calc R . C11 C 0.1964(5) 0.4521(4) 0.2815(4) 0.0332(13) Uani 1 d . . H11 H 0.2630(5) 0.5025(4) 0.2527(4) 0.040 Uiso 1 calc R . C12 C 0.2111(5) 0.4390(4) 0.3761(4) 0.0334(13) Uani 1 d . . H12 H 0.2873(5) 0.4818(4) 0.4127(4) 0.040 Uiso 1 calc R . C13 C 0.1160(5) 0.3643(5) 0.4178(4) 0.0348(13) Uani 1 d . . H13 H 0.1269(5) 0.3554(5) 0.4830(4) 0.042 Uiso 1 calc R . C14 C 0.0055(5) 0.3026(4) 0.3650(3) 0.0338(13) Uani 1 d . . H14 H -0.0588(5) 0.2500(4) 0.3940(3) 0.041 Uiso 1 calc R . C15 C -0.2799(5) 0.3064(4) 0.2465(3) 0.0258(12) Uani 1 d . . C16 C -0.2491(5) 0.3992(4) 0.3186(3) 0.0299(13) Uani 1 d . . H16 H -0.1648(5) 0.4257(4) 0.3484(3) 0.036 Uiso 1 calc R . C17 C -0.3417(6) 0.4521(5) 0.3463(4) 0.0398(15) Uani 1 d . . H17 H -0.3200(6) 0.5149(5) 0.3954(4) 0.048 Uiso 1 calc R . C18 C -0.4632(6) 0.4163(5) 0.3049(4) 0.041(2) Uani 1 d . . H18 H -0.5254(6) 0.4542(5) 0.3245(4) 0.050 Uiso 1 calc R . C19 C -0.4953(5) 0.3247(5) 0.2343(4) 0.0418(15) Uani 1 d . . H19 H -0.5805(5) 0.2983(5) 0.2060(4) 0.050 Uiso 1 calc R . C20 C -0.4034(5) 0.2703(5) 0.2041(4) 0.0355(14) Uani 1 d . . H20 H -0.4256(5) 0.2084(5) 0.1542(4) 0.043 Uiso 1 calc R . C21 C -0.0707(5) -0.1726(4) 0.3130(3) 0.0239(12) Uani 1 d . . C22 C -0.0535(5) -0.2829(4) 0.3077(3) 0.0277(12) Uani 1 d . . H22 H -0.1113(5) -0.3445(4) 0.2678(3) 0.033 Uiso 1 calc R . C23 C 0.0464(5) -0.3041(5) 0.3595(4) 0.0344(14) Uani 1 d . . H23 H 0.0567(5) -0.3799(5) 0.3555(4) 0.041 Uiso 1 calc R . C24 C 0.1311(5) -0.2150(5) 0.4170(4) 0.0390(15) Uani 1 d . . H24 H 0.2002(5) -0.2292(5) 0.4525(4) 0.047 Uiso 1 calc R . C25 C 0.1156(6) -0.1049(5) 0.4231(4) 0.0404(14) Uani 1 d . . H25 H 0.1735(6) -0.0437(5) 0.4633(4) 0.048 Uiso 1 calc R . C26 C 0.0159(5) -0.0835(5) 0.3705(4) 0.0348(14) Uani 1 d . . H26 H 0.0067(5) -0.0073(5) 0.3739(4) 0.042 Uiso 1 calc R . C27 C -0.2493(5) -0.2441(4) 0.1452(3) 0.0238(12) Uani 1 d . . C28 C -0.2072(5) -0.2001(4) 0.0612(3) 0.0304(13) Uani 1 d . . H28 H -0.1592(5) -0.1214(4) 0.0633(3) 0.036 Uiso 1 calc R . C29 C -0.2344(5) -0.2692(5) -0.0241(4) 0.0360(14) Uani 1 d . . H29 H -0.2047(5) -0.2386(5) -0.0805(4) 0.043 Uiso 1 calc R . C30 C -0.3052(5) -0.3836(5) -0.0278(4) 0.0352(14) Uani 1 d . . H30 H -0.3259(5) -0.4311(5) -0.0868(4) 0.042 Uiso 1 calc R . C31 C -0.3457(5) -0.4287(4) 0.0547(3) 0.0309(13) Uani 1 d . . H31 H -0.3921(5) -0.5078(4) 0.0523(3) 0.037 Uiso 1 calc R . C32 C -0.3189(5) -0.3591(4) 0.1407(3) 0.0275(12) Uani 1 d . . H32 H -0.3483(5) -0.3904(4) 0.1969(3) 0.033 Uiso 1 calc R . C33 C -0.3372(5) -0.2090(4) 0.3326(3) 0.0254(12) Uani 1 d . . C34 C -0.3053(5) -0.2141(4) 0.4280(3) 0.0310(13) Uani 1 d . . H34 H -0.2179(5) -0.1921(4) 0.4516(3) 0.037 Uiso 1 calc R . C35 C -0.4013(6) -0.2514(5) 0.4882(4) 0.0394(15) Uani 1 d . . H35 H -0.3797(6) -0.2550(5) 0.5530(4) 0.047 Uiso 1 calc R . C36 C -0.5265(6) -0.2829(5) 0.4542(4) 0.044(2) Uani 1 d . . H36 H -0.5918(6) -0.3084(5) 0.4957(4) 0.053 Uiso 1 calc R . C37 C -0.5595(6) -0.2781(4) 0.3607(4) 0.0378(14) Uani 1 d . . H37 H -0.6471(6) -0.2997(4) 0.3376(4) 0.045 Uiso 1 calc R . C38 C -0.4635(5) -0.2413(4) 0.3000(4) 0.0294(13) Uani 1 d . . H38 H -0.4861(5) -0.2387(4) 0.2352(4) 0.035 Uiso 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 0.02492(13) 0.02061(11) 0.02373(11) 0.00779(7) 0.00296(8) 0.00506(8) Cl1 0.0358(9) 0.0305(8) 0.0503(9) 0.0143(6) 0.0179(7) 0.0125(6) B1 0.025(6) 0.014(4) 0.026(5) 0.000(4) -0.023(4) -0.003(4) N1 0.026(4) 0.032(4) 0.026(4) 0.006(3) -0.001(3) 0.005(3) Cl2 0.037(2) 0.046(2) 0.0188(14) 0.0008(11) 0.0019(13) 0.0154(13) C1 0.020(5) 0.071(8) 0.040(7) -0.001(6) -0.008(5) 0.002(4) C2 0.043(11) 0.038(7) 0.024(8) -0.007(5) 0.005(6) 0.001(6) B1' 0.027(6) 0.026(6) 0.027(6) 0.0033(12) 0.0018(11) 0.007(2) N1' 0.014(13) 0.030(12) 0.083(19) 0.029(13) -0.013(14) 0.004(10) Cl2' 0.052(8) 0.060(6) 0.018(5) -0.001(4) -0.010(5) 0.016(5) C1' 0.027(9) 0.028(9) 0.028(9) 0.003(2) 0.002(2) 0.008(3) C2' 0.017(11) 0.016(11) 0.017(11) 0.001(2) 0.001(2) 0.005(4) P1 0.0244(8) 0.0203(7) 0.0208(7) 0.0071(5) 0.0030(6) 0.0064(6) P2 0.0262(8) 0.0200(7) 0.0198(7) 0.0069(5) 0.0035(6) 0.0058(6) C3 0.022(3) 0.029(3) 0.020(3) 0.007(2) 0.003(2) 0.008(2) C4 0.057(4) 0.031(3) 0.023(3) 0.007(2) 0.011(3) 0.021(3) C5 0.070(5) 0.050(4) 0.035(3) 0.026(3) 0.015(3) 0.034(3) C6 0.063(5) 0.070(4) 0.023(3) 0.018(3) 0.017(3) 0.036(4) C7 0.047(4) 0.056(4) 0.024(3) -0.002(3) 0.005(3) 0.025(3) C8 0.034(3) 0.030(3) 0.026(3) 0.004(2) 0.000(3) 0.011(3) C9 0.022(3) 0.021(3) 0.023(3) 0.002(2) 0.003(2) 0.010(2) C10 0.034(4) 0.030(3) 0.020(3) 0.004(2) 0.008(3) 0.008(3) C11 0.025(3) 0.036(3) 0.034(3) 0.002(2) 0.005(3) 0.001(3) C12 0.025(3) 0.040(3) 0.034(3) 0.000(3) 0.001(3) 0.008(3) C13 0.035(4) 0.047(4) 0.023(3) 0.005(3) -0.003(3) 0.013(3) C14 0.033(4) 0.038(3) 0.028(3) 0.014(2) 0.006(3) 0.002(3) C15 0.029(3) 0.026(3) 0.025(3) 0.012(2) 0.008(3) 0.008(2) C16 0.037(4) 0.029(3) 0.028(3) 0.009(2) 0.009(3) 0.012(3) C17 0.054(4) 0.042(3) 0.034(3) 0.010(3) 0.018(3) 0.025(3) C18 0.044(4) 0.054(4) 0.041(4) 0.026(3) 0.018(3) 0.031(3) C19 0.026(4) 0.050(4) 0.053(4) 0.022(3) 0.000(3) 0.013(3) C20 0.032(4) 0.035(3) 0.039(3) 0.011(3) -0.001(3) 0.008(3) C21 0.025(3) 0.030(3) 0.018(3) 0.008(2) 0.010(2) 0.007(2) C22 0.032(3) 0.030(3) 0.024(3) 0.005(2) 0.007(3) 0.012(3) C23 0.045(4) 0.039(3) 0.029(3) 0.010(3) 0.009(3) 0.023(3) C24 0.030(4) 0.066(4) 0.027(3) 0.014(3) 0.004(3) 0.021(3) C25 0.042(4) 0.047(4) 0.032(3) 0.003(3) -0.002(3) 0.011(3) C26 0.043(4) 0.033(3) 0.028(3) 0.006(2) 0.004(3) 0.009(3) C27 0.024(3) 0.029(3) 0.020(3) 0.006(2) 0.003(2) 0.008(2) C28 0.037(4) 0.030(3) 0.023(3) 0.007(2) 0.006(3) 0.006(3) C29 0.045(4) 0.043(4) 0.022(3) 0.008(3) 0.006(3) 0.012(3) C30 0.043(4) 0.040(3) 0.023(3) -0.005(2) 0.000(3) 0.016(3) C31 0.034(3) 0.027(3) 0.031(3) 0.001(2) -0.002(3) 0.008(3) C32 0.029(3) 0.027(3) 0.025(3) 0.007(2) 0.001(2) 0.004(2) C33 0.035(4) 0.018(3) 0.027(3) 0.008(2) 0.014(3) 0.009(2) C34 0.039(4) 0.031(3) 0.026(3) 0.007(2) 0.006(3) 0.013(3) C35 0.059(5) 0.038(3) 0.029(3) 0.012(3) 0.020(3) 0.020(3) C36 0.056(5) 0.031(3) 0.053(4) 0.020(3) 0.039(4) 0.013(3) C37 0.036(4) 0.026(3) 0.051(4) 0.004(3) 0.018(3) 0.004(3) C38 0.031(4) 0.025(3) 0.030(3) 0.003(2) 0.005(3) 0.005(3) _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 B1' 2.03(2) . ? Pt1 B1 2.075(10) . ? Pt1 P2 2.288(2) . ? Pt1 P1 2.291(2) . ? Pt1 Cl1 2.470(2) . ? B1 N1 1.385(10) . ? B1 Cl2 1.815(8) . ? N1 C2 1.433(14) . ? N1 C1 1.460(9) . ? B1' N1' 1.36(2) . ? B1' Cl2' 1.78(2) . ? N1' C2' 1.43(2) . ? N1' C1' 1.45(2) . ? P1 C9 1.809(5) . ? P1 C3 1.817(5) . ? P1 C15 1.838(5) . ? P2 C21 1.821(5) . ? P2 C27 1.823(5) . ? P2 C33 1.844(5) . ? C3 C4 1.392(6) . ? C3 C8 1.395(6) . ? C4 C5 1.386(7) . ? C5 C6 1.373(7) . ? C6 C7 1.375(7) . ? C7 C8 1.382(7) . ? C9 C10 1.392(6) . ? C9 C14 1.397(7) . ? C10 C11 1.397(7) . ? C11 C12 1.378(7) . ? C12 C13 1.377(7) . ? C13 C14 1.374(7) . ? C15 C20 1.384(7) . ? C15 C16 1.398(7) . ? C16 C17 1.381(7) . ? C17 C18 1.360(8) . ? C18 C19 1.376(8) . ? C19 C20 1.396(7) . ? C21 C26 1.387(7) . ? C21 C22 1.390(6) . ? C22 C23 1.380(7) . ? C23 C24 1.378(8) . ? C24 C25 1.381(7) . ? C25 C26 1.385(7) . ? C27 C32 1.386(6) . ? C27 C28 1.403(6) . ? C28 C29 1.375(7) . ? C29 C30 1.384(7) . ? C30 C31 1.383(7) . ? C31 C32 1.385(7) . ? C33 C38 1.367(7) . ? C33 C34 1.397(7) . ? C34 C35 1.389(7) . ? C35 C36 1.362(8) . ? C36 C37 1.374(8) . ? C37 C38 1.392(7) . ? 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 B1' Pt1 P2 86.0(7) . . ? B1 Pt1 P2 89.9(2) . . ? B1' Pt1 P1 94.7(7) . . ? B1 Pt1 P1 90.4(2) . . ? P2 Pt1 P1 178.73(5) . . ? B1' Pt1 Cl1 159.9(6) . . ? B1 Pt1 Cl1 175.9(2) . . ? P2 Pt1 Cl1 91.82(4) . . ? P1 Pt1 Cl1 87.79(4) . . ? N1 B1 Cl2 117.4(7) . . ? N1 B1 Pt1 126.7(6) . . ? Cl2 B1 Pt1 115.9(4) . . ? B1 N1 C2 122.9(9) . . ? B1 N1 C1 126.4(7) . . ? C2 N1 C1 110.7(9) . . ? N1' B1' Cl2' 118.6(17) . . ? N1' B1' Pt1 124.4(16) . . ? Cl2' B1' Pt1 116.6(11) . . ? B1' N1' C2' 122.8(26) . . ? B1' N1' C1' 129.6(22) . . ? C2' N1' C1' 107.5(24) . . ? C9 P1 C3 106.8(2) . . ? C9 P1 C15 103.3(2) . . ? C3 P1 C15 102.5(2) . . ? C9 P1 Pt1 107.77(15) . . ? C3 P1 Pt1 114.9(2) . . ? C15 P1 Pt1 120.4(2) . . ? C21 P2 C27 106.1(2) . . ? C21 P2 C33 101.6(2) . . ? C27 P2 C33 104.6(2) . . ? C21 P2 Pt1 114.9(2) . . ? C27 P2 Pt1 111.7(2) . . ? C33 P2 Pt1 116.76(15) . . ? C4 C3 C8 118.6(4) . . ? C4 C3 P1 120.6(3) . . ? C8 C3 P1 120.8(4) . . ? C5 C4 C3 120.0(5) . . ? C6 C5 C4 120.5(5) . . ? C5 C6 C7 120.3(5) . . ? C6 C7 C8 119.7(5) . . ? C7 C8 C3 120.9(5) . . ? C10 C9 C14 118.1(5) . . ? C10 C9 P1 123.6(4) . . ? C14 C9 P1 118.3(4) . . ? C9 C10 C11 120.5(4) . . ? C12 C11 C10 119.7(5) . . ? C13 C12 C11 120.5(5) . . ? C14 C13 C12 119.8(5) . . ? C13 C14 C9 121.4(5) . . ? C20 C15 C16 118.7(5) . . ? C20 C15 P1 118.7(4) . . ? C16 C15 P1 122.6(4) . . ? C17 C16 C15 119.8(5) . . ? C18 C17 C16 121.5(6) . . ? C17 C18 C19 119.4(5) . . ? C18 C19 C20 120.4(6) . . ? C15 C20 C19 120.2(5) . . ? C26 C21 C22 118.6(5) . . ? C26 C21 P2 119.7(4) . . ? C22 C21 P2 121.4(4) . . ? C23 C22 C21 121.0(5) . . ? C24 C23 C22 119.8(5) . . ? C23 C24 C25 120.1(5) . . ? C24 C25 C26 120.1(6) . . ? C25 C26 C21 120.4(5) . . ? C32 C27 C28 118.7(4) . . ? C32 C27 P2 123.1(3) . . ? C28 C27 P2 118.2(4) . . ? C29 C28 C27 120.9(5) . . ? C28 C29 C30 119.8(5) . . ? C31 C30 C29 120.0(5) . . ? C30 C31 C32 120.3(5) . . ? C31 C32 C27 120.3(4) . . ? C38 C33 C34 119.1(5) . . ? C38 C33 P2 120.7(4) . . ? C34 C33 P2 120.0(4) . . ? C35 C34 C33 120.0(5) . . ? C36 C35 C34 119.9(5) . . ? C35 C36 C37 120.8(5) . . ? C36 C37 C38 119.4(6) . . ? C33 C38 C37 120.8(5) . . ? _refine_diff_density_max 1.222 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.116