Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.D.Kennedy ; Department of Chemistry University of Leeds Leeds, LS2 9JT, UK ; 'Jonathan Bould' ; Department of Chemistry University of Leeds Leeds, LS2 9JT, UK ; 'Colin Kilner' ; Department of Chemistry University of Leeds Leeds, LS2 9JT, UK ; _publ_contact_author_address ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_email J.D.Kennedy@chemistry.leeds.ac.uk _publ_contact_author_phone '+44 (0)113 34 36414 ' _publ_contact_author_name 'Professor J.D.Kennedy' _publ_section_title ; Metallaborane reaction chemistry. Part 11. The capture of dioxygen, carbon monoxide and sulphur dioxide by [(PMe2Ph)4Pt2B10H10]. ; data_jbpt2b10 _database_code_depnum_ccdc_archive 'CCDC 235553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H54 B10 O2 P4 Pt2' _chemical_formula_sum 'C32 H54 B10 O2 P4 Pt2' _chemical_formula_weight 1092.91 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 11.16130(10) _cell_length_b 28.0289(4) _cell_length_c 16.3931(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.6300(10) _cell_angle_gamma 90.00 _cell_volume 5082.99(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 5.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1537 _exptl_absorpt_correction_T_max 0.6020 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Fine-focus Sealed tube' _diffrn_radiation_collimation miracol _diffrn_radiation_polarisn_norm ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33449 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9930 _reflns_number_gt 7989 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS-97 (Sheldrick, 1986) ; _computing_structure_refinement ; SHELXS-97 (Sheldrick, 1986) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; 'enCIFer (CCDC, 2002)' ; _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. Two disordered dichloromethane solvent molecules were not modelled and the disordered density was taken into account using SQUEEZE/PLATON (Spek, 2003) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0664P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9930 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.000 _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 0.209649(19) 0.114542(8) 0.217259(13) 0.01871(9) Uani 1 1 d . . . Pt2 Pt 0.033517(19) 0.181176(8) 0.218877(13) 0.01851(9) Uani 1 1 d . . . P11 P 0.34261(14) 0.09982(6) 0.12014(10) 0.0234(4) Uani 1 1 d . . . P12 P 0.15907(15) 0.03443(6) 0.24692(10) 0.0259(4) Uani 1 1 d . . . P21 P -0.00400(14) 0.22221(6) 0.09023(10) 0.0241(4) Uani 1 1 d . . . P22 P -0.16322(14) 0.18503(6) 0.25451(10) 0.0237(4) Uani 1 1 d . . . O1 O 0.0670(4) 0.09733(16) 0.1212(3) 0.0290(11) Uani 1 1 d . . . O2 O -0.0361(4) 0.12425(15) 0.1382(3) 0.0269(10) Uani 1 1 d . . . C30 C 0.4099(6) 0.1493(2) 0.0734(4) 0.0294(15) Uani 1 1 d . . . H30A H 0.4479 0.1708 0.1164 0.044 Uiso 1 1 calc R . . H30B H 0.3473 0.1666 0.0375 0.044 Uiso 1 1 calc R . . H30C H 0.4712 0.1375 0.0408 0.044 Uiso 1 1 calc R . . C31 C 0.2721(6) 0.0682(2) 0.0293(4) 0.0278(15) Uani 1 1 d . . . H31A H 0.3178 0.0743 -0.0167 0.042 Uiso 1 1 calc R . . H31B H 0.1888 0.0794 0.0150 0.042 Uiso 1 1 calc R . . H31C H 0.2718 0.0339 0.0408 0.042 Uiso 1 1 calc R . . C32 C 0.4737(6) 0.0647(2) 0.1595(4) 0.0275(15) Uani 1 1 d . . . C33 C 0.5056(6) 0.0580(2) 0.2446(4) 0.0304(16) Uani 1 1 d . . . H33 H 0.4577 0.0723 0.2817 0.036 Uiso 1 1 calc R . . C34 C 0.6058(6) 0.0309(2) 0.2758(5) 0.0346(17) Uani 1 1 d . . . H34 H 0.6241 0.0260 0.3334 0.042 Uiso 1 1 calc R . . C35 C 0.6790(6) 0.0111(3) 0.2225(5) 0.0387(18) Uani 1 1 d . . . H35 H 0.7490 -0.0066 0.2435 0.046 Uiso 1 1 calc R . . C36 C 0.6483(6) 0.0174(3) 0.1359(5) 0.0428(19) Uani 1 1 d . . . H36 H 0.6964 0.0035 0.0986 0.051 Uiso 1 1 calc R . . C37 C 0.5488(6) 0.0437(3) 0.1077(4) 0.0368(17) Uani 1 1 d . . . H37 H 0.5295 0.0481 0.0499 0.044 Uiso 1 1 calc R . . C38 C 0.0016(6) 0.0270(3) 0.2574(5) 0.0401(18) Uani 1 1 d . . . H38A H -0.0476 0.0457 0.2149 0.060 Uiso 1 1 calc R . . H38B H -0.0130 0.0381 0.3119 0.060 Uiso 1 1 calc R . . H38C H -0.0202 -0.0068 0.2510 0.060 Uiso 1 1 calc R . . C39 C 0.2336(8) 0.0056(3) 0.3380(4) 0.048(2) Uani 1 1 d . . . H39A H 0.2183 -0.0288 0.3344 0.073 Uiso 1 1 calc R . . H39B H 0.2022 0.0185 0.3866 0.073 Uiso 1 1 calc R . . H39C H 0.3208 0.0115 0.3427 0.073 Uiso 1 1 calc R . . C40 C 0.1807(6) -0.0077(2) 0.1669(4) 0.0265(14) Uani 1 1 d . . . C41 C 0.0835(6) -0.0192(2) 0.1052(4) 0.0314(16) Uani 1 1 d . . . H41 H 0.0056 -0.0059 0.1074 0.038 Uiso 1 1 calc R . . C42 C 0.1032(7) -0.0507(3) 0.0400(4) 0.0374(17) Uani 1 1 d . . . H42 H 0.0384 -0.0594 -0.0009 0.045 Uiso 1 1 calc R . . C43 C 0.2201(8) -0.0687(3) 0.0374(5) 0.047(2) Uani 1 1 d . . . H43 H 0.2355 -0.0873 -0.0086 0.056 Uiso 1 1 calc R . . C44 C 0.3134(7) -0.0600(2) 0.0999(5) 0.0408(18) Uani 1 1 d . . . H44 H 0.3905 -0.0742 0.0990 0.049 Uiso 1 1 calc R . . C45 C 0.2921(6) -0.0301(2) 0.1643(4) 0.0313(16) Uani 1 1 d . . . H45 H 0.3555 -0.0246 0.2080 0.038 Uiso 1 1 calc R . . C46 C 0.0657(6) 0.1911(2) 0.0118(4) 0.0305(15) Uani 1 1 d . . . H46A H 0.0457 0.1571 0.0131 0.046 Uiso 1 1 calc R . . H46B H 0.1536 0.1951 0.0224 0.046 Uiso 1 1 calc R . . H46C H 0.0355 0.2042 -0.0424 0.046 Uiso 1 1 calc R . . C47 C 0.0497(7) 0.2828(3) 0.0867(4) 0.0390(18) Uani 1 1 d . . . H47A H 0.0282 0.2956 0.0310 0.058 Uiso 1 1 calc R . . H47B H 0.1378 0.2833 0.1012 0.058 Uiso 1 1 calc R . . H47C H 0.0123 0.3024 0.1259 0.058 Uiso 1 1 calc R . . C48 C -0.1598(5) 0.2275(2) 0.0433(4) 0.0214(13) Uani 1 1 d . . . C49 C -0.2092(6) 0.1915(2) -0.0106(4) 0.0320(16) Uani 1 1 d . . . H49 H -0.1606 0.1653 -0.0229 0.038 Uiso 1 1 calc R . . C50 C -0.3299(6) 0.1942(3) -0.0461(4) 0.0386(18) Uani 1 1 d . . . H50 H -0.3634 0.1691 -0.0810 0.046 Uiso 1 1 calc R . . C51 C -0.4008(7) 0.2323(3) -0.0315(4) 0.0402(19) Uani 1 1 d . . . H51 H -0.4818 0.2343 -0.0577 0.048 Uiso 1 1 calc R . . C52 C -0.3526(6) 0.2683(3) 0.0225(4) 0.0432(19) Uani 1 1 d . . . H52 H -0.4014 0.2945 0.0342 0.052 Uiso 1 1 calc R . . C53 C -0.2319(6) 0.2652(3) 0.0591(4) 0.0377(18) Uani 1 1 d . . . H53 H -0.1993 0.2897 0.0956 0.045 Uiso 1 1 calc R . . C54 C -0.1952(6) 0.1586(3) 0.3530(4) 0.0377(18) Uani 1 1 d . . . H54A H -0.1412 0.1727 0.3986 0.056 Uiso 1 1 calc R . . H54B H -0.1818 0.1240 0.3519 0.056 Uiso 1 1 calc R . . H54C H -0.2794 0.1650 0.3604 0.056 Uiso 1 1 calc R . . C55 C -0.2709(6) 0.1523(3) 0.1827(4) 0.0327(16) Uani 1 1 d . . . H55A H -0.3480 0.1498 0.2049 0.049 Uiso 1 1 calc R . . H55B H -0.2395 0.1202 0.1746 0.049 Uiso 1 1 calc R . . H55C H -0.2834 0.1691 0.1299 0.049 Uiso 1 1 calc R . . C56 C -0.2200(6) 0.2460(2) 0.2580(4) 0.0293(15) Uani 1 1 d . . . C57 C -0.3473(6) 0.2547(2) 0.2408(4) 0.0297(15) Uani 1 1 d . . . H57 H -0.4018 0.2286 0.2337 0.036 Uiso 1 1 calc R . . C58 C -0.3904(7) 0.2996(3) 0.2347(5) 0.0411(18) Uani 1 1 d . . . H58 H -0.4750 0.3048 0.2226 0.049 Uiso 1 1 calc R . . C59 C -0.3102(6) 0.3396(3) 0.2461(5) 0.0408(18) Uani 1 1 d . . . H59 H -0.3405 0.3713 0.2414 0.049 Uiso 1 1 calc R . . C60 C -0.1842(7) 0.3308(3) 0.2646(4) 0.0367(17) Uani 1 1 d . . . H60 H -0.1291 0.3567 0.2737 0.044 Uiso 1 1 calc R . . C61 C -0.1414(6) 0.2835(2) 0.2696(4) 0.0318(16) Uani 1 1 d . . . H61 H -0.0570 0.2776 0.2810 0.038 Uiso 1 1 calc R . . B3 B 0.1156(6) 0.1364(3) 0.3290(4) 0.0222(15) Uani 1 1 d . . . H3 H 0.0508 0.1085 0.3450 0.027 Uiso 1 1 calc R . . B4 B 0.2829(6) 0.1278(3) 0.3461(4) 0.0234(16) Uani 1 1 d . . . H4 H 0.3238 0.0940 0.3736 0.028 Uiso 1 1 calc R . . B5 B 0.3546(7) 0.1621(3) 0.2734(4) 0.0257(16) Uani 1 1 d . . . H5 H 0.4427 0.1513 0.2531 0.031 Uiso 1 1 calc R . . B6 B 0.2343(6) 0.1952(3) 0.2048(5) 0.0235(16) Uani 1 1 d . . . H6 H 0.2460 0.2053 0.1402 0.028 Uiso 1 1 calc R . . B7 B 0.0917(6) 0.2022(3) 0.3481(4) 0.0229(15) Uani 1 1 d . . . H7 H 0.0128 0.2161 0.3765 0.027 Uiso 1 1 calc R . . B8 B 0.2083(7) 0.1678(3) 0.4065(4) 0.0260(16) Uani 1 1 d . . . H8 H 0.1991 0.1584 0.4718 0.031 Uiso 1 1 calc R . . B9 B 0.3506(7) 0.1832(3) 0.3739(5) 0.0302(18) Uani 1 1 d . . . H9 H 0.4363 0.1850 0.4180 0.036 Uiso 1 1 calc R . . B10 B 0.3200(6) 0.2239(3) 0.2889(4) 0.0255(16) Uani 1 1 d . . . H10 H 0.3850 0.2524 0.2755 0.031 Uiso 1 1 calc R . . B11 B 0.1617(7) 0.2363(3) 0.2722(4) 0.0283(17) Uani 1 1 d . . . H11 H 0.1277 0.2723 0.2501 0.034 Uiso 1 1 calc R . . B12 B 0.2382(6) 0.2280(3) 0.3765(4) 0.0254(16) Uani 1 1 d . . . H12 H 0.2518 0.2581 0.4218 0.030 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 0.01598(13) 0.01893(15) 0.02203(14) -0.00113(9) 0.00548(9) -0.00141(9) Pt2 0.01533(13) 0.01899(15) 0.02199(14) -0.00047(9) 0.00535(9) -0.00126(9) P11 0.0208(8) 0.0253(9) 0.0259(9) -0.0030(7) 0.0098(7) -0.0019(7) P12 0.0266(9) 0.0216(9) 0.0306(9) 0.0001(7) 0.0077(7) -0.0036(7) P21 0.0225(8) 0.0253(10) 0.0251(8) 0.0033(7) 0.0054(7) -0.0014(7) P22 0.0176(8) 0.0252(10) 0.0296(9) -0.0001(7) 0.0079(7) -0.0007(7) O1 0.020(2) 0.035(3) 0.031(2) -0.016(2) -0.0018(18) 0.006(2) O2 0.015(2) 0.026(3) 0.039(3) -0.015(2) 0.0011(18) -0.0010(18) C30 0.029(3) 0.032(4) 0.031(3) 0.004(3) 0.014(3) 0.006(3) C31 0.030(3) 0.025(4) 0.029(3) -0.002(3) 0.005(3) -0.006(3) C32 0.025(3) 0.025(4) 0.034(4) -0.007(3) 0.008(3) -0.004(3) C33 0.027(3) 0.030(4) 0.035(4) -0.003(3) 0.008(3) 0.007(3) C34 0.027(3) 0.026(4) 0.050(4) -0.008(3) 0.003(3) 0.008(3) C35 0.027(3) 0.034(5) 0.057(5) 0.007(4) 0.010(3) 0.003(3) C36 0.034(4) 0.033(5) 0.065(5) -0.004(4) 0.019(4) 0.005(3) C37 0.036(4) 0.040(5) 0.035(4) -0.005(3) 0.005(3) 0.003(3) C38 0.040(4) 0.028(4) 0.056(5) -0.009(4) 0.024(4) -0.011(3) C39 0.083(6) 0.029(4) 0.032(4) 0.005(3) 0.006(4) -0.004(4) C40 0.030(3) 0.019(4) 0.031(3) 0.008(3) 0.007(3) -0.003(3) C41 0.043(4) 0.022(4) 0.031(4) 0.009(3) 0.010(3) -0.002(3) C42 0.047(4) 0.026(4) 0.038(4) -0.009(3) 0.003(3) -0.010(4) C43 0.077(6) 0.026(4) 0.044(4) 0.002(3) 0.027(4) -0.008(4) C44 0.038(4) 0.019(4) 0.069(5) -0.003(4) 0.019(4) -0.008(3) C45 0.033(4) 0.024(4) 0.036(4) 0.006(3) 0.005(3) -0.003(3) C46 0.028(3) 0.030(4) 0.035(4) 0.002(3) 0.009(3) -0.001(3) C47 0.043(4) 0.033(4) 0.042(4) 0.003(3) 0.010(3) -0.001(3) C48 0.026(3) 0.015(3) 0.022(3) 0.002(3) 0.003(2) 0.011(3) C49 0.025(3) 0.030(4) 0.040(4) 0.003(3) 0.002(3) 0.001(3) C50 0.024(4) 0.043(5) 0.045(4) 0.001(4) -0.008(3) -0.002(3) C51 0.038(4) 0.039(5) 0.041(4) 0.001(3) -0.005(3) 0.006(4) C52 0.037(4) 0.046(5) 0.044(4) -0.001(4) -0.004(3) 0.018(4) C53 0.044(4) 0.036(5) 0.031(4) -0.004(3) -0.002(3) -0.001(4) C54 0.032(4) 0.046(5) 0.038(4) 0.011(3) 0.015(3) -0.006(3) C55 0.021(3) 0.035(4) 0.044(4) -0.006(3) 0.013(3) -0.011(3) C56 0.026(3) 0.024(4) 0.040(4) -0.008(3) 0.012(3) 0.001(3) C57 0.026(3) 0.021(4) 0.044(4) -0.007(3) 0.012(3) 0.000(3) C58 0.037(4) 0.041(5) 0.049(5) -0.004(4) 0.018(3) 0.003(4) C59 0.029(4) 0.036(5) 0.057(5) -0.004(4) 0.003(3) 0.000(3) C60 0.044(4) 0.020(4) 0.049(4) -0.005(3) 0.015(3) 0.007(3) C61 0.025(3) 0.032(4) 0.041(4) -0.004(3) 0.013(3) 0.004(3) B3 0.021(3) 0.028(4) 0.020(3) -0.005(3) 0.010(3) -0.002(3) B4 0.019(3) 0.025(4) 0.027(4) 0.003(3) 0.005(3) 0.003(3) B5 0.029(4) 0.019(4) 0.030(4) -0.002(3) 0.007(3) -0.006(3) B6 0.018(3) 0.020(4) 0.034(4) -0.010(3) 0.010(3) -0.002(3) B7 0.022(4) 0.027(4) 0.021(3) 0.002(3) 0.008(3) 0.000(3) B8 0.031(4) 0.024(4) 0.023(4) -0.003(3) 0.005(3) 0.005(3) B9 0.029(4) 0.033(5) 0.027(4) -0.004(3) -0.001(3) -0.002(3) B10 0.018(3) 0.028(4) 0.030(4) -0.006(3) 0.002(3) -0.005(3) B11 0.032(4) 0.033(5) 0.020(4) -0.002(3) 0.006(3) 0.003(3) B12 0.023(4) 0.028(4) 0.026(4) -0.008(3) 0.003(3) 0.003(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 O1 2.141(4) . ? Pt1 B4 2.192(7) . ? Pt1 B5 2.201(7) . ? Pt1 B6 2.291(7) . ? Pt1 B3 2.312(7) . ? Pt1 P11 2.3525(16) . ? Pt1 P12 2.3812(17) . ? Pt1 Pt2 2.7143(3) . ? Pt2 O2 2.151(4) . ? Pt2 B11 2.207(8) . ? Pt2 B7 2.212(7) . ? Pt2 B3 2.287(7) . ? Pt2 B6 2.317(7) . ? Pt2 P22 2.3485(16) . ? Pt2 P21 2.3898(16) . ? P11 C30 1.798(7) . ? P11 C32 1.810(7) . ? P11 C31 1.819(6) . ? P12 C38 1.800(7) . ? P12 C39 1.802(7) . ? P12 C40 1.804(7) . ? P21 C47 1.804(7) . ? P21 C48 1.812(6) . ? P21 C46 1.812(7) . ? P22 C55 1.816(6) . ? P22 C56 1.826(7) . ? P22 C54 1.853(7) . ? O1 O2 1.434(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.400(9) . ? C32 C33 1.406(9) . ? C33 C34 1.391(9) . ? C33 H33 0.9500 . ? C34 C35 1.389(10) . ? C34 H34 0.9500 . ? C35 C36 1.426(10) . ? C35 H35 0.9500 . ? C36 C37 1.362(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.398(9) . ? C40 C41 1.419(9) . ? C41 C42 1.428(9) . ? C41 H41 0.9500 . ? C42 C43 1.405(11) . ? C42 H42 0.9500 . ? C43 C44 1.383(10) . ? C43 H43 0.9500 . ? C44 C45 1.394(10) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.375(9) . ? C48 C49 1.404(9) . ? C49 C50 1.397(9) . ? C49 H49 0.9500 . ? C50 C51 1.370(10) . ? C50 H50 0.9500 . ? C51 C52 1.400(10) . ? C51 H51 0.9500 . ? C52 C53 1.403(9) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C61 1.366(9) . ? C56 C57 1.432(9) . ? C57 C58 1.347(10) . ? C57 H57 0.9500 . ? C58 C59 1.431(10) . ? C58 H58 0.9500 . ? C59 C60 1.420(9) . ? C59 H59 0.9500 . ? C60 C61 1.410(9) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? B3 B8 1.762(10) . ? B3 B4 1.867(10) . ? B3 B7 1.894(11) . ? B3 H3 1.1200 . ? B4 B9 1.761(11) . ? B4 B8 1.775(10) . ? B4 B5 1.799(10) . ? B4 H4 1.1200 . ? B5 B9 1.757(10) . ? B5 B10 1.802(11) . ? B5 B6 1.879(10) . ? B5 H5 1.1200 . ? B6 B10 1.764(9) . ? B6 B11 1.855(10) . ? B6 H6 1.1200 . ? B7 B8 1.791(10) . ? B7 B12 1.793(10) . ? B7 B11 1.826(10) . ? B7 H7 1.1200 . ? B8 B9 1.795(11) . ? B8 B12 1.802(11) . ? B8 H8 1.1200 . ? B9 B12 1.779(11) . ? B9 B10 1.798(11) . ? B9 H9 1.1200 . ? B10 B11 1.785(10) . ? B10 B12 1.804(10) . ? B10 H10 1.1200 . ? B11 B12 1.822(10) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? 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 O1 Pt1 B4 153.2(2) . . ? O1 Pt1 B5 151.4(2) . . ? B4 Pt1 B5 48.3(3) . . ? O1 Pt1 B6 104.1(2) . . ? B4 Pt1 B6 83.4(3) . . ? B5 Pt1 B6 49.4(3) . . ? O1 Pt1 B3 105.7(2) . . ? B4 Pt1 B3 48.9(2) . . ? B5 Pt1 B3 83.9(3) . . ? B6 Pt1 B3 83.2(3) . . ? O1 Pt1 P11 86.38(12) . . ? B4 Pt1 P11 119.56(19) . . ? B5 Pt1 P11 83.9(2) . . ? B6 Pt1 P11 91.08(19) . . ? B3 Pt1 P11 167.52(17) . . ? O1 Pt1 P12 76.38(13) . . ? B4 Pt1 P12 91.8(2) . . ? B5 Pt1 P12 131.8(2) . . ? B6 Pt1 P12 169.66(19) . . ? B3 Pt1 P12 86.8(2) . . ? P11 Pt1 P12 99.25(6) . . ? O1 Pt1 Pt2 72.15(11) . . ? B4 Pt1 Pt2 93.00(19) . . ? B5 Pt1 Pt2 94.2(2) . . ? B6 Pt1 Pt2 54.36(17) . . ? B3 Pt1 Pt2 53.41(18) . . ? P11 Pt1 Pt2 130.55(4) . . ? P12 Pt1 Pt2 117.08(4) . . ? O2 Pt2 B11 157.8(2) . . ? O2 Pt2 B7 145.3(2) . . ? B11 Pt2 B7 48.8(3) . . ? O2 Pt2 B3 98.8(2) . . ? B11 Pt2 B3 84.3(3) . . ? B7 Pt2 B3 49.7(3) . . ? O2 Pt2 B6 109.9(2) . . ? B11 Pt2 B6 48.3(3) . . ? B7 Pt2 B6 83.4(3) . . ? B3 Pt2 B6 83.1(3) . . ? O2 Pt2 P22 85.04(12) . . ? B11 Pt2 P22 116.6(2) . . ? B7 Pt2 P22 85.11(19) . . ? B3 Pt2 P22 96.81(18) . . ? B6 Pt2 P22 164.94(18) . . ? O2 Pt2 P21 78.92(13) . . ? B11 Pt2 P21 92.4(2) . . ? B7 Pt2 P21 135.4(2) . . ? B3 Pt2 P21 164.85(18) . . ? B6 Pt2 P21 83.62(19) . . ? P22 Pt2 P21 97.89(6) . . ? O2 Pt2 Pt1 71.73(11) . . ? B11 Pt2 Pt1 93.1(2) . . ? B7 Pt2 Pt1 94.10(19) . . ? B3 Pt2 Pt1 54.25(17) . . ? B6 Pt2 Pt1 53.46(18) . . ? P22 Pt2 Pt1 137.43(4) . . ? P21 Pt2 Pt1 111.39(4) . . ? C30 P11 C32 102.0(3) . . ? C30 P11 C31 100.8(3) . . ? C32 P11 C31 105.6(3) . . ? C30 P11 Pt1 119.3(2) . . ? C32 P11 Pt1 114.0(2) . . ? C31 P11 Pt1 113.3(2) . . ? C38 P12 C39 102.6(4) . . ? C38 P12 C40 102.7(3) . . ? C39 P12 C40 102.6(3) . . ? C38 P12 Pt1 112.9(3) . . ? C39 P12 Pt1 119.7(3) . . ? C40 P12 Pt1 114.2(2) . . ? C47 P21 C48 102.4(3) . . ? C47 P21 C46 104.7(3) . . ? C48 P21 C46 102.5(3) . . ? C47 P21 Pt2 117.5(2) . . ? C48 P21 Pt2 117.4(2) . . ? C46 P21 Pt2 110.6(2) . . ? C55 P22 C56 106.9(3) . . ? C55 P22 C54 100.1(3) . . ? C56 P22 C54 103.9(3) . . ? C55 P22 Pt2 112.1(2) . . ? C56 P22 Pt2 113.0(2) . . ? C54 P22 Pt2 119.5(2) . . ? O2 O1 Pt1 106.0(3) . . ? O1 O2 Pt2 106.0(3) . . ? P11 C30 H30A 109.5 . . ? P11 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P11 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P11 C31 H31A 109.5 . . ? P11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 116.9(6) . . ? C37 C32 P11 122.2(5) . . ? C33 C32 P11 120.9(5) . . ? C34 C33 C32 121.5(6) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C33 119.9(7) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 119.5(6) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 118.9(7) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C32 123.2(7) . . ? C36 C37 H37 118.4 . . ? C32 C37 H37 118.4 . . ? P12 C38 H38A 109.5 . . ? P12 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P12 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P12 C39 H39A 109.5 . . ? P12 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P12 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 118.4(6) . . ? C45 C40 P12 121.4(5) . . ? C41 C40 P12 120.2(5) . . ? C40 C41 C42 119.7(6) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 118.8(7) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C44 C43 C42 121.7(7) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C45 118.6(7) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C44 C45 C40 122.4(6) . . ? C44 C45 H45 118.8 . . ? C40 C45 H45 118.8 . . ? P21 C46 H46A 109.5 . . ? P21 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? P21 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? P21 C47 H47A 109.5 . . ? P21 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? P21 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 118.7(6) . . ? C53 C48 P21 122.3(5) . . ? C49 C48 P21 118.9(5) . . ? C50 C49 C48 120.0(7) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 121.1(7) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 119.3(7) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C51 C52 C53 119.5(7) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C48 C53 C52 121.2(6) . . ? C48 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? P22 C54 H54A 109.5 . . ? P22 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? P22 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? P22 C55 H55A 109.5 . . ? P22 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? P22 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C61 C56 C57 119.9(6) . . ? C61 C56 P22 120.3(5) . . ? C57 C56 P22 119.5(5) . . ? C58 C57 C56 120.6(6) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 120.8(7) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C60 C59 C58 118.5(7) . . ? C60 C59 H59 120.8 . . ? C58 C59 H59 120.8 . . ? C61 C60 C59 119.6(7) . . ? C61 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C56 C61 C60 120.7(6) . . ? C56 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? B8 B3 B4 58.5(4) . . ? B8 B3 B7 58.5(4) . . ? B4 B3 B7 105.2(5) . . ? B8 B3 Pt2 115.5(5) . . ? B4 B3 Pt2 118.5(4) . . ? B7 B3 Pt2 63.1(3) . . ? B8 B3 Pt1 114.7(4) . . ? B4 B3 Pt1 62.2(3) . . ? B7 B3 Pt1 118.6(4) . . ? Pt2 B3 Pt1 72.3(2) . . ? B8 B3 H3 120.9 . . ? B4 B3 H3 122.5 . . ? B7 B3 H3 122.1 . . ? Pt2 B3 H3 111.4 . . ? Pt1 B3 H3 112.1 . . ? B9 B4 B8 61.0(4) . . ? B9 B4 B5 59.1(4) . . ? B8 B4 B5 108.4(5) . . ? B9 B4 B3 108.1(5) . . ? B8 B4 B3 57.8(4) . . ? B5 B4 B3 110.8(5) . . ? B9 B4 Pt1 119.4(5) . . ? B8 B4 Pt1 120.1(4) . . ? B5 B4 Pt1 66.1(3) . . ? B3 B4 Pt1 68.9(3) . . ? B9 B4 H4 120.2 . . ? B8 B4 H4 120.4 . . ? B5 B4 H4 121.7 . . ? B3 B4 H4 121.1 . . ? Pt1 B4 H4 109.0 . . ? B9 B5 B4 59.4(4) . . ? B9 B5 B10 60.7(4) . . ? B4 B5 B10 107.3(5) . . ? B9 B5 B6 106.8(5) . . ? B4 B5 B6 108.4(5) . . ? B10 B5 B6 57.2(4) . . ? B9 B5 Pt1 119.2(5) . . ? B4 B5 Pt1 65.6(3) . . ? B10 B5 Pt1 118.8(4) . . ? B6 B5 Pt1 67.8(3) . . ? B9 B5 H5 120.2 . . ? B4 B5 H5 122.6 . . ? B10 B5 H5 120.9 . . ? B6 B5 H5 122.7 . . ? Pt1 B5 H5 109.8 . . ? B10 B6 B11 59.0(4) . . ? B10 B6 B5 59.2(4) . . ? B11 B6 B5 106.5(5) . . ? B10 B6 Pt1 116.1(5) . . ? B11 B6 Pt1 119.5(4) . . ? B5 B6 Pt1 62.8(3) . . ? B10 B6 Pt2 115.5(4) . . ? B11 B6 Pt2 62.7(3) . . ? B5 B6 Pt2 118.7(4) . . ? Pt1 B6 Pt2 72.2(2) . . ? B10 B6 H6 120.4 . . ? B11 B6 H6 121.5 . . ? B5 B6 H6 121.8 . . ? Pt1 B6 H6 111.3 . . ? Pt2 B6 H6 111.9 . . ? B8 B7 B12 60.4(4) . . ? B8 B7 B11 107.5(5) . . ? B12 B7 B11 60.4(4) . . ? B8 B7 B3 57.1(4) . . ? B12 B7 B3 107.0(5) . . ? B11 B7 B3 108.4(5) . . ? B8 B7 Pt2 117.9(4) . . ? B12 B7 Pt2 119.9(4) . . ? B11 B7 Pt2 65.5(3) . . ? B3 B7 Pt2 67.2(3) . . ? B8 B7 H7 121.4 . . ? B12 B7 H7 119.5 . . ? B11 B7 H7 122.1 . . ? B3 B7 H7 123.0 . . ? Pt2 B7 H7 110.1 . . ? B3 B8 B4 63.7(4) . . ? B3 B8 B7 64.4(4) . . ? B4 B8 B7 113.8(5) . . ? B3 B8 B9 111.3(5) . . ? B4 B8 B9 59.1(4) . . ? B7 B8 B9 108.7(5) . . ? B3 B8 B12 112.5(5) . . ? B4 B8 B12 108.8(5) . . ? B7 B8 B12 59.9(4) . . ? B9 B8 B12 59.3(4) . . ? B3 B8 H8 116.9 . . ? B4 B8 H8 119.6 . . ? B7 B8 H8 119.0 . . ? B9 B8 H8 122.5 . . ? B12 B8 H8 121.6 . . ? B5 B9 B4 61.5(4) . . ? B5 B9 B12 111.5(5) . . ? B4 B9 B12 110.4(5) . . ? B5 B9 B8 109.4(5) . . ? B4 B9 B8 59.9(4) . . ? B12 B9 B8 60.6(4) . . ? B5 B9 B10 60.9(4) . . ? B4 B9 B10 109.2(5) . . ? B12 B9 B10 60.5(4) . . ? B8 B9 B10 107.4(5) . . ? B5 B9 H9 119.6 . . ? B4 B9 H9 120.6 . . ? B12 B9 H9 119.7 . . ? B8 B9 H9 122.2 . . ? B10 B9 H9 121.9 . . ? B6 B10 B11 63.0(4) . . ? B6 B10 B9 110.1(5) . . ? B11 B10 B9 109.0(5) . . ? B6 B10 B5 63.6(4) . . ? B11 B10 B5 113.1(5) . . ? B9 B10 B5 58.4(4) . . ? B6 B10 B12 111.9(5) . . ? B11 B10 B12 61.0(4) . . ? B9 B10 B12 59.2(4) . . ? B5 B10 B12 108.3(5) . . ? B6 B10 H10 118.0 . . ? B11 B10 H10 119.0 . . ? B9 B10 H10 122.9 . . ? B5 B10 H10 120.1 . . ? B12 B10 H10 121.4 . . ? B10 B11 B12 60.0(4) . . ? B10 B11 B7 107.3(5) . . ? B12 B11 B7 58.9(4) . . ? B10 B11 B6 57.9(4) . . ? B12 B11 B6 107.0(5) . . ? B7 B11 B6 109.9(5) . . ? B10 B11 Pt2 120.0(5) . . ? B12 B11 Pt2 118.7(5) . . ? B7 B11 Pt2 65.7(3) . . ? B6 B11 Pt2 68.9(3) . . ? B10 B11 H11 120.7 . . ? B12 B11 H11 121.1 . . ? B7 B11 H11 122.3 . . ? B6 B11 H11 121.4 . . ? Pt2 B11 H11 109.1 . . ? B9 B12 B7 109.3(5) . . ? B9 B12 B8 60.2(4) . . ? B7 B12 B8 59.8(4) . . ? B9 B12 B10 60.2(4) . . ? B7 B12 B10 107.9(5) . . ? B8 B12 B10 106.8(5) . . ? B9 B12 B11 108.2(5) . . ? B7 B12 B11 60.7(4) . . ? B8 B12 B11 107.2(5) . . ? B10 B12 B11 59.0(4) . . ? B9 B12 H12 120.9 . . ? B7 B12 H12 121.0 . . ? B8 B12 H12 122.5 . . ? B10 B12 H12 122.5 . . ? B11 B12 H12 122.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.048 _refine_diff_density_min -2.058 _refine_diff_density_rms 0.238 data_jb303 _database_code_depnum_ccdc_archive 'CCDC 254027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H54 B10 O P4 Pt2, 1.5(C H2 Cl2)' _chemical_formula_sum 'C34.50 H57 B10 Cl3 O P4 Pt2' _chemical_formula_weight 1216.31 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' O O 0.0106 0.0060 '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' 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/n _symmetry_space_group_name_Hall '-P 2yn' 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 12.58500(10) _cell_length_b 24.1210(2) _cell_length_c 15.4290(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.8930(4) _cell_angle_gamma 90.00 _cell_volume 4639.30(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49889 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2356 _exptl_absorpt_coefficient_mu 6.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.126 _exptl_absorpt_correction_T_max 0.601 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38. ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method 'phi and omega scans to fill asymmetric unit' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 44822 _diffrn_reflns_av_R_equivalents 0.1593 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9102 _reflns_number_gt 8186 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'local program' _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^)+(0.0566P)^2^+11.7251P] 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 9102 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Pt2 Pt 0.639753(18) 0.333332(9) 0.849938(15) 0.02232(9) Uani 1 1 d . . . Pt1 Pt 0.616711(17) 0.230623(9) 0.922243(15) 0.02144(9) Uani 1 1 d . . . P4 P 0.60522(14) 0.41484(7) 0.92394(11) 0.0300(4) Uani 1 1 d . . . P3 P 0.54561(13) 0.35943(7) 0.71523(11) 0.0270(3) Uani 1 1 d . . . P2 P 0.49781(13) 0.16827(6) 0.84186(11) 0.0256(3) Uani 1 1 d . . . P1 P 0.56911(13) 0.21364(7) 1.06121(11) 0.0263(3) Uani 1 1 d . . . B4 B 0.7926(6) 0.2256(3) 0.9778(5) 0.0300(17) Uani 1 1 d . . . H4 H 0.8018 0.2006 1.0396 0.036 Uiso 1 1 calc R . . C44 C 0.6771(7) 0.4176(3) 1.1054(5) 0.0464(19) Uani 1 1 d . . . H44 H 0.7456 0.4268 1.0902 0.056 Uiso 1 1 calc R . . C41 C 0.4814(6) 0.4501(3) 0.8831(4) 0.0382(16) Uani 1 1 d . . . H41A H 0.4743 0.4834 0.9181 0.046 Uiso 1 1 calc R . . H41B H 0.4206 0.4253 0.8872 0.046 Uiso 1 1 calc R . . H41C H 0.4824 0.4606 0.8218 0.046 Uiso 1 1 calc R . . C22 C 0.4373(7) 0.1909(4) 0.7349(5) 0.051(2) Uani 1 1 d . . . H22A H 0.3896 0.1618 0.7076 0.061 Uiso 1 1 calc R . . H22B H 0.4935 0.1984 0.6984 0.061 Uiso 1 1 calc R . . H22C H 0.3958 0.2248 0.7406 0.061 Uiso 1 1 calc R . . B9 B 0.8906(6) 0.2218(4) 0.9036(6) 0.0363(18) Uani 1 1 d . . . H9 H 0.9611 0.1933 0.9173 0.044 Uiso 1 1 calc R . . C31 C 0.3987(5) 0.3614(3) 0.7065(5) 0.0347(15) Uani 1 1 d . . . H31A H 0.3685 0.3728 0.6473 0.042 Uiso 1 1 calc R . . H31B H 0.3774 0.3879 0.7490 0.042 Uiso 1 1 calc R . . H31C H 0.3718 0.3244 0.7185 0.042 Uiso 1 1 calc R . . C37 C 0.7192(8) 0.4980(4) 0.6721(6) 0.061(2) Uani 1 1 d . . . H37 H 0.7917 0.5097 0.6857 0.073 Uiso 1 1 calc R . . C38 C 0.6892(7) 0.4455(3) 0.6981(5) 0.0468(19) Uani 1 1 d . . . H38 H 0.7414 0.4213 0.7281 0.056 Uiso 1 1 calc R . . C23 C 0.3809(5) 0.1477(3) 0.8915(5) 0.0352(16) Uani 1 1 d . . . C42 C 0.7022(8) 0.4705(3) 0.9231(6) 0.056(2) Uani 1 1 d . . . H42A H 0.6797 0.5023 0.9558 0.067 Uiso 1 1 calc R . . H42B H 0.7064 0.4816 0.8626 0.067 Uiso 1 1 calc R . . H42C H 0.7727 0.4577 0.9506 0.067 Uiso 1 1 calc R . . C14 C 0.5420(8) 0.1205(3) 1.1665(5) 0.055(2) Uani 1 1 d . . . H14 H 0.4963 0.1434 1.1952 0.067 Uiso 1 1 calc R . . B10 B 0.8263(6) 0.2349(3) 0.7951(5) 0.0318(17) Uani 1 1 d . . . H10 H 0.8521 0.2142 0.7364 0.038 Uiso 1 1 calc R . . C33 C 0.5826(6) 0.4285(3) 0.6800(4) 0.0328(15) Uani 1 1 d . . . B12 B 0.9052(6) 0.2871(4) 0.8551(5) 0.0355(18) Uani 1 1 d . . . H12 H 0.9849 0.3000 0.8374 0.043 Uiso 1 1 calc R . . C47 C 0.4802(8) 0.3895(4) 1.1526(6) 0.055(2) Uani 1 1 d . . . H47 H 0.4121 0.3801 1.1682 0.066 Uiso 1 1 calc R . . B5 B 0.7603(6) 0.1946(3) 0.8697(5) 0.0317(16) Uani 1 1 d . . . H5 H 0.7487 0.1488 0.8603 0.038 Uiso 1 1 calc R . . C15 C 0.5616(10) 0.0663(4) 1.1932(6) 0.069(3) Uani 1 1 d . . . H15 H 0.5286 0.0520 1.2403 0.083 Uiso 1 1 calc R . . C34 C 0.5090(7) 0.4639(3) 0.6351(5) 0.0483(19) Uani 1 1 d . . . H34 H 0.4361 0.4529 0.6215 0.058 Uiso 1 1 calc R . . C32 C 0.5616(6) 0.3172(3) 0.6205(4) 0.0357(15) Uani 1 1 d . . . H32A H 0.5180 0.3326 0.5686 0.043 Uiso 1 1 calc R . . H32B H 0.5382 0.2792 0.6302 0.043 Uiso 1 1 calc R . . H32C H 0.6372 0.3169 0.6116 0.043 Uiso 1 1 calc R . . C46 C 0.5631(10) 0.3991(4) 1.2167(6) 0.065(3) Uani 1 1 d . . . H46 H 0.5534 0.3957 1.2764 0.078 Uiso 1 1 calc R . . B8 B 0.8780(6) 0.2835(4) 0.9649(5) 0.0349(17) Uani 1 1 d . . . H8 H 0.9396 0.2955 1.0212 0.042 Uiso 1 1 calc R . . C43 C 0.5919(6) 0.4079(3) 1.0404(5) 0.0363(15) Uani 1 1 d . . . C13 C 0.5900(6) 0.1414(3) 1.0971(4) 0.0362(15) Uani 1 1 d . . . C11 C 0.4312(6) 0.2293(3) 1.0774(5) 0.0398(18) Uani 1 1 d . . . H11A H 0.4212 0.2204 1.1377 0.048 Uiso 1 1 calc R . . H11B H 0.3816 0.2070 1.0369 0.048 Uiso 1 1 calc R . . H11C H 0.4167 0.2687 1.0662 0.048 Uiso 1 1 calc R . . C48 C 0.4924(7) 0.3933(3) 1.0647(5) 0.0434(18) Uani 1 1 d . . . H48 H 0.4332 0.3859 1.0211 0.052 Uiso 1 1 calc R . . C45 C 0.6624(8) 0.4138(4) 1.1943(5) 0.058(2) Uani 1 1 d . . . H45 H 0.7205 0.4214 1.2389 0.070 Uiso 1 1 calc R . . C12 C 0.6433(6) 0.2498(3) 1.1527(4) 0.0332(14) Uani 1 1 d . . . H12A H 0.6158 0.2392 1.2068 0.040 Uiso 1 1 calc R . . H12B H 0.6349 0.2899 1.1439 0.040 Uiso 1 1 calc R . . H12C H 0.7194 0.2400 1.1571 0.040 Uiso 1 1 calc R . . O1 O 0.4154(3) 0.30491(18) 0.8976(3) 0.0329(10) Uani 1 1 d . . . C1 C 0.5058(5) 0.2951(2) 0.8928(4) 0.0226(12) Uani 1 1 d . . . C18 C 0.6575(6) 0.1071(3) 1.0559(5) 0.0369(16) Uani 1 1 d . . . H18 H 0.6906 0.1208 1.0086 0.044 Uiso 1 1 calc R . . B7 B 0.8190(6) 0.3367(3) 0.8956(5) 0.0303(17) Uani 1 1 d . . . H7 H 0.8453 0.3808 0.9055 0.036 Uiso 1 1 calc R . . B3 B 0.7419(5) 0.2985(3) 0.9728(5) 0.0276(15) Uani 1 1 d . . . H3 H 0.7184 0.3193 1.0323 0.033 Uiso 1 1 calc R . . B11 B 0.7848(6) 0.3063(3) 0.7889(5) 0.0277(15) Uani 1 1 d . . . H11 H 0.7874 0.3312 0.7279 0.033 Uiso 1 1 calc R . . C28 C 0.3851(8) 0.1030(3) 0.9471(5) 0.053(2) Uani 1 1 d . . . H28 H 0.4491 0.0817 0.9582 0.064 Uiso 1 1 calc R . . C17 C 0.6759(7) 0.0527(3) 1.0847(6) 0.052(2) Uani 1 1 d . . . H17 H 0.7219 0.0296 1.0567 0.063 Uiso 1 1 calc R . . C21 C 0.5524(6) 0.1024(3) 0.8140(6) 0.0462(19) Uani 1 1 d . . . H21A H 0.4957 0.0801 0.7808 0.055 Uiso 1 1 calc R . . H21B H 0.5811 0.0827 0.8677 0.055 Uiso 1 1 calc R . . H21C H 0.6101 0.1087 0.7785 0.055 Uiso 1 1 calc R . . C36 C 0.6453(10) 0.5328(3) 0.6272(6) 0.065(3) Uani 1 1 d . . . H36 H 0.6663 0.5682 0.6087 0.078 Uiso 1 1 calc R . . C35 C 0.5417(10) 0.5162(3) 0.6092(6) 0.069(3) Uani 1 1 d . . . H35 H 0.4903 0.5404 0.5785 0.083 Uiso 1 1 calc R . . C16 C 0.6290(9) 0.0325(4) 1.1520(6) 0.066(3) Uani 1 1 d . . . H16 H 0.6421 -0.0046 1.1710 0.079 Uiso 1 1 calc R . . C24 C 0.2869(6) 0.1788(4) 0.8752(6) 0.058(2) Uani 1 1 d . . . H24 H 0.2834 0.2098 0.8370 0.069 Uiso 1 1 calc R . . B6 B 0.6873(5) 0.2475(3) 0.7946(4) 0.0228(13) Uani 1 1 d . . . H6 H 0.6285 0.2350 0.7368 0.027 Uiso 1 1 calc R . . C27 C 0.2977(11) 0.0887(5) 0.9868(7) 0.094(5) Uani 1 1 d . . . H27 H 0.3019 0.0577 1.0251 0.112 Uiso 1 1 calc R . . C25 C 0.1973(8) 0.1641(6) 0.9155(10) 0.099(5) Uani 1 1 d . . . H25 H 0.1327 0.1849 0.9045 0.119 Uiso 1 1 calc R . . C26 C 0.2049(13) 0.1188(8) 0.9716(11) 0.133(9) Uani 1 1 d . . . H26 H 0.1451 0.1086 0.9997 0.160 Uiso 1 1 calc R . . Cl3 Cl 0.5129(3) -0.0137(2) 1.4108(3) 0.1288(15) Uani 1 1 d . . . Cl1 Cl 0.1965(2) 0.38299(18) 0.9040(2) 0.1119(14) Uani 1 1 d . . . Cl2 Cl 0.1955(3) 0.3410(2) 1.0797(2) 0.1159(14) Uani 1 1 d . . . C50 C 0.1797(15) 0.3191(8) 0.9663(12) 0.054(4) Uani 0.50 1 d P A 1 H50A H 0.1077 0.3029 0.9488 0.065 Uiso 0.50 1 calc PR A 1 H50B H 0.2347 0.2913 0.9568 0.065 Uiso 0.50 1 calc PR A 1 C51 C 0.124(2) 0.3640(13) 0.9828(15) 0.096(9) Uani 0.50 1 d P A 2 H51A H 0.0742 0.3342 0.9593 0.116 Uiso 0.50 1 calc PR A 2 H51B H 0.0799 0.3961 0.9961 0.116 Uiso 0.50 1 calc PR A 2 C53 C 0.4711(16) -0.0443(9) 1.4910(17) 0.080(7) Uani 0.50 1 d P . . H53A H 0.5150 -0.0775 1.5085 0.096 Uiso 0.50 1 calc PR . . H53B H 0.3952 -0.0556 1.4758 0.096 Uiso 0.50 1 calc PR . . 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 Pt2 0.02672(14) 0.01848(14) 0.02189(15) 0.00000(8) 0.00375(10) -0.00223(8) Pt1 0.02418(14) 0.01828(14) 0.02270(15) 0.00017(9) 0.00623(10) 0.00107(8) P4 0.0380(9) 0.0216(8) 0.0301(9) -0.0051(7) 0.0038(7) -0.0035(7) P3 0.0358(8) 0.0198(8) 0.0248(8) 0.0019(6) 0.0018(6) -0.0032(6) P2 0.0317(8) 0.0196(8) 0.0264(9) -0.0030(6) 0.0078(7) -0.0022(6) P1 0.0341(8) 0.0238(8) 0.0225(8) -0.0005(7) 0.0093(6) -0.0013(7) B4 0.020(3) 0.034(4) 0.036(4) 0.012(3) 0.005(3) 0.010(3) C44 0.058(5) 0.040(4) 0.038(4) -0.012(3) -0.006(3) 0.016(4) C41 0.061(5) 0.027(4) 0.027(4) -0.003(3) 0.009(3) 0.007(3) C22 0.052(5) 0.054(5) 0.042(5) 0.006(4) -0.011(4) -0.022(4) B9 0.027(4) 0.040(4) 0.043(5) 0.002(4) 0.011(3) 0.008(3) C31 0.038(4) 0.033(4) 0.031(4) 0.004(3) -0.005(3) -0.002(3) C37 0.082(6) 0.043(5) 0.059(6) 0.005(4) 0.020(5) -0.025(5) C38 0.056(5) 0.037(4) 0.048(5) 0.001(4) 0.008(4) -0.016(4) C23 0.038(4) 0.035(4) 0.035(4) -0.014(3) 0.015(3) -0.016(3) C42 0.074(6) 0.037(4) 0.062(6) -0.019(4) 0.023(5) -0.022(4) C14 0.103(7) 0.033(4) 0.032(4) -0.004(3) 0.014(4) -0.019(4) B10 0.028(4) 0.042(5) 0.026(4) 0.004(3) 0.005(3) 0.001(3) C33 0.054(4) 0.025(3) 0.018(3) 0.001(3) 0.001(3) -0.005(3) B12 0.026(4) 0.046(5) 0.035(4) 0.011(4) 0.007(3) -0.002(3) C47 0.079(6) 0.048(5) 0.041(5) 0.002(4) 0.023(4) 0.020(4) B5 0.032(4) 0.027(4) 0.038(4) 0.007(3) 0.011(3) 0.004(3) C15 0.128(9) 0.041(5) 0.040(5) 0.014(4) 0.017(5) -0.032(6) C34 0.071(5) 0.026(4) 0.046(4) 0.012(3) -0.001(4) 0.003(4) C32 0.054(4) 0.031(4) 0.020(3) 0.005(3) -0.003(3) 0.001(3) C46 0.109(8) 0.055(6) 0.032(5) 0.000(4) 0.015(5) 0.029(6) B8 0.026(4) 0.045(5) 0.033(4) 0.001(4) 0.001(3) -0.002(3) C43 0.049(4) 0.026(3) 0.032(4) -0.002(3) -0.003(3) 0.010(3) C13 0.051(4) 0.032(4) 0.026(3) 0.003(3) 0.005(3) -0.002(3) C11 0.039(4) 0.050(5) 0.033(4) -0.008(3) 0.016(3) -0.003(3) C48 0.060(5) 0.030(4) 0.041(4) -0.001(3) 0.010(4) 0.006(3) C45 0.083(6) 0.047(5) 0.036(4) -0.009(4) -0.019(4) 0.022(5) C12 0.046(4) 0.029(3) 0.025(3) 0.000(3) 0.005(3) -0.005(3) O1 0.029(2) 0.026(2) 0.044(3) 0.000(2) 0.006(2) 0.0027(19) C1 0.032(3) 0.021(3) 0.016(3) -0.004(2) 0.004(2) -0.001(2) C18 0.046(4) 0.025(3) 0.038(4) 0.004(3) 0.003(3) 0.001(3) B7 0.023(3) 0.036(4) 0.031(4) -0.001(3) -0.001(3) -0.008(3) B3 0.022(3) 0.029(4) 0.031(4) 0.005(3) 0.002(3) -0.003(3) B11 0.033(4) 0.024(4) 0.027(4) 0.001(3) 0.008(3) 0.001(3) C28 0.081(6) 0.042(4) 0.043(5) -0.017(4) 0.030(4) -0.033(4) C17 0.064(5) 0.019(4) 0.070(6) -0.001(4) -0.006(4) 0.001(3) C21 0.045(4) 0.038(4) 0.058(5) -0.015(4) 0.016(4) 0.003(3) C36 0.123(9) 0.027(4) 0.046(5) 0.005(4) 0.020(6) -0.022(5) C35 0.134(10) 0.024(4) 0.050(5) 0.008(4) 0.012(6) 0.009(5) C16 0.107(8) 0.031(4) 0.053(6) 0.011(4) -0.011(5) -0.015(5) C24 0.034(4) 0.074(6) 0.066(6) -0.041(5) 0.011(4) -0.008(4) B6 0.033(3) 0.020(3) 0.017(3) -0.003(3) 0.010(3) 0.002(3) C27 0.136(11) 0.080(8) 0.082(8) -0.047(6) 0.077(8) -0.080(8) C25 0.037(5) 0.133(12) 0.133(12) -0.099(10) 0.035(6) -0.028(6) C26 0.114(11) 0.177(16) 0.133(13) -0.125(12) 0.101(11) -0.117(12) Cl3 0.116(3) 0.150(4) 0.116(3) 0.054(3) 0.001(2) -0.023(3) Cl1 0.0575(15) 0.180(4) 0.104(2) 0.073(3) 0.0308(16) 0.0258(19) Cl2 0.086(2) 0.185(4) 0.071(2) 0.041(2) -0.0090(16) -0.026(2) C50 0.049(10) 0.068(12) 0.047(10) 0.007(9) 0.014(8) 0.002(9) C51 0.076(15) 0.15(3) 0.064(14) 0.023(16) -0.003(12) -0.052(16) C53 0.045(10) 0.067(13) 0.12(2) -0.008(13) -0.007(11) 0.002(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 Pt2 C1 2.106(6) . ? Pt2 B11 2.261(7) . ? Pt2 B7 2.271(7) . ? Pt2 B3 2.298(7) . ? Pt2 P3 2.3331(17) . ? Pt2 P4 2.3440(17) . ? Pt2 B6 2.348(7) . ? Pt2 Pt1 2.7487(3) . ? Pt1 C1 2.098(6) . ? Pt1 B5 2.255(7) . ? Pt1 B4 2.264(7) . ? Pt1 B6 2.305(6) . ? Pt1 B3 2.332(7) . ? Pt1 P1 2.3402(16) . ? Pt1 P2 2.3516(17) . ? P4 C41 1.810(8) . ? P4 C42 1.815(8) . ? P4 C43 1.835(7) . ? P3 C32 1.815(7) . ? P3 C33 1.833(7) . ? P3 C31 1.835(7) . ? P2 C22 1.804(8) . ? P2 C21 1.805(7) . ? P2 C23 1.819(6) . ? P1 C12 1.807(7) . ? P1 C11 1.827(7) . ? P1 C13 1.837(7) . ? B4 B8 1.791(11) . ? B4 B9 1.796(10) . ? B4 B5 1.822(12) . ? B4 B3 1.870(10) . ? B4 H4 1.1200 . ? C44 C43 1.384(10) . ? C44 C45 1.413(12) . ? C44 H44 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? B9 B12 1.765(12) . ? B9 B5 1.777(11) . ? B9 B10 1.783(12) . ? B9 B8 1.783(12) . ? B9 H9 1.1200 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C37 C36 1.369(14) . ? C37 C38 1.396(11) . ? C37 H37 0.9500 . ? C38 C33 1.394(10) . ? C38 H38 0.9500 . ? C23 C28 1.374(11) . ? C23 C24 1.395(11) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C14 C15 1.382(12) . ? C14 C13 1.392(10) . ? C14 H14 0.9500 . ? B10 B6 1.775(10) . ? B10 B12 1.783(12) . ? B10 B5 1.794(10) . ? B10 B11 1.801(11) . ? B10 H10 1.1200 . ? C33 C34 1.374(10) . ? B12 B11 1.769(11) . ? B12 B8 1.776(11) . ? B12 B7 1.783(11) . ? B12 H12 1.1200 . ? C47 C46 1.355(14) . ? C47 C48 1.388(11) . ? C47 H47 0.9500 . ? B5 B6 1.877(11) . ? B5 H5 1.1200 . ? C15 C16 1.393(14) . ? C15 H15 0.9500 . ? C34 C35 1.402(11) . ? C34 H34 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C46 C45 1.387(14) . ? C46 H46 0.9500 . ? B8 B7 1.766(11) . ? B8 B3 1.771(10) . ? B8 H8 1.1200 . ? C43 C48 1.401(11) . ? C13 C18 1.399(10) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C48 H48 0.9500 . ? C45 H45 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O1 C1 1.174(7) . ? C18 C17 1.393(10) . ? C18 H18 0.9500 . ? B7 B11 1.798(11) . ? B7 B3 1.877(10) . ? B7 H7 1.1200 . ? B3 H3 1.1200 . ? B11 B6 1.886(10) . ? B11 H11 1.1200 . ? C28 C27 1.374(12) . ? C28 H28 0.9500 . ? C17 C16 1.353(13) . ? C17 H17 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C36 C35 1.355(15) . ? C36 H36 0.9500 . ? C35 H35 0.9500 . ? C16 H16 0.9500 . ? C24 C25 1.405(14) . ? C24 H24 0.9500 . ? B6 H6 1.1200 . ? C27 C26 1.37(2) . ? C27 H27 0.9500 . ? C25 C26 1.39(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Cl3 C53 1.59(3) . ? Cl3 C53 2.05(2) 3_658 ? Cl1 C51 1.68(2) . ? Cl1 C50 1.844(19) . ? Cl2 C51 1.73(2) . ? Cl2 C50 1.811(19) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C53 Cl3 2.05(2) 3_658 ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 C1 Pt2 B11 137.0(2) . . ? C1 Pt2 B7 136.3(3) . . ? B11 Pt2 B7 46.8(3) . . ? C1 Pt2 B3 87.9(2) . . ? B11 Pt2 B3 81.1(3) . . ? B7 Pt2 B3 48.5(3) . . ? C1 Pt2 P3 93.85(17) . . ? B11 Pt2 P3 92.7(2) . . ? B7 Pt2 P3 128.9(2) . . ? B3 Pt2 P3 172.5(2) . . ? C1 Pt2 P4 90.24(16) . . ? B11 Pt2 P4 131.19(19) . . ? B7 Pt2 P4 93.6(2) . . ? B3 Pt2 P4 91.4(2) . . ? P3 Pt2 P4 95.87(6) . . ? C1 Pt2 B6 89.0(2) . . ? B11 Pt2 B6 48.3(2) . . ? B7 Pt2 B6 81.5(3) . . ? B3 Pt2 B6 80.6(3) . . ? P3 Pt2 B6 92.17(18) . . ? P4 Pt2 B6 171.96(18) . . ? C1 Pt2 Pt1 49.05(16) . . ? B11 Pt2 Pt1 92.62(19) . . ? B7 Pt2 Pt1 93.5(2) . . ? B3 Pt2 Pt1 54.16(18) . . ? P3 Pt2 Pt1 122.39(4) . . ? P4 Pt2 Pt1 121.42(4) . . ? B6 Pt2 Pt1 53.06(16) . . ? C1 Pt1 B5 138.6(2) . . ? C1 Pt1 B4 135.1(3) . . ? B5 Pt1 B4 47.6(3) . . ? C1 Pt1 B6 90.4(2) . . ? B5 Pt1 B6 48.6(3) . . ? B4 Pt1 B6 82.0(3) . . ? C1 Pt1 B3 87.2(2) . . ? B5 Pt1 B3 81.6(3) . . ? B4 Pt1 B3 48.0(3) . . ? B6 Pt1 B3 80.8(3) . . ? C1 Pt1 P1 94.70(16) . . ? B5 Pt1 P1 125.5(2) . . ? B4 Pt1 P1 90.2(2) . . ? B6 Pt1 P1 172.22(18) . . ? B3 Pt1 P1 93.60(19) . . ? C1 Pt1 P2 90.22(17) . . ? B5 Pt1 P2 92.7(2) . . ? B4 Pt1 P2 133.1(2) . . ? B6 Pt1 P2 87.39(18) . . ? B3 Pt1 P2 167.85(19) . . ? P1 Pt1 P2 98.44(6) . . ? C1 Pt1 Pt2 49.29(16) . . ? B5 Pt1 Pt2 93.86(19) . . ? B4 Pt1 Pt2 92.85(19) . . ? B6 Pt1 Pt2 54.52(17) . . ? B3 Pt1 Pt2 53.02(18) . . ? P1 Pt1 Pt2 125.74(4) . . ? P2 Pt1 Pt2 117.22(4) . . ? C41 P4 C42 101.4(4) . . ? C41 P4 C43 101.2(3) . . ? C42 P4 C43 103.1(4) . . ? C41 P4 Pt2 115.6(2) . . ? C42 P4 Pt2 116.6(3) . . ? C43 P4 Pt2 116.6(2) . . ? C32 P3 C33 102.2(3) . . ? C32 P3 C31 100.2(3) . . ? C33 P3 C31 104.4(3) . . ? C32 P3 Pt2 117.8(2) . . ? C33 P3 Pt2 113.0(2) . . ? C31 P3 Pt2 117.1(2) . . ? C22 P2 C21 100.1(4) . . ? C22 P2 C23 101.7(4) . . ? C21 P2 C23 102.5(3) . . ? C22 P2 Pt1 116.6(3) . . ? C21 P2 Pt1 116.9(3) . . ? C23 P2 Pt1 116.5(2) . . ? C12 P1 C11 101.1(3) . . ? C12 P1 C13 100.7(3) . . ? C11 P1 C13 104.7(3) . . ? C12 P1 Pt1 117.5(2) . . ? C11 P1 Pt1 117.2(3) . . ? C13 P1 Pt1 113.5(2) . . ? B8 B4 B9 59.6(4) . . ? B8 B4 B5 106.3(5) . . ? B9 B4 B5 58.8(4) . . ? B8 B4 B3 57.8(4) . . ? B9 B4 B3 106.4(5) . . ? B5 B4 B3 108.5(5) . . ? B8 B4 Pt1 119.1(4) . . ? B9 B4 Pt1 118.9(5) . . ? B5 B4 Pt1 65.9(3) . . ? B3 B4 Pt1 67.9(3) . . ? B8 B4 H4 121.3 . . ? B9 B4 H4 121.0 . . ? B5 B4 H4 122.9 . . ? B3 B4 H4 122.4 . . ? Pt1 B4 H4 109.4 . . ? C43 C44 C45 120.1(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? P4 C41 H41A 109.5 . . ? P4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? B12 B9 B5 110.6(6) . . ? B12 B9 B10 60.3(5) . . ? B5 B9 B10 60.5(5) . . ? B12 B9 B8 60.1(5) . . ? B5 B9 B8 108.7(5) . . ? B10 B9 B8 106.8(6) . . ? B12 B9 B4 110.2(5) . . ? B5 B9 B4 61.3(4) . . ? B10 B9 B4 109.1(5) . . ? B8 B9 B4 60.0(4) . . ? B12 B9 H9 120.2 . . ? B5 B9 H9 120.2 . . ? B10 B9 H9 122.1 . . ? B8 B9 H9 122.6 . . ? B4 B9 H9 120.4 . . ? P3 C31 H31A 109.5 . . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C36 C37 C38 120.6(9) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C33 C38 C37 120.0(8) . . ? C33 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C28 C23 C24 119.6(7) . . ? C28 C23 P2 120.9(6) . . ? C24 C23 P2 119.5(6) . . ? P4 C42 H42A 109.5 . . ? P4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C15 C14 C13 119.5(9) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? B6 B10 B9 110.7(5) . . ? B6 B10 B12 111.0(5) . . ? B9 B10 B12 59.3(5) . . ? B6 B10 B5 63.5(4) . . ? B9 B10 B5 59.6(4) . . ? B12 B10 B5 108.9(6) . . ? B6 B10 B11 63.7(4) . . ? B9 B10 B11 108.0(6) . . ? B12 B10 B11 59.1(4) . . ? B5 B10 B11 113.3(5) . . ? B6 B10 H10 117.9 . . ? B9 B10 H10 122.5 . . ? B12 B10 H10 122.1 . . ? B5 B10 H10 119.3 . . ? B11 B10 H10 119.7 . . ? C34 C33 C38 118.9(7) . . ? C34 C33 P3 122.2(6) . . ? C38 C33 P3 118.9(6) . . ? B9 B12 B11 110.3(6) . . ? B9 B12 B8 60.5(5) . . ? B11 B12 B8 107.6(5) . . ? B9 B12 B7 110.3(5) . . ? B11 B12 B7 60.8(4) . . ? B8 B12 B7 59.5(5) . . ? B9 B12 B10 60.3(5) . . ? B11 B12 B10 60.9(4) . . ? B8 B12 B10 107.1(5) . . ? B7 B12 B10 109.5(5) . . ? B9 B12 H12 120.0 . . ? B11 B12 H12 120.8 . . ? B8 B12 H12 122.9 . . ? B7 B12 H12 120.5 . . ? B10 B12 H12 121.5 . . ? C46 C47 C48 121.7(9) . . ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 . . ? B9 B5 B10 59.9(4) . . ? B9 B5 B4 59.9(4) . . ? B10 B5 B4 107.4(5) . . ? B9 B5 B6 106.5(5) . . ? B10 B5 B6 57.8(4) . . ? B4 B5 B6 108.3(5) . . ? B9 B5 Pt1 120.3(5) . . ? B10 B5 Pt1 119.1(5) . . ? B4 B5 Pt1 66.5(3) . . ? B6 B5 Pt1 67.1(3) . . ? B9 B5 H5 120.1 . . ? B10 B5 H5 121.0 . . ? B4 B5 H5 122.1 . . ? B6 B5 H5 123.1 . . ? Pt1 B5 H5 109.2 . . ? C14 C15 C16 120.8(8) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C33 C34 C35 119.8(9) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C47 C46 C45 119.4(8) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? B7 B8 B3 64.1(4) . . ? B7 B8 B12 60.4(5) . . ? B3 B8 B12 111.7(6) . . ? B7 B8 B9 110.2(6) . . ? B3 B8 B9 111.4(6) . . ? B12 B8 B9 59.5(5) . . ? B7 B8 B4 115.1(5) . . ? B3 B8 B4 63.3(4) . . ? B12 B8 B4 109.9(6) . . ? B9 B8 B4 60.3(5) . . ? B7 B8 H8 118.1 . . ? B3 B8 H8 117.8 . . ? B12 B8 H8 121.6 . . ? B9 B8 H8 121.7 . . ? B4 B8 H8 118.6 . . ? C44 C43 C48 118.7(7) . . ? C44 C43 P4 121.9(6) . . ? C48 C43 P4 119.4(6) . . ? C14 C13 C18 119.3(7) . . ? C14 C13 P1 121.0(6) . . ? C18 C13 P1 119.6(5) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C47 C48 C43 120.0(8) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C46 C45 C44 120.1(8) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C1 Pt1 139.2(5) . . ? O1 C1 Pt2 139.2(5) . . ? Pt1 C1 Pt2 81.7(2) . . ? C17 C18 C13 119.8(7) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? B8 B7 B12 60.0(4) . . ? B8 B7 B11 106.7(5) . . ? B12 B7 B11 59.2(4) . . ? B8 B7 B3 58.1(4) . . ? B12 B7 B3 106.6(5) . . ? B11 B7 B3 107.6(5) . . ? B8 B7 Pt2 118.6(4) . . ? B12 B7 Pt2 119.6(5) . . ? B11 B7 Pt2 66.3(3) . . ? B3 B7 Pt2 66.5(3) . . ? B8 B7 H7 121.1 . . ? B12 B7 H7 120.2 . . ? B11 B7 H7 122.8 . . ? B3 B7 H7 123.2 . . ? Pt2 B7 H7 109.8 . . ? B8 B3 B4 58.9(4) . . ? B8 B3 B7 57.8(4) . . ? B4 B3 B7 106.5(5) . . ? B8 B3 Pt2 117.1(4) . . ? B4 B3 Pt2 121.8(5) . . ? B7 B3 Pt2 65.0(3) . . ? B8 B3 Pt1 116.7(5) . . ? B4 B3 Pt1 64.1(3) . . ? B7 B3 Pt1 121.1(4) . . ? Pt2 B3 Pt1 72.8(2) . . ? B8 B3 H3 121.0 . . ? B4 B3 H3 120.9 . . ? B7 B3 H3 121.3 . . ? Pt2 B3 H3 109.3 . . ? Pt1 B3 H3 110.2 . . ? B12 B11 B7 60.0(4) . . ? B12 B11 B10 59.9(4) . . ? B7 B11 B10 108.0(5) . . ? B12 B11 B6 106.7(5) . . ? B7 B11 B6 109.8(5) . . ? B10 B11 B6 57.5(4) . . ? B12 B11 Pt2 120.8(4) . . ? B7 B11 Pt2 66.9(3) . . ? B10 B11 Pt2 119.9(4) . . ? B6 B11 Pt2 68.3(3) . . ? B12 B11 H11 120.2 . . ? B7 B11 H11 121.4 . . ? B10 B11 H11 121.0 . . ? B6 B11 H11 122.4 . . ? Pt2 B11 H11 108.3 . . ? C27 C28 C23 120.6(11) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C16 C17 C18 120.8(8) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C35 C36 C37 119.3(8) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C36 C35 C34 121.3(9) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C17 C16 C15 119.7(8) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C23 C24 C25 119.8(11) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? B10 B6 B5 58.8(4) . . ? B10 B6 B11 58.8(4) . . ? B5 B6 B11 105.9(5) . . ? B10 B6 Pt1 117.5(4) . . ? B5 B6 Pt1 64.3(3) . . ? B11 B6 Pt1 120.2(4) . . ? B10 B6 Pt2 116.8(4) . . ? B5 B6 Pt2 120.2(4) . . ? B11 B6 Pt2 63.5(3) . . ? Pt1 B6 Pt2 72.42(18) . . ? B10 B6 H6 120.0 . . ? B5 B6 H6 121.5 . . ? B11 B6 H6 121.9 . . ? Pt1 B6 H6 110.1 . . ? Pt2 B6 H6 110.7 . . ? C26 C27 C28 120.6(13) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C26 C25 C24 118.9(12) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C27 C26 C25 120.5(9) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C53 Cl3 C53 75.5(11) . 3_658 ? C51 Cl1 C50 44.1(12) . . ? C51 Cl2 C50 44.2(11) . . ? Cl2 C50 Cl1 104.8(10) . . ? Cl2 C50 H50A 110.8 . . ? Cl1 C50 H50A 110.8 . . ? Cl2 C50 H50B 110.8 . . ? Cl1 C50 H50B 110.8 . . ? H50A C50 H50B 108.9 . . ? Cl1 C51 Cl2 116.3(15) . . ? Cl1 C51 H51A 108.2 . . ? Cl2 C51 H51A 108.2 . . ? Cl1 C51 H51B 108.2 . . ? Cl2 C51 H51B 108.2 . . ? H51A C51 H51B 107.4 . . ? Cl3 C53 Cl3 104.5(11) . 3_658 ? Cl3 C53 H53A 110.9 . . ? Cl3 C53 H53A 110.9 3_658 . ? Cl3 C53 H53B 110.9 . . ? Cl3 C53 H53B 110.9 3_658 . ? H53A C53 H53B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.818 _refine_diff_density_min -3.266 _refine_diff_density_rms 0.301 data_jb309 _database_code_depnum_ccdc_archive 'CCDC 254028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H54 B10 O2 P4 Pt2 S, C6 H14' _chemical_formula_sum 'C38 H68 B10 O2 P4 Pt2 S' _chemical_formula_weight 1211.14 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' O O 0.0106 0.0060 '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' 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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 23.8520(2) _cell_length_b 10.84800(10) _cell_length_c 17.71000(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4582.40(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 95436 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 6.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.161 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38. ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; phi and omega scans to fill the asymmetric unit ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 100727 _diffrn_reflns_av_R_equivalents 0.1633 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8981 _reflns_number_gt 8662 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-III _computing_publication_material 'local program' _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^)+(0.0954P)^2^+15.2827P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(9) _refine_ls_number_reflns 8981 _refine_ls_number_parameters 485 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.041 _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 Pt2 Pt 0.462213(11) 0.20435(3) 0.22430(2) 0.02036(10) Uani 1 1 d . . . Pt1 Pt 0.376483(12) 0.04655(3) 0.27597(2) 0.02099(10) Uani 1 1 d . . . P1 P 0.37871(10) -0.0392(2) 0.39980(16) 0.0273(6) Uani 1 1 d . . . P3 P 0.45809(9) 0.3993(2) 0.16738(14) 0.0236(5) Uani 1 1 d . . . S1 S 0.38871(9) 0.2593(2) 0.30640(12) 0.0224(4) Uani 1 1 d . . . P4 P 0.53415(8) 0.2535(2) 0.31211(13) 0.0238(5) Uani 1 1 d . . . P2 P 0.27813(9) 0.0630(2) 0.27456(17) 0.0284(4) Uani 1 1 d . . . O1 O 0.3485(2) 0.3409(6) 0.2703(4) 0.0313(13) Uani 1 1 d . . . C32 C 0.4410(4) 0.5327(8) 0.2264(6) 0.0297(18) Uani 1 1 d . . . H32A H 0.4407 0.6074 0.1953 0.036 Uiso 1 1 calc R . . H32B H 0.4692 0.5412 0.2663 0.036 Uiso 1 1 calc R . . H32C H 0.4039 0.5210 0.2492 0.036 Uiso 1 1 calc R . . C33 C 0.5228(4) 0.4417(8) 0.1188(5) 0.0255(18) Uani 1 1 d . . . C11 C 0.4410(4) -0.1241(10) 0.4273(6) 0.031(2) Uani 1 1 d . . . H11A H 0.4367 -0.1542 0.4791 0.038 Uiso 1 1 calc R . . H11B H 0.4738 -0.0697 0.4245 0.038 Uiso 1 1 calc R . . H11C H 0.4463 -0.1942 0.3931 0.038 Uiso 1 1 calc R . . O2 O 0.4027(3) 0.2950(6) 0.3837(4) 0.0308(15) Uani 1 1 d . . . C43 C 0.5445(4) 0.4166(10) 0.3344(6) 0.0270(19) Uani 1 1 d . . . C23 C 0.2418(4) 0.1271(9) 0.3561(6) 0.031(2) Uani 1 1 d . . . C13 C 0.3238(4) -0.1535(11) 0.4193(6) 0.037(2) Uani 1 1 d . . . C44 C 0.5152(4) 0.4703(9) 0.3948(5) 0.029(2) Uani 1 1 d . . . H44 H 0.4904 0.4216 0.4244 0.035 Uiso 1 1 calc R . . C42 C 0.6024(4) 0.2062(9) 0.2853(7) 0.039(2) Uani 1 1 d . . . H42A H 0.6293 0.2300 0.3246 0.047 Uiso 1 1 calc R . . H42B H 0.6127 0.2458 0.2376 0.047 Uiso 1 1 calc R . . H42C H 0.6031 0.1164 0.2790 0.047 Uiso 1 1 calc R . . C21 C 0.2505(4) 0.1552(12) 0.1980(6) 0.037(3) Uani 1 1 d . . . H21A H 0.2095 0.1576 0.2013 0.045 Uiso 1 1 calc R . . H21B H 0.2617 0.1188 0.1496 0.045 Uiso 1 1 calc R . . H21C H 0.2654 0.2392 0.2016 0.045 Uiso 1 1 calc R . . C31 C 0.4050(4) 0.4178(10) 0.0950(6) 0.031(2) Uani 1 1 d . . . H31A H 0.4066 0.5018 0.0748 0.038 Uiso 1 1 calc R . . H31B H 0.3678 0.4029 0.1169 0.038 Uiso 1 1 calc R . . H31C H 0.4118 0.3587 0.0542 0.038 Uiso 1 1 calc R . . C45 C 0.5223(5) 0.5938(10) 0.4113(6) 0.034(2) Uani 1 1 d . . . H45 H 0.5037 0.6287 0.4536 0.041 Uiso 1 1 calc R . . C46 C 0.5564(5) 0.6672(10) 0.3666(7) 0.040(2) Uani 1 1 d . . . H46 H 0.5602 0.7526 0.3774 0.048 Uiso 1 1 calc R . . C34 C 0.5639(4) 0.3572(9) 0.1030(5) 0.030(2) Uani 1 1 d . . . H34 H 0.5588 0.2739 0.1180 0.036 Uiso 1 1 calc R . . C35 C 0.6128(5) 0.3902(11) 0.0658(6) 0.038(2) Uani 1 1 d . . . H35 H 0.6408 0.3302 0.0556 0.046 Uiso 1 1 calc R . . C48 C 0.5793(4) 0.4916(9) 0.2898(5) 0.030(2) Uani 1 1 d . . . H48 H 0.5991 0.4572 0.2483 0.036 Uiso 1 1 calc R . . C37 C 0.5785(5) 0.6005(11) 0.0591(6) 0.044(3) Uani 1 1 d . . . H37 H 0.5832 0.6837 0.0437 0.052 Uiso 1 1 calc R . . C38 C 0.5306(5) 0.5651(10) 0.0972(7) 0.035(2) Uani 1 1 d . . . H38 H 0.5027 0.6246 0.1088 0.042 Uiso 1 1 calc R . . C36 C 0.6205(5) 0.5128(13) 0.0433(7) 0.045(3) Uani 1 1 d . . . H36 H 0.6538 0.5366 0.0176 0.054 Uiso 1 1 calc R . . C12 C 0.3711(5) 0.0705(12) 0.4774(6) 0.040(3) Uani 1 1 d . . . H12A H 0.3725 0.0262 0.5256 0.048 Uiso 1 1 calc R . . H12B H 0.3351 0.1133 0.4728 0.048 Uiso 1 1 calc R . . H12C H 0.4017 0.1307 0.4754 0.048 Uiso 1 1 calc R . . C47 C 0.5846(4) 0.6158(9) 0.3065(6) 0.037(2) Uani 1 1 d . . . H47 H 0.6081 0.6662 0.2761 0.045 Uiso 1 1 calc R . . B4 B 0.4187(4) -0.1208(9) 0.2258(7) 0.0278(19) Uani 1 1 d . . . H4 H 0.4070 -0.2040 0.2597 0.033 Uiso 1 1 calc R . . C41 C 0.5282(5) 0.1838(11) 0.4049(6) 0.036(2) Uani 1 1 d . . . H41A H 0.5632 0.1963 0.4328 0.043 Uiso 1 1 calc R . . H41B H 0.5211 0.0953 0.3995 0.043 Uiso 1 1 calc R . . H41C H 0.4972 0.2221 0.4325 0.043 Uiso 1 1 calc R . . C22 C 0.2440(5) -0.0814(12) 0.2610(7) 0.048(3) Uani 1 1 d . . . H22A H 0.2033 -0.0692 0.2610 0.057 Uiso 1 1 calc R . . H22B H 0.2544 -0.1378 0.3019 0.057 Uiso 1 1 calc R . . H22C H 0.2557 -0.1167 0.2125 0.057 Uiso 1 1 calc R . . B7 B 0.5102(4) 0.0497(9) 0.1701(6) 0.024(2) Uani 1 1 d . . . H7 H 0.5558 0.0741 0.1691 0.029 Uiso 1 1 calc R . . B3 B 0.4714(4) 0.0007(9) 0.2585(6) 0.024(2) Uani 1 1 d . . . H3 H 0.4930 -0.0041 0.3146 0.028 Uiso 1 1 calc R . . C26 C 0.1828(5) 0.2377(13) 0.4759(7) 0.045(3) Uani 1 1 d . . . H26 H 0.1636 0.2727 0.5178 0.055 Uiso 1 1 calc R . . B12 B 0.4802(4) -0.0359(9) 0.0963(6) 0.024(2) Uani 1 1 d . . . H12 H 0.5070 -0.0652 0.0475 0.029 Uiso 1 1 calc R . . C27 C 0.1707(4) 0.1213(12) 0.4525(6) 0.041(2) Uani 1 1 d . . . H27 H 0.1411 0.0777 0.4765 0.049 Uiso 1 1 calc R . . B10 B 0.4098(4) 0.0096(10) 0.0836(6) 0.028(2) Uani 1 1 d . . . H10 H 0.3900 0.0147 0.0264 0.033 Uiso 1 1 calc R . . C15 C 0.2865(6) -0.3585(12) 0.4018(9) 0.059(3) Uani 1 1 d . . . H15 H 0.2877 -0.4366 0.3776 0.070 Uiso 1 1 calc R . . C16 C 0.2445(5) -0.3309(15) 0.4538(10) 0.062(4) Uani 1 1 d . . . H16 H 0.2167 -0.3908 0.4652 0.075 Uiso 1 1 calc R . . C25 C 0.2229(5) 0.3036(12) 0.4384(8) 0.049(3) Uani 1 1 d . . . H25 H 0.2298 0.3868 0.4523 0.059 Uiso 1 1 calc R . . C24 C 0.2537(5) 0.2507(12) 0.3804(7) 0.044(3) Uani 1 1 d . . . H24 H 0.2827 0.2964 0.3566 0.052 Uiso 1 1 calc R . . B9 B 0.4271(5) -0.1340(10) 0.1276(6) 0.026(2) Uani 1 1 d . . . H9 H 0.4194 -0.2246 0.0991 0.031 Uiso 1 1 calc R . . C18 C 0.2818(5) -0.1317(13) 0.4716(8) 0.050(3) Uani 1 1 d . . . H18 H 0.2797 -0.0545 0.4967 0.060 Uiso 1 1 calc R . . C14 C 0.3268(6) -0.2691(13) 0.3860(7) 0.050(3) Uani 1 1 d . . . H14 H 0.3566 -0.2874 0.3521 0.060 Uiso 1 1 calc R . . C28 C 0.1997(4) 0.0646(11) 0.3954(7) 0.036(2) Uani 1 1 d . . . H28 H 0.1910 -0.0182 0.3824 0.044 Uiso 1 1 calc R . . B11 B 0.4611(4) 0.1192(10) 0.1078(6) 0.023(2) Uani 1 1 d . . . H11 H 0.4742 0.1903 0.0654 0.028 Uiso 1 1 calc R . . C17 C 0.2430(6) -0.2224(14) 0.4871(10) 0.061(4) Uani 1 1 d . . . H17 H 0.2143 -0.2062 0.5230 0.073 Uiso 1 1 calc R . . B8 B 0.4870(4) -0.1076(9) 0.1855(5) 0.0224(19) Uani 1 1 d . . . H8 H 0.5187 -0.1809 0.1979 0.027 Uiso 1 1 calc R . . B5 B 0.3706(4) -0.0427(9) 0.1635(7) 0.023(2) Uani 1 1 d . . . H5 H 0.3261 -0.0735 0.1562 0.027 Uiso 1 1 calc R . . B6 B 0.3885(4) 0.1199(9) 0.1538(5) 0.0215(19) Uani 1 1 d . . . H6 H 0.3560 0.1917 0.1416 0.026 Uiso 1 1 calc R . . C1S C 0.6725(5) 0.8913(10) 0.2836(7) 0.043(2) Uiso 1 1 d D . . H1SA H 0.6547 0.9611 0.3094 0.052 Uiso 1 1 calc R . . H1SB H 0.7133 0.9003 0.2859 0.052 Uiso 1 1 calc R . . H1SC H 0.6615 0.8143 0.3084 0.052 Uiso 1 1 calc R . . C3S C 0.6732(6) 0.7979(12) 0.1474(9) 0.058(4) Uiso 1 1 d D . . H3S1 H 0.6698 0.7168 0.1726 0.070 Uiso 1 1 calc R . . H3S2 H 0.6452 0.7982 0.1061 0.070 Uiso 1 1 calc R . . C4S C 0.7115(7) 0.7984(17) 0.1218(12) 0.079(5) Uiso 1 1 d D . . H4S1 H 0.7033 0.8169 0.0682 0.094 Uiso 1 1 calc R . . H4S2 H 0.7237 0.7112 0.1228 0.094 Uiso 1 1 calc R . . C2S C 0.6539(9) 0.8886(19) 0.2020(10) 0.086(5) Uiso 1 1 d D . . H2S1 H 0.6125 0.8830 0.2027 0.104 Uiso 1 1 calc R . . H2S2 H 0.6632 0.9704 0.1807 0.104 Uiso 1 1 calc R . . C5S C 0.7595(11) 0.864(2) 0.1370(16) 0.113(8) Uiso 1 1 d D . . H5S1 H 0.7801 0.8650 0.0884 0.136 Uiso 1 1 calc R . . H5S2 H 0.7464 0.9496 0.1449 0.136 Uiso 1 1 calc R . . C6S C 0.7979(12) 0.848(3) 0.1874(19) 0.144(11) Uiso 1 1 d D . . H6S1 H 0.7859 0.7850 0.2233 0.216 Uiso 1 1 calc R . . H6S2 H 0.8043 0.9261 0.2143 0.216 Uiso 1 1 calc R . . H6S3 H 0.8328 0.8223 0.1629 0.216 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 Pt2 0.01720(16) 0.02401(17) 0.01987(16) 0.00021(14) 0.00014(13) 0.00066(10) Pt1 0.01729(16) 0.02419(17) 0.02148(16) -0.00054(14) 0.00011(12) -0.00010(11) P1 0.0257(14) 0.0322(15) 0.0240(13) 0.0037(10) 0.0008(9) -0.0006(9) P3 0.0236(11) 0.0231(11) 0.0240(11) 0.0026(9) -0.0003(8) 0.0013(8) S1 0.0195(9) 0.0236(10) 0.0241(9) -0.0036(8) 0.0019(8) -0.0002(8) P4 0.0173(10) 0.0308(13) 0.0234(11) -0.0014(10) -0.0048(8) -0.0018(9) P2 0.0203(10) 0.0364(11) 0.0285(10) -0.0035(11) -0.0009(11) -0.0011(8) O1 0.022(3) 0.032(3) 0.040(4) 0.004(3) 0.002(3) 0.005(3) C32 0.023(4) 0.033(4) 0.033(4) 0.008(4) 0.005(4) 0.005(3) C33 0.024(4) 0.030(5) 0.023(4) -0.004(4) -0.003(4) -0.005(4) C11 0.028(5) 0.035(5) 0.031(5) 0.004(4) 0.001(4) 0.002(4) O2 0.031(4) 0.036(4) 0.025(3) -0.009(3) 0.007(3) -0.004(3) C43 0.018(4) 0.037(5) 0.026(4) 0.005(4) -0.004(3) 0.007(4) C23 0.018(4) 0.028(5) 0.046(6) 0.001(4) -0.004(4) 0.000(4) C13 0.033(5) 0.042(6) 0.037(5) 0.008(5) -0.006(4) -0.001(4) C44 0.033(5) 0.033(5) 0.022(4) -0.001(4) -0.003(4) -0.004(4) C42 0.030(5) 0.041(6) 0.046(6) 0.000(5) 0.003(5) -0.003(4) C21 0.025(5) 0.057(7) 0.030(5) -0.002(4) -0.009(4) 0.008(5) C31 0.025(5) 0.033(5) 0.036(5) 0.005(4) -0.004(4) 0.003(4) C45 0.040(5) 0.032(5) 0.030(5) -0.005(4) 0.000(4) 0.005(4) C46 0.038(6) 0.030(5) 0.052(7) 0.002(5) -0.011(5) -0.001(5) C34 0.033(5) 0.032(5) 0.026(4) -0.001(4) -0.003(4) 0.000(4) C35 0.034(5) 0.043(6) 0.037(5) 0.001(5) 0.002(4) -0.009(4) C48 0.018(4) 0.040(5) 0.033(5) 0.003(4) -0.003(3) -0.006(4) C37 0.049(7) 0.044(6) 0.038(6) 0.007(5) 0.008(5) -0.011(5) C38 0.035(5) 0.032(5) 0.038(6) 0.010(4) 0.001(4) -0.001(4) C36 0.045(7) 0.048(7) 0.041(6) 0.002(6) 0.012(5) -0.018(5) C12 0.046(7) 0.044(6) 0.029(5) 0.003(5) 0.002(4) -0.008(5) C47 0.028(5) 0.035(5) 0.049(6) 0.003(4) -0.004(4) -0.006(4) B4 0.025(5) 0.028(4) 0.030(5) -0.013(5) -0.007(5) 0.002(4) C41 0.037(5) 0.037(5) 0.033(5) 0.004(4) -0.008(4) -0.006(4) C22 0.030(5) 0.052(6) 0.061(8) -0.027(6) 0.006(5) -0.015(5) B7 0.015(4) 0.034(5) 0.023(5) -0.004(4) -0.004(4) 0.002(4) B3 0.029(5) 0.018(4) 0.024(5) 0.004(4) 0.002(4) 0.013(4) C26 0.038(6) 0.057(7) 0.042(6) -0.009(6) 0.013(5) 0.007(6) B12 0.024(5) 0.024(5) 0.024(5) -0.004(4) 0.003(4) 0.002(4) C27 0.033(5) 0.056(7) 0.034(5) 0.001(5) 0.007(4) -0.005(5) B10 0.024(5) 0.036(5) 0.023(5) -0.006(4) -0.003(4) 0.007(4) C15 0.068(9) 0.034(6) 0.074(9) 0.006(6) -0.004(7) -0.012(6) C16 0.035(7) 0.058(8) 0.094(11) 0.027(8) 0.007(7) -0.010(6) C25 0.033(6) 0.055(8) 0.060(8) -0.018(6) 0.008(5) 0.003(5) C24 0.040(6) 0.048(6) 0.044(6) -0.010(5) 0.014(5) -0.012(5) B9 0.028(5) 0.029(5) 0.021(5) -0.004(4) 0.001(4) -0.011(4) C18 0.030(6) 0.057(7) 0.064(8) 0.028(6) 0.004(5) -0.001(5) C14 0.052(7) 0.051(7) 0.046(6) 0.010(6) -0.006(5) -0.010(6) C28 0.019(5) 0.043(6) 0.047(6) 0.007(5) 0.005(4) -0.001(4) B11 0.023(5) 0.020(5) 0.027(5) -0.005(4) -0.003(3) 0.003(3) C17 0.039(7) 0.059(8) 0.084(10) 0.028(8) 0.012(7) -0.001(6) B8 0.028(5) 0.021(5) 0.018(4) -0.003(4) 0.001(4) 0.005(4) B5 0.019(5) 0.022(5) 0.027(6) -0.003(4) -0.002(4) 0.002(3) B6 0.021(4) 0.023(5) 0.021(4) -0.002(4) -0.014(4) -0.008(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 Pt2 B7 2.247(10) . ? Pt2 B11 2.261(11) . ? Pt2 B3 2.301(9) . ? Pt2 B6 2.343(9) . ? Pt2 P3 2.345(2) . ? Pt2 S1 2.355(2) . ? Pt2 P4 2.376(2) . ? Pt2 Pt1 2.8194(4) . ? Pt1 B5 2.219(12) . ? Pt1 B4 2.258(10) . ? Pt1 B6 2.322(10) . ? Pt1 B3 2.339(10) . ? Pt1 P2 2.353(2) . ? Pt1 P1 2.383(3) . ? Pt1 S1 2.388(2) . ? P1 C11 1.815(10) . ? P1 C12 1.827(13) . ? P1 C13 1.836(11) . ? P3 C31 1.813(10) . ? P3 C33 1.826(10) . ? P3 C32 1.831(10) . ? S1 O1 1.454(7) . ? S1 O2 1.461(7) . ? P4 C42 1.772(11) . ? P4 C41 1.815(11) . ? P4 C43 1.829(11) . ? P2 C22 1.781(11) . ? P2 C21 1.809(11) . ? P2 C23 1.823(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.371(14) . ? C33 C38 1.405(14) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C43 C44 1.404(14) . ? C43 C48 1.405(13) . ? C23 C28 1.398(14) . ? C23 C24 1.437(16) . ? C13 C18 1.385(17) . ? C13 C14 1.387(19) . ? C44 C45 1.381(14) . ? C44 H44 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C45 C46 1.387(16) . ? C45 H45 0.9500 . ? C46 C47 1.377(16) . ? C46 H46 0.9500 . ? C34 C35 1.385(14) . ? C34 H34 0.9500 . ? C35 C36 1.401(18) . ? C35 H35 0.9500 . ? C48 C47 1.385(15) . ? C48 H48 0.9500 . ? C37 C38 1.382(15) . ? C37 C36 1.410(18) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C36 H36 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C47 H47 0.9500 . ? B4 B9 1.757(15) . ? B4 B8 1.785(15) . ? B4 B5 1.803(15) . ? B4 B3 1.912(14) . ? B4 H4 1.1200 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? B7 B12 1.756(14) . ? B7 B11 1.778(14) . ? B7 B8 1.814(14) . ? B7 B3 1.894(15) . ? B7 H7 1.1200 . ? B3 B8 1.786(13) . ? B3 H3 1.1200 . ? C26 C27 1.361(18) . ? C26 C25 1.366(19) . ? C26 H26 0.9500 . ? B12 B9 1.744(14) . ? B12 B11 1.755(14) . ? B12 B10 1.763(14) . ? B12 B8 1.768(14) . ? B12 H12 1.1200 . ? C27 C28 1.370(16) . ? C27 H27 0.9500 . ? B10 B11 1.758(14) . ? B10 B5 1.788(16) . ? B10 B9 1.789(16) . ? B10 B6 1.799(14) . ? B10 H10 1.1200 . ? C15 C14 1.394(18) . ? C15 C16 1.39(2) . ? C15 H15 0.9500 . ? C16 C17 1.32(2) . ? C16 H16 0.9500 . ? C25 C24 1.388(17) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? B9 B8 1.782(14) . ? B9 B5 1.790(15) . ? B9 H9 1.1200 . ? C18 C17 1.379(18) . ? C18 H18 0.9500 . ? C14 H14 0.9500 . ? C28 H28 0.9500 . ? B11 B6 1.914(14) . ? B11 H11 1.1200 . ? C17 H17 0.9500 . ? B8 H8 1.1200 . ? B5 B6 1.822(15) . ? B5 H5 1.1200 . ? B6 H6 1.1200 . ? C1S C2S 1.51(2) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C3S C4S 1.02(2) . ? C3S C2S 1.45(2) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.37(3) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C5S C6S 1.29(3) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? 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 B7 Pt2 B11 46.5(4) . . ? B7 Pt2 B3 49.2(4) . . ? B11 Pt2 B3 81.3(4) . . ? B7 Pt2 B6 82.1(4) . . ? B11 Pt2 B6 49.1(4) . . ? B3 Pt2 B6 80.6(4) . . ? B7 Pt2 P3 120.7(3) . . ? B11 Pt2 P3 88.6(3) . . ? B3 Pt2 P3 169.4(3) . . ? B6 Pt2 P3 95.3(3) . . ? B7 Pt2 S1 146.4(3) . . ? B11 Pt2 S1 131.1(2) . . ? B3 Pt2 S1 98.7(3) . . ? B6 Pt2 S1 82.5(3) . . ? P3 Pt2 S1 90.33(8) . . ? B7 Pt2 P4 94.6(3) . . ? B11 Pt2 P4 134.3(2) . . ? B3 Pt2 P4 88.5(3) . . ? B6 Pt2 P4 168.0(3) . . ? P3 Pt2 P4 96.27(9) . . ? S1 Pt2 P4 94.39(8) . . ? B7 Pt2 Pt1 93.1(3) . . ? B11 Pt2 Pt1 92.3(3) . . ? B3 Pt2 Pt1 53.2(3) . . ? B6 Pt2 Pt1 52.5(2) . . ? P3 Pt2 Pt1 131.05(5) . . ? S1 Pt2 Pt1 54.08(6) . . ? P4 Pt2 Pt1 116.59(6) . . ? B5 Pt1 B4 47.5(4) . . ? B5 Pt1 B6 47.3(4) . . ? B4 Pt1 B6 81.6(4) . . ? B5 Pt1 B3 81.4(4) . . ? B4 Pt1 B3 49.1(3) . . ? B6 Pt1 B3 80.2(3) . . ? B5 Pt1 P2 87.7(3) . . ? B4 Pt1 P2 120.1(2) . . ? B6 Pt1 P2 95.0(3) . . ? B3 Pt1 P2 168.5(3) . . ? B5 Pt1 P1 131.1(3) . . ? B4 Pt1 P1 92.2(3) . . ? B6 Pt1 P1 171.2(3) . . ? B3 Pt1 P1 91.0(2) . . ? P2 Pt1 P1 93.53(9) . . ? B5 Pt1 S1 129.2(3) . . ? B4 Pt1 S1 144.2(3) . . ? B6 Pt1 S1 82.2(2) . . ? B3 Pt1 S1 96.7(3) . . ? P2 Pt1 S1 92.92(8) . . ? P1 Pt1 S1 99.61(8) . . ? B5 Pt1 Pt2 91.1(3) . . ? B4 Pt1 Pt2 92.1(3) . . ? B6 Pt1 Pt2 53.2(2) . . ? B3 Pt1 Pt2 52.0(2) . . ? P2 Pt1 Pt2 132.35(6) . . ? P1 Pt1 Pt2 121.31(6) . . ? S1 Pt1 Pt2 52.98(5) . . ? C11 P1 C12 102.1(5) . . ? C11 P1 C13 101.0(5) . . ? C12 P1 C13 103.1(5) . . ? C11 P1 Pt1 117.6(3) . . ? C12 P1 Pt1 115.8(4) . . ? C13 P1 Pt1 114.9(4) . . ? C31 P3 C33 103.3(5) . . ? C31 P3 C32 99.2(5) . . ? C33 P3 C32 105.0(4) . . ? C31 P3 Pt2 115.7(3) . . ? C33 P3 Pt2 113.2(3) . . ? C32 P3 Pt2 118.5(3) . . ? O1 S1 O2 113.7(4) . . ? O1 S1 Pt2 112.0(3) . . ? O2 S1 Pt2 118.4(3) . . ? O1 S1 Pt1 114.1(3) . . ? O2 S1 Pt1 119.7(3) . . ? Pt2 S1 Pt1 72.94(6) . . ? C42 P4 C41 101.1(6) . . ? C42 P4 C43 102.4(4) . . ? C41 P4 C43 102.6(5) . . ? C42 P4 Pt2 115.0(4) . . ? C41 P4 Pt2 116.3(4) . . ? C43 P4 Pt2 117.1(3) . . ? C22 P2 C21 102.6(6) . . ? C22 P2 C23 103.1(5) . . ? C21 P2 C23 102.1(4) . . ? C22 P2 Pt1 112.9(4) . . ? C21 P2 Pt1 114.4(4) . . ? C23 P2 Pt1 119.6(3) . . ? P3 C32 H32A 109.5 . . ? P3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 119.1(9) . . ? C34 C33 P3 122.2(7) . . ? C38 C33 P3 118.7(8) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C44 C43 C48 118.8(10) . . ? C44 C43 P4 119.9(8) . . ? C48 C43 P4 121.2(8) . . ? C28 C23 C24 116.5(10) . . ? C28 C23 P2 123.5(8) . . ? C24 C23 P2 120.0(7) . . ? C18 C13 C14 118.5(11) . . ? C18 C13 P1 121.7(10) . . ? C14 C13 P1 119.6(9) . . ? C45 C44 C43 120.2(10) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? P4 C42 H42A 109.5 . . ? P4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P3 C31 H31A 109.5 . . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C44 C45 C46 120.5(10) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 119.7(10) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C33 C34 C35 121.8(10) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C36 119.4(11) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C47 C48 C43 119.8(9) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? C38 C37 C36 119.9(11) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 120.5(10) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C35 C36 C37 119.3(10) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C46 C47 C48 120.9(10) . . ? C46 C47 H47 119.5 . . ? C48 C47 H47 119.5 . . ? B9 B4 B8 60.4(6) . . ? B9 B4 B5 60.4(7) . . ? B8 B4 B5 107.4(8) . . ? B9 B4 B3 106.3(7) . . ? B8 B4 B3 57.7(5) . . ? B5 B4 B3 106.3(7) . . ? B9 B4 Pt1 120.4(7) . . ? B8 B4 Pt1 120.0(6) . . ? B5 B4 Pt1 65.1(5) . . ? B3 B4 Pt1 67.7(4) . . ? B9 B4 H4 119.6 . . ? B8 B4 H4 120.4 . . ? B5 B4 H4 123.3 . . ? B3 B4 H4 123.8 . . ? Pt1 B4 H4 109.0 . . ? P4 C41 H41A 109.5 . . ? P4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? B12 B7 B11 59.5(6) . . ? B12 B7 B8 59.4(5) . . ? B11 B7 B8 106.9(7) . . ? B12 B7 B3 105.6(7) . . ? B11 B7 B3 108.0(7) . . ? B8 B7 B3 57.5(5) . . ? B12 B7 Pt2 120.3(6) . . ? B11 B7 Pt2 67.2(5) . . ? B8 B7 Pt2 118.9(6) . . ? B3 B7 Pt2 66.9(4) . . ? B12 B7 H7 120.6 . . ? B11 B7 H7 122.0 . . ? B8 B7 H7 121.4 . . ? B3 B7 H7 123.6 . . ? Pt2 B7 H7 109.0 . . ? B8 B3 B7 59.0(5) . . ? B8 B3 B4 57.6(6) . . ? B7 B3 B4 105.3(7) . . ? B8 B3 Pt2 117.4(6) . . ? B7 B3 Pt2 63.9(4) . . ? B4 B3 Pt2 121.3(6) . . ? B8 B3 Pt1 115.9(6) . . ? B7 B3 Pt1 121.5(5) . . ? B4 B3 Pt1 63.2(4) . . ? Pt2 B3 Pt1 74.8(3) . . ? B8 B3 H3 121.1 . . ? B7 B3 H3 121.5 . . ? B4 B3 H3 122.6 . . ? Pt2 B3 H3 108.8 . . ? Pt1 B3 H3 109.7 . . ? C27 C26 C25 119.0(10) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? B9 B12 B11 111.1(7) . . ? B9 B12 B7 112.5(7) . . ? B11 B12 B7 60.9(6) . . ? B9 B12 B10 61.3(6) . . ? B11 B12 B10 59.9(6) . . ? B7 B12 B10 109.6(7) . . ? B9 B12 B8 60.9(6) . . ? B11 B12 B8 110.0(7) . . ? B7 B12 B8 62.0(6) . . ? B10 B12 B8 108.9(7) . . ? B9 B12 H12 119.0 . . ? B11 B12 H12 120.7 . . ? B7 B12 H12 119.5 . . ? B10 B12 H12 121.6 . . ? B8 B12 H12 120.8 . . ? C26 C27 C28 122.4(10) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? B11 B10 B12 59.8(6) . . ? B11 B10 B5 112.7(8) . . ? B12 B10 B5 108.0(7) . . ? B11 B10 B9 108.9(7) . . ? B12 B10 B9 58.8(6) . . ? B5 B10 B9 60.1(6) . . ? B11 B10 B6 65.1(6) . . ? B12 B10 B6 111.6(7) . . ? B5 B10 B6 61.1(6) . . ? B9 B10 B6 110.1(7) . . ? B11 B10 H10 118.7 . . ? B12 B10 H10 122.1 . . ? B5 B10 H10 120.6 . . ? B9 B10 H10 122.3 . . ? B6 B10 H10 118.2 . . ? C14 C15 C16 118.7(14) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C17 C16 C15 120.5(13) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C26 C25 C24 121.0(12) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C24 C23 120.2(10) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? B12 B9 B4 110.3(7) . . ? B12 B9 B8 60.2(6) . . ? B4 B9 B8 60.6(6) . . ? B12 B9 B10 59.9(6) . . ? B4 B9 B10 109.4(7) . . ? B8 B9 B10 107.2(7) . . ? B12 B9 B5 108.8(7) . . ? B4 B9 B5 61.1(6) . . ? B8 B9 B5 108.1(7) . . ? B10 B9 B5 59.9(6) . . ? B12 B9 H9 120.8 . . ? B4 B9 H9 119.9 . . ? B8 B9 H9 122.2 . . ? B10 B9 H9 122.0 . . ? B5 B9 H9 121.4 . . ? C17 C18 C13 119.8(14) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C13 C14 C15 120.5(13) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C27 C28 C23 120.8(11) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? B12 B11 B10 60.3(6) . . ? B12 B11 B7 59.6(6) . . ? B10 B11 B7 108.8(7) . . ? B12 B11 B6 106.8(7) . . ? B10 B11 B6 58.5(5) . . ? B7 B11 B6 109.5(7) . . ? B12 B11 Pt2 119.6(6) . . ? B10 B11 Pt2 120.4(6) . . ? B7 B11 Pt2 66.3(5) . . ? B6 B11 Pt2 67.7(4) . . ? B12 B11 H11 120.7 . . ? B10 B11 H11 119.8 . . ? B7 B11 H11 121.6 . . ? B6 B11 H11 122.4 . . ? Pt2 B11 H11 109.0 . . ? C16 C17 C18 122.0(15) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? B12 B8 B9 58.9(6) . . ? B12 B8 B4 108.0(7) . . ? B9 B8 B4 59.0(6) . . ? B12 B8 B3 109.8(7) . . ? B9 B8 B3 110.8(7) . . ? B4 B8 B3 64.7(6) . . ? B12 B8 B7 58.7(5) . . ? B9 B8 B7 108.0(7) . . ? B4 B8 B7 114.5(7) . . ? B3 B8 B7 63.5(6) . . ? B12 B8 H8 123.3 . . ? B9 B8 H8 122.7 . . ? B4 B8 H8 118.8 . . ? B3 B8 H8 117.8 . . ? B7 B8 H8 119.4 . . ? B10 B5 B9 60.0(6) . . ? B10 B5 B4 107.5(7) . . ? B9 B5 B4 58.6(6) . . ? B10 B5 B6 59.8(6) . . ? B9 B5 B6 109.0(8) . . ? B4 B5 B6 111.3(7) . . ? B10 B5 Pt1 122.6(6) . . ? B9 B5 Pt1 120.9(6) . . ? B4 B5 Pt1 67.4(5) . . ? B6 B5 Pt1 69.3(4) . . ? B10 B5 H5 119.9 . . ? B9 B5 H5 120.5 . . ? B4 B5 H5 122.2 . . ? B6 B5 H5 120.0 . . ? Pt1 B5 H5 107.1 . . ? B10 B6 B5 59.2(6) . . ? B10 B6 B11 56.4(5) . . ? B5 B6 B11 104.3(7) . . ? B10 B6 Pt1 116.8(6) . . ? B5 B6 Pt1 63.4(5) . . ? B11 B6 Pt1 120.5(5) . . ? B10 B6 Pt2 114.5(6) . . ? B5 B6 Pt2 120.3(6) . . ? B11 B6 Pt2 63.2(4) . . ? Pt1 B6 Pt2 74.4(3) . . ? B10 B6 H6 121.7 . . ? B5 B6 H6 121.9 . . ? B11 B6 H6 123.1 . . ? Pt1 B6 H6 109.4 . . ? Pt2 B6 H6 110.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C4S C3S C2S 125.1(19) . . ? C4S C3S H3S1 106.1 . . ? C2S C3S H3S1 106.1 . . ? C4S C3S H3S2 106.1 . . ? C2S C3S H3S2 106.1 . . ? H3S1 C3S H3S2 106.3 . . ? C3S C4S C5S 131(2) . . ? C3S C4S H4S1 104.4 . . ? C5S C4S H4S1 104.4 . . ? C3S C4S H4S2 104.4 . . ? C5S C4S H4S2 104.4 . . ? H4S1 C4S H4S2 105.6 . . ? C3S C2S C1S 123.8(16) . . ? C3S C2S H2S1 106.4 . . ? C1S C2S H2S1 106.4 . . ? C3S C2S H2S2 106.4 . . ? C1S C2S H2S2 106.4 . . ? H2S1 C2S H2S2 106.4 . . ? C6S C5S C4S 131(3) . . ? C6S C5S H5S1 104.5 . . ? C4S C5S H5S1 104.5 . . ? C6S C5S H5S2 104.5 . . ? C4S C5S H5S2 104.5 . . ? H5S1 C5S H5S2 105.6 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.643 _refine_diff_density_min -3.738 _refine_diff_density_rms 0.215 data_c:\xray\pt2b10~1\ssd0264 _database_code_depnum_ccdc_archive 'CCDC 254127' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H54 B10 P4 Pt2' _chemical_formula_weight 1060.91 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' 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 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.164(2) _cell_length_b 11.3966(9) _cell_length_c 20.0425(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.659(2) _cell_angle_gamma 90.00 _cell_volume 3825.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7085 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 30.87 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 7.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5853 _exptl_absorpt_correction_T_max 0.8645 _exptl_absorpt_process_details 'Bruker SADABS' # absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.851 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6933 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'fine-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 20269 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 30.92 _reflns_number_total 5919 _reflns_number_gt 5656 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' # Appropriate references: # Data collection: APEX2, Bruker AXS Inc., Madison, USA, 2004 # Data reduction (frames integration): SAINT, Bruker AXS Inc., Madison, USA, #2004 # Cell refinement: SAINT, Bruker AXS Inc., Madison, USA, 2004 # Absorption correction: SADABS, Bruker AXS Inc., Madison, USA, 2004 # Station 9.8: R. J. Cernik, W. Clegg, C. R. A. Catlow, G. Bushnell-Wye, #J. V. Flaherty, G. N. Greaves, M. Hamichi, I. Burrows, D. J. Taylor and S. #J. Teat, J. Synchotron Radiation 1997, 4, 279-286; 7, 40. # Synchrotron chemical crystallography: # W. Clegg, J. Chem. Soc., Dalton Trans. 2000, 3223-3232. _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565. CorelDraw 11, Corel Corporation. ; _computing_publication_material ; CCDC (2003). enCIFer - a program for CIF editing. CCDC, 12 Union Road, Cambridge, UK. ; _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^)+(0.0226P)^2^+2.0708P] 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 5919 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.008 _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 Pt2 Pt 0.663750(3) 0.837474(4) 0.468263(3) 0.00932(3) Uani 1 1 d . . . P1 P 0.58306(2) 0.74021(3) 0.53033(2) 0.01133(7) Uani 1 1 d . . . P2 P 0.62460(3) 0.72919(4) 0.36738(2) 0.01408(8) Uani 1 1 d . . . C11 C 0.54663(12) 0.83100(13) 0.59159(10) 0.0175(3) Uani 1 1 d . . . H11A H 0.5232 0.9031 0.5691 0.026 Uiso 1 1 calc R . . H11B H 0.5911 0.8510 0.6296 0.026 Uiso 1 1 calc R . . H11C H 0.5059 0.7878 0.6091 0.026 Uiso 1 1 calc R . . C12 C 0.48713(11) 0.68558(17) 0.48219(9) 0.0190(3) Uani 1 1 d . . . H12A H 0.4598 0.6435 0.5131 0.029 Uiso 1 1 calc R . . H12B H 0.4960 0.6321 0.4463 0.029 Uiso 1 1 calc R . . H12C H 0.4541 0.7517 0.4614 0.029 Uiso 1 1 calc R . . C21 C 0.68541(11) 0.7398(2) 0.30397(10) 0.0266(4) Uani 1 1 d . . . H21A H 0.7380 0.7050 0.3223 0.040 Uiso 1 1 calc R . . H21B H 0.6919 0.8225 0.2929 0.040 Uiso 1 1 calc R . . H21C H 0.6592 0.6976 0.2625 0.040 Uiso 1 1 calc R . . C22 C 0.61225(12) 0.56998(16) 0.36977(10) 0.0234(4) Uani 1 1 d . . . H22A H 0.5909 0.5408 0.3234 0.035 Uiso 1 1 calc R . . H22B H 0.5751 0.5506 0.3989 0.035 Uiso 1 1 calc R . . H22C H 0.6641 0.5332 0.3883 0.035 Uiso 1 1 calc R . . C111 C 0.62386(9) 0.61112(14) 0.57985(8) 0.0141(3) Uani 1 1 d . . . C112 C 0.66959(10) 0.53170(15) 0.55221(9) 0.0175(3) Uani 1 1 d . . . H112 H 0.6846 0.5501 0.5105 0.021 Uiso 1 1 calc R . . C113 C 0.69369(11) 0.42563(16) 0.58467(10) 0.0220(3) Uani 1 1 d . . . H113 H 0.7237 0.3712 0.5646 0.026 Uiso 1 1 calc R . . C114 C 0.67360(11) 0.39958(16) 0.64667(10) 0.0230(4) Uani 1 1 d . . . H114 H 0.6891 0.3267 0.6686 0.028 Uiso 1 1 calc R . . C115 C 0.63095(12) 0.48004(17) 0.67623(10) 0.0257(4) Uani 1 1 d . . . H115 H 0.6194 0.4638 0.7195 0.031 Uiso 1 1 calc R . . C116 C 0.60494(11) 0.58470(16) 0.64271(9) 0.0210(3) Uani 1 1 d . . . H116 H 0.5742 0.6384 0.6626 0.025 Uiso 1 1 calc R . . C211 C 0.52653(9) 0.77695(14) 0.31941(8) 0.0138(3) Uani 1 1 d . . . C212 C 0.48516(10) 0.86632(15) 0.34439(9) 0.0162(3) Uani 1 1 d . . . H212 H 0.5087 0.9047 0.3860 0.019 Uiso 1 1 calc R . . C213 C 0.40939(10) 0.89935(15) 0.30844(9) 0.0188(3) Uani 1 1 d . . . H213 H 0.3811 0.9593 0.3261 0.023 Uiso 1 1 calc R . . C214 C 0.37493(12) 0.84529(15) 0.24701(11) 0.0207(4) Uani 1 1 d . . . H214 H 0.3232 0.8682 0.2228 0.025 Uiso 1 1 calc R . . C215 C 0.41595(11) 0.75787(16) 0.22091(9) 0.0201(3) Uani 1 1 d . . . H215 H 0.3928 0.7219 0.1784 0.024 Uiso 1 1 calc R . . C216 C 0.49119(10) 0.72294(15) 0.25708(8) 0.0171(3) Uani 1 1 d . . . H216 H 0.5188 0.6622 0.2395 0.020 Uiso 1 1 calc R . . B6 B 0.72899(11) 0.92933(15) 0.56760(9) 0.0132(3) Uani 1 1 d . . . H6 H 0.7157 0.8780 0.6114 0.016 Uiso 1 1 calc R . . B7 B 0.67856(11) 1.01295(16) 0.42427(10) 0.0151(3) Uani 1 1 d . . . H7 H 0.6346 1.0190 0.3740 0.018 Uiso 1 1 calc R . . B8 B 0.65167(11) 1.01467(16) 0.50880(10) 0.0144(3) Uani 1 1 d . . . H8 H 0.5892 1.0233 0.5164 0.017 Uiso 1 1 calc R . . B11 B 0.72939(11) 1.08632(16) 0.56636(10) 0.0166(3) Uani 1 1 d . . . H11 H 0.7158 1.1367 0.6104 0.020 Uiso 1 1 calc R . . B12 B 0.69875(12) 1.13529(17) 0.47945(11) 0.0182(3) Uani 1 1 d . . . H12 H 0.6651 1.2193 0.4658 0.022 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 Pt2 0.00818(4) 0.00956(4) 0.00978(4) 0.00005(1) 0.00102(3) 0.00001(2) P1 0.00972(17) 0.01100(17) 0.01303(18) 0.00003(13) 0.00196(14) -0.00111(13) P2 0.01121(18) 0.01819(19) 0.01205(18) -0.00319(14) 0.00081(14) 0.00176(14) C11 0.0202(9) 0.0147(8) 0.0199(9) -0.0007(5) 0.0093(7) -0.0001(5) C12 0.0124(7) 0.0223(8) 0.0207(8) 0.0015(7) 0.0000(6) -0.0046(6) C21 0.0155(8) 0.0490(12) 0.0160(8) -0.0094(8) 0.0046(6) -0.0002(8) C22 0.0244(9) 0.0186(8) 0.0235(9) -0.0071(6) -0.0030(7) 0.0068(7) C111 0.0126(7) 0.0130(7) 0.0154(7) 0.0001(5) 0.0003(5) -0.0028(5) C112 0.0131(7) 0.0179(8) 0.0206(8) -0.0004(6) 0.0019(6) 0.0005(6) C113 0.0157(8) 0.0149(8) 0.0318(10) 0.0005(6) -0.0025(7) 0.0016(6) C114 0.0168(8) 0.0161(8) 0.0314(10) 0.0080(7) -0.0052(7) -0.0032(6) C115 0.0286(10) 0.0239(9) 0.0233(9) 0.0093(7) 0.0032(7) -0.0031(7) C116 0.0243(9) 0.0196(8) 0.0198(8) 0.0035(6) 0.0065(7) 0.0003(7) C211 0.0113(7) 0.0172(7) 0.0120(7) 0.0009(5) 0.0009(5) -0.0004(5) C212 0.0150(7) 0.0166(7) 0.0157(7) -0.0002(6) 0.0007(6) 0.0000(6) C213 0.0146(7) 0.0163(7) 0.0245(8) 0.0027(6) 0.0022(6) 0.0005(6) C214 0.0141(8) 0.0230(9) 0.0226(9) 0.0076(6) -0.0011(7) -0.0026(6) C215 0.0178(8) 0.0250(8) 0.0143(7) 0.0022(6) -0.0031(6) -0.0053(6) C216 0.0168(8) 0.0206(8) 0.0135(7) -0.0002(6) 0.0027(6) -0.0006(6) B6 0.0123(7) 0.0120(7) 0.0152(8) -0.0030(6) 0.0029(6) -0.0004(6) B7 0.0127(8) 0.0139(8) 0.0189(9) 0.0057(6) 0.0038(6) 0.0022(6) B8 0.0114(8) 0.0120(7) 0.0203(9) 0.0003(6) 0.0048(6) 0.0013(6) B11 0.0155(8) 0.0109(7) 0.0246(9) -0.0046(6) 0.0070(7) -0.0011(6) B12 0.0155(8) 0.0104(7) 0.0301(10) 0.0019(7) 0.0081(7) 0.0021(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt2 B8 2.2035(18) . ? Pt2 B7 2.2225(18) . ? Pt2 B6 2.3101(18) . ? Pt2 P1 2.3344(4) . ? Pt2 P2 2.3382(4) . ? Pt2 B6 2.3626(18) 2_656 ? Pt2 Pt2 2.9552(4) 2_656 ? P1 C11 1.8180(18) . ? P1 C12 1.8258(18) . ? P1 C111 1.8262(16) . ? P2 C21 1.8167(18) . ? P2 C22 1.829(2) . ? P2 C211 1.8288(17) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C111 C112 1.390(2) . ? C111 C116 1.401(2) . ? C112 C113 1.392(2) . ? C112 H112 0.9500 . ? C113 C114 1.392(3) . ? C113 H113 0.9500 . ? C114 C115 1.385(3) . ? C114 H114 0.9500 . ? C115 C116 1.393(3) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C211 C212 1.396(2) . ? C211 C216 1.405(2) . ? C212 C213 1.393(2) . ? C212 H212 0.9500 . ? C213 C214 1.388(3) . ? C213 H213 0.9500 . ? C214 C215 1.387(3) . ? C214 H214 0.9500 . ? C215 C216 1.393(2) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? B6 B11 1.789(3) . ? B6 B7 1.827(3) 2_656 ? B6 B8 1.847(3) . ? B6 Pt2 2.3626(17) 2_656 ? B6 H6 1.1200 . ? B7 B11 1.761(3) 2_656 ? B7 B12 1.766(3) . ? B7 B6 1.827(3) 2_656 ? B7 B8 1.851(3) . ? B7 H7 1.1200 . ? B8 B12 1.760(3) . ? B8 B11 1.761(3) . ? B8 H8 1.1200 . ? B11 B7 1.761(3) 2_656 ? B11 B12 1.781(3) 2_656 ? B11 B12 1.795(3) . ? B11 H11 1.1200 . ? B12 B12 1.772(4) 2_656 ? B12 B11 1.781(3) 2_656 ? B12 H12 1.1200 . ? 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 B8 Pt2 B7 49.45(8) . . ? B8 Pt2 B6 48.23(7) . . ? B7 Pt2 B6 81.85(7) . . ? B8 Pt2 P1 97.12(5) . . ? B7 Pt2 P1 140.49(5) . . ? B6 Pt2 P1 89.31(5) . . ? B8 Pt2 P2 140.37(5) . . ? B7 Pt2 P2 99.67(5) . . ? B6 Pt2 P2 167.85(5) . . ? P1 Pt2 P2 96.812(16) . . ? B8 Pt2 B6 81.30(7) . 2_656 ? B7 Pt2 B6 46.85(6) . 2_656 ? B6 Pt2 B6 78.38(8) . 2_656 ? P1 Pt2 B6 164.88(5) . 2_656 ? P2 Pt2 B6 93.80(5) . 2_656 ? B8 Pt2 Pt2 90.44(5) . 2_656 ? B7 Pt2 Pt2 88.85(5) . 2_656 ? B6 Pt2 Pt2 51.56(4) . 2_656 ? P1 Pt2 Pt2 115.212(12) . 2_656 ? P2 Pt2 Pt2 116.307(11) . 2_656 ? B6 Pt2 Pt2 49.99(4) 2_656 2_656 ? C11 P1 C12 98.46(9) . . ? C11 P1 C111 103.84(8) . . ? C12 P1 C111 101.92(8) . . ? C11 P1 Pt2 114.94(6) . . ? C12 P1 Pt2 116.87(6) . . ? C111 P1 Pt2 118.07(5) . . ? C21 P2 C22 99.90(10) . . ? C21 P2 C211 102.48(8) . . ? C22 P2 C211 102.15(8) . . ? C21 P2 Pt2 118.01(7) . . ? C22 P2 Pt2 120.93(6) . . ? C211 P2 Pt2 110.76(5) . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C112 C111 C116 118.73(15) . . ? C112 C111 P1 119.39(12) . . ? C116 C111 P1 121.67(13) . . ? C111 C112 C113 121.00(16) . . ? C111 C112 H112 119.5 . . ? C113 C112 H112 119.5 . . ? C112 C113 C114 119.73(17) . . ? C112 C113 H113 120.1 . . ? C114 C113 H113 120.1 . . ? C115 C114 C113 119.87(16) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.27(18) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C111 120.31(17) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C212 C211 C216 118.95(15) . . ? C212 C211 P2 120.71(12) . . ? C216 C211 P2 120.34(13) . . ? C213 C212 C211 120.14(16) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 120.45(17) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C215 C214 C213 120.05(18) . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 119.88(16) . . ? C214 C215 H215 120.1 . . ? C216 C215 H215 120.1 . . ? C215 C216 C211 120.51(16) . . ? C215 C216 H216 119.7 . . ? C211 C216 H216 119.7 . . ? B11 B6 B7 58.26(10) . 2_656 ? B11 B6 B8 57.92(10) . . ? B7 B6 B8 105.71(12) 2_656 . ? B11 B6 Pt2 116.34(11) . . ? B7 B6 Pt2 124.10(11) 2_656 . ? B8 B6 Pt2 62.86(8) . . ? B11 B6 Pt2 115.67(10) . 2_656 ? B7 B6 Pt2 62.54(8) 2_656 2_656 ? B8 B6 Pt2 122.56(10) . 2_656 ? Pt2 B6 Pt2 78.45(5) . 2_656 ? B11 B6 H6 122.4 . . ? B7 B6 H6 121.6 2_656 . ? B8 B6 H6 122.3 . . ? Pt2 B6 H6 107.2 . . ? Pt2 B6 H6 108.2 2_656 . ? B11 B7 B12 60.65(11) 2_656 . ? B11 B7 B6 59.79(10) 2_656 2_656 ? B12 B7 B6 107.96(14) . 2_656 ? B11 B7 B8 107.17(14) 2_656 . ? B12 B7 B8 58.17(10) . . ? B6 B7 B8 108.04(13) 2_656 . ? B11 B7 Pt2 124.26(11) 2_656 . ? B12 B7 Pt2 119.06(12) . . ? B6 B7 Pt2 70.61(8) 2_656 . ? B8 B7 Pt2 64.74(7) . . ? B11 B7 H7 118.6 2_656 . ? B12 B7 H7 121.0 . . ? B6 B7 H7 120.8 2_656 . ? B8 B7 H7 124.6 . . ? Pt2 B7 H7 107.4 . . ? B12 B8 B11 61.28(11) . . ? B12 B8 B6 107.83(13) . . ? B11 B8 B6 59.40(10) . . ? B12 B8 B7 58.49(11) . . ? B11 B8 B7 107.42(13) . . ? B6 B8 B7 106.86(12) . . ? B12 B8 Pt2 120.35(11) . . ? B11 B8 Pt2 123.19(11) . . ? B6 B8 Pt2 68.91(8) . . ? B7 B8 Pt2 65.81(8) . . ? B12 B8 H8 120.0 . . ? B11 B8 H8 118.7 . . ? B6 B8 H8 122.3 . . ? B7 B8 H8 124.3 . . ? Pt2 B8 H8 107.5 . . ? B7 B11 B8 112.51(13) 2_656 . ? B7 B11 B12 59.82(11) 2_656 2_656 ? B8 B11 B12 108.57(14) . 2_656 ? B7 B11 B6 61.95(10) 2_656 . ? B8 B11 B6 62.67(10) . . ? B12 B11 B6 109.01(13) 2_656 . ? B7 B11 B12 108.45(13) 2_656 . ? B8 B11 B12 59.32(11) . . ? B12 B11 B12 59.40(13) 2_656 . ? B6 B11 B12 108.86(13) . . ? B7 B11 H11 119.8 2_656 . ? B8 B11 H11 119.7 . . ? B12 B11 H11 122.2 2_656 . ? B6 B11 H11 120.0 . . ? B12 B11 H11 122.6 . . ? B8 B12 B7 63.34(12) . . ? B8 B12 B12 109.06(13) . 2_656 ? B7 B12 B12 109.26(12) . 2_656 ? B8 B12 B11 110.38(13) . 2_656 ? B7 B12 B11 59.53(11) . 2_656 ? B12 B12 B11 60.69(12) 2_656 2_656 ? B8 B12 B11 59.40(11) . . ? B7 B12 B11 109.75(13) . . ? B12 B12 B11 59.91(13) 2_656 . ? B11 B12 B11 108.31(13) 2_656 . ? B8 B12 H12 120.0 . . ? B7 B12 H12 120.1 . . ? B12 B12 H12 121.3 2_656 . ? B11 B12 H12 121.3 2_656 . ? B11 B12 H12 121.9 . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.996 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.116