Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Paul Robert Raithby' 'Birte Ahrens' 'Muna R.A. Al-Mandhary' 'Mohammad Al-Suti' 'Jens K. Bjern' 'Richard Friend' 'Muhammad S. Khan' 'Anna Kohler' 'M. Mahon' 'Louise Male' 'Joanne S. Wilson' _publ_contact_author_name 'Prof Paul Robert Raithby' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down BATH Avon BA2 7AY UNITED KINGDOM ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and characterisation of new acetylide-functionalised aromatic and hetero-aromatic ligands and their dinuclear platinum complexes ; data_h01prr55 _database_code_CSD 192672 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H75 N1 P4 Pt2' _chemical_formula_sum 'C49.50 H76 Cl N P4 Pt2' _chemical_formula_weight 1234.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.17940(10) _cell_length_b 16.7290(2) _cell_length_c 18.8959(2) _cell_angle_alpha 112.3960(10) _cell_angle_beta 95.2000(10) _cell_angle_gamma 94.2820(10) _cell_volume 2652.93(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 58387 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.03 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 5.470 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.622 _exptl_absorpt_process_details 'Gaussian integration (Coppens, 1970)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '346 1.7 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54771 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 30.05 _reflns_number_total 15461 _reflns_number_gt 12734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution 'DirDif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0365P)^2^+8.8287P] 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 15461 _refine_ls_number_parameters 534 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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 0.444325(17) 0.323168(12) 0.829083(9) 0.03144(5) Uani 1 1 d . . . Pt2 Pt 1.189068(18) 0.204924(11) 0.307445(9) 0.03212(5) Uani 1 1 d . . . P11 P 0.26474(13) 0.38506(9) 0.78300(7) 0.0376(3) Uani 1 1 d . . . P12 P 0.62278(12) 0.25215(8) 0.86404(7) 0.0323(2) Uani 1 1 d . . . P21 P 0.97381(13) 0.13309(9) 0.23034(7) 0.0375(3) Uani 1 1 d . A . P22 P 1.40970(17) 0.26720(11) 0.38367(8) 0.0531(4) Uani 1 1 d . A . C1 C 0.7263(5) 0.3031(4) 0.6322(3) 0.0476(14) Uani 1 1 d . . . C2 C 0.7508(6) 0.2206(5) 0.5855(3) 0.0513(14) Uani 1 1 d . . . H2 H 0.7069 0.1720 0.5934 0.062 Uiso 1 1 calc R . . C3 C 0.8408(6) 0.2068(5) 0.5254(3) 0.0508(14) Uani 1 1 d . . . H3 H 0.8542 0.1489 0.4936 0.061 Uiso 1 1 calc R . . C4 C 0.9092(5) 0.2754(4) 0.5122(3) 0.0424(12) Uani 1 1 d . A . C5 C 0.8867(5) 0.3613(4) 0.5607(3) 0.0459(13) Uani 1 1 d . . . N6 N 0.9594(6) 0.4362(5) 0.5511(4) 0.0651(15) Uani 0.69 1 d P A 1 C6 C 0.9594(6) 0.4362(5) 0.5511(4) 0.0651(15) Uani 0.31 1 d P A 2 H6 H 1.0267 0.4269 0.5142 0.078 Uiso 0.31 1 calc PR A 2 C7 C 0.9338(8) 0.5202(6) 0.5939(5) 0.077(2) Uani 1 1 d . . . H7 H 0.9793 0.5674 0.5844 0.092 Uiso 1 1 calc R A 1 C8 C 0.8382(9) 0.5363(6) 0.6527(5) 0.074(2) Uani 1 1 d . A . H8 H 0.8216 0.5942 0.6827 0.089 Uiso 1 1 calc R B 1 C9 C 0.7699(8) 0.4667(5) 0.6656(4) 0.0722(18) Uani 0.69 1 d P A 1 H9 H 0.7069 0.4778 0.7047 0.087 Uiso 0.69 1 calc PR A 1 N9 N 0.7699(8) 0.4667(5) 0.6656(4) 0.0722(18) Uani 0.31 1 d P A 2 C10 C 0.7940(5) 0.3752(4) 0.6192(3) 0.0488(14) Uani 1 1 d . A . C11 C 0.6359(6) 0.3167(4) 0.6929(3) 0.0507(14) Uani 1 1 d . . . C12 C 0.5624(5) 0.3228(4) 0.7446(3) 0.0444(12) Uani 1 1 d . . . C41 C 0.9984(6) 0.2585(4) 0.4504(3) 0.0441(12) Uani 1 1 d . . . C42 C 1.0712(6) 0.2400(4) 0.3975(3) 0.0416(11) Uani 1 1 d . A . C101 C 0.3254(5) 0.3183(4) 0.9151(3) 0.0380(11) Uani 1 1 d . . . C102 C 0.2268(5) 0.2452(4) 0.9046(4) 0.0484(13) Uani 1 1 d . . . H102 H 0.2142 0.1969 0.8563 0.058 Uiso 1 1 calc R . . C103 C 0.1471(6) 0.2409(6) 0.9624(5) 0.070(2) Uani 1 1 d . . . H103 H 0.0836 0.1896 0.9533 0.084 Uiso 1 1 calc R . . C104 C 0.1586(7) 0.3087(6) 1.0315(5) 0.073(2) Uani 1 1 d . . . H104 H 0.1015 0.3061 1.0702 0.088 Uiso 1 1 calc R . . C105 C 0.2542(7) 0.3810(5) 1.0444(4) 0.0630(18) Uani 1 1 d . . . H105 H 0.2651 0.4285 1.0931 0.076 Uiso 1 1 calc R . . C106 C 0.3363(6) 0.3861(4) 0.9872(3) 0.0473(13) Uani 1 1 d . . . H106 H 0.4012 0.4374 0.9978 0.057 Uiso 1 1 calc R . . C111 C 0.1382(7) 0.4373(5) 0.8491(4) 0.0607(17) Uani 1 1 d . . . H11A H 0.0901 0.3934 0.8656 0.073 Uiso 1 1 calc R . . H11B H 0.1960 0.4829 0.8956 0.073 Uiso 1 1 calc R . . C112 C 0.0176(8) 0.4790(6) 0.8191(4) 0.075(2) Uani 1 1 d . . . H11C H -0.0412 0.5074 0.8604 0.112 Uiso 1 1 calc R . . H11D H -0.0461 0.4340 0.7756 0.112 Uiso 1 1 calc R . . H11E H 0.0629 0.5223 0.8020 0.112 Uiso 1 1 calc R . . C113 C 0.3315(8) 0.4684(6) 0.7495(6) 0.088(3) Uani 1 1 d . . . H11F H 0.3975 0.4437 0.7099 0.105 Uiso 1 1 calc R . . H11G H 0.2469 0.4863 0.7251 0.105 Uiso 1 1 calc R . . C114 C 0.4163(14) 0.5494(8) 0.8169(11) 0.182(8) Uani 1 1 d . . . H11H H 0.4497 0.5930 0.7971 0.274 Uiso 1 1 calc R . . H11I H 0.5017 0.5321 0.8402 0.274 Uiso 1 1 calc R . . H11J H 0.3509 0.5742 0.8559 0.274 Uiso 1 1 calc R . . C115 C 0.1521(10) 0.3066(6) 0.6982(5) 0.097(3) Uani 1 1 d . . . H11K H 0.0706 0.3357 0.6845 0.116 Uiso 1 1 calc R . . H11L H 0.2127 0.2906 0.6552 0.116 Uiso 1 1 calc R . . C116 C 0.0926(12) 0.2321(7) 0.7022(7) 0.128(5) Uani 1 1 d . . . H11M H 0.0362 0.1949 0.6523 0.192 Uiso 1 1 calc R . . H11N H 0.0272 0.2462 0.7424 0.192 Uiso 1 1 calc R . . H11O H 0.1715 0.2015 0.7148 0.192 Uiso 1 1 calc R . . C121 C 0.6045(5) 0.2258(4) 0.9483(3) 0.0455(12) Uani 1 1 d . . . H12A H 0.5909 0.2799 0.9920 0.055 Uiso 1 1 calc R . . H12B H 0.5137 0.1849 0.9371 0.055 Uiso 1 1 calc R . . C122 C 0.7318(6) 0.1861(5) 0.9743(4) 0.0554(16) Uani 1 1 d . . . H12C H 0.7135 0.1783 1.0216 0.083 Uiso 1 1 calc R . . H12D H 0.8234 0.2249 0.9841 0.083 Uiso 1 1 calc R . . H12E H 0.7406 0.1295 0.9337 0.083 Uiso 1 1 calc R . . C123 C 0.6299(7) 0.1474(4) 0.7867(4) 0.0605(16) Uani 1 1 d . . . H12F H 0.6648 0.1569 0.7421 0.073 Uiso 1 1 calc R . . H12G H 0.7020 0.1156 0.8044 0.073 Uiso 1 1 calc R . . C124 C 0.4793(9) 0.0912(5) 0.7605(6) 0.094(3) Uani 1 1 d . . . H12H H 0.4892 0.0352 0.7194 0.140 Uiso 1 1 calc R . . H12I H 0.4084 0.1214 0.7410 0.140 Uiso 1 1 calc R . . H12J H 0.4445 0.0813 0.8043 0.140 Uiso 1 1 calc R . . C125 C 0.8083(5) 0.3083(4) 0.8819(3) 0.0406(11) Uani 1 1 d . . . H12K H 0.8803 0.2692 0.8875 0.049 Uiso 1 1 calc R . . H12L H 0.8276 0.3224 0.8370 0.049 Uiso 1 1 calc R . . C126 C 0.8302(7) 0.3922(4) 0.9545(4) 0.0585(15) Uani 1 1 d . . . H12M H 0.9308 0.4207 0.9617 0.088 Uiso 1 1 calc R . . H12N H 0.8143 0.3783 0.9994 0.088 Uiso 1 1 calc R . . H12O H 0.7597 0.4313 0.9490 0.088 Uiso 1 1 calc R . . C201 C 1.3048(4) 0.1657(3) 0.2138(2) 0.0299(8) Uani 1 1 d . A . C202 C 1.3245(5) 0.2149(3) 0.1686(3) 0.0379(10) Uani 1 1 d . . . H202 H 1.2868 0.2695 0.1832 0.045 Uiso 1 1 calc R . . C203 C 1.3969(5) 0.1866(4) 0.1033(3) 0.0416(11) Uani 1 1 d . . . H203 H 1.4075 0.2215 0.0741 0.050 Uiso 1 1 calc R . . C204 C 1.4536(5) 0.1074(4) 0.0811(3) 0.0408(11) Uani 1 1 d . . . H204 H 1.5026 0.0875 0.0365 0.049 Uiso 1 1 calc R . . C205 C 1.4380(5) 0.0578(3) 0.1245(3) 0.0400(11) Uani 1 1 d . . . H205 H 1.4777 0.0038 0.1100 0.048 Uiso 1 1 calc R . . C206 C 1.3647(5) 0.0864(3) 0.1893(3) 0.0355(9) Uani 1 1 d . . . H206 H 1.3547 0.0508 0.2179 0.043 Uiso 1 1 calc R . . C211 C 0.9858(6) 0.0728(5) 0.1278(3) 0.0562(16) Uani 1 1 d . . . H21A H 1.0218 0.1148 0.1061 0.067 Uiso 1 1 calc R . . H21B H 1.0607 0.0321 0.1235 0.067 Uiso 1 1 calc R . . C212 C 0.8431(6) 0.0207(5) 0.0781(3) 0.0611(17) Uani 1 1 d . . . H21C H 0.8604 -0.0058 0.0240 0.092 Uiso 1 1 calc R . . H21D H 0.7666 0.0596 0.0828 0.092 Uiso 1 1 calc R . . H21E H 0.8109 -0.0251 0.0956 0.092 Uiso 1 1 calc R . . C213 C 0.8915(8) 0.0527(5) 0.2619(4) 0.074(2) Uani 1 1 d . . . H21F H 0.8692 0.0825 0.3154 0.089 Uiso 1 1 calc R . . H21G H 0.7971 0.0249 0.2287 0.089 Uiso 1 1 calc R . . C214 C 0.9877(15) -0.0162(7) 0.2595(8) 0.140(5) Uani 1 1 d . . . H21H H 0.9379 -0.0572 0.2778 0.211 Uiso 1 1 calc R . . H21I H 1.0809 0.0108 0.2928 0.211 Uiso 1 1 calc R . . H21J H 1.0074 -0.0474 0.2064 0.211 Uiso 1 1 calc R . . C215 C 0.8303(6) 0.2030(5) 0.2324(4) 0.0621(17) Uani 1 1 d . . . H21K H 0.7395 0.1664 0.2008 0.075 Uiso 1 1 calc R . . H21L H 0.8085 0.2310 0.2862 0.075 Uiso 1 1 calc R . . C216 C 0.8687(10) 0.2723(6) 0.2033(6) 0.101(3) Uani 1 1 d . . . H21M H 0.7873 0.3078 0.2070 0.151 Uiso 1 1 calc R . . H21N H 0.8863 0.2452 0.1493 0.151 Uiso 1 1 calc R . . H21O H 0.9580 0.3094 0.2345 0.151 Uiso 1 1 calc R . . C221 C 1.5178(8) 0.3431(6) 0.3537(4) 0.078(2) Uani 1 1 d . . . H22A H 1.5325 0.3122 0.2991 0.094 Uiso 1 1 calc R . . H22B H 1.4596 0.3914 0.3565 0.094 Uiso 1 1 calc R . . C222 C 1.6713(8) 0.3826(6) 0.4022(5) 0.089(3) Uani 1 1 d . . . H22C H 1.7205 0.4220 0.3821 0.134 Uiso 1 1 calc R . . H22D H 1.7316 0.3356 0.3987 0.134 Uiso 1 1 calc R . . H22E H 1.6585 0.4149 0.4563 0.134 Uiso 1 1 calc R . . C223 C 1.4113(10) 0.3211(7) 0.4867(4) 0.103(4) Uani 1 1 d . . . H22F H 1.3544 0.2814 0.5047 0.123 Uiso 1 1 calc R . . H22G H 1.5143 0.3303 0.5115 0.123 Uiso 1 1 calc R . . C224 C 1.3549(12) 0.4005(7) 0.5123(6) 0.107(3) Uani 1 1 d . . . H22H H 1.3609 0.4239 0.5687 0.160 Uiso 1 1 calc R . . H22I H 1.2518 0.3923 0.4897 0.160 Uiso 1 1 calc R . . H22J H 1.4122 0.4413 0.4966 0.160 Uiso 1 1 calc R . . C225 C 1.5399(8) 0.1865(7) 0.3770(5) 0.088(3) Uani 1 1 d . . . H22K H 1.5584 0.1579 0.3227 0.105 Uiso 1 1 calc R . . H22L H 1.6348 0.2167 0.4085 0.105 Uiso 1 1 calc R . . C226 C 1.4819(12) 0.1188(8) 0.4044(6) 0.106(3) Uani 1 1 d . . . H22M H 1.5520 0.0759 0.3981 0.159 Uiso 1 1 calc R . . H22N H 1.3869 0.0895 0.3740 0.159 Uiso 1 1 calc R . . H22O H 1.4688 0.1466 0.4590 0.159 Uiso 1 1 calc R . . C60 C 0.8123(19) -0.0999(14) 0.4928(10) 0.076(5) Uani 0.42 1 d P . . H61 H 0.9048 -0.1096 0.4692 0.091 Uiso 0.42 1 calc PR . . H62 H 0.7975 -0.1405 0.5190 0.091 Uiso 0.42 1 calc PR . . Cl61 Cl 0.6679(7) -0.1161(7) 0.4244(3) 0.135(3) Uani 0.42 1 d P . . Cl62 Cl 0.8209(15) 0.0109(4) 0.5604(5) 0.191(5) Uani 0.42 1 d P . . 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 0.02425(8) 0.05030(11) 0.02905(8) 0.02323(7) 0.01029(6) 0.00995(7) Pt2 0.03066(9) 0.04119(10) 0.02233(8) 0.00974(6) 0.00902(6) -0.00119(7) P11 0.0292(5) 0.0586(8) 0.0345(6) 0.0268(6) 0.0075(5) 0.0123(5) P12 0.0242(5) 0.0461(6) 0.0324(5) 0.0205(5) 0.0070(4) 0.0070(4) P21 0.0282(5) 0.0488(7) 0.0305(5) 0.0102(5) 0.0073(4) -0.0014(5) P22 0.0472(8) 0.0677(10) 0.0292(6) 0.0072(6) -0.0009(6) -0.0130(7) C1 0.031(2) 0.093(4) 0.035(2) 0.038(3) 0.0130(19) 0.020(3) C2 0.033(2) 0.092(5) 0.042(3) 0.040(3) 0.012(2) 0.007(3) C3 0.031(2) 0.092(4) 0.038(3) 0.033(3) 0.009(2) 0.009(3) C4 0.029(2) 0.078(4) 0.028(2) 0.027(2) 0.0092(18) 0.012(2) C5 0.031(2) 0.085(4) 0.035(2) 0.035(3) 0.0102(19) 0.016(2) N6 0.054(3) 0.088(4) 0.059(3) 0.035(3) 0.008(3) 0.006(3) C6 0.054(3) 0.088(4) 0.059(3) 0.035(3) 0.008(3) 0.006(3) C7 0.053(4) 0.080(5) 0.084(5) 0.019(4) 0.018(4) -0.002(4) C8 0.067(4) 0.079(5) 0.077(5) 0.034(4) 0.001(4) 0.001(4) C9 0.066(4) 0.089(5) 0.064(4) 0.029(4) 0.018(3) 0.015(4) N9 0.066(4) 0.089(5) 0.064(4) 0.029(4) 0.018(3) 0.015(4) C10 0.030(2) 0.095(4) 0.035(2) 0.037(3) 0.0118(19) 0.018(3) C11 0.039(3) 0.090(4) 0.040(3) 0.040(3) 0.014(2) 0.021(3) C12 0.031(2) 0.079(4) 0.039(2) 0.038(3) 0.013(2) 0.016(2) C41 0.035(2) 0.069(4) 0.033(2) 0.025(2) 0.0067(19) 0.004(2) C42 0.038(2) 0.057(3) 0.027(2) 0.014(2) 0.0079(18) -0.005(2) C101 0.026(2) 0.064(3) 0.043(2) 0.038(2) 0.0141(18) 0.016(2) C102 0.030(2) 0.074(4) 0.064(3) 0.048(3) 0.016(2) 0.016(2) C103 0.035(3) 0.118(6) 0.113(6) 0.097(6) 0.037(3) 0.033(3) C104 0.053(4) 0.140(7) 0.086(5) 0.093(5) 0.048(4) 0.054(4) C105 0.053(3) 0.108(6) 0.049(3) 0.042(4) 0.026(3) 0.042(4) C106 0.045(3) 0.073(4) 0.037(3) 0.031(3) 0.017(2) 0.022(3) C111 0.059(4) 0.088(5) 0.055(3) 0.041(3) 0.022(3) 0.042(3) C112 0.061(4) 0.112(6) 0.078(5) 0.055(5) 0.026(4) 0.053(4) C113 0.063(4) 0.135(8) 0.129(7) 0.109(7) 0.040(5) 0.048(5) C114 0.113(9) 0.127(10) 0.35(2) 0.163(14) -0.043(12) -0.041(8) C115 0.090(6) 0.078(5) 0.088(6) 0.005(4) -0.051(5) 0.027(5) C116 0.106(7) 0.091(7) 0.173(11) 0.065(7) -0.086(8) -0.025(6) C121 0.028(2) 0.073(4) 0.054(3) 0.045(3) 0.004(2) 0.005(2) C122 0.034(3) 0.085(4) 0.073(4) 0.061(4) 0.000(3) 0.003(3) C123 0.066(4) 0.051(3) 0.054(3) 0.008(3) -0.003(3) 0.021(3) C124 0.083(5) 0.054(4) 0.112(7) 0.009(4) -0.044(5) 0.005(4) C125 0.025(2) 0.061(3) 0.048(3) 0.034(2) 0.0109(19) 0.009(2) C126 0.049(3) 0.050(3) 0.072(4) 0.021(3) 0.002(3) -0.002(3) C201 0.0240(18) 0.042(2) 0.0209(17) 0.0099(16) 0.0035(15) -0.0008(16) C202 0.035(2) 0.047(3) 0.036(2) 0.020(2) 0.0102(19) 0.008(2) C203 0.037(2) 0.061(3) 0.033(2) 0.024(2) 0.0115(19) 0.007(2) C204 0.029(2) 0.062(3) 0.025(2) 0.008(2) 0.0088(17) 0.005(2) C205 0.030(2) 0.046(3) 0.036(2) 0.007(2) 0.0083(18) 0.0050(19) C206 0.032(2) 0.043(2) 0.032(2) 0.0153(19) 0.0058(17) 0.0013(18) C211 0.034(3) 0.081(4) 0.032(2) -0.002(3) 0.003(2) 0.006(3) C212 0.035(3) 0.076(4) 0.045(3) -0.004(3) -0.007(2) 0.003(3) C213 0.069(4) 0.080(5) 0.068(4) 0.036(4) -0.012(3) -0.037(4) C214 0.173(12) 0.082(7) 0.170(12) 0.081(8) -0.060(9) -0.040(7) C215 0.034(3) 0.070(4) 0.062(4) 0.004(3) 0.000(3) 0.011(3) C216 0.088(6) 0.087(6) 0.130(8) 0.056(6) -0.032(6) 0.011(5) C221 0.050(4) 0.106(6) 0.054(4) 0.010(4) 0.002(3) -0.028(4) C222 0.056(4) 0.099(6) 0.092(6) 0.021(5) -0.002(4) -0.014(4) C223 0.086(6) 0.128(8) 0.043(4) -0.012(4) 0.010(4) -0.043(6) C224 0.116(8) 0.094(7) 0.084(6) 0.010(5) 0.008(6) -0.005(6) C225 0.046(4) 0.140(8) 0.061(4) 0.027(5) -0.017(3) 0.005(4) C226 0.105(7) 0.134(9) 0.080(6) 0.051(6) -0.010(5) -0.004(7) C60 0.062(10) 0.111(15) 0.055(9) 0.029(9) 0.000(8) 0.038(10) Cl61 0.096(4) 0.267(10) 0.070(3) 0.081(5) 0.032(3) 0.093(5) Cl62 0.350(15) 0.065(4) 0.134(6) 0.011(4) 0.100(8) -0.054(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 P11 Pt1 2.2868(12) . ? P12 Pt1 2.2856(12) . ? P21 Pt2 2.2936(12) . ? P22 Pt2 2.2966(14) . ? C1 C2 1.373(9) . ? C1 C10 1.429(9) . ? C1 C11 1.435(7) . ? C2 C3 1.422(7) . ? C3 C4 1.383(8) . ? C4 C5 1.422(8) . ? C4 C41 1.438(6) . ? C5 C10 1.417(6) . ? C5 N6 1.455(8) . ? N6 C7 1.379(10) . ? C7 C8 1.435(11) . ? C8 C9 1.395(10) . ? C9 C10 1.491(10) . ? C11 C12 1.214(7) . ? C12 Pt1 2.007(5) . ? C41 C42 1.209(7) . ? C42 Pt2 2.019(5) . ? C101 C106 1.390(8) . ? C101 C102 1.405(8) . ? C101 Pt1 2.061(4) . ? C102 C103 1.390(8) . ? C103 C104 1.352(12) . ? C104 C105 1.368(11) . ? C105 C106 1.397(7) . ? C111 C112 1.529(8) . ? C111 P11 1.805(6) . ? C113 C114 1.553(17) . ? C113 P11 1.826(7) . ? C115 C116 1.354(13) . ? C115 P11 1.804(7) . ? C121 C122 1.519(7) . ? C121 P12 1.825(5) . ? C123 C124 1.538(10) . ? C123 P12 1.815(6) . ? C125 C126 1.527(8) . ? C125 P12 1.820(5) . ? C201 C206 1.401(7) . ? C201 C202 1.408(6) . ? C201 Pt2 2.061(4) . ? C202 C203 1.392(6) . ? C203 C204 1.386(8) . ? C204 C205 1.380(7) . ? C205 C206 1.389(6) . ? C211 C212 1.530(7) . ? C211 P21 1.830(5) . ? C213 C214 1.494(14) . ? C213 P21 1.810(7) . ? C215 C216 1.494(11) . ? C215 P21 1.819(6) . ? C221 C222 1.558(10) . ? C221 P22 1.837(8) . ? C223 C224 1.388(14) . ? C223 P22 1.805(7) . ? C225 C226 1.498(13) . ? C225 P22 1.845(9) . ? C60 Cl61 1.693(16) . ? C60 Cl62 1.80(2) . ? 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 C12 Pt1 C101 177.6(2) . . ? C12 Pt1 P12 86.54(14) . . ? C101 Pt1 P12 91.52(13) . . ? C12 Pt1 P11 90.17(14) . . ? C101 Pt1 P11 91.66(13) . . ? P12 Pt1 P11 174.83(5) . . ? C42 Pt2 C201 178.23(18) . . ? C42 Pt2 P21 87.41(14) . . ? C201 Pt2 P21 91.03(12) . . ? C42 Pt2 P22 93.73(15) . . ? C201 Pt2 P22 87.76(12) . . ? P21 Pt2 P22 175.85(6) . . ? C115 P11 C111 105.8(4) . . ? C115 P11 C113 102.6(5) . . ? C111 P11 C113 103.9(4) . . ? C115 P11 Pt1 111.8(3) . . ? C111 P11 Pt1 116.18(19) . . ? C113 P11 Pt1 115.1(2) . . ? C123 P12 C125 104.7(3) . . ? C123 P12 C121 104.0(3) . . ? C125 P12 C121 104.8(2) . . ? C123 P12 Pt1 110.3(2) . . ? C125 P12 Pt1 114.07(17) . . ? C121 P12 Pt1 117.78(17) . . ? C213 P21 C215 103.9(4) . . ? C213 P21 C211 104.5(4) . . ? C215 P21 C211 105.0(3) . . ? C213 P21 Pt2 111.3(2) . . ? C215 P21 Pt2 114.0(2) . . ? C211 P21 Pt2 116.89(18) . . ? C223 P22 C221 106.3(4) . . ? C223 P22 C225 102.0(5) . . ? C221 P22 C225 100.6(4) . . ? C223 P22 Pt2 119.0(3) . . ? C221 P22 Pt2 114.5(2) . . ? C225 P22 Pt2 112.2(3) . . ? C2 C1 C10 118.3(5) . . ? C2 C1 C11 121.0(6) . . ? C10 C1 C11 120.7(6) . . ? C1 C2 C3 121.2(6) . . ? C4 C3 C2 121.8(6) . . ? C3 C4 C5 117.8(5) . . ? C3 C4 C41 119.9(5) . . ? C5 C4 C41 122.2(5) . . ? C10 C5 C4 120.5(5) . . ? C10 C5 N6 119.1(6) . . ? C4 C5 N6 120.4(5) . . ? C7 N6 C5 122.2(6) . . ? N6 C7 C8 119.9(7) . . ? C9 C8 C7 119.8(8) . . ? C8 C9 C10 121.2(6) . . ? C5 C10 C1 120.3(6) . . ? C5 C10 C9 117.7(6) . . ? C1 C10 C9 122.0(5) . . ? C12 C11 C1 175.3(7) . . ? C11 C12 Pt1 175.4(5) . . ? C42 C41 C4 176.8(6) . . ? C41 C42 Pt2 178.0(5) . . ? C106 C101 C102 115.1(5) . . ? C106 C101 Pt1 123.2(4) . . ? C102 C101 Pt1 121.8(4) . . ? C103 C102 C101 122.2(7) . . ? C104 C103 C102 121.1(7) . . ? C103 C104 C105 118.6(5) . . ? C104 C105 C106 121.1(7) . . ? C101 C106 C105 121.9(6) . . ? C112 C111 P11 116.7(4) . . ? C114 C113 P11 111.5(7) . . ? C116 C115 P11 117.7(8) . . ? C122 C121 P12 116.4(4) . . ? C124 C123 P12 112.5(5) . . ? C126 C125 P12 112.0(4) . . ? C206 C201 C202 115.5(4) . . ? C206 C201 Pt2 122.0(3) . . ? C202 C201 Pt2 122.5(3) . . ? C203 C202 C201 122.6(5) . . ? C204 C203 C202 119.8(5) . . ? C205 C204 C203 119.3(4) . . ? C204 C205 C206 120.4(5) . . ? C205 C206 C201 122.4(4) . . ? C212 C211 P21 116.2(4) . . ? C214 C213 P21 113.3(7) . . ? C216 C215 P21 114.2(5) . . ? C222 C221 P22 115.4(6) . . ? C224 C223 P22 116.1(9) . . ? C226 C225 P22 111.8(7) . . ? Cl61 C60 Cl62 106.5(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.946 _refine_diff_density_min -2.259 _refine_diff_density_rms 0.140 ####END data_k01prr4 _database_code_CSD 192673 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H82 N2 P4 Pt2' _chemical_formula_weight 1345.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.33060(10) _cell_length_b 35.3016(4) _cell_length_c 18.0831(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.7930(10) _cell_angle_gamma 90.00 _cell_volume 5925.88(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31318 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 4.861 _exptl_absorpt_correction_type 'Sortav, Blessing 1995' _exptl_absorpt_correction_T_min 0.3233 _exptl_absorpt_correction_T_max 0.6421 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD Diffractometer' _diffrn_measurement_method '0.6 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30974 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12537 _reflns_number_gt 9359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Supergui' _computing_cell_refinement 'Nonius Supergui' _computing_data_reduction Maxus _computing_structure_solution 'DirDif 99' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WinGX _computing_publication_material WinGX _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^)+(0.0221P)^2^+12.3894P] 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 12537 _refine_ls_number_parameters 611 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.95075(2) 0.200547(7) 0.615975(11) 0.02516(7) Uani 1 1 d . . . Pt2 Pt 0.08980(2) 0.091187(7) 0.117628(11) 0.02823(7) Uani 1 1 d . A . P1 P 0.80443(16) 0.18719(5) 0.70673(8) 0.0303(4) Uani 1 1 d . . . P2 P 1.10251(16) 0.21370(5) 0.52739(8) 0.0323(4) Uani 1 1 d . . . P3 P -0.06728(16) 0.07425(5) 0.20113(8) 0.0340(4) Uani 1 1 d . . . P4 P 0.25779(17) 0.10338(5) 0.03676(8) 0.0332(4) Uani 1 1 d . . . N1 N 0.5254(5) 0.10302(15) 0.5234(2) 0.0293(11) Uani 1 1 d . . . N2 N 0.3503(5) 0.06823(14) 0.4078(2) 0.0283(11) Uani 1 1 d . . . C1 C 1.2838(7) 0.2704(2) 0.7940(3) 0.0448(18) Uani 1 1 d . . . H1 H 1.3492 0.2840 0.8278 0.054 Uiso 1 1 calc R . . C2 C 1.2890(6) 0.2316(2) 0.7914(3) 0.0428(17) Uani 1 1 d . . . H2 H 1.3580 0.2184 0.8240 0.051 Uiso 1 1 calc R . . C3 C 1.1942(6) 0.21129(19) 0.7416(3) 0.0357(15) Uani 1 1 d . . . H3 H 1.2015 0.1845 0.7401 0.043 Uiso 1 1 calc R . . C4 C 1.0881(5) 0.22965(18) 0.6936(3) 0.0265(13) Uani 1 1 d . . . C5 C 1.0865(6) 0.26882(19) 0.6984(3) 0.0364(15) Uani 1 1 d . . . H5 H 1.0163 0.2823 0.6670 0.044 Uiso 1 1 calc R . . C6 C 1.1821(7) 0.2896(2) 0.7468(3) 0.0403(16) Uani 1 1 d . . . H6 H 1.1777 0.3165 0.7475 0.048 Uiso 1 1 calc R . . C7 C 0.8119(6) 0.17465(18) 0.5394(3) 0.0298(14) Uani 1 1 d . . . C8 C 0.7239(6) 0.16109(16) 0.4939(3) 0.0258(13) Uani 1 1 d . . . C9 C 0.6206(6) 0.14571(17) 0.4370(3) 0.0268(13) Uani 1 1 d . . . C10 C 0.5257(6) 0.11578(17) 0.4526(3) 0.0270(13) Uani 1 1 d . . . C11 C 0.4292(5) 0.09944(17) 0.3944(3) 0.0249(13) Uani 1 1 d . . . C12 C 0.4184(6) 0.11599(18) 0.3215(3) 0.0275(13) Uani 1 1 d . . . C13 C 0.5083(6) 0.14620(18) 0.3096(3) 0.0316(14) Uani 1 1 d . . . H13 H 0.5020 0.1578 0.2620 0.038 Uiso 1 1 calc R . . C14 C 0.6084(6) 0.16015(18) 0.3662(3) 0.0317(14) Uani 1 1 d . . . H14 H 0.6700 0.1803 0.3550 0.038 Uiso 1 1 calc R . . C15 C 0.4406(6) 0.07392(18) 0.5362(3) 0.0301(14) Uani 1 1 d . . . C16 C 0.3578(6) 0.05470(17) 0.4763(3) 0.0281(13) Uani 1 1 d . . . C17 C 0.4355(6) 0.06420(18) 0.6167(3) 0.0346(15) Uani 1 1 d . . . C18 C 0.3081(7) 0.0662(2) 0.6493(3) 0.0417(17) Uani 1 1 d . . . H18 H 0.2219 0.0732 0.6200 0.050 Uiso 1 1 calc R . . C19 C 0.3039(8) 0.0580(2) 0.7233(4) 0.0483(18) Uani 1 1 d . . . H19 H 0.2158 0.0598 0.7453 0.058 Uiso 1 1 calc R . . C20 C 0.4289(9) 0.0473(2) 0.7655(4) 0.057(2) Uani 1 1 d . . . H20 H 0.4268 0.0416 0.8167 0.068 Uiso 1 1 calc R . . C21 C 0.5572(8) 0.0450(2) 0.7336(3) 0.0503(19) Uani 1 1 d . . . H21 H 0.6424 0.0369 0.7625 0.060 Uiso 1 1 calc R . . C22 C 0.5616(7) 0.0544(2) 0.6592(3) 0.0427(17) Uani 1 1 d . . . H22 H 0.6504 0.0541 0.6378 0.051 Uiso 1 1 calc R . . C23 C 0.2794(6) 0.01853(18) 0.4857(3) 0.0335(14) Uani 1 1 d . . . C24 C 0.3211(7) -0.00823(19) 0.5407(3) 0.0372(15) Uani 1 1 d . . . H24 H 0.4011 -0.0031 0.5761 0.045 Uiso 1 1 calc R . . C25 C 0.2481(7) -0.0418(2) 0.5443(4) 0.0449(17) Uani 1 1 d . . . H25 H 0.2761 -0.0592 0.5832 0.054 Uiso 1 1 calc R . . C26 C 0.1351(8) -0.0506(2) 0.4925(4) 0.058(2) Uani 1 1 d . . . H26 H 0.0872 -0.0743 0.4947 0.069 Uiso 1 1 calc R . . C27 C 0.0922(8) -0.0252(2) 0.4380(4) 0.059(2) Uani 1 1 d . . . H27 H 0.0141 -0.0313 0.4020 0.071 Uiso 1 1 calc R . . C28 C 0.1619(7) 0.0096(2) 0.4345(3) 0.0487(19) Uani 1 1 d . . . H28 H 0.1292 0.0273 0.3971 0.058 Uiso 1 1 calc R . . C29 C 0.3180(6) 0.10196(17) 0.2610(3) 0.0294(14) Uani 1 1 d . A . C30 C 0.2392(6) 0.09598(18) 0.2060(3) 0.0298(14) Uani 1 1 d . . . C31 C -0.0730(6) 0.0912(2) 0.0317(3) 0.0339(15) Uani 1 1 d . . . C32 C -0.1145(6) 0.0596(2) -0.0122(3) 0.0434(17) Uani 1 1 d . A . H32 H -0.0644 0.0364 -0.0032 0.052 Uiso 1 1 calc R . . C33 C -0.2274(7) 0.0615(3) -0.0688(3) 0.054(2) Uani 1 1 d . . . H33 H -0.2536 0.0394 -0.0970 0.065 Uiso 1 1 calc R A . C34 C -0.3008(7) 0.0942(3) -0.0844(3) 0.052(2) Uani 1 1 d . A . H34 H -0.3770 0.0950 -0.1233 0.063 Uiso 1 1 calc R . . C35 C -0.2639(6) 0.1259(2) -0.0435(3) 0.048(2) Uani 1 1 d . . . H35 H -0.3157 0.1488 -0.0537 0.057 Uiso 1 1 calc R A . C36 C -0.1506(6) 0.1249(2) 0.0134(3) 0.0402(17) Uani 1 1 d . A . H36 H -0.1251 0.1474 0.0404 0.048 Uiso 1 1 calc R . . C37 C 0.8917(6) 0.1579(2) 0.7805(3) 0.0435(18) Uani 1 1 d . . . H37A H 0.9762 0.1717 0.8050 0.052 Uiso 1 1 calc R . . H37B H 0.8238 0.1534 0.8183 0.052 Uiso 1 1 calc R . . C38 C 0.9401(8) 0.1207(2) 0.7527(4) 0.056(2) Uani 1 1 d . . . H38A H 0.9861 0.1059 0.7945 0.084 Uiso 1 1 calc R . . H38B H 1.0092 0.1249 0.7162 0.084 Uiso 1 1 calc R . . H38C H 0.8567 0.1067 0.7293 0.084 Uiso 1 1 calc R . . C39 C 0.6365(6) 0.16305(19) 0.6761(3) 0.0364(15) Uani 1 1 d . . . H39A H 0.5807 0.1793 0.6391 0.044 Uiso 1 1 calc R . . H39B H 0.6601 0.1394 0.6503 0.044 Uiso 1 1 calc R . . C40 C 0.5407(7) 0.1529(2) 0.7358(4) 0.0481(19) Uani 1 1 d . . . H40A H 0.4541 0.1400 0.7132 0.072 Uiso 1 1 calc R . . H40B H 0.5130 0.1760 0.7608 0.072 Uiso 1 1 calc R . . H40C H 0.5931 0.1361 0.7723 0.072 Uiso 1 1 calc R . . C41 C 0.7469(7) 0.2300(2) 0.7556(3) 0.0440(17) Uani 1 1 d . . . H41A H 0.6889 0.2222 0.7959 0.053 Uiso 1 1 calc R . . H41B H 0.8331 0.2435 0.7785 0.053 Uiso 1 1 calc R . . C42 C 0.6574(8) 0.2569(2) 0.7024(4) 0.060(2) Uani 1 1 d . . . H42A H 0.6287 0.2791 0.7301 0.089 Uiso 1 1 calc R . . H42B H 0.5713 0.2437 0.6802 0.089 Uiso 1 1 calc R . . H42C H 0.7154 0.2652 0.6631 0.089 Uiso 1 1 calc R . . C43 C 1.0961(7) 0.1792(2) 0.4524(4) 0.052(2) Uani 1 1 d . . . H43A H 0.9976 0.1786 0.4264 0.063 Uiso 1 1 calc R . . H43B H 1.1629 0.1871 0.4162 0.063 Uiso 1 1 calc R . . C44 C 1.1367(8) 0.1400(2) 0.4807(5) 0.067(2) Uani 1 1 d . . . H44A H 1.1319 0.1222 0.4388 0.100 Uiso 1 1 calc R . . H44B H 1.0697 0.1318 0.5160 0.100 Uiso 1 1 calc R . . H44C H 1.2349 0.1404 0.5057 0.100 Uiso 1 1 calc R . . C45 C 1.0613(8) 0.2600(2) 0.4823(4) 0.060(2) Uani 1 1 d . . . H45A H 1.0965 0.2803 0.5173 0.072 Uiso 1 1 calc R . . H45B H 1.1151 0.2620 0.4380 0.072 Uiso 1 1 calc R . . C46 C 0.9080(10) 0.2665(3) 0.4593(5) 0.090(3) Uani 1 1 d . . . H46A H 0.8954 0.2915 0.4362 0.135 Uiso 1 1 calc R . . H46B H 0.8537 0.2653 0.5029 0.135 Uiso 1 1 calc R . . H46C H 0.8724 0.2470 0.4235 0.135 Uiso 1 1 calc R . . C47 C 1.2939(6) 0.2177(2) 0.5610(4) 0.0476(18) Uani 1 1 d . . . H47A H 1.3050 0.2389 0.5969 0.057 Uiso 1 1 calc R . . H47B H 1.3227 0.1942 0.5886 0.057 Uiso 1 1 calc R . . C48 C 1.3992(7) 0.2240(2) 0.5027(4) 0.055(2) Uani 1 1 d . . . H48A H 1.4975 0.2257 0.5273 0.083 Uiso 1 1 calc R . . H48B H 1.3748 0.2476 0.4758 0.083 Uiso 1 1 calc R . . H48C H 1.3928 0.2028 0.4676 0.083 Uiso 1 1 calc R . . C49 C -0.0045(7) 0.0323(2) 0.2518(4) 0.057(2) Uani 1 1 d . . . H49A H 0.0900 0.0379 0.2797 0.069 Uiso 1 1 calc R . . H49B H -0.0730 0.0261 0.2884 0.069 Uiso 1 1 calc R . . C50 C 0.0110(10) -0.0015(3) 0.2027(6) 0.102(4) Uani 1 1 d . . . H50A H 0.0459 -0.0232 0.2333 0.153 Uiso 1 1 calc R . . H50B H 0.0799 0.0042 0.1668 0.153 Uiso 1 1 calc R . . H50C H -0.0828 -0.0077 0.1760 0.153 Uiso 1 1 calc R . . C51 C -0.0801(8) 0.1104(3) 0.2720(4) 0.066(3) Uani 1 1 d . . . H51A H -0.1461 0.1016 0.3079 0.080 Uiso 1 1 calc R . . H51B H 0.0161 0.1143 0.2994 0.080 Uiso 1 1 calc R . . C52 C -0.1348(10) 0.1478(3) 0.2383(5) 0.088(3) Uani 1 1 d . . . H52A H -0.1399 0.1666 0.2779 0.133 Uiso 1 1 calc R . . H52B H -0.2310 0.1442 0.2121 0.133 Uiso 1 1 calc R . . H52C H -0.0689 0.1568 0.2033 0.133 Uiso 1 1 calc R . . C53 C -0.2526(6) 0.0643(2) 0.1663(3) 0.0419(17) Uani 1 1 d . . . H53A H -0.2924 0.0870 0.1393 0.050 Uiso 1 1 calc R . . H53B H -0.2528 0.0435 0.1297 0.050 Uiso 1 1 calc R . . C54 C -0.3541(7) 0.0535(2) 0.2243(4) 0.0521(19) Uani 1 1 d . . . H54A H -0.4507 0.0488 0.1996 0.078 Uiso 1 1 calc R . . H54B H -0.3581 0.0743 0.2601 0.078 Uiso 1 1 calc R . . H54C H -0.3183 0.0306 0.2505 0.078 Uiso 1 1 calc R . . C55 C 0.1930(7) 0.1277(2) -0.0489(3) 0.052(2) Uani 1 1 d . A . H55A H 0.1152 0.1122 -0.0750 0.063 Uiso 1 1 calc R . . H55B H 0.1496 0.1520 -0.0355 0.063 Uiso 1 1 calc R . . C56 C 0.3029(7) 0.1360(2) -0.1031(3) 0.058(2) Uani 1 1 d . . . H56A H 0.2558 0.1492 -0.1467 0.087 Uiso 1 1 calc R A . H56B H 0.3445 0.1122 -0.1187 0.087 Uiso 1 1 calc R . . H56C H 0.3795 0.1521 -0.0789 0.087 Uiso 1 1 calc R . . C57 C 0.4144(6) 0.1299(2) 0.0740(4) 0.051(2) Uani 1 1 d . A . H57A H 0.4571 0.1175 0.1201 0.061 Uiso 1 1 calc R . . H57B H 0.4870 0.1294 0.0377 0.061 Uiso 1 1 calc R . . C58 C 0.3807(9) 0.1711(3) 0.0914(4) 0.074(3) Uani 1 1 d . . . H58A H 0.4694 0.1840 0.1115 0.111 Uiso 1 1 calc R A . H58B H 0.3105 0.1719 0.1282 0.111 Uiso 1 1 calc R . . H58C H 0.3408 0.1839 0.0458 0.111 Uiso 1 1 calc R . . C59A C 0.3067(17) 0.0584(4) -0.0060(8) 0.045(4) Uiso 0.50 1 d P A 1 H59A H 0.2185 0.0458 -0.0292 0.054 Uiso 0.50 1 calc PR A 1 H59B H 0.3702 0.0636 -0.0454 0.054 Uiso 0.50 1 calc PR A 1 C60A C 0.3851(17) 0.0318(5) 0.0531(8) 0.067(4) Uiso 0.50 1 d P A 1 H60A H 0.4104 0.0081 0.0294 0.100 Uiso 0.50 1 calc PR A 1 H60B H 0.3214 0.0263 0.0917 0.100 Uiso 0.50 1 calc PR A 1 H60C H 0.4729 0.0441 0.0757 0.100 Uiso 0.50 1 calc PR A 1 C59B C 0.3690(15) 0.0605(4) 0.0170(8) 0.038(3) Uiso 0.50 1 d P A 2 H59D H 0.4506 0.0682 -0.0106 0.045 Uiso 0.50 1 calc PR A 2 H59E H 0.4086 0.0486 0.0644 0.045 Uiso 0.50 1 calc PR A 2 C60B C 0.2779(17) 0.0332(5) -0.0272(9) 0.069(5) Uiso 0.50 1 d P A 2 H60D H 0.3351 0.0108 -0.0371 0.104 Uiso 0.50 1 calc PR A 2 H60E H 0.2404 0.0449 -0.0743 0.104 Uiso 0.50 1 calc PR A 2 H60F H 0.1974 0.0257 0.0004 0.104 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02498(12) 0.02640(14) 0.02371(11) -0.00130(9) 0.00054(8) -0.00114(9) Pt2 0.02591(12) 0.03654(16) 0.02160(11) 0.00072(10) -0.00081(8) -0.00309(10) P1 0.0293(8) 0.0363(11) 0.0256(7) -0.0019(7) 0.0040(6) -0.0034(7) P2 0.0333(9) 0.0335(11) 0.0309(8) 0.0040(7) 0.0063(7) -0.0003(7) P3 0.0308(9) 0.0433(12) 0.0279(8) 0.0054(7) 0.0031(6) -0.0031(7) P4 0.0357(9) 0.0386(11) 0.0261(8) 0.0024(7) 0.0064(6) 0.0004(7) N1 0.028(3) 0.036(3) 0.024(2) -0.002(2) 0.001(2) -0.001(2) N2 0.030(3) 0.033(3) 0.023(2) -0.001(2) 0.0051(19) 0.000(2) C1 0.043(4) 0.056(6) 0.036(4) -0.014(3) 0.007(3) -0.019(4) C2 0.034(4) 0.055(6) 0.039(4) 0.000(3) -0.005(3) -0.004(3) C3 0.036(4) 0.036(4) 0.034(3) -0.002(3) 0.001(3) -0.006(3) C4 0.021(3) 0.035(4) 0.022(3) -0.004(3) -0.002(2) -0.006(2) C5 0.041(4) 0.037(5) 0.030(3) -0.001(3) 0.000(3) -0.002(3) C6 0.049(4) 0.031(4) 0.041(4) -0.010(3) 0.006(3) -0.008(3) C7 0.028(3) 0.035(4) 0.027(3) -0.003(3) 0.001(2) -0.003(3) C8 0.031(3) 0.023(4) 0.024(3) -0.001(2) 0.007(2) 0.007(2) C9 0.027(3) 0.026(4) 0.027(3) -0.007(3) 0.005(2) 0.000(2) C10 0.027(3) 0.030(4) 0.023(3) -0.006(2) -0.001(2) 0.004(3) C11 0.022(3) 0.028(4) 0.025(3) -0.003(2) 0.003(2) 0.003(2) C12 0.026(3) 0.033(4) 0.024(3) -0.004(3) 0.001(2) 0.005(3) C13 0.037(3) 0.030(4) 0.027(3) 0.002(3) 0.002(3) 0.000(3) C14 0.026(3) 0.036(4) 0.033(3) 0.000(3) 0.002(2) -0.004(3) C15 0.031(3) 0.031(4) 0.028(3) 0.001(3) 0.003(2) 0.004(3) C16 0.025(3) 0.029(4) 0.030(3) -0.003(3) 0.002(2) -0.003(3) C17 0.040(4) 0.036(4) 0.028(3) -0.001(3) 0.003(3) -0.004(3) C18 0.047(4) 0.042(5) 0.037(3) 0.000(3) 0.009(3) -0.014(3) C19 0.065(5) 0.043(5) 0.040(4) -0.004(3) 0.020(4) -0.015(4) C20 0.089(6) 0.053(6) 0.028(3) 0.001(3) 0.012(4) -0.017(4) C21 0.066(5) 0.050(5) 0.032(4) 0.000(3) -0.007(3) -0.003(4) C22 0.053(4) 0.048(5) 0.028(3) 0.001(3) 0.005(3) -0.006(3) C23 0.038(3) 0.031(4) 0.033(3) -0.005(3) 0.012(3) -0.008(3) C24 0.038(4) 0.036(4) 0.038(3) -0.004(3) 0.006(3) -0.003(3) C25 0.050(4) 0.035(5) 0.052(4) -0.001(3) 0.019(3) 0.001(3) C26 0.068(5) 0.050(6) 0.060(5) -0.009(4) 0.025(4) -0.023(4) C27 0.063(5) 0.063(7) 0.052(4) -0.001(4) 0.010(4) -0.035(4) C28 0.050(4) 0.060(6) 0.035(3) 0.006(3) 0.001(3) -0.021(4) C29 0.029(3) 0.034(4) 0.025(3) 0.002(3) 0.002(2) 0.002(3) C30 0.023(3) 0.037(4) 0.029(3) 0.003(3) 0.003(2) -0.003(3) C31 0.026(3) 0.050(5) 0.025(3) 0.007(3) 0.000(2) -0.008(3) C32 0.038(4) 0.055(5) 0.036(3) 0.002(3) -0.005(3) -0.004(3) C33 0.043(4) 0.083(7) 0.034(4) 0.003(4) -0.012(3) -0.023(4) C34 0.035(4) 0.089(7) 0.030(3) 0.017(4) -0.009(3) -0.014(4) C35 0.029(4) 0.076(6) 0.039(4) 0.022(4) 0.006(3) 0.007(3) C36 0.037(4) 0.053(5) 0.030(3) 0.007(3) 0.003(3) -0.002(3) C37 0.031(4) 0.059(6) 0.039(4) 0.016(3) -0.004(3) 0.000(3) C38 0.054(5) 0.045(6) 0.066(5) 0.017(4) -0.001(4) 0.005(4) C39 0.029(3) 0.041(5) 0.038(3) -0.007(3) -0.001(3) -0.004(3) C40 0.036(4) 0.061(6) 0.049(4) -0.007(4) 0.012(3) -0.011(3) C41 0.042(4) 0.045(5) 0.047(4) -0.012(3) 0.012(3) -0.005(3) C42 0.054(5) 0.047(6) 0.077(5) -0.007(4) 0.006(4) 0.015(4) C43 0.053(4) 0.062(6) 0.044(4) -0.017(4) 0.019(3) -0.016(4) C44 0.059(5) 0.041(6) 0.104(7) -0.028(5) 0.026(4) -0.007(4) C45 0.058(5) 0.065(6) 0.058(5) 0.026(4) 0.007(4) 0.003(4) C46 0.102(8) 0.075(8) 0.089(7) 0.038(6) -0.007(6) 0.016(6) C47 0.041(4) 0.057(6) 0.046(4) -0.003(3) 0.007(3) -0.011(3) C48 0.042(4) 0.076(7) 0.048(4) -0.005(4) 0.008(3) 0.002(4) C49 0.035(4) 0.071(7) 0.068(5) 0.041(4) 0.012(3) 0.004(4) C50 0.113(8) 0.044(7) 0.163(10) 0.045(7) 0.080(7) 0.023(6) C51 0.062(5) 0.094(8) 0.049(4) -0.023(5) 0.032(4) -0.032(5) C52 0.108(7) 0.047(7) 0.124(8) -0.025(6) 0.076(6) -0.023(5) C53 0.031(3) 0.054(5) 0.042(4) 0.005(3) 0.009(3) -0.003(3) C54 0.044(4) 0.053(6) 0.060(4) 0.011(4) 0.010(3) 0.001(3) C55 0.048(4) 0.075(6) 0.033(3) 0.018(4) -0.002(3) -0.014(4) C56 0.058(5) 0.082(7) 0.036(4) 0.022(4) 0.006(3) -0.006(4) C57 0.029(4) 0.085(7) 0.039(4) 0.012(4) 0.001(3) -0.006(4) C58 0.081(6) 0.081(8) 0.057(5) -0.011(5) -0.003(4) -0.031(5) _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 C7 2.018(5) . ? Pt1 C4 2.075(5) . ? Pt1 P1 2.2873(15) . ? Pt1 P2 2.2902(15) . ? Pt2 C30 2.019(5) . ? Pt2 C31 2.060(5) . ? Pt2 P3 2.2874(15) . ? Pt2 P4 2.2899(15) . ? P1 C37 1.815(6) . ? P1 C39 1.820(6) . ? P1 C41 1.856(7) . ? P2 C43 1.818(7) . ? P2 C47 1.833(6) . ? P2 C45 1.849(7) . ? P3 C49 1.807(7) . ? P3 C53 1.814(6) . ? P3 C51 1.821(8) . ? P4 C57 1.808(7) . ? P4 C55 1.820(6) . ? P4 C59A 1.844(15) . ? P4 C59B 1.890(14) . ? N1 C15 1.331(7) . ? N1 C10 1.358(7) . ? N2 C16 1.322(7) . ? N2 C11 1.361(7) . ? C1 C2 1.371(9) . ? C1 C6 1.386(9) . ? C2 C3 1.395(8) . ? C3 C4 1.408(8) . ? C4 C5 1.386(8) . ? C5 C6 1.393(8) . ? C7 C8 1.202(7) . ? C8 C9 1.443(7) . ? C9 C14 1.372(7) . ? C9 C10 1.425(8) . ? C10 C11 1.435(7) . ? C11 C12 1.436(7) . ? C12 C13 1.387(8) . ? C12 C29 1.453(7) . ? C13 C14 1.402(7) . ? C15 C16 1.436(8) . ? C15 C17 1.502(7) . ? C16 C23 1.490(8) . ? C17 C18 1.381(8) . ? C17 C22 1.383(8) . ? C18 C19 1.374(8) . ? C19 C20 1.381(10) . ? C20 C21 1.383(10) . ? C21 C22 1.390(8) . ? C23 C28 1.398(8) . ? C23 C24 1.399(8) . ? C24 C25 1.372(9) . ? C25 C26 1.373(9) . ? C26 C27 1.364(10) . ? C27 C28 1.393(9) . ? C29 C30 1.194(7) . ? C31 C32 1.399(9) . ? C31 C36 1.416(9) . ? C32 C33 1.395(8) . ? C33 C34 1.357(10) . ? C34 C35 1.366(10) . ? C35 C36 1.399(8) . ? C37 C38 1.494(9) . ? C39 C40 1.513(8) . ? C41 C42 1.538(9) . ? C43 C44 1.512(10) . ? C45 C46 1.467(10) . ? C47 C48 1.528(8) . ? C49 C50 1.505(11) . ? C51 C52 1.521(12) . ? C53 C54 1.531(8) . ? C55 C56 1.517(8) . ? C57 C58 1.527(10) . ? C59A C60A 1.55(2) . ? C59B C60B 1.47(2) . ? 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 C7 Pt1 C4 177.2(2) . . ? C7 Pt1 P1 90.62(16) . . ? C4 Pt1 P1 89.38(15) . . ? C7 Pt1 P2 90.63(16) . . ? C4 Pt1 P2 89.41(15) . . ? P1 Pt1 P2 178.46(5) . . ? C30 Pt2 C31 174.0(3) . . ? C30 Pt2 P3 86.36(16) . . ? C31 Pt2 P3 91.41(16) . . ? C30 Pt2 P4 91.57(15) . . ? C31 Pt2 P4 91.08(16) . . ? P3 Pt2 P4 175.01(6) . . ? C37 P1 C39 105.4(3) . . ? C37 P1 C41 104.1(3) . . ? C39 P1 C41 104.2(3) . . ? C37 P1 Pt1 112.9(2) . . ? C39 P1 Pt1 115.83(19) . . ? C41 P1 Pt1 113.3(2) . . ? C43 P2 C47 104.9(3) . . ? C43 P2 C45 105.9(4) . . ? C47 P2 C45 103.3(3) . . ? C43 P2 Pt1 114.2(2) . . ? C47 P2 Pt1 115.7(2) . . ? C45 P2 Pt1 111.8(2) . . ? C49 P3 C53 105.5(3) . . ? C49 P3 C51 105.0(4) . . ? C53 P3 C51 104.6(3) . . ? C49 P3 Pt2 110.6(2) . . ? C53 P3 Pt2 118.2(2) . . ? C51 P3 Pt2 111.9(3) . . ? C57 P4 C55 105.0(3) . . ? C57 P4 C59A 112.2(6) . . ? C55 P4 C59A 97.2(5) . . ? C57 P4 C59B 92.7(5) . . ? C55 P4 C59B 111.0(5) . . ? C59A P4 C59B 21.1(5) . . ? C57 P4 Pt2 116.0(2) . . ? C55 P4 Pt2 116.3(2) . . ? C59A P4 Pt2 108.7(5) . . ? C59B P4 Pt2 113.2(4) . . ? C15 N1 C10 118.5(5) . . ? C16 N2 C11 118.8(5) . . ? C2 C1 C6 119.4(6) . . ? C1 C2 C3 120.9(6) . . ? C2 C3 C4 121.4(6) . . ? C5 C4 C3 115.6(5) . . ? C5 C4 Pt1 121.8(4) . . ? C3 C4 Pt1 122.5(5) . . ? C4 C5 C6 123.7(6) . . ? C1 C6 C5 119.0(7) . . ? C8 C7 Pt1 176.0(5) . . ? C7 C8 C9 177.7(6) . . ? C14 C9 C10 117.8(5) . . ? C14 C9 C8 120.8(5) . . ? C10 C9 C8 121.4(5) . . ? N1 C10 C9 119.6(5) . . ? N1 C10 C11 119.8(5) . . ? C9 C10 C11 120.6(5) . . ? N2 C11 C10 120.3(5) . . ? N2 C11 C12 120.3(5) . . ? C10 C11 C12 119.4(5) . . ? C13 C12 C11 117.8(5) . . ? C13 C12 C29 120.0(5) . . ? C11 C12 C29 122.2(5) . . ? C12 C13 C14 121.8(5) . . ? C9 C14 C13 122.4(6) . . ? N1 C15 C16 121.2(5) . . ? N1 C15 C17 115.0(5) . . ? C16 C15 C17 123.8(5) . . ? N2 C16 C15 120.6(5) . . ? N2 C16 C23 115.9(5) . . ? C15 C16 C23 123.5(5) . . ? C18 C17 C22 119.7(6) . . ? C18 C17 C15 121.1(5) . . ? C22 C17 C15 119.2(5) . . ? C19 C18 C17 121.1(6) . . ? C18 C19 C20 119.4(6) . . ? C19 C20 C21 120.2(6) . . ? C20 C21 C22 120.1(7) . . ? C17 C22 C21 119.4(6) . . ? C28 C23 C24 117.5(6) . . ? C28 C23 C16 118.7(6) . . ? C24 C23 C16 123.8(5) . . ? C25 C24 C23 120.9(6) . . ? C24 C25 C26 121.0(7) . . ? C27 C26 C25 119.5(7) . . ? C26 C27 C28 120.5(7) . . ? C27 C28 C23 120.6(7) . . ? C30 C29 C12 169.3(6) . . ? C29 C30 Pt2 172.6(5) . . ? C32 C31 C36 115.5(6) . . ? C32 C31 Pt2 124.7(5) . . ? C36 C31 Pt2 119.8(5) . . ? C33 C32 C31 121.6(7) . . ? C34 C33 C32 121.4(7) . . ? C33 C34 C35 119.3(6) . . ? C34 C35 C36 120.6(7) . . ? C35 C36 C31 121.5(7) . . ? C38 C37 P1 112.5(5) . . ? C40 C39 P1 116.4(4) . . ? C42 C41 P1 111.7(5) . . ? C44 C43 P2 111.9(5) . . ? C46 C45 P2 114.6(6) . . ? C48 C47 P2 117.1(5) . . ? C50 C49 P3 113.4(6) . . ? C52 C51 P3 111.7(6) . . ? C54 C53 P3 116.3(4) . . ? C56 C55 P4 116.9(5) . . ? C58 C57 P4 113.3(5) . . ? C60A C59A P4 110.7(11) . . ? C60B C59B P4 109.3(11) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.881 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.138 ####END data_k00prr17 _database_code_CSD 192674 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common k00prr17 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H72 N2 P4 Pt2 S' _chemical_formula_weight 1199.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.24500(10) _cell_length_b 38.0140(4) _cell_length_c 14.6550(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.0650(10) _cell_angle_gamma 90.00 _cell_volume 4973.33(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 65524 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 5.822 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.3239 _exptl_absorpt_correction_T_max 0.7595 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '726 0.5 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28015 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10244 _reflns_number_gt 7182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DirDif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-99' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0523P)^2^+13.6540P] 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 10244 _refine_ls_number_parameters 612 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.23478(3) 0.067793(9) -0.22811(2) 0.02070(9) Uani 1 1 d . A . Pt2 Pt 1.07228(3) 0.316161(11) -0.20847(3) 0.04337(13) Uani 1 1 d . A . P1 P 0.3774(2) 0.03312(6) -0.29798(14) 0.0218(4) Uani 1 1 d . . . P2 P 0.0927(2) 0.10142(6) -0.15451(15) 0.0280(5) Uani 1 1 d . . . P3 P 1.2272(3) 0.27815(11) -0.2596(2) 0.0767(13) Uani 1 1 d . . . P4 P 0.9086(2) 0.35219(8) -0.15922(18) 0.0395(6) Uani 1 1 d . . . S1 S 0.7018(3) 0.19803(8) 0.00040(18) 0.0517(7) Uani 1 1 d . . . N1 N 0.5872(8) 0.1733(2) -0.0735(5) 0.044(2) Uani 1 1 d . . . N2 N 0.7675(8) 0.2225(2) -0.0694(6) 0.044(2) Uani 1 1 d . A . C1 C -0.0198(10) -0.0376(3) -0.1565(6) 0.038(2) Uani 1 1 d . . . H1 H -0.0700 -0.0577 -0.1413 0.046 Uiso 1 1 calc R . . C2 C -0.0669(9) -0.0219(3) -0.2444(6) 0.034(2) Uani 1 1 d . . . H2 H -0.1496 -0.0315 -0.2903 0.041 Uiso 1 1 calc R . . C3 C 0.1027(9) -0.0233(3) -0.0906(6) 0.038(2) Uani 1 1 d . . . H3 H 0.1370 -0.0336 -0.0298 0.046 Uiso 1 1 calc R . . C4 C 0.0043(8) 0.0073(2) -0.2660(5) 0.0253(18) Uani 1 1 d . A . H4 H -0.0303 0.0176 -0.3269 0.030 Uiso 1 1 calc R . . C5 C 0.1748(9) 0.0062(2) -0.1140(6) 0.033(2) Uani 1 1 d . A . H5 H 0.2594 0.0154 -0.0688 0.040 Uiso 1 1 calc R . . C6 C 0.1275(8) 0.0225(2) -0.2006(5) 0.0209(17) Uani 1 1 d . . . C7 C 0.3466(9) 0.1120(2) -0.2449(6) 0.0287(19) Uani 1 1 d . . . C8 C 0.4211(10) 0.1378(3) -0.2483(6) 0.037(2) Uani 1 1 d . A . C9 C 0.5201(10) 0.1663(2) -0.2462(6) 0.037(2) Uani 1 1 d . . . C10 C 0.5480(12) 0.1810(3) -0.3261(8) 0.052(3) Uani 1 1 d . A . H10 H 0.4969 0.1714 -0.3857 0.062 Uiso 1 1 calc R . . C11 C 0.5964(9) 0.1829(2) -0.1593(6) 0.033(2) Uani 1 1 d . A . C12 C 0.6492(11) 0.2096(3) -0.3247(8) 0.051(3) Uani 1 1 d . . . H12 H 0.6638 0.2177 -0.3830 0.061 Uiso 1 1 calc R A . C13 C 0.7023(9) 0.2115(2) -0.1566(7) 0.038(2) Uani 1 1 d . . . C14 C 0.7267(10) 0.2259(2) -0.2419(7) 0.039(2) Uani 1 1 d . A . C15 C 0.8285(10) 0.2539(2) -0.2390(7) 0.039(2) Uani 1 1 d . . . C16 C 0.9164(10) 0.2778(3) -0.2328(7) 0.045(3) Uani 1 1 d . A . C17 C 1.2333(9) 0.3555(3) -0.1803(7) 0.042(3) Uani 1 1 d . . . C18 C 1.2506(8) 0.3802(2) -0.2473(6) 0.030(2) Uani 1 1 d . B . H18 H 1.1875 0.3785 -0.3097 0.036 Uiso 1 1 calc R . . C19 C 1.3282(9) 0.3600(3) -0.0895(7) 0.055(3) Uani 1 1 d . B . H19 H 1.3191 0.3443 -0.0409 0.066 Uiso 1 1 calc R . . C20 C 1.3545(9) 0.4065(3) -0.2270(6) 0.036(2) Uani 1 1 d . . . H20 H 1.3643 0.4225 -0.2749 0.043 Uiso 1 1 calc R B . C21 C 1.4314(10) 0.3857(3) -0.0683(7) 0.049(3) Uani 1 1 d . . . H21 H 1.4951 0.3871 -0.0060 0.059 Uiso 1 1 calc R B . C22 C 1.4469(9) 0.4099(3) -0.1346(6) 0.037(2) Uani 1 1 d . B . H22 H 1.5180 0.4284 -0.1185 0.044 Uiso 1 1 calc R . . C23 C 0.2682(8) 0.0099(2) -0.4019(5) 0.030(2) Uani 1 1 d . . . H23A H 0.3362 -0.0051 -0.4273 0.036 Uiso 1 1 calc R . . H23B H 0.1953 -0.0057 -0.3830 0.036 Uiso 1 1 calc R . . C24 C 0.1847(10) 0.0346(3) -0.4789(6) 0.050(3) Uani 1 1 d . . . H24A H 0.1285 0.0208 -0.5331 0.075 Uiso 1 1 calc R . . H24B H 0.2565 0.0498 -0.4987 0.075 Uiso 1 1 calc R . . H24C H 0.1151 0.0490 -0.4548 0.075 Uiso 1 1 calc R . . C25 C 0.4764(10) -0.0027(3) -0.2246(6) 0.041(2) Uani 1 1 d . . . H25A H 0.4016 -0.0186 -0.2090 0.049 Uiso 1 1 calc R . . H25B H 0.5321 -0.0164 -0.2619 0.049 Uiso 1 1 calc R . . C26 C 0.5848(12) 0.0090(4) -0.1338(7) 0.068(4) Uani 1 1 d . . . H26A H 0.6325 -0.0117 -0.0986 0.102 Uiso 1 1 calc R . . H26B H 0.5306 0.0221 -0.0955 0.102 Uiso 1 1 calc R . . H26C H 0.6616 0.0241 -0.1484 0.102 Uiso 1 1 calc R . . C27 C 0.5223(9) 0.0567(3) -0.3375(6) 0.036(2) Uani 1 1 d . . . H27A H 0.4754 0.0774 -0.3747 0.043 Uiso 1 1 calc R . . H27B H 0.5969 0.0656 -0.2810 0.043 Uiso 1 1 calc R . . C28 C 0.6059(9) 0.0358(3) -0.3973(6) 0.044(3) Uani 1 1 d . . . H28A H 0.6810 0.0509 -0.4139 0.066 Uiso 1 1 calc R . . H28B H 0.5345 0.0276 -0.4551 0.066 Uiso 1 1 calc R . . H28C H 0.6556 0.0155 -0.3610 0.066 Uiso 1 1 calc R . . C29 C -0.0728(14) 0.0824(4) -0.1355(9) 0.082(4) Uiso 1 1 d . A . H29A H -0.1343 0.0739 -0.1973 0.098 Uiso 1 1 calc R . . H29B H -0.0428 0.0615 -0.0947 0.098 Uiso 1 1 calc R . . C30 C -0.1715(13) 0.1047(3) -0.0921(10) 0.078(4) Uani 1 1 d . . . H30A H -0.2575 0.0908 -0.0857 0.117 Uiso 1 1 calc R A . H30B H -0.2070 0.1251 -0.1327 0.117 Uiso 1 1 calc R . . H30C H -0.1144 0.1128 -0.0297 0.117 Uiso 1 1 calc R . . C31 C 0.1837(19) 0.1012(6) -0.0216(13) 0.043(5) Uani 0.50 1 d P A 1 H31A H 0.1355 0.1199 0.0072 0.052 Uiso 0.50 1 calc PR A 1 H31B H 0.1590 0.0785 0.0038 0.052 Uiso 0.50 1 calc PR A 1 C32 C 0.3277(13) 0.1055(4) 0.0077(7) 0.079(4) Uani 0.50 1 d P A 1 H32A H 0.3500 0.1233 0.0579 0.095 Uiso 0.50 1 calc PR A 1 H32B H 0.3666 0.1134 -0.0450 0.095 Uiso 0.50 1 calc PR A 1 H32C H 0.3751 0.0832 0.0323 0.095 Uiso 0.50 1 calc PR A 1 C31A C 0.208(2) 0.1254(5) -0.0595(11) 0.037(4) Uani 0.50 1 d P A 2 H31C H 0.2549 0.1448 -0.0862 0.044 Uiso 0.50 1 calc PR A 2 H31D H 0.1422 0.1361 -0.0233 0.044 Uiso 0.50 1 calc PR A 2 C32A C 0.3277(13) 0.1055(4) 0.0077(7) 0.079(4) Uani 0.50 1 d P A 2 H32D H 0.3667 0.1197 0.0647 0.095 Uiso 0.50 1 calc PR A 2 H32E H 0.4088 0.1004 -0.0220 0.095 Uiso 0.50 1 calc PR A 2 H32F H 0.2868 0.0834 0.0248 0.095 Uiso 0.50 1 calc PR A 2 C33 C 0.0733(19) 0.1475(5) -0.1795(12) 0.036(4) Uiso 0.50 1 d P A 1 H33A H 0.0186 0.1587 -0.1374 0.044 Uiso 0.50 1 calc PR A 1 H33B H 0.1737 0.1584 -0.1672 0.044 Uiso 0.50 1 calc PR A 1 C34 C -0.011(2) 0.1535(6) -0.2812(14) 0.049(6) Uani 0.50 1 d P A 1 H34A H -0.0203 0.1788 -0.2938 0.074 Uiso 0.50 1 calc PR A 1 H34B H -0.1106 0.1429 -0.2931 0.074 Uiso 0.50 1 calc PR A 1 H34C H 0.0442 0.1426 -0.3227 0.074 Uiso 0.50 1 calc PR A 1 C33A C -0.011(2) 0.1354(5) -0.2394(12) 0.030(4) Uani 0.50 1 d P A 2 H33C H -0.0643 0.1514 -0.2059 0.036 Uiso 0.50 1 calc PR A 2 H33D H 0.0617 0.1496 -0.2629 0.036 Uiso 0.50 1 calc PR A 2 C34A C -0.1263(19) 0.1186(5) -0.3250(12) 0.041(5) Uani 0.50 1 d P A 2 H34D H -0.1781 0.1372 -0.3674 0.061 Uiso 0.50 1 calc PR A 2 H34E H -0.1995 0.1049 -0.3022 0.061 Uiso 0.50 1 calc PR A 2 H34F H -0.0738 0.1031 -0.3593 0.061 Uiso 0.50 1 calc PR A 2 C35 C 1.1160(16) 0.2524(5) -0.3846(11) 0.031(4) Uani 0.50 1 d P B 1 H35A H 1.0198 0.2434 -0.3761 0.038 Uiso 0.50 1 calc PR B 1 H35B H 1.0917 0.2702 -0.4355 0.038 Uiso 0.50 1 calc PR B 1 C36 C 1.1968(19) 0.2210(5) -0.4205(13) 0.040(5) Uani 0.50 1 d P B 1 H36A H 1.1315 0.2115 -0.4791 0.060 Uiso 0.50 1 calc PR B 1 H36B H 1.2187 0.2024 -0.3723 0.060 Uiso 0.50 1 calc PR B 1 H36C H 1.2905 0.2293 -0.4324 0.060 Uiso 0.50 1 calc PR B 1 C35A C 1.258(3) 0.2968(7) -0.3621(15) 0.069(7) Uani 0.50 1 d P B 2 H35C H 1.2948 0.3213 -0.3501 0.083 Uiso 0.50 1 calc PR B 2 H35D H 1.3325 0.2830 -0.3847 0.083 Uiso 0.50 1 calc PR B 2 C36A C 1.107(2) 0.2961(7) -0.4340(15) 0.070(7) Uani 0.50 1 d P B 2 H36D H 1.1165 0.3059 -0.4940 0.106 Uiso 0.50 1 calc PR B 2 H36E H 1.0349 0.3101 -0.4107 0.106 Uiso 0.50 1 calc PR B 2 H36F H 1.0713 0.2717 -0.4439 0.106 Uiso 0.50 1 calc PR B 2 C37 C 1.3988(16) 0.2860(5) -0.2822(11) 0.034(5) Uani 0.50 1 d P B 1 H37A H 1.4637 0.2982 -0.2269 0.041 Uiso 0.50 1 calc PR B 1 H37B H 1.4461 0.2630 -0.2884 0.041 Uiso 0.50 1 calc PR B 1 C38 C 1.394(2) 0.3074(6) -0.3691(16) 0.060(7) Uani 0.50 1 d P B 1 H38A H 1.4964 0.3102 -0.3762 0.091 Uiso 0.50 1 calc PR B 1 H38B H 1.3519 0.3307 -0.3629 0.091 Uiso 0.50 1 calc PR B 1 H38C H 1.3323 0.2955 -0.4248 0.091 Uiso 0.50 1 calc PR B 1 C37A C 1.4442(16) 0.2907(5) -0.1794(11) 0.035(4) Uani 0.50 1 d P B 2 H37C H 1.5165 0.2778 -0.2064 0.042 Uiso 0.50 1 calc PR B 2 H37D H 1.4607 0.3161 -0.1873 0.042 Uiso 0.50 1 calc PR B 2 C38A C 1.480(2) 0.2829(7) -0.0762(14) 0.066(7) Uani 0.50 1 d P B 2 H38D H 1.5833 0.2904 -0.0463 0.099 Uiso 0.50 1 calc PR B 2 H38E H 1.4708 0.2576 -0.0667 0.099 Uiso 0.50 1 calc PR B 2 H38F H 1.4110 0.2957 -0.0479 0.099 Uiso 0.50 1 calc PR B 2 C39 C 1.252(3) 0.2349(6) -0.1895(15) 0.037(6) Uani 0.50 1 d P B 1 H39A H 1.1548 0.2250 -0.1866 0.045 Uiso 0.50 1 calc PR B 1 H39B H 1.3070 0.2173 -0.2175 0.045 Uiso 0.50 1 calc PR B 1 C40 C 1.346(2) 0.2467(6) -0.0910(13) 0.052(6) Uani 0.50 1 d P B 1 H40A H 1.3655 0.2264 -0.0484 0.078 Uiso 0.50 1 calc PR B 1 H40B H 1.2898 0.2645 -0.0658 0.078 Uiso 0.50 1 calc PR B 1 H40C H 1.4408 0.2568 -0.0963 0.078 Uiso 0.50 1 calc PR B 1 C39A C 1.217(2) 0.2388(5) -0.2454(16) 0.036(5) Uani 0.50 1 d P B 2 H39C H 1.1261 0.2306 -0.2928 0.043 Uiso 0.50 1 calc PR B 2 H39D H 1.3035 0.2281 -0.2631 0.043 Uiso 0.50 1 calc PR B 2 C40A C 1.212(3) 0.2225(6) -0.1542(18) 0.059(7) Uani 0.50 1 d P B 2 H40D H 1.2062 0.1969 -0.1611 0.089 Uiso 0.50 1 calc PR B 2 H40E H 1.1234 0.2311 -0.1358 0.089 Uiso 0.50 1 calc PR B 2 H40F H 1.3024 0.2289 -0.1054 0.089 Uiso 0.50 1 calc PR B 2 C41 C 0.8519(18) 0.3270(5) -0.0700(12) 0.033(4) Uani 0.50 1 d P B 1 H41A H 0.7813 0.3412 -0.0448 0.039 Uiso 0.50 1 calc PR B 1 H41B H 0.7982 0.3057 -0.0995 0.039 Uiso 0.50 1 calc PR B 1 C42 C 0.982(2) 0.3162(6) 0.0103(13) 0.056(6) Uani 0.50 1 d P B 1 H42A H 0.9444 0.3027 0.0566 0.084 Uiso 0.50 1 calc PR B 1 H42B H 1.0342 0.3372 0.0406 0.084 Uiso 0.50 1 calc PR B 1 H42C H 1.0506 0.3016 -0.0139 0.084 Uiso 0.50 1 calc PR B 1 C41A C 0.7327(17) 0.3369(6) -0.1432(14) 0.046(5) Uani 0.50 1 d P B 2 H41C H 0.6703 0.3575 -0.1374 0.056 Uiso 0.50 1 calc PR B 2 H41D H 0.6795 0.3236 -0.2002 0.056 Uiso 0.50 1 calc PR B 2 C42A C 0.748(2) 0.3135(5) -0.0568(13) 0.041(5) Uani 0.50 1 d P B 2 H42D H 0.6480 0.3062 -0.0524 0.062 Uiso 0.50 1 calc PR B 2 H42E H 0.7982 0.3265 0.0003 0.062 Uiso 0.50 1 calc PR B 2 H42F H 0.8068 0.2926 -0.0627 0.062 Uiso 0.50 1 calc PR B 2 C43 C 0.7342(15) 0.3558(5) -0.2586(12) 0.035(4) Uani 0.50 1 d P B 1 H43A H 0.7022 0.3322 -0.2845 0.042 Uiso 0.50 1 calc PR B 1 H43B H 0.6523 0.3662 -0.2353 0.042 Uiso 0.50 1 calc PR B 1 C44 C 0.7679(11) 0.3796(3) -0.3368(7) 0.060(3) Uani 0.50 1 d P B 1 H44A H 0.6776 0.3818 -0.3891 0.091 Uiso 0.50 1 calc PR B 1 H44B H 0.8485 0.3691 -0.3598 0.091 Uiso 0.50 1 calc PR B 1 H44C H 0.7990 0.4029 -0.3106 0.091 Uiso 0.50 1 calc PR B 1 C43A C 0.850(2) 0.3937(5) -0.2330(12) 0.044(5) Uani 0.50 1 d P B 2 H43C H 0.7800 0.4080 -0.2070 0.053 Uiso 0.50 1 calc PR B 2 H43D H 0.9379 0.4082 -0.2343 0.053 Uiso 0.50 1 calc PR B 2 C44A C 0.7679(11) 0.3796(3) -0.3368(7) 0.060(3) Uani 0.50 1 d P B 2 H44D H 0.6698 0.3909 -0.3588 0.091 Uiso 0.50 1 calc PR B 2 H44E H 0.7548 0.3540 -0.3347 0.091 Uiso 0.50 1 calc PR B 2 H44F H 0.8294 0.3852 -0.3801 0.091 Uiso 0.50 1 calc PR B 2 C45 C 0.9739(17) 0.3919(5) -0.1208(13) 0.036(5) Uani 0.50 1 d P B 1 H45A H 1.0589 0.3892 -0.0641 0.044 Uiso 0.50 1 calc PR B 1 H45B H 1.0120 0.4036 -0.1703 0.044 Uiso 0.50 1 calc PR B 1 C46 C 0.8566(17) 0.4150(5) -0.0965(14) 0.042(5) Uani 0.50 1 d P B 1 H46A H 0.9007 0.4379 -0.0743 0.063 Uiso 0.50 1 calc PR B 1 H46B H 0.8197 0.4038 -0.0467 0.063 Uiso 0.50 1 calc PR B 1 H46C H 0.7732 0.4184 -0.1528 0.063 Uiso 0.50 1 calc PR B 1 C45A C 0.9826(18) 0.3787(5) -0.0360(13) 0.036(4) Uani 0.50 1 d P B 2 H45C H 1.0183 0.3610 0.0145 0.043 Uiso 0.50 1 calc PR B 2 H45D H 1.0710 0.3926 -0.0406 0.043 Uiso 0.50 1 calc PR B 2 C46A C 0.8769(19) 0.4035(6) -0.0030(14) 0.048(5) Uani 0.50 1 d P B 2 H46D H 0.9296 0.4141 0.0574 0.071 Uiso 0.50 1 calc PR B 2 H46E H 0.7901 0.3902 0.0051 0.071 Uiso 0.50 1 calc PR B 2 H46F H 0.8432 0.4220 -0.0502 0.071 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02046(15) 0.01840(18) 0.02461(16) -0.00117(13) 0.00834(11) -0.00199(13) Pt2 0.01953(17) 0.0342(3) 0.0779(3) 0.0295(2) 0.01534(16) 0.00136(16) P1 0.0185(9) 0.0225(12) 0.0242(10) -0.0010(9) 0.0053(8) 0.0026(9) P2 0.0293(11) 0.0247(14) 0.0344(12) -0.0023(10) 0.0162(9) 0.0003(10) P3 0.0589(17) 0.102(3) 0.088(2) 0.070(2) 0.0536(17) 0.054(2) P4 0.0191(10) 0.0490(18) 0.0513(15) 0.0195(13) 0.0106(10) -0.0020(11) S1 0.0583(16) 0.0467(19) 0.0506(15) 0.0014(13) 0.0153(12) -0.0110(14) N1 0.052(5) 0.034(5) 0.049(5) -0.005(4) 0.020(4) -0.005(4) N2 0.048(5) 0.029(5) 0.055(5) -0.002(4) 0.016(4) -0.010(4) C1 0.044(5) 0.031(6) 0.045(5) 0.002(4) 0.020(4) -0.011(5) C2 0.027(4) 0.035(6) 0.041(5) -0.001(4) 0.008(4) -0.002(4) C3 0.040(5) 0.036(6) 0.034(5) 0.009(4) 0.001(4) -0.010(5) C4 0.026(4) 0.025(5) 0.025(4) 0.005(4) 0.009(3) -0.001(4) C5 0.036(5) 0.028(6) 0.032(5) 0.005(4) 0.001(4) -0.008(4) C6 0.019(3) 0.017(5) 0.028(4) -0.004(3) 0.008(3) -0.007(3) C7 0.039(5) 0.016(5) 0.036(5) -0.010(4) 0.018(4) -0.010(4) C8 0.043(5) 0.026(6) 0.044(5) -0.007(4) 0.017(4) -0.003(5) C9 0.049(5) 0.020(5) 0.050(6) -0.005(4) 0.027(4) -0.012(5) C10 0.077(7) 0.030(6) 0.060(7) -0.011(5) 0.041(6) -0.009(6) C11 0.045(5) 0.019(5) 0.041(5) -0.006(4) 0.023(4) -0.005(4) C12 0.076(7) 0.024(6) 0.072(7) -0.005(5) 0.054(6) -0.011(5) C13 0.038(5) 0.015(5) 0.068(7) 0.000(5) 0.028(5) 0.000(4) C14 0.048(5) 0.011(5) 0.069(7) -0.002(4) 0.037(5) -0.005(4) C15 0.050(5) 0.013(5) 0.066(6) 0.003(4) 0.035(5) 0.003(4) C16 0.045(5) 0.030(6) 0.070(7) 0.009(5) 0.028(5) 0.000(5) C17 0.024(4) 0.042(7) 0.058(6) 0.020(5) 0.009(4) -0.009(4) C18 0.025(4) 0.022(5) 0.042(5) 0.004(4) 0.007(4) -0.001(4) C19 0.020(4) 0.085(10) 0.058(6) 0.032(6) 0.007(4) -0.004(5) C20 0.033(4) 0.029(6) 0.050(6) 0.002(4) 0.018(4) -0.002(4) C21 0.030(5) 0.075(9) 0.043(6) 0.005(6) 0.011(4) 0.009(5) C22 0.023(4) 0.032(6) 0.058(6) -0.019(5) 0.014(4) -0.007(4) C23 0.028(4) 0.031(6) 0.031(4) -0.010(4) 0.009(3) 0.000(4) C24 0.034(5) 0.077(9) 0.031(5) -0.007(5) -0.006(4) 0.008(5) C25 0.049(5) 0.033(6) 0.038(5) 0.002(4) 0.009(4) 0.019(5) C26 0.067(7) 0.088(11) 0.036(6) 0.006(6) -0.008(5) 0.022(7) C27 0.033(4) 0.040(6) 0.036(5) -0.011(4) 0.011(4) -0.003(4) C28 0.031(4) 0.064(8) 0.047(6) -0.008(5) 0.027(4) 0.004(5) C30 0.081(8) 0.049(8) 0.136(11) -0.009(8) 0.084(8) 0.012(7) C31 0.033(10) 0.045(15) 0.052(12) -0.001(10) 0.013(9) 0.003(10) C32 0.087(9) 0.118(13) 0.025(5) -0.008(6) 0.003(5) 0.041(8) C31A 0.051(11) 0.036(13) 0.026(9) 0.001(8) 0.015(8) 0.001(10) C32A 0.087(9) 0.118(13) 0.025(5) -0.008(6) 0.003(5) 0.041(8) C34 0.066(14) 0.026(13) 0.052(13) 0.014(10) 0.008(11) 0.026(11) C33A 0.044(11) 0.019(11) 0.031(10) 0.006(8) 0.018(8) 0.019(9) C34A 0.042(10) 0.039(13) 0.039(11) 0.011(9) 0.008(8) 0.011(10) C35 0.021(7) 0.049(13) 0.024(8) -0.008(8) 0.005(6) 0.016(8) C36 0.042(10) 0.034(12) 0.047(11) -0.012(9) 0.017(8) 0.008(9) C35A 0.076(16) 0.07(2) 0.058(14) -0.016(13) 0.015(12) 0.016(15) C36A 0.052(13) 0.09(2) 0.063(15) -0.020(14) 0.002(11) -0.003(14) C37 0.023(8) 0.055(14) 0.027(9) 0.010(9) 0.014(7) 0.011(8) C38 0.047(12) 0.046(15) 0.102(18) -0.034(13) 0.044(12) -0.035(11) C37A 0.023(8) 0.044(13) 0.041(10) 0.008(9) 0.013(7) 0.011(8) C38A 0.043(12) 0.09(2) 0.063(15) 0.007(14) 0.004(10) -0.018(13) C39 0.062(15) 0.032(13) 0.029(12) 0.025(11) 0.030(11) 0.017(11) C40 0.061(13) 0.050(15) 0.045(12) 0.011(10) 0.013(10) 0.009(12) C39A 0.036(11) 0.013(11) 0.054(14) 0.005(10) 0.004(10) 0.008(8) C40A 0.054(14) 0.028(15) 0.083(19) 0.021(13) -0.004(13) 0.009(11) C41 0.041(10) 0.017(10) 0.049(11) -0.007(8) 0.027(8) -0.008(8) C42 0.063(13) 0.073(18) 0.040(11) 0.015(11) 0.027(10) 0.038(12) C41A 0.018(8) 0.055(15) 0.070(13) 0.029(11) 0.019(8) 0.007(9) C42A 0.038(10) 0.026(12) 0.062(13) -0.005(9) 0.017(9) -0.010(9) C43 0.012(7) 0.036(12) 0.056(11) -0.010(9) 0.008(7) -0.004(8) C44 0.055(6) 0.068(9) 0.052(7) 0.025(6) 0.002(5) 0.010(6) C43A 0.042(10) 0.038(13) 0.049(12) 0.015(10) 0.006(9) 0.001(10) C44A 0.055(6) 0.068(9) 0.052(7) 0.025(6) 0.002(5) 0.010(6) C45 0.022(8) 0.038(13) 0.051(11) -0.022(9) 0.014(8) -0.012(8) C46 0.025(9) 0.030(12) 0.072(14) -0.027(10) 0.015(9) -0.016(8) C45A 0.035(9) 0.016(10) 0.061(12) -0.014(9) 0.021(9) -0.004(8) C46A 0.041(10) 0.049(15) 0.058(13) -0.022(11) 0.022(9) -0.021(10) _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 C7 2.021(8) . ? Pt1 C6 2.077(7) . ? Pt1 P1 2.286(2) . ? Pt1 P2 2.293(2) . ? Pt2 C16 2.015(10) . ? Pt2 C17 2.074(9) . ? Pt2 P4 2.292(3) . ? Pt2 P3 2.293(3) . ? P1 C23 1.821(8) . ? P1 C25 1.827(9) . ? P1 C27 1.827(8) . ? P2 C31A 1.767(18) . ? P2 C29 1.778(12) . ? P2 C33 1.788(19) . ? P2 C33A 1.876(18) . ? P2 C31 1.911(19) . ? P3 C39A 1.52(2) . ? P3 C37 1.728(14) . ? P3 C35A 1.75(2) . ? P3 C39 1.92(2) . ? P3 C35 2.096(16) . ? P3 C37A 2.100(16) . ? P4 C45 1.669(17) . ? P4 C41A 1.799(15) . ? P4 C41 1.805(16) . ? P4 C43 1.876(15) . ? P4 C43A 1.910(18) . ? P4 C45A 2.025(17) . ? S1 N1 1.608(8) . ? S1 N2 1.615(8) . ? N1 C11 1.333(11) . ? N2 C13 1.330(11) . ? C1 C2 1.384(12) . ? C1 C3 1.394(12) . ? C2 C4 1.369(11) . ? C3 C5 1.391(11) . ? C4 C6 1.409(10) . ? C5 C6 1.378(11) . ? C7 C8 1.207(11) . ? C8 C9 1.414(12) . ? C9 C10 1.380(12) . ? C9 C11 1.431(12) . ? C10 C12 1.432(13) . ? C11 C13 1.458(12) . ? C12 C14 1.385(13) . ? C13 C14 1.435(12) . ? C14 C15 1.414(12) . ? C15 C16 1.208(12) . ? C17 C18 1.398(11) . ? C17 C19 1.400(13) . ? C18 C20 1.366(12) . ? C19 C21 1.343(14) . ? C20 C22 1.407(12) . ? C21 C22 1.373(13) . ? C23 C24 1.515(12) . ? C25 C26 1.510(12) . ? C27 C28 1.531(11) . ? C29 C30 1.503(15) . ? C31 C32 1.298(19) . ? C33 C34 1.51(2) . ? C33A C34A 1.56(3) . ? C35 C36 1.57(2) . ? C35A C36A 1.52(3) . ? C37 C38 1.50(3) . ? C37A C38A 1.49(2) . ? C39 C40 1.54(3) . ? C39A C40A 1.48(3) . ? C41 C42 1.50(2) . ? C41A C42A 1.52(2) . ? C43 C44 1.55(2) . ? C45 C46 1.51(2) . ? C45A C46A 1.52(2) . ? 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 C7 Pt1 C6 175.9(3) . . ? C7 Pt1 P1 93.0(2) . . ? C6 Pt1 P1 88.2(2) . . ? C7 Pt1 P2 88.1(2) . . ? C6 Pt1 P2 90.6(2) . . ? P1 Pt1 P2 178.34(8) . . ? C16 Pt2 C17 178.7(4) . . ? C16 Pt2 P4 89.3(3) . . ? C17 Pt2 P4 90.3(3) . . ? C16 Pt2 P3 88.0(3) . . ? C17 Pt2 P3 92.4(3) . . ? P4 Pt2 P3 177.28(12) . . ? C23 P1 C25 102.4(4) . . ? C23 P1 C27 105.4(4) . . ? C25 P1 C27 104.8(4) . . ? C23 P1 Pt1 113.2(3) . . ? C25 P1 Pt1 115.2(3) . . ? C27 P1 Pt1 114.5(3) . . ? C31A P2 C29 116.8(7) . . ? C31A P2 C33 70.4(9) . . ? C29 P2 C33 112.7(7) . . ? C31A P2 C33A 105.5(9) . . ? C29 P2 C33A 94.1(7) . . ? C33 P2 C33A 35.2(7) . . ? C31A P2 C31 35.4(8) . . ? C29 P2 C31 90.4(7) . . ? C33 P2 C31 102.0(9) . . ? C33A P2 C31 133.9(9) . . ? C31A P2 Pt1 110.9(6) . . ? C29 P2 Pt1 117.9(5) . . ? C33 P2 Pt1 119.2(6) . . ? C33A P2 Pt1 109.2(5) . . ? C31 P2 Pt1 108.8(6) . . ? C39A P3 C37 106.8(10) . . ? C39A P3 C35A 123.3(12) . . ? C37 P3 C35A 53.4(9) . . ? C39A P3 C39 23.9(10) . . ? C37 P3 C39 105.1(9) . . ? C35A P3 C39 141.5(10) . . ? C39A P3 C35 68.0(10) . . ? C37 P3 C35 100.3(7) . . ? C35A P3 C35 65.9(10) . . ? C39 P3 C35 91.8(9) . . ? C39A P3 C37A 103.4(9) . . ? C37 P3 C37A 43.7(7) . . ? C35A P3 C37A 92.5(9) . . ? C39 P3 C37A 85.9(9) . . ? C35 P3 C37A 140.8(6) . . ? C39A P3 Pt2 120.6(8) . . ? C37 P3 Pt2 129.5(7) . . ? C35A P3 Pt2 106.2(8) . . ? C39 P3 Pt2 111.3(6) . . ? C35 P3 Pt2 112.0(4) . . ? C37A P3 Pt2 105.1(5) . . ? C45 P4 C41A 120.6(9) . . ? C45 P4 C41 112.6(9) . . ? C41A P4 C41 44.9(8) . . ? C45 P4 C43 110.9(9) . . ? C41A P4 C43 60.1(8) . . ? C41 P4 C43 104.4(8) . . ? C45 P4 C43A 57.9(9) . . ? C41A P4 C43A 101.9(8) . . ? C41 P4 C43A 138.9(8) . . ? C43 P4 C43A 55.8(8) . . ? C45 P4 C45A 40.6(8) . . ? C41A P4 C45A 98.7(9) . . ? C41 P4 C45A 73.3(8) . . ? C43 P4 C45A 132.7(8) . . ? C43A P4 C45A 94.3(8) . . ? C45 P4 Pt2 115.9(5) . . ? C41A P4 Pt2 122.8(7) . . ? C41 P4 Pt2 104.5(5) . . ? C43 P4 Pt2 107.7(6) . . ? C43A P4 Pt2 115.5(6) . . ? C45A P4 Pt2 118.7(5) . . ? N1 S1 N2 101.6(4) . . ? C11 N1 S1 106.4(6) . . ? C13 N2 S1 106.0(6) . . ? C2 C1 C3 118.6(8) . . ? C4 C2 C1 120.8(8) . . ? C5 C3 C1 119.9(8) . . ? C2 C4 C6 121.9(7) . . ? C6 C5 C3 122.2(8) . . ? C5 C6 C4 116.6(7) . . ? C5 C6 Pt1 119.9(6) . . ? C4 C6 Pt1 123.4(6) . . ? C8 C7 Pt1 175.0(8) . . ? C7 C8 C9 174.5(10) . . ? C10 C9 C8 123.6(9) . . ? C10 C9 C11 114.8(8) . . ? C8 C9 C11 121.6(8) . . ? C9 C10 C12 124.0(10) . . ? N1 C11 C9 125.5(8) . . ? N1 C11 C13 112.7(8) . . ? C9 C11 C13 121.7(8) . . ? C14 C12 C10 122.7(9) . . ? N2 C13 C14 125.6(9) . . ? N2 C13 C11 113.2(8) . . ? C14 C13 C11 121.1(9) . . ? C12 C14 C15 123.5(9) . . ? C12 C14 C13 115.5(8) . . ? C15 C14 C13 120.9(9) . . ? C16 C15 C14 177.5(11) . . ? C15 C16 Pt2 174.0(9) . . ? C18 C17 C19 115.2(9) . . ? C18 C17 Pt2 123.4(7) . . ? C19 C17 Pt2 121.2(7) . . ? C20 C18 C17 122.8(8) . . ? C21 C19 C17 122.8(9) . . ? C18 C20 C22 119.6(9) . . ? C19 C21 C22 121.4(9) . . ? C21 C22 C20 118.1(9) . . ? C24 C23 P1 112.8(6) . . ? C26 C25 P1 114.5(8) . . ? C28 C27 P1 116.6(7) . . ? C30 C29 P2 118.6(10) . . ? C32 C31 P2 118.5(13) . . ? C34 C33 P2 110.4(14) . . ? C34A C33A P2 112.1(13) . . ? C36 C35 P3 118.7(10) . . ? C36A C35A P3 105.2(17) . . ? C38 C37 P3 115.6(12) . . ? C38A C37A P3 116.9(12) . . ? C40 C39 P3 102.3(15) . . ? C40A C39A P3 123.5(18) . . ? C42 C41 P4 113.0(12) . . ? C42A C41A P4 114.0(12) . . ? C44 C43 P4 108.6(9) . . ? C46 C45 P4 112.8(11) . . ? C46A C45A P4 119.7(12) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 2.504 _refine_diff_density_min -3.848 _refine_diff_density_rms 0.196 ####END