# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jerzy Pikies' _publ_contact_author_email PIKIES@CHEM.PG.GDA.PL _publ_section_title ; Reactions of R2P-P(SiMe3)Li with [(R'3P)2PtCl2]. A General and Efficient Entrance to Phosphanylphosphinidene Complexes of Platinum. Syntheses and Structures of [(?2-P=PiPr2)Pt(p-Tol3P)2], [(?2-P=PtBu2)Pt(p-Tol3P)2], [{?2-P=P(NiPr2)2}Pt(p-Tol3P)2] and [{(Et2PhP)2Pt}2P2] ; _publ_requested_category FM loop_ _publ_author_name 'Jerzy Pikies' 'Jaroslaw Chojnacki' 'Wioleta Domanska-Babul' 'Eberhard Matern' #END data_compound_13 _database_code_depnum_ccdc_archive 'CCDC 668504' _audit_creation_date 2007-11-30T11:57:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C61 H78 N2 P4 Pt' _chemical_formula_moiety 'C54 H70 N2 P4 Pt, C7 H8' _chemical_formula_weight 1158.22 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 15.336(3) _cell_length_b 24.002(5) _cell_length_c 18.974(7) _cell_angle_alpha 90 _cell_angle_beta 125.737(19) _cell_angle_gamma 90 _cell_volume 5669(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14431 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.627 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.53879 _exptl_absorpt_correction_T_max 0.614 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k geometry, 4 circle diffractometer' _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method '\w--scans 0.75\%, 612 frames' _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0296 _diffrn_reflns_number 41630 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 13012 _reflns_number_gt 12026 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0229P)^2^+19.0456P] 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_number_reflns 13012 _refine_ls_number_parameters 622 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.245 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.128 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' 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' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 N 0.2838(2) 0.30765(10) 0.49684(16) 0.0136(5) Uani 1 1 d . . . N2 N 0.3490(2) 0.27117(11) 0.40443(17) 0.0169(5) Uani 1 1 d . . . P1 P 0.23504(6) 0.27763(3) 0.39844(5) 0.01331(14) Uani 1 1 d . . . P2 P 0.12042(6) 0.21580(3) 0.34588(5) 0.01623(15) Uani 1 1 d . . . P3 P -0.10662(6) 0.28134(3) 0.18132(5) 0.01356(14) Uani 1 1 d . . . P4 P 0.06385(6) 0.39325(3) 0.22771(5) 0.01359(14) Uani 1 1 d . . . Pt1 Pt 0.071788(8) 0.306162(4) 0.278794(7) 0.01181(4) Uani 1 1 d . . . C1 C 0.1452(3) 0.31613(16) 0.5295(2) 0.0254(7) Uani 1 1 d . . . H1A H 0.119 0.2798 0.5011 0.038 Uiso 1 1 calc R . . H1B H 0.0841 0.3395 0.5141 0.038 Uiso 1 1 calc R . . H1C H 0.1926 0.311 0.5926 0.038 Uiso 1 1 calc R . . C2 C 0.2077(3) 0.34440(14) 0.4992(2) 0.0186(6) Uani 1 1 d . . . H2 H 0.1524 0.3555 0.4375 0.022 Uiso 1 1 calc R . . C3 C 0.2583(3) 0.39906(14) 0.5486(2) 0.0241(7) Uani 1 1 d . . . H3A H 0.2977 0.3923 0.6111 0.036 Uiso 1 1 calc R . . H3B H 0.2016 0.4266 0.5303 0.036 Uiso 1 1 calc R . . H3C H 0.3078 0.4132 0.536 0.036 Uiso 1 1 calc R . . C4 C 0.3249(3) 0.22206(15) 0.5916(2) 0.0236(7) Uani 1 1 d . . . H4A H 0.2891 0.2331 0.6186 0.035 Uiso 1 1 calc R . . H4B H 0.3851 0.1972 0.631 0.035 Uiso 1 1 calc R . . H4C H 0.2736 0.2026 0.5369 0.035 Uiso 1 1 calc R . . C5 C 0.3669(3) 0.27397(14) 0.5735(2) 0.0207(6) Uani 1 1 d . . . H5 H 0.4156 0.2597 0.5587 0.025 Uiso 1 1 calc R . . C6 C 0.4381(3) 0.30862(15) 0.6552(2) 0.0254(7) Uani 1 1 d . . . H6A H 0.4641 0.3414 0.6418 0.038 Uiso 1 1 calc R . . H6B H 0.4995 0.2862 0.6997 0.038 Uiso 1 1 calc R . . H6C H 0.3967 0.3207 0.6769 0.038 Uiso 1 1 calc R . . C7 C 0.3036(3) 0.20646(16) 0.2823(2) 0.0298(8) Uani 1 1 d . . . H7A H 0.2332 0.1965 0.2685 0.045 Uiso 1 1 calc R . . H7B H 0.3325 0.1748 0.2695 0.045 Uiso 1 1 calc R . . H7C H 0.2958 0.2386 0.2471 0.045 Uiso 1 1 calc R . . C8 C 0.3800(3) 0.22128(14) 0.3782(2) 0.0233(7) Uani 1 1 d . . . H8 H 0.4503 0.2304 0.3887 0.028 Uiso 1 1 calc R . . C9 C 0.4012(3) 0.17184(15) 0.4357(3) 0.0296(8) Uani 1 1 d . . . H9A H 0.4605 0.1806 0.4958 0.044 Uiso 1 1 calc R . . H9B H 0.4202 0.1394 0.4159 0.044 Uiso 1 1 calc R . . H9C H 0.3364 0.1635 0.4327 0.044 Uiso 1 1 calc R . . C10 C 0.3837(3) 0.34004(16) 0.3229(2) 0.0284(8) Uani 1 1 d . . . H10A H 0.4199 0.3132 0.3092 0.043 Uiso 1 1 calc R . . H10B H 0.4128 0.3774 0.3283 0.043 Uiso 1 1 calc R . . H10C H 0.3064 0.3399 0.2764 0.043 Uiso 1 1 calc R . . C11 C 0.4022(2) 0.32368(15) 0.4090(2) 0.0200(6) Uani 1 1 d . . . H11 H 0.3693 0.3538 0.4228 0.024 Uiso 1 1 calc R . . C12 C 0.5219(3) 0.32353(17) 0.4823(3) 0.0299(8) Uani 1 1 d . . . H12A H 0.5322 0.3164 0.5376 0.045 Uiso 1 1 calc R . . H12B H 0.5529 0.3598 0.4848 0.045 Uiso 1 1 calc R . . H12C H 0.5575 0.2943 0.4717 0.045 Uiso 1 1 calc R . . C13 C -0.1797(2) 0.28296(13) 0.2312(2) 0.0147(6) Uani 1 1 d . . . C14 C -0.1227(2) 0.28487(14) 0.3209(2) 0.0185(6) Uani 1 1 d . . . H14 H -0.0468 0.2807 0.356 0.022 Uiso 1 1 calc R . . C15 C -0.1751(3) 0.29284(14) 0.3606(2) 0.0208(6) Uani 1 1 d . . . H15 H -0.1344 0.2935 0.4222 0.025 Uiso 1 1 calc R . . C16 C -0.2863(3) 0.29980(14) 0.3110(2) 0.0204(6) Uani 1 1 d . . . C17 C -0.3437(3) 0.29570(15) 0.2209(2) 0.0237(7) Uani 1 1 d . . . H17 H -0.4198 0.2989 0.186 0.028 Uiso 1 1 calc R . . C18 C -0.2925(3) 0.28703(15) 0.1810(2) 0.0207(6) Uani 1 1 d . . . H18 H -0.3337 0.2838 0.1196 0.025 Uiso 1 1 calc R . . C19 C -0.3436(3) 0.31136(16) 0.3526(3) 0.0282(8) Uani 1 1 d . . . H19A H -0.3945 0.3421 0.322 0.042 Uiso 1 1 calc R . . H19B H -0.2909 0.3216 0.4136 0.042 Uiso 1 1 calc R . . H19C H -0.3825 0.2779 0.3493 0.042 Uiso 1 1 calc R . . C20 C -0.1996(2) 0.32061(13) 0.08048(19) 0.0148(6) Uani 1 1 d . . . C21 C -0.2493(2) 0.36944(14) 0.0817(2) 0.0183(6) Uani 1 1 d . . . H21 H -0.2329 0.3829 0.1353 0.022 Uiso 1 1 calc R . . C22 C -0.3220(3) 0.39827(14) 0.0056(2) 0.0203(6) Uani 1 1 d . . . H22 H -0.3547 0.4312 0.0078 0.024 Uiso 1 1 calc R . . C23 C -0.3476(3) 0.37974(14) -0.0741(2) 0.0198(6) Uani 1 1 d . . . C24 C -0.2948(3) 0.33273(14) -0.0747(2) 0.0213(6) Uani 1 1 d . . . H24 H -0.3085 0.3204 -0.1279 0.026 Uiso 1 1 calc R . . C25 C -0.2225(3) 0.30363(13) 0.0012(2) 0.0179(6) Uani 1 1 d . . . H25 H -0.1879 0.2715 -0.0011 0.022 Uiso 1 1 calc R . . C26 C -0.4300(3) 0.41025(15) -0.1570(2) 0.0276(7) Uani 1 1 d . . . H26A H -0.4191 0.4014 -0.2017 0.041 Uiso 1 1 calc R . . H26B H -0.4221 0.4505 -0.1461 0.041 Uiso 1 1 calc R . . H26C H -0.5023 0.3987 -0.1768 0.041 Uiso 1 1 calc R . . C27 C -0.1212(2) 0.21055(13) 0.14054(19) 0.0150(6) Uani 1 1 d . . . C28 C -0.0537(3) 0.19329(13) 0.1174(2) 0.0191(6) Uani 1 1 d . . . H28 H 0.0002 0.2178 0.1257 0.023 Uiso 1 1 calc R . . C29 C -0.0651(3) 0.14063(14) 0.0826(2) 0.0214(7) Uani 1 1 d . . . H29 H -0.0208 0.1302 0.065 0.026 Uiso 1 1 calc R . . C30 C -0.1406(3) 0.10276(14) 0.0730(2) 0.0212(6) Uani 1 1 d . . . C31 C -0.2049(3) 0.11958(14) 0.0989(2) 0.0217(7) Uani 1 1 d . . . H31 H -0.2555 0.0942 0.0944 0.026 Uiso 1 1 calc R . . C32 C -0.1966(2) 0.17261(14) 0.1312(2) 0.0179(6) Uani 1 1 d . . . H32 H -0.2425 0.1833 0.1471 0.021 Uiso 1 1 calc R . . C33 C -0.1518(3) 0.04532(16) 0.0360(3) 0.0310(8) Uani 1 1 d . . . H33A H -0.1148 0.0182 0.0834 0.047 Uiso 1 1 calc R . . H33B H -0.1199 0.045 0.0039 0.047 Uiso 1 1 calc R . . H33C H -0.2281 0.0356 -0.0033 0.047 Uiso 1 1 calc R . . C34 C 0.0082(2) 0.39089(13) 0.11213(19) 0.0150(6) Uani 1 1 d . . . C35 C -0.0662(3) 0.42830(13) 0.0499(2) 0.0182(6) Uani 1 1 d . . . H35 H -0.0938 0.4572 0.0659 0.022 Uiso 1 1 calc R . . C36 C -0.1004(3) 0.42369(14) -0.0358(2) 0.0208(6) Uani 1 1 d . . . H36 H -0.1512 0.4497 -0.0776 0.025 Uiso 1 1 calc R . . C37 C -0.0618(3) 0.38184(14) -0.0619(2) 0.0203(6) Uani 1 1 d . . . C38 C 0.0134(3) 0.34484(15) 0.0006(2) 0.0224(7) Uani 1 1 d . . . H38 H 0.042 0.3165 -0.0154 0.027 Uiso 1 1 calc R . . C39 C 0.0475(3) 0.34871(13) 0.0862(2) 0.0183(6) Uani 1 1 d . . . H39 H 0.098 0.3225 0.1278 0.022 Uiso 1 1 calc R . . C40 C -0.1037(3) 0.37527(17) -0.1561(2) 0.0305(8) Uani 1 1 d . . . H40A H -0.1571 0.3453 -0.1826 0.046 Uiso 1 1 calc R . . H40B H -0.0441 0.3661 -0.1596 0.046 Uiso 1 1 calc R . . H40C H -0.1372 0.4102 -0.1872 0.046 Uiso 1 1 calc R . . C41 C 0.1842(2) 0.43613(13) 0.2697(2) 0.0160(6) Uani 1 1 d . . . C42 C 0.2103(3) 0.45954(15) 0.2172(2) 0.0227(7) Uani 1 1 d . . . H42 H 0.1688 0.4506 0.1571 0.027 Uiso 1 1 calc R . . C43 C 0.2969(3) 0.49584(16) 0.2521(2) 0.0280(8) Uani 1 1 d . . . H43 H 0.3146 0.5108 0.2156 0.034 Uiso 1 1 calc R . . C44 C 0.3579(3) 0.51070(16) 0.3394(2) 0.0282(8) Uani 1 1 d . . . C45 C 0.3319(3) 0.48698(15) 0.3917(2) 0.0259(7) Uani 1 1 d . . . H45 H 0.373 0.4963 0.4516 0.031 Uiso 1 1 calc R . . C46 C 0.2468(3) 0.44980(14) 0.3579(2) 0.0213(7) Uani 1 1 d . . . H46 H 0.2312 0.4336 0.395 0.026 Uiso 1 1 calc R . . C47 C 0.4471(4) 0.5531(2) 0.3746(3) 0.0488(12) Uani 1 1 d . . . H47A H 0.4809 0.5589 0.4366 0.073 Uiso 1 1 calc R . . H47B H 0.4173 0.5884 0.3435 0.073 Uiso 1 1 calc R . . H47C H 0.5009 0.5394 0.3664 0.073 Uiso 1 1 calc R . . C48 C -0.0136(2) 0.44426(13) 0.2420(2) 0.0162(6) Uani 1 1 d . . . C49 C -0.0216(3) 0.50062(14) 0.2186(2) 0.0230(7) Uani 1 1 d . . . H49 H 0.0125 0.5133 0.1929 0.028 Uiso 1 1 calc R . . C50 C -0.0790(3) 0.53765(14) 0.2330(2) 0.0265(7) Uani 1 1 d . . . H50 H -0.0835 0.5756 0.2169 0.032 Uiso 1 1 calc R . . C51 C -0.1303(3) 0.52072(16) 0.2703(3) 0.0290(8) Uani 1 1 d . . . C52 C -0.1198(3) 0.46551(16) 0.2958(2) 0.0270(7) Uani 1 1 d . . . H52 H -0.1527 0.4534 0.3228 0.032 Uiso 1 1 calc R . . C53 C -0.0615(3) 0.42745(15) 0.2826(2) 0.0206(6) Uani 1 1 d . . . H53 H -0.0545 0.39 0.3012 0.025 Uiso 1 1 calc R . . C54 C -0.1954(4) 0.5614(2) 0.2835(4) 0.0492(12) Uani 1 1 d . . . H54A H -0.1662 0.5991 0.2916 0.074 Uiso 1 1 calc R . . H54B H -0.1915 0.5506 0.3351 0.074 Uiso 1 1 calc R . . H54C H -0.2704 0.5609 0.2325 0.074 Uiso 1 1 calc R . . C55 C 0.4609(5) 0.4477(3) 0.0677(5) 0.0512(19) Uiso 0.703(8) 1 d PD A 1 H55 H 0.4481 0.4524 0.0127 0.061 Uiso 0.703(8) 1 calc PR A 1 C56 C 0.5649(6) 0.4518(5) 0.1428(5) 0.049(2) Uiso 0.703(8) 1 d PD A 1 H56 H 0.6228 0.458 0.1385 0.058 Uiso 0.703(8) 1 calc PR A 1 C57 C 0.5853(5) 0.4470(3) 0.2235(4) 0.0394(15) Uiso 0.703(8) 1 d PD A 1 H57 H 0.656 0.4516 0.2748 0.047 Uiso 0.703(8) 1 calc PR A 1 C58 C 0.5001(4) 0.4354(3) 0.2285(4) 0.0397(15) Uiso 0.703(8) 1 d PD A 1 H58 H 0.5129 0.4316 0.2836 0.048 Uiso 0.703(8) 1 calc PR A 1 C59 C 0.3965(5) 0.4294(3) 0.1535(4) 0.0408(16) Uiso 0.703(8) 1 d PD A 1 H59 H 0.3392 0.4201 0.1574 0.049 Uiso 0.703(8) 1 calc PR A 1 C60 C 0.3764(6) 0.4369(3) 0.0723(5) 0.047(2) Uiso 0.703(8) 1 d PD A 1 C61 C 0.2623(8) 0.4330(4) -0.0067(7) 0.077(3) Uiso 0.703(8) 1 d P A 1 H61A H 0.215 0.4249 0.011 0.115 Uiso 0.703(8) 1 calc PR A 1 H61B H 0.2562 0.4031 -0.0445 0.115 Uiso 0.703(8) 1 calc PR A 1 H61C H 0.2411 0.4684 -0.0383 0.115 Uiso 0.703(8) 1 calc PR A 1 C55A C 0.3699(9) 0.4498(6) 0.0112(8) 0.036(3) Uiso 0.297(8) 1 d PD A 2 H55A H 0.3125 0.4545 -0.0483 0.043 Uiso 0.297(8) 1 calc PR A 2 C56A C 0.4748(8) 0.4608(6) 0.0382(8) 0.036(3) Uiso 0.297(8) 1 d PD A 2 H56A H 0.488 0.4711 -0.0031 0.043 Uiso 0.297(8) 1 calc PR A 2 C57A C 0.5590(12) 0.4567(8) 0.1250(9) 0.034(4) Uiso 0.297(8) 1 d PD A 2 H57A H 0.6294 0.4674 0.1446 0.041 Uiso 0.297(8) 1 calc PR A 2 C58A C 0.5398(11) 0.4367(7) 0.1835(11) 0.046(4) Uiso 0.297(8) 1 d PD A 2 H58A H 0.5978 0.4298 0.2422 0.055 Uiso 0.297(8) 1 calc PR A 2 C59A C 0.4337(9) 0.4270(6) 0.1546(7) 0.036(3) Uiso 0.297(8) 1 d PD A 2 H59A H 0.4211 0.4165 0.1962 0.043 Uiso 0.297(8) 1 calc PR A 2 C60A C 0.3464(9) 0.4319(5) 0.0691(6) 0.016(3) Uiso 0.297(8) 1 d PD A 2 C61A C 0.2325(11) 0.4206(7) 0.0296(10) 0.038(3) Uiso 0.297(8) 1 d P A 2 H61D H 0.1902 0.4279 -0.0329 0.057 Uiso 0.297(8) 1 calc PR A 2 H61E H 0.2076 0.4447 0.0561 0.057 Uiso 0.297(8) 1 calc PR A 2 H61F H 0.2238 0.3815 0.0393 0.057 Uiso 0.297(8) 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 N1 0.0140(11) 0.0144(13) 0.0110(11) 0.0014(9) 0.0065(10) 0.0003(9) N2 0.0143(12) 0.0146(13) 0.0211(13) -0.0011(10) 0.0099(11) -0.0004(10) P1 0.0119(3) 0.0126(4) 0.0128(3) 0.0007(3) 0.0057(3) 0.0001(3) P2 0.0156(3) 0.0125(4) 0.0170(4) 0.0021(3) 0.0074(3) -0.0013(3) P3 0.0125(3) 0.0140(4) 0.0126(3) 0.0000(3) 0.0065(3) -0.0001(3) P4 0.0147(3) 0.0118(4) 0.0140(3) 0.0012(3) 0.0083(3) 0.0006(3) Pt1 0.01143(6) 0.01153(6) 0.01175(6) 0.00101(4) 0.00636(4) 0.00001(4) C1 0.0248(16) 0.035(2) 0.0220(17) -0.0009(14) 0.0167(14) -0.0011(14) C2 0.0190(14) 0.0227(17) 0.0154(14) 0.0009(12) 0.0106(12) 0.0017(12) C3 0.0333(18) 0.0183(16) 0.0225(16) 0.0011(13) 0.0173(15) 0.0057(14) C4 0.0247(16) 0.0222(17) 0.0203(16) 0.0041(13) 0.0112(14) 0.0022(13) C5 0.0186(14) 0.0205(16) 0.0173(15) 0.0032(12) 0.0072(13) 0.0013(12) C6 0.0200(16) 0.0291(19) 0.0165(16) 0.0018(13) 0.0047(13) -0.0004(13) C7 0.042(2) 0.0270(19) 0.0297(19) -0.0049(15) 0.0266(18) 0.0005(16) C8 0.0244(16) 0.0192(17) 0.0284(18) -0.0032(14) 0.0166(15) 0.0027(13) C9 0.037(2) 0.0198(18) 0.039(2) 0.0040(15) 0.0258(18) 0.0080(15) C10 0.0308(18) 0.0273(19) 0.0297(19) 0.0092(15) 0.0192(16) 0.0040(15) C11 0.0141(14) 0.0247(17) 0.0242(16) -0.0032(13) 0.0129(13) -0.0031(12) C12 0.0180(16) 0.036(2) 0.033(2) 0.0004(16) 0.0137(15) -0.0046(15) C13 0.0152(13) 0.0122(14) 0.0187(14) 0.0003(11) 0.0109(12) -0.0010(11) C14 0.0156(14) 0.0210(16) 0.0200(15) -0.0006(12) 0.0111(13) -0.0006(12) C15 0.0247(16) 0.0231(17) 0.0196(15) 0.0041(13) 0.0157(14) 0.0021(13) C16 0.0244(16) 0.0198(16) 0.0266(17) 0.0023(13) 0.0202(14) 0.0018(13) C17 0.0166(15) 0.0292(18) 0.0281(18) 0.0034(14) 0.0147(14) 0.0017(13) C18 0.0165(14) 0.0272(18) 0.0169(15) 0.0002(13) 0.0089(13) 0.0000(13) C19 0.0296(18) 0.034(2) 0.034(2) 0.0063(16) 0.0260(17) 0.0065(15) C20 0.0116(12) 0.0171(15) 0.0148(14) 0.0006(11) 0.0072(11) -0.0014(11) C21 0.0161(14) 0.0218(16) 0.0142(14) -0.0015(12) 0.0073(12) -0.0008(12) C22 0.0188(15) 0.0165(16) 0.0217(16) 0.0001(12) 0.0096(13) 0.0030(12) C23 0.0192(15) 0.0177(16) 0.0167(15) 0.0034(12) 0.0073(12) -0.0021(12) C24 0.0261(16) 0.0206(16) 0.0148(14) -0.0002(12) 0.0106(13) -0.0020(13) C25 0.0192(14) 0.0182(16) 0.0169(15) -0.0008(12) 0.0109(13) 0.0005(12) C26 0.0286(17) 0.0229(18) 0.0220(17) 0.0049(14) 0.0095(15) 0.0017(14) C27 0.0129(13) 0.0152(15) 0.0133(13) 0.0025(11) 0.0056(11) 0.0025(11) C28 0.0207(15) 0.0179(16) 0.0220(16) 0.0001(12) 0.0144(13) -0.0021(12) C29 0.0267(16) 0.0202(16) 0.0218(16) -0.0009(13) 0.0167(14) 0.0019(13) C30 0.0257(16) 0.0157(16) 0.0170(15) 0.0003(12) 0.0095(13) 0.0026(13) C31 0.0199(15) 0.0193(16) 0.0228(16) -0.0013(13) 0.0107(13) -0.0041(12) C32 0.0152(13) 0.0213(16) 0.0169(14) -0.0016(12) 0.0092(12) -0.0016(12) C33 0.039(2) 0.0208(18) 0.033(2) -0.0067(15) 0.0214(18) -0.0023(15) C34 0.0164(13) 0.0149(14) 0.0142(14) 0.0004(11) 0.0091(12) -0.0025(11) C35 0.0212(15) 0.0147(15) 0.0190(15) 0.0010(12) 0.0119(13) 0.0040(12) C36 0.0248(16) 0.0175(16) 0.0182(15) 0.0053(12) 0.0115(13) 0.0046(13) C37 0.0255(16) 0.0209(17) 0.0170(15) -0.0002(12) 0.0139(13) 0.0001(13) C38 0.0268(16) 0.0219(17) 0.0231(16) -0.0009(13) 0.0173(14) 0.0034(13) C39 0.0197(14) 0.0154(15) 0.0192(15) 0.0038(12) 0.0110(13) 0.0044(12) C40 0.044(2) 0.029(2) 0.0194(17) -0.0001(14) 0.0192(16) 0.0058(16) C41 0.0173(14) 0.0124(14) 0.0160(14) 0.0012(11) 0.0084(12) 0.0003(11) C42 0.0215(15) 0.0239(17) 0.0185(15) 0.0041(13) 0.0094(13) -0.0025(13) C43 0.0238(16) 0.0274(19) 0.0274(18) 0.0099(15) 0.0119(15) -0.0053(14) C44 0.0214(16) 0.0228(18) 0.0293(18) 0.0046(14) 0.0086(14) -0.0061(14) C45 0.0245(16) 0.0234(18) 0.0200(16) -0.0040(13) 0.0074(14) -0.0061(14) C46 0.0225(15) 0.0180(16) 0.0229(16) 0.0019(13) 0.0129(14) 0.0003(12) C47 0.041(2) 0.048(3) 0.038(2) 0.002(2) 0.011(2) -0.026(2) C48 0.0187(14) 0.0121(14) 0.0161(14) -0.0038(11) 0.0092(12) -0.0002(11) C49 0.0273(17) 0.0190(16) 0.0199(16) -0.0005(13) 0.0123(14) 0.0012(13) C50 0.0332(18) 0.0082(15) 0.0319(19) 0.0010(13) 0.0156(16) 0.0043(13) C51 0.0264(17) 0.0237(18) 0.0328(19) -0.0091(15) 0.0150(16) 0.0061(14) C52 0.0275(17) 0.031(2) 0.0277(18) -0.0069(15) 0.0191(15) -0.0004(15) C53 0.0208(15) 0.0219(17) 0.0196(15) -0.0025(13) 0.0121(13) -0.0001(13) C54 0.050(3) 0.041(3) 0.065(3) -0.012(2) 0.038(3) 0.011(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 Pt1 2.2916(11) . ? P2 Pt1 2.4024(9) . ? P3 Pt1 2.3131(10) . ? P4 Pt1 2.2773(9) . ? P1 P2 2.0590(12) . ? N1 C2 1.484(4) . ? N1 C5 1.493(4) . ? N1 P1 1.713(3) . ? N2 C11 1.477(4) . ? N2 C8 1.478(4) . ? N2 P1 1.691(3) . ? P3 C27 1.826(3) . ? P3 C13 1.842(3) . ? P3 C20 1.843(3) . ? P4 C34 1.831(3) . ? P4 C48 1.834(3) . ? P4 C41 1.839(3) . ? C1 C2 1.534(4) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.534(5) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C5 1.530(5) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.520(5) . ? C5 H5 1 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.524(5) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.513(5) . ? C8 H8 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.536(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.523(5) . ? C11 H11 1 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.389(4) . ? C13 C18 1.408(4) . ? C14 C15 1.399(4) . ? C14 H14 0.95 . ? C15 C16 1.396(5) . ? C15 H15 0.95 . ? C16 C17 1.396(5) . ? C16 C19 1.511(4) . ? C17 C18 1.389(5) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C25 1.392(4) . ? C20 C21 1.405(4) . ? C21 C22 1.388(4) . ? C21 H21 0.95 . ? C22 C23 1.395(5) . ? C22 H22 0.95 . ? C23 C24 1.393(5) . ? C23 C26 1.511(4) . ? C24 C25 1.388(4) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C32 1.399(4) . ? C27 C28 1.402(4) . ? C28 C29 1.389(5) . ? C28 H28 0.95 . ? C29 C30 1.397(5) . ? C29 H29 0.95 . ? C30 C31 1.396(5) . ? C30 C33 1.510(5) . ? C31 C32 1.385(5) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 C35 1.388(4) . ? C34 C39 1.406(4) . ? C35 C36 1.392(4) . ? C35 H35 0.95 . ? C36 C37 1.394(5) . ? C36 H36 0.95 . ? C37 C38 1.389(5) . ? C37 C40 1.514(5) . ? C38 C39 1.388(5) . ? C38 H38 0.95 . ? C39 H39 0.95 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C42 1.392(4) . ? C41 C46 1.397(4) . ? C42 C43 1.390(5) . ? C42 H42 0.95 . ? C43 C44 1.391(5) . ? C43 H43 0.95 . ? C44 C45 1.390(5) . ? C44 C47 1.511(5) . ? C45 C46 1.390(5) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 C53 1.398(4) . ? C48 C49 1.407(5) . ? C49 C50 1.386(5) . ? C49 H49 0.95 . ? C50 C51 1.391(6) . ? C50 H50 0.95 . ? C51 C52 1.388(6) . ? C51 C54 1.519(5) . ? C52 C53 1.399(5) . ? C52 H52 0.95 . ? C53 H53 0.95 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 C60 1.374(8) . ? C55 C56 1.389(8) . ? C55 H55 0.95 . ? C56 C57 1.377(8) . ? C56 H56 0.95 . ? C57 C58 1.392(7) . ? C57 H57 0.95 . ? C58 C59 1.389(7) . ? C58 H58 0.95 . ? C59 C60 1.394(7) . ? C59 H59 0.95 . ? C60 C61 1.502(12) . ? C61 H61A 0.98 . ? C61 H61B 0.98 . ? C61 H61C 0.98 . ? C55A C56A 1.399(9) . ? C55A C60A 1.407(9) . ? C55A H55A 0.95 . ? C56A C57A 1.380(9) . ? C56A H56A 0.95 . ? C57A C58A 1.388(9) . ? C57A H57A 0.95 . ? C58A C59A 1.401(9) . ? C58A H58A 0.95 . ? C59A C60A 1.379(9) . ? C59A H59A 0.95 . ? C60A C61A 1.469(18) . ? C61A H61D 0.98 . ? C61A H61E 0.98 . ? C61A H61F 0.98 . ? 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 P1 Pt1 P2 51.97(3) . . ? P1 Pt1 P3 144.37(3) . . ? P3 Pt1 P2 92.71(3) . . ? P4 Pt1 P1 116.86(3) . . ? P4 Pt1 P3 98.74(3) . . ? P4 Pt1 P2 167.71(3) . . ? C2 N1 C5 122.1(2) . . ? C2 N1 P1 115.6(2) . . ? C5 N1 P1 114.5(2) . . ? C11 N2 C8 115.9(3) . . ? C11 N2 P1 116.1(2) . . ? C8 N2 P1 125.1(2) . . ? N2 P1 N1 100.92(13) . . ? N2 P1 P2 121.53(10) . . ? N1 P1 P2 122.46(10) . . ? N2 P1 Pt1 125.61(10) . . ? N1 P1 Pt1 118.87(9) . . ? P2 P1 Pt1 66.79(4) . . ? P1 P2 Pt1 61.24(4) . . ? C27 P3 C13 106.05(14) . . ? C27 P3 C20 101.95(14) . . ? C13 P3 C20 100.84(14) . . ? C27 P3 Pt1 111.93(10) . . ? C13 P3 Pt1 112.00(10) . . ? C20 P3 Pt1 122.36(10) . . ? C34 P4 C48 108.00(14) . . ? C34 P4 C41 100.62(14) . . ? C48 P4 C41 97.76(14) . . ? C34 P4 Pt1 110.66(10) . . ? C48 P4 Pt1 115.34(11) . . ? C41 P4 Pt1 122.59(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 113.6(3) . . ? N1 C2 C1 115.0(3) . . ? C3 C2 C1 110.6(3) . . ? N1 C2 H2 105.5 . . ? C3 C2 H2 105.5 . . ? C1 C2 H2 105.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 113.2(3) . . ? N1 C5 C4 115.3(3) . . ? C6 C5 C4 111.3(3) . . ? N1 C5 H5 105.3 . . ? C6 C5 H5 105.3 . . ? C4 C5 H5 105.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 111.6(3) . . ? N2 C8 C7 114.6(3) . . ? C9 C8 C7 111.7(3) . . ? N2 C8 H8 106 . . ? C9 C8 H8 106 . . ? C7 C8 H8 106 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 112.4(3) . . ? N2 C11 C10 113.8(3) . . ? C12 C11 C10 110.4(3) . . ? N2 C11 H11 106.6 . . ? C12 C11 H11 106.6 . . ? C10 C11 H11 106.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P3 119.6(2) . . ? C18 C13 P3 122.0(2) . . ? C13 C14 C15 121.1(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 117.8(3) . . ? C15 C16 C19 121.6(3) . . ? C17 C16 C19 120.6(3) . . ? C18 C17 C16 121.7(3) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.8(3) . . ? C25 C20 P3 121.7(2) . . ? C21 C20 P3 120.5(2) . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 121.1(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 118.0(3) . . ? C24 C23 C26 121.4(3) . . ? C22 C23 C26 120.6(3) . . ? C25 C24 C23 121.0(3) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C20 121.2(3) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.3(3) . . ? C32 C27 P3 123.2(2) . . ? C28 C27 P3 118.5(2) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 121.2(3) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 117.9(3) . . ? C31 C30 C33 121.0(3) . . ? C29 C30 C33 121.1(3) . . ? C32 C31 C30 121.3(3) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C27 120.7(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 118.4(3) . . ? C35 C34 P4 125.1(2) . . ? C39 C34 P4 116.5(2) . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C37 121.5(3) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C38 C37 C36 118.1(3) . . ? C38 C37 C40 120.6(3) . . ? C36 C37 C40 121.2(3) . . ? C39 C38 C37 120.9(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C34 120.8(3) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 118.6(3) . . ? C42 C41 P4 123.5(2) . . ? C46 C41 P4 117.7(2) . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 121.3(3) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C45 C44 C43 118.1(3) . . ? C45 C44 C47 121.6(4) . . ? C43 C44 C47 120.3(4) . . ? C44 C45 C46 121.1(3) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C41 120.5(3) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 118.4(3) . . ? C53 C48 P4 118.9(2) . . ? C49 C48 P4 122.6(2) . . ? C50 C49 C48 120.2(3) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 121.7(3) . . ? C49 C50 H50 119.1 . . ? C51 C50 H50 119.1 . . ? C52 C51 C50 118.2(3) . . ? C52 C51 C54 120.6(4) . . ? C50 C51 C54 121.2(4) . . ? C51 C52 C53 121.1(3) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C48 C53 C52 120.4(3) . . ? C48 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C60 C55 C56 120.6(7) . . ? C60 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C57 C56 C55 120.9(8) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 118.7(7) . . ? C56 C57 H57 120.7 . . ? C58 C57 H57 120.7 . . ? C59 C58 C57 120.6(6) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C58 C59 C60 120.0(7) . . ? C58 C59 H59 120 . . ? C60 C59 H59 120 . . ? C55 C60 C59 119.1(7) . . ? C55 C60 C61 122.8(7) . . ? C59 C60 C61 118.1(7) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C56A C55A C60A 122.4(12) . . ? C56A C55A H55A 118.8 . . ? C60A C55A H55A 118.8 . . ? C57A C56A C55A 119.9(13) . . ? C57A C56A H56A 120.1 . . ? C55A C56A H56A 120.1 . . ? C56A C57A C58A 119.4(14) . . ? C56A C57A H57A 120.3 . . ? C58A C57A H57A 120.3 . . ? C57A C58A C59A 119.0(14) . . ? C57A C58A H58A 120.5 . . ? C59A C58A H58A 120.5 . . ? C60A C59A C58A 123.6(14) . . ? C60A C59A H59A 118.2 . . ? C58A C59A H59A 118.2 . . ? C59A C60A C55A 115.5(12) . . ? C59A C60A C61A 129.2(11) . . ? C55A C60A C61A 115.4(10) . . ? C60A C61A H61D 109.5 . . ? C60A C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C60A C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? # start Validation Reply Form _vrf_PLAT432_compound_13 ; PROBLEM: Short Inter X...Y Contact C56A .. C56A .. 2.75 Ang. RESPONSE: ... The contacts are between disordered parts of the structure. Within the real structure atoms C56A with occupation factors of 0.297(8) can avoid to be present at neighbour molecules simultaneously. ; # Attachment 'PtPPR2All.CIF' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 668505' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H56 P4 Pt, C7 H8' _chemical_formula_sum 'C55 H64 P4 Pt' _chemical_formula_weight 1044.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2476(5) _cell_length_b 13.3322(5) _cell_length_c 15.2573(6) _cell_angle_alpha 74.503(3) _cell_angle_beta 77.636(3) _cell_angle_gamma 75.331(4) _cell_volume 2480.93(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11378 _cell_measurement_theta_min 2.0844 _cell_measurement_theta_max 32.5016 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.992 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.815 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device '\k geometry, 4 circle diffractometer' _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.0470402237 _diffrn_orient_matrix_ub_12 -0.0244739124 _diffrn_orient_matrix_ub_13 0.0191183535 _diffrn_orient_matrix_ub_21 0.0239731374 _diffrn_orient_matrix_ub_22 0.0425438553 _diffrn_orient_matrix_ub_23 -0.0271150158 _diffrn_orient_matrix_ub_31 -0.0188882028 _diffrn_orient_matrix_ub_32 0.0278668929 _diffrn_orient_matrix_ub_33 0.0358941318 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_number 17416 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.1 _diffrn_reflns_theta_full 25.1 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8813 _reflns_number_gt 7246 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0669P)^2^] 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_number_reflns 8813 _refine_ls_number_parameters 517 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.104 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.781 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.172 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.753400(17) 0.822971(17) 0.739947(14) 0.02711(9) Uani 1 1 d . . . P1 P 0.76183(13) 0.73540(12) 0.62751(10) 0.0322(3) Uani 1 1 d . . . P2 P 0.80845(15) 0.63507(12) 0.74611(11) 0.0400(4) Uani 1 1 d . . . P3 P 0.76791(11) 0.80899(11) 0.88993(9) 0.0253(3) Uani 1 1 d . . . P4 P 0.70424(11) 0.99906(11) 0.67805(9) 0.0252(3) Uani 1 1 d . . . C1 C 0.9477(5) 0.8009(6) 0.5358(5) 0.0534(18) Uani 1 1 d . . . H1A H 0.9856 0.7476 0.5822 0.08 Uiso 1 1 calc R . . H1B H 0.919 0.8669 0.5576 0.08 Uiso 1 1 calc R . . H1C H 0.9965 0.8151 0.478 0.08 Uiso 1 1 calc R . . C2 C 0.8584(5) 0.7597(6) 0.5200(4) 0.0481(17) Uani 1 1 d . . . H2 H 0.8208 0.8154 0.4727 0.062 Uiso 1 1 calc R . . C3 C 0.9028(7) 0.6588(8) 0.4819(6) 0.075(3) Uani 1 1 d . . . H3A H 0.9601 0.6716 0.4304 0.112 Uiso 1 1 calc R . . H3B H 0.8465 0.6408 0.4603 0.112 Uiso 1 1 calc R . . H3C H 0.93 0.5998 0.5306 0.112 Uiso 1 1 calc R . . C4 C 0.6465(7) 0.6166(6) 0.5777(6) 0.063(2) Uani 1 1 d . . . H4A H 0.6622 0.5633 0.634 0.095 Uiso 1 1 calc R . . H4B H 0.7027 0.6024 0.5264 0.095 Uiso 1 1 calc R . . H4C H 0.5789 0.6129 0.5638 0.095 Uiso 1 1 calc R . . C5 C 0.6402(5) 0.7275(5) 0.5917(4) 0.0417(15) Uani 1 1 d . . . H5 H 0.6321 0.7797 0.5315 0.054 Uiso 1 1 calc R . . C6 C 0.5435(5) 0.7575(6) 0.6617(5) 0.0496(17) Uani 1 1 d . . . H6A H 0.4794 0.7586 0.6389 0.074 Uiso 1 1 calc R . . H6B H 0.541 0.828 0.671 0.074 Uiso 1 1 calc R . . H6C H 0.548 0.705 0.7204 0.074 Uiso 1 1 calc R . . C7 C 0.8949(4) 0.7278(4) 0.9207(4) 0.0269(12) Uani 1 1 d . . . C8 C 0.9818(5) 0.7214(5) 0.8502(4) 0.0348(13) Uani 1 1 d . . . H8 H 0.9731 0.7565 0.7885 0.042 Uiso 1 1 calc R . . C9 C 1.0805(5) 0.6640(5) 0.8698(4) 0.0375(14) Uani 1 1 d . . . H9 H 1.1388 0.6617 0.8212 0.045 Uiso 1 1 calc R . . C10 C 1.0961(5) 0.6099(4) 0.9587(4) 0.0359(14) Uani 1 1 d . . . C11 C 1.0100(5) 0.6169(4) 1.0275(4) 0.0344(13) Uani 1 1 d . . . H11 H 1.0186 0.5805 1.089 0.041 Uiso 1 1 calc R . . C12 C 0.9110(5) 0.6757(4) 1.0093(4) 0.0309(12) Uani 1 1 d . . . H12 H 0.8537 0.6801 1.0585 0.037 Uiso 1 1 calc R . . C13 C 1.2030(5) 0.5442(5) 0.9789(5) 0.0463(16) Uani 1 1 d . . . H13A H 1.2146 0.4757 0.9621 0.069 Uiso 1 1 calc R . . H13B H 1.2055 0.532 1.0447 0.069 Uiso 1 1 calc R . . H13C H 1.2582 0.5824 0.943 0.069 Uiso 1 1 calc R . . C14 C 0.7581(5) 0.9272(4) 0.9336(4) 0.0282(12) Uani 1 1 d . . . C15 C 0.8446(5) 0.9512(5) 0.9555(4) 0.0367(14) Uani 1 1 d . . . H15 H 0.9111 0.9032 0.9513 0.044 Uiso 1 1 calc R . . C16 C 0.8347(5) 1.0443(5) 0.9833(4) 0.0403(15) Uani 1 1 d . . . H16 H 0.8946 1.0587 0.9986 0.048 Uiso 1 1 calc R . . C17 C 0.7394(5) 1.1170(4) 0.9894(4) 0.0349(14) Uani 1 1 d . . . C18 C 0.6532(5) 1.0922(5) 0.9685(4) 0.0401(15) Uani 1 1 d . . . H18 H 0.5867 1.1403 0.9728 0.048 Uiso 1 1 calc R . . C19 C 0.6619(5) 0.9998(4) 0.9417(4) 0.0351(14) Uani 1 1 d . . . H19 H 0.6011 0.9848 0.9284 0.042 Uiso 1 1 calc R . . C20 C 0.7303(6) 1.2210(5) 1.0146(5) 0.0518(18) Uani 1 1 d . . . H20A H 0.7945 1.2196 1.0373 0.078 Uiso 1 1 calc R . . H20B H 0.669 1.2317 1.0627 0.078 Uiso 1 1 calc R . . H20C H 0.7212 1.2793 0.9601 0.078 Uiso 1 1 calc R . . C21 C 0.6675(4) 0.7458(4) 0.9728(4) 0.0269(12) Uani 1 1 d . . . C22 C 0.6431(4) 0.7540(4) 1.0647(4) 0.0305(12) Uani 1 1 d . . . H22 H 0.6743 0.7993 1.0845 0.037 Uiso 1 1 calc R . . C23 C 0.5746(5) 0.6976(5) 1.1270(4) 0.0360(14) Uani 1 1 d . . . H23 H 0.5601 0.7035 1.1893 0.043 Uiso 1 1 calc R . . C24 C 0.5260(4) 0.6318(5) 1.1002(4) 0.0357(13) Uani 1 1 d . . . C25 C 0.5447(5) 0.6294(4) 1.0079(4) 0.0323(13) Uani 1 1 d . . . H25 H 0.5085 0.589 0.9873 0.039 Uiso 1 1 calc R . . C26 C 0.6148(4) 0.6845(4) 0.9449(4) 0.0284(12) Uani 1 1 d . . . H26 H 0.6271 0.6804 0.8822 0.034 Uiso 1 1 calc R . . C27 C 0.4566(6) 0.5632(6) 1.1691(5) 0.0510(17) Uani 1 1 d . . . H27A H 0.4959 0.4894 1.1825 0.077 Uiso 1 1 calc R . . H27B H 0.3937 0.5666 1.1434 0.077 Uiso 1 1 calc R . . H27C H 0.4351 0.5892 1.226 0.077 Uiso 1 1 calc R . . C28 C 0.7720(4) 1.0862(4) 0.7083(4) 0.0298(12) Uani 1 1 d . . . C29 C 0.8788(5) 1.0532(5) 0.7122(4) 0.0377(14) Uani 1 1 d . . . H29 H 0.9151 0.9857 0.7004 0.045 Uiso 1 1 calc R . . C30 C 0.9336(5) 1.1170(5) 0.7330(5) 0.0445(16) Uani 1 1 d . . . H30 H 1.0072 1.0925 0.7345 0.053 Uiso 1 1 calc R . . C31 C 0.8844(5) 1.2157(5) 0.7516(4) 0.0399(15) Uani 1 1 d . . . C32 C 0.7793(5) 1.2480(6) 0.7471(6) 0.058(2) Uani 1 1 d . . . H32 H 0.7435 1.3159 0.7581 0.07 Uiso 1 1 calc R . . C33 C 0.7225(5) 1.1844(5) 0.7267(5) 0.0446(16) Uani 1 1 d . . . H33 H 0.6488 1.209 0.7255 0.053 Uiso 1 1 calc R . . C34 C 0.9420(6) 1.2823(7) 0.7795(6) 0.062(2) Uani 1 1 d . . . H34A H 0.8978 1.3536 0.7781 0.094 Uiso 1 1 calc R . . H34B H 1.0081 1.2875 0.7367 0.094 Uiso 1 1 calc R . . H34C H 0.9578 1.2493 0.842 0.094 Uiso 1 1 calc R . . C35 C 0.5625(4) 1.0587(4) 0.7011(3) 0.0254(11) Uani 1 1 d . . . C36 C 0.4988(4) 1.0057(4) 0.7746(3) 0.0278(12) Uani 1 1 d . . . H36 H 0.5287 0.9404 0.8125 0.033 Uiso 1 1 calc R . . C37 C 0.3914(4) 1.0489(5) 0.7921(4) 0.0333(13) Uani 1 1 d . . . H37 H 0.3483 1.0124 0.8423 0.04 Uiso 1 1 calc R . . C38 C 0.3464(5) 1.1422(5) 0.7390(4) 0.0367(14) Uani 1 1 d . . . C39 C 0.4101(5) 1.1948(5) 0.6656(4) 0.0358(14) Uani 1 1 d . . . H39 H 0.3799 1.2603 0.6281 0.043 Uiso 1 1 calc R . . C40 C 0.5160(5) 1.1530(4) 0.6470(4) 0.0327(13) Uani 1 1 d . . . H40 H 0.5583 1.1895 0.596 0.039 Uiso 1 1 calc R . . C41 C 0.2281(5) 1.1859(6) 0.7560(5) 0.0529(19) Uani 1 1 d . . . H41A H 0.1944 1.1686 0.7123 0.079 Uiso 1 1 calc R . . H41B H 0.2146 1.2634 0.7477 0.079 Uiso 1 1 calc R . . H41C H 0.1989 1.1541 0.8191 0.079 Uiso 1 1 calc R . . C42 C 0.7269(4) 1.0366(4) 0.5509(3) 0.0260(11) Uani 1 1 d . . . C43 C 0.8050(5) 1.0906(5) 0.5010(4) 0.0412(15) Uani 1 1 d . . . H43 H 0.8476 1.1125 0.5322 0.049 Uiso 1 1 calc R . . C44 C 0.8214(6) 1.1129(6) 0.4057(4) 0.0491(17) Uani 1 1 d . . . H44 H 0.876 1.1491 0.3723 0.059 Uiso 1 1 calc R . . C45 C 0.7601(6) 1.0836(5) 0.3583(4) 0.0433(15) Uani 1 1 d . . . C46 C 0.6821(5) 1.0300(5) 0.4079(4) 0.0356(13) Uani 1 1 d . . . H46 H 0.6394 1.0088 0.3763 0.043 Uiso 1 1 calc R . . C47 C 0.6652(4) 1.0067(5) 0.5034(4) 0.0320(13) Uani 1 1 d . . . H47 H 0.611 0.97 0.5366 0.038 Uiso 1 1 calc R . . C48 C 0.7791(7) 1.1104(7) 0.2546(5) 0.063(2) Uani 1 1 d . . . H48A H 0.7726 1.0503 0.2321 0.095 Uiso 1 1 calc R . . H48B H 0.8502 1.1247 0.2322 0.095 Uiso 1 1 calc R . . H48C H 0.7268 1.1736 0.2319 0.095 Uiso 1 1 calc R . . C50 C 0.8099(7) 0.4157(7) 0.4368(6) 0.073(2) Uiso 1 1 d D . . H50 H 0.8737 0.4027 0.4607 0.087 Uiso 1 1 calc R . . C51 C 0.7254(12) 0.3780(14) 0.4986(10) 0.189(8) Uiso 1 1 d D . . H51 H 0.7344 0.3398 0.5596 0.227 Uiso 1 1 calc R . . C52 C 0.6322(10) 0.3967(12) 0.4701(9) 0.140(5) Uiso 1 1 d D . . H52 H 0.5724 0.3726 0.5083 0.168 Uiso 1 1 calc R . . C53 C 0.6306(11) 0.4588(13) 0.3727(10) 0.172(7) Uiso 1 1 d D . . H53 H 0.5649 0.4763 0.351 0.207 Uiso 1 1 calc R . . C54 C 0.7107(10) 0.4919(10) 0.3138(8) 0.117(4) Uiso 1 1 d D . . H54 H 0.7044 0.5293 0.2521 0.141 Uiso 1 1 calc R . . C55 C 0.8116(10) 0.4663(12) 0.3510(9) 0.135(5) Uiso 1 1 d D . . C56 C 0.8844(10) 0.5075(11) 0.2882(9) 0.125(4) Uiso 1 1 d D . . H56A H 0.9007 0.5654 0.3074 0.188 Uiso 1 1 calc R . . H56B H 0.858 0.5354 0.2292 0.188 Uiso 1 1 calc R . . H56C H 0.9485 0.4524 0.2813 0.188 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 0.03265(13) 0.02395(12) 0.02686(12) -0.00707(8) -0.00896(8) -0.00467(8) P1 0.0432(9) 0.0303(8) 0.0259(7) -0.0086(6) -0.0063(6) -0.0092(7) P2 0.0608(11) 0.0254(8) 0.0349(8) -0.0103(6) -0.0159(8) -0.0003(7) P3 0.0303(7) 0.0199(7) 0.0283(7) -0.0073(5) -0.0102(6) -0.0032(6) P4 0.0275(7) 0.0250(7) 0.0245(7) -0.0046(5) -0.0067(6) -0.0071(6) C1 0.045(4) 0.053(4) 0.063(5) -0.026(4) 0.014(3) -0.016(3) C2 0.050(4) 0.059(4) 0.034(3) -0.014(3) -0.002(3) -0.008(3) C3 0.065(5) 0.110(7) 0.071(6) -0.066(5) 0.017(4) -0.032(5) C4 0.078(6) 0.058(5) 0.069(5) -0.029(4) -0.005(4) -0.031(4) C5 0.056(4) 0.043(4) 0.034(3) -0.011(3) -0.014(3) -0.017(3) C6 0.044(4) 0.059(4) 0.053(4) -0.014(3) -0.013(3) -0.018(3) C7 0.030(3) 0.015(2) 0.039(3) -0.008(2) -0.011(2) -0.005(2) C8 0.036(3) 0.030(3) 0.039(3) -0.007(2) -0.007(3) -0.009(3) C9 0.027(3) 0.033(3) 0.051(4) -0.011(3) 0.001(3) -0.009(3) C10 0.033(3) 0.020(3) 0.060(4) -0.013(3) -0.014(3) -0.006(2) C11 0.044(4) 0.022(3) 0.042(3) -0.003(2) -0.020(3) -0.007(3) C12 0.037(3) 0.029(3) 0.032(3) -0.008(2) -0.014(3) -0.007(3) C13 0.038(4) 0.025(3) 0.078(5) -0.010(3) -0.025(3) -0.001(3) C14 0.041(3) 0.021(3) 0.024(3) -0.003(2) -0.011(2) -0.007(2) C15 0.038(3) 0.031(3) 0.045(4) -0.014(3) -0.010(3) -0.005(3) C16 0.046(4) 0.036(3) 0.049(4) -0.013(3) -0.014(3) -0.016(3) C17 0.055(4) 0.022(3) 0.032(3) -0.006(2) -0.015(3) -0.009(3) C18 0.058(4) 0.027(3) 0.037(3) -0.011(3) -0.026(3) 0.009(3) C19 0.049(4) 0.028(3) 0.034(3) -0.009(2) -0.023(3) -0.003(3) C20 0.081(5) 0.030(3) 0.056(4) -0.015(3) -0.034(4) -0.007(3) C21 0.032(3) 0.021(3) 0.028(3) -0.005(2) -0.009(2) -0.002(2) C22 0.031(3) 0.029(3) 0.036(3) -0.013(2) -0.008(2) -0.004(2) C23 0.036(3) 0.037(3) 0.034(3) -0.012(3) -0.002(3) -0.003(3) C24 0.028(3) 0.027(3) 0.046(4) -0.007(3) -0.003(3) 0.002(2) C25 0.034(3) 0.023(3) 0.042(3) -0.010(2) -0.007(3) -0.006(2) C26 0.036(3) 0.022(3) 0.029(3) -0.009(2) -0.009(2) -0.002(2) C27 0.048(4) 0.047(4) 0.053(4) -0.010(3) 0.004(3) -0.013(3) C28 0.032(3) 0.027(3) 0.030(3) -0.003(2) -0.005(2) -0.010(2) C29 0.035(3) 0.034(3) 0.047(4) -0.010(3) -0.011(3) -0.009(3) C30 0.031(3) 0.051(4) 0.059(4) -0.019(3) -0.012(3) -0.012(3) C31 0.033(3) 0.054(4) 0.040(3) -0.019(3) -0.001(3) -0.018(3) C32 0.040(4) 0.057(5) 0.095(6) -0.050(4) -0.006(4) -0.008(3) C33 0.031(3) 0.046(4) 0.069(4) -0.034(3) -0.011(3) -0.005(3) C34 0.042(4) 0.084(6) 0.083(6) -0.050(5) -0.005(4) -0.023(4) C35 0.026(3) 0.030(3) 0.025(3) -0.010(2) -0.008(2) -0.005(2) C36 0.033(3) 0.031(3) 0.023(3) -0.008(2) -0.008(2) -0.009(2) C37 0.034(3) 0.046(4) 0.030(3) -0.015(3) -0.005(2) -0.018(3) C38 0.029(3) 0.052(4) 0.037(3) -0.021(3) -0.013(3) -0.005(3) C39 0.039(3) 0.036(3) 0.035(3) -0.012(3) -0.015(3) 0.000(3) C40 0.038(3) 0.031(3) 0.031(3) -0.008(2) -0.009(3) -0.008(3) C41 0.031(4) 0.070(5) 0.062(5) -0.031(4) -0.008(3) -0.002(3) C42 0.030(3) 0.023(3) 0.025(3) -0.007(2) -0.002(2) -0.006(2) C43 0.044(4) 0.058(4) 0.029(3) -0.009(3) -0.005(3) -0.026(3) C44 0.063(5) 0.059(4) 0.035(3) -0.006(3) 0.001(3) -0.039(4) C45 0.062(4) 0.044(4) 0.028(3) -0.009(3) -0.007(3) -0.018(3) C46 0.046(4) 0.038(3) 0.029(3) -0.008(2) -0.011(3) -0.014(3) C47 0.031(3) 0.036(3) 0.031(3) -0.003(2) -0.003(2) -0.014(3) C48 0.094(6) 0.077(6) 0.032(4) -0.005(3) -0.011(4) -0.047(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2893(14) . ? Pt1 P2 2.4072(15) . ? Pt1 P3 2.2915(13) . ? Pt1 P4 2.2653(14) . ? P1 C5 1.845(6) . ? P1 C2 1.860(7) . ? P1 P2 2.052(2) . ? P3 C21 1.832(6) . ? P3 C14 1.835(5) . ? P3 C7 1.835(5) . ? P4 C28 1.833(6) . ? P4 C35 1.842(5) . ? P4 C42 1.847(5) . ? C1 C2 1.511(10) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.538(10) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C5 1.529(9) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.525(9) . ? C5 H5 1 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C12 1.379(8) . ? C7 C8 1.400(8) . ? C8 C9 1.387(8) . ? C8 H8 0.95 . ? C9 C10 1.387(9) . ? C9 H9 0.95 . ? C10 C11 1.378(9) . ? C10 C13 1.510(8) . ? C11 C12 1.390(8) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.390(8) . ? C14 C19 1.396(8) . ? C15 C16 1.383(8) . ? C15 H15 0.95 . ? C16 C17 1.386(9) . ? C16 H16 0.95 . ? C17 C18 1.386(9) . ? C17 C20 1.504(8) . ? C18 C19 1.369(8) . ? C18 H18 0.95 . ? C19 H19 0.95 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C26 1.393(7) . ? C21 C22 1.397(7) . ? C22 C23 1.373(8) . ? C22 H22 0.95 . ? C23 C24 1.394(8) . ? C23 H23 0.95 . ? C24 C25 1.385(8) . ? C24 C27 1.511(9) . ? C25 C26 1.382(8) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.380(8) . ? C28 C33 1.381(8) . ? C29 C30 1.381(8) . ? C29 H29 0.95 . ? C30 C31 1.387(9) . ? C30 H30 0.95 . ? C31 C32 1.361(9) . ? C31 C34 1.495(9) . ? C32 C33 1.394(9) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C40 1.383(8) . ? C35 C36 1.394(7) . ? C36 C37 1.390(8) . ? C36 H36 0.95 . ? C37 C38 1.361(9) . ? C37 H37 0.95 . ? C38 C39 1.390(9) . ? C38 C41 1.520(8) . ? C39 C40 1.371(8) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 C43 1.385(8) . ? C42 C47 1.387(8) . ? C43 C44 1.384(8) . ? C43 H43 0.95 . ? C44 C45 1.378(9) . ? C44 H44 0.95 . ? C45 C46 1.378(9) . ? C45 C48 1.506(9) . ? C46 C47 1.388(8) . ? C46 H46 0.95 . ? C47 H47 0.95 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C50 C55 1.301(11) . ? C50 C51 1.405(13) . ? C50 H50 0.95 . ? C51 C52 1.338(14) . ? C51 H51 0.95 . ? C52 C53 1.497(13) . ? C52 H52 0.95 . ? C53 C54 1.321(13) . ? C53 H53 0.95 . ? C54 C55 1.490(12) . ? C54 H54 0.95 . ? C55 C56 1.319(13) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? 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 P1 Pt1 P2 51.75(5) . . ? P1 Pt1 P3 146.87(5) . . ? P3 Pt1 P2 95.30(5) . . ? P4 Pt1 P2 158.33(5) . . ? P4 Pt1 P1 106.81(5) . . ? P4 Pt1 P3 106.27(5) . . ? C5 P1 C2 106.1(3) . . ? C5 P1 P2 119.6(2) . . ? C2 P1 P2 121.1(2) . . ? C5 P1 Pt1 120.6(2) . . ? C2 P1 Pt1 119.0(2) . . ? P2 P1 Pt1 67.09(6) . . ? P1 P2 Pt1 61.16(6) . . ? C21 P3 C14 101.3(2) . . ? C21 P3 C7 105.1(2) . . ? C14 P3 C7 101.6(2) . . ? C21 P3 Pt1 112.99(17) . . ? C14 P3 Pt1 121.28(18) . . ? C7 P3 Pt1 112.74(18) . . ? C28 P4 C35 105.1(2) . . ? C28 P4 C42 102.4(2) . . ? C35 P4 C42 100.0(2) . . ? C28 P4 Pt1 115.66(18) . . ? C35 P4 Pt1 116.50(18) . . ? C42 P4 Pt1 115.09(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 110.0(6) . . ? C1 C2 P1 110.9(4) . . ? C3 C2 P1 111.7(5) . . ? C1 C2 H2 108.1 . . ? C3 C2 H2 108.1 . . ? P1 C2 H2 108.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C4 110.2(6) . . ? C6 C5 P1 110.8(4) . . ? C4 C5 P1 111.3(5) . . ? C6 C5 H5 108.1 . . ? C4 C5 H5 108.1 . . ? P1 C5 H5 108.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 117.9(5) . . ? C12 C7 P3 124.2(4) . . ? C8 C7 P3 117.9(4) . . ? C9 C8 C7 120.4(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 121.6(6) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 117.5(5) . . ? C11 C10 C13 121.3(6) . . ? C9 C10 C13 121.3(6) . . ? C10 C11 C12 121.7(6) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C7 C12 C11 120.9(6) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.5(5) . . ? C15 C14 P3 122.6(4) . . ? C19 C14 P3 119.8(4) . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.6(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 117.6(5) . . ? C18 C17 C20 120.9(6) . . ? C16 C17 C20 121.5(6) . . ? C19 C18 C17 121.3(6) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C14 121.4(6) . . ? C18 C19 H19 119.3 . . ? C14 C19 H19 119.3 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 117.9(5) . . ? C26 C21 P3 119.5(4) . . ? C22 C21 P3 122.6(4) . . ? C23 C22 C21 121.0(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 121.1(5) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 117.8(5) . . ? C25 C24 C27 120.5(6) . . ? C23 C24 C27 121.7(6) . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C21 120.5(5) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 117.6(5) . . ? C29 C28 P4 118.8(4) . . ? C33 C28 P4 123.7(5) . . ? C28 C29 C30 120.8(6) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 122.0(6) . . ? C29 C30 H30 119 . . ? C31 C30 H30 119 . . ? C32 C31 C30 116.9(6) . . ? C32 C31 C34 120.9(6) . . ? C30 C31 C34 122.2(6) . . ? C31 C32 C33 122.0(6) . . ? C31 C32 H32 119 . . ? C33 C32 H32 119 . . ? C28 C33 C32 120.8(6) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 118.5(5) . . ? C40 C35 P4 122.6(4) . . ? C36 C35 P4 118.9(4) . . ? C37 C36 C35 119.6(5) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C38 C37 C36 121.5(6) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C39 118.8(5) . . ? C37 C38 C41 121.0(6) . . ? C39 C38 C41 120.1(6) . . ? C40 C39 C38 120.5(6) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C35 121.1(6) . . ? C39 C40 H40 119.5 . . ? C35 C40 H40 119.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 118.6(5) . . ? C43 C42 P4 122.7(4) . . ? C47 C42 P4 118.7(4) . . ? C44 C43 C42 120.3(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 121.3(6) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 118.6(5) . . ? C44 C45 C48 119.9(6) . . ? C46 C45 C48 121.5(6) . . ? C45 C46 C47 120.7(5) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C42 C47 C46 120.6(5) . . ? C42 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C55 C50 C51 128.2(10) . . ? C55 C50 H50 115.9 . . ? C51 C50 H50 115.9 . . ? C52 C51 C50 118.9(11) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C51 C52 C53 114.1(11) . . ? C51 C52 H52 123 . . ? C53 C52 H52 123 . . ? C54 C53 C52 127.1(11) . . ? C54 C53 H53 116.5 . . ? C52 C53 H53 116.5 . . ? C53 C54 C55 115.1(10) . . ? C53 C54 H54 122.5 . . ? C55 C54 H54 122.5 . . ? C50 C55 C56 133.3(13) . . ? C50 C55 C54 116.6(9) . . ? C56 C55 C54 110.0(12) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? #END data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 668506' _audit_creation_date 2007-11-30T12:52:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H60 P4 Pt, C7 H8' _chemical_formula_sum 'C57 H68 P4 Pt' _chemical_formula_weight 1072.08 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3097(8) _cell_length_b 13.4111(10) _cell_length_c 15.3900(12) _cell_angle_alpha 77.834(6) _cell_angle_beta 77.293(6) _cell_angle_gamma 76.611(6) _cell_volume 2569.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.1042 _cell_measurement_theta_max 32.5421 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.89 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.861 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_probe x-ray _diffrn_measurement_device '\k geometry, 4 circle diffractometer' _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.0240267872 _diffrn_orient_matrix_ub_12 0.0421421545 _diffrn_orient_matrix_ub_13 -0.0242221543 _diffrn_orient_matrix_ub_21 -0.0501551496 _diffrn_orient_matrix_ub_22 0.0328782922 _diffrn_orient_matrix_ub_23 0.0003956326 _diffrn_orient_matrix_ub_31 0.0029349189 _diffrn_orient_matrix_ub_32 0.0136037841 _diffrn_orient_matrix_ub_33 0.0413571682 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_unetI/netI 0.1006 _diffrn_reflns_number 18854 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 10040 _reflns_number_gt 7502 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0679P)^2^] 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_number_reflns 10040 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 0.99 _refine_ls_restrained_S_all 0.99 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.563 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.203 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.77610(2) 0.82058(2) 0.727946(17) 0.02381(10) Uani 1 1 d . . . P1 P 0.78470(14) 0.71905(13) 0.62183(11) 0.0230(4) Uani 1 1 d . . . P2 P 0.84378(16) 0.63678(14) 0.73487(12) 0.0312(4) Uani 1 1 d . . . P3 P 0.78854(13) 0.81241(13) 0.87548(11) 0.0212(4) Uani 1 1 d . . . P4 P 0.71670(13) 0.99132(13) 0.67269(11) 0.0211(4) Uani 1 1 d . . . C1 C 0.8853(5) 0.7319(5) 0.5139(4) 0.0260(15) Uani 1 1 d . . . C2 C 0.9405(6) 0.6225(6) 0.4944(5) 0.0356(18) Uani 1 1 d . . . H2A H 0.9994 0.6282 0.4438 0.053 Uiso 1 1 calc R . . H2B H 0.8905 0.5888 0.4788 0.053 Uiso 1 1 calc R . . H2C H 0.9668 0.5809 0.5481 0.053 Uiso 1 1 calc R . . C3 C 0.8380(6) 0.7952(6) 0.4320(4) 0.0303(16) Uani 1 1 d . . . H3A H 0.8944 0.8041 0.3797 0.045 Uiso 1 1 calc R . . H3B H 0.8 0.8636 0.4457 0.045 Uiso 1 1 calc R . . H3C H 0.7894 0.7583 0.4182 0.045 Uiso 1 1 calc R . . C4 C 0.9655(5) 0.7861(6) 0.5304(5) 0.0302(16) Uani 1 1 d . . . H4A H 0.9893 0.7516 0.5871 0.045 Uiso 1 1 calc R . . H4B H 0.9336 0.859 0.5343 0.045 Uiso 1 1 calc R . . H4C H 1.0256 0.7829 0.4804 0.045 Uiso 1 1 calc R . . C5 C 0.6567(6) 0.6934(6) 0.6028(5) 0.0299(16) Uani 1 1 d . . . C6 C 0.5942(6) 0.6618(6) 0.6964(5) 0.0373(18) Uani 1 1 d . . . H6A H 0.5748 0.7207 0.7291 0.056 Uiso 1 1 calc R . . H6B H 0.6371 0.6032 0.7299 0.056 Uiso 1 1 calc R . . H6C H 0.5304 0.6411 0.6903 0.056 Uiso 1 1 calc R . . C7 C 0.6791(7) 0.6039(6) 0.5491(5) 0.0404(19) Uani 1 1 d . . . H7A H 0.6128 0.5849 0.5474 0.061 Uiso 1 1 calc R . . H7B H 0.7245 0.5436 0.5783 0.061 Uiso 1 1 calc R . . H7C H 0.7143 0.6259 0.4873 0.061 Uiso 1 1 calc R . . C8 C 0.5935(6) 0.7914(6) 0.5558(5) 0.0328(17) Uani 1 1 d . . . H8A H 0.6332 0.8132 0.4958 0.049 Uiso 1 1 calc R . . H8B H 0.58 0.847 0.5918 0.049 Uiso 1 1 calc R . . H8C H 0.5266 0.7773 0.5497 0.049 Uiso 1 1 calc R . . C9 C 0.6801(5) 0.7578(5) 0.9539(4) 0.0225(14) Uani 1 1 d . . . C10 C 0.6373(6) 0.6847(5) 0.9286(4) 0.0259(15) Uani 1 1 d . . . H10 H 0.66 0.6668 0.8699 0.031 Uiso 1 1 calc R . . C11 C 0.5614(6) 0.6386(5) 0.9898(5) 0.0336(17) Uani 1 1 d . . . H11 H 0.5333 0.5887 0.9719 0.04 Uiso 1 1 calc R . . C12 C 0.5247(5) 0.6618(5) 1.0754(5) 0.0302(16) Uani 1 1 d . . . C13 C 0.5666(6) 0.7365(6) 1.0982(5) 0.0318(17) Uani 1 1 d . . . H13 H 0.5424 0.7552 1.1566 0.038 Uiso 1 1 calc R . . C14 C 0.6414(5) 0.7840(5) 1.0395(4) 0.0261(15) Uani 1 1 d . . . H14 H 0.6673 0.8354 1.0573 0.031 Uiso 1 1 calc R . . C15 C 0.4449(7) 0.6075(7) 1.1416(5) 0.046(2) Uani 1 1 d . . . H15A H 0.4113 0.5725 1.1093 0.07 Uiso 1 1 calc R . . H15B H 0.3915 0.6586 1.1723 0.07 Uiso 1 1 calc R . . H15C H 0.4798 0.5559 1.1864 0.07 Uiso 1 1 calc R . . C16 C 0.9080(5) 0.7287(5) 0.9102(4) 0.0238(14) Uani 1 1 d . . . C17 C 0.9113(6) 0.6851(5) 1.0006(5) 0.0280(15) Uani 1 1 d . . . H17 H 0.8508 0.6987 1.0457 0.034 Uiso 1 1 calc R . . C18 C 1.0034(6) 0.6216(5) 1.0249(5) 0.0333(18) Uani 1 1 d . . . H18 H 1.004 0.5908 1.0864 0.04 Uiso 1 1 calc R . . C19 C 1.0934(6) 0.6027(5) 0.9615(5) 0.0306(17) Uani 1 1 d . . . C20 C 1.0896(6) 0.6485(5) 0.8730(5) 0.0315(16) Uani 1 1 d . . . H20 H 1.1511 0.637 0.8285 0.038 Uiso 1 1 calc R . . C21 C 0.9989(5) 0.7109(5) 0.8467(5) 0.0279(15) Uani 1 1 d . . . H21 H 0.9991 0.7415 0.7851 0.033 Uiso 1 1 calc R . . C22 C 1.1917(7) 0.5345(6) 0.9886(6) 0.047(2) Uani 1 1 d . . . H22A H 1.2055 0.4693 0.9651 0.07 Uiso 1 1 calc R . . H22B H 1.183 0.5194 1.0547 0.07 Uiso 1 1 calc R . . H22C H 1.2509 0.5702 0.9639 0.07 Uiso 1 1 calc R . . C23 C 0.7813(6) 0.9308(5) 0.9203(4) 0.0250(15) Uani 1 1 d . . . C24 C 0.6913(6) 1.0062(5) 0.9221(4) 0.0287(16) Uani 1 1 d . . . H24 H 0.6334 0.9946 0.9016 0.034 Uiso 1 1 calc R . . C25 C 0.6824(6) 1.0976(5) 0.9525(4) 0.0298(16) Uani 1 1 d . . . H25 H 0.6187 1.1474 0.9536 0.036 Uiso 1 1 calc R . . C26 C 0.7660(6) 1.1174(5) 0.9816(4) 0.0308(17) Uani 1 1 d . . . C27 C 0.8568(6) 1.0433(6) 0.9804(5) 0.0353(18) Uani 1 1 d . . . H27 H 0.9145 1.0558 1.0006 0.042 Uiso 1 1 calc R . . C28 C 0.8659(6) 0.9500(5) 0.9502(5) 0.0303(16) Uani 1 1 d . . . H28 H 0.9293 0.8998 0.95 0.036 Uiso 1 1 calc R . . C29 C 0.7581(7) 1.2186(6) 1.0125(5) 0.0397(19) Uani 1 1 d . . . H29A H 0.8142 1.2119 1.0465 0.06 Uiso 1 1 calc R . . H29B H 0.6898 1.2361 1.0513 0.06 Uiso 1 1 calc R . . H29C H 0.7653 1.2738 0.9598 0.06 Uiso 1 1 calc R . . C30 C 0.7352(5) 1.0339(5) 0.5486(4) 0.0236(14) Uani 1 1 d . . . C31 C 0.6585(5) 1.0356(5) 0.4989(4) 0.0261(15) Uani 1 1 d . . . H31 H 0.5936 1.0162 0.5287 0.031 Uiso 1 1 calc R . . C32 C 0.6776(5) 1.0658(5) 0.4057(4) 0.0268(15) Uani 1 1 d . . . H32 H 0.6245 1.0676 0.3727 0.032 Uiso 1 1 calc R . . C33 C 0.7717(6) 1.0934(5) 0.3591(4) 0.0299(16) Uani 1 1 d . . . C34 C 0.8477(6) 1.0898(6) 0.4103(5) 0.0329(17) Uani 1 1 d . . . H34 H 0.913 1.1079 0.3804 0.039 Uiso 1 1 calc R . . C35 C 0.8303(5) 1.0605(5) 0.5033(4) 0.0272(15) Uani 1 1 d . . . H35 H 0.8835 1.0586 0.5363 0.033 Uiso 1 1 calc R . . C36 C 0.7893(7) 1.1285(7) 0.2590(5) 0.047(2) Uani 1 1 d . . . H36A H 0.7361 1.1098 0.2337 0.071 Uiso 1 1 calc R . . H36B H 0.8593 1.0946 0.2321 0.071 Uiso 1 1 calc R . . H36C H 0.7839 1.2041 0.2457 0.071 Uiso 1 1 calc R . . C37 C 0.5740(5) 1.0364(5) 0.7075(4) 0.0219(14) Uani 1 1 d . . . C38 C 0.5194(5) 0.9748(5) 0.7748(4) 0.0235(14) Uani 1 1 d . . . H38 H 0.5558 0.9102 0.802 0.028 Uiso 1 1 calc R . . C39 C 0.4117(6) 1.0042(6) 0.8046(4) 0.0302(16) Uani 1 1 d . . . H39 H 0.3761 0.9608 0.8527 0.036 Uiso 1 1 calc R . . C40 C 0.3562(5) 1.0973(6) 0.7638(4) 0.0290(16) Uani 1 1 d . . . C41 C 0.4116(6) 1.1586(5) 0.6952(4) 0.0289(16) Uani 1 1 d . . . H41 H 0.3752 1.2227 0.6672 0.035 Uiso 1 1 calc R . . C42 C 0.5181(5) 1.1297(5) 0.6661(4) 0.0252(15) Uani 1 1 d . . . H42 H 0.5537 1.173 0.618 0.03 Uiso 1 1 calc R . . C43 C 0.2381(6) 1.1292(7) 0.7936(5) 0.043(2) Uani 1 1 d . . . H43A H 0.22 1.204 0.7953 0.065 Uiso 1 1 calc R . . H43B H 0.2166 1.0907 0.8539 0.065 Uiso 1 1 calc R . . H43C H 0.2017 1.1136 0.7507 0.065 Uiso 1 1 calc R . . C44 C 0.7805(5) 1.0856(5) 0.7019(4) 0.0250(15) Uani 1 1 d . . . C45 C 0.8778(5) 1.0501(5) 0.7272(4) 0.0272(15) Uani 1 1 d . . . H45 H 0.9083 0.9782 0.7311 0.033 Uiso 1 1 calc R . . C46 C 0.9322(6) 1.1167(6) 0.7472(5) 0.0328(17) Uani 1 1 d . . . H46 H 0.9998 1.0904 0.7627 0.039 Uiso 1 1 calc R . . C47 C 0.8882(6) 1.2214(6) 0.7447(5) 0.0329(17) Uani 1 1 d . . . C48 C 0.7923(6) 1.2568(6) 0.7178(5) 0.0327(17) Uani 1 1 d . . . H48 H 0.7625 1.3289 0.7127 0.039 Uiso 1 1 calc R . . C49 C 0.7382(6) 1.1909(6) 0.6980(5) 0.0305(16) Uani 1 1 d . . . H49 H 0.6711 1.2178 0.6815 0.037 Uiso 1 1 calc R . . C50 C 0.9440(7) 1.2925(7) 0.7722(6) 0.044(2) Uani 1 1 d . . . H50A H 0.9041 1.3639 0.7632 0.066 Uiso 1 1 calc R . . H50B H 1.0144 1.2895 0.7354 0.066 Uiso 1 1 calc R . . H50C H 0.9497 1.2702 0.8361 0.066 Uiso 1 1 calc R . . C51 C 0.6985(9) 0.4184(7) 0.4068(6) 0.055(2) Uani 1 1 d . . . C52 C 0.6374(10) 0.4922(8) 0.3510(8) 0.077(4) Uani 1 1 d . . . H52 H 0.5635 0.4975 0.3614 0.092 Uiso 1 1 calc R . . C53 C 0.6861(12) 0.5575(8) 0.2803(9) 0.091(5) Uani 1 1 d . . . H53 H 0.6451 0.6069 0.2414 0.109 Uiso 1 1 calc R . . C54 C 0.7980(13) 0.5515(10) 0.2648(8) 0.086(4) Uani 1 1 d . . . H54 H 0.8332 0.5941 0.2158 0.103 Uiso 1 1 calc R . . C55 C 0.8468(11) 0.4845(12) 0.3220(9) 0.091(4) Uani 1 1 d . . . H55 H 0.92 0.4815 0.3159 0.109 Uiso 1 1 calc R . . C56 C 0.8028(7) 0.4190(7) 0.3888(7) 0.054(2) Uani 1 1 d . . . H56 H 0.8465 0.3702 0.4258 0.065 Uiso 1 1 calc R . . C57 C 0.6500(13) 0.3508(9) 0.4798(9) 0.104(5) Uani 1 1 d . . . H57A H 0.6992 0.2847 0.4911 0.155 Uiso 1 1 calc R . . H57B H 0.587 0.3379 0.4644 0.155 Uiso 1 1 calc R . . H57C H 0.6304 0.3831 0.5342 0.155 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 0.03098(16) 0.01697(14) 0.02428(14) -0.00368(9) -0.01161(10) 0.00022(10) P1 0.0291(10) 0.0157(8) 0.0252(8) -0.0030(7) -0.0105(7) -0.0015(7) P2 0.0430(11) 0.0175(9) 0.0323(10) -0.0053(7) -0.0170(9) 0.0062(8) P3 0.0253(9) 0.0153(8) 0.0234(8) -0.0021(7) -0.0086(7) -0.0017(7) P4 0.0251(9) 0.0153(8) 0.0231(8) -0.0020(7) -0.0078(7) -0.0022(7) C1 0.028(4) 0.023(4) 0.025(3) -0.007(3) -0.005(3) 0.003(3) C2 0.041(4) 0.027(4) 0.041(4) -0.015(3) -0.013(3) 0.002(3) C3 0.031(4) 0.029(4) 0.031(4) -0.007(3) -0.009(3) -0.002(3) C4 0.030(4) 0.029(4) 0.032(4) -0.012(3) -0.008(3) 0.001(3) C5 0.038(4) 0.026(4) 0.031(4) -0.009(3) -0.015(3) -0.005(3) C6 0.045(5) 0.036(4) 0.037(4) -0.003(3) -0.013(4) -0.018(4) C7 0.046(5) 0.036(5) 0.047(5) -0.017(4) -0.014(4) -0.010(4) C8 0.029(4) 0.035(4) 0.035(4) -0.003(3) -0.011(3) -0.004(3) C9 0.027(4) 0.014(3) 0.029(3) -0.003(3) -0.010(3) -0.003(3) C10 0.037(4) 0.018(3) 0.022(3) 0.000(3) -0.006(3) -0.006(3) C11 0.043(5) 0.020(4) 0.041(4) -0.009(3) -0.015(4) -0.002(3) C12 0.026(4) 0.023(4) 0.039(4) -0.002(3) -0.004(3) -0.003(3) C13 0.034(4) 0.032(4) 0.027(4) -0.006(3) -0.008(3) 0.001(3) C14 0.030(4) 0.021(4) 0.030(4) -0.005(3) -0.010(3) -0.004(3) C15 0.056(6) 0.036(5) 0.046(5) -0.010(4) 0.004(4) -0.017(4) C16 0.026(4) 0.014(3) 0.036(4) -0.006(3) -0.016(3) 0.000(3) C17 0.036(4) 0.019(3) 0.033(4) -0.004(3) -0.014(3) -0.006(3) C18 0.048(5) 0.022(4) 0.036(4) -0.003(3) -0.028(4) -0.003(3) C19 0.028(4) 0.011(3) 0.058(5) -0.004(3) -0.022(4) -0.003(3) C20 0.032(4) 0.021(4) 0.044(4) -0.009(3) -0.013(3) -0.002(3) C21 0.031(4) 0.023(4) 0.029(4) 0.003(3) -0.006(3) -0.011(3) C22 0.042(5) 0.024(4) 0.078(6) -0.007(4) -0.031(4) 0.002(4) C23 0.047(4) 0.012(3) 0.019(3) 0.003(2) -0.013(3) -0.010(3) C24 0.036(4) 0.023(4) 0.032(4) -0.006(3) -0.018(3) -0.003(3) C25 0.041(4) 0.018(4) 0.029(4) -0.004(3) -0.015(3) 0.006(3) C26 0.054(5) 0.017(3) 0.026(3) -0.002(3) -0.018(3) -0.006(3) C27 0.045(5) 0.024(4) 0.042(4) -0.004(3) -0.017(4) -0.009(4) C28 0.038(4) 0.018(4) 0.037(4) -0.005(3) -0.012(3) -0.003(3) C29 0.062(5) 0.023(4) 0.041(4) -0.010(3) -0.018(4) -0.010(4) C30 0.034(4) 0.010(3) 0.025(3) 0.000(3) -0.008(3) -0.002(3) C31 0.028(4) 0.025(4) 0.026(3) -0.003(3) -0.010(3) -0.003(3) C32 0.029(4) 0.018(3) 0.034(4) -0.002(3) -0.012(3) -0.002(3) C33 0.040(4) 0.024(4) 0.028(4) -0.003(3) -0.007(3) -0.012(3) C34 0.036(4) 0.033(4) 0.034(4) -0.007(3) -0.004(3) -0.016(3) C35 0.031(4) 0.022(4) 0.030(4) -0.006(3) -0.011(3) -0.003(3) C36 0.067(6) 0.043(5) 0.035(4) -0.004(4) -0.008(4) -0.023(5) C37 0.020(3) 0.016(3) 0.033(4) -0.007(3) -0.011(3) -0.001(3) C38 0.030(4) 0.019(3) 0.023(3) -0.003(3) -0.010(3) -0.004(3) C39 0.035(4) 0.039(4) 0.021(3) -0.003(3) -0.009(3) -0.015(4) C40 0.029(4) 0.038(4) 0.024(3) -0.008(3) -0.009(3) -0.007(3) C41 0.037(4) 0.023(4) 0.030(4) -0.010(3) -0.016(3) 0.001(3) C42 0.030(4) 0.026(4) 0.020(3) -0.004(3) -0.007(3) -0.004(3) C43 0.033(4) 0.058(6) 0.039(4) -0.016(4) -0.008(3) -0.002(4) C44 0.035(4) 0.021(3) 0.020(3) -0.003(3) -0.007(3) -0.005(3) C45 0.027(4) 0.022(4) 0.032(4) 0.000(3) -0.009(3) -0.005(3) C46 0.027(4) 0.036(4) 0.035(4) -0.001(3) -0.007(3) -0.009(3) C47 0.036(4) 0.038(4) 0.028(4) -0.009(3) -0.002(3) -0.013(4) C48 0.034(4) 0.021(4) 0.043(4) -0.010(3) -0.002(3) -0.004(3) C49 0.030(4) 0.026(4) 0.039(4) -0.012(3) -0.011(3) -0.002(3) C50 0.046(5) 0.042(5) 0.053(5) -0.019(4) -0.005(4) -0.019(4) C51 0.082(7) 0.034(5) 0.055(5) -0.016(4) -0.019(5) -0.008(5) C52 0.093(9) 0.048(6) 0.108(9) -0.026(6) -0.076(8) 0.016(6) C53 0.135(12) 0.038(6) 0.115(10) -0.019(7) -0.093(10) 0.028(7) C54 0.134(13) 0.068(8) 0.055(7) -0.025(6) -0.022(7) -0.001(8) C55 0.096(10) 0.098(11) 0.081(9) -0.050(8) 0.017(8) -0.023(9) C56 0.042(5) 0.044(5) 0.075(7) -0.021(5) -0.022(5) 0.014(4) C57 0.168(15) 0.054(7) 0.107(10) -0.014(7) -0.042(10) -0.042(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.3059(17) . ? Pt1 P2 2.4088(18) . ? Pt1 P3 2.2906(16) . ? Pt1 P4 2.2864(16) . ? P1 P2 2.062(2) . ? P1 C1 1.895(7) . ? P1 C5 1.907(7) . ? P3 C23 1.835(6) . ? P3 C16 1.835(6) . ? P3 C9 1.851(7) . ? P4 C37 1.849(7) . ? P4 C44 1.851(7) . ? P4 C30 1.853(6) . ? C1 C4 1.513(10) . ? C1 C3 1.535(9) . ? C1 C2 1.541(9) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C8 1.521(9) . ? C5 C6 1.525(10) . ? C5 C7 1.536(10) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C14 1.392(9) . ? C9 C10 1.399(9) . ? C10 C11 1.384(10) . ? C10 H10 0.95 . ? C11 C12 1.375(10) . ? C11 H11 0.95 . ? C12 C13 1.389(10) . ? C12 C15 1.505(11) . ? C13 C14 1.367(10) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C21 1.386(10) . ? C16 C17 1.397(9) . ? C17 C18 1.397(9) . ? C17 H17 0.95 . ? C18 C19 1.379(11) . ? C18 H18 0.95 . ? C19 C20 1.377(10) . ? C19 C22 1.500(9) . ? C20 C21 1.388(9) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.376(9) . ? C23 C28 1.400(10) . ? C24 C25 1.374(9) . ? C24 H24 0.95 . ? C25 C26 1.383(10) . ? C25 H25 0.95 . ? C26 C27 1.375(10) . ? C26 C29 1.505(9) . ? C27 C28 1.394(10) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C35 1.389(10) . ? C30 C31 1.398(9) . ? C31 C32 1.388(9) . ? C31 H31 0.95 . ? C32 C33 1.389(10) . ? C32 H32 0.95 . ? C33 C34 1.399(10) . ? C33 C36 1.495(10) . ? C34 C35 1.385(9) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C38 1.368(9) . ? C37 C42 1.402(9) . ? C38 C39 1.394(10) . ? C38 H38 0.95 . ? C39 C40 1.395(10) . ? C39 H39 0.95 . ? C40 C41 1.381(10) . ? C40 C43 1.523(10) . ? C41 C42 1.378(10) . ? C41 H41 0.95 . ? C42 H42 0.95 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.384(9) . ? C44 C49 1.387(9) . ? C45 C46 1.389(10) . ? C45 H45 0.95 . ? C46 C47 1.386(11) . ? C46 H46 0.95 . ? C47 C48 1.377(10) . ? C47 C50 1.510(10) . ? C48 C49 1.377(10) . ? C48 H48 0.95 . ? C49 H49 0.95 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 C56 1.356(13) . ? C51 C52 1.398(13) . ? C51 C57 1.423(15) . ? C52 C53 1.386(18) . ? C52 H52 0.95 . ? C53 C54 1.442(19) . ? C53 H53 0.95 . ? C54 C55 1.284(17) . ? C54 H54 0.95 . ? C55 C56 1.329(16) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? 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 P1 Pt1 P2 51.82(6) . . ? P3 Pt1 P2 91.92(6) . . ? P4 Pt1 P3 106.82(6) . . ? P4 Pt1 P1 109.86(6) . . ? P3 Pt1 P1 142.87(6) . . ? P4 Pt1 P2 161.14(6) . . ? C1 P1 C5 112.5(3) . . ? C1 P1 P2 115.2(2) . . ? C5 P1 P2 118.2(2) . . ? C1 P1 Pt1 118.8(2) . . ? C5 P1 Pt1 118.3(2) . . ? P2 P1 Pt1 66.66(7) . . ? P1 P2 Pt1 61.52(7) . . ? C23 P3 C16 102.2(3) . . ? C23 P3 C9 101.1(3) . . ? C16 P3 C9 104.3(3) . . ? C23 P3 Pt1 120.9(2) . . ? C16 P3 Pt1 115.0(2) . . ? C9 P3 Pt1 111.2(2) . . ? C37 P4 C44 105.8(3) . . ? C37 P4 C30 102.0(3) . . ? C44 P4 C30 98.9(3) . . ? C37 P4 Pt1 114.1(2) . . ? C44 P4 Pt1 115.4(2) . . ? C30 P4 Pt1 118.5(2) . . ? C4 C1 C3 108.8(6) . . ? C4 C1 C2 108.8(6) . . ? C3 C1 C2 109.7(5) . . ? C4 C1 P1 107.1(4) . . ? C3 C1 P1 113.3(5) . . ? C2 C1 P1 109.0(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C6 108.6(6) . . ? C8 C5 C7 111.3(6) . . ? C6 C5 C7 109.2(6) . . ? C8 C5 P1 111.0(5) . . ? C6 C5 P1 106.2(5) . . ? C7 C5 P1 110.4(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 118.0(6) . . ? C14 C9 P3 122.3(5) . . ? C10 C9 P3 119.6(5) . . ? C11 C10 C9 119.4(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 123.0(7) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C11 C12 C13 116.5(7) . . ? C11 C12 C15 121.7(7) . . ? C13 C12 C15 121.8(7) . . ? C14 C13 C12 122.2(7) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C9 120.8(6) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.4(6) . . ? C21 C16 P3 120.0(5) . . ? C17 C16 P3 121.5(5) . . ? C18 C17 C16 120.2(7) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 121.3(7) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 117.8(6) . . ? C20 C19 C22 121.6(7) . . ? C18 C19 C22 120.7(7) . . ? C19 C20 C21 122.2(7) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 120.1(6) . . ? C16 C21 H21 120 . . ? C20 C21 H21 120 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 117.8(6) . . ? C24 C23 P3 119.7(5) . . ? C28 C23 P3 122.5(5) . . ? C25 C24 C23 122.3(6) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 118.6(6) . . ? C27 C26 C29 120.8(7) . . ? C25 C26 C29 120.6(7) . . ? C26 C27 C28 121.4(7) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C23 119.7(7) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 119.2(6) . . ? C35 C30 P4 118.7(5) . . ? C31 C30 P4 122.0(5) . . ? C32 C31 C30 119.6(7) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 122.2(6) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C34 117.0(6) . . ? C32 C33 C36 121.2(7) . . ? C34 C33 C36 121.8(7) . . ? C35 C34 C33 121.9(7) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C30 120.1(6) . . ? C34 C35 H35 120 . . ? C30 C35 H35 120 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 118.2(6) . . ? C38 C37 P4 118.8(5) . . ? C42 C37 P4 123.0(5) . . ? C37 C38 C39 121.8(6) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 120.0(7) . . ? C38 C39 H39 120 . . ? C40 C39 H39 120 . . ? C41 C40 C39 117.9(6) . . ? C41 C40 C43 121.3(7) . . ? C39 C40 C43 120.8(7) . . ? C42 C41 C40 122.0(6) . . ? C42 C41 H41 119 . . ? C40 C41 H41 119 . . ? C41 C42 C37 120.1(7) . . ? C41 C42 H42 120 . . ? C37 C42 H42 120 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 117.4(6) . . ? C45 C44 P4 118.4(5) . . ? C49 C44 P4 124.2(5) . . ? C44 C45 C46 121.8(7) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C47 C46 C45 120.3(7) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 117.8(7) . . ? C48 C47 C50 121.9(7) . . ? C46 C47 C50 120.3(7) . . ? C49 C48 C47 122.0(7) . . ? C49 C48 H48 119 . . ? C47 C48 H48 119 . . ? C48 C49 C44 120.7(7) . . ? C48 C49 H49 119.6 . . ? C44 C49 H49 119.6 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C56 C51 C52 116.3(11) . . ? C56 C51 C57 123.7(10) . . ? C52 C51 C57 120.0(12) . . ? C53 C52 C51 119.2(11) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? C52 C53 C54 120.9(10) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C55 C54 C53 115.4(14) . . ? C55 C54 H54 122.3 . . ? C53 C54 H54 122.3 . . ? C54 C55 C56 125.1(14) . . ? C54 C55 H55 117.5 . . ? C56 C55 H55 117.5 . . ? C55 C56 C51 123.1(10) . . ? C55 C56 H56 118.4 . . ? C51 C56 H56 118.4 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? # end Validation Reply Form #END data_compound_14 _database_code_depnum_ccdc_archive 'CCDC 668507' _audit_creation_date 2007-11-30T12:59:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H60 P6 Pt2' _chemical_formula_sum 'C56 H60 P6 Pt2' _chemical_formula_weight 1309.04 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.5441(16) _cell_length_b 9.6862(10) _cell_length_c 29.7907(17) _cell_angle_alpha 90 _cell_angle_beta 107.751(9) _cell_angle_gamma 90 _cell_volume 5371.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17040 _cell_measurement_theta_min 2.0949 _cell_measurement_theta_max 32.4158 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour pale-brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.0696 _exptl_crystal_size_min 0.0108 _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.417 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.427 _exptl_absorpt_correction_T_max 0.981 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k geometry, 4 circle diffractometer' _diffrn_measurement_device_type 'KM4 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.0195339994 _diffrn_orient_matrix_ub_12 0.0493796644 _diffrn_orient_matrix_ub_13 -0.0087736697 _diffrn_orient_matrix_ub_21 0.0325642044 _diffrn_orient_matrix_ub_22 -0.0251419278 _diffrn_orient_matrix_ub_23 0.0157810488 _diffrn_orient_matrix_ub_31 0.003007081 _diffrn_orient_matrix_ub_32 -0.0479401519 _diffrn_orient_matrix_ub_33 -0.0172860068 _diffrn_reflns_av_R_equivalents 0.1484 _diffrn_reflns_av_unetI/netI 0.144 _diffrn_reflns_number 27697 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 9542 _reflns_number_gt 6149 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1100P)^2^+407.1000P] 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_number_reflns 9542 _refine_ls_number_parameters 581 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1777 _refine_ls_R_factor_gt 0.1227 _refine_ls_wR_factor_ref 0.3115 _refine_ls_wR_factor_gt 0.2875 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.351 _refine_diff_density_min -4.018 _refine_diff_density_rms 0.38 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.27834(6) 0.69055(10) 0.24994(4) 0.0246(3) Uani 1 1 d . . . Pt2 Pt 0.28144(6) 0.73547(10) 0.35892(4) 0.0257(3) Uani 1 1 d . . . P1 P 0.2279(4) 0.8624(7) 0.2879(2) 0.0285(15) Uani 1 1 d . . . P2 P 0.3414(4) 0.8447(6) 0.3105(2) 0.0225(14) Uani 1 1 d . . . P3 P 0.3708(4) 0.5672(6) 0.2382(2) 0.0226(14) Uani 1 1 d . . . P4 P 0.1747(4) 0.6203(7) 0.1965(2) 0.0286(16) Uani 1 1 d . . . P5 P 0.3723(4) 0.6317(7) 0.4151(2) 0.0269(15) Uani 1 1 d . . . P6 P 0.1822(4) 0.6937(7) 0.3808(2) 0.0280(15) Uani 1 1 d . . . C1 C 0.4515(16) 0.543(3) 0.2902(9) 0.033(7) Uani 1 1 d . . . H1A H 0.4361 0.5156 0.3177 0.044 Uiso 1 1 calc R . . H1B H 0.4809 0.4663 0.2837 0.044 Uiso 1 1 calc R . . C2 C 0.4974(17) 0.672(3) 0.3024(10) 0.039(7) Uani 1 1 d . . . H2A H 0.5152 0.6957 0.276 0.058 Uiso 1 1 calc R . . H2B H 0.5382 0.6547 0.3306 0.058 Uiso 1 1 calc R . . H2C H 0.4684 0.7479 0.3084 0.058 Uiso 1 1 calc R . . C3 C 0.4125(13) 0.634(2) 0.1964(8) 0.022(5) Uani 1 1 d . . . C4 C 0.3933(15) 0.765(3) 0.1743(10) 0.037(7) Uani 1 1 d . . . H4 H 0.3567 0.8182 0.1811 0.044 Uiso 1 1 calc R . . C5 C 0.4263(16) 0.815(3) 0.1438(10) 0.035(7) Uani 1 1 d . . . H5 H 0.4121 0.9024 0.1293 0.043 Uiso 1 1 calc R . . C6 C 0.4788(17) 0.744(3) 0.1337(9) 0.036(7) Uani 1 1 d . . . H6 H 0.4997 0.7785 0.111 0.043 Uiso 1 1 calc R . . C7 C 0.5015(17) 0.623(3) 0.1560(11) 0.038(7) Uani 1 1 d . . . H7 H 0.5416 0.5775 0.151 0.045 Uiso 1 1 calc R . . C8 C 0.4672(14) 0.565(3) 0.1860(9) 0.026(6) Uani 1 1 d . . . H8 H 0.4818 0.4767 0.1994 0.031 Uiso 1 1 calc R . . C9 C 0.3526(16) 0.387(3) 0.2191(10) 0.033(5) Uani 1 1 d U . . C10 C 0.3554(17) 0.282(3) 0.2514(11) 0.037(5) Uani 1 1 d U . . H10 H 0.3732 0.3022 0.2842 0.044 Uiso 1 1 calc R . . C11 C 0.3328(17) 0.151(3) 0.2371(13) 0.045(8) Uani 1 1 d . . . H11 H 0.3345 0.0822 0.2601 0.054 Uiso 1 1 calc R . . C12 C 0.3076(19) 0.116(3) 0.1897(14) 0.051(9) Uani 1 1 d . . . H12 H 0.2956 0.0235 0.1803 0.061 Uiso 1 1 calc R . . C13 C 0.3003(17) 0.220(3) 0.1564(11) 0.040(7) Uani 1 1 d . . . H13 H 0.2789 0.2008 0.1239 0.048 Uiso 1 1 calc R . . C14 C 0.3247(16) 0.354(3) 0.1712(10) 0.036(5) Uani 1 1 d U . . H14 H 0.3223 0.424 0.1483 0.043 Uiso 1 1 calc R . . C15 C 0.1096(15) 0.753(3) 0.1794(10) 0.036(5) Uani 1 1 d U . . H15A H 0.0672 0.7166 0.1547 0.047 Uiso 1 1 calc R . . H15B H 0.0939 0.7788 0.2069 0.047 Uiso 1 1 calc R . . C16 C 0.1366(15) 0.888(3) 0.1598(10) 0.034(5) Uani 1 1 d U . . H16A H 0.1719 0.9358 0.1857 0.051 Uiso 1 1 calc R . . H16B H 0.0957 0.9495 0.146 0.051 Uiso 1 1 calc R . . H16C H 0.1588 0.8625 0.1356 0.051 Uiso 1 1 calc R . . C17 C 0.1752(19) 0.559(3) 0.1394(12) 0.046(8) Uani 1 1 d . . . C18 C 0.2192(18) 0.623(4) 0.1164(11) 0.047(8) Uani 1 1 d . . . H18 H 0.2479 0.6992 0.1315 0.057 Uiso 1 1 calc R . . C19 C 0.2229(19) 0.581(4) 0.0723(12) 0.053(7) Uani 1 1 d U . . H19 H 0.2513 0.6316 0.0571 0.064 Uiso 1 1 calc R . . C20 C 0.1853(19) 0.468(4) 0.0512(12) 0.054(6) Uani 1 1 d U . . H20 H 0.1875 0.4375 0.0213 0.065 Uiso 1 1 calc R . . C21 C 0.145(2) 0.398(4) 0.0736(12) 0.056(7) Uani 1 1 d U . . H21 H 0.1196 0.3176 0.0591 0.068 Uiso 1 1 calc R . . C22 C 0.1390(17) 0.439(3) 0.1160(10) 0.040(7) Uani 1 1 d . . . H22 H 0.1101 0.3873 0.1303 0.048 Uiso 1 1 calc R . . C23 C 0.1268(13) 0.482(2) 0.2168(8) 0.020(5) Uani 1 1 d . . . C24 C 0.1657(17) 0.369(3) 0.2389(11) 0.043(8) Uani 1 1 d . . . H24 H 0.2161 0.3665 0.2441 0.052 Uiso 1 1 calc R . . C25 C 0.1329(17) 0.257(4) 0.2537(12) 0.049(8) Uani 1 1 d . . . H25 H 0.1597 0.177 0.2669 0.059 Uiso 1 1 calc R . . C26 C 0.0627(18) 0.266(3) 0.2490(11) 0.044(8) Uani 1 1 d . . . H26 H 0.041 0.1927 0.2612 0.053 Uiso 1 1 calc R . . C27 C 0.0197(18) 0.376(3) 0.2271(11) 0.041(7) Uani 1 1 d . . . H27 H -0.0303 0.3781 0.2234 0.049 Uiso 1 1 calc R . . C28 C 0.0531(17) 0.485(3) 0.2109(10) 0.037(7) Uani 1 1 d . . . H28 H 0.0253 0.5619 0.1957 0.045 Uiso 1 1 calc R . . C29 C 0.3762(18) 0.652(3) 0.4768(10) 0.037(6) Uani 1 1 d U . . H29A H 0.3385 0.5936 0.4829 0.048 Uiso 1 1 calc R . . H29B H 0.4232 0.6172 0.4969 0.048 Uiso 1 1 calc R . . C30 C 0.3665(17) 0.801(2) 0.4921(10) 0.035(5) Uani 1 1 d U . . H30A H 0.4097 0.8551 0.494 0.052 Uiso 1 1 calc R . . H30B H 0.3587 0.7999 0.5231 0.052 Uiso 1 1 calc R . . H30C H 0.3249 0.8435 0.469 0.052 Uiso 1 1 calc R . . C31 C 0.4660(15) 0.683(3) 0.4194(9) 0.031(6) Uani 1 1 d . . . C32 C 0.4784(14) 0.822(3) 0.4190(9) 0.029(6) Uani 1 1 d . . . H32 H 0.4397 0.8853 0.4134 0.035 Uiso 1 1 calc R . . C33 C 0.5490(13) 0.869(3) 0.4268(8) 0.022(5) Uani 1 1 d . . . H33 H 0.5592 0.9646 0.4267 0.027 Uiso 1 1 calc R . . C34 C 0.6023(17) 0.773(3) 0.4346(9) 0.037(7) Uani 1 1 d . . . H34 H 0.6504 0.805 0.4412 0.044 Uiso 1 1 calc R . . C35 C 0.5898(16) 0.630(3) 0.4335(9) 0.032(6) Uani 1 1 d . . . H35 H 0.628 0.5655 0.4376 0.038 Uiso 1 1 calc R . . C36 C 0.5214(13) 0.586(3) 0.4263(9) 0.029(6) Uani 1 1 d . . . H36 H 0.5111 0.4903 0.426 0.035 Uiso 1 1 calc R . . C37 C 0.3691(16) 0.440(3) 0.4091(9) 0.031(7) Uani 1 1 d . . . C38 C 0.4018(16) 0.353(3) 0.4459(10) 0.034(7) Uani 1 1 d . . . H38 H 0.4319 0.389 0.4748 0.041 Uiso 1 1 calc R . . C39 C 0.3904(18) 0.212(3) 0.4404(10) 0.037(7) Uani 1 1 d . . . H39 H 0.412 0.1501 0.4655 0.044 Uiso 1 1 calc R . . C40 C 0.3477(17) 0.163(3) 0.3985(9) 0.034(7) Uani 1 1 d . . . H40 H 0.3392 0.0668 0.3953 0.04 Uiso 1 1 calc R . . C41 C 0.3164(15) 0.246(3) 0.3605(8) 0.026(6) Uani 1 1 d . . . H41 H 0.2874 0.2086 0.3314 0.032 Uiso 1 1 calc R . . C42 C 0.3288(17) 0.388(3) 0.3662(10) 0.038(8) Uani 1 1 d . . . H42 H 0.3094 0.4489 0.3404 0.045 Uiso 1 1 calc R . . C43 C 0.1110(15) 0.601(3) 0.3345(10) 0.034(7) Uani 1 1 d U . . H43A H 0.0967 0.6606 0.3062 0.044 Uiso 1 1 calc R . . H43B H 0.1334 0.5171 0.3258 0.044 Uiso 1 1 calc R . . C44 C 0.0452(16) 0.557(3) 0.3441(11) 0.041(7) Uani 1 1 d U . . H44A H 0.0575 0.4997 0.3726 0.062 Uiso 1 1 calc R . . H44B H 0.0155 0.503 0.3173 0.062 Uiso 1 1 calc R . . H44C H 0.0184 0.6383 0.3487 0.062 Uiso 1 1 calc R . . C45 C 0.1389(14) 0.854(3) 0.3920(11) 0.033(7) Uani 1 1 d . . . C46 C 0.1587(15) 0.977(3) 0.3805(10) 0.032(6) Uani 1 1 d . . . H46 H 0.196 0.9787 0.3662 0.038 Uiso 1 1 calc R . . C47 C 0.1310(18) 1.099(3) 0.3871(12) 0.044(8) Uani 1 1 d . . . H47 H 0.1476 1.1835 0.3781 0.053 Uiso 1 1 calc R . . C48 C 0.0765(18) 1.093(3) 0.4077(13) 0.050(9) Uani 1 1 d . . . H48 H 0.0556 1.178 0.4129 0.061 Uiso 1 1 calc R . . C49 C 0.050(2) 0.971(4) 0.4216(12) 0.058(10) Uani 1 1 d . . . H49 H 0.013 0.9707 0.4361 0.069 Uiso 1 1 calc R . . C50 C 0.0828(16) 0.850(3) 0.4124(9) 0.036(7) Uani 1 1 d . . . H50 H 0.0666 0.7631 0.4201 0.043 Uiso 1 1 calc R . . C51 C 0.1947(14) 0.589(3) 0.4353(8) 0.026(6) Uani 1 1 d . . . C52 C 0.2033(14) 0.444(3) 0.4318(9) 0.030(6) Uani 1 1 d . . . H52 H 0.1994 0.4048 0.4019 0.036 Uiso 1 1 calc R . . C53 C 0.2171(17) 0.359(3) 0.4705(10) 0.038(7) Uani 1 1 d . . . H53 H 0.2252 0.2633 0.4683 0.046 Uiso 1 1 calc R . . C54 C 0.2189(16) 0.421(3) 0.5138(10) 0.037(7) Uani 1 1 d U . . H54 H 0.2267 0.3645 0.541 0.044 Uiso 1 1 calc R . . C55 C 0.2095(15) 0.562(3) 0.5177(9) 0.035(6) Uani 1 1 d U . . H55 H 0.2109 0.6013 0.5471 0.043 Uiso 1 1 calc R . . C56 C 0.1978(13) 0.645(3) 0.4770(9) 0.027(6) Uani 1 1 d U . . H56 H 0.1921 0.742 0.4794 0.033 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 0.0275(6) 0.0181(5) 0.0293(5) 0.0002(4) 0.0102(4) -0.0006(4) Pt2 0.0315(6) 0.0173(5) 0.0292(5) 0.0006(4) 0.0109(4) 0.0002(4) P1 0.024(4) 0.031(4) 0.029(4) -0.003(3) 0.005(3) 0.004(3) P2 0.032(4) 0.009(3) 0.027(3) -0.003(2) 0.010(3) -0.001(3) P3 0.026(4) 0.018(3) 0.025(3) -0.002(2) 0.010(3) 0.001(3) P4 0.033(4) 0.028(4) 0.027(4) 0.004(3) 0.013(3) 0.008(3) P5 0.039(4) 0.017(3) 0.024(3) -0.002(3) 0.008(3) 0.000(3) P6 0.037(4) 0.020(3) 0.029(4) 0.000(3) 0.013(3) -0.002(3) C1 0.05(2) 0.028(15) 0.026(14) -0.005(11) 0.018(14) -0.005(13) C2 0.050(19) 0.034(16) 0.040(16) -0.001(13) 0.026(15) -0.017(14) C3 0.022(14) 0.020(12) 0.024(13) -0.011(10) 0.009(11) 0.004(10) C4 0.025(15) 0.033(16) 0.051(18) -0.012(13) 0.011(13) 0.002(12) C5 0.046(18) 0.017(13) 0.052(18) 0.010(12) 0.027(15) 0.001(12) C6 0.06(2) 0.027(15) 0.029(14) 0.003(12) 0.019(14) -0.010(14) C7 0.046(19) 0.021(14) 0.056(19) 0.003(13) 0.030(16) -0.006(13) C8 0.028(15) 0.017(12) 0.030(14) -0.003(10) 0.005(12) -0.007(10) C9 0.045(11) 0.019(9) 0.041(10) 0.014(8) 0.024(9) -0.001(8) C10 0.049(13) 0.021(10) 0.045(11) 0.013(9) 0.020(10) -0.003(9) C11 0.04(2) 0.014(14) 0.08(2) 0.006(14) 0.021(18) -0.014(13) C12 0.05(2) 0.020(15) 0.09(3) 0.000(16) 0.03(2) 0.001(14) C13 0.044(19) 0.034(17) 0.042(17) -0.010(13) 0.014(15) 0.007(13) C14 0.047(12) 0.021(10) 0.043(11) 0.004(9) 0.020(10) 0.003(9) C15 0.028(12) 0.044(13) 0.043(13) 0.006(11) 0.019(10) 0.000(10) C16 0.026(12) 0.042(13) 0.042(13) 0.016(10) 0.021(10) -0.007(10) C17 0.06(2) 0.018(15) 0.06(2) 0.007(14) 0.017(18) 0.014(14) C18 0.037(19) 0.06(2) 0.045(19) 0.001(16) 0.012(16) 0.017(16) C19 0.058(16) 0.061(15) 0.051(14) -0.011(11) 0.031(12) 0.022(12) C20 0.059(15) 0.062(14) 0.048(13) -0.017(10) 0.027(11) 0.022(11) C21 0.060(16) 0.058(15) 0.052(14) -0.020(12) 0.018(12) 0.023(12) C22 0.04(2) 0.042(18) 0.026(15) -0.011(12) -0.002(14) 0.009(14) C23 0.020(14) 0.026(13) 0.020(12) 0.000(10) 0.014(11) -0.003(10) C24 0.031(18) 0.033(17) 0.06(2) 0.005(14) 0.005(15) 0.001(13) C25 0.030(18) 0.05(2) 0.06(2) 0.002(17) 0.012(16) -0.011(15) C26 0.05(2) 0.032(16) 0.043(18) 0.006(14) 0.010(16) -0.012(15) C27 0.040(19) 0.037(17) 0.048(19) 0.001(14) 0.017(15) 0.000(14) C28 0.05(2) 0.026(15) 0.042(17) -0.012(12) 0.021(15) -0.006(13) C29 0.055(15) 0.016(11) 0.044(13) -0.013(9) 0.022(12) -0.005(10) C30 0.054(15) 0.011(10) 0.045(13) -0.013(9) 0.024(11) -0.010(10) C31 0.034(16) 0.030(15) 0.026(14) 0.005(11) 0.002(12) 0.008(12) C32 0.025(15) 0.033(15) 0.027(14) -0.004(11) 0.005(12) -0.002(12) C33 0.013(13) 0.025(13) 0.027(13) 0.001(10) 0.003(11) -0.001(10) C34 0.039(18) 0.052(19) 0.021(14) 0.007(12) 0.011(13) -0.009(14) C35 0.039(18) 0.035(16) 0.020(13) -0.002(11) 0.006(12) 0.001(13) C36 0.010(13) 0.039(16) 0.037(16) -0.013(12) 0.004(12) 0.003(11) C37 0.048(19) 0.030(15) 0.027(15) 0.000(11) 0.028(14) 0.009(13) C38 0.037(17) 0.031(15) 0.035(16) 0.009(12) 0.011(13) 0.000(12) C39 0.06(2) 0.015(13) 0.031(15) -0.005(11) 0.015(15) 0.010(13) C40 0.05(2) 0.009(12) 0.037(16) -0.004(11) 0.014(14) -0.001(12) C41 0.040(16) 0.024(14) 0.014(12) -0.011(10) 0.009(11) -0.006(12) C42 0.06(2) 0.039(17) 0.033(16) 0.015(13) 0.036(16) 0.018(14) C43 0.039(17) 0.022(14) 0.047(17) -0.003(12) 0.025(14) -0.012(12) C44 0.029(17) 0.035(16) 0.051(18) 0.005(14) 0.000(14) -0.008(13) C45 0.010(13) 0.037(16) 0.055(18) -0.008(13) 0.014(13) 0.003(11) C46 0.025(16) 0.029(15) 0.047(17) 0.005(12) 0.017(14) 0.003(12) C47 0.05(2) 0.028(16) 0.06(2) -0.016(14) 0.016(17) -0.007(14) C48 0.04(2) 0.039(19) 0.08(2) -0.001(17) 0.025(18) 0.000(15) C49 0.06(2) 0.07(3) 0.05(2) -0.009(18) 0.027(18) 0.03(2) C50 0.038(17) 0.049(18) 0.026(14) -0.013(12) 0.017(13) 0.013(14) C51 0.023(14) 0.038(15) 0.016(13) 0.017(11) 0.007(11) 0.009(11) C52 0.017(14) 0.040(16) 0.025(14) 0.009(12) -0.005(11) -0.005(12) C53 0.048(19) 0.021(14) 0.047(18) 0.018(12) 0.015(15) -0.004(13) C54 0.032(16) 0.047(16) 0.025(14) 0.006(12) -0.002(12) -0.014(13) C55 0.027(14) 0.057(16) 0.022(13) 0.005(12) 0.008(11) -0.013(12) C56 0.008(12) 0.032(14) 0.040(15) 0.005(11) 0.004(11) 0.011(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P4 2.265(8) . ? Pt1 P3 2.280(6) . ? Pt1 P2 2.377(6) . ? Pt1 P1 2.388(7) . ? Pt2 P6 2.264(7) . ? Pt2 P5 2.270(7) . ? Pt2 P2 2.367(6) . ? Pt2 P1 2.395(7) . ? P1 P2 2.121(10) . ? P3 C3 1.80(2) . ? P3 C9 1.83(3) . ? P3 C1 1.86(3) . ? P4 C15 1.77(3) . ? P4 C17 1.81(3) . ? P4 C23 1.84(2) . ? P5 C29 1.83(3) . ? P5 C37 1.86(3) . ? P5 C31 1.86(3) . ? P6 C45 1.85(3) . ? P6 C43 1.87(3) . ? P6 C51 1.87(2) . ? C1 C2 1.52(4) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C8 1.37(3) . ? C3 C4 1.43(4) . ? C4 C5 1.36(4) . ? C4 H4 0.95 . ? C5 C6 1.34(4) . ? C5 H5 0.95 . ? C6 C7 1.35(4) . ? C6 H6 0.95 . ? C7 C8 1.39(4) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? C9 C10 1.39(3) . ? C9 C14 1.40(4) . ? C10 C11 1.37(4) . ? C10 H10 0.95 . ? C11 C12 1.39(5) . ? C11 H11 0.95 . ? C12 C13 1.39(4) . ? C12 H12 0.95 . ? C13 C14 1.41(4) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.59(4) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.40(5) . ? C17 C22 1.43(4) . ? C18 C19 1.40(4) . ? C18 H18 0.95 . ? C19 C20 1.37(5) . ? C19 H19 0.95 . ? C20 C21 1.36(5) . ? C20 H20 0.95 . ? C21 C22 1.36(4) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 C24 1.38(4) . ? C23 C28 1.40(4) . ? C24 C25 1.40(4) . ? C24 H24 0.95 . ? C25 C26 1.34(5) . ? C25 H25 0.95 . ? C26 C27 1.40(4) . ? C26 H26 0.95 . ? C27 C28 1.40(4) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? C29 C30 1.54(3) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C32 1.37(4) . ? C31 C36 1.40(4) . ? C32 C33 1.40(3) . ? C32 H32 0.95 . ? C33 C34 1.36(4) . ? C33 H33 0.95 . ? C34 C35 1.41(4) . ? C34 H34 0.95 . ? C35 C36 1.35(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C42 1.38(4) . ? C37 C38 1.38(4) . ? C38 C39 1.39(4) . ? C38 H38 0.95 . ? C39 C40 1.36(4) . ? C39 H39 0.95 . ? C40 C41 1.37(4) . ? C40 H40 0.95 . ? C41 C42 1.40(4) . ? C41 H41 0.95 . ? C42 H42 0.95 . ? C43 C44 1.46(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 C46 1.33(4) . ? C45 C50 1.41(4) . ? C46 C47 1.33(4) . ? C46 H46 0.95 . ? C47 C48 1.38(4) . ? C47 H47 0.95 . ? C48 C49 1.40(5) . ? C48 H48 0.95 . ? C49 C50 1.40(4) . ? C49 H49 0.95 . ? C50 H50 0.95 . ? C51 C56 1.34(4) . ? C51 C52 1.42(4) . ? C52 C53 1.37(4) . ? C52 H52 0.95 . ? C53 C54 1.41(4) . ? C53 H53 0.95 . ? C54 C55 1.38(4) . ? C54 H54 0.95 . ? C55 C56 1.42(4) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? 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 P4 Pt1 P3 108.4(2) . . ? P4 Pt1 P2 150.2(2) . . ? P3 Pt1 P2 101.2(2) . . ? P4 Pt1 P1 97.6(2) . . ? P3 Pt1 P1 154.0(2) . . ? P2 Pt1 P1 52.8(2) . . ? P6 Pt2 P5 104.8(3) . . ? P6 Pt2 P2 151.9(2) . . ? P5 Pt2 P2 103.1(2) . . ? P6 Pt2 P1 99.4(3) . . ? P5 Pt2 P1 155.8(2) . . ? P2 Pt2 P1 52.9(2) . . ? P2 P1 Pt1 63.3(2) . . ? P2 P1 Pt2 62.9(3) . . ? Pt1 P1 Pt2 85.9(2) . . ? P1 P2 Pt2 64.2(3) . . ? P1 P2 Pt1 63.8(3) . . ? Pt2 P2 Pt1 86.7(2) . . ? C3 P3 C9 102.2(11) . . ? C3 P3 C1 100.0(12) . . ? C9 P3 C1 99.9(13) . . ? C3 P3 Pt1 117.7(8) . . ? C9 P3 Pt1 117.3(10) . . ? C1 P3 Pt1 116.8(9) . . ? C15 P4 C17 100.2(14) . . ? C15 P4 C23 103.3(12) . . ? C17 P4 C23 102.7(13) . . ? C15 P4 Pt1 113.2(11) . . ? C17 P4 Pt1 120.0(12) . . ? C23 P4 Pt1 115.1(8) . . ? C29 P5 C37 101.2(12) . . ? C29 P5 C31 99.4(13) . . ? C37 P5 C31 105.9(13) . . ? C29 P5 Pt2 118.6(10) . . ? C37 P5 Pt2 112.0(10) . . ? C31 P5 Pt2 117.7(8) . . ? C45 P6 C43 105.1(13) . . ? C45 P6 C51 104.1(13) . . ? C43 P6 C51 104.6(12) . . ? C45 P6 Pt2 112.5(9) . . ? C43 P6 Pt2 112.6(8) . . ? C51 P6 Pt2 116.8(9) . . ? C2 C1 P3 113(2) . . ? C2 C1 H1A 109.1 . . ? P3 C1 H1A 109.1 . . ? C2 C1 H1B 109.1 . . ? P3 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 116(2) . . ? C8 C3 P3 122.1(19) . . ? C4 C3 P3 121.7(18) . . ? C5 C4 C3 121(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 121(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 119(3) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 121(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C3 C8 C7 121(2) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C14 118(3) . . ? C10 C9 P3 121(2) . . ? C14 C9 P3 120.7(19) . . ? C11 C10 C9 121(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 122(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 119(3) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C14 120(3) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C9 C14 C13 121(3) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 P4 114.5(19) . . ? C16 C15 H15A 108.6 . . ? P4 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P4 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 114(3) . . ? C18 C17 P4 120(3) . . ? C22 C17 P4 126(3) . . ? C17 C18 C19 123(4) . . ? C17 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C20 C19 C18 119(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 119(3) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 122(4) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C21 C22 C17 122(3) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C24 C23 C28 118(2) . . ? C24 C23 P4 118(2) . . ? C28 C23 P4 124(2) . . ? C23 C24 C25 122(3) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 118(3) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? C25 C26 C27 123(3) . . ? C25 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C28 118(3) . . ? C26 C27 H27 121.2 . . ? C28 C27 H27 121.2 . . ? C23 C28 C27 121(3) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 P5 115(2) . . ? C30 C29 H29A 108.5 . . ? P5 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? P5 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 122(3) . . ? C32 C31 P5 116(2) . . ? C36 C31 P5 122(2) . . ? C31 C32 C33 119(3) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 118(3) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C33 C34 C35 123(3) . . ? C33 C34 H34 118.4 . . ? C35 C34 H34 118.4 . . ? C36 C35 C34 118(3) . . ? C36 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? C35 C36 C31 120(3) . . ? C35 C36 H36 120 . . ? C31 C36 H36 120 . . ? C42 C37 C38 121(3) . . ? C42 C37 P5 117(2) . . ? C38 C37 P5 123(2) . . ? C37 C38 C39 120(3) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 119(3) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 124(2) . . ? C39 C40 H40 118.2 . . ? C41 C40 H40 118.2 . . ? C40 C41 C42 117(2) . . ? C40 C41 H41 121.4 . . ? C42 C41 H41 121.4 . . ? C37 C42 C41 120(2) . . ? C37 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 P6 120(2) . . ? C44 C43 H43A 107.4 . . ? P6 C43 H43A 107.4 . . ? C44 C43 H43B 107.4 . . ? P6 C43 H43B 107.4 . . ? H43A C43 H43B 106.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 118(3) . . ? C46 C45 P6 121(2) . . ? C50 C45 P6 121(2) . . ? C45 C46 C47 126(3) . . ? C45 C46 H46 117 . . ? C47 C46 H46 117 . . ? C46 C47 C48 116(3) . . ? C46 C47 H47 122.2 . . ? C48 C47 H47 122.2 . . ? C47 C48 C49 124(3) . . ? C47 C48 H48 117.8 . . ? C49 C48 H48 117.8 . . ? C48 C49 C50 115(3) . . ? C48 C49 H49 122.6 . . ? C50 C49 H49 122.6 . . ? C49 C50 C45 121(3) . . ? C49 C50 H50 119.3 . . ? C45 C50 H50 119.3 . . ? C56 C51 C52 120(2) . . ? C56 C51 P6 123(2) . . ? C52 C51 P6 117.2(19) . . ? C53 C52 C51 122(3) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 117(3) . . ? C52 C53 H53 121.3 . . ? C54 C53 H53 121.3 . . ? C55 C54 C53 122(3) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C54 C55 C56 119(3) . . ? C54 C55 H55 120.6 . . ? C56 C55 H55 120.6 . . ? C51 C56 C55 121(3) . . ? C51 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 184.5 29.0 2 1.000 0.500 0.500 184.4 28.6 _platon_squeeze_details ; Program fails before normal ending. ; #END