# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'J. Nixon' _publ_contact_author_address ; School of Chemistry and Molecular S University of Sussex BRIGHTON Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email J.NIXON@SUSSEX.AC.UK _publ_section_title ; Facile insertion and halogen migration reactions of the hexaphosphapentaprismane cage, P6C4tBu4 , with zerovalent and divalent platinum complexes. ; _publ_requested_category FM loop_ _publ_author_name 'J. Nixon' 'Mahmoud M. Al-Ktaifani' 'P. B Hitchcock' data_jul301 _database_code_depnum_ccdc_archive 'CCDC 666874' _audit_creation_date 2001-07-03T14:45:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H66 P8 Pt, 2(C H2 Cl2)' _chemical_formula_sum 'C58 H70 Cl4 P8 Pt' _chemical_formula_weight 1351.79 _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 14.4626(5) _cell_length_b 14.5380(5) _cell_length_c 16.4301(4) _cell_angle_alpha 109.342(2) _cell_angle_beta 90.658(2) _cell_angle_gamma 112.736(2) _cell_volume 2967.41(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12610 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.493 _exptl_absorpt_correction_T_max 0.546 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 21171 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0648 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 10414 _reflns_number_gt 8984 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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 ; There are two molecules of dichloromethane solvate; one of which is very poorly defined. C-Cl distance constraints (SADI) were applied. There is residual density in the region of the poorly defined CH2Cl2 molecule. 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^)+(0.0555P)^2^+12.2383P] 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 10414 _refine_ls_number_parameters 640 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.084 _refine_diff_density_min -3.005 _refine_diff_density_rms 0.146 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 Pt Pt 0.648039(17) 0.882290(18) 0.721815(14) 0.02001(9) Uani 1 1 d . . . P1 P 0.68563(12) 1.03865(13) 0.68718(10) 0.0214(3) Uani 1 1 d . . . P2 P 0.83207(12) 1.06365(13) 0.64344(10) 0.0238(3) Uani 1 1 d . . . P3 P 0.84867(14) 1.26665(14) 0.80699(11) 0.0312(4) Uani 1 1 d . . . P4 P 0.98755(13) 1.18082(14) 0.78009(11) 0.0306(4) Uani 1 1 d . . . P5 P 0.81949(12) 0.97394(13) 0.79434(10) 0.0240(3) Uani 1 1 d . . . P6 P 0.79883(13) 1.11260(14) 0.87823(10) 0.0256(4) Uani 1 1 d . . . P7 P 0.62048(13) 0.77474(13) 0.80549(10) 0.0254(4) Uani 1 1 d . . . P8 P 0.50162(12) 0.79379(12) 0.61583(10) 0.0210(3) Uani 1 1 d . . . C1 C 0.7303(5) 1.1462(5) 0.8010(4) 0.0218(13) Uani 1 1 d . . . C2 C 0.6421(5) 1.1760(5) 0.8368(4) 0.0290(14) Uani 1 1 d . . . C3 C 0.5599(6) 1.0798(6) 0.8496(5) 0.0405(18) Uani 1 1 d . . . H3A H 0.5341 1.0193 0.7936 0.061 Uiso 1 1 calc R . . H3B H 0.5042 1.0983 0.8713 0.061 Uiso 1 1 calc R . . H3C H 0.5888 1.06 0.892 0.061 Uiso 1 1 calc R . . C4 C 0.6800(6) 1.2688(6) 0.9263(5) 0.0416(18) Uani 1 1 d . . . H4A H 0.7328 1.3321 0.9201 0.062 Uiso 1 1 calc R . . H4B H 0.7082 1.2477 0.968 0.062 Uiso 1 1 calc R . . H4C H 0.6232 1.2855 0.9475 0.062 Uiso 1 1 calc R . . C5 C 0.5981(6) 1.2117(7) 0.7741(5) 0.0452(19) Uani 1 1 d . . . H5A H 0.6517 1.2736 0.7668 0.068 Uiso 1 1 calc R . . H5B H 0.5438 1.2315 0.798 0.068 Uiso 1 1 calc R . . H5C H 0.5705 1.1528 0.7173 0.068 Uiso 1 1 calc R . . C6 C 0.9025(5) 1.0342(5) 0.7212(4) 0.0245(13) Uani 1 1 d . . . C7 C 0.9636(5) 0.9655(6) 0.6771(4) 0.0334(16) Uani 1 1 d . . . C8 C 1.0369(5) 1.0186(6) 0.6234(5) 0.0386(17) Uani 1 1 d . . . H8A H 0.9986 1.0254 0.5778 0.058 Uiso 1 1 calc R . . H8B H 1.0732 0.9746 0.5963 0.058 Uiso 1 1 calc R . . H8C H 1.0858 1.0898 0.6617 0.058 Uiso 1 1 calc R . . C9 C 1.0272(6) 0.9574(7) 0.7479(5) 0.0417(18) Uani 1 1 d . . . H9A H 0.9823 0.9236 0.7836 0.063 Uiso 1 1 calc R . . H9B H 1.0759 1.0293 0.7851 0.063 Uiso 1 1 calc R . . H9C H 1.0639 0.9141 0.7201 0.063 Uiso 1 1 calc R . . C10 C 0.8883(6) 0.8533(6) 0.6169(5) 0.0445(19) Uani 1 1 d . . . H10A H 0.8482 0.8594 0.5721 0.067 Uiso 1 1 calc R . . H10B H 0.8429 0.8177 0.6514 0.067 Uiso 1 1 calc R . . H10C H 0.9258 0.8111 0.5887 0.067 Uiso 1 1 calc R . . C11 C 0.9044(5) 1.2105(5) 0.7104(4) 0.0269(14) Uani 1 1 d . . . C12 C 0.9497(6) 1.2868(6) 0.6594(5) 0.0372(17) Uani 1 1 d . . . C13 C 1.0088(7) 1.2452(7) 0.5927(5) 0.053(2) Uani 1 1 d . . . H13A H 0.9642 1.1735 0.5518 0.079 Uiso 1 1 calc R . . H13B H 1.0657 1.2415 0.6225 0.079 Uiso 1 1 calc R . . H13C H 1.0351 1.2935 0.5606 0.079 Uiso 1 1 calc R . . C14 C 1.0210(7) 1.3989(6) 0.7219(6) 0.056(2) Uani 1 1 d . . . H14A H 0.9838 1.4273 0.7656 0.084 Uiso 1 1 calc R . . H14B H 1.0468 1.4462 0.6888 0.084 Uiso 1 1 calc R . . H14C H 1.078 1.395 0.7512 0.084 Uiso 1 1 calc R . . C15 C 0.8594(7) 1.2915(7) 0.6127(6) 0.053(2) Uani 1 1 d . . . H15A H 0.821 1.3182 0.6561 0.079 Uiso 1 1 calc R . . H15B H 0.815 1.2196 0.572 0.079 Uiso 1 1 calc R . . H15C H 0.8849 1.3397 0.5804 0.079 Uiso 1 1 calc R . . C16 C 0.9209(5) 1.2217(5) 0.8733(4) 0.0288(14) Uani 1 1 d . . . C17 C 0.9919(6) 1.2953(6) 0.9621(4) 0.0385(17) Uani 1 1 d . . . C18 C 1.0348(6) 1.2306(7) 0.9931(5) 0.0458(19) Uani 1 1 d . . . H18A H 1.08 1.2762 1.0491 0.069 Uiso 1 1 calc R . . H18B H 1.0732 1.2036 0.9498 0.069 Uiso 1 1 calc R . . H18C H 0.9791 1.1702 1.0004 0.069 Uiso 1 1 calc R . . C19 C 1.0802(6) 1.3904(6) 0.9504(6) 0.053(2) Uani 1 1 d . . . H19A H 1.1246 1.4367 1.0067 0.079 Uiso 1 1 calc R . . H19B H 1.0527 1.4316 0.9291 0.079 Uiso 1 1 calc R . . H19C H 1.1193 1.3631 0.9081 0.079 Uiso 1 1 calc R . . C20 C 0.9335(7) 1.3402(7) 1.0305(5) 0.052(2) Uani 1 1 d . . . H20A H 0.9797 1.3867 1.0859 0.078 Uiso 1 1 calc R . . H20B H 0.8779 1.2809 1.0394 0.078 Uiso 1 1 calc R . . H20C H 0.9056 1.3816 1.0099 0.078 Uiso 1 1 calc R . . C21 C 0.4881(5) 0.7050(5) 0.8169(4) 0.0304(15) Uani 1 1 d . . . C22 C 0.4272(5) 0.7626(6) 0.8318(4) 0.0374(17) Uani 1 1 d . . . H22 H 0.455 0.8342 0.8337 0.045 Uiso 1 1 calc R . . C23 C 0.3292(6) 0.7173(7) 0.8435(5) 0.0448(19) Uani 1 1 d . . . H23 H 0.2899 0.7583 0.8547 0.054 Uiso 1 1 calc R . . C24 C 0.2860(6) 0.6130(7) 0.8393(5) 0.053(2) Uani 1 1 d . . . H24 H 0.2175 0.5815 0.8473 0.064 Uiso 1 1 calc R . . C25 C 0.3446(7) 0.5552(7) 0.8231(6) 0.059(2) Uani 1 1 d . . . H25 H 0.3151 0.4828 0.8193 0.07 Uiso 1 1 calc R . . C26 C 0.4456(6) 0.6000(6) 0.8123(5) 0.045(2) Uani 1 1 d . . . H26 H 0.4848 0.559 0.802 0.054 Uiso 1 1 calc R . . C27 C 0.6819(5) 0.8612(5) 0.9187(4) 0.0305(15) Uani 1 1 d . . . C28 C 0.6354(6) 0.9163(5) 0.9762(4) 0.0345(16) Uani 1 1 d . . . H28 H 0.5665 0.9018 0.96 0.041 Uiso 1 1 calc R . . C29 C 0.6880(6) 0.9925(6) 1.0571(5) 0.0419(18) Uani 1 1 d . . . H29 H 0.6553 1.0307 1.0951 0.05 Uiso 1 1 calc R . . C30 C 0.7881(6) 1.0136(6) 1.0831(4) 0.0426(19) Uani 1 1 d . . . H30 H 0.8238 1.0655 1.1388 0.051 Uiso 1 1 calc R . . C31 C 0.8348(6) 0.9583(6) 1.0275(5) 0.0413(19) Uani 1 1 d . . . H31 H 0.9032 0.9721 1.045 0.05 Uiso 1 1 calc R . . C32 C 0.7831(5) 0.8818(6) 0.9453(4) 0.0327(16) Uani 1 1 d . . . H32 H 0.8162 0.8439 0.9075 0.039 Uiso 1 1 calc R . . C33 C 0.6718(6) 0.6743(6) 0.7789(5) 0.0374(17) Uani 1 1 d . . . C34 C 0.7013(6) 0.6434(6) 0.6978(5) 0.0413(18) Uani 1 1 d . . . H34 H 0.6931 0.6739 0.6567 0.05 Uiso 1 1 calc R . . C35 C 0.7432(7) 0.5672(7) 0.6758(7) 0.065(3) Uani 1 1 d . . . H35 H 0.7633 0.546 0.6202 0.078 Uiso 1 1 calc R . . C36 C 0.7548(8) 0.5240(8) 0.7363(9) 0.078(3) Uani 1 1 d . . . H36 H 0.7822 0.4719 0.7215 0.094 Uiso 1 1 calc R . . C37 C 0.7278(8) 0.5543(7) 0.8168(8) 0.069(3) Uani 1 1 d . . . H37 H 0.7386 0.525 0.8579 0.083 Uiso 1 1 calc R . . C38 C 0.6840(7) 0.6286(6) 0.8393(5) 0.051(2) Uani 1 1 d . . . H38 H 0.6628 0.6477 0.8947 0.061 Uiso 1 1 calc R . . C39 C 0.4220(5) 0.8648(5) 0.6158(4) 0.0247(13) Uani 1 1 d . . . C40 C 0.3629(5) 0.8788(6) 0.6818(4) 0.0331(16) Uani 1 1 d . . . H40 H 0.3633 0.8487 0.7251 0.04 Uiso 1 1 calc R . . C41 C 0.3036(5) 0.9355(6) 0.6857(5) 0.0363(16) Uani 1 1 d . . . H41 H 0.2636 0.9435 0.7308 0.044 Uiso 1 1 calc R . . C42 C 0.3032(5) 0.9801(6) 0.6232(5) 0.0382(17) Uani 1 1 d . . . H42 H 0.2635 1.0197 0.6258 0.046 Uiso 1 1 calc R . . C43 C 0.3600(6) 0.9671(6) 0.5579(5) 0.0399(18) Uani 1 1 d . . . H43 H 0.3591 0.9972 0.5148 0.048 Uiso 1 1 calc R . . C44 C 0.4194(5) 0.9098(5) 0.5541(4) 0.0324(15) Uani 1 1 d . . . H44 H 0.4586 0.9016 0.5084 0.039 Uiso 1 1 calc R . . C45 C 0.5407(5) 0.7678(5) 0.5074(4) 0.0224(13) Uani 1 1 d . . . C46 C 0.6424(5) 0.8050(5) 0.4993(4) 0.0270(14) Uani 1 1 d . . . H46 H 0.6926 0.847 0.5501 0.032 Uiso 1 1 calc R . . C47 C 0.6719(6) 0.7813(5) 0.4171(4) 0.0333(16) Uani 1 1 d . . . H47 H 0.7419 0.8078 0.4121 0.04 Uiso 1 1 calc R . . C48 C 0.5993(6) 0.7193(6) 0.3428(5) 0.0386(18) Uani 1 1 d . . . H48 H 0.6194 0.7029 0.2868 0.046 Uiso 1 1 calc R . . C49 C 0.4981(6) 0.6815(6) 0.3504(5) 0.0417(18) Uani 1 1 d . . . H49 H 0.4485 0.6391 0.2992 0.05 Uiso 1 1 calc R . . C50 C 0.4671(5) 0.7042(6) 0.4311(4) 0.0339(16) Uani 1 1 d . . . H50 H 0.3969 0.6772 0.4353 0.041 Uiso 1 1 calc R . . C51 C 0.4105(5) 0.6568(5) 0.5996(4) 0.0249(14) Uani 1 1 d . . . C52 C 0.3060(6) 0.6241(6) 0.5925(5) 0.0415(18) Uani 1 1 d . . . H52 H 0.2774 0.6744 0.5987 0.05 Uiso 1 1 calc R . . C53 C 0.2435(6) 0.5171(6) 0.5763(6) 0.051(2) Uani 1 1 d . . . H53 H 0.1721 0.495 0.5722 0.061 Uiso 1 1 calc R . . C54 C 0.2835(6) 0.4431(6) 0.5662(5) 0.0429(19) Uani 1 1 d . . . H54 H 0.2402 0.3702 0.5546 0.052 Uiso 1 1 calc R . . C55 C 0.3869(6) 0.4761(6) 0.5733(5) 0.0371(17) Uani 1 1 d . . . H55 H 0.4155 0.4256 0.5663 0.045 Uiso 1 1 calc R . . C56 C 0.4494(5) 0.5818(5) 0.5903(4) 0.0296(15) Uani 1 1 d . . . H56 H 0.5208 0.6034 0.5957 0.036 Uiso 1 1 calc R . . C57 C 1.3592(7) 1.2471(9) 0.8850(8) 0.081(3) Uani 1 1 d D A 1 H57A H 1.3446 1.2161 0.9312 0.097 Uiso 1 1 calc R A 1 H57B H 1.3852 1.2028 0.8401 0.097 Uiso 1 1 calc R A 1 Cl1 Cl 1.2488(2) 1.2350(3) 0.8387(2) 0.0824(8) Uani 1 1 d D A 1 Cl2 Cl 1.4523(3) 1.3708(3) 0.9294(3) 0.1172(13) Uani 1 1 d D A 1 C58 C 1.009(2) 0.6715(18) 0.6703(8) 0.31(2) Uani 1 1 d D B 1 H58A H 0.9376 0.6285 0.6743 0.371 Uiso 1 1 calc R B 1 H58B H 1.0107 0.7406 0.6711 0.371 Uiso 1 1 calc R B 1 Cl3 Cl 1.0242(8) 0.6163(13) 0.5800(4) 0.350(8) Uani 1 1 d D B 1 Cl4 Cl 1.0724(6) 0.6979(3) 0.7579(3) 0.209(3) Uani 1 1 d D B 1 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 Pt 0.02137(14) 0.01762(14) 0.01912(13) 0.00612(9) 0.00125(9) 0.00665(10) P1 0.0231(8) 0.0186(8) 0.0221(8) 0.0082(6) 0.0026(6) 0.0074(7) P2 0.0243(9) 0.0214(9) 0.0217(8) 0.0066(7) 0.0042(6) 0.0063(7) P3 0.0351(10) 0.0207(9) 0.0303(9) 0.0055(7) 0.0045(7) 0.0072(8) P4 0.0241(9) 0.0259(9) 0.0297(9) 0.0050(7) 0.0001(7) 0.0025(8) P5 0.0247(9) 0.0230(9) 0.0218(8) 0.0064(7) 0.0001(6) 0.0089(7) P6 0.0277(9) 0.0252(9) 0.0211(8) 0.0059(7) 0.0024(6) 0.0102(7) P7 0.0325(9) 0.0192(8) 0.0231(8) 0.0083(7) 0.0007(7) 0.0088(7) P8 0.0203(8) 0.0178(8) 0.0223(8) 0.0068(6) 0.0000(6) 0.0058(7) C1 0.026(3) 0.016(3) 0.017(3) 0.003(2) 0.001(2) 0.005(3) C2 0.037(4) 0.028(4) 0.026(3) 0.009(3) 0.008(3) 0.018(3) C3 0.038(4) 0.043(5) 0.046(4) 0.022(4) 0.018(3) 0.018(4) C4 0.051(5) 0.034(4) 0.039(4) 0.003(3) 0.011(3) 0.025(4) C5 0.054(5) 0.053(5) 0.050(5) 0.025(4) 0.015(4) 0.039(4) C6 0.020(3) 0.025(3) 0.024(3) 0.005(3) -0.001(2) 0.008(3) C7 0.025(4) 0.038(4) 0.034(4) 0.006(3) 0.007(3) 0.016(3) C8 0.024(4) 0.050(5) 0.039(4) 0.011(4) 0.013(3) 0.016(3) C9 0.036(4) 0.049(5) 0.044(4) 0.013(4) 0.002(3) 0.025(4) C10 0.043(5) 0.038(4) 0.046(4) 0.001(4) 0.006(4) 0.023(4) C11 0.028(4) 0.020(3) 0.028(3) 0.008(3) 0.001(3) 0.006(3) C12 0.043(4) 0.023(4) 0.038(4) 0.011(3) 0.013(3) 0.005(3) C13 0.064(6) 0.041(5) 0.049(5) 0.022(4) 0.030(4) 0.011(4) C14 0.064(6) 0.029(4) 0.053(5) 0.015(4) 0.013(4) -0.005(4) C15 0.063(6) 0.041(5) 0.059(5) 0.032(4) 0.009(4) 0.015(4) C16 0.029(4) 0.025(4) 0.029(3) 0.009(3) 0.001(3) 0.008(3) C17 0.038(4) 0.034(4) 0.028(4) -0.001(3) -0.006(3) 0.009(3) C18 0.046(5) 0.044(5) 0.038(4) 0.011(4) -0.007(3) 0.013(4) C19 0.051(5) 0.021(4) 0.059(5) 0.003(4) -0.017(4) -0.002(4) C20 0.055(5) 0.048(5) 0.036(4) -0.002(4) -0.008(4) 0.019(4) C21 0.036(4) 0.025(4) 0.025(3) 0.009(3) 0.007(3) 0.007(3) C22 0.036(4) 0.040(4) 0.034(4) 0.017(3) 0.003(3) 0.009(3) C23 0.033(4) 0.053(5) 0.041(4) 0.015(4) 0.013(3) 0.012(4) C24 0.036(5) 0.054(6) 0.045(5) 0.014(4) 0.012(4) -0.004(4) C25 0.061(6) 0.033(5) 0.058(5) 0.013(4) 0.011(4) -0.002(4) C26 0.052(5) 0.026(4) 0.040(4) 0.007(3) 0.007(4) 0.004(4) C27 0.042(4) 0.023(3) 0.024(3) 0.008(3) 0.001(3) 0.011(3) C28 0.039(4) 0.025(4) 0.030(4) 0.008(3) 0.002(3) 0.006(3) C29 0.057(5) 0.036(4) 0.031(4) 0.011(3) 0.014(3) 0.018(4) C30 0.052(5) 0.038(4) 0.020(3) 0.007(3) -0.003(3) 0.004(4) C31 0.046(5) 0.040(4) 0.029(4) 0.014(3) -0.007(3) 0.008(4) C32 0.037(4) 0.029(4) 0.031(4) 0.011(3) -0.001(3) 0.011(3) C33 0.037(4) 0.028(4) 0.040(4) 0.005(3) -0.006(3) 0.012(3) C34 0.036(4) 0.026(4) 0.050(5) 0.000(3) 0.000(3) 0.013(3) C35 0.058(6) 0.038(5) 0.083(7) -0.001(5) 0.008(5) 0.024(5) C36 0.068(7) 0.039(6) 0.114(10) 0.002(6) -0.013(6) 0.031(5) C37 0.074(7) 0.033(5) 0.089(8) 0.012(5) -0.040(6) 0.021(5) C38 0.075(6) 0.029(4) 0.044(4) 0.007(3) -0.016(4) 0.022(4) C39 0.021(3) 0.022(3) 0.028(3) 0.006(3) -0.001(2) 0.009(3) C40 0.038(4) 0.040(4) 0.029(3) 0.017(3) 0.007(3) 0.021(3) C41 0.034(4) 0.042(4) 0.040(4) 0.015(3) 0.010(3) 0.023(4) C42 0.033(4) 0.036(4) 0.053(5) 0.020(4) 0.005(3) 0.019(3) C43 0.041(4) 0.044(5) 0.045(4) 0.028(4) 0.005(3) 0.018(4) C44 0.037(4) 0.030(4) 0.035(4) 0.017(3) 0.014(3) 0.015(3) C45 0.028(3) 0.016(3) 0.022(3) 0.007(2) 0.002(2) 0.009(3) C46 0.031(4) 0.018(3) 0.029(3) 0.008(3) 0.002(3) 0.008(3) C47 0.039(4) 0.025(4) 0.038(4) 0.012(3) 0.017(3) 0.015(3) C48 0.060(5) 0.037(4) 0.028(4) 0.016(3) 0.013(3) 0.026(4) C49 0.056(5) 0.041(5) 0.026(4) 0.007(3) -0.002(3) 0.021(4) C50 0.032(4) 0.032(4) 0.034(4) 0.011(3) -0.002(3) 0.010(3) C51 0.026(3) 0.027(4) 0.019(3) 0.010(3) 0.002(2) 0.008(3) C52 0.033(4) 0.027(4) 0.059(5) 0.013(4) 0.011(3) 0.009(3) C53 0.028(4) 0.034(5) 0.083(6) 0.022(4) 0.009(4) 0.004(4) C54 0.042(5) 0.016(4) 0.057(5) 0.012(3) 0.009(4) -0.001(3) C55 0.042(4) 0.025(4) 0.042(4) 0.013(3) 0.003(3) 0.010(3) C56 0.026(4) 0.020(3) 0.036(4) 0.009(3) -0.002(3) 0.005(3) C57 0.066(7) 0.087(8) 0.095(8) 0.057(7) 0.005(6) 0.018(6) Cl1 0.0580(16) 0.102(2) 0.099(2) 0.0559(18) 0.0189(14) 0.0289(15) Cl2 0.084(2) 0.086(2) 0.130(3) -0.014(2) -0.020(2) 0.0278(19) C58 0.40(5) 0.124(18) 0.33(4) -0.08(2) -0.20(4) 0.18(3) Cl3 0.403(12) 0.82(2) 0.130(4) 0.231(9) 0.133(6) 0.503(16) Cl4 0.352(9) 0.075(3) 0.132(4) 0.000(2) -0.120(5) 0.057(4) #----------------------------------------------------------------------------# # 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 Pt P7 2.3342(16) . ? Pt P8 2.3446(15) . ? Pt P5 2.3812(16) . ? Pt P1 2.3865(15) . ? P1 C1 1.901(6) . ? P1 P2 2.179(2) . ? P2 C6 1.877(6) . ? P2 C11 1.885(7) . ? P3 C11 1.874(7) . ? P3 C1 1.891(6) . ? P3 C16 1.917(7) . ? P4 C16 1.871(7) . ? P4 C6 1.891(7) . ? P4 C11 1.907(7) . ? P5 C6 1.890(6) . ? P5 P6 2.165(2) . ? P6 C16 1.888(7) . ? P6 C1 1.893(6) . ? P7 C33 1.816(8) . ? P7 C21 1.834(7) . ? P7 C27 1.839(7) . ? P8 C39 1.820(6) . ? P8 C45 1.839(6) . ? P8 C51 1.840(6) . ? C1 C2 1.561(9) . ? C2 C5 1.525(9) . ? C2 C3 1.526(10) . ? C2 C4 1.542(9) . ? C6 C7 1.586(9) . ? C7 C8 1.529(10) . ? C7 C10 1.536(10) . ? C7 C9 1.536(10) . ? C11 C12 1.559(9) . ? C12 C13 1.510(11) . ? C12 C14 1.530(10) . ? C12 C15 1.542(11) . ? C16 C17 1.552(9) . ? C17 C18 1.514(11) . ? C17 C20 1.539(11) . ? C17 C19 1.548(11) . ? C21 C26 1.383(10) . ? C21 C22 1.405(10) . ? C22 C23 1.360(10) . ? C23 C24 1.375(12) . ? C24 C25 1.379(13) . ? C25 C26 1.392(12) . ? C27 C28 1.385(10) . ? C27 C32 1.407(10) . ? C28 C29 1.387(10) . ? C29 C30 1.389(11) . ? C30 C31 1.372(11) . ? C31 C32 1.400(10) . ? C33 C34 1.386(11) . ? C33 C38 1.409(10) . ? C34 C35 1.409(12) . ? C35 C36 1.379(15) . ? C36 C37 1.362(16) . ? C37 C38 1.405(13) . ? C39 C44 1.383(9) . ? C39 C40 1.399(9) . ? C40 C41 1.391(10) . ? C41 C42 1.385(10) . ? C42 C43 1.367(11) . ? C43 C44 1.399(10) . ? C45 C46 1.382(9) . ? C45 C50 1.414(9) . ? C46 C47 1.394(9) . ? C47 C48 1.384(10) . ? C48 C49 1.374(11) . ? C49 C50 1.380(10) . ? C51 C56 1.377(9) . ? C51 C52 1.388(10) . ? C52 C53 1.393(10) . ? C53 C54 1.372(11) . ? C54 C55 1.374(11) . ? C55 C56 1.376(9) . ? C57 Cl2 1.679(9) . ? C57 Cl1 1.680(9) . ? C58 Cl3 1.502(14) . ? C58 Cl4 1.548(13) . ? 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 P7 Pt P8 103.81(6) . . ? P7 Pt P5 87.46(6) . . ? P8 Pt P5 163.81(6) . . ? P7 Pt P1 159.43(6) . . ? P8 Pt P1 88.86(5) . . ? P5 Pt P1 83.91(5) . . ? C1 P1 P2 99.3(2) . . ? C1 P1 Pt 100.45(19) . . ? P2 P1 Pt 101.96(8) . . ? C6 P2 C11 88.1(3) . . ? C6 P2 P1 104.4(2) . . ? C11 P2 P1 99.3(2) . . ? C11 P3 C1 102.5(3) . . ? C11 P3 C16 87.7(3) . . ? C1 P3 C16 87.5(3) . . ? C16 P4 C6 103.0(3) . . ? C16 P4 C11 88.1(3) . . ? C6 P4 C11 87.1(3) . . ? C6 P5 P6 99.9(2) . . ? C6 P5 Pt 108.89(19) . . ? P6 P5 Pt 94.12(8) . . ? C16 P6 C1 88.3(3) . . ? C16 P6 P5 99.4(2) . . ? C1 P6 P5 104.1(2) . . ? C33 P7 C21 105.4(3) . . ? C33 P7 C27 103.4(3) . . ? C21 P7 C27 103.1(3) . . ? C33 P7 Pt 118.7(3) . . ? C21 P7 Pt 116.1(2) . . ? C27 P7 Pt 108.4(2) . . ? C39 P8 C45 104.7(3) . . ? C39 P8 C51 104.0(3) . . ? C45 P8 C51 98.6(3) . . ? C39 P8 Pt 117.3(2) . . ? C45 P8 Pt 108.3(2) . . ? C51 P8 Pt 121.2(2) . . ? C2 C1 P3 113.0(4) . . ? C2 C1 P6 114.3(4) . . ? P3 C1 P6 92.0(3) . . ? C2 C1 P1 111.0(4) . . ? P3 C1 P1 112.6(3) . . ? P6 C1 P1 112.7(3) . . ? C5 C2 C3 110.5(6) . . ? C5 C2 C4 107.8(6) . . ? C3 C2 C4 107.5(6) . . ? C5 C2 C1 110.4(5) . . ? C3 C2 C1 109.5(5) . . ? C4 C2 C1 111.1(6) . . ? C7 C6 P2 115.0(4) . . ? C7 C6 P5 110.6(4) . . ? P2 C6 P5 112.8(3) . . ? C7 C6 P4 112.8(4) . . ? P2 C6 P4 92.3(3) . . ? P5 C6 P4 112.1(3) . . ? C8 C7 C10 109.1(6) . . ? C8 C7 C9 107.4(6) . . ? C10 C7 C9 110.2(6) . . ? C8 C7 C6 110.8(6) . . ? C10 C7 C6 109.2(5) . . ? C9 C7 C6 110.1(5) . . ? C12 C11 P3 114.0(5) . . ? C12 C11 P2 116.9(4) . . ? P3 C11 P2 116.1(3) . . ? C12 C11 P4 122.4(5) . . ? P3 C11 P4 91.8(3) . . ? P2 C11 P4 91.6(3) . . ? C13 C12 C14 108.3(7) . . ? C13 C12 C15 109.7(7) . . ? C14 C12 C15 110.1(7) . . ? C13 C12 C11 111.1(6) . . ? C14 C12 C11 110.7(6) . . ? C15 C12 C11 106.9(6) . . ? C17 C16 P4 114.6(5) . . ? C17 C16 P6 115.6(5) . . ? P4 C16 P6 115.5(4) . . ? C17 C16 P3 124.6(5) . . ? P4 C16 P3 91.6(3) . . ? P6 C16 P3 91.4(3) . . ? C18 C17 C20 109.9(7) . . ? C18 C17 C19 109.2(7) . . ? C20 C17 C19 108.5(7) . . ? C18 C17 C16 108.6(6) . . ? C20 C17 C16 110.8(6) . . ? C19 C17 C16 109.8(6) . . ? C26 C21 C22 118.6(7) . . ? C26 C21 P7 123.7(6) . . ? C22 C21 P7 117.7(5) . . ? C23 C22 C21 121.1(7) . . ? C22 C23 C24 120.9(8) . . ? C23 C24 C25 118.5(8) . . ? C24 C25 C26 121.8(8) . . ? C21 C26 C25 119.1(8) . . ? C28 C27 C32 118.5(6) . . ? C28 C27 P7 121.6(5) . . ? C32 C27 P7 119.5(5) . . ? C27 C28 C29 120.9(7) . . ? C28 C29 C30 120.7(7) . . ? C31 C30 C29 119.1(7) . . ? C30 C31 C32 121.0(7) . . ? C31 C32 C27 119.8(7) . . ? C34 C33 C38 119.4(7) . . ? C34 C33 P7 119.2(6) . . ? C38 C33 P7 121.4(6) . . ? C33 C34 C35 120.6(8) . . ? C36 C35 C34 119.0(10) . . ? C37 C36 C35 121.5(9) . . ? C36 C37 C38 120.4(9) . . ? C37 C38 C33 119.2(9) . . ? C44 C39 C40 117.4(6) . . ? C44 C39 P8 122.7(5) . . ? C40 C39 P8 119.9(5) . . ? C41 C40 C39 121.6(6) . . ? C42 C41 C40 119.5(7) . . ? C43 C42 C41 119.9(7) . . ? C42 C43 C44 120.4(6) . . ? C39 C44 C43 121.2(6) . . ? C46 C45 C50 119.0(6) . . ? C46 C45 P8 120.6(5) . . ? C50 C45 P8 120.3(5) . . ? C45 C46 C47 120.5(6) . . ? C48 C47 C46 120.1(7) . . ? C49 C48 C47 119.7(7) . . ? C48 C49 C50 121.2(7) . . ? C49 C50 C45 119.5(7) . . ? C56 C51 C52 118.6(6) . . ? C56 C51 P8 117.1(5) . . ? C52 C51 P8 124.3(5) . . ? C51 C52 C53 119.6(7) . . ? C54 C53 C52 121.1(7) . . ? C53 C54 C55 119.0(7) . . ? C54 C55 C56 120.4(7) . . ? C55 C56 C51 121.4(7) . . ? Cl2 C57 Cl1 117.4(7) . . ? Cl3 C58 Cl4 127.0(15) . . ? #===END # Attachment 'jun801.cif' data_jun801 _database_code_depnum_ccdc_archive 'CCDC 666875' _audit_creation_date 2001-06-19T09:25:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H72 Cl2 P12 Pt' _chemical_formula_sum 'C40 H72 Cl2 P12 Pt' _chemical_formula_weight 1190.61 _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 9.9079(5) _cell_length_b 12.0315(7) _cell_length_c 24.4729(15) _cell_angle_alpha 80.534(3) _cell_angle_beta 78.741(4) _cell_angle_gamma 66.069(4) _cell_volume 2603.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37063 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.829 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 15262 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_unetI/netI 0.0737 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 7162 _reflns_number_gt 6013 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0000P)^2^+3.6666P] 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 7162 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.71 _refine_diff_density_min -1 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 Pt Pt 0.34568(3) 0.43010(2) 0.233237(10) 0.02443(9) Uani 1 1 d . . . Cl1 Cl 0.46480(18) 0.38452(16) 0.14230(7) 0.0410(4) Uani 1 1 d . . . Cl2 Cl 0.05657(17) 0.56804(15) 0.34745(7) 0.0379(4) Uani 1 1 d . . . P1 P 0.27357(17) 0.45326(14) 0.32272(7) 0.0255(4) Uani 1 1 d . . . P2 P 0.26981(16) 0.28188(14) 0.36534(7) 0.0234(4) Uani 1 1 d . . . P3 P 0.43954(19) 0.39036(15) 0.42711(7) 0.0305(4) Uani 1 1 d . . . P4 P 0.54758(17) 0.26745(15) 0.27170(7) 0.0299(4) Uani 1 1 d . . . P5 P 0.59181(18) 0.37994(16) 0.32119(7) 0.0314(4) Uani 1 1 d . . . P6 P 0.54247(17) 0.15543(14) 0.39761(7) 0.0254(4) Uani 1 1 d . . . P7 P 0.15179(17) 0.58066(14) 0.19092(7) 0.0241(4) Uani 1 1 d . . . P8 P 0.22598(16) 0.68888(14) 0.11931(7) 0.0251(4) Uani 1 1 d . . . P9 P -0.02127(17) 0.60591(15) 0.09105(7) 0.0261(4) Uani 1 1 d . . . P10 P -0.00925(17) 0.76571(15) 0.21634(7) 0.0276(4) Uani 1 1 d . . . P11 P -0.16421(17) 0.69562(15) 0.19176(7) 0.0280(4) Uani 1 1 d . . . P12 P -0.04161(17) 0.84076(15) 0.08585(7) 0.0267(4) Uani 1 1 d . . . C1 C 0.4015(7) 0.4833(5) 0.3579(3) 0.0288(15) Uani 1 1 d . . . C2 C 0.3573(6) 0.2743(5) 0.4282(2) 0.0254(14) Uani 1 1 d . . . C3 C 0.4595(6) 0.1841(5) 0.3303(2) 0.0246(14) Uani 1 1 d . . . C4 C 0.6163(7) 0.2790(6) 0.3887(3) 0.0320(16) Uani 1 1 d . . . C5 C -0.0003(6) 0.5530(5) 0.1673(2) 0.0256(14) Uani 1 1 d . . . C6 C 0.1095(6) 0.6851(5) 0.0675(2) 0.0255(14) Uani 1 1 d . . . C7 C 0.0589(6) 0.8284(5) 0.1457(3) 0.0272(15) Uani 1 1 d . . . C8 C -0.1668(6) 0.7569(6) 0.1162(2) 0.0264(15) Uani 1 1 d . . . C9 C 0.3844(7) 0.6207(6) 0.3549(3) 0.0348(17) Uani 1 1 d . . . C10 C 0.5250(9) 0.6243(7) 0.3716(3) 0.058(2) Uani 1 1 d . . . H10A H 0.5368 0.5857 0.4098 0.088 Uiso 1 1 calc R . . H10B H 0.5143 0.7094 0.3698 0.088 Uiso 1 1 calc R . . H10C H 0.6129 0.5802 0.3458 0.088 Uiso 1 1 calc R . . C11 C 0.2505(9) 0.6902(6) 0.3969(3) 0.052(2) Uani 1 1 d . . . H11A H 0.2641 0.6494 0.4347 0.078 Uiso 1 1 calc R . . H11B H 0.1587 0.6913 0.387 0.078 Uiso 1 1 calc R . . H11C H 0.2433 0.7742 0.3957 0.078 Uiso 1 1 calc R . . C12 C 0.3668(8) 0.6820(6) 0.2954(3) 0.0421(18) Uani 1 1 d . . . H12A H 0.4534 0.6365 0.2694 0.063 Uiso 1 1 calc R . . H12B H 0.3598 0.766 0.2937 0.063 Uiso 1 1 calc R . . H12C H 0.2759 0.6827 0.2849 0.063 Uiso 1 1 calc R . . C13 C 0.2700(7) 0.2490(5) 0.4855(3) 0.0284(15) Uani 1 1 d . . . C14 C 0.2230(7) 0.1414(6) 0.4858(3) 0.0374(17) Uani 1 1 d . . . H14A H 0.3121 0.0672 0.4785 0.056 Uiso 1 1 calc R . . H14B H 0.1597 0.1599 0.4567 0.056 Uiso 1 1 calc R . . H14C H 0.1675 0.1288 0.5225 0.056 Uiso 1 1 calc R . . C15 C 0.3688(8) 0.2176(6) 0.5318(3) 0.0425(18) Uani 1 1 d . . . H15A H 0.4575 0.1432 0.5243 0.064 Uiso 1 1 calc R . . H15B H 0.3123 0.2046 0.5682 0.064 Uiso 1 1 calc R . . H15C H 0.3995 0.2853 0.5324 0.064 Uiso 1 1 calc R . . C16 C 0.1327(7) 0.3649(6) 0.4970(3) 0.0417(18) Uani 1 1 d . . . H16A H 0.0697 0.3847 0.4677 0.063 Uiso 1 1 calc R . . H16B H 0.1637 0.4324 0.4974 0.063 Uiso 1 1 calc R . . H16C H 0.0762 0.3522 0.5335 0.063 Uiso 1 1 calc R . . C17 C 0.4619(7) 0.0653(6) 0.3103(3) 0.0313(16) Uani 1 1 d . . . C18 C 0.3803(8) 0.0997(6) 0.2588(3) 0.0396(18) Uani 1 1 d . . . H18A H 0.4282 0.1422 0.229 0.059 Uiso 1 1 calc R . . H18B H 0.2758 0.1533 0.269 0.059 Uiso 1 1 calc R . . H18C H 0.3848 0.0253 0.2457 0.059 Uiso 1 1 calc R . . C19 C 0.6243(7) -0.0225(6) 0.2942(3) 0.048(2) Uani 1 1 d . . . H19A H 0.6753 0.0193 0.2652 0.073 Uiso 1 1 calc R . . H19B H 0.6252 -0.0943 0.2799 0.073 Uiso 1 1 calc R . . H19C H 0.6759 -0.0484 0.3272 0.073 Uiso 1 1 calc R . . C20 C 0.3837(7) -0.0004(6) 0.3554(3) 0.0383(17) Uani 1 1 d . . . H20A H 0.4331 -0.0233 0.3889 0.058 Uiso 1 1 calc R . . H20B H 0.3886 -0.0741 0.3416 0.058 Uiso 1 1 calc R . . H20C H 0.2791 0.0539 0.3648 0.058 Uiso 1 1 calc R . . C21 C 0.7716(7) 0.2361(6) 0.4091(3) 0.0375(17) Uani 1 1 d . . . C22 C 0.8874(7) 0.1447(7) 0.3694(3) 0.049(2) Uani 1 1 d . . . H22A H 0.8905 0.1846 0.3312 0.073 Uiso 1 1 calc R . . H22B H 0.8596 0.0748 0.3705 0.073 Uiso 1 1 calc R . . H22C H 0.9859 0.1162 0.3813 0.073 Uiso 1 1 calc R . . C23 C 0.7671(8) 0.1745(7) 0.4686(3) 0.047(2) Uani 1 1 d . . . H23A H 0.693 0.2329 0.4938 0.07 Uiso 1 1 calc R . . H23B H 0.8656 0.1467 0.4804 0.07 Uiso 1 1 calc R . . H23C H 0.7398 0.1043 0.4699 0.07 Uiso 1 1 calc R . . C24 C 0.8169(8) 0.3447(7) 0.4081(3) 0.050(2) Uani 1 1 d . . . H24A H 0.8208 0.3852 0.37 0.076 Uiso 1 1 calc R . . H24B H 0.9153 0.3151 0.4201 0.076 Uiso 1 1 calc R . . H24C H 0.7433 0.4029 0.4335 0.076 Uiso 1 1 calc R . . C25 C -0.0153(6) 0.4269(5) 0.1869(3) 0.0287(15) Uani 1 1 d . . . C26 C -0.1649(7) 0.4342(6) 0.1740(3) 0.0369(17) Uani 1 1 d . . . H26A H -0.2472 0.498 0.1943 0.055 Uiso 1 1 calc R . . H26B H -0.1741 0.3554 0.1859 0.055 Uiso 1 1 calc R . . H26C H -0.1687 0.4538 0.1337 0.055 Uiso 1 1 calc R . . C27 C 0.1133(7) 0.3274(6) 0.1555(3) 0.0405(18) Uani 1 1 d . . . H27A H 0.1111 0.3474 0.1151 0.061 Uiso 1 1 calc R . . H27B H 0.1032 0.2488 0.1669 0.061 Uiso 1 1 calc R . . H27C H 0.2082 0.322 0.1643 0.061 Uiso 1 1 calc R . . C28 C -0.0157(7) 0.3985(6) 0.2501(3) 0.0383(17) Uani 1 1 d . . . H28A H -0.0996 0.4632 0.2693 0.057 Uiso 1 1 calc R . . H28B H 0.0781 0.3941 0.2596 0.057 Uiso 1 1 calc R . . H28C H -0.0258 0.3201 0.2619 0.057 Uiso 1 1 calc R . . C29 C 0.1927(7) 0.6669(6) 0.0074(3) 0.0314(16) Uani 1 1 d . . . C30 C 0.2816(7) 0.7496(6) -0.0114(3) 0.0410(18) Uani 1 1 d . . . H30A H 0.3329 0.7354 -0.0496 0.062 Uiso 1 1 calc R . . H30B H 0.3552 0.7306 0.0139 0.062 Uiso 1 1 calc R . . H30C H 0.2131 0.8354 -0.0103 0.062 Uiso 1 1 calc R . . C31 C 0.0808(7) 0.6990(6) -0.0340(3) 0.0404(18) Uani 1 1 d . . . H31A H 0.1348 0.687 -0.072 0.061 Uiso 1 1 calc R . . H31B H 0.0116 0.7845 -0.0322 0.061 Uiso 1 1 calc R . . H31C H 0.0246 0.6459 -0.024 0.061 Uiso 1 1 calc R . . C32 C 0.2983(7) 0.5320(6) 0.0047(3) 0.0421(18) Uani 1 1 d . . . H32A H 0.3518 0.5193 -0.0334 0.063 Uiso 1 1 calc R . . H32B H 0.2402 0.4804 0.0148 0.063 Uiso 1 1 calc R . . H32C H 0.3702 0.5101 0.0309 0.063 Uiso 1 1 calc R . . C33 C 0.0834(7) 0.9475(6) 0.1492(3) 0.0315(16) Uani 1 1 d . . . C34 C 0.1632(7) 0.9830(6) 0.0929(3) 0.0382(17) Uani 1 1 d . . . H34A H 0.2595 0.9161 0.0838 0.057 Uiso 1 1 calc R . . H34B H 0.1795 1.0569 0.0956 0.057 Uiso 1 1 calc R . . H34C H 0.1015 0.9986 0.0635 0.057 Uiso 1 1 calc R . . C35 C 0.1826(7) 0.9272(6) 0.1945(3) 0.0383(17) Uani 1 1 d . . . H35A H 0.2795 0.861 0.1853 0.057 Uiso 1 1 calc R . . H35B H 0.1338 0.9053 0.231 0.057 Uiso 1 1 calc R . . H35C H 0.1974 1.0024 0.1958 0.057 Uiso 1 1 calc R . . C36 C -0.0655(7) 1.0505(6) 0.1636(3) 0.0376(17) Uani 1 1 d . . . H36A H -0.1164 1.0274 0.1994 0.056 Uiso 1 1 calc R . . H36B H -0.1272 1.0666 0.1341 0.056 Uiso 1 1 calc R . . H36C H -0.0492 1.1243 0.1665 0.056 Uiso 1 1 calc R . . C37 C -0.3243(7) 0.8171(6) 0.0974(3) 0.0334(16) Uani 1 1 d . . . C38 C -0.3136(7) 0.8442(7) 0.0340(3) 0.048(2) Uani 1 1 d . . . H38A H -0.2587 0.7678 0.0164 0.072 Uiso 1 1 calc R . . H38B H -0.261 0.8995 0.0214 0.072 Uiso 1 1 calc R . . H38C H -0.4141 0.8827 0.0235 0.072 Uiso 1 1 calc R . . C39 C -0.4103(7) 0.9364(6) 0.1250(3) 0.048(2) Uani 1 1 d . . . H39A H -0.4177 0.9188 0.1658 0.072 Uiso 1 1 calc R . . H39B H -0.5107 0.975 0.1143 0.072 Uiso 1 1 calc R . . H39C H -0.3577 0.9917 0.1126 0.072 Uiso 1 1 calc R . . C40 C -0.4058(7) 0.7293(6) 0.1151(3) 0.046(2) Uani 1 1 d . . . H40A H -0.4147 0.7103 0.1558 0.069 Uiso 1 1 calc R . . H40B H -0.3491 0.6537 0.0969 0.069 Uiso 1 1 calc R . . H40C H -0.5055 0.7678 0.1038 0.069 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 Pt 0.02726(14) 0.02474(15) 0.02271(15) -0.00173(10) -0.00705(10) -0.01010(10) Cl1 0.0433(10) 0.0477(11) 0.0242(9) -0.0050(8) -0.0015(7) -0.0108(8) Cl2 0.0350(9) 0.0335(9) 0.0364(10) -0.0060(8) -0.0050(7) -0.0034(7) P1 0.0307(9) 0.0236(9) 0.0250(10) -0.0002(7) -0.0102(7) -0.0113(7) P2 0.0240(8) 0.0225(9) 0.0250(9) -0.0017(7) -0.0063(7) -0.0092(7) P3 0.0418(10) 0.0276(9) 0.0281(10) -0.0005(8) -0.0148(8) -0.0160(8) P4 0.0294(9) 0.0321(10) 0.0278(10) 0.0006(8) -0.0066(7) -0.0114(8) P5 0.0317(9) 0.0343(10) 0.0330(11) 0.0061(8) -0.0112(7) -0.0182(8) P6 0.0263(9) 0.0242(9) 0.0278(10) 0.0002(7) -0.0082(7) -0.0110(7) P7 0.0270(9) 0.0236(9) 0.0249(9) -0.0008(7) -0.0078(7) -0.0117(7) P8 0.0241(8) 0.0254(9) 0.0278(10) 0.0003(7) -0.0073(7) -0.0109(7) P9 0.0272(9) 0.0279(9) 0.0264(10) -0.0017(7) -0.0073(7) -0.0128(7) P10 0.0316(9) 0.0276(9) 0.0269(10) -0.0026(8) -0.0051(7) -0.0144(8) P11 0.0267(9) 0.0302(10) 0.0303(10) -0.0034(8) -0.0045(7) -0.0139(8) P12 0.0271(9) 0.0265(9) 0.0286(10) -0.0007(7) -0.0092(7) -0.0110(7) C1 0.038(4) 0.021(3) 0.036(4) 0.000(3) -0.019(3) -0.015(3) C2 0.033(4) 0.020(3) 0.026(4) 0.005(3) -0.012(3) -0.013(3) C3 0.030(3) 0.021(3) 0.023(4) -0.003(3) -0.004(3) -0.010(3) C4 0.036(4) 0.025(4) 0.037(4) 0.005(3) -0.013(3) -0.014(3) C5 0.029(3) 0.028(4) 0.025(4) 0.001(3) -0.009(3) -0.015(3) C6 0.029(3) 0.027(3) 0.024(4) 0.002(3) -0.006(3) -0.014(3) C7 0.033(4) 0.025(3) 0.031(4) 0.000(3) -0.008(3) -0.018(3) C8 0.027(3) 0.035(4) 0.024(4) -0.002(3) -0.004(3) -0.019(3) C9 0.050(4) 0.026(4) 0.035(4) -0.001(3) -0.021(3) -0.015(3) C10 0.092(6) 0.035(4) 0.071(6) 0.005(4) -0.049(5) -0.035(4) C11 0.087(6) 0.034(4) 0.044(5) -0.010(4) -0.017(4) -0.027(4) C12 0.070(5) 0.025(4) 0.047(5) 0.010(3) -0.027(4) -0.031(4) C13 0.035(4) 0.029(4) 0.024(4) 0.001(3) -0.003(3) -0.016(3) C14 0.040(4) 0.037(4) 0.037(4) 0.000(3) -0.005(3) -0.019(3) C15 0.057(5) 0.047(4) 0.024(4) 0.008(3) -0.012(3) -0.022(4) C16 0.045(4) 0.040(4) 0.034(4) -0.003(3) -0.001(3) -0.013(3) C17 0.036(4) 0.027(4) 0.030(4) -0.004(3) -0.008(3) -0.010(3) C18 0.056(4) 0.023(4) 0.044(5) -0.006(3) -0.018(3) -0.013(3) C19 0.041(4) 0.032(4) 0.060(5) -0.013(4) -0.002(4) -0.002(3) C20 0.051(4) 0.030(4) 0.041(4) -0.007(3) -0.014(3) -0.019(3) C21 0.036(4) 0.040(4) 0.046(5) 0.010(3) -0.023(3) -0.023(3) C22 0.031(4) 0.057(5) 0.058(5) 0.014(4) -0.014(3) -0.019(4) C23 0.049(4) 0.052(5) 0.052(5) 0.015(4) -0.032(4) -0.029(4) C24 0.048(5) 0.052(5) 0.067(6) 0.015(4) -0.032(4) -0.033(4) C25 0.031(4) 0.026(4) 0.030(4) 0.005(3) -0.008(3) -0.013(3) C26 0.041(4) 0.041(4) 0.042(4) -0.006(3) -0.012(3) -0.026(3) C27 0.042(4) 0.025(4) 0.060(5) -0.004(3) -0.017(4) -0.014(3) C28 0.053(4) 0.041(4) 0.034(4) 0.007(3) -0.007(3) -0.035(4) C29 0.034(4) 0.037(4) 0.020(4) -0.002(3) -0.002(3) -0.011(3) C30 0.046(4) 0.041(4) 0.032(4) -0.005(3) 0.011(3) -0.020(3) C31 0.049(4) 0.042(4) 0.025(4) -0.010(3) -0.007(3) -0.009(3) C32 0.048(4) 0.047(4) 0.030(4) -0.002(3) -0.006(3) -0.017(4) C33 0.032(4) 0.029(4) 0.041(4) -0.002(3) -0.013(3) -0.017(3) C34 0.045(4) 0.035(4) 0.041(4) 0.008(3) -0.019(3) -0.021(3) C35 0.049(4) 0.035(4) 0.040(4) 0.006(3) -0.020(3) -0.024(3) C36 0.047(4) 0.024(4) 0.047(5) -0.003(3) -0.005(3) -0.020(3) C37 0.024(3) 0.031(4) 0.044(4) -0.003(3) -0.010(3) -0.008(3) C38 0.032(4) 0.061(5) 0.050(5) 0.007(4) -0.025(3) -0.012(4) C39 0.035(4) 0.044(5) 0.065(6) -0.010(4) -0.015(4) -0.010(3) C40 0.030(4) 0.040(4) 0.070(6) 0.004(4) -0.026(4) -0.010(3) #----------------------------------------------------------------------------# # 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 Pt P1 2.1935(16) . ? Pt P7 2.3196(15) . ? Pt Cl1 2.3447(16) . ? Pt P4 2.3813(16) . ? Cl2 P1 2.063(2) . ? P1 C1 1.839(6) . ? P1 P2 2.164(2) . ? P2 C2 1.880(6) . ? P2 C3 1.887(6) . ? P3 C2 1.876(6) . ? P3 C1 1.882(6) . ? P3 C4 1.900(6) . ? P4 C3 1.890(6) . ? P4 P5 2.172(2) . ? P5 C4 1.877(6) . ? P5 C1 1.927(6) . ? P6 C4 1.872(6) . ? P6 C3 1.903(6) . ? P6 C2 1.913(6) . ? P7 C5 1.879(6) . ? P7 P8 2.198(2) . ? P7 P10 2.253(2) . ? P8 C6 1.892(6) . ? P8 C7 1.913(6) . ? P9 C6 1.857(6) . ? P9 C5 1.892(6) . ? P9 C8 1.911(6) . ? P10 C7 1.883(6) . ? P10 P11 2.238(2) . ? P11 C8 1.876(6) . ? P11 C5 1.907(6) . ? P12 C8 1.875(6) . ? P12 C7 1.880(6) . ? P12 C6 1.921(6) . ? C1 C9 1.583(9) . ? C2 C13 1.553(8) . ? C3 C17 1.574(8) . ? C4 C21 1.567(8) . ? C5 C25 1.571(8) . ? C6 C29 1.541(8) . ? C7 C33 1.565(8) . ? C8 C37 1.557(8) . ? C9 C12 1.528(9) . ? C9 C11 1.539(9) . ? C9 C10 1.545(9) . ? C13 C16 1.522(8) . ? C13 C15 1.542(8) . ? C13 C14 1.541(9) . ? C17 C20 1.523(9) . ? C17 C18 1.539(8) . ? C17 C19 1.540(8) . ? C21 C23 1.523(9) . ? C21 C22 1.537(10) . ? C21 C24 1.538(9) . ? C25 C27 1.526(8) . ? C25 C28 1.528(8) . ? C25 C26 1.540(8) . ? C29 C31 1.538(8) . ? C29 C32 1.538(9) . ? C29 C30 1.543(9) . ? C33 C36 1.515(8) . ? C33 C34 1.537(9) . ? C33 C35 1.548(8) . ? C37 C38 1.523(9) . ? C37 C39 1.531(9) . ? C37 C40 1.537(9) . ? 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 Pt P7 103.69(6) . . ? P1 Pt Cl1 169.79(6) . . ? P7 Pt Cl1 86.15(6) . . ? P1 Pt P4 79.61(6) . . ? P7 Pt P4 176.16(6) . . ? Cl1 Pt P4 90.65(6) . . ? C1 P1 Cl2 109.9(2) . . ? C1 P1 P2 103.6(2) . . ? Cl2 P1 P2 99.92(9) . . ? C1 P1 Pt 115.1(2) . . ? Cl2 P1 Pt 118.01(8) . . ? P2 P1 Pt 108.09(8) . . ? C2 P2 C3 88.9(3) . . ? C2 P2 P1 99.40(19) . . ? C3 P2 P1 95.4(2) . . ? C2 P3 C1 103.0(3) . . ? C2 P3 C4 86.2(3) . . ? C1 P3 C4 88.1(3) . . ? C3 P4 P5 98.74(19) . . ? C3 P4 Pt 105.84(18) . . ? P5 P4 Pt 95.45(7) . . ? C4 P5 C1 87.4(3) . . ? C4 P5 P4 100.0(2) . . ? C1 P5 P4 106.81(19) . . ? C4 P6 C3 102.0(3) . . ? C4 P6 C2 85.9(3) . . ? C3 P6 C2 87.5(2) . . ? C5 P7 P8 104.3(2) . . ? C5 P7 P10 91.23(19) . . ? P8 P7 P10 83.22(8) . . ? C5 P7 Pt 124.2(2) . . ? P8 P7 Pt 113.73(8) . . ? P10 P7 Pt 131.20(8) . . ? C6 P8 C7 87.3(3) . . ? C6 P8 P7 99.0(2) . . ? C7 P8 P7 87.0(2) . . ? C6 P9 C5 104.3(3) . . ? C6 P9 C8 87.6(3) . . ? C5 P9 C8 86.7(3) . . ? C7 P10 P11 99.97(19) . . ? C7 P10 P7 86.12(19) . . ? P11 P10 P7 79.16(8) . . ? C8 P11 C5 87.2(3) . . ? C8 P11 P10 101.3(2) . . ? C5 P11 P10 90.94(18) . . ? C8 P12 C7 103.2(3) . . ? C8 P12 C6 86.8(3) . . ? C7 P12 C6 87.4(3) . . ? C9 C1 P1 117.1(4) . . ? C9 C1 P3 115.8(4) . . ? P1 C1 P3 114.6(3) . . ? C9 C1 P5 112.8(4) . . ? P1 C1 P5 100.9(3) . . ? P3 C1 P5 91.4(3) . . ? C13 C2 P3 114.5(4) . . ? C13 C2 P2 115.2(4) . . ? P3 C2 P2 116.9(3) . . ? C13 C2 P6 122.4(4) . . ? P3 C2 P6 93.4(3) . . ? P2 C2 P6 91.2(3) . . ? C17 C3 P2 112.9(4) . . ? C17 C3 P4 110.5(4) . . ? P2 C3 P4 114.9(3) . . ? C17 C3 P6 113.6(4) . . ? P2 C3 P6 91.3(3) . . ? P4 C3 P6 112.5(3) . . ? C21 C4 P6 113.6(4) . . ? C21 C4 P5 116.1(4) . . ? P6 C4 P5 115.8(3) . . ? C21 C4 P3 121.9(5) . . ? P6 C4 P3 93.9(3) . . ? P5 C4 P3 92.4(3) . . ? C25 C5 P7 118.1(4) . . ? C25 C5 P9 113.6(4) . . ? P7 C5 P9 113.8(3) . . ? C25 C5 P11 117.0(4) . . ? P7 C5 P11 98.2(3) . . ? P9 C5 P11 92.4(3) . . ? C29 C6 P9 115.6(4) . . ? C29 C6 P8 114.2(4) . . ? P9 C6 P8 118.2(3) . . ? C29 C6 P12 120.7(4) . . ? P9 C6 P12 92.7(3) . . ? P8 C6 P12 91.5(3) . . ? C33 C7 P12 113.0(4) . . ? C33 C7 P10 111.8(4) . . ? P12 C7 P10 117.4(3) . . ? C33 C7 P8 118.8(4) . . ? P12 C7 P8 92.2(3) . . ? P10 C7 P8 102.3(3) . . ? C37 C8 P12 114.0(4) . . ? C37 C8 P11 115.1(4) . . ? P12 C8 P11 117.1(3) . . ? C37 C8 P9 122.3(4) . . ? P12 C8 P9 92.4(3) . . ? P11 C8 P9 92.8(3) . . ? C12 C9 C11 110.9(6) . . ? C12 C9 C10 108.9(6) . . ? C11 C9 C10 107.2(6) . . ? C12 C9 C1 110.2(5) . . ? C11 C9 C1 110.1(6) . . ? C10 C9 C1 109.4(5) . . ? C16 C13 C15 109.5(5) . . ? C16 C13 C14 110.1(5) . . ? C15 C13 C14 108.3(5) . . ? C16 C13 C2 107.6(5) . . ? C15 C13 C2 109.6(5) . . ? C14 C13 C2 111.8(5) . . ? C20 C17 C18 107.5(5) . . ? C20 C17 C19 109.1(5) . . ? C18 C17 C19 108.8(5) . . ? C20 C17 C3 112.0(5) . . ? C18 C17 C3 109.6(5) . . ? C19 C17 C3 109.8(5) . . ? C23 C21 C22 109.6(6) . . ? C23 C21 C24 108.4(6) . . ? C22 C21 C24 109.4(6) . . ? C23 C21 C4 110.5(5) . . ? C22 C21 C4 107.7(5) . . ? C24 C21 C4 111.2(5) . . ? C27 C25 C28 111.0(5) . . ? C27 C25 C26 109.7(5) . . ? C28 C25 C26 107.6(5) . . ? C27 C25 C5 109.1(5) . . ? C28 C25 C5 110.1(5) . . ? C26 C25 C5 109.3(5) . . ? C31 C29 C32 108.6(5) . . ? C31 C29 C6 110.1(5) . . ? C32 C29 C6 108.8(5) . . ? C31 C29 C30 107.3(5) . . ? C32 C29 C30 110.1(5) . . ? C6 C29 C30 111.9(5) . . ? C36 C33 C34 109.7(5) . . ? C36 C33 C35 109.0(5) . . ? C34 C33 C35 107.6(5) . . ? C36 C33 C7 109.9(5) . . ? C34 C33 C7 109.8(5) . . ? C35 C33 C7 110.8(5) . . ? C38 C37 C39 109.5(6) . . ? C38 C37 C40 107.6(6) . . ? C39 C37 C40 110.8(6) . . ? C38 C37 C8 111.3(5) . . ? C39 C37 C8 108.2(5) . . ? C40 C37 C8 109.5(5) . . ? #===END # Attachment 'may3300.cif' data_may3300 _database_code_depnum_ccdc_archive 'CCDC 666876' _audit_creation_date 2000-05-23T10:28:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H72 Cl4 P12 Pt2, 2(C H2 Cl2)' _chemical_formula_sum 'C42 H76 Cl8 P12 Pt2' _chemical_formula_weight 1626.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 10.0916(2) _cell_length_b 19.9361(5) _cell_length_c 15.0292(4) _cell_angle_alpha 90 _cell_angle_beta 101.825(2) _cell_angle_gamma 90 _cell_volume 2959.51(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10666 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.419 _exptl_absorpt_correction_T_max 0.531 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 16538 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0504 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6985 _reflns_number_gt 6059 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0267P)^2^+10.1649P] 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 6985 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.812 _refine_diff_density_min -1.928 _refine_diff_density_rms 0.149 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 Pt Pt 0.590934(16) 0.073794(8) 0.980375(11) 0.01928(6) Uani 1 1 d . . . Cl1 Cl 0.66530(13) 0.17817(6) 1.04607(9) 0.0353(3) Uani 1 1 d . . . Cl2 Cl 0.80560(12) 0.15667(6) 0.83716(9) 0.0342(3) Uani 1 1 d . . . P1 P 0.68071(11) 0.07974(6) 0.85600(8) 0.0201(2) Uani 1 1 d . . . P2 P 0.81914(11) -0.00393(6) 0.86849(8) 0.0220(2) Uani 1 1 d . . . P3 P 0.62306(11) -0.00040(6) 0.67215(8) 0.0215(2) Uani 1 1 d . . . P4 P 0.68241(11) -0.11084(6) 0.78414(8) 0.0211(2) Uani 1 1 d . . . P5 P 0.54311(11) -0.03089(6) 0.92204(8) 0.0187(2) Uani 1 1 d . . . P6 P 0.44159(11) -0.00701(6) 0.78317(8) 0.0193(2) Uani 1 1 d . . . C1 C 0.5575(4) 0.0615(2) 0.7502(3) 0.0204(9) Uani 1 1 d . . . C2 C 0.4768(5) 0.1229(2) 0.7004(3) 0.0258(10) Uani 1 1 d . . . C3 C 0.4264(5) 0.1670(2) 0.7700(4) 0.0318(11) Uani 1 1 d . . . H3A H 0.5037 0.1822 0.8162 0.048 Uiso 1 1 calc R . . H3B H 0.3645 0.1411 0.7991 0.048 Uiso 1 1 calc R . . H3C H 0.3787 0.2061 0.7392 0.048 Uiso 1 1 calc R . . C4 C 0.3563(5) 0.0994(3) 0.6293(4) 0.0330(11) Uani 1 1 d . . . H4A H 0.3879 0.0706 0.585 0.05 Uiso 1 1 calc R . . H4B H 0.3088 0.1383 0.5981 0.05 Uiso 1 1 calc R . . H4C H 0.2944 0.0739 0.659 0.05 Uiso 1 1 calc R . . C5 C 0.5665(5) 0.1649(3) 0.6507(4) 0.0320(11) Uani 1 1 d . . . H5A H 0.6461 0.1808 0.6944 0.048 Uiso 1 1 calc R . . H5B H 0.5149 0.2036 0.6217 0.048 Uiso 1 1 calc R . . H5C H 0.5956 0.1374 0.6043 0.048 Uiso 1 1 calc R . . C6 C 0.7027(4) -0.0706(2) 0.9013(3) 0.0195(9) Uani 1 1 d . . . C7 C 0.7797(5) -0.1166(2) 0.9805(3) 0.0243(9) Uani 1 1 d . . . C8 C 0.9176(5) -0.1382(3) 0.9617(4) 0.0337(12) Uani 1 1 d . . . H8A H 0.9037 -0.1632 0.9043 0.051 Uiso 1 1 calc R . . H8B H 0.9642 -0.1668 1.0113 0.051 Uiso 1 1 calc R . . H8C H 0.9727 -0.0983 0.9572 0.051 Uiso 1 1 calc R . . C9 C 0.6978(5) -0.1805(2) 0.9882(4) 0.0343(12) Uani 1 1 d . . . H9A H 0.6091 -0.1682 1.0003 0.051 Uiso 1 1 calc R . . H9B H 0.7465 -0.2083 1.0382 0.051 Uiso 1 1 calc R . . H9C H 0.6856 -0.2057 0.9312 0.051 Uiso 1 1 calc R . . C10 C 0.8054(5) -0.0774(2) 1.0703(3) 0.0287(11) Uani 1 1 d . . . H10A H 0.7188 -0.0631 1.0839 0.043 Uiso 1 1 calc R . . H10B H 0.8609 -0.0378 1.0649 0.043 Uiso 1 1 calc R . . H10C H 0.853 -0.1062 1.1195 0.043 Uiso 1 1 calc R . . C11 C 0.7788(4) -0.0358(2) 0.7491(3) 0.0230(9) Uani 1 1 d . . . C12 C 0.9020(5) -0.0429(3) 0.7014(4) 0.0312(11) Uani 1 1 d . . . C13 C 1.0208(5) -0.0788(3) 0.7626(4) 0.0391(13) Uani 1 1 d . . . H13A H 0.9929 -0.1241 0.7763 0.059 Uiso 1 1 calc R . . H13B H 1.0488 -0.0535 0.8193 0.059 Uiso 1 1 calc R . . H13C H 1.0968 -0.0817 0.7313 0.059 Uiso 1 1 calc R . . C14 C 0.8611(6) -0.0826(3) 0.6129(4) 0.0441(14) Uani 1 1 d . . . H14A H 0.785 -0.0601 0.5731 0.066 Uiso 1 1 calc R . . H14B H 0.8341 -0.1281 0.6265 0.066 Uiso 1 1 calc R . . H14C H 0.9381 -0.085 0.5825 0.066 Uiso 1 1 calc R . . C15 C 0.9456(6) 0.0281(3) 0.6799(4) 0.0413(13) Uani 1 1 d . . . H15A H 0.8693 0.0512 0.6412 0.062 Uiso 1 1 calc R . . H15B H 1.0211 0.0252 0.6482 0.062 Uiso 1 1 calc R . . H15C H 0.9743 0.0532 0.7367 0.062 Uiso 1 1 calc R . . C16 C 0.5251(4) -0.0690(2) 0.7188(3) 0.0200(9) Uani 1 1 d . . . C17 C 0.4285(5) -0.1173(2) 0.6555(3) 0.0243(10) Uani 1 1 d . . . C18 C 0.3635(5) -0.1640(2) 0.7161(4) 0.0290(10) Uani 1 1 d . . . H18A H 0.4348 -0.1882 0.7581 0.043 Uiso 1 1 calc R . . H18B H 0.3041 -0.1962 0.678 0.043 Uiso 1 1 calc R . . H18C H 0.3104 -0.1373 0.751 0.043 Uiso 1 1 calc R . . C19 C 0.5082(6) -0.1594(3) 0.5989(4) 0.0355(12) Uani 1 1 d . . . H19A H 0.5792 -0.1846 0.6397 0.053 Uiso 1 1 calc R . . H19B H 0.5496 -0.1298 0.5603 0.053 Uiso 1 1 calc R . . H19C H 0.4467 -0.1908 0.5607 0.053 Uiso 1 1 calc R . . C20 C 0.3182(5) -0.0792(3) 0.5890(4) 0.0348(12) Uani 1 1 d . . . H20A H 0.2652 -0.052 0.6233 0.052 Uiso 1 1 calc R . . H20B H 0.2585 -0.1114 0.551 0.052 Uiso 1 1 calc R . . H20C H 0.3606 -0.0501 0.5504 0.052 Uiso 1 1 calc R . . C21 C 0.9359(6) 0.2831(4) 1.1393(5) 0.0610(19) Uani 1 1 d . . . H21A H 0.8639 0.3125 1.1536 0.073 Uiso 1 1 calc R . . H21B H 0.8956 0.2385 1.1223 0.073 Uiso 1 1 calc R . . Cl3 Cl 0.9949(2) 0.31681(10) 1.04681(19) 0.0850(7) Uani 1 1 d . . . Cl4 Cl 1.06410(19) 0.27517(11) 1.23524(16) 0.0780(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.02166(9) 0.01604(10) 0.01973(10) -0.00096(6) 0.00329(7) -0.00041(6) Cl1 0.0409(7) 0.0258(6) 0.0393(7) -0.0113(5) 0.0081(6) -0.0106(5) Cl2 0.0332(6) 0.0282(6) 0.0400(7) 0.0028(5) 0.0046(5) -0.0091(5) P1 0.0201(5) 0.0164(5) 0.0234(6) 0.0000(4) 0.0035(4) -0.0018(4) P2 0.0191(5) 0.0200(6) 0.0266(6) -0.0017(5) 0.0037(4) 0.0001(4) P3 0.0236(5) 0.0199(6) 0.0215(6) 0.0010(5) 0.0054(4) -0.0004(4) P4 0.0229(5) 0.0174(5) 0.0226(6) -0.0030(5) 0.0039(5) 0.0017(4) P5 0.0225(5) 0.0151(5) 0.0189(6) 0.0003(4) 0.0049(4) 0.0002(4) P6 0.0186(5) 0.0163(5) 0.0228(6) 0.0004(4) 0.0038(4) 0.0001(4) C1 0.021(2) 0.021(2) 0.019(2) 0.0000(17) 0.0017(17) 0.0014(17) C2 0.028(2) 0.018(2) 0.031(3) 0.0067(19) 0.003(2) 0.0005(18) C3 0.037(3) 0.025(2) 0.035(3) 0.004(2) 0.010(2) 0.006(2) C4 0.031(2) 0.027(3) 0.037(3) 0.006(2) -0.004(2) -0.001(2) C5 0.040(3) 0.027(3) 0.029(3) 0.006(2) 0.007(2) -0.001(2) C6 0.020(2) 0.016(2) 0.022(2) -0.0014(17) 0.0032(17) 0.0010(16) C7 0.026(2) 0.020(2) 0.025(2) 0.0006(19) 0.0016(18) 0.0033(18) C8 0.029(2) 0.032(3) 0.038(3) 0.002(2) 0.003(2) 0.013(2) C9 0.037(3) 0.022(2) 0.041(3) 0.005(2) 0.001(2) 0.003(2) C10 0.029(2) 0.031(3) 0.025(3) 0.002(2) 0.002(2) 0.006(2) C11 0.020(2) 0.020(2) 0.029(2) 0.0011(19) 0.0045(18) 0.0006(17) C12 0.027(2) 0.035(3) 0.034(3) -0.002(2) 0.013(2) 0.001(2) C13 0.026(2) 0.044(3) 0.052(4) 0.003(3) 0.017(2) 0.010(2) C14 0.040(3) 0.054(4) 0.043(3) -0.015(3) 0.018(3) 0.002(3) C15 0.036(3) 0.042(3) 0.051(4) 0.002(3) 0.020(3) -0.008(2) C16 0.023(2) 0.017(2) 0.020(2) -0.0023(17) 0.0033(17) -0.0004(17) C17 0.029(2) 0.017(2) 0.025(2) -0.0024(18) 0.0003(19) -0.0045(18) C18 0.033(2) 0.020(2) 0.032(3) 0.001(2) 0.002(2) -0.0057(19) C19 0.046(3) 0.033(3) 0.028(3) -0.010(2) 0.011(2) -0.007(2) C20 0.034(3) 0.035(3) 0.030(3) 0.001(2) -0.006(2) -0.005(2) C21 0.037(3) 0.052(4) 0.092(6) -0.015(4) 0.011(3) 0.001(3) Cl3 0.0893(15) 0.0524(11) 0.122(2) 0.0158(12) 0.0426(14) 0.0148(10) Cl4 0.0548(10) 0.0717(13) 0.1007(16) -0.0319(12) 0.0000(10) 0.0064(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 Pt P1 2.2413(12) . ? Pt P5 2.2769(11) . ? Pt P5 2.3507(11) 3_657 ? Pt Cl1 2.3588(12) . ? Cl2 P1 2.0414(16) . ? P1 C1 1.843(5) . ? P1 P2 2.1591(16) . ? P2 C11 1.867(5) . ? P2 C6 1.904(4) . ? P3 C11 1.887(5) . ? P3 C16 1.904(4) . ? P3 C1 1.911(5) . ? P4 C16 1.882(5) . ? P4 C6 1.908(5) . ? P4 C11 1.916(5) . ? P5 C6 1.877(4) . ? P5 P6 2.1808(16) . ? P5 Pt 2.3507(11) 3_657 ? P6 C16 1.873(4) . ? P6 C1 1.927(5) . ? C1 C2 1.574(6) . ? C2 C4 1.519(7) . ? C2 C3 1.531(7) . ? C2 C5 1.534(7) . ? C6 C7 1.576(6) . ? C7 C9 1.535(7) . ? C7 C10 1.535(7) . ? C7 C8 1.538(7) . ? C11 C12 1.564(6) . ? C12 C13 1.530(7) . ? C12 C14 1.530(8) . ? C12 C15 1.537(8) . ? C16 C17 1.550(6) . ? C17 C20 1.535(7) . ? C17 C19 1.534(7) . ? C17 C18 1.540(7) . ? C21 Cl4 1.737(7) . ? C21 Cl3 1.754(8) . ? 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 Pt P5 79.47(4) . . ? P1 Pt P5 157.26(4) . 3_657 ? P5 Pt P5 78.64(4) . 3_657 ? P1 Pt Cl1 98.87(4) . . ? P5 Pt Cl1 173.68(4) . . ? P5 Pt Cl1 103.55(4) 3_657 . ? C1 P1 Cl2 110.82(16) . . ? C1 P1 P2 103.44(15) . . ? Cl2 P1 P2 100.70(7) . . ? C1 P1 Pt 113.11(15) . . ? Cl2 P1 Pt 121.46(7) . . ? P2 P1 Pt 104.57(6) . . ? C11 P2 C6 89.3(2) . . ? C11 P2 P1 99.73(15) . . ? C6 P2 P1 97.99(14) . . ? C11 P3 C16 86.3(2) . . ? C11 P3 C1 102.4(2) . . ? C16 P3 C1 88.06(19) . . ? C16 P4 C6 102.41(19) . . ? C16 P4 C11 86.09(19) . . ? C6 P4 C11 87.7(2) . . ? C6 P5 P6 100.61(15) . . ? C6 P5 Pt 109.21(14) . . ? P6 P5 Pt 100.91(5) . . ? C6 P5 Pt 124.98(14) . 3_657 ? P6 P5 Pt 117.32(6) . 3_657 ? Pt P5 Pt 101.36(4) . 3_657 ? C16 P6 C1 88.49(19) . . ? C16 P6 P5 100.22(15) . . ? C1 P6 P5 102.11(14) . . ? C2 C1 P1 116.6(3) . . ? C2 C1 P3 114.9(3) . . ? P1 C1 P3 113.6(2) . . ? C2 C1 P6 113.1(3) . . ? P1 C1 P6 104.8(2) . . ? P3 C1 P6 90.31(19) . . ? C4 C2 C3 109.1(4) . . ? C4 C2 C5 107.1(4) . . ? C3 C2 C5 109.3(4) . . ? C4 C2 C1 110.8(4) . . ? C3 C2 C1 109.5(4) . . ? C5 C2 C1 111.0(4) . . ? C7 C6 P5 115.3(3) . . ? C7 C6 P2 111.5(3) . . ? P5 C6 P2 110.2(2) . . ? C7 C6 P4 113.3(3) . . ? P5 C6 P4 113.4(2) . . ? P2 C6 P4 90.6(2) . . ? C9 C7 C10 110.7(4) . . ? C9 C7 C8 107.6(4) . . ? C10 C7 C8 108.0(4) . . ? C9 C7 C6 110.5(4) . . ? C10 C7 C6 109.6(4) . . ? C8 C7 C6 110.4(4) . . ? C12 C11 P2 115.7(3) . . ? C12 C11 P3 113.2(3) . . ? P2 C11 P3 116.9(2) . . ? C12 C11 P4 123.4(3) . . ? P2 C11 P4 91.4(2) . . ? P3 C11 P4 93.13(19) . . ? C13 C12 C14 108.6(5) . . ? C13 C12 C15 109.5(4) . . ? C14 C12 C15 109.3(5) . . ? C13 C12 C11 111.5(4) . . ? C14 C12 C11 110.3(4) . . ? C15 C12 C11 107.5(4) . . ? C17 C16 P6 115.7(3) . . ? C17 C16 P4 113.7(3) . . ? P6 C16 P4 116.3(2) . . ? C17 C16 P3 121.9(3) . . ? P6 C16 P3 92.22(19) . . ? P4 C16 P3 93.7(2) . . ? C20 C17 C19 107.6(4) . . ? C20 C17 C18 110.2(4) . . ? C19 C17 C18 109.4(4) . . ? C20 C17 C16 111.9(4) . . ? C19 C17 C16 110.2(4) . . ? C18 C17 C16 107.6(4) . . ? Cl4 C21 Cl3 112.1(4) . . ? #===END # Attachment 'sep1901.cif' data_sep1901 _database_code_depnum_ccdc_archive 'CCDC 666877' _audit_creation_date 2001-09-26T11:15:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C23 H45 Cl2 P7 Pt1, 1/2(C4 H10 O)' _chemical_formula_sum 'C25 H50 Cl2 O0.5 P7 Pt' _chemical_formula_weight 841.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.241(6) _cell_length_b 9.998(2) _cell_length_c 30.941(8) _cell_angle_alpha 90 _cell_angle_beta 94.772(8) _cell_angle_gamma 90 _cell_volume 6857(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 155493 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.63 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.705 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 10104 _diffrn_reflns_av_R_equivalents 0.09 _diffrn_reflns_av_unetI/netI 0.0964 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 21.93 _diffrn_reflns_theta_full 21.93 _diffrn_measured_fraction_theta_full 0.913 _diffrn_measured_fraction_theta_max 0.913 _reflns_number_total 3811 _reflns_number_gt 2849 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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 ; The solvate electron density near a 2-fold rotation axis is very diffuse, but two carbon atoms were included in the refinement and are presumed to be part of a diethylether molecule disordered about the axis. 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^)+(0.0168P)^2^+273.9670P] 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 3811 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.44 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.151 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 Pt Pt 0.31709(3) 0.67610(7) 0.68681(2) 0.0413(3) Uani 1 1 d . . . Cl1 Cl 0.4353(2) 0.4149(5) 0.71485(15) 0.0632(15) Uani 1 1 d . . . Cl2 Cl 0.3518(2) 0.7018(5) 0.76122(13) 0.0568(14) Uani 1 1 d . . . P1 P 0.3827(2) 0.5158(5) 0.66803(14) 0.0415(12) Uani 1 1 d . . . P2 P 0.3300(2) 0.3527(5) 0.63882(15) 0.0467(13) Uani 1 1 d . . . P3 P 0.4336(2) 0.4474(5) 0.57914(15) 0.0428(13) Uani 1 1 d . . . P4 P 0.2847(2) 0.6465(4) 0.61417(14) 0.0418(12) Uani 1 1 d . . . P5 P 0.3724(2) 0.6791(5) 0.59023(14) 0.0452(12) Uani 1 1 d . . . P6 P 0.3133(2) 0.4096(5) 0.55308(15) 0.0446(13) Uani 1 1 d . . . P7 P 0.2513(2) 0.8494(5) 0.69495(15) 0.0458(13) Uani 1 1 d . . . C1 C 0.4298(8) 0.5705(16) 0.6259(5) 0.040(5) Uani 1 1 d . . . C2 C 0.3736(7) 0.3212(17) 0.5893(5) 0.040(4) Uani 1 1 d . . . C3 C 0.2764(8) 0.4616(16) 0.6037(5) 0.043(5) Uani 1 1 d . . . C4 C 0.3712(8) 0.5446(16) 0.5482(5) 0.040(4) Uani 1 1 d . . . C5 C 0.4908(8) 0.6416(17) 0.6405(5) 0.044(5) Uani 1 1 d . . . C6 C 0.5412(8) 0.543(2) 0.6535(6) 0.064(6) Uani 1 1 d . . . H6A H 0.5781 0.5926 0.6628 0.096 Uiso 1 1 calc R . . H6B H 0.5485 0.4864 0.6287 0.096 Uiso 1 1 calc R . . H6C H 0.5296 0.4873 0.6774 0.096 Uiso 1 1 calc R . . C7 C 0.4807(9) 0.737(2) 0.6780(6) 0.067(6) Uani 1 1 d . . . H7A H 0.5181 0.786 0.6862 0.101 Uiso 1 1 calc R . . H7B H 0.4691 0.6852 0.7029 0.101 Uiso 1 1 calc R . . H7C H 0.4485 0.8003 0.6688 0.101 Uiso 1 1 calc R . . C8 C 0.5123(8) 0.7236(17) 0.6029(6) 0.051(5) Uani 1 1 d . . . H8A H 0.5193 0.6639 0.5787 0.076 Uiso 1 1 calc R . . H8B H 0.5499 0.7698 0.6125 0.076 Uiso 1 1 calc R . . H8C H 0.4814 0.7897 0.5934 0.076 Uiso 1 1 calc R . . C9 C 0.3922(8) 0.175(2) 0.5831(5) 0.051(5) Uani 1 1 d . . . C10 C 0.4389(10) 0.1360(18) 0.6176(6) 0.073(7) Uani 1 1 d . . . H10A H 0.4226 0.1445 0.6459 0.109 Uiso 1 1 calc R . . H10B H 0.4741 0.1945 0.6165 0.109 Uiso 1 1 calc R . . H10C H 0.451 0.043 0.6132 0.109 Uiso 1 1 calc R . . C11 C 0.3363(9) 0.0816(18) 0.5830(7) 0.073(7) Uani 1 1 d . . . H11A H 0.3065 0.1077 0.5595 0.109 Uiso 1 1 calc R . . H11B H 0.3185 0.0894 0.6108 0.109 Uiso 1 1 calc R . . H11C H 0.3488 -0.0111 0.5788 0.109 Uiso 1 1 calc R . . C12 C 0.4167(8) 0.1594(18) 0.5377(6) 0.060(5) Uani 1 1 d . . . H12A H 0.4516 0.2183 0.5357 0.09 Uiso 1 1 calc R . . H12B H 0.3851 0.1837 0.5151 0.09 Uiso 1 1 calc R . . H12C H 0.4289 0.0664 0.5336 0.09 Uiso 1 1 calc R . . C13 C 0.2096(10) 0.4169(18) 0.6046(6) 0.056(6) Uani 1 1 d . . . C14 C 0.1698(9) 0.489(2) 0.5690(6) 0.069(6) Uani 1 1 d . . . H14A H 0.1841 0.4686 0.5406 0.103 Uiso 1 1 calc R . . H14B H 0.1722 0.5862 0.5739 0.103 Uiso 1 1 calc R . . H14C H 0.1279 0.4598 0.5696 0.103 Uiso 1 1 calc R . . C15 C 0.2007(8) 0.2683(19) 0.5969(8) 0.077(7) Uani 1 1 d . . . H15A H 0.2246 0.2183 0.6196 0.115 Uiso 1 1 calc R . . H15B H 0.214 0.2446 0.5685 0.115 Uiso 1 1 calc R . . H15C H 0.1579 0.246 0.5978 0.115 Uiso 1 1 calc R . . C16 C 0.1835(9) 0.451(2) 0.6479(6) 0.069(6) Uani 1 1 d . . . H16A H 0.185 0.5485 0.6524 0.104 Uiso 1 1 calc R . . H16B H 0.2073 0.4069 0.6718 0.104 Uiso 1 1 calc R . . H16C H 0.1415 0.421 0.6471 0.104 Uiso 1 1 calc R . . C17 C 0.3755(9) 0.5965(19) 0.5012(5) 0.050(5) Uani 1 1 d . . . C18 C 0.3164(8) 0.660(2) 0.4856(6) 0.062(6) Uani 1 1 d . . . H18A H 0.3173 0.6859 0.4551 0.093 Uiso 1 1 calc R . . H18B H 0.3099 0.74 0.5031 0.093 Uiso 1 1 calc R . . H18C H 0.2835 0.5964 0.4885 0.093 Uiso 1 1 calc R . . C19 C 0.3871(9) 0.4764(18) 0.4706(5) 0.059(6) Uani 1 1 d . . . H19A H 0.4264 0.436 0.4795 0.089 Uiso 1 1 calc R . . H19B H 0.3871 0.5086 0.4406 0.089 Uiso 1 1 calc R . . H19C H 0.3553 0.4094 0.4724 0.089 Uiso 1 1 calc R . . C20 C 0.4258(8) 0.693(2) 0.4971(5) 0.060(6) Uani 1 1 d . . . H20A H 0.4193 0.773 0.5144 0.089 Uiso 1 1 calc R . . H20B H 0.4271 0.7186 0.4666 0.089 Uiso 1 1 calc R . . H20C H 0.4642 0.6512 0.5075 0.089 Uiso 1 1 calc R . . C21 C 0.2900(8) 0.9996(19) 0.7144(6) 0.062(6) Uani 1 1 d . . . H21A H 0.2603 1.0665 0.7218 0.093 Uiso 1 1 calc R . . H21B H 0.3138 1.0352 0.6918 0.093 Uiso 1 1 calc R . . H21C H 0.3168 0.9784 0.7403 0.093 Uiso 1 1 calc R . . C22 C 0.1999(9) 0.8275(19) 0.7358(6) 0.066(6) Uani 1 1 d . . . H22A H 0.1696 0.7602 0.7262 0.1 Uiso 1 1 calc R . . H22B H 0.1798 0.9126 0.7408 0.1 Uiso 1 1 calc R . . H22C H 0.222 0.7975 0.7628 0.1 Uiso 1 1 calc R . . C23 C 0.2034(9) 0.9044(19) 0.6480(6) 0.066(6) Uani 1 1 d . . . H23A H 0.1825 0.9869 0.6551 0.1 Uiso 1 1 calc R . . H23B H 0.1737 0.8348 0.6397 0.1 Uiso 1 1 calc R . . H23C H 0.2282 0.9213 0.6238 0.1 Uiso 1 1 calc R . . C24 C 0.5384(8) 0.0586(19) 0.7411(6) 0.057(5) Uiso 1 1 d . . . C25 C 0.5534(7) 0.1016(14) 0.7096(5) 0.024(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0478(5) 0.0432(4) 0.0331(4) -0.0037(4) 0.0049(3) 0.0030(4) Cl1 0.071(4) 0.074(4) 0.043(3) 0.007(2) -0.003(3) 0.021(3) Cl2 0.076(4) 0.064(3) 0.029(2) -0.011(2) -0.002(2) 0.006(3) P1 0.049(3) 0.045(3) 0.030(3) 0.000(2) 0.002(2) 0.003(2) P2 0.056(4) 0.042(3) 0.042(3) 0.004(2) 0.004(2) 0.000(2) P3 0.048(4) 0.042(3) 0.038(3) -0.007(2) 0.006(2) 0.000(2) P4 0.053(4) 0.042(3) 0.031(3) -0.003(2) 0.004(2) 0.005(2) P5 0.059(4) 0.040(3) 0.038(3) -0.003(2) 0.013(2) -0.004(3) P6 0.052(4) 0.044(3) 0.038(3) -0.008(2) 0.006(2) -0.004(2) P7 0.055(4) 0.041(3) 0.043(3) -0.004(2) 0.010(2) 0.003(2) C1 0.042(13) 0.046(12) 0.033(10) -0.016(8) 0.005(8) 0.002(9) C2 0.049(12) 0.043(11) 0.029(9) 0.005(8) 0.000(8) -0.005(10) C3 0.060(14) 0.044(11) 0.023(9) -0.006(8) -0.006(9) 0.000(10) C4 0.048(13) 0.050(11) 0.022(9) -0.005(8) 0.009(8) 0.012(9) C5 0.051(14) 0.042(12) 0.039(11) -0.013(8) 0.005(9) -0.001(9) C6 0.040(14) 0.086(16) 0.064(14) -0.022(12) 0.000(10) 0.000(12) C7 0.052(15) 0.081(15) 0.067(14) -0.032(12) -0.007(11) -0.018(11) C8 0.035(13) 0.046(12) 0.071(14) -0.011(10) 0.000(10) -0.007(9) C9 0.052(13) 0.060(13) 0.042(11) -0.017(10) 0.007(9) 0.013(11) C10 0.11(2) 0.040(13) 0.066(14) 0.008(10) -0.009(13) 0.016(12) C11 0.074(18) 0.038(13) 0.111(19) -0.022(11) 0.031(14) -0.015(11) C12 0.058(14) 0.040(12) 0.082(15) -0.019(11) 0.003(11) 0.005(10) C13 0.083(18) 0.049(13) 0.035(11) -0.010(9) 0.003(11) -0.007(11) C14 0.060(16) 0.096(17) 0.050(13) -0.001(12) 0.002(11) -0.018(13) C15 0.029(14) 0.067(15) 0.13(2) -0.024(13) -0.003(12) -0.021(10) C16 0.049(15) 0.102(18) 0.059(14) -0.002(12) 0.013(11) -0.019(12) C17 0.050(15) 0.061(13) 0.041(11) 0.007(9) 0.013(10) 0.002(11) C18 0.063(15) 0.075(14) 0.050(12) 0.019(11) 0.010(10) 0.034(12) C19 0.080(16) 0.062(13) 0.039(11) -0.016(10) 0.020(10) 0.014(11) C20 0.068(15) 0.071(15) 0.043(11) 0.012(10) 0.017(10) 0.012(12) C21 0.049(14) 0.065(14) 0.073(14) -0.018(11) 0.005(11) 0.008(11) C22 0.074(15) 0.044(12) 0.086(15) -0.006(11) 0.038(12) -0.002(12) C23 0.067(16) 0.063(14) 0.070(14) 0.009(11) 0.004(11) 0.039(12) #----------------------------------------------------------------------------# # 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 Pt P1 2.275(5) . ? Pt P7 2.295(5) . ? Pt P4 2.322(4) . ? Pt Cl2 2.380(4) . ? Cl1 P1 2.050(6) . ? P1 C1 1.823(17) . ? P1 P2 2.162(7) . ? P2 C3 1.892(17) . ? P2 C2 1.907(16) . ? P3 C2 1.881(17) . ? P3 C4 1.888(16) . ? P3 C1 1.907(15) . ? P4 C3 1.883(17) . ? P4 P5 2.168(7) . ? P5 C4 1.869(16) . ? P5 C1 1.948(17) . ? P6 C4 1.881(18) . ? P6 C2 1.893(16) . ? P6 C3 1.900(17) . ? P7 C22 1.788(17) . ? P7 C21 1.809(19) . ? P7 C23 1.814(18) . ? C1 C5 1.56(2) . ? C2 C9 1.54(2) . ? C3 C13 1.55(2) . ? C4 C17 1.55(2) . ? C5 C6 1.52(2) . ? C5 C8 1.53(2) . ? C5 C7 1.53(2) . ? C9 C10 1.48(2) . ? C9 C11 1.55(2) . ? C9 C12 1.56(2) . ? C13 C15 1.51(2) . ? C13 C14 1.54(3) . ? C13 C16 1.54(2) . ? C17 C20 1.49(2) . ? C17 C18 1.50(2) . ? C17 C19 1.57(2) . ? C24 C25 1.14(2) . ? C24 C24 1.84(4) 2_656 ? 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 Pt P7 171.13(16) . . ? P1 Pt P4 79.47(16) . . ? P7 Pt P4 93.02(16) . . ? P1 Pt Cl2 99.21(16) . . ? P7 Pt Cl2 88.32(16) . . ? P4 Pt Cl2 178.65(17) . . ? C1 P1 Cl1 109.0(6) . . ? C1 P1 P2 104.5(5) . . ? Cl1 P1 P2 100.5(3) . . ? C1 P1 Pt 113.0(6) . . ? Cl1 P1 Pt 120.4(2) . . ? P2 P1 Pt 107.6(2) . . ? C3 P2 C2 88.4(7) . . ? C3 P2 P1 95.7(6) . . ? C2 P2 P1 99.6(6) . . ? C2 P3 C4 85.9(7) . . ? C2 P3 C1 103.3(7) . . ? C4 P3 C1 88.6(7) . . ? C3 P4 P5 99.6(6) . . ? C3 P4 Pt 108.1(5) . . ? P5 P4 Pt 95.5(2) . . ? C4 P5 C1 87.9(7) . . ? C4 P5 P4 99.7(6) . . ? C1 P5 P4 106.8(6) . . ? C4 P6 C2 85.8(7) . . ? C4 P6 C3 102.4(7) . . ? C2 P6 C3 88.5(7) . . ? C22 P7 C21 100.4(9) . . ? C22 P7 C23 103.6(10) . . ? C21 P7 C23 104.3(9) . . ? C22 P7 Pt 115.9(7) . . ? C21 P7 Pt 111.9(6) . . ? C23 P7 Pt 118.6(6) . . ? C5 C1 P1 117.8(11) . . ? C5 C1 P3 114.8(11) . . ? P1 C1 P3 114.4(9) . . ? C5 C1 P5 115.0(12) . . ? P1 C1 P5 100.6(8) . . ? P3 C1 P5 89.9(7) . . ? C9 C2 P3 114.6(12) . . ? C9 C2 P6 123.8(11) . . ? P3 C2 P6 93.8(7) . . ? C9 C2 P2 114.6(11) . . ? P3 C2 P2 116.0(9) . . ? P6 C2 P2 90.9(8) . . ? C13 C3 P4 111.1(12) . . ? C13 C3 P2 112.5(12) . . ? P4 C3 P2 114.7(8) . . ? C13 C3 P6 114.6(11) . . ? P4 C3 P6 111.6(9) . . ? P2 C3 P6 91.2(8) . . ? C17 C4 P5 114.3(12) . . ? C17 C4 P6 114.2(12) . . ? P5 C4 P6 115.5(8) . . ? C17 C4 P3 123.2(12) . . ? P5 C4 P3 92.9(7) . . ? P6 C4 P3 94.0(8) . . ? C6 C5 C8 106.2(15) . . ? C6 C5 C7 110.7(15) . . ? C8 C5 C7 108.5(15) . . ? C6 C5 C1 112.6(14) . . ? C8 C5 C1 110.0(14) . . ? C7 C5 C1 108.8(14) . . ? C10 C9 C2 110.0(14) . . ? C10 C9 C11 110.9(17) . . ? C2 C9 C11 110.4(14) . . ? C10 C9 C12 110.3(16) . . ? C2 C9 C12 109.0(15) . . ? C11 C9 C12 106.2(15) . . ? C15 C13 C14 106.9(16) . . ? C15 C13 C16 107.6(17) . . ? C14 C13 C16 106.4(17) . . ? C15 C13 C3 113.0(16) . . ? C14 C13 C3 110.1(15) . . ? C16 C13 C3 112.4(14) . . ? C20 C17 C18 109.9(16) . . ? C20 C17 C4 113.7(15) . . ? C18 C17 C4 108.8(14) . . ? C20 C17 C19 106.3(15) . . ? C18 C17 C19 108.4(15) . . ? C4 C17 C19 109.7(14) . . ? C25 C24 C24 127.0(19) . 2_656 ? #===END # Attachment 'sep4600.cif' data_sep4600 _database_code_depnum_ccdc_archive 'CCDC 666878' _audit_creation_date 2000-10-02T11:25:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H54 Cl4 P8 Pt2, 3(C4 H8 O)' _chemical_formula_sum 'C38 H78 Cl4 O3 P8 Pt2' _chemical_formula_weight 1362.74 _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 11.7635(8) _cell_length_b 14.2516(10) _cell_length_c 18.5472(13) _cell_angle_alpha 100.054(3) _cell_angle_beta 101.270(4) _cell_angle_gamma 113.195(3) _cell_volume 2691.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19076 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.66 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18350 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0935 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 24.86 _diffrn_reflns_theta_full 24.86 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 9195 _reflns_number_gt 6758 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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 ; There are three poorly defined molecules of thf solvate for which the C and O atoms were left isotropic. 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^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9195 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.135 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.554 _refine_diff_density_min -2.59 _refine_diff_density_rms 0.193 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 0.25291(3) 0.91357(3) 0.37418(2) 0.02706(13) Uani 1 1 d . . . Pt2 Pt 0.25272(3) 1.34484(3) 0.32788(2) 0.03269(14) Uani 1 1 d . A . Cl1 Cl 0.2344(3) 0.7963(2) 0.45094(14) 0.0406(6) Uani 1 1 d . . . Cl2 Cl 0.2176(3) 0.7774(2) 0.26632(15) 0.0423(6) Uani 1 1 d . . . Cl3 Cl 0.0400(2) 1.2706(2) 0.32583(18) 0.0540(8) Uani 1 1 d . . . Cl4 Cl 0.4707(3) 1.4256(2) 0.3394(2) 0.0616(9) Uani 1 1 d . . . P1 P 0.2607(2) 1.19381(19) 0.26040(14) 0.0272(6) Uani 1 1 d . . . P2 P 0.4331(2) 1.1864(2) 0.32738(13) 0.0282(6) Uani 1 1 d . . . P3 P 0.4177(2) 1.1490(2) 0.14938(14) 0.0298(6) Uani 1 1 d . . . P4 P 0.2852(2) 1.01666(19) 0.29651(13) 0.0255(5) Uani 1 1 d . . . P5 P 0.4007(2) 0.9928(2) 0.22074(14) 0.0291(6) Uani 1 1 d . . . P6 P 0.1644(2) 1.0278(2) 0.13300(14) 0.0292(6) Uani 1 1 d . . . P7 P 0.2821(2) 1.0346(2) 0.48038(14) 0.0313(6) Uani 1 1 d . . . P8 P 0.2623(3) 1.5043(2) 0.38361(19) 0.0491(8) Uani 1 1 d . . . C1 C 0.4934(8) 1.1426(7) 0.2470(5) 0.026(2) Uani 1 1 d . . . C2 C 0.2776(8) 1.1774(7) 0.1616(5) 0.028(2) Uani 1 1 d . . . C3 C 0.3049(9) 1.0012(7) 0.1301(5) 0.029(2) Uani 1 1 d . . . C4 C 0.1582(9) 1.0422(8) 0.2354(5) 0.031(2) Uani 1 1 d . . . C5 C 0.6434(8) 1.1909(8) 0.2711(5) 0.033(2) Uani 1 1 d . . . C6 C 0.7041(9) 1.3125(8) 0.2874(6) 0.045(3) Uani 1 1 d . . . H6A H 0.6714 1.3313 0.242 0.068 Uiso 1 1 calc R . . H6B H 0.7983 1.3409 0.2999 0.068 Uiso 1 1 calc R . . H6C H 0.6811 1.3429 0.3306 0.068 Uiso 1 1 calc R . . C7 C 0.6885(9) 1.1461(9) 0.2049(6) 0.045(3) Uani 1 1 d . . . H7A H 0.6577 1.1641 0.1587 0.068 Uiso 1 1 calc R . . H7B H 0.6531 1.0687 0.1944 0.068 Uiso 1 1 calc R . . H7C H 0.7832 1.1775 0.2202 0.068 Uiso 1 1 calc R . . C8 C 0.6937(10) 1.1614(10) 0.3422(6) 0.048(3) Uani 1 1 d . . . H8A H 0.7883 1.1929 0.3566 0.073 Uiso 1 1 calc R . . H8B H 0.6585 1.0839 0.3308 0.073 Uiso 1 1 calc R . . H8C H 0.6664 1.1885 0.3845 0.073 Uiso 1 1 calc R . . C9 C 0.2496(10) 1.2471(8) 0.1117(5) 0.036(2) Uani 1 1 d . . . C10 C 0.1289(11) 1.2614(9) 0.1217(7) 0.052(3) Uani 1 1 d . . . H10A H 0.0545 1.1915 0.1079 0.078 Uiso 1 1 calc R . . H10B H 0.1102 1.3031 0.0884 0.078 Uiso 1 1 calc R . . H10C H 0.1457 1.2987 0.1752 0.078 Uiso 1 1 calc R . . C11 C 0.2196(12) 1.1919(10) 0.0277(6) 0.057(3) Uani 1 1 d . . . H11A H 0.1457 1.1217 0.0139 0.086 Uiso 1 1 calc R . . H11B H 0.2951 1.1838 0.0189 0.086 Uiso 1 1 calc R . . H11C H 0.1985 1.2347 -0.0038 0.086 Uiso 1 1 calc R . . C12 C 0.3632(12) 1.3563(10) 0.1329(7) 0.062(3) Uani 1 1 d . . . H12A H 0.3821 1.3922 0.1869 0.092 Uiso 1 1 calc R . . H12B H 0.3416 1.3984 0.101 0.092 Uiso 1 1 calc R . . H12C H 0.4391 1.3487 0.1244 0.092 Uiso 1 1 calc R . . C13 C 0.2850(9) 0.9148(8) 0.0572(5) 0.032(2) Uani 1 1 d . . . C14 C 0.2358(11) 0.9427(9) -0.0159(5) 0.045(3) Uani 1 1 d . . . H14A H 0.3008 1.0112 -0.0169 0.067 Uiso 1 1 calc R . . H14B H 0.1549 0.9474 -0.016 0.067 Uiso 1 1 calc R . . H14C H 0.2206 0.8873 -0.0612 0.067 Uiso 1 1 calc R . . C15 C 0.4114(10) 0.9079(9) 0.0561(6) 0.047(3) Uani 1 1 d . . . H15A H 0.4756 0.9764 0.0547 0.07 Uiso 1 1 calc R . . H15B H 0.3955 0.8524 0.0107 0.07 Uiso 1 1 calc R . . H15C H 0.4438 0.8906 0.1023 0.07 Uiso 1 1 calc R . . C16 C 0.1843(10) 0.8088(8) 0.0592(6) 0.042(3) Uani 1 1 d . . . H16A H 0.1037 0.8138 0.0598 0.064 Uiso 1 1 calc R . . H16B H 0.216 0.7912 0.1054 0.064 Uiso 1 1 calc R . . H16C H 0.1682 0.7532 0.0138 0.064 Uiso 1 1 calc R . . C17 C 0.0138(9) 0.9851(8) 0.2363(5) 0.033(2) Uani 1 1 d . . . C18 C -0.0702(8) 1.0238(8) 0.1880(5) 0.035(2) Uani 1 1 d . . . H18A H -0.0633 1.0115 0.1357 0.052 Uiso 1 1 calc R . . H18B H -0.0407 1.0999 0.2105 0.052 Uiso 1 1 calc R . . H18C H -0.1605 0.9847 0.1869 0.052 Uiso 1 1 calc R . . C19 C 0.0026(9) 1.0048(8) 0.3176(5) 0.038(3) Uani 1 1 d . . . H19A H 0.0557 0.9797 0.3488 0.057 Uiso 1 1 calc R . . H19B H -0.0879 0.9663 0.3163 0.057 Uiso 1 1 calc R . . H19C H 0.0328 1.0811 0.3399 0.057 Uiso 1 1 calc R . . C20 C -0.0347(9) 0.8658(7) 0.2002(6) 0.040(3) Uani 1 1 d . . . H20A H -0.0286 0.854 0.1478 0.06 Uiso 1 1 calc R . . H20B H -0.1249 0.8275 0.1995 0.06 Uiso 1 1 calc R . . H20C H 0.0185 0.8398 0.2304 0.06 Uiso 1 1 calc R . . C21 C 0.2970(11) 1.1640(8) 0.4748(6) 0.044(3) Uani 1 1 d . . . H21A H 0.3662 1.1964 0.452 0.066 Uiso 1 1 calc R . . H21B H 0.3177 1.2094 0.5263 0.066 Uiso 1 1 calc R . . H21C H 0.2152 1.1565 0.4429 0.066 Uiso 1 1 calc R . . C22 C 0.4270(9) 1.0647(9) 0.5553(5) 0.041(3) Uani 1 1 d . . . H22A H 0.4274 0.9983 0.5625 0.062 Uiso 1 1 calc R . . H22B H 0.428 1.1072 0.6033 0.062 Uiso 1 1 calc R . . H22C H 0.5037 1.1049 0.5406 0.062 Uiso 1 1 calc R . . C23 C 0.1519(10) 0.9836(9) 0.5229(6) 0.045(3) Uani 1 1 d . . . H23A H 0.1388 0.913 0.5279 0.068 Uiso 1 1 calc R . . H23B H 0.0723 0.9784 0.4902 0.068 Uiso 1 1 calc R . . H23C H 0.1744 1.0317 0.5736 0.068 Uiso 1 1 calc R . . C24 C 0.213(3) 1.517(2) 0.4666(14) 0.065(8) Uani 0.54(2) 1 d P A 1 H24A H 0.1286 1.4568 0.4581 0.098 Uiso 0.54(2) 1 calc PR A 1 H24B H 0.2061 1.5834 0.4788 0.098 Uiso 0.54(2) 1 calc PR A 1 H24C H 0.2766 1.5161 0.5093 0.098 Uiso 0.54(2) 1 calc PR A 1 C25 C 0.410(3) 1.617(2) 0.413(2) 0.093(14) Uani 0.54(2) 1 d P A 1 H25A H 0.4502 1.6207 0.3713 0.14 Uiso 0.54(2) 1 calc PR A 1 H25B H 0.4673 1.6137 0.4577 0.14 Uiso 0.54(2) 1 calc PR A 1 H25C H 0.3965 1.6807 0.4269 0.14 Uiso 0.54(2) 1 calc PR A 1 C26 C 0.1444(19) 1.5266(16) 0.3139(14) 0.050(7) Uani 0.54(2) 1 d P A 1 H26A H 0.164 1.5212 0.2648 0.075 Uiso 0.54(2) 1 calc PR A 1 H26B H 0.1509 1.5975 0.3337 0.075 Uiso 0.54(2) 1 calc PR A 1 H26C H 0.0566 1.4727 0.3067 0.075 Uiso 0.54(2) 1 calc PR A 1 C24A C 0.377(3) 1.555(3) 0.483(2) 0.112(17) Uani 0.46(2) 1 d P A 2 H24D H 0.4607 1.5572 0.4805 0.168 Uiso 0.46(2) 1 calc PR A 2 H24E H 0.3414 1.508 0.5139 0.168 Uiso 0.46(2) 1 calc PR A 2 H24F H 0.3901 1.6271 0.507 0.168 Uiso 0.46(2) 1 calc PR A 2 C25A C 0.341(7) 1.598(4) 0.342(3) 0.16(3) Uani 0.46(2) 1 d P A 2 H25D H 0.4163 1.5902 0.3324 0.247 Uiso 0.46(2) 1 calc PR A 2 H25E H 0.3695 1.6694 0.3754 0.247 Uiso 0.46(2) 1 calc PR A 2 H25F H 0.2822 1.5894 0.2927 0.247 Uiso 0.46(2) 1 calc PR A 2 C26A C 0.123(3) 1.509(2) 0.403(3) 0.12(2) Uani 0.46(2) 1 d P A 2 H26D H 0.0811 1.4503 0.4243 0.182 Uiso 0.46(2) 1 calc PR A 2 H26E H 0.0622 1.5011 0.3551 0.182 Uiso 0.46(2) 1 calc PR A 2 H26F H 0.1472 1.5767 0.4395 0.182 Uiso 0.46(2) 1 calc PR A 2 O1 O 0.1661(11) 1.2429(9) 0.5985(7) 0.107(4) Uiso 1 1 d . B 3 C27 C 0.137(2) 1.3061(16) 0.5531(12) 0.133(7) Uiso 1 1 d . B 3 H27A H 0.054 1.2624 0.5127 0.159 Uiso 1 1 calc R B 3 H27B H 0.2058 1.3345 0.5282 0.159 Uiso 1 1 calc R B 3 C28 C 0.129(2) 1.3955(16) 0.6039(12) 0.125(7) Uiso 1 1 d . B 3 H28A H 0.1993 1.4648 0.6067 0.15 Uiso 1 1 calc R B 3 H28B H 0.0449 1.396 0.5854 0.15 Uiso 1 1 calc R B 3 C29 C 0.1431(19) 1.3753(16) 0.6715(11) 0.116(6) Uiso 1 1 d . B 3 H29A H 0.0577 1.3442 0.6808 0.139 Uiso 1 1 calc R B 3 H29B H 0.1992 1.4424 0.7124 0.139 Uiso 1 1 calc R B 3 C30 C 0.201(3) 1.301(3) 0.674(2) 0.248(16) Uiso 1 1 d . B 3 H30A H 0.2965 1.3397 0.6948 0.298 Uiso 1 1 calc R B 3 H30B H 0.1672 1.2535 0.7055 0.298 Uiso 1 1 calc R B 3 O2 O 0.3855(15) 1.1936(13) -0.1848(10) 0.155(5) Uiso 1 1 d . C 3 C31 C 0.477(2) 1.2445(19) -0.2245(15) 0.164(9) Uiso 1 1 d . C 3 H31A H 0.4375 1.2643 -0.2678 0.196 Uiso 1 1 calc R C 3 H31B H 0.5186 1.2001 -0.2426 0.196 Uiso 1 1 calc R C 3 C32 C 0.567(2) 1.3372(19) -0.1601(15) 0.161(9) Uiso 1 1 d . C 3 H32A H 0.6376 1.3227 -0.1344 0.193 Uiso 1 1 calc R C 3 H32B H 0.6057 1.3987 -0.1803 0.193 Uiso 1 1 calc R C 3 C33 C 0.510(4) 1.365(3) -0.106(2) 0.268(17) Uiso 1 1 d . C 3 H33A H 0.5693 1.3932 -0.0538 0.322 Uiso 1 1 calc R C 3 H33B H 0.4766 1.4158 -0.1182 0.322 Uiso 1 1 calc R C 3 C34 C 0.414(2) 1.2677(19) -0.1176(14) 0.148(8) Uiso 1 1 d . C 3 H34A H 0.3345 1.2757 -0.1154 0.177 Uiso 1 1 calc R C 3 H34B H 0.4365 1.2397 -0.0745 0.177 Uiso 1 1 calc R C 3 O3 O -0.238(3) 0.422(3) 0.1001(19) 0.310(14) Uiso 1 1 d . D 3 C35 C -0.243(5) 0.530(4) 0.076(3) 0.34(3) Uiso 1 1 d . D 3 H35A H -0.299 0.5137 0.0242 0.408 Uiso 1 1 calc R D 3 H35B H -0.2639 0.5736 0.1145 0.408 Uiso 1 1 calc R D 3 C36 C -0.115(4) 0.570(3) 0.0820(19) 0.218(14) Uiso 1 1 d . D 3 H36A H -0.0723 0.6403 0.1208 0.262 Uiso 1 1 calc R D 3 H36B H -0.1066 0.5837 0.0324 0.262 Uiso 1 1 calc R D 3 C37 C -0.042(3) 0.513(3) 0.101(2) 0.228(14) Uiso 1 1 d . D 3 H37A H 0.0439 0.5625 0.138 0.274 Uiso 1 1 calc R D 3 H37B H -0.0279 0.4789 0.0544 0.274 Uiso 1 1 calc R D 3 C38 C -0.120(4) 0.431(3) 0.136(2) 0.234(15) Uiso 1 1 d . D 3 H38A H -0.1126 0.3632 0.1213 0.281 Uiso 1 1 calc R D 3 H38B H -0.0963 0.4568 0.1921 0.281 Uiso 1 1 calc R D 3 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 0.0257(2) 0.0359(2) 0.0232(2) 0.00824(17) 0.00586(16) 0.01788(18) Pt2 0.0248(2) 0.0327(2) 0.0366(2) 0.00170(18) 0.00325(18) 0.01478(19) Cl1 0.0489(16) 0.0451(16) 0.0357(14) 0.0172(12) 0.0132(13) 0.0256(13) Cl2 0.0584(17) 0.0352(14) 0.0358(14) 0.0054(11) 0.0151(13) 0.0244(13) Cl3 0.0290(14) 0.0475(17) 0.078(2) 0.0008(15) 0.0126(15) 0.0178(13) Cl4 0.0290(15) 0.0375(16) 0.104(3) 0.0019(16) 0.0167(16) 0.0088(13) P1 0.0200(12) 0.0318(14) 0.0272(13) 0.0044(11) 0.0023(11) 0.0127(11) P2 0.0228(13) 0.0370(15) 0.0214(12) 0.0033(11) 0.0026(11) 0.0138(12) P3 0.0276(13) 0.0393(15) 0.0241(13) 0.0105(11) 0.0066(11) 0.0160(12) P4 0.0227(12) 0.0356(14) 0.0197(12) 0.0045(10) 0.0040(10) 0.0166(11) P5 0.0260(13) 0.0403(15) 0.0257(13) 0.0079(11) 0.0068(11) 0.0202(12) P6 0.0264(13) 0.0369(15) 0.0217(13) 0.0063(11) 0.0024(11) 0.0146(12) P7 0.0277(13) 0.0454(16) 0.0261(13) 0.0090(12) 0.0073(11) 0.0222(13) P8 0.0480(18) 0.0373(17) 0.057(2) -0.0028(15) 0.0118(16) 0.0223(15) C1 0.016(4) 0.037(6) 0.019(5) 0.005(4) 0.004(4) 0.009(4) C2 0.023(5) 0.034(6) 0.026(5) 0.010(4) -0.003(4) 0.016(4) C3 0.030(5) 0.034(6) 0.015(5) 0.006(4) -0.002(4) 0.011(5) C4 0.027(5) 0.041(6) 0.024(5) 0.007(4) -0.003(4) 0.021(5) C5 0.018(5) 0.051(7) 0.031(5) 0.009(5) 0.003(4) 0.019(5) C6 0.026(6) 0.047(7) 0.053(7) 0.008(6) 0.014(5) 0.009(5) C7 0.021(5) 0.063(8) 0.044(7) 0.003(6) 0.004(5) 0.019(5) C8 0.034(6) 0.077(9) 0.047(7) 0.030(6) 0.018(5) 0.029(6) C9 0.039(6) 0.034(6) 0.030(6) 0.013(5) 0.006(5) 0.012(5) C10 0.052(7) 0.068(8) 0.052(7) 0.031(6) 0.003(6) 0.042(7) C11 0.066(8) 0.083(9) 0.040(7) 0.034(7) 0.012(6) 0.045(8) C12 0.061(8) 0.070(9) 0.070(9) 0.043(7) 0.017(7) 0.037(7) C13 0.038(6) 0.047(6) 0.015(5) 0.001(4) 0.007(4) 0.027(5) C14 0.052(7) 0.059(7) 0.021(5) 0.002(5) 0.002(5) 0.029(6) C15 0.049(7) 0.067(8) 0.032(6) 0.006(5) 0.020(5) 0.034(6) C16 0.040(6) 0.038(6) 0.034(6) -0.005(5) 0.006(5) 0.011(5) C17 0.029(5) 0.036(6) 0.029(5) 0.009(4) 0.005(4) 0.012(5) C18 0.016(5) 0.056(7) 0.019(5) 0.008(5) -0.009(4) 0.010(5) C19 0.035(6) 0.061(7) 0.034(6) 0.015(5) 0.019(5) 0.033(6) C20 0.026(5) 0.036(6) 0.052(7) 0.007(5) 0.008(5) 0.012(5) C21 0.062(7) 0.050(7) 0.027(6) 0.009(5) 0.014(5) 0.032(6) C22 0.034(6) 0.069(8) 0.015(5) -0.005(5) -0.008(4) 0.031(6) C23 0.042(6) 0.052(7) 0.039(6) 0.002(5) 0.016(5) 0.021(6) C24 0.063(18) 0.075(18) 0.058(16) 0.005(13) 0.032(14) 0.028(14) C25 0.057(17) 0.036(15) 0.16(4) -0.02(2) 0.03(2) 0.012(13) C26 0.038(12) 0.038(12) 0.073(17) 0.008(11) -0.001(11) 0.028(11) C24A 0.08(3) 0.16(4) 0.07(2) -0.02(3) 0.01(2) 0.05(3) C25A 0.35(9) 0.12(4) 0.19(5) 0.13(4) 0.22(7) 0.17(5) C26A 0.05(2) 0.06(2) 0.25(7) 0.00(3) 0.04(3) 0.038(18) #----------------------------------------------------------------------------# # 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 2.212(3) . ? Pt1 P7 2.248(2) . ? Pt1 Cl1 2.352(3) . ? Pt1 Cl2 2.371(2) . ? Pt2 P8 2.275(3) . ? Pt2 Cl3 2.291(3) . ? Pt2 Cl4 2.307(3) . ? Pt2 P1 2.340(2) . ? P1 C2 1.866(9) . ? P1 C4 1.928(10) . ? P1 P2 2.213(3) . ? P2 C1 1.885(8) . ? P2 P4 2.240(3) . ? P3 C1 1.890(9) . ? P3 C2 1.890(9) . ? P3 C3 1.917(10) . ? P4 C4 1.887(9) . ? P4 P5 2.210(3) . ? P5 C3 1.884(9) . ? P5 C1 1.892(9) . ? P6 C3 1.843(9) . ? P6 C4 1.893(9) . ? P6 C2 1.922(10) . ? P7 C21 1.807(11) . ? P7 C23 1.814(10) . ? P7 C22 1.820(9) . ? P8 C25A 1.71(3) . ? P8 C25 1.74(3) . ? P8 C24 1.75(2) . ? P8 C26A 1.77(3) . ? P8 C26 1.87(2) . ? P8 C24A 1.88(3) . ? C1 C5 1.554(12) . ? C2 C9 1.552(13) . ? C3 C13 1.571(12) . ? C4 C17 1.573(12) . ? C5 C8 1.533(14) . ? C5 C6 1.537(14) . ? C5 C7 1.563(12) . ? C9 C12 1.518(14) . ? C9 C11 1.520(14) . ? C9 C10 1.553(14) . ? C13 C16 1.521(13) . ? C13 C15 1.532(12) . ? C13 C14 1.548(14) . ? C17 C19 1.526(12) . ? C17 C18 1.529(13) . ? C17 C20 1.534(13) . ? O1 C30 1.38(3) . ? O1 C27 1.42(2) . ? C27 C28 1.49(2) . ? C28 C29 1.33(2) . ? C29 C30 1.48(3) . ? O2 C34 1.37(2) . ? O2 C31 1.45(2) . ? C31 C32 1.46(3) . ? C32 C33 1.39(3) . ? C33 C34 1.34(3) . ? O3 C38 1.36(4) . ? O3 C35 1.70(5) . ? C35 C36 1.35(5) . ? C36 C37 1.44(4) . ? C37 C38 1.52(4) . ? 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 P7 98.68(9) . . ? P4 Pt1 Cl1 173.21(8) . . ? P7 Pt1 Cl1 86.14(9) . . ? P4 Pt1 Cl2 84.96(9) . . ? P7 Pt1 Cl2 176.32(9) . . ? Cl1 Pt1 Cl2 90.27(9) . . ? P8 Pt2 Cl3 86.99(10) . . ? P8 Pt2 Cl4 90.39(11) . . ? Cl3 Pt2 Cl4 175.77(11) . . ? P8 Pt2 P1 171.84(10) . . ? Cl3 Pt2 P1 99.13(9) . . ? Cl4 Pt2 P1 83.80(9) . . ? C2 P1 C4 89.2(4) . . ? C2 P1 P2 103.5(3) . . ? C4 P1 P2 92.5(3) . . ? C2 P1 Pt2 122.3(3) . . ? C4 P1 Pt2 136.0(3) . . ? P2 P1 Pt2 106.88(11) . . ? C1 P2 P1 99.8(3) . . ? C1 P2 P4 86.5(3) . . ? P1 P2 P4 78.82(12) . . ? C1 P3 C2 104.2(4) . . ? C1 P3 C3 86.1(4) . . ? C2 P3 C3 87.6(4) . . ? C4 P4 P5 104.5(3) . . ? C4 P4 Pt1 126.1(3) . . ? P5 P4 Pt1 115.02(12) . . ? C4 P4 P2 92.7(3) . . ? P5 P4 P2 82.71(12) . . ? Pt1 P4 P2 126.26(12) . . ? C3 P5 C1 87.0(4) . . ? C3 P5 P4 98.8(3) . . ? C1 P5 P4 87.2(3) . . ? C3 P6 C4 105.5(4) . . ? C3 P6 C2 88.8(4) . . ? C4 P6 C2 88.6(4) . . ? C21 P7 C23 105.1(5) . . ? C21 P7 C22 103.6(5) . . ? C23 P7 C22 104.2(5) . . ? C21 P7 Pt1 119.6(3) . . ? C23 P7 Pt1 111.0(3) . . ? C22 P7 Pt1 112.0(3) . . ? C25A P8 C25 45(2) . . ? C25A P8 C24 130.9(17) . . ? C25 P8 C24 100.4(15) . . ? C25A P8 C26A 115(2) . . ? C25 P8 C26A 121.7(14) . . ? C24 P8 C26A 46.2(17) . . ? C25A P8 C26 69(2) . . ? C25 P8 C26 108.4(15) . . ? C24 P8 C26 103.0(12) . . ? C26A P8 C26 57.9(18) . . ? C25A P8 C24A 102(3) . . ? C25 P8 C24A 56.3(18) . . ? C24 P8 C24A 56.8(13) . . ? C26A P8 C24A 101(2) . . ? C26 P8 C24A 145.6(14) . . ? C25A P8 Pt2 110.3(13) . . ? C25 P8 Pt2 119.0(9) . . ? C24 P8 Pt2 118.0(9) . . ? C26A P8 Pt2 119.1(10) . . ? C26 P8 Pt2 106.7(6) . . ? C24A P8 Pt2 107.5(13) . . ? C5 C1 P2 111.6(6) . . ? C5 C1 P3 114.7(6) . . ? P2 C1 P3 116.4(5) . . ? C5 C1 P5 117.2(6) . . ? P2 C1 P5 102.2(4) . . ? P3 C1 P5 93.1(4) . . ? C9 C2 P1 120.9(6) . . ? C9 C2 P3 113.6(6) . . ? P1 C2 P3 114.8(5) . . ? C9 C2 P6 119.6(6) . . ? P1 C2 P6 91.5(4) . . ? P3 C2 P6 90.8(4) . . ? C13 C3 P6 115.6(6) . . ? C13 C3 P5 112.8(7) . . ? P6 C3 P5 118.2(5) . . ? C13 C3 P3 122.3(6) . . ? P6 C3 P3 92.4(4) . . ? P5 C3 P3 92.4(4) . . ? C17 C4 P4 119.3(7) . . ? C17 C4 P6 109.7(6) . . ? P4 C4 P6 112.7(4) . . ? C17 C4 P1 125.4(6) . . ? P4 C4 P1 95.6(4) . . ? P6 C4 P1 90.4(4) . . ? C8 C5 C6 109.6(9) . . ? C8 C5 C1 110.7(8) . . ? C6 C5 C1 110.9(8) . . ? C8 C5 C7 107.9(8) . . ? C6 C5 C7 107.9(8) . . ? C1 C5 C7 109.8(7) . . ? C12 C9 C11 109.4(9) . . ? C12 C9 C2 111.7(9) . . ? C11 C9 C2 109.6(8) . . ? C12 C9 C10 108.5(9) . . ? C11 C9 C10 107.2(9) . . ? C2 C9 C10 110.3(8) . . ? C16 C13 C15 110.0(8) . . ? C16 C13 C14 109.7(9) . . ? C15 C13 C14 108.6(8) . . ? C16 C13 C3 107.4(7) . . ? C15 C13 C3 111.3(8) . . ? C14 C13 C3 109.8(8) . . ? C19 C17 C18 109.0(7) . . ? C19 C17 C20 110.2(8) . . ? C18 C17 C20 108.4(8) . . ? C19 C17 C4 111.6(8) . . ? C18 C17 C4 110.5(8) . . ? C20 C17 C4 107.1(7) . . ? C30 O1 C27 106(2) . . ? O1 C27 C28 108.6(17) . . ? C29 C28 C27 103.7(19) . . ? C28 C29 C30 110(2) . . ? O1 C30 C29 105(3) . . ? C34 O2 C31 106.8(19) . . ? O2 C31 C32 97(2) . . ? C33 C32 C31 114(3) . . ? C34 C33 C32 98(3) . . ? C33 C34 O2 116(3) . . ? C38 O3 C35 117(3) . . ? C36 C35 O3 90(3) . . ? C35 C36 C37 122(4) . . ? C36 C37 C38 106(3) . . ? O3 C38 C37 97(3) . . ? #===END