# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Platinum(II) tetramesityltetraphosphane-1,4-diides ; _publ_requested_category FM loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Beatriz Gallego' 'Santiago Gomez-Ruiz' # Attachment 'Hey-Hawkins_Pt.cif' data_c2c _database_code_depnum_ccdc_archive 'CCDC 713498' _audit_creation_date 2007-08-03T12:06:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C56 H68 P4 Pt' _chemical_formula_weight 1060.07 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 16.960(4) _cell_length_b 11.376(2) _cell_length_c 26.197(6) _cell_angle_alpha 90 _cell_angle_beta 94.319(19) _cell_angle_gamma 90 _cell_volume 5040.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 13086 _cell_measurement_theta_min 2.5491 _cell_measurement_theta_max 32.4524 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.943 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0017736434 _diffrn_orient_matrix_ub_12 -0.0570370529 _diffrn_orient_matrix_ub_13 -0.011294726 _diffrn_orient_matrix_ub_21 -0.0410193481 _diffrn_orient_matrix_ub_22 -0.0038844449 _diffrn_orient_matrix_ub_23 0.004357386 _diffrn_orient_matrix_ub_31 -0.0100713415 _diffrn_orient_matrix_ub_32 0.0256877806 _diffrn_orient_matrix_ub_33 -0.0244190459 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_number 53039 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4961 _reflns_number_gt 3881 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^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 4961 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.755 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.137 #----------------------------------------------------------------------------# # 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 Pt Pt -1.7033 8.3905 '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' 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' 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 0.30760(2) 0.25 0.02218(10) Uani 1 2 d S . . P1 P 0.08109(7) 0.45160(10) 0.28922(4) 0.0213(3) Uani 1 1 d . . . P2 P 0.01003(7) 0.61539(10) 0.29225(4) 0.0213(3) Uani 1 1 d . . . C1 C 0.0960(3) 0.4214(4) 0.35920(17) 0.0230(10) Uani 1 1 d . . . C2 C 0.0340(3) 0.4039(4) 0.39196(17) 0.0261(11) Uani 1 1 d . . . C3 C 0.0535(3) 0.3834(4) 0.44386(18) 0.0328(12) Uani 1 1 d . . . H3 H 0.0118 0.3738 0.4658 0.039 Uiso 1 1 calc R . . C4 C 0.1304(3) 0.3762(4) 0.46487(19) 0.0362(13) Uani 1 1 d . . . C5 C 0.1901(3) 0.3930(4) 0.43244(19) 0.0333(12) Uani 1 1 d . . . H5 H 0.2435 0.3874 0.446 0.04 Uiso 1 1 calc R . . C6 C 0.1747(3) 0.4178(4) 0.38041(18) 0.0270(11) Uani 1 1 d . . . C7 C -0.0526(3) 0.4059(5) 0.37345(19) 0.0337(12) Uani 1 1 d . . . H7A H -0.0841 0.3753 0.4004 0.051 Uiso 1 1 calc R . . H7B H -0.0611 0.3569 0.3428 0.051 Uiso 1 1 calc R . . H7C H -0.0688 0.4869 0.3652 0.051 Uiso 1 1 calc R . . C8 C 0.1483(4) 0.3513(5) 0.5217(2) 0.0517(16) Uani 1 1 d . . . H8A H 0.1228 0.4111 0.5418 0.078 Uiso 1 1 calc R . . H8B H 0.2056 0.3535 0.5301 0.078 Uiso 1 1 calc R . . H8C H 0.128 0.2734 0.5299 0.078 Uiso 1 1 calc R . . C9 C 0.2450(3) 0.4430(5) 0.3498(2) 0.0397(13) Uani 1 1 d . . . H9A H 0.2939 0.424 0.3705 0.06 Uiso 1 1 calc R . . H9B H 0.2452 0.5264 0.3405 0.06 Uiso 1 1 calc R . . H9C H 0.2415 0.3949 0.3187 0.06 Uiso 1 1 calc R . . C10 C 0.0850(3) 0.7320(4) 0.30961(18) 0.0248(11) Uani 1 1 d . . . C11 C 0.0673(3) 0.7998(4) 0.35236(17) 0.0255(10) Uani 1 1 d . . . C12 C 0.1166(3) 0.8917(4) 0.36844(19) 0.0328(12) Uani 1 1 d . . . H12 H 0.1033 0.9374 0.3969 0.039 Uiso 1 1 calc R . . C13 C 0.1849(3) 0.9201(4) 0.34478(18) 0.0304(12) Uani 1 1 d . . . C14 C 0.2029(3) 0.8511(4) 0.30364(19) 0.0302(11) Uani 1 1 d . . . H14 H 0.2498 0.8676 0.2873 0.036 Uiso 1 1 calc R . . C15 C 0.1545(3) 0.7575(4) 0.28505(18) 0.0251(10) Uani 1 1 d . . . C16 C -0.0037(3) 0.7754(5) 0.3831(2) 0.0425(14) Uani 1 1 d . . . H16A H -0.0043 0.8318 0.4113 0.064 Uiso 1 1 calc R . . H16B H 0 0.6954 0.3969 0.064 Uiso 1 1 calc R . . H16C H -0.0524 0.7835 0.3608 0.064 Uiso 1 1 calc R . . C17 C 0.2366(3) 1.0203(5) 0.3635(2) 0.0450(14) Uani 1 1 d . . . H17A H 0.2047 1.0918 0.3652 0.067 Uiso 1 1 calc R . . H17B H 0.278 1.0328 0.3398 0.067 Uiso 1 1 calc R . . H17C H 0.2612 1.0019 0.3976 0.067 Uiso 1 1 calc R . . C18 C 0.1804(3) 0.6914(5) 0.23894(18) 0.0320(11) Uani 1 1 d . . . H18A H 0.179 0.6067 0.2456 0.048 Uiso 1 1 calc R . . H18B H 0.2344 0.7147 0.2325 0.048 Uiso 1 1 calc R . . H18C H 0.1447 0.71 0.2089 0.048 Uiso 1 1 calc R . . C19 C -0.0296(3) 0.1591(4) 0.19189(18) 0.0270(11) Uani 1 1 d . . . H19 H -0.042 0.1874 0.1561 0.032 Uiso 1 1 calc R . . C20 C -0.0906(3) 0.1723(4) 0.22273(19) 0.0280(12) Uani 1 1 d . . . H20 H -0.1393 0.2068 0.2048 0.034 Uiso 1 1 calc R . . C21 C -0.1067(3) 0.1000(5) 0.2695(2) 0.0378(13) Uani 1 1 d . . . H21A H -0.135 0.0275 0.258 0.045 Uiso 1 1 calc R . . H21B H -0.1422 0.1455 0.2904 0.045 Uiso 1 1 calc R . . C22 C -0.0335(3) 0.0655(5) 0.3033(2) 0.0388(13) Uani 1 1 d . . . H22A H -0.0496 0.0464 0.3379 0.047 Uiso 1 1 calc R . . H22B H -0.0107 -0.0066 0.2892 0.047 Uiso 1 1 calc R . . C31 C 0.6844(3) 0.1821(5) 0.5069(2) 0.0460(15) Uani 1 1 d . . . H31 H 0.6397 0.1343 0.5118 0.055 Uiso 1 1 calc R . . C32 C 0.7090(3) 0.1981(5) 0.4584(2) 0.0433(14) Uani 1 1 d . . . H32 H 0.6804 0.1634 0.4297 0.052 Uiso 1 1 calc R . . C33 C 0.7753(3) 0.2648(5) 0.4519(2) 0.0430(14) Uani 1 1 d . . . H33 H 0.7934 0.2741 0.4187 0.052 Uiso 1 1 calc R . . C41 C 0.9199(4) 0.0203(5) 0.4912(2) 0.0503(15) Uani 1 1 d . . . H41 H 0.8648 0.0344 0.4854 0.06 Uiso 1 1 calc R . . C42 C 0.9731(4) 0.0900(5) 0.4680(2) 0.0520(16) Uani 1 1 d . . . H42 H 0.9544 0.1516 0.4458 0.062 Uiso 1 1 calc R . . C43 C 1.0526(4) 0.0714(5) 0.4764(2) 0.0485(15) Uani 1 1 d . . . H43 H 1.089 0.1204 0.4605 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02489(15) 0.01834(14) 0.02319(15) 0 0.00094(10) 0 P1 0.0234(6) 0.0190(6) 0.0214(6) 0.0001(5) 0.0009(5) -0.0006(5) P2 0.0228(6) 0.0198(6) 0.0214(6) -0.0001(5) 0.0022(5) -0.0010(5) C1 0.027(2) 0.021(2) 0.022(2) -0.001(2) 0.004(2) 0.001(2) C2 0.036(3) 0.020(2) 0.022(3) 0.001(2) 0.003(2) -0.001(2) C3 0.047(3) 0.027(3) 0.026(3) 0.004(2) 0.010(2) -0.004(2) C4 0.059(4) 0.023(3) 0.026(3) -0.004(2) -0.004(3) -0.007(3) C5 0.034(3) 0.031(3) 0.033(3) -0.001(2) -0.014(2) -0.001(2) C6 0.032(3) 0.021(2) 0.027(3) -0.001(2) -0.001(2) 0.000(2) C7 0.034(3) 0.039(3) 0.029(3) 0.008(2) 0.010(2) -0.003(2) C8 0.084(5) 0.044(3) 0.024(3) 0.002(3) -0.012(3) -0.008(3) C9 0.026(3) 0.048(3) 0.044(3) 0.000(3) -0.004(2) 0.001(2) C10 0.027(3) 0.019(2) 0.027(3) 0.003(2) -0.004(2) -0.0001(19) C11 0.032(2) 0.022(2) 0.022(2) -0.003(2) 0.0008(19) 0.002(2) C12 0.041(3) 0.027(3) 0.028(3) -0.006(2) -0.008(2) 0.002(2) C13 0.039(3) 0.022(3) 0.028(3) 0.005(2) -0.012(2) -0.003(2) C14 0.024(3) 0.031(3) 0.034(3) 0.009(2) -0.005(2) -0.002(2) C15 0.028(3) 0.020(2) 0.027(3) 0.005(2) -0.002(2) -0.002(2) C16 0.048(3) 0.047(4) 0.034(3) -0.017(3) 0.015(3) -0.004(3) C17 0.050(3) 0.033(3) 0.049(3) 0.001(3) -0.015(3) -0.009(3) C18 0.028(2) 0.037(3) 0.031(3) -0.002(3) 0.008(2) -0.006(2) C19 0.031(3) 0.025(3) 0.023(3) -0.008(2) -0.008(2) 0.000(2) C20 0.020(2) 0.019(3) 0.042(3) 0.005(2) -0.016(2) -0.0067(19) C21 0.037(3) 0.033(3) 0.043(3) 0.004(3) -0.003(2) -0.010(2) C22 0.042(3) 0.034(3) 0.039(3) 0.005(3) -0.003(2) -0.013(3) C31 0.042(3) 0.037(3) 0.061(4) 0.014(3) 0.011(3) -0.003(3) C32 0.052(3) 0.034(3) 0.042(3) 0.001(3) -0.009(3) 0.010(3) C33 0.055(4) 0.038(3) 0.038(3) 0.010(3) 0.012(3) 0.006(3) C41 0.059(4) 0.038(3) 0.053(4) -0.018(3) -0.001(3) 0.003(3) C42 0.084(5) 0.031(3) 0.041(4) -0.007(3) 0.004(3) 0.007(3) C43 0.071(4) 0.029(3) 0.046(4) -0.011(3) 0.012(3) -0.002(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 Pt1 C20 2.253(4) . ? Pt1 C20 2.253(4) 2 ? Pt1 C19 2.304(4) . ? Pt1 C19 2.304(4) 2 ? Pt1 P1 2.3277(12) . ? Pt1 P1 2.3277(12) 2 ? P1 C1 1.863(5) . ? P1 P2 2.2237(17) . ? P2 C10 1.870(5) . ? P2 P2 2.214(2) 2 ? C1 C6 1.407(6) . ? C1 C2 1.421(6) . ? C2 C3 1.395(7) . ? C2 C7 1.512(6) . ? C3 C4 1.380(7) . ? C4 C5 1.382(7) . ? C4 C8 1.524(7) . ? C5 C6 1.397(7) . ? C6 C9 1.513(7) . ? C10 C11 1.411(6) . ? C10 C15 1.414(6) . ? C11 C12 1.384(7) . ? C11 C16 1.523(7) . ? C12 C13 1.392(7) . ? C13 C14 1.386(7) . ? C13 C17 1.498(7) . ? C14 C15 1.408(7) . ? C15 C18 1.517(7) . ? C19 C20 1.368(7) . ? C19 C22 1.508(6) 2 ? C20 C21 1.518(7) . ? C21 C22 1.521(7) . ? C22 C19 1.508(6) 2 ? C31 C33 1.372(8) 7_656 ? C31 C32 1.377(8) . ? C32 C33 1.379(8) . ? C33 C31 1.372(8) 7_656 ? C41 C42 1.378(8) . ? C41 C43 1.402(8) 5_756 ? C42 C43 1.365(8) . ? C43 C41 1.402(8) 5_756 ? 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 C20 Pt1 C20 93.8(2) . 2 ? C20 Pt1 C19 34.92(17) . . ? C20 Pt1 C19 79.50(16) 2 . ? C20 Pt1 C19 79.50(16) . 2 ? C20 Pt1 C19 34.92(17) 2 2 ? C19 Pt1 C19 85.7(2) . 2 ? C20 Pt1 P1 170.77(14) . . ? C20 Pt1 P1 88.55(12) 2 . ? C19 Pt1 P1 154.13(12) . . ? C19 Pt1 P1 97.61(12) 2 . ? C20 Pt1 P1 88.55(11) . 2 ? C20 Pt1 P1 170.77(14) 2 2 ? C19 Pt1 P1 97.61(12) . 2 ? C19 Pt1 P1 154.13(12) 2 2 ? P1 Pt1 P1 90.54(6) . 2 ? C1 P1 P2 98.82(15) . . ? C1 P1 Pt1 109.65(15) . . ? P2 P1 Pt1 107.55(6) . . ? C10 P2 P2 107.08(15) . 2 ? C10 P2 P1 104.03(15) . . ? P2 P2 P1 90.42(5) 2 . ? C6 C1 C2 118.7(4) . . ? C6 C1 P1 116.6(3) . . ? C2 C1 P1 124.6(3) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C7 117.9(4) . . ? C1 C2 C7 123.4(4) . . ? C4 C3 C2 123.1(5) . . ? C3 C4 C5 117.4(4) . . ? C3 C4 C8 120.9(5) . . ? C5 C4 C8 121.7(5) . . ? C4 C5 C6 122.4(5) . . ? C5 C6 C1 119.5(4) . . ? C5 C6 C9 117.3(4) . . ? C1 C6 C9 123.2(4) . . ? C11 C10 C15 118.9(4) . . ? C11 C10 P2 113.5(3) . . ? C15 C10 P2 127.6(4) . . ? C12 C11 C10 119.6(4) . . ? C12 C11 C16 117.4(4) . . ? C10 C11 C16 122.9(4) . . ? C11 C12 C13 122.9(5) . . ? C14 C13 C12 117.0(4) . . ? C14 C13 C17 121.8(5) . . ? C12 C13 C17 121.2(5) . . ? C13 C14 C15 122.7(5) . . ? C14 C15 C10 118.8(4) . . ? C14 C15 C18 117.0(4) . . ? C10 C15 C18 124.2(4) . . ? C20 C19 C22 126.3(5) . 2 ? C20 C19 Pt1 70.5(3) . . ? C22 C19 Pt1 110.2(3) 2 . ? C19 C20 C21 127.4(4) . . ? C19 C20 Pt1 74.6(3) . . ? C21 C20 Pt1 105.9(3) . . ? C20 C21 C22 115.0(4) . . ? C19 C22 C21 114.1(4) 2 . ? C33 C31 C32 119.9(5) 7_656 . ? C31 C32 C33 119.5(5) . . ? C31 C33 C32 120.5(5) 7_656 . ? C42 C41 C43 119.8(6) . 5_756 ? C43 C42 C41 120.7(6) . . ? C42 C43 C41 119.5(6) . 5_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 Pt1 P1 C1 44.7(8) . . . . ? C20 Pt1 P1 C1 -60.2(2) 2 . . . ? C19 Pt1 P1 C1 -122.1(3) . . . . ? C19 Pt1 P1 C1 -26.4(2) 2 . . . ? P1 Pt1 P1 C1 129.01(16) 2 . . . ? C20 Pt1 P1 P2 -61.7(7) . . . . ? C20 Pt1 P1 P2 -166.66(14) 2 . . . ? C19 Pt1 P1 P2 131.4(3) . . . . ? C19 Pt1 P1 P2 -132.84(13) 2 . . . ? P1 Pt1 P1 P2 22.53(4) 2 . . . ? C1 P1 P2 C10 78.9(2) . . . . ? Pt1 P1 P2 C10 -167.17(15) . . . . ? C1 P1 P2 P2 -173.39(15) . . . 2 ? Pt1 P1 P2 P2 -59.44(7) . . . 2 ? P2 P1 C1 C6 -120.0(3) . . . . ? Pt1 P1 C1 C6 127.7(3) . . . . ? P2 P1 C1 C2 58.9(4) . . . . ? Pt1 P1 C1 C2 -53.4(4) . . . . ? C6 C1 C2 C3 -0.3(7) . . . . ? P1 C1 C2 C3 -179.3(3) . . . . ? C6 C1 C2 C7 180.0(4) . . . . ? P1 C1 C2 C7 1.0(7) . . . . ? C1 C2 C3 C4 -1.7(7) . . . . ? C7 C2 C3 C4 178.1(5) . . . . ? C2 C3 C4 C5 1.4(7) . . . . ? C2 C3 C4 C8 -178.9(5) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C8 C4 C5 C6 -178.9(5) . . . . ? C4 C5 C6 C1 -2.7(7) . . . . ? C4 C5 C6 C9 175.7(5) . . . . ? C2 C1 C6 C5 2.4(7) . . . . ? P1 C1 C6 C5 -178.6(4) . . . . ? C2 C1 C6 C9 -175.9(5) . . . . ? P1 C1 C6 C9 3.2(6) . . . . ? P2 P2 C10 C11 137.9(3) 2 . . . ? P1 P2 C10 C11 -127.2(3) . . . . ? P2 P2 C10 C15 -42.0(4) 2 . . . ? P1 P2 C10 C15 52.9(4) . . . . ? C15 C10 C11 C12 1.9(7) . . . . ? P2 C10 C11 C12 -178.0(3) . . . . ? C15 C10 C11 C16 -176.8(4) . . . . ? P2 C10 C11 C16 3.3(6) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? C16 C11 C12 C13 177.6(5) . . . . ? C11 C12 C13 C14 -0.5(7) . . . . ? C11 C12 C13 C17 -180.0(4) . . . . ? C12 C13 C14 C15 1.4(7) . . . . ? C17 C13 C14 C15 -179.1(4) . . . . ? C13 C14 C15 C10 -0.7(7) . . . . ? C13 C14 C15 C18 178.5(4) . . . . ? C11 C10 C15 C14 -1.0(6) . . . . ? P2 C10 C15 C14 178.9(3) . . . . ? C11 C10 C15 C18 179.9(4) . . . . ? P2 C10 C15 C18 -0.3(7) . . . . ? C20 Pt1 C19 C20 112.5(3) 2 . . . ? C19 Pt1 C19 C20 77.8(3) 2 . . . ? P1 Pt1 C19 C20 176.4(2) . . . . ? P1 Pt1 C19 C20 -76.3(3) 2 . . . ? C20 Pt1 C19 C22 -122.6(5) . . . 2 ? C20 Pt1 C19 C22 -10.1(3) 2 . . 2 ? C19 Pt1 C19 C22 -44.8(3) 2 . . 2 ? P1 Pt1 C19 C22 53.7(5) . . . 2 ? P1 Pt1 C19 C22 161.0(3) 2 . . 2 ? C22 C19 C20 C21 2.8(8) 2 . . . ? Pt1 C19 C20 C21 -98.4(5) . . . . ? C22 C19 C20 Pt1 101.2(4) 2 . . . ? C20 Pt1 C20 C19 -65.5(3) 2 . . . ? C19 Pt1 C20 C19 -97.5(3) 2 . . . ? P1 Pt1 C20 C19 -170.0(6) . . . . ? P1 Pt1 C20 C19 105.5(3) 2 . . . ? C20 Pt1 C20 C21 59.7(3) 2 . . . ? C19 Pt1 C20 C21 125.2(4) . . . . ? C19 Pt1 C20 C21 27.7(3) 2 . . . ? P1 Pt1 C20 C21 -44.8(9) . . . . ? P1 Pt1 C20 C21 -129.3(3) 2 . . . ? C19 C20 C21 C22 38.8(7) . . . . ? Pt1 C20 C21 C22 -43.7(5) . . . . ? C20 C21 C22 C19 37.4(7) . . . 2 ? C33 C31 C32 C33 1.9(9) 7_656 . . . ? C31 C32 C33 C31 -1.9(9) . . . 7_656 ? C43 C41 C42 C43 -0.7(9) 5_756 . . . ? C41 C42 C43 C41 0.7(9) . . . 5_756 ? #============================================================================ data_x0383fin _database_code_depnum_ccdc_archive 'CCDC 713499' _audit_creation_date 2008-03-06T19:11:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C70 H88 O2 P6 Pt' _chemical_formula_weight 1342.31 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.502(5) _cell_length_b 22.115(5) _cell_length_c 21.960(5) _cell_angle_alpha 90.000 _cell_angle_beta 98.764(5) _cell_angle_gamma 90.000 _cell_volume 6481(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 7604 _cell_measurement_theta_min 2.5866 _cell_measurement_theta_max 30.3534 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_T_max 0.977 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0141703727 _diffrn_orient_matrix_ub_12 0.028574647 _diffrn_orient_matrix_ub_13 0.0133584132 _diffrn_orient_matrix_ub_21 0.0510186539 _diffrn_orient_matrix_ub_22 -0.0070715084 _diffrn_orient_matrix_ub_23 -0.0006063961 _diffrn_orient_matrix_ub_31 -0.0034581018 _diffrn_orient_matrix_ub_32 0.0128684204 _diffrn_orient_matrix_ub_33 -0.0298899578 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.1111 _diffrn_reflns_av_unetI/netI 0.1588 _diffrn_reflns_number 46497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.19 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 11400 _reflns_number_gt 6374 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET) (compiled Nov 29 2007,17:23:28) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. 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^)+(0.0341P)^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 11400 _refine_ls_number_parameters 728 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.867 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.523 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # 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 Pt Pt -1.7033 8.3905 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.35398(2) 0.231327(14) 0.592291(13) 0.02811(9) Uani 1 1 d . . . P1 P 0.40286(14) 0.16302(9) 0.67305(8) 0.0289(5) Uani 1 1 d . . . P2 P 0.56760(14) 0.16481(9) 0.70035(8) 0.0311(5) Uani 1 1 d . . . P3 P 0.57375(14) 0.26262(10) 0.71761(8) 0.0313(5) Uani 1 1 d . . . P4 P 0.50065(14) 0.28684(8) 0.62245(8) 0.0314(5) Uani 1 1 d . . . P5 P 0.22176(15) 0.17195(9) 0.54806(9) 0.0319(5) Uani 1 1 d . . . P6 P 0.28422(15) 0.30351(9) 0.52261(8) 0.0316(5) Uani 1 1 d . . . C1 C 0.4035(5) 0.0825(3) 0.6472(3) 0.0295(19) Uani 1 1 d . . . C2 C 0.4536(5) 0.0620(3) 0.5997(3) 0.0255(18) Uani 1 1 d . . . C3 C 0.4598(5) 0.0004(3) 0.5894(3) 0.0319(19) Uani 1 1 d . . . H3 H 0.4938 -0.0131 0.5571 0.038 Uiso 1 1 calc R . . C4 C 0.4183(5) -0.0425(4) 0.6244(4) 0.036(2) Uani 1 1 d . . . C5 C 0.3679(5) -0.0212(3) 0.6699(3) 0.035(2) Uani 1 1 d . . . H5 H 0.3371 -0.0497 0.6934 0.042 Uiso 1 1 calc R . . C6 C 0.3596(5) 0.0399(3) 0.6831(3) 0.0304(19) Uani 1 1 d . . . C7 C 0.5031(5) 0.1043(3) 0.5595(3) 0.035(2) Uani 1 1 d . . . H7A H 0.5239 0.0815 0.5253 0.053 Uiso 1 1 calc R . . H7B H 0.562 0.1229 0.584 0.053 Uiso 1 1 calc R . . H7C H 0.4556 0.136 0.5431 0.053 Uiso 1 1 calc R . . C8 C 0.4284(6) -0.1094(3) 0.6111(3) 0.051(2) Uani 1 1 d . . . H8A H 0.3806 -0.1205 0.5747 0.076 Uiso 1 1 calc R . . H8B H 0.4144 -0.1331 0.6466 0.076 Uiso 1 1 calc R . . H8C H 0.4967 -0.1179 0.6036 0.076 Uiso 1 1 calc R . . C9 C 0.3046(5) 0.0577(3) 0.7356(3) 0.040(2) Uani 1 1 d . . . H9A H 0.2516 0.0868 0.7207 0.061 Uiso 1 1 calc R . . H9B H 0.3519 0.0762 0.7687 0.061 Uiso 1 1 calc R . . H9C H 0.2748 0.0217 0.7514 0.061 Uiso 1 1 calc R . . C10 C 0.5748(5) 0.1237(3) 0.7755(3) 0.0274(18) Uani 1 1 d . . . C11 C 0.6286(6) 0.0683(4) 0.7760(3) 0.036(2) Uani 1 1 d . . . C12 C 0.6336(6) 0.0302(3) 0.8282(4) 0.045(2) Uani 1 1 d . . . H12 H 0.6722 -0.0059 0.8299 0.054 Uiso 1 1 calc R . . C13 C 0.5840(6) 0.0440(4) 0.8765(4) 0.047(2) Uani 1 1 d . . . C14 C 0.5317(6) 0.0978(4) 0.8747(3) 0.044(2) Uani 1 1 d . . . H14 H 0.4976 0.1074 0.9082 0.053 Uiso 1 1 calc R . . C15 C 0.5268(5) 0.1380(4) 0.8265(3) 0.035(2) Uani 1 1 d . . . C16 C 0.6831(6) 0.0480(3) 0.7246(3) 0.050(2) Uani 1 1 d . . . H16A H 0.7192 0.0103 0.7365 0.075 Uiso 1 1 calc R . . H16B H 0.7309 0.0792 0.7167 0.075 Uiso 1 1 calc R . . H16C H 0.6347 0.0411 0.6872 0.075 Uiso 1 1 calc R . . C17 C 0.5896(6) 0.0004(4) 0.9303(3) 0.066(3) Uani 1 1 d . . . H17A H 0.5845 0.023 0.9681 0.099 Uiso 1 1 calc R . . H17B H 0.6536 -0.0213 0.9351 0.099 Uiso 1 1 calc R . . H17C H 0.5343 -0.0286 0.9225 0.099 Uiso 1 1 calc R . . C18 C 0.4713(6) 0.1951(4) 0.8317(3) 0.046(2) Uani 1 1 d . . . H18A H 0.5184 0.229 0.8364 0.069 Uiso 1 1 calc R . . H18B H 0.4366 0.193 0.8677 0.069 Uiso 1 1 calc R . . H18C H 0.4221 0.2009 0.7945 0.069 Uiso 1 1 calc R . . C19 C 0.7029(5) 0.2876(3) 0.7115(3) 0.031(2) Uani 1 1 d . . . C20 C 0.7644(5) 0.2683(4) 0.6695(3) 0.0362(18) Uani 1 1 d . . . C21 C 0.8587(6) 0.2945(3) 0.6696(3) 0.040(2) Uani 1 1 d . . . H21 H 0.8994 0.2802 0.641 0.048 Uiso 1 1 calc R . . C22 C 0.8949(6) 0.3402(4) 0.7096(4) 0.044(2) Uani 1 1 d . . . C23 C 0.8323(6) 0.3593(3) 0.7493(3) 0.042(2) Uani 1 1 d . . . H23 H 0.855 0.3914 0.7768 0.05 Uiso 1 1 calc R . . C24 C 0.7385(6) 0.3353(3) 0.7522(3) 0.0329(19) Uani 1 1 d . . . C25 C 0.7348(5) 0.2203(3) 0.6208(3) 0.048(2) Uani 1 1 d . . . H25A H 0.7851 0.2185 0.5931 0.072 Uiso 1 1 calc R . . H25B H 0.6694 0.2304 0.5971 0.072 Uiso 1 1 calc R . . H25C H 0.7307 0.1809 0.6407 0.072 Uiso 1 1 calc R . . C26 C 0.9967(6) 0.3671(4) 0.7075(4) 0.066(3) Uani 1 1 d . . . H26A H 1.0004 0.4073 0.7265 0.1 Uiso 1 1 calc R . . H26B H 1.0079 0.3705 0.6646 0.1 Uiso 1 1 calc R . . H26C H 1.0483 0.341 0.7302 0.1 Uiso 1 1 calc R . . C27 C 0.6768(6) 0.3623(3) 0.7973(3) 0.051(2) Uani 1 1 d . . . H27A H 0.6154 0.38 0.7746 0.076 Uiso 1 1 calc R . . H27B H 0.7157 0.3939 0.8215 0.076 Uiso 1 1 calc R . . H27C H 0.6591 0.3306 0.8249 0.076 Uiso 1 1 calc R . . C28 C 0.4860(5) 0.3669(3) 0.6450(3) 0.0282(18) Uani 1 1 d . . . C29 C 0.5507(6) 0.4101(4) 0.6261(4) 0.045(2) Uani 1 1 d . . . C30 C 0.5498(6) 0.4694(4) 0.6483(4) 0.055(3) Uani 1 1 d . . . H30 H 0.5948 0.4982 0.6357 0.066 Uiso 1 1 calc R . . C31 C 0.4851(7) 0.4874(4) 0.6880(4) 0.051(2) Uani 1 1 d . . . C32 C 0.4217(7) 0.4447(4) 0.7055(4) 0.048(2) Uani 1 1 d . . . H32 H 0.3768 0.4566 0.7326 0.057 Uiso 1 1 calc R . . C33 C 0.4192(6) 0.3847(4) 0.6858(3) 0.034(2) Uani 1 1 d . . . C34 C 0.6238(6) 0.3929(4) 0.5833(4) 0.062(3) Uani 1 1 d . . . H34A H 0.6703 0.3622 0.6031 0.093 Uiso 1 1 calc R . . H34B H 0.6616 0.4287 0.5741 0.093 Uiso 1 1 calc R . . H34C H 0.587 0.3765 0.5449 0.093 Uiso 1 1 calc R . . C35 C 0.4870(7) 0.5533(4) 0.7098(5) 0.094(4) Uani 1 1 d . . . H35A H 0.4182 0.5677 0.7091 0.142 Uiso 1 1 calc R . . H35B H 0.5207 0.5784 0.6824 0.142 Uiso 1 1 calc R . . H35C H 0.5234 0.5559 0.7519 0.142 Uiso 1 1 calc R . . C36 C 0.3473(5) 0.3434(3) 0.7101(3) 0.043(2) Uani 1 1 d . . . H36A H 0.2995 0.3672 0.7294 0.064 Uiso 1 1 calc R . . H36B H 0.3841 0.3161 0.7406 0.064 Uiso 1 1 calc R . . H36C H 0.3111 0.3196 0.6761 0.064 Uiso 1 1 calc R . . C37 C 0.2397(5) 0.0969(3) 0.5153(3) 0.0312(19) Uani 1 1 d . . . C38 C 0.2852(5) 0.0926(4) 0.4634(3) 0.036(2) Uani 1 1 d . . . H38 H 0.309 0.1282 0.4463 0.043 Uiso 1 1 calc R . . C39 C 0.2967(5) 0.0380(4) 0.4359(3) 0.036(2) Uani 1 1 d . . . H39 H 0.3279 0.036 0.4 0.044 Uiso 1 1 calc R . . C40 C 0.2630(6) -0.0137(4) 0.4607(4) 0.047(2) Uani 1 1 d . . . H40 H 0.2707 -0.0517 0.4417 0.056 Uiso 1 1 calc R . . C41 C 0.2178(6) -0.0109(4) 0.5130(4) 0.042(2) Uani 1 1 d . . . H41 H 0.1951 -0.0468 0.5301 0.051 Uiso 1 1 calc R . . C42 C 0.2058(5) 0.0444(3) 0.5402(3) 0.0326(19) Uani 1 1 d . . . H42 H 0.1744 0.0465 0.576 0.039 Uiso 1 1 calc R . . C43 C 0.1243(5) 0.1628(3) 0.5952(3) 0.0303(18) Uani 1 1 d . . . C44 C 0.0345(6) 0.1327(3) 0.5738(4) 0.044(2) Uani 1 1 d . . . H44 H 0.0247 0.1151 0.5338 0.052 Uiso 1 1 calc R . . C45 C -0.0394(6) 0.1285(4) 0.6101(4) 0.049(2) Uani 1 1 d . . . H45 H -0.0994 0.1073 0.5952 0.059 Uiso 1 1 calc R . . C46 C -0.0278(7) 0.1543(4) 0.6677(4) 0.056(3) Uani 1 1 d . . . H46 H -0.0797 0.1512 0.6923 0.068 Uiso 1 1 calc R . . C47 C 0.0603(7) 0.1850(4) 0.6900(4) 0.051(2) Uani 1 1 d . . . H47 H 0.069 0.2033 0.7296 0.061 Uiso 1 1 calc R . . C48 C 0.1348(6) 0.1886(3) 0.6536(3) 0.040(2) Uani 1 1 d . . . H48 H 0.1952 0.2093 0.6689 0.048 Uiso 1 1 calc R . . C49 C 0.1546(5) 0.2119(3) 0.4798(3) 0.036(2) Uani 1 1 d . . . H49A H 0.1893 0.2055 0.4437 0.043 Uiso 1 1 calc R . . H49B H 0.0852 0.1964 0.4697 0.043 Uiso 1 1 calc R . . C50 C 0.1536(5) 0.2789(3) 0.4959(3) 0.033(2) Uani 1 1 d . . . H50A H 0.1121 0.2856 0.5288 0.04 Uiso 1 1 calc R . . H50B H 0.1245 0.3026 0.4593 0.04 Uiso 1 1 calc R . . C51 C 0.3372(5) 0.3023(3) 0.4514(3) 0.0337(19) Uani 1 1 d . . . C52 C 0.4199(5) 0.2689(4) 0.4465(3) 0.0390(19) Uani 1 1 d . . . H52 H 0.456 0.251 0.4826 0.047 Uiso 1 1 calc R . . C53 C 0.4530(6) 0.2600(4) 0.3907(3) 0.051(2) Uani 1 1 d . . . H53 H 0.5102 0.2355 0.3885 0.061 Uiso 1 1 calc R . . C54 C 0.4031(6) 0.2867(3) 0.3383(4) 0.046(2) Uani 1 1 d . . . H54 H 0.426 0.2809 0.2999 0.055 Uiso 1 1 calc R . . C55 C 0.3217(6) 0.3211(4) 0.3416(4) 0.054(2) Uani 1 1 d . . . H55 H 0.2864 0.3389 0.3053 0.064 Uiso 1 1 calc R . . C56 C 0.2895(6) 0.3306(4) 0.3974(3) 0.045(2) Uani 1 1 d . . . H56 H 0.2342 0.3567 0.3994 0.054 Uiso 1 1 calc R . . C57 C 0.2680(6) 0.3821(3) 0.5448(3) 0.035(2) Uani 1 1 d . . . C58 C 0.1971(6) 0.3963(4) 0.5819(3) 0.045(2) Uani 1 1 d . . . H58 H 0.155 0.3655 0.5937 0.055 Uiso 1 1 calc R . . C59 C 0.1872(7) 0.4547(5) 0.6018(4) 0.054(3) Uani 1 1 d . . . H59 H 0.1381 0.4638 0.6272 0.065 Uiso 1 1 calc R . . C60 C 0.2469(8) 0.4992(4) 0.5856(4) 0.059(3) Uani 1 1 d . . . H60 H 0.2384 0.5394 0.5992 0.071 Uiso 1 1 calc R . . C61 C 0.3198(7) 0.4872(4) 0.5497(4) 0.057(3) Uani 1 1 d . . . H61 H 0.3621 0.5187 0.5394 0.068 Uiso 1 1 calc R . . C62 C 0.3312(6) 0.4276(4) 0.5282(3) 0.044(2) Uani 1 1 d . . . H62 H 0.3807 0.4187 0.503 0.052 Uiso 1 1 calc R . . O1 O 0.4204(4) 0.3772(3) 0.9207(2) 0.0557(16) Uani 1 1 d . . . C101 C 0.4406(7) 0.4094(5) 0.8683(4) 0.073(3) Uani 1 1 d . . . H10A H 0.3785 0.4285 0.847 0.088 Uiso 1 1 calc R . . H10B H 0.4665 0.3815 0.8391 0.088 Uiso 1 1 calc R . . C102 C 0.5162(7) 0.4561(4) 0.8894(4) 0.067(3) Uani 1 1 d . . . H10C H 0.4959 0.4784 0.9241 0.101 Uiso 1 1 calc R . . H10D H 0.5215 0.4842 0.8555 0.101 Uiso 1 1 calc R . . H10E H 0.5813 0.4369 0.9025 0.101 Uiso 1 1 calc R . . C103 C 0.3467(7) 0.3325(4) 0.9042(4) 0.075(3) Uani 1 1 d . . . H10F H 0.3729 0.3014 0.8783 0.089 Uiso 1 1 calc R . . H10G H 0.2867 0.351 0.8798 0.089 Uiso 1 1 calc R . . C104 C 0.3182(8) 0.3034(5) 0.9602(5) 0.110(4) Uani 1 1 d . . . H10H H 0.3733 0.2777 0.9795 0.165 Uiso 1 1 calc R . . H10I H 0.2581 0.2786 0.9485 0.165 Uiso 1 1 calc R . . H10J H 0.3044 0.3347 0.9893 0.165 Uiso 1 1 calc R . . O2 O 0.2971(7) 0.1610(4) 0.9366(4) 0.130(3) Uani 1 1 d . . . C201 C 0.3090(10) 0.1490(6) 1.0039(5) 0.130(5) Uani 1 1 d . . . H20A H 0.2812 0.109 1.0124 0.155 Uiso 1 1 calc R . . H20B H 0.2753 0.1805 1.0253 0.155 Uiso 1 1 calc R . . C202 C 0.4248(9) 0.1506(6) 1.0246(6) 0.151(6) Uani 1 1 d . . . H20C H 0.4568 0.1206 1.0011 0.226 Uiso 1 1 calc R . . H20D H 0.4401 0.1413 1.0687 0.226 Uiso 1 1 calc R . . H20E H 0.4503 0.191 1.0171 0.226 Uiso 1 1 calc R . . C203 C 0.1855(10) 0.1672(8) 0.9133(6) 0.172(7) Uani 1 1 d . . . H20F H 0.1548 0.1984 0.9368 0.206 Uiso 1 1 calc R . . H20G H 0.1503 0.1283 0.9165 0.206 Uiso 1 1 calc R . . C204 C 0.1818(12) 0.1867(7) 0.8436(5) 0.188(7) Uani 1 1 d . . . H20H H 0.2171 0.2252 0.8417 0.282 Uiso 1 1 calc R . . H20I H 0.1118 0.1914 0.8243 0.282 Uiso 1 1 calc R . . H20J H 0.2141 0.1556 0.8216 0.282 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02812(15) 0.02637(17) 0.02701(14) -0.00068(17) -0.00485(11) -0.00081(18) P1 0.0290(12) 0.0278(14) 0.0278(11) -0.0017(9) -0.0030(10) -0.0026(9) P2 0.0280(12) 0.0347(14) 0.0280(11) -0.0017(9) -0.0040(10) 0.0003(10) P3 0.0287(11) 0.0344(13) 0.0291(10) -0.0046(10) -0.0014(9) 0.0004(11) P4 0.0280(11) 0.0318(15) 0.0320(11) -0.0002(9) -0.0032(10) -0.0016(9) P5 0.0317(13) 0.0321(14) 0.0291(11) 0.0009(9) -0.0048(10) -0.0018(10) P6 0.0296(12) 0.0305(14) 0.0314(11) 0.0022(9) -0.0060(10) 0.0009(10) C1 0.027(5) 0.025(5) 0.031(5) -0.003(4) -0.011(4) 0.000(4) C2 0.024(4) 0.021(5) 0.028(4) -0.003(3) -0.007(4) -0.003(3) C3 0.029(5) 0.036(6) 0.031(4) -0.008(4) 0.004(4) 0.005(4) C4 0.028(5) 0.037(6) 0.039(5) -0.001(4) -0.011(4) -0.003(4) C5 0.037(5) 0.030(6) 0.035(5) 0.001(4) -0.004(4) -0.006(4) C6 0.023(4) 0.030(5) 0.034(5) -0.003(4) -0.010(4) 0.002(4) C7 0.034(5) 0.038(5) 0.033(4) -0.005(4) 0.007(4) 0.001(4) C8 0.054(6) 0.037(6) 0.060(6) -0.007(4) 0.006(5) 0.002(4) C9 0.036(5) 0.040(6) 0.045(5) 0.008(4) 0.007(4) -0.008(4) C10 0.023(4) 0.023(5) 0.032(4) 0.000(3) -0.010(4) -0.005(4) C11 0.033(5) 0.039(6) 0.032(5) -0.009(4) -0.009(4) -0.009(4) C12 0.045(6) 0.031(6) 0.049(6) 0.005(4) -0.023(5) -0.002(4) C13 0.048(6) 0.057(7) 0.030(5) 0.009(4) -0.012(4) -0.022(5) C14 0.039(5) 0.060(7) 0.031(5) 0.001(4) -0.004(4) -0.015(5) C15 0.032(5) 0.045(6) 0.021(4) -0.006(4) -0.011(4) -0.007(4) C16 0.049(6) 0.041(6) 0.054(5) -0.007(4) -0.010(5) 0.019(4) C17 0.069(7) 0.084(8) 0.039(5) 0.019(5) -0.016(5) -0.015(6) C18 0.046(5) 0.054(6) 0.038(5) -0.010(4) 0.007(4) 0.010(5) C19 0.030(4) 0.038(6) 0.023(4) -0.003(3) -0.006(4) -0.001(3) C20 0.036(5) 0.034(5) 0.035(4) -0.003(4) -0.005(4) -0.007(5) C21 0.039(5) 0.039(6) 0.043(5) 0.001(4) 0.005(4) -0.002(4) C22 0.022(5) 0.044(6) 0.061(6) 0.006(5) -0.012(5) -0.003(4) C23 0.044(6) 0.032(6) 0.042(5) -0.001(4) -0.014(5) -0.010(4) C24 0.040(5) 0.019(5) 0.035(4) 0.004(4) -0.009(4) 0.000(4) C25 0.036(5) 0.054(7) 0.054(5) -0.012(4) 0.007(4) 0.005(4) C26 0.045(6) 0.066(7) 0.084(7) 0.010(5) -0.004(5) -0.022(5) C27 0.066(6) 0.046(6) 0.039(5) -0.017(4) 0.003(5) -0.019(5) C28 0.019(4) 0.027(5) 0.033(4) 0.001(4) -0.013(4) -0.001(4) C29 0.040(6) 0.043(7) 0.046(5) 0.014(4) -0.013(5) -0.003(5) C30 0.047(6) 0.037(7) 0.071(7) 0.011(5) -0.022(5) -0.018(5) C31 0.047(6) 0.035(7) 0.063(6) -0.007(5) -0.020(5) 0.007(5) C32 0.057(6) 0.034(6) 0.047(5) -0.006(4) -0.010(5) 0.013(5) C33 0.037(5) 0.034(6) 0.026(4) -0.004(4) -0.008(4) 0.002(4) C34 0.054(6) 0.057(7) 0.074(7) 0.022(5) 0.007(6) -0.015(5) C35 0.102(9) 0.040(7) 0.127(9) -0.021(6) -0.026(8) 0.009(6) C36 0.043(5) 0.050(6) 0.034(5) -0.007(4) 0.002(4) 0.019(4) C37 0.029(5) 0.034(6) 0.029(4) -0.003(4) -0.002(4) -0.002(4) C38 0.031(5) 0.040(6) 0.035(5) -0.009(4) -0.001(4) -0.006(4) C39 0.037(5) 0.042(6) 0.029(4) -0.004(4) 0.000(4) 0.007(4) C40 0.046(6) 0.035(6) 0.050(6) -0.015(4) -0.018(5) 0.006(4) C41 0.041(5) 0.031(6) 0.049(5) 0.003(4) -0.014(5) 0.000(4) C42 0.028(5) 0.035(6) 0.035(5) -0.009(4) 0.004(4) 0.003(4) C43 0.034(5) 0.023(5) 0.030(4) -0.002(3) -0.005(4) 0.007(4) C44 0.038(5) 0.044(6) 0.045(5) -0.005(4) -0.004(5) -0.011(4) C45 0.031(5) 0.053(7) 0.064(6) -0.003(5) 0.007(5) -0.009(4) C46 0.050(6) 0.065(7) 0.057(6) 0.012(5) 0.015(5) 0.017(5) C47 0.053(6) 0.065(7) 0.034(5) 0.004(4) 0.008(5) 0.018(5) C48 0.039(5) 0.037(6) 0.043(5) -0.005(4) 0.004(4) 0.012(4) C49 0.033(5) 0.034(6) 0.035(4) 0.014(3) -0.009(4) 0.001(4) C50 0.025(4) 0.048(7) 0.025(4) 0.010(4) -0.001(3) 0.004(4) C51 0.034(5) 0.027(5) 0.037(5) -0.003(4) -0.003(4) -0.003(4) C52 0.048(5) 0.033(5) 0.035(4) -0.001(4) 0.003(4) 0.012(5) C53 0.056(6) 0.053(6) 0.046(5) 0.001(4) 0.017(5) 0.027(5) C54 0.058(6) 0.049(7) 0.035(5) 0.000(4) 0.022(5) 0.006(5) C55 0.051(6) 0.077(7) 0.032(5) 0.021(5) 0.003(5) 0.013(5) C56 0.031(5) 0.062(7) 0.041(5) 0.017(4) -0.001(4) 0.010(4) C57 0.040(5) 0.019(5) 0.039(5) 0.001(4) -0.015(4) 0.005(4) C58 0.044(6) 0.047(7) 0.040(5) -0.010(4) -0.009(5) 0.012(5) C59 0.058(7) 0.056(8) 0.044(6) -0.004(5) -0.005(5) 0.016(6) C60 0.088(8) 0.040(7) 0.041(6) -0.014(5) -0.020(6) 0.023(6) C61 0.080(8) 0.038(7) 0.042(6) 0.013(4) -0.024(5) -0.006(5) C62 0.050(6) 0.035(6) 0.040(5) 0.001(4) -0.009(4) 0.007(5) O1 0.062(4) 0.057(5) 0.047(4) 0.004(3) 0.005(3) -0.004(3) C101 0.058(7) 0.100(9) 0.061(7) -0.011(6) 0.005(6) -0.023(6) C102 0.068(7) 0.070(8) 0.061(6) -0.004(5) 0.002(6) 0.004(6) C103 0.076(8) 0.067(8) 0.081(8) -0.007(6) 0.014(6) -0.014(6) C104 0.083(9) 0.138(11) 0.108(9) 0.062(8) 0.011(8) -0.025(8) O2 0.123(8) 0.161(9) 0.097(7) 0.013(6) -0.007(6) 0.001(6) C201 0.124(13) 0.187(15) 0.071(9) 0.011(9) -0.009(9) 0.012(11) C202 0.118(12) 0.176(16) 0.145(13) 0.033(10) -0.023(11) -0.013(11) C203 0.087(11) 0.29(2) 0.131(13) 0.005(13) -0.019(11) 0.037(12) C204 0.24(2) 0.257(19) 0.062(9) -0.006(10) 0.009(11) 0.032(15) #----------------------------------------------------------------------------# # 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 P5 2.308(2) . ? Pt1 P6 2.310(2) . ? Pt1 P4 2.338(2) . ? Pt1 P1 2.3465(19) . ? P1 C1 1.869(7) . ? P1 P2 2.214(3) . ? P2 C10 1.874(7) . ? P2 P3 2.195(3) . ? P3 C19 1.854(7) . ? P3 P4 2.236(3) . ? P4 C28 1.858(7) . ? P5 C43 1.806(7) . ? P5 C37 1.839(7) . ? P5 C49 1.854(6) . ? P6 C51 1.816(7) . ? P6 C57 1.827(8) . ? P6 C50 1.854(7) . ? C1 C2 1.402(9) . ? C1 C6 1.416(10) . ? C2 C3 1.385(9) . ? C2 C7 1.510(9) . ? C3 C4 1.392(10) . ? C4 C5 1.374(9) . ? C4 C8 1.519(10) . ? C5 C6 1.392(9) . ? C6 C9 1.515(9) . ? C10 C15 1.412(9) . ? C10 C11 1.424(9) . ? C11 C12 1.417(10) . ? C11 C16 1.506(9) . ? C12 C13 1.371(10) . ? C13 C14 1.381(11) . ? C13 C17 1.519(10) . ? C14 C15 1.378(10) . ? C15 C18 1.481(10) . ? C19 C20 1.398(9) . ? C19 C24 1.417(9) . ? C20 C21 1.398(9) . ? C20 C25 1.519(9) . ? C21 C22 1.378(10) . ? C22 C23 1.371(10) . ? C22 C26 1.505(10) . ? C23 C24 1.385(10) . ? C24 C27 1.511(9) . ? C28 C29 1.400(10) . ? C28 C33 1.420(9) . ? C29 C30 1.400(11) . ? C29 C34 1.511(10) . ? C30 C31 1.384(11) . ? C31 C32 1.367(11) . ? C31 C35 1.533(11) . ? C32 C33 1.394(10) . ? C33 C36 1.489(10) . ? C37 C38 1.379(9) . ? C37 C42 1.391(9) . ? C38 C39 1.367(9) . ? C39 C40 1.375(10) . ? C40 C41 1.381(10) . ? C41 C42 1.381(9) . ? C43 C48 1.390(9) . ? C43 C44 1.400(9) . ? C44 C45 1.372(9) . ? C45 C46 1.375(10) . ? C46 C47 1.392(11) . ? C47 C48 1.378(9) . ? C49 C50 1.524(9) . ? C51 C52 1.357(9) . ? C51 C56 1.407(9) . ? C52 C53 1.382(9) . ? C53 C54 1.374(10) . ? C54 C55 1.349(10) . ? C55 C56 1.377(10) . ? C57 C58 1.384(10) . ? C57 C62 1.403(10) . ? C58 C59 1.375(10) . ? C59 C60 1.355(12) . ? C60 C61 1.376(11) . ? C61 C62 1.415(10) . ? O1 C103 1.411(9) . ? O1 C101 1.414(9) . ? C101 C102 1.476(10) . ? C103 C104 1.488(11) . ? O2 C201 1.486(11) . ? O2 C203 1.522(13) . ? C201 C202 1.561(14) . ? C203 C204 1.585(15) . ? 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 P5 Pt1 P6 84.45(7) . . ? P5 Pt1 P4 170.18(7) . . ? P6 Pt1 P4 93.84(7) . . ? P5 Pt1 P1 93.57(7) . . ? P6 Pt1 P1 169.98(7) . . ? P4 Pt1 P1 89.74(7) . . ? C1 P1 P2 92.8(2) . . ? C1 P1 Pt1 113.4(2) . . ? P2 P1 Pt1 110.39(10) . . ? C10 P2 P3 109.3(2) . . ? C10 P2 P1 98.3(2) . . ? P3 P2 P1 94.27(10) . . ? C19 P3 P2 107.0(2) . . ? C19 P3 P4 98.5(2) . . ? P2 P3 P4 94.30(10) . . ? C28 P4 P3 91.6(2) . . ? C28 P4 Pt1 117.1(2) . . ? P3 P4 Pt1 111.91(10) . . ? C43 P5 C37 105.9(3) . . ? C43 P5 C49 102.0(3) . . ? C37 P5 C49 101.0(3) . . ? C43 P5 Pt1 114.0(2) . . ? C37 P5 Pt1 122.6(2) . . ? C49 P5 Pt1 108.7(2) . . ? C51 P6 C57 108.8(4) . . ? C51 P6 C50 101.8(3) . . ? C57 P6 C50 102.5(3) . . ? C51 P6 Pt1 112.7(3) . . ? C57 P6 Pt1 122.3(2) . . ? C50 P6 Pt1 106.2(2) . . ? C2 C1 C6 119.4(7) . . ? C2 C1 P1 124.0(6) . . ? C6 C1 P1 116.2(6) . . ? C3 C2 C1 119.2(6) . . ? C3 C2 C7 118.1(6) . . ? C1 C2 C7 122.8(7) . . ? C2 C3 C4 122.7(7) . . ? C5 C4 C3 117.0(8) . . ? C5 C4 C8 122.8(7) . . ? C3 C4 C8 120.2(7) . . ? C4 C5 C6 123.3(7) . . ? C5 C6 C1 118.4(7) . . ? C5 C6 C9 118.4(7) . . ? C1 C6 C9 123.2(7) . . ? C15 C10 C11 118.8(6) . . ? C15 C10 P2 128.4(6) . . ? C11 C10 P2 112.5(5) . . ? C12 C11 C10 118.6(7) . . ? C12 C11 C16 117.4(7) . . ? C10 C11 C16 123.9(7) . . ? C13 C12 C11 121.6(8) . . ? C12 C13 C14 118.6(7) . . ? C12 C13 C17 119.2(9) . . ? C14 C13 C17 122.2(9) . . ? C15 C14 C13 122.8(8) . . ? C14 C15 C10 119.4(8) . . ? C14 C15 C18 117.1(7) . . ? C10 C15 C18 123.5(7) . . ? C20 C19 C24 117.7(7) . . ? C20 C19 P3 128.0(5) . . ? C24 C19 P3 114.1(5) . . ? C21 C20 C19 120.4(7) . . ? C21 C20 C25 115.6(7) . . ? C19 C20 C25 124.0(6) . . ? C22 C21 C20 122.6(8) . . ? C23 C22 C21 116.1(7) . . ? C23 C22 C26 123.4(8) . . ? C21 C22 C26 120.5(8) . . ? C22 C23 C24 124.6(7) . . ? C23 C24 C19 118.8(7) . . ? C23 C24 C27 118.6(7) . . ? C19 C24 C27 122.7(7) . . ? C29 C28 C33 119.0(7) . . ? C29 C28 P4 118.3(6) . . ? C33 C28 P4 122.4(6) . . ? C28 C29 C30 119.7(8) . . ? C28 C29 C34 120.6(8) . . ? C30 C29 C34 119.6(8) . . ? C31 C30 C29 121.9(8) . . ? C32 C31 C30 117.4(9) . . ? C32 C31 C35 123.5(9) . . ? C30 C31 C35 119.2(9) . . ? C31 C32 C33 123.9(9) . . ? C32 C33 C28 118.0(7) . . ? C32 C33 C36 117.4(7) . . ? C28 C33 C36 124.5(7) . . ? C38 C37 C42 118.8(7) . . ? C38 C37 P5 119.2(6) . . ? C42 C37 P5 122.0(6) . . ? C39 C38 C37 121.4(7) . . ? C38 C39 C40 119.5(8) . . ? C39 C40 C41 120.4(8) . . ? C42 C41 C40 119.7(8) . . ? C41 C42 C37 120.1(8) . . ? C48 C43 C44 117.9(7) . . ? C48 C43 P5 120.1(6) . . ? C44 C43 P5 121.9(6) . . ? C45 C44 C43 120.3(7) . . ? C44 C45 C46 121.0(8) . . ? C45 C46 C47 119.8(8) . . ? C48 C47 C46 119.0(8) . . ? C47 C48 C43 121.9(8) . . ? C50 C49 P5 107.2(5) . . ? C49 C50 P6 108.5(5) . . ? C52 C51 C56 116.9(7) . . ? C52 C51 P6 120.8(6) . . ? C56 C51 P6 122.0(6) . . ? C51 C52 C53 121.9(7) . . ? C54 C53 C52 119.8(7) . . ? C55 C54 C53 119.9(7) . . ? C54 C55 C56 120.3(7) . . ? C55 C56 C51 121.1(7) . . ? C58 C57 C62 119.5(8) . . ? C58 C57 P6 119.6(6) . . ? C62 C57 P6 120.7(7) . . ? C59 C58 C57 120.7(8) . . ? C60 C59 C58 120.5(9) . . ? C59 C60 C61 121.1(9) . . ? C60 C61 C62 119.7(9) . . ? C57 C62 C61 118.6(8) . . ? C103 O1 C101 111.1(7) . . ? O1 C101 C102 107.9(7) . . ? O1 C103 C104 110.6(8) . . ? C201 O2 C203 107.6(10) . . ? O2 C201 C202 103.7(11) . . ? O2 C203 C204 103.5(11) . . ? #============================================================================ data_p-1 _database_code_depnum_ccdc_archive 'CCDC 713500' _audit_creation_date 2008-09-30T15:51:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C49 H65 N2 P4 Pt' _chemical_formula_weight 1001 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6057(2) _cell_length_b 11.8615(9) _cell_length_c 19.3947(11) _cell_angle_alpha 74.4470(10) _cell_angle_beta 75.845(7) _cell_angle_gamma 69.4700(10) _cell_volume 2375.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 14485 _cell_measurement_theta_min 2.5832 _cell_measurement_theta_max 32.4222 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.4 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1022 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.939 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.001835802 _diffrn_orient_matrix_ub_12 -0.0084821032 _diffrn_orient_matrix_ub_13 0.0356231781 _diffrn_orient_matrix_ub_21 0.0352272308 _diffrn_orient_matrix_ub_22 -0.0211986606 _diffrn_orient_matrix_ub_23 0.0104898934 _diffrn_orient_matrix_ub_31 0.0159434924 _diffrn_orient_matrix_ub_32 0.0478990628 _diffrn_orient_matrix_ub_33 0.0101305612 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_unetI/netI 0.071 _diffrn_reflns_number 32029 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 9585 _reflns_number_gt 7585 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^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 9585 _refine_ls_number_parameters 524 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0455 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.341 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # 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 Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.902264(12) 0.561832(11) 0.735734(8) 0.02063(4) Uani 1 1 d . . . P1 P 0.89981(7) 0.36749(7) 0.80094(5) 0.02059(19) Uani 1 1 d . . . P2 P 0.88950(7) 0.25993(6) 0.72659(5) 0.02038(19) Uani 1 1 d . . . P3 P 0.72607(7) 0.39542(6) 0.68056(5) 0.02016(19) Uani 1 1 d . . . P4 P 0.79683(7) 0.55659(7) 0.64870(5) 0.01977(19) Uani 1 1 d . . . N1 N 1.1019(2) 0.5510(2) 0.82222(16) 0.0300(7) Uani 1 1 d . A . N2 N 0.8426(2) 0.8402(2) 0.66205(15) 0.0256(6) Uani 1 1 d . . . C1 C 1.0552(3) 0.2631(2) 0.82240(18) 0.0232(7) Uani 1 1 d . . . C2 C 1.0560(3) 0.1886(3) 0.89287(18) 0.0246(8) Uani 1 1 d . . . C3 C 1.1656(3) 0.1005(3) 0.9108(2) 0.0339(9) Uani 1 1 d . . . H3 H 1.1647 0.0509 0.9583 0.041 Uiso 1 1 calc R . . C4 C 1.2759(3) 0.0823(3) 0.8622(2) 0.0356(9) Uani 1 1 d . . . C5 C 1.2755(3) 0.1578(3) 0.7941(2) 0.0319(9) Uani 1 1 d . . . H5 H 1.3515 0.1483 0.7607 0.038 Uiso 1 1 calc R . . C6 C 1.1679(3) 0.2473(3) 0.77245(19) 0.0239(8) Uani 1 1 d . . . C7 C 0.9390(3) 0.1981(3) 0.94982(19) 0.0376(9) Uani 1 1 d . . . H7A H 0.8815 0.1685 0.9352 0.056 Uiso 1 1 calc R . . H7B H 0.8986 0.2841 0.9545 0.056 Uiso 1 1 calc R . . H7C H 0.9614 0.148 0.9966 0.056 Uiso 1 1 calc R . . C8 C 1.3926(3) -0.0172(3) 0.8824(2) 0.0536(12) Uani 1 1 d . . . H8A H 1.3874 -0.097 0.8805 0.08 Uiso 1 1 calc R . . H8B H 1.4008 -0.018 0.9316 0.08 Uiso 1 1 calc R . . H8C H 1.4654 -0.0014 0.8482 0.08 Uiso 1 1 calc R . . C9 C 1.1786(3) 0.3192(3) 0.69593(19) 0.0322(9) Uani 1 1 d . . . H9A H 1.2664 0.2986 0.6728 0.048 Uiso 1 1 calc R . . H9B H 1.1461 0.4073 0.6963 0.048 Uiso 1 1 calc R . . H9C H 1.1303 0.2987 0.6688 0.048 Uiso 1 1 calc R . . C10 C 0.8359(3) 0.1364(2) 0.79500(17) 0.0220(7) Uani 1 1 d . . . C11 C 0.7180(3) 0.1482(3) 0.83843(18) 0.0257(8) Uani 1 1 d . . . C12 C 0.6923(3) 0.0437(3) 0.8841(2) 0.0373(9) Uani 1 1 d . . . H12 H 0.6131 0.0528 0.9144 0.045 Uiso 1 1 calc R . . C13 C 0.7774(4) -0.0718(3) 0.8868(2) 0.0451(11) Uani 1 1 d . . . C14 C 0.8937(3) -0.0813(3) 0.8457(2) 0.0405(10) Uani 1 1 d . . . H14 H 0.9544 -0.1601 0.8482 0.049 Uiso 1 1 calc R . . C15 C 0.9263(3) 0.0193(3) 0.80067(19) 0.0280(8) Uani 1 1 d . . . C16 C 0.6148(3) 0.2679(3) 0.83957(19) 0.0337(9) Uani 1 1 d . . . H16A H 0.6496 0.3327 0.8386 0.051 Uiso 1 1 calc R . . H16B H 0.5533 0.2597 0.8838 0.051 Uiso 1 1 calc R . . H16C H 0.5743 0.2894 0.797 0.051 Uiso 1 1 calc R . . C17 C 0.7441(4) -0.1841(4) 0.9350(3) 0.0782(16) Uani 1 1 d . . . H17A H 0.6533 -0.1634 0.9496 0.117 Uiso 1 1 calc R . . H17B H 0.7835 -0.2101 0.9783 0.117 Uiso 1 1 calc R . . H17C H 0.774 -0.251 0.9082 0.117 Uiso 1 1 calc R . . C18 C 1.0599(3) -0.0024(3) 0.7626(2) 0.0362(9) Uani 1 1 d . . . H18A H 1.109 0.0102 0.7928 0.054 Uiso 1 1 calc R . . H18B H 1.0629 0.0553 0.7159 0.054 Uiso 1 1 calc R . . H18C H 1.0945 -0.0868 0.7545 0.054 Uiso 1 1 calc R . . C19 C 0.7469(3) 0.3622(2) 0.58945(17) 0.0196(7) Uani 1 1 d . . . C20 C 0.6373(3) 0.3628(2) 0.56973(18) 0.0214(7) Uani 1 1 d . . . C21 C 0.6401(3) 0.3453(3) 0.50133(19) 0.0275(8) Uani 1 1 d . . . H21 H 0.5657 0.3443 0.4896 0.033 Uiso 1 1 calc R . . C22 C 0.7472(3) 0.3293(3) 0.44959(19) 0.0277(8) Uani 1 1 d . . . C23 C 0.8544(3) 0.3297(2) 0.46941(19) 0.0261(8) Uani 1 1 d . . . H23 H 0.9291 0.3188 0.4348 0.031 Uiso 1 1 calc R . . C24 C 0.8576(3) 0.3449(2) 0.53695(18) 0.0201(7) Uani 1 1 d . . . C25 C 0.5132(3) 0.3824(3) 0.62162(18) 0.0292(8) Uani 1 1 d . . . H25A H 0.4482 0.3837 0.597 0.044 Uiso 1 1 calc R . . H25B H 0.4909 0.4608 0.6369 0.044 Uiso 1 1 calc R . . H25C H 0.5208 0.3152 0.6643 0.044 Uiso 1 1 calc R . . C26 C 0.7487(3) 0.3136(3) 0.3753(2) 0.0437(10) Uani 1 1 d . . . H26A H 0.7686 0.3825 0.339 0.066 Uiso 1 1 calc R . . H26B H 0.6666 0.3115 0.372 0.066 Uiso 1 1 calc R . . H26C H 0.812 0.2364 0.3661 0.066 Uiso 1 1 calc R . . C27 C 0.9828(3) 0.3397(3) 0.54983(18) 0.0286(8) Uani 1 1 d . . . H27A H 1.0229 0.2574 0.5762 0.043 Uiso 1 1 calc R . . H27B H 0.971 0.4007 0.5785 0.043 Uiso 1 1 calc R . . H27C H 1.0358 0.3576 0.5031 0.043 Uiso 1 1 calc R . . C28 C 0.6437(3) 0.6798(2) 0.64613(17) 0.0194(7) Uani 1 1 d . . . C29 C 0.6101(3) 0.7358(2) 0.57669(17) 0.0190(7) Uani 1 1 d . . . C30 C 0.5039(3) 0.8382(2) 0.56995(18) 0.0231(7) Uani 1 1 d . . . H30 H 0.4817 0.8751 0.5232 0.028 Uiso 1 1 calc R . . C31 C 0.4307(3) 0.8877(3) 0.62841(19) 0.0251(8) Uani 1 1 d . . . C32 C 0.4602(3) 0.8278(3) 0.69670(19) 0.0267(8) Uani 1 1 d . . . H32 H 0.408 0.8582 0.738 0.032 Uiso 1 1 calc R . . C33 C 0.5643(3) 0.7243(2) 0.70673(18) 0.0221(7) Uani 1 1 d . . . C34 C 0.6832(3) 0.6895(3) 0.50925(17) 0.0262(8) Uani 1 1 d . . . H34A H 0.6372 0.7328 0.4688 0.039 Uiso 1 1 calc R . . H34B H 0.6959 0.6012 0.5171 0.039 Uiso 1 1 calc R . . H34C H 0.7643 0.7044 0.4977 0.039 Uiso 1 1 calc R . . C35 C 0.3190(3) 1.0007(3) 0.6191(2) 0.0386(9) Uani 1 1 d . . . H35A H 0.336 1.0549 0.5724 0.058 Uiso 1 1 calc R . . H35B H 0.3026 1.0443 0.6585 0.058 Uiso 1 1 calc R . . H35C H 0.246 0.9764 0.6202 0.058 Uiso 1 1 calc R . . C36 C 0.5844(3) 0.6642(3) 0.78332(18) 0.0329(8) Uani 1 1 d . . . H36A H 0.6535 0.6832 0.7934 0.049 Uiso 1 1 calc R . . H36B H 0.6044 0.575 0.7896 0.049 Uiso 1 1 calc R . . H36C H 0.5083 0.6952 0.817 0.049 Uiso 1 1 calc R . . C37 C 1.0252(3) 0.5566(2) 0.79263(19) 0.0234(8) Uani 1 1 d . . . C38 C 0.8665(3) 0.7394(3) 0.69074(18) 0.0245(8) Uani 1 1 d . . . C39 C 1.1991(3) 0.5295(3) 0.8637(2) 0.0440(11) Uani 1 1 d D . . C40 C 1.3299(7) 0.5124(7) 0.8006(4) 0.0581(12) Uani 0.529(4) 1 d P A 1 H40A H 1.4031 0.4835 0.8246 0.087 Uiso 0.529(4) 1 calc PR A 1 H40B H 1.3276 0.5915 0.7675 0.087 Uiso 0.529(4) 1 calc PR A 1 H40C H 1.3349 0.4522 0.773 0.087 Uiso 0.529(4) 1 calc PR A 1 C41 C 1.2210(8) 0.4115(8) 0.9120(5) 0.0581(12) Uani 0.529(4) 1 d P A 1 H41A H 1.2343 0.3479 0.8848 0.087 Uiso 0.529(4) 1 calc PR A 1 H41B H 1.1485 0.4118 0.9506 0.087 Uiso 0.529(4) 1 calc PR A 1 H41C H 1.2951 0.3942 0.9334 0.087 Uiso 0.529(4) 1 calc PR A 1 C42 C 1.1887(8) 0.6391(8) 0.8875(5) 0.0581(12) Uani 0.529(4) 1 d P A 1 H42A H 1.1147 0.6569 0.925 0.087 Uiso 0.529(4) 1 calc PR A 1 H42B H 1.1811 0.7086 0.8461 0.087 Uiso 0.529(4) 1 calc PR A 1 H42C H 1.2633 0.6258 0.9075 0.087 Uiso 0.529(4) 1 calc PR A 1 C40A C 1.2788(9) 0.4080(8) 0.8669(6) 0.0581(12) Uani 0.471(4) 1 d P A 2 H40D H 1.2288 0.3514 0.8806 0.087 Uiso 0.471(4) 1 calc PR A 2 H40E H 1.3326 0.3883 0.9031 0.087 Uiso 0.471(4) 1 calc PR A 2 H40F H 1.3305 0.3997 0.8192 0.087 Uiso 0.471(4) 1 calc PR A 2 C41A C 1.1165(7) 0.5248(8) 0.9470(5) 0.0581(12) Uani 0.471(4) 1 d PD A 2 H41D H 1.0764 0.4602 0.9585 0.087 Uiso 0.471(4) 1 calc PR A 2 H41E H 1.0524 0.6043 0.9497 0.087 Uiso 0.471(4) 1 calc PR A 2 H41F H 1.1719 0.5071 0.982 0.087 Uiso 0.471(4) 1 calc PR A 2 C42A C 1.2406(9) 0.6371(9) 0.8489(6) 0.0581(12) Uani 0.471(4) 1 d P A 2 H42D H 1.2936 0.6265 0.884 0.087 Uiso 0.471(4) 1 calc PR A 2 H42E H 1.168 0.7102 0.8532 0.087 Uiso 0.471(4) 1 calc PR A 2 H42F H 1.2884 0.6473 0.7997 0.087 Uiso 0.471(4) 1 calc PR A 2 C43 C 0.8054(3) 0.9673(3) 0.62334(19) 0.0273(8) Uani 1 1 d . . . C44 C 0.7701(3) 0.9671(3) 0.5532(2) 0.0461(11) Uani 1 1 d . . . H44A H 0.8423 0.918 0.5242 0.069 Uiso 1 1 calc R . . H44B H 0.7436 1.0516 0.5257 0.069 Uiso 1 1 calc R . . H44C H 0.7015 0.9316 0.5642 0.069 Uiso 1 1 calc R . . C45 C 0.6957(3) 1.0372(3) 0.6722(2) 0.0511(11) Uani 1 1 d . . . H45A H 0.6248 1.0065 0.6787 0.077 Uiso 1 1 calc R . . H45B H 0.6723 1.1249 0.6499 0.077 Uiso 1 1 calc R . . H45C H 0.7191 1.0255 0.7194 0.077 Uiso 1 1 calc R . . C46 C 0.9170(3) 1.0145(3) 0.6084(2) 0.0401(10) Uani 1 1 d . . . H46A H 0.9394 1.0118 0.6545 0.06 Uiso 1 1 calc R . . H46B H 0.8958 1.0993 0.5809 0.06 Uiso 1 1 calc R . . H46C H 0.9879 0.9626 0.5802 0.06 Uiso 1 1 calc R . . C100 C 0.5905(4) 0.3951(4) 0.9852(2) 0.0533(11) Uani 1 1 d D . . H100 H 0.6533 0.3218 0.9751 0.064 Uiso 1 1 calc R . . C101 C 0.6109(4) 0.5059(5) 0.9579(2) 0.0550(12) Uani 1 1 d D . . H101 H 0.6885 0.5099 0.9285 0.066 Uiso 1 1 calc R . . C102 C 0.4777(4) 0.3902(4) 1.0277(2) 0.0525(11) Uani 1 1 d D . . H102 H 0.4624 0.3132 1.047 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02141(7) 0.01646(6) 0.02466(8) -0.00105(5) -0.00921(5) -0.00522(5) P1 0.0207(5) 0.0175(4) 0.0223(5) 0.0000(3) -0.0076(4) -0.0046(3) P2 0.0206(5) 0.0172(4) 0.0217(5) -0.0004(3) -0.0048(4) -0.0057(3) P3 0.0192(4) 0.0182(4) 0.0227(5) -0.0018(3) -0.0053(4) -0.0056(3) P4 0.0201(5) 0.0169(4) 0.0224(5) -0.0011(3) -0.0068(4) -0.0057(3) N1 0.0307(18) 0.0230(14) 0.038(2) -0.0030(13) -0.0185(15) -0.0044(12) N2 0.0309(16) 0.0204(14) 0.0293(18) -0.0033(12) -0.0117(14) -0.0093(12) C1 0.0245(19) 0.0165(15) 0.030(2) -0.0021(14) -0.0107(16) -0.0060(13) C2 0.026(2) 0.0218(16) 0.028(2) -0.0023(15) -0.0099(16) -0.0083(15) C3 0.039(2) 0.0261(18) 0.036(2) 0.0045(16) -0.0206(19) -0.0074(16) C4 0.032(2) 0.0267(18) 0.053(3) -0.0077(18) -0.023(2) -0.0042(16) C5 0.0197(19) 0.0316(18) 0.045(3) -0.0115(17) -0.0069(17) -0.0053(15) C6 0.0193(19) 0.0217(16) 0.033(2) -0.0077(15) -0.0069(16) -0.0057(14) C7 0.044(2) 0.0333(19) 0.031(2) 0.0031(16) -0.0112(19) -0.0107(17) C8 0.040(2) 0.043(2) 0.075(4) -0.007(2) -0.032(2) 0.0022(19) C9 0.025(2) 0.0325(18) 0.034(2) -0.0048(16) 0.0008(17) -0.0087(15) C10 0.0245(19) 0.0191(15) 0.025(2) 0.0001(13) -0.0108(16) -0.0081(14) C11 0.028(2) 0.0282(17) 0.023(2) 0.0014(14) -0.0101(16) -0.0131(15) C12 0.033(2) 0.047(2) 0.034(2) 0.0038(18) -0.0096(18) -0.0212(18) C13 0.049(3) 0.037(2) 0.052(3) 0.0148(19) -0.022(2) -0.025(2) C14 0.044(2) 0.0234(17) 0.054(3) 0.0102(17) -0.026(2) -0.0106(17) C15 0.031(2) 0.0223(16) 0.034(2) 0.0016(15) -0.0172(17) -0.0096(15) C16 0.030(2) 0.041(2) 0.028(2) -0.0053(16) 0.0038(17) -0.0156(17) C17 0.083(3) 0.051(3) 0.098(4) 0.037(3) -0.033(3) -0.045(3) C18 0.033(2) 0.0220(17) 0.051(3) -0.0050(16) -0.0149(19) -0.0016(15) C19 0.0217(18) 0.0121(14) 0.024(2) -0.0010(13) -0.0067(15) -0.0042(13) C20 0.0219(19) 0.0154(15) 0.025(2) -0.0023(13) -0.0035(15) -0.0051(13) C21 0.028(2) 0.0254(17) 0.034(2) -0.0035(15) -0.0121(18) -0.0109(15) C22 0.031(2) 0.0223(16) 0.031(2) -0.0073(15) -0.0061(18) -0.0078(15) C23 0.0248(19) 0.0209(16) 0.029(2) -0.0068(14) 0.0024(16) -0.0066(14) C24 0.0187(18) 0.0129(14) 0.027(2) -0.0034(13) -0.0048(15) -0.0029(13) C25 0.0193(18) 0.0353(18) 0.034(2) -0.0081(16) -0.0051(16) -0.0075(15) C26 0.046(2) 0.054(2) 0.036(3) -0.021(2) -0.004(2) -0.0156(19) C27 0.0239(19) 0.0289(17) 0.030(2) -0.0047(15) 0.0016(16) -0.0095(15) C28 0.0215(18) 0.0167(14) 0.0214(19) -0.0005(13) -0.0052(15) -0.0089(13) C29 0.0179(17) 0.0182(15) 0.0213(19) -0.0007(13) -0.0067(15) -0.0061(13) C30 0.0240(19) 0.0235(16) 0.021(2) 0.0018(14) -0.0098(16) -0.0074(14) C31 0.0211(18) 0.0220(16) 0.031(2) -0.0039(15) -0.0093(16) -0.0036(14) C32 0.0237(19) 0.0274(17) 0.026(2) -0.0097(15) 0.0006(16) -0.0045(15) C33 0.0210(18) 0.0204(15) 0.024(2) -0.0025(14) -0.0060(15) -0.0057(14) C34 0.0248(19) 0.0312(17) 0.021(2) -0.0025(15) -0.0094(16) -0.0044(14) C35 0.037(2) 0.0313(19) 0.037(2) -0.0034(17) -0.0091(19) 0.0018(16) C36 0.032(2) 0.0372(19) 0.024(2) -0.0063(16) -0.0041(17) -0.0033(16) C37 0.0208(19) 0.0146(15) 0.032(2) 0.0003(14) -0.0066(16) -0.0036(13) C38 0.0230(19) 0.0233(17) 0.032(2) -0.0097(15) -0.0116(16) -0.0048(14) C39 0.056(3) 0.0255(18) 0.062(3) -0.0018(18) -0.047(2) -0.0061(17) C40 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C41 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C42 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C40A 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C41A 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C42A 0.049(3) 0.068(2) 0.065(4) -0.008(2) -0.037(2) -0.012(2) C43 0.033(2) 0.0150(15) 0.034(2) -0.0005(14) -0.0151(17) -0.0051(14) C44 0.066(3) 0.036(2) 0.044(3) 0.0109(18) -0.031(2) -0.0238(19) C45 0.047(2) 0.0246(19) 0.071(3) -0.0070(19) -0.005(2) -0.0034(17) C46 0.052(2) 0.0301(18) 0.046(3) -0.0007(17) -0.015(2) -0.0222(17) C100 0.043(3) 0.065(3) 0.047(3) -0.026(2) -0.022(2) 0.010(2) C101 0.032(3) 0.101(4) 0.027(3) -0.002(3) -0.007(2) -0.021(3) C102 0.063(3) 0.056(3) 0.049(3) 0.003(2) -0.033(3) -0.025(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C37 1.982(3) . ? Pt1 C38 1.987(3) . ? Pt1 P1 2.3193(7) . ? Pt1 P4 2.3388(8) . ? P1 C1 1.867(3) . ? P1 P2 2.2134(11) . ? P2 C10 1.868(3) . ? P2 P3 2.2132(11) . ? P3 C19 1.853(3) . ? P3 P4 2.2205(10) . ? P4 C28 1.866(3) . ? N1 C37 1.147(4) . ? N1 C39 1.455(4) . ? N2 C38 1.142(3) . ? N2 C43 1.455(4) . ? C1 C6 1.410(4) . ? C1 C2 1.415(4) . ? C2 C3 1.386(4) . ? C2 C7 1.517(4) . ? C3 C4 1.378(5) . ? C4 C5 1.381(5) . ? C4 C8 1.507(4) . ? C5 C6 1.397(4) . ? C6 C9 1.500(4) . ? C10 C11 1.402(4) . ? C10 C15 1.412(4) . ? C11 C12 1.396(4) . ? C11 C16 1.504(4) . ? C12 C13 1.377(5) . ? C13 C14 1.373(5) . ? C13 C17 1.521(4) . ? C14 C15 1.389(4) . ? C15 C18 1.508(4) . ? C19 C20 1.412(4) . ? C19 C24 1.420(4) . ? C20 C21 1.388(4) . ? C20 C25 1.524(4) . ? C21 C22 1.383(4) . ? C22 C23 1.391(4) . ? C22 C26 1.497(5) . ? C23 C24 1.381(4) . ? C24 C27 1.511(4) . ? C28 C33 1.404(4) . ? C28 C29 1.415(4) . ? C29 C30 1.398(4) . ? C29 C34 1.499(4) . ? C30 C31 1.374(4) . ? C31 C32 1.387(4) . ? C31 C35 1.508(4) . ? C32 C33 1.396(4) . ? C33 C36 1.501(4) . ? C39 C40A 1.407(9) . ? C39 C41 1.437(9) . ? C39 C42 1.450(9) . ? C39 C42A 1.453(10) . ? C39 C41A 1.663(9) . ? C39 C40 1.689(9) . ? C43 C45 1.515(5) . ? C43 C44 1.515(4) . ? C43 C46 1.521(4) . ? C100 C101 1.359(5) . ? C100 C102 1.377(5) . ? C101 C102 1.345(5) 2_667 ? C102 C101 1.345(5) 2_667 ? 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 C37 Pt1 C38 95.86(11) . . ? C37 Pt1 P1 89.05(8) . . ? C38 Pt1 P1 167.62(9) . . ? C37 Pt1 P4 167.09(9) . . ? C38 Pt1 P4 84.46(9) . . ? P1 Pt1 P4 93.29(3) . . ? C1 P1 P2 94.20(10) . . ? C1 P1 Pt1 114.01(9) . . ? P2 P1 Pt1 108.89(4) . . ? C10 P2 P3 108.21(10) . . ? C10 P2 P1 99.25(10) . . ? P3 P2 P1 97.32(4) . . ? C19 P3 P2 103.88(10) . . ? C19 P3 P4 99.06(9) . . ? P2 P3 P4 97.49(4) . . ? C28 P4 P3 98.12(8) . . ? C28 P4 Pt1 112.48(10) . . ? P3 P4 Pt1 111.80(4) . . ? C37 N1 C39 173.3(3) . . ? C38 N2 C43 175.9(3) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 P1 124.9(2) . . ? C2 C1 P1 116.2(2) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 C7 117.9(3) . . ? C1 C2 C7 122.3(3) . . ? C4 C3 C2 122.3(3) . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C8 121.0(3) . . ? C5 C4 C8 121.2(4) . . ? C4 C5 C6 122.8(3) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C9 117.6(3) . . ? C1 C6 C9 123.6(3) . . ? C11 C10 C15 118.7(3) . . ? C11 C10 P2 127.2(2) . . ? C15 C10 P2 114.1(2) . . ? C12 C11 C10 119.2(3) . . ? C12 C11 C16 116.7(3) . . ? C10 C11 C16 124.1(3) . . ? C13 C12 C11 122.5(3) . . ? C14 C13 C12 117.5(3) . . ? C14 C13 C17 121.5(3) . . ? C12 C13 C17 120.9(4) . . ? C13 C14 C15 122.8(3) . . ? C14 C15 C10 119.1(3) . . ? C14 C15 C18 117.4(3) . . ? C10 C15 C18 123.5(3) . . ? C20 C19 C24 117.8(3) . . ? C20 C19 P3 115.0(2) . . ? C24 C19 P3 127.0(2) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 C25 117.8(3) . . ? C19 C20 C25 122.0(3) . . ? C22 C21 C20 122.5(3) . . ? C21 C22 C23 116.9(3) . . ? C21 C22 C26 122.2(3) . . ? C23 C22 C26 121.0(3) . . ? C24 C23 C22 123.2(3) . . ? C23 C24 C19 119.4(3) . . ? C23 C24 C27 116.1(3) . . ? C19 C24 C27 124.4(3) . . ? C33 C28 C29 118.6(3) . . ? C33 C28 P4 125.0(2) . . ? C29 C28 P4 116.3(2) . . ? C30 C29 C28 119.2(3) . . ? C30 C29 C34 118.0(3) . . ? C28 C29 C34 122.8(3) . . ? C31 C30 C29 122.4(3) . . ? C30 C31 C32 117.8(3) . . ? C30 C31 C35 121.2(3) . . ? C32 C31 C35 121.0(3) . . ? C31 C32 C33 122.1(3) . . ? C32 C33 C28 119.6(3) . . ? C32 C33 C36 117.5(3) . . ? C28 C33 C36 122.9(3) . . ? N1 C37 Pt1 175.9(3) . . ? N2 C38 Pt1 175.9(3) . . ? C40A C39 C41 39.6(5) . . ? C40A C39 C42 138.5(5) . . ? C41 C39 C42 121.5(6) . . ? C40A C39 C42A 124.8(6) . . ? C41 C39 C42A 137.3(5) . . ? C42 C39 C42A 33.6(5) . . ? C40A C39 N1 109.8(4) . . ? C41 C39 N1 111.4(4) . . ? C42 C39 N1 111.7(4) . . ? C42A C39 N1 111.1(4) . . ? C40A C39 C41A 102.7(6) . . ? C42A C39 C41A 104.9(6) . . ? N1 C39 C41A 100.3(4) . . ? C41 C39 C40 103.3(5) . . ? C42 C39 C40 103.1(5) . . ? N1 C39 C40 103.3(4) . . ? N2 C43 C45 106.9(3) . . ? N2 C43 C44 107.1(2) . . ? C45 C43 C44 112.1(3) . . ? N2 C43 C46 107.5(2) . . ? C45 C43 C46 112.1(3) . . ? C44 C43 C46 111.0(3) . . ? C101 C100 C102 119.3(4) . . ? C102 C101 C100 120.6(4) 2_667 . ? C101 C102 C100 120.1(4) 2_667 . ? #============================================================================ data_x0299fin _database_code_depnum_ccdc_archive 'CCDC 713501' _audit_creation_date 2008-09-30T16:14:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C54 H76 N2 O P4 Pt' _chemical_formula_weight 1088.14 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1799(3) _cell_length_b 12.2375(3) _cell_length_c 19.2324(5) _cell_angle_alpha 85.943(2) _cell_angle_beta 72.943(2) _cell_angle_gamma 74.195(2) _cell_volume 2636.79(11) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.6288 _cell_measurement_theta_max 32.3127 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.945 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0233239185 _diffrn_orient_matrix_ub_12 0.0222529831 _diffrn_orient_matrix_ub_13 -0.0345110004 _diffrn_orient_matrix_ub_21 -0.0185445558 _diffrn_orient_matrix_ub_22 0.0551352165 _diffrn_orient_matrix_ub_23 0.0155194533 _diffrn_orient_matrix_ub_31 0.055692712 _diffrn_orient_matrix_ub_32 -0.0089780438 _diffrn_orient_matrix_ub_33 0.0070907096 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_unetI/netI 0.1238 _diffrn_reflns_number 44928 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 9985 _reflns_number_gt 6288 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^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 9985 _refine_ls_number_parameters 543 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.7 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # 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 Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.002407(17) 0.494299(16) 0.233421(11) 0.03258(7) Uani 1 1 d . . . P1 P -0.19953(10) 0.51385(9) 0.28961(6) 0.0300(3) Uani 1 1 d . . . P2 P -0.27859(10) 0.47137(9) 0.20861(6) 0.0299(3) Uani 1 1 d . . . P3 P -0.15161(10) 0.30314(9) 0.17711(6) 0.0308(3) Uani 1 1 d . . . P4 P 0.01179(10) 0.36338(9) 0.14812(6) 0.0298(3) Uani 1 1 d . . . N1 N -0.0182(3) 0.6997(3) 0.3288(2) 0.0369(10) Uani 1 1 d . . . N2 N 0.2777(4) 0.4298(3) 0.1673(2) 0.0443(11) Uani 1 1 d . . . O1 O 0.8156(3) 0.2769(3) 0.55193(16) 0.0432(8) Uani 1 1 d . . . C1 C -0.2829(4) 0.6673(3) 0.3005(2) 0.0290(11) Uani 1 1 d . . . C2 C -0.2694(4) 0.7493(4) 0.2461(2) 0.0327(11) Uani 1 1 d . . . C3 C -0.3365(4) 0.8618(4) 0.2624(3) 0.0408(13) Uani 1 1 d . . . H3 H -0.3272 0.917 0.2254 0.049 Uiso 1 1 calc R . . C4 C -0.4151(4) 0.8961(4) 0.3293(3) 0.0458(13) Uani 1 1 d . . . C5 C -0.4291(4) 0.8138(4) 0.3821(3) 0.0436(13) Uani 1 1 d . . . H5 H -0.4833 0.8353 0.4288 0.052 Uiso 1 1 calc R . . C6 C -0.3659(4) 0.7005(4) 0.3685(2) 0.0321(11) Uani 1 1 d . . . C7 C -0.1874(4) 0.7234(4) 0.1717(2) 0.0441(13) Uani 1 1 d . . . H7A H -0.1811 0.7945 0.146 0.066 Uiso 1 1 calc R . . H7B H -0.2185 0.679 0.1452 0.066 Uiso 1 1 calc R . . H7C H -0.1086 0.6795 0.1746 0.066 Uiso 1 1 calc R . . C8 C -0.4854(5) 1.0190(4) 0.3440(3) 0.0747(18) Uani 1 1 d . . . H8A H -0.4366 1.0685 0.317 0.112 Uiso 1 1 calc R . . H8B H -0.5077 1.0354 0.3962 0.112 Uiso 1 1 calc R . . H8C H -0.5576 1.0327 0.3282 0.112 Uiso 1 1 calc R . . C9 C -0.3890(4) 0.6180(4) 0.4291(2) 0.0483(13) Uani 1 1 d . . . H9A H -0.3162 0.5856 0.4436 0.072 Uiso 1 1 calc R . . H9B H -0.4135 0.5569 0.4124 0.072 Uiso 1 1 calc R . . H9C H -0.4525 0.6575 0.4707 0.072 Uiso 1 1 calc R . . C10 C -0.4178(4) 0.4446(3) 0.2688(2) 0.0278(11) Uani 1 1 d . . . C11 C -0.5217(4) 0.5207(3) 0.2588(2) 0.0327(12) Uani 1 1 d . . . C12 C -0.6324(4) 0.5055(4) 0.2969(2) 0.0369(12) Uani 1 1 d . . . H12 H -0.7017 0.5576 0.2895 0.044 Uiso 1 1 calc R . . C13 C -0.6459(4) 0.4185(4) 0.3447(2) 0.0358(12) Uani 1 1 d . . . C14 C -0.5442(4) 0.3466(4) 0.3568(2) 0.0354(11) Uani 1 1 d . . . H14 H -0.5518 0.2873 0.3911 0.042 Uiso 1 1 calc R . . C15 C -0.4315(4) 0.3582(3) 0.3207(2) 0.0310(11) Uani 1 1 d . . . C16 C -0.5191(4) 0.6203(4) 0.2074(3) 0.0516(14) Uani 1 1 d . . . H16A H -0.4807 0.6714 0.2226 0.077 Uiso 1 1 calc R . . H16B H -0.6007 0.6616 0.2084 0.077 Uiso 1 1 calc R . . H16C H -0.4742 0.5924 0.1579 0.077 Uiso 1 1 calc R . . C17 C -0.7664(4) 0.3984(4) 0.3819(3) 0.0565(15) Uani 1 1 d . . . H17A H -0.829 0.4655 0.3765 0.085 Uiso 1 1 calc R . . H17B H -0.774 0.3843 0.4337 0.085 Uiso 1 1 calc R . . H17C H -0.7742 0.3324 0.3596 0.085 Uiso 1 1 calc R . . C18 C -0.3272(4) 0.2756(4) 0.3402(2) 0.0407(12) Uani 1 1 d . . . H18A H -0.3551 0.245 0.3887 0.061 Uiso 1 1 calc R . . H18B H -0.2672 0.3152 0.34 0.061 Uiso 1 1 calc R . . H18C H -0.2921 0.2133 0.3045 0.061 Uiso 1 1 calc R . . C19 C -0.1505(4) 0.2769(4) 0.0829(2) 0.0331(11) Uani 1 1 d . . . C20 C -0.1501(4) 0.3553(4) 0.0256(3) 0.0337(12) Uani 1 1 d . . . C21 C -0.1382(4) 0.3175(4) -0.0435(3) 0.0454(13) Uani 1 1 d . . . H21 H -0.1372 0.3707 -0.082 0.055 Uiso 1 1 calc R . . C22 C -0.1280(5) 0.2067(4) -0.0582(3) 0.0567(15) Uani 1 1 d . . . C23 C -0.1261(5) 0.1295(4) -0.0027(3) 0.0618(16) Uani 1 1 d . . . H23 H -0.1164 0.0519 -0.0126 0.074 Uiso 1 1 calc R . . C24 C -0.1383(4) 0.1622(4) 0.0680(3) 0.0470(13) Uani 1 1 d . . . C25 C -0.1598(4) 0.4795(3) 0.0332(2) 0.0352(11) Uani 1 1 d . . . H25A H -0.1315 0.5111 -0.0149 0.053 Uiso 1 1 calc R . . H25B H -0.1111 0.4884 0.0639 0.053 Uiso 1 1 calc R . . H25C H -0.2431 0.52 0.0557 0.053 Uiso 1 1 calc R . . C26 C -0.1163(5) 0.1714(5) -0.1350(3) 0.082(2) Uani 1 1 d . . . H26A H -0.1782 0.2239 -0.1531 0.124 Uiso 1 1 calc R . . H26B H -0.1253 0.0942 -0.1344 0.124 Uiso 1 1 calc R . . H26C H -0.0377 0.1735 -0.167 0.124 Uiso 1 1 calc R . . C27 C -0.1369(5) 0.0713(4) 0.1257(3) 0.0699(17) Uani 1 1 d . . . H27A H -0.1257 -0.0023 0.1038 0.105 Uiso 1 1 calc R . . H27B H -0.2127 0.09 0.1642 0.105 Uiso 1 1 calc R . . H27C H -0.0715 0.0673 0.1465 0.105 Uiso 1 1 calc R . . C28 C 0.1186(4) 0.2243(3) 0.1553(2) 0.0299(11) Uani 1 1 d . . . C29 C 0.1913(4) 0.1691(4) 0.0892(2) 0.0335(11) Uani 1 1 d . . . C30 C 0.2802(4) 0.0698(4) 0.0901(3) 0.0471(13) Uani 1 1 d . . . H30 H 0.3287 0.0334 0.0453 0.057 Uiso 1 1 calc R . . C31 C 0.2999(4) 0.0225(4) 0.1544(3) 0.0450(13) Uani 1 1 d . . . C32 C 0.2246(4) 0.0742(4) 0.2186(3) 0.0428(13) Uani 1 1 d . . . H32 H 0.2345 0.0407 0.2632 0.051 Uiso 1 1 calc R . . C33 C 0.1346(4) 0.1734(4) 0.2208(2) 0.0336(11) Uani 1 1 d . . . C34 C 0.1773(4) 0.2111(4) 0.0158(2) 0.0414(13) Uani 1 1 d . . . H34A H 0.2482 0.173 -0.0224 0.062 Uiso 1 1 calc R . . H34B H 0.1677 0.2933 0.0132 0.062 Uiso 1 1 calc R . . H34C H 0.1069 0.1943 0.0089 0.062 Uiso 1 1 calc R . . C35 C 0.4020(4) -0.0826(4) 0.1533(3) 0.0687(17) Uani 1 1 d . . . H35A H 0.4386 -0.0756 0.1913 0.103 Uiso 1 1 calc R . . H35B H 0.4617 -0.0898 0.1057 0.103 Uiso 1 1 calc R . . H35C H 0.3714 -0.1501 0.1622 0.103 Uiso 1 1 calc R . . C36 C 0.0568(4) 0.2218(4) 0.2938(2) 0.0444(13) Uani 1 1 d . . . H36A H 0.0737 0.1678 0.3319 0.067 Uiso 1 1 calc R . . H36B H -0.027 0.236 0.2953 0.067 Uiso 1 1 calc R . . H36C H 0.0729 0.2934 0.302 0.067 Uiso 1 1 calc R . . C37 C -0.0100(4) 0.6248(4) 0.2937(3) 0.0369(13) Uani 1 1 d . . . C38 C 0.1777(5) 0.4549(4) 0.1931(3) 0.0406(13) Uani 1 1 d . . . C39 C -0.0427(4) 0.7944(3) 0.3768(2) 0.0354(12) Uani 1 1 d U . . H39 H 0.028 0.7886 0.3946 0.043 Uiso 1 1 calc R . . C40 C -0.1492(4) 0.7892(4) 0.4411(3) 0.0515(14) Uani 1 1 d U . . H40A H -0.2187 0.7918 0.4237 0.062 Uiso 1 1 calc R . . H40B H -0.1309 0.7171 0.4674 0.062 Uiso 1 1 calc R . . C41 C -0.1781(5) 0.8889(5) 0.4918(3) 0.0818(19) Uani 1 1 d U . . H41A H -0.1099 0.8842 0.511 0.098 Uiso 1 1 calc R . . H41B H -0.2481 0.8865 0.5335 0.098 Uiso 1 1 calc R . . C42 C -0.2046(6) 1.0001(5) 0.4513(4) 0.096(2) Uani 1 1 d U . . H42A H -0.2756 1.0067 0.4345 0.115 Uiso 1 1 calc R . . H42B H -0.222 1.0648 0.4844 0.115 Uiso 1 1 calc R . . C43 C -0.1002(6) 1.0044(4) 0.3870(4) 0.0782(19) Uani 1 1 d U . . H43A H -0.0309 1.0035 0.4042 0.094 Uiso 1 1 calc R . . H43B H -0.1196 1.0762 0.3606 0.094 Uiso 1 1 calc R . . C44 C -0.0678(5) 0.9043(4) 0.3354(3) 0.0550(14) Uani 1 1 d U . . H44A H -0.1344 0.9082 0.3148 0.066 Uiso 1 1 calc R . . H44B H 0.0034 0.9072 0.2948 0.066 Uiso 1 1 calc R . . C45 C 0.4017(5) 0.3805(6) 0.1313(3) 0.0899(9) Uani 1 1 d . . . H45 H 0.4511 0.4287 0.1398 0.108 Uiso 1 1 calc R . . C46 C 0.4346(5) 0.2610(5) 0.1661(3) 0.0899(9) Uani 1 1 d . . . H46A H 0.4312 0.2711 0.2173 0.108 Uiso 1 1 calc R . . H46B H 0.3748 0.2203 0.1659 0.108 Uiso 1 1 calc R . . C47 C 0.5518(5) 0.1926(5) 0.1281(3) 0.0899(9) Uani 1 1 d . . . H47A H 0.565 0.1154 0.1488 0.108 Uiso 1 1 calc R . . H47B H 0.6132 0.2269 0.1343 0.108 Uiso 1 1 calc R . . C48 C 0.5625(5) 0.1855(5) 0.0475(3) 0.0899(9) Uani 1 1 d . . . H48A H 0.6439 0.1411 0.0217 0.108 Uiso 1 1 calc R . . H48B H 0.5057 0.1451 0.0415 0.108 Uiso 1 1 calc R . . C49 C 0.5381(5) 0.2998(5) 0.0145(3) 0.0899(9) Uani 1 1 d . . . H49A H 0.5976 0.3386 0.0183 0.108 Uiso 1 1 calc R . . H49B H 0.5468 0.2911 -0.0378 0.108 Uiso 1 1 calc R . . C50 C 0.4189(5) 0.3699(5) 0.0495(3) 0.0899(9) Uani 1 1 d . . . H50A H 0.3587 0.3353 0.0419 0.108 Uiso 1 1 calc R . . H50B H 0.4077 0.4463 0.0275 0.108 Uiso 1 1 calc R . . C51 C 0.7062(4) 0.2521(4) 0.5868(3) 0.0457(13) Uani 1 1 d . . . H51A H 0.6762 0.2241 0.5508 0.055 Uiso 1 1 calc R . . H51B H 0.6465 0.3214 0.6104 0.055 Uiso 1 1 calc R . . C52 C 0.7260(4) 0.1628(4) 0.6427(3) 0.0643(16) Uani 1 1 d . . . H52A H 0.7835 0.0938 0.6187 0.096 Uiso 1 1 calc R . . H52B H 0.6504 0.1456 0.6684 0.096 Uiso 1 1 calc R . . H52C H 0.757 0.1907 0.6776 0.096 Uiso 1 1 calc R . . C53 C 0.8055(5) 0.3581(4) 0.4961(3) 0.0517(15) Uani 1 1 d . . . H53A H 0.7433 0.4281 0.5163 0.062 Uiso 1 1 calc R . . H53B H 0.7826 0.3272 0.4577 0.062 Uiso 1 1 calc R . . C54 C 0.9242(4) 0.3847(4) 0.4642(3) 0.0577(15) Uani 1 1 d . . . H54A H 0.9449 0.4176 0.5021 0.087 Uiso 1 1 calc R . . H54B H 0.9192 0.4391 0.4246 0.087 Uiso 1 1 calc R . . H54C H 0.9856 0.3147 0.4452 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03441(12) 0.02934(10) 0.03570(12) 0.00181(8) -0.01311(9) -0.00820(8) P1 0.0350(8) 0.0256(6) 0.0298(8) 0.0006(6) -0.0120(6) -0.0056(6) P2 0.0343(8) 0.0280(7) 0.0289(7) 0.0051(6) -0.0108(6) -0.0099(6) P3 0.0385(8) 0.0279(7) 0.0270(7) 0.0027(6) -0.0078(6) -0.0126(6) P4 0.0328(7) 0.0260(7) 0.0296(8) 0.0025(6) -0.0094(6) -0.0058(6) N1 0.039(3) 0.034(2) 0.044(3) 0.005(2) -0.018(2) -0.013(2) N2 0.049(3) 0.042(3) 0.043(3) -0.009(2) -0.019(3) -0.006(2) O1 0.045(2) 0.051(2) 0.035(2) 0.0081(17) -0.0167(17) -0.0114(17) C1 0.025(3) 0.032(3) 0.030(3) -0.001(2) -0.011(2) -0.005(2) C2 0.035(3) 0.032(3) 0.035(3) 0.005(2) -0.015(2) -0.009(2) C3 0.035(3) 0.028(3) 0.064(4) 0.009(3) -0.021(3) -0.010(2) C4 0.036(3) 0.033(3) 0.066(4) -0.005(3) -0.016(3) -0.002(2) C5 0.036(3) 0.038(3) 0.050(4) -0.010(3) -0.012(3) 0.001(2) C6 0.028(3) 0.035(3) 0.037(3) -0.005(2) -0.015(2) -0.007(2) C7 0.053(3) 0.036(3) 0.040(3) 0.011(2) -0.010(3) -0.013(2) C8 0.069(4) 0.030(3) 0.112(5) -0.010(3) -0.022(4) 0.008(3) C9 0.041(3) 0.053(3) 0.039(3) -0.002(3) 0.001(3) -0.005(3) C10 0.034(3) 0.027(3) 0.024(3) -0.003(2) -0.011(2) -0.008(2) C11 0.040(3) 0.027(3) 0.032(3) -0.002(2) -0.007(2) -0.013(3) C12 0.032(3) 0.040(3) 0.034(3) -0.007(2) -0.005(2) -0.004(2) C13 0.030(3) 0.051(3) 0.023(3) -0.011(2) 0.003(2) -0.015(3) C14 0.041(3) 0.042(3) 0.025(3) 0.001(2) -0.007(2) -0.017(3) C15 0.041(3) 0.029(3) 0.027(3) -0.002(2) -0.012(2) -0.014(2) C16 0.041(3) 0.045(3) 0.065(4) 0.017(3) -0.017(3) -0.008(3) C17 0.044(3) 0.070(4) 0.047(4) -0.007(3) 0.002(3) -0.016(3) C18 0.054(3) 0.041(3) 0.032(3) 0.015(2) -0.015(3) -0.020(3) C19 0.043(3) 0.034(3) 0.026(3) 0.000(2) -0.006(2) -0.020(2) C20 0.037(3) 0.039(3) 0.030(3) 0.002(2) -0.010(2) -0.018(2) C21 0.058(4) 0.058(4) 0.030(3) 0.011(3) -0.017(3) -0.029(3) C22 0.094(4) 0.051(3) 0.037(4) -0.001(3) -0.020(3) -0.036(3) C23 0.109(5) 0.043(3) 0.046(4) 0.001(3) -0.020(3) -0.042(3) C24 0.071(4) 0.038(3) 0.037(3) 0.006(3) -0.012(3) -0.028(3) C25 0.043(3) 0.038(3) 0.027(3) 0.009(2) -0.010(2) -0.018(2) C26 0.142(6) 0.086(5) 0.038(4) -0.002(3) -0.028(4) -0.057(4) C27 0.137(5) 0.030(3) 0.048(4) 0.005(3) -0.020(4) -0.038(3) C28 0.032(3) 0.022(2) 0.033(3) 0.004(2) -0.008(2) -0.006(2) C29 0.036(3) 0.032(3) 0.031(3) 0.002(2) -0.008(2) -0.007(2) C30 0.049(3) 0.031(3) 0.047(4) -0.004(3) -0.006(3) 0.005(3) C31 0.050(3) 0.029(3) 0.047(4) 0.002(3) -0.015(3) 0.003(2) C32 0.058(4) 0.035(3) 0.031(3) 0.011(2) -0.014(3) -0.008(3) C33 0.041(3) 0.035(3) 0.026(3) 0.006(2) -0.012(2) -0.011(2) C34 0.051(3) 0.040(3) 0.027(3) 0.001(2) -0.009(2) -0.004(2) C35 0.074(4) 0.047(3) 0.062(4) 0.009(3) -0.012(3) 0.013(3) C36 0.060(3) 0.039(3) 0.028(3) 0.009(2) -0.013(3) -0.007(3) C37 0.030(3) 0.029(3) 0.056(4) 0.014(3) -0.017(3) -0.013(2) C38 0.053(4) 0.029(3) 0.043(4) -0.008(2) -0.023(3) -0.004(3) C39 0.049(3) 0.026(3) 0.039(3) -0.005(2) -0.021(3) -0.011(2) C40 0.052(4) 0.057(4) 0.039(4) 0.002(3) -0.004(3) -0.013(3) C41 0.069(4) 0.090(5) 0.056(4) -0.024(4) -0.001(3) 0.014(4) C42 0.104(6) 0.065(5) 0.100(6) -0.038(4) -0.037(5) 0.025(4) C43 0.119(6) 0.029(3) 0.100(5) 0.001(3) -0.061(5) -0.009(3) C44 0.075(4) 0.047(3) 0.050(4) 0.001(3) -0.025(3) -0.020(3) C45 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C46 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C47 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C48 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C49 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C50 0.0736(19) 0.107(2) 0.0662(19) -0.0188(18) -0.0095(17) 0.0071(17) C51 0.044(3) 0.051(3) 0.045(3) -0.006(3) -0.017(3) -0.011(3) C52 0.061(4) 0.079(4) 0.058(4) 0.024(3) -0.022(3) -0.026(3) C53 0.071(4) 0.050(3) 0.043(4) 0.007(3) -0.031(3) -0.015(3) C54 0.065(4) 0.065(4) 0.038(3) 0.011(3) -0.012(3) -0.016(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 Pt1 C38 1.978(6) . ? Pt1 C37 1.985(5) . ? Pt1 P1 2.3305(12) . ? Pt1 P4 2.3309(11) . ? P1 C1 1.869(4) . ? P1 P2 2.2117(16) . ? P2 C10 1.849(4) . ? P2 P3 2.2113(16) . ? P3 C19 1.857(4) . ? P3 P4 2.2149(16) . ? P4 C28 1.864(4) . ? N1 C37 1.143(5) . ? N1 C39 1.444(5) . ? N2 C38 1.135(5) . ? N2 C45 1.440(6) . ? O1 C51 1.409(5) . ? O1 C53 1.420(5) . ? C1 C2 1.403(6) . ? C1 C6 1.405(6) . ? C2 C3 1.400(6) . ? C2 C7 1.484(6) . ? C3 C4 1.372(6) . ? C4 C5 1.386(6) . ? C4 C8 1.514(6) . ? C5 C6 1.391(6) . ? C6 C9 1.501(6) . ? C10 C11 1.407(5) . ? C10 C15 1.411(5) . ? C11 C12 1.389(6) . ? C11 C16 1.516(6) . ? C12 C13 1.368(6) . ? C13 C14 1.382(6) . ? C13 C17 1.510(6) . ? C14 C15 1.385(6) . ? C15 C18 1.518(5) . ? C19 C20 1.409(6) . ? C19 C24 1.411(6) . ? C20 C21 1.393(6) . ? C20 C25 1.507(5) . ? C21 C22 1.369(6) . ? C22 C23 1.376(6) . ? C22 C26 1.524(6) . ? C23 C24 1.398(6) . ? C24 C27 1.516(6) . ? C28 C33 1.407(5) . ? C28 C29 1.410(6) . ? C29 C30 1.393(6) . ? C29 C34 1.510(5) . ? C30 C31 1.386(6) . ? C31 C32 1.376(6) . ? C31 C35 1.523(6) . ? C32 C33 1.390(6) . ? C33 C36 1.502(6) . ? C39 C44 1.518(6) . ? C39 C40 1.519(6) . ? C40 C41 1.517(6) . ? C41 C42 1.524(8) . ? C42 C43 1.500(8) . ? C43 C44 1.523(6) . ? C45 C50 1.534(7) . ? C45 C46 1.563(8) . ? C46 C47 1.448(7) . ? C47 C48 1.523(7) . ? C48 C49 1.486(8) . ? C49 C50 1.458(7) . ? C51 C52 1.500(6) . ? C53 C54 1.511(6) . ? 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 C38 Pt1 C37 96.01(17) . . ? C38 Pt1 P1 171.22(14) . . ? C37 Pt1 P1 87.71(13) . . ? C38 Pt1 P4 84.61(13) . . ? C37 Pt1 P4 170.56(13) . . ? P1 Pt1 P4 93.03(4) . . ? C1 P1 P2 96.69(13) . . ? C1 P1 Pt1 110.47(14) . . ? P2 P1 Pt1 108.07(6) . . ? C10 P2 P3 106.53(14) . . ? C10 P2 P1 100.83(13) . . ? P3 P2 P1 96.57(6) . . ? C19 P3 P2 105.39(14) . . ? C19 P3 P4 97.17(14) . . ? P2 P3 P4 96.28(6) . . ? C28 P4 P3 97.51(13) . . ? C28 P4 Pt1 111.46(14) . . ? P3 P4 Pt1 111.40(6) . . ? C37 N1 C39 173.4(4) . . ? C38 N2 C45 170.4(5) . . ? C51 O1 C53 111.7(3) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 P1 125.0(3) . . ? C6 C1 P1 116.3(3) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C7 117.8(4) . . ? C1 C2 C7 123.5(4) . . ? C4 C3 C2 123.2(4) . . ? C3 C4 C5 117.5(4) . . ? C3 C4 C8 120.9(5) . . ? C5 C4 C8 121.6(5) . . ? C4 C5 C6 121.7(5) . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C9 117.5(4) . . ? C1 C6 C9 122.4(4) . . ? C11 C10 C15 117.7(4) . . ? C11 C10 P2 113.7(3) . . ? C15 C10 P2 128.5(3) . . ? C12 C11 C10 119.7(4) . . ? C12 C11 C16 117.4(4) . . ? C10 C11 C16 122.8(4) . . ? C13 C12 C11 122.7(4) . . ? C12 C13 C14 117.6(4) . . ? C12 C13 C17 122.1(4) . . ? C14 C13 C17 120.3(4) . . ? C13 C14 C15 122.1(4) . . ? C14 C15 C10 120.0(4) . . ? C14 C15 C18 117.0(4) . . ? C10 C15 C18 123.0(4) . . ? C20 C19 C24 118.6(4) . . ? C20 C19 P3 127.3(3) . . ? C24 C19 P3 113.9(3) . . ? C21 C20 C19 119.1(4) . . ? C21 C20 C25 116.5(4) . . ? C19 C20 C25 124.4(4) . . ? C22 C21 C20 122.6(4) . . ? C21 C22 C23 118.3(5) . . ? C21 C22 C26 119.8(5) . . ? C23 C22 C26 121.8(5) . . ? C22 C23 C24 121.8(5) . . ? C23 C24 C19 119.5(4) . . ? C23 C24 C27 117.9(4) . . ? C19 C24 C27 122.6(4) . . ? C33 C28 C29 118.3(4) . . ? C33 C28 P4 125.1(3) . . ? C29 C28 P4 116.6(3) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 C34 116.9(4) . . ? C28 C29 C34 123.3(4) . . ? C31 C30 C29 121.9(4) . . ? C32 C31 C30 117.6(4) . . ? C32 C31 C35 121.8(5) . . ? C30 C31 C35 120.6(4) . . ? C31 C32 C33 122.7(4) . . ? C32 C33 C28 119.5(4) . . ? C32 C33 C36 118.2(4) . . ? C28 C33 C36 122.3(4) . . ? N1 C37 Pt1 179.4(5) . . ? N2 C38 Pt1 176.8(4) . . ? N1 C39 C44 109.1(4) . . ? N1 C39 C40 108.3(4) . . ? C44 C39 C40 111.1(4) . . ? C41 C40 C39 109.4(4) . . ? C40 C41 C42 110.0(5) . . ? C43 C42 C41 110.4(5) . . ? C42 C43 C44 111.4(5) . . ? C39 C44 C43 109.2(4) . . ? N2 C45 C50 109.3(5) . . ? N2 C45 C46 105.8(5) . . ? C50 C45 C46 111.1(5) . . ? C47 C46 C45 112.8(6) . . ? C46 C47 C48 109.8(5) . . ? C49 C48 C47 111.9(5) . . ? C50 C49 C48 112.3(6) . . ? C49 C50 C45 110.0(5) . . ? O1 C51 C52 108.2(4) . . ? O1 C53 C54 108.5(4) . . ?