# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 891983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H104 B2 Cl6 N4 P4 Pt2' _chemical_formula_weight 1569.80 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.0190(16) _cell_length_b 30.009(6) _cell_length_c 14.163(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.391(4) _cell_angle_gamma 90.00 _cell_volume 3398.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 93.1500 _cell_measurement_reflns_used 9282 _cell_measurement_theta_min 2.4953 _cell_measurement_theta_max 31.1268 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 4.479 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5531 _exptl_absorpt_correction_T_max 0.8071 _exptl_absorpt_process_details '(NUMABS; Rigaku, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93.1500 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSC Meacury CCD' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22840 _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5971 _reflns_number_gt 4956 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5971 _refine_ls_number_parameters 418 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.44094(3) 0.186352(9) 0.267589(18) 0.02697(12) Uani 1 1 d . . . Cl1 Cl 0.5745(2) 0.22532(6) 0.14112(12) 0.0387(5) Uani 1 1 d . . . P1 P 0.3401(2) 0.24587(6) 0.35027(12) 0.0267(4) Uani 1 1 d . . . P2 P 0.5088(2) 0.11312(6) 0.23796(12) 0.0275(4) Uani 1 1 d . . . B1 B 0.3209(10) 0.1540(3) 0.3645(6) 0.0322(19) Uani 1 1 d . . . N1 N 0.2408(7) 0.1741(2) 0.4404(4) 0.0300(14) Uani 1 1 d . . . N2 N 0.3019(7) 0.10779(19) 0.3732(4) 0.0302(14) Uani 1 1 d . . . C1 C 0.1732(9) 0.1409(2) 0.4929(5) 0.0298(16) Uani 1 1 d . . . C2 C 0.0851(9) 0.1427(3) 0.5737(5) 0.0332(17) Uani 1 1 d . . . H1 H 0.0608 0.1704 0.6021 0.019(16) Uiso 1 1 calc R . . C3 C 0.0334(10) 0.1024(3) 0.6115(5) 0.0399(19) Uani 1 1 d . . . H2 H -0.0272 0.1029 0.6666 0.04(2) Uiso 1 1 calc R . . C4 C 0.0686(9) 0.0617(3) 0.5707(5) 0.0377(18) Uani 1 1 d . . . H3 H 0.0305 0.0350 0.5979 0.016(16) Uiso 1 1 calc R . . C5 C 0.1593(9) 0.0594(3) 0.4900(5) 0.0360(18) Uani 1 1 d . . . H4 H 0.1850 0.0314 0.4632 0.005(14) Uiso 1 1 calc R . . C6 C 0.2102(9) 0.0986(2) 0.4505(5) 0.0297(16) Uani 1 1 d . . . C7 C 0.2437(9) 0.2220(2) 0.4570(5) 0.0345(18) Uani 1 1 d . . . H5 H 0.3123 0.2293 0.5160 0.05(2) Uiso 1 1 calc R . . H6 H 0.1292 0.2337 0.4615 0.04(2) Uiso 1 1 calc R . . C8 C 0.5071(9) 0.2840(3) 0.4060(5) 0.0329(17) Uani 1 1 d . . . C9 C 0.5780(11) 0.3137(3) 0.3307(6) 0.041(2) Uani 1 1 d . . . H7 H 0.4907 0.3340 0.3045 0.05(3) Uiso 1 1 calc R . . H8 H 0.6164 0.2950 0.2799 0.026(18) Uiso 1 1 calc R . . H9 H 0.6722 0.3310 0.3596 0.07(3) Uiso 1 1 calc R . . C10 C 0.6447(10) 0.2536(3) 0.4472(6) 0.050(2) Uani 1 1 d . . . H10 H 0.6937 0.2375 0.3959 0.06(3) Uiso 1 1 calc R . . H11 H 0.5981 0.2322 0.4904 0.04(2) Uiso 1 1 calc R . . H12 H 0.7315 0.2714 0.4821 0.07(3) Uiso 1 1 calc R . . C11 C 0.4453(11) 0.3138(2) 0.4853(6) 0.041(2) Uani 1 1 d . . . H13 H 0.5415 0.3278 0.5205 0.04(2) Uiso 1 1 calc R . . H14 H 0.3840 0.2956 0.5284 0.027(19) Uiso 1 1 calc R . . H15 H 0.3712 0.3370 0.4570 0.05(2) Uiso 1 1 calc R . . C12 C 0.1619(8) 0.2762(2) 0.2846(5) 0.0321(17) Uani 1 1 d . . . C13 C 0.2178(10) 0.2968(3) 0.1935(5) 0.044(2) Uani 1 1 d . . . H16 H 0.1200 0.3084 0.1554 0.03(2) Uiso 1 1 calc R . . H17 H 0.2731 0.2741 0.1573 0.07(3) Uiso 1 1 calc R . . H18 H 0.2961 0.3213 0.2093 0.05(3) Uiso 1 1 calc R . . C14 C 0.0279(9) 0.2402(3) 0.2598(7) 0.050(2) Uani 1 1 d . . . H19 H -0.0097 0.2275 0.3183 0.07(3) Uiso 1 1 calc R . . H20 H 0.0760 0.2165 0.2226 0.04(2) Uiso 1 1 calc R . . H21 H -0.0674 0.2536 0.2229 0.04(2) Uiso 1 1 calc R . . C15 C 0.0847(10) 0.3128(3) 0.3440(6) 0.040(2) Uani 1 1 d . . . H22 H -0.0179 0.3240 0.3101 0.03(2) Uiso 1 1 calc R . . H23 H 0.1647 0.3373 0.3547 0.05(2) Uiso 1 1 calc R . . H24 H 0.0583 0.3004 0.4051 0.12(5) Uiso 1 1 calc R . . C16 C 0.3677(9) 0.0768(2) 0.3058(5) 0.0333(17) Uani 1 1 d . . . H25 H 0.2766 0.0639 0.2633 0.07(3) Uiso 1 1 calc R . . H26 H 0.4313 0.0524 0.3389 0.025(18) Uiso 1 1 calc R . . C17 C 0.7254(9) 0.0993(3) 0.2911(5) 0.0337(18) Uani 1 1 d . . . C18 C 0.8502(10) 0.1318(3) 0.2543(6) 0.051(2) Uani 1 1 d . . . H27 H 0.8107 0.1624 0.2626 0.11(4) Uiso 1 1 calc R . . H28 H 0.8613 0.1261 0.1870 0.05(3) Uiso 1 1 calc R . . H29 H 0.9591 0.1280 0.2897 0.04(2) Uiso 1 1 calc R . . C19 C 0.7789(10) 0.0509(3) 0.2774(6) 0.041(2) Uani 1 1 d . . . H30 H 0.7955 0.0458 0.2104 0.06(3) Uiso 1 1 calc R . . H31 H 0.6918 0.0309 0.2973 0.07(3) Uiso 1 1 calc R . . H32 H 0.8838 0.0452 0.3156 0.030(19) Uiso 1 1 calc R . . C20 C 0.7206(12) 0.1086(4) 0.3983(6) 0.055(3) Uani 1 1 d . . . H33 H 0.8335 0.1058 0.4294 0.03(2) Uiso 1 1 calc R . . H34 H 0.6463 0.0871 0.4259 0.24(9) Uiso 1 1 calc R . . H35 H 0.6787 0.1389 0.4076 0.13(5) Uiso 1 1 calc R . . C21 C 0.4689(9) 0.0919(2) 0.1135(5) 0.0332(17) Uani 1 1 d . . . C22 C 0.6067(11) 0.1094(3) 0.0531(5) 0.048(2) Uani 1 1 d . . . H36 H 0.7102 0.0926 0.0686 0.06(3) Uiso 1 1 calc R . . H37 H 0.6263 0.1410 0.0665 0.016(16) Uiso 1 1 calc R . . H38 H 0.5714 0.1055 -0.0142 0.13(4) Uiso 1 1 calc R . . C23 C 0.4580(10) 0.0415(2) 0.1050(5) 0.0389(19) Uani 1 1 d . . . H39 H 0.4292 0.0333 0.0388 0.06(3) Uiso 1 1 calc R . . H40 H 0.3717 0.0304 0.1444 0.001(13) Uiso 1 1 calc R . . H41 H 0.5661 0.0284 0.1265 0.025(19) Uiso 1 1 calc R . . C24 C 0.3041(11) 0.1131(3) 0.0767(6) 0.052(2) Uani 1 1 d . . . H42 H 0.2746 0.1031 0.0117 0.06(3) Uiso 1 1 calc R . . H43 H 0.3155 0.1456 0.0776 0.08(3) Uiso 1 1 calc R . . H44 H 0.2159 0.1043 0.1172 0.06(3) Uiso 1 1 calc R . . C25 C 0.462(2) 0.0853(5) 0.6811(10) 0.052(4) Uiso 0.57(2) 1 d PDU A 1 H45 H 0.3632 0.0887 0.6354 0.02(4) Uiso 0.57(2) 1 calc PR A 1 H46 H 0.5207 0.1144 0.6857 0.12(7) Uiso 0.57(2) 1 calc PR A 1 Cl2 Cl 0.3946(15) 0.0717(3) 0.7922(5) 0.0588(17) Uani 0.57(2) 1 d PDU A 1 Cl5 Cl 0.5713(16) 0.0386(4) 0.6043(10) 0.070(2) Uani 0.43(2) 1 d PDU A 2 C26 C 0.504(4) 0.0841(7) 0.6699(16) 0.056(4) Uiso 0.43(2) 1 d PDU A 2 H47 H 0.5932 0.1071 0.6745 0.03(4) Uiso 0.43(2) 1 calc PR A 2 H48 H 0.4037 0.0974 0.6361 0.11(10) Uiso 0.43(2) 1 calc PR A 2 Cl4 Cl 0.4572(19) 0.0685(4) 0.7848(8) 0.065(2) Uani 0.43(2) 1 d PU A 2 Cl3 Cl 0.5974(13) 0.0453(3) 0.6370(9) 0.076(2) Uani 0.57(2) 1 d PDU A 1 C27 C 1.0000 0.0000 1.0000 0.099(3) Uani 1 2 d SDU . . C28 C 0.9305(15) 0.0519(4) 0.8586(7) 0.103(3) Uani 1 1 d DU . . H49 H 0.9648 0.0560 0.7942 0.155 Uiso 0.50 1 calc PR B 1 H50 H 0.9567 0.0789 0.8958 0.155 Uiso 0.50 1 calc PR B 1 H51 H 0.8099 0.0462 0.8561 0.155 Uiso 0.50 1 calc PR B 1 H52 H 0.8614 0.0782 0.8425 0.155 Uiso 0.50 1 calc PR B 2 H53 H 0.8945 0.0272 0.8168 0.155 Uiso 0.50 1 calc PR B 2 H54 H 1.0480 0.0589 0.8507 0.155 Uiso 0.50 1 calc PR B 2 C29 C 1.023(3) 0.0130(6) 0.9043(9) 0.099(3) Uani 0.50 1 d PDU C 1 H55 H 0.9956 -0.0133 0.8639 0.119 Uiso 0.50 1 calc PR C 1 H56 H 1.1437 0.0189 0.9009 0.119 Uiso 0.50 1 calc PR C 1 C30 C 0.912(3) 0.0394(6) 0.9561(10) 0.100(3) Uani 0.50 1 d PDU C 2 H57 H 0.7911 0.0349 0.9623 0.120 Uiso 0.50 1 calc PR C 2 H58 H 0.9462 0.0655 0.9957 0.120 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0305(2) 0.02780(19) 0.02311(19) -0.00016(10) 0.00537(14) 0.00034(11) Cl1 0.0483(11) 0.0366(11) 0.0337(10) 0.0061(8) 0.0181(9) 0.0027(9) P1 0.0289(10) 0.0297(10) 0.0219(9) -0.0006(7) 0.0050(8) -0.0010(8) P2 0.0301(10) 0.0291(10) 0.0236(10) -0.0017(7) 0.0035(8) 0.0014(8) B1 0.027(4) 0.031(5) 0.038(5) -0.002(4) 0.003(4) 0.000(4) N1 0.040(4) 0.024(3) 0.027(3) 0.004(2) 0.010(3) -0.003(3) N2 0.032(3) 0.027(3) 0.031(3) -0.007(3) 0.003(3) -0.002(3) C1 0.035(4) 0.030(4) 0.023(4) 0.000(3) -0.001(3) 0.005(3) C2 0.038(4) 0.038(5) 0.023(4) -0.004(3) 0.001(3) -0.001(4) C3 0.048(5) 0.042(5) 0.032(4) 0.003(3) 0.014(4) 0.001(4) C4 0.038(4) 0.042(5) 0.033(4) 0.013(4) 0.004(3) -0.002(4) C5 0.041(4) 0.038(5) 0.029(4) 0.005(3) -0.002(3) 0.002(4) C6 0.029(4) 0.035(4) 0.026(4) 0.000(3) 0.004(3) 0.000(3) C7 0.042(5) 0.036(5) 0.027(4) 0.000(3) 0.011(4) -0.001(4) C8 0.033(4) 0.038(5) 0.028(4) -0.007(3) 0.003(3) -0.003(3) C9 0.044(5) 0.049(5) 0.031(5) -0.001(4) 0.010(4) -0.018(4) C10 0.045(5) 0.061(6) 0.042(5) -0.007(4) -0.006(4) 0.005(5) C11 0.042(5) 0.039(5) 0.043(5) -0.011(4) 0.009(4) -0.007(4) C12 0.031(4) 0.031(4) 0.035(4) -0.002(3) 0.004(3) 0.000(3) C13 0.047(5) 0.061(6) 0.023(4) 0.010(4) -0.002(4) 0.015(5) C14 0.033(5) 0.054(6) 0.062(6) -0.017(5) -0.011(4) 0.003(4) C15 0.041(5) 0.044(5) 0.036(5) -0.007(3) 0.002(4) 0.004(4) C16 0.033(4) 0.034(4) 0.032(4) -0.003(3) 0.006(3) -0.007(3) C17 0.026(4) 0.039(5) 0.035(4) 0.002(3) -0.006(3) 0.003(3) C18 0.034(5) 0.048(6) 0.069(7) 0.006(5) -0.004(4) 0.003(4) C19 0.038(5) 0.039(5) 0.046(5) -0.001(4) 0.000(4) 0.009(4) C20 0.051(6) 0.066(7) 0.043(5) -0.009(5) -0.018(5) 0.018(5) C21 0.033(4) 0.037(5) 0.029(4) -0.005(3) 0.001(3) -0.006(3) C22 0.064(6) 0.054(6) 0.027(5) -0.001(4) 0.012(4) -0.002(5) C23 0.048(5) 0.034(5) 0.036(5) -0.009(3) 0.012(4) -0.004(4) C24 0.061(6) 0.047(6) 0.044(5) -0.007(4) -0.023(5) 0.003(5) Cl2 0.067(4) 0.057(2) 0.052(2) 0.0015(18) 0.001(3) -0.004(3) Cl5 0.072(3) 0.065(3) 0.073(4) 0.008(3) 0.009(3) 0.008(3) Cl4 0.072(4) 0.061(3) 0.061(3) 0.000(2) -0.004(3) -0.005(4) Cl3 0.075(3) 0.074(3) 0.080(4) 0.010(3) 0.015(3) 0.013(3) C27 0.092(4) 0.095(4) 0.109(4) 0.004(3) 0.001(3) -0.005(3) C28 0.096(4) 0.099(4) 0.114(4) 0.008(3) 0.004(3) -0.005(3) C29 0.094(4) 0.097(4) 0.106(4) 0.003(3) 0.004(3) -0.005(3) C30 0.094(4) 0.097(4) 0.108(4) 0.004(3) 0.004(3) -0.004(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 1.989(9) . ? Pt1 P2 2.3101(19) . ? Pt1 P1 2.3152(19) . ? Pt1 Cl1 2.4530(18) . ? P1 C12 1.879(7) . ? P1 C8 1.888(7) . ? P1 C7 1.890(7) . ? P2 C21 1.879(7) . ? P2 C16 1.885(7) . ? P2 C17 1.886(7) . ? B1 N2 1.402(10) . ? B1 N1 1.427(10) . ? N1 C1 1.378(9) . ? N1 C7 1.457(9) . ? N2 C6 1.393(8) . ? N2 C16 1.459(8) . ? C1 C2 1.390(9) . ? C1 C6 1.446(9) . ? C2 C3 1.399(10) . ? C3 C4 1.390(10) . ? C4 C5 1.402(9) . ? C5 C6 1.378(10) . ? C8 C10 1.514(10) . ? C8 C9 1.532(10) . ? C8 C11 1.547(10) . ? C12 C13 1.530(10) . ? C12 C15 1.542(9) . ? C12 C14 1.546(10) . ? C17 C18 1.518(10) . ? C17 C19 1.530(10) . ? C17 C20 1.548(10) . ? C21 C23 1.518(9) . ? C21 C24 1.522(10) . ? C21 C22 1.540(10) . ? C25 Cl3 1.764(9) . ? C25 Cl2 1.752(10) . ? Cl5 C26 1.759(7) . ? C26 Cl4 1.76(2) . ? C27 C29 1.435(9) 3_757 ? C27 C29 1.435(9) . ? C27 C30 1.488(10) . ? C27 C30 1.488(10) 3_757 ? C28 C30 1.449(10) . ? C28 C29 1.502(10) . ? 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 78.1(3) . . ? B1 Pt1 P1 79.7(3) . . ? P2 Pt1 P1 157.22(6) . . ? B1 Pt1 Cl1 176.5(2) . . ? P2 Pt1 Cl1 101.47(6) . . ? P1 Pt1 Cl1 100.98(6) . . ? C12 P1 C8 113.7(3) . . ? C12 P1 C7 103.7(3) . . ? C8 P1 C7 102.5(3) . . ? C12 P1 Pt1 113.9(2) . . ? C8 P1 Pt1 114.5(2) . . ? C7 P1 Pt1 107.0(2) . . ? C21 P2 C16 102.5(3) . . ? C21 P2 C17 112.7(3) . . ? C16 P2 C17 103.9(3) . . ? C21 P2 Pt1 117.8(2) . . ? C16 P2 Pt1 107.3(2) . . ? C17 P2 Pt1 111.1(2) . . ? N2 B1 N1 107.0(7) . . ? N2 B1 Pt1 127.2(6) . . ? N1 B1 Pt1 125.7(6) . . ? C1 N1 B1 108.7(6) . . ? C1 N1 C7 128.9(6) . . ? B1 N1 C7 122.3(6) . . ? C6 N2 B1 109.4(6) . . ? C6 N2 C16 128.8(6) . . ? B1 N2 C16 121.7(6) . . ? N1 C1 C2 131.4(7) . . ? N1 C1 C6 108.0(6) . . ? C2 C1 C6 120.6(7) . . ? C1 C2 C3 117.7(7) . . ? C4 C3 C2 121.7(7) . . ? C3 C4 C5 121.1(7) . . ? C6 C5 C4 118.5(7) . . ? C5 C6 N2 132.8(7) . . ? C5 C6 C1 120.3(7) . . ? N2 C6 C1 106.8(6) . . ? N1 C7 P1 104.4(4) . . ? C10 C8 C9 108.7(7) . . ? C10 C8 C11 109.5(6) . . ? C9 C8 C11 109.0(6) . . ? C10 C8 P1 105.6(5) . . ? C9 C8 P1 110.5(5) . . ? C11 C8 P1 113.4(5) . . ? C13 C12 C15 109.1(6) . . ? C13 C12 C14 109.6(6) . . ? C15 C12 C14 108.7(6) . . ? C13 C12 P1 110.7(5) . . ? C15 C12 P1 113.4(5) . . ? C14 C12 P1 105.2(5) . . ? N2 C16 P2 103.1(5) . . ? C18 C17 C19 111.6(7) . . ? C18 C17 C20 106.7(7) . . ? C19 C17 C20 108.9(7) . . ? C18 C17 P2 109.5(5) . . ? C19 C17 P2 114.6(5) . . ? C20 C17 P2 105.1(5) . . ? C23 C21 C24 110.2(6) . . ? C23 C21 C22 109.5(6) . . ? C24 C21 C22 108.0(7) . . ? C23 C21 P2 114.6(5) . . ? C24 C21 P2 105.1(5) . . ? C22 C21 P2 109.2(5) . . ? Cl3 C25 Cl2 113.6(8) . . ? Cl4 C26 Cl5 112.1(12) . . ? C29 C27 C29 180.000(6) 3_757 . ? C29 C27 C30 121.3(8) 3_757 . ? C29 C27 C30 58.7(8) . . ? C29 C27 C30 58.7(8) 3_757 3_757 ? C29 C27 C30 121.3(8) . 3_757 ? C30 C27 C30 180.0(8) . 3_757 ? C30 C28 C29 58.1(8) . . ? C27 C29 C28 121.6(10) . . ? C28 C30 C27 121.6(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.764 _refine_diff_density_min -1.331 _refine_diff_density_rms 0.147 _chemical_absolute_configuration ? data_3 _database_code_depnum_ccdc_archive 'CCDC 891984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H44 B F3 N2 O3 P2 Pt S' _chemical_formula_weight 777.52 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.0942(18) _cell_length_b 17.423(4) _cell_length_c 21.755(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.554(4) _cell_angle_gamma 90.00 _cell_volume 3062.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 93.1500 _cell_measurement_reflns_used 11819 _cell_measurement_theta_min 2.5192 _cell_measurement_theta_max 31.0697 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 4.803 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4468 _exptl_absorpt_correction_T_max 0.6452 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSCIO Saturn CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 20222 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5379 _reflns_number_gt 4858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5379 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.316377(12) 0.234376(6) 0.146737(4) 0.00857(4) Uani 1 1 d . . . P1 P 0.23811(8) 0.30119(4) 0.05672(3) 0.01001(15) Uani 1 1 d . . . P2 P 0.43970(8) 0.13957(4) 0.20899(3) 0.00924(15) Uani 1 1 d . . . B1 B 0.4412(4) 0.17756(18) 0.08669(14) 0.0127(7) Uani 1 1 d . . . N1 N 0.4550(3) 0.19654(13) 0.02388(10) 0.0129(5) Uani 1 1 d . . . C1 C 0.5565(3) 0.14240(15) -0.00255(12) 0.0118(6) Uani 1 1 d . . . C2 C 0.6099(3) 0.13672(16) -0.06154(12) 0.0143(6) Uani 1 1 d . . . H1 H 0.5769 0.1733 -0.0923 0.019(8) Uiso 1 1 calc R . . C3 C 0.7137(3) 0.07569(16) -0.07446(12) 0.0157(6) Uani 1 1 d . . . H2 H 0.7523 0.0709 -0.1146 0.016(8) Uiso 1 1 calc R . . C4 C 0.7617(3) 0.02196(16) -0.03004(13) 0.0158(6) Uani 1 1 d . . . H3 H 0.8324 -0.0190 -0.0403 0.020(8) Uiso 1 1 calc R . . C5 C 0.7081(3) 0.02704(16) 0.02958(13) 0.0148(6) Uani 1 1 d . . . H4 H 0.7407 -0.0101 0.0599 0.010(7) Uiso 1 1 calc R . . C6 C 0.6061(3) 0.08754(15) 0.04325(12) 0.0111(6) Uani 1 1 d . . . N2 N 0.5354(3) 0.10933(12) 0.09780(10) 0.0117(5) Uani 1 1 d . . . C7 C 0.3800(3) 0.26558(15) -0.00218(13) 0.0148(6) Uani 1 1 d . . . H5 H 0.3170 0.2541 -0.0416 0.026(9) Uiso 1 1 calc R . . H6 H 0.4657 0.3044 -0.0098 0.014(7) Uiso 1 1 calc R . . C8 C 0.5345(3) 0.06942(15) 0.15598(12) 0.0119(6) Uani 1 1 d . . . H7 H 0.6485 0.0558 0.1713 0.024(8) Uiso 1 1 calc R . . H8 H 0.4675 0.0220 0.1519 0.014(7) Uiso 1 1 calc R . . C9 C 0.0268(3) 0.27005(15) 0.02671(14) 0.0154(6) Uani 1 1 d . . . C10 C -0.0343(4) 0.30879(18) -0.03435(13) 0.0208(7) Uani 1 1 d . . . H9 H -0.1382 0.2849 -0.0499 0.030(9) Uiso 1 1 calc R . . H10 H 0.0493 0.3025 -0.0647 0.030(9) Uiso 1 1 calc R . . H11 H -0.0526 0.3636 -0.0272 0.015(8) Uiso 1 1 calc R . . C11 C -0.0966(3) 0.28467(19) 0.07560(14) 0.0224(7) Uani 1 1 d . . . H12 H -0.2032 0.2612 0.0627 0.035(10) Uiso 1 1 calc R . . H13 H -0.1113 0.3401 0.0807 0.024(9) Uiso 1 1 calc R . . H14 H -0.0547 0.2621 0.1148 0.040(11) Uiso 1 1 calc R . . C12 C 0.0380(4) 0.18264(16) 0.01568(14) 0.0204(7) Uani 1 1 d . . . H15 H 0.0719 0.1569 0.0545 0.039(10) Uiso 1 1 calc R . . H16 H 0.1196 0.1724 -0.0147 0.036(10) Uiso 1 1 calc R . . H17 H -0.0704 0.1632 0.0003 0.019(8) Uiso 1 1 calc R . . C13 C 0.2693(4) 0.40774(16) 0.05289(13) 0.0158(6) Uani 1 1 d . . . C14 C 0.1279(4) 0.45111(16) 0.08142(13) 0.0216(7) Uani 1 1 d . . . H18 H 0.1092 0.4293 0.1219 0.035(9) Uiso 1 1 calc R . . H19 H 0.0267 0.4463 0.0545 0.035(10) Uiso 1 1 calc R . . H20 H 0.1574 0.5054 0.0860 0.029(9) Uiso 1 1 calc R . . C15 C 0.2853(4) 0.43851(17) -0.01263(13) 0.0206(7) Uani 1 1 d . . . H21 H 0.2948 0.4946 -0.0114 0.025(9) Uiso 1 1 calc R . . H22 H 0.1870 0.4240 -0.0386 0.035(10) Uiso 1 1 calc R . . H23 H 0.3841 0.4166 -0.0297 0.032(9) Uiso 1 1 calc R . . C16 C 0.4310(4) 0.42247(17) 0.09167(14) 0.0219(7) Uani 1 1 d . . . H24 H 0.5206 0.3927 0.0750 0.032(9) Uiso 1 1 calc R . . H25 H 0.4175 0.4069 0.1344 0.021(8) Uiso 1 1 calc R . . H26 H 0.4582 0.4772 0.0905 0.025(9) Uiso 1 1 calc R . . C17 C 0.6216(3) 0.17740(16) 0.25714(12) 0.0137(6) Uani 1 1 d . . . C18 C 0.7449(3) 0.20683(17) 0.21168(13) 0.0181(6) Uani 1 1 d . . . H27 H 0.8448 0.2257 0.2346 0.029(9) Uiso 1 1 calc R . . H28 H 0.6941 0.2487 0.1870 0.036(11) Uiso 1 1 calc R . . H29 H 0.7744 0.1649 0.1844 0.014(7) Uiso 1 1 calc R . . C19 C 0.7049(4) 0.11772(17) 0.30033(13) 0.0206(7) Uani 1 1 d . . . H30 H 0.7306 0.0718 0.2767 0.024(8) Uiso 1 1 calc R . . H31 H 0.6300 0.1040 0.3323 0.037(10) Uiso 1 1 calc R . . H32 H 0.8074 0.1391 0.3196 0.035(9) Uiso 1 1 calc R . . C20 C 0.5671(4) 0.24674(17) 0.29469(14) 0.0205(7) Uani 1 1 d . . . H33 H 0.4929 0.2294 0.3258 0.019(8) Uiso 1 1 calc R . . H34 H 0.5089 0.2837 0.2671 0.037(10) Uiso 1 1 calc R . . H35 H 0.6647 0.2713 0.3150 0.023(9) Uiso 1 1 calc R . . C21 C 0.2920(3) 0.08002(16) 0.25217(13) 0.0131(6) Uani 1 1 d . . . C22 C 0.3622(4) 0.00023(16) 0.26976(14) 0.0197(7) Uani 1 1 d . . . H36 H 0.4680 0.0062 0.2937 0.039(10) Uiso 1 1 calc R . . H37 H 0.3793 -0.0291 0.2323 0.034(10) Uiso 1 1 calc R . . H38 H 0.2839 -0.0271 0.2945 0.022(8) Uiso 1 1 calc R . . C23 C 0.2407(4) 0.12197(17) 0.31018(13) 0.0206(7) Uani 1 1 d . . . H39 H 0.2080 0.1747 0.2995 0.024(9) Uiso 1 1 calc R . . H40 H 0.3341 0.1228 0.3411 0.022(8) Uiso 1 1 calc R . . H41 H 0.1471 0.0951 0.3270 0.025(9) Uiso 1 1 calc R . . C24 C 0.1380(3) 0.07062(17) 0.20790(14) 0.0180(7) Uani 1 1 d . . . H42 H 0.0606 0.0349 0.2258 0.020(8) Uiso 1 1 calc R . . H43 H 0.1709 0.0503 0.1685 0.021(8) Uiso 1 1 calc R . . H44 H 0.0843 0.1206 0.2012 0.022(8) Uiso 1 1 calc R . . O1 O 0.1752(2) 0.28626(11) 0.22436(8) 0.0158(4) Uani 1 1 d . . . S1 S 0.14073(9) 0.36480(4) 0.24371(3) 0.01541(16) Uani 1 1 d . . . O2 O -0.0166(3) 0.39384(13) 0.21990(9) 0.0281(5) Uani 1 1 d . . . O3 O 0.2796(3) 0.41549(13) 0.24300(10) 0.0313(6) Uani 1 1 d . . . C25 C 0.1119(3) 0.35198(16) 0.32563(13) 0.0167(6) Uani 1 1 d . . . F1 F 0.0779(2) 0.41904(10) 0.35170(8) 0.0274(4) Uani 1 1 d . . . F2 F -0.0133(2) 0.30400(11) 0.33498(8) 0.0293(4) Uani 1 1 d . . . F3 F 0.2461(2) 0.32324(11) 0.35562(7) 0.0295(4) Uani 1 1 d . . . 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 0.00947(6) 0.00960(7) 0.00657(6) 0.00035(4) -0.00015(4) 0.00080(4) P1 0.0114(3) 0.0103(4) 0.0082(3) 0.0012(3) -0.0011(3) 0.0007(3) P2 0.0096(3) 0.0113(4) 0.0067(3) 0.0002(3) -0.0007(3) 0.0006(3) B1 0.0115(15) 0.0149(18) 0.0116(16) -0.0020(13) 0.0002(13) -0.0020(12) N1 0.0153(12) 0.0135(13) 0.0099(12) 0.0022(10) 0.0004(10) 0.0056(10) C1 0.0098(13) 0.0139(15) 0.0117(14) -0.0031(11) 0.0005(11) -0.0013(11) C2 0.0134(14) 0.0194(16) 0.0101(14) -0.0007(12) 0.0003(12) -0.0032(11) C3 0.0141(14) 0.0239(17) 0.0096(14) -0.0073(12) 0.0049(12) -0.0035(12) C4 0.0117(14) 0.0159(16) 0.0198(16) -0.0067(12) 0.0016(12) 0.0009(11) C5 0.0153(14) 0.0136(16) 0.0151(15) -0.0004(12) -0.0034(12) -0.0019(11) C6 0.0110(13) 0.0143(15) 0.0078(13) -0.0024(11) -0.0018(11) -0.0030(11) N2 0.0134(12) 0.0133(13) 0.0081(12) 0.0006(9) -0.0003(10) 0.0017(9) C7 0.0151(14) 0.0185(16) 0.0109(15) 0.0022(12) 0.0010(12) -0.0003(12) C8 0.0164(14) 0.0100(15) 0.0092(14) 0.0006(11) -0.0001(11) 0.0016(11) C9 0.0120(14) 0.0098(15) 0.0240(17) -0.0017(12) -0.0012(13) -0.0004(11) C10 0.0205(16) 0.0237(19) 0.0172(16) 0.0015(13) -0.0059(13) 0.0016(13) C11 0.0138(15) 0.033(2) 0.0201(17) -0.0009(14) -0.0006(13) -0.0045(13) C12 0.0210(16) 0.0162(17) 0.0231(17) 0.0012(13) -0.0059(14) -0.0036(12) C13 0.0248(16) 0.0095(15) 0.0129(15) 0.0005(11) -0.0002(12) -0.0025(12) C14 0.0354(19) 0.0120(17) 0.0176(16) 0.0015(13) 0.0035(15) 0.0041(13) C15 0.0290(17) 0.0152(17) 0.0175(16) 0.0030(13) 0.0000(14) 0.0003(13) C16 0.0283(17) 0.0182(17) 0.0188(17) 0.0012(13) -0.0010(14) -0.0117(13) C17 0.0099(13) 0.0198(16) 0.0106(14) -0.0026(12) -0.0050(11) 0.0011(11) C18 0.0131(14) 0.0208(17) 0.0202(16) -0.0032(14) -0.0006(13) -0.0027(12) C19 0.0167(15) 0.0304(19) 0.0139(15) -0.0002(13) -0.0049(13) 0.0018(13) C20 0.0144(15) 0.0281(19) 0.0187(17) -0.0103(14) -0.0013(13) -0.0034(12) C21 0.0113(13) 0.0151(15) 0.0130(14) 0.0058(12) 0.0009(12) 0.0000(11) C22 0.0185(15) 0.0188(17) 0.0216(17) 0.0106(14) -0.0011(13) 0.0014(12) C23 0.0206(16) 0.0248(19) 0.0168(16) 0.0031(13) 0.0052(13) -0.0028(13) C24 0.0117(14) 0.0181(17) 0.0237(17) 0.0045(13) -0.0029(13) -0.0024(12) O1 0.0209(10) 0.0170(11) 0.0102(10) -0.0024(8) 0.0063(9) 0.0043(8) S1 0.0184(4) 0.0158(4) 0.0122(4) -0.0005(3) 0.0023(3) 0.0013(3) O2 0.0295(12) 0.0357(14) 0.0185(12) -0.0010(10) -0.0040(10) 0.0194(10) O3 0.0382(14) 0.0299(14) 0.0271(13) -0.0051(10) 0.0109(11) -0.0166(10) C25 0.0154(14) 0.0188(17) 0.0159(15) -0.0055(12) 0.0004(12) 0.0001(12) F1 0.0355(11) 0.0274(11) 0.0196(9) -0.0100(8) 0.0031(8) 0.0050(8) F2 0.0298(10) 0.0395(12) 0.0195(10) -0.0008(9) 0.0092(8) -0.0132(9) F3 0.0246(9) 0.0478(13) 0.0152(9) 0.0000(8) -0.0056(8) 0.0137(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 1.967(3) . ? Pt1 O1 2.2835(18) . ? Pt1 P2 2.3219(8) . ? Pt1 P1 2.3319(8) . ? P1 C9 1.873(3) . ? P1 C13 1.876(3) . ? P1 C7 1.879(3) . ? P2 C17 1.873(3) . ? P2 C8 1.877(3) . ? P2 C21 1.878(3) . ? B1 N1 1.417(4) . ? B1 N2 1.425(4) . ? N1 C1 1.397(3) . ? N1 C7 1.447(3) . ? C1 C2 1.383(4) . ? C1 C6 1.420(4) . ? C2 C3 1.395(4) . ? C3 C4 1.384(4) . ? C4 C5 1.396(4) . ? C5 C6 1.383(4) . ? C6 N2 1.401(3) . ? N2 C8 1.445(3) . ? C9 C11 1.525(4) . ? C9 C10 1.544(4) . ? C9 C12 1.545(4) . ? C13 C16 1.534(4) . ? C13 C14 1.535(4) . ? C13 C15 1.536(4) . ? C17 C19 1.530(4) . ? C17 C18 1.536(4) . ? C17 C20 1.538(4) . ? C21 C24 1.536(4) . ? C21 C23 1.538(4) . ? C21 C22 1.541(4) . ? O1 S1 1.464(2) . ? S1 O3 1.430(2) . ? S1 O2 1.437(2) . ? S1 C25 1.825(3) . ? C25 F3 1.330(3) . ? C25 F1 1.335(3) . ? C25 F2 1.339(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 O1 172.47(10) . . ? B1 Pt1 P2 79.01(10) . . ? O1 Pt1 P2 93.85(5) . . ? B1 Pt1 P1 79.48(10) . . ? O1 Pt1 P1 107.52(5) . . ? P2 Pt1 P1 158.36(2) . . ? C9 P1 C13 113.19(13) . . ? C9 P1 C7 104.51(13) . . ? C13 P1 C7 101.93(12) . . ? C9 P1 Pt1 110.05(10) . . ? C13 P1 Pt1 120.06(9) . . ? C7 P1 Pt1 105.19(9) . . ? C17 P2 C8 103.63(12) . . ? C17 P2 C21 114.65(12) . . ? C8 P2 C21 104.17(12) . . ? C17 P2 Pt1 111.75(9) . . ? C8 P2 Pt1 106.40(9) . . ? C21 P2 Pt1 114.89(9) . . ? N1 B1 N2 106.5(2) . . ? N1 B1 Pt1 126.7(2) . . ? N2 B1 Pt1 126.8(2) . . ? C1 N1 B1 108.8(2) . . ? C1 N1 C7 130.0(2) . . ? B1 N1 C7 121.0(2) . . ? C2 C1 N1 131.0(3) . . ? C2 C1 C6 120.8(2) . . ? N1 C1 C6 108.3(2) . . ? C1 C2 C3 117.9(3) . . ? C4 C3 C2 121.5(2) . . ? C3 C4 C5 121.1(3) . . ? C6 C5 C4 118.2(3) . . ? C5 C6 N2 132.0(3) . . ? C5 C6 C1 120.6(2) . . ? N2 C6 C1 107.4(2) . . ? C6 N2 B1 108.9(2) . . ? C6 N2 C8 129.5(2) . . ? B1 N2 C8 121.3(2) . . ? N1 C7 P1 105.48(18) . . ? N2 C8 P2 104.42(17) . . ? C11 C9 C10 109.8(2) . . ? C11 C9 C12 108.7(2) . . ? C10 C9 C12 108.4(2) . . ? C11 C9 P1 109.4(2) . . ? C10 C9 P1 114.2(2) . . ? C12 C9 P1 106.17(18) . . ? C16 C13 C14 109.1(2) . . ? C16 C13 C15 109.5(2) . . ? C14 C13 C15 108.1(2) . . ? C16 C13 P1 104.70(19) . . ? C14 C13 P1 111.29(19) . . ? C15 C13 P1 114.0(2) . . ? C19 C17 C18 110.1(2) . . ? C19 C17 C20 109.7(2) . . ? C18 C17 C20 107.4(2) . . ? C19 C17 P2 113.9(2) . . ? C18 C17 P2 106.06(18) . . ? C20 C17 P2 109.39(19) . . ? C24 C21 C23 108.4(2) . . ? C24 C21 C22 109.4(2) . . ? C23 C21 C22 109.8(2) . . ? C24 C21 P2 105.20(18) . . ? C23 C21 P2 111.15(19) . . ? C22 C21 P2 112.74(19) . . ? S1 O1 Pt1 134.09(11) . . ? O3 S1 O2 117.27(15) . . ? O3 S1 O1 114.23(13) . . ? O2 S1 O1 113.94(13) . . ? O3 S1 C25 103.55(13) . . ? O2 S1 C25 103.35(13) . . ? O1 S1 C25 101.81(12) . . ? F3 C25 F1 107.8(2) . . ? F3 C25 F2 107.1(2) . . ? F1 C25 F2 107.7(2) . . ? F3 C25 S1 112.02(19) . . ? F1 C25 S1 110.5(2) . . ? F2 C25 S1 111.6(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.151 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.089 data_4 _database_code_depnum_ccdc_archive 'CCDC 891985' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H50 B F6 N3 O4 P2 Pt S2' _chemical_formula_weight 986.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 12.497(2) _cell_length_b 22.313(4) _cell_length_c 14.664(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.678(2) _cell_angle_gamma 90.00 _cell_volume 4030.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 113.1500 _cell_measurement_reflns_used 11248 _cell_measurement_theta_min 1.6531 _cell_measurement_theta_max 27.4774 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 3.730 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3169 _exptl_absorpt_correction_T_max 0.6046 _exptl_absorpt_process_details '(NUMABS; Rigaku, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSC Meacury CCD' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 25111 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6974 _reflns_number_gt 6248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+2.0078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6974 _refine_ls_number_parameters 522 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.823899(12) 0.124432(7) 0.806395(10) 0.01577(8) Uani 1 1 d . . . B1 B 0.7810(4) 0.2082(2) 0.8189(3) 0.0207(11) Uani 1 1 d . . . N1 N 0.8432(3) 0.25958(17) 0.8047(2) 0.0199(8) Uani 1 1 d . . . C1 C 0.7856(3) 0.31098(19) 0.8238(3) 0.0182(9) Uani 1 1 d . . . C2 C 0.8113(4) 0.3707(2) 0.8211(3) 0.0262(11) Uani 1 1 d . . . H1 H 0.8780 0.3834 0.8046 0.047(17) Uiso 1 1 calc R . . C3 C 0.7357(4) 0.4119(2) 0.8434(3) 0.0315(11) Uani 1 1 d . . . H2 H 0.7510 0.4535 0.8414 0.036(14) Uiso 1 1 calc R . . C4 C 0.6384(4) 0.3932(2) 0.8686(3) 0.0330(12) Uani 1 1 d . . . H3 H 0.5889 0.4223 0.8840 0.026(12) Uiso 1 1 calc R . . C5 C 0.6126(4) 0.3331(2) 0.8716(3) 0.0258(10) Uani 1 1 d . . . H4 H 0.5459 0.3206 0.8885 0.037(14) Uiso 1 1 calc R . . C6 C 0.6869(3) 0.2913(2) 0.8493(3) 0.0212(9) Uani 1 1 d . . . N2 N 0.6841(3) 0.22906(16) 0.8470(2) 0.0212(8) Uani 1 1 d . . . P1 P 0.96482(8) 0.17320(5) 0.75158(7) 0.0166(2) Uani 1 1 d . . . P2 P 0.66086(9) 0.11132(5) 0.86023(8) 0.0208(3) Uani 1 1 d . . . C7 C 0.9477(4) 0.2550(2) 0.7755(3) 0.0264(11) Uani 1 1 d . . . H5 H 1.0062 0.2692 0.8249 0.049(16) Uiso 1 1 calc R . . H6 H 0.9492 0.2792 0.7191 0.030(13) Uiso 1 1 calc R . . C8 C 0.9454(4) 0.1674(2) 0.6222(3) 0.0229(10) Uani 1 1 d . . . C9 C 0.8358(4) 0.1973(3) 0.5864(3) 0.0421(14) Uani 1 1 d . . . H7 H 0.8180 0.1923 0.5192 0.067(19) Uiso 1 1 calc R . . H8 H 0.8402 0.2401 0.6016 0.08(2) Uiso 1 1 calc R . . H9 H 0.7792 0.1785 0.6156 0.08(2) Uiso 1 1 calc R . . C10 C 0.9361(5) 0.1014(3) 0.5938(3) 0.0398(14) Uani 1 1 d . . . H10 H 0.9163 0.0985 0.5264 0.051(16) Uiso 1 1 calc R . . H11 H 0.8801 0.0820 0.6230 0.040(15) Uiso 1 1 calc R . . H12 H 1.0059 0.0814 0.6139 0.035(14) Uiso 1 1 calc R . . C11 C 1.0340(4) 0.1987(3) 0.5795(3) 0.0382(13) Uani 1 1 d . . . H13 H 1.1040 0.1793 0.6013 0.045(16) Uiso 1 1 calc R . . H14 H 1.0380 0.2409 0.5979 0.032(13) Uiso 1 1 calc R . . H15 H 1.0167 0.1958 0.5120 0.055(17) Uiso 1 1 calc R . . C12 C 1.1057(4) 0.1574(2) 0.8113(3) 0.0267(11) Uani 1 1 d . . . C13 C 1.0989(5) 0.1576(4) 0.9147(4) 0.058(2) Uani 1 1 d . . . H16 H 1.0433 0.1291 0.9267 0.11(3) Uiso 1 1 calc R . . H17 H 1.0798 0.1979 0.9332 0.05(2) Uiso 1 1 calc R . . H18 H 1.1693 0.1461 0.9504 0.067(19) Uiso 1 1 calc R . . C14 C 1.1413(4) 0.0949(3) 0.7852(5) 0.0490(16) Uani 1 1 d . . . H19 H 1.1540 0.0953 0.7210 0.13(3) Uiso 1 1 calc R . . H20 H 1.0842 0.0658 0.7914 0.12(3) Uiso 1 1 calc R . . H21 H 1.2084 0.0837 0.8264 0.065(19) Uiso 1 1 calc R . . C15 C 1.1912(4) 0.2029(2) 0.7932(3) 0.0333(12) Uani 1 1 d . . . H22 H 1.2582 0.1966 0.8374 0.041(15) Uiso 1 1 calc R . . H23 H 1.1642 0.2436 0.8005 0.07(2) Uiso 1 1 calc R . . H24 H 1.2059 0.1978 0.7301 0.035(13) Uiso 1 1 calc R . . C16 C 0.5971(4) 0.1881(2) 0.8567(3) 0.0279(11) Uani 1 1 d . . . H25 H 0.5371 0.1917 0.8035 0.050(17) Uiso 1 1 calc R . . H26 H 0.5684 0.1963 0.9144 0.032(13) Uiso 1 1 calc R . . C17 C 0.6833(4) 0.0905(2) 0.9864(3) 0.0292(11) Uani 1 1 d . . . C18 C 0.5775(4) 0.0834(3) 1.0251(4) 0.0418(14) Uani 1 1 d . . . H27 H 0.5376 0.0485 0.9966 0.051(16) Uiso 1 1 calc R . . H28 H 0.5330 0.1194 1.0113 0.036(16) Uiso 1 1 calc R . . H29 H 0.5943 0.0776 1.0923 0.044(15) Uiso 1 1 calc R . . C19 C 0.7508(4) 0.0335(2) 1.0024(3) 0.0367(13) Uani 1 1 d . . . H30 H 0.8157 0.0376 0.9736 0.045(15) Uiso 1 1 calc R . . H31 H 0.7076 -0.0006 0.9750 0.034(14) Uiso 1 1 calc R . . H32 H 0.7725 0.0269 1.0690 0.048(15) Uiso 1 1 calc R . . C20 C 0.7491(4) 0.1425(2) 1.0379(3) 0.0299(11) Uani 1 1 d . . . H33 H 0.7647 0.1335 1.1042 0.029(13) Uiso 1 1 calc R . . H34 H 0.7070 0.1796 1.0278 0.033(14) Uiso 1 1 calc R . . H35 H 0.8175 0.1472 1.0143 0.046(15) Uiso 1 1 calc R . . C21 C 0.5555(3) 0.0636(2) 0.7870(3) 0.0279(11) Uani 1 1 d . . . C22 C 0.4389(4) 0.0783(3) 0.7999(4) 0.0451(15) Uani 1 1 d . . . H36 H 0.3879 0.0530 0.7588 0.044(15) Uiso 1 1 calc R . . H37 H 0.4235 0.1206 0.7848 0.039(17) Uiso 1 1 calc R . . H38 H 0.4310 0.0709 0.8643 0.033(14) Uiso 1 1 calc R . . C23 C 0.5781(4) -0.0024(2) 0.8058(3) 0.0327(12) Uani 1 1 d . . . H39 H 0.5298 -0.0264 0.7604 0.054(17) Uiso 1 1 calc R . . H40 H 0.5655 -0.0122 0.8682 0.054(17) Uiso 1 1 calc R . . H41 H 0.6538 -0.0111 0.8008 0.043(15) Uiso 1 1 calc R . . C24 C 0.5671(4) 0.0776(3) 0.6862(3) 0.0363(12) Uani 1 1 d . . . H42 H 0.6408 0.0677 0.6767 0.055(17) Uiso 1 1 calc R . . H43 H 0.5532 0.1203 0.6738 0.10(3) Uiso 1 1 calc R . . H44 H 0.5146 0.0537 0.6441 0.055(17) Uiso 1 1 calc R . . O1 O 0.8865(3) 0.02732(14) 0.8061(2) 0.0293(7) Uani 1 1 d . . . S1 S 0.90037(9) -0.02875(5) 0.76029(8) 0.0261(3) Uani 1 1 d . . . O2 O 0.9962(3) -0.03621(16) 0.7212(3) 0.0421(9) Uani 1 1 d . . . N3 N 0.7892(3) -0.04490(18) 0.6998(3) 0.0302(9) Uani 1 1 d . . . S2 S 0.76960(11) -0.09705(6) 0.62522(8) 0.0349(3) Uani 1 1 d . . . O3 O 0.6626(4) -0.11936(19) 0.6232(3) 0.0600(13) Uani 1 1 d . . . O4 O 0.8570(4) -0.13748(17) 0.6241(3) 0.0523(11) Uani 1 1 d . . . C25 C 0.9145(4) -0.0810(2) 0.8570(3) 0.0358(12) Uani 1 1 d . . . F1 F 0.8245(2) -0.08255(13) 0.89456(18) 0.0415(7) Uani 1 1 d . . . F2 F 0.9340(3) -0.13623(14) 0.8317(2) 0.0544(9) Uani 1 1 d . . . F3 F 0.9962(3) -0.06394(17) 0.9224(2) 0.0680(10) Uani 1 1 d . . . C26 C 0.7602(5) -0.0539(3) 0.5182(3) 0.0405(13) Uani 1 1 d . . . F4 F 0.6847(3) -0.01300(17) 0.5116(2) 0.0668(11) Uani 1 1 d . . . F5 F 0.7363(3) -0.09125(16) 0.44603(19) 0.0552(9) Uani 1 1 d . . . F6 F 0.8536(3) -0.02798(15) 0.5123(2) 0.0577(10) Uani 1 1 d . . . C27 C 0.5174(4) 0.2423(3) 0.5841(4) 0.0393(13) Uani 1 1 d . . . H45 H 0.5845 0.2270 0.5720 0.034(13) Uiso 1 1 calc R . . C28 C 0.5165(5) 0.2877(3) 0.6461(3) 0.0458(15) Uani 1 1 d . . . H46 H 0.5831 0.3041 0.6767 0.066(19) Uiso 1 1 calc R . . C29 C 0.4201(5) 0.3100(3) 0.6644(4) 0.0491(16) Uani 1 1 d . . . H47 H 0.4196 0.3413 0.7083 0.08(2) Uiso 1 1 calc R . . C30 C 0.3240(5) 0.2865(3) 0.6185(4) 0.0434(14) Uani 1 1 d . . . H48 H 0.2567 0.3018 0.6301 0.065(19) Uiso 1 1 calc R . . C31 C 0.3258(4) 0.2409(3) 0.5560(4) 0.0455(15) Uani 1 1 d . . . H49 H 0.2597 0.2246 0.5242 0.049(17) Uiso 1 1 calc R . . C32 C 0.4225(4) 0.2190(3) 0.5397(4) 0.0444(14) Uani 1 1 d . . . H50 H 0.4236 0.1871 0.4969 0.10(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01366(12) 0.01320(12) 0.02162(11) 0.00127(6) 0.00636(8) -0.00018(6) B1 0.022(3) 0.014(3) 0.026(2) 0.001(2) 0.005(2) 0.004(2) N1 0.0212(19) 0.013(2) 0.0276(19) 0.0010(14) 0.0092(16) -0.0006(15) C1 0.023(2) 0.017(2) 0.0146(19) -0.0005(16) 0.0037(17) 0.0009(18) C2 0.036(3) 0.019(3) 0.024(2) -0.0012(17) 0.007(2) -0.004(2) C3 0.045(3) 0.016(3) 0.033(2) -0.001(2) 0.004(2) 0.003(2) C4 0.040(3) 0.022(3) 0.034(3) -0.001(2) 0.001(2) 0.010(2) C5 0.028(3) 0.021(3) 0.029(2) -0.0012(19) 0.005(2) 0.005(2) C6 0.021(2) 0.022(3) 0.019(2) -0.0028(17) 0.0008(18) 0.0045(19) N2 0.0184(19) 0.014(2) 0.0325(19) 0.0008(15) 0.0078(16) 0.0022(15) P1 0.0141(5) 0.0167(6) 0.0203(5) 0.0013(4) 0.0065(4) -0.0007(4) P2 0.0160(6) 0.0181(6) 0.0305(6) -0.0014(5) 0.0108(5) -0.0034(5) C7 0.028(3) 0.023(3) 0.031(2) -0.004(2) 0.015(2) -0.009(2) C8 0.023(2) 0.025(3) 0.021(2) 0.0029(18) 0.0032(18) 0.000(2) C9 0.038(3) 0.056(4) 0.029(3) 0.009(2) -0.002(2) 0.010(3) C10 0.063(4) 0.031(3) 0.027(3) -0.006(2) 0.012(3) -0.002(3) C11 0.048(4) 0.039(4) 0.031(3) 0.001(2) 0.018(2) -0.012(3) C12 0.019(2) 0.030(3) 0.031(2) 0.006(2) 0.0034(19) -0.004(2) C13 0.032(3) 0.110(7) 0.028(3) 0.017(3) -0.005(2) -0.011(4) C14 0.019(3) 0.035(4) 0.090(5) 0.015(3) -0.002(3) 0.010(3) C15 0.016(2) 0.039(3) 0.044(3) 0.005(2) 0.004(2) -0.005(2) C16 0.022(2) 0.023(3) 0.042(3) -0.004(2) 0.014(2) 0.000(2) C17 0.040(3) 0.021(3) 0.031(2) -0.002(2) 0.018(2) -0.008(2) C18 0.052(4) 0.034(3) 0.047(3) -0.005(3) 0.030(3) -0.017(3) C19 0.058(4) 0.019(3) 0.035(3) 0.005(2) 0.014(3) -0.004(2) C20 0.038(3) 0.024(3) 0.028(2) -0.004(2) 0.007(2) -0.003(2) C21 0.016(2) 0.026(3) 0.043(3) -0.006(2) 0.008(2) -0.0037(19) C22 0.020(3) 0.042(4) 0.076(4) -0.024(3) 0.014(3) -0.006(2) C23 0.027(3) 0.031(3) 0.043(3) -0.009(2) 0.015(2) -0.008(2) C24 0.029(3) 0.046(4) 0.032(3) -0.004(2) -0.001(2) -0.001(2) O1 0.0330(19) 0.0122(18) 0.0437(18) 0.0010(14) 0.0096(15) 0.0028(14) S1 0.0256(6) 0.0158(6) 0.0382(6) 0.0008(5) 0.0092(5) 0.0053(5) O2 0.033(2) 0.028(2) 0.071(3) -0.0021(18) 0.0261(19) 0.0051(16) N3 0.031(2) 0.029(3) 0.032(2) -0.0014(17) 0.0068(18) 0.0047(18) S2 0.0487(8) 0.0249(7) 0.0325(6) -0.0016(5) 0.0109(6) -0.0054(6) O3 0.067(3) 0.069(3) 0.048(2) -0.0097(19) 0.018(2) -0.039(2) O4 0.081(3) 0.024(2) 0.051(2) -0.0044(17) 0.007(2) 0.019(2) C25 0.034(3) 0.025(3) 0.044(3) 0.004(2) -0.006(2) 0.007(2) F1 0.056(2) 0.0303(18) 0.0393(16) 0.0121(13) 0.0120(15) 0.0064(15) F2 0.078(3) 0.0213(18) 0.066(2) 0.0111(15) 0.019(2) 0.0219(17) F3 0.064(2) 0.055(3) 0.070(2) 0.0161(18) -0.0314(19) -0.0024(19) C26 0.052(4) 0.038(3) 0.033(3) -0.004(2) 0.012(3) 0.002(3) F4 0.090(3) 0.060(3) 0.0487(19) 0.0047(17) 0.0057(19) 0.036(2) F5 0.083(3) 0.050(2) 0.0325(16) -0.0089(15) 0.0074(16) -0.0079(19) F6 0.081(3) 0.050(2) 0.0479(18) -0.0011(15) 0.0273(18) -0.0207(19) C27 0.031(3) 0.042(4) 0.048(3) 0.015(3) 0.014(3) 0.004(3) C28 0.039(3) 0.067(5) 0.028(3) 0.006(3) -0.002(2) -0.024(3) C29 0.081(5) 0.031(3) 0.040(3) -0.009(2) 0.023(3) -0.016(3) C30 0.042(3) 0.034(3) 0.058(3) 0.008(3) 0.022(3) 0.006(3) C31 0.031(3) 0.054(4) 0.052(3) 0.000(3) 0.011(3) -0.010(3) C32 0.043(3) 0.037(4) 0.058(3) -0.012(3) 0.022(3) -0.012(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 1.961(5) . ? Pt1 O1 2.304(3) . ? Pt1 P2 2.3240(11) . ? Pt1 P1 2.3254(10) . ? B1 N1 1.420(6) . ? B1 N2 1.422(6) . ? N1 C1 1.407(5) . ? N1 C7 1.445(5) . ? C1 C2 1.372(6) . ? C1 C6 1.417(6) . ? C2 C3 1.397(7) . ? C3 C4 1.393(7) . ? C4 C5 1.381(7) . ? C5 C6 1.395(6) . ? C6 N2 1.388(6) . ? N2 C16 1.445(5) . ? P1 C12 1.863(5) . ? P1 C8 1.876(4) . ? P1 C7 1.878(5) . ? P2 C17 1.882(5) . ? P2 C21 1.883(5) . ? P2 C16 1.887(5) . ? C8 C11 1.529(6) . ? C8 C10 1.529(7) . ? C8 C9 1.535(7) . ? C12 C15 1.529(6) . ? C12 C14 1.531(7) . ? C12 C13 1.533(6) . ? C17 C19 1.523(7) . ? C17 C18 1.532(6) . ? C17 C20 1.543(7) . ? C21 C23 1.515(7) . ? C21 C22 1.535(6) . ? C21 C24 1.542(6) . ? O1 S1 1.444(3) . ? S1 O2 1.422(3) . ? S1 N3 1.559(4) . ? S1 C25 1.821(5) . ? N3 S2 1.588(4) . ? S2 O4 1.419(4) . ? S2 O3 1.423(4) . ? S2 C26 1.828(5) . ? C25 F2 1.322(6) . ? C25 F1 1.333(6) . ? C25 F3 1.334(6) . ? C26 F4 1.305(6) . ? C26 F6 1.319(6) . ? C26 F5 1.341(6) . ? C27 C32 1.357(8) . ? C27 C28 1.362(8) . ? C28 C29 1.371(8) . ? C29 C30 1.378(8) . ? C30 C31 1.373(7) . ? C31 C32 1.361(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 O1 174.02(17) . . ? B1 Pt1 P2 79.57(14) . . ? O1 Pt1 P2 101.52(8) . . ? B1 Pt1 P1 79.71(14) . . ? O1 Pt1 P1 99.34(8) . . ? P2 Pt1 P1 159.14(4) . . ? N1 B1 N2 107.0(4) . . ? N1 B1 Pt1 126.2(3) . . ? N2 B1 Pt1 126.8(3) . . ? C1 N1 B1 108.5(3) . . ? C1 N1 C7 129.4(4) . . ? B1 N1 C7 122.1(4) . . ? C2 C1 N1 130.9(4) . . ? C2 C1 C6 121.8(4) . . ? N1 C1 C6 107.2(4) . . ? C1 C2 C3 117.5(5) . . ? C4 C3 C2 121.3(5) . . ? C5 C4 C3 121.3(5) . . ? C4 C5 C6 118.3(5) . . ? N2 C6 C5 131.3(4) . . ? N2 C6 C1 108.9(3) . . ? C5 C6 C1 119.8(4) . . ? C6 N2 B1 108.3(3) . . ? C6 N2 C16 130.2(3) . . ? B1 N2 C16 120.9(4) . . ? C12 P1 C8 114.43(19) . . ? C12 P1 C7 102.9(2) . . ? C8 P1 C7 104.9(2) . . ? C12 P1 Pt1 117.36(14) . . ? C8 P1 Pt1 109.91(14) . . ? C7 P1 Pt1 105.89(13) . . ? C17 P2 C21 113.3(2) . . ? C17 P2 C16 104.1(2) . . ? C21 P2 C16 104.3(2) . . ? C17 P2 Pt1 111.77(16) . . ? C21 P2 Pt1 116.52(14) . . ? C16 P2 Pt1 105.45(13) . . ? N1 C7 P1 105.1(3) . . ? C11 C8 C10 110.8(4) . . ? C11 C8 C9 109.1(4) . . ? C10 C8 C9 107.6(4) . . ? C11 C8 P1 113.8(3) . . ? C10 C8 P1 109.4(3) . . ? C9 C8 P1 105.8(3) . . ? C15 C12 C14 108.7(4) . . ? C15 C12 C13 109.0(4) . . ? C14 C12 C13 108.5(5) . . ? C15 C12 P1 115.2(3) . . ? C14 C12 P1 110.2(3) . . ? C13 C12 P1 105.0(3) . . ? N2 C16 P2 104.8(3) . . ? C19 C17 C18 110.2(4) . . ? C19 C17 C20 108.4(4) . . ? C18 C17 C20 108.6(4) . . ? C19 C17 P2 110.2(3) . . ? C18 C17 P2 113.3(4) . . ? C20 C17 P2 105.9(3) . . ? C23 C21 C22 109.8(4) . . ? C23 C21 C24 109.0(4) . . ? C22 C21 C24 108.6(4) . . ? C23 C21 P2 110.8(3) . . ? C22 C21 P2 113.3(3) . . ? C24 C21 P2 105.2(3) . . ? S1 O1 Pt1 152.0(2) . . ? O2 S1 O1 117.6(2) . . ? O2 S1 N3 118.3(2) . . ? O1 S1 N3 107.4(2) . . ? O2 S1 C25 105.1(2) . . ? O1 S1 C25 101.3(2) . . ? N3 S1 C25 104.8(2) . . ? S1 N3 S2 125.5(3) . . ? O4 S2 O3 120.0(3) . . ? O4 S2 N3 116.3(2) . . ? O3 S2 N3 107.8(2) . . ? O4 S2 C26 105.3(2) . . ? O3 S2 C26 104.0(3) . . ? N3 S2 C26 100.7(2) . . ? F2 C25 F1 107.5(4) . . ? F2 C25 F3 108.3(4) . . ? F1 C25 F3 107.9(4) . . ? F2 C25 S1 112.1(4) . . ? F1 C25 S1 111.1(3) . . ? F3 C25 S1 109.9(4) . . ? F4 C26 F6 109.0(5) . . ? F4 C26 F5 108.3(5) . . ? F6 C26 F5 107.6(4) . . ? F4 C26 S2 111.9(3) . . ? F6 C26 S2 111.0(4) . . ? F5 C26 S2 108.9(4) . . ? C32 C27 C28 120.1(5) . . ? C27 C28 C29 120.4(5) . . ? C28 C29 C30 119.2(5) . . ? C31 C30 C29 119.9(5) . . ? C32 C31 C30 119.9(6) . . ? C27 C32 C31 120.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 B1 N1 175.4(4) . . . . ? P1 Pt1 B1 N1 -7.0(4) . . . . ? P2 Pt1 B1 N2 -2.1(4) . . . . ? P1 Pt1 B1 N2 175.5(4) . . . . ? N2 B1 N1 C1 0.1(5) . . . . ? Pt1 B1 N1 C1 -177.8(3) . . . . ? N2 B1 N1 C7 179.9(4) . . . . ? Pt1 B1 N1 C7 2.0(6) . . . . ? B1 N1 C1 C2 179.4(5) . . . . ? C7 N1 C1 C2 -0.3(7) . . . . ? B1 N1 C1 C6 -0.5(5) . . . . ? C7 N1 C1 C6 179.7(4) . . . . ? N1 C1 C2 C3 179.4(4) . . . . ? C6 C1 C2 C3 -0.7(7) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 0.4(7) . . . . ? C4 C5 C6 N2 179.3(4) . . . . ? C4 C5 C6 C1 -0.3(6) . . . . ? C2 C1 C6 N2 -179.2(4) . . . . ? N1 C1 C6 N2 0.8(5) . . . . ? C2 C1 C6 C5 0.5(6) . . . . ? N1 C1 C6 C5 -179.5(4) . . . . ? C5 C6 N2 B1 179.6(5) . . . . ? C1 C6 N2 B1 -0.7(5) . . . . ? C5 C6 N2 C16 8.3(8) . . . . ? C1 C6 N2 C16 -172.0(4) . . . . ? N1 B1 N2 C6 0.4(5) . . . . ? Pt1 B1 N2 C6 178.3(3) . . . . ? N1 B1 N2 C16 172.7(4) . . . . ? Pt1 B1 N2 C16 -9.4(6) . . . . ? B1 Pt1 P1 C12 122.5(2) . . . . ? O1 Pt1 P1 C12 -51.48(19) . . . . ? P2 Pt1 P1 C12 129.2(2) . . . . ? B1 Pt1 P1 C8 -104.4(2) . . . . ? O1 Pt1 P1 C8 81.57(18) . . . . ? P2 Pt1 P1 C8 -97.71(19) . . . . ? B1 Pt1 P1 C7 8.4(2) . . . . ? O1 Pt1 P1 C7 -165.65(18) . . . . ? P2 Pt1 P1 C7 15.1(2) . . . . ? B1 Pt1 P2 C17 -103.2(2) . . . . ? O1 Pt1 P2 C17 70.85(19) . . . . ? P1 Pt1 P2 C17 -109.88(19) . . . . ? B1 Pt1 P2 C21 124.4(2) . . . . ? O1 Pt1 P2 C21 -61.6(2) . . . . ? P1 Pt1 P2 C21 117.7(2) . . . . ? B1 Pt1 P2 C16 9.3(2) . . . . ? O1 Pt1 P2 C16 -176.68(18) . . . . ? P1 Pt1 P2 C16 2.6(2) . . . . ? C1 N1 C7 P1 -174.2(3) . . . . ? B1 N1 C7 P1 6.0(5) . . . . ? C12 P1 C7 N1 -133.3(3) . . . . ? C8 P1 C7 N1 106.6(3) . . . . ? Pt1 P1 C7 N1 -9.6(3) . . . . ? C12 P1 C8 C11 -45.9(4) . . . . ? C7 P1 C8 C11 66.1(4) . . . . ? Pt1 P1 C8 C11 179.6(3) . . . . ? C12 P1 C8 C10 78.6(4) . . . . ? C7 P1 C8 C10 -169.3(3) . . . . ? Pt1 P1 C8 C10 -55.9(3) . . . . ? C12 P1 C8 C9 -165.7(3) . . . . ? C7 P1 C8 C9 -53.7(4) . . . . ? Pt1 P1 C8 C9 59.8(4) . . . . ? C8 P1 C12 C15 66.4(4) . . . . ? C7 P1 C12 C15 -46.8(4) . . . . ? Pt1 P1 C12 C15 -162.6(3) . . . . ? C8 P1 C12 C14 -57.0(4) . . . . ? C7 P1 C12 C14 -170.2(3) . . . . ? Pt1 P1 C12 C14 74.0(4) . . . . ? C8 P1 C12 C13 -173.7(4) . . . . ? C7 P1 C12 C13 73.1(4) . . . . ? Pt1 P1 C12 C13 -42.7(4) . . . . ? C6 N2 C16 P2 -173.4(4) . . . . ? B1 N2 C16 P2 16.2(5) . . . . ? C17 P2 C16 N2 102.3(3) . . . . ? C21 P2 C16 N2 -138.7(3) . . . . ? Pt1 P2 C16 N2 -15.5(3) . . . . ? C21 P2 C17 C19 76.3(4) . . . . ? C16 P2 C17 C19 -171.1(3) . . . . ? Pt1 P2 C17 C19 -57.8(4) . . . . ? C21 P2 C17 C18 -47.7(4) . . . . ? C16 P2 C17 C18 64.9(4) . . . . ? Pt1 P2 C17 C18 178.2(3) . . . . ? C21 P2 C17 C20 -166.7(3) . . . . ? C16 P2 C17 C20 -54.0(4) . . . . ? Pt1 P2 C17 C20 59.3(3) . . . . ? C17 P2 C21 C23 -50.1(4) . . . . ? C16 P2 C21 C23 -162.7(3) . . . . ? Pt1 P2 C21 C23 81.6(3) . . . . ? C17 P2 C21 C22 73.7(4) . . . . ? C16 P2 C21 C22 -38.8(4) . . . . ? Pt1 P2 C21 C22 -154.5(3) . . . . ? C17 P2 C21 C24 -167.8(3) . . . . ? C16 P2 C21 C24 79.6(3) . . . . ? Pt1 P2 C21 C24 -36.1(4) . . . . ? P2 Pt1 O1 S1 96.6(4) . . . . ? P1 Pt1 O1 S1 -83.1(4) . . . . ? Pt1 O1 S1 O2 91.4(5) . . . . ? Pt1 O1 S1 N3 -45.0(5) . . . . ? Pt1 O1 S1 C25 -154.7(4) . . . . ? O2 S1 N3 S2 33.8(4) . . . . ? O1 S1 N3 S2 169.9(3) . . . . ? C25 S1 N3 S2 -82.9(3) . . . . ? S1 N3 S2 O4 10.1(4) . . . . ? S1 N3 S2 O3 148.3(3) . . . . ? S1 N3 S2 C26 -103.1(3) . . . . ? O2 S1 C25 F2 -53.8(4) . . . . ? O1 S1 C25 F2 -176.7(4) . . . . ? N3 S1 C25 F2 71.6(4) . . . . ? O2 S1 C25 F1 -174.1(3) . . . . ? O1 S1 C25 F1 63.0(4) . . . . ? N3 S1 C25 F1 -48.7(4) . . . . ? O2 S1 C25 F3 66.6(4) . . . . ? O1 S1 C25 F3 -56.3(4) . . . . ? N3 S1 C25 F3 -168.0(3) . . . . ? O4 S2 C26 F4 -177.7(4) . . . . ? O3 S2 C26 F4 55.2(5) . . . . ? N3 S2 C26 F4 -56.4(5) . . . . ? O4 S2 C26 F6 -55.6(4) . . . . ? O3 S2 C26 F6 177.3(4) . . . . ? N3 S2 C26 F6 65.7(4) . . . . ? O4 S2 C26 F5 62.6(4) . . . . ? O3 S2 C26 F5 -64.4(4) . . . . ? N3 S2 C26 F5 -176.0(4) . . . . ? C32 C27 C28 C29 0.4(8) . . . . ? C27 C28 C29 C30 -0.9(8) . . . . ? C28 C29 C30 C31 0.7(8) . . . . ? C29 C30 C31 C32 0.1(9) . . . . ? C28 C27 C32 C31 0.4(8) . . . . ? C30 C31 C32 C27 -0.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.780 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.144 data_8 _database_code_depnum_ccdc_archive 'CCDC 907928' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H51 B N2 P2 Pt' _chemical_formula_weight 707.57 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' 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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 11.379(2) _cell_length_b 15.463(3) _cell_length_c 18.824(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.350(2) _cell_angle_gamma 90.00 _cell_volume 3194.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 12248 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 31.3 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 4.514 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.4655 _exptl_absorpt_correction_T_max 0.8765 _exptl_absorpt_process_details '(NUMABS; Rigaku, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU/MSCIO Saturn CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 21044 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5621 _reflns_number_gt 5084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0115P)^2^+7.4800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5621 _refine_ls_number_parameters 371 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.473459(16) 0.990839(11) 0.740419(10) 0.01583(6) Uani 1 1 d . . . H1 H 0.607(4) 0.937(3) 0.822(2) 0.016 Uiso 1 1 d . . . P1 P 0.30313(11) 0.93412(8) 0.76502(7) 0.0158(3) Uani 1 1 d . . . P2 P 0.58480(11) 1.07599(8) 0.68382(7) 0.0161(3) Uani 1 1 d . . . B1 B 0.3407(5) 1.0508(4) 0.6643(3) 0.0183(12) Uani 1 1 d . . . N1 N 0.2128(3) 1.0361(3) 0.6492(2) 0.0195(9) Uani 1 1 d . . . C1 C 0.1527(4) 1.0866(3) 0.5896(3) 0.0188(11) Uani 1 1 d . . . C2 C 0.0303(4) 1.0942(3) 0.5545(3) 0.0215(11) Uani 1 1 d . . . H2 H -0.0286 1.0608 0.5699 0.026 Uiso 1 1 calc R . . C3 C -0.0051(5) 1.1523(3) 0.4955(3) 0.0257(12) Uani 1 1 d . . . H3 H -0.0891 1.1588 0.4710 0.031 Uiso 1 1 calc R . . C4 C 0.0814(5) 1.2004(3) 0.4725(3) 0.0246(12) Uani 1 1 d . . . H4 H 0.0555 1.2399 0.4327 0.030 Uiso 1 1 calc R . . C5 C 0.2055(4) 1.1916(3) 0.5068(3) 0.0199(11) Uani 1 1 d . . . H5 H 0.2642 1.2243 0.4906 0.024 Uiso 1 1 calc R . . C6 C 0.2410(4) 1.1341(3) 0.5650(3) 0.0171(10) Uani 1 1 d . . . N2 N 0.3551(3) 1.1129(3) 0.6109(2) 0.0203(9) Uani 1 1 d . . . C7 C 0.1652(4) 0.9731(3) 0.6911(3) 0.0198(11) Uani 1 1 d . . . H6 H 0.1261 0.9245 0.6592 0.024 Uiso 1 1 calc R . . H7 H 0.1045 0.9999 0.7135 0.024 Uiso 1 1 calc R . . C8 C 0.2744(5) 0.9767(3) 0.8522(3) 0.0229(12) Uani 1 1 d . . . C9 C 0.2627(5) 1.0754(3) 0.8420(3) 0.0345(14) Uani 1 1 d . . . H8 H 0.1932 1.0886 0.8001 0.052 Uiso 1 1 calc R . . H9 H 0.3375 1.0985 0.8328 0.052 Uiso 1 1 calc R . . H10 H 0.2499 1.1017 0.8867 0.052 Uiso 1 1 calc R . . C10 C 0.3872(5) 0.9594(4) 0.9169(3) 0.0406(16) Uani 1 1 d . . . H11 H 0.3804 0.9924 0.9601 0.061 Uiso 1 1 calc R . . H12 H 0.4608 0.9773 0.9031 0.061 Uiso 1 1 calc R . . H13 H 0.3922 0.8975 0.9286 0.061 Uiso 1 1 calc R . . C11 C 0.1613(5) 0.9421(4) 0.8706(3) 0.0376(15) Uani 1 1 d . . . H14 H 0.1465 0.9749 0.9120 0.056 Uiso 1 1 calc R . . H15 H 0.1731 0.8809 0.8842 0.056 Uiso 1 1 calc R . . H16 H 0.0911 0.9481 0.8276 0.056 Uiso 1 1 calc R . . C12 C 0.2895(4) 0.8141(3) 0.7561(3) 0.0185(11) Uani 1 1 d . . . C13 C 0.3231(5) 0.7935(3) 0.6842(3) 0.0250(12) Uani 1 1 d . . . H17 H 0.4064 0.8131 0.6880 0.037 Uiso 1 1 calc R . . H18 H 0.2665 0.8231 0.6431 0.037 Uiso 1 1 calc R . . H19 H 0.3179 0.7309 0.6756 0.037 Uiso 1 1 calc R . . C14 C 0.3840(5) 0.7714(3) 0.8204(3) 0.0261(12) Uani 1 1 d . . . H20 H 0.3914 0.7099 0.8096 0.039 Uiso 1 1 calc R . . H21 H 0.3576 0.7772 0.8657 0.039 Uiso 1 1 calc R . . H22 H 0.4631 0.7997 0.8269 0.039 Uiso 1 1 calc R . . C15 C 0.1630(5) 0.7774(3) 0.7528(3) 0.0310(14) Uani 1 1 d . . . H23 H 0.1629 0.7148 0.7446 0.046 Uiso 1 1 calc R . . H24 H 0.1022 0.8048 0.7124 0.046 Uiso 1 1 calc R . . H25 H 0.1431 0.7891 0.7995 0.046 Uiso 1 1 calc R . . C16 C 0.4757(4) 1.1374(3) 0.6065(3) 0.0191(11) Uani 1 1 d . . . H26 H 0.4879 1.2006 0.6134 0.023 Uiso 1 1 calc R . . H27 H 0.4881 1.1211 0.5582 0.023 Uiso 1 1 calc R . . C17 C 0.6714(4) 1.1637(3) 0.7439(3) 0.0222(11) Uani 1 1 d . . . C18 C 0.5756(5) 1.2172(3) 0.7679(3) 0.0317(13) Uani 1 1 d . . . H28 H 0.6163 1.2607 0.8040 0.048 Uiso 1 1 calc R . . H29 H 0.5266 1.1791 0.7903 0.048 Uiso 1 1 calc R . . H30 H 0.5226 1.2461 0.7249 0.048 Uiso 1 1 calc R . . C19 C 0.7445(5) 1.2211(4) 0.7057(3) 0.0394(16) Uani 1 1 d . . . H31 H 0.6921 1.2408 0.6584 0.059 Uiso 1 1 calc R . . H32 H 0.8132 1.1882 0.6972 0.059 Uiso 1 1 calc R . . H33 H 0.7754 1.2713 0.7369 0.059 Uiso 1 1 calc R . . C20 C 0.7557(5) 1.1240(4) 0.8142(3) 0.0399(16) Uani 1 1 d . . . H34 H 0.8216 1.0919 0.8014 0.060 Uiso 1 1 calc R . . H35 H 0.7086 1.0846 0.8368 0.060 Uiso 1 1 calc R . . H36 H 0.7906 1.1702 0.8490 0.060 Uiso 1 1 calc R . . C21 C 0.6806(4) 1.0141(3) 0.6335(3) 0.0210(11) Uani 1 1 d . . . C22 C 0.7204(5) 1.0652(4) 0.5736(3) 0.0334(14) Uani 1 1 d . . . H37 H 0.7765 1.1115 0.5967 0.050 Uiso 1 1 calc R . . H38 H 0.6486 1.0905 0.5392 0.050 Uiso 1 1 calc R . . H39 H 0.7615 1.0262 0.5468 0.050 Uiso 1 1 calc R . . C23 C 0.7943(5) 0.9772(4) 0.6882(3) 0.0334(14) Uani 1 1 d . . . H40 H 0.8310 0.9327 0.6637 0.050 Uiso 1 1 calc R . . H41 H 0.7713 0.9515 0.7302 0.050 Uiso 1 1 calc R . . H42 H 0.8534 1.0237 0.7057 0.050 Uiso 1 1 calc R . . C24 C 0.5995(5) 0.9384(3) 0.5976(3) 0.0304(13) Uani 1 1 d . . . H43 H 0.6423 0.9036 0.5687 0.046 Uiso 1 1 calc R . . H44 H 0.5236 0.9608 0.5651 0.046 Uiso 1 1 calc R . . H45 H 0.5807 0.9022 0.6359 0.046 Uiso 1 1 calc R . . C25 C 0.7528(17) 0.8689(16) 0.9452(8) 0.0362(16) Uani 0.48(6) 1 d PGU A 1 H46 H 0.6852 0.8978 0.9138 0.043 Uiso 0.48(6) 1 calc PR A 1 C26 C 0.869(2) 0.9051(7) 0.9594(8) 0.0377(15) Uani 0.48(6) 1 d PGU A 1 H47 H 0.8799 0.9588 0.9376 0.045 Uiso 0.48(6) 1 calc PR A 1 C27 C 0.9675(13) 0.8627(12) 1.0055(10) 0.0386(15) Uani 0.48(6) 1 d PGU A 1 H48 H 1.0466 0.8875 1.0151 0.046 Uiso 0.48(6) 1 calc PR A 1 C28 C 0.9508(13) 0.7842(10) 1.0373(9) 0.0386(15) Uani 0.48(6) 1 d PGU A 1 H49 H 1.0185 0.7552 1.0688 0.046 Uiso 0.48(6) 1 calc PR A 1 C29 C 0.835(2) 0.7480(9) 1.0232(9) 0.0374(16) Uani 0.48(6) 1 d PGU A 1 H50 H 0.8237 0.6943 1.0449 0.045 Uiso 0.48(6) 1 calc PR A 1 C30 C 0.7361(10) 0.7903(18) 0.9771(11) 0.0356(16) Uani 0.48(6) 1 d PGU A 1 H51 H 0.6570 0.7656 0.9674 0.043 Uiso 0.48(6) 1 calc PR A 1 C31 C 0.7751(18) 0.8875(14) 0.9398(7) 0.0361(16) Uani 0.52(6) 1 d PGU A 2 H52 H 0.7210 0.9256 0.9072 0.043 Uiso 0.52(6) 1 calc PR A 2 C32 C 0.899(2) 0.9048(6) 0.9608(8) 0.0373(16) Uani 0.52(6) 1 d PGU A 2 H53 H 0.9302 0.9547 0.9425 0.045 Uiso 0.52(6) 1 calc PR A 2 C33 C 0.9785(8) 0.8491(12) 1.0085(8) 0.0386(15) Uani 0.52(6) 1 d PGU A 2 H54 H 1.0634 0.8609 1.0229 0.046 Uiso 0.52(6) 1 calc PR A 2 C34 C 0.9333(16) 0.7760(9) 1.0353(8) 0.0392(14) Uani 0.52(6) 1 d PGU A 2 H55 H 0.9873 0.7379 1.0680 0.047 Uiso 0.52(6) 1 calc PR A 2 C35 C 0.8090(19) 0.7587(10) 1.0144(10) 0.0369(14) Uani 0.52(6) 1 d PGU A 2 H56 H 0.7781 0.7087 1.0327 0.044 Uiso 0.52(6) 1 calc PR A 2 C36 C 0.7299(7) 0.8144(18) 0.9666(9) 0.0354(16) Uani 0.52(6) 1 d PGU A 2 H57 H 0.6449 0.8026 0.9523 0.043 Uiso 0.52(6) 1 calc PR A 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 0.01069(9) 0.01678(10) 0.01807(10) 0.00490(8) 0.00039(7) -0.00292(8) P1 0.0151(6) 0.0140(6) 0.0189(7) 0.0011(5) 0.0052(5) -0.0029(5) P2 0.0111(6) 0.0166(6) 0.0203(7) 0.0031(5) 0.0038(5) -0.0024(5) B1 0.021(3) 0.016(3) 0.019(3) 0.004(2) 0.008(2) 0.000(2) N1 0.012(2) 0.026(2) 0.019(2) 0.0099(18) 0.0031(17) 0.0015(17) C1 0.013(2) 0.025(3) 0.019(3) -0.001(2) 0.003(2) 0.004(2) C2 0.016(3) 0.026(3) 0.023(3) -0.001(2) 0.004(2) 0.003(2) C3 0.020(3) 0.032(3) 0.022(3) -0.006(2) 0.001(2) 0.010(2) C4 0.029(3) 0.031(3) 0.014(3) 0.002(2) 0.006(2) 0.017(2) C5 0.018(3) 0.026(3) 0.017(3) 0.000(2) 0.006(2) 0.006(2) C6 0.013(2) 0.024(3) 0.014(3) 0.001(2) 0.004(2) 0.004(2) N2 0.011(2) 0.028(2) 0.022(2) 0.0070(19) 0.0051(17) -0.0003(18) C7 0.011(2) 0.025(3) 0.022(3) 0.002(2) 0.004(2) -0.001(2) C8 0.031(3) 0.019(3) 0.020(3) -0.002(2) 0.008(2) 0.002(2) C9 0.047(4) 0.027(3) 0.035(4) -0.008(3) 0.020(3) 0.001(3) C10 0.050(4) 0.040(4) 0.027(3) -0.010(3) 0.003(3) 0.005(3) C11 0.048(4) 0.039(4) 0.036(4) -0.006(3) 0.028(3) -0.003(3) C12 0.019(3) 0.014(2) 0.026(3) 0.000(2) 0.012(2) -0.004(2) C13 0.031(3) 0.020(3) 0.024(3) -0.006(2) 0.008(2) -0.003(2) C14 0.034(3) 0.018(3) 0.030(3) 0.008(2) 0.013(3) 0.004(2) C15 0.030(3) 0.020(3) 0.049(4) -0.002(3) 0.019(3) -0.011(2) C16 0.017(3) 0.023(3) 0.017(3) 0.006(2) 0.004(2) 0.001(2) C17 0.017(3) 0.027(3) 0.022(3) -0.004(2) 0.003(2) -0.006(2) C18 0.030(3) 0.027(3) 0.040(4) -0.011(3) 0.014(3) -0.007(3) C19 0.042(4) 0.029(3) 0.053(4) -0.014(3) 0.024(3) -0.025(3) C20 0.038(4) 0.044(4) 0.030(4) -0.008(3) -0.005(3) -0.001(3) C21 0.015(2) 0.019(3) 0.030(3) -0.005(2) 0.007(2) -0.001(2) C22 0.027(3) 0.032(3) 0.048(4) 0.000(3) 0.022(3) 0.001(3) C23 0.021(3) 0.030(3) 0.048(4) -0.008(3) 0.006(3) 0.005(2) C24 0.028(3) 0.031(3) 0.035(3) -0.007(3) 0.011(3) -0.002(3) C25 0.037(2) 0.038(3) 0.034(3) -0.005(2) 0.011(2) 0.003(2) C26 0.037(2) 0.040(2) 0.036(2) -0.004(2) 0.010(2) 0.003(2) C27 0.037(2) 0.041(2) 0.037(2) -0.003(2) 0.009(2) 0.002(2) C28 0.038(2) 0.043(2) 0.036(2) -0.002(2) 0.010(2) 0.001(2) C29 0.037(3) 0.042(2) 0.034(2) -0.003(2) 0.011(2) 0.003(2) C30 0.037(2) 0.039(3) 0.033(3) -0.004(2) 0.012(2) 0.004(2) C31 0.037(2) 0.038(3) 0.034(2) -0.005(2) 0.010(2) 0.002(2) C32 0.036(3) 0.040(2) 0.037(2) -0.004(2) 0.010(2) 0.003(2) C33 0.038(2) 0.041(2) 0.037(2) -0.003(2) 0.009(2) 0.002(2) C34 0.039(2) 0.043(2) 0.036(2) -0.002(2) 0.010(2) 0.002(2) C35 0.038(2) 0.041(2) 0.033(2) -0.003(2) 0.011(2) 0.003(2) C36 0.037(2) 0.038(3) 0.033(3) -0.005(2) 0.012(2) 0.002(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 2.012(6) . ? Pt1 P2 2.2779(13) . ? Pt1 P1 2.2837(13) . ? Pt1 H1 2.03(4) . ? P1 C12 1.866(5) . ? P1 C8 1.875(5) . ? P1 C7 1.900(5) . ? P2 C17 1.871(5) . ? P2 C21 1.883(5) . ? P2 C16 1.898(5) . ? B1 N1 1.425(7) . ? B1 N2 1.430(7) . ? N1 C1 1.389(6) . ? N1 C7 1.447(6) . ? C1 C2 1.380(6) . ? C1 C6 1.417(7) . ? C2 C3 1.401(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(8) . ? C3 H3 0.9500 . ? C4 C5 1.395(7) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 N2 1.394(6) . ? N2 C16 1.448(6) . ? C7 H6 0.9900 . ? C7 H7 0.9900 . ? C8 C11 1.517(7) . ? C8 C9 1.539(7) . ? C8 C10 1.541(7) . ? C9 H8 0.9800 . ? C9 H9 0.9800 . ? C9 H10 0.9800 . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C12 C15 1.533(6) . ? C12 C13 1.535(7) . ? C12 C14 1.539(7) . ? C13 H17 0.9800 . ? C13 H18 0.9800 . ? C13 H19 0.9800 . ? C14 H20 0.9800 . ? C14 H21 0.9800 . ? C14 H22 0.9800 . ? C15 H23 0.9800 . ? C15 H24 0.9800 . ? C15 H25 0.9800 . ? C16 H26 0.9900 . ? C16 H27 0.9900 . ? C17 C19 1.521(7) . ? C17 C18 1.530(7) . ? C17 C20 1.542(7) . ? C18 H28 0.9800 . ? C18 H29 0.9800 . ? C18 H30 0.9800 . ? C19 H31 0.9800 . ? C19 H32 0.9800 . ? C19 H33 0.9800 . ? C20 H34 0.9800 . ? C20 H35 0.9800 . ? C20 H36 0.9800 . ? C21 C24 1.533(7) . ? C21 C23 1.534(7) . ? C21 C22 1.541(7) . ? C22 H37 0.9800 . ? C22 H38 0.9800 . ? C22 H39 0.9800 . ? C23 H40 0.9800 . ? C23 H41 0.9800 . ? C23 H42 0.9800 . ? C24 H43 0.9800 . ? C24 H44 0.9800 . ? C24 H45 0.9800 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 H46 0.9500 . ? C26 C27 1.3900 . ? C26 H47 0.9500 . ? C27 C28 1.3900 . ? C27 H48 0.9500 . ? C28 C29 1.3900 . ? C28 H49 0.9500 . ? C29 C30 1.3900 . ? C29 H50 0.9500 . ? C30 H51 0.9500 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 H52 0.9500 . ? C32 C33 1.3900 . ? C32 H53 0.9500 . ? C33 C34 1.3900 . ? C33 H54 0.9500 . ? C34 C35 1.3900 . ? C34 H55 0.9500 . ? C35 C36 1.3900 . ? C35 H56 0.9500 . ? C36 H57 0.9500 . ? 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 78.83(16) . . ? B1 Pt1 P1 78.69(16) . . ? P2 Pt1 P1 157.49(4) . . ? B1 Pt1 H1 176.2(12) . . ? P2 Pt1 H1 101.1(12) . . ? P1 Pt1 H1 101.3(12) . . ? C12 P1 C8 113.5(2) . . ? C12 P1 C7 102.5(2) . . ? C8 P1 C7 103.2(2) . . ? C12 P1 Pt1 114.73(16) . . ? C8 P1 Pt1 113.36(17) . . ? C7 P1 Pt1 108.09(15) . . ? C17 P2 C21 112.9(2) . . ? C17 P2 C16 103.5(2) . . ? C21 P2 C16 102.6(2) . . ? C17 P2 Pt1 113.94(17) . . ? C21 P2 Pt1 114.12(16) . . ? C16 P2 Pt1 108.42(15) . . ? N1 B1 N2 105.5(4) . . ? N1 B1 Pt1 127.1(4) . . ? N2 B1 Pt1 127.3(4) . . ? C1 N1 B1 109.3(4) . . ? C1 N1 C7 130.0(4) . . ? B1 N1 C7 120.6(4) . . ? C2 C1 N1 130.8(5) . . ? C2 C1 C6 120.9(5) . . ? N1 C1 C6 108.3(4) . . ? C1 C2 C3 118.4(5) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 121.1(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 118.4(5) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 N2 132.1(5) . . ? C5 C6 C1 120.4(4) . . ? N2 C6 C1 107.5(4) . . ? C6 N2 B1 109.4(4) . . ? C6 N2 C16 130.1(4) . . ? B1 N2 C16 120.2(4) . . ? N1 C7 P1 104.9(3) . . ? N1 C7 H6 110.8 . . ? P1 C7 H6 110.8 . . ? N1 C7 H7 110.8 . . ? P1 C7 H7 110.8 . . ? H6 C7 H7 108.8 . . ? C11 C8 C9 109.1(4) . . ? C11 C8 C10 109.8(5) . . ? C9 C8 C10 107.3(4) . . ? C11 C8 P1 115.6(4) . . ? C9 C8 P1 105.6(4) . . ? C10 C8 P1 109.2(4) . . ? C8 C9 H8 109.5 . . ? C8 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? C8 C9 H10 109.5 . . ? H8 C9 H10 109.5 . . ? H9 C9 H10 109.5 . . ? C8 C10 H11 109.5 . . ? C8 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C8 C10 H13 109.5 . . ? H11 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? C8 C11 H14 109.5 . . ? C8 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C8 C11 H16 109.5 . . ? H14 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? C15 C12 C13 109.8(4) . . ? C15 C12 C14 109.0(4) . . ? C13 C12 C14 108.6(4) . . ? C15 C12 P1 115.2(3) . . ? C13 C12 P1 104.6(3) . . ? C14 C12 P1 109.4(3) . . ? C12 C13 H17 109.5 . . ? C12 C13 H18 109.5 . . ? H17 C13 H18 109.5 . . ? C12 C13 H19 109.5 . . ? H17 C13 H19 109.5 . . ? H18 C13 H19 109.5 . . ? C12 C14 H20 109.5 . . ? C12 C14 H21 109.5 . . ? H20 C14 H21 109.5 . . ? C12 C14 H22 109.5 . . ? H20 C14 H22 109.5 . . ? H21 C14 H22 109.5 . . ? C12 C15 H23 109.5 . . ? C12 C15 H24 109.5 . . ? H23 C15 H24 109.5 . . ? C12 C15 H25 109.5 . . ? H23 C15 H25 109.5 . . ? H24 C15 H25 109.5 . . ? N2 C16 P2 105.2(3) . . ? N2 C16 H26 110.7 . . ? P2 C16 H26 110.7 . . ? N2 C16 H27 110.7 . . ? P2 C16 H27 110.7 . . ? H26 C16 H27 108.8 . . ? C19 C17 C18 110.2(4) . . ? C19 C17 C20 110.2(5) . . ? C18 C17 C20 106.9(4) . . ? C19 C17 P2 113.9(4) . . ? C18 C17 P2 105.6(3) . . ? C20 C17 P2 109.8(4) . . ? C17 C18 H28 109.5 . . ? C17 C18 H29 109.5 . . ? H28 C18 H29 109.5 . . ? C17 C18 H30 109.5 . . ? H28 C18 H30 109.5 . . ? H29 C18 H30 109.5 . . ? C17 C19 H31 109.5 . . ? C17 C19 H32 109.5 . . ? H31 C19 H32 109.5 . . ? C17 C19 H33 109.5 . . ? H31 C19 H33 109.5 . . ? H32 C19 H33 109.5 . . ? C17 C20 H34 109.5 . . ? C17 C20 H35 109.5 . . ? H34 C20 H35 109.5 . . ? C17 C20 H36 109.5 . . ? H34 C20 H36 109.5 . . ? H35 C20 H36 109.5 . . ? C24 C21 C23 108.3(4) . . ? C24 C21 C22 109.1(4) . . ? C23 C21 C22 108.8(4) . . ? C24 C21 P2 104.4(3) . . ? C23 C21 P2 110.5(3) . . ? C22 C21 P2 115.4(3) . . ? C21 C22 H37 109.5 . . ? C21 C22 H38 109.5 . . ? H37 C22 H38 109.5 . . ? C21 C22 H39 109.5 . . ? H37 C22 H39 109.5 . . ? H38 C22 H39 109.5 . . ? C21 C23 H40 109.5 . . ? C21 C23 H41 109.5 . . ? H40 C23 H41 109.5 . . ? C21 C23 H42 109.5 . . ? H40 C23 H42 109.5 . . ? H41 C23 H42 109.5 . . ? C21 C24 H43 109.5 . . ? C21 C24 H44 109.5 . . ? H43 C24 H44 109.5 . . ? C21 C24 H45 109.5 . . ? H43 C24 H45 109.5 . . ? H44 C24 H45 109.5 . . ? C26 C25 C30 120.0 . . ? C26 C25 H46 120.0 . . ? C30 C25 H46 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H47 120.0 . . ? C27 C26 H47 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H48 120.0 . . ? C26 C27 H48 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H49 120.0 . . ? C29 C28 H49 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H50 120.0 . . ? C30 C29 H50 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H51 120.0 . . ? C25 C30 H51 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 H52 120.0 . . ? C36 C31 H52 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H53 120.0 . . ? C33 C32 H53 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H54 120.0 . . ? C34 C33 H54 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H55 120.0 . . ? C33 C34 H55 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H56 120.0 . . ? C36 C35 H56 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H57 120.0 . . ? C31 C36 H57 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 Pt1 P1 C12 120.2(2) . . . . ? P2 Pt1 P1 C12 123.0(2) . . . . ? B1 Pt1 P1 C8 -107.3(2) . . . . ? P2 Pt1 P1 C8 -104.4(2) . . . . ? B1 Pt1 P1 C7 6.5(2) . . . . ? P2 Pt1 P1 C7 9.3(2) . . . . ? B1 Pt1 P2 C17 113.1(2) . . . . ? P1 Pt1 P2 C17 110.2(2) . . . . ? B1 Pt1 P2 C21 -115.2(2) . . . . ? P1 Pt1 P2 C21 -118.0(2) . . . . ? B1 Pt1 P2 C16 -1.6(2) . . . . ? P1 Pt1 P2 C16 -4.4(2) . . . . ? P2 Pt1 B1 N1 176.0(5) . . . . ? P1 Pt1 B1 N1 -5.1(4) . . . . ? P2 Pt1 B1 N2 0.4(4) . . . . ? P1 Pt1 B1 N2 179.3(5) . . . . ? N2 B1 N1 C1 0.1(6) . . . . ? Pt1 B1 N1 C1 -176.3(4) . . . . ? N2 B1 N1 C7 177.2(4) . . . . ? Pt1 B1 N1 C7 0.8(7) . . . . ? B1 N1 C1 C2 179.4(5) . . . . ? C7 N1 C1 C2 2.7(9) . . . . ? B1 N1 C1 C6 0.5(6) . . . . ? C7 N1 C1 C6 -176.2(5) . . . . ? N1 C1 C2 C3 178.9(5) . . . . ? C6 C1 C2 C3 -2.2(7) . . . . ? C1 C2 C3 C4 0.7(8) . . . . ? C2 C3 C4 C5 0.7(8) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 N2 -178.0(5) . . . . ? C4 C5 C6 C1 -1.0(7) . . . . ? C2 C1 C6 C5 2.4(7) . . . . ? N1 C1 C6 C5 -178.5(4) . . . . ? C2 C1 C6 N2 -179.9(4) . . . . ? N1 C1 C6 N2 -0.9(5) . . . . ? C5 C6 N2 B1 178.2(5) . . . . ? C1 C6 N2 B1 0.9(5) . . . . ? C5 C6 N2 C16 -8.4(9) . . . . ? C1 C6 N2 C16 174.4(5) . . . . ? N1 B1 N2 C6 -0.7(6) . . . . ? Pt1 B1 N2 C6 175.7(4) . . . . ? N1 B1 N2 C16 -174.9(4) . . . . ? Pt1 B1 N2 C16 1.5(7) . . . . ? C1 N1 C7 P1 -178.5(4) . . . . ? B1 N1 C7 P1 5.1(5) . . . . ? C12 P1 C7 N1 -129.4(3) . . . . ? C8 P1 C7 N1 112.5(3) . . . . ? Pt1 P1 C7 N1 -7.9(3) . . . . ? C12 P1 C8 C11 -47.7(5) . . . . ? C7 P1 C8 C11 62.5(4) . . . . ? Pt1 P1 C8 C11 179.1(3) . . . . ? C12 P1 C8 C9 -168.3(3) . . . . ? C7 P1 C8 C9 -58.2(4) . . . . ? Pt1 P1 C8 C9 58.5(4) . . . . ? C12 P1 C8 C10 76.6(4) . . . . ? C7 P1 C8 C10 -173.2(4) . . . . ? Pt1 P1 C8 C10 -56.6(4) . . . . ? C8 P1 C12 C15 62.5(4) . . . . ? C7 P1 C12 C15 -48.1(4) . . . . ? Pt1 P1 C12 C15 -165.0(3) . . . . ? C8 P1 C12 C13 -177.0(3) . . . . ? C7 P1 C12 C13 72.5(4) . . . . ? Pt1 P1 C12 C13 -44.4(4) . . . . ? C8 P1 C12 C14 -60.8(4) . . . . ? C7 P1 C12 C14 -171.3(3) . . . . ? Pt1 P1 C12 C14 71.7(3) . . . . ? C6 N2 C16 P2 -175.5(4) . . . . ? B1 N2 C16 P2 -2.6(6) . . . . ? C17 P2 C16 N2 -118.7(3) . . . . ? C21 P2 C16 N2 123.7(3) . . . . ? Pt1 P2 C16 N2 2.6(4) . . . . ? C21 P2 C17 C19 48.4(5) . . . . ? C16 P2 C17 C19 -61.8(4) . . . . ? Pt1 P2 C17 C19 -179.3(3) . . . . ? C21 P2 C17 C18 169.4(3) . . . . ? C16 P2 C17 C18 59.2(4) . . . . ? Pt1 P2 C17 C18 -58.3(4) . . . . ? C21 P2 C17 C20 -75.7(4) . . . . ? C16 P2 C17 C20 174.2(4) . . . . ? Pt1 P2 C17 C20 56.7(4) . . . . ? C17 P2 C21 C24 171.8(3) . . . . ? C16 P2 C21 C24 -77.4(4) . . . . ? Pt1 P2 C21 C24 39.6(4) . . . . ? C17 P2 C21 C23 55.6(4) . . . . ? C16 P2 C21 C23 166.3(3) . . . . ? Pt1 P2 C21 C23 -76.7(4) . . . . ? C17 P2 C21 C22 -68.4(4) . . . . ? C16 P2 C21 C22 42.3(4) . . . . ? Pt1 P2 C21 C22 159.4(3) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? C36 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.678 _refine_diff_density_min -2.135 _refine_diff_density_rms 0.114