Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Youichi Ishii' 'Masakazu Iwasaki' 'Sou Kamimura' 'Shigeki Kuwata' _publ_contact_author_name 'Prof Youichi Ishii' _publ_contact_author_address ; Department of Applied Chemistry Chuo University Faculty of Science & Engineering Kasuga,Bunkyo-ku Tokyo 112-8551 JAPAN ; _publ_contact_author_email ishii@chem.chuo-u.ac.jp _publ_contact_author_fax ' +81-3-3817-1895 ' _publ_contact_author_phone ' +81-3-3817-1901 ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses, structures and solution behaviour of cyclotriphosphato complexes of Pd(II), Pt(II) and Pt(IV) ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; #------------------------------------------------------------------------------ data_(PPN)[Pd(P3O9)(PPh3)2](1) _database_code_CSD 202873 _audit_creation_date 'Thu Apr 3 13:55:39 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C74.50 H65 Cl5 N O9 P7 Pd ' _chemical_formula_moiety (PPN)[Pd(P3O9)(PPh3)2] _chemical_formula_weight 1618.82 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.19(1) _cell_length_b 16.079(6) _cell_length_c 17.426(5) _cell_angle_alpha 105.52(3) _cell_angle_beta 92.75(4) _cell_angle_gamma 103.84(5) _cell_volume 3693(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.6 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 13510 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max ? _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3.36 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; for calculating R-factor (gt). ; _reflns_number_total 13005 _reflns_number_gt 7283 _reflns_threshold_criterion F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0509 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7283 _refine_ls_number_parameters 869 _refine_ls_goodness_of_fit_ref 1.507 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_shift/su_max 0.0150 _refine_diff_density_max 0.75 _refine_diff_density_min -0.72 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0006(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.11781(4) 0.28163(3) 0.22499(3) 0.0286(1) Uani 1.00 d . . . Cl(1) Cl -0.0261(3) -0.0491(3) 0.3834(3) 0.205(3) Uani 1.00 d . . . Cl(2) Cl 0.0781(3) -0.1721(2) 0.3091(2) 0.159(2) Uani 1.00 d . . . Cl(3) Cl 0.4365(3) 0.2737(2) 0.5473(2) 0.124(1) Uani 1.00 d . . . Cl(4) Cl 0.5585(3) 0.1752(3) 0.4574(2) 0.149(2) Uani 1.00 d . . . Cl(5) Cl 0.5846(3) 0.4704(3) 0.4794(3) 0.182(2) Uani 1.00 d . . . P(1) P 0.2513(1) 0.1583(1) 0.1330(1) 0.0378(5) Uani 1.00 d . . . P(2) P 0.2300(1) 0.1567(1) 0.2937(1) 0.0388(5) Uani 1.00 d . . . P(3) P 0.3797(1) 0.2985(1) 0.2653(1) 0.0384(5) Uani 1.00 d . . . P(4) P 0.0564(1) 0.3593(1) 0.3297(1) 0.0339(5) Uani 1.00 d . . . P(5) P 0.0695(1) 0.3419(1) 0.1312(1) 0.0336(5) Uani 1.00 d . . . P(6) P 0.6881(1) 0.9350(1) 0.2171(1) 0.0356(5) Uani 1.00 d . . . P(7) P 0.5258(1) 0.7716(1) 0.1822(1) 0.0355(5) Uani 1.00 d . . . O(1) O 0.1690(3) 0.2022(3) 0.1293(2) 0.037(1) Uani 1.00 d . . . O(2) O 0.1519(3) 0.2058(3) 0.2966(2) 0.036(1) Uani 1.00 d . . . O(3) O 0.3237(3) 0.3668(3) 0.2781(3) 0.044(1) Uani 1.00 d . . . O(4) O 0.2691(3) 0.0988(3) 0.0594(3) 0.054(2) Uani 1.00 d . . . O(5) O 0.2318(3) 0.1057(3) 0.2003(3) 0.040(1) Uani 1.00 d . . . O(6) O 0.2256(3) 0.0947(3) 0.3419(3) 0.056(2) Uani 1.00 d . . . O(7) O 0.3349(3) 0.2267(3) 0.3136(3) 0.040(1) Uani 1.00 d . . . O(8) O 0.4861(3) 0.3214(3) 0.2816(3) 0.058(2) Uani 1.00 d . . . O(9) O 0.3498(3) 0.2338(3) 0.1737(3) 0.041(1) Uani 1.00 d . . . N(1) N 0.6316(4) 0.8322(3) 0.1841(3) 0.042(2) Uani 1.00 d . . . C(1) C 0.1067(5) 0.4793(4) 0.3517(4) 0.036(2) Uani 1.00 d . . . C(2) C 0.2080(5) 0.5108(5) 0.3519(4) 0.043(2) Uani 1.00 d . . . C(3) C 0.2514(6) 0.6013(5) 0.3718(5) 0.059(3) Uani 1.00 d . . . C(4) C 0.1960(7) 0.6615(5) 0.3896(5) 0.065(3) Uani 1.00 d . . . C(5) C 0.0971(7) 0.6322(5) 0.3886(5) 0.059(3) Uani 1.00 d . . . C(6) C 0.0519(5) 0.5412(5) 0.3696(4) 0.048(2) Uani 1.00 d . . . C(7) C -0.0755(4) 0.3352(4) 0.3233(4) 0.037(2) Uani 1.00 d . . . C(8) C -0.1336(5) 0.2772(5) 0.2551(4) 0.051(2) Uani 1.00 d . . . C(9) C -0.2349(6) 0.2612(6) 0.2494(5) 0.063(3) Uani 1.00 d . . . C(10) C -0.2795(6) 0.3004(6) 0.3122(6) 0.074(3) Uani 1.00 d . . . C(11) C -0.2220(6) 0.3543(6) 0.3823(6) 0.073(3) Uani 1.00 d . . . C(12) C -0.1206(5) 0.3720(5) 0.3876(4) 0.058(3) Uani 1.00 d . . . C(13) C 0.0883(5) 0.3326(5) 0.4208(4) 0.038(2) Uani 1.00 d . . . C(14) C 0.0389(6) 0.2504(5) 0.4303(5) 0.059(3) Uani 1.00 d . . . C(15) C 0.0642(8) 0.2266(6) 0.4973(6) 0.074(3) Uani 1.00 d . . . C(16) C 0.1378(8) 0.2823(8) 0.5544(6) 0.086(4) Uani 1.00 d . . . C(17) C 0.1865(8) 0.3620(8) 0.5453(6) 0.104(4) Uani 1.00 d . . . C(18) C 0.1616(6) 0.3870(6) 0.4787(5) 0.068(3) Uani 1.00 d . . . C(19) C 0.1697(5) 0.3639(4) 0.0714(4) 0.040(2) Uani 1.00 d . . . C(20) C 0.2646(5) 0.3968(5) 0.1090(4) 0.047(2) Uani 1.00 d . . . C(21) C 0.3414(5) 0.4167(5) 0.0655(5) 0.054(3) Uani 1.00 d . . . C(22) C 0.3240(6) 0.4047(6) -0.0149(5) 0.061(3) Uani 1.00 d . . . C(23) C 0.2306(7) 0.3726(6) -0.0525(4) 0.065(3) Uani 1.00 d . . . C(24) C 0.1528(5) 0.3520(5) -0.0101(4) 0.054(3) Uani 1.00 d . . . C(25) C -0.0338(5) 0.2610(4) 0.0639(4) 0.040(2) Uani 1.00 d . . . C(26) C -0.0580(5) 0.1745(5) 0.0674(4) 0.037(2) Uani 1.00 d . . . C(27) C -0.1375(5) 0.1103(5) 0.0182(4) 0.047(2) Uani 1.00 d . . . C(28) C -0.1907(5) 0.1351(6) -0.0356(5) 0.061(3) Uani 1.00 d . . . C(29) C -0.1654(6) 0.2205(6) -0.0411(5) 0.071(3) Uani 1.00 d . . . C(30) C -0.0878(5) 0.2849(5) 0.0083(5) 0.056(3) Uani 1.00 d . . . C(31) C 0.0322(5) 0.4462(4) 0.1562(4) 0.039(2) Uani 1.00 d . . . C(32) C -0.0639(6) 0.4454(5) 0.1674(5) 0.058(3) Uani 1.00 d . . . C(33) C -0.0932(6) 0.5243(6) 0.1844(5) 0.072(3) Uani 1.00 d . . . C(34) C -0.0262(8) 0.6028(6) 0.1912(6) 0.081(4) Uani 1.00 d . . . C(35) C 0.0701(7) 0.6053(5) 0.1807(5) 0.071(3) Uani 1.00 d . . . C(36) C 0.0988(6) 0.5265(5) 0.1635(5) 0.056(3) Uani 1.00 d . . . C(37) C 0.8042(4) 0.9479(4) 0.1796(4) 0.033(2) Uani 1.00 d . . . C(38) C 0.8804(5) 1.0232(4) 0.2131(4) 0.044(2) Uani 1.00 d . . . C(39) C 0.9690(5) 1.0342(5) 0.1838(4) 0.048(2) Uani 1.00 d . . . C(40) C 0.9810(5) 0.9705(5) 0.1173(5) 0.058(3) Uani 1.00 d . . . C(41) C 0.9062(6) 0.8963(5) 0.0820(5) 0.065(3) Uani 1.00 d . . . C(42) C 0.8192(5) 0.8849(5) 0.1135(4) 0.050(2) Uani 1.00 d . . . C(43) C 0.7149(5) 0.9753(5) 0.3255(4) 0.050(2) Uani 1.00 d . . . C(44) C 0.7431(6) 1.0666(6) 0.3640(5) 0.070(3) Uani 1.00 d . . . C(45) C 0.7750(7) 1.0960(8) 0.4455(6) 0.100(4) Uani 1.00 d . . . C(46) C 0.7753(8) 1.035(1) 0.4867(6) 0.118(5) Uani 1.00 d . . . C(47) C 0.7454(8) 0.945(1) 0.4504(7) 0.108(5) Uani 1.00 d . . . C(48) C 0.7153(6) 0.9157(6) 0.3692(5) 0.067(3) Uani 1.00 d . . . C(49) C 0.6267(5) 1.0065(4) 0.1839(4) 0.039(2) Uani 1.00 d . . . C(50) C 0.6359(5) 1.0165(5) 0.1081(5) 0.052(3) Uani 1.00 d . . . C(51) C 0.5817(6) 1.0648(6) 0.0783(5) 0.071(3) Uani 1.00 d . . . C(52) C 0.5187(7) 1.1025(6) 0.1249(7) 0.079(4) Uani 1.00 d . . . C(53) C 0.5114(6) 1.0950(6) 0.2007(7) 0.076(3) Uani 1.00 d . . . C(54) C 0.5641(6) 1.0478(5) 0.2310(5) 0.055(3) Uani 1.00 d . . . C(55) C 0.4446(4) 0.8285(4) 0.2378(4) 0.034(2) Uani 1.00 d . . . C(56) C 0.4510(5) 0.8455(5) 0.3200(4) 0.053(3) Uani 1.00 d . . . C(57) C 0.4008(6) 0.9028(6) 0.3639(5) 0.065(3) Uani 1.00 d . . . C(58) C 0.3431(6) 0.9403(5) 0.3256(5) 0.059(3) Uani 1.00 d . . . C(59) C 0.3350(5) 0.9225(5) 0.2442(5) 0.056(3) Uani 1.00 d . . . C(60) C 0.3859(5) 0.8675(5) 0.1998(4) 0.047(2) Uani 1.00 d . . . C(61) C 0.4674(5) 0.7220(4) 0.0802(4) 0.038(2) Uani 1.00 d . . . C(62) C 0.5138(5) 0.7402(5) 0.0171(5) 0.054(3) Uani 1.00 d . . . C(63) C 0.4678(7) 0.7011(6) -0.0608(5) 0.067(3) Uani 1.00 d . . . C(64) C 0.3758(7) 0.6451(6) -0.0750(5) 0.067(3) Uani 1.00 d . . . C(65) C 0.3288(6) 0.6258(6) -0.0128(5) 0.073(3) Uani 1.00 d . . . C(66) C 0.3733(6) 0.6638(5) 0.0647(5) 0.060(3) Uani 1.00 d . . . C(67) C 0.5388(5) 0.6815(4) 0.2215(4) 0.037(2) Uani 1.00 d . . . C(68) C 0.6299(6) 0.6660(5) 0.2286(4) 0.053(3) Uani 1.00 d . . . C(69) C 0.6404(6) 0.5927(6) 0.2529(5) 0.064(3) Uani 1.00 d . . . C(70) C 0.5606(8) 0.5354(5) 0.2694(5) 0.068(3) Uani 1.00 d . . . C(71) C 0.4710(7) 0.5517(5) 0.2646(5) 0.062(3) Uani 1.00 d . . . C(72) C 0.4598(5) 0.6241(5) 0.2407(4) 0.050(2) Uani 1.00 d . . . C(73) C 0.0448(8) -0.0789(7) 0.3079(7) 0.108(4) Uiso 1.00 d . . . C(74) C 0.4616(8) 0.2179(7) 0.4538(6) 0.101(3) Uiso 1.00 d . . . C(75) C 0.466(2) 0.471(1) 0.462(1) 0.101(7) Uiso 0.50 d P . . H(1) H 0.2467 0.4695 0.3383 0.0519 Uiso 1.00 calc . . . H(2) H 0.3202 0.6221 0.3731 0.0714 Uiso 1.00 calc . . . H(3) H 0.2264 0.7238 0.4028 0.0777 Uiso 1.00 calc . . . H(4) H 0.0590 0.6742 0.4010 0.0713 Uiso 1.00 calc . . . H(5) H -0.0169 0.5214 0.3689 0.0573 Uiso 1.00 calc . . . H(6) H -0.1042 0.2478 0.2117 0.0613 Uiso 1.00 calc . . . H(7) H -0.2737 0.2227 0.2014 0.0762 Uiso 1.00 calc . . . H(8) H -0.3485 0.2907 0.3075 0.0892 Uiso 1.00 calc . . . H(9) H -0.2519 0.3794 0.4273 0.0878 Uiso 1.00 calc . . . H(10) H -0.0820 0.4097 0.4360 0.0692 Uiso 1.00 calc . . . H(11) H -0.0121 0.2108 0.3906 0.0706 Uiso 1.00 calc . . . H(12) H 0.0300 0.1708 0.5037 0.0893 Uiso 1.00 calc . . . H(13) H 0.1549 0.2654 0.6003 0.1035 Uiso 1.00 calc . . . H(14) H 0.2380 0.4009 0.5849 0.1246 Uiso 1.00 calc . . . H(15) H 0.1961 0.4431 0.4732 0.0818 Uiso 1.00 calc . . . H(16) H 0.2770 0.4059 0.1651 0.0561 Uiso 1.00 calc . . . H(17) H 0.4065 0.4387 0.0916 0.0643 Uiso 1.00 calc . . . H(18) H 0.3769 0.4186 -0.0447 0.0727 Uiso 1.00 calc . . . H(19) H 0.2189 0.3643 -0.1085 0.0775 Uiso 1.00 calc . . . H(20) H 0.0880 0.3298 -0.0368 0.0651 Uiso 1.00 calc . . . H(21) H -0.0198 0.1577 0.1041 0.0439 Uiso 1.00 calc . . . H(22) H -0.1545 0.0508 0.0219 0.0561 Uiso 1.00 calc . . . H(23) H -0.2454 0.0926 -0.0693 0.0729 Uiso 1.00 calc . . . H(24) H -0.2020 0.2361 -0.0796 0.0857 Uiso 1.00 calc . . . H(25) H -0.0715 0.3443 0.0043 0.0669 Uiso 1.00 calc . . . H(26) H -0.1102 0.3904 0.1634 0.0700 Uiso 1.00 calc . . . H(27) H -0.1595 0.5234 0.1911 0.0868 Uiso 1.00 calc . . . H(28) H -0.0459 0.6569 0.2035 0.0969 Uiso 1.00 calc . . . H(29) H 0.1162 0.6605 0.1853 0.0846 Uiso 1.00 calc . . . H(30) H 0.1651 0.5279 0.1565 0.0674 Uiso 1.00 calc . . . H(31) H 0.8710 1.0686 0.2575 0.0525 Uiso 1.00 calc . . . H(32) H 1.0214 1.0851 0.2091 0.0580 Uiso 1.00 calc . . . H(33) H 1.0416 0.9782 0.0957 0.0695 Uiso 1.00 calc . . . H(34) H 0.9146 0.8528 0.0356 0.0775 Uiso 1.00 calc . . . H(35) H 0.7681 0.8325 0.0894 0.0604 Uiso 1.00 calc . . . H(36) H 0.7407 1.1084 0.3348 0.0842 Uiso 1.00 calc . . . H(37) H 0.7964 1.1582 0.4725 0.1201 Uiso 1.00 calc . . . H(38) H 0.7972 1.0553 0.5426 0.1418 Uiso 1.00 calc . . . H(39) H 0.7453 0.9036 0.4804 0.1298 Uiso 1.00 calc . . . H(40) H 0.6946 0.8533 0.3429 0.0801 Uiso 1.00 calc . . . H(41) H 0.6795 0.9903 0.0762 0.0625 Uiso 1.00 calc . . . H(42) H 0.5880 1.0717 0.0262 0.0856 Uiso 1.00 calc . . . H(43) H 0.4799 1.1340 0.1041 0.0948 Uiso 1.00 calc . . . H(44) H 0.4692 1.1230 0.2328 0.0913 Uiso 1.00 calc . . . H(45) H 0.5584 1.0430 0.2838 0.0662 Uiso 1.00 calc . . . H(46) H 0.4895 0.8183 0.3464 0.0632 Uiso 1.00 calc . . . H(47) H 0.4066 0.9160 0.4207 0.0780 Uiso 1.00 calc . . . H(48) H 0.3085 0.9789 0.3559 0.0705 Uiso 1.00 calc . . . H(49) H 0.2940 0.9480 0.2181 0.0668 Uiso 1.00 calc . . . H(50) H 0.3811 0.8562 0.1432 0.0570 Uiso 1.00 calc . . . H(51) H 0.5776 0.7795 0.0266 0.0652 Uiso 1.00 calc . . . H(52) H 0.5006 0.7133 -0.1044 0.0805 Uiso 1.00 calc . . . H(53) H 0.3442 0.6195 -0.1284 0.0810 Uiso 1.00 calc . . . H(54) H 0.2653 0.5860 -0.0231 0.0880 Uiso 1.00 calc . . . H(55) H 0.3402 0.6506 0.1079 0.0721 Uiso 1.00 calc . . . H(56) H 0.6852 0.7052 0.2170 0.0642 Uiso 1.00 calc . . . H(57) H 0.7031 0.5822 0.2582 0.0769 Uiso 1.00 calc . . . H(58) H 0.5679 0.4843 0.2841 0.0811 Uiso 1.00 calc . . . H(59) H 0.4163 0.5132 0.2778 0.0747 Uiso 1.00 calc . . . H(60) H 0.3971 0.6350 0.2373 0.0596 Uiso 1.00 calc . . . H(61) H 0.0084 -0.0890 0.2576 0.1290 Uiso 1.00 calc . . . H(62) H 0.1020 -0.0313 0.3147 0.1290 Uiso 1.00 calc . . . H(63) H 0.4058 0.1703 0.4286 0.1210 Uiso 1.00 calc . . . H(64) H 0.4742 0.2588 0.4226 0.1210 Uiso 1.00 calc . . . H(65) H 0.4611 0.4874 0.4138 0.1217 Uiso 0.50 calc P . . H(66) H 0.4289 0.4116 0.4541 0.1217 Uiso 0.50 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0289(3) 0.0268(3) 0.0303(3) 0.0107(2) 0.0017(2) 0.0056(2) Cl(1) 0.184(4) 0.283(6) 0.264(5) 0.138(4) 0.117(4) 0.187(5) Cl(2) 0.192(4) 0.076(2) 0.184(4) 0.020(2) -0.003(3) 0.014(2) Cl(3) 0.173(3) 0.123(3) 0.103(2) 0.078(2) 0.027(2) 0.041(2) Cl(4) 0.172(3) 0.208(4) 0.100(2) 0.110(3) 0.021(2) 0.044(3) Cl(5) 0.109(3) 0.208(5) 0.239(5) 0.050(3) 0.043(3) 0.068(4) P(1) 0.034(1) 0.034(1) 0.042(1) 0.0134(8) 0.0027(8) 0.0005(8) P(2) 0.039(1) 0.032(1) 0.049(1) 0.0115(8) 0.0011(9) 0.0161(9) P(3) 0.030(1) 0.032(1) 0.049(1) 0.0062(8) -0.0020(9) 0.0092(9) P(4) 0.034(1) 0.035(1) 0.033(1) 0.0123(8) 0.0048(8) 0.0067(8) P(5) 0.036(1) 0.0318(10) 0.033(1) 0.0119(8) 0.0003(8) 0.0077(8) P(6) 0.033(1) 0.032(1) 0.039(1) 0.0072(8) 0.0081(8) 0.0064(8) P(7) 0.0317(10) 0.033(1) 0.042(1) 0.0061(8) 0.0075(8) 0.0126(9) O(1) 0.039(3) 0.040(3) 0.032(3) 0.018(2) 0.004(2) 0.004(2) O(2) 0.040(3) 0.037(3) 0.036(3) 0.017(2) 0.005(2) 0.014(2) O(3) 0.047(3) 0.033(3) 0.052(3) 0.015(2) 0.006(2) 0.010(2) O(4) 0.052(3) 0.054(3) 0.051(3) 0.026(3) 0.005(3) -0.006(3) O(5) 0.039(3) 0.025(2) 0.054(3) 0.013(2) 0.002(2) 0.007(2) O(6) 0.054(3) 0.056(3) 0.077(4) 0.023(3) 0.013(3) 0.042(3) O(7) 0.037(3) 0.038(3) 0.046(3) 0.007(2) -0.006(2) 0.016(2) O(8) 0.027(3) 0.052(3) 0.088(4) 0.002(2) -0.007(3) 0.017(3) O(9) 0.037(3) 0.040(3) 0.040(3) 0.008(2) 0.002(2) 0.004(2) N(1) 0.042(3) 0.029(3) 0.051(4) 0.006(3) 0.013(3) 0.008(3) C(1) 0.043(4) 0.038(4) 0.031(4) 0.017(3) 0.004(3) 0.008(3) C(2) 0.044(4) 0.040(4) 0.041(4) 0.016(4) 0.006(3) 0.001(3) C(3) 0.054(5) 0.047(5) 0.070(6) 0.003(4) 0.008(4) 0.015(4) C(4) 0.084(7) 0.038(5) 0.062(6) 0.011(5) 0.013(5) 0.000(4) C(5) 0.086(7) 0.040(5) 0.055(5) 0.033(5) 0.016(5) 0.002(4) C(6) 0.044(4) 0.052(5) 0.049(5) 0.020(4) 0.006(4) 0.012(4) C(7) 0.029(4) 0.038(4) 0.041(4) 0.009(3) 0.009(3) 0.007(3) C(8) 0.046(5) 0.049(5) 0.051(5) 0.010(4) 0.011(4) 0.004(4) C(9) 0.037(5) 0.070(6) 0.068(6) -0.004(4) 0.002(4) 0.012(5) C(10) 0.034(5) 0.089(7) 0.098(8) 0.013(5) 0.017(5) 0.025(6) C(11) 0.054(6) 0.077(7) 0.083(7) 0.023(5) 0.032(5) 0.005(5) C(12) 0.047(5) 0.069(6) 0.049(5) 0.018(4) 0.014(4) 0.002(4) C(13) 0.040(4) 0.046(4) 0.031(4) 0.019(4) 0.008(3) 0.007(3) C(14) 0.067(6) 0.054(5) 0.058(5) 0.016(4) 0.015(4) 0.020(4) C(15) 0.108(8) 0.071(7) 0.065(6) 0.038(6) 0.035(6) 0.037(5) C(16) 0.104(9) 0.105(9) 0.070(7) 0.038(7) 0.005(6) 0.050(7) C(17) 0.110(9) 0.127(10) 0.065(7) 0.002(8) -0.028(6) 0.045(7) C(18) 0.073(6) 0.067(6) 0.060(6) 0.005(5) -0.011(5) 0.025(5) C(19) 0.042(4) 0.041(4) 0.038(4) 0.016(3) 0.004(3) 0.012(3) C(20) 0.049(5) 0.047(5) 0.045(4) 0.013(4) -0.002(4) 0.015(4) C(21) 0.038(4) 0.063(5) 0.061(5) 0.011(4) 0.010(4) 0.020(4) C(22) 0.070(6) 0.066(6) 0.059(6) 0.026(5) 0.029(5) 0.029(5) C(23) 0.078(6) 0.087(7) 0.035(5) 0.027(5) 0.014(4) 0.022(5) C(24) 0.052(5) 0.070(6) 0.041(5) 0.014(4) 0.002(4) 0.017(4) C(25) 0.041(4) 0.042(4) 0.034(4) 0.016(3) -0.002(3) 0.003(3) C(26) 0.038(4) 0.043(4) 0.029(4) 0.015(3) 0.004(3) 0.008(3) C(27) 0.049(5) 0.037(4) 0.047(5) 0.006(4) 0.005(4) 0.006(4) C(28) 0.047(5) 0.061(6) 0.055(5) -0.001(4) -0.012(4) 0.002(4) C(29) 0.067(6) 0.077(7) 0.067(6) 0.018(5) -0.029(5) 0.021(5) C(30) 0.054(5) 0.050(5) 0.059(5) 0.012(4) -0.012(4) 0.015(4) C(31) 0.050(5) 0.035(4) 0.036(4) 0.019(4) 0.001(3) 0.009(3) C(32) 0.063(5) 0.050(5) 0.065(6) 0.028(4) 0.001(4) 0.011(4) C(33) 0.067(6) 0.067(6) 0.089(7) 0.043(5) -0.002(5) 0.012(5) C(34) 0.111(8) 0.050(6) 0.085(7) 0.047(6) -0.016(6) 0.007(5) C(35) 0.100(8) 0.039(5) 0.075(6) 0.021(5) 0.005(5) 0.019(4) C(36) 0.067(6) 0.045(5) 0.057(5) 0.020(4) -0.002(4) 0.012(4) C(37) 0.037(4) 0.025(4) 0.039(4) 0.010(3) 0.013(3) 0.009(3) C(38) 0.044(4) 0.030(4) 0.051(5) 0.005(3) 0.012(4) 0.006(3) C(39) 0.040(4) 0.041(4) 0.059(5) 0.002(4) -0.002(4) 0.015(4) C(40) 0.036(4) 0.061(6) 0.082(6) 0.014(4) 0.025(4) 0.025(5) C(41) 0.052(5) 0.055(5) 0.073(6) 0.009(4) 0.030(4) -0.005(4) C(42) 0.036(4) 0.047(5) 0.055(5) 0.003(4) 0.010(4) -0.002(4) C(43) 0.036(4) 0.068(6) 0.041(5) 0.014(4) 0.008(3) 0.006(4) C(44) 0.064(6) 0.079(7) 0.050(5) 0.016(5) 0.007(4) -0.009(5) C(45) 0.066(7) 0.14(1) 0.054(7) 0.018(7) 0.003(6) -0.032(7) C(46) 0.063(7) 0.23(2) 0.032(6) 0.019(9) 0.009(5) -0.005(8) C(47) 0.076(8) 0.20(1) 0.056(7) 0.023(9) 0.011(6) 0.057(8) C(48) 0.045(5) 0.105(8) 0.048(5) 0.008(5) 0.007(4) 0.029(5) C(49) 0.029(4) 0.029(4) 0.054(5) 0.002(3) 0.002(3) 0.010(3) C(50) 0.040(4) 0.060(5) 0.062(5) 0.019(4) 0.007(4) 0.023(4) C(51) 0.054(6) 0.088(7) 0.083(7) 0.024(5) 0.005(5) 0.038(6) C(52) 0.067(6) 0.069(6) 0.122(9) 0.032(5) 0.004(6) 0.051(7) C(53) 0.056(6) 0.063(6) 0.126(9) 0.040(5) 0.028(6) 0.030(6) C(54) 0.055(5) 0.040(5) 0.069(6) 0.016(4) 0.014(4) 0.008(4) C(55) 0.029(4) 0.039(4) 0.036(4) 0.008(3) 0.007(3) 0.011(3) C(56) 0.058(5) 0.063(5) 0.051(5) 0.031(4) 0.016(4) 0.024(4) C(57) 0.081(6) 0.079(6) 0.051(5) 0.043(5) 0.030(5) 0.022(5) C(58) 0.057(5) 0.067(6) 0.061(6) 0.034(5) 0.020(4) 0.015(5) C(59) 0.048(5) 0.058(5) 0.067(6) 0.028(4) 0.010(4) 0.015(4) C(60) 0.039(4) 0.058(5) 0.046(5) 0.017(4) 0.001(3) 0.013(4) C(61) 0.045(4) 0.030(4) 0.038(4) 0.011(3) 0.003(3) 0.007(3) C(62) 0.055(5) 0.055(5) 0.059(5) 0.021(4) 0.012(4) 0.021(4) C(63) 0.089(7) 0.075(6) 0.051(5) 0.032(6) 0.021(5) 0.028(5) C(64) 0.087(7) 0.062(6) 0.047(5) 0.023(5) -0.003(5) 0.004(4) C(65) 0.074(6) 0.060(6) 0.064(6) -0.007(5) -0.018(5) 0.008(5) C(66) 0.055(5) 0.065(6) 0.049(5) -0.002(4) 0.001(4) 0.014(4) C(67) 0.045(4) 0.027(4) 0.038(4) 0.008(3) 0.005(3) 0.007(3) C(68) 0.068(6) 0.048(5) 0.058(5) 0.026(4) 0.022(4) 0.026(4) C(69) 0.075(6) 0.070(6) 0.067(6) 0.045(5) 0.013(5) 0.027(5) C(70) 0.112(8) 0.041(5) 0.056(6) 0.025(5) 0.006(5) 0.021(4) C(71) 0.080(6) 0.042(5) 0.058(5) -0.004(5) 0.006(5) 0.022(4) C(72) 0.042(4) 0.045(5) 0.062(5) 0.002(4) 0.002(4) 0.023(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) P(4) 2.258(2) . . yes Pd(1) P(5) 2.267(2) . . yes Pd(1) O(1) 2.089(4) . . yes Pd(1) O(2) 2.078(4) . . yes Cl(1) C(73) 1.73(1) . . yes Cl(2) C(73) 1.68(1) . . yes Cl(3) C(74) 1.74(1) . . yes Cl(4) C(74) 1.68(1) . . yes Cl(5) C(75) 1.70(2) . . yes Cl(5) C(75) 1.52(2) . 2_666 yes P(1) O(1) 1.509(4) . . yes P(1) O(4) 1.455(4) . . yes P(1) O(5) 1.617(5) . . yes P(1) O(9) 1.601(4) . . yes P(2) O(2) 1.502(4) . . yes P(2) O(5) 1.620(5) . . yes P(2) O(6) 1.458(4) . . yes P(2) O(7) 1.594(4) . . yes P(3) O(3) 1.480(4) . . yes P(3) O(7) 1.632(4) . . yes P(3) O(8) 1.460(5) . . yes P(3) O(9) 1.628(4) . . yes P(4) C(1) 1.816(7) . . yes P(4) C(7) 1.811(6) . . yes P(4) C(13) 1.817(7) . . yes P(5) C(19) 1.827(7) . . yes P(5) C(25) 1.824(7) . . yes P(5) C(31) 1.826(7) . . yes P(6) N(1) 1.587(5) . . yes P(6) C(37) 1.789(6) . . yes P(6) C(43) 1.814(7) . . yes P(6) C(49) 1.789(7) . . yes P(7) N(1) 1.575(5) . . yes P(7) C(55) 1.800(6) . . yes P(7) C(61) 1.807(7) . . yes P(7) C(67) 1.802(6) . . yes C(1) C(2) 1.404(9) . . yes C(1) C(6) 1.386(9) . . yes C(2) C(3) 1.377(9) . . yes C(3) C(4) 1.37(1) . . yes C(4) C(5) 1.37(1) . . yes C(5) C(6) 1.390(10) . . yes C(7) C(8) 1.381(9) . . yes C(7) C(12) 1.382(9) . . yes C(8) C(9) 1.393(10) . . yes C(9) C(10) 1.37(1) . . yes C(10) C(11) 1.38(1) . . yes C(11) C(12) 1.39(1) . . yes C(13) C(14) 1.397(10) . . yes C(13) C(18) 1.363(10) . . yes C(14) C(15) 1.38(1) . . yes C(15) C(16) 1.36(1) . . yes C(16) C(17) 1.36(1) . . yes C(17) C(18) 1.38(1) . . yes C(19) C(20) 1.382(9) . . yes C(19) C(24) 1.382(9) . . yes C(20) C(21) 1.382(9) . . yes C(21) C(22) 1.365(10) . . yes C(22) C(23) 1.36(1) . . yes C(23) C(24) 1.38(1) . . yes C(25) C(26) 1.370(9) . . yes C(25) C(30) 1.393(9) . . yes C(26) C(27) 1.396(9) . . yes C(27) C(28) 1.373(10) . . yes C(28) C(29) 1.36(1) . . yes C(29) C(30) 1.38(1) . . yes C(31) C(32) 1.385(10) . . yes C(31) C(36) 1.377(9) . . yes C(32) C(33) 1.391(10) . . yes C(33) C(34) 1.36(1) . . yes C(34) C(35) 1.38(1) . . yes C(35) C(36) 1.38(1) . . yes C(37) C(38) 1.382(8) . . yes C(37) C(42) 1.378(9) . . yes C(38) C(39) 1.370(9) . . yes C(39) C(40) 1.374(10) . . yes C(40) C(41) 1.366(10) . . yes C(41) C(42) 1.368(9) . . yes C(43) C(44) 1.39(1) . . yes C(43) C(48) 1.38(1) . . yes C(44) C(45) 1.39(1) . . yes C(45) C(46) 1.37(2) . . yes C(46) C(47) 1.36(2) . . yes C(47) C(48) 1.38(1) . . yes C(49) C(50) 1.382(9) . . yes C(49) C(54) 1.402(9) . . yes C(50) C(51) 1.39(1) . . yes C(51) C(52) 1.37(1) . . yes C(52) C(53) 1.37(1) . . yes C(53) C(54) 1.36(1) . . yes C(55) C(56) 1.377(9) . . yes C(55) C(60) 1.396(9) . . yes C(56) C(57) 1.388(9) . . yes C(57) C(58) 1.37(1) . . yes C(58) C(59) 1.362(10) . . yes C(59) C(60) 1.377(9) . . yes C(61) C(62) 1.371(9) . . yes C(61) C(66) 1.402(9) . . yes C(62) C(63) 1.39(1) . . yes C(63) C(64) 1.37(1) . . yes C(64) C(65) 1.37(1) . . yes C(65) C(66) 1.37(1) . . yes C(67) C(68) 1.379(9) . . yes C(67) C(72) 1.388(9) . . yes C(68) C(69) 1.393(10) . . yes C(69) C(70) 1.37(1) . . yes C(70) C(71) 1.36(1) . . yes C(71) C(72) 1.378(10) . . yes C(75) C(75) 1.52(4) . 2_666 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(4) Pd(1) P(5) 97.84(7) . . . yes P(4) Pd(1) O(1) 176.3(1) . . . yes P(4) Pd(1) O(2) 88.5(1) . . . yes P(5) Pd(1) O(1) 84.1(1) . . . yes P(5) Pd(1) O(2) 170.4(1) . . . yes O(1) Pd(1) O(2) 89.1(2) . . . yes C(75) Cl(5) C(75) 55(1) . . 2_666 yes O(1) P(1) O(4) 118.3(3) . . . yes O(1) P(1) O(5) 107.0(2) . . . yes O(1) P(1) O(9) 109.0(3) . . . yes O(4) P(1) O(5) 109.9(3) . . . yes O(4) P(1) O(9) 110.0(3) . . . yes O(5) P(1) O(9) 101.3(2) . . . yes O(2) P(2) O(5) 107.0(2) . . . yes O(2) P(2) O(6) 118.6(3) . . . yes O(2) P(2) O(7) 109.5(2) . . . yes O(5) P(2) O(6) 110.1(3) . . . yes O(5) P(2) O(7) 100.7(2) . . . yes O(6) P(2) O(7) 109.4(3) . . . yes O(3) P(3) O(7) 108.5(3) . . . yes O(3) P(3) O(8) 122.7(3) . . . yes O(3) P(3) O(9) 108.7(2) . . . yes O(7) P(3) O(8) 107.7(3) . . . yes O(7) P(3) O(9) 99.5(2) . . . yes O(8) P(3) O(9) 107.3(3) . . . yes Pd(1) P(4) C(1) 112.4(2) . . . yes Pd(1) P(4) C(7) 116.3(2) . . . yes Pd(1) P(4) C(13) 110.6(2) . . . yes C(1) P(4) C(7) 108.8(3) . . . yes C(1) P(4) C(13) 105.3(3) . . . yes C(7) P(4) C(13) 102.5(3) . . . yes Pd(1) P(5) C(19) 108.3(2) . . . yes Pd(1) P(5) C(25) 109.4(2) . . . yes Pd(1) P(5) C(31) 123.2(2) . . . yes C(19) P(5) C(25) 107.5(3) . . . yes C(19) P(5) C(31) 103.3(3) . . . yes C(25) P(5) C(31) 104.2(3) . . . yes N(1) P(6) C(37) 107.1(3) . . . yes N(1) P(6) C(43) 114.0(3) . . . yes N(1) P(6) C(49) 113.2(3) . . . yes C(37) P(6) C(43) 105.7(3) . . . yes C(37) P(6) C(49) 107.7(3) . . . yes C(43) P(6) C(49) 108.7(3) . . . yes N(1) P(7) C(55) 115.0(3) . . . yes N(1) P(7) C(61) 110.6(3) . . . yes N(1) P(7) C(67) 107.4(3) . . . yes C(55) P(7) C(61) 107.0(3) . . . yes C(55) P(7) C(67) 109.3(3) . . . yes C(61) P(7) C(67) 107.3(3) . . . yes Pd(1) O(1) P(1) 127.5(2) . . . yes Pd(1) O(2) P(2) 130.6(3) . . . yes P(1) O(5) P(2) 122.5(3) . . . yes P(2) O(7) P(3) 127.1(3) . . . yes P(1) O(9) P(3) 130.1(3) . . . yes P(6) N(1) P(7) 137.5(4) . . . yes P(4) C(1) C(2) 117.4(5) . . . yes P(4) C(1) C(6) 124.2(5) . . . yes C(2) C(1) C(6) 118.4(6) . . . yes C(1) C(2) C(3) 120.3(6) . . . yes C(2) C(3) C(4) 120.4(7) . . . yes C(3) C(4) C(5) 120.2(7) . . . yes C(4) C(5) C(6) 120.3(7) . . . yes C(1) C(6) C(5) 120.3(7) . . . yes P(4) C(7) C(8) 120.8(5) . . . yes P(4) C(7) C(12) 120.8(5) . . . yes C(8) C(7) C(12) 118.4(6) . . . yes C(7) C(8) C(9) 120.6(7) . . . yes C(8) C(9) C(10) 120.9(7) . . . yes C(9) C(10) C(11) 118.6(7) . . . yes C(10) C(11) C(12) 120.6(7) . . . yes C(7) C(12) C(11) 120.7(7) . . . yes P(4) C(13) C(14) 118.6(5) . . . yes P(4) C(13) C(18) 123.1(6) . . . yes C(14) C(13) C(18) 118.2(7) . . . yes C(13) C(14) C(15) 120.0(8) . . . yes C(14) C(15) C(16) 120.6(9) . . . yes C(15) C(16) C(17) 119.7(9) . . . yes C(16) C(17) C(18) 120.2(9) . . . yes C(13) C(18) C(17) 121.2(8) . . . yes P(5) C(19) C(20) 119.2(5) . . . yes P(5) C(19) C(24) 121.6(5) . . . yes C(20) C(19) C(24) 119.1(7) . . . yes C(19) C(20) C(21) 120.3(7) . . . yes C(20) C(21) C(22) 120.2(7) . . . yes C(21) C(22) C(23) 119.9(7) . . . yes C(22) C(23) C(24) 120.8(7) . . . yes C(19) C(24) C(23) 119.7(7) . . . yes P(5) C(25) C(26) 119.1(5) . . . yes P(5) C(25) C(30) 121.5(5) . . . yes C(26) C(25) C(30) 119.3(6) . . . yes C(25) C(26) C(27) 121.4(6) . . . yes C(26) C(27) C(28) 118.6(7) . . . yes C(27) C(28) C(29) 120.4(7) . . . yes C(28) C(29) C(30) 121.5(7) . . . yes C(25) C(30) C(29) 118.8(7) . . . yes P(5) C(31) C(32) 120.3(6) . . . yes P(5) C(31) C(36) 120.7(6) . . . yes C(32) C(31) C(36) 119.0(7) . . . yes C(31) C(32) C(33) 120.6(8) . . . yes C(32) C(33) C(34) 119.3(8) . . . yes C(33) C(34) C(35) 121.1(8) . . . yes C(34) C(35) C(36) 119.4(8) . . . yes C(31) C(36) C(35) 120.6(8) . . . yes P(6) C(37) C(38) 121.4(5) . . . yes P(6) C(37) C(42) 120.9(5) . . . yes C(38) C(37) C(42) 117.6(6) . . . yes C(37) C(38) C(39) 121.7(6) . . . yes C(38) C(39) C(40) 119.1(7) . . . yes C(39) C(40) C(41) 120.4(7) . . . yes C(40) C(41) C(42) 119.8(7) . . . yes C(37) C(42) C(41) 121.4(7) . . . yes P(6) C(43) C(44) 120.2(6) . . . yes P(6) C(43) C(48) 119.9(6) . . . yes C(44) C(43) C(48) 119.7(7) . . . yes C(43) C(44) C(45) 119.2(10) . . . yes C(44) C(45) C(46) 119(1) . . . yes C(45) C(46) C(47) 122(1) . . . yes C(46) C(47) C(48) 118(1) . . . yes C(43) C(48) C(47) 121.0(10) . . . yes P(6) C(49) C(50) 119.5(5) . . . yes P(6) C(49) C(54) 121.4(6) . . . yes C(50) C(49) C(54) 119.0(7) . . . yes C(49) C(50) C(51) 120.3(7) . . . yes C(50) C(51) C(52) 119.5(8) . . . yes C(51) C(52) C(53) 120.5(8) . . . yes C(52) C(53) C(54) 120.9(8) . . . yes C(49) C(54) C(53) 119.8(8) . . . yes P(7) C(55) C(56) 120.1(5) . . . yes P(7) C(55) C(60) 119.8(5) . . . yes C(56) C(55) C(60) 119.3(6) . . . yes C(55) C(56) C(57) 119.7(7) . . . yes C(56) C(57) C(58) 120.2(7) . . . yes C(57) C(58) C(59) 120.5(7) . . . yes C(58) C(59) C(60) 120.2(7) . . . yes C(55) C(60) C(59) 120.1(7) . . . yes P(7) C(61) C(62) 121.0(6) . . . yes P(7) C(61) C(66) 120.0(5) . . . yes C(62) C(61) C(66) 119.0(7) . . . yes C(61) C(62) C(63) 120.1(7) . . . yes C(62) C(63) C(64) 120.3(8) . . . yes C(63) C(64) C(65) 120.3(8) . . . yes C(64) C(65) C(66) 120.2(8) . . . yes C(61) C(66) C(65) 120.1(7) . . . yes P(7) C(67) C(68) 118.7(5) . . . yes P(7) C(67) C(72) 122.5(5) . . . yes C(68) C(67) C(72) 118.7(6) . . . yes C(67) C(68) C(69) 119.7(7) . . . yes C(68) C(69) C(70) 120.4(8) . . . yes C(69) C(70) C(71) 120.1(7) . . . yes C(70) C(71) C(72) 119.9(7) . . . yes C(67) C(72) C(71) 121.0(7) . . . yes Cl(1) C(73) Cl(2) 111.9(7) . . . yes Cl(3) C(74) Cl(4) 113.8(6) . . . yes Cl(5) C(75) Cl(5) 124(1) . . 2_666 yes Cl(5) C(75) C(75) 56(1) . . 2_666 yes Cl(5) C(75) C(75) 67(1) 2_666 . 2_666 yes #------------------------------------------------------------------------------ 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 Pd(1) P(4) C(1) C(2) -44.2(6) . . . . yes Pd(1) P(4) C(1) C(6) 137.1(5) . . . . yes Pd(1) P(4) C(7) C(8) -4.5(7) . . . . yes Pd(1) P(4) C(7) C(12) 173.1(5) . . . . yes Pd(1) P(4) C(13) C(14) -74.8(6) . . . . yes Pd(1) P(4) C(13) C(18) 101.8(6) . . . . yes Pd(1) P(5) C(19) C(20) -39.6(6) . . . . yes Pd(1) P(5) C(19) C(24) 143.1(6) . . . . yes Pd(1) P(5) C(25) C(26) -10.9(6) . . . . yes Pd(1) P(5) C(25) C(30) 170.0(5) . . . . yes Pd(1) P(5) C(31) C(32) -87.4(6) . . . . yes Pd(1) P(5) C(31) C(36) 93.3(6) . . . . yes Pd(1) O(1) P(1) O(4) 174.4(3) . . . . yes Pd(1) O(1) P(1) O(5) 49.8(4) . . . . yes Pd(1) O(1) P(1) O(9) -59.0(4) . . . . yes Pd(1) O(2) P(2) O(5) -43.2(4) . . . . yes Pd(1) O(2) P(2) O(6) -168.4(3) . . . . yes Pd(1) O(2) P(2) O(7) 65.1(4) . . . . yes Cl(5) C(75) Cl(5) C(75) 0.0 . . 2_666 2_666 yes Cl(5) C(75) C(75) Cl(5) 180.0 . . 2_666 2_666 yes Cl(5) C(75) Cl(5) C(75) 0.0 . 2_666 2_666 . yes Cl(5) C(75) C(75) Cl(5) 180.0 . 2_666 . 2_666 yes P(1) O(1) Pd(1) P(4) -84(1) . . . . yes P(1) O(1) Pd(1) P(5) 153.9(3) . . . . yes P(1) O(1) Pd(1) O(2) -33.0(3) . . . . yes P(1) O(5) P(2) O(2) 58.3(4) . . . . yes P(1) O(5) P(2) O(6) -171.5(3) . . . . yes P(1) O(5) P(2) O(7) -56.0(3) . . . . yes P(1) O(9) P(3) O(3) -72.5(4) . . . . yes P(1) O(9) P(3) O(7) 40.8(4) . . . . yes P(1) O(9) P(3) O(8) 152.8(4) . . . . yes P(2) O(2) Pd(1) P(4) -153.0(3) . . . . yes P(2) O(2) Pd(1) P(5) 75.4(9) . . . . yes P(2) O(2) Pd(1) O(1) 29.9(3) . . . . yes P(2) O(5) P(1) O(1) -62.3(4) . . . . yes P(2) O(5) P(1) O(4) 168.1(3) . . . . yes P(2) O(5) P(1) O(9) 51.8(3) . . . . yes P(2) O(7) P(3) O(3) 68.0(4) . . . . yes P(2) O(7) P(3) O(8) -157.2(4) . . . . yes P(2) O(7) P(3) O(9) -45.5(4) . . . . yes P(3) O(7) P(2) O(2) -58.7(4) . . . . yes P(3) O(7) P(2) O(5) 53.8(4) . . . . yes P(3) O(7) P(2) O(6) 169.8(3) . . . . yes P(3) O(9) P(1) O(1) 67.6(4) . . . . yes P(3) O(9) P(1) O(4) -161.2(4) . . . . yes P(3) O(9) P(1) O(5) -45.0(4) . . . . yes P(4) Pd(1) P(5) C(19) 137.6(2) . . . . yes P(4) Pd(1) P(5) C(25) -105.5(2) . . . . yes P(4) Pd(1) P(5) C(31) 17.2(3) . . . . yes P(4) C(1) C(2) C(3) -177.0(6) . . . . yes P(4) C(1) C(6) C(5) 177.6(6) . . . . yes P(4) C(7) C(8) C(9) -177.8(6) . . . . yes P(4) C(7) C(12) C(11) 179.2(7) . . . . yes P(4) C(13) C(14) C(15) 177.4(6) . . . . yes P(4) C(13) C(18) C(17) -176.8(8) . . . . yes P(5) Pd(1) P(4) C(1) -59.2(2) . . . . yes P(5) Pd(1) P(4) C(7) 67.1(2) . . . . yes P(5) Pd(1) P(4) C(13) -176.6(2) . . . . yes P(5) C(19) C(20) C(21) -178.0(6) . . . . yes P(5) C(19) C(24) C(23) 177.6(6) . . . . yes P(5) C(25) C(26) C(27) 178.8(5) . . . . yes P(5) C(25) C(30) C(29) -179.9(6) . . . . yes P(5) C(31) C(32) C(33) -178.3(6) . . . . yes P(5) C(31) C(36) C(35) 178.6(6) . . . . yes P(6) N(1) P(7) C(55) -5.8(7) . . . . yes P(6) N(1) P(7) C(61) 115.5(5) . . . . yes P(6) N(1) P(7) C(67) -127.7(5) . . . . yes P(6) C(37) C(38) C(39) -179.0(6) . . . . yes P(6) C(37) C(42) C(41) 176.8(6) . . . . yes P(6) C(43) C(44) C(45) -172.0(7) . . . . yes P(6) C(43) C(48) C(47) 173.1(7) . . . . yes P(6) C(49) C(50) C(51) 173.9(6) . . . . yes P(6) C(49) C(54) C(53) -173.8(6) . . . . yes P(7) N(1) P(6) C(37) -171.6(5) . . . . yes P(7) N(1) P(6) C(43) 71.9(6) . . . . yes P(7) N(1) P(6) C(49) -53.0(6) . . . . yes P(7) C(55) C(56) C(57) 168.6(6) . . . . yes P(7) C(55) C(60) C(59) -170.1(6) . . . . yes P(7) C(61) C(62) C(63) 179.7(6) . . . . yes P(7) C(61) C(66) C(65) -179.8(6) . . . . yes P(7) C(67) C(68) C(69) -175.1(6) . . . . yes P(7) C(67) C(72) C(71) 174.8(6) . . . . yes O(1) Pd(1) P(4) C(1) 179(1) . . . . yes O(1) Pd(1) P(4) C(7) -54(1) . . . . yes O(1) Pd(1) P(4) C(13) 61(1) . . . . yes O(1) Pd(1) P(5) C(19) -45.5(3) . . . . yes O(1) Pd(1) P(5) C(25) 71.3(3) . . . . yes O(1) Pd(1) P(5) C(31) -166.0(3) . . . . yes O(2) Pd(1) P(4) C(1) 128.1(3) . . . . yes O(2) Pd(1) P(4) C(7) -105.6(3) . . . . yes O(2) Pd(1) P(4) C(13) 10.7(3) . . . . yes O(2) Pd(1) P(5) C(19) -91.3(8) . . . . yes O(2) Pd(1) P(5) C(25) 25.5(8) . . . . yes O(2) Pd(1) P(5) C(31) 148.2(8) . . . . yes N(1) P(6) C(37) C(38) -163.0(6) . . . . yes N(1) P(6) C(37) C(42) 20.2(7) . . . . yes N(1) P(6) C(43) C(44) -165.1(6) . . . . yes N(1) P(6) C(43) C(48) 20.4(7) . . . . yes N(1) P(6) C(49) C(50) -80.5(6) . . . . yes N(1) P(6) C(49) C(54) 95.1(6) . . . . yes N(1) P(7) C(55) C(56) -79.5(6) . . . . yes N(1) P(7) C(55) C(60) 90.5(6) . . . . yes N(1) P(7) C(61) C(62) -1.3(7) . . . . yes N(1) P(7) C(61) C(66) 178.5(6) . . . . yes N(1) P(7) C(67) C(68) -14.6(6) . . . . yes N(1) P(7) C(67) C(72) 169.1(6) . . . . yes C(1) P(4) C(7) C(8) 123.5(6) . . . . yes C(1) P(4) C(7) C(12) -58.9(7) . . . . yes C(1) P(4) C(13) C(14) 163.6(6) . . . . yes C(1) P(4) C(13) C(18) -19.8(7) . . . . yes C(1) C(2) C(3) C(4) -1(1) . . . . yes C(1) C(6) C(5) C(4) 0(1) . . . . yes C(2) C(1) P(4) C(7) -174.5(5) . . . . yes C(2) C(1) P(4) C(13) 76.3(6) . . . . yes C(2) C(1) C(6) C(5) -1(1) . . . . yes C(2) C(3) C(4) C(5) 0(1) . . . . yes C(3) C(2) C(1) C(6) 1(1) . . . . yes C(3) C(4) C(5) C(6) 0(1) . . . . yes C(6) C(1) P(4) C(7) 6.8(7) . . . . yes C(6) C(1) P(4) C(13) -102.4(6) . . . . yes C(7) P(4) C(13) C(14) 49.8(6) . . . . yes C(7) P(4) C(13) C(18) -133.6(7) . . . . yes C(7) C(8) C(9) C(10) -2(1) . . . . yes C(7) C(12) C(11) C(10) 0(1) . . . . yes C(8) C(7) P(4) C(13) -125.3(6) . . . . yes C(8) C(7) C(12) C(11) -3(1) . . . . yes C(8) C(9) C(10) C(11) -1(1) . . . . yes C(9) C(8) C(7) C(12) 4(1) . . . . yes C(9) C(10) C(11) C(12) 3(1) . . . . yes C(12) C(7) P(4) C(13) 52.3(7) . . . . yes C(13) C(14) C(15) C(16) 0(1) . . . . yes C(13) C(18) C(17) C(16) 0(1) . . . . yes C(14) C(13) C(18) C(17) 0(1) . . . . yes C(14) C(15) C(16) C(17) 0(1) . . . . yes C(15) C(14) C(13) C(18) 0(1) . . . . yes C(15) C(16) C(17) C(18) 0(1) . . . . yes C(19) P(5) C(25) C(26) 106.5(6) . . . . yes C(19) P(5) C(25) C(30) -72.6(6) . . . . yes C(19) P(5) C(31) C(32) 149.9(6) . . . . yes C(19) P(5) C(31) C(36) -29.4(6) . . . . yes C(19) C(20) C(21) C(22) 0(1) . . . . yes C(19) C(24) C(23) C(22) 0(1) . . . . yes C(20) C(19) P(5) C(25) -157.7(6) . . . . yes C(20) C(19) P(5) C(31) 92.5(6) . . . . yes C(20) C(19) C(24) C(23) 0(1) . . . . yes C(20) C(21) C(22) C(23) 0(1) . . . . yes C(21) C(20) C(19) C(24) 0(1) . . . . yes C(21) C(22) C(23) C(24) 0(1) . . . . yes C(24) C(19) P(5) C(25) 25.1(7) . . . . yes C(24) C(19) P(5) C(31) -84.7(6) . . . . yes C(25) P(5) C(31) C(32) 37.7(7) . . . . yes C(25) P(5) C(31) C(36) -141.6(6) . . . . yes C(25) C(26) C(27) C(28) 1(1) . . . . yes C(25) C(30) C(29) C(28) 0(1) . . . . yes C(26) C(25) P(5) C(31) -144.3(5) . . . . yes C(26) C(25) C(30) C(29) 1(1) . . . . yes C(26) C(27) C(28) C(29) 0(1) . . . . yes C(27) C(26) C(25) C(30) -2(1) . . . . yes C(27) C(28) C(29) C(30) -1(1) . . . . yes C(30) C(25) P(5) C(31) 36.5(7) . . . . yes C(31) C(32) C(33) C(34) -1(1) . . . . yes C(31) C(36) C(35) C(34) 0(1) . . . . yes C(32) C(31) C(36) C(35) 0(1) . . . . yes C(32) C(33) C(34) C(35) 0(1) . . . . yes C(33) C(32) C(31) C(36) 1(1) . . . . yes C(33) C(34) C(35) C(36) 0(1) . . . . yes C(37) P(6) C(43) C(44) 77.5(7) . . . . yes C(37) P(6) C(43) C(48) -96.9(6) . . . . yes C(37) P(6) C(49) C(50) 37.7(6) . . . . yes C(37) P(6) C(49) C(54) -146.7(6) . . . . yes C(37) C(38) C(39) C(40) 2(1) . . . . yes C(37) C(42) C(41) C(40) 1(1) . . . . yes C(38) C(37) P(6) C(43) -41.1(7) . . . . yes C(38) C(37) P(6) C(49) 74.9(6) . . . . yes C(38) C(37) C(42) C(41) 0(1) . . . . yes C(38) C(39) C(40) C(41) -1(1) . . . . yes C(39) C(38) C(37) C(42) -2(1) . . . . yes C(39) C(40) C(41) C(42) 0(1) . . . . yes C(42) C(37) P(6) C(43) 142.1(6) . . . . yes C(42) C(37) P(6) C(49) -101.8(6) . . . . yes C(43) P(6) C(49) C(50) 151.7(6) . . . . yes C(43) P(6) C(49) C(54) -32.7(7) . . . . yes C(43) C(44) C(45) C(46) -1(1) . . . . yes C(43) C(48) C(47) C(46) 0(1) . . . . yes C(44) C(43) P(6) C(49) -37.9(7) . . . . yes C(44) C(43) C(48) C(47) -1(1) . . . . yes C(44) C(45) C(46) C(47) 0(1) . . . . yes C(45) C(44) C(43) C(48) 2(1) . . . . yes C(45) C(46) C(47) C(48) 1(1) . . . . yes C(48) C(43) P(6) C(49) 147.7(6) . . . . yes C(49) C(50) C(51) C(52) 0(1) . . . . yes C(49) C(54) C(53) C(52) 0(1) . . . . yes C(50) C(49) C(54) C(53) 1(1) . . . . yes C(50) C(51) C(52) C(53) 1(1) . . . . yes C(51) C(50) C(49) C(54) -1(1) . . . . yes C(51) C(52) C(53) C(54) -1(1) . . . . yes C(55) P(7) C(61) C(62) 124.6(6) . . . . yes C(55) P(7) C(61) C(66) -55.6(7) . . . . yes C(55) P(7) C(67) C(68) -139.9(6) . . . . yes C(55) P(7) C(67) C(72) 43.8(7) . . . . yes C(55) C(56) C(57) C(58) 1(1) . . . . yes C(55) C(60) C(59) C(58) 1(1) . . . . yes C(56) C(55) P(7) C(61) 157.3(6) . . . . yes C(56) C(55) P(7) C(67) 41.4(7) . . . . yes C(56) C(55) C(60) C(59) 0(1) . . . . yes C(56) C(57) C(58) C(59) 0(1) . . . . yes C(57) C(56) C(55) C(60) -1(1) . . . . yes C(57) C(58) C(59) C(60) 0(1) . . . . yes C(60) C(55) P(7) C(61) -32.7(6) . . . . yes C(60) C(55) P(7) C(67) -148.6(5) . . . . yes C(61) P(7) C(67) C(68) 104.3(6) . . . . yes C(61) P(7) C(67) C(72) -72.0(6) . . . . yes C(61) C(62) C(63) C(64) 0(1) . . . . yes C(61) C(66) C(65) C(64) 0(1) . . . . yes C(62) C(61) P(7) C(67) -118.1(6) . . . . yes C(62) C(61) C(66) C(65) 0(1) . . . . yes C(62) C(63) C(64) C(65) -1(1) . . . . yes C(63) C(62) C(61) C(66) 0(1) . . . . yes C(63) C(64) C(65) C(66) 1(1) . . . . yes C(66) C(61) P(7) C(67) 61.7(7) . . . . yes C(67) C(68) C(69) C(70) 0(1) . . . . yes C(67) C(72) C(71) C(70) 0(1) . . . . yes C(68) C(67) C(72) C(71) -1(1) . . . . yes C(68) C(69) C(70) C(71) -2(1) . . . . yes C(69) C(68) C(67) C(72) 1(1) . . . . yes C(69) C(70) C(71) C(72) 2(1) . . . . yes C(75) Cl(5) C(75) Cl(5) 0.0 . . 2_666 2_666 yes C(75) Cl(5) C(75) Cl(5) 0.0 . 2_666 2_666 . yes C(75) Cl(5) C(75) Cl(5) 0.0 . 2_666 2_666 . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(47) 3.49(1) . 1_445 ? Cl(1) C(48) 3.563(9) . 1_445 ? Cl(2) C(34) 3.561(10) . 1_545 ? Cl(4) C(45) 3.59(1) . 1_545 ? O(1) C(41) 3.590(9) . 2_665 ? O(2) C(39) 3.376(8) . 1_445 ? O(3) C(71) 3.273(9) . . ? O(3) C(75) 3.48(2) . . ? O(4) C(42) 3.307(9) . 2_665 ? O(4) C(27) 3.307(8) . 2_555 ? O(4) C(41) 3.45(1) . 2_665 ? O(4) C(50) 3.529(9) . 2_665 ? O(4) C(28) 3.560(10) . 2_555 ? O(6) C(73) 3.20(1) . . ? O(6) C(58) 3.267(9) . 1_545 ? O(6) C(59) 3.572(9) . 1_545 ? O(7) C(74) 3.02(1) . . ? O(8) C(70) 3.416(9) . . ? O(8) C(10) 3.454(9) . 1_655 ? O(8) C(75) 3.49(2) . . ? O(9) C(63) 3.457(10) . 2_665 ? O(9) C(52) 3.55(1) . 1_545 ? C(22) C(65) 3.53(1) . . ? C(26) C(39) 3.484(9) . 1_445 ? C(26) C(41) 3.582(9) . 2_665 ? C(27) C(40) 3.53(1) . 2_665 ? C(39) C(73) 3.46(1) . 1_665 ? C(51) C(51) 3.35(2) . 2_675 ? C(52) C(63) 3.59(1) . 2_675 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_(PPN)[Pd(P3O9)(PMePh2)2](2) _database_code_CSD 202874 _audit_creation_date 'Thu Apr 3 14:01:19 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C64 H59 N2 O9 P7 Pd ' _chemical_formula_moiety (PPN)[Pd(P3O9)(PMePh2)2] _chemical_formula_weight 1323.39 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.690(6) _cell_length_b 14.844(4) _cell_length_c 18.925(5) _cell_angle_alpha 106.07(2) _cell_angle_beta 97.30(4) _cell_angle_gamma 109.98(3) _cell_volume 3121(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.9 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour paleyellowprismatic _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 14880 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9985 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.28 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; for calculating R-factor (gt). ; _reflns_number_total 14327 _reflns_number_gt 9596 _reflns_threshold_criterion F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0354 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9596 _refine_ls_number_parameters 748 _refine_ls_goodness_of_fit_ref 1.408 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_shift/su_max 0.0365 _refine_diff_density_max 0.43 _refine_diff_density_min -0.32 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.14794(2) 0.22906(2) 0.95014(1) 0.02878(6) Uani 1.00 d . . . P(1) P -0.06148(6) 0.17596(6) 0.81010(4) 0.0320(2) Uani 1.00 d . . . P(2) P 0.05520(7) 0.04137(6) 0.78891(4) 0.0321(2) Uani 1.00 d . . . P(3) P 0.14705(7) 0.22700(7) 0.75570(5) 0.0411(2) Uani 1.00 d . . . P(4) P 0.31397(6) 0.22447(6) 1.00021(4) 0.0310(2) Uani 1.00 d . . . P(5) P 0.14593(7) 0.35486(6) 1.04738(5) 0.0378(2) Uani 1.00 d . . . P(6) P 0.32335(7) 0.67664(6) 1.54269(4) 0.0344(2) Uani 1.00 d . . . P(7) P 0.28048(7) 0.71010(6) 1.39791(4) 0.0323(2) Uani 1.00 d . . . O(1) O -0.0044(2) 0.2284(1) 0.8937(1) 0.0372(6) Uani 1.00 d . . . O(2) O 0.1248(2) 0.0886(1) 0.8703(1) 0.0351(6) Uani 1.00 d . . . O(3) O 0.2293(2) 0.2878(2) 0.8302(1) 0.0515(7) Uani 1.00 d . . . O(4) O -0.1785(2) 0.1691(2) 0.7852(1) 0.0434(6) Uani 1.00 d . . . O(5) O -0.0606(2) 0.0637(1) 0.7863(1) 0.0325(5) Uani 1.00 d . . . O(6) O 0.0248(2) -0.0671(1) 0.7509(1) 0.0476(7) Uani 1.00 d . . . O(7) O 0.1193(2) 0.1060(2) 0.7407(1) 0.0388(6) Uani 1.00 d . . . O(8) O 0.1681(2) 0.2473(2) 0.6864(1) 0.0642(9) Uani 1.00 d . . . O(9) O 0.0200(2) 0.2266(2) 0.7624(1) 0.0399(6) Uani 1.00 d . . . N(1) N 0.3300(2) 0.6696(2) 1.4585(1) 0.0380(7) Uani 1.00 d . . . N(2) N 0.3272(6) 0.7865(6) 1.8492(6) 0.252(5) Uani 1.00 d . . . C(1) C 0.2911(3) 0.1129(2) 1.0278(2) 0.0344(8) Uani 1.00 d . . . C(2) C 0.3787(3) 0.0795(3) 1.0393(2) 0.049(1) Uani 1.00 d . . . C(3) C 0.3579(4) -0.0070(3) 1.0602(2) 0.060(1) Uani 1.00 d . . . C(4) C 0.2525(4) -0.0581(3) 1.0702(2) 0.062(1) Uani 1.00 d . . . C(5) C 0.1648(3) -0.0259(3) 1.0582(2) 0.056(1) Uani 1.00 d . . . C(6) C 0.1833(3) 0.0588(2) 1.0366(2) 0.0426(9) Uani 1.00 d . . . C(7) C 0.4210(2) 0.3329(2) 1.0776(2) 0.0344(8) Uani 1.00 d . . . C(8) C 0.4572(3) 0.4275(2) 1.0683(2) 0.0379(9) Uani 1.00 d . . . C(9) C 0.5407(3) 0.5123(2) 1.1240(2) 0.0468(10) Uani 1.00 d . . . C(10) C 0.5902(3) 0.5038(3) 1.1898(2) 0.056(1) Uani 1.00 d . . . C(11) C 0.5550(3) 0.4112(3) 1.1997(2) 0.064(1) Uani 1.00 d . . . C(12) C 0.4701(3) 0.3252(2) 1.1440(2) 0.050(1) Uani 1.00 d . . . C(13) C 0.3896(3) 0.2107(3) 0.9254(2) 0.0437(9) Uani 1.00 d . . . C(14) C 0.2073(3) 0.4808(2) 1.0407(2) 0.0406(9) Uani 1.00 d . . . C(15) C 0.2389(3) 0.4910(2) 0.9753(2) 0.0427(9) Uani 1.00 d . . . C(16) C 0.2751(3) 0.5855(3) 0.9657(2) 0.055(1) Uani 1.00 d . . . C(17) C 0.2799(3) 0.6696(3) 1.0224(3) 0.060(1) Uani 1.00 d . . . C(18) C 0.2483(3) 0.6609(3) 1.0876(2) 0.065(1) Uani 1.00 d . . . C(19) C 0.2111(3) 0.5672(3) 1.0972(2) 0.055(1) Uani 1.00 d . . . C(20) C 0.1996(3) 0.3580(2) 1.1420(2) 0.0406(9) Uani 1.00 d . . . C(21) C 0.2906(3) 0.4395(2) 1.1973(2) 0.0497(10) Uani 1.00 d . . . C(22) C 0.3240(4) 0.4326(3) 1.2675(2) 0.066(1) Uani 1.00 d . . . C(23) C 0.2693(4) 0.3465(3) 1.2832(2) 0.074(1) Uani 1.00 d . . . C(24) C 0.1785(4) 0.2648(3) 1.2292(2) 0.070(1) Uani 1.00 d . . . C(25) C 0.1449(3) 0.2708(3) 1.1593(2) 0.054(1) Uani 1.00 d . . . C(26) C -0.0034(3) 0.3361(3) 1.0452(2) 0.057(1) Uani 1.00 d . . . C(27) C 0.4586(3) 0.7649(2) 1.6080(2) 0.0433(9) Uani 1.00 d . . . C(28) C 0.4725(3) 0.7808(3) 1.6849(2) 0.068(1) Uani 1.00 d . . . C(29) C 0.5759(4) 0.8512(3) 1.7357(2) 0.093(2) Uani 1.00 d . . . C(30) C 0.6640(4) 0.9040(4) 1.7098(3) 0.103(2) Uani 1.00 d . . . C(31) C 0.6517(4) 0.8878(4) 1.6341(3) 0.097(2) Uani 1.00 d . . . C(32) C 0.5484(3) 0.8188(3) 1.5828(2) 0.063(1) Uani 1.00 d . . . C(33) C 0.2985(3) 0.5536(2) 1.5516(2) 0.0379(8) Uani 1.00 d . . . C(34) C 0.2449(3) 0.5241(3) 1.6060(2) 0.049(1) Uani 1.00 d . . . C(35) C 0.2310(3) 0.4304(3) 1.6130(2) 0.064(1) Uani 1.00 d . . . C(36) C 0.2708(4) 0.3674(3) 1.5670(3) 0.074(1) Uani 1.00 d . . . C(37) C 0.3237(4) 0.3956(3) 1.5136(3) 0.073(2) Uani 1.00 d . . . C(38) C 0.3378(3) 0.4892(3) 1.5051(2) 0.055(1) Uani 1.00 d . . . C(39) C 0.2105(3) 0.7130(2) 1.5722(2) 0.0375(8) Uani 1.00 d . . . C(40) C 0.2332(3) 0.8110(3) 1.6201(2) 0.054(1) Uani 1.00 d . . . C(41) C 0.1438(4) 0.8382(3) 1.6357(2) 0.070(1) Uani 1.00 d . . . C(42) C 0.0316(4) 0.7698(3) 1.6048(2) 0.066(1) Uani 1.00 d . . . C(43) C 0.0074(3) 0.6733(3) 1.5567(2) 0.057(1) Uani 1.00 d . . . C(44) C 0.0963(3) 0.6450(2) 1.5399(2) 0.0453(10) Uani 1.00 d . . . C(45) C 0.2451(3) 0.8186(2) 1.4368(2) 0.0373(9) Uani 1.00 d . . . C(46) C 0.3358(3) 0.9091(2) 1.4857(2) 0.050(1) Uani 1.00 d . . . C(47) C 0.3142(4) 0.9929(3) 1.5209(2) 0.066(1) Uani 1.00 d . . . C(48) C 0.2044(5) 0.9888(3) 1.5082(3) 0.077(2) Uani 1.00 d . . . C(49) C 0.1144(4) 0.9017(3) 1.4601(3) 0.075(2) Uani 1.00 d . . . C(50) C 0.1347(3) 0.8157(3) 1.4248(2) 0.052(1) Uani 1.00 d . . . C(51) C 0.3909(3) 0.7513(2) 1.3495(2) 0.0375(8) Uani 1.00 d . . . C(52) C 0.3868(3) 0.8157(3) 1.3095(2) 0.056(1) Uani 1.00 d . . . C(53) C 0.4732(4) 0.8470(4) 1.2725(2) 0.075(2) Uani 1.00 d . . . C(54) C 0.5617(3) 0.8140(4) 1.2758(2) 0.072(1) Uani 1.00 d . . . C(55) C 0.5670(3) 0.7507(3) 1.3157(2) 0.061(1) Uani 1.00 d . . . C(56) C 0.4820(3) 0.7193(2) 1.3524(2) 0.0453(10) Uani 1.00 d . . . C(57) C 0.1523(2) 0.6095(2) 1.3313(2) 0.0333(8) Uani 1.00 d . . . C(58) C 0.1070(3) 0.5157(2) 1.3407(2) 0.0462(10) Uani 1.00 d . . . C(59) C 0.0047(3) 0.4407(3) 1.2920(2) 0.056(1) Uani 1.00 d . . . C(60) C -0.0529(3) 0.4594(3) 1.2345(2) 0.056(1) Uani 1.00 d . . . C(61) C -0.0071(3) 0.5513(3) 1.2238(2) 0.054(1) Uani 1.00 d . . . C(62) C 0.0960(3) 0.6268(2) 1.2716(2) 0.0443(9) Uani 1.00 d . . . C(63) C 0.2702(5) 0.8287(5) 1.8465(4) 0.109(2) Uani 1.00 d . . . C(64) C 0.1925(6) 0.8722(5) 1.8472(3) 0.135(3) Uani 1.00 d . . . H(1) H 0.4528 0.1152 1.0330 0.0594 Uiso 1.00 calc . . . H(2) H 0.4181 -0.0304 1.0675 0.0722 Uiso 1.00 calc . . . H(3) H 0.2397 -0.1159 1.0855 0.0750 Uiso 1.00 calc . . . H(4) H 0.0909 -0.0619 1.0647 0.0675 Uiso 1.00 calc . . . H(5) H 0.1219 0.0802 1.0278 0.0509 Uiso 1.00 calc . . . H(6) H 0.4237 0.4337 1.0230 0.0454 Uiso 1.00 calc . . . H(7) H 0.5645 0.5767 1.1173 0.0561 Uiso 1.00 calc . . . H(8) H 0.6485 0.5621 1.2281 0.0675 Uiso 1.00 calc . . . H(9) H 0.5888 0.4056 1.2452 0.0770 Uiso 1.00 calc . . . H(10) H 0.4458 0.2613 1.1515 0.0597 Uiso 1.00 calc . . . H(11) H 0.4142 0.2719 0.9139 0.0524 Uiso 1.00 calc . . . H(12) H 0.3392 0.1556 0.8814 0.0524 Uiso 1.00 calc . . . H(13) H 0.4550 0.1976 0.9417 0.0524 Uiso 1.00 calc . . . H(14) H 0.2361 0.4331 0.9366 0.0512 Uiso 1.00 calc . . . H(15) H 0.2962 0.5921 0.9204 0.0658 Uiso 1.00 calc . . . H(16) H 0.3056 0.7343 1.0162 0.0724 Uiso 1.00 calc . . . H(17) H 0.2519 0.7194 1.1262 0.0774 Uiso 1.00 calc . . . H(18) H 0.1880 0.5610 1.1421 0.0654 Uiso 1.00 calc . . . H(19) H 0.3299 0.4997 1.1869 0.0596 Uiso 1.00 calc . . . H(20) H 0.3858 0.4886 1.3052 0.0790 Uiso 1.00 calc . . . H(21) H 0.2937 0.3428 1.3315 0.0882 Uiso 1.00 calc . . . H(22) H 0.1396 0.2051 1.2402 0.0834 Uiso 1.00 calc . . . H(23) H 0.0830 0.2144 1.1220 0.0647 Uiso 1.00 calc . . . H(24) H -0.0062 0.3878 1.0869 0.0688 Uiso 1.00 calc . . . H(25) H -0.0440 0.2710 1.0485 0.0688 Uiso 1.00 calc . . . H(26) H -0.0383 0.3396 0.9992 0.0688 Uiso 1.00 calc . . . H(27) H 0.4112 0.7436 1.7028 0.0820 Uiso 1.00 calc . . . H(28) H 0.5852 0.8626 1.7885 0.1118 Uiso 1.00 calc . . . H(29) H 0.7347 0.9523 1.7447 0.1237 Uiso 1.00 calc . . . H(30) H 0.7141 0.9240 1.6164 0.1167 Uiso 1.00 calc . . . H(31) H 0.5396 0.8085 1.5303 0.0753 Uiso 1.00 calc . . . H(32) H 0.2179 0.5681 1.6383 0.0589 Uiso 1.00 calc . . . H(33) H 0.1937 0.4099 1.6498 0.0771 Uiso 1.00 calc . . . H(34) H 0.2617 0.3035 1.5722 0.0889 Uiso 1.00 calc . . . H(35) H 0.3512 0.3514 1.4819 0.0871 Uiso 1.00 calc . . . H(36) H 0.3742 0.5086 1.4678 0.0663 Uiso 1.00 calc . . . H(37) H 0.3108 0.8589 1.6419 0.0649 Uiso 1.00 calc . . . H(38) H 0.1597 0.9052 1.6683 0.0839 Uiso 1.00 calc . . . H(39) H -0.0299 0.7893 1.6168 0.0789 Uiso 1.00 calc . . . H(40) H -0.0705 0.6261 1.5350 0.0679 Uiso 1.00 calc . . . H(41) H 0.0796 0.5784 1.5061 0.0543 Uiso 1.00 calc . . . H(42) H 0.4127 0.9124 1.4946 0.0598 Uiso 1.00 calc . . . H(43) H 0.3760 1.0537 1.5541 0.0792 Uiso 1.00 calc . . . H(44) H 0.1900 1.0468 1.5330 0.0933 Uiso 1.00 calc . . . H(45) H 0.0381 0.8998 1.4508 0.0899 Uiso 1.00 calc . . . H(46) H 0.0722 0.7549 1.3923 0.0630 Uiso 1.00 calc . . . H(47) H 0.3254 0.8384 1.3073 0.0674 Uiso 1.00 calc . . . H(48) H 0.4707 0.8912 1.2449 0.0897 Uiso 1.00 calc . . . H(49) H 0.6203 0.8353 1.2503 0.0862 Uiso 1.00 calc . . . H(50) H 0.6290 0.7287 1.3180 0.0726 Uiso 1.00 calc . . . H(51) H 0.4854 0.6754 1.3800 0.0542 Uiso 1.00 calc . . . H(52) H 0.1461 0.5029 1.3807 0.0553 Uiso 1.00 calc . . . H(53) H -0.0258 0.3760 1.2981 0.0666 Uiso 1.00 calc . . . H(54) H -0.1244 0.4086 1.2022 0.0673 Uiso 1.00 calc . . . H(55) H -0.0463 0.5633 1.1835 0.0644 Uiso 1.00 calc . . . H(56) H 0.1279 0.6900 1.2637 0.0530 Uiso 1.00 calc . . . H(57) H 0.1849 0.8962 1.8976 0.1631 Uiso 1.00 calc . . . H(58) H 0.1199 0.8233 1.8153 0.1631 Uiso 1.00 calc . . . H(59) H 0.2182 0.9280 1.8294 0.1631 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0275(1) 0.0273(1) 0.0260(1) 0.00851(9) 0.00229(9) 0.00561(9) P(1) 0.0274(4) 0.0333(4) 0.0337(4) 0.0114(3) 0.0031(3) 0.0117(3) P(2) 0.0328(4) 0.0272(4) 0.0311(4) 0.0098(3) 0.0063(3) 0.0053(3) P(3) 0.0337(4) 0.0460(5) 0.0474(5) 0.0107(4) 0.0124(4) 0.0263(4) P(4) 0.0278(4) 0.0330(4) 0.0297(4) 0.0084(3) 0.0044(3) 0.0124(3) P(5) 0.0341(4) 0.0374(4) 0.0327(4) 0.0110(4) 0.0070(3) 0.0026(4) P(6) 0.0332(4) 0.0358(4) 0.0275(4) 0.0074(3) 0.0026(3) 0.0109(3) P(7) 0.0323(4) 0.0366(4) 0.0292(4) 0.0135(3) 0.0065(3) 0.0134(3) O(1) 0.035(1) 0.037(1) 0.034(1) 0.0161(9) 0.0010(9) 0.0047(9) O(2) 0.039(1) 0.032(1) 0.032(1) 0.0163(9) 0.0016(9) 0.0074(9) O(3) 0.037(1) 0.042(1) 0.060(2) 0.002(1) -0.001(1) 0.018(1) O(4) 0.030(1) 0.053(1) 0.046(1) 0.018(1) 0.0019(10) 0.016(1) O(5) 0.027(1) 0.028(1) 0.035(1) 0.0050(8) 0.0041(8) 0.0069(9) O(6) 0.056(1) 0.029(1) 0.048(1) 0.016(1) 0.010(1) 0.0012(10) O(7) 0.039(1) 0.042(1) 0.037(1) 0.0158(10) 0.0142(10) 0.0144(10) O(8) 0.059(2) 0.087(2) 0.067(2) 0.026(1) 0.031(1) 0.053(2) O(9) 0.036(1) 0.043(1) 0.049(1) 0.0167(10) 0.0128(10) 0.027(1) N(1) 0.042(1) 0.046(2) 0.030(1) 0.021(1) 0.009(1) 0.016(1) N(2) 0.145(6) 0.214(8) 0.41(1) 0.120(6) 0.028(7) 0.075(8) C(1) 0.040(2) 0.031(2) 0.029(2) 0.013(1) 0.006(1) 0.008(1) C(2) 0.047(2) 0.052(2) 0.055(2) 0.024(2) 0.011(2) 0.021(2) C(3) 0.072(3) 0.059(2) 0.065(3) 0.042(2) 0.011(2) 0.025(2) C(4) 0.094(3) 0.042(2) 0.057(2) 0.027(2) 0.019(2) 0.026(2) C(5) 0.066(2) 0.044(2) 0.062(2) 0.016(2) 0.023(2) 0.028(2) C(6) 0.046(2) 0.040(2) 0.044(2) 0.016(2) 0.013(2) 0.017(2) C(7) 0.028(2) 0.037(2) 0.031(2) 0.007(1) 0.002(1) 0.010(1) C(8) 0.033(2) 0.042(2) 0.039(2) 0.010(1) 0.007(1) 0.019(1) C(9) 0.043(2) 0.035(2) 0.055(2) 0.006(1) 0.011(2) 0.017(2) C(10) 0.046(2) 0.044(2) 0.052(2) 0.002(2) -0.007(2) 0.006(2) C(11) 0.070(3) 0.053(2) 0.045(2) 0.011(2) -0.019(2) 0.011(2) C(12) 0.059(2) 0.037(2) 0.041(2) 0.008(2) -0.006(2) 0.016(2) C(13) 0.037(2) 0.055(2) 0.042(2) 0.017(2) 0.012(1) 0.019(2) C(14) 0.038(2) 0.036(2) 0.043(2) 0.019(1) 0.004(1) 0.002(1) C(15) 0.042(2) 0.038(2) 0.046(2) 0.020(1) 0.009(2) 0.007(2) C(16) 0.050(2) 0.050(2) 0.073(3) 0.025(2) 0.016(2) 0.026(2) C(17) 0.049(2) 0.041(2) 0.091(3) 0.021(2) 0.010(2) 0.021(2) C(18) 0.065(3) 0.037(2) 0.079(3) 0.027(2) 0.004(2) -0.003(2) C(19) 0.060(2) 0.050(2) 0.053(2) 0.029(2) 0.016(2) 0.007(2) C(20) 0.043(2) 0.041(2) 0.033(2) 0.014(1) 0.014(1) 0.006(1) C(21) 0.056(2) 0.041(2) 0.035(2) 0.007(2) 0.008(2) 0.004(1) C(22) 0.084(3) 0.057(2) 0.032(2) 0.014(2) -0.002(2) 0.004(2) C(23) 0.109(4) 0.069(3) 0.037(2) 0.030(3) 0.013(2) 0.018(2) C(24) 0.095(3) 0.052(2) 0.060(3) 0.020(2) 0.025(2) 0.025(2) C(25) 0.058(2) 0.043(2) 0.046(2) 0.008(2) 0.014(2) 0.008(2) C(26) 0.039(2) 0.068(2) 0.050(2) 0.021(2) 0.012(2) -0.001(2) C(27) 0.039(2) 0.038(2) 0.041(2) 0.003(1) -0.005(1) 0.017(1) C(28) 0.069(3) 0.058(2) 0.045(2) -0.009(2) -0.012(2) 0.021(2) C(29) 0.094(4) 0.070(3) 0.060(3) -0.019(3) -0.034(2) 0.026(2) C(30) 0.074(3) 0.079(3) 0.097(4) -0.026(3) -0.038(3) 0.038(3) C(31) 0.052(3) 0.094(4) 0.106(4) -0.021(2) -0.011(3) 0.052(3) C(32) 0.042(2) 0.067(3) 0.064(3) 0.002(2) -0.001(2) 0.032(2) C(33) 0.038(2) 0.037(2) 0.032(2) 0.008(1) -0.001(1) 0.014(1) C(34) 0.051(2) 0.050(2) 0.038(2) 0.007(2) 0.004(2) 0.022(2) C(35) 0.066(3) 0.063(3) 0.049(2) 0.002(2) -0.004(2) 0.034(2) C(36) 0.084(3) 0.055(3) 0.076(3) 0.020(2) -0.009(2) 0.035(2) C(37) 0.093(3) 0.059(3) 0.079(3) 0.045(2) 0.018(3) 0.027(2) C(38) 0.062(2) 0.053(2) 0.055(2) 0.024(2) 0.015(2) 0.024(2) C(39) 0.038(2) 0.042(2) 0.025(2) 0.010(1) 0.007(1) 0.009(1) C(40) 0.051(2) 0.053(2) 0.043(2) 0.011(2) 0.014(2) 0.004(2) C(41) 0.080(3) 0.063(3) 0.060(3) 0.031(2) 0.030(2) 0.001(2) C(42) 0.064(3) 0.086(3) 0.058(3) 0.041(2) 0.030(2) 0.022(2) C(43) 0.043(2) 0.074(3) 0.052(2) 0.019(2) 0.014(2) 0.024(2) C(44) 0.043(2) 0.047(2) 0.039(2) 0.013(2) 0.007(1) 0.012(2) C(45) 0.043(2) 0.036(2) 0.033(2) 0.015(1) 0.008(1) 0.013(1) C(46) 0.050(2) 0.040(2) 0.051(2) 0.011(2) 0.008(2) 0.014(2) C(47) 0.077(3) 0.038(2) 0.070(3) 0.015(2) 0.017(2) 0.009(2) C(48) 0.103(4) 0.052(3) 0.085(3) 0.042(3) 0.036(3) 0.014(2) C(49) 0.070(3) 0.074(3) 0.095(4) 0.045(3) 0.030(3) 0.024(3) C(50) 0.047(2) 0.052(2) 0.056(2) 0.023(2) 0.013(2) 0.011(2) C(51) 0.034(2) 0.044(2) 0.029(2) 0.010(1) 0.006(1) 0.012(1) C(52) 0.043(2) 0.084(3) 0.053(2) 0.023(2) 0.011(2) 0.042(2) C(53) 0.058(3) 0.113(4) 0.066(3) 0.022(3) 0.016(2) 0.062(3) C(54) 0.053(2) 0.108(4) 0.052(2) 0.020(2) 0.023(2) 0.035(2) C(55) 0.050(2) 0.074(3) 0.061(3) 0.027(2) 0.025(2) 0.019(2) C(56) 0.045(2) 0.047(2) 0.045(2) 0.020(2) 0.014(2) 0.014(2) C(57) 0.036(2) 0.037(2) 0.027(2) 0.014(1) 0.008(1) 0.011(1) C(58) 0.052(2) 0.044(2) 0.039(2) 0.013(2) 0.007(2) 0.017(2) C(59) 0.061(2) 0.041(2) 0.049(2) 0.004(2) 0.009(2) 0.013(2) C(60) 0.045(2) 0.053(2) 0.045(2) 0.005(2) 0.002(2) 0.001(2) C(61) 0.050(2) 0.053(2) 0.047(2) 0.019(2) -0.005(2) 0.012(2) C(62) 0.047(2) 0.041(2) 0.042(2) 0.016(2) 0.004(2) 0.014(2) C(63) 0.081(4) 0.105(4) 0.135(5) 0.051(3) 0.006(3) 0.025(4) C(64) 0.198(7) 0.143(5) 0.088(4) 0.130(5) -0.006(4) 0.015(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) P(4) 2.229(1) . . yes Pd(1) P(5) 2.2397(8) . . yes Pd(1) O(1) 2.081(2) . . yes Pd(1) O(2) 2.107(2) . . yes P(1) O(1) 1.509(2) . . yes P(1) O(4) 1.459(2) . . yes P(1) O(5) 1.605(2) . . yes P(1) O(9) 1.591(2) . . yes P(2) O(2) 1.508(2) . . yes P(2) O(5) 1.611(2) . . yes P(2) O(6) 1.456(2) . . yes P(2) O(7) 1.599(2) . . yes P(3) O(3) 1.473(2) . . yes P(3) O(7) 1.640(2) . . yes P(3) O(8) 1.461(2) . . yes P(3) O(9) 1.631(2) . . yes P(4) C(1) 1.814(3) . . yes P(4) C(7) 1.810(3) . . yes P(4) C(13) 1.812(3) . . yes P(5) C(14) 1.811(3) . . yes P(5) C(20) 1.816(3) . . yes P(5) C(26) 1.812(4) . . yes P(6) N(1) 1.582(3) . . yes P(6) C(27) 1.794(3) . . yes P(6) C(33) 1.803(3) . . yes P(6) C(39) 1.795(3) . . yes P(7) N(1) 1.590(2) . . yes P(7) C(45) 1.805(3) . . yes P(7) C(51) 1.797(3) . . yes P(7) C(57) 1.801(3) . . yes N(2) C(63) 1.112(7) . . yes C(1) C(2) 1.379(4) . . yes C(1) C(6) 1.388(4) . . yes C(2) C(3) 1.396(5) . . yes C(3) C(4) 1.361(5) . . yes C(4) C(5) 1.371(5) . . yes C(5) C(6) 1.381(4) . . yes C(7) C(8) 1.389(4) . . yes C(7) C(12) 1.382(4) . . yes C(8) C(9) 1.374(4) . . yes C(9) C(10) 1.379(5) . . yes C(10) C(11) 1.367(5) . . yes C(11) C(12) 1.389(4) . . yes C(14) C(15) 1.379(4) . . yes C(14) C(19) 1.406(4) . . yes C(15) C(16) 1.391(4) . . yes C(16) C(17) 1.380(5) . . yes C(17) C(18) 1.370(6) . . yes C(18) C(19) 1.380(5) . . yes C(20) C(21) 1.389(4) . . yes C(20) C(25) 1.393(4) . . yes C(21) C(22) 1.384(5) . . yes C(22) C(23) 1.363(5) . . yes C(23) C(24) 1.380(5) . . yes C(24) C(25) 1.373(5) . . yes C(27) C(28) 1.385(5) . . yes C(27) C(32) 1.375(4) . . yes C(28) C(29) 1.387(5) . . yes C(29) C(30) 1.363(7) . . yes C(30) C(31) 1.365(7) . . yes C(31) C(32) 1.385(5) . . yes C(33) C(34) 1.393(4) . . yes C(33) C(38) 1.382(5) . . yes C(34) C(35) 1.387(5) . . yes C(35) C(36) 1.368(6) . . yes C(36) C(37) 1.365(6) . . yes C(37) C(38) 1.396(5) . . yes C(39) C(40) 1.392(4) . . yes C(39) C(44) 1.387(4) . . yes C(40) C(41) 1.367(5) . . yes C(41) C(42) 1.368(5) . . yes C(42) C(43) 1.372(5) . . yes C(43) C(44) 1.375(5) . . yes C(45) C(46) 1.405(4) . . yes C(45) C(50) 1.373(4) . . yes C(46) C(47) 1.373(5) . . yes C(47) C(48) 1.361(6) . . yes C(48) C(49) 1.372(6) . . yes C(49) C(50) 1.393(5) . . yes C(51) C(52) 1.384(4) . . yes C(51) C(56) 1.392(4) . . yes C(52) C(53) 1.390(5) . . yes C(53) C(54) 1.373(6) . . yes C(54) C(55) 1.372(5) . . yes C(55) C(56) 1.374(5) . . yes C(57) C(58) 1.385(4) . . yes C(57) C(62) 1.390(4) . . yes C(58) C(59) 1.384(4) . . yes C(59) C(60) 1.378(5) . . yes C(60) C(61) 1.371(5) . . yes C(61) C(62) 1.387(4) . . yes C(63) C(64) 1.349(7) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(4) Pd(1) P(5) 98.38(3) . . . yes P(4) Pd(1) O(1) 174.77(6) . . . yes P(4) Pd(1) O(2) 83.37(6) . . . yes P(5) Pd(1) O(1) 86.25(6) . . . yes P(5) Pd(1) O(2) 166.56(6) . . . yes O(1) Pd(1) O(2) 92.69(7) . . . yes O(1) P(1) O(4) 116.8(1) . . . yes O(1) P(1) O(5) 107.4(1) . . . yes O(1) P(1) O(9) 109.8(1) . . . yes O(4) P(1) O(5) 109.8(1) . . . yes O(4) P(1) O(9) 110.3(1) . . . yes O(5) P(1) O(9) 101.5(1) . . . yes O(2) P(2) O(5) 107.4(1) . . . yes O(2) P(2) O(6) 117.6(1) . . . yes O(2) P(2) O(7) 109.1(1) . . . yes O(5) P(2) O(6) 109.6(1) . . . yes O(5) P(2) O(7) 101.4(1) . . . yes O(6) P(2) O(7) 110.5(1) . . . yes O(3) P(3) O(7) 108.5(1) . . . yes O(3) P(3) O(8) 122.4(1) . . . yes O(3) P(3) O(9) 108.7(1) . . . yes O(7) P(3) O(8) 108.0(1) . . . yes O(7) P(3) O(9) 99.4(1) . . . yes O(8) P(3) O(9) 107.5(1) . . . yes Pd(1) P(4) C(1) 112.1(1) . . . yes Pd(1) P(4) C(7) 120.7(1) . . . yes Pd(1) P(4) C(13) 106.6(1) . . . yes C(1) P(4) C(7) 107.1(1) . . . yes C(1) P(4) C(13) 105.8(1) . . . yes C(7) P(4) C(13) 103.2(1) . . . yes Pd(1) P(5) C(14) 114.6(1) . . . yes Pd(1) P(5) C(20) 116.7(1) . . . yes Pd(1) P(5) C(26) 108.2(1) . . . yes C(14) P(5) C(20) 110.5(1) . . . yes C(14) P(5) C(26) 102.7(2) . . . yes C(20) P(5) C(26) 102.4(2) . . . yes N(1) P(6) C(27) 110.4(1) . . . yes N(1) P(6) C(33) 109.0(1) . . . yes N(1) P(6) C(39) 114.4(1) . . . yes C(27) P(6) C(33) 106.8(1) . . . yes C(27) P(6) C(39) 108.5(2) . . . yes C(33) P(6) C(39) 107.4(1) . . . yes N(1) P(7) C(45) 115.3(1) . . . yes N(1) P(7) C(51) 107.5(1) . . . yes N(1) P(7) C(57) 110.1(1) . . . yes C(45) P(7) C(51) 106.0(1) . . . yes C(45) P(7) C(57) 107.7(1) . . . yes C(51) P(7) C(57) 110.1(1) . . . yes Pd(1) O(1) P(1) 126.3(1) . . . yes Pd(1) O(2) P(2) 127.6(1) . . . yes P(1) O(5) P(2) 124.1(1) . . . yes P(2) O(7) P(3) 125.6(1) . . . yes P(1) O(9) P(3) 128.1(1) . . . yes P(6) N(1) P(7) 135.4(2) . . . yes P(4) C(1) C(2) 121.2(2) . . . yes P(4) C(1) C(6) 119.8(2) . . . yes C(2) C(1) C(6) 119.0(3) . . . yes C(1) C(2) C(3) 119.7(3) . . . yes C(2) C(3) C(4) 120.7(3) . . . yes C(3) C(4) C(5) 119.9(3) . . . yes C(4) C(5) C(6) 120.2(3) . . . yes C(1) C(6) C(5) 120.5(3) . . . yes P(4) C(7) C(8) 117.9(2) . . . yes P(4) C(7) C(12) 123.1(2) . . . yes C(8) C(7) C(12) 119.0(3) . . . yes C(7) C(8) C(9) 120.7(3) . . . yes C(8) C(9) C(10) 120.0(3) . . . yes C(9) C(10) C(11) 119.8(3) . . . yes C(10) C(11) C(12) 120.7(3) . . . yes C(7) C(12) C(11) 119.8(3) . . . yes P(5) C(14) C(15) 119.5(2) . . . yes P(5) C(14) C(19) 121.1(3) . . . yes C(15) C(14) C(19) 119.1(3) . . . yes C(14) C(15) C(16) 120.5(3) . . . yes C(15) C(16) C(17) 119.4(4) . . . yes C(16) C(17) C(18) 120.9(3) . . . yes C(17) C(18) C(19) 120.0(3) . . . yes C(14) C(19) C(18) 120.1(3) . . . yes P(5) C(20) C(21) 125.1(3) . . . yes P(5) C(20) C(25) 116.6(2) . . . yes C(21) C(20) C(25) 118.3(3) . . . yes C(20) C(21) C(22) 119.7(3) . . . yes C(21) C(22) C(23) 121.0(3) . . . yes C(22) C(23) C(24) 120.2(4) . . . yes C(23) C(24) C(25) 119.2(4) . . . yes C(20) C(25) C(24) 121.5(3) . . . yes P(6) C(27) C(28) 119.9(3) . . . yes P(6) C(27) C(32) 120.7(3) . . . yes C(28) C(27) C(32) 119.4(3) . . . yes C(27) C(28) C(29) 120.0(4) . . . yes C(28) C(29) C(30) 119.9(4) . . . yes C(29) C(30) C(31) 120.5(4) . . . yes C(30) C(31) C(32) 120.2(4) . . . yes C(27) C(32) C(31) 120.0(4) . . . yes P(6) C(33) C(34) 121.6(3) . . . yes P(6) C(33) C(38) 118.9(2) . . . yes C(34) C(33) C(38) 119.5(3) . . . yes C(33) C(34) C(35) 120.0(3) . . . yes C(34) C(35) C(36) 120.0(4) . . . yes C(35) C(36) C(37) 120.6(4) . . . yes C(36) C(37) C(38) 120.3(4) . . . yes C(33) C(38) C(37) 119.6(3) . . . yes P(6) C(39) C(40) 122.0(2) . . . yes P(6) C(39) C(44) 118.8(2) . . . yes C(40) C(39) C(44) 118.9(3) . . . yes C(39) C(40) C(41) 120.0(3) . . . yes C(40) C(41) C(42) 120.7(4) . . . yes C(41) C(42) C(43) 120.2(4) . . . yes C(42) C(43) C(44) 119.9(3) . . . yes C(39) C(44) C(43) 120.4(3) . . . yes P(7) C(45) C(46) 117.2(2) . . . yes P(7) C(45) C(50) 123.9(2) . . . yes C(46) C(45) C(50) 118.7(3) . . . yes C(45) C(46) C(47) 120.4(3) . . . yes C(46) C(47) C(48) 120.1(4) . . . yes C(47) C(48) C(49) 120.7(4) . . . yes C(48) C(49) C(50) 119.9(4) . . . yes C(45) C(50) C(49) 120.2(3) . . . yes P(7) C(51) C(52) 120.4(2) . . . yes P(7) C(51) C(56) 120.2(2) . . . yes C(52) C(51) C(56) 119.4(3) . . . yes C(51) C(52) C(53) 119.6(3) . . . yes C(52) C(53) C(54) 120.0(4) . . . yes C(53) C(54) C(55) 120.9(4) . . . yes C(54) C(55) C(56) 119.6(4) . . . yes C(51) C(56) C(55) 120.6(3) . . . yes P(7) C(57) C(58) 120.2(2) . . . yes P(7) C(57) C(62) 120.1(2) . . . yes C(58) C(57) C(62) 119.6(3) . . . yes C(57) C(58) C(59) 120.0(3) . . . yes C(58) C(59) C(60) 120.2(3) . . . yes C(59) C(60) C(61) 120.1(3) . . . yes C(60) C(61) C(62) 120.4(3) . . . yes C(57) C(62) C(61) 119.7(3) . . . yes N(2) C(63) C(64) 172.8(9) . . . yes #------------------------------------------------------------------------------ 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 Pd(1) P(4) C(1) C(2) 161.2(2) . . . . yes Pd(1) P(4) C(1) C(6) -17.8(3) . . . . yes Pd(1) P(4) C(7) C(8) -53.0(3) . . . . yes Pd(1) P(4) C(7) C(12) 128.8(3) . . . . yes Pd(1) P(5) C(14) C(15) 6.7(3) . . . . yes Pd(1) P(5) C(14) C(19) 179.5(2) . . . . yes Pd(1) P(5) C(20) C(21) 121.8(3) . . . . yes Pd(1) P(5) C(20) C(25) -57.5(3) . . . . yes Pd(1) O(1) P(1) O(4) 168.7(1) . . . . yes Pd(1) O(1) P(1) O(5) 44.8(2) . . . . yes Pd(1) O(1) P(1) O(9) -64.7(2) . . . . yes Pd(1) O(2) P(2) O(5) -39.1(2) . . . . yes Pd(1) O(2) P(2) O(6) -163.2(1) . . . . yes Pd(1) O(2) P(2) O(7) 70.1(2) . . . . yes P(1) O(1) Pd(1) P(4) 14.3(8) . . . . yes P(1) O(1) Pd(1) P(5) 166.7(1) . . . . yes P(1) O(1) Pd(1) O(2) -26.8(2) . . . . yes P(1) O(5) P(2) O(2) 61.5(2) . . . . yes P(1) O(5) P(2) O(6) -169.7(1) . . . . yes P(1) O(5) P(2) O(7) -52.8(2) . . . . yes P(1) O(9) P(3) O(3) -66.5(2) . . . . yes P(1) O(9) P(3) O(7) 46.8(2) . . . . yes P(1) O(9) P(3) O(8) 159.2(2) . . . . yes P(2) O(2) Pd(1) P(4) -152.7(1) . . . . yes P(2) O(2) Pd(1) P(5) 109.0(2) . . . . yes P(2) O(2) Pd(1) O(1) 23.9(2) . . . . yes P(2) O(5) P(1) O(1) -64.7(2) . . . . yes P(2) O(5) P(1) O(4) 167.2(1) . . . . yes P(2) O(5) P(1) O(9) 50.5(2) . . . . yes P(2) O(7) P(3) O(3) 64.9(2) . . . . yes P(2) O(7) P(3) O(8) -160.5(2) . . . . yes P(2) O(7) P(3) O(9) -48.5(2) . . . . yes P(3) O(7) P(2) O(2) -60.7(2) . . . . yes P(3) O(7) P(2) O(5) 52.4(2) . . . . yes P(3) O(7) P(2) O(6) 168.6(1) . . . . yes P(3) O(9) P(1) O(1) 65.0(2) . . . . yes P(3) O(9) P(1) O(4) -164.8(2) . . . . yes P(3) O(9) P(1) O(5) -48.5(2) . . . . yes P(4) Pd(1) P(5) C(14) 93.8(1) . . . . yes P(4) Pd(1) P(5) C(20) -37.5(1) . . . . yes P(4) Pd(1) P(5) C(26) -152.3(1) . . . . yes P(4) C(1) C(2) C(3) -179.7(3) . . . . yes P(4) C(1) C(6) C(5) -179.5(3) . . . . yes P(4) C(7) C(8) C(9) -178.0(3) . . . . yes P(4) C(7) C(12) C(11) 177.6(3) . . . . yes P(5) Pd(1) P(4) C(1) 107.0(1) . . . . yes P(5) Pd(1) P(4) C(7) -20.7(1) . . . . yes P(5) Pd(1) P(4) C(13) -137.7(1) . . . . yes P(5) C(14) C(15) C(16) 173.4(2) . . . . yes P(5) C(14) C(19) C(18) -174.0(3) . . . . yes P(5) C(20) C(21) C(22) -179.7(3) . . . . yes P(5) C(20) C(25) C(24) 180.0(3) . . . . yes P(6) N(1) P(7) C(45) 22.7(3) . . . . yes P(6) N(1) P(7) C(51) 140.7(2) . . . . yes P(6) N(1) P(7) C(57) -99.4(2) . . . . yes P(6) C(27) C(28) C(29) -178.2(4) . . . . yes P(6) C(27) C(32) C(31) 179.0(4) . . . . yes P(6) C(33) C(34) C(35) -177.7(3) . . . . yes P(6) C(33) C(38) C(37) 177.2(3) . . . . yes P(6) C(39) C(40) C(41) 174.2(3) . . . . yes P(6) C(39) C(44) C(43) -174.9(3) . . . . yes P(7) N(1) P(6) C(27) -105.8(2) . . . . yes P(7) N(1) P(6) C(33) 137.1(2) . . . . yes P(7) N(1) P(6) C(39) 16.9(3) . . . . yes P(7) C(45) C(46) C(47) -176.2(3) . . . . yes P(7) C(45) C(50) C(49) 176.7(3) . . . . yes P(7) C(51) C(52) C(53) 179.8(3) . . . . yes P(7) C(51) C(56) C(55) -179.8(3) . . . . yes P(7) C(57) C(58) C(59) 176.2(3) . . . . yes P(7) C(57) C(62) C(61) -175.4(3) . . . . yes O(1) Pd(1) P(4) C(1) -100.9(7) . . . . yes O(1) Pd(1) P(4) C(7) 131.5(7) . . . . yes O(1) Pd(1) P(4) C(13) 14.4(7) . . . . yes O(1) Pd(1) P(5) C(14) -83.7(1) . . . . yes O(1) Pd(1) P(5) C(20) 144.9(1) . . . . yes O(1) Pd(1) P(5) C(26) 30.1(2) . . . . yes O(2) Pd(1) P(4) C(1) -59.6(1) . . . . yes O(2) Pd(1) P(4) C(7) 172.8(1) . . . . yes O(2) Pd(1) P(4) C(13) 55.7(1) . . . . yes O(2) Pd(1) P(5) C(14) -169.6(3) . . . . yes O(2) Pd(1) P(5) C(20) 59.0(3) . . . . yes O(2) Pd(1) P(5) C(26) -55.7(3) . . . . yes N(1) P(6) C(27) C(28) -178.5(3) . . . . yes N(1) P(6) C(27) C(32) 2.8(4) . . . . yes N(1) P(6) C(33) C(34) -154.4(3) . . . . yes N(1) P(6) C(33) C(38) 28.3(3) . . . . yes N(1) P(6) C(39) C(40) -103.8(3) . . . . yes N(1) P(6) C(39) C(44) 69.3(3) . . . . yes N(1) P(7) C(45) C(46) 61.8(3) . . . . yes N(1) P(7) C(45) C(50) -114.2(3) . . . . yes N(1) P(7) C(51) C(52) -161.6(3) . . . . yes N(1) P(7) C(51) C(56) 17.7(3) . . . . yes N(1) P(7) C(57) C(58) 4.2(3) . . . . yes N(1) P(7) C(57) C(62) -178.1(2) . . . . yes C(1) P(4) C(7) C(8) 177.2(2) . . . . yes C(1) P(4) C(7) C(12) -1.1(3) . . . . yes C(1) C(2) C(3) C(4) -0.8(6) . . . . yes C(1) C(6) C(5) C(4) -0.8(5) . . . . yes C(2) C(1) P(4) C(7) -64.2(3) . . . . yes C(2) C(1) P(4) C(13) 45.4(3) . . . . yes C(2) C(1) C(6) C(5) 1.4(5) . . . . yes C(2) C(3) C(4) C(5) 1.4(6) . . . . yes C(3) C(2) C(1) C(6) -0.6(5) . . . . yes C(3) C(4) C(5) C(6) -0.6(6) . . . . yes C(6) C(1) P(4) C(7) 116.8(3) . . . . yes C(6) C(1) P(4) C(13) -133.6(3) . . . . yes C(7) C(8) C(9) C(10) 0.4(5) . . . . yes C(7) C(12) C(11) C(10) 0.4(6) . . . . yes C(8) C(7) P(4) C(13) 65.8(3) . . . . yes C(8) C(7) C(12) C(11) -0.6(5) . . . . yes C(8) C(9) C(10) C(11) -0.7(6) . . . . yes C(9) C(8) C(7) C(12) 0.3(5) . . . . yes C(9) C(10) C(11) C(12) 0.3(6) . . . . yes C(12) C(7) P(4) C(13) -112.4(3) . . . . yes C(14) P(5) C(20) C(21) -11.4(3) . . . . yes C(14) P(5) C(20) C(25) 169.3(3) . . . . yes C(14) C(15) C(16) C(17) 0.5(5) . . . . yes C(14) C(19) C(18) C(17) 0.9(6) . . . . yes C(15) C(14) P(5) C(20) 141.1(3) . . . . yes C(15) C(14) P(5) C(26) -110.3(3) . . . . yes C(15) C(14) C(19) C(18) -1.2(5) . . . . yes C(15) C(16) C(17) C(18) -0.8(6) . . . . yes C(16) C(15) C(14) C(19) 0.5(5) . . . . yes C(16) C(17) C(18) C(19) 0.1(6) . . . . yes C(19) C(14) P(5) C(20) -46.2(3) . . . . yes C(19) C(14) P(5) C(26) 62.4(3) . . . . yes C(20) C(21) C(22) C(23) 0.5(6) . . . . yes C(20) C(25) C(24) C(23) -0.8(6) . . . . yes C(21) C(20) P(5) C(26) -120.2(3) . . . . yes C(21) C(20) C(25) C(24) 0.6(6) . . . . yes C(21) C(22) C(23) C(24) -0.7(7) . . . . yes C(22) C(21) C(20) C(25) -0.5(5) . . . . yes C(22) C(23) C(24) C(25) 0.8(7) . . . . yes C(25) C(20) P(5) C(26) 60.5(3) . . . . yes C(27) P(6) C(33) C(34) 86.3(3) . . . . yes C(27) P(6) C(33) C(38) -91.1(3) . . . . yes C(27) P(6) C(39) C(40) 20.0(3) . . . . yes C(27) P(6) C(39) C(44) -167.0(2) . . . . yes C(27) C(28) C(29) C(30) -0.5(8) . . . . yes C(27) C(32) C(31) C(30) -1.2(8) . . . . yes C(28) C(27) P(6) C(33) -60.1(3) . . . . yes C(28) C(27) P(6) C(39) 55.4(3) . . . . yes C(28) C(27) C(32) C(31) 0.3(6) . . . . yes C(28) C(29) C(30) C(31) -0.4(9) . . . . yes C(29) C(28) C(27) C(32) 0.5(6) . . . . yes C(29) C(30) C(31) C(32) 1.2(9) . . . . yes C(32) C(27) P(6) C(33) 121.2(3) . . . . yes C(32) C(27) P(6) C(39) -123.3(3) . . . . yes C(33) P(6) C(39) C(40) 135.1(3) . . . . yes C(33) P(6) C(39) C(44) -51.8(3) . . . . yes C(33) C(34) C(35) C(36) 0.6(5) . . . . yes C(33) C(38) C(37) C(36) 0.4(6) . . . . yes C(34) C(33) P(6) C(39) -29.9(3) . . . . yes C(34) C(33) C(38) C(37) -0.2(5) . . . . yes C(34) C(35) C(36) C(37) -0.4(6) . . . . yes C(35) C(34) C(33) C(38) -0.3(5) . . . . yes C(35) C(36) C(37) C(38) -0.1(7) . . . . yes C(38) C(33) P(6) C(39) 152.7(3) . . . . yes C(39) C(40) C(41) C(42) 0.2(6) . . . . yes C(39) C(44) C(43) C(42) 0.8(5) . . . . yes C(40) C(39) C(44) C(43) -1.6(5) . . . . yes C(40) C(41) C(42) C(43) -1.0(7) . . . . yes C(41) C(40) C(39) C(44) 1.1(5) . . . . yes C(41) C(42) C(43) C(44) 0.5(6) . . . . yes C(45) P(7) C(51) C(52) -37.8(3) . . . . yes C(45) P(7) C(51) C(56) 141.6(3) . . . . yes C(45) P(7) C(57) C(58) -122.3(3) . . . . yes C(45) P(7) C(57) C(62) 55.4(3) . . . . yes C(45) C(46) C(47) C(48) -0.2(6) . . . . yes C(45) C(50) C(49) C(48) -1.4(7) . . . . yes C(46) C(45) P(7) C(51) -57.1(3) . . . . yes C(46) C(45) P(7) C(57) -174.9(2) . . . . yes C(46) C(45) C(50) C(49) 0.8(5) . . . . yes C(46) C(47) C(48) C(49) -0.4(7) . . . . yes C(47) C(46) C(45) C(50) 0.1(5) . . . . yes C(47) C(48) C(49) C(50) 1.3(7) . . . . yes C(50) C(45) P(7) C(51) 126.9(3) . . . . yes C(50) C(45) P(7) C(57) 9.1(3) . . . . yes C(51) P(7) C(57) C(58) 122.5(3) . . . . yes C(51) P(7) C(57) C(62) -59.7(3) . . . . yes C(51) C(52) C(53) C(54) 0.0(6) . . . . yes C(51) C(56) C(55) C(54) 0.0(6) . . . . yes C(52) C(51) P(7) C(57) 78.5(3) . . . . yes C(52) C(51) C(56) C(55) -0.4(5) . . . . yes C(52) C(53) C(54) C(55) -0.5(7) . . . . yes C(53) C(52) C(51) C(56) 0.5(5) . . . . yes C(53) C(54) C(55) C(56) 0.5(6) . . . . yes C(56) C(51) P(7) C(57) -102.2(3) . . . . yes C(57) C(58) C(59) C(60) -0.7(6) . . . . yes C(57) C(62) C(61) C(60) -0.9(5) . . . . yes C(58) C(57) C(62) C(61) 2.4(5) . . . . yes C(58) C(59) C(60) C(61) 2.2(6) . . . . yes C(59) C(58) C(57) C(62) -1.5(5) . . . . yes C(59) C(60) C(61) C(62) -1.4(6) . . . . yes C(59) C(60) C(61) C(62) -1.4(6) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(5) 3.437(4) . 2_557 ? O(1) C(4) 3.583(5) . 2_557 ? O(2) C(64) 3.530(6) . 1_544 ? O(3) C(9) 3.176(4) . 2_667 ? O(3) C(10) 3.315(4) . 2_667 ? O(4) C(52) 3.110(4) . 2_567 ? O(4) C(62) 3.369(4) . 2_567 ? O(4) C(18) 3.414(4) . 2_567 ? O(4) C(30) 3.509(5) . 1_444 ? O(5) C(30) 3.329(5) . 1_444 ? O(5) C(5) 3.482(4) . 2_557 ? O(6) C(41) 3.099(4) . 1_544 ? O(6) C(64) 3.147(6) . 1_544 ? O(6) C(42) 3.164(4) . 1_544 ? O(6) C(24) 3.331(4) . 2_557 ? O(8) C(35) 3.292(4) . 1_554 ? O(8) C(55) 3.357(5) . 2_667 ? O(8) C(36) 3.374(5) . 1_554 ? O(9) C(62) 3.170(4) . 2_567 ? O(9) C(61) 3.298(4) . 2_567 ? O(9) C(50) 3.599(4) . 2_567 ? N(2) C(12) 3.512(7) . 2_668 ? N(2) C(2) 3.597(8) . 2_668 ? C(8) C(16) 3.596(5) . 2_667 ? C(9) C(16) 3.523(5) . 2_667 ? C(9) C(15) 3.568(5) . 2_667 ? C(17) C(26) 3.543(5) . 2_567 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #============================================================================== data_(PPN)[Pt(P3O9)(PPh3)2](3) _database_code_CSD 202875 _audit_creation_date 2003-04-03 _audit_creation_method 'by CrystalStructure v3.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C74.50 H65 Cl5 N O9 P7 Pt ' _chemical_formula_moiety (PPN)[Pt(P3O9)(PPh3)2] _chemical_formula_weight 1707.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 14.1829(7) _cell_length_b 15.9737(4) _cell_length_c 17.0641(7) _cell_angle_alpha 105.188(2) _cell_angle_beta 92.784(2) _cell_angle_gamma 103.9060(9) _cell_volume 3595.8(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 14577 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 103.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1718.00 _exptl_absorpt_coefficient_mu 2.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.442 _exptl_absorpt_correction_T_max 0.626 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 24088 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.9406 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9372 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #============================================================================== # REFINEMENT DATA _refine_special_details ; ; _reflns_number_total 15499 _reflns_number_gt 13232 _reflns_threshold_criterion F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0390 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 13232 _refine_ls_number_parameters 932 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.0000\s^2^(Fo) + 0.0001]' _refine_ls_shift/su_max 0.0060 _refine_diff_density_max 1.58 _refine_diff_density_min -1.79 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pt Pt -2.013 8.802 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.38624(1) 0.21921(1) 0.77339(1) 0.00845(3) Uani 1.00 1 d . . . Cl1 Cl 0.41550(9) 0.67516(6) 0.68667(7) 0.0364(3) Uani 1.00 1 d . . . Cl2 Cl 0.52799(9) 0.54760(9) 0.61868(7) 0.0434(3) Uani 1.00 1 d . . . Cl3 Cl 0.95007(9) 0.78222(8) 0.54636(7) 0.0415(3) Uani 1.00 1 d . . . Cl4 Cl 1.07750(9) 0.67897(9) 0.46051(7) 0.0427(3) Uani 1.00 1 d . . . Cl5 Cl 1.0881(1) 0.9715(1) 0.4752(1) 0.0750(6) Uani 1.00 1 d . . . P1 P 0.26934(6) 0.34217(5) 0.70034(5) 0.0129(2) Uani 1.00 1 d . . . P2 P 0.24817(6) 0.34249(5) 0.86460(5) 0.0125(2) Uani 1.00 1 d . . . P3 P 0.11783(6) 0.20117(5) 0.73084(5) 0.0134(2) Uani 1.00 1 d . . . P4 P 0.43232(6) 0.15969(5) 0.86900(5) 0.0110(2) Uani 1.00 1 d . . . P5 P 0.44649(6) 0.14154(5) 0.66820(5) 0.0112(2) Uani 1.00 1 d . . . P6 P 0.97604(6) 0.72908(5) 0.82065(5) 0.0119(2) Uani 1.00 1 d . . . P7 P 0.81146(6) 0.56764(5) 0.78387(5) 0.0115(2) Uani 1.00 1 d . . . O1 O 0.3479(2) 0.2925(1) 0.6987(1) 0.0136(5) Uani 1.00 1 d . . . O2 O 0.3318(2) 0.2988(1) 0.8688(1) 0.0135(5) Uani 1.00 1 d . . . O3 O 0.1708(2) 0.1306(1) 0.7176(1) 0.0176(6) Uani 1.00 1 d . . . O4 O 0.2756(2) 0.4041(1) 0.6495(1) 0.0195(6) Uani 1.00 1 d . . . O5 O 0.2674(2) 0.3949(1) 0.7947(1) 0.0144(5) Uani 1.00 1 d . . . O6 O 0.2312(2) 0.4029(2) 0.9400(1) 0.0195(6) Uani 1.00 1 d . . . O7 O 0.1499(2) 0.2668(1) 0.8242(1) 0.0152(5) Uani 1.00 1 d . . . O8 O 0.0111(2) 0.1814(1) 0.7148(2) 0.0207(6) Uani 1.00 1 d . . . O9 O 0.1642(2) 0.2725(1) 0.6806(1) 0.0151(5) Uani 1.00 1 d . . . N1 N 0.8691(2) 0.6702(2) 0.8210(2) 0.0143(6) Uani 1.00 1 d . . . C1 C 0.3320(2) 0.1361(2) 0.9297(2) 0.0126(7) Uani 1.00 1 d . . . C2 C 0.2369(3) 0.1037(2) 0.8894(2) 0.0169(8) Uani 1.00 1 d . . . C3 C 0.1584(3) 0.0827(2) 0.9332(2) 0.0194(8) Uani 1.00 1 d . . . C4 C 0.1745(3) 0.0935(2) 1.0164(2) 0.0201(8) Uani 1.00 1 d . . . C5 C 0.2692(3) 0.1257(3) 1.0560(2) 0.0234(9) Uani 1.00 1 d . . . C6 C 0.3478(3) 0.1469(2) 1.0130(2) 0.0183(8) Uani 1.00 1 d . . . C7 C 0.4707(2) 0.0554(2) 0.8434(2) 0.0126(7) Uani 1.00 1 d . . . C8 C 0.4022(3) -0.0266(2) 0.8347(2) 0.0178(8) Uani 1.00 1 d . . . C9 C 0.4316(3) -0.1058(2) 0.8170(2) 0.0235(9) Uani 1.00 1 d . . . C10 C 0.5288(3) -0.1041(2) 0.8074(2) 0.0245(9) Uani 1.00 1 d . . . C11 C 0.5962(3) -0.0227(2) 0.8159(2) 0.0236(9) Uani 1.00 1 d . . . C12 C 0.5671(3) 0.0568(2) 0.8338(2) 0.0180(8) Uani 1.00 1 d . . . C13 C 0.5350(2) 0.2395(2) 0.9383(2) 0.0128(7) Uani 1.00 1 d . . . C14 C 0.5621(2) 0.3280(2) 0.9330(2) 0.0140(7) Uani 1.00 1 d . . . C15 C 0.6415(2) 0.3912(2) 0.9828(2) 0.0161(8) Uani 1.00 1 d . . . C16 C 0.6939(3) 0.3665(2) 1.0395(2) 0.0219(8) Uani 1.00 1 d . . . C17 C 0.6666(3) 0.2804(2) 1.0475(2) 0.0224(9) Uani 1.00 1 d . . . C18 C 0.5884(3) 0.2164(2) 0.9966(2) 0.0180(8) Uani 1.00 1 d . . . C19 C 0.3962(2) 0.0206(2) 0.6460(2) 0.0136(7) Uani 1.00 1 d . . . C20 C 0.2945(3) -0.0100(2) 0.6444(2) 0.0162(8) Uani 1.00 1 d . . . C21 C 0.2502(3) -0.1017(2) 0.6245(2) 0.0194(8) Uani 1.00 1 d . . . C22 C 0.3062(3) -0.1629(2) 0.6078(2) 0.0225(9) Uani 1.00 1 d . . . C23 C 0.4070(3) -0.1331(2) 0.6106(2) 0.0211(9) Uani 1.00 1 d . . . C24 C 0.4520(3) -0.0412(2) 0.6291(2) 0.0164(8) Uani 1.00 1 d . . . C25 C 0.4156(2) 0.1692(2) 0.5747(2) 0.0144(7) Uani 1.00 1 d . . . C26 C 0.4652(3) 0.2525(2) 0.5663(2) 0.0213(9) Uani 1.00 1 d . . . C27 C 0.4398(3) 0.2799(3) 0.4990(2) 0.026(1) Uani 1.00 1 d . . . C28 C 0.3653(3) 0.2241(3) 0.4403(2) 0.031(1) Uani 1.00 1 d . . . C29 C 0.3161(3) 0.1415(3) 0.4480(3) 0.038(1) Uani 1.00 1 d . . . C30 C 0.3406(3) 0.1140(3) 0.5156(2) 0.028(1) Uani 1.00 1 d . . . C31 C 0.5786(2) 0.1657(2) 0.6750(2) 0.0137(7) Uani 1.00 1 d . . . C32 C 0.6376(3) 0.2250(2) 0.7444(2) 0.0173(8) Uani 1.00 1 d . . . C33 C 0.7389(3) 0.2422(2) 0.7492(2) 0.0222(9) Uani 1.00 1 d . . . C34 C 0.7827(3) 0.2007(3) 0.6847(2) 0.0241(9) Uani 1.00 1 d . . . C35 C 0.7245(3) 0.1439(3) 0.6138(2) 0.0247(9) Uani 1.00 1 d . . . C36 C 0.6238(3) 0.1274(2) 0.6083(2) 0.0191(8) Uani 1.00 1 d . . . C37 C 0.9652(2) 0.8197(2) 0.7792(2) 0.0149(7) Uani 1.00 1 d . . . C38 C 1.0463(3) 0.8748(2) 0.7580(2) 0.0203(8) Uani 1.00 1 d . . . C39 C 1.0353(3) 0.9479(2) 0.7326(2) 0.0251(9) Uani 1.00 1 d . . . C40 C 0.9459(3) 0.9673(2) 0.7287(2) 0.0247(9) Uani 1.00 1 d . . . C41 C 0.8649(3) 0.9119(3) 0.7487(2) 0.025(1) Uani 1.00 1 d . . . C42 C 0.8746(3) 0.8378(2) 0.7736(2) 0.0187(8) Uani 1.00 1 d . . . C43 C 1.0542(2) 0.6691(2) 0.7637(2) 0.0144(7) Uani 1.00 1 d . . . C44 C 1.1131(3) 0.6301(2) 0.8029(2) 0.0178(8) Uani 1.00 1 d . . . C45 C 1.1622(3) 0.5718(2) 0.7570(2) 0.0193(8) Uani 1.00 1 d . . . C46 C 1.1519(3) 0.5516(2) 0.6726(2) 0.0231(9) Uani 1.00 1 d . . . C47 C 1.0941(3) 0.5910(3) 0.6335(2) 0.0236(9) Uani 1.00 1 d . . . C48 C 1.0452(3) 0.6500(2) 0.6786(2) 0.0192(8) Uani 1.00 1 d . . . C49 C 1.0367(2) 0.7791(2) 0.9235(2) 0.0146(7) Uani 1.00 1 d . . . C50 C 0.9897(3) 0.7647(2) 0.9904(2) 0.0199(8) Uani 1.00 1 d . . . C51 C 1.0375(3) 0.8055(3) 1.0688(2) 0.0238(9) Uani 1.00 1 d . . . C52 C 1.1319(3) 0.8599(2) 1.0809(2) 0.0243(9) Uani 1.00 1 d . . . C53 C 1.1800(3) 0.8750(2) 1.0147(2) 0.0234(9) Uani 1.00 1 d . . . C54 C 1.1322(3) 0.8354(2) 0.9367(2) 0.0204(8) Uani 1.00 1 d . . . C55 C 0.7855(2) 0.5330(2) 0.6740(2) 0.0180(8) Uani 1.00 1 d . . . C56 C 0.7875(3) 0.5984(3) 0.6334(2) 0.0216(9) Uani 1.00 1 d . . . C57 C 0.7566(3) 0.5737(3) 0.5498(2) 0.031(1) Uani 1.00 1 d . . . C58 C 0.7221(3) 0.4834(3) 0.5079(2) 0.036(1) Uani 1.00 1 d . . . C59 C 0.7209(3) 0.4181(3) 0.5474(2) 0.033(1) Uani 1.00 1 d . . . C60 C 0.7532(3) 0.4420(3) 0.6308(2) 0.0230(9) Uani 1.00 1 d . . . C61 C 0.6954(2) 0.5542(2) 0.8229(2) 0.0121(7) Uani 1.00 1 d . . . C62 C 0.6190(2) 0.4776(2) 0.7858(2) 0.0162(8) Uani 1.00 1 d . . . C63 C 0.5298(2) 0.4662(2) 0.8170(2) 0.0168(8) Uani 1.00 1 d . . . C64 C 0.5166(3) 0.5297(2) 0.8853(2) 0.0187(8) Uani 1.00 1 d . . . C65 C 0.5920(3) 0.6054(2) 0.9224(2) 0.0209(8) Uani 1.00 1 d . . . C66 C 0.6814(3) 0.6188(2) 0.8910(2) 0.0180(8) Uani 1.00 1 d . . . C67 C 0.8648(3) 0.4830(2) 0.8933(2) 0.0170(8) Uani 1.00 1 d . . . C68 C 0.9193(3) 0.4328(3) 0.9210(2) 0.0244(9) Uani 1.00 1 d . . . C69 C 0.9807(3) 0.3927(3) 0.8713(3) 0.026(1) Uani 1.00 1 d . . . C70 C 0.9866(3) 0.4008(2) 0.7932(3) 0.0249(9) Uani 1.00 1 d . . . C71 C 0.9321(2) 0.4507(2) 0.7640(2) 0.0178(8) Uani 1.00 1 d . . . C72 C 0.8714(2) 0.4919(2) 0.8139(2) 0.0140(7) Uani 1.00 1 d . . . C73 C 0.4540(3) 0.5800(3) 0.6949(2) 0.0277(8) Uiso 1.00 1 d . . . C74 C 0.9755(3) 0.7220(3) 0.4508(3) 0.0335(9) Uiso 1.00 1 d . . . C75 C 0.9670(6) 0.9715(5) 0.4616(5) 0.027(2) Uiso 0.50 1 d P . . H1 H 0.2257(3) 0.0962(2) 0.8323(2) 0.020(1) Uiso 1.00 1 c . . . H2 H 0.0936(3) 0.0609(2) 0.9060(2) 0.023(1) Uiso 1.00 1 c . . . H3 H 0.1210(3) 0.0789(2) 1.0462(2) 0.025(1) Uiso 1.00 1 c . . . H4 H 0.2804(3) 0.1332(3) 1.1131(2) 0.030(1) Uiso 1.00 1 c . . . H5 H 0.4125(3) 0.1690(2) 1.0407(2) 0.022(1) Uiso 1.00 1 c . . . H6 H 0.3358(3) -0.0279(2) 0.8414(2) 0.021(1) Uiso 1.00 1 c . . . H7 H 0.3848(3) -0.1614(2) 0.8113(2) 0.027(1) Uiso 1.00 1 c . . . H8 H 0.5487(3) -0.1584(2) 0.7948(2) 0.029(1) Uiso 1.00 1 c . . . H9 H 0.6628(3) -0.0211(2) 0.8097(2) 0.029(1) Uiso 1.00 1 c . . . H10 H 0.6138(3) 0.1124(2) 0.8395(2) 0.021(1) Uiso 1.00 1 c . . . H11 H 0.5253(2) 0.3450(2) 0.8947(2) 0.017(1) Uiso 1.00 1 c . . . H12 H 0.6599(2) 0.4508(2) 0.9782(2) 0.018(1) Uiso 1.00 1 c . . . H13 H 0.7491(3) 0.4092(2) 1.0732(2) 0.024(1) Uiso 1.00 1 c . . . H14 H 0.7016(3) 0.2650(2) 1.0881(2) 0.027(1) Uiso 1.00 1 c . . . H15 H 0.5710(3) 0.1568(2) 1.0014(2) 0.022(1) Uiso 1.00 1 c . . . H16 H 0.2562(3) 0.0320(2) 0.6575(2) 0.019(1) Uiso 1.00 1 c . . . H17 H 0.1812(3) -0.1226(2) 0.6221(2) 0.022(1) Uiso 1.00 1 c . . . H18 H 0.2757(3) -0.2255(2) 0.5942(2) 0.025(1) Uiso 1.00 1 c . . . H19 H 0.4454(3) -0.1751(2) 0.6003(2) 0.026(1) Uiso 1.00 1 c . . . H20 H 0.5208(3) -0.0208(2) 0.6301(2) 0.020(1) Uiso 1.00 1 c . . . H21 H 0.5170(3) 0.2908(2) 0.6067(2) 0.025(1) Uiso 1.00 1 c . . . H22 H 0.4738(3) 0.3368(3) 0.4938(2) 0.035(2) Uiso 1.00 1 c . . . H23 H 0.3476(3) 0.2426(3) 0.3943(2) 0.041(2) Uiso 1.00 1 c . . . H24 H 0.2653(3) 0.1028(3) 0.4069(3) 0.045(2) Uiso 1.00 1 c . . . H25 H 0.3059(3) 0.0574(3) 0.5212(2) 0.033(1) Uiso 1.00 1 c . . . H26 H 0.6081(3) 0.2538(2) 0.7888(2) 0.021(1) Uiso 1.00 1 c . . . H27 H 0.7782(3) 0.2824(2) 0.7972(2) 0.024(1) Uiso 1.00 1 c . . . H28 H 0.8518(3) 0.2106(3) 0.6888(2) 0.028(1) Uiso 1.00 1 c . . . H29 H 0.7541(3) 0.1170(3) 0.5686(2) 0.030(1) Uiso 1.00 1 c . . . H30 H 0.5847(3) 0.0895(2) 0.5593(2) 0.022(1) Uiso 1.00 1 c . . . H31 H 1.1083(3) 0.8621(2) 0.7609(2) 0.024(1) Uiso 1.00 1 c . . . H32 H 1.0902(3) 0.9853(2) 0.7177(2) 0.029(1) Uiso 1.00 1 c . . . H33 H 0.9398(3) 1.0182(2) 0.7121(2) 0.030(1) Uiso 1.00 1 c . . . H34 H 0.8029(3) 0.9245(3) 0.7455(2) 0.033(1) Uiso 1.00 1 c . . . H35 H 0.8193(3) 0.7997(2) 0.7874(2) 0.024(1) Uiso 1.00 1 c . . . H36 H 1.1197(3) 0.6435(2) 0.8608(2) 0.020(1) Uiso 1.00 1 c . . . H37 H 1.2031(3) 0.5460(2) 0.7837(2) 0.024(1) Uiso 1.00 1 c . . . H38 H 1.1842(3) 0.5108(2) 0.6415(2) 0.029(1) Uiso 1.00 1 c . . . H39 H 1.0874(3) 0.5774(3) 0.5756(2) 0.031(1) Uiso 1.00 1 c . . . H40 H 1.0064(3) 0.6776(2) 0.6519(2) 0.026(1) Uiso 1.00 1 c . . . H41 H 0.9250(3) 0.7270(2) 0.9818(2) 0.023(1) Uiso 1.00 1 c . . . H42 H 1.0053(3) 0.7958(3) 1.1144(2) 0.029(1) Uiso 1.00 1 c . . . H43 H 1.1644(3) 0.8876(2) 1.1348(2) 0.027(1) Uiso 1.00 1 c . . . H44 H 1.2452(3) 0.9119(2) 1.0234(2) 0.026(1) Uiso 1.00 1 c . . . H45 H 1.1642(3) 0.8466(2) 0.8914(2) 0.024(1) Uiso 1.00 1 c . . . H46 H 0.8103(3) 0.6602(3) 0.6627(2) 0.026(1) Uiso 1.00 1 c . . . H47 H 0.7588(3) 0.6183(3) 0.5219(2) 0.039(2) Uiso 1.00 1 c . . . H48 H 0.6988(3) 0.4661(3) 0.4514(2) 0.042(2) Uiso 1.00 1 c . . . H49 H 0.6984(3) 0.3564(3) 0.5176(2) 0.035(1) Uiso 1.00 1 c . . . H50 H 0.7532(3) 0.3972(3) 0.6581(2) 0.026(1) Uiso 1.00 1 c . . . H51 H 0.6285(2) 0.4334(2) 0.7396(2) 0.020(1) Uiso 1.00 1 c . . . H52 H 0.4776(2) 0.4148(2) 0.7913(2) 0.020(1) Uiso 1.00 1 c . . . H53 H 0.4556(3) 0.5215(2) 0.9068(2) 0.023(1) Uiso 1.00 1 c . . . H54 H 0.5830(3) 0.6484(2) 0.9698(2) 0.025(1) Uiso 1.00 1 c . . . H55 H 0.7326(3) 0.6714(2) 0.9157(2) 0.020(1) Uiso 1.00 1 c . . . H56 H 0.8235(3) 0.5110(2) 0.9273(2) 0.020(1) Uiso 1.00 1 c . . . H57 H 0.9145(3) 0.4259(3) 0.9744(2) 0.030(1) Uiso 1.00 1 c . . . H58 H 1.0186(3) 0.3594(3) 0.8913(3) 0.034(2) Uiso 1.00 1 c . . . H59 H 1.0277(3) 0.3726(2) 0.7591(3) 0.031(1) Uiso 1.00 1 c . . . H60 H 0.9362(2) 0.4566(2) 0.7102(2) 0.021(1) Uiso 1.00 1 c . . . H61 H 0.4906(3) 0.5941(3) 0.7469(2) 0.033(1) Uiso 1.00 1 c . . . H62 H 0.3980(3) 0.5314(3) 0.6900(2) 0.033(1) Uiso 1.00 1 c . . . H63 H 0.9200(3) 0.6734(3) 0.4262(3) 0.040(1) Uiso 1.00 1 c . . . H64 H 0.9883(3) 0.7611(3) 0.4169(3) 0.040(1) Uiso 1.00 1 c . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.00798(6) 0.00801(6) 0.00929(6) 0.00273(4) 0.00054(4) 0.00182(4) Cl1 0.0473(6) 0.0175(4) 0.0414(6) 0.0076(4) -0.0000(5) 0.0048(4) Cl2 0.0414(6) 0.0608(7) 0.0492(7) 0.0294(6) 0.0193(5) 0.0344(6) Cl3 0.0522(7) 0.0403(6) 0.0399(6) 0.0182(5) 0.0083(5) 0.0186(5) Cl4 0.0471(7) 0.0569(7) 0.0321(6) 0.0223(6) 0.0039(5) 0.0182(5) Cl5 0.0343(7) 0.088(1) 0.127(2) 0.0219(7) 0.0197(8) 0.066(1) P1 0.0129(4) 0.0112(4) 0.0157(4) 0.0035(3) 0.0004(3) 0.0055(3) P2 0.0120(4) 0.0106(4) 0.0132(4) 0.0033(3) 0.0009(3) 0.0003(3) P3 0.0106(4) 0.0111(4) 0.0169(4) 0.0020(3) -0.0010(3) 0.0025(3) P4 0.0107(4) 0.0106(4) 0.0114(4) 0.0028(3) 0.0001(3) 0.0026(3) P5 0.0106(4) 0.0112(4) 0.0117(4) 0.0040(3) 0.0019(3) 0.0022(3) P6 0.0111(4) 0.0110(4) 0.0142(4) 0.0027(3) 0.0030(3) 0.0044(3) P7 0.0110(4) 0.0106(4) 0.0121(4) 0.0022(3) 0.0026(3) 0.0021(3) O1 0.017(1) 0.012(1) 0.012(1) 0.0037(9) 0.0018(9) 0.0043(9) O2 0.013(1) 0.012(1) 0.016(1) 0.0077(9) 0.0032(9) 0.0015(9) O3 0.016(1) 0.014(1) 0.023(1) 0.0044(9) 0.002(1) 0.0043(9) O4 0.021(1) 0.016(1) 0.026(1) 0.007(1) 0.003(1) 0.012(1) O5 0.015(1) 0.011(1) 0.017(1) 0.0035(9) 0.0011(9) 0.0027(9) O6 0.020(1) 0.019(1) 0.017(1) 0.008(1) 0.002(1) -0.0022(9) O7 0.013(1) 0.013(1) 0.017(1) 0.0013(9) 0.0032(9) 0.0030(9) O8 0.013(1) 0.015(1) 0.031(1) 0.0017(9) -0.002(1) 0.005(1) O9 0.013(1) 0.014(1) 0.018(1) 0.0033(9) -0.0012(9) 0.0051(9) N1 0.011(1) 0.013(1) 0.019(1) 0.002(1) 0.004(1) 0.005(1) C1 0.012(1) 0.012(1) 0.016(2) 0.005(1) 0.003(1) 0.004(1) C2 0.017(2) 0.019(2) 0.015(2) 0.005(1) 0.003(1) 0.004(1) C3 0.014(2) 0.021(2) 0.021(2) 0.002(1) 0.002(1) 0.006(1) C4 0.018(2) 0.021(2) 0.024(2) 0.007(1) 0.009(1) 0.006(1) C5 0.026(2) 0.031(2) 0.017(2) 0.011(2) 0.004(1) 0.010(1) C6 0.018(2) 0.023(2) 0.015(2) 0.005(1) 0.002(1) 0.006(1) C7 0.014(1) 0.012(1) 0.012(1) 0.005(1) -0.001(1) 0.002(1) C8 0.020(2) 0.016(2) 0.017(2) 0.006(1) 0.003(1) 0.003(1) C9 0.032(2) 0.013(2) 0.023(2) 0.003(1) -0.000(2) 0.005(1) C10 0.033(2) 0.016(2) 0.024(2) 0.011(2) -0.004(2) 0.001(1) C11 0.022(2) 0.024(2) 0.025(2) 0.013(2) -0.000(1) 0.003(1) C12 0.019(2) 0.017(2) 0.016(2) 0.004(1) -0.001(1) 0.002(1) C13 0.012(1) 0.016(1) 0.009(1) 0.007(1) 0.002(1) -0.000(1) C14 0.012(1) 0.018(2) 0.012(1) 0.006(1) 0.002(1) 0.003(1) C15 0.015(2) 0.013(1) 0.017(2) 0.001(1) 0.003(1) 0.000(1) C16 0.017(2) 0.022(2) 0.020(2) 0.003(1) -0.005(1) -0.002(1) C17 0.019(2) 0.027(2) 0.022(2) 0.008(1) -0.008(1) 0.007(1) C18 0.019(2) 0.017(2) 0.021(2) 0.007(1) 0.001(1) 0.007(1) C19 0.018(2) 0.011(1) 0.009(1) 0.003(1) 0.002(1) -0.001(1) C20 0.017(2) 0.013(1) 0.017(2) 0.005(1) 0.004(1) 0.001(1) C21 0.016(2) 0.018(2) 0.021(2) 0.003(1) 0.003(1) 0.002(1) C22 0.028(2) 0.011(1) 0.023(2) 0.002(1) -0.000(2) 0.001(1) C23 0.030(2) 0.015(2) 0.020(2) 0.014(1) 0.002(1) 0.000(1) C24 0.018(2) 0.016(2) 0.015(2) 0.007(1) 0.002(1) 0.001(1) C25 0.016(2) 0.021(2) 0.009(1) 0.009(1) 0.005(1) 0.005(1) C26 0.025(2) 0.021(2) 0.018(2) 0.006(1) 0.002(1) 0.005(1) C27 0.036(2) 0.026(2) 0.025(2) 0.017(2) 0.011(2) 0.015(2) C28 0.037(2) 0.044(2) 0.022(2) 0.019(2) 0.005(2) 0.019(2) C29 0.039(2) 0.046(3) 0.026(2) 0.003(2) -0.014(2) 0.014(2) C30 0.031(2) 0.027(2) 0.023(2) 0.001(2) -0.005(2) 0.011(2) C31 0.012(1) 0.015(1) 0.015(2) 0.005(1) 0.002(1) 0.004(1) C32 0.016(2) 0.018(2) 0.018(2) 0.004(1) 0.005(1) 0.005(1) C33 0.014(2) 0.022(2) 0.024(2) -0.002(1) -0.001(1) 0.004(1) C34 0.013(2) 0.026(2) 0.032(2) 0.004(1) 0.002(1) 0.007(2) C35 0.019(2) 0.027(2) 0.028(2) 0.008(2) 0.012(2) 0.005(2) C36 0.018(2) 0.023(2) 0.015(2) 0.005(1) 0.005(1) 0.002(1) C37 0.018(2) 0.013(1) 0.014(1) 0.003(1) 0.002(1) 0.003(1) C38 0.017(2) 0.017(2) 0.026(2) 0.001(1) 0.002(1) 0.008(1) C39 0.032(2) 0.016(2) 0.025(2) -0.002(1) 0.001(2) 0.009(1) C40 0.042(2) 0.012(2) 0.020(2) 0.008(2) 0.003(2) 0.006(1) C41 0.032(2) 0.025(2) 0.025(2) 0.019(2) 0.009(2) 0.008(2) C42 0.020(2) 0.020(2) 0.021(2) 0.010(1) 0.008(1) 0.009(1) C43 0.010(1) 0.013(1) 0.019(2) 0.002(1) 0.003(1) 0.004(1) C44 0.017(2) 0.017(2) 0.017(2) 0.001(1) -0.002(1) 0.005(1) C45 0.016(2) 0.021(2) 0.024(2) 0.009(1) 0.003(1) 0.006(1) C46 0.020(2) 0.023(2) 0.030(2) 0.010(1) 0.012(2) 0.008(2) C47 0.028(2) 0.030(2) 0.018(2) 0.015(2) 0.011(1) 0.009(1) C48 0.020(2) 0.023(2) 0.021(2) 0.012(1) 0.007(1) 0.010(1) C49 0.015(2) 0.012(1) 0.016(2) 0.004(1) 0.001(1) 0.004(1) C50 0.019(2) 0.017(2) 0.022(2) 0.003(1) 0.004(1) 0.005(1) C51 0.030(2) 0.026(2) 0.017(2) 0.010(2) 0.004(1) 0.006(1) C52 0.032(2) 0.020(2) 0.016(2) 0.006(2) -0.005(1) -0.002(1) C53 0.021(2) 0.020(2) 0.025(2) 0.001(1) -0.003(1) 0.002(1) C54 0.020(2) 0.019(2) 0.020(2) 0.002(1) 0.002(1) 0.005(1) C55 0.011(1) 0.027(2) 0.014(2) 0.005(1) 0.003(1) 0.003(1) C56 0.015(2) 0.033(2) 0.018(2) 0.006(1) 0.006(1) 0.008(1) C57 0.019(2) 0.056(3) 0.022(2) 0.006(2) 0.004(2) 0.020(2) C58 0.016(2) 0.072(3) 0.017(2) 0.012(2) 0.003(1) 0.006(2) C59 0.022(2) 0.044(2) 0.021(2) 0.006(2) 0.004(2) -0.010(2) C60 0.019(2) 0.027(2) 0.018(2) 0.005(1) 0.005(1) -0.003(1) C61 0.012(1) 0.012(1) 0.014(1) 0.005(1) 0.004(1) 0.005(1) C62 0.017(2) 0.014(1) 0.017(2) 0.006(1) 0.003(1) 0.003(1) C63 0.014(2) 0.016(2) 0.021(2) 0.000(1) 0.001(1) 0.008(1) C64 0.016(2) 0.021(2) 0.022(2) 0.005(1) 0.009(1) 0.009(1) C65 0.019(2) 0.022(2) 0.021(2) 0.007(1) 0.009(1) 0.000(1) C66 0.015(2) 0.017(2) 0.017(2) -0.000(1) 0.002(1) 0.001(1) C67 0.016(2) 0.016(2) 0.019(2) 0.005(1) 0.004(1) 0.004(1) C68 0.023(2) 0.025(2) 0.026(2) 0.005(2) -0.001(2) 0.012(2) C69 0.018(2) 0.022(2) 0.044(2) 0.010(1) 0.003(2) 0.016(2) C70 0.020(2) 0.019(2) 0.039(2) 0.009(1) 0.007(2) 0.009(2) C71 0.015(2) 0.014(1) 0.024(2) 0.005(1) 0.007(1) 0.002(1) C72 0.011(1) 0.010(1) 0.019(2) 0.001(1) -0.001(1) 0.003(1) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . P4 . 2.2361(8) yes Pt1 . P5 . 2.2322(8) yes Pt1 . O1 . 2.076(2) yes Pt1 . O2 . 2.091(2) yes Cl1 . C73 . 1.770(4) yes Cl2 . C73 . 1.762(4) yes Cl3 . C74 . 1.765(4) yes Cl4 . C74 . 1.763(4) yes Cl5 . C75 . 1.722(8) yes P1 . O1 . 1.513(2) yes P1 . O4 . 1.468(2) yes P1 . O5 . 1.615(2) yes P1 . O9 . 1.592(2) yes P2 . O2 . 1.522(2) yes P2 . O5 . 1.625(2) yes P2 . O6 . 1.462(2) yes P2 . O7 . 1.594(2) yes P3 . O3 . 1.476(2) yes P3 . O7 . 1.633(2) yes P3 . O8 . 1.467(2) yes P3 . O9 . 1.634(2) yes P4 . C1 . 1.824(3) yes P4 . C7 . 1.827(3) yes P4 . C13 . 1.815(3) yes P5 . C19 . 1.820(3) yes P5 . C25 . 1.824(3) yes P5 . C31 . 1.811(3) yes P6 . N1 . 1.582(3) yes P6 . C37 . 1.804(3) yes P6 . C43 . 1.795(3) yes P6 . C49 . 1.802(3) yes P7 . N1 . 1.586(3) yes P7 . C55 . 1.801(3) yes P7 . C61 . 1.792(3) yes P7 . C72 . 1.796(3) yes C1 . C2 . 1.396(4) yes C1 . C6 . 1.388(4) yes C2 . C3 . 1.394(5) yes C3 . C4 . 1.386(5) yes C4 . C5 . 1.387(5) yes C5 . C6 . 1.387(5) yes C7 . C8 . 1.398(4) yes C7 . C12 . 1.381(5) yes C8 . C9 . 1.389(5) yes C9 . C10 . 1.392(5) yes C10 . C11 . 1.384(5) yes C11 . C12 . 1.392(5) yes C13 . C14 . 1.401(4) yes C13 . C18 . 1.398(4) yes C14 . C15 . 1.385(4) yes C15 . C16 . 1.384(5) yes C16 . C17 . 1.381(5) yes C17 . C18 . 1.387(5) yes C19 . C20 . 1.404(5) yes C19 . C24 . 1.391(5) yes C20 . C21 . 1.390(4) yes C21 . C22 . 1.384(5) yes C22 . C23 . 1.387(5) yes C23 . C24 . 1.396(5) yes C25 . C26 . 1.394(5) yes C25 . C30 . 1.380(5) yes C26 . C27 . 1.392(5) yes C27 . C28 . 1.376(6) yes C28 . C29 . 1.379(6) yes C29 . C30 . 1.395(5) yes C31 . C32 . 1.391(5) yes C31 . C36 . 1.405(5) yes C32 . C33 . 1.391(5) yes C33 . C34 . 1.385(5) yes C34 . C35 . 1.392(5) yes C35 . C36 . 1.383(5) yes C37 . C38 . 1.396(4) yes C37 . C42 . 1.388(5) yes C38 . C39 . 1.388(5) yes C39 . C40 . 1.378(6) yes C40 . C41 . 1.389(5) yes C41 . C42 . 1.391(5) yes C43 . C44 . 1.395(5) yes C43 . C48 . 1.396(5) yes C44 . C45 . 1.395(5) yes C45 . C46 . 1.383(5) yes C46 . C47 . 1.389(5) yes C47 . C48 . 1.394(5) yes C49 . C50 . 1.390(5) yes C49 . C54 . 1.406(5) yes C50 . C51 . 1.385(5) yes C51 . C52 . 1.382(5) yes C52 . C53 . 1.391(5) yes C53 . C54 . 1.378(5) yes C55 . C56 . 1.394(5) yes C55 . C60 . 1.397(5) yes C56 . C57 . 1.394(5) yes C57 . C58 . 1.385(6) yes C58 . C59 . 1.379(6) yes C59 . C60 . 1.396(5) yes C61 . C62 . 1.401(4) yes C61 . C66 . 1.395(5) yes C62 . C63 . 1.386(5) yes C63 . C64 . 1.384(5) yes C64 . C65 . 1.385(5) yes C65 . C66 . 1.392(5) yes C67 . C68 . 1.387(5) yes C67 . C72 . 1.404(4) yes C68 . C69 . 1.394(6) yes C69 . C70 . 1.377(5) yes C70 . C71 . 1.395(5) yes C71 . C72 . 1.395(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P4 . Pt1 . P5 . 98.38(3) yes P4 . Pt1 . O1 . 171.34(6) yes P5 . Pt1 . O1 . 88.65(7) yes P4 . Pt1 . O2 . 84.59(6) yes P5 . Pt1 . O2 . 176.43(6) yes O1 . Pt1 . O2 . 88.22(9) yes O1 . P1 . O4 . 117.82(14) yes O1 . P1 . O5 . 107.14(12) yes O4 . P1 . O5 . 110.03(13) yes O1 . P1 . O9 . 109.84(12) yes O4 . P1 . O9 . 109.80(13) yes O5 . P1 . O9 . 100.84(12) yes O2 . P2 . O5 . 106.58(12) yes O2 . P2 . O6 . 117.81(14) yes O5 . P2 . O6 . 110.20(13) yes O2 . P2 . O7 . 109.42(12) yes O5 . P2 . O7 . 101.32(12) yes O6 . P2 . O7 . 110.19(13) yes O3 . P3 . O7 . 109.06(13) yes O3 . P3 . O8 . 123.00(14) yes O7 . P3 . O8 . 107.22(14) yes O3 . P3 . O9 . 108.67(13) yes O7 . P3 . O9 . 99.35(12) yes O8 . P3 . O9 . 106.99(13) yes Pt1 . P4 . C1 . 109.3(1) yes Pt1 . P4 . C7 . 122.4(1) yes C1 . P4 . C7 . 103.32(14) yes Pt1 . P4 . C13 . 110.2(1) yes C1 . P4 . C13 . 107.19(14) yes C7 . P4 . C13 . 103.42(14) yes Pt1 . P5 . C19 . 112.76(11) yes Pt1 . P5 . C25 . 110.68(11) yes C19 . P5 . C25 . 105.59(15) yes Pt1 . P5 . C31 . 115.99(11) yes C19 . P5 . C31 . 108.68(15) yes C25 . P5 . C31 . 102.16(15) yes N1 . P6 . C37 . 107.71(15) yes N1 . P6 . C43 . 114.88(15) yes C37 . P6 . C43 . 109.29(15) yes N1 . P6 . C49 . 110.49(15) yes C37 . P6 . C49 . 107.26(15) yes C43 . P6 . C49 . 106.97(15) yes N1 . P7 . C55 . 113.93(15) yes N1 . P7 . C61 . 106.59(15) yes C55 . P7 . C61 . 106.34(15) yes N1 . P7 . C72 . 113.26(14) yes C55 . P7 . C72 . 108.57(16) yes C61 . P7 . C72 . 107.74(14) yes Pt1 . O1 . P1 . 132.09(13) yes Pt1 . O2 . P2 . 128.80(13) yes P1 . O5 . P2 . 121.87(14) yes P2 . O7 . P3 . 130.76(15) yes P1 . O9 . P3 . 127.33(14) yes P6 . N1 . P7 . 135.67(19) yes P4 . C1 . C2 . 118.0(2) yes P4 . C1 . C6 . 122.2(2) yes C2 . C1 . C6 . 119.7(3) yes C1 . C2 . C3 . 119.8(3) yes C2 . C3 . C4 . 120.3(3) yes C3 . C4 . C5 . 119.6(3) yes C4 . C5 . C6 . 120.6(3) yes C1 . C6 . C5 . 120.0(3) yes P4 . C7 . C8 . 119.8(3) yes P4 . C7 . C12 . 120.7(2) yes C8 . C7 . C12 . 119.5(3) yes C7 . C8 . C9 . 120.0(3) yes C8 . C9 . C10 . 120.4(3) yes C9 . C10 . C11 . 119.4(3) yes C10 . C11 . C12 . 120.4(4) yes C7 . C12 . C11 . 120.4(3) yes P4 . C13 . C14 . 118.7(2) yes P4 . C13 . C18 . 122.8(2) yes C14 . C13 . C18 . 118.6(3) yes C13 . C14 . C15 . 121.2(3) yes C14 . C15 . C16 . 119.2(3) yes C15 . C16 . C17 . 120.5(3) yes C16 . C17 . C18 . 120.5(3) yes C13 . C18 . C17 . 119.9(3) yes P5 . C19 . C20 . 116.6(2) yes P5 . C19 . C24 . 123.9(3) yes C20 . C19 . C24 . 119.5(3) yes C19 . C20 . C21 . 119.9(3) yes C20 . C21 . C22 . 120.3(3) yes C21 . C22 . C23 . 120.2(3) yes C22 . C23 . C24 . 120.0(3) yes C19 . C24 . C23 . 120.1(3) yes P5 . C25 . C26 . 118.1(3) yes P5 . C25 . C30 . 122.4(3) yes C26 . C25 . C30 . 119.4(3) yes C25 . C26 . C27 . 120.6(3) yes C26 . C27 . C28 . 119.6(3) yes C27 . C28 . C29 . 120.2(3) yes C28 . C29 . C30 . 120.5(4) yes C25 . C30 . C29 . 119.8(3) yes P5 . C31 . C32 . 121.2(3) yes P5 . C31 . C36 . 120.3(2) yes C32 . C31 . C36 . 118.5(3) yes C31 . C32 . C33 . 120.6(3) yes C32 . C33 . C34 . 120.5(3) yes C33 . C34 . C35 . 119.3(3) yes C34 . C35 . C36 . 120.4(3) yes C31 . C36 . C35 . 120.5(3) yes P6 . C37 . C38 . 121.6(3) yes P6 . C37 . C42 . 118.3(2) yes C38 . C37 . C42 . 119.9(3) yes C37 . C38 . C39 . 119.3(3) yes C38 . C39 . C40 . 120.9(3) yes C39 . C40 . C41 . 119.8(3) yes C40 . C41 . C42 . 119.9(4) yes C37 . C42 . C41 . 120.1(3) yes P6 . C43 . C44 . 119.8(3) yes P6 . C43 . C48 . 119.8(3) yes C44 . C43 . C48 . 119.7(3) yes C43 . C44 . C45 . 120.0(3) yes C44 . C45 . C46 . 120.3(3) yes C45 . C46 . C47 . 119.8(3) yes C46 . C47 . C48 . 120.6(3) yes C43 . C48 . C47 . 119.6(3) yes P6 . C49 . C50 . 121.2(3) yes P6 . C49 . C54 . 119.4(2) yes C50 . C49 . C54 . 119.3(3) yes C49 . C50 . C51 . 119.9(3) yes C50 . C51 . C52 . 120.2(3) yes C51 . C52 . C53 . 120.7(3) yes C52 . C53 . C54 . 119.2(3) yes C49 . C54 . C53 . 120.6(3) yes P7 . C55 . C56 . 118.9(3) yes P7 . C55 . C60 . 120.8(3) yes C56 . C55 . C60 . 119.9(3) yes C55 . C56 . C57 . 120.4(4) yes C56 . C57 . C58 . 119.2(4) yes C57 . C58 . C59 . 120.8(4) yes C58 . C59 . C60 . 120.5(4) yes C55 . C60 . C59 . 119.1(4) yes P7 . C61 . C62 . 119.8(2) yes P7 . C61 . C66 . 120.3(2) yes C62 . C61 . C66 . 119.9(3) yes C61 . C62 . C63 . 119.8(3) yes C62 . C63 . C64 . 120.1(3) yes C63 . C64 . C65 . 120.3(3) yes C64 . C65 . C66 . 120.3(3) yes C61 . C66 . C65 . 119.5(3) yes C68 . C67 . C72 . 119.0(3) yes C67 . C68 . C69 . 120.6(3) yes C68 . C69 . C70 . 120.4(3) yes C69 . C70 . C71 . 119.9(4) yes C70 . C71 . C72 . 120.0(3) yes P7 . C72 . C67 . 118.0(3) yes P7 . C72 . C71 . 121.5(2) yes C67 . C72 . C71 . 120.1(3) yes Cl1 . C73 . Cl2 . 111.7(2) yes Cl3 . C74 . Cl4 . 112.0(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag P5 . Pt1 . P4 . C1 . -136.7(2) yes P5 . Pt1 . P4 . C7 . -15.9(2) yes P5 . Pt1 . P4 . C13 . 105.8(2) yes O1 . Pt1 . P4 . C1 . 79.3(2) yes O1 . Pt1 . P4 . C7 . -160.0(2) yes O1 . Pt1 . P4 . C13 . -38.3(2) yes O2 . Pt1 . P4 . C1 . 45.3(3) yes O2 . Pt1 . P4 . C7 . 166.1(3) yes O2 . Pt1 . P4 . C13 . -72.2(3) yes P4 . Pt1 . P5 . C19 . 58.8(2) yes P4 . Pt1 . P5 . C25 . 176.8(2) yes P4 . Pt1 . P5 . C31 . -67.4(2) yes O1 . Pt1 . P5 . C19 . -126.3(3) yes O1 . Pt1 . P5 . C25 . -8.2(3) yes O1 . Pt1 . P5 . C31 . 107.5(3) yes O2 . Pt1 . P5 . C19 . -155.1(4) yes O2 . Pt1 . P5 . C25 . -37.1(4) yes O2 . Pt1 . P5 . C31 . 78.7(4) yes P4 . Pt1 . O1 . P1 . -61.6(1) yes P5 . Pt1 . O1 . P1 . 154.0(4) yes O2 . Pt1 . O1 . P1 . -27.8(4) yes P4 . Pt1 . O2 . P2 . -153.3(3) yes P5 . Pt1 . O2 . P2 . 60.3(3) yes O1 . Pt1 . O2 . P2 . 31.5(4) yes O4 . P1 . O1 . Pt1 . 166.6(3) yes O5 . P1 . O1 . Pt1 . 42.0(4) yes O9 . P1 . O1 . Pt1 . -66.7(4) yes O1 . P1 . O5 . P2 . -58.0(4) yes O4 . P1 . O5 . P2 . 172.8(3) yes O9 . P1 . O5 . P2 . 56.9(4) yes O1 . P1 . O9 . P3 . 58.8(4) yes O4 . P1 . O9 . P3 . -170.2(3) yes O5 . P1 . O9 . P3 . -54.1(4) yes O5 . P2 . O2 . Pt1 . -49.4(4) yes O6 . P2 . O2 . Pt1 . -173.8(2) yes O7 . P2 . O2 . Pt1 . 59.4(4) yes O2 . P2 . O5 . P1 . 62.2(4) yes O6 . P2 . O5 . P1 . -168.9(3) yes O7 . P2 . O5 . P1 . -52.2(4) yes O2 . P2 . O7 . P3 . -68.1(4) yes O5 . P2 . O7 . P3 . 44.1(4) yes O6 . P2 . O7 . P3 . 160.8(3) yes O3 . P3 . O7 . P2 . 74.4(4) yes O8 . P3 . O7 . P2 . -150.4(3) yes O9 . P3 . O7 . P2 . -39.2(4) yes O3 . P3 . O9 . P1 . -69.6(4) yes O7 . P3 . O9 . P1 . 44.3(4) yes O8 . P3 . O9 . P1 . 155.7(3) yes Pt1 . P4 . C1 . C2 . 38.2(5) yes Pt1 . P4 . C1 . C6 . -143.8(4) yes C7 . P4 . C1 . C2 . -93.6(5) yes C7 . P4 . C1 . C6 . 84.4(6) yes C13 . P4 . C1 . C2 . 157.6(5) yes C13 . P4 . C1 . C6 . -24.4(6) yes Pt1 . P4 . C7 . C8 . -93.1(4) yes Pt1 . P4 . C7 . C12 . 87.9(5) yes C1 . P4 . C7 . C8 . 30.5(6) yes C1 . P4 . C7 . C12 . -148.6(5) yes C13 . P4 . C7 . C8 . 142.1(5) yes C13 . P4 . C7 . C12 . -36.9(6) yes Pt1 . P4 . C13 . C14 . 9.5(5) yes Pt1 . P4 . C13 . C18 . -170.3(4) yes C1 . P4 . C13 . C14 . -109.4(5) yes C1 . P4 . C13 . C18 . 70.9(6) yes C7 . P4 . C13 . C14 . 141.9(5) yes C7 . P4 . C13 . C18 . -37.9(6) yes Pt1 . P5 . C19 . C20 . 45.5(5) yes Pt1 . P5 . C19 . C24 . -136.1(4) yes C25 . P5 . C19 . C20 . -75.5(6) yes C25 . P5 . C19 . C24 . 103.0(6) yes C31 . P5 . C19 . C20 . 175.6(4) yes C31 . P5 . C19 . C24 . -6.0(7) yes Pt1 . P5 . C25 . C26 . 73.5(5) yes Pt1 . P5 . C25 . C30 . -101.4(5) yes C19 . P5 . C25 . C26 . -164.2(5) yes C19 . P5 . C25 . C30 . 20.9(7) yes C31 . P5 . C25 . C26 . -50.6(6) yes C31 . P5 . C25 . C30 . 134.5(5) yes Pt1 . P5 . C31 . C32 . 4.1(5) yes Pt1 . P5 . C31 . C36 . -173.4(4) yes C19 . P5 . C31 . C32 . -124.2(5) yes C19 . P5 . C31 . C36 . 58.3(6) yes C25 . P5 . C31 . C32 . 124.5(5) yes C25 . P5 . C31 . C36 . -52.9(6) yes C37 . P6 . N1 . P7 . 123.3(5) yes C43 . P6 . N1 . P7 . 1.3(7) yes C49 . P6 . N1 . P7 . -119.8(5) yes N1 . P6 . C37 . C38 . -169.1(5) yes N1 . P6 . C37 . C42 . 15.2(6) yes C43 . P6 . C37 . C38 . -43.7(7) yes C43 . P6 . C37 . C42 . 140.6(5) yes C49 . P6 . C37 . C38 . 71.9(6) yes C49 . P6 . C37 . C42 . -103.7(5) yes N1 . P6 . C43 . C44 . -91.3(6) yes N1 . P6 . C43 . C48 . 79.1(6) yes C37 . P6 . C43 . C44 . 147.5(5) yes C37 . P6 . C43 . C48 . -42.0(6) yes C49 . P6 . C43 . C44 . 31.7(6) yes C49 . P6 . C43 . C48 . -157.9(5) yes N1 . P6 . C49 . C50 . -0.5(7) yes N1 . P6 . C49 . C54 . -178.9(5) yes C37 . P6 . C49 . C50 . 116.6(5) yes C37 . P6 . C49 . C54 . -61.8(6) yes C43 . P6 . C49 . C50 . -126.2(5) yes C43 . P6 . C49 . C54 . 55.4(6) yes C55 . P7 . N1 . P6 . -69.3(6) yes C61 . P7 . N1 . P6 . 173.8(4) yes C72 . P7 . N1 . P6 . 55.5(6) yes N1 . P7 . C55 . C56 . -20.1(7) yes N1 . P7 . C55 . C60 . 167.1(5) yes C61 . P7 . C55 . C56 . 97.0(6) yes C61 . P7 . C55 . C60 . -75.8(6) yes C72 . P7 . C55 . C56 . -147.3(5) yes C72 . P7 . C55 . C60 . 39.9(7) yes N1 . P7 . C61 . C62 . 164.0(4) yes N1 . P7 . C61 . C66 . -17.3(6) yes C55 . P7 . C61 . C62 . 42.1(6) yes C55 . P7 . C61 . C66 . -139.2(5) yes C72 . P7 . C61 . C62 . -74.1(6) yes C72 . P7 . C61 . C66 . 104.5(5) yes N1 . P7 . C72 . C67 . 76.7(6) yes N1 . P7 . C72 . C71 . -96.2(6) yes C55 . P7 . C72 . C67 . -155.7(5) yes C55 . P7 . C72 . C71 . 31.4(7) yes C61 . P7 . C72 . C67 . -41.0(6) yes C61 . P7 . C72 . C71 . 146.2(5) yes P4 . C1 . C2 . C3 . 178.4(3) yes C6 . C1 . C2 . C3 . 0.4(7) yes P4 . C1 . C6 . C5 . -178.2(3) yes C2 . C1 . C6 . C5 . -0.3(7) yes C1 . C2 . C3 . C4 . -0.3(7) yes C2 . C3 . C4 . C5 . 0.2(7) yes C3 . C4 . C5 . C6 . -0.1(8) yes C4 . C5 . C6 . C1 . 0.2(7) yes P4 . C7 . C8 . C9 . -178.6(3) yes C12 . C7 . C8 . C9 . 0.5(7) yes P4 . C7 . C12 . C11 . 178.8(3) yes C8 . C7 . C12 . C11 . -0.3(7) yes C7 . C8 . C9 . C10 . -0.5(7) yes C8 . C9 . C10 . C11 . 0.3(8) yes C9 . C10 . C11 . C12 . -0.1(8) yes C10 . C11 . C12 . C7 . 0.1(8) yes P4 . C13 . C14 . C15 . -178.2(3) yes C18 . C13 . C14 . C15 . 1.5(7) yes P4 . C13 . C18 . C17 . 179.6(3) yes C14 . C13 . C18 . C17 . -0.2(7) yes C13 . C14 . C15 . C16 . -0.9(7) yes C14 . C15 . C16 . C17 . -1.1(7) yes C15 . C16 . C17 . C18 . 2.5(7) yes C16 . C17 . C18 . C13 . -1.8(7) yes P5 . C19 . C20 . C21 . 177.3(3) yes C24 . C19 . C20 . C21 . -1.2(7) yes P5 . C19 . C24 . C23 . -178.3(3) yes C20 . C19 . C24 . C23 . 0.1(7) yes C19 . C20 . C21 . C22 . 1.2(7) yes C20 . C21 . C22 . C23 . -0.2(7) yes C21 . C22 . C23 . C24 . -0.9(7) yes C22 . C23 . C24 . C19 . 1.0(7) yes P5 . C25 . C26 . C27 . -175.4(4) yes C30 . C25 . C26 . C27 . -0.3(8) yes P5 . C25 . C30 . C29 . 175.7(4) yes C26 . C25 . C30 . C29 . 0.8(8) yes C25 . C26 . C27 . C28 . -0.1(8) yes C26 . C27 . C28 . C29 . -0.1(8) yes C27 . C28 . C29 . C30 . 0.6(9) yes C28 . C29 . C30 . C25 . -0.9(9) yes P5 . C31 . C32 . C33 . 179.2(3) yes C36 . C31 . C32 . C33 . -3.2(7) yes P5 . C31 . C36 . C35 . -178.5(3) yes C32 . C31 . C36 . C35 . 3.9(7) yes C31 . C32 . C33 . C34 . 0.2(7) yes C32 . C33 . C34 . C35 . 2.3(8) yes C33 . C34 . C35 . C36 . -1.6(8) yes C34 . C35 . C36 . C31 . -1.6(8) yes P6 . C37 . C38 . C39 . -174.8(3) yes C42 . C37 . C38 . C39 . 0.8(7) yes P6 . C37 . C42 . C41 . 174.4(3) yes C38 . C37 . C42 . C41 . -1.3(8) yes C37 . C38 . C39 . C40 . 0.6(7) yes C38 . C39 . C40 . C41 . -1.4(8) yes C39 . C40 . C41 . C42 . 0.8(8) yes C40 . C41 . C42 . C37 . 0.5(8) yes P6 . C43 . C44 . C45 . 169.9(3) yes C48 . C43 . C44 . C45 . -0.5(7) yes P6 . C43 . C48 . C47 . -169.4(3) yes C44 . C43 . C48 . C47 . 1.0(7) yes C43 . C44 . C45 . C46 . -0.8(7) yes C44 . C45 . C46 . C47 . 1.4(8) yes C45 . C46 . C47 . C48 . -0.9(8) yes C46 . C47 . C48 . C43 . -0.3(8) yes P6 . C49 . C50 . C51 . -178.7(3) yes C54 . C49 . C50 . C51 . -0.3(7) yes P6 . C49 . C54 . C53 . 179.5(3) yes C50 . C49 . C54 . C53 . 1.1(8) yes C49 . C50 . C51 . C52 . -0.4(8) yes C50 . C51 . C52 . C53 . 0.4(8) yes C51 . C52 . C53 . C54 . 0.4(8) yes C52 . C53 . C54 . C49 . -1.1(8) yes P7 . C55 . C56 . C57 . -172.4(4) yes C60 . C55 . C56 . C57 . 0.5(8) yes P7 . C55 . C60 . C59 . 171.1(4) yes C56 . C55 . C60 . C59 . -1.6(8) yes C55 . C56 . C57 . C58 . 1.3(8) yes C56 . C57 . C58 . C59 . -2.1(8) yes C57 . C58 . C59 . C60 . 1.0(9) yes C58 . C59 . C60 . C55 . 0.9(8) yes P7 . C61 . C62 . C63 . 178.7(3) yes C66 . C61 . C62 . C63 . 0.0(7) yes P7 . C61 . C66 . C65 . -177.4(3) yes C62 . C61 . C66 . C65 . 1.2(7) yes C61 . C62 . C63 . C64 . -0.9(7) yes C62 . C63 . C64 . C65 . 0.7(7) yes C63 . C64 . C65 . C66 . 0.6(7) yes C64 . C65 . C66 . C61 . -1.5(7) yes C72 . C67 . C68 . C69 . 0.8(7) yes C68 . C67 . C72 . P7 . -172.9(4) yes C68 . C67 . C72 . C71 . 0.0(7) yes C67 . C68 . C69 . C70 . -1.3(8) yes C68 . C69 . C70 . C71 . 1.1(8) yes C69 . C70 . C71 . C72 . -0.3(8) yes C70 . C71 . C72 . P7 . 172.4(4) yes C70 . C71 . C72 . C67 . -0.3(7) yes #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #===END data_(PPN)[Pt(P3O9)(PMePh2)2](4) _database_code_CSD 202876 _audit_creation_date 'Thu Apr 3 14:10:45 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C64 H59 N2 O9 P7 Pt ' _chemical_formula_moiety (PPN)[Pt(P3O9)(PMePh2)2] _chemical_formula_weight 1412.08 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.687(1) _cell_length_b 14.866(2) _cell_length_c 18.923(2) _cell_angle_alpha 106.24(1) _cell_angle_beta 97.076(9) _cell_angle_gamma 110.016(9) _cell_volume 3123.3(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.6 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.474 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 14891 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max ? _diffrn_measured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3.16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; for calculating R-factor (gt). ; _reflns_number_total 14339 _reflns_number_gt 10966 _reflns_threshold_criterion F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0320 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 10966 _refine_ls_number_parameters 749 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00020|Fo|^2^]' _refine_ls_shift/su_max 0.0410 _refine_diff_density_max 1.02 _refine_diff_density_min -0.76 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0025(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt 0.14766(1) 0.22915(1) 0.451513(8) 0.03014(4) Uani 1.00 d . . . P(1) P -0.06045(8) 0.17632(7) 0.30935(6) 0.0337(2) Uani 1.00 d . . . P(2) P 0.05567(8) 0.04241(7) 0.28756(5) 0.0337(2) Uani 1.00 d . . . P(3) P 0.14540(9) 0.22434(9) 0.24961(7) 0.0454(3) Uani 1.00 d . . . P(4) P 0.31247(8) 0.22356(7) 0.50026(5) 0.0322(2) Uani 1.00 d . . . P(5) P 0.14498(8) 0.35598(8) 0.54613(6) 0.0377(3) Uani 1.00 d . . . P(6) P 0.71929(8) 0.28959(7) 0.10170(5) 0.0336(3) Uani 1.00 d . . . P(7) P 0.67627(8) 0.32351(8) -0.04257(5) 0.0354(3) Uani 1.00 d . . . O(1) O -0.0030(2) 0.2284(2) 0.3930(1) 0.0416(7) Uani 1.00 d . . . O(2) O 0.1265(2) 0.0925(2) 0.3684(1) 0.0374(7) Uani 1.00 d . . . O(3) O 0.2332(2) 0.2874(2) 0.3214(2) 0.0587(9) Uani 1.00 d . . . O(4) O -0.1770(2) 0.1708(2) 0.2862(2) 0.0451(8) Uani 1.00 d . . . O(5) O -0.0603(2) 0.0639(2) 0.2854(1) 0.0348(7) Uani 1.00 d . . . O(6) O 0.0264(2) -0.0664(2) 0.2523(2) 0.0502(8) Uani 1.00 d . . . O(7) O 0.1173(2) 0.1040(2) 0.2373(1) 0.0418(8) Uani 1.00 d . . . O(8) O 0.1582(3) 0.2394(3) 0.1775(2) 0.070(1) Uani 1.00 d . . . O(9) O 0.0205(2) 0.2264(2) 0.2615(2) 0.0443(8) Uani 1.00 d . . . N(1) N 0.6700(3) 0.3301(2) 0.0413(2) 0.0394(9) Uani 1.00 d . . . N(2) N 0.6742(8) 0.2142(8) 0.6521(7) 0.238(6) Uani 1.00 d . . . C(1) C 0.2914(3) 0.1120(3) 0.5278(2) 0.0362(10) Uani 1.00 d . . . C(2) C 0.3797(4) 0.0794(3) 0.5395(3) 0.052(1) Uani 1.00 d . . . C(3) C 0.3608(4) -0.0058(4) 0.5604(3) 0.063(2) Uani 1.00 d . . . C(4) C 0.2542(5) -0.0591(4) 0.5692(3) 0.063(2) Uani 1.00 d . . . C(5) C 0.1663(4) -0.0281(3) 0.5569(3) 0.060(1) Uani 1.00 d . . . C(6) C 0.1832(3) 0.0566(3) 0.5359(2) 0.045(1) Uani 1.00 d . . . C(7) C 0.4183(3) 0.3322(3) 0.5782(2) 0.0353(10) Uani 1.00 d . . . C(8) C 0.4547(3) 0.4271(3) 0.5686(2) 0.040(1) Uani 1.00 d . . . C(9) C 0.5377(3) 0.5122(3) 0.6254(3) 0.048(1) Uani 1.00 d . . . C(10) C 0.5863(4) 0.5040(3) 0.6912(3) 0.055(1) Uani 1.00 d . . . C(11) C 0.5504(4) 0.4113(4) 0.7011(3) 0.061(1) Uani 1.00 d . . . C(12) C 0.4664(4) 0.3253(3) 0.6451(2) 0.052(1) Uani 1.00 d . . . C(13) C 0.3900(3) 0.2105(3) 0.4262(2) 0.045(1) Uani 1.00 d . . . C(14) C 0.2077(3) 0.4816(3) 0.5392(2) 0.041(1) Uani 1.00 d . . . C(15) C 0.2406(3) 0.4909(3) 0.4736(2) 0.043(1) Uani 1.00 d . . . C(16) C 0.2771(4) 0.5850(3) 0.4641(3) 0.053(1) Uani 1.00 d . . . C(17) C 0.2820(4) 0.6692(3) 0.5199(3) 0.060(2) Uani 1.00 d . . . C(18) C 0.2503(4) 0.6622(3) 0.5856(3) 0.064(2) Uani 1.00 d . . . C(19) C 0.2118(4) 0.5685(3) 0.5951(3) 0.054(1) Uani 1.00 d . . . C(20) C 0.1977(3) 0.3595(3) 0.6408(2) 0.042(1) Uani 1.00 d . . . C(21) C 0.2861(4) 0.4411(3) 0.6969(2) 0.051(1) Uani 1.00 d . . . C(22) C 0.3185(4) 0.4336(4) 0.7668(2) 0.065(1) Uani 1.00 d . . . C(23) C 0.2645(5) 0.3465(4) 0.7819(3) 0.071(2) Uani 1.00 d . . . C(24) C 0.1770(5) 0.2652(4) 0.7271(3) 0.068(2) Uani 1.00 d . . . C(25) C 0.1432(4) 0.2711(3) 0.6574(3) 0.054(1) Uani 1.00 d . . . C(26) C -0.0036(4) 0.3405(4) 0.5444(3) 0.058(1) Uani 1.00 d . . . C(27) C 0.6092(3) 0.2494(3) 0.1507(2) 0.039(1) Uani 1.00 d . . . C(28) C 0.6133(4) 0.1860(4) 0.1914(3) 0.058(1) Uani 1.00 d . . . C(29) C 0.5283(4) 0.1544(5) 0.2286(3) 0.074(2) Uani 1.00 d . . . C(30) C 0.4389(4) 0.1871(5) 0.2256(3) 0.075(2) Uani 1.00 d . . . C(31) C 0.4319(4) 0.2492(4) 0.1845(3) 0.063(2) Uani 1.00 d . . . C(32) C 0.5182(3) 0.2806(3) 0.1474(2) 0.045(1) Uani 1.00 d . . . C(33) C 0.8477(3) 0.3899(3) 0.1681(2) 0.0349(10) Uani 1.00 d . . . C(34) C 0.9040(4) 0.3730(3) 0.2272(2) 0.046(1) Uani 1.00 d . . . C(35) C 1.0078(4) 0.4476(4) 0.2752(2) 0.056(1) Uani 1.00 d . . . C(36) C 1.0536(4) 0.5402(3) 0.2649(3) 0.057(1) Uani 1.00 d . . . C(37) C 0.9959(4) 0.5581(3) 0.2071(3) 0.057(1) Uani 1.00 d . . . C(38) C 0.8933(4) 0.4835(3) 0.1585(2) 0.046(1) Uani 1.00 d . . . C(39) C 0.7532(3) 0.1807(3) 0.0620(2) 0.038(1) Uani 1.00 d . . . C(40) C 0.8644(4) 0.1835(3) 0.0740(2) 0.052(1) Uani 1.00 d . . . C(41) C 0.8840(5) 0.0976(4) 0.0380(3) 0.072(2) Uani 1.00 d . . . C(42) C 0.7940(5) 0.0102(4) -0.0101(3) 0.076(2) Uani 1.00 d . . . C(43) C 0.6834(5) 0.0067(3) -0.0220(3) 0.066(2) Uani 1.00 d . . . C(44) C 0.6631(4) 0.0910(3) 0.0134(3) 0.051(1) Uani 1.00 d . . . C(45) C 0.5411(3) 0.2351(3) -0.1080(2) 0.045(1) Uani 1.00 d . . . C(46) C 0.4518(4) 0.1821(4) -0.0820(3) 0.063(1) Uani 1.00 d . . . C(47) C 0.3489(5) 0.1126(5) -0.1335(4) 0.097(2) Uani 1.00 d . . . C(48) C 0.3360(5) 0.0969(5) -0.2093(4) 0.109(2) Uani 1.00 d . . . C(49) C 0.4233(5) 0.1492(4) -0.2345(3) 0.093(2) Uani 1.00 d . . . C(50) C 0.5265(4) 0.2193(4) -0.1849(3) 0.068(1) Uani 1.00 d . . . C(51) C 0.7887(3) 0.2872(3) -0.0725(2) 0.040(1) Uani 1.00 d . . . C(52) C 0.9033(3) 0.3554(3) -0.0405(2) 0.047(1) Uani 1.00 d . . . C(53) C 0.9927(4) 0.3269(4) -0.0572(3) 0.059(1) Uani 1.00 d . . . C(54) C 0.9680(4) 0.2303(4) -0.1052(3) 0.067(2) Uani 1.00 d . . . C(55) C 0.8565(5) 0.1613(4) -0.1361(3) 0.070(2) Uani 1.00 d . . . C(56) C 0.7655(4) 0.1890(3) -0.1207(3) 0.057(1) Uani 1.00 d . . . C(57) C 0.7014(3) 0.4463(3) -0.0509(2) 0.041(1) Uani 1.00 d . . . C(58) C 0.7543(4) 0.4759(3) -0.1060(2) 0.050(1) Uani 1.00 d . . . C(59) C 0.7695(4) 0.5693(4) -0.1126(3) 0.063(2) Uani 1.00 d . . . C(60) C 0.7306(5) 0.6327(4) -0.0669(3) 0.074(2) Uani 1.00 d . . . C(61) C 0.6773(5) 0.6051(4) -0.0118(3) 0.074(2) Uani 1.00 d . . . C(62) C 0.6619(4) 0.5118(4) -0.0047(3) 0.056(1) Uani 1.00 d . . . C(63) C 0.7308(6) 0.1721(6) 0.6539(5) 0.111(3) Uani 1.00 d . . . C(64) C 0.8070(8) 0.1291(6) 0.6529(4) 0.140(4) Uani 1.00 d . . . H(1) H 0.4536 0.1156 0.5331 0.0619 Uiso 1.00 calc . . . H(2) H 0.4221 -0.0276 0.5686 0.0759 Uiso 1.00 calc . . . H(3) H 0.2418 -0.1172 0.5840 0.0762 Uiso 1.00 calc . . . H(4) H 0.0925 -0.0653 0.5628 0.0723 Uiso 1.00 calc . . . H(5) H 0.1211 0.0771 0.5271 0.0538 Uiso 1.00 calc . . . H(6) H 0.4224 0.4331 0.5230 0.0475 Uiso 1.00 calc . . . H(7) H 0.5614 0.5767 0.6188 0.0580 Uiso 1.00 calc . . . H(8) H 0.6444 0.5624 0.7296 0.0659 Uiso 1.00 calc . . . H(9) H 0.5835 0.4058 0.7468 0.0735 Uiso 1.00 calc . . . H(10) H 0.4419 0.2615 0.6527 0.0620 Uiso 1.00 calc . . . H(11) H 0.3980 0.2637 0.4061 0.0543 Uiso 1.00 calc . . . H(12) H 0.3484 0.1464 0.3870 0.0543 Uiso 1.00 calc . . . H(13) H 0.4645 0.2149 0.4469 0.0543 Uiso 1.00 calc . . . H(14) H 0.2382 0.4328 0.4351 0.0509 Uiso 1.00 calc . . . H(15) H 0.2987 0.5911 0.4188 0.0634 Uiso 1.00 calc . . . H(16) H 0.3077 0.7334 0.5130 0.0721 Uiso 1.00 calc . . . H(17) H 0.2548 0.7212 0.6241 0.0770 Uiso 1.00 calc . . . H(18) H 0.1880 0.5628 0.6399 0.0648 Uiso 1.00 calc . . . H(19) H 0.3246 0.5020 0.6873 0.0606 Uiso 1.00 calc . . . H(20) H 0.3793 0.4899 0.8052 0.0776 Uiso 1.00 calc . . . H(21) H 0.2878 0.3426 0.8302 0.0851 Uiso 1.00 calc . . . H(22) H 0.1395 0.2046 0.7372 0.0817 Uiso 1.00 calc . . . H(23) H 0.0818 0.2144 0.6198 0.0650 Uiso 1.00 calc . . . H(24) H -0.0375 0.3449 0.4986 0.0691 Uiso 1.00 calc . . . H(25) H -0.0459 0.2757 0.5474 0.0691 Uiso 1.00 calc . . . H(26) H -0.0052 0.3927 0.5864 0.0691 Uiso 1.00 calc . . . H(27) H 0.6753 0.1640 0.1938 0.0695 Uiso 1.00 calc . . . H(28) H 0.5314 0.1105 0.2562 0.0887 Uiso 1.00 calc . . . H(29) H 0.3813 0.1665 0.2520 0.0899 Uiso 1.00 calc . . . H(30) H 0.3693 0.2703 0.1816 0.0759 Uiso 1.00 calc . . . H(31) H 0.5147 0.3240 0.1195 0.0544 Uiso 1.00 calc . . . H(32) H 0.8714 0.3099 0.2351 0.0546 Uiso 1.00 calc . . . H(33) H 1.0471 0.4349 0.3150 0.0675 Uiso 1.00 calc . . . H(34) H 1.1246 0.5914 0.2974 0.0678 Uiso 1.00 calc . . . H(35) H 1.0268 0.6223 0.2007 0.0686 Uiso 1.00 calc . . . H(36) H 0.8544 0.4964 0.1188 0.0547 Uiso 1.00 calc . . . H(37) H 0.9271 0.2441 0.1067 0.0620 Uiso 1.00 calc . . . H(38) H 0.9601 0.0993 0.0468 0.0857 Uiso 1.00 calc . . . H(39) H 0.8083 -0.0479 -0.0352 0.0914 Uiso 1.00 calc . . . H(40) H 0.6211 -0.0541 -0.0548 0.0789 Uiso 1.00 calc . . . H(41) H 0.5865 0.0882 0.0048 0.0608 Uiso 1.00 calc . . . H(42) H 0.4604 0.1930 -0.0293 0.0760 Uiso 1.00 calc . . . H(43) H 0.2869 0.0755 -0.1160 0.1163 Uiso 1.00 calc . . . H(44) H 0.2652 0.0490 -0.2441 0.1310 Uiso 1.00 calc . . . H(45) H 0.4139 0.1376 -0.2874 0.1117 Uiso 1.00 calc . . . H(46) H 0.5873 0.2567 -0.2032 0.0817 Uiso 1.00 calc . . . H(47) H 0.9201 0.4221 -0.0067 0.0558 Uiso 1.00 calc . . . H(48) H 1.0707 0.3740 -0.0357 0.0707 Uiso 1.00 calc . . . H(49) H 1.0295 0.2110 -0.1170 0.0804 Uiso 1.00 calc . . . H(50) H 0.8410 0.0942 -0.1684 0.0838 Uiso 1.00 calc . . . H(51) H 0.6878 0.1413 -0.1427 0.0678 Uiso 1.00 calc . . . H(52) H 0.7799 0.4313 -0.1391 0.0603 Uiso 1.00 calc . . . H(53) H 0.8073 0.5895 -0.1492 0.0751 Uiso 1.00 calc . . . H(54) H 0.7398 0.6963 -0.0726 0.0884 Uiso 1.00 calc . . . H(55) H 0.6516 0.6502 0.0207 0.0890 Uiso 1.00 calc . . . H(56) H 0.6240 0.4921 0.0321 0.0670 Uiso 1.00 calc . . . H(57) H 0.7810 0.0733 0.6707 0.1682 Uiso 1.00 calc . . . H(58) H 0.8146 0.1050 0.6025 0.1682 Uiso 1.00 calc . . . H(59) H 0.8797 0.1778 0.6848 0.1682 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.02741(7) 0.02991(7) 0.02849(8) 0.00822(5) 0.00323(5) 0.00850(5) P(1) 0.0274(5) 0.0359(5) 0.0366(5) 0.0110(4) 0.0036(4) 0.0143(4) P(2) 0.0328(5) 0.0299(5) 0.0331(5) 0.0091(4) 0.0067(4) 0.0077(4) P(3) 0.0342(5) 0.0527(7) 0.0547(7) 0.0105(5) 0.0139(5) 0.0330(6) P(4) 0.0271(5) 0.0354(5) 0.0321(5) 0.0084(4) 0.0054(4) 0.0138(4) P(5) 0.0322(5) 0.0386(5) 0.0348(5) 0.0107(4) 0.0075(4) 0.0058(4) P(6) 0.0312(5) 0.0394(5) 0.0304(5) 0.0121(4) 0.0068(4) 0.0146(4) P(7) 0.0319(5) 0.0388(5) 0.0292(5) 0.0072(4) 0.0031(4) 0.0125(4) O(1) 0.037(1) 0.041(2) 0.040(2) 0.017(1) -0.001(1) 0.006(1) O(2) 0.041(1) 0.034(1) 0.035(1) 0.017(1) 0.003(1) 0.009(1) O(3) 0.038(2) 0.049(2) 0.073(2) 0.001(1) -0.001(1) 0.023(2) O(4) 0.028(1) 0.057(2) 0.048(2) 0.017(1) 0.001(1) 0.017(1) O(5) 0.028(1) 0.032(1) 0.038(1) 0.005(1) 0.005(1) 0.011(1) O(6) 0.056(2) 0.034(1) 0.051(2) 0.015(1) 0.010(1) 0.005(1) O(7) 0.038(1) 0.051(2) 0.041(2) 0.017(1) 0.015(1) 0.019(1) O(8) 0.062(2) 0.102(3) 0.069(2) 0.030(2) 0.032(2) 0.061(2) O(9) 0.037(1) 0.049(2) 0.059(2) 0.017(1) 0.016(1) 0.034(1) N(1) 0.040(2) 0.049(2) 0.035(2) 0.020(2) 0.009(1) 0.020(2) N(2) 0.147(8) 0.22(1) 0.39(2) 0.121(8) 0.058(9) 0.10(1) C(1) 0.037(2) 0.035(2) 0.034(2) 0.010(2) 0.004(2) 0.014(2) C(2) 0.046(2) 0.054(3) 0.059(3) 0.021(2) 0.010(2) 0.024(2) C(3) 0.072(3) 0.063(3) 0.072(3) 0.044(3) 0.011(3) 0.028(3) C(4) 0.091(4) 0.047(3) 0.062(3) 0.029(3) 0.020(3) 0.029(2) C(5) 0.063(3) 0.050(3) 0.070(3) 0.013(2) 0.023(3) 0.031(2) C(6) 0.044(2) 0.044(2) 0.053(3) 0.017(2) 0.016(2) 0.024(2) C(7) 0.026(2) 0.039(2) 0.035(2) 0.007(2) 0.002(1) 0.013(2) C(8) 0.031(2) 0.045(2) 0.043(2) 0.009(2) 0.009(2) 0.022(2) C(9) 0.041(2) 0.039(2) 0.058(3) 0.005(2) 0.009(2) 0.020(2) C(10) 0.042(2) 0.046(3) 0.053(3) 0.004(2) -0.004(2) 0.005(2) C(11) 0.065(3) 0.056(3) 0.042(3) 0.013(2) -0.018(2) 0.011(2) C(12) 0.057(3) 0.042(2) 0.043(2) 0.007(2) -0.008(2) 0.018(2) C(13) 0.037(2) 0.063(3) 0.037(2) 0.017(2) 0.013(2) 0.021(2) C(14) 0.036(2) 0.035(2) 0.046(2) 0.016(2) 0.006(2) 0.008(2) C(15) 0.036(2) 0.042(2) 0.049(2) 0.018(2) 0.007(2) 0.012(2) C(16) 0.049(3) 0.050(3) 0.070(3) 0.024(2) 0.018(2) 0.028(2) C(17) 0.048(3) 0.040(2) 0.093(4) 0.019(2) 0.012(3) 0.025(3) C(18) 0.062(3) 0.040(3) 0.079(4) 0.027(2) 0.002(3) 0.000(2) C(19) 0.056(3) 0.050(3) 0.052(3) 0.026(2) 0.012(2) 0.005(2) C(20) 0.042(2) 0.045(2) 0.036(2) 0.015(2) 0.015(2) 0.007(2) C(21) 0.055(3) 0.042(2) 0.040(2) 0.009(2) 0.008(2) 0.007(2) C(22) 0.081(4) 0.057(3) 0.034(2) 0.013(3) 0.000(2) 0.006(2) C(23) 0.102(4) 0.067(3) 0.041(3) 0.031(3) 0.015(3) 0.019(3) C(24) 0.089(4) 0.058(3) 0.057(3) 0.018(3) 0.027(3) 0.028(3) C(25) 0.059(3) 0.041(2) 0.047(3) 0.006(2) 0.013(2) 0.009(2) C(26) 0.038(2) 0.069(3) 0.052(3) 0.022(2) 0.008(2) 0.000(2) C(27) 0.033(2) 0.048(2) 0.031(2) 0.011(2) 0.007(2) 0.013(2) C(28) 0.042(2) 0.088(4) 0.057(3) 0.022(2) 0.014(2) 0.047(3) C(29) 0.057(3) 0.110(5) 0.070(3) 0.024(3) 0.020(3) 0.064(3) C(30) 0.058(3) 0.111(5) 0.054(3) 0.016(3) 0.028(3) 0.040(3) C(31) 0.049(3) 0.079(3) 0.060(3) 0.025(3) 0.024(2) 0.017(3) C(32) 0.044(2) 0.047(2) 0.047(2) 0.019(2) 0.017(2) 0.015(2) C(33) 0.033(2) 0.039(2) 0.031(2) 0.013(2) 0.007(2) 0.011(2) C(34) 0.047(2) 0.045(2) 0.042(2) 0.015(2) 0.003(2) 0.016(2) C(35) 0.055(3) 0.060(3) 0.044(3) 0.020(2) -0.005(2) 0.014(2) C(36) 0.048(3) 0.054(3) 0.045(3) 0.006(2) 0.003(2) 0.004(2) C(37) 0.063(3) 0.044(2) 0.048(3) 0.003(2) 0.011(2) 0.015(2) C(38) 0.050(2) 0.045(2) 0.039(2) 0.013(2) 0.008(2) 0.017(2) C(39) 0.039(2) 0.037(2) 0.038(2) 0.013(2) 0.008(2) 0.015(2) C(40) 0.048(3) 0.054(3) 0.051(3) 0.022(2) 0.013(2) 0.014(2) C(41) 0.065(3) 0.072(4) 0.089(4) 0.042(3) 0.026(3) 0.022(3) C(42) 0.096(4) 0.056(3) 0.087(4) 0.041(3) 0.035(3) 0.019(3) C(43) 0.072(3) 0.041(3) 0.068(3) 0.013(2) 0.012(3) 0.008(2) C(44) 0.045(2) 0.047(2) 0.055(3) 0.012(2) 0.009(2) 0.018(2) C(45) 0.038(2) 0.044(2) 0.043(2) 0.005(2) -0.003(2) 0.018(2) C(46) 0.041(2) 0.066(3) 0.070(3) 0.002(2) 0.003(2) 0.033(3) C(47) 0.049(3) 0.098(5) 0.109(5) -0.018(3) -0.007(3) 0.054(4) C(48) 0.073(4) 0.091(5) 0.102(5) -0.033(3) -0.038(4) 0.049(4) C(49) 0.091(4) 0.075(4) 0.060(3) -0.014(3) -0.035(3) 0.026(3) C(50) 0.068(3) 0.062(3) 0.043(3) -0.008(2) -0.010(2) 0.022(2) C(51) 0.042(2) 0.044(2) 0.030(2) 0.012(2) 0.010(2) 0.014(2) C(52) 0.043(2) 0.052(3) 0.041(2) 0.016(2) 0.009(2) 0.016(2) C(53) 0.046(3) 0.076(3) 0.054(3) 0.020(2) 0.013(2) 0.026(3) C(54) 0.064(3) 0.086(4) 0.061(3) 0.037(3) 0.031(3) 0.024(3) C(55) 0.077(4) 0.068(3) 0.059(3) 0.031(3) 0.029(3) 0.003(3) C(56) 0.053(3) 0.053(3) 0.049(3) 0.012(2) 0.018(2) 0.004(2) C(57) 0.037(2) 0.042(2) 0.034(2) 0.006(2) -0.003(2) 0.016(2) C(58) 0.051(3) 0.054(3) 0.037(2) 0.009(2) 0.001(2) 0.022(2) C(59) 0.062(3) 0.061(3) 0.055(3) 0.005(2) -0.001(2) 0.035(3) C(60) 0.075(4) 0.055(3) 0.087(4) 0.016(3) -0.006(3) 0.043(3) C(61) 0.090(4) 0.060(3) 0.080(4) 0.039(3) 0.011(3) 0.028(3) C(62) 0.060(3) 0.058(3) 0.057(3) 0.026(2) 0.014(2) 0.027(2) C(63) 0.084(5) 0.110(6) 0.141(7) 0.053(5) 0.013(5) 0.032(5) C(64) 0.194(9) 0.152(7) 0.097(6) 0.127(7) -0.005(5) 0.023(5) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(4) 2.217(1) . . yes Pt(1) P(5) 2.221(1) . . yes Pt(1) O(1) 2.082(2) . . yes Pt(1) O(2) 2.100(2) . . yes P(1) O(1) 1.511(3) . . yes P(1) O(4) 1.457(3) . . yes P(1) O(5) 1.606(3) . . yes P(1) O(9) 1.585(3) . . yes P(2) O(2) 1.506(3) . . yes P(2) O(5) 1.607(3) . . yes P(2) O(6) 1.457(3) . . yes P(2) O(7) 1.593(3) . . yes P(3) O(3) 1.472(3) . . yes P(3) O(7) 1.640(3) . . yes P(3) O(8) 1.463(3) . . yes P(3) O(9) 1.637(3) . . yes P(4) C(1) 1.819(4) . . yes P(4) C(7) 1.811(4) . . yes P(4) C(13) 1.813(4) . . yes P(5) C(14) 1.813(4) . . yes P(5) C(20) 1.814(4) . . yes P(5) C(26) 1.815(4) . . yes P(6) N(1) 1.590(3) . . yes P(6) C(27) 1.796(4) . . yes P(6) C(33) 1.801(4) . . yes P(6) C(39) 1.802(4) . . yes P(7) N(1) 1.576(3) . . yes P(7) C(45) 1.796(4) . . yes P(7) C(51) 1.789(4) . . yes P(7) C(57) 1.798(4) . . yes N(2) C(63) 1.106(9) . . yes C(1) C(2) 1.381(5) . . yes C(1) C(6) 1.391(5) . . yes C(2) C(3) 1.384(6) . . yes C(3) C(4) 1.372(7) . . yes C(4) C(5) 1.364(7) . . yes C(5) C(6) 1.381(6) . . yes C(7) C(8) 1.398(5) . . yes C(7) C(12) 1.382(5) . . yes C(8) C(9) 1.383(5) . . yes C(9) C(10) 1.376(6) . . yes C(10) C(11) 1.372(6) . . yes C(11) C(12) 1.387(6) . . yes C(14) C(15) 1.385(6) . . yes C(14) C(19) 1.401(5) . . yes C(15) C(16) 1.386(6) . . yes C(16) C(17) 1.371(6) . . yes C(17) C(18) 1.372(7) . . yes C(18) C(19) 1.381(7) . . yes C(20) C(21) 1.383(5) . . yes C(20) C(25) 1.401(6) . . yes C(21) C(22) 1.384(6) . . yes C(22) C(23) 1.368(7) . . yes C(23) C(24) 1.366(7) . . yes C(24) C(25) 1.371(6) . . yes C(27) C(28) 1.384(6) . . yes C(27) C(32) 1.385(5) . . yes C(28) C(29) 1.380(6) . . yes C(29) C(30) 1.379(7) . . yes C(30) C(31) 1.381(7) . . yes C(31) C(32) 1.388(6) . . yes C(33) C(34) 1.381(5) . . yes C(33) C(38) 1.386(5) . . yes C(34) C(35) 1.389(6) . . yes C(35) C(36) 1.379(6) . . yes C(36) C(37) 1.378(6) . . yes C(37) C(38) 1.384(6) . . yes C(39) C(40) 1.385(5) . . yes C(39) C(44) 1.393(5) . . yes C(40) C(41) 1.389(6) . . yes C(41) C(42) 1.374(7) . . yes C(42) C(43) 1.373(7) . . yes C(43) C(44) 1.372(6) . . yes C(45) C(46) 1.375(6) . . yes C(45) C(50) 1.386(6) . . yes C(46) C(47) 1.386(7) . . yes C(47) C(48) 1.366(9) . . yes C(48) C(49) 1.345(8) . . yes C(49) C(50) 1.378(6) . . yes C(51) C(52) 1.393(5) . . yes C(51) C(56) 1.394(6) . . yes C(52) C(53) 1.382(6) . . yes C(53) C(54) 1.370(7) . . yes C(54) C(55) 1.365(7) . . yes C(55) C(56) 1.389(6) . . yes C(57) C(58) 1.399(5) . . yes C(57) C(62) 1.389(6) . . yes C(58) C(59) 1.379(6) . . yes C(59) C(60) 1.359(7) . . yes C(60) C(61) 1.390(8) . . yes C(61) C(62) 1.381(6) . . yes C(63) C(64) 1.329(9) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(4) Pt(1) P(5) 99.69(4) . . . yes P(4) Pt(1) O(1) 173.12(8) . . . yes P(4) Pt(1) O(2) 83.50(7) . . . yes P(5) Pt(1) O(1) 86.24(7) . . . yes P(5) Pt(1) O(2) 169.74(7) . . . yes O(1) Pt(1) O(2) 91.26(10) . . . yes O(1) P(1) O(4) 115.9(2) . . . yes O(1) P(1) O(5) 107.2(1) . . . yes O(1) P(1) O(9) 110.1(2) . . . yes O(4) P(1) O(5) 110.3(1) . . . yes O(4) P(1) O(9) 110.7(2) . . . yes O(5) P(1) O(9) 101.7(1) . . . yes O(2) P(2) O(5) 107.3(1) . . . yes O(2) P(2) O(6) 116.8(2) . . . yes O(2) P(2) O(7) 109.2(1) . . . yes O(5) P(2) O(6) 109.9(1) . . . yes O(5) P(2) O(7) 101.6(1) . . . yes O(6) P(2) O(7) 110.9(2) . . . yes O(3) P(3) O(7) 108.4(2) . . . yes O(3) P(3) O(8) 122.9(2) . . . yes O(3) P(3) O(9) 108.7(2) . . . yes O(7) P(3) O(8) 107.8(2) . . . yes O(7) P(3) O(9) 99.2(1) . . . yes O(8) P(3) O(9) 107.3(2) . . . yes Pt(1) P(4) C(1) 113.0(1) . . . yes Pt(1) P(4) C(7) 119.9(1) . . . yes Pt(1) P(4) C(13) 107.6(1) . . . yes C(1) P(4) C(7) 106.7(2) . . . yes C(1) P(4) C(13) 105.1(2) . . . yes C(7) P(4) C(13) 103.1(2) . . . yes Pt(1) P(5) C(14) 115.4(1) . . . yes Pt(1) P(5) C(20) 115.6(1) . . . yes Pt(1) P(5) C(26) 109.3(1) . . . yes C(14) P(5) C(20) 110.4(2) . . . yes C(14) P(5) C(26) 101.9(2) . . . yes C(20) P(5) C(26) 102.4(2) . . . yes N(1) P(6) C(27) 107.5(2) . . . yes N(1) P(6) C(33) 110.1(2) . . . yes N(1) P(6) C(39) 114.9(2) . . . yes C(27) P(6) C(33) 109.9(2) . . . yes C(27) P(6) C(39) 106.2(2) . . . yes C(33) P(6) C(39) 108.1(2) . . . yes N(1) P(7) C(45) 110.6(2) . . . yes N(1) P(7) C(51) 114.2(2) . . . yes N(1) P(7) C(57) 109.1(2) . . . yes C(45) P(7) C(51) 108.3(2) . . . yes C(45) P(7) C(57) 107.1(2) . . . yes C(51) P(7) C(57) 107.3(2) . . . yes Pt(1) O(1) P(1) 127.8(2) . . . yes Pt(1) O(2) P(2) 130.3(1) . . . yes P(1) O(5) P(2) 123.4(1) . . . yes P(2) O(7) P(3) 126.1(2) . . . yes P(1) O(9) P(3) 129.7(2) . . . yes P(6) N(1) P(7) 135.7(2) . . . yes P(4) C(1) C(2) 121.7(3) . . . yes P(4) C(1) C(6) 119.4(3) . . . yes C(2) C(1) C(6) 118.9(4) . . . yes C(1) C(2) C(3) 120.3(4) . . . yes C(2) C(3) C(4) 120.4(4) . . . yes C(3) C(4) C(5) 119.7(4) . . . yes C(4) C(5) C(6) 120.8(4) . . . yes C(1) C(6) C(5) 119.9(4) . . . yes P(4) C(7) C(8) 117.6(3) . . . yes P(4) C(7) C(12) 123.5(3) . . . yes C(8) C(7) C(12) 118.9(3) . . . yes C(7) C(8) C(9) 120.2(4) . . . yes C(8) C(9) C(10) 120.4(4) . . . yes C(9) C(10) C(11) 119.8(4) . . . yes C(10) C(11) C(12) 120.6(4) . . . yes C(7) C(12) C(11) 120.2(4) . . . yes P(5) C(14) C(15) 119.3(3) . . . yes P(5) C(14) C(19) 121.3(3) . . . yes C(15) C(14) C(19) 118.9(4) . . . yes C(14) C(15) C(16) 120.0(4) . . . yes C(15) C(16) C(17) 120.1(4) . . . yes C(16) C(17) C(18) 121.1(4) . . . yes C(17) C(18) C(19) 119.4(4) . . . yes C(14) C(19) C(18) 120.5(4) . . . yes P(5) C(20) C(21) 125.5(3) . . . yes P(5) C(20) C(25) 116.3(3) . . . yes C(21) C(20) C(25) 118.2(4) . . . yes C(20) C(21) C(22) 119.8(4) . . . yes C(21) C(22) C(23) 121.2(4) . . . yes C(22) C(23) C(24) 119.7(4) . . . yes C(23) C(24) C(25) 120.1(4) . . . yes C(20) C(25) C(24) 121.1(4) . . . yes P(6) C(27) C(28) 120.6(3) . . . yes P(6) C(27) C(32) 120.3(3) . . . yes C(28) C(27) C(32) 119.1(4) . . . yes C(27) C(28) C(29) 120.7(4) . . . yes C(28) C(29) C(30) 119.5(4) . . . yes C(29) C(30) C(31) 120.9(4) . . . yes C(30) C(31) C(32) 118.9(4) . . . yes C(27) C(32) C(31) 120.8(4) . . . yes P(6) C(33) C(34) 120.4(3) . . . yes P(6) C(33) C(38) 120.1(3) . . . yes C(34) C(33) C(38) 119.5(3) . . . yes C(33) C(34) C(35) 120.5(4) . . . yes C(34) C(35) C(36) 119.8(4) . . . yes C(35) C(36) C(37) 119.7(4) . . . yes C(36) C(37) C(38) 120.7(4) . . . yes C(33) C(38) C(37) 119.8(4) . . . yes P(6) C(39) C(40) 123.4(3) . . . yes P(6) C(39) C(44) 117.7(3) . . . yes C(40) C(39) C(44) 118.8(4) . . . yes C(39) C(40) C(41) 119.8(4) . . . yes C(40) C(41) C(42) 120.4(5) . . . yes C(41) C(42) C(43) 120.1(5) . . . yes C(42) C(43) C(44) 119.9(4) . . . yes C(39) C(44) C(43) 120.9(4) . . . yes P(7) C(45) C(46) 120.1(3) . . . yes P(7) C(45) C(50) 120.2(3) . . . yes C(46) C(45) C(50) 119.7(4) . . . yes C(45) C(46) C(47) 119.2(5) . . . yes C(46) C(47) C(48) 120.6(5) . . . yes C(47) C(48) C(49) 120.1(5) . . . yes C(48) C(49) C(50) 120.9(5) . . . yes C(45) C(50) C(49) 119.5(5) . . . yes P(7) C(51) C(52) 118.9(3) . . . yes P(7) C(51) C(56) 121.8(3) . . . yes C(52) C(51) C(56) 119.0(4) . . . yes C(51) C(52) C(53) 120.6(4) . . . yes C(52) C(53) C(54) 119.5(4) . . . yes C(53) C(54) C(55) 121.1(4) . . . yes C(54) C(55) C(56) 120.2(5) . . . yes C(51) C(56) C(55) 119.7(4) . . . yes P(7) C(57) C(58) 121.7(3) . . . yes P(7) C(57) C(62) 119.7(3) . . . yes C(58) C(57) C(62) 118.5(4) . . . yes C(57) C(58) C(59) 120.5(4) . . . yes C(58) C(59) C(60) 120.3(5) . . . yes C(59) C(60) C(61) 120.4(5) . . . yes C(60) C(61) C(62) 119.7(5) . . . yes C(57) C(62) C(61) 120.6(4) . . . yes N(2) C(63) C(64) 173(1) . . . yes #------------------------------------------------------------------------------ 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 Pt(1) P(4) C(1) C(2) 162.0(3) . . . . yes Pt(1) P(4) C(1) C(6) -16.8(4) . . . . yes Pt(1) P(4) C(7) C(8) -53.9(3) . . . . yes Pt(1) P(4) C(7) C(12) 127.9(3) . . . . yes Pt(1) P(5) C(14) C(15) 7.3(4) . . . . yes Pt(1) P(5) C(14) C(19) -179.9(3) . . . . yes Pt(1) P(5) C(20) C(21) 123.9(3) . . . . yes Pt(1) P(5) C(20) C(25) -55.9(3) . . . . yes Pt(1) O(1) P(1) O(4) 167.9(2) . . . . yes Pt(1) O(1) P(1) O(5) 44.3(2) . . . . yes Pt(1) O(1) P(1) O(9) -65.5(2) . . . . yes Pt(1) O(2) P(2) O(5) -35.6(2) . . . . yes Pt(1) O(2) P(2) O(6) -159.5(2) . . . . yes Pt(1) O(2) P(2) O(7) 73.8(2) . . . . yes P(1) O(1) Pt(1) P(4) 16.2(8) . . . . yes P(1) O(1) Pt(1) P(5) 166.0(2) . . . . yes P(1) O(1) Pt(1) O(2) -24.0(2) . . . . yes P(1) O(5) P(2) O(2) 60.2(2) . . . . yes P(1) O(5) P(2) O(6) -171.8(2) . . . . yes P(1) O(5) P(2) O(7) -54.3(2) . . . . yes P(1) O(9) P(3) O(3) -70.3(3) . . . . yes P(1) O(9) P(3) O(7) 42.8(3) . . . . yes P(1) O(9) P(3) O(8) 154.9(2) . . . . yes P(2) O(2) Pt(1) P(4) -156.0(2) . . . . yes P(2) O(2) Pt(1) P(5) 95.2(4) . . . . yes P(2) O(2) Pt(1) O(1) 19.5(2) . . . . yes P(2) O(5) P(1) O(1) -65.1(2) . . . . yes P(2) O(5) P(1) O(4) 167.9(2) . . . . yes P(2) O(5) P(1) O(9) 50.4(2) . . . . yes P(2) O(7) P(3) O(3) 67.1(2) . . . . yes P(2) O(7) P(3) O(8) -157.8(2) . . . . yes P(2) O(7) P(3) O(9) -46.2(2) . . . . yes P(3) O(7) P(2) O(2) -60.1(2) . . . . yes P(3) O(7) P(2) O(5) 53.0(2) . . . . yes P(3) O(7) P(2) O(6) 169.8(2) . . . . yes P(3) O(9) P(1) O(1) 67.7(3) . . . . yes P(3) O(9) P(1) O(4) -162.8(2) . . . . yes P(3) O(9) P(1) O(5) -45.7(3) . . . . yes P(4) Pt(1) P(5) C(14) 92.9(1) . . . . yes P(4) Pt(1) P(5) C(20) -38.1(1) . . . . yes P(4) Pt(1) P(5) C(26) -153.1(2) . . . . yes P(4) C(1) C(2) C(3) -180.0 . . . . yes P(4) C(1) C(6) C(5) -179.9(3) . . . . yes P(4) C(7) C(8) C(9) -178.2(3) . . . . yes P(4) C(7) C(12) C(11) 177.5(4) . . . . yes P(5) Pt(1) P(4) C(1) 108.3(1) . . . . yes P(5) Pt(1) P(4) C(7) -18.9(1) . . . . yes P(5) Pt(1) P(4) C(13) -136.1(2) . . . . yes P(5) C(14) C(15) C(16) 173.1(3) . . . . yes P(5) C(14) C(19) C(18) -174.1(3) . . . . yes P(5) C(20) C(21) C(22) -179.6(4) . . . . yes P(5) C(20) C(25) C(24) 179.4(4) . . . . yes P(6) N(1) P(7) C(45) 105.6(3) . . . . yes P(6) N(1) P(7) C(51) -16.9(4) . . . . yes P(6) N(1) P(7) C(57) -136.9(3) . . . . yes P(6) C(27) C(28) C(29) -179.5(4) . . . . yes P(6) C(27) C(32) C(31) 179.4(3) . . . . yes P(6) C(33) C(34) C(35) 175.1(3) . . . . yes P(6) C(33) C(38) C(37) -176.1(3) . . . . yes P(6) C(39) C(40) C(41) -176.6(4) . . . . yes P(6) C(39) C(44) C(43) 176.6(4) . . . . yes P(7) N(1) P(6) C(27) -141.1(3) . . . . yes P(7) N(1) P(6) C(33) 99.2(3) . . . . yes P(7) N(1) P(6) C(39) -23.1(4) . . . . yes P(7) C(45) C(46) C(47) -178.6(5) . . . . yes P(7) C(45) C(50) C(49) 178.3(5) . . . . yes P(7) C(51) C(52) C(53) 174.4(3) . . . . yes P(7) C(51) C(56) C(55) -173.4(4) . . . . yes P(7) C(57) C(58) C(59) 178.1(3) . . . . yes P(7) C(57) C(62) C(61) -178.0(4) . . . . yes O(1) Pt(1) P(4) C(1) -102.4(7) . . . . yes O(1) Pt(1) P(4) C(7) 130.4(7) . . . . yes O(1) Pt(1) P(4) C(13) 13.2(7) . . . . yes O(1) Pt(1) P(5) C(14) -83.6(2) . . . . yes O(1) Pt(1) P(5) C(20) 145.4(2) . . . . yes O(1) Pt(1) P(5) C(26) 30.5(2) . . . . yes O(2) Pt(1) P(4) C(1) -61.8(1) . . . . yes O(2) Pt(1) P(4) C(7) 171.0(2) . . . . yes O(2) Pt(1) P(4) C(13) 53.7(2) . . . . yes O(2) Pt(1) P(5) C(14) -159.8(4) . . . . yes O(2) Pt(1) P(5) C(20) 69.2(4) . . . . yes O(2) Pt(1) P(5) C(26) -45.7(5) . . . . yes N(1) P(6) C(27) C(28) 162.4(4) . . . . yes N(1) P(6) C(27) C(32) -16.9(4) . . . . yes N(1) P(6) C(33) C(34) 178.2(3) . . . . yes N(1) P(6) C(33) C(38) -4.2(4) . . . . yes N(1) P(6) C(39) C(40) 114.7(4) . . . . yes N(1) P(6) C(39) C(44) -61.7(4) . . . . yes N(1) P(7) C(45) C(46) -2.1(5) . . . . yes N(1) P(7) C(45) C(50) 178.5(4) . . . . yes N(1) P(7) C(51) C(52) -69.4(4) . . . . yes N(1) P(7) C(51) C(56) 103.5(4) . . . . yes N(1) P(7) C(57) C(58) 154.8(3) . . . . yes N(1) P(7) C(57) C(62) -29.0(4) . . . . yes C(1) P(4) C(7) C(8) 176.1(3) . . . . yes C(1) P(4) C(7) C(12) -2.1(4) . . . . yes C(1) C(2) C(3) C(4) 0.4(7) . . . . yes C(1) C(6) C(5) C(4) -0.5(7) . . . . yes C(2) C(1) P(4) C(7) -64.1(4) . . . . yes C(2) C(1) P(4) C(13) 45.0(4) . . . . yes C(2) C(1) C(6) C(5) 1.3(6) . . . . yes C(2) C(3) C(4) C(5) 0.4(8) . . . . yes C(3) C(2) C(1) C(6) -1.2(6) . . . . yes C(3) C(4) C(5) C(6) -0.3(8) . . . . yes C(6) C(1) P(4) C(7) 117.1(3) . . . . yes C(6) C(1) P(4) C(13) -133.8(3) . . . . yes C(7) C(8) C(9) C(10) 0.9(6) . . . . yes C(7) C(12) C(11) C(10) 0.4(8) . . . . yes C(8) C(7) P(4) C(13) 65.6(3) . . . . yes C(8) C(7) C(12) C(11) -0.8(7) . . . . yes C(8) C(9) C(10) C(11) -1.3(7) . . . . yes C(9) C(8) C(7) C(12) 0.1(6) . . . . yes C(9) C(10) C(11) C(12) 0.6(8) . . . . yes C(12) C(7) P(4) C(13) -112.6(4) . . . . yes C(14) P(5) C(20) C(21) -9.4(4) . . . . yes C(14) P(5) C(20) C(25) 170.8(3) . . . . yes C(14) C(15) C(16) C(17) 0.8(6) . . . . yes C(14) C(19) C(18) C(17) 1.5(7) . . . . yes C(15) C(14) P(5) C(20) 140.7(3) . . . . yes C(15) C(14) P(5) C(26) -111.0(3) . . . . yes C(15) C(14) C(19) C(18) -1.3(6) . . . . yes C(15) C(16) C(17) C(18) -0.5(7) . . . . yes C(16) C(15) C(14) C(19) 0.1(6) . . . . yes C(16) C(17) C(18) C(19) -0.6(7) . . . . yes C(19) C(14) P(5) C(20) -46.5(4) . . . . yes C(19) C(14) P(5) C(26) 61.8(4) . . . . yes C(20) C(21) C(22) C(23) 0.0(8) . . . . yes C(20) C(25) C(24) C(23) 0.6(8) . . . . yes C(21) C(20) P(5) C(26) -117.3(4) . . . . yes C(21) C(20) C(25) C(24) -0.5(7) . . . . yes C(21) C(22) C(23) C(24) 0.0(9) . . . . yes C(22) C(21) C(20) C(25) 0.2(7) . . . . yes C(22) C(23) C(24) C(25) -0.3(9) . . . . yes C(25) C(20) P(5) C(26) 62.9(4) . . . . yes C(27) P(6) C(33) C(34) 60.0(4) . . . . yes C(27) P(6) C(33) C(38) -122.5(3) . . . . yes C(27) P(6) C(39) C(40) -126.6(4) . . . . yes C(27) P(6) C(39) C(44) 57.0(4) . . . . yes C(27) C(28) C(29) C(30) -0.6(8) . . . . yes C(27) C(32) C(31) C(30) 0.8(7) . . . . yes C(28) C(27) P(6) C(33) -77.8(4) . . . . yes C(28) C(27) P(6) C(39) 38.9(4) . . . . yes C(28) C(27) C(32) C(31) 0.1(6) . . . . yes C(28) C(29) C(30) C(31) 1.5(9) . . . . yes C(29) C(28) C(27) C(32) -0.2(7) . . . . yes C(29) C(30) C(31) C(32) -1.6(8) . . . . yes C(32) C(27) P(6) C(33) 102.9(3) . . . . yes C(32) C(27) P(6) C(39) -140.4(3) . . . . yes C(33) P(6) C(39) C(40) -8.7(4) . . . . yes C(33) P(6) C(39) C(44) 174.9(3) . . . . yes C(33) C(34) C(35) C(36) 1.7(7) . . . . yes C(33) C(38) C(37) C(36) 0.3(7) . . . . yes C(34) C(33) P(6) C(39) -55.5(4) . . . . yes C(34) C(33) C(38) C(37) 1.5(6) . . . . yes C(34) C(35) C(36) C(37) 0.1(7) . . . . yes C(35) C(34) C(33) C(38) -2.5(6) . . . . yes C(35) C(36) C(37) C(38) -1.0(7) . . . . yes C(38) C(33) P(6) C(39) 122.0(3) . . . . yes C(39) C(40) C(41) C(42) 0.8(8) . . . . yes C(39) C(44) C(43) C(42) -0.3(8) . . . . yes C(40) C(39) C(44) C(43) 0.0(7) . . . . yes C(40) C(41) C(42) C(43) -1.1(9) . . . . yes C(41) C(40) C(39) C(44) -0.3(7) . . . . yes C(41) C(42) C(43) C(44) 0.9(9) . . . . yes C(45) P(7) C(51) C(52) 166.9(3) . . . . yes C(45) P(7) C(51) C(56) -20.1(4) . . . . yes C(45) P(7) C(57) C(58) -85.5(4) . . . . yes C(45) P(7) C(57) C(62) 90.7(4) . . . . yes C(45) C(46) C(47) C(48) 0(1) . . . . yes C(45) C(50) C(49) C(48) 0(1) . . . . yes C(46) C(45) P(7) C(51) 123.8(4) . . . . yes C(46) C(45) P(7) C(57) -120.8(4) . . . . yes C(46) C(45) C(50) C(49) -1.2(8) . . . . yes C(46) C(47) C(48) C(49) 0(1) . . . . yes C(47) C(46) C(45) C(50) 0.8(8) . . . . yes C(47) C(48) C(49) C(50) 0(1) . . . . yes C(50) C(45) P(7) C(51) -55.7(4) . . . . yes C(50) C(45) P(7) C(57) 59.7(4) . . . . yes C(51) P(7) C(57) C(58) 30.5(4) . . . . yes C(51) P(7) C(57) C(62) -153.2(3) . . . . yes C(51) C(52) C(53) C(54) -0.8(7) . . . . yes C(51) C(56) C(55) C(54) -0.9(8) . . . . yes C(52) C(51) P(7) C(57) 51.6(4) . . . . yes C(52) C(51) C(56) C(55) -0.4(7) . . . . yes C(52) C(53) C(54) C(55) -0.6(8) . . . . yes C(53) C(52) C(51) C(56) 1.2(6) . . . . yes C(53) C(54) C(55) C(56) 1.4(8) . . . . yes C(56) C(51) P(7) C(57) -135.4(4) . . . . yes C(57) C(58) C(59) C(60) -1.7(7) . . . . yes C(57) C(62) C(61) C(60) 1.5(8) . . . . yes C(58) C(57) C(62) C(61) -1.7(7) . . . . yes C(58) C(59) C(60) C(61) 1.5(8) . . . . yes C(59) C(58) C(57) C(62) 1.8(6) . . . . yes C(59) C(60) C(61) C(62) -1.3(8) . . . . yes C(59) C(60) C(61) C(62) -1.3(8) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(5) 3.448(5) . 2_556 ? O(3) C(9) 3.164(5) . 2_666 ? O(3) C(10) 3.257(5) . 2_666 ? O(4) C(28) 3.132(5) . 1_455 ? O(4) C(34) 3.374(5) . 1_455 ? O(4) C(18) 3.418(5) . 2_566 ? O(4) C(48) 3.544(7) . 2_555 ? O(5) C(48) 3.336(6) . 2_555 ? O(5) C(5) 3.519(5) . 2_556 ? O(6) C(55) 3.089(5) . 2_655 ? O(6) C(64) 3.146(8) . 2_656 ? O(6) C(54) 3.173(6) . 2_655 ? O(6) C(24) 3.350(6) . 2_556 ? O(8) C(59) 3.299(5) . 2_665 ? O(8) C(60) 3.332(6) . 2_665 ? O(8) C(31) 3.410(6) . . ? O(9) C(34) 3.181(5) . 1_455 ? O(9) C(35) 3.287(5) . 1_455 ? N(2) C(12) 3.564(9) . . ? C(8) C(16) 3.587(6) . 2_666 ? C(9) C(16) 3.522(6) . 2_666 ? C(9) C(15) 3.571(6) . 2_666 ? C(17) C(26) 3.531(6) . 2_566 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_(PPh4)[Pt(P3O9)(dppe)](5) _database_code_CSD 202877 _audit_creation_date 'Thu Apr 3 12:10:39 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C52.50 H48 Cl N O9 P6 Pt ' _chemical_formula_moiety ? _chemical_formula_weight 1253.34 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.939(1) _cell_length_b 15.728(2) _cell_length_c 17.660(2) _cell_angle_alpha 103.29(1) _cell_angle_beta 95.04(1) _cell_angle_gamma 93.56(1) _cell_volume 2666.5(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.9 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.906 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 12667 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 1.0001 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.0001 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.66 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; for calculating R-factor (gt). ; _reflns_number_total 12226 _reflns_number_gt 9598 _reflns_threshold_criterion F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0322 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9598 _refine_ls_number_parameters 638 _refine_ls_goodness_of_fit_ref 1.562 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_shift/su_max 0.0344 _refine_diff_density_max 0.78 _refine_diff_density_min -0.71 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0007(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt -0.18460(2) -0.22045(1) -0.255033(9) 0.03138(4) Uani 1.00 d . . . Cl(1) Cl -0.5000 0.0000 -0.5000 0.316(4) Uani 1.00 d S . . Cl(2) Cl -0.3725(6) 0.0047(4) -0.3385(5) 0.234(3) Uani 0.50 d P . . P(1) P -0.50801(10) -0.25056(8) -0.31474(6) 0.0421(3) Uani 1.00 d . . . P(2) P -0.4354(1) -0.18617(8) -0.15265(6) 0.0397(3) Uani 1.00 d . . . P(3) P -0.5117(1) -0.37482(9) -0.21420(8) 0.0553(4) Uani 1.00 d . . . P(4) P 0.00888(9) -0.20182(7) -0.17816(6) 0.0330(3) Uani 1.00 d . . . P(5) P -0.06910(9) -0.28433(7) -0.35055(6) 0.0313(3) Uani 1.00 d . . . P(6) P -0.2859(1) -0.29004(8) -0.74761(7) 0.0468(4) Uani 1.00 d . . . O(1) O -0.3630(2) -0.2373(2) -0.3311(1) 0.0408(8) Uani 1.00 d . . . O(2) O -0.2906(3) -0.1607(2) -0.1628(2) 0.0484(9) Uani 1.00 d . . . O(3) O -0.4117(6) -0.4353(3) -0.2216(3) 0.130(2) Uani 1.00 d . . . O(4) O -0.6118(3) -0.2404(3) -0.3747(2) 0.064(1) Uani 1.00 d . . . O(5) O -0.5255(2) -0.1846(2) -0.2324(2) 0.0425(8) Uani 1.00 d . . . O(6) O -0.4919(3) -0.1343(2) -0.0856(2) 0.061(1) Uani 1.00 d . . . O(7) O -0.4443(4) -0.2866(2) -0.1545(2) 0.078(1) Uani 1.00 d . . . O(8) O -0.6440(4) -0.3929(4) -0.1914(3) 0.121(2) Uani 1.00 d . . . O(9) O -0.5325(4) -0.3429(2) -0.2954(2) 0.064(1) Uani 1.00 d . . . N(1) N -0.708(1) -0.1648(7) -0.8213(6) 0.175(5) Uani 1.00 d . . . C(1) C 0.0046(4) -0.2654(3) -0.1048(2) 0.039(1) Uani 1.00 d . . . C(2) C -0.1120(5) -0.3149(3) -0.0993(3) 0.057(2) Uani 1.00 d . . . C(3) C -0.1171(6) -0.3618(4) -0.0419(4) 0.081(2) Uani 1.00 d . . . C(4) C -0.0077(8) -0.3597(5) 0.0101(4) 0.087(2) Uani 1.00 d . . . C(5) C 0.1095(7) -0.3109(5) 0.0055(3) 0.084(2) Uani 1.00 d . . . C(6) C 0.1171(5) -0.2641(4) -0.0517(3) 0.063(2) Uani 1.00 d . . . C(7) C 0.0638(4) -0.0895(3) -0.1278(2) 0.037(1) Uani 1.00 d . . . C(8) C -0.0295(4) -0.0277(3) -0.1136(3) 0.046(1) Uani 1.00 d . . . C(9) C 0.0136(5) 0.0583(3) -0.0739(3) 0.057(2) Uani 1.00 d . . . C(10) C 0.1464(6) 0.0816(3) -0.0468(3) 0.064(2) Uani 1.00 d . . . C(11) C 0.2375(5) 0.0210(4) -0.0604(3) 0.069(2) Uani 1.00 d . . . C(12) C 0.1993(4) -0.0651(3) -0.1012(3) 0.056(1) Uani 1.00 d . . . C(13) C 0.1463(4) -0.2389(3) -0.2369(2) 0.039(1) Uani 1.00 d . . . C(14) C 0.0889(4) -0.3130(3) -0.3069(2) 0.036(1) Uani 1.00 d . . . C(15) C -0.1555(4) -0.3827(3) -0.4145(2) 0.038(1) Uani 1.00 d . . . C(16) C -0.1215(5) -0.4124(3) -0.4899(3) 0.051(1) Uani 1.00 d . . . C(17) C -0.1905(6) -0.4867(4) -0.5381(3) 0.069(2) Uani 1.00 d . . . C(18) C -0.2907(6) -0.5315(4) -0.5116(4) 0.080(2) Uani 1.00 d . . . C(19) C -0.3245(5) -0.5038(3) -0.4365(4) 0.074(2) Uani 1.00 d . . . C(20) C -0.2564(5) -0.4287(3) -0.3876(3) 0.051(1) Uani 1.00 d . . . C(21) C -0.0301(4) -0.2144(3) -0.4157(2) 0.034(1) Uani 1.00 d . . . C(22) C -0.1354(5) -0.1742(3) -0.4450(3) 0.053(1) Uani 1.00 d . . . C(23) C -0.1137(5) -0.1247(4) -0.4991(3) 0.066(2) Uani 1.00 d . . . C(24) C 0.0112(6) -0.1143(3) -0.5228(3) 0.062(2) Uani 1.00 d . . . C(25) C 0.1162(5) -0.1526(3) -0.4929(3) 0.057(2) Uani 1.00 d . . . C(26) C 0.0977(4) -0.2027(3) -0.4396(3) 0.046(1) Uani 1.00 d . . . C(27) C -0.1563(5) -0.3630(3) -0.7430(3) 0.051(1) Uani 1.00 d . . . C(28) C -0.0494(6) -0.3413(4) -0.6838(3) 0.068(2) Uani 1.00 d . . . C(29) C 0.0553(6) -0.3946(5) -0.6833(4) 0.085(2) Uani 1.00 d . . . C(30) C 0.0562(6) -0.4682(4) -0.7440(4) 0.087(2) Uani 1.00 d . . . C(31) C -0.0531(7) -0.4914(4) -0.8028(4) 0.086(2) Uani 1.00 d . . . C(32) C -0.1591(6) -0.4396(3) -0.8017(3) 0.064(2) Uani 1.00 d . . . C(33) C -0.3836(5) -0.3187(3) -0.8408(3) 0.049(1) Uani 1.00 d . . . C(34) C -0.4767(6) -0.3906(3) -0.8586(3) 0.064(2) Uani 1.00 d . . . C(35) C -0.5524(6) -0.4118(4) -0.9323(4) 0.078(2) Uani 1.00 d . . . C(36) C -0.5335(7) -0.3617(5) -0.9851(3) 0.081(2) Uani 1.00 d . . . C(37) C -0.4426(7) -0.2905(5) -0.9667(3) 0.085(2) Uani 1.00 d . . . C(38) C -0.3662(6) -0.2683(4) -0.8944(3) 0.064(2) Uani 1.00 d . . . C(39) C -0.3995(5) -0.2901(3) -0.6744(2) 0.048(1) Uani 1.00 d . . . C(40) C -0.5283(6) -0.2619(4) -0.6861(3) 0.064(2) Uani 1.00 d . . . C(41) C -0.6123(6) -0.2524(4) -0.6276(3) 0.072(2) Uani 1.00 d . . . C(42) C -0.5687(6) -0.2720(4) -0.5566(3) 0.066(2) Uani 1.00 d . . . C(43) C -0.4447(6) -0.3015(4) -0.5463(3) 0.065(2) Uani 1.00 d . . . C(44) C -0.3588(5) -0.3111(3) -0.6043(3) 0.056(2) Uani 1.00 d . . . C(45) C -0.2046(5) -0.1812(3) -0.7314(3) 0.054(1) Uani 1.00 d . . . C(46) C -0.2709(7) -0.1105(4) -0.6998(3) 0.079(2) Uani 1.00 d . . . C(47) C -0.2066(9) -0.0257(4) -0.6892(4) 0.102(3) Uani 1.00 d . . . C(48) C -0.0776(10) -0.0152(5) -0.7088(4) 0.100(3) Uani 1.00 d . . . C(49) C -0.0104(7) -0.0853(5) -0.7396(4) 0.091(2) Uani 1.00 d . . . C(50) C -0.0738(6) -0.1693(4) -0.7519(3) 0.073(2) Uani 1.00 d . . . C(51) C -0.657(1) -0.1283(7) -0.8562(6) 0.108(4) Uani 1.00 d . . . C(52) C -0.595(1) -0.0727(8) -0.892(1) 0.234(7) Uani 1.00 d . . . C(53) C -0.4659 -0.0551 -0.4216 0.3166 Uiso 0.50 d P . . H(1) H -0.1895 -0.3168 -0.1353 0.0680 Uiso 1.00 calc . . . H(2) H -0.1980 -0.3958 -0.0391 0.0969 Uiso 1.00 calc . . . H(3) H -0.0119 -0.3915 0.0496 0.1042 Uiso 1.00 calc . . . H(4) H 0.1864 -0.3094 0.0418 0.1013 Uiso 1.00 calc . . . H(5) H 0.1990 -0.2309 -0.0547 0.0761 Uiso 1.00 calc . . . H(6) H -0.1228 -0.0438 -0.1307 0.0546 Uiso 1.00 calc . . . H(7) H -0.0504 0.1010 -0.0658 0.0682 Uiso 1.00 calc . . . H(8) H 0.1748 0.1400 -0.0186 0.0761 Uiso 1.00 calc . . . H(9) H 0.3300 0.0376 -0.0415 0.0825 Uiso 1.00 calc . . . H(10) H 0.2650 -0.1064 -0.1109 0.0677 Uiso 1.00 calc . . . H(11) H 0.2137 -0.2597 -0.2059 0.0467 Uiso 1.00 calc . . . H(12) H 0.1849 -0.1915 -0.2550 0.0467 Uiso 1.00 calc . . . H(13) H 0.1524 -0.3218 -0.3445 0.0434 Uiso 1.00 calc . . . H(14) H 0.0727 -0.3654 -0.2897 0.0434 Uiso 1.00 calc . . . H(15) H -0.0508 -0.3817 -0.5084 0.0612 Uiso 1.00 calc . . . H(16) H -0.1680 -0.5068 -0.5900 0.0823 Uiso 1.00 calc . . . H(17) H -0.3375 -0.5825 -0.5455 0.0952 Uiso 1.00 calc . . . H(18) H -0.3938 -0.5356 -0.4183 0.0885 Uiso 1.00 calc . . . H(19) H -0.2791 -0.4090 -0.3357 0.0613 Uiso 1.00 calc . . . H(20) H -0.2227 -0.1804 -0.4281 0.0631 Uiso 1.00 calc . . . H(21) H -0.1869 -0.0980 -0.5198 0.0795 Uiso 1.00 calc . . . H(22) H 0.0254 -0.0804 -0.5600 0.0736 Uiso 1.00 calc . . . H(23) H 0.2037 -0.1445 -0.5091 0.0687 Uiso 1.00 calc . . . H(24) H 0.1718 -0.2292 -0.4194 0.0547 Uiso 1.00 calc . . . H(25) H -0.0488 -0.2897 -0.6435 0.0817 Uiso 1.00 calc . . . H(26) H 0.1265 -0.3809 -0.6419 0.1007 Uiso 1.00 calc . . . H(27) H 0.1307 -0.5031 -0.7456 0.1044 Uiso 1.00 calc . . . H(28) H -0.0534 -0.5429 -0.8431 0.1032 Uiso 1.00 calc . . . H(29) H -0.2340 -0.4558 -0.8407 0.0769 Uiso 1.00 calc . . . H(30) H -0.4896 -0.4253 -0.8219 0.0763 Uiso 1.00 calc . . . H(31) H -0.6177 -0.4610 -0.9455 0.0931 Uiso 1.00 calc . . . H(32) H -0.5846 -0.3768 -1.0349 0.0973 Uiso 1.00 calc . . . H(33) H -0.4313 -0.2556 -1.0032 0.1021 Uiso 1.00 calc . . . H(34) H -0.3019 -0.2186 -0.8817 0.0766 Uiso 1.00 calc . . . H(35) H -0.5575 -0.2491 -0.7346 0.0770 Uiso 1.00 calc . . . H(36) H -0.6994 -0.2325 -0.6353 0.0864 Uiso 1.00 calc . . . H(37) H -0.6259 -0.2648 -0.5158 0.0789 Uiso 1.00 calc . . . H(38) H -0.4164 -0.3158 -0.4982 0.0779 Uiso 1.00 calc . . . H(39) H -0.2724 -0.3320 -0.5964 0.0674 Uiso 1.00 calc . . . H(40) H -0.3598 -0.1185 -0.6851 0.0943 Uiso 1.00 calc . . . H(41) H -0.2532 0.0240 -0.6689 0.1214 Uiso 1.00 calc . . . H(42) H -0.0341 0.0423 -0.7006 0.1202 Uiso 1.00 calc . . . H(43) H 0.0793 -0.0772 -0.7527 0.1086 Uiso 1.00 calc . . . H(44) H -0.0280 -0.2186 -0.7742 0.0871 Uiso 1.00 calc . . . H(45) H -0.5656 -0.1054 -0.9397 0.2838 Uiso 1.00 calc . . . H(46) H -0.5200 -0.0408 -0.8596 0.2838 Uiso 1.00 calc . . . H(47) H -0.6579 -0.0334 -0.9051 0.2838 Uiso 1.00 calc . . . H(48) H -0.4188 -0.1048 -0.4416 0.3799 Uiso 0.50 calc P . . H(49) H -0.5507 -0.0738 -0.4073 0.3799 Uiso 0.50 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.02037(7) 0.04240(10) 0.02941(8) 0.00323(5) 0.00240(5) 0.00446(6) Cl(1) 0.359(9) 0.214(6) 0.361(9) 0.028(6) -0.001(8) 0.053(6) Cl(2) 0.177(6) 0.106(4) 0.37(1) 0.037(4) -0.079(6) -0.014(5) P(1) 0.0243(5) 0.0677(8) 0.0329(6) -0.0007(5) -0.0005(4) 0.0117(5) P(2) 0.0279(5) 0.0576(7) 0.0321(5) 0.0046(5) 0.0055(4) 0.0067(5) P(3) 0.0528(7) 0.0568(8) 0.0573(8) -0.0073(6) 0.0075(6) 0.0184(7) P(4) 0.0227(5) 0.0426(6) 0.0307(5) 0.0034(4) 0.0011(4) 0.0029(5) P(5) 0.0256(5) 0.0358(6) 0.0307(5) 0.0027(4) 0.0022(4) 0.0045(4) P(6) 0.0613(8) 0.0433(7) 0.0388(6) 0.0050(6) 0.0084(6) 0.0145(5) O(1) 0.023(1) 0.065(2) 0.032(1) 0.002(1) 0.001(1) 0.009(1) O(2) 0.026(1) 0.074(2) 0.037(2) 0.006(1) 0.005(1) -0.005(2) O(3) 0.170(5) 0.133(4) 0.094(4) 0.091(4) 0.012(3) 0.021(3) O(4) 0.028(2) 0.123(3) 0.041(2) 0.006(2) -0.006(1) 0.023(2) O(5) 0.026(1) 0.064(2) 0.038(2) 0.010(1) 0.003(1) 0.012(1) O(6) 0.038(2) 0.098(3) 0.041(2) 0.011(2) 0.013(1) -0.002(2) O(7) 0.124(3) 0.062(2) 0.044(2) -0.017(2) -0.018(2) 0.020(2) O(8) 0.073(3) 0.200(5) 0.094(3) -0.064(3) 0.003(2) 0.064(3) O(9) 0.088(3) 0.057(2) 0.041(2) -0.021(2) 0.000(2) 0.009(2) N(1) 0.160(9) 0.20(1) 0.176(10) 0.056(8) 0.000(7) 0.063(8) C(1) 0.038(2) 0.042(2) 0.039(2) 0.009(2) 0.006(2) 0.007(2) C(2) 0.046(3) 0.060(3) 0.072(3) 0.010(2) 0.010(2) 0.030(3) C(3) 0.066(4) 0.087(5) 0.114(5) 0.023(3) 0.034(4) 0.060(4) C(4) 0.107(5) 0.103(5) 0.077(4) 0.041(4) 0.035(4) 0.057(4) C(5) 0.093(5) 0.103(5) 0.063(4) 0.020(4) -0.015(3) 0.038(4) C(6) 0.059(3) 0.073(4) 0.056(3) 0.001(3) -0.013(2) 0.020(3) C(7) 0.034(2) 0.043(2) 0.032(2) -0.002(2) 0.002(2) 0.005(2) C(8) 0.041(2) 0.049(3) 0.046(3) 0.004(2) 0.005(2) 0.007(2) C(9) 0.072(3) 0.048(3) 0.051(3) 0.008(3) 0.016(2) 0.006(2) C(10) 0.080(4) 0.048(3) 0.054(3) -0.020(3) 0.017(3) -0.001(2) C(11) 0.052(3) 0.073(4) 0.065(3) -0.024(3) 0.001(3) -0.008(3) C(12) 0.035(2) 0.064(3) 0.061(3) -0.001(2) -0.001(2) 0.000(3) C(13) 0.024(2) 0.054(3) 0.038(2) 0.006(2) 0.002(2) 0.006(2) C(14) 0.028(2) 0.045(2) 0.037(2) 0.010(2) 0.006(2) 0.009(2) C(15) 0.035(2) 0.034(2) 0.041(2) 0.005(2) -0.005(2) 0.006(2) C(16) 0.062(3) 0.044(3) 0.042(3) 0.006(2) 0.003(2) 0.000(2) C(17) 0.095(4) 0.052(3) 0.048(3) 0.013(3) -0.006(3) -0.010(3) C(18) 0.085(4) 0.044(3) 0.088(5) -0.002(3) -0.027(3) -0.013(3) C(19) 0.055(3) 0.046(3) 0.108(5) -0.013(3) -0.004(3) 0.002(3) C(20) 0.046(3) 0.041(3) 0.061(3) -0.003(2) 0.001(2) 0.006(2) C(21) 0.034(2) 0.038(2) 0.029(2) 0.001(2) 0.003(2) 0.006(2) C(22) 0.044(3) 0.058(3) 0.062(3) 0.003(2) 0.004(2) 0.027(3) C(23) 0.063(3) 0.075(4) 0.070(4) 0.013(3) 0.000(3) 0.040(3) C(24) 0.087(4) 0.056(3) 0.048(3) 0.001(3) 0.014(3) 0.023(2) C(25) 0.062(3) 0.058(3) 0.056(3) 0.000(3) 0.027(3) 0.017(3) C(26) 0.038(2) 0.055(3) 0.047(3) 0.005(2) 0.012(2) 0.014(2) C(27) 0.054(3) 0.048(3) 0.056(3) 0.004(2) 0.008(2) 0.020(2) C(28) 0.063(3) 0.066(4) 0.075(4) 0.005(3) 0.000(3) 0.018(3) C(29) 0.069(4) 0.087(5) 0.099(5) 0.001(3) -0.007(3) 0.030(4) C(30) 0.077(4) 0.082(5) 0.116(6) 0.026(4) 0.011(4) 0.047(4) C(31) 0.101(5) 0.066(4) 0.091(5) 0.026(4) 0.010(4) 0.013(3) C(32) 0.076(4) 0.051(3) 0.064(3) 0.012(3) -0.004(3) 0.015(3) C(33) 0.062(3) 0.050(3) 0.038(2) 0.009(2) 0.009(2) 0.014(2) C(34) 0.082(4) 0.059(3) 0.050(3) 0.004(3) -0.001(3) 0.012(3) C(35) 0.079(4) 0.075(4) 0.068(4) 0.006(3) -0.005(3) -0.001(3) C(36) 0.094(5) 0.109(6) 0.040(3) 0.031(4) -0.001(3) 0.014(3) C(37) 0.114(5) 0.106(5) 0.046(3) 0.024(4) 0.017(3) 0.031(3) C(38) 0.085(4) 0.070(4) 0.043(3) 0.009(3) 0.011(3) 0.023(3) C(39) 0.065(3) 0.046(3) 0.035(2) 0.003(2) 0.006(2) 0.014(2) C(40) 0.074(4) 0.081(4) 0.044(3) 0.023(3) 0.010(2) 0.025(3) C(41) 0.068(4) 0.089(4) 0.066(4) 0.024(3) 0.016(3) 0.023(3) C(42) 0.075(4) 0.071(4) 0.053(3) 0.000(3) 0.021(3) 0.015(3) C(43) 0.076(4) 0.083(4) 0.039(3) -0.011(3) 0.003(2) 0.026(3) C(44) 0.057(3) 0.069(3) 0.048(3) 0.002(3) 0.004(2) 0.027(3) C(45) 0.076(3) 0.046(3) 0.041(3) -0.003(3) 0.008(2) 0.013(2) C(46) 0.109(5) 0.053(4) 0.077(4) 0.005(3) 0.016(4) 0.019(3) C(47) 0.161(8) 0.055(4) 0.086(5) 0.006(5) 0.017(5) 0.010(4) C(48) 0.156(8) 0.070(5) 0.070(4) -0.042(5) -0.001(5) 0.025(4) C(49) 0.110(5) 0.088(5) 0.076(4) -0.026(4) 0.011(4) 0.032(4) C(50) 0.096(4) 0.061(4) 0.063(4) -0.012(3) 0.010(3) 0.021(3) C(51) 0.120(8) 0.102(7) 0.119(7) 0.034(6) 0.023(6) 0.048(5) C(52) 0.136(9) 0.137(9) 0.47(2) 0.040(7) 0.10(1) 0.12(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(4) 2.217(1) . . yes Pt(1) P(5) 2.208(1) . . yes Pt(1) O(1) 2.093(3) . . yes Pt(1) O(2) 2.090(3) . . yes Cl(1) C(53) 1.813 . . yes Cl(1) C(53) 1.813 . 2_454 yes Cl(2) C(53) 1.708(7) . . yes P(1) O(1) 1.506(3) . . yes P(1) O(4) 1.456(3) . . yes P(1) O(5) 1.611(3) . . yes P(1) O(9) 1.575(4) . . yes P(2) O(2) 1.508(3) . . yes P(2) O(5) 1.607(3) . . yes P(2) O(6) 1.453(3) . . yes P(2) O(7) 1.570(4) . . yes P(3) O(3) 1.413(4) . . yes P(3) O(7) 1.603(4) . . yes P(3) O(8) 1.439(4) . . yes P(3) O(9) 1.626(4) . . yes P(4) C(1) 1.811(4) . . yes P(4) C(7) 1.811(4) . . yes P(4) C(13) 1.830(4) . . yes P(5) C(14) 1.817(4) . . yes P(5) C(15) 1.808(4) . . yes P(5) C(21) 1.814(4) . . yes P(6) C(27) 1.786(5) . . yes P(6) C(33) 1.782(5) . . yes P(6) C(39) 1.789(4) . . yes P(6) C(45) 1.797(5) . . yes N(1) C(51) 1.07(1) . . yes C(1) C(2) 1.378(6) . . yes C(1) C(6) 1.391(6) . . yes C(2) C(3) 1.387(7) . . yes C(3) C(4) 1.354(9) . . yes C(4) C(5) 1.373(9) . . yes C(5) C(6) 1.385(8) . . yes C(7) C(8) 1.381(6) . . yes C(7) C(12) 1.387(5) . . yes C(8) C(9) 1.393(6) . . yes C(9) C(10) 1.361(7) . . yes C(10) C(11) 1.351(7) . . yes C(11) C(12) 1.392(7) . . yes C(13) C(14) 1.531(5) . . yes C(15) C(16) 1.386(6) . . yes C(15) C(20) 1.381(6) . . yes C(16) C(17) 1.378(6) . . yes C(17) C(18) 1.361(8) . . yes C(18) C(19) 1.376(8) . . yes C(19) C(20) 1.388(6) . . yes C(21) C(22) 1.378(6) . . yes C(21) C(26) 1.389(5) . . yes C(22) C(23) 1.387(7) . . yes C(23) C(24) 1.356(7) . . yes C(24) C(25) 1.363(7) . . yes C(25) C(26) 1.376(6) . . yes C(27) C(28) 1.391(7) . . yes C(27) C(32) 1.393(7) . . yes C(28) C(29) 1.377(8) . . yes C(29) C(30) 1.386(9) . . yes C(30) C(31) 1.403(9) . . yes C(31) C(32) 1.370(8) . . yes C(33) C(34) 1.375(7) . . yes C(33) C(38) 1.383(6) . . yes C(34) C(35) 1.402(7) . . yes C(35) C(36) 1.370(9) . . yes C(36) C(37) 1.352(9) . . yes C(37) C(38) 1.385(8) . . yes C(39) C(40) 1.394(7) . . yes C(39) C(44) 1.387(6) . . yes C(40) C(41) 1.372(7) . . yes C(41) C(42) 1.397(8) . . yes C(42) C(43) 1.356(7) . . yes C(43) C(44) 1.379(7) . . yes C(45) C(46) 1.361(7) . . yes C(45) C(50) 1.392(7) . . yes C(46) C(47) 1.408(8) . . yes C(47) C(48) 1.367(10) . . yes C(48) C(49) 1.356(10) . . yes C(49) C(50) 1.389(8) . . yes C(51) C(52) 1.34(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(4) Pt(1) P(5) 86.52(4) . . . yes P(4) Pt(1) O(1) 177.78(8) . . . yes P(4) Pt(1) O(2) 92.27(8) . . . yes P(5) Pt(1) O(1) 91.66(7) . . . yes P(5) Pt(1) O(2) 178.68(9) . . . yes O(1) Pt(1) O(2) 89.57(10) . . . yes C(53) Cl(1) C(53) 180.0 . . 2_454 yes O(1) P(1) O(4) 116.5(2) . . . yes O(1) P(1) O(5) 107.7(1) . . . yes O(1) P(1) O(9) 109.2(2) . . . yes O(4) P(1) O(5) 110.3(2) . . . yes O(4) P(1) O(9) 110.2(2) . . . yes O(5) P(1) O(9) 102.0(2) . . . yes O(2) P(2) O(5) 107.1(2) . . . yes O(2) P(2) O(6) 116.7(2) . . . yes O(2) P(2) O(7) 106.5(2) . . . yes O(5) P(2) O(6) 110.5(2) . . . yes O(5) P(2) O(7) 102.0(2) . . . yes O(6) P(2) O(7) 112.8(2) . . . yes O(3) P(3) O(7) 106.7(3) . . . yes O(3) P(3) O(8) 123.4(4) . . . yes O(3) P(3) O(9) 108.1(3) . . . yes O(7) P(3) O(8) 107.3(3) . . . yes O(7) P(3) O(9) 101.4(2) . . . yes O(8) P(3) O(9) 107.6(2) . . . yes Pt(1) P(4) C(1) 112.2(1) . . . yes Pt(1) P(4) C(7) 115.5(1) . . . yes Pt(1) P(4) C(13) 109.5(1) . . . yes C(1) P(4) C(7) 107.3(2) . . . yes C(1) P(4) C(13) 106.8(2) . . . yes C(7) P(4) C(13) 104.9(2) . . . yes Pt(1) P(5) C(14) 108.1(1) . . . yes Pt(1) P(5) C(15) 114.5(1) . . . yes Pt(1) P(5) C(21) 112.9(1) . . . yes C(14) P(5) C(15) 108.1(2) . . . yes C(14) P(5) C(21) 108.7(2) . . . yes C(15) P(5) C(21) 104.3(2) . . . yes C(27) P(6) C(33) 110.8(2) . . . yes C(27) P(6) C(39) 112.6(2) . . . yes C(27) P(6) C(45) 107.7(2) . . . yes C(33) P(6) C(39) 107.9(2) . . . yes C(33) P(6) C(45) 109.8(2) . . . yes C(39) P(6) C(45) 108.1(2) . . . yes Pt(1) O(1) P(1) 129.5(2) . . . yes Pt(1) O(2) P(2) 125.3(2) . . . yes P(1) O(5) P(2) 122.4(2) . . . yes P(2) O(7) P(3) 136.0(2) . . . yes P(1) O(9) P(3) 132.3(2) . . . yes P(4) C(1) C(2) 120.5(3) . . . yes P(4) C(1) C(6) 121.1(4) . . . yes C(2) C(1) C(6) 118.5(4) . . . yes C(1) C(2) C(3) 120.7(5) . . . yes C(2) C(3) C(4) 120.6(6) . . . yes C(3) C(4) C(5) 119.5(5) . . . yes C(4) C(5) C(6) 120.8(5) . . . yes C(1) C(6) C(5) 119.8(5) . . . yes P(4) C(7) C(8) 120.3(3) . . . yes P(4) C(7) C(12) 120.5(3) . . . yes C(8) C(7) C(12) 119.2(4) . . . yes C(7) C(8) C(9) 119.9(4) . . . yes C(8) C(9) C(10) 120.7(5) . . . yes C(9) C(10) C(11) 119.4(4) . . . yes C(10) C(11) C(12) 121.8(5) . . . yes C(7) C(12) C(11) 119.0(4) . . . yes P(4) C(13) C(14) 109.0(2) . . . yes P(5) C(14) C(13) 109.7(3) . . . yes P(5) C(15) C(16) 120.8(3) . . . yes P(5) C(15) C(20) 119.4(3) . . . yes C(16) C(15) C(20) 119.8(4) . . . yes C(15) C(16) C(17) 119.7(5) . . . yes C(16) C(17) C(18) 120.4(5) . . . yes C(17) C(18) C(19) 120.8(5) . . . yes C(18) C(19) C(20) 119.5(5) . . . yes C(15) C(20) C(19) 119.9(5) . . . yes P(5) C(21) C(22) 117.5(3) . . . yes P(5) C(21) C(26) 123.4(3) . . . yes C(22) C(21) C(26) 119.1(4) . . . yes C(21) C(22) C(23) 120.1(4) . . . yes C(22) C(23) C(24) 120.5(5) . . . yes C(23) C(24) C(25) 119.6(5) . . . yes C(24) C(25) C(26) 121.3(4) . . . yes C(21) C(26) C(25) 119.4(4) . . . yes P(6) C(27) C(28) 120.3(4) . . . yes P(6) C(27) C(32) 119.4(4) . . . yes C(28) C(27) C(32) 120.2(5) . . . yes C(27) C(28) C(29) 120.3(5) . . . yes C(28) C(29) C(30) 119.4(6) . . . yes C(29) C(30) C(31) 120.3(6) . . . yes C(30) C(31) C(32) 119.9(6) . . . yes C(27) C(32) C(31) 119.7(5) . . . yes P(6) C(33) C(34) 119.7(4) . . . yes P(6) C(33) C(38) 120.0(4) . . . yes C(34) C(33) C(38) 120.4(5) . . . yes C(33) C(34) C(35) 118.6(5) . . . yes C(34) C(35) C(36) 120.5(6) . . . yes C(35) C(36) C(37) 120.5(5) . . . yes C(36) C(37) C(38) 120.2(6) . . . yes C(33) C(38) C(37) 119.9(5) . . . yes P(6) C(39) C(40) 118.9(3) . . . yes P(6) C(39) C(44) 121.5(4) . . . yes C(40) C(39) C(44) 119.5(4) . . . yes C(39) C(40) C(41) 120.2(5) . . . yes C(40) C(41) C(42) 119.7(5) . . . yes C(41) C(42) C(43) 120.0(5) . . . yes C(42) C(43) C(44) 121.1(5) . . . yes C(39) C(44) C(43) 119.6(5) . . . yes P(6) C(45) C(46) 120.2(4) . . . yes P(6) C(45) C(50) 119.8(4) . . . yes C(46) C(45) C(50) 120.1(5) . . . yes C(45) C(46) C(47) 119.3(6) . . . yes C(46) C(47) C(48) 119.9(7) . . . yes C(47) C(48) C(49) 121.1(6) . . . yes C(48) C(49) C(50) 119.5(7) . . . yes C(45) C(50) C(49) 120.1(6) . . . yes N(1) C(51) C(52) 171(1) . . . yes Cl(1) C(53) Cl(2) 116.9(3) . . . yes #------------------------------------------------------------------------------ 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 Pt(1) P(4) C(1) C(2) -2.7(4) . . . . yes Pt(1) P(4) C(1) C(6) 178.8(3) . . . . yes Pt(1) P(4) C(7) C(8) 24.4(4) . . . . yes Pt(1) P(4) C(7) C(12) -157.2(3) . . . . yes Pt(1) P(4) C(13) C(14) -30.2(3) . . . . yes Pt(1) P(5) C(14) C(13) -40.4(3) . . . . yes Pt(1) P(5) C(15) C(16) 157.2(3) . . . . yes Pt(1) P(5) C(15) C(20) -22.9(4) . . . . yes Pt(1) P(5) C(21) C(22) -50.2(4) . . . . yes Pt(1) P(5) C(21) C(26) 132.8(3) . . . . yes Pt(1) O(1) P(1) O(4) 166.4(2) . . . . yes Pt(1) O(1) P(1) O(5) 42.0(3) . . . . yes Pt(1) O(1) P(1) O(9) -68.0(3) . . . . yes Pt(1) O(2) P(2) O(5) -53.6(3) . . . . yes Pt(1) O(2) P(2) O(6) -178.1(2) . . . . yes Pt(1) O(2) P(2) O(7) 54.9(3) . . . . yes P(1) O(1) Pt(1) P(4) -176(2) . . . . yes P(1) O(1) Pt(1) P(5) 149.2(2) . . . . yes P(1) O(1) Pt(1) O(2) -30.3(2) . . . . yes P(1) O(5) P(2) O(2) 64.5(3) . . . . yes P(1) O(5) P(2) O(6) -167.4(2) . . . . yes P(1) O(5) P(2) O(7) -47.1(3) . . . . yes P(1) O(9) P(3) O(3) -116.7(4) . . . . yes P(1) O(9) P(3) O(7) -4.7(4) . . . . yes P(1) O(9) P(3) O(8) 107.9(4) . . . . yes P(2) O(2) Pt(1) P(4) -145.3(2) . . . . yes P(2) O(2) Pt(1) P(5) -121(3) . . . . yes P(2) O(2) Pt(1) O(1) 36.0(2) . . . . yes P(2) O(5) P(1) O(1) -57.8(3) . . . . yes P(2) O(5) P(1) O(4) 174.1(2) . . . . yes P(2) O(5) P(1) O(9) 57.1(2) . . . . yes P(2) O(7) P(3) O(3) 132.8(4) . . . . yes P(2) O(7) P(3) O(8) -93.1(4) . . . . yes P(2) O(7) P(3) O(9) 19.7(4) . . . . yes P(3) O(7) P(2) O(2) -109.4(4) . . . . yes P(3) O(7) P(2) O(5) 2.7(4) . . . . yes P(3) O(7) P(2) O(6) 121.3(4) . . . . yes P(3) O(9) P(1) O(1) 87.2(3) . . . . yes P(3) O(9) P(1) O(4) -143.6(3) . . . . yes P(3) O(9) P(1) O(5) -26.6(4) . . . . yes P(4) Pt(1) P(5) C(14) 17.0(1) . . . . yes P(4) Pt(1) P(5) C(15) 137.5(2) . . . . yes P(4) Pt(1) P(5) C(21) -103.2(1) . . . . yes P(4) C(1) C(2) C(3) -178.2(4) . . . . yes P(4) C(1) C(6) C(5) 177.7(4) . . . . yes P(4) C(7) C(8) C(9) 179.2(4) . . . . yes P(4) C(7) C(12) C(11) -177.8(4) . . . . yes P(4) C(13) C(14) P(5) 44.4(3) . . . . yes P(5) Pt(1) P(4) C(1) -113.6(1) . . . . yes P(5) Pt(1) P(4) C(7) 123.0(1) . . . . yes P(5) Pt(1) P(4) C(13) 4.9(2) . . . . yes P(5) C(15) C(16) C(17) -178.8(4) . . . . yes P(5) C(15) C(20) C(19) 179.3(4) . . . . yes P(5) C(21) C(22) C(23) -175.7(4) . . . . yes P(5) C(21) C(26) C(25) 176.1(3) . . . . yes P(6) C(27) C(28) C(29) -175.6(5) . . . . yes P(6) C(27) C(32) C(31) 173.5(5) . . . . yes P(6) C(33) C(34) C(35) 179.9(4) . . . . yes P(6) C(33) C(38) C(37) -179.8(4) . . . . yes P(6) C(39) C(40) C(41) -173.1(4) . . . . yes P(6) C(39) C(44) C(43) 173.2(4) . . . . yes P(6) C(45) C(46) C(47) -178.6(5) . . . . yes P(6) C(45) C(50) C(49) 180.0(4) . . . . yes O(1) Pt(1) P(4) C(1) -148(2) . . . . yes O(1) Pt(1) P(4) C(7) 88(2) . . . . yes O(1) Pt(1) P(4) C(13) -29(2) . . . . yes O(1) Pt(1) P(5) C(14) -164.3(2) . . . . yes O(1) Pt(1) P(5) C(15) -43.7(2) . . . . yes O(1) Pt(1) P(5) C(21) 75.5(2) . . . . yes O(2) Pt(1) P(4) C(1) 65.9(2) . . . . yes O(2) Pt(1) P(4) C(7) -57.5(2) . . . . yes O(2) Pt(1) P(4) C(13) -175.6(2) . . . . yes O(2) Pt(1) P(5) C(14) -6(4) . . . . yes O(2) Pt(1) P(5) C(15) 114(4) . . . . yes O(2) Pt(1) P(5) C(21) -126(4) . . . . yes C(1) P(4) C(7) C(8) -101.5(4) . . . . yes C(1) P(4) C(7) C(12) 76.8(4) . . . . yes C(1) P(4) C(13) C(14) 91.5(3) . . . . yes C(1) C(2) C(3) C(4) 0.2(9) . . . . yes C(1) C(6) C(5) C(4) 0.8(9) . . . . yes C(2) C(1) P(4) C(7) 125.2(4) . . . . yes C(2) C(1) P(4) C(13) -122.7(4) . . . . yes C(2) C(1) C(6) C(5) -0.8(8) . . . . yes C(2) C(3) C(4) C(5) 0(1) . . . . yes C(3) C(2) C(1) C(6) 0.4(7) . . . . yes C(3) C(4) C(5) C(6) 0(1) . . . . yes C(6) C(1) P(4) C(7) -53.4(4) . . . . yes C(6) C(1) P(4) C(13) 58.7(4) . . . . yes C(7) P(4) C(13) C(14) -154.8(3) . . . . yes C(7) C(8) C(9) C(10) -2.0(7) . . . . yes C(7) C(12) C(11) C(10) -0.9(9) . . . . yes C(8) C(7) P(4) C(13) 145.1(4) . . . . yes C(8) C(7) C(12) C(11) 0.6(7) . . . . yes C(8) C(9) C(10) C(11) 1.6(8) . . . . yes C(9) C(8) C(7) C(12) 0.9(7) . . . . yes C(9) C(10) C(11) C(12) -0.1(9) . . . . yes C(12) C(7) P(4) C(13) -36.6(4) . . . . yes C(13) C(14) P(5) C(15) -164.9(3) . . . . yes C(13) C(14) P(5) C(21) 82.4(3) . . . . yes C(14) P(5) C(15) C(16) -82.3(4) . . . . yes C(14) P(5) C(15) C(20) 97.7(4) . . . . yes C(14) P(5) C(21) C(22) -170.0(3) . . . . yes C(14) P(5) C(21) C(26) 13.0(4) . . . . yes C(15) P(5) C(21) C(22) 74.8(4) . . . . yes C(15) P(5) C(21) C(26) -102.2(4) . . . . yes C(15) C(16) C(17) C(18) -0.7(8) . . . . yes C(15) C(20) C(19) C(18) -0.2(8) . . . . yes C(16) C(15) P(5) C(21) 33.2(4) . . . . yes C(16) C(15) C(20) C(19) -0.8(7) . . . . yes C(16) C(17) C(18) C(19) -0.3(9) . . . . yes C(17) C(16) C(15) C(20) 1.2(7) . . . . yes C(17) C(18) C(19) C(20) 0.7(9) . . . . yes C(20) C(15) P(5) C(21) -146.8(4) . . . . yes C(21) C(22) C(23) C(24) -0.9(8) . . . . yes C(21) C(26) C(25) C(24) -0.2(7) . . . . yes C(22) C(21) C(26) C(25) -0.9(6) . . . . yes C(22) C(23) C(24) C(25) -0.2(8) . . . . yes C(23) C(22) C(21) C(26) 1.5(7) . . . . yes C(23) C(24) C(25) C(26) 0.8(8) . . . . yes C(27) P(6) C(33) C(34) 75.0(4) . . . . yes C(27) P(6) C(33) C(38) -105.5(4) . . . . yes C(27) P(6) C(39) C(40) -158.2(4) . . . . yes C(27) P(6) C(39) C(44) 26.7(5) . . . . yes C(27) P(6) C(45) C(46) -152.5(5) . . . . yes C(27) P(6) C(45) C(50) 28.0(5) . . . . yes C(27) C(28) C(29) C(30) 2.7(10) . . . . yes C(27) C(32) C(31) C(30) 1.5(10) . . . . yes C(28) C(27) P(6) C(33) 164.8(4) . . . . yes C(28) C(27) P(6) C(39) -74.2(5) . . . . yes C(28) C(27) P(6) C(45) 44.8(5) . . . . yes C(28) C(27) C(32) C(31) -3.0(8) . . . . yes C(28) C(29) C(30) C(31) -4(1) . . . . yes C(29) C(28) C(27) C(32) 0.9(8) . . . . yes C(29) C(30) C(31) C(32) 2(1) . . . . yes C(32) C(27) P(6) C(33) -11.7(5) . . . . yes C(32) C(27) P(6) C(39) 109.3(4) . . . . yes C(32) C(27) P(6) C(45) -131.7(4) . . . . yes C(33) P(6) C(39) C(40) -35.6(5) . . . . yes C(33) P(6) C(39) C(44) 149.3(4) . . . . yes C(33) P(6) C(45) C(46) 86.7(5) . . . . yes C(33) P(6) C(45) C(50) -92.7(5) . . . . yes C(33) C(34) C(35) C(36) 0.1(9) . . . . yes C(33) C(38) C(37) C(36) -0.4(9) . . . . yes C(34) C(33) P(6) C(39) -48.7(5) . . . . yes C(34) C(33) P(6) C(45) -166.2(4) . . . . yes C(34) C(33) C(38) C(37) -0.3(8) . . . . yes C(34) C(35) C(36) C(37) -0.8(10) . . . . yes C(35) C(34) C(33) C(38) 0.5(8) . . . . yes C(35) C(36) C(37) C(38) 0(1) . . . . yes C(38) C(33) P(6) C(39) 130.8(4) . . . . yes C(38) C(33) P(6) C(45) 13.3(5) . . . . yes C(39) P(6) C(45) C(46) -30.7(5) . . . . yes C(39) P(6) C(45) C(50) 149.9(4) . . . . yes C(39) C(40) C(41) C(42) -0.8(9) . . . . yes C(39) C(44) C(43) C(42) 0.2(8) . . . . yes C(40) C(39) P(6) C(45) 83.1(4) . . . . yes C(40) C(39) C(44) C(43) -1.9(8) . . . . yes C(40) C(41) C(42) C(43) -0.9(9) . . . . yes C(41) C(40) C(39) C(44) 2.1(8) . . . . yes C(41) C(42) C(43) C(44) 1.2(9) . . . . yes C(44) C(39) P(6) C(45) -92.0(4) . . . . yes C(45) C(46) C(47) C(48) -1(1) . . . . yes C(45) C(50) C(49) C(48) -1.2(10) . . . . yes C(46) C(45) C(50) C(49) 0.5(9) . . . . yes C(46) C(47) C(48) C(49) 1(1) . . . . yes C(47) C(46) C(45) C(50) 0.9(9) . . . . yes C(47) C(48) C(49) C(50) 0(1) . . . . yes C(47) C(48) C(49) C(50) 0(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) N(1) 3.32(1) . 2_454 ? Cl(2) C(51) 3.52(1) . 2_454 ? O(3) C(34) 3.523(8) . 2_444 ? O(4) C(26) 3.153(5) . 1_455 ? O(4) C(42) 3.207(6) . . ? O(4) C(53) 3.476(4) . . ? O(4) C(14) 3.524(5) . 1_455 ? O(4) C(43) 3.550(6) . . ? O(4) C(13) 3.566(5) . 1_455 ? O(5) C(13) 3.309(4) . 1_455 ? O(6) C(12) 3.330(5) . 1_455 ? O(6) C(52) 3.43(1) . 2_454 ? O(6) C(11) 3.520(6) . 2_555 ? O(6) C(52) 3.59(2) . 1_556 ? O(7) C(37) 3.331(6) . 1_556 ? O(8) C(32) 3.155(7) . 2_444 ? O(8) C(31) 3.401(8) . 2_444 ? O(8) C(13) 3.476(7) . 1_455 ? N(1) C(40) 3.53(1) . . ? C(8) C(10) 3.414(7) . 2_555 ? C(8) C(9) 3.444(7) . 2_555 ? C(8) C(49) 3.501(8) . 2_554 ? C(8) C(48) 3.592(8) . 2_554 ? C(9) C(49) 3.415(8) . 2_554 ? C(9) C(9) 3.54(1) . 2_555 ? C(19) C(42) 3.591(8) . 2_444 ? C(24) C(24) 3.52(1) . 2_554 ? C(35) C(35) 3.50(1) . 2_443 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_(PPN)[Pt(P3O9)(dppb)](6) _database_code_CSD 202878 _audit_creation_date 'Thu Apr 3 12:28:18 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C66.50 H62 Cl N2 O9 P7 Pt ' _chemical_formula_moiety (PPN)[Pt(P3O9)(dppb)] _chemical_formula_weight 1480.59 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 19.420(4) _cell_length_b 17.066(3) _cell_length_c 20.321(3) _cell_angle_alpha 90 _cell_angle_beta 104.99(1) _cell_angle_gamma 90 _cell_volume 6505(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.419 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 15389 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.39 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; for calculating R-factor (gt). ; _reflns_number_total 14959 _reflns_number_gt 9237 _reflns_threshold_criterion F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0394 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9237 _refine_ls_number_parameters 767 _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0361 _refine_diff_density_max 1.25 _refine_diff_density_min -0.93 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0002(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt -0.12929(1) -0.20926(1) -0.28395(1) 0.03087(5) Uani 1.00 d . . . Cl(1) Cl -0.0918 0.0314 -0.0130 0.3166 Uiso 0.50 d P . . Cl(2) Cl 0.0545 0.0087 0.0191 0.3166 Uiso 0.50 d P . . P(1) P -0.17826(9) -0.14687(9) -0.15091(7) 0.0418(4) Uani 1.00 d . . . P(2) P -0.07558(8) -0.26847(9) -0.12665(7) 0.0384(4) Uani 1.00 d . . . P(3) P -0.22729(8) -0.30810(9) -0.17085(8) 0.0429(5) Uani 1.00 d . . . P(4) P -0.06986(8) -0.27912(8) -0.34303(7) 0.0359(4) Uani 1.00 d . . . P(5) P -0.19981(8) -0.15414(8) -0.37607(7) 0.0338(4) Uani 1.00 d . . . P(6) P -0.33754(8) -0.62149(9) -0.48532(8) 0.0390(4) Uani 1.00 d . . . P(7) P -0.43024(9) -0.76056(9) -0.53845(8) 0.0415(4) Uani 1.00 d . . . O(1) O -0.1700(2) -0.1345(2) -0.2222(2) 0.038(1) Uani 1.00 d . . . O(2) O -0.0608(2) -0.2568(2) -0.1957(2) 0.040(1) Uani 1.00 d . . . O(3) O -0.2381(2) -0.3145(2) -0.2450(2) 0.050(1) Uani 1.00 d . . . O(4) O -0.1970(2) -0.0783(2) -0.1157(2) 0.061(1) Uani 1.00 d . . . O(5) O -0.1056(2) -0.1861(2) -0.1067(2) 0.044(1) Uani 1.00 d . . . O(6) O -0.0169(2) -0.2965(3) -0.0714(2) 0.055(1) Uani 1.00 d . . . O(7) O -0.1439(2) -0.3237(2) -0.1338(2) 0.043(1) Uani 1.00 d . . . O(8) O -0.2695(2) -0.3544(3) -0.1347(2) 0.069(2) Uani 1.00 d . . . O(9) O -0.2338(2) -0.2164(2) -0.1512(2) 0.045(1) Uani 1.00 d . . . N(1) N -0.3861(3) -0.6960(3) -0.4908(2) 0.051(2) Uani 1.00 d . . . N(2) N -0.3038(5) -0.8177(5) -0.2484(5) 0.122(4) Uani 1.00 d . . . C(1) C -0.0537(3) -0.3795(3) -0.3158(3) 0.038(2) Uani 1.00 d . . . C(2) C -0.0977(3) -0.4169(4) -0.2819(3) 0.049(2) Uani 1.00 d . . . C(3) C -0.0876(4) -0.4961(4) -0.2654(4) 0.073(3) Uani 1.00 d . . . C(4) C -0.0352(5) -0.5369(4) -0.2843(4) 0.077(3) Uani 1.00 d . . . C(5) C 0.0087(4) -0.5006(4) -0.3170(4) 0.071(3) Uani 1.00 d . . . C(6) C -0.0004(4) -0.4222(4) -0.3328(3) 0.056(2) Uani 1.00 d . . . C(7) C 0.0172(3) -0.2352(3) -0.3326(3) 0.043(2) Uani 1.00 d . . . C(8) C 0.0688(4) -0.2476(4) -0.2721(4) 0.061(2) Uani 1.00 d . . . C(9) C 0.1359(4) -0.2122(5) -0.2628(4) 0.077(3) Uani 1.00 d . . . C(10) C 0.1496(4) -0.1639(5) -0.3139(6) 0.088(3) Uani 1.00 d . . . C(11) C 0.0975(4) -0.1512(5) -0.3709(5) 0.080(3) Uani 1.00 d . . . C(12) C 0.0312(4) -0.1858(4) -0.3813(4) 0.064(2) Uani 1.00 d . . . C(13) C -0.1055(3) -0.2901(4) -0.4345(3) 0.047(2) Uani 1.00 d . . . C(14) C -0.1733(4) -0.3394(4) -0.4541(3) 0.058(2) Uani 1.00 d . . . C(15) C -0.2354(4) -0.3084(4) -0.4308(3) 0.056(2) Uani 1.00 d . . . C(16) C -0.2502(3) -0.2206(4) -0.4424(3) 0.046(2) Uani 1.00 d . . . C(17) C -0.2724(3) -0.0978(3) -0.3573(3) 0.038(2) Uani 1.00 d . . . C(18) C -0.3142(3) -0.1347(4) -0.3200(3) 0.049(2) Uani 1.00 d . . . C(19) C -0.3735(4) -0.0962(5) -0.3087(4) 0.067(3) Uani 1.00 d . . . C(20) C -0.3905(4) -0.0228(5) -0.3339(4) 0.071(3) Uani 1.00 d . . . C(21) C -0.3502(4) 0.0135(4) -0.3712(4) 0.072(3) Uani 1.00 d . . . C(22) C -0.2904(4) -0.0240(4) -0.3827(3) 0.056(2) Uani 1.00 d . . . C(23) C -0.1501(3) -0.0839(3) -0.4120(3) 0.038(2) Uani 1.00 d . . . C(24) C -0.1098(3) -0.0294(4) -0.3675(3) 0.054(2) Uani 1.00 d . . . C(25) C -0.0699(4) 0.0266(4) -0.3899(4) 0.064(2) Uani 1.00 d . . . C(26) C -0.0675(4) 0.0263(4) -0.4578(4) 0.064(2) Uani 1.00 d . . . C(27) C -0.1063(4) -0.0269(4) -0.5025(3) 0.057(2) Uani 1.00 d . . . C(28) C -0.1483(3) -0.0813(3) -0.4801(3) 0.044(2) Uani 1.00 d . . . C(29) C -0.3273(3) -0.5814(3) -0.4022(3) 0.039(2) Uani 1.00 d . . . C(30) C -0.3399(3) -0.6257(4) -0.3501(3) 0.050(2) Uani 1.00 d . . . C(31) C -0.3298(4) -0.5943(5) -0.2855(3) 0.063(2) Uani 1.00 d . . . C(32) C -0.3046(4) -0.5197(5) -0.2728(4) 0.067(3) Uani 1.00 d . . . C(33) C -0.2918(4) -0.4745(4) -0.3239(4) 0.063(2) Uani 1.00 d . . . C(34) C -0.3024(4) -0.5050(4) -0.3884(3) 0.055(2) Uani 1.00 d . . . C(35) C -0.2495(3) -0.6441(4) -0.4929(3) 0.056(2) Uani 1.00 d . . . C(36) C -0.1945(4) -0.6524(7) -0.4367(4) 0.112(4) Uani 1.00 d . . . C(37) C -0.1313(5) -0.6850(9) -0.4399(5) 0.162(5) Uani 1.00 d . . . C(38) C -0.1230(5) -0.7040(8) -0.5031(5) 0.152(5) Uani 1.00 d . . . C(39) C -0.1762(5) -0.6931(6) -0.5614(4) 0.098(3) Uani 1.00 d . . . C(40) C -0.2410(4) -0.6670(4) -0.5552(3) 0.062(2) Uani 1.00 d . . . C(41) C -0.3762(3) -0.5475(3) -0.5469(3) 0.039(2) Uani 1.00 d . . . C(42) C -0.4499(3) -0.5380(4) -0.5648(3) 0.051(2) Uani 1.00 d . . . C(43) C -0.4824(3) -0.4821(4) -0.6110(4) 0.063(2) Uani 1.00 d . . . C(44) C -0.4417(4) -0.4342(4) -0.6395(4) 0.070(3) Uani 1.00 d . . . C(45) C -0.3692(4) -0.4410(4) -0.6207(4) 0.072(3) Uani 1.00 d . . . C(46) C -0.3354(3) -0.4979(4) -0.5754(3) 0.052(2) Uani 1.00 d . . . C(47) C -0.4938(3) -0.7985(4) -0.4960(3) 0.044(2) Uani 1.00 d . . . C(48) C -0.5223(4) -0.7496(4) -0.4556(4) 0.065(2) Uani 1.00 d . . . C(49) C -0.5746(4) -0.7768(5) -0.4258(3) 0.070(3) Uani 1.00 d . . . C(50) C -0.5976(4) -0.8521(5) -0.4347(3) 0.057(2) Uani 1.00 d . . . C(51) C -0.5692(4) -0.9008(4) -0.4739(3) 0.059(2) Uani 1.00 d . . . C(52) C -0.5185(4) -0.8755(4) -0.5049(3) 0.054(2) Uani 1.00 d . . . C(53) C -0.3761(3) -0.8398(3) -0.5556(3) 0.042(2) Uani 1.00 d . . . C(54) C -0.3077(4) -0.8493(4) -0.5157(3) 0.054(2) Uani 1.00 d . . . C(55) C -0.2665(4) -0.9111(4) -0.5282(4) 0.065(2) Uani 1.00 d . . . C(56) C -0.2931(5) -0.9623(4) -0.5804(4) 0.069(3) Uani 1.00 d . . . C(57) C -0.3614(4) -0.9536(4) -0.6202(4) 0.061(2) Uani 1.00 d . . . C(58) C -0.4025(3) -0.8918(4) -0.6081(3) 0.052(2) Uani 1.00 d . . . C(59) C -0.4792(3) -0.7260(3) -0.6205(3) 0.044(2) Uani 1.00 d . . . C(60) C -0.5512(3) -0.7101(4) -0.6349(3) 0.057(2) Uani 1.00 d . . . C(61) C -0.5870(4) -0.6798(5) -0.6979(4) 0.076(3) Uani 1.00 d . . . C(62) C -0.5515(5) -0.6645(5) -0.7450(4) 0.080(3) Uani 1.00 d . . . C(63) C -0.4801(5) -0.6799(5) -0.7319(4) 0.086(3) Uani 1.00 d . . . C(64) C -0.4442(3) -0.7110(4) -0.6701(3) 0.062(2) Uani 1.00 d . . . C(65) C -0.2653(5) -0.8669(6) -0.2365(5) 0.088(3) Uani 1.00 d . . . C(66) C -0.2133(6) -0.9301(6) -0.2206(5) 0.116(4) Uani 1.00 d . . . C(67) C -0.0097 0.0887 0.0136 0.3166 Uiso 0.50 d P . . H(1) H -0.1349 -0.3887 -0.2700 0.0588 Uiso 1.00 calc . . . H(2) H -0.1168 -0.5216 -0.2410 0.0871 Uiso 1.00 calc . . . H(3) H -0.0293 -0.5912 -0.2746 0.0929 Uiso 1.00 calc . . . H(4) H 0.0456 -0.5293 -0.3291 0.0850 Uiso 1.00 calc . . . H(5) H 0.0305 -0.3970 -0.3556 0.0674 Uiso 1.00 calc . . . H(6) H 0.0589 -0.2797 -0.2375 0.0736 Uiso 1.00 calc . . . H(7) H 0.1719 -0.2207 -0.2219 0.0922 Uiso 1.00 calc . . . H(8) H 0.1951 -0.1406 -0.3084 0.1051 Uiso 1.00 calc . . . H(9) H 0.1064 -0.1176 -0.4050 0.0966 Uiso 1.00 calc . . . H(10) H -0.0047 -0.1755 -0.4220 0.0771 Uiso 1.00 calc . . . H(11) H -0.0703 -0.3145 -0.4524 0.0568 Uiso 1.00 calc . . . H(12) H -0.1158 -0.2395 -0.4539 0.0568 Uiso 1.00 calc . . . H(13) H -0.1623 -0.3902 -0.4351 0.0703 Uiso 1.00 calc . . . H(14) H -0.1875 -0.3431 -0.5024 0.0703 Uiso 1.00 calc . . . H(15) H -0.2265 -0.3184 -0.3833 0.0666 Uiso 1.00 calc . . . H(16) H -0.2768 -0.3362 -0.4545 0.0666 Uiso 1.00 calc . . . H(17) H -0.2396 -0.2069 -0.4840 0.0549 Uiso 1.00 calc . . . H(18) H -0.2995 -0.2123 -0.4464 0.0549 Uiso 1.00 calc . . . H(19) H -0.3023 -0.1860 -0.3025 0.0591 Uiso 1.00 calc . . . H(20) H -0.4020 -0.1212 -0.2833 0.0804 Uiso 1.00 calc . . . H(21) H -0.4306 0.0035 -0.3257 0.0853 Uiso 1.00 calc . . . H(22) H -0.3630 0.0643 -0.3895 0.0863 Uiso 1.00 calc . . . H(23) H -0.2621 0.0017 -0.4079 0.0672 Uiso 1.00 calc . . . H(24) H -0.1098 -0.0308 -0.3208 0.0648 Uiso 1.00 calc . . . H(25) H -0.0442 0.0649 -0.3592 0.0764 Uiso 1.00 calc . . . H(26) H -0.0386 0.0634 -0.4731 0.0763 Uiso 1.00 calc . . . H(27) H -0.1047 -0.0265 -0.5488 0.0684 Uiso 1.00 calc . . . H(28) H -0.1763 -0.1174 -0.5116 0.0525 Uiso 1.00 calc . . . H(29) H -0.3558 -0.6783 -0.3585 0.0598 Uiso 1.00 calc . . . H(30) H -0.3404 -0.6246 -0.2501 0.0761 Uiso 1.00 calc . . . H(31) H -0.2957 -0.4990 -0.2280 0.0802 Uiso 1.00 calc . . . H(32) H -0.2757 -0.4221 -0.3149 0.0756 Uiso 1.00 calc . . . H(33) H -0.2925 -0.4739 -0.4236 0.0658 Uiso 1.00 calc . . . H(34) H -0.1999 -0.6351 -0.3939 0.1343 Uiso 1.00 calc . . . H(35) H -0.0942 -0.6931 -0.4000 0.1954 Uiso 1.00 calc . . . H(36) H -0.0792 -0.7261 -0.5063 0.1825 Uiso 1.00 calc . . . H(37) H -0.1684 -0.7030 -0.6049 0.1178 Uiso 1.00 calc . . . H(38) H -0.2803 -0.6648 -0.5943 0.0749 Uiso 1.00 calc . . . H(39) H -0.4783 -0.5709 -0.5447 0.0610 Uiso 1.00 calc . . . H(40) H -0.5327 -0.4767 -0.6231 0.0758 Uiso 1.00 calc . . . H(41) H -0.4637 -0.3963 -0.6725 0.0835 Uiso 1.00 calc . . . H(42) H -0.3413 -0.4054 -0.6389 0.0870 Uiso 1.00 calc . . . H(43) H -0.2849 -0.5029 -0.5642 0.0630 Uiso 1.00 calc . . . H(44) H -0.5061 -0.6970 -0.4481 0.0772 Uiso 1.00 calc . . . H(45) H -0.5944 -0.7424 -0.3989 0.0835 Uiso 1.00 calc . . . H(46) H -0.6330 -0.8706 -0.4138 0.0689 Uiso 1.00 calc . . . H(47) H -0.5851 -0.9536 -0.4799 0.0709 Uiso 1.00 calc . . . H(48) H -0.5001 -0.9104 -0.5326 0.0651 Uiso 1.00 calc . . . H(49) H -0.2887 -0.8136 -0.4797 0.0649 Uiso 1.00 calc . . . H(50) H -0.2194 -0.9180 -0.5003 0.0775 Uiso 1.00 calc . . . H(51) H -0.2643 -1.0039 -0.5891 0.0826 Uiso 1.00 calc . . . H(52) H -0.3804 -0.9898 -0.6558 0.0735 Uiso 1.00 calc . . . H(53) H -0.4495 -0.8850 -0.6363 0.0617 Uiso 1.00 calc . . . H(54) H -0.5765 -0.7197 -0.6014 0.0677 Uiso 1.00 calc . . . H(55) H -0.6367 -0.6700 -0.7078 0.0911 Uiso 1.00 calc . . . H(56) H -0.5761 -0.6428 -0.7877 0.0955 Uiso 1.00 calc . . . H(57) H -0.4553 -0.6692 -0.7655 0.1029 Uiso 1.00 calc . . . H(58) H -0.3947 -0.7221 -0.6615 0.0746 Uiso 1.00 calc . . . H(59) H -0.2184 -0.9628 -0.2594 0.1396 Uiso 1.00 calc . . . H(60) H -0.2207 -0.9601 -0.1837 0.1396 Uiso 1.00 calc . . . H(61) H -0.1665 -0.9086 -0.2084 0.1396 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0351(1) 0.0335(1) 0.02556(10) 0.0013(1) 0.01074(7) 0.0017(1) P(1) 0.0521(10) 0.0452(9) 0.0307(8) 0.0028(8) 0.0153(7) -0.0041(7) P(2) 0.0374(8) 0.0472(10) 0.0282(7) 0.0002(7) 0.0044(6) 0.0026(6) P(3) 0.0381(9) 0.047(1) 0.0455(9) -0.0046(7) 0.0146(7) 0.0067(7) P(4) 0.0433(8) 0.0339(8) 0.0340(7) 0.0034(7) 0.0161(6) 0.0006(6) P(5) 0.0374(8) 0.0361(8) 0.0280(7) -0.0001(7) 0.0088(6) 0.0031(6) P(6) 0.0400(9) 0.0386(9) 0.0379(8) 0.0029(7) 0.0093(7) -0.0048(7) P(7) 0.0457(9) 0.0358(8) 0.0403(9) 0.0012(7) 0.0060(7) -0.0021(7) O(1) 0.049(2) 0.038(2) 0.029(2) 0.006(2) 0.013(2) -0.001(2) O(2) 0.037(2) 0.054(2) 0.030(2) 0.006(2) 0.008(2) 0.006(2) O(3) 0.048(3) 0.053(3) 0.044(2) -0.008(2) 0.004(2) -0.005(2) O(4) 0.094(4) 0.050(3) 0.044(3) 0.012(3) 0.028(2) -0.011(2) O(5) 0.051(3) 0.050(3) 0.029(2) 0.001(2) 0.004(2) -0.005(2) O(6) 0.046(2) 0.071(3) 0.040(2) 0.003(2) -0.003(2) 0.009(2) O(7) 0.041(2) 0.040(2) 0.046(2) -0.003(2) 0.008(2) 0.006(2) O(8) 0.055(3) 0.075(3) 0.083(3) -0.010(3) 0.031(3) 0.029(3) O(9) 0.043(2) 0.051(2) 0.045(2) 0.005(2) 0.019(2) 0.003(2) N(1) 0.065(3) 0.033(3) 0.048(3) -0.003(2) 0.000(3) -0.004(2) N(2) 0.108(7) 0.101(7) 0.157(9) 0.006(5) 0.035(6) 0.006(6) C(1) 0.046(3) 0.036(3) 0.033(3) 0.004(3) 0.010(3) 0.000(3) C(2) 0.058(4) 0.038(4) 0.050(4) -0.002(3) 0.014(3) 0.002(3) C(3) 0.088(6) 0.049(4) 0.078(5) -0.012(4) 0.014(5) 0.023(4) C(4) 0.094(7) 0.041(4) 0.085(6) 0.010(4) 0.000(5) 0.005(4) C(5) 0.069(5) 0.055(5) 0.085(6) 0.019(4) 0.016(5) -0.005(4) C(6) 0.065(5) 0.040(4) 0.066(4) 0.009(3) 0.022(4) 0.000(3) C(7) 0.041(3) 0.037(3) 0.058(4) 0.004(3) 0.023(3) -0.008(3) C(8) 0.053(4) 0.070(5) 0.066(5) -0.003(4) 0.024(4) -0.019(4) C(9) 0.047(4) 0.100(6) 0.081(5) -0.004(5) 0.012(4) -0.044(5) C(10) 0.057(5) 0.068(6) 0.152(9) -0.021(5) 0.053(6) -0.044(6) C(11) 0.059(5) 0.058(5) 0.135(8) -0.004(4) 0.046(5) 0.002(5) C(12) 0.056(4) 0.051(4) 0.094(6) 0.004(3) 0.033(4) 0.012(4) C(13) 0.063(4) 0.049(4) 0.036(3) 0.011(4) 0.024(3) -0.001(3) C(14) 0.079(5) 0.055(4) 0.040(4) 0.006(4) 0.011(4) -0.013(3) C(15) 0.073(5) 0.047(4) 0.043(4) -0.018(3) 0.008(3) -0.009(3) C(16) 0.048(3) 0.049(4) 0.038(3) -0.004(3) 0.006(3) -0.006(3) C(17) 0.035(3) 0.044(3) 0.032(3) 0.003(3) 0.004(3) -0.004(3) C(18) 0.041(4) 0.059(4) 0.047(4) -0.003(3) 0.010(3) 0.001(3) C(19) 0.041(4) 0.100(6) 0.062(5) -0.009(4) 0.017(4) -0.010(4) C(20) 0.053(5) 0.079(6) 0.078(6) 0.021(4) 0.011(4) -0.019(5) C(21) 0.073(6) 0.051(5) 0.082(6) 0.017(4) 0.003(5) 0.003(4) C(22) 0.058(4) 0.051(4) 0.057(4) 0.011(4) 0.012(4) 0.005(3) C(23) 0.039(3) 0.041(3) 0.035(3) 0.004(3) 0.012(3) 0.009(3) C(24) 0.060(4) 0.060(4) 0.039(4) -0.011(4) 0.008(3) 0.004(3) C(25) 0.058(4) 0.066(5) 0.063(5) -0.021(4) 0.008(4) 0.001(4) C(26) 0.058(5) 0.059(5) 0.082(6) -0.001(4) 0.035(4) 0.029(4) C(27) 0.068(5) 0.056(4) 0.057(4) 0.009(4) 0.034(4) 0.017(4) C(28) 0.059(4) 0.038(3) 0.038(3) 0.003(3) 0.018(3) 0.004(3) C(29) 0.036(3) 0.041(3) 0.041(3) 0.002(3) 0.010(3) -0.002(3) C(30) 0.053(4) 0.045(4) 0.048(4) 0.001(3) 0.007(3) -0.003(3) C(31) 0.071(5) 0.077(5) 0.042(4) 0.003(4) 0.015(4) 0.009(4) C(32) 0.067(5) 0.084(6) 0.048(4) -0.011(4) 0.014(4) -0.019(4) C(33) 0.066(5) 0.063(5) 0.062(5) -0.015(4) 0.020(4) -0.028(4) C(34) 0.064(5) 0.052(4) 0.053(4) -0.019(3) 0.022(4) -0.014(3) C(35) 0.044(4) 0.074(5) 0.048(4) 0.023(4) 0.007(3) -0.001(4) C(36) 0.065(6) 0.21(1) 0.056(5) 0.053(7) 0.012(4) -0.025(6) C(37) 0.067(6) 0.35(2) 0.065(6) 0.079(9) 0.009(5) -0.021(9) C(38) 0.090(7) 0.27(2) 0.090(7) 0.108(9) 0.015(6) -0.002(9) C(39) 0.098(7) 0.142(9) 0.060(5) 0.065(6) 0.031(5) 0.001(5) C(40) 0.063(5) 0.078(5) 0.047(4) 0.023(4) 0.017(3) 0.004(4) C(41) 0.044(4) 0.035(3) 0.038(3) 0.006(3) 0.011(3) 0.001(3) C(42) 0.045(4) 0.046(4) 0.065(4) 0.005(3) 0.020(3) 0.003(3) C(43) 0.046(4) 0.063(5) 0.079(5) 0.021(4) 0.013(4) 0.012(4) C(44) 0.081(6) 0.068(5) 0.061(5) 0.021(5) 0.020(4) 0.019(4) C(45) 0.076(6) 0.069(5) 0.080(6) 0.004(4) 0.036(5) 0.026(4) C(46) 0.049(4) 0.057(4) 0.055(4) 0.007(3) 0.019(3) 0.007(3) C(47) 0.045(3) 0.048(4) 0.037(3) 0.006(3) 0.008(3) 0.002(3) C(48) 0.085(6) 0.048(4) 0.066(5) 0.001(4) 0.030(4) -0.008(4) C(49) 0.083(6) 0.082(6) 0.053(4) 0.011(5) 0.033(4) -0.004(4) C(50) 0.055(4) 0.078(5) 0.041(4) 0.004(4) 0.016(3) 0.001(4) C(51) 0.067(5) 0.053(4) 0.060(4) -0.015(4) 0.021(4) 0.003(4) C(52) 0.067(5) 0.047(4) 0.055(4) -0.002(4) 0.025(4) -0.004(3) C(53) 0.041(4) 0.036(3) 0.049(4) -0.001(3) 0.016(3) 0.004(3) C(54) 0.059(4) 0.043(4) 0.060(4) 0.002(3) 0.016(4) 0.004(3) C(55) 0.064(5) 0.065(5) 0.068(5) 0.024(4) 0.023(4) 0.016(4) C(56) 0.094(6) 0.051(4) 0.073(5) 0.025(4) 0.043(5) 0.010(4) C(57) 0.088(6) 0.046(4) 0.060(5) 0.000(4) 0.037(4) -0.007(3) C(58) 0.056(4) 0.055(4) 0.048(4) -0.005(3) 0.022(3) -0.007(3) C(59) 0.040(3) 0.043(4) 0.043(3) -0.002(3) 0.002(3) -0.002(3) C(60) 0.047(4) 0.056(4) 0.064(4) -0.006(4) 0.008(3) -0.007(4) C(61) 0.047(4) 0.076(5) 0.086(6) 0.004(4) -0.018(4) 0.000(5) C(62) 0.085(6) 0.091(6) 0.051(5) 0.011(5) -0.005(4) 0.010(4) C(63) 0.083(6) 0.119(7) 0.054(5) 0.010(5) 0.014(4) 0.020(5) C(64) 0.056(4) 0.078(5) 0.049(4) 0.004(4) 0.008(3) 0.012(4) C(65) 0.095(8) 0.071(6) 0.092(7) -0.017(6) 0.012(6) -0.005(6) C(66) 0.142(9) 0.085(7) 0.100(7) 0.019(7) -0.005(7) -0.012(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) P(4) 2.216(1) . . yes Pt(1) P(5) 2.222(1) . . yes Pt(1) O(1) 2.084(3) . . yes Pt(1) O(2) 2.101(4) . . yes Cl(1) Cl(2) 1.0266(1) . 3_555 yes Cl(1) C(67) 1.8279(3) . . yes Cl(2) Cl(2) 2.0785(4) . 3_555 yes Cl(2) C(67) 1.8325(2) . . yes Cl(2) C(67) 1.9132(1) . 3_555 yes P(1) O(1) 1.512(4) . . yes P(1) O(4) 1.465(4) . . yes P(1) O(5) 1.609(4) . . yes P(1) O(9) 1.603(4) . . yes P(2) O(2) 1.515(4) . . yes P(2) O(5) 1.613(4) . . yes P(2) O(6) 1.457(4) . . yes P(2) O(7) 1.604(4) . . yes P(3) O(3) 1.471(4) . . yes P(3) O(7) 1.621(4) . . yes P(3) O(8) 1.465(4) . . yes P(3) O(9) 1.627(4) . . yes P(4) C(1) 1.802(6) . . yes P(4) C(7) 1.811(6) . . yes P(4) C(13) 1.817(6) . . yes P(5) C(16) 1.838(6) . . yes P(5) C(17) 1.827(6) . . yes P(5) C(23) 1.807(5) . . yes P(6) N(1) 1.570(5) . . yes P(6) C(29) 1.785(6) . . yes P(6) C(35) 1.797(6) . . yes P(6) C(41) 1.799(6) . . yes P(7) N(1) 1.568(5) . . yes P(7) C(47) 1.800(6) . . yes P(7) C(53) 1.801(6) . . yes P(7) C(59) 1.791(6) . . yes N(2) C(65) 1.11(1) . . yes C(1) C(2) 1.385(8) . . yes C(1) C(6) 1.380(8) . . yes C(2) C(3) 1.393(9) . . yes C(3) C(4) 1.37(1) . . yes C(4) C(5) 1.36(1) . . yes C(5) C(6) 1.377(9) . . yes C(7) C(8) 1.387(9) . . yes C(7) C(12) 1.381(9) . . yes C(8) C(9) 1.405(10) . . yes C(9) C(10) 1.40(1) . . yes C(10) C(11) 1.34(1) . . yes C(11) C(12) 1.381(10) . . yes C(13) C(14) 1.527(9) . . yes C(14) C(15) 1.502(9) . . yes C(15) C(16) 1.532(8) . . yes C(17) C(18) 1.395(8) . . yes C(17) C(22) 1.372(8) . . yes C(18) C(19) 1.395(9) . . yes C(19) C(20) 1.36(1) . . yes C(20) C(21) 1.37(1) . . yes C(21) C(22) 1.397(9) . . yes C(23) C(24) 1.389(8) . . yes C(23) C(28) 1.393(7) . . yes C(24) C(25) 1.380(9) . . yes C(25) C(26) 1.393(9) . . yes C(26) C(27) 1.365(9) . . yes C(27) C(28) 1.390(8) . . yes C(29) C(30) 1.373(8) . . yes C(29) C(34) 1.394(8) . . yes C(30) C(31) 1.384(9) . . yes C(31) C(32) 1.364(10) . . yes C(32) C(33) 1.366(10) . . yes C(33) C(34) 1.375(8) . . yes C(35) C(36) 1.356(9) . . yes C(35) C(40) 1.376(8) . . yes C(36) C(37) 1.36(1) . . yes C(37) C(38) 1.37(1) . . yes C(38) C(39) 1.37(1) . . yes C(39) C(40) 1.370(9) . . yes C(41) C(42) 1.393(8) . . yes C(41) C(46) 1.386(8) . . yes C(42) C(43) 1.373(8) . . yes C(43) C(44) 1.365(9) . . yes C(44) C(45) 1.365(10) . . yes C(45) C(46) 1.381(9) . . yes C(47) C(48) 1.382(8) . . yes C(47) C(52) 1.394(8) . . yes C(48) C(49) 1.390(9) . . yes C(49) C(50) 1.358(10) . . yes C(50) C(51) 1.362(9) . . yes C(51) C(52) 1.371(8) . . yes C(53) C(54) 1.375(8) . . yes C(53) C(58) 1.380(8) . . yes C(54) C(55) 1.387(9) . . yes C(55) C(56) 1.368(10) . . yes C(56) C(57) 1.372(10) . . yes C(57) C(58) 1.383(9) . . yes C(59) C(60) 1.380(8) . . yes C(59) C(64) 1.379(8) . . yes C(60) C(61) 1.390(9) . . yes C(61) C(62) 1.34(1) . . yes C(62) C(63) 1.37(1) . . yes C(63) C(64) 1.375(9) . . yes C(65) C(66) 1.46(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(4) Pt(1) P(5) 93.74(5) . . . yes P(4) Pt(1) O(1) 171.0(1) . . . yes P(4) Pt(1) O(2) 87.2(1) . . . yes P(5) Pt(1) O(1) 90.1(1) . . . yes P(5) Pt(1) O(2) 177.7(1) . . . yes O(1) Pt(1) O(2) 88.7(1) . . . yes Cl(2) Cl(1) C(67) 78.71(1) 3_555 . . yes Cl(1) Cl(2) Cl(2) 122.788(8) 3_555 . 3_555 yes Cl(1) Cl(2) C(67) 168.304(1) 3_555 . . yes Cl(1) Cl(2) C(67) 69.54(1) 3_555 . 3_555 yes Cl(2) Cl(2) C(67) 58.168(8) 3_555 . . yes Cl(2) Cl(2) C(67) 54.464(2) 3_555 . 3_555 yes C(67) Cl(2) C(67) 112.632(10) . . 3_555 yes O(1) P(1) O(4) 117.2(2) . . . yes O(1) P(1) O(5) 107.3(2) . . . yes O(1) P(1) O(9) 109.7(2) . . . yes O(4) P(1) O(5) 110.6(2) . . . yes O(4) P(1) O(9) 110.0(2) . . . yes O(5) P(1) O(9) 100.7(2) . . . yes O(2) P(2) O(5) 106.6(2) . . . yes O(2) P(2) O(6) 117.3(2) . . . yes O(2) P(2) O(7) 110.1(2) . . . yes O(5) P(2) O(6) 110.7(2) . . . yes O(5) P(2) O(7) 101.0(2) . . . yes O(6) P(2) O(7) 109.9(2) . . . yes O(3) P(3) O(7) 108.9(2) . . . yes O(3) P(3) O(8) 121.6(3) . . . yes O(3) P(3) O(9) 108.8(2) . . . yes O(7) P(3) O(8) 107.4(2) . . . yes O(7) P(3) O(9) 100.1(2) . . . yes O(8) P(3) O(9) 107.8(3) . . . yes Pt(1) P(4) C(1) 114.8(2) . . . yes Pt(1) P(4) C(7) 108.3(2) . . . yes Pt(1) P(4) C(13) 119.7(2) . . . yes C(1) P(4) C(7) 105.9(3) . . . yes C(1) P(4) C(13) 101.8(3) . . . yes C(7) P(4) C(13) 105.1(3) . . . yes Pt(1) P(5) C(16) 116.9(2) . . . yes Pt(1) P(5) C(17) 112.8(2) . . . yes Pt(1) P(5) C(23) 110.1(2) . . . yes C(16) P(5) C(17) 100.7(3) . . . yes C(16) P(5) C(23) 110.5(3) . . . yes C(17) P(5) C(23) 104.9(3) . . . yes N(1) P(6) C(29) 107.1(3) . . . yes N(1) P(6) C(35) 112.8(3) . . . yes N(1) P(6) C(41) 112.6(3) . . . yes C(29) P(6) C(35) 106.7(3) . . . yes C(29) P(6) C(41) 108.3(3) . . . yes C(35) P(6) C(41) 109.0(3) . . . yes N(1) P(7) C(47) 106.8(3) . . . yes N(1) P(7) C(53) 113.2(3) . . . yes N(1) P(7) C(59) 114.7(3) . . . yes C(47) P(7) C(53) 109.3(3) . . . yes C(47) P(7) C(59) 107.4(3) . . . yes C(53) P(7) C(59) 105.2(3) . . . yes Pt(1) O(1) P(1) 129.9(2) . . . yes Pt(1) O(2) P(2) 127.7(2) . . . yes P(1) O(5) P(2) 123.0(2) . . . yes P(2) O(7) P(3) 130.5(3) . . . yes P(1) O(9) P(3) 128.2(2) . . . yes P(6) N(1) P(7) 146.6(4) . . . yes P(4) C(1) C(2) 120.6(4) . . . yes P(4) C(1) C(6) 120.5(5) . . . yes C(2) C(1) C(6) 118.7(6) . . . yes C(1) C(2) C(3) 120.0(6) . . . yes C(2) C(3) C(4) 119.6(7) . . . yes C(3) C(4) C(5) 120.9(7) . . . yes C(4) C(5) C(6) 119.8(7) . . . yes C(1) C(6) C(5) 121.0(7) . . . yes P(4) C(7) C(8) 118.7(5) . . . yes P(4) C(7) C(12) 121.4(5) . . . yes C(8) C(7) C(12) 119.8(6) . . . yes C(7) C(8) C(9) 119.1(7) . . . yes C(8) C(9) C(10) 120.0(7) . . . yes C(9) C(10) C(11) 119.2(7) . . . yes C(10) C(11) C(12) 121.8(8) . . . yes C(7) C(12) C(11) 120.0(7) . . . yes P(4) C(13) C(14) 113.5(4) . . . yes C(13) C(14) C(15) 115.6(5) . . . yes C(14) C(15) C(16) 115.4(5) . . . yes P(5) C(16) C(15) 116.6(4) . . . yes P(5) C(17) C(18) 117.7(5) . . . yes P(5) C(17) C(22) 122.7(5) . . . yes C(18) C(17) C(22) 119.4(6) . . . yes C(17) C(18) C(19) 119.8(6) . . . yes C(18) C(19) C(20) 120.2(7) . . . yes C(19) C(20) C(21) 120.4(7) . . . yes C(20) C(21) C(22) 120.2(7) . . . yes C(17) C(22) C(21) 120.0(6) . . . yes P(5) C(23) C(24) 116.8(4) . . . yes P(5) C(23) C(28) 125.2(5) . . . yes C(24) C(23) C(28) 118.1(5) . . . yes C(23) C(24) C(25) 121.3(6) . . . yes C(24) C(25) C(26) 119.3(6) . . . yes C(25) C(26) C(27) 120.5(6) . . . yes C(26) C(27) C(28) 119.8(6) . . . yes C(23) C(28) C(27) 121.0(6) . . . yes P(6) C(29) C(30) 121.4(5) . . . yes P(6) C(29) C(34) 119.8(5) . . . yes C(30) C(29) C(34) 118.7(6) . . . yes C(29) C(30) C(31) 120.6(6) . . . yes C(30) C(31) C(32) 119.7(6) . . . yes C(31) C(32) C(33) 120.7(6) . . . yes C(32) C(33) C(34) 119.9(6) . . . yes C(29) C(34) C(33) 120.3(6) . . . yes P(6) C(35) C(36) 120.7(5) . . . yes P(6) C(35) C(40) 119.0(5) . . . yes C(36) C(35) C(40) 119.3(6) . . . yes C(35) C(36) C(37) 121.7(7) . . . yes C(36) C(37) C(38) 117.7(8) . . . yes C(37) C(38) C(39) 122.2(8) . . . yes C(38) C(39) C(40) 118.0(7) . . . yes C(35) C(40) C(39) 120.7(7) . . . yes P(6) C(41) C(42) 118.6(5) . . . yes P(6) C(41) C(46) 122.6(5) . . . yes C(42) C(41) C(46) 118.7(5) . . . yes C(41) C(42) C(43) 121.2(6) . . . yes C(42) C(43) C(44) 119.5(6) . . . yes C(43) C(44) C(45) 119.9(7) . . . yes C(44) C(45) C(46) 121.7(7) . . . yes C(41) C(46) C(45) 118.9(6) . . . yes P(7) C(47) C(48) 119.8(5) . . . yes P(7) C(47) C(52) 122.1(5) . . . yes C(48) C(47) C(52) 118.0(6) . . . yes C(47) C(48) C(49) 120.4(6) . . . yes C(48) C(49) C(50) 120.8(6) . . . yes C(49) C(50) C(51) 119.1(6) . . . yes C(50) C(51) C(52) 121.6(6) . . . yes C(47) C(52) C(51) 120.0(6) . . . yes P(7) C(53) C(54) 119.9(5) . . . yes P(7) C(53) C(58) 120.9(5) . . . yes C(54) C(53) C(58) 119.3(6) . . . yes C(53) C(54) C(55) 119.8(6) . . . yes C(54) C(55) C(56) 120.5(7) . . . yes C(55) C(56) C(57) 120.1(6) . . . yes C(56) C(57) C(58) 119.5(7) . . . yes C(53) C(58) C(57) 120.8(6) . . . yes P(7) C(59) C(60) 121.8(5) . . . yes P(7) C(59) C(64) 119.9(5) . . . yes C(60) C(59) C(64) 118.2(6) . . . yes C(59) C(60) C(61) 120.4(7) . . . yes C(60) C(61) C(62) 120.3(7) . . . yes C(61) C(62) C(63) 120.3(7) . . . yes C(62) C(63) C(64) 120.1(8) . . . yes C(59) C(64) C(63) 120.7(7) . . . yes N(2) C(65) C(66) 178(1) . . . yes Cl(1) C(67) Cl(2) 98.46(1) . . . yes Cl(1) C(67) Cl(2) 31.749(1) . . 3_555 yes Cl(2) C(67) Cl(2) 67.368(10) . . 3_555 yes #------------------------------------------------------------------------------ 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 Pt(1) P(4) C(1) C(2) 24.6(5) . . . . yes Pt(1) P(4) C(1) C(6) -160.1(4) . . . . yes Pt(1) P(4) C(7) C(8) 76.8(5) . . . . yes Pt(1) P(4) C(7) C(12) -98.8(5) . . . . yes Pt(1) P(4) C(13) C(14) -68.3(5) . . . . yes Pt(1) P(5) C(16) C(15) -4.0(5) . . . . yes Pt(1) P(5) C(17) C(18) -51.4(5) . . . . yes Pt(1) P(5) C(17) C(22) 133.9(5) . . . . yes Pt(1) P(5) C(23) C(24) -49.8(5) . . . . yes Pt(1) P(5) C(23) C(28) 129.0(5) . . . . yes Pt(1) O(1) P(1) O(4) 169.3(3) . . . . yes Pt(1) O(1) P(1) O(5) 44.3(3) . . . . yes Pt(1) O(1) P(1) O(9) -64.3(3) . . . . yes Pt(1) O(2) P(2) O(5) -50.0(3) . . . . yes Pt(1) O(2) P(2) O(6) -174.7(3) . . . . yes Pt(1) O(2) P(2) O(7) 58.7(3) . . . . yes Cl(1) Cl(2) Cl(2) Cl(1) -180.0 . 3_555 . 3_555 yes Cl(1) Cl(2) Cl(2) C(67) -13.8019(1) . 3_555 . . yes Cl(1) Cl(2) Cl(2) C(67) 166.1981(1) . 3_555 . 3_555 yes Cl(1) Cl(2) C(67) Cl(2) 167.639(2) . 3_555 . . yes Cl(1) Cl(2) C(67) Cl(2) -98.366(4) . 3_555 3_555 . yes Cl(1) C(67) Cl(2) Cl(2) 6.5390(7) . . . 3_555 yes Cl(1) C(67) Cl(2) C(67) 6.5390(7) . . . 3_555 yes Cl(1) C(67) Cl(2) Cl(2) -167.639(2) . . 3_555 . yes Cl(1) C(67) Cl(2) C(67) -167.639(2) . . 3_555 3_555 yes Cl(2) Cl(2) Cl(1) C(67) 11.959(1) . 3_555 . . yes Cl(2) C(67) Cl(2) C(67) 0.0 . . 3_555 3_555 yes Cl(2) C(67) Cl(2) C(67) 0.0 . 3_555 3_555 . yes P(1) O(1) Pt(1) P(4) -94.1(7) . . . . yes P(1) O(1) Pt(1) P(5) 150.9(3) . . . . yes P(1) O(1) Pt(1) O(2) -31.1(3) . . . . yes P(1) O(5) P(2) O(2) 61.9(3) . . . . yes P(1) O(5) P(2) O(6) -169.4(3) . . . . yes P(1) O(5) P(2) O(7) -53.1(3) . . . . yes P(1) O(9) P(3) O(3) -72.6(4) . . . . yes P(1) O(9) P(3) O(7) 41.6(3) . . . . yes P(1) O(9) P(3) O(8) 153.7(3) . . . . yes P(2) O(2) Pt(1) P(4) -154.0(3) . . . . yes P(2) O(2) Pt(1) P(5) 91(2) . . . . yes P(2) O(2) Pt(1) O(1) 34.0(3) . . . . yes P(2) O(5) P(1) O(1) -58.8(3) . . . . yes P(2) O(5) P(1) O(4) 172.3(3) . . . . yes P(2) O(5) P(1) O(9) 56.0(3) . . . . yes P(2) O(7) P(3) O(3) 75.6(4) . . . . yes P(2) O(7) P(3) O(8) -150.9(3) . . . . yes P(2) O(7) P(3) O(9) -38.5(4) . . . . yes P(3) O(7) P(2) O(2) -67.9(4) . . . . yes P(3) O(7) P(2) O(5) 44.5(4) . . . . yes P(3) O(7) P(2) O(6) 161.5(3) . . . . yes P(3) O(9) P(1) O(1) 62.4(4) . . . . yes P(3) O(9) P(1) O(4) -167.3(3) . . . . yes P(3) O(9) P(1) O(5) -50.6(3) . . . . yes P(4) Pt(1) P(5) C(16) 55.4(2) . . . . yes P(4) Pt(1) P(5) C(17) 171.4(2) . . . . yes P(4) Pt(1) P(5) C(23) -71.8(2) . . . . yes P(4) C(1) C(2) C(3) 175.6(5) . . . . yes P(4) C(1) C(6) C(5) -174.7(6) . . . . yes P(4) C(7) C(8) C(9) -178.4(5) . . . . yes P(4) C(7) C(12) C(11) 178.0(6) . . . . yes P(4) C(13) C(14) C(15) 60.5(7) . . . . yes P(5) Pt(1) P(4) C(1) -136.2(2) . . . . yes P(5) Pt(1) P(4) C(7) 105.7(2) . . . . yes P(5) Pt(1) P(4) C(13) -14.6(3) . . . . yes P(5) C(16) C(15) C(14) -85.6(6) . . . . yes P(5) C(17) C(18) C(19) -175.3(5) . . . . yes P(5) C(17) C(22) C(21) 174.5(5) . . . . yes P(5) C(23) C(24) C(25) 179.9(5) . . . . yes P(5) C(23) C(28) C(27) -177.5(5) . . . . yes P(6) N(1) P(7) C(47) -158.5(6) . . . . yes P(6) N(1) P(7) C(53) 81.1(7) . . . . yes P(6) N(1) P(7) C(59) -39.6(7) . . . . yes P(6) C(29) C(30) C(31) 178.1(5) . . . . yes P(6) C(29) C(34) C(33) -177.6(5) . . . . yes P(6) C(35) C(36) C(37) 166(1) . . . . yes P(6) C(35) C(40) C(39) -172.7(7) . . . . yes P(6) C(41) C(42) C(43) 179.4(5) . . . . yes P(6) C(41) C(46) C(45) -177.9(5) . . . . yes P(7) N(1) P(6) C(29) 169.8(6) . . . . yes P(7) N(1) P(6) C(35) -73.0(7) . . . . yes P(7) N(1) P(6) C(41) 50.9(7) . . . . yes P(7) C(47) C(48) C(49) 176.1(6) . . . . yes P(7) C(47) C(52) C(51) -177.2(5) . . . . yes P(7) C(53) C(54) C(55) 178.9(5) . . . . yes P(7) C(53) C(58) C(57) -178.5(5) . . . . yes P(7) C(59) C(60) C(61) 176.9(5) . . . . yes P(7) C(59) C(64) C(63) -176.0(6) . . . . yes O(1) Pt(1) P(4) C(1) 109.1(7) . . . . yes O(1) Pt(1) P(4) C(7) -9.0(7) . . . . yes O(1) Pt(1) P(4) C(13) -129.3(7) . . . . yes O(1) Pt(1) P(5) C(16) -132.8(2) . . . . yes O(1) Pt(1) P(5) C(17) -16.8(2) . . . . yes O(1) Pt(1) P(5) C(23) 100.0(2) . . . . yes O(2) Pt(1) P(4) C(1) 45.9(2) . . . . yes O(2) Pt(1) P(4) C(7) -72.2(2) . . . . yes O(2) Pt(1) P(4) C(13) 167.5(3) . . . . yes O(2) Pt(1) P(5) C(16) 169(2) . . . . yes O(2) Pt(1) P(5) C(17) -74(2) . . . . yes O(2) Pt(1) P(5) C(23) 42(2) . . . . yes N(1) P(6) C(29) C(30) 19.7(6) . . . . yes N(1) P(6) C(29) C(34) -163.8(5) . . . . yes N(1) P(6) C(35) C(36) -97.6(8) . . . . yes N(1) P(6) C(35) C(40) 70.5(7) . . . . yes N(1) P(6) C(41) C(42) 34.7(6) . . . . yes N(1) P(6) C(41) C(46) -147.7(5) . . . . yes N(1) P(7) C(47) C(48) 33.0(6) . . . . yes N(1) P(7) C(47) C(52) -150.2(5) . . . . yes N(1) P(7) C(53) C(54) 15.7(6) . . . . yes N(1) P(7) C(53) C(58) -165.0(5) . . . . yes N(1) P(7) C(59) C(60) -100.0(6) . . . . yes N(1) P(7) C(59) C(64) 76.7(6) . . . . yes C(1) P(4) C(7) C(8) -46.8(5) . . . . yes C(1) P(4) C(7) C(12) 137.6(5) . . . . yes C(1) P(4) C(13) C(14) 59.5(5) . . . . yes C(1) C(2) C(3) C(4) -1(1) . . . . yes C(1) C(6) C(5) C(4) 0(1) . . . . yes C(2) C(1) P(4) C(7) 144.1(5) . . . . yes C(2) C(1) P(4) C(13) -106.3(5) . . . . yes C(2) C(1) C(6) C(5) 0.6(10) . . . . yes C(2) C(3) C(4) C(5) 2(1) . . . . yes C(3) C(2) C(1) C(6) 0.2(9) . . . . yes C(3) C(4) C(5) C(6) -1(1) . . . . yes C(6) C(1) P(4) C(7) -40.6(6) . . . . yes C(6) C(1) P(4) C(13) 69.0(6) . . . . yes C(7) P(4) C(13) C(14) 169.8(4) . . . . yes C(7) C(8) C(9) C(10) 1(1) . . . . yes C(7) C(12) C(11) C(10) 0(1) . . . . yes C(8) C(7) P(4) C(13) -154.1(5) . . . . yes C(8) C(7) C(12) C(11) 2(1) . . . . yes C(8) C(9) C(10) C(11) 1(1) . . . . yes C(9) C(8) C(7) C(12) -2.7(10) . . . . yes C(9) C(10) C(11) C(12) -1(1) . . . . yes C(12) C(7) P(4) C(13) 30.3(6) . . . . yes C(13) C(14) C(15) C(16) 45.6(8) . . . . yes C(15) C(16) P(5) C(17) -126.5(5) . . . . yes C(15) C(16) P(5) C(23) 123.0(5) . . . . yes C(16) P(5) C(17) C(18) 73.9(5) . . . . yes C(16) P(5) C(17) C(22) -100.8(5) . . . . yes C(16) P(5) C(23) C(24) 179.6(5) . . . . yes C(16) P(5) C(23) C(28) -1.6(6) . . . . yes C(17) P(5) C(23) C(24) 71.8(5) . . . . yes C(17) P(5) C(23) C(28) -109.4(5) . . . . yes C(17) C(18) C(19) C(20) 0(1) . . . . yes C(17) C(22) C(21) C(20) 0(1) . . . . yes C(18) C(17) P(5) C(23) -171.3(4) . . . . yes C(18) C(17) C(22) C(21) -0.1(9) . . . . yes C(18) C(19) C(20) C(21) 0(1) . . . . yes C(19) C(18) C(17) C(22) -0.4(9) . . . . yes C(19) C(20) C(21) C(22) -1(1) . . . . yes C(22) C(17) P(5) C(23) 14.0(6) . . . . yes C(23) C(24) C(25) C(26) -2(1) . . . . yes C(23) C(28) C(27) C(26) -1.7(10) . . . . yes C(24) C(23) C(28) C(27) 1.3(9) . . . . yes C(24) C(25) C(26) C(27) 2(1) . . . . yes C(25) C(24) C(23) C(28) 1.0(10) . . . . yes C(25) C(26) C(27) C(28) 0(1) . . . . yes C(29) P(6) C(35) C(36) 19.8(9) . . . . yes C(29) P(6) C(35) C(40) -172.1(6) . . . . yes C(29) P(6) C(41) C(42) -83.6(5) . . . . yes C(29) P(6) C(41) C(46) 94.1(5) . . . . yes C(29) C(30) C(31) C(32) -2(1) . . . . yes C(29) C(34) C(33) C(32) 1(1) . . . . yes C(30) C(29) P(6) C(35) -101.4(5) . . . . yes C(30) C(29) P(6) C(41) 141.4(5) . . . . yes C(30) C(29) C(34) C(33) -0.9(10) . . . . yes C(30) C(31) C(32) C(33) 2(1) . . . . yes C(31) C(30) C(29) C(34) 1.5(10) . . . . yes C(31) C(32) C(33) C(34) -1(1) . . . . yes C(34) C(29) P(6) C(35) 75.1(6) . . . . yes C(34) C(29) P(6) C(41) -42.1(6) . . . . yes C(35) P(6) C(41) C(42) 160.7(5) . . . . yes C(35) P(6) C(41) C(46) -21.7(6) . . . . yes C(35) C(36) C(37) C(38) 4(2) . . . . yes C(35) C(40) C(39) C(38) 7(1) . . . . yes C(36) C(35) P(6) C(41) 136.5(8) . . . . yes C(36) C(35) C(40) C(39) -4(1) . . . . yes C(36) C(37) C(38) C(39) -1(2) . . . . yes C(37) C(36) C(35) C(40) -1(1) . . . . yes C(37) C(38) C(39) C(40) -4(2) . . . . yes C(40) C(35) P(6) C(41) -55.4(7) . . . . yes C(41) C(42) C(43) C(44) 0(1) . . . . yes C(41) C(46) C(45) C(44) -2(1) . . . . yes C(42) C(41) C(46) C(45) -0.2(10) . . . . yes C(42) C(43) C(44) C(45) -1(1) . . . . yes C(43) C(42) C(41) C(46) 1.7(10) . . . . yes C(43) C(44) C(45) C(46) 3(1) . . . . yes C(47) P(7) C(53) C(54) -103.3(5) . . . . yes C(47) P(7) C(53) C(58) 76.1(5) . . . . yes C(47) P(7) C(59) C(60) 18.6(6) . . . . yes C(47) P(7) C(59) C(64) -164.7(5) . . . . yes C(47) C(48) C(49) C(50) 1(1) . . . . yes C(47) C(52) C(51) C(50) 0(1) . . . . yes C(48) C(47) P(7) C(53) 155.9(5) . . . . yes C(48) C(47) P(7) C(59) -90.5(6) . . . . yes C(48) C(47) C(52) C(51) -0.4(10) . . . . yes C(48) C(49) C(50) C(51) 0(1) . . . . yes C(49) C(48) C(47) C(52) 0(1) . . . . yes C(49) C(50) C(51) C(52) 0(1) . . . . yes C(52) C(47) P(7) C(53) -27.4(6) . . . . yes C(52) C(47) P(7) C(59) 86.3(6) . . . . yes C(53) P(7) C(59) C(60) 135.0(5) . . . . yes C(53) P(7) C(59) C(64) -48.4(6) . . . . yes C(53) C(54) C(55) C(56) 0(1) . . . . yes C(53) C(58) C(57) C(56) -1(1) . . . . yes C(54) C(53) P(7) C(59) 141.6(5) . . . . yes C(54) C(53) C(58) C(57) 0.8(9) . . . . yes C(54) C(55) C(56) C(57) -1(1) . . . . yes C(55) C(54) C(53) C(58) -0.4(9) . . . . yes C(55) C(56) C(57) C(58) 1(1) . . . . yes C(58) C(53) P(7) C(59) -39.1(6) . . . . yes C(59) C(60) C(61) C(62) -1(1) . . . . yes C(59) C(64) C(63) C(62) 0(1) . . . . yes C(60) C(59) C(64) C(63) 0(1) . . . . yes C(60) C(61) C(62) C(63) 1(1) . . . . yes C(61) C(60) C(59) C(64) 0(1) . . . . yes C(61) C(62) C(63) C(64) 0(1) . . . . yes C(67) Cl(2) Cl(2) C(67) 180.0 . . 3_555 3_555 yes C(67) Cl(2) C(67) Cl(2) 0.0 . . 3_555 3_555 yes C(67) Cl(2) Cl(2) C(67) 180.0 . 3_555 . 3_555 yes C(67) Cl(2) C(67) Cl(2) 0.0 . 3_555 3_555 . yes C(67) Cl(2) C(67) Cl(2) 0.0 . 3_555 3_555 . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(38) 3.02(1) . 4_545 ? Cl(1) O(4) 3.135(4) . . ? Cl(1) C(37) 3.20(1) . 4_545 ? Cl(1) C(39) 3.23(1) . 4_545 ? Cl(1) C(36) 3.50(1) . 4_545 ? Cl(2) O(4) 3.180(5) . 3_555 ? Cl(2) O(5) 3.523(4) . 3_555 ? O(1) C(66) 3.59(1) . 1_565 ? O(3) C(33) 3.202(7) . . ? O(3) C(61) 3.295(8) . 3_444 ? O(4) C(66) 3.27(1) . 1_565 ? O(4) C(46) 3.274(8) . 4_545 ? O(4) C(45) 3.337(9) . 4_545 ? O(4) C(14) 3.491(7) . 4_545 ? O(5) C(67) 3.028(4) . 3_555 ? O(5) C(13) 3.523(6) . 4_545 ? O(6) C(38) 3.169(10) . 2_554 ? O(6) C(37) 3.41(1) . 2_554 ? O(6) C(26) 3.418(8) . 2_544 ? O(7) C(28) 3.539(7) . 4_545 ? O(8) C(50) 3.246(8) . 2_454 ? O(8) C(56) 3.388(8) . 4_535 ? O(8) C(28) 3.576(8) . 4_545 ? N(2) C(63) 3.53(1) . 4_535 ? N(2) C(64) 3.53(1) . 4_535 ? C(11) C(39) 3.52(1) . 3_544 ? C(16) C(50) 3.563(9) . 3_444 ? C(21) C(65) 3.47(1) . 1_565 ? C(26) C(26) 3.60(1) . 3_554 ? C(32) C(57) 3.580(10) . 4_535 ? C(37) C(67) 3.21(1) . 4_544 ? C(38) C(67) 2.91(1) . 4_544 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_(PPN)2[PtMe3(P3O9)](7) _database_code_CSD 202879 _audit_creation_date 'Mon Apr 7 14:43:48 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C75 H69 N2 O9 P7 Pt ' _chemical_formula_moiety ? _chemical_formula_weight 1554.28 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _cell_length_a 29.960(8) _cell_length_b 13.177(9) _cell_length_c 21.038(7) _cell_angle_alpha 90 _cell_angle_beta 122.45(2) _cell_angle_gamma 90 _cell_volume 7008(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.7 _cell_measurement_theta_max 19.5 _cell_measurement_temperature 294.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.212 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 8564 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9987 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.48 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8050 _reflns_number_gt 5695 _reflns_threshold_criterion F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0918 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8050 _refine_ls_number_parameters 849 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0236 _refine_diff_density_max 0.74 _refine_diff_density_min -1.07 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00051(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.43(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt Pt -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt -0.0073(4) 0.80698(3) -0.0060(6) 0.0737(1) Uani 1.00 d . . . P(1) P -0.1112(5) 0.7758(2) 0.0027(6) 0.0586(6) Uani 1.00 d . . . P(2) P -0.0220(4) 0.6506(1) 0.1004(6) 0.0421(5) Uani 1.00 d . . . P(3) P -0.0201(5) 0.8607(2) 0.1338(6) 0.0598(6) Uani 1.00 d . . . P(4) P 0.1307(4) 0.6314(2) 0.4172(6) 0.0408(5) Uani 1.00 d . . . P(5) P 0.1994(5) 0.6668(1) 0.5843(6) 0.0373(5) Uani 1.00 d . . . P(6) P 0.2767(5) 0.8372(1) -0.0665(6) 0.0383(5) Uani 1.00 d . . . P(7) P 0.3392(4) 0.8621(1) 0.1021(6) 0.0372(5) Uani 1.00 d . . . O(1) O -0.0918(5) 0.8010(5) -0.0476(8) 0.073(2) Uani 1.00 d . . . O(2) O 0.0040(5) 0.6656(5) 0.0563(7) 0.057(2) Uani 1.00 d . . . O(3) O 0.0061(5) 0.8920(5) 0.0941(7) 0.070(2) Uani 1.00 d . . . O(4) O -0.1681(5) 0.7738(5) -0.0299(7) 0.081(2) Uani 1.00 d . . . O(5) O -0.0844(5) 0.6700(4) 0.0447(7) 0.048(1) Uani 1.00 d . . . O(6) O -0.0127(5) 0.5553(4) 0.1412(7) 0.055(2) Uani 1.00 d . . . O(7) O -0.0067(5) 0.7443(4) 0.1570(7) 0.046(1) Uani 1.00 d . . . O(8) O -0.0102(5) 0.9194(5) 0.1997(7) 0.086(2) Uani 1.00 d . . . O(9) O -0.0836(5) 0.8532(4) 0.0731(7) 0.059(1) Uani 1.00 d . . . N(1) N 0.1788(5) 0.6334(5) 0.5010(7) 0.050(2) Uani 1.00 d . . . N(2) N 0.2942(5) 0.8679(5) 0.0156(7) 0.046(2) Uani 1.00 d . . . C(1) C -0.0195(7) 0.721(1) -0.0948(9) 0.104(4) Uani 1.00 d . . . C(2) C -0.0191(7) 0.938(1) -0.062(1) 0.145(5) Uani 1.00 d . . . C(3) C 0.0697(7) 0.8115(9) 0.0313(10) 0.089(4) Uani 1.00 d . . . C(4) C 0.1508(5) 0.6920(6) 0.3592(7) 0.041(2) Uani 1.00 d . . . C(5) C 0.1161(5) 0.6916(7) 0.2809(8) 0.062(2) Uani 1.00 d . . . C(6) C 0.1301(6) 0.7430(8) 0.2373(8) 0.069(3) Uani 1.00 d . . . C(7) C 0.1788(6) 0.7924(8) 0.2710(8) 0.070(3) Uani 1.00 d . . . C(8) C 0.2122(6) 0.7895(8) 0.3468(8) 0.069(3) Uani 1.00 d . . . C(9) C 0.1983(5) 0.7416(7) 0.3909(8) 0.057(2) Uani 1.00 d . . . C(10) C 0.0719(6) 0.6943(7) 0.4004(8) 0.048(2) Uani 1.00 d . . . C(11) C 0.0525(6) 0.7813(7) 0.3596(8) 0.065(3) Uani 1.00 d . . . C(12) C 0.0103(6) 0.8332(8) 0.3577(10) 0.078(4) Uani 1.00 d . . . C(13) C -0.0117(6) 0.7941(9) 0.3940(9) 0.085(3) Uani 1.00 d . . . C(14) C 0.0068(5) 0.7056(9) 0.4335(8) 0.074(3) Uani 1.00 d . . . C(15) C 0.0482(5) 0.6546(7) 0.4370(8) 0.061(3) Uani 1.00 d . . . C(16) C 0.1125(5) 0.5019(6) 0.3885(7) 0.045(2) Uani 1.00 d . . . C(17) C 0.0650(5) 0.4789(6) 0.3207(8) 0.055(2) Uani 1.00 d . . . C(18) C 0.0520(5) 0.3789(7) 0.2999(8) 0.062(2) Uani 1.00 d . . . C(19) C 0.0844(6) 0.3003(7) 0.3452(9) 0.072(3) Uani 1.00 d . . . C(20) C 0.1295(6) 0.3237(7) 0.4107(8) 0.067(2) Uani 1.00 d . . . C(21) C 0.1441(5) 0.4226(6) 0.4325(8) 0.055(2) Uani 1.00 d . . . C(22) C 0.1578(5) 0.6266(6) 0.6174(7) 0.041(2) Uani 1.00 d . . . C(23) C 0.1398(6) 0.5274(7) 0.6038(8) 0.059(2) Uani 1.00 d . . . C(24) C 0.1032(6) 0.4969(7) 0.6211(9) 0.069(3) Uani 1.00 d . . . C(25) C 0.0871(5) 0.5635(8) 0.6559(8) 0.071(3) Uani 1.00 d . . . C(26) C 0.1062(6) 0.6588(8) 0.6710(8) 0.072(3) Uani 1.00 d . . . C(27) C 0.1414(6) 0.6934(7) 0.6512(8) 0.057(3) Uani 1.00 d . . . C(28) C 0.2633(5) 0.6112(6) 0.6439(7) 0.040(2) Uani 1.00 d . . . C(29) C 0.2838(5) 0.5931(7) 0.7201(7) 0.052(2) Uani 1.00 d . . . C(30) C 0.3339(6) 0.5523(8) 0.7655(8) 0.064(2) Uani 1.00 d . . . C(31) C 0.3636(5) 0.5307(8) 0.7355(8) 0.062(3) Uani 1.00 d . . . C(32) C 0.3442(6) 0.5477(7) 0.6602(8) 0.059(2) Uani 1.00 d . . . C(33) C 0.2935(5) 0.5869(6) 0.6143(8) 0.045(2) Uani 1.00 d . . . C(34) C 0.2055(5) 0.8024(6) 0.5976(8) 0.045(2) Uani 1.00 d . . . C(35) C 0.2483(5) 0.8472(6) 0.6617(8) 0.055(2) Uani 1.00 d . . . C(36) C 0.2494(6) 0.9493(7) 0.6725(9) 0.076(3) Uani 1.00 d . . . C(37) C 0.2079(7) 1.0107(7) 0.6215(9) 0.078(3) Uani 1.00 d . . . C(38) C 0.1671(7) 0.9694(9) 0.5599(9) 0.088(3) Uani 1.00 d . . . C(39) C 0.1646(6) 0.8666(9) 0.5475(8) 0.085(3) Uani 1.00 d . . . C(40) C 0.2128(5) 0.8937(6) -0.1286(8) 0.044(2) Uani 1.00 d . . . C(41) C 0.1924(6) 0.9037(7) -0.2050(8) 0.058(2) Uani 1.00 d . . . C(42) C 0.1427(6) 0.9452(8) -0.2516(8) 0.071(3) Uani 1.00 d . . . C(43) C 0.1139(6) 0.9778(8) -0.2240(9) 0.073(3) Uani 1.00 d . . . C(44) C 0.1339(6) 0.9711(8) -0.1483(9) 0.071(3) Uani 1.00 d . . . C(45) C 0.1831(5) 0.9296(7) -0.1008(8) 0.055(2) Uani 1.00 d . . . C(46) C 0.2709(5) 0.7026(6) -0.0833(8) 0.045(2) Uani 1.00 d . . . C(47) C 0.2258(5) 0.6558(6) -0.1379(8) 0.060(2) Uani 1.00 d . . . C(48) C 0.2251(6) 0.5514(7) -0.1480(9) 0.069(3) Uani 1.00 d . . . C(49) C 0.2685(6) 0.4944(7) -0.1039(9) 0.074(3) Uani 1.00 d . . . C(50) C 0.3138(7) 0.5408(7) -0.0496(8) 0.079(3) Uani 1.00 d . . . C(51) C 0.3160(6) 0.6431(8) -0.0393(8) 0.074(3) Uani 1.00 d . . . C(52) C 0.3205(5) 0.8835(6) -0.0949(7) 0.043(2) Uani 1.00 d . . . C(53) C 0.3355(6) 0.8222(6) -0.1332(8) 0.057(3) Uani 1.00 d . . . C(54) C 0.3695(6) 0.8575(8) -0.1530(8) 0.068(3) Uani 1.00 d . . . C(55) C 0.3875(6) 0.9565(8) -0.1355(8) 0.071(3) Uani 1.00 d . . . C(56) C 0.3732(6) 1.0189(7) -0.0966(8) 0.071(3) Uani 1.00 d . . . C(57) C 0.3390(6) 0.9823(6) -0.0775(8) 0.059(2) Uani 1.00 d . . . C(58) C 0.3124(5) 0.7990(6) 0.1505(7) 0.044(2) Uani 1.00 d . . . C(59) C 0.2678(6) 0.7404(9) 0.1102(8) 0.072(3) Uani 1.00 d . . . C(60) C 0.2481(6) 0.6890(9) 0.1476(9) 0.091(4) Uani 1.00 d . . . C(61) C 0.2717(6) 0.6949(8) 0.2230(9) 0.077(3) Uani 1.00 d . . . C(62) C 0.3153(6) 0.7537(9) 0.2631(8) 0.085(4) Uani 1.00 d . . . C(63) C 0.3357(6) 0.8071(8) 0.2279(8) 0.070(3) Uani 1.00 d . . . C(64) C 0.3970(5) 0.7944(6) 0.1220(8) 0.044(2) Uani 1.00 d . . . C(65) C 0.4097(5) 0.6997(7) 0.1570(8) 0.065(3) Uani 1.00 d . . . C(66) C 0.4499(6) 0.6448(8) 0.1622(9) 0.085(4) Uani 1.00 d . . . C(67) C 0.4784(7) 0.6799(9) 0.134(1) 0.085(4) Uani 1.00 d . . . C(68) C 0.4672(6) 0.7728(8) 0.1007(8) 0.071(3) Uani 1.00 d . . . C(69) C 0.4263(6) 0.8327(7) 0.0945(9) 0.053(3) Uani 1.00 d . . . C(70) C 0.3603(5) 0.9878(5) 0.1381(8) 0.043(2) Uani 1.00 d . . . C(71) C 0.3299(5) 1.0708(6) 0.0975(8) 0.053(2) Uani 1.00 d . . . C(72) C 0.3463(6) 1.1677(6) 0.1222(9) 0.070(3) Uani 1.00 d . . . C(73) C 0.3939(6) 1.1821(7) 0.1894(9) 0.072(3) Uani 1.00 d . . . C(74) C 0.4246(6) 1.1029(7) 0.2312(8) 0.062(2) Uani 1.00 d . . . C(75) C 0.4081(5) 1.0034(6) 0.2055(8) 0.053(2) Uani 1.00 d . . . H(1) H 0.0067 0.7377 -0.1056 0.1251 Uiso 1.00 calc . . . H(2) H -0.0156 0.6508 -0.0806 0.1251 Uiso 1.00 calc . . . H(3) H -0.0533 0.7332 -0.1362 0.1251 Uiso 1.00 calc . . . H(4) H -0.0530 0.9380 -0.1044 0.1744 Uiso 1.00 calc . . . H(5) H -0.0147 0.9928 -0.0289 0.1744 Uiso 1.00 calc . . . H(6) H 0.0069 0.9438 -0.0742 0.1744 Uiso 1.00 calc . . . H(7) H 0.0749 0.8426 -0.0044 0.1068 Uiso 1.00 calc . . . H(8) H 0.0888 0.8496 0.0778 0.1068 Uiso 1.00 calc . . . H(9) H 0.0841 0.7444 0.0417 0.1068 Uiso 1.00 calc . . . H(10) H 0.0841 0.6564 0.2594 0.0740 Uiso 1.00 calc . . . H(11) H 0.1072 0.7449 0.1853 0.0822 Uiso 1.00 calc . . . H(12) H 0.1892 0.8278 0.2421 0.0838 Uiso 1.00 calc . . . H(13) H 0.2465 0.8213 0.3706 0.0826 Uiso 1.00 calc . . . H(14) H 0.2224 0.7424 0.4452 0.0690 Uiso 1.00 calc . . . H(15) H 0.0678 0.8071 0.3336 0.0781 Uiso 1.00 calc . . . H(16) H -0.0018 0.8954 0.3322 0.0942 Uiso 1.00 calc . . . H(17) H -0.0397 0.8285 0.3931 0.1020 Uiso 1.00 calc . . . H(18) H -0.0084 0.6789 0.4599 0.0887 Uiso 1.00 calc . . . H(19) H 0.0613 0.5927 0.4653 0.0732 Uiso 1.00 calc . . . H(20) H 0.0429 0.5317 0.2906 0.0660 Uiso 1.00 calc . . . H(21) H 0.0208 0.3634 0.2549 0.0749 Uiso 1.00 calc . . . H(22) H 0.0757 0.2316 0.3315 0.0859 Uiso 1.00 calc . . . H(23) H 0.1523 0.2705 0.4436 0.0804 Uiso 1.00 calc . . . H(24) H 0.1771 0.4366 0.4796 0.0661 Uiso 1.00 calc . . . H(25) H 0.1531 0.4804 0.5839 0.0705 Uiso 1.00 calc . . . H(26) H 0.0898 0.4301 0.6101 0.0830 Uiso 1.00 calc . . . H(27) H 0.0635 0.5420 0.6702 0.0854 Uiso 1.00 calc . . . H(28) H 0.0962 0.7038 0.6968 0.0860 Uiso 1.00 calc . . . H(29) H 0.1543 0.7616 0.6621 0.0680 Uiso 1.00 calc . . . H(30) H 0.2639 0.6089 0.7420 0.0629 Uiso 1.00 calc . . . H(31) H 0.3482 0.5394 0.8184 0.0764 Uiso 1.00 calc . . . H(32) H 0.3989 0.5037 0.7681 0.0743 Uiso 1.00 calc . . . H(33) H 0.3659 0.5328 0.6412 0.0705 Uiso 1.00 calc . . . H(34) H 0.2801 0.5969 0.5633 0.0542 Uiso 1.00 calc . . . H(35) H 0.2774 0.8062 0.6991 0.0656 Uiso 1.00 calc . . . H(36) H 0.2799 0.9789 0.7167 0.0913 Uiso 1.00 calc . . . H(37) H 0.2092 1.0816 0.6315 0.0930 Uiso 1.00 calc . . . H(38) H 0.1398 1.0116 0.5250 0.1058 Uiso 1.00 calc . . . H(39) H 0.1352 0.8387 0.5051 0.1019 Uiso 1.00 calc . . . H(40) H 0.2132 0.8822 -0.2241 0.0701 Uiso 1.00 calc . . . H(41) H 0.1293 0.9508 -0.3030 0.0846 Uiso 1.00 calc . . . H(42) H 0.0804 1.0056 -0.2558 0.0877 Uiso 1.00 calc . . . H(43) H 0.1144 0.9950 -0.1276 0.0848 Uiso 1.00 calc . . . H(44) H 0.1975 0.9255 -0.0472 0.0664 Uiso 1.00 calc . . . H(45) H 0.1955 0.6947 -0.1680 0.0716 Uiso 1.00 calc . . . H(46) H 0.1942 0.5197 -0.1853 0.0831 Uiso 1.00 calc . . . H(47) H 0.2682 0.4230 -0.1096 0.0885 Uiso 1.00 calc . . . H(48) H 0.3451 0.5009 -0.0171 0.0949 Uiso 1.00 calc . . . H(49) H 0.3490 0.6741 -0.0011 0.0886 Uiso 1.00 calc . . . H(50) H 0.3229 0.7549 -0.1448 0.0688 Uiso 1.00 calc . . . H(51) H 0.3812 0.8146 -0.1773 0.0811 Uiso 1.00 calc . . . H(52) H 0.4107 0.9821 -0.1494 0.0856 Uiso 1.00 calc . . . H(53) H 0.3875 1.0859 -0.0820 0.0853 Uiso 1.00 calc . . . H(54) H 0.3285 1.0251 -0.0511 0.0703 Uiso 1.00 calc . . . H(55) H 0.2511 0.7352 0.0581 0.0865 Uiso 1.00 calc . . . H(56) H 0.2180 0.6484 0.1206 0.1098 Uiso 1.00 calc . . . H(57) H 0.2586 0.6584 0.2489 0.0923 Uiso 1.00 calc . . . H(58) H 0.3327 0.7582 0.3173 0.1014 Uiso 1.00 calc . . . H(59) H 0.3663 0.8496 0.2578 0.0846 Uiso 1.00 calc . . . H(60) H 0.3910 0.6736 0.1783 0.0778 Uiso 1.00 calc . . . H(61) H 0.4588 0.5801 0.1870 0.1016 Uiso 1.00 calc . . . H(62) H 0.5068 0.6400 0.1393 0.1021 Uiso 1.00 calc . . . H(63) H 0.4881 0.7973 0.0825 0.0858 Uiso 1.00 calc . . . H(64) H 0.4196 0.8980 0.0730 0.0640 Uiso 1.00 calc . . . H(65) H 0.2976 1.0602 0.0528 0.0639 Uiso 1.00 calc . . . H(66) H 0.3259 1.2240 0.0948 0.0837 Uiso 1.00 calc . . . H(67) H 0.4061 1.2493 0.2080 0.0861 Uiso 1.00 calc . . . H(68) H 0.4577 1.1147 0.2788 0.0748 Uiso 1.00 calc . . . H(69) H 0.4302 0.9473 0.2350 0.0632 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0559(2) 0.0982(3) 0.0553(2) -0.0113(2) 0.0222(1) 0.0297(2) P(1) 0.0348(10) 0.063(1) 0.054(1) 0.0027(9) 0.0081(9) 0.0021(10) P(2) 0.0380(9) 0.038(1) 0.051(1) 0.0037(8) 0.0240(8) 0.0043(8) P(3) 0.049(1) 0.040(1) 0.060(1) 0.0010(10) 0.0092(10) -0.0003(10) P(4) 0.0361(9) 0.051(1) 0.0315(9) 0.0042(8) 0.0153(8) -0.0032(8) P(5) 0.0352(9) 0.042(1) 0.0299(9) 0.0025(8) 0.0146(8) -0.0007(8) P(6) 0.0410(10) 0.038(1) 0.0330(9) 0.0039(8) 0.0177(8) -0.0015(7) P(7) 0.0387(9) 0.037(1) 0.0344(9) 0.0004(8) 0.0183(8) -0.0028(8) O(1) 0.051(2) 0.095(6) 0.050(4) 0.003(3) 0.013(3) 0.024(3) O(2) 0.053(3) 0.072(3) 0.062(4) 0.004(3) 0.042(3) 0.009(3) O(3) 0.064(4) 0.059(4) 0.075(4) -0.013(3) 0.029(3) 0.015(2) O(4) 0.033(2) 0.111(5) 0.063(4) 0.003(3) 0.002(3) 0.001(4) O(5) 0.038(2) 0.048(2) 0.054(3) -0.007(2) 0.023(2) -0.010(2) O(6) 0.062(3) 0.033(3) 0.083(4) 0.008(2) 0.046(3) 0.013(2) O(7) 0.034(2) 0.042(2) 0.043(3) 0.003(2) 0.009(2) -0.002(2) O(8) 0.093(5) 0.056(4) 0.073(4) 0.004(3) 0.021(4) -0.027(3) O(9) 0.048(2) 0.046(3) 0.061(3) 0.013(2) 0.016(2) 0.000(2) N(1) 0.048(3) 0.068(5) 0.029(2) 0.017(3) 0.017(2) -0.001(3) N(2) 0.049(3) 0.051(4) 0.034(2) 0.009(3) 0.021(2) -0.006(3) C(1) 0.102(9) 0.16(1) 0.056(6) -0.027(9) 0.047(6) -0.006(5) C(2) 0.107(9) 0.120(10) 0.17(1) 0.000(8) 0.048(9) 0.121(10) C(3) 0.059(3) 0.13(1) 0.061(7) -0.011(6) 0.022(6) 0.040(6) C(4) 0.038(3) 0.046(4) 0.038(3) 0.003(3) 0.019(2) -0.001(3) C(5) 0.057(5) 0.077(6) 0.039(3) -0.006(4) 0.018(3) -0.008(4) C(6) 0.088(6) 0.083(7) 0.038(5) 0.002(5) 0.036(4) 0.009(4) C(7) 0.079(5) 0.080(7) 0.070(4) 0.024(4) 0.053(4) 0.027(5) C(8) 0.051(5) 0.085(7) 0.070(4) 0.003(5) 0.032(4) 0.021(5) C(9) 0.034(3) 0.061(6) 0.059(5) 0.003(3) 0.013(4) 0.002(4) C(10) 0.035(4) 0.066(5) 0.034(4) 0.010(3) 0.013(3) -0.007(3) C(11) 0.055(5) 0.060(5) 0.068(6) 0.012(4) 0.026(5) -0.002(4) C(12) 0.052(6) 0.063(7) 0.093(8) 0.017(5) 0.021(6) -0.019(6) C(13) 0.048(5) 0.103(7) 0.099(8) 0.007(5) 0.036(5) -0.045(5) C(14) 0.039(4) 0.124(8) 0.065(5) -0.004(4) 0.032(4) -0.023(5) C(15) 0.036(4) 0.098(7) 0.048(4) -0.001(4) 0.022(3) 0.000(4) C(16) 0.052(4) 0.050(3) 0.040(3) 0.003(3) 0.028(3) -0.004(3) C(17) 0.048(4) 0.060(4) 0.050(4) 0.005(4) 0.022(3) -0.001(4) C(18) 0.064(5) 0.065(4) 0.055(5) -0.011(4) 0.029(4) -0.016(4) C(19) 0.088(6) 0.049(5) 0.082(6) -0.006(4) 0.049(4) -0.015(4) C(20) 0.082(5) 0.050(4) 0.075(5) 0.010(4) 0.046(4) 0.003(4) C(21) 0.059(5) 0.051(4) 0.051(4) 0.005(3) 0.027(4) 0.003(3) C(22) 0.033(3) 0.047(4) 0.038(4) 0.000(3) 0.016(3) 0.008(3) C(23) 0.067(5) 0.048(4) 0.069(5) 0.000(4) 0.042(5) 0.002(4) C(24) 0.059(6) 0.063(6) 0.080(7) -0.021(5) 0.034(5) -0.002(5) C(25) 0.051(5) 0.094(6) 0.085(7) -0.004(4) 0.047(5) 0.010(5) C(26) 0.067(6) 0.102(6) 0.078(6) -0.030(5) 0.060(5) -0.027(5) C(27) 0.040(4) 0.062(6) 0.066(5) -0.007(4) 0.027(4) -0.031(4) C(28) 0.035(3) 0.039(4) 0.035(3) -0.003(3) 0.011(2) -0.002(3) C(29) 0.045(4) 0.068(6) 0.035(3) -0.003(4) 0.016(3) 0.000(4) C(30) 0.050(4) 0.083(7) 0.031(4) 0.002(4) 0.004(3) 0.007(4) C(31) 0.039(5) 0.068(6) 0.064(4) 0.012(4) 0.017(4) 0.010(5) C(32) 0.046(4) 0.066(6) 0.066(4) 0.017(4) 0.031(4) 0.004(4) C(33) 0.044(4) 0.049(5) 0.048(4) 0.004(3) 0.028(3) 0.003(3) C(34) 0.050(4) 0.043(2) 0.049(4) 0.000(3) 0.032(3) 0.000(3) C(35) 0.046(4) 0.050(4) 0.066(5) -0.008(3) 0.029(3) -0.009(4) C(36) 0.091(7) 0.050(4) 0.101(7) -0.024(4) 0.061(6) -0.020(5) C(37) 0.118(8) 0.039(6) 0.108(7) -0.006(4) 0.082(5) -0.005(4) C(38) 0.133(9) 0.055(5) 0.077(6) 0.032(6) 0.056(6) 0.012(5) C(39) 0.092(7) 0.057(5) 0.063(6) 0.027(5) 0.013(5) 0.008(4) C(40) 0.040(3) 0.032(4) 0.045(3) -0.002(3) 0.013(3) 0.004(3) C(41) 0.065(5) 0.052(5) 0.045(3) 0.006(4) 0.021(4) 0.000(4) C(42) 0.067(5) 0.061(6) 0.051(5) 0.009(5) 0.010(4) 0.000(4) C(43) 0.037(5) 0.058(6) 0.089(5) 0.008(4) 0.011(4) 0.004(5) C(44) 0.046(4) 0.070(7) 0.094(5) 0.018(4) 0.036(4) 0.011(6) C(45) 0.048(4) 0.060(5) 0.066(5) 0.012(4) 0.036(4) 0.008(4) C(46) 0.060(4) 0.038(2) 0.055(4) 0.000(3) 0.042(3) -0.002(3) C(47) 0.058(4) 0.047(4) 0.082(6) -0.004(4) 0.043(4) -0.008(4) C(48) 0.081(6) 0.048(4) 0.092(7) -0.020(4) 0.055(5) -0.015(4) C(49) 0.100(6) 0.042(6) 0.104(7) -0.001(4) 0.071(5) -0.003(4) C(50) 0.110(7) 0.040(4) 0.066(6) 0.027(5) 0.033(5) 0.000(4) C(51) 0.080(6) 0.040(4) 0.064(6) 0.011(4) 0.013(5) -0.006(4) C(52) 0.037(4) 0.045(3) 0.038(4) -0.001(3) 0.014(3) 0.006(3) C(53) 0.061(5) 0.055(6) 0.066(6) -0.005(4) 0.041(4) -0.024(4) C(54) 0.059(6) 0.088(6) 0.072(6) 0.001(4) 0.046(5) -0.015(5) C(55) 0.068(6) 0.095(6) 0.070(6) -0.025(5) 0.050(5) -0.013(5) C(56) 0.099(7) 0.064(6) 0.083(7) -0.020(5) 0.071(6) -0.010(5) C(57) 0.088(6) 0.042(4) 0.052(5) -0.006(4) 0.041(5) -0.012(4) C(58) 0.050(4) 0.041(4) 0.043(3) 0.000(3) 0.027(3) 0.007(3) C(59) 0.048(5) 0.080(7) 0.059(5) -0.013(4) 0.009(4) -0.020(5) C(60) 0.108(8) 0.105(9) 0.099(6) -0.055(7) 0.080(7) -0.014(7) C(61) 0.098(7) 0.074(7) 0.098(5) 0.003(5) 0.078(6) 0.024(5) C(62) 0.101(7) 0.115(9) 0.050(5) -0.021(5) 0.049(5) 0.016(5) C(63) 0.068(6) 0.083(7) 0.042(3) -0.018(5) 0.017(4) -0.004(4) C(64) 0.037(3) 0.040(4) 0.047(4) -0.001(3) 0.016(3) -0.013(3) C(65) 0.062(5) 0.045(4) 0.077(6) 0.012(4) 0.030(5) 0.011(4) C(66) 0.067(6) 0.063(7) 0.122(9) 0.019(5) 0.050(6) -0.001(6) C(67) 0.055(6) 0.079(7) 0.105(10) 0.023(5) 0.033(6) -0.025(5) C(68) 0.052(5) 0.098(7) 0.074(6) 0.011(4) 0.041(5) -0.007(5) C(69) 0.049(5) 0.061(5) 0.055(5) -0.004(4) 0.031(4) 0.003(4) C(70) 0.055(4) 0.037(3) 0.050(4) -0.006(3) 0.036(3) -0.005(2) C(71) 0.066(5) 0.042(3) 0.059(5) 0.004(3) 0.038(4) -0.002(3) C(72) 0.099(6) 0.037(4) 0.102(6) 0.010(4) 0.072(5) -0.003(4) C(73) 0.099(6) 0.043(5) 0.109(6) -0.026(4) 0.079(5) -0.024(4) C(74) 0.070(5) 0.066(4) 0.063(5) -0.020(4) 0.044(4) -0.031(4) C(75) 0.054(4) 0.057(4) 0.052(4) -0.007(4) 0.032(3) -0.008(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) O(1) 2.191(8) . . yes Pt(1) O(2) 2.197(6) . . yes Pt(1) O(3) 2.223(7) . . yes Pt(1) C(1) 2.05(1) . . yes Pt(1) C(2) 2.002(10) . . yes Pt(1) C(3) 2.00(1) . . yes P(1) O(1) 1.492(9) . . yes P(1) O(4) 1.458(6) . . yes P(1) O(5) 1.614(6) . . yes P(1) O(9) 1.613(6) . . yes P(2) O(2) 1.510(6) . . yes P(2) O(5) 1.606(5) . . yes P(2) O(6) 1.462(5) . . yes P(2) O(7) 1.603(5) . . yes P(3) O(3) 1.478(7) . . yes P(3) O(7) 1.594(6) . . yes P(3) O(8) 1.472(7) . . yes P(3) O(9) 1.629(6) . . yes P(4) N(1) 1.569(6) . . yes P(4) C(4) 1.808(8) . . yes P(4) C(10) 1.802(9) . . yes P(4) C(16) 1.794(8) . . yes P(5) N(1) 1.575(6) . . yes P(5) C(22) 1.803(8) . . yes P(5) C(28) 1.789(8) . . yes P(5) C(34) 1.802(8) . . yes P(6) N(2) 1.566(6) . . yes P(6) C(40) 1.801(8) . . yes P(6) C(46) 1.798(8) . . yes P(6) C(52) 1.814(8) . . yes P(7) N(2) 1.582(6) . . yes P(7) C(58) 1.804(8) . . yes P(7) C(64) 1.786(8) . . yes P(7) C(70) 1.789(8) . . yes C(4) C(5) 1.40(1) . . yes C(4) C(9) 1.37(1) . . yes C(5) C(6) 1.37(1) . . yes C(6) C(7) 1.40(1) . . yes C(7) C(8) 1.35(1) . . yes C(8) C(9) 1.36(1) . . yes C(10) C(11) 1.36(1) . . yes C(10) C(15) 1.40(1) . . yes C(11) C(12) 1.42(1) . . yes C(12) C(13) 1.35(2) . . yes C(13) C(14) 1.37(2) . . yes C(14) C(15) 1.38(1) . . yes C(16) C(17) 1.40(1) . . yes C(16) C(21) 1.38(1) . . yes C(17) C(18) 1.38(1) . . yes C(18) C(19) 1.39(1) . . yes C(19) C(20) 1.35(1) . . yes C(20) C(21) 1.37(1) . . yes C(22) C(23) 1.39(1) . . yes C(22) C(27) 1.38(1) . . yes C(23) C(24) 1.39(1) . . yes C(24) C(25) 1.38(1) . . yes C(25) C(26) 1.35(1) . . yes C(26) C(27) 1.40(1) . . yes C(28) C(29) 1.40(1) . . yes C(28) C(33) 1.38(1) . . yes C(29) C(30) 1.38(1) . . yes C(30) C(31) 1.37(1) . . yes C(31) C(32) 1.38(1) . . yes C(32) C(33) 1.39(1) . . yes C(34) C(35) 1.40(1) . . yes C(34) C(39) 1.39(1) . . yes C(35) C(36) 1.36(1) . . yes C(36) C(37) 1.39(1) . . yes C(37) C(38) 1.33(2) . . yes C(38) C(39) 1.37(2) . . yes C(40) C(41) 1.39(1) . . yes C(40) C(45) 1.38(1) . . yes C(41) C(42) 1.38(1) . . yes C(42) C(43) 1.34(1) . . yes C(43) C(44) 1.37(1) . . yes C(44) C(45) 1.37(1) . . yes C(46) C(47) 1.36(1) . . yes C(46) C(51) 1.40(1) . . yes C(47) C(48) 1.39(1) . . yes C(48) C(49) 1.35(1) . . yes C(49) C(50) 1.36(2) . . yes C(50) C(51) 1.36(1) . . yes C(52) C(53) 1.37(1) . . yes C(52) C(57) 1.39(1) . . yes C(53) C(54) 1.37(1) . . yes C(54) C(55) 1.38(1) . . yes C(55) C(56) 1.38(1) . . yes C(56) C(57) 1.37(1) . . yes C(58) C(59) 1.37(1) . . yes C(58) C(63) 1.39(1) . . yes C(59) C(60) 1.39(1) . . yes C(60) C(61) 1.35(1) . . yes C(61) C(62) 1.35(1) . . yes C(62) C(63) 1.38(1) . . yes C(64) C(65) 1.39(1) . . yes C(64) C(69) 1.38(1) . . yes C(65) C(66) 1.36(1) . . yes C(66) C(67) 1.35(2) . . yes C(67) C(68) 1.36(2) . . yes C(68) C(69) 1.40(1) . . yes C(70) C(71) 1.39(1) . . yes C(70) C(75) 1.39(1) . . yes C(71) C(72) 1.37(1) . . yes C(72) C(73) 1.38(1) . . yes C(73) C(74) 1.36(1) . . yes C(74) C(75) 1.40(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Pt(1) O(2) 89.0(2) . . . yes O(1) Pt(1) O(3) 88.8(3) . . . yes O(1) Pt(1) C(1) 90.8(5) . . . yes O(1) Pt(1) C(2) 89.6(4) . . . yes O(1) Pt(1) C(3) 179.4(5) . . . yes O(2) Pt(1) O(3) 88.3(2) . . . yes O(2) Pt(1) C(1) 88.2(5) . . . yes O(2) Pt(1) C(2) 178.1(6) . . . yes O(2) Pt(1) C(3) 90.9(4) . . . yes O(3) Pt(1) C(1) 176.5(5) . . . yes O(3) Pt(1) C(2) 90.3(6) . . . yes O(3) Pt(1) C(3) 91.7(5) . . . yes C(1) Pt(1) C(2) 93.2(7) . . . yes C(1) Pt(1) C(3) 88.7(6) . . . yes C(2) Pt(1) C(3) 90.5(5) . . . yes O(1) P(1) O(4) 118.2(4) . . . yes O(1) P(1) O(5) 108.1(4) . . . yes O(1) P(1) O(9) 107.8(4) . . . yes O(4) P(1) O(5) 110.8(4) . . . yes O(4) P(1) O(9) 109.8(4) . . . yes O(5) P(1) O(9) 100.6(3) . . . yes O(2) P(2) O(5) 108.3(3) . . . yes O(2) P(2) O(6) 118.3(3) . . . yes O(2) P(2) O(7) 108.6(3) . . . yes O(5) P(2) O(6) 110.2(3) . . . yes O(5) P(2) O(7) 100.2(3) . . . yes O(6) P(2) O(7) 109.7(3) . . . yes O(3) P(3) O(7) 108.6(4) . . . yes O(3) P(3) O(8) 119.1(4) . . . yes O(3) P(3) O(9) 108.9(4) . . . yes O(7) P(3) O(8) 109.1(4) . . . yes O(7) P(3) O(9) 100.2(3) . . . yes O(8) P(3) O(9) 109.3(4) . . . yes N(1) P(4) C(4) 108.3(4) . . . yes N(1) P(4) C(10) 115.0(4) . . . yes N(1) P(4) C(16) 108.9(4) . . . yes C(4) P(4) C(10) 107.9(4) . . . yes C(4) P(4) C(16) 110.1(4) . . . yes C(10) P(4) C(16) 106.5(4) . . . yes N(1) P(5) C(22) 114.1(4) . . . yes N(1) P(5) C(28) 107.4(4) . . . yes N(1) P(5) C(34) 113.4(4) . . . yes C(22) P(5) C(28) 108.1(4) . . . yes C(22) P(5) C(34) 105.3(4) . . . yes C(28) P(5) C(34) 108.4(4) . . . yes N(2) P(6) C(40) 106.8(4) . . . yes N(2) P(6) C(46) 114.3(4) . . . yes N(2) P(6) C(52) 113.7(4) . . . yes C(40) P(6) C(46) 108.3(4) . . . yes C(40) P(6) C(52) 107.3(4) . . . yes C(46) P(6) C(52) 106.1(4) . . . yes N(2) P(7) C(58) 108.0(4) . . . yes N(2) P(7) C(64) 114.5(3) . . . yes N(2) P(7) C(70) 109.4(4) . . . yes C(58) P(7) C(64) 107.8(4) . . . yes C(58) P(7) C(70) 110.5(4) . . . yes C(64) P(7) C(70) 106.6(4) . . . yes Pt(1) O(1) P(1) 122.0(4) . . . yes Pt(1) O(2) P(2) 120.7(3) . . . yes Pt(1) O(3) P(3) 120.9(4) . . . yes P(1) O(5) P(2) 125.4(3) . . . yes P(2) O(7) P(3) 126.1(3) . . . yes P(1) O(9) P(3) 124.5(4) . . . yes P(4) N(1) P(5) 146.1(5) . . . yes P(6) N(2) P(7) 146.2(4) . . . yes P(4) C(4) C(5) 119.1(6) . . . yes P(4) C(4) C(9) 121.2(6) . . . yes C(5) C(4) C(9) 119.6(8) . . . yes C(4) C(5) C(6) 119.0(8) . . . yes C(5) C(6) C(7) 120.1(8) . . . yes C(6) C(7) C(8) 119.7(9) . . . yes C(7) C(8) C(9) 120.9(10) . . . yes C(4) C(9) C(8) 120.6(9) . . . yes P(4) C(10) C(11) 123.6(8) . . . yes P(4) C(10) C(15) 116.8(7) . . . yes C(11) C(10) C(15) 119.3(9) . . . yes C(10) C(11) C(12) 119(1) . . . yes C(11) C(12) C(13) 119(1) . . . yes C(12) C(13) C(14) 120.6(9) . . . yes C(13) C(14) C(15) 120.5(10) . . . yes C(10) C(15) C(14) 119.8(10) . . . yes P(4) C(16) C(17) 120.4(6) . . . yes P(4) C(16) C(21) 121.3(6) . . . yes C(17) C(16) C(21) 118.3(8) . . . yes C(16) C(17) C(18) 119.3(8) . . . yes C(17) C(18) C(19) 121.4(8) . . . yes C(18) C(19) C(20) 118.5(9) . . . yes C(19) C(20) C(21) 121.5(9) . . . yes C(16) C(21) C(20) 120.9(8) . . . yes P(5) C(22) C(23) 118.1(7) . . . yes P(5) C(22) C(27) 121.7(7) . . . yes C(23) C(22) C(27) 120.1(8) . . . yes C(22) C(23) C(24) 119.6(9) . . . yes C(23) C(24) C(25) 120.2(9) . . . yes C(24) C(25) C(26) 119.5(8) . . . yes C(25) C(26) C(27) 121.7(9) . . . yes C(22) C(27) C(26) 118.7(9) . . . yes P(5) C(28) C(29) 121.3(6) . . . yes P(5) C(28) C(33) 119.4(6) . . . yes C(29) C(28) C(33) 119.2(7) . . . yes C(28) C(29) C(30) 120.3(8) . . . yes C(29) C(30) C(31) 119.7(8) . . . yes C(30) C(31) C(32) 121.1(8) . . . yes C(31) C(32) C(33) 119.2(8) . . . yes C(28) C(33) C(32) 120.5(8) . . . yes P(5) C(34) C(35) 122.2(6) . . . yes P(5) C(34) C(39) 120.6(8) . . . yes C(35) C(34) C(39) 116.8(9) . . . yes C(34) C(35) C(36) 120.4(9) . . . yes C(35) C(36) C(37) 121.1(10) . . . yes C(36) C(37) C(38) 119.2(10) . . . yes C(37) C(38) C(39) 121(1) . . . yes C(34) C(39) C(38) 121(1) . . . yes P(6) C(40) C(41) 121.0(7) . . . yes P(6) C(40) C(45) 120.6(6) . . . yes C(41) C(40) C(45) 118.4(8) . . . yes C(40) C(41) C(42) 119.8(9) . . . yes C(41) C(42) C(43) 121.1(10) . . . yes C(42) C(43) C(44) 120.1(9) . . . yes C(43) C(44) C(45) 120.0(9) . . . yes C(40) C(45) C(44) 120.6(9) . . . yes P(6) C(46) C(47) 123.9(7) . . . yes P(6) C(46) C(51) 117.8(7) . . . yes C(47) C(46) C(51) 118.2(9) . . . yes C(46) C(47) C(48) 120.2(9) . . . yes C(47) C(48) C(49) 121.0(10) . . . yes C(48) C(49) C(50) 119.1(10) . . . yes C(49) C(50) C(51) 121(1) . . . yes C(46) C(51) C(50) 120(1) . . . yes P(6) C(52) C(53) 121.1(7) . . . yes P(6) C(52) C(57) 119.1(7) . . . yes C(53) C(52) C(57) 119.8(8) . . . yes C(52) C(53) C(54) 120.5(9) . . . yes C(53) C(54) C(55) 119.0(9) . . . yes C(54) C(55) C(56) 121.3(9) . . . yes C(55) C(56) C(57) 118.8(9) . . . yes C(52) C(57) C(56) 120.5(8) . . . yes P(7) C(58) C(59) 119.4(7) . . . yes P(7) C(58) C(63) 122.1(7) . . . yes C(59) C(58) C(63) 118.5(9) . . . yes C(58) C(59) C(60) 119.5(9) . . . yes C(59) C(60) C(61) 121.7(10) . . . yes C(60) C(61) C(62) 119.1(9) . . . yes C(61) C(62) C(63) 121.0(9) . . . yes C(58) C(63) C(62) 120.1(9) . . . yes P(7) C(64) C(65) 121.8(7) . . . yes P(7) C(64) C(69) 118.3(7) . . . yes C(65) C(64) C(69) 119.5(8) . . . yes C(64) C(65) C(66) 119(1) . . . yes C(65) C(66) C(67) 121(1) . . . yes C(66) C(67) C(68) 119.8(10) . . . yes C(67) C(68) C(69) 120(1) . . . yes C(64) C(69) C(68) 118.4(9) . . . yes P(7) C(70) C(71) 120.2(6) . . . yes P(7) C(70) C(75) 120.4(6) . . . yes C(71) C(70) C(75) 119.3(7) . . . yes C(70) C(71) C(72) 121.3(9) . . . yes C(71) C(72) C(73) 118.8(9) . . . yes C(72) C(73) C(74) 121.8(9) . . . yes C(73) C(74) C(75) 119.5(9) . . . yes C(70) C(75) C(74) 119.3(8) . . . yes #------------------------------------------------------------------------------ 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 Pt(1) O(1) P(1) O(4) 179.8(4) . . . . yes Pt(1) O(1) P(1) O(5) -53.3(5) . . . . yes Pt(1) O(1) P(1) O(9) 54.7(5) . . . . yes Pt(1) O(2) P(2) O(5) 54.2(5) . . . . yes Pt(1) O(2) P(2) O(6) -179.5(3) . . . . yes Pt(1) O(2) P(2) O(7) -53.7(5) . . . . yes Pt(1) O(3) P(3) O(7) 54.6(5) . . . . yes Pt(1) O(3) P(3) O(8) -179.8(4) . . . . yes Pt(1) O(3) P(3) O(9) -53.6(5) . . . . yes P(1) O(1) Pt(1) O(2) 44.1(5) . . . . yes P(1) O(1) Pt(1) O(3) -44.2(5) . . . . yes P(1) O(1) Pt(1) C(1) 132.3(6) . . . . yes P(1) O(1) Pt(1) C(2) -134.6(7) . . . . yes P(1) O(1) Pt(1) C(3) 123(44) . . . . yes P(1) O(5) P(2) O(2) -62.3(5) . . . . yes P(1) O(5) P(2) O(6) 166.9(4) . . . . yes P(1) O(5) P(2) O(7) 51.4(5) . . . . yes P(1) O(9) P(3) O(3) 62.6(6) . . . . yes P(1) O(9) P(3) O(7) -51.2(5) . . . . yes P(1) O(9) P(3) O(8) -165.8(5) . . . . yes P(2) O(2) Pt(1) O(1) -44.1(4) . . . . yes P(2) O(2) Pt(1) O(3) 44.8(4) . . . . yes P(2) O(2) Pt(1) C(1) -134.9(5) . . . . yes P(2) O(2) Pt(1) C(2) 0(15) . . . . yes P(2) O(2) Pt(1) C(3) 136.5(6) . . . . yes P(2) O(5) P(1) O(1) 61.4(5) . . . . yes P(2) O(5) P(1) O(4) -167.6(4) . . . . yes P(2) O(5) P(1) O(9) -51.5(5) . . . . yes P(2) O(7) P(3) O(3) -61.5(5) . . . . yes P(2) O(7) P(3) O(8) 167.2(4) . . . . yes P(2) O(7) P(3) O(9) 52.5(5) . . . . yes P(3) O(3) Pt(1) O(1) 43.5(4) . . . . yes P(3) O(3) Pt(1) O(2) -45.6(4) . . . . yes P(3) O(3) Pt(1) C(1) -39(7) . . . . yes P(3) O(3) Pt(1) C(2) 133.1(5) . . . . yes P(3) O(3) Pt(1) C(3) -136.4(5) . . . . yes P(3) O(7) P(2) O(2) 60.9(5) . . . . yes P(3) O(7) P(2) O(5) -52.5(5) . . . . yes P(3) O(7) P(2) O(6) -168.4(4) . . . . yes P(3) O(9) P(1) O(1) -62.2(6) . . . . yes P(3) O(9) P(1) O(4) 167.8(5) . . . . yes P(3) O(9) P(1) O(5) 51.0(5) . . . . yes P(4) N(1) P(5) C(22) 51(1) . . . . yes P(4) N(1) P(5) C(28) 171.2(9) . . . . yes P(4) N(1) P(5) C(34) -69(1) . . . . yes P(4) C(4) C(5) C(6) 176.1(8) . . . . yes P(4) C(4) C(9) C(8) -178.0(8) . . . . yes P(4) C(10) C(11) C(12) -171.5(8) . . . . yes P(4) C(10) C(15) C(14) 172.7(7) . . . . yes P(4) C(16) C(17) C(18) -180.0 . . . . yes P(4) C(16) C(21) C(20) 179.0(7) . . . . yes P(5) N(1) P(4) C(4) 123.4(9) . . . . yes P(5) N(1) P(4) C(10) 2(1) . . . . yes P(5) N(1) P(4) C(16) -116.9(9) . . . . yes P(5) C(22) C(23) C(24) -173.0(7) . . . . yes P(5) C(22) C(27) C(26) 175.7(7) . . . . yes P(5) C(28) C(29) C(30) -178.4(7) . . . . yes P(5) C(28) C(33) C(32) 177.2(7) . . . . yes P(5) C(34) C(35) C(36) -174.9(8) . . . . yes P(5) C(34) C(39) C(38) 175(1) . . . . yes P(6) N(2) P(7) C(58) -119.4(9) . . . . yes P(6) N(2) P(7) C(64) 0(1) . . . . yes P(6) N(2) P(7) C(70) 120.3(9) . . . . yes P(6) C(40) C(41) C(42) 178.4(8) . . . . yes P(6) C(40) C(45) C(44) -178.8(8) . . . . yes P(6) C(46) C(47) C(48) 178.8(7) . . . . yes P(6) C(46) C(51) C(50) 179.8(9) . . . . yes P(6) C(52) C(53) C(54) -178.7(8) . . . . yes P(6) C(52) C(57) C(56) 178.4(8) . . . . yes P(7) N(2) P(6) C(40) -177.4(8) . . . . yes P(7) N(2) P(6) C(46) 62.8(10) . . . . yes P(7) N(2) P(6) C(52) -59.2(10) . . . . yes P(7) C(58) C(59) C(60) 177.8(10) . . . . yes P(7) C(58) C(63) C(62) -177.0(9) . . . . yes P(7) C(64) C(65) C(66) 171.3(8) . . . . yes P(7) C(64) C(69) C(68) -171.1(7) . . . . yes P(7) C(70) C(71) C(72) -177.1(7) . . . . yes P(7) C(70) C(75) C(74) 177.9(6) . . . . yes N(1) P(4) C(4) C(5) 174.3(7) . . . . yes N(1) P(4) C(4) C(9) -8.3(8) . . . . yes N(1) P(4) C(10) C(11) 112.2(8) . . . . yes N(1) P(4) C(10) C(15) -62.6(8) . . . . yes N(1) P(4) C(16) C(17) 168.7(6) . . . . yes N(1) P(4) C(16) C(21) -10.3(8) . . . . yes N(1) P(5) C(22) C(23) 45.6(8) . . . . yes N(1) P(5) C(22) C(27) -130.3(7) . . . . yes N(1) P(5) C(28) C(29) -155.6(7) . . . . yes N(1) P(5) C(28) C(33) 25.3(8) . . . . yes N(1) P(5) C(34) C(35) -139.3(7) . . . . yes N(1) P(5) C(34) C(39) 47.4(9) . . . . yes N(2) P(6) C(40) C(41) 162.9(7) . . . . yes N(2) P(6) C(40) C(45) -16.2(8) . . . . yes N(2) P(6) C(46) C(47) 122.9(8) . . . . yes N(2) P(6) C(46) C(51) -59.5(9) . . . . yes N(2) P(6) C(52) C(53) 136.6(7) . . . . yes N(2) P(6) C(52) C(57) -43.5(8) . . . . yes N(2) P(7) C(58) C(59) 19.3(9) . . . . yes N(2) P(7) C(58) C(63) -161.1(8) . . . . yes N(2) P(7) C(64) C(65) -109.2(7) . . . . yes N(2) P(7) C(64) C(69) 63.7(8) . . . . yes N(2) P(7) C(70) C(71) 15.1(8) . . . . yes N(2) P(7) C(70) C(75) -162.4(6) . . . . yes C(4) P(4) C(10) C(11) -8.8(9) . . . . yes C(4) P(4) C(10) C(15) 176.4(7) . . . . yes C(4) P(4) C(16) C(17) -72.6(7) . . . . yes C(4) P(4) C(16) C(21) 108.3(7) . . . . yes C(4) C(5) C(6) C(7) 1(1) . . . . yes C(4) C(9) C(8) C(7) 2(1) . . . . yes C(5) C(4) P(4) C(10) -60.6(8) . . . . yes C(5) C(4) P(4) C(16) 55.3(8) . . . . yes C(5) C(4) C(9) C(8) 0(1) . . . . yes C(5) C(6) C(7) C(8) 0(1) . . . . yes C(6) C(5) C(4) C(9) -1(1) . . . . yes C(6) C(7) C(8) C(9) -1(1) . . . . yes C(9) C(4) P(4) C(10) 116.9(7) . . . . yes C(9) C(4) P(4) C(16) -127.3(7) . . . . yes C(10) P(4) C(16) C(17) 44.2(7) . . . . yes C(10) P(4) C(16) C(21) -134.9(7) . . . . yes C(10) C(11) C(12) C(13) -2(1) . . . . yes C(10) C(15) C(14) C(13) 0(1) . . . . yes C(11) C(10) P(4) C(16) -127.1(8) . . . . yes C(11) C(10) C(15) C(14) -2(1) . . . . yes C(11) C(12) C(13) C(14) 0(1) . . . . yes C(12) C(11) C(10) C(15) 3(1) . . . . yes C(12) C(13) C(14) C(15) 0(1) . . . . yes C(15) C(10) P(4) C(16) 58.2(8) . . . . yes C(16) C(17) C(18) C(19) 0(1) . . . . yes C(16) C(21) C(20) C(19) 1(1) . . . . yes C(17) C(16) C(21) C(20) 0(1) . . . . yes C(17) C(18) C(19) C(20) 0(1) . . . . yes C(18) C(17) C(16) C(21) 0(1) . . . . yes C(18) C(19) C(20) C(21) -1(1) . . . . yes C(22) P(5) C(28) C(29) -32.1(8) . . . . yes C(22) P(5) C(28) C(33) 148.7(7) . . . . yes C(22) P(5) C(34) C(35) 95.3(7) . . . . yes C(22) P(5) C(34) C(39) -78.0(9) . . . . yes C(22) C(23) C(24) C(25) -3(1) . . . . yes C(22) C(27) C(26) C(25) -1(1) . . . . yes C(23) C(22) P(5) C(28) -73.7(7) . . . . yes C(23) C(22) P(5) C(34) 170.6(7) . . . . yes C(23) C(22) C(27) C(26) 0(1) . . . . yes C(23) C(24) C(25) C(26) 1(1) . . . . yes C(24) C(23) C(22) C(27) 2(1) . . . . yes C(24) C(25) C(26) C(27) 1(1) . . . . yes C(27) C(22) P(5) C(28) 110.4(7) . . . . yes C(27) C(22) P(5) C(34) -5.3(8) . . . . yes C(28) P(5) C(34) C(35) -20.1(8) . . . . yes C(28) P(5) C(34) C(39) 166.6(8) . . . . yes C(28) C(29) C(30) C(31) 0(1) . . . . yes C(28) C(33) C(32) C(31) 1(1) . . . . yes C(29) C(28) P(5) C(34) 81.5(8) . . . . yes C(29) C(28) C(33) C(32) -1(1) . . . . yes C(29) C(30) C(31) C(32) 0(1) . . . . yes C(30) C(29) C(28) C(33) 0(1) . . . . yes C(30) C(31) C(32) C(33) 0(1) . . . . yes C(33) C(28) P(5) C(34) -97.6(7) . . . . yes C(34) C(35) C(36) C(37) 1(1) . . . . yes C(34) C(39) C(38) C(37) -2(2) . . . . yes C(35) C(34) C(39) C(38) 1(1) . . . . yes C(35) C(36) C(37) C(38) -2(1) . . . . yes C(36) C(35) C(34) C(39) -1(1) . . . . yes C(36) C(37) C(38) C(39) 2(1) . . . . yes C(40) P(6) C(46) C(47) 4.0(9) . . . . yes C(40) P(6) C(46) C(51) -178.4(8) . . . . yes C(40) P(6) C(52) C(53) -105.5(8) . . . . yes C(40) P(6) C(52) C(57) 74.4(7) . . . . yes C(40) C(41) C(42) C(43) 1(1) . . . . yes C(40) C(45) C(44) C(43) 0(1) . . . . yes C(41) C(40) P(6) C(46) -73.5(8) . . . . yes C(41) C(40) P(6) C(52) 40.6(8) . . . . yes C(41) C(40) C(45) C(44) 2(1) . . . . yes C(41) C(42) C(43) C(44) 0(1) . . . . yes C(42) C(41) C(40) C(45) -2(1) . . . . yes C(42) C(43) C(44) C(45) 0(1) . . . . yes C(45) C(40) P(6) C(46) 107.4(8) . . . . yes C(45) C(40) P(6) C(52) -138.5(7) . . . . yes C(46) P(6) C(52) C(53) 10.0(8) . . . . yes C(46) P(6) C(52) C(57) -170.0(7) . . . . yes C(46) C(47) C(48) C(49) 0(1) . . . . yes C(46) C(51) C(50) C(49) 2(1) . . . . yes C(47) C(46) P(6) C(52) -110.9(8) . . . . yes C(47) C(46) C(51) C(50) -2(1) . . . . yes C(47) C(48) C(49) C(50) 0(1) . . . . yes C(48) C(47) C(46) C(51) 1(1) . . . . yes C(48) C(49) C(50) C(51) 0(1) . . . . yes C(51) C(46) P(6) C(52) 66.7(8) . . . . yes C(52) C(53) C(54) C(55) -1(1) . . . . yes C(52) C(57) C(56) C(55) 2(1) . . . . yes C(53) C(52) C(57) C(56) -1(1) . . . . yes C(53) C(54) C(55) C(56) 2(1) . . . . yes C(54) C(53) C(52) C(57) 1(1) . . . . yes C(54) C(55) C(56) C(57) -2(1) . . . . yes C(58) P(7) C(64) C(65) 11.0(8) . . . . yes C(58) P(7) C(64) C(69) -176.1(7) . . . . yes C(58) P(7) C(70) C(71) -103.6(7) . . . . yes C(58) P(7) C(70) C(75) 78.8(7) . . . . yes C(58) C(59) C(60) C(61) 0(2) . . . . yes C(58) C(63) C(62) C(61) -1(1) . . . . yes C(59) C(58) P(7) C(64) -104.9(8) . . . . yes C(59) C(58) P(7) C(70) 138.9(8) . . . . yes C(59) C(58) C(63) C(62) 2(1) . . . . yes C(59) C(60) C(61) C(62) 0(2) . . . . yes C(60) C(59) C(58) C(63) -1(1) . . . . yes C(60) C(61) C(62) C(63) 0(1) . . . . yes C(63) C(58) P(7) C(64) 74.7(8) . . . . yes C(63) C(58) P(7) C(70) -41.5(9) . . . . yes C(64) P(7) C(70) C(71) 139.4(7) . . . . yes C(64) P(7) C(70) C(75) -38.1(7) . . . . yes C(64) C(65) C(66) C(67) 0(1) . . . . yes C(64) C(69) C(68) C(67) -1(1) . . . . yes C(65) C(64) P(7) C(70) 129.7(7) . . . . yes C(65) C(64) C(69) C(68) 1(1) . . . . yes C(65) C(66) C(67) C(68) 0(2) . . . . yes C(66) C(65) C(64) C(69) -1(1) . . . . yes C(66) C(67) C(68) C(69) 0(1) . . . . yes C(69) C(64) P(7) C(70) -57.4(7) . . . . yes C(70) C(71) C(72) C(73) 0(1) . . . . yes C(70) C(75) C(74) C(73) 0(1) . . . . yes C(71) C(70) C(75) C(74) 0(1) . . . . yes C(71) C(72) C(73) C(74) 0(1) . . . . yes C(72) C(71) C(70) C(75) 0(1) . . . . yes C(72) C(73) C(74) C(75) 0(1) . . . . yes C(72) C(73) C(74) C(75) 0(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(62) 3.50(1) . 4_464 ? O(2) C(24) 3.31(1) . 2_564 ? O(4) C(8) 3.21(1) . 4_464 ? O(4) C(72) 3.30(1) . 3_445 ? O(4) C(49) 3.36(1) . 3_455 ? O(4) C(9) 3.42(1) . 4_464 ? O(4) C(50) 3.55(1) . 3_455 ? O(5) C(56) 3.22(1) . 3_445 ? O(5) C(72) 3.26(1) . 3_445 ? O(5) C(57) 3.415(10) . 3_445 ? O(5) C(73) 3.44(1) . 3_445 ? O(5) C(71) 3.55(1) . 3_445 ? O(6) C(25) 3.24(1) . 2_564 ? O(6) C(69) 3.31(1) . 3_445 ? O(6) C(17) 3.36(1) . . ? O(6) C(74) 3.36(1) . 3_445 ? O(6) C(75) 3.370(10) . 3_445 ? O(7) C(5) 3.243(10) . . ? O(7) C(73) 3.49(1) . 3_445 ? O(7) C(6) 3.49(1) . . ? O(8) C(66) 3.14(1) . 3_455 ? O(8) C(12) 3.25(2) . . ? O(8) C(11) 3.37(1) . . ? O(8) C(43) 3.44(1) . 2_575 ? C(7) C(42) 3.58(1) . 2_575 ? C(14) C(54) 3.59(1) . 4_465 ? C(20) C(47) 3.55(1) . 2_565 ? C(33) C(72) 3.57(1) . 2_575 ? C(35) C(72) 3.46(1) . 2_575 ? C(35) C(71) 3.54(1) . 2_575 ? C(36) C(71) 3.53(1) . 2_575 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------