# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Storr, Tim' _publ_contact_author_email tsa34@sfu.ca _publ_section_title ; Influence of the Chelate Effect on the Electronic Structure of One-electron Oxidized Group 10 Metal(II)-(Disalicylidene) diamine Complexes ; loop_ _publ_author_name T.Storr Y.Shimazaki # Attachment '- Nisalpn.cif' #============================================================================== data__1 _database_code_depnum_ccdc_archive 'CCDC 801075' #TrackingRef '- Nisalpn.cif' _audit_creation_date 2008-12-25 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H48 N2 Ni O2 ' _chemical_formula_moiety 'C33 H48 N2 Ni O2 ' _chemical_formula_weight 563.45 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,-Y,1/2+Z 4 1/2-X,1/2-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,+Y,1/2-Z 8 1/2+X,1/2+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 26.3739(6) _cell_length_b 11.1334(3) _cell_length_c 10.7486(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3156.10(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 19150 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216.00 _exptl_absorpt_coefficient_mu 0.644 _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 0.640 _exptl_absorpt_correction_T_max 0.950 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_ambient_temperature 133(2) _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 29029 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 3605 _reflns_number_gt 2271 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1597 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3605 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0016Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0045 _refine_diff_density_max 0.65 _refine_diff_density_min -0.60 _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 0.003 0.002 ; 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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; 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 Ni(1) Ni 1.0000 0.02279(5) 0.2500 0.01755(14) Uani 1.00 2 d S . . O(1) O 0.96406(7) 0.14589(19) 0.17372(19) 0.0233(5) Uani 1.00 1 d . . . N(1) N 1.02276(9) -0.0942(2) 0.3612(2) 0.0206(6) Uani 1.00 1 d . . . C(1) C 0.92409(11) 0.1345(2) 0.1006(2) 0.0199(7) Uani 1.00 1 d . . . C(2) C 0.89157(10) 0.2371(3) 0.0809(2) 0.0202(7) Uani 1.00 1 d . . . C(3) C 0.85225(11) 0.2235(3) -0.0040(2) 0.0239(8) Uani 1.00 1 d . . . C(4) C 0.84235(11) 0.1185(3) -0.0729(2) 0.0228(8) Uani 1.00 1 d . . . C(5) C 0.87283(11) 0.0213(3) -0.0502(3) 0.0244(8) Uani 1.00 1 d . . . C(6) C 0.91273(11) 0.0265(2) 0.0379(3) 0.0226(8) Uani 1.00 1 d . . . C(7) C 1.05708(11) -0.0785(3) 0.4460(2) 0.0237(8) Uani 1.00 1 d . . . C(8) C 0.99327(13) -0.2052(3) 0.3658(3) 0.0306(9) Uani 1.00 1 d . . . C(9) C 1.000000(10) -0.2819(4) 0.250000(10) 0.0373(14) Uani 1.00 2 d S . . C(10) C 0.90088(11) 0.3559(3) 0.1494(3) 0.0230(8) Uani 1.00 1 d . . . C(11) C 0.90101(12) 0.3346(3) 0.2916(3) 0.0316(9) Uani 1.00 1 d . . . C(12) C 0.95201(12) 0.4094(3) 0.1087(3) 0.0295(9) Uani 1.00 1 d . . . C(13) C 0.85982(12) 0.4497(3) 0.1215(3) 0.0331(9) Uani 1.00 1 d . . . C(14) C 0.79790(11) 0.1149(3) -0.1666(3) 0.0294(9) Uani 1.00 1 d . . . C(15) C 0.74844(12) 0.1429(4) -0.0957(3) 0.0536(13) Uani 1.00 1 d . . . C(16) C 0.80634(15) 0.2120(4) -0.2655(3) 0.0472(12) Uani 1.00 1 d . . . C(17) C 0.79334(14) -0.0068(3) -0.2310(3) 0.0426(11) Uani 1.00 1 d . . . H(1) H 0.8323 0.2940 -0.0178 0.029 Uiso 1.00 1 c R . . H(2) H 0.8703 -0.0493 -0.0991 0.029 Uiso 1.00 1 c R . . H(3) H 1.0649 -0.1469 0.5061 0.029 Uiso 1.00 1 c R . . H(4) H 1.0007 -0.2539 0.4436 0.037 Uiso 1.00 1 c R . . H(5) H 0.9517 -0.1749 0.3726 0.037 Uiso 1.00 1 c R . . H(6) H 0.9630 -0.3177 0.2410 0.045 Uiso 1.00 1 c R . . H(7) H 0.8676 0.3429 0.3237 0.038 Uiso 1.00 1 c R . . H(8) H 0.9226 0.3924 0.3295 0.038 Uiso 1.00 1 c R . . H(9) H 0.9133 0.2562 0.3092 0.039 Uiso 1.00 1 c R . . H(10) H 0.9782 0.3812 0.1619 0.036 Uiso 1.00 1 c R . . H(11) H 0.9501 0.4945 0.1137 0.036 Uiso 1.00 1 c R . . H(12) H 0.9592 0.3863 0.0255 0.036 Uiso 1.00 1 c R . . H(13) H 0.8700 0.4959 0.0515 0.040 Uiso 1.00 1 c R . . H(14) H 0.8559 0.5008 0.1916 0.040 Uiso 1.00 1 c R . . H(15) H 0.8285 0.4111 0.1040 0.040 Uiso 1.00 1 c R . . H(16) H 0.7344 0.0694 -0.0668 0.065 Uiso 1.00 1 c R . . H(17) H 0.7248 0.1820 -0.1487 0.064 Uiso 1.00 1 c R . . H(18) H 0.7559 0.1932 -0.0268 0.065 Uiso 1.00 1 c R . . H(19) H 0.7908 0.2845 -0.2387 0.057 Uiso 1.00 1 c R . . H(20) H 0.7918 0.1875 -0.3423 0.057 Uiso 1.00 1 c R . . H(21) H 0.8417 0.2247 -0.2762 0.057 Uiso 1.00 1 c R . . H(22) H 0.8134 -0.0079 -0.3044 0.052 Uiso 1.00 1 c R . . H(23) H 0.7588 -0.0206 -0.2520 0.052 Uiso 1.00 1 c R . . H(24) H 0.8047 -0.0680 -0.1760 0.052 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0168(2) 0.0143(3) 0.0216(3) 0.0000 -0.0008(2) 0.0000 O(1) 0.0203(9) 0.0187(12) 0.0308(11) 0.0029(9) -0.0090(9) -0.0030(10) N(1) 0.0231(12) 0.0161(15) 0.0227(13) -0.0035(10) 0.0009(11) 0.0004(11) C(1) 0.0186(14) 0.0181(17) 0.0231(15) -0.0007(12) 0.0008(12) -0.0003(13) C(2) 0.0194(14) 0.0180(17) 0.0232(15) 0.0010(12) -0.0002(12) 0.0015(13) C(3) 0.0207(15) 0.023(2) 0.0283(17) 0.0048(13) 0.0030(13) 0.0042(14) C(4) 0.0199(14) 0.0259(19) 0.0226(15) -0.0020(13) -0.0019(12) 0.0027(13) C(5) 0.0256(15) 0.0226(19) 0.0250(16) -0.0061(13) -0.0032(13) -0.0018(14) C(6) 0.0228(15) 0.0200(18) 0.0250(15) -0.0001(12) -0.0044(13) -0.0027(14) C(7) 0.0285(16) 0.0173(18) 0.0251(16) 0.0043(13) 0.0007(13) 0.0063(14) C(8) 0.048(2) 0.0187(18) 0.0252(16) -0.0123(15) 0.0018(15) 0.0021(14) C(9) 0.061(3) 0.017(2) 0.034(2) 0.0000 -0.002(2) 0.0000 C(10) 0.0228(14) 0.0185(18) 0.0278(16) 0.0043(12) 0.0003(13) -0.0020(14) C(11) 0.0348(18) 0.030(2) 0.0302(17) 0.0104(15) -0.0010(14) -0.0038(16) C(12) 0.0324(17) 0.0172(19) 0.0389(19) 0.0003(14) 0.0028(15) -0.0028(15) C(13) 0.0351(18) 0.028(2) 0.0356(19) 0.0125(15) -0.0013(15) -0.0043(16) C(14) 0.0231(15) 0.038(2) 0.0274(16) 0.0013(14) -0.0075(13) -0.0017(15) C(15) 0.0195(16) 0.099(4) 0.043(2) 0.002(2) -0.0097(16) -0.008(2) C(16) 0.054(2) 0.054(2) 0.034(2) 0.003(2) -0.0145(17) 0.0068(19) C(17) 0.0321(18) 0.057(2) 0.039(2) -0.0017(18) -0.0160(16) -0.0058(18) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni(1) O(1) 1.857(2) yes . . Ni(1) O(1) 1.857(2) yes . 7_755 Ni(1) N(1) 1.867(2) yes . . Ni(1) N(1) 1.867(2) yes . 7_755 O(1) C(1) 1.321(3) yes . . N(1) C(7) 1.296(3) yes . . N(1) C(8) 1.461(4) yes . . C(1) C(2) 1.444(4) yes . . C(1) C(6) 1.411(4) yes . . C(2) C(3) 1.389(4) yes . . C(2) C(10) 1.533(4) yes . . C(3) C(4) 1.408(4) yes . . C(4) C(5) 1.370(4) yes . . C(4) C(14) 1.546(4) yes . . C(5) C(6) 1.417(4) yes . . C(6) C(7) 1.425(4) yes . 7_755 C(8) C(9) 1.520(4) yes . . C(10) C(11) 1.547(4) yes . . C(10) C(12) 1.538(4) yes . . C(10) C(13) 1.534(4) yes . . C(14) C(15) 1.542(4) yes . . C(14) C(16) 1.533(5) yes . . C(14) C(17) 1.526(5) yes . . C(3) H(1) 0.957 no . . C(5) H(2) 0.948 no . . C(7) H(3) 1.019 no . . C(8) H(4) 1.017 no . . C(8) H(5) 1.151 no . . C(9) H(6) 1.058 no . . C(9) H(6) 1.058 no . 7_755 C(11) H(7) 0.950 no . . C(11) H(8) 0.950 no . . C(11) H(9) 0.950 no . . C(12) H(10) 0.950 no . . C(12) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(13) H(13) 0.950 no . . C(13) H(14) 0.950 no . . C(13) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(15) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(16) H(21) 0.950 no . . C(17) H(22) 0.950 no . . C(17) H(23) 0.950 no . . C(17) H(24) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Ni(1) O(1) 84.88(9) yes . . 7_755 O(1) Ni(1) N(1) 164.07(9) yes . . . O(1) Ni(1) N(1) 93.90(9) yes . . 7_755 O(1) Ni(1) N(1) 93.90(9) yes 7_755 . . O(1) Ni(1) N(1) 164.07(9) yes 7_755 . 7_755 N(1) Ni(1) N(1) 91.53(11) yes . . 7_755 Ni(1) O(1) C(1) 126.83(19) yes . . . Ni(1) N(1) C(7) 125.5(2) yes . . . Ni(1) N(1) C(8) 116.11(19) yes . . . C(7) N(1) C(8) 117.5(2) yes . . . O(1) C(1) C(2) 119.1(2) yes . . . O(1) C(1) C(6) 122.4(2) yes . . . C(2) C(1) C(6) 118.6(2) yes . . . C(1) C(2) C(3) 117.0(2) yes . . . C(1) C(2) C(10) 121.1(2) yes . . . C(3) C(2) C(10) 122.0(2) yes . . . C(2) C(3) C(4) 125.1(2) yes . . . C(3) C(4) C(5) 117.0(2) yes . . . C(3) C(4) C(14) 120.3(2) yes . . . C(5) C(4) C(14) 122.7(2) yes . . . C(4) C(5) C(6) 121.5(3) yes . . . C(1) C(6) C(5) 120.8(2) yes . . . C(1) C(6) C(7) 121.5(2) yes . . 7_755 C(5) C(6) C(7) 117.5(2) yes . . 7_755 N(1) C(7) C(6) 125.9(2) yes . . 7_755 N(1) C(8) C(9) 112.7(2) yes . . . C(8) C(9) C(8) 111.5(3) yes . . 7_755 C(2) C(10) C(11) 110.1(2) yes . . . C(2) C(10) C(12) 109.7(2) yes . . . C(2) C(10) C(13) 112.3(2) yes . . . C(11) C(10) C(12) 109.8(2) yes . . . C(11) C(10) C(13) 107.4(2) yes . . . C(12) C(10) C(13) 107.4(2) yes . . . C(4) C(14) C(15) 108.3(2) yes . . . C(4) C(14) C(16) 108.9(2) yes . . . C(4) C(14) C(17) 112.2(2) yes . . . C(15) C(14) C(16) 108.8(3) yes . . . C(15) C(14) C(17) 109.7(2) yes . . . C(16) C(14) C(17) 108.9(2) yes . . . C(2) C(3) H(1) 115.0 no . . . C(4) C(3) H(1) 119.8 no . . . C(4) C(5) H(2) 121.0 no . . . C(6) C(5) H(2) 117.2 no . . . N(1) C(7) H(3) 119.0 no . . . C(6) C(7) H(3) 115.1 no 7_755 . . N(1) C(8) H(4) 112.2 no . . . N(1) C(8) H(5) 105.2 no . . . C(9) C(8) H(4) 110.6 no . . . C(9) C(8) H(5) 109.2 no . . . H(4) C(8) H(5) 106.6 no . . . C(8) C(9) H(6) 100.3 no . . . C(8) C(9) H(6) 104.1 no . . 7_755 C(8) C(9) H(6) 104.1 no 7_755 . . C(8) C(9) H(6) 100.3 no 7_755 . 7_755 H(6) C(9) H(6) 135.8 no . . 7_755 C(10) C(11) H(7) 109.9 no . . . C(10) C(11) H(8) 108.7 no . . . C(10) C(11) H(9) 109.8 no . . . H(7) C(11) H(8) 109.5 no . . . H(7) C(11) H(9) 109.5 no . . . H(8) C(11) H(9) 109.5 no . . . C(10) C(12) H(10) 109.8 no . . . C(10) C(12) H(11) 108.9 no . . . C(10) C(12) H(12) 109.7 no . . . H(10) C(12) H(11) 109.5 no . . . H(10) C(12) H(12) 109.5 no . . . H(11) C(12) H(12) 109.5 no . . . C(10) C(13) H(13) 109.0 no . . . C(10) C(13) H(14) 109.2 no . . . C(10) C(13) H(15) 110.2 no . . . H(13) C(13) H(14) 109.5 no . . . H(13) C(13) H(15) 109.5 no . . . H(14) C(13) H(15) 109.5 no . . . C(14) C(15) H(16) 108.6 no . . . C(14) C(15) H(17) 110.6 no . . . C(14) C(15) H(18) 109.2 no . . . H(16) C(15) H(17) 109.5 no . . . H(16) C(15) H(18) 109.5 no . . . H(17) C(15) H(18) 109.5 no . . . C(14) C(16) H(19) 109.1 no . . . C(14) C(16) H(20) 110.0 no . . . C(14) C(16) H(21) 109.4 no . . . H(19) C(16) H(20) 109.5 no . . . H(19) C(16) H(21) 109.5 no . . . H(20) C(16) H(21) 109.5 no . . . C(14) C(17) H(22) 110.1 no . . . C(14) C(17) H(23) 109.1 no . . . C(14) C(17) H(24) 109.2 no . . . H(22) C(17) H(23) 109.5 no . . . H(22) C(17) H(24) 109.5 no . . . H(23) C(17) H(24) 109.5 no . . . #============================================================================== # 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 #============================================================================== # Attachment '- NisalpnOXfin.cif' #============================================================================== data__2 _database_code_depnum_ccdc_archive 'CCDC 801076' #TrackingRef '- NisalpnOXfin.cif' _audit_creation_date 2009-11-10 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H52 F6 N2 Ni O2 Sb ' _chemical_formula_moiety 'C40 H52 F6 N2 Ni O2 Sb ' _chemical_formula_weight 887.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.3915(2) _cell_length_b 15.7860(3) _cell_length_c 24.3478(5) _cell_angle_alpha 85.8860(7) _cell_angle_beta 84.3560(7) _cell_angle_gamma 72.8900(7) _cell_volume 4160.08(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 34674 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664.00 _exptl_absorpt_coefficient_mu 1.160 _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 0.814 _exptl_absorpt_correction_T_max 0.911 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_ambient_temperature 133(2) _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 40943 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 18351 _reflns_number_gt 15397 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1668 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 18351 _refine_ls_number_parameters 965 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1061P)^2^+6.2792P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 1.78 _refine_diff_density_min -0.87 _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 0.003 0.002 ; 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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sb Sb -0.587 1.546 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; 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 Sb(1) Sb 0.77347(2) 0.331959(16) 0.197181(12) 0.02877(8) Uani 1.00 1 d . . . Sb(2) Sb 0.59515(2) 0.896761(17) 0.228522(12) 0.02907(8) Uani 1.00 1 d . . . Ni(1) Ni 0.38634(4) 0.27048(3) 0.32530(2) 0.02186(11) Uani 1.00 1 d . . . Ni(2) Ni 0.40005(4) 0.58408(3) 0.103778(18) 0.01571(10) Uani 1.00 1 d . . . F(1) F 0.7888(4) 0.4356(2) 0.2205(2) 0.0909(15) Uani 1.00 1 d . . . F(2) F 0.8138(3) 0.3649(4) 0.12550(15) 0.1010(18) Uani 1.00 1 d . . . F(3) F 0.9406(2) 0.27569(19) 0.20804(13) 0.0450(6) Uani 1.00 1 d . . . F(4) F 0.7541(3) 0.2283(2) 0.1747(3) 0.135(2) Uani 1.00 1 d . . . F(5) F 0.6064(2) 0.38948(18) 0.18640(13) 0.0416(6) Uani 1.00 1 d . . . F(6) F 0.7289(4) 0.2990(4) 0.2685(2) 0.124(2) Uani 1.00 1 d . . . F(7) F 0.4548(4) 0.9358(3) 0.1919(3) 0.140(2) Uani 1.00 1 d . . . F(8) F 0.5363(3) 0.8060(2) 0.26266(18) 0.0678(10) Uani 1.00 1 d . . . F(9) F 0.6507(3) 0.9881(2) 0.19397(16) 0.0656(10) Uani 1.00 1 d . . . F(10) F 0.7354(4) 0.8591(3) 0.2660(2) 0.113(2) Uani 1.00 1 d . . . F(11) F 0.5210(6) 0.9751(3) 0.2831(2) 0.121(2) Uani 1.00 1 d . . . F(12) F 0.6668(5) 0.8168(3) 0.1745(2) 0.1056(17) Uani 1.00 1 d . . . O(1) O 0.2901(2) 0.36074(18) 0.36776(11) 0.0250(5) Uani 1.00 1 d . . . O(2) O 0.4956(2) 0.24921(19) 0.37900(12) 0.0282(5) Uani 1.00 1 d . . . O(3) O 0.2411(2) 0.65665(16) 0.10768(11) 0.0206(5) Uani 1.00 1 d . . . O(4) O 0.3343(2) 0.49867(15) 0.08439(11) 0.0186(4) Uani 1.00 1 d . . . N(1) N 0.2575(2) 0.2673(2) 0.28478(13) 0.0212(5) Uani 1.00 1 d . . . N(2) N 0.5025(2) 0.2014(2) 0.27552(13) 0.0245(6) Uani 1.00 1 d . . . N(3) N 0.4540(2) 0.65967(18) 0.14329(12) 0.0167(5) Uani 1.00 1 d . . . N(4) N 0.5590(2) 0.52603(19) 0.07599(12) 0.0180(5) Uani 1.00 1 d . . . C(1) C 0.1817(3) 0.4159(2) 0.35965(15) 0.0222(7) Uani 1.00 1 d . . . C(2) C 0.1331(3) 0.4929(2) 0.39214(15) 0.0240(7) Uani 1.00 1 d . . . C(3) C 0.0177(3) 0.5475(2) 0.38136(16) 0.0263(7) Uani 1.00 1 d . . . C(4) C -0.0569(3) 0.5331(2) 0.34188(16) 0.0257(7) Uani 1.00 1 d . . . C(5) C -0.0099(3) 0.4575(2) 0.31212(16) 0.0237(7) Uani 1.00 1 d . . . C(6) C 0.1071(3) 0.3997(2) 0.31942(15) 0.0231(7) Uani 1.00 1 d . . . C(7) C 0.1484(3) 0.3228(2) 0.28751(15) 0.0225(7) Uani 1.00 1 d . . . C(8) C 0.2779(3) 0.1866(2) 0.25353(16) 0.0240(7) Uani 1.00 1 d . . . C(9) C 0.3739(3) 0.1807(2) 0.20498(16) 0.0272(7) Uani 1.00 1 d . . . C(10) C 0.4764(3) 0.2190(2) 0.21684(17) 0.0286(8) Uani 1.00 1 d . . . C(11) C 0.6024(3) 0.1426(2) 0.28749(17) 0.0268(7) Uani 1.00 1 d . . . C(12) C 0.6432(3) 0.1215(2) 0.34179(17) 0.0274(7) Uani 1.00 1 d . . . C(13) C 0.5908(3) 0.1806(2) 0.38529(17) 0.0273(7) Uani 1.00 1 d . . . C(14) C 0.6459(3) 0.1626(3) 0.43731(18) 0.0309(8) Uani 1.00 1 d . . . C(15) C 0.7354(3) 0.0823(3) 0.44383(19) 0.0331(9) Uani 1.00 1 d . . . C(16) C 0.7798(3) 0.0193(2) 0.40291(19) 0.0306(8) Uani 1.00 1 d . . . C(17) C 0.7374(3) 0.0423(2) 0.35098(18) 0.0293(8) Uani 1.00 1 d . . . C(18) C 0.2058(3) 0.5115(2) 0.43708(17) 0.0307(8) Uani 1.00 1 d . . . C(19) C 0.2241(4) 0.4364(3) 0.48122(18) 0.0381(9) Uani 1.00 1 d . . . C(20) C 0.3310(4) 0.5203(3) 0.4126(2) 0.0364(9) Uani 1.00 1 d . . . C(21) C 0.1375(4) 0.5986(3) 0.4656(2) 0.0467(12) Uani 1.00 1 d . . . C(22) C -0.1849(4) 0.5951(2) 0.33271(18) 0.0326(9) Uani 1.00 1 d . . . C(23) C -0.2806(4) 0.5457(3) 0.3504(2) 0.0458(11) Uani 1.00 1 d . . . C(24) C -0.1898(5) 0.6239(3) 0.2712(2) 0.0464(12) Uani 1.00 1 d . . . C(25) C -0.2168(4) 0.6791(3) 0.3657(2) 0.0416(11) Uani 1.00 1 d . . . C(26) C 0.6009(4) 0.2270(3) 0.48397(19) 0.0407(11) Uani 1.00 1 d . . . C(27) C 0.4705(4) 0.2241(4) 0.5072(2) 0.0560(15) Uani 1.00 1 d . . . C(28) C 0.6004(5) 0.3211(3) 0.4633(2) 0.0524(14) Uani 1.00 1 d . . . C(29) C 0.6851(5) 0.2014(4) 0.5318(2) 0.0550(15) Uani 1.00 1 d . . . C(30) C 0.8640(4) -0.0739(2) 0.4162(2) 0.0344(9) Uani 1.00 1 d . . . C(31) C 0.7787(4) -0.1292(3) 0.4399(2) 0.0430(10) Uani 1.00 1 d . . . C(32) C 0.9382(4) -0.1168(3) 0.3648(2) 0.0442(11) Uani 1.00 1 d . . . C(33) C 0.9521(4) -0.0729(3) 0.4592(2) 0.0489(12) Uani 1.00 1 d . . . C(34) C 0.1989(3) 0.7398(2) 0.11786(15) 0.0192(6) Uani 1.00 1 d . . . C(35) C 0.0759(3) 0.7890(2) 0.10401(16) 0.0211(6) Uani 1.00 1 d . . . C(36) C 0.0333(3) 0.8761(2) 0.11712(17) 0.0244(7) Uani 1.00 1 d . . . C(37) C 0.1029(3) 0.9210(2) 0.14260(17) 0.0238(7) Uani 1.00 1 d . . . C(38) C 0.2218(3) 0.8745(2) 0.15467(16) 0.0221(7) Uani 1.00 1 d . . . C(39) C 0.2702(3) 0.7853(2) 0.14246(15) 0.0198(6) Uani 1.00 1 d . . . C(40) C 0.3925(3) 0.7384(2) 0.15751(15) 0.0196(6) Uani 1.00 1 d . . . C(41) C 0.5751(3) 0.6189(2) 0.16631(16) 0.0225(7) Uani 1.00 1 d . . . C(42) C 0.6784(3) 0.6080(2) 0.12075(17) 0.0252(7) Uani 1.00 1 d . . . C(43) C 0.6452(3) 0.5801(2) 0.06680(16) 0.0219(7) Uani 1.00 1 d . . . C(44) C 0.5944(3) 0.4466(2) 0.05778(15) 0.0189(6) Uani 1.00 1 d . . . C(45) C 0.5207(3) 0.3875(2) 0.05857(14) 0.0175(6) Uani 1.00 1 d . . . C(46) C 0.3919(3) 0.4159(2) 0.07313(14) 0.0169(6) Uani 1.00 1 d . . . C(47) C 0.3234(3) 0.3521(2) 0.07424(14) 0.0172(6) Uani 1.00 1 d . . . C(48) C 0.3880(3) 0.2674(2) 0.05872(14) 0.0193(6) Uani 1.00 1 d . . . C(49) C 0.5159(3) 0.2383(2) 0.04213(14) 0.0189(6) Uani 1.00 1 d . . . C(50) C 0.5807(3) 0.2997(2) 0.04273(15) 0.0198(6) Uani 1.00 1 d . . . C(51) C -0.0014(3) 0.7428(2) 0.07535(17) 0.0236(7) Uani 1.00 1 d . . . C(52) C -0.0283(3) 0.6681(2) 0.11340(19) 0.0302(8) Uani 1.00 1 d . . . C(53) C -0.1256(3) 0.8086(2) 0.0610(2) 0.0319(8) Uani 1.00 1 d . . . C(54) C 0.0685(3) 0.7061(2) 0.02043(17) 0.0265(7) Uani 1.00 1 d . . . C(55) C 0.0458(3) 1.0184(2) 0.15647(19) 0.0293(8) Uani 1.00 1 d . . . C(56) C -0.0613(5) 1.0238(3) 0.2008(2) 0.0605(16) Uani 1.00 1 d . . . C(57) C 0.0007(6) 1.0729(3) 0.1047(2) 0.0633(17) Uani 1.00 1 d . . . C(58) C 0.1368(4) 1.0580(3) 0.1792(3) 0.0551(15) Uani 1.00 1 d . . . C(59) C 0.1847(3) 0.3775(2) 0.09189(15) 0.0192(6) Uani 1.00 1 d . . . C(60) C 0.1588(3) 0.4163(2) 0.14968(16) 0.0244(7) Uani 1.00 1 d . . . C(61) C 0.1338(3) 0.2976(2) 0.09454(17) 0.0250(7) Uani 1.00 1 d . . . C(62) C 0.1126(3) 0.4464(2) 0.05023(16) 0.0222(7) Uani 1.00 1 d . . . C(63) C 0.5758(3) 0.1425(2) 0.02526(16) 0.0236(7) Uani 1.00 1 d . . . C(64) C 0.5599(4) 0.0786(2) 0.07398(18) 0.0360(9) Uani 1.00 1 d . . . C(65) C 0.5139(4) 0.1253(2) -0.02413(19) 0.0343(9) Uani 1.00 1 d . . . C(66) C 0.7136(3) 0.1247(2) 0.0089(2) 0.0323(8) Uani 1.00 1 d . . . C(67) C 0.2485(9) 0.7930(6) 0.2993(3) 0.105(2) Uani 1.00 1 d . . . C(68) C 0.2743(6) 0.7071(5) 0.2842(2) 0.0759(17) Uani 1.00 1 d . . . C(69) C 0.1690(9) 0.6838(7) 0.2622(2) 0.111(2) Uani 1.00 1 d . . . C(70) C 0.1953(7) 0.5994(6) 0.2481(2) 0.095(2) Uani 1.00 1 d . . . C(71) C 0.3209(7) 0.5281(7) 0.2508(2) 0.110(2) Uani 1.00 1 d . . . C(72) C 0.4067(8) 0.5557(6) 0.2710(3) 0.094(2) Uani 1.00 1 d . . . C(73) C 0.3785(6) 0.6403(4) 0.2854(2) 0.0649(15) Uani 1.00 1 d . . . C(74) C 0.3196(10) 0.0479(8) 0.3889(5) 0.147(4) Uani 1.00 1 d . . . C(75) C 0.2010(12) 0.1124(7) 0.3894(4) 0.079(3) Uani 0.50 1 d P . . C(75a) C 0.0749(11) 0.1635(8) 0.3838(4) 0.077(2) Uani 0.50 1 d P . . C(76) C 0.1567(9) 0.1902(5) 0.4123(2) 0.086(2) Uani 1.00 1 d . . . C(77) C 0.0304(14) 0.2442(8) 0.4073(5) 0.086(3) Uani 0.50 1 d P . . C(77a) C 0.2756(14) 0.1258(10) 0.4070(5) 0.096(3) Uani 0.50 1 d P . . C(78) C -0.0461(9) 0.2213(7) 0.3775(4) 0.116(3) Uani 1.00 1 d . . . C(79) C 0.0089(14) 0.1387(11) 0.3491(6) 0.109(4) Uani 0.50 1 d P . . C(79a) C 0.2239(17) 0.0193(9) 0.3590(6) 0.122(4) Uani 0.50 1 d P . . C(80) C 0.1171(10) 0.0822(6) 0.3579(3) 0.103(2) Uani 1.00 1 d . . . H(1) H -0.0142 0.5992 0.4022 0.032 Uiso 1.00 1 c R . . H(2) H -0.0583 0.4446 0.2861 0.028 Uiso 1.00 1 c R . . H(3) H 0.0900 0.3112 0.2661 0.027 Uiso 1.00 1 c R . . H(4) H 0.1991 0.1863 0.2398 0.029 Uiso 1.00 1 c R . . H(5) H 0.3048 0.1337 0.2787 0.029 Uiso 1.00 1 c R . . H(6) H 0.3333 0.2131 0.1724 0.033 Uiso 1.00 1 c R . . H(7) H 0.4103 0.1177 0.1959 0.033 Uiso 1.00 1 c R . . H(8) H 0.5519 0.1918 0.1930 0.034 Uiso 1.00 1 c R . . H(9) H 0.4514 0.2838 0.2083 0.034 Uiso 1.00 1 c R . . H(10) H 0.6532 0.1107 0.2580 0.032 Uiso 1.00 1 c R . . H(11) H 0.7696 0.0686 0.4786 0.040 Uiso 1.00 1 c R . . H(12) H 0.7720 0.0043 0.3213 0.035 Uiso 1.00 1 c R . . H(13) H 0.1550 0.4502 0.5097 0.046 Uiso 1.00 1 c R . . H(14) H 0.3013 0.4295 0.4981 0.046 Uiso 1.00 1 c R . . H(15) H 0.2280 0.3810 0.4643 0.046 Uiso 1.00 1 c R . . H(16) H 0.3926 0.4620 0.4136 0.044 Uiso 1.00 1 c R . . H(17) H 0.3562 0.5610 0.4343 0.044 Uiso 1.00 1 c R . . H(18) H 0.3244 0.5437 0.3743 0.044 Uiso 1.00 1 c R . . H(19) H 0.1619 0.6479 0.4459 0.056 Uiso 1.00 1 c R . . H(20) H 0.1588 0.5938 0.5039 0.056 Uiso 1.00 1 c R . . H(21) H 0.0484 0.6094 0.4650 0.056 Uiso 1.00 1 c R . . H(22) H -0.2939 0.5153 0.3189 0.055 Uiso 1.00 1 c R . . H(23) H -0.3584 0.5881 0.3634 0.055 Uiso 1.00 1 c R . . H(24) H -0.2508 0.5019 0.3803 0.055 Uiso 1.00 1 c R . . H(25) H -0.1646 0.6782 0.2645 0.056 Uiso 1.00 1 c R . . H(26) H -0.2741 0.6351 0.2606 0.056 Uiso 1.00 1 c R . . H(27) H -0.1340 0.5768 0.2490 0.056 Uiso 1.00 1 c R . . H(28) H -0.2574 0.6687 0.4019 0.050 Uiso 1.00 1 c R . . H(29) H -0.2722 0.7283 0.3456 0.050 Uiso 1.00 1 c R . . H(30) H -0.1410 0.6940 0.3709 0.050 Uiso 1.00 1 c R . . H(31) H 0.4084 0.2680 0.4867 0.067 Uiso 1.00 1 c R . . H(32) H 0.4581 0.2377 0.5464 0.067 Uiso 1.00 1 c R . . H(33) H 0.4625 0.1648 0.5033 0.067 Uiso 1.00 1 c R . . H(34) H 0.6805 0.3297 0.4680 0.063 Uiso 1.00 1 c R . . H(35) H 0.5355 0.3643 0.4846 0.063 Uiso 1.00 1 c R . . H(36) H 0.5849 0.3293 0.4241 0.063 Uiso 1.00 1 c R . . H(37) H 0.6550 0.1618 0.5587 0.066 Uiso 1.00 1 c R . . H(38) H 0.6847 0.2551 0.5498 0.066 Uiso 1.00 1 c R . . H(39) H 0.7693 0.1710 0.5174 0.066 Uiso 1.00 1 c R . . H(40) H 0.7658 -0.1246 0.4801 0.052 Uiso 1.00 1 c R . . H(41) H 0.8166 -0.1915 0.4311 0.052 Uiso 1.00 1 c R . . H(42) H 0.6993 -0.1070 0.4238 0.052 Uiso 1.00 1 c R . . H(43) H 0.8918 -0.1499 0.3478 0.053 Uiso 1.00 1 c R . . H(44) H 1.0169 -0.1574 0.3750 0.053 Uiso 1.00 1 c R . . H(45) H 0.9538 -0.0706 0.3384 0.053 Uiso 1.00 1 c R . . H(46) H 1.0282 -0.0641 0.4406 0.059 Uiso 1.00 1 c R . . H(47) H 0.9714 -0.1295 0.4807 0.059 Uiso 1.00 1 c R . . H(48) H 0.9134 -0.0243 0.4839 0.059 Uiso 1.00 1 c R . . H(49) H -0.0478 0.9085 0.1086 0.029 Uiso 1.00 1 c R . . H(50) H 0.2706 0.9035 0.1713 0.027 Uiso 1.00 1 c R . . H(51) H 0.4308 0.7679 0.1797 0.024 Uiso 1.00 1 c R . . H(52) H 0.5770 0.5602 0.1842 0.027 Uiso 1.00 1 c R . . H(53) H 0.5867 0.6570 0.1947 0.027 Uiso 1.00 1 c R . . H(54) H 0.7526 0.5628 0.1331 0.030 Uiso 1.00 1 c R . . H(55) H 0.6987 0.6648 0.1139 0.030 Uiso 1.00 1 c R . . H(56) H 0.6076 0.6339 0.0439 0.026 Uiso 1.00 1 c R . . H(57) H 0.7215 0.5458 0.0460 0.026 Uiso 1.00 1 c R . . H(58) H 0.6771 0.4258 0.0425 0.023 Uiso 1.00 1 c R . . H(59) H 0.3431 0.2252 0.0592 0.023 Uiso 1.00 1 c R . . H(60) H 0.6667 0.2828 0.0323 0.024 Uiso 1.00 1 c R . . H(61) H 0.0372 0.6127 0.1068 0.036 Uiso 1.00 1 c R . . H(62) H -0.1075 0.6605 0.1058 0.036 Uiso 1.00 1 c R . . H(63) H -0.0321 0.6831 0.1520 0.036 Uiso 1.00 1 c R . . H(64) H -0.1876 0.8095 0.0921 0.038 Uiso 1.00 1 c R . . H(65) H -0.1523 0.7900 0.0280 0.038 Uiso 1.00 1 c R . . H(66) H -0.1157 0.8681 0.0539 0.038 Uiso 1.00 1 c R . . H(67) H 0.0458 0.7513 -0.0095 0.032 Uiso 1.00 1 c R . . H(68) H 0.0466 0.6531 0.0122 0.032 Uiso 1.00 1 c R . . H(69) H 0.1575 0.6907 0.0237 0.032 Uiso 1.00 1 c R . . H(70) H -0.1376 1.0324 0.1829 0.073 Uiso 1.00 1 c R . . H(71) H -0.0701 1.0739 0.2240 0.073 Uiso 1.00 1 c R . . H(72) H -0.0445 0.9687 0.2237 0.073 Uiso 1.00 1 c R . . H(73) H 0.0671 1.0946 0.0858 0.076 Uiso 1.00 1 c R . . H(74) H -0.0701 1.1235 0.1149 0.076 Uiso 1.00 1 c R . . H(75) H -0.0238 1.0359 0.0800 0.076 Uiso 1.00 1 c R . . H(76) H 0.1329 1.0493 0.2195 0.066 Uiso 1.00 1 c R . . H(77) H 0.1158 1.1216 0.1691 0.066 Uiso 1.00 1 c R . . H(78) H 0.2204 1.0285 0.1635 0.066 Uiso 1.00 1 c R . . H(79) H 0.1627 0.3682 0.1779 0.029 Uiso 1.00 1 c R . . H(80) H 0.0766 0.4591 0.1527 0.029 Uiso 1.00 1 c R . . H(81) H 0.2207 0.4461 0.1552 0.029 Uiso 1.00 1 c R . . H(82) H 0.1055 0.2922 0.0586 0.030 Uiso 1.00 1 c R . . H(83) H 0.0646 0.3059 0.1229 0.030 Uiso 1.00 1 c R . . H(84) H 0.1987 0.2436 0.1038 0.030 Uiso 1.00 1 c R . . H(85) H 0.1050 0.5062 0.0615 0.027 Uiso 1.00 1 c R . . H(86) H 0.0303 0.4391 0.0492 0.027 Uiso 1.00 1 c R . . H(87) H 0.1566 0.4376 0.0135 0.027 Uiso 1.00 1 c R . . H(88) H 0.6302 0.0663 0.0965 0.043 Uiso 1.00 1 c R . . H(89) H 0.5555 0.0231 0.0600 0.043 Uiso 1.00 1 c R . . H(90) H 0.4837 0.1057 0.0966 0.043 Uiso 1.00 1 c R . . H(91) H 0.4439 0.1031 -0.0108 0.041 Uiso 1.00 1 c R . . H(92) H 0.5734 0.0811 -0.0470 0.041 Uiso 1.00 1 c R . . H(93) H 0.4846 0.1807 -0.0462 0.041 Uiso 1.00 1 c R . . H(94) H 0.7264 0.1383 -0.0308 0.039 Uiso 1.00 1 c R . . H(95) H 0.7562 0.0621 0.0172 0.039 Uiso 1.00 1 c R . . H(96) H 0.7466 0.1622 0.0297 0.039 Uiso 1.00 1 c R . . H(97) H 0.2678 0.8298 0.2675 0.127 Uiso 1.00 1 c R . . H(98) H 0.2985 0.7953 0.3294 0.127 Uiso 1.00 1 c R . . H(99) H 0.1610 0.8154 0.3117 0.127 Uiso 1.00 1 c R . . H(100) H 0.0905 0.7255 0.2586 0.133 Uiso 1.00 1 c R . . H(101) H 0.1304 0.5817 0.2352 0.113 Uiso 1.00 1 c R . . H(102) H 0.3355 0.4695 0.2391 0.132 Uiso 1.00 1 c R . . H(103) H 0.4866 0.5163 0.2751 0.112 Uiso 1.00 1 c R . . H(104) H 0.4447 0.6555 0.2990 0.078 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb(1) 0.02492(15) 0.02160(13) 0.03949(17) -0.00590(10) -0.00354(11) -0.00167(11) Sb(2) 0.02680(15) 0.02346(14) 0.03950(17) -0.00911(10) -0.00855(11) -0.00238(11) Ni(1) 0.0180(2) 0.0275(2) 0.0218(2) -0.00747(18) -0.00293(18) -0.00655(19) Ni(2) 0.0106(2) 0.0152(2) 0.0218(2) -0.00378(15) -0.00256(16) -0.00256(16) F(1) 0.099(3) 0.0431(18) 0.143(4) -0.0144(18) -0.074(3) -0.026(2) F(2) 0.0304(17) 0.213(5) 0.0414(19) -0.014(2) -0.0045(14) 0.023(2) F(3) 0.0309(13) 0.0474(15) 0.0559(17) -0.0094(11) -0.0110(12) 0.0046(13) F(4) 0.045(2) 0.0435(19) 0.321(8) 0.0019(16) -0.040(3) -0.074(3) F(5) 0.0279(12) 0.0356(13) 0.0561(17) -0.0001(10) -0.0041(11) -0.0048(12) F(6) 0.061(2) 0.174(5) 0.099(3) -0.003(2) 0.006(2) 0.087(3) F(7) 0.102(3) 0.069(2) 0.279(8) -0.047(2) -0.137(4) 0.055(3) F(8) 0.068(2) 0.0561(19) 0.091(2) -0.0406(17) -0.0062(19) 0.0118(19) F(9) 0.080(2) 0.066(2) 0.068(2) -0.0474(19) -0.0310(19) 0.0292(18) F(10) 0.105(3) 0.079(2) 0.178(5) -0.054(2) -0.100(3) 0.067(3) F(11) 0.156(5) 0.091(3) 0.122(4) -0.055(3) 0.066(3) -0.060(3) F(12) 0.142(4) 0.090(3) 0.084(3) -0.039(3) 0.041(3) -0.044(2) O(1) 0.0213(12) 0.0299(13) 0.0246(13) -0.0057(10) -0.0062(10) -0.0076(10) O(2) 0.0192(12) 0.0347(14) 0.0304(14) -0.0043(10) -0.0051(10) -0.0116(11) O(3) 0.0140(11) 0.0182(11) 0.0297(13) -0.0033(8) -0.0038(9) -0.0051(9) O(4) 0.0131(10) 0.0163(10) 0.0273(12) -0.0042(8) -0.0028(9) -0.0049(9) N(1) 0.0216(14) 0.0244(14) 0.0197(14) -0.0088(11) -0.0024(11) -0.0041(11) N(2) 0.0227(15) 0.0309(16) 0.0233(15) -0.0119(12) -0.0002(12) -0.0071(12) N(3) 0.0118(12) 0.0175(12) 0.0216(14) -0.0050(9) -0.0037(10) -0.0005(10) N(4) 0.0134(13) 0.0198(13) 0.0217(14) -0.0061(10) -0.0020(10) 0.0001(11) C(1) 0.0200(16) 0.0272(17) 0.0211(17) -0.0092(13) -0.0014(13) -0.0034(14) C(2) 0.0249(18) 0.0273(17) 0.0206(17) -0.0077(14) -0.0029(14) -0.0036(14) C(3) 0.0294(19) 0.0259(17) 0.0240(18) -0.0068(14) -0.0042(15) -0.0045(14) C(4) 0.0258(18) 0.0251(17) 0.0251(18) -0.0055(14) -0.0024(14) -0.0013(14) C(5) 0.0256(18) 0.0263(17) 0.0216(17) -0.0099(14) -0.0059(14) -0.0018(14) C(6) 0.0233(17) 0.0262(17) 0.0218(17) -0.0091(13) -0.0043(14) -0.0028(14) C(7) 0.0224(17) 0.0267(17) 0.0199(16) -0.0094(13) -0.0018(13) -0.0010(14) C(8) 0.0254(18) 0.0239(16) 0.0252(18) -0.0103(13) -0.0030(14) -0.0036(14) C(9) 0.0260(19) 0.0294(18) 0.0238(18) -0.0032(14) -0.0040(14) -0.0017(15) C(10) 0.030(2) 0.0318(19) 0.0249(18) -0.0109(15) 0.0011(15) -0.0035(15) C(11) 0.0229(18) 0.0329(19) 0.0276(19) -0.0120(15) 0.0011(14) -0.0078(15) C(12) 0.0208(17) 0.0349(19) 0.0302(19) -0.0108(14) -0.0063(15) -0.0078(16) C(13) 0.0184(17) 0.0346(19) 0.031(2) -0.0095(14) -0.0018(14) -0.0097(16) C(14) 0.0195(17) 0.042(2) 0.033(2) -0.0077(15) -0.0045(15) -0.0139(18) C(15) 0.0211(18) 0.046(2) 0.034(2) -0.0081(16) -0.0095(16) -0.0083(18) C(16) 0.0218(18) 0.034(2) 0.039(2) -0.0106(15) -0.0063(16) -0.0073(17) C(17) 0.0223(18) 0.034(2) 0.034(2) -0.0100(15) -0.0024(15) -0.0121(16) C(18) 0.029(2) 0.037(2) 0.028(2) -0.0107(16) -0.0030(16) -0.0099(16) C(19) 0.043(2) 0.052(2) 0.0233(19) -0.019(2) -0.0063(17) -0.0041(18) C(20) 0.033(2) 0.046(2) 0.037(2) -0.0187(18) -0.0035(18) -0.0090(19) C(21) 0.038(2) 0.056(2) 0.047(2) -0.006(2) -0.008(2) -0.033(2) C(22) 0.031(2) 0.0284(19) 0.034(2) 0.0029(15) -0.0097(17) -0.0081(16) C(23) 0.024(2) 0.049(2) 0.061(3) -0.0024(18) -0.006(2) -0.010(2) C(24) 0.061(3) 0.032(2) 0.038(2) 0.007(2) -0.022(2) -0.0064(19) C(25) 0.042(2) 0.035(2) 0.038(2) 0.0082(18) -0.012(2) -0.0118(19) C(26) 0.029(2) 0.053(2) 0.037(2) 0.0016(19) -0.0149(18) -0.021(2) C(27) 0.035(2) 0.094(4) 0.035(2) -0.006(2) -0.001(2) -0.024(2) C(28) 0.050(3) 0.046(2) 0.061(3) -0.000(2) -0.027(2) -0.029(2) C(29) 0.051(3) 0.063(3) 0.047(2) 0.003(2) -0.025(2) -0.025(2) C(30) 0.029(2) 0.034(2) 0.041(2) -0.0071(16) -0.0111(18) -0.0032(18) C(31) 0.048(2) 0.038(2) 0.047(2) -0.019(2) -0.006(2) -0.005(2) C(32) 0.035(2) 0.040(2) 0.050(2) 0.0025(19) -0.002(2) -0.007(2) C(33) 0.038(2) 0.046(2) 0.064(3) -0.006(2) -0.025(2) -0.005(2) C(34) 0.0163(15) 0.0197(15) 0.0216(16) -0.0048(12) -0.0027(12) -0.0013(12) C(35) 0.0136(15) 0.0220(16) 0.0279(18) -0.0047(12) -0.0025(13) -0.0031(14) C(36) 0.0171(16) 0.0233(16) 0.0320(19) -0.0030(13) -0.0058(14) -0.0031(14) C(37) 0.0214(17) 0.0183(15) 0.0312(19) -0.0038(13) -0.0035(14) -0.0037(14) C(38) 0.0205(16) 0.0201(15) 0.0268(18) -0.0056(12) -0.0037(13) -0.0061(13) C(39) 0.0164(15) 0.0191(15) 0.0234(17) -0.0034(12) -0.0030(13) -0.0026(13) C(40) 0.0190(16) 0.0203(15) 0.0222(16) -0.0083(12) -0.0050(13) -0.0025(13) C(41) 0.0159(16) 0.0219(16) 0.0293(18) -0.0021(12) -0.0100(14) -0.0005(14) C(42) 0.0148(16) 0.0240(16) 0.039(2) -0.0068(13) -0.0063(14) -0.0026(15) C(43) 0.0163(15) 0.0221(15) 0.0292(18) -0.0091(12) 0.0006(13) -0.0018(14) C(44) 0.0117(14) 0.0202(15) 0.0231(16) -0.0012(11) -0.0035(12) -0.0013(13) C(45) 0.0143(15) 0.0182(14) 0.0199(16) -0.0035(11) -0.0034(12) -0.0020(12) C(46) 0.0156(15) 0.0189(14) 0.0169(15) -0.0048(11) -0.0041(12) -0.0025(12) C(47) 0.0147(15) 0.0193(14) 0.0174(15) -0.0047(11) -0.0013(12) 0.0002(12) C(48) 0.0197(16) 0.0203(15) 0.0197(16) -0.0083(12) -0.0026(12) -0.0003(13) C(49) 0.0198(16) 0.0172(14) 0.0186(15) -0.0026(12) -0.0039(12) -0.0024(12) C(50) 0.0148(15) 0.0225(16) 0.0212(16) -0.0029(12) -0.0026(12) -0.0035(13) C(51) 0.0122(15) 0.0263(17) 0.0328(19) -0.0044(12) -0.0046(13) -0.0067(15) C(52) 0.0175(17) 0.0294(18) 0.045(2) -0.0086(14) -0.0003(16) -0.0037(17) C(53) 0.0144(17) 0.034(2) 0.047(2) -0.0008(14) -0.0100(16) -0.0100(18) C(54) 0.0189(17) 0.0304(18) 0.032(2) -0.0059(14) -0.0061(14) -0.0097(15) C(55) 0.0223(18) 0.0201(16) 0.044(2) -0.0009(13) -0.0049(16) -0.0084(16) C(56) 0.054(3) 0.036(2) 0.086(4) -0.011(2) 0.029(3) -0.026(2) C(57) 0.092(4) 0.025(2) 0.066(3) 0.004(2) -0.036(3) -0.003(2) C(58) 0.040(2) 0.026(2) 0.100(4) -0.0013(18) -0.024(2) -0.020(2) C(59) 0.0139(15) 0.0203(15) 0.0237(17) -0.0062(12) -0.0012(12) 0.0016(13) C(60) 0.0211(17) 0.0285(17) 0.0246(18) -0.0086(13) -0.0007(14) -0.0026(14) C(61) 0.0226(17) 0.0254(17) 0.0297(19) -0.0115(14) -0.0035(14) 0.0012(14) C(62) 0.0141(15) 0.0245(16) 0.0279(18) -0.0052(12) -0.0043(13) 0.0012(14) C(63) 0.0255(18) 0.0177(15) 0.0250(18) -0.0027(13) 0.0002(14) -0.0017(13) C(64) 0.051(2) 0.0201(17) 0.032(2) -0.0045(17) 0.0052(19) -0.0018(16) C(65) 0.035(2) 0.033(2) 0.035(2) -0.0091(17) 0.0013(17) -0.0112(17) C(66) 0.0253(19) 0.0210(17) 0.048(2) -0.0014(14) -0.0010(17) -0.0100(17) C(67) 0.097(6) 0.119(6) 0.093(6) -0.027(5) 0.012(5) -0.001(5) C(68) 0.078(4) 0.111(4) 0.038(3) -0.034(3) 0.008(2) 0.011(3) C(69) 0.134(6) 0.200(7) 0.045(3) -0.128(5) 0.005(4) 0.010(5) C(70) 0.101(4) 0.178(7) 0.042(3) -0.104(5) -0.004(3) 0.013(4) C(71) 0.090(4) 0.238(8) 0.036(3) -0.109(5) -0.014(3) 0.044(4) C(72) 0.086(5) 0.110(5) 0.074(5) -0.021(4) 0.003(4) 0.018(4) C(73) 0.071(3) 0.085(3) 0.034(2) -0.023(3) 0.017(2) 0.003(2) C(74) 0.133(7) 0.137(7) 0.143(10) -0.029(5) 0.034(6) 0.071(7) C(75) 0.108(7) 0.081(6) 0.060(7) -0.057(5) 0.024(6) 0.011(5) C(75a) 0.103(7) 0.088(6) 0.053(6) -0.062(5) 0.019(6) 0.016(5) C(76) 0.135(5) 0.089(4) 0.055(3) -0.072(4) -0.005(4) 0.019(3) C(77) 0.148(9) 0.066(7) 0.044(6) -0.042(6) 0.029(7) 0.004(5) C(77a) 0.124(8) 0.154(10) 0.035(6) -0.087(7) -0.007(7) 0.039(7) C(78) 0.103(5) 0.132(7) 0.118(7) -0.061(5) 0.015(5) 0.040(5) C(79) 0.127(9) 0.175(12) 0.076(9) -0.132(7) 0.023(8) -0.008(8) C(79a) 0.230(13) 0.061(7) 0.068(9) -0.056(6) 0.053(10) 0.009(6) C(80) 0.180(7) 0.104(5) 0.054(4) -0.096(5) 0.017(5) -0.008(4) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sb(1) F(1) 1.831(4) yes . . Sb(1) F(2) 1.839(3) yes . . Sb(1) F(3) 1.885(2) yes . . Sb(1) F(4) 1.842(5) yes . . Sb(1) F(5) 1.888(2) yes . . Sb(1) F(6) 1.843(5) yes . . Sb(2) F(7) 1.831(6) yes . . Sb(2) F(8) 1.865(4) yes . . Sb(2) F(9) 1.857(4) yes . . Sb(2) F(10) 1.841(5) yes . . Sb(2) F(11) 1.846(5) yes . . Sb(2) F(12) 1.847(4) yes . . Ni(1) O(1) 1.836(2) yes . . Ni(1) O(2) 1.839(2) yes . . Ni(1) N(1) 1.862(3) yes . . Ni(1) N(2) 1.853(2) yes . . Ni(2) O(3) 1.834(2) yes . . Ni(2) O(4) 1.832(2) yes . . Ni(2) N(3) 1.855(3) yes . . Ni(2) N(4) 1.857(2) yes . . O(1) C(1) 1.309(4) yes . . O(2) C(13) 1.300(4) yes . . O(3) C(34) 1.292(4) yes . . O(4) C(46) 1.313(3) yes . . N(1) C(7) 1.291(4) yes . . N(1) C(8) 1.478(5) yes . . N(2) C(10) 1.478(5) yes . . N(2) C(11) 1.283(4) yes . . N(3) C(40) 1.287(4) yes . . N(3) C(41) 1.486(4) yes . . N(4) C(43) 1.472(5) yes . . N(4) C(44) 1.296(4) yes . . C(1) C(2) 1.437(5) yes . . C(1) C(6) 1.440(5) yes . . C(2) C(3) 1.381(5) yes . . C(2) C(18) 1.529(6) yes . . C(3) C(4) 1.416(6) yes . . C(4) C(5) 1.381(5) yes . . C(4) C(22) 1.526(5) yes . . C(5) C(6) 1.396(4) yes . . C(6) C(7) 1.422(5) yes . . C(8) C(9) 1.518(5) yes . . C(9) C(10) 1.524(6) yes . . C(11) C(12) 1.429(5) yes . . C(12) C(13) 1.428(5) yes . . C(12) C(17) 1.408(5) yes . . C(13) C(14) 1.442(6) yes . . C(14) C(15) 1.384(5) yes . . C(14) C(26) 1.527(6) yes . . C(15) C(16) 1.409(6) yes . . C(16) C(17) 1.384(6) yes . . C(16) C(30) 1.534(5) yes . . C(18) C(19) 1.523(6) yes . . C(18) C(20) 1.533(6) yes . . C(18) C(21) 1.542(6) yes . . C(22) C(23) 1.530(7) yes . . C(22) C(24) 1.536(6) yes . . C(22) C(25) 1.533(6) yes . . C(26) C(27) 1.549(7) yes . . C(26) C(28) 1.531(7) yes . . C(26) C(29) 1.538(7) yes . . C(30) C(31) 1.535(7) yes . . C(30) C(32) 1.522(6) yes . . C(30) C(33) 1.524(8) yes . . C(34) C(35) 1.447(4) yes . . C(34) C(39) 1.426(5) yes . . C(35) C(36) 1.368(5) yes . . C(35) C(51) 1.537(6) yes . . C(36) C(37) 1.416(6) yes . . C(37) C(38) 1.387(4) yes . . C(37) C(55) 1.530(5) yes . . C(38) C(39) 1.395(4) yes . . C(39) C(40) 1.442(4) yes . . C(41) C(42) 1.515(5) yes . . C(42) C(43) 1.530(6) yes . . C(44) C(45) 1.425(5) yes . . C(45) C(46) 1.419(4) yes . . C(45) C(50) 1.414(4) yes . . C(46) C(47) 1.442(5) yes . . C(47) C(48) 1.382(4) yes . . C(47) C(59) 1.536(4) yes . . C(48) C(49) 1.419(4) yes . . C(49) C(50) 1.382(5) yes . . C(49) C(63) 1.532(4) yes . . C(51) C(52) 1.531(5) yes . . C(51) C(53) 1.543(4) yes . . C(51) C(54) 1.545(5) yes . . C(55) C(56) 1.533(7) yes . . C(55) C(57) 1.518(7) yes . . C(55) C(58) 1.522(8) yes . . C(59) C(60) 1.542(5) yes . . C(59) C(61) 1.531(5) yes . . C(59) C(62) 1.538(4) yes . . C(63) C(64) 1.533(5) yes . . C(63) C(65) 1.531(6) yes . . C(63) C(66) 1.528(5) yes . . C(67) C(68) 1.371(13) yes . . C(68) C(69) 1.508(14) yes . . C(68) C(73) 1.337(9) yes . . C(69) C(70) 1.339(15) yes . . C(70) C(71) 1.541(11) yes . . C(71) C(72) 1.328(14) yes . . C(72) C(73) 1.343(11) yes . . C(74) C(75) 1.433(15) yes . . C(74) C(77a) 1.28(2) yes . . C(74) C(79a) 1.55(2) yes . . C(75) C(75a) 1.440(17) yes . . C(75) C(76) 1.323(14) yes . . C(75) C(77a) 1.07(2) yes . . C(75) C(79a) 1.635(19) yes . . C(75) C(80) 1.482(18) yes . . C(75a) C(76) 1.388(17) yes . . C(75a) C(77) 1.369(17) yes . . C(75a) C(78) 1.427(14) yes . . C(75a) C(79) 1.34(2) yes . . C(75a) C(80) 1.404(15) yes . . C(76) C(77) 1.453(16) yes . . C(76) C(77a) 1.435(16) yes . . C(77) C(78) 1.33(2) yes . . C(78) C(79) 1.462(19) yes . . C(79) C(80) 1.318(17) yes . . C(79a) C(80) 1.326(18) yes . . C(3) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.990 no . . C(8) H(5) 0.990 no . . C(9) H(6) 0.990 no . . C(9) H(7) 0.990 no . . C(10) H(8) 0.990 no . . C(10) H(9) 0.990 no . . C(11) H(10) 0.950 no . . C(15) H(11) 0.950 no . . C(17) H(12) 0.950 no . . C(19) H(13) 0.980 no . . C(19) H(14) 0.980 no . . C(19) H(15) 0.980 no . . C(20) H(16) 0.980 no . . C(20) H(17) 0.980 no . . C(20) H(18) 0.980 no . . C(21) H(19) 0.980 no . . C(21) H(20) 0.980 no . . C(21) H(21) 0.980 no . . C(23) H(22) 0.980 no . . C(23) H(23) 0.980 no . . C(23) H(24) 0.980 no . . C(24) H(25) 0.980 no . . C(24) H(26) 0.980 no . . C(24) H(27) 0.980 no . . C(25) H(28) 0.980 no . . C(25) H(29) 0.980 no . . C(25) H(30) 0.980 no . . C(27) H(31) 0.980 no . . C(27) H(32) 0.980 no . . C(27) H(33) 0.980 no . . C(28) H(34) 0.980 no . . C(28) H(35) 0.980 no . . C(28) H(36) 0.980 no . . C(29) H(37) 0.980 no . . C(29) H(38) 0.980 no . . C(29) H(39) 0.980 no . . C(31) H(40) 0.980 no . . C(31) H(41) 0.980 no . . C(31) H(42) 0.980 no . . C(32) H(43) 0.980 no . . C(32) H(44) 0.980 no . . C(32) H(45) 0.980 no . . C(33) H(46) 0.980 no . . C(33) H(47) 0.980 no . . C(33) H(48) 0.980 no . . C(36) H(49) 0.950 no . . C(38) H(50) 0.950 no . . C(40) H(51) 0.950 no . . C(41) H(52) 0.990 no . . C(41) H(53) 0.990 no . . C(42) H(54) 0.990 no . . C(42) H(55) 0.990 no . . C(43) H(56) 0.990 no . . C(43) H(57) 0.990 no . . C(44) H(58) 0.950 no . . C(48) H(59) 0.950 no . . C(50) H(60) 0.950 no . . C(52) H(61) 0.980 no . . C(52) H(62) 0.980 no . . C(52) H(63) 0.980 no . . C(53) H(64) 0.980 no . . C(53) H(65) 0.980 no . . C(53) H(66) 0.980 no . . C(54) H(67) 0.980 no . . C(54) H(68) 0.980 no . . C(54) H(69) 0.980 no . . C(56) H(70) 0.980 no . . C(56) H(71) 0.980 no . . C(56) H(72) 0.980 no . . C(57) H(73) 0.980 no . . C(57) H(74) 0.980 no . . C(57) H(75) 0.980 no . . C(58) H(76) 0.980 no . . C(58) H(77) 0.980 no . . C(58) H(78) 0.980 no . . C(60) H(79) 0.980 no . . C(60) H(80) 0.980 no . . C(60) H(81) 0.980 no . . C(61) H(82) 0.980 no . . C(61) H(83) 0.980 no . . C(61) H(84) 0.980 no . . C(62) H(85) 0.980 no . . C(62) H(86) 0.980 no . . C(62) H(87) 0.980 no . . C(64) H(88) 0.980 no . . C(64) H(89) 0.980 no . . C(64) H(90) 0.980 no . . C(65) H(91) 0.980 no . . C(65) H(92) 0.980 no . . C(65) H(93) 0.980 no . . C(66) H(94) 0.980 no . . C(66) H(95) 0.980 no . . C(66) H(96) 0.980 no . . C(67) H(97) 0.980 no . . C(67) H(98) 0.980 no . . C(67) H(99) 0.980 no . . C(69) H(100) 0.950 no . . C(70) H(101) 0.950 no . . C(71) H(102) 0.950 no . . C(72) H(103) 0.950 no . . C(73) H(104) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 F(1) Sb(1) F(2) 90.0(2) yes . . . F(1) Sb(1) F(3) 89.91(17) yes . . . F(1) Sb(1) F(4) 178.5(2) yes . . . F(1) Sb(1) F(5) 89.50(16) yes . . . F(1) Sb(1) F(6) 90.7(2) yes . . . F(2) Sb(1) F(3) 91.16(14) yes . . . F(2) Sb(1) F(4) 90.9(3) yes . . . F(2) Sb(1) F(5) 88.71(14) yes . . . F(2) Sb(1) F(6) 178.5(2) yes . . . F(3) Sb(1) F(4) 91.24(15) yes . . . F(3) Sb(1) F(5) 179.39(13) yes . . . F(3) Sb(1) F(6) 90.21(16) yes . . . F(4) Sb(1) F(5) 89.36(15) yes . . . F(4) Sb(1) F(6) 88.3(3) yes . . . F(5) Sb(1) F(6) 89.93(16) yes . . . F(7) Sb(2) F(8) 89.1(2) yes . . . F(7) Sb(2) F(9) 89.8(2) yes . . . F(7) Sb(2) F(10) 179.0(2) yes . . . F(7) Sb(2) F(11) 89.3(2) yes . . . F(7) Sb(2) F(12) 90.2(2) yes . . . F(8) Sb(2) F(9) 178.86(16) yes . . . F(8) Sb(2) F(10) 91.3(2) yes . . . F(8) Sb(2) F(11) 93.5(2) yes . . . F(8) Sb(2) F(12) 85.2(2) yes . . . F(9) Sb(2) F(10) 89.9(2) yes . . . F(9) Sb(2) F(11) 86.4(2) yes . . . F(9) Sb(2) F(12) 95.0(2) yes . . . F(10) Sb(2) F(11) 89.7(2) yes . . . F(10) Sb(2) F(12) 90.7(2) yes . . . F(11) Sb(2) F(12) 178.6(2) yes . . . O(1) Ni(1) O(2) 86.03(12) yes . . . O(1) Ni(1) N(1) 93.83(12) yes . . . O(1) Ni(1) N(2) 165.30(15) yes . . . O(2) Ni(1) N(1) 162.41(14) yes . . . O(2) Ni(1) N(2) 92.58(13) yes . . . N(1) Ni(1) N(2) 91.87(14) yes . . . O(3) Ni(2) O(4) 85.53(11) yes . . . O(3) Ni(2) N(3) 92.73(11) yes . . . O(3) Ni(2) N(4) 161.00(12) yes . . . O(4) Ni(2) N(3) 163.80(12) yes . . . O(4) Ni(2) N(4) 94.30(12) yes . . . N(3) Ni(2) N(4) 92.53(13) yes . . . Ni(1) O(1) C(1) 129.6(2) yes . . . Ni(1) O(2) C(13) 127.7(2) yes . . . Ni(2) O(3) C(34) 129.8(2) yes . . . Ni(2) O(4) C(46) 128.2(2) yes . . . Ni(1) N(1) C(7) 125.7(2) yes . . . Ni(1) N(1) C(8) 115.8(2) yes . . . C(7) N(1) C(8) 117.8(3) yes . . . Ni(1) N(2) C(10) 115.4(2) yes . . . Ni(1) N(2) C(11) 126.0(2) yes . . . C(10) N(2) C(11) 118.5(3) yes . . . Ni(2) N(3) C(40) 126.9(2) yes . . . Ni(2) N(3) C(41) 114.8(2) yes . . . C(40) N(3) C(41) 117.9(3) yes . . . Ni(2) N(4) C(43) 116.2(2) yes . . . Ni(2) N(4) C(44) 125.2(2) yes . . . C(43) N(4) C(44) 118.0(2) yes . . . O(1) C(1) C(2) 120.3(3) yes . . . O(1) C(1) C(6) 121.1(3) yes . . . C(2) C(1) C(6) 118.6(3) yes . . . C(1) C(2) C(3) 116.9(3) yes . . . C(1) C(2) C(18) 120.9(3) yes . . . C(3) C(2) C(18) 122.2(3) yes . . . C(2) C(3) C(4) 125.5(3) yes . . . C(3) C(4) C(5) 116.7(3) yes . . . C(3) C(4) C(22) 123.0(3) yes . . . C(5) C(4) C(22) 120.2(3) yes . . . C(4) C(5) C(6) 121.6(3) yes . . . C(1) C(6) C(5) 120.7(3) yes . . . C(1) C(6) C(7) 121.1(3) yes . . . C(5) C(6) C(7) 118.1(3) yes . . . N(1) C(7) C(6) 126.4(3) yes . . . N(1) C(8) C(9) 112.6(3) yes . . . C(8) C(9) C(10) 112.4(3) yes . . . N(2) C(10) C(9) 110.2(3) yes . . . N(2) C(11) C(12) 125.0(3) yes . . . C(11) C(12) C(13) 120.4(3) yes . . . C(11) C(12) C(17) 118.5(3) yes . . . C(13) C(12) C(17) 121.1(3) yes . . . O(2) C(13) C(12) 121.7(3) yes . . . O(2) C(13) C(14) 119.9(3) yes . . . C(12) C(13) C(14) 118.3(3) yes . . . C(13) C(14) C(15) 116.8(4) yes . . . C(13) C(14) C(26) 121.0(3) yes . . . C(15) C(14) C(26) 122.0(3) yes . . . C(14) C(15) C(16) 125.0(4) yes . . . C(15) C(16) C(17) 117.5(3) yes . . . C(15) C(16) C(30) 121.6(4) yes . . . C(17) C(16) C(30) 120.8(3) yes . . . C(12) C(17) C(16) 120.4(3) yes . . . C(2) C(18) C(19) 109.3(4) yes . . . C(2) C(18) C(20) 110.8(3) yes . . . C(2) C(18) C(21) 112.0(3) yes . . . C(19) C(18) C(20) 110.0(3) yes . . . C(19) C(18) C(21) 107.7(3) yes . . . C(20) C(18) C(21) 107.1(4) yes . . . C(4) C(22) C(23) 108.9(3) yes . . . C(4) C(22) C(24) 108.8(3) yes . . . C(4) C(22) C(25) 112.7(3) yes . . . C(23) C(22) C(24) 110.4(4) yes . . . C(23) C(22) C(25) 108.4(3) yes . . . C(24) C(22) C(25) 107.8(3) yes . . . C(14) C(26) C(27) 108.8(4) yes . . . C(14) C(26) C(28) 110.6(3) yes . . . C(14) C(26) C(29) 111.7(3) yes . . . C(27) C(26) C(28) 111.2(4) yes . . . C(27) C(26) C(29) 107.6(4) yes . . . C(28) C(26) C(29) 106.8(4) yes . . . C(16) C(30) C(31) 106.2(3) yes . . . C(16) C(30) C(32) 111.9(3) yes . . . C(16) C(30) C(33) 111.8(4) yes . . . C(31) C(30) C(32) 109.0(4) yes . . . C(31) C(30) C(33) 108.8(4) yes . . . C(32) C(30) C(33) 109.1(3) yes . . . O(3) C(34) C(35) 119.5(3) yes . . . O(3) C(34) C(39) 121.9(2) yes . . . C(35) C(34) C(39) 118.6(3) yes . . . C(34) C(35) C(36) 117.6(3) yes . . . C(34) C(35) C(51) 119.9(2) yes . . . C(36) C(35) C(51) 122.5(3) yes . . . C(35) C(36) C(37) 123.9(3) yes . . . C(36) C(37) C(38) 118.4(3) yes . . . C(36) C(37) C(55) 119.8(3) yes . . . C(38) C(37) C(55) 121.7(3) yes . . . C(37) C(38) C(39) 120.3(3) yes . . . C(34) C(39) C(38) 121.1(3) yes . . . C(34) C(39) C(40) 120.2(3) yes . . . C(38) C(39) C(40) 118.6(3) yes . . . N(3) C(40) C(39) 125.3(3) yes . . . N(3) C(41) C(42) 110.2(3) yes . . . C(41) C(42) C(43) 112.7(3) yes . . . N(4) C(43) C(42) 112.6(3) yes . . . N(4) C(44) C(45) 126.1(2) yes . . . C(44) C(45) C(46) 121.5(2) yes . . . C(44) C(45) C(50) 117.2(2) yes . . . C(46) C(45) C(50) 121.3(3) yes . . . O(4) C(46) C(45) 121.6(3) yes . . . O(4) C(46) C(47) 119.9(2) yes . . . C(45) C(46) C(47) 118.5(2) yes . . . C(46) C(47) C(48) 117.1(3) yes . . . C(46) C(47) C(59) 121.2(2) yes . . . C(48) C(47) C(59) 121.7(3) yes . . . C(47) C(48) C(49) 125.3(3) yes . . . C(48) C(49) C(50) 116.8(3) yes . . . C(48) C(49) C(63) 119.9(3) yes . . . C(50) C(49) C(63) 123.2(3) yes . . . C(45) C(50) C(49) 120.9(3) yes . . . C(35) C(51) C(52) 110.0(3) yes . . . C(35) C(51) C(53) 111.2(3) yes . . . C(35) C(51) C(54) 109.5(3) yes . . . C(52) C(51) C(53) 108.2(3) yes . . . C(52) C(51) C(54) 110.7(3) yes . . . C(53) C(51) C(54) 107.2(3) yes . . . C(37) C(55) C(56) 108.2(3) yes . . . C(37) C(55) C(57) 109.6(3) yes . . . C(37) C(55) C(58) 112.7(3) yes . . . C(56) C(55) C(57) 110.8(4) yes . . . C(56) C(55) C(58) 107.9(4) yes . . . C(57) C(55) C(58) 107.6(4) yes . . . C(47) C(59) C(60) 110.4(3) yes . . . C(47) C(59) C(61) 112.1(2) yes . . . C(47) C(59) C(62) 110.4(2) yes . . . C(60) C(59) C(61) 107.6(3) yes . . . C(60) C(59) C(62) 109.2(2) yes . . . C(61) C(59) C(62) 107.1(3) yes . . . C(49) C(63) C(64) 109.4(2) yes . . . C(49) C(63) C(65) 109.1(2) yes . . . C(49) C(63) C(66) 111.8(3) yes . . . C(64) C(63) C(65) 109.9(3) yes . . . C(64) C(63) C(66) 108.1(3) yes . . . C(65) C(63) C(66) 108.5(3) yes . . . C(67) C(68) C(69) 115.2(7) yes . . . C(67) C(68) C(73) 130.3(8) yes . . . C(69) C(68) C(73) 114.5(7) yes . . . C(68) C(69) C(70) 114.5(7) yes . . . C(69) C(70) C(71) 126.2(9) yes . . . C(70) C(71) C(72) 114.1(9) yes . . . C(71) C(72) C(73) 118.9(8) yes . . . C(68) C(73) C(72) 131.7(8) yes . . . C(75) C(74) C(77a) 45.9(10) yes . . . C(75) C(74) C(79a) 66.2(9) yes . . . C(77a) C(74) C(79a) 112.1(11) yes . . . C(74) C(75) C(75a) 167.9(13) yes . . . C(74) C(75) C(76) 132.0(13) yes . . . C(74) C(75) C(77a) 59.2(11) yes . . . C(74) C(75) C(79a) 60.5(9) yes . . . C(74) C(75) C(80) 110.5(10) yes . . . C(75a) C(75) C(76) 60.1(8) yes . . . C(75a) C(75) C(77a) 132.9(13) yes . . . C(75a) C(75) C(79a) 107.4(12) yes . . . C(75a) C(75) C(80) 57.4(8) yes . . . C(76) C(75) C(77a) 72.9(11) yes . . . C(76) C(75) C(79a) 167.3(13) yes . . . C(76) C(75) C(80) 117.5(10) yes . . . C(77a) C(75) C(79a) 119.6(13) yes . . . C(77a) C(75) C(80) 168.5(12) yes . . . C(79a) C(75) C(80) 50.1(8) yes . . . C(75) C(75a) C(76) 55.8(8) yes . . . C(75) C(75a) C(77) 119.4(13) yes . . . C(75) C(75a) C(78) 174.7(13) yes . . . C(75) C(75a) C(79) 119.6(11) yes . . . C(75) C(75a) C(80) 62.8(8) yes . . . C(76) C(75a) C(77) 63.6(9) yes . . . C(76) C(75a) C(78) 120.1(10) yes . . . C(76) C(75a) C(79) 170.5(12) yes . . . C(76) C(75a) C(80) 118.6(10) yes . . . C(77) C(75a) C(78) 56.6(9) yes . . . C(77) C(75a) C(79) 120.2(12) yes . . . C(77) C(75a) C(80) 177.4(12) yes . . . C(78) C(75a) C(79) 63.8(9) yes . . . C(78) C(75a) C(80) 121.1(12) yes . . . C(79) C(75a) C(80) 57.5(9) yes . . . C(75) C(76) C(75a) 64.1(8) yes . . . C(75) C(76) C(77) 121.7(11) yes . . . C(75) C(76) C(77a) 45.2(9) yes . . . C(75a) C(76) C(77) 57.6(8) yes . . . C(75a) C(76) C(77a) 109.2(10) yes . . . C(77) C(76) C(77a) 166.4(11) yes . . . C(75a) C(77) C(76) 58.8(8) yes . . . C(75a) C(77) C(78) 63.9(9) yes . . . C(76) C(77) C(78) 122.7(11) yes . . . C(74) C(77a) C(75) 74.8(13) yes . . . C(74) C(77a) C(76) 136.4(16) yes . . . C(75) C(77a) C(76) 61.8(10) yes . . . C(75a) C(78) C(77) 59.5(8) yes . . . C(75a) C(78) C(79) 55.0(9) yes . . . C(77) C(78) C(79) 114.2(10) yes . . . C(75a) C(79) C(78) 61.2(10) yes . . . C(75a) C(79) C(80) 63.9(10) yes . . . C(78) C(79) C(80) 124.9(14) yes . . . C(74) C(79a) C(75) 53.3(8) yes . . . C(74) C(79a) C(80) 112.2(12) yes . . . C(75) C(79a) C(80) 59.0(8) yes . . . C(75) C(80) C(75a) 59.8(8) yes . . . C(75) C(80) C(79) 117.8(11) yes . . . C(75) C(80) C(79a) 71.0(10) yes . . . C(75a) C(80) C(79) 58.6(10) yes . . . C(75a) C(80) C(79a) 130.6(13) yes . . . C(79) C(80) C(79a) 170.3(13) yes . . . C(2) C(3) H(1) 117.3 no . . . C(4) C(3) H(1) 117.3 no . . . C(4) C(5) H(2) 119.2 no . . . C(6) C(5) H(2) 119.2 no . . . N(1) C(7) H(3) 116.8 no . . . C(6) C(7) H(3) 116.8 no . . . N(1) C(8) H(4) 109.1 no . . . N(1) C(8) H(5) 109.1 no . . . C(9) C(8) H(4) 109.1 no . . . C(9) C(8) H(5) 109.1 no . . . H(4) C(8) H(5) 107.8 no . . . C(8) C(9) H(6) 109.1 no . . . C(8) C(9) H(7) 109.1 no . . . C(10) C(9) H(6) 109.1 no . . . C(10) C(9) H(7) 109.1 no . . . H(6) C(9) H(7) 107.9 no . . . N(2) C(10) H(8) 109.6 no . . . N(2) C(10) H(9) 109.6 no . . . C(9) C(10) H(8) 109.6 no . . . C(9) C(10) H(9) 109.6 no . . . H(8) C(10) H(9) 108.1 no . . . N(2) C(11) H(10) 117.5 no . . . C(12) C(11) H(10) 117.5 no . . . C(14) C(15) H(11) 117.5 no . . . C(16) C(15) H(11) 117.5 no . . . C(12) C(17) H(12) 119.8 no . . . C(16) C(17) H(12) 119.8 no . . . C(18) C(19) H(13) 109.5 no . . . C(18) C(19) H(14) 109.5 no . . . C(18) C(19) H(15) 109.5 no . . . H(13) C(19) H(14) 109.5 no . . . H(13) C(19) H(15) 109.5 no . . . H(14) C(19) H(15) 109.5 no . . . C(18) C(20) H(16) 109.5 no . . . C(18) C(20) H(17) 109.5 no . . . C(18) C(20) H(18) 109.5 no . . . H(16) C(20) H(17) 109.5 no . . . H(16) C(20) H(18) 109.5 no . . . H(17) C(20) H(18) 109.5 no . . . C(18) C(21) H(19) 109.5 no . . . C(18) C(21) H(20) 109.5 no . . . C(18) C(21) H(21) 109.5 no . . . H(19) C(21) H(20) 109.5 no . . . H(19) C(21) H(21) 109.5 no . . . H(20) C(21) H(21) 109.5 no . . . C(22) C(23) H(22) 109.5 no . . . C(22) C(23) H(23) 109.5 no . . . C(22) C(23) H(24) 109.5 no . . . H(22) C(23) H(23) 109.5 no . . . H(22) C(23) H(24) 109.5 no . . . H(23) C(23) H(24) 109.5 no . . . C(22) C(24) H(25) 109.5 no . . . C(22) C(24) H(26) 109.5 no . . . C(22) C(24) H(27) 109.5 no . . . H(25) C(24) H(26) 109.5 no . . . H(25) C(24) H(27) 109.5 no . . . H(26) C(24) H(27) 109.5 no . . . C(22) C(25) H(28) 109.5 no . . . C(22) C(25) H(29) 109.5 no . . . C(22) C(25) H(30) 109.5 no . . . H(28) C(25) H(29) 109.5 no . . . H(28) C(25) H(30) 109.5 no . . . H(29) C(25) H(30) 109.5 no . . . C(26) C(27) H(31) 109.5 no . . . C(26) C(27) H(32) 109.5 no . . . C(26) C(27) H(33) 109.5 no . . . H(31) C(27) H(32) 109.5 no . . . H(31) C(27) H(33) 109.5 no . . . H(32) C(27) H(33) 109.5 no . . . C(26) C(28) H(34) 109.5 no . . . C(26) C(28) H(35) 109.5 no . . . C(26) C(28) H(36) 109.5 no . . . H(34) C(28) H(35) 109.5 no . . . H(34) C(28) H(36) 109.5 no . . . H(35) C(28) H(36) 109.5 no . . . C(26) C(29) H(37) 109.5 no . . . C(26) C(29) H(38) 109.5 no . . . C(26) C(29) H(39) 109.5 no . . . H(37) C(29) H(38) 109.5 no . . . H(37) C(29) H(39) 109.5 no . . . H(38) C(29) H(39) 109.5 no . . . C(30) C(31) H(40) 109.5 no . . . C(30) C(31) H(41) 109.5 no . . . C(30) C(31) H(42) 109.5 no . . . H(40) C(31) H(41) 109.5 no . . . H(40) C(31) H(42) 109.5 no . . . H(41) C(31) H(42) 109.5 no . . . C(30) C(32) H(43) 109.5 no . . . C(30) C(32) H(44) 109.5 no . . . C(30) C(32) H(45) 109.5 no . . . H(43) C(32) H(44) 109.5 no . . . H(43) C(32) H(45) 109.5 no . . . H(44) C(32) H(45) 109.5 no . . . C(30) C(33) H(46) 109.5 no . . . C(30) C(33) H(47) 109.5 no . . . C(30) C(33) H(48) 109.5 no . . . H(46) C(33) H(47) 109.5 no . . . H(46) C(33) H(48) 109.5 no . . . H(47) C(33) H(48) 109.5 no . . . C(35) C(36) H(49) 118.0 no . . . C(37) C(36) H(49) 118.0 no . . . C(37) C(38) H(50) 119.9 no . . . C(39) C(38) H(50) 119.9 no . . . N(3) C(40) H(51) 117.4 no . . . C(39) C(40) H(51) 117.4 no . . . N(3) C(41) H(52) 109.6 no . . . N(3) C(41) H(53) 109.6 no . . . C(42) C(41) H(52) 109.6 no . . . C(42) C(41) H(53) 109.6 no . . . H(52) C(41) H(53) 108.1 no . . . C(41) C(42) H(54) 109.0 no . . . C(41) C(42) H(55) 109.0 no . . . C(43) C(42) H(54) 109.1 no . . . C(43) C(42) H(55) 109.0 no . . . H(54) C(42) H(55) 107.8 no . . . N(4) C(43) H(56) 109.1 no . . . N(4) C(43) H(57) 109.1 no . . . C(42) C(43) H(56) 109.1 no . . . C(42) C(43) H(57) 109.1 no . . . H(56) C(43) H(57) 107.8 no . . . N(4) C(44) H(58) 116.9 no . . . C(45) C(44) H(58) 116.9 no . . . C(47) C(48) H(59) 117.4 no . . . C(49) C(48) H(59) 117.4 no . . . C(45) C(50) H(60) 119.5 no . . . C(49) C(50) H(60) 119.5 no . . . C(51) C(52) H(61) 109.5 no . . . C(51) C(52) H(62) 109.5 no . . . C(51) C(52) H(63) 109.5 no . . . H(61) C(52) H(62) 109.5 no . . . H(61) C(52) H(63) 109.5 no . . . H(62) C(52) H(63) 109.5 no . . . C(51) C(53) H(64) 109.5 no . . . C(51) C(53) H(65) 109.5 no . . . C(51) C(53) H(66) 109.5 no . . . H(64) C(53) H(65) 109.5 no . . . H(64) C(53) H(66) 109.5 no . . . H(65) C(53) H(66) 109.5 no . . . C(51) C(54) H(67) 109.5 no . . . C(51) C(54) H(68) 109.5 no . . . C(51) C(54) H(69) 109.5 no . . . H(67) C(54) H(68) 109.5 no . . . H(67) C(54) H(69) 109.5 no . . . H(68) C(54) H(69) 109.5 no . . . C(55) C(56) H(70) 109.5 no . . . C(55) C(56) H(71) 109.5 no . . . C(55) C(56) H(72) 109.5 no . . . H(70) C(56) H(71) 109.5 no . . . H(70) C(56) H(72) 109.5 no . . . H(71) C(56) H(72) 109.5 no . . . C(55) C(57) H(73) 109.5 no . . . C(55) C(57) H(74) 109.5 no . . . C(55) C(57) H(75) 109.5 no . . . H(73) C(57) H(74) 109.5 no . . . H(73) C(57) H(75) 109.5 no . . . H(74) C(57) H(75) 109.5 no . . . C(55) C(58) H(76) 109.5 no . . . C(55) C(58) H(77) 109.5 no . . . C(55) C(58) H(78) 109.5 no . . . H(76) C(58) H(77) 109.5 no . . . H(76) C(58) H(78) 109.5 no . . . H(77) C(58) H(78) 109.5 no . . . C(59) C(60) H(79) 109.5 no . . . C(59) C(60) H(80) 109.5 no . . . C(59) C(60) H(81) 109.5 no . . . H(79) C(60) H(80) 109.5 no . . . H(79) C(60) H(81) 109.5 no . . . H(80) C(60) H(81) 109.5 no . . . C(59) C(61) H(82) 109.5 no . . . C(59) C(61) H(83) 109.5 no . . . C(59) C(61) H(84) 109.5 no . . . H(82) C(61) H(83) 109.5 no . . . H(82) C(61) H(84) 109.5 no . . . H(83) C(61) H(84) 109.5 no . . . C(59) C(62) H(85) 109.5 no . . . C(59) C(62) H(86) 109.5 no . . . C(59) C(62) H(87) 109.5 no . . . H(85) C(62) H(86) 109.5 no . . . H(85) C(62) H(87) 109.5 no . . . H(86) C(62) H(87) 109.5 no . . . C(63) C(64) H(88) 109.5 no . . . C(63) C(64) H(89) 109.5 no . . . C(63) C(64) H(90) 109.5 no . . . H(88) C(64) H(89) 109.5 no . . . H(88) C(64) H(90) 109.5 no . . . H(89) C(64) H(90) 109.5 no . . . C(63) C(65) H(91) 109.5 no . . . C(63) C(65) H(92) 109.5 no . . . C(63) C(65) H(93) 109.5 no . . . H(91) C(65) H(92) 109.5 no . . . H(91) C(65) H(93) 109.5 no . . . H(92) C(65) H(93) 109.5 no . . . C(63) C(66) H(94) 109.5 no . . . C(63) C(66) H(95) 109.5 no . . . C(63) C(66) H(96) 109.5 no . . . H(94) C(66) H(95) 109.5 no . . . H(94) C(66) H(96) 109.5 no . . . H(95) C(66) H(96) 109.5 no . . . C(68) C(67) H(97) 109.5 no . . . C(68) C(67) H(98) 109.5 no . . . C(68) C(67) H(99) 109.5 no . . . H(97) C(67) H(98) 109.5 no . . . H(97) C(67) H(99) 109.5 no . . . H(98) C(67) H(99) 109.5 no . . . C(68) C(69) H(100) 122.8 no . . . C(70) C(69) H(100) 122.8 no . . . C(69) C(70) H(101) 116.9 no . . . C(71) C(70) H(101) 116.9 no . . . C(70) C(71) H(102) 122.9 no . . . C(72) C(71) H(102) 122.9 no . . . C(71) C(72) H(103) 120.6 no . . . C(73) C(72) H(103) 120.5 no . . . C(68) C(73) H(104) 114.1 no . . . C(72) C(73) H(104) 114.1 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Ni(1) O(2) C(13) 167.9(3) ? . . . . O(2) Ni(1) O(1) C(1) -178.6(3) ? . . . . O(1) Ni(1) N(1) C(7) 6.9(3) ? . . . . O(1) Ni(1) N(1) C(8) -163.4(2) ? . . . . N(1) Ni(1) O(1) C(1) -16.3(3) ? . . . . O(1) Ni(1) N(2) C(10) -75.5(6) ? . . . . O(1) Ni(1) N(2) C(11) 102.7(5) ? . . . . N(2) Ni(1) O(1) C(1) 96.3(6) ? . . . . O(2) Ni(1) N(1) C(7) 95.8(4) ? . . . . O(2) Ni(1) N(1) C(8) -74.5(4) ? . . . . N(1) Ni(1) O(2) C(13) 77.8(5) ? . . . . O(2) Ni(1) N(2) C(10) -159.7(3) ? . . . . O(2) Ni(1) N(2) C(11) 18.5(4) ? . . . . N(2) Ni(1) O(2) C(13) -26.7(3) ? . . . . N(1) Ni(1) N(2) C(10) 37.3(3) ? . . . . N(1) Ni(1) N(2) C(11) -144.4(4) ? . . . . N(2) Ni(1) N(1) C(7) -159.6(3) ? . . . . N(2) Ni(1) N(1) C(8) 30.1(2) ? . . . . O(3) Ni(2) O(4) C(46) -179.5(2) ? . . . . O(4) Ni(2) O(3) C(34) -176.7(3) ? . . . . O(3) Ni(2) N(3) C(40) -8.6(3) ? . . . . O(3) Ni(2) N(3) C(41) 163.1(2) ? . . . . N(3) Ni(2) O(3) C(34) 19.4(3) ? . . . . O(3) Ni(2) N(4) C(43) 74.1(5) ? . . . . O(3) Ni(2) N(4) C(44) -96.6(4) ? . . . . N(4) Ni(2) O(3) C(34) -86.5(5) ? . . . . O(4) Ni(2) N(3) C(40) -92.0(4) ? . . . . O(4) Ni(2) N(3) C(41) 79.7(4) ? . . . . N(3) Ni(2) O(4) C(46) -95.1(4) ? . . . . O(4) Ni(2) N(4) C(43) 162.8(2) ? . . . . O(4) Ni(2) N(4) C(44) -7.8(3) ? . . . . N(4) Ni(2) O(4) C(46) 19.6(2) ? . . . . N(3) Ni(2) N(4) C(43) -31.9(2) ? . . . . N(3) Ni(2) N(4) C(44) 157.5(2) ? . . . . N(4) Ni(2) N(3) C(40) 153.1(3) ? . . . . N(4) Ni(2) N(3) C(41) -35.2(2) ? . . . . Ni(1) O(1) C(1) C(2) -167.5(2) ? . . . . Ni(1) O(1) C(1) C(6) 14.4(5) ? . . . . Ni(1) O(2) C(13) C(12) 17.1(6) ? . . . . Ni(1) O(2) C(13) C(14) -162.8(3) ? . . . . Ni(2) O(3) C(34) C(35) 163.0(2) ? . . . . Ni(2) O(3) C(34) C(39) -17.0(5) ? . . . . Ni(2) O(4) C(46) C(45) -19.2(4) ? . . . . Ni(2) O(4) C(46) C(47) 162.2(2) ? . . . . Ni(1) N(1) C(7) C(6) 3.7(5) ? . . . . Ni(1) N(1) C(8) C(9) -69.9(3) ? . . . . C(7) N(1) C(8) C(9) 119.0(3) ? . . . . C(8) N(1) C(7) C(6) 173.9(3) ? . . . . Ni(1) N(2) C(10) C(9) -74.6(3) ? . . . . Ni(1) N(2) C(11) C(12) -1.5(6) ? . . . . C(10) N(2) C(11) C(12) 176.7(4) ? . . . . C(11) N(2) C(10) C(9) 107.1(4) ? . . . . Ni(2) N(3) C(40) C(39) -3.7(5) ? . . . . Ni(2) N(3) C(41) C(42) 74.6(3) ? . . . . C(40) N(3) C(41) C(42) -112.9(3) ? . . . . C(41) N(3) C(40) C(39) -175.3(3) ? . . . . Ni(2) N(4) C(43) C(42) 68.7(3) ? . . . . Ni(2) N(4) C(44) C(45) -3.9(5) ? . . . . C(43) N(4) C(44) C(45) -174.3(3) ? . . . . C(44) N(4) C(43) C(42) -120.0(3) ? . . . . O(1) C(1) C(2) C(3) -179.6(3) ? . . . . O(1) C(1) C(2) C(18) -0.7(5) ? . . . . O(1) C(1) C(6) C(5) 178.2(3) ? . . . . O(1) C(1) C(6) C(7) 0.5(5) ? . . . . C(2) C(1) C(6) C(5) 0.1(4) ? . . . . C(2) C(1) C(6) C(7) -177.6(3) ? . . . . C(6) C(1) C(2) C(3) -1.5(5) ? . . . . C(6) C(1) C(2) C(18) 177.5(3) ? . . . . C(1) C(2) C(3) C(4) 1.3(6) ? . . . . C(1) C(2) C(18) C(19) -62.2(4) ? . . . . C(1) C(2) C(18) C(20) 59.1(4) ? . . . . C(1) C(2) C(18) C(21) 178.5(3) ? . . . . C(3) C(2) C(18) C(19) 116.7(4) ? . . . . C(3) C(2) C(18) C(20) -122.0(4) ? . . . . C(3) C(2) C(18) C(21) -2.6(5) ? . . . . C(18) C(2) C(3) C(4) -177.7(3) ? . . . . C(2) C(3) C(4) C(5) 0.4(6) ? . . . . C(2) C(3) C(4) C(22) 178.7(3) ? . . . . C(3) C(4) C(5) C(6) -1.9(5) ? . . . . C(3) C(4) C(22) C(23) -113.6(4) ? . . . . C(3) C(4) C(22) C(24) 126.1(4) ? . . . . C(3) C(4) C(22) C(25) 6.6(5) ? . . . . C(5) C(4) C(22) C(23) 64.6(5) ? . . . . C(5) C(4) C(22) C(24) -55.7(5) ? . . . . C(5) C(4) C(22) C(25) -175.2(3) ? . . . . C(22) C(4) C(5) C(6) 179.8(3) ? . . . . C(4) C(5) C(6) C(1) 1.7(6) ? . . . . C(4) C(5) C(6) C(7) 179.5(3) ? . . . . C(1) C(6) C(7) N(1) -9.7(6) ? . . . . C(5) C(6) C(7) N(1) 172.6(3) ? . . . . N(1) C(8) C(9) C(10) 34.4(4) ? . . . . C(8) C(9) C(10) N(2) 34.8(3) ? . . . . N(2) C(11) C(12) C(13) -16.4(7) ? . . . . N(2) C(11) C(12) C(17) 164.8(4) ? . . . . C(11) C(12) C(13) O(2) 8.4(6) ? . . . . C(11) C(12) C(13) C(14) -171.7(4) ? . . . . C(11) C(12) C(17) C(16) 179.9(3) ? . . . . C(13) C(12) C(17) C(16) 1.1(6) ? . . . . C(17) C(12) C(13) O(2) -172.9(4) ? . . . . C(17) C(12) C(13) C(14) 7.0(6) ? . . . . O(2) C(13) C(14) C(15) 171.1(4) ? . . . . O(2) C(13) C(14) C(26) -5.0(6) ? . . . . C(12) C(13) C(14) C(15) -8.7(6) ? . . . . C(12) C(13) C(14) C(26) 175.2(4) ? . . . . C(13) C(14) C(15) C(16) 2.9(7) ? . . . . C(13) C(14) C(26) C(27) 69.8(5) ? . . . . C(13) C(14) C(26) C(28) -52.7(5) ? . . . . C(13) C(14) C(26) C(29) -171.5(4) ? . . . . C(15) C(14) C(26) C(27) -106.1(5) ? . . . . C(15) C(14) C(26) C(28) 131.4(4) ? . . . . C(15) C(14) C(26) C(29) 12.6(6) ? . . . . C(26) C(14) C(15) C(16) 178.9(4) ? . . . . C(14) C(15) C(16) C(17) 5.1(7) ? . . . . C(14) C(15) C(16) C(30) -170.3(4) ? . . . . C(15) C(16) C(17) C(12) -7.0(6) ? . . . . C(15) C(16) C(30) C(31) 83.0(5) ? . . . . C(15) C(16) C(30) C(32) -158.1(4) ? . . . . C(15) C(16) C(30) C(33) -35.5(6) ? . . . . C(17) C(16) C(30) C(31) -92.2(5) ? . . . . C(17) C(16) C(30) C(32) 26.7(6) ? . . . . C(17) C(16) C(30) C(33) 149.3(4) ? . . . . C(30) C(16) C(17) C(12) 168.4(4) ? . . . . O(3) C(34) C(35) C(36) 177.9(3) ? . . . . O(3) C(34) C(35) C(51) -2.4(5) ? . . . . O(3) C(34) C(39) C(38) -178.1(3) ? . . . . O(3) C(34) C(39) C(40) -0.9(5) ? . . . . C(35) C(34) C(39) C(38) 2.0(5) ? . . . . C(35) C(34) C(39) C(40) 179.2(3) ? . . . . C(39) C(34) C(35) C(36) -2.1(5) ? . . . . C(39) C(34) C(35) C(51) 177.6(3) ? . . . . C(34) C(35) C(36) C(37) 0.9(5) ? . . . . C(34) C(35) C(51) C(52) 63.8(4) ? . . . . C(34) C(35) C(51) C(53) -176.3(3) ? . . . . C(34) C(35) C(51) C(54) -58.1(4) ? . . . . C(36) C(35) C(51) C(52) -116.4(3) ? . . . . C(36) C(35) C(51) C(53) 3.4(5) ? . . . . C(36) C(35) C(51) C(54) 121.7(3) ? . . . . C(51) C(35) C(36) C(37) -178.8(3) ? . . . . C(35) C(36) C(37) C(38) 0.6(6) ? . . . . C(35) C(36) C(37) C(55) -178.9(3) ? . . . . C(36) C(37) C(38) C(39) -0.8(5) ? . . . . C(36) C(37) C(55) C(56) 65.6(5) ? . . . . C(36) C(37) C(55) C(57) -55.3(5) ? . . . . C(36) C(37) C(55) C(58) -175.2(4) ? . . . . C(38) C(37) C(55) C(56) -114.0(4) ? . . . . C(38) C(37) C(55) C(57) 125.1(4) ? . . . . C(38) C(37) C(55) C(58) 5.3(5) ? . . . . C(55) C(37) C(38) C(39) 178.7(3) ? . . . . C(37) C(38) C(39) C(34) -0.5(5) ? . . . . C(37) C(38) C(39) C(40) -177.7(3) ? . . . . C(34) C(39) C(40) N(3) 11.2(5) ? . . . . C(38) C(39) C(40) N(3) -171.5(3) ? . . . . N(3) C(41) C(42) C(43) -38.5(4) ? . . . . C(41) C(42) C(43) N(4) -30.5(3) ? . . . . N(4) C(44) C(45) C(46) 9.1(5) ? . . . . N(4) C(44) C(45) C(50) -172.6(3) ? . . . . C(44) C(45) C(46) O(4) 2.7(5) ? . . . . C(44) C(45) C(46) C(47) -178.7(3) ? . . . . C(44) C(45) C(50) C(49) -179.7(3) ? . . . . C(46) C(45) C(50) C(49) -1.5(5) ? . . . . C(50) C(45) C(46) O(4) -175.5(3) ? . . . . C(50) C(45) C(46) C(47) 3.1(4) ? . . . . O(4) C(46) C(47) C(48) 176.1(3) ? . . . . O(4) C(46) C(47) C(59) -3.8(4) ? . . . . C(45) C(46) C(47) C(48) -2.5(4) ? . . . . C(45) C(46) C(47) C(59) 177.5(3) ? . . . . C(46) C(47) C(48) C(49) 0.3(5) ? . . . . C(46) C(47) C(59) C(60) -55.4(4) ? . . . . C(46) C(47) C(59) C(61) -175.2(3) ? . . . . C(46) C(47) C(59) C(62) 65.5(4) ? . . . . C(48) C(47) C(59) C(60) 124.7(3) ? . . . . C(48) C(47) C(59) C(61) 4.8(4) ? . . . . C(48) C(47) C(59) C(62) -114.5(3) ? . . . . C(59) C(47) C(48) C(49) -179.7(3) ? . . . . C(47) C(48) C(49) C(50) 1.3(5) ? . . . . C(47) C(48) C(49) C(63) -179.3(3) ? . . . . C(48) C(49) C(50) C(45) -0.8(5) ? . . . . C(48) C(49) C(63) C(64) -60.3(4) ? . . . . C(48) C(49) C(63) C(65) 59.9(4) ? . . . . C(48) C(49) C(63) C(66) 180.0(2) ? . . . . C(50) C(49) C(63) C(64) 119.1(4) ? . . . . C(50) C(49) C(63) C(65) -120.7(3) ? . . . . C(50) C(49) C(63) C(66) -0.7(5) ? . . . . C(63) C(49) C(50) C(45) 179.9(2) ? . . . . C(67) C(68) C(69) C(70) -179.4(7) ? . . . . C(67) C(68) C(73) C(72) -180.0(8) ? . . . . C(69) C(68) C(73) C(72) -0.5(10) ? . . . . C(73) C(68) C(69) C(70) 1.0(9) ? . . . . C(68) C(69) C(70) C(71) -1.9(10) ? . . . . C(69) C(70) C(71) C(72) 2.2(11) ? . . . . C(70) C(71) C(72) C(73) -1.4(10) ? . . . . C(71) C(72) C(73) C(68) 0.8(12) ? . . . . C(75) C(74) C(77a) C(76) 5.7(13) ? . . . . C(77a) C(74) C(75) C(75a) 179(4) ? . . . . C(77a) C(74) C(75) C(76) -5.8(13) ? . . . . C(77a) C(74) C(75) C(79a) 177.2(13) ? . . . . C(77a) C(74) C(75) C(80) 174.4(14) ? . . . . C(75) C(74) C(79a) C(80) 3.1(11) ? . . . . C(79a) C(74) C(75) C(75a) 1(4) ? . . . . C(79a) C(74) C(75) C(76) 177.1(15) ? . . . . C(79a) C(74) C(75) C(77a) -177.2(13) ? . . . . C(79a) C(74) C(75) C(80) -2.8(9) ? . . . . C(77a) C(74) C(79a) C(75) -2.2(10) ? . . . . C(77a) C(74) C(79a) C(80) 0.9(17) ? . . . . C(79a) C(74) C(77a) C(75) 2.8(13) ? . . . . C(79a) C(74) C(77a) C(76) 9(2) ? . . . . C(74) C(75) C(75a) C(76) 176(5) ? . . . . C(74) C(75) C(75a) C(77) 177(4) ? . . . . C(74) C(75) C(75a) C(78) -143(10) ? . . . . C(74) C(75) C(75a) C(79) -13(5) ? . . . . C(74) C(75) C(75a) C(80) -5(5) ? . . . . C(74) C(75) C(76) C(75a) -178.9(15) ? . . . . C(74) C(75) C(76) C(77) -179.5(11) ? . . . . C(74) C(75) C(76) C(77a) 5.2(12) ? . . . . C(74) C(75) C(77a) C(76) -175.5(10) ? . . . . C(74) C(75) C(79a) C(80) -176.6(11) ? . . . . C(74) C(75) C(80) C(75a) 179.0(11) ? . . . . C(74) C(75) C(80) C(79) -172.2(11) ? . . . . C(74) C(75) C(80) C(79a) 3.1(11) ? . . . . C(75a) C(75) C(76) C(77) -0.6(10) ? . . . . C(75a) C(75) C(76) C(77a) -175.9(12) ? . . . . C(76) C(75) C(75a) C(77) 0.6(10) ? . . . . C(76) C(75) C(75a) C(78) 41(11) ? . . . . C(76) C(75) C(75a) C(79) 170.2(14) ? . . . . C(76) C(75) C(75a) C(80) 179.1(9) ? . . . . C(75a) C(75) C(77a) C(74) -179.6(13) ? . . . . C(75a) C(75) C(77a) C(76) 4.9(14) ? . . . . C(77a) C(75) C(75a) C(76) -5.4(15) ? . . . . C(77a) C(75) C(75a) C(77) -5(2) ? . . . . C(77a) C(75) C(75a) C(78) 36(11) ? . . . . C(77a) C(75) C(75a) C(79) 164.8(17) ? . . . . C(77a) C(75) C(75a) C(80) 173.7(18) ? . . . . C(75a) C(75) C(79a) C(74) -179.7(9) ? . . . . C(75a) C(75) C(79a) C(80) 3.7(9) ? . . . . C(79a) C(75) C(75a) C(76) 177.6(11) ? . . . . C(79a) C(75) C(75a) C(77) 178.2(11) ? . . . . C(79a) C(75) C(75a) C(78) -141(11) ? . . . . C(79a) C(75) C(75a) C(79) -12.2(16) ? . . . . C(79a) C(75) C(75a) C(80) -3.3(8) ? . . . . C(75a) C(75) C(80) C(79) 8.8(11) ? . . . . C(75a) C(75) C(80) C(79a) -175.8(11) ? . . . . C(80) C(75) C(75a) C(76) -179.1(9) ? . . . . C(80) C(75) C(75a) C(77) -178.5(13) ? . . . . C(80) C(75) C(75a) C(78) -138(11) ? . . . . C(80) C(75) C(75a) C(79) -8.8(12) ? . . . . C(76) C(75) C(77a) C(74) 175.5(10) ? . . . . C(77a) C(75) C(76) C(75a) 175.9(12) ? . . . . C(77a) C(75) C(76) C(77) 175.3(12) ? . . . . C(76) C(75) C(79a) C(74) -170(4) ? . . . . C(76) C(75) C(79a) C(80) 13(4) ? . . . . C(79a) C(75) C(76) C(75a) -11(4) ? . . . . C(79a) C(75) C(76) C(77) -11(5) ? . . . . C(79a) C(75) C(76) C(77a) 174(5) ? . . . . C(76) C(75) C(80) C(75a) -0.9(9) ? . . . . C(76) C(75) C(80) C(79) 7.9(15) ? . . . . C(76) C(75) C(80) C(79a) -176.7(12) ? . . . . C(80) C(75) C(76) C(75a) 0.9(9) ? . . . . C(80) C(75) C(76) C(77) 0.3(11) ? . . . . C(80) C(75) C(76) C(77a) -175.0(15) ? . . . . C(77a) C(75) C(79a) C(74) 2.8(13) ? . . . . C(77a) C(75) C(79a) C(80) -173.8(15) ? . . . . C(79a) C(75) C(77a) C(74) -2.8(13) ? . . . . C(79a) C(75) C(77a) C(76) -178.4(13) ? . . . . C(77a) C(75) C(80) C(75a) -156(6) ? . . . . C(77a) C(75) C(80) C(79) -147(6) ? . . . . C(77a) C(75) C(80) C(79a) 28(6) ? . . . . C(80) C(75) C(77a) C(74) -27(6) ? . . . . C(80) C(75) C(77a) C(76) 157(6) ? . . . . C(79a) C(75) C(80) C(75a) 175.8(11) ? . . . . C(79a) C(75) C(80) C(79) -175.4(14) ? . . . . C(80) C(75) C(79a) C(74) 176.6(11) ? . . . . C(75) C(75a) C(76) C(77) 179.4(10) ? . . . . C(75) C(75a) C(76) C(77a) 3.1(9) ? . . . . C(75) C(75a) C(77) C(76) -0.6(10) ? . . . . C(75) C(75a) C(77) C(78) 175.9(12) ? . . . . C(75) C(75a) C(78) C(77) -43(11) ? . . . . C(75) C(75a) C(78) C(79) 131(11) ? . . . . C(75) C(75a) C(79) C(78) -175.4(13) ? . . . . C(75) C(75a) C(79) C(80) 9.3(12) ? . . . . C(75) C(75a) C(80) C(79) -170.9(12) ? . . . . C(75) C(75a) C(80) C(79a) 5.2(14) ? . . . . C(76) C(75a) C(77) C(78) 176.4(10) ? . . . . C(77) C(75a) C(76) C(75) -179.4(10) ? . . . . C(77) C(75a) C(76) C(77a) -176.3(10) ? . . . . C(76) C(75a) C(78) C(77) -3.7(11) ? . . . . C(76) C(75a) C(78) C(79) 170.2(14) ? . . . . C(78) C(75a) C(76) C(75) -176.0(12) ? . . . . C(78) C(75a) C(76) C(77) 3.4(10) ? . . . . C(78) C(75a) C(76) C(77a) -172.9(10) ? . . . . C(76) C(75a) C(79) C(78) -117(7) ? . . . . C(76) C(75a) C(79) C(80) 68(7) ? . . . . C(79) C(75a) C(76) C(75) -64(7) ? . . . . C(79) C(75a) C(76) C(77) 116(7) ? . . . . C(79) C(75a) C(76) C(77a) -61(7) ? . . . . C(76) C(75a) C(80) C(75) 0.9(9) ? . . . . C(76) C(75a) C(80) C(79) -170.0(14) ? . . . . C(76) C(75a) C(80) C(79a) 6.1(18) ? . . . . C(80) C(75a) C(76) C(75) -0.9(9) ? . . . . C(80) C(75a) C(76) C(77) 178.5(13) ? . . . . C(80) C(75a) C(76) C(77a) 2.2(13) ? . . . . C(77) C(75a) C(78) C(79) 173.9(13) ? . . . . C(78) C(75a) C(77) C(76) -176.4(10) ? . . . . C(77) C(75a) C(79) C(78) -5.9(13) ? . . . . C(77) C(75a) C(79) C(80) 178.9(14) ? . . . . C(79) C(75a) C(77) C(76) -170.1(14) ? . . . . C(79) C(75a) C(77) C(78) 6.3(13) ? . . . . C(77) C(75a) C(80) C(75) 148(29) ? . . . . C(77) C(75a) C(80) C(79) -23(29) ? . . . . C(77) C(75a) C(80) C(79a) 154(28) ? . . . . C(80) C(75a) C(77) C(76) -148(29) ? . . . . C(80) C(75a) C(77) C(78) 28(29) ? . . . . C(78) C(75a) C(79) C(80) -175.3(12) ? . . . . C(79) C(75a) C(78) C(77) -173.9(13) ? . . . . C(78) C(75a) C(80) C(75) 175.8(13) ? . . . . C(78) C(75a) C(80) C(79) 5.0(12) ? . . . . C(78) C(75a) C(80) C(79a) -179.0(13) ? . . . . C(80) C(75a) C(78) C(77) -178.6(13) ? . . . . C(80) C(75a) C(78) C(79) -4.7(11) ? . . . . C(79) C(75a) C(80) C(75) 170.9(12) ? . . . . C(79) C(75a) C(80) C(79a) 176.1(17) ? . . . . C(80) C(75a) C(79) C(78) 175.3(12) ? . . . . C(75) C(76) C(77) C(75a) 0.6(11) ? . . . . C(75) C(76) C(77) C(78) -3.2(17) ? . . . . C(75) C(76) C(77a) C(74) -6.3(14) ? . . . . C(75a) C(76) C(77) C(78) -3.8(11) ? . . . . C(75a) C(76) C(77a) C(74) -10(2) ? . . . . C(75a) C(76) C(77a) C(75) -3.9(11) ? . . . . C(77) C(76) C(77a) C(74) -24(5) ? . . . . C(77) C(76) C(77a) C(75) -17(4) ? . . . . C(77a) C(76) C(77) C(75a) 15(4) ? . . . . C(77a) C(76) C(77) C(78) 11(5) ? . . . . C(75a) C(77) C(78) C(79) -5.5(11) ? . . . . C(76) C(77) C(78) C(75a) 3.6(10) ? . . . . C(76) C(77) C(78) C(79) -1.8(18) ? . . . . C(75a) C(78) C(79) C(80) 5.2(13) ? . . . . C(77) C(78) C(79) C(75a) 5.7(12) ? . . . . C(77) C(78) C(79) C(80) 11(2) ? . . . . C(75a) C(79) C(80) C(75) -8.9(11) ? . . . . C(75a) C(79) C(80) C(79a) -162(8) ? . . . . C(78) C(79) C(80) C(75) -14(2) ? . . . . C(78) C(79) C(80) C(75a) -5.0(13) ? . . . . C(78) C(79) C(80) C(79a) -167(7) ? . . . . C(74) C(79a) C(80) C(75) -2.9(10) ? . . . . C(74) C(79a) C(80) C(75a) -7.7(19) ? . . . . C(74) C(79a) C(80) C(79) 152(8) ? . . . . C(75) C(79a) C(80) C(75a) -4.7(13) ? . . . . C(75) C(79a) C(80) C(79) 155(8) ? . . . . #============================================================================== # 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 #============================================================================== # Attachment '- Pdsalpn.cif' #============================================================================== data__3 _database_code_depnum_ccdc_archive 'CCDC 801077' #TrackingRef '- Pdsalpn.cif' _audit_creation_date 2008-12-26 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H48 N2 O2 Pd ' _chemical_formula_moiety 'C33 H48 N2 O2 Pd ' _chemical_formula_weight 611.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,-Y,1/2+Z 4 1/2-X,1/2-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,+Y,1/2-Z 8 1/2+X,1/2+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 26.6710(13) _cell_length_b 11.3844(5) _cell_length_c 10.1169(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3071.8(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15320 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288.00 _exptl_absorpt_coefficient_mu 0.635 _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 0.440 _exptl_absorpt_correction_T_max 0.981 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_ambient_temperature 133(2) _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27589 _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 3513 _reflns_number_gt 13776 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2252 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 27589 _refine_ls_number_parameters 200 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0023Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.70 _refine_diff_density_min -1.80 _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 0.003 0.002 ; 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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.999 1.007 ; 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 Pd(1) Pd 0.5000 0.02018(2) 0.7500 0.02096(7) Uani 1.00 2 d S . . O(2) O 0.53565(6) 0.15326(13) 0.83812(18) 0.0265(4) Uani 1.00 1 d . . . N(3) N 0.53371(7) -0.09819(15) 0.8658(2) 0.0263(5) Uani 1.00 1 d . . . C(1) C 0.57488(8) 0.14627(19) 0.9164(2) 0.0248(6) Uani 1.00 1 d . . . C(2) C 0.60582(9) 0.24817(19) 0.9383(2) 0.0262(6) Uani 1.00 1 d . . . C(3) C 0.64398(9) 0.2402(2) 1.0299(2) 0.0300(7) Uani 1.00 1 d . . . C(4) C 0.65566(9) 0.1386(2) 1.1031(2) 0.0287(7) Uani 1.00 1 d . . . C(5) C 0.62675(9) 0.0409(2) 1.0795(2) 0.0287(7) Uani 1.00 1 d . . . C(6) C 0.58776(10) 0.0424(2) 0.9845(2) 0.0265(6) Uani 1.00 1 d . . . C(7) C 0.56480(9) -0.0690(2) 0.9578(2) 0.0281(7) Uani 1.00 1 d . . . C(8) C 0.52263(11) -0.2258(2) 0.8588(3) 0.0365(8) Uani 1.00 1 d . . . C(9) C 0.52268(19) -0.2620(4) 0.7216(5) 0.0267(14) Uani 0.50 1 d P . . C(10) C 0.59595(8) 0.3613(2) 0.8592(2) 0.0268(6) Uani 1.00 1 d . . . C(11) C 0.54478(8) 0.4144(2) 0.8985(2) 0.0323(7) Uani 1.00 1 d . . . C(12) C 0.59684(9) 0.3364(2) 0.7114(2) 0.0353(8) Uani 1.00 1 d . . . C(13) C 0.63563(10) 0.4558(2) 0.8882(3) 0.0391(8) Uani 1.00 1 d . . . C(14) C 0.69905(10) 0.1378(2) 1.2016(3) 0.0371(8) Uani 1.00 1 d . . . C(15) C 0.70663(13) 0.0185(2) 1.2653(3) 0.0568(11) Uani 1.00 1 d . . . C(16) C 0.68749(13) 0.2255(3) 1.3127(3) 0.0732(13) Uani 1.00 1 d . . . C(17) C 0.74684(10) 0.1733(3) 1.1327(3) 0.0672(11) Uani 1.00 1 d . . . H(1) H 0.6641 0.3080 1.0436 0.036 Uiso 1.00 1 c R . . H(2) H 0.6332 -0.0290 1.1280 0.035 Uiso 1.00 1 c R . . H(3) H 0.5732 -0.1303 1.0177 0.034 Uiso 1.00 1 c R . . H(4) H 0.5474 -0.2688 0.9058 0.044 Uiso 1.00 1 c R . . H(5) H 0.4906 -0.2405 0.8965 0.044 Uiso 1.00 1 c R . . H(6) H 0.5193 0.3834 0.8428 0.040 Uiso 1.00 1 c R . . H(7) H 0.5457 0.4975 0.8899 0.040 Uiso 1.00 1 c R . . H(8) H 0.5378 0.3942 0.9878 0.040 Uiso 1.00 1 c R . . H(9) H 0.6300 0.3458 0.6786 0.043 Uiso 1.00 1 c R . . H(10) H 0.5750 0.3896 0.6674 0.044 Uiso 1.00 1 c R . . H(11) H 0.5859 0.2582 0.6961 0.044 Uiso 1.00 1 c R . . H(12) H 0.6249 0.5024 0.9608 0.048 Uiso 1.00 1 c R . . H(13) H 0.6396 0.5043 0.8125 0.048 Uiso 1.00 1 c R . . H(14) H 0.6667 0.4196 0.9091 0.048 Uiso 1.00 1 c R . . H(15) H 0.6871 0.0139 1.3437 0.069 Uiso 1.00 1 c R . . H(16) H 0.7410 0.0080 1.2865 0.069 Uiso 1.00 1 c R . . H(17) H 0.6963 -0.0411 1.2055 0.069 Uiso 1.00 1 c R . . H(18) H 0.7002 0.3006 1.2896 0.088 Uiso 1.00 1 c R . . H(19) H 0.7026 0.1999 1.3927 0.088 Uiso 1.00 1 c R . . H(20) H 0.6522 0.2302 1.3242 0.088 Uiso 1.00 1 c R . . H(21) H 0.7628 0.1051 1.0985 0.081 Uiso 1.00 1 c R . . H(22) H 0.7686 0.2113 1.1935 0.081 Uiso 1.00 1 c R . . H(23) H 0.7392 0.2254 1.0622 0.081 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.02054(14) 0.01629(13) 0.02604(16) 0.0000 0.00072(12) 0.0000 O(2) 0.0235(8) 0.0196(8) 0.0366(11) 0.0016(6) -0.0051(8) -0.0008(7) N(3) 0.0252(10) 0.0175(9) 0.0362(14) 0.0040(8) 0.0037(10) 0.0007(9) C(1) 0.0191(11) 0.0242(12) 0.0310(16) -0.0012(9) 0.0008(10) -0.0060(11) C(2) 0.0266(13) 0.0227(12) 0.0292(16) -0.0009(10) 0.0051(11) -0.0020(10) C(3) 0.0258(13) 0.0331(14) 0.0312(17) 0.0015(10) 0.0045(11) -0.0031(11) C(4) 0.0270(12) 0.0353(14) 0.0238(15) 0.0098(11) -0.0004(11) -0.0045(11) C(5) 0.0306(13) 0.0285(13) 0.0271(15) 0.0093(11) -0.0027(11) 0.0035(11) C(6) 0.0291(13) 0.0246(12) 0.0257(15) 0.0012(10) -0.0031(11) -0.0019(10) C(7) 0.0289(13) 0.0275(13) 0.0279(15) 0.0063(11) -0.0007(12) 0.0046(11) C(8) 0.0428(16) 0.0231(13) 0.0435(19) -0.0030(12) -0.0073(15) 0.0044(12) C(9) 0.039(2) 0.021(2) 0.020(3) 0.002(2) 0.002(2) 0.0006(18) C(10) 0.0221(12) 0.0245(12) 0.0338(16) -0.0045(9) 0.0007(11) -0.0003(11) C(11) 0.0266(13) 0.0249(12) 0.0454(19) 0.0016(10) 0.0024(12) 0.0018(12) C(12) 0.0325(14) 0.0351(15) 0.0381(18) -0.0058(12) 0.0026(12) 0.0039(12) C(13) 0.0381(15) 0.0301(14) 0.049(2) -0.0119(12) -0.0033(14) 0.0025(13) C(14) 0.0299(14) 0.0398(15) 0.0416(18) 0.0050(12) -0.0104(13) -0.0011(13) C(15) 0.0331(16) 0.082(2) 0.055(2) -0.0065(15) -0.0150(15) 0.0243(19) C(16) 0.075(2) 0.101(2) 0.043(2) 0.003(2) -0.018(2) -0.020(2) C(17) 0.0337(16) 0.105(2) 0.063(2) -0.0050(18) -0.0152(17) 0.025(2) #============================================================================== _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 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) O(2) 1.9985(15) yes . . Pd(1) O(2) 1.9985(15) yes . 7_656 Pd(1) N(3) 1.9992(19) yes . . Pd(1) N(3) 1.9992(19) yes . 7_656 O(2) C(1) 1.315(2) yes . . N(3) C(7) 1.290(3) yes . . N(3) C(8) 1.484(2) yes . . C(1) C(2) 1.441(3) yes . . C(1) C(6) 1.411(3) yes . . C(2) C(3) 1.380(3) yes . . C(2) C(10) 1.539(3) yes . . C(3) C(4) 1.409(3) yes . . C(4) C(5) 1.374(3) yes . . C(4) C(14) 1.527(3) yes . . C(5) C(6) 1.416(3) yes . . C(6) C(7) 1.434(3) yes . . C(8) C(9) 1.448(5) yes . . C(8) C(9) 1.514(5) yes . 7_656 C(9) C(9) 1.340(7) yes . 7_656 C(10) C(11) 1.545(3) yes . . C(10) C(12) 1.522(3) yes . . C(10) C(13) 1.538(3) yes . . C(14) C(15) 1.517(4) yes . . C(14) C(16) 1.534(4) yes . . C(14) C(17) 1.508(4) yes . . C(3) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.950 no . . C(8) H(5) 0.950 no . . C(9) H(5) 1.270 no . 7_656 C(11) H(6) 0.950 no . . C(11) H(7) 0.950 no . . C(11) H(8) 0.950 no . . C(12) H(9) 0.950 no . . C(12) H(10) 0.950 no . . C(12) H(11) 0.950 no . . C(13) H(12) 0.950 no . . C(13) H(13) 0.950 no . . C(13) H(14) 0.950 no . . C(15) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(15) H(17) 0.950 no . . C(16) H(18) 0.950 no . . C(16) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(17) H(21) 0.950 no . . C(17) H(22) 0.950 no . . C(17) H(23) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(2) Pd(1) O(2) 81.41(6) yes . . 7_656 O(2) Pd(1) N(3) 92.04(7) yes . . . O(2) Pd(1) N(3) 170.52(7) yes . . 7_656 O(2) Pd(1) N(3) 170.52(7) yes 7_656 . . O(2) Pd(1) N(3) 92.04(7) yes 7_656 . 7_656 N(3) Pd(1) N(3) 95.24(7) yes . . 7_656 Pd(1) O(2) C(1) 126.98(13) yes . . . Pd(1) N(3) C(7) 122.58(15) yes . . . Pd(1) N(3) C(8) 122.84(16) yes . . . C(7) N(3) C(8) 114.5(2) yes . . . O(2) C(1) C(2) 120.0(2) yes . . . O(2) C(1) C(6) 122.6(2) yes . . . C(2) C(1) C(6) 117.4(2) yes . . . C(1) C(2) C(3) 118.2(2) yes . . . C(1) C(2) C(10) 119.8(2) yes . . . C(3) C(2) C(10) 122.0(2) yes . . . C(2) C(3) C(4) 124.8(2) yes . . . C(3) C(4) C(5) 116.7(2) yes . . . C(3) C(4) C(14) 121.1(2) yes . . . C(5) C(4) C(14) 122.3(2) yes . . . C(4) C(5) C(6) 121.3(2) yes . . . C(1) C(6) C(5) 121.4(2) yes . . . C(1) C(6) C(7) 123.1(2) yes . . . C(5) C(6) C(7) 115.5(2) yes . . . N(3) C(7) C(6) 129.6(2) yes . . . N(3) C(8) C(9) 108.9(2) yes . . . N(3) C(8) C(9) 116.8(2) yes . . 7_656 C(9) C(8) C(9) 53.7(2) yes . . 7_656 C(8) C(9) C(8) 115.9(3) yes . . 7_656 C(8) C(9) C(9) 65.6(3) yes . . 7_656 C(8) C(9) C(9) 60.6(3) yes 7_656 . 7_656 C(2) C(10) C(11) 110.1(2) yes . . . C(2) C(10) C(12) 110.6(2) yes . . . C(2) C(10) C(13) 111.6(2) yes . . . C(11) C(10) C(12) 109.9(2) yes . . . C(11) C(10) C(13) 106.57(19) yes . . . C(12) C(10) C(13) 107.9(2) yes . . . C(4) C(14) C(15) 112.6(2) yes . . . C(4) C(14) C(16) 108.8(2) yes . . . C(4) C(14) C(17) 109.7(2) yes . . . C(15) C(14) C(16) 107.3(2) yes . . . C(15) C(14) C(17) 108.9(2) yes . . . C(16) C(14) C(17) 109.5(2) yes . . . C(2) C(3) H(1) 117.5 no . . . C(4) C(3) H(1) 117.7 no . . . C(4) C(5) H(2) 119.2 no . . . C(6) C(5) H(2) 119.5 no . . . N(3) C(7) H(3) 115.0 no . . . C(6) C(7) H(3) 115.4 no . . . N(3) C(8) H(4) 110.0 no . . . N(3) C(8) H(5) 109.5 no . . . C(9) C(8) H(4) 109.4 no . . . C(9) C(8) H(5) 109.6 no . . . C(9) C(8) H(4) 133.2 no 7_656 . . C(9) C(8) H(5) 56.6 no 7_656 . . H(4) C(8) H(5) 109.5 no . . . C(8) C(9) H(5) 147.9 no . . 7_656 C(8) C(9) H(5) 38.7 no 7_656 . 7_656 C(9) C(9) H(5) 98.7 no 7_656 . 7_656 C(10) C(11) H(6) 109.4 no . . . C(10) C(11) H(7) 110.1 no . . . C(10) C(11) H(8) 108.9 no . . . H(6) C(11) H(7) 109.5 no . . . H(6) C(11) H(8) 109.5 no . . . H(7) C(11) H(8) 109.5 no . . . C(10) C(12) H(9) 109.7 no . . . C(10) C(12) H(10) 109.4 no . . . C(10) C(12) H(11) 109.3 no . . . H(9) C(12) H(10) 109.5 no . . . H(9) C(12) H(11) 109.5 no . . . H(10) C(12) H(11) 109.5 no . . . C(10) C(13) H(12) 109.3 no . . . C(10) C(13) H(13) 109.3 no . . . C(10) C(13) H(14) 109.8 no . . . H(12) C(13) H(13) 109.5 no . . . H(12) C(13) H(14) 109.5 no . . . H(13) C(13) H(14) 109.5 no . . . C(14) C(15) H(15) 109.4 no . . . C(14) C(15) H(16) 109.7 no . . . C(14) C(15) H(17) 109.3 no . . . H(15) C(15) H(16) 109.5 no . . . H(15) C(15) H(17) 109.5 no . . . H(16) C(15) H(17) 109.5 no . . . C(14) C(16) H(18) 109.5 no . . . C(14) C(16) H(19) 109.9 no . . . C(14) C(16) H(20) 109.0 no . . . H(18) C(16) H(19) 109.5 no . . . H(18) C(16) H(20) 109.5 no . . . H(19) C(16) H(20) 109.5 no . . . C(14) C(17) H(21) 109.2 no . . . C(14) C(17) H(22) 109.8 no . . . C(14) C(17) H(23) 109.4 no . . . H(21) C(17) H(22) 109.5 no . . . H(21) C(17) H(23) 109.5 no . . . H(22) C(17) H(23) 109.5 no . . . C(8) H(5) C(9) 84.7 no . . 7_656 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(2) Pd(1) O(2) C(1) -172.5(2) ? . . 7_656 7_656 O(2) Pd(1) O(2) C(1) -172.5(2) ? 7_656 . . . O(2) Pd(1) N(3) C(7) 1.3(2) ? . . . . O(2) Pd(1) N(3) C(8) 177.25(19) ? . . . . N(3) Pd(1) O(2) C(1) 14.4(2) ? . . . . O(2) Pd(1) N(3) C(7) -44.8(5) ? . . 7_656 7_656 O(2) Pd(1) N(3) C(8) 131.2(3) ? . . 7_656 7_656 N(3) Pd(1) O(2) C(1) -125.8(4) ? 7_656 . . . O(2) Pd(1) N(3) C(7) -44.8(5) ? 7_656 . . . O(2) Pd(1) N(3) C(8) 131.2(3) ? 7_656 . . . N(3) Pd(1) O(2) C(1) -125.8(4) ? . . 7_656 7_656 O(2) Pd(1) N(3) C(7) 1.3(2) ? 7_656 . 7_656 7_656 O(2) Pd(1) N(3) C(8) 177.25(19) ? 7_656 . 7_656 7_656 N(3) Pd(1) O(2) C(1) 14.4(2) ? 7_656 . 7_656 7_656 N(3) Pd(1) N(3) C(7) 175.2(2) ? . . 7_656 7_656 N(3) Pd(1) N(3) C(8) -8.8(2) ? . . 7_656 7_656 N(3) Pd(1) N(3) C(7) 175.2(2) ? 7_656 . . . N(3) Pd(1) N(3) C(8) -8.8(2) ? 7_656 . . . Pd(1) O(2) C(1) C(2) 160.13(17) ? . . . . Pd(1) O(2) C(1) C(6) -21.6(3) ? . . . . Pd(1) N(3) C(7) C(6) -10.9(3) ? . . . . Pd(1) N(3) C(8) C(9) 46.7(3) ? . . . . Pd(1) N(3) C(8) C(9) -11.5(3) ? . . . 7_656 C(7) N(3) C(8) C(9) -137.0(3) ? . . . . C(7) N(3) C(8) C(9) 164.8(2) ? . . . 7_656 C(8) N(3) C(7) C(6) 172.8(2) ? . . . . O(2) C(1) C(2) C(3) 174.4(2) ? . . . . O(2) C(1) C(2) C(10) -6.1(3) ? . . . . O(2) C(1) C(6) C(5) -172.7(2) ? . . . . O(2) C(1) C(6) C(7) 10.9(3) ? . . . . C(2) C(1) C(6) C(5) 5.5(3) ? . . . . C(2) C(1) C(6) C(7) -170.8(2) ? . . . . C(6) C(1) C(2) C(3) -3.9(3) ? . . . . C(6) C(1) C(2) C(10) 175.6(2) ? . . . . C(1) C(2) C(3) C(4) 1.0(3) ? . . . . C(1) C(2) C(10) C(11) 66.7(2) ? . . . . C(1) C(2) C(10) C(12) -55.0(2) ? . . . . C(1) C(2) C(10) C(13) -175.1(2) ? . . . . C(3) C(2) C(10) C(11) -113.8(2) ? . . . . C(3) C(2) C(10) C(12) 124.5(2) ? . . . . C(3) C(2) C(10) C(13) 4.4(3) ? . . . . C(10) C(2) C(3) C(4) -178.5(2) ? . . . . C(2) C(3) C(4) C(5) 0.5(3) ? . . . . C(2) C(3) C(4) C(14) 179.4(2) ? . . . . C(3) C(4) C(5) C(6) 1.0(3) ? . . . . C(3) C(4) C(14) C(15) -177.5(2) ? . . . . C(3) C(4) C(14) C(16) 63.7(3) ? . . . . C(3) C(4) C(14) C(17) -56.1(3) ? . . . . C(5) C(4) C(14) C(15) 1.4(3) ? . . . . C(5) C(4) C(14) C(16) -117.5(2) ? . . . . C(5) C(4) C(14) C(17) 122.7(2) ? . . . . C(14) C(4) C(5) C(6) -177.8(2) ? . . . . C(4) C(5) C(6) C(1) -4.2(3) ? . . . . C(4) C(5) C(6) C(7) 172.4(2) ? . . . . C(1) C(6) C(7) N(3) 6.8(4) ? . . . . C(5) C(6) C(7) N(3) -169.7(2) ? . . . . N(3) C(8) C(9) C(8) -74.8(3) ? . . . 7_656 N(3) C(8) C(9) C(9) -109.9(3) ? . . . 7_656 N(3) C(8) C(9) C(8) 57.6(4) ? . . 7_656 7_656 N(3) C(8) C(9) C(9) 94.6(3) ? . . 7_656 . C(9) C(8) C(9) C(8) -36.9(3) ? . . 7_656 7_656 C(9) C(8) C(9) C(8) 35.1(3) ? 7_656 . . 7_656 C(8) C(9) C(9) C(8) 143.6(3) ? . . 7_656 7_656 C(8) C(9) C(9) C(8) -143.6(3) ? 7_656 . 7_656 . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Pd(1) C(1) 2.981(2) ? . . Pd(1) C(1) 2.981(2) ? . 7_656 Pd(1) C(6) 3.342(2) ? . . Pd(1) C(6) 3.342(2) ? . 7_656 Pd(1) C(7) 2.905(2) ? . . Pd(1) C(7) 3.469(2) ? . 3_554 Pd(1) C(7) 3.469(2) ? . 5_657 Pd(1) C(7) 2.905(2) ? . 7_656 Pd(1) C(8) 3.069(2) ? . . Pd(1) C(8) 3.069(2) ? . 7_656 Pd(1) C(9) 3.281(4) ? . . Pd(1) C(9) 3.281(4) ? . 7_656 O(2) O(2) 2.607(2) ? . 7_656 O(2) N(3) 2.877(2) ? . . O(2) N(3) 3.576(2) ? . 5_657 O(2) C(2) 2.387(2) ? . . O(2) C(6) 2.391(3) ? . . O(2) C(7) 2.911(2) ? . . O(2) C(7) 3.516(3) ? . 5_657 O(2) C(8) 3.535(3) ? . 5_657 O(2) C(10) 2.871(2) ? . . O(2) C(11) 3.045(2) ? . . O(2) C(12) 2.942(3) ? . . N(3) O(2) 2.877(2) ? . . N(3) O(2) 3.576(2) ? . 5_657 N(3) N(3) 2.954(2) ? . 7_656 N(3) C(1) 3.035(2) ? . . N(3) C(6) 2.466(3) ? . . N(3) C(8) 3.087(3) ? . 7_656 N(3) C(9) 2.386(5) ? . . N(3) C(9) 2.553(5) ? . 7_656 C(1) Pd(1) 2.981(2) ? . . C(1) N(3) 3.035(2) ? . . C(1) C(3) 2.420(3) ? . . C(1) C(4) 2.867(3) ? . . C(1) C(5) 2.465(3) ? . . C(1) C(7) 2.501(3) ? . . C(1) C(8) 3.571(3) ? . 5_657 C(1) C(10) 2.578(3) ? . . C(1) C(11) 3.161(3) ? . . C(1) C(12) 3.055(3) ? . . C(2) O(2) 2.387(2) ? . . C(2) C(4) 2.471(3) ? . . C(2) C(5) 2.815(3) ? . . C(2) C(6) 2.437(3) ? . . C(2) C(11) 2.528(3) ? . . C(2) C(12) 2.517(3) ? . . C(2) C(13) 2.545(3) ? . . C(3) C(1) 2.420(3) ? . . C(3) C(5) 2.369(3) ? . . C(3) C(6) 2.744(3) ? . . C(3) C(10) 2.554(3) ? . . C(3) C(11) 3.563(3) ? . . C(3) C(13) 2.851(3) ? . . C(3) C(14) 2.557(3) ? . . C(3) C(16) 3.092(4) ? . . C(3) C(17) 3.031(3) ? . . C(4) C(1) 2.867(3) ? . . C(4) C(2) 2.471(3) ? . . C(4) C(6) 2.433(3) ? . . C(4) C(15) 2.532(4) ? . . C(4) C(16) 2.489(4) ? . . C(4) C(17) 2.482(3) ? . . C(5) C(1) 2.465(3) ? . . C(5) C(2) 2.815(3) ? . . C(5) C(3) 2.369(3) ? . . C(5) C(7) 2.411(3) ? . . C(5) C(14) 2.542(3) ? . . C(5) C(15) 2.852(4) ? . . C(5) C(16) 3.550(4) ? . . C(5) C(17) 3.580(3) ? . . C(6) Pd(1) 3.342(2) ? . . C(6) O(2) 2.391(3) ? . . C(6) N(3) 2.466(3) ? . . C(6) C(2) 2.437(3) ? . . C(6) C(3) 2.744(3) ? . . C(6) C(4) 2.433(3) ? . . C(7) Pd(1) 2.905(2) ? . . C(7) Pd(1) 3.469(2) ? . 3_555 C(7) O(2) 2.911(2) ? . . C(7) O(2) 3.516(3) ? . 5_657 C(7) C(1) 2.501(3) ? . . C(7) C(5) 2.411(3) ? . . C(7) C(8) 2.335(3) ? . . C(7) C(9) 3.435(5) ? . . C(8) Pd(1) 3.069(2) ? . . C(8) O(2) 3.535(3) ? . 5_657 C(8) N(3) 3.087(3) ? . 7_656 C(8) C(1) 3.571(3) ? . 5_657 C(8) C(7) 2.335(3) ? . . C(8) C(8) 2.511(4) ? . 7_656 C(9) Pd(1) 3.281(4) ? . . C(9) N(3) 2.386(5) ? . . C(9) N(3) 2.553(5) ? . 7_656 C(9) C(7) 3.435(5) ? . . C(10) O(2) 2.871(2) ? . . C(10) C(1) 2.578(3) ? . . C(10) C(3) 2.554(3) ? . . C(11) O(2) 3.045(2) ? . . C(11) C(1) 3.161(3) ? . . C(11) C(2) 2.528(3) ? . . C(11) C(3) 3.563(3) ? . . C(11) C(12) 2.510(3) ? . . C(11) C(13) 2.471(3) ? . . C(12) O(2) 2.942(3) ? . . C(12) C(1) 3.055(3) ? . . C(12) C(2) 2.517(3) ? . . C(12) C(11) 2.510(3) ? . . C(12) C(13) 2.473(3) ? . . C(13) C(2) 2.545(3) ? . . C(13) C(3) 2.851(3) ? . . C(13) C(11) 2.471(3) ? . . C(13) C(12) 2.473(3) ? . . C(14) C(3) 2.557(3) ? . . C(14) C(5) 2.542(3) ? . . C(15) C(4) 2.532(4) ? . . C(15) C(5) 2.852(4) ? . . C(15) C(16) 2.458(5) ? . . C(15) C(17) 2.460(4) ? . . C(16) C(3) 3.092(4) ? . . C(16) C(4) 2.489(4) ? . . C(16) C(5) 3.550(4) ? . . C(16) C(15) 2.458(5) ? . . C(16) C(17) 2.485(4) ? . . C(17) C(3) 3.031(3) ? . . C(17) C(4) 2.482(3) ? . . C(17) C(5) 3.580(3) ? . . C(17) C(15) 2.460(4) ? . . C(17) C(16) 2.485(4) ? . . Pd(1) H(3) 3.302 ? . 3_554 Pd(1) H(3) 3.302 ? . 5_657 Pd(1) H(5) 3.327 ? . . Pd(1) H(5) 3.327 ? . 7_656 Pd(1) H(11) 3.590 ? . . Pd(1) H(11) 3.590 ? . 7_656 O(2) H(3) 3.403 ? . 3_554 O(2) H(3) 3.259 ? . 5_657 O(2) H(5) 2.947 ? . 5_657 O(2) H(6) 2.656 ? . . O(2) H(6) 3.516 ? . 7_656 O(2) H(8) 3.134 ? . . O(2) H(10) 3.365 ? . . O(2) H(11) 2.300 ? . . O(2) H(11) 3.473 ? . 7_656 N(3) H(3) 1.898 ? . . N(3) H(4) 2.017 ? . . N(3) H(5) 2.011 ? . . N(3) H(5) 3.177 ? . 7_656 N(3) H(20) 3.524 ? . 3_554 C(1) H(1) 3.272 ? . . C(1) H(2) 3.313 ? . . C(1) H(2) 3.566 ? . 3_554 C(1) H(3) 3.311 ? . . C(1) H(5) 2.790 ? . 5_657 C(1) H(6) 3.168 ? . . C(1) H(8) 3.077 ? . . C(1) H(11) 2.584 ? . . C(1) H(15) 3.582 ? . 3_554 C(2) H(1) 2.004 ? . . C(2) H(5) 3.069 ? . 5_657 C(2) H(6) 2.936 ? . . C(2) H(7) 3.296 ? . . C(2) H(8) 2.512 ? . . C(2) H(9) 2.924 ? . . C(2) H(10) 3.283 ? . . C(2) H(11) 2.509 ? . . C(2) H(12) 2.947 ? . . C(2) H(13) 3.307 ? . . C(2) H(14) 2.556 ? . . C(3) H(2) 3.235 ? . . C(3) H(8) 3.359 ? . . C(3) H(12) 3.107 ? . . C(3) H(14) 2.456 ? . . C(3) H(18) 3.103 ? . . C(3) H(20) 2.988 ? . . C(3) H(21) 3.590 ? . . C(3) H(23) 2.565 ? . . C(4) H(1) 2.033 ? . . C(4) H(2) 2.016 ? . . C(4) H(15) 2.940 ? . . C(4) H(15) 3.257 ? . 3_554 C(4) H(16) 3.292 ? . . C(4) H(17) 2.537 ? . . C(4) H(18) 2.894 ? . . C(4) H(19) 3.262 ? . . C(4) H(20) 2.469 ? . . C(4) H(21) 2.883 ? . . C(4) H(22) 3.255 ? . . C(4) H(23) 2.471 ? . . C(5) H(1) 3.220 ? . . C(5) H(3) 2.496 ? . . C(5) H(15) 3.135 ? . . C(5) H(15) 2.945 ? . 3_554 C(5) H(17) 2.437 ? . . C(5) H(20) 3.351 ? . . C(6) H(2) 2.058 ? . . C(6) H(3) 2.032 ? . . C(6) H(5) 3.303 ? . 5_657 C(6) H(15) 3.076 ? . 3_554 C(7) H(2) 2.548 ? . . C(7) H(4) 2.379 ? . . C(7) H(5) 2.848 ? . . C(7) H(11) 3.281 ? . 3_555 C(7) H(15) 3.517 ? . 3_554 C(7) H(20) 3.260 ? . 3_554 C(8) H(3) 2.363 ? . . C(8) H(4) 3.301 ? . 7_656 C(8) H(5) 2.613 ? . 7_656 C(8) H(7) 3.226 ? . 1_545 C(8) H(8) 2.946 ? . 5_657 C(8) H(20) 3.474 ? . 3_554 C(9) H(4) 1.979 ? . . C(9) H(4) 2.272 ? . 7_656 C(9) H(5) 1.981 ? . . C(9) H(7) 3.283 ? . 1_545 C(9) H(7) 3.478 ? . 7_646 C(9) H(8) 2.833 ? . 3_554 C(10) H(1) 2.674 ? . . C(10) H(6) 2.065 ? . . C(10) H(7) 2.073 ? . . C(10) H(8) 2.059 ? . . C(10) H(9) 2.048 ? . . C(10) H(10) 2.045 ? . . C(10) H(11) 2.043 ? . . C(10) H(12) 2.057 ? . . C(10) H(13) 2.057 ? . . C(10) H(14) 2.063 ? . . C(11) H(4) 3.565 ? . 5_657 C(11) H(5) 3.018 ? . 5_657 C(11) H(6) 3.002 ? . 7_656 C(11) H(7) 3.378 ? . 5_667 C(11) H(8) 3.304 ? . 5_667 C(11) H(9) 3.275 ? . . C(11) H(10) 2.490 ? . . C(11) H(10) 3.277 ? . 7_656 C(11) H(11) 2.926 ? . . C(11) H(12) 2.442 ? . . C(11) H(13) 2.865 ? . . C(11) H(14) 3.255 ? . . C(12) H(3) 3.122 ? . 3_554 C(12) H(4) 3.448 ? . 3_554 C(12) H(6) 2.515 ? . . C(12) H(6) 3.192 ? . 7_656 C(12) H(7) 2.912 ? . . C(12) H(8) 3.276 ? . . C(12) H(12) 3.239 ? . . C(12) H(12) 3.218 ? . 3_564 C(12) H(13) 2.450 ? . . C(12) H(14) 2.893 ? . . C(13) H(1) 2.425 ? . . C(13) H(6) 3.242 ? . . C(13) H(7) 2.445 ? . . C(13) H(8) 2.885 ? . . C(13) H(9) 2.467 ? . . C(13) H(10) 2.859 ? . . C(13) H(11) 3.255 ? . . C(13) H(16) 3.471 ? . 4_654 C(13) H(18) 3.413 ? . 3_564 C(14) H(1) 2.680 ? . . C(14) H(2) 2.693 ? . . C(14) H(15) 2.039 ? . . C(14) H(16) 2.044 ? . . C(14) H(17) 2.039 ? . . C(14) H(18) 2.057 ? . . C(14) H(19) 2.061 ? . . C(14) H(20) 2.050 ? . . C(14) H(21) 2.029 ? . . C(14) H(22) 2.037 ? . . C(14) H(23) 2.032 ? . . C(15) H(2) 2.462 ? . . C(15) H(18) 3.226 ? . . C(15) H(18) 3.520 ? . 2_645 C(15) H(19) 2.437 ? . . C(15) H(20) 2.875 ? . . C(15) H(21) 2.462 ? . . C(15) H(22) 2.842 ? . . C(15) H(23) 3.244 ? . . C(16) H(1) 2.947 ? . . C(16) H(13) 3.330 ? . 3_565 C(16) H(15) 2.429 ? . . C(16) H(16) 2.870 ? . . C(16) H(17) 3.231 ? . . C(16) H(21) 3.256 ? . . C(16) H(22) 2.482 ? . . C(16) H(23) 2.885 ? . . C(16) H(23) 3.242 ? . 4_655 C(17) H(1) 2.835 ? . . C(17) H(9) 3.325 ? . 4_655 C(17) H(15) 3.223 ? . . C(17) H(16) 2.447 ? . . C(17) H(17) 2.884 ? . . C(17) H(18) 2.484 ? . . C(17) H(19) 2.899 ? . . C(17) H(19) 3.130 ? . 4_654 C(17) H(20) 3.247 ? . . H(1) C(1) 3.272 ? . . H(1) C(2) 2.004 ? . . H(1) C(4) 2.033 ? . . H(1) C(5) 3.220 ? . . H(1) C(10) 2.674 ? . . H(1) C(13) 2.425 ? . . H(1) C(14) 2.680 ? . . H(1) C(16) 2.947 ? . . H(1) C(17) 2.835 ? . . H(1) H(8) 3.554 ? . . H(1) H(12) 2.586 ? . . H(1) H(13) 3.299 ? . . H(1) H(13) 3.520 ? . 3_565 H(1) H(14) 1.863 ? . . H(1) H(18) 2.670 ? . . H(1) H(20) 2.991 ? . . H(1) H(21) 3.546 ? . . H(1) H(22) 3.359 ? . . H(1) H(23) 2.220 ? . . H(2) C(1) 3.313 ? . . H(2) C(1) 3.566 ? . 3_555 H(2) C(3) 3.235 ? . . H(2) C(4) 2.016 ? . . H(2) C(6) 2.058 ? . . H(2) C(7) 2.548 ? . . H(2) C(14) 2.693 ? . . H(2) C(15) 2.462 ? . . H(2) H(3) 2.265 ? . . H(2) H(11) 2.978 ? . 3_555 H(2) H(15) 2.660 ? . . H(2) H(15) 3.220 ? . 3_554 H(2) H(16) 3.321 ? . . H(2) H(17) 1.863 ? . . H(2) H(19) 3.589 ? . 3_554 H(2) H(20) 3.592 ? . . H(3) Pd(1) 3.302 ? . 3_555 H(3) O(2) 3.403 ? . 3_555 H(3) O(2) 3.259 ? . 5_657 H(3) N(3) 1.898 ? . . H(3) C(1) 3.311 ? . . H(3) C(5) 2.496 ? . . H(3) C(6) 2.032 ? . . H(3) C(8) 2.363 ? . . H(3) C(12) 3.122 ? . 3_555 H(3) H(2) 2.265 ? . . H(3) H(4) 2.059 ? . . H(3) H(5) 2.816 ? . . H(3) H(9) 3.312 ? . 3_555 H(3) H(10) 3.318 ? . 3_555 H(3) H(11) 2.344 ? . 3_555 H(3) H(20) 3.093 ? . 3_554 H(4) N(3) 2.017 ? . . H(4) C(7) 2.379 ? . . H(4) C(8) 3.301 ? . 7_656 H(4) C(9) 1.979 ? . . H(4) C(9) 2.272 ? . 7_656 H(4) C(11) 3.565 ? . 5_657 H(4) C(12) 3.448 ? . 3_555 H(4) H(3) 2.059 ? . . H(4) H(5) 1.551 ? . . H(4) H(5) 3.238 ? . 7_656 H(4) H(6) 3.368 ? . 5_657 H(4) H(7) 2.667 ? . 1_545 H(4) H(8) 2.891 ? . 5_657 H(4) H(10) 3.072 ? . 3_555 H(4) H(11) 3.114 ? . 3_555 H(4) H(12) 3.372 ? . 1_545 H(4) H(20) 2.947 ? . 3_554 H(5) Pd(1) 3.327 ? . . H(5) O(2) 2.947 ? . 5_657 H(5) N(3) 2.011 ? . . H(5) N(3) 3.177 ? . 7_656 H(5) C(1) 2.790 ? . 5_657 H(5) C(2) 3.069 ? . 5_657 H(5) C(6) 3.303 ? . 5_657 H(5) C(7) 2.848 ? . . H(5) C(8) 2.613 ? . 7_656 H(5) C(9) 1.981 ? . . H(5) C(11) 3.018 ? . 5_657 H(5) H(3) 2.816 ? . . H(5) H(4) 1.551 ? . . H(5) H(4) 3.238 ? . 7_656 H(5) H(5) 3.007 ? . 7_656 H(5) H(6) 3.110 ? . 5_657 H(5) H(7) 3.325 ? . 1_545 H(5) H(8) 2.237 ? . 5_657 H(6) O(2) 2.656 ? . . H(6) O(2) 3.516 ? . 7_656 H(6) C(1) 3.168 ? . . H(6) C(2) 2.936 ? . . H(6) C(10) 2.065 ? . . H(6) C(11) 3.002 ? . 7_656 H(6) C(12) 2.515 ? . . H(6) C(12) 3.192 ? . 7_656 H(6) C(13) 3.242 ? . . H(6) H(4) 3.368 ? . 5_657 H(6) H(5) 3.110 ? . 5_657 H(6) H(6) 2.143 ? . 7_656 H(6) H(7) 1.551 ? . . H(6) H(7) 3.487 ? . 5_667 H(6) H(7) 3.199 ? . 7_656 H(6) H(8) 1.551 ? . . H(6) H(8) 3.416 ? . 5_667 H(6) H(9) 3.413 ? . . H(6) H(10) 2.315 ? . . H(6) H(10) 2.521 ? . 7_656 H(6) H(11) 2.718 ? . . H(6) H(11) 3.173 ? . 7_656 H(6) H(12) 3.344 ? . . H(6) H(13) 3.505 ? . . H(7) C(2) 3.296 ? . . H(7) C(8) 3.226 ? . 1_565 H(7) C(9) 3.283 ? . 1_565 H(7) C(9) 3.478 ? . 7_666 H(7) C(10) 2.073 ? . . H(7) C(11) 3.378 ? . 5_667 H(7) C(12) 2.912 ? . . H(7) C(13) 2.445 ? . . H(7) H(4) 2.667 ? . 1_565 H(7) H(5) 3.325 ? . 1_565 H(7) H(6) 1.551 ? . . H(7) H(6) 3.487 ? . 5_667 H(7) H(6) 3.199 ? . 7_656 H(7) H(7) 3.302 ? . 5_667 H(7) H(8) 1.551 ? . . H(7) H(8) 2.829 ? . 5_667 H(7) H(9) 3.550 ? . . H(7) H(10) 2.681 ? . . H(7) H(10) 3.186 ? . 3_565 H(7) H(10) 3.494 ? . 7_656 H(7) H(11) 3.524 ? . . H(7) H(12) 2.232 ? . . H(7) H(13) 2.627 ? . . H(7) H(14) 3.353 ? . . H(8) O(2) 3.134 ? . . H(8) C(1) 3.077 ? . . H(8) C(2) 2.512 ? . . H(8) C(3) 3.359 ? . . H(8) C(8) 2.946 ? . 5_657 H(8) C(9) 2.833 ? . 3_555 H(8) C(10) 2.059 ? . . H(8) C(11) 3.304 ? . 5_667 H(8) C(12) 3.276 ? . . H(8) C(13) 2.885 ? . . H(8) H(1) 3.554 ? . . H(8) H(4) 2.891 ? . 5_657 H(8) H(5) 2.237 ? . 5_657 H(8) H(6) 1.551 ? . . H(8) H(6) 3.416 ? . 5_667 H(8) H(7) 1.551 ? . . H(8) H(7) 2.829 ? . 5_667 H(8) H(8) 3.150 ? . 5_667 H(8) H(10) 3.391 ? . . H(8) H(10) 3.217 ? . 3_565 H(8) H(10) 3.394 ? . 7_656 H(8) H(11) 3.571 ? . . H(8) H(12) 2.644 ? . . H(8) H(13) 3.478 ? . . H(8) H(14) 3.542 ? . . H(9) C(2) 2.924 ? . . H(9) C(10) 2.048 ? . . H(9) C(11) 3.275 ? . . H(9) C(13) 2.467 ? . . H(9) C(17) 3.325 ? . 4_654 H(9) H(3) 3.312 ? . 3_554 H(9) H(6) 3.413 ? . . H(9) H(7) 3.550 ? . . H(9) H(10) 1.552 ? . . H(9) H(11) 1.551 ? . . H(9) H(12) 3.369 ? . . H(9) H(12) 2.803 ? . 3_564 H(9) H(13) 2.271 ? . . H(9) H(14) 2.665 ? . . H(9) H(21) 3.025 ? . 4_654 H(9) H(22) 2.786 ? . 4_654 H(10) O(2) 3.365 ? . . H(10) C(2) 3.283 ? . . H(10) C(10) 2.045 ? . . H(10) C(11) 2.490 ? . . H(10) C(11) 3.277 ? . 7_656 H(10) C(13) 2.859 ? . . H(10) H(3) 3.318 ? . 3_554 H(10) H(4) 3.072 ? . 3_554 H(10) H(6) 2.315 ? . . H(10) H(6) 2.521 ? . 7_656 H(10) H(7) 2.681 ? . . H(10) H(7) 3.186 ? . 3_564 H(10) H(7) 3.494 ? . 7_656 H(10) H(8) 3.391 ? . . H(10) H(8) 3.217 ? . 3_564 H(10) H(8) 3.394 ? . 7_656 H(10) H(9) 1.552 ? . . H(10) H(11) 1.551 ? . . H(10) H(12) 3.497 ? . . H(10) H(12) 2.765 ? . 3_564 H(10) H(13) 2.614 ? . . H(10) H(14) 3.475 ? . . H(11) Pd(1) 3.590 ? . . H(11) O(2) 2.300 ? . . H(11) O(2) 3.473 ? . 7_656 H(11) C(1) 2.584 ? . . H(11) C(2) 2.509 ? . . H(11) C(7) 3.281 ? . 3_554 H(11) C(10) 2.043 ? . . H(11) C(11) 2.926 ? . . H(11) C(13) 3.255 ? . . H(11) H(2) 2.978 ? . 3_554 H(11) H(3) 2.344 ? . 3_554 H(11) H(4) 3.114 ? . 3_554 H(11) H(6) 2.718 ? . . H(11) H(6) 3.173 ? . 7_656 H(11) H(7) 3.524 ? . . H(11) H(8) 3.571 ? . . H(11) H(9) 1.551 ? . . H(11) H(10) 1.551 ? . . H(11) H(13) 3.360 ? . . H(11) H(14) 3.559 ? . . H(12) C(2) 2.947 ? . . H(12) C(3) 3.107 ? . . H(12) C(10) 2.057 ? . . H(12) C(11) 2.442 ? . . H(12) C(12) 3.239 ? . . H(12) C(12) 3.218 ? . 3_565 H(12) H(1) 2.586 ? . . H(12) H(4) 3.372 ? . 1_565 H(12) H(6) 3.344 ? . . H(12) H(7) 2.232 ? . . H(12) H(8) 2.644 ? . . H(12) H(9) 3.369 ? . . H(12) H(9) 2.803 ? . 3_565 H(12) H(10) 3.497 ? . . H(12) H(10) 2.765 ? . 3_565 H(12) H(13) 1.551 ? . . H(12) H(13) 3.581 ? . 3_565 H(12) H(14) 1.551 ? . . H(12) H(18) 3.474 ? . 3_564 H(12) H(20) 3.422 ? . 3_564 H(12) H(21) 3.505 ? . 2_655 H(13) C(2) 3.307 ? . . H(13) C(10) 2.057 ? . . H(13) C(11) 2.865 ? . . H(13) C(12) 2.450 ? . . H(13) C(16) 3.330 ? . 3_564 H(13) H(1) 3.299 ? . . H(13) H(1) 3.520 ? . 3_564 H(13) H(6) 3.505 ? . . H(13) H(7) 2.627 ? . . H(13) H(8) 3.478 ? . . H(13) H(9) 2.271 ? . . H(13) H(10) 2.614 ? . . H(13) H(11) 3.360 ? . . H(13) H(12) 1.551 ? . . H(13) H(12) 3.581 ? . 3_564 H(13) H(14) 1.551 ? . . H(13) H(16) 3.196 ? . 4_654 H(13) H(18) 2.755 ? . 3_564 H(13) H(20) 3.043 ? . 3_564 H(14) C(2) 2.556 ? . . H(14) C(3) 2.456 ? . . H(14) C(10) 2.063 ? . . H(14) C(11) 3.255 ? . . H(14) C(12) 2.893 ? . . H(14) H(1) 1.863 ? . . H(14) H(7) 3.353 ? . . H(14) H(8) 3.542 ? . . H(14) H(9) 2.665 ? . . H(14) H(10) 3.475 ? . . H(14) H(11) 3.559 ? . . H(14) H(12) 1.551 ? . . H(14) H(13) 1.551 ? . . H(14) H(16) 2.876 ? . 4_654 H(14) H(18) 3.521 ? . 3_564 H(14) H(21) 3.416 ? . 2_655 H(14) H(22) 3.154 ? . 4_654 H(14) H(23) 3.320 ? . . H(15) C(1) 3.582 ? . 3_555 H(15) C(4) 2.940 ? . . H(15) C(4) 3.257 ? . 3_555 H(15) C(5) 3.135 ? . . H(15) C(5) 2.945 ? . 3_555 H(15) C(6) 3.076 ? . 3_555 H(15) C(7) 3.517 ? . 3_555 H(15) C(14) 2.039 ? . . H(15) C(16) 2.429 ? . . H(15) C(17) 3.223 ? . . H(15) H(2) 2.660 ? . . H(15) H(2) 3.220 ? . 3_555 H(15) H(16) 1.551 ? . . H(15) H(17) 1.551 ? . . H(15) H(18) 3.328 ? . . H(15) H(19) 2.214 ? . . H(15) H(20) 2.640 ? . . H(15) H(21) 3.362 ? . . H(15) H(21) 3.543 ? . 3_555 H(15) H(22) 3.476 ? . . H(16) C(4) 3.292 ? . . H(16) C(13) 3.471 ? . 4_655 H(16) C(14) 2.044 ? . . H(16) C(16) 2.870 ? . . H(16) C(17) 2.447 ? . . H(16) H(2) 3.321 ? . . H(16) H(13) 3.196 ? . 4_655 H(16) H(14) 2.876 ? . 4_655 H(16) H(15) 1.551 ? . . H(16) H(17) 1.552 ? . . H(16) H(18) 3.505 ? . . H(16) H(18) 2.833 ? . 2_645 H(16) H(19) 2.642 ? . . H(16) H(20) 3.487 ? . . H(16) H(21) 2.275 ? . . H(16) H(21) 3.459 ? . 3_555 H(16) H(22) 2.604 ? . . H(16) H(22) 3.516 ? . 2_645 H(16) H(23) 3.358 ? . . H(17) C(4) 2.537 ? . . H(17) C(5) 2.437 ? . . H(17) C(14) 2.039 ? . . H(17) C(16) 3.231 ? . . H(17) C(17) 2.884 ? . . H(17) H(2) 1.863 ? . . H(17) H(15) 1.551 ? . . H(17) H(16) 1.552 ? . . H(17) H(18) 3.404 ? . 2_645 H(17) H(19) 3.339 ? . . H(17) H(20) 3.516 ? . . H(17) H(21) 2.662 ? . . H(17) H(22) 3.463 ? . . H(17) H(22) 2.973 ? . 2_645 H(17) H(23) 3.552 ? . . H(17) H(23) 3.483 ? . 2_645 H(18) C(3) 3.103 ? . . H(18) C(4) 2.894 ? . . H(18) C(13) 3.413 ? . 3_565 H(18) C(14) 2.057 ? . . H(18) C(15) 3.226 ? . . H(18) C(15) 3.520 ? . 2_655 H(18) C(17) 2.484 ? . . H(18) H(1) 2.670 ? . . H(18) H(12) 3.474 ? . 3_565 H(18) H(13) 2.755 ? . 3_565 H(18) H(14) 3.521 ? . 3_565 H(18) H(15) 3.328 ? . . H(18) H(16) 3.505 ? . . H(18) H(16) 2.833 ? . 2_655 H(18) H(17) 3.404 ? . 2_655 H(18) H(19) 1.551 ? . . H(18) H(20) 1.551 ? . . H(18) H(21) 3.388 ? . . H(18) H(21) 3.449 ? . 4_655 H(18) H(22) 2.304 ? . . H(18) H(23) 2.666 ? . . H(18) H(23) 3.211 ? . 4_655 H(19) C(4) 3.262 ? . . H(19) C(14) 2.061 ? . . H(19) C(15) 2.437 ? . . H(19) C(17) 2.899 ? . . H(19) C(17) 3.130 ? . 4_655 H(19) H(2) 3.589 ? . 3_555 H(19) H(15) 2.214 ? . . H(19) H(16) 2.642 ? . . H(19) H(17) 3.339 ? . . H(19) H(18) 1.551 ? . . H(19) H(20) 1.551 ? . . H(19) H(21) 3.549 ? . . H(19) H(21) 3.180 ? . 4_655 H(19) H(22) 2.679 ? . . H(19) H(22) 3.297 ? . 4_655 H(19) H(23) 3.495 ? . . H(19) H(23) 2.465 ? . 4_655 H(20) N(3) 3.524 ? . 3_555 H(20) C(3) 2.988 ? . . H(20) C(4) 2.469 ? . . H(20) C(5) 3.351 ? . . H(20) C(7) 3.260 ? . 3_555 H(20) C(8) 3.474 ? . 3_555 H(20) C(14) 2.050 ? . . H(20) C(15) 2.875 ? . . H(20) C(17) 3.247 ? . . H(20) H(1) 2.991 ? . . H(20) H(2) 3.592 ? . . H(20) H(3) 3.093 ? . 3_555 H(20) H(4) 2.947 ? . 3_555 H(20) H(12) 3.422 ? . 3_565 H(20) H(13) 3.043 ? . 3_565 H(20) H(15) 2.640 ? . . H(20) H(16) 3.487 ? . . H(20) H(17) 3.516 ? . . H(20) H(18) 1.551 ? . . H(20) H(19) 1.551 ? . . H(20) H(22) 3.382 ? . . H(20) H(23) 3.523 ? . . H(21) C(3) 3.590 ? . . H(21) C(4) 2.883 ? . . H(21) C(14) 2.029 ? . . H(21) C(15) 2.462 ? . . H(21) C(16) 3.256 ? . . H(21) H(1) 3.546 ? . . H(21) H(9) 3.025 ? . 4_655 H(21) H(12) 3.505 ? . 2_645 H(21) H(14) 3.416 ? . 2_645 H(21) H(15) 3.362 ? . . H(21) H(15) 3.543 ? . 3_554 H(21) H(16) 2.275 ? . . H(21) H(16) 3.459 ? . 3_554 H(21) H(17) 2.662 ? . . H(21) H(18) 3.388 ? . . H(21) H(18) 3.449 ? . 4_654 H(21) H(19) 3.549 ? . . H(21) H(19) 3.180 ? . 4_654 H(21) H(22) 1.551 ? . . H(21) H(23) 1.551 ? . . H(22) C(4) 3.255 ? . . H(22) C(14) 2.037 ? . . H(22) C(15) 2.842 ? . . H(22) C(16) 2.482 ? . . H(22) H(1) 3.359 ? . . H(22) H(9) 2.786 ? . 4_655 H(22) H(14) 3.154 ? . 4_655 H(22) H(15) 3.476 ? . . H(22) H(16) 2.604 ? . . H(22) H(16) 3.516 ? . 2_655 H(22) H(17) 3.463 ? . . H(22) H(17) 2.973 ? . 2_655 H(22) H(18) 2.304 ? . . H(22) H(19) 2.679 ? . . H(22) H(19) 3.297 ? . 4_654 H(22) H(20) 3.382 ? . . H(22) H(21) 1.551 ? . . H(22) H(23) 1.551 ? . . H(23) C(3) 2.565 ? . . H(23) C(4) 2.471 ? . . H(23) C(14) 2.032 ? . . H(23) C(15) 3.244 ? . . H(23) C(16) 2.885 ? . . H(23) C(16) 3.242 ? . 4_654 H(23) H(1) 2.220 ? . . H(23) H(14) 3.320 ? . . H(23) H(16) 3.358 ? . . H(23) H(17) 3.552 ? . . H(23) H(17) 3.483 ? . 2_655 H(23) H(18) 2.666 ? . . H(23) H(18) 3.211 ? . 4_654 H(23) H(19) 3.495 ? . . H(23) H(19) 2.465 ? . 4_654 H(23) H(20) 3.523 ? . . H(23) H(21) 1.551 ? . . H(23) H(22) 1.551 ? . . #============================================================================== # 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 #============================================================================== # Attachment '- PdsalpnOXfincif.cif' #------------------------------------------------------------------------------ data_4 _database_code_depnum_ccdc_archive 'CCDC 801078' #TrackingRef '- PdsalpnOXfincif.cif' _audit_creation_date 'Mon Feb 16 09:51:56 2009' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C33 H48 F6 N2 O2 Pd Sb ' _chemical_formula_moiety ? _chemical_formula_weight 846.89 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 11.6784(5) _cell_length_b 17.5605(6) _cell_length_c 18.3113(9) _cell_angle_alpha 90 _cell_angle_beta 109.816(2) _cell_angle_gamma 90 _cell_volume 3532.9(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20484 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 133.2 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.983 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_ambient_temperature 133(2) _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 31598 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9933 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9933 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # 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 8048 _reflns_number_gt 6373 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1586 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8048 _refine_ls_number_parameters 406 _refine_ls_goodness_of_fit_ref 1.882 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.89 _refine_diff_density_min -0.91 _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) ; 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) ; Pd Pd -0.999 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb Sb -0.587 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;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 Sb(1) Sb 0.73993(3) 0.04916(2) 1.01839(2) 0.0315(1) Uani 1.00 d . . . Pd(1) Pd 0.73435(3) 0.20260(2) 0.77766(2) 0.0211(1) Uani 1.00 d . . . F(1) F 0.8414(4) 0.0627(3) 1.1215(2) 0.055(1) Uani 1.00 d . . . F(2) F 0.8588(4) -0.0162(3) 1.0045(3) 0.085(2) Uani 1.00 d . . . F(3) F 0.6637(5) -0.0315(3) 1.0491(3) 0.088(2) Uani 1.00 d . . . F(4) F 0.6273(3) 0.1164(2) 1.0342(2) 0.051(1) Uani 1.00 d . . . F(5) F 0.8148(4) 0.1317(3) 0.9878(3) 0.067(1) Uani 1.00 d . . . F(6) F 0.6422(3) 0.0362(2) 0.9149(2) 0.049(1) Uani 1.00 d . . . O(1) O 0.6549(3) 0.1018(2) 0.7366(2) 0.0274(10) Uani 1.00 d . . . O(2) O 0.5805(3) 0.2426(2) 0.7028(2) 0.0258(10) Uani 1.00 d . . . N(1) N 0.8872(4) 0.1489(3) 0.8409(3) 0.023(1) Uani 1.00 d . . . N(2) N 0.7857(4) 0.3054(3) 0.8210(3) 0.027(1) Uani 1.00 d . . . C(1) C 0.6866(5) 0.0348(3) 0.7614(3) 0.024(1) Uani 1.00 d . . . C(2) C 0.5994(5) -0.0275(3) 0.7379(4) 0.030(1) Uani 1.00 d . . . C(3) C 0.6383(5) -0.0991(3) 0.7658(4) 0.032(2) Uani 1.00 d . . . C(4) C 0.7578(5) -0.1168(3) 0.8154(3) 0.030(1) Uani 1.00 d . . . C(5) C 0.8414(5) -0.0566(3) 0.8375(3) 0.028(1) Uani 1.00 d . . . C(6) C 0.8069(5) 0.0178(3) 0.8133(3) 0.027(1) Uani 1.00 d . . . C(7) C 0.8983(4) 0.0760(3) 0.8452(3) 0.025(1) Uani 1.00 d . . . C(8) C 1.0012(5) 0.1887(3) 0.8889(4) 0.031(1) Uani 1.00 d . . . C(9) C 1.0020(5) 0.2726(3) 0.8728(4) 0.033(2) Uani 1.00 d . . . C(10) C 0.9010(5) 0.3148(4) 0.8871(4) 0.037(2) Uani 1.00 d . . . C(11) C 0.7216(5) 0.3659(3) 0.7957(3) 0.028(1) Uani 1.00 d . . . C(12) C 0.6126(5) 0.3758(3) 0.7316(3) 0.026(1) Uani 1.00 d . . . C(13) C 0.5491(5) 0.3143(3) 0.6850(3) 0.024(1) Uani 1.00 d . . . C(14) C 0.4452(5) 0.3309(3) 0.6176(3) 0.025(1) Uani 1.00 d . . . C(15) C 0.4124(4) 0.4065(3) 0.6032(3) 0.025(1) Uani 1.00 d . . . C(16) C 0.4727(5) 0.4688(3) 0.6491(3) 0.026(1) Uani 1.00 d . . . C(17) C 0.5714(5) 0.4516(3) 0.7129(3) 0.025(1) Uani 1.00 d . . . C(18) C 0.4679(5) -0.0126(4) 0.6860(4) 0.037(2) Uani 1.00 d . . . C(19) C 0.4107(5) 0.0420(4) 0.7304(5) 0.044(2) Uani 1.00 d . . . C(20) C 0.4647(6) 0.0198(4) 0.6090(4) 0.048(2) Uani 1.00 d . . . C(21) C 0.3910(6) -0.0854(4) 0.6704(5) 0.055(2) Uani 1.00 d . . . C(22) C 0.7891(5) -0.1967(3) 0.8482(4) 0.036(2) Uani 1.00 d . . . C(23) C 0.9247(6) -0.2109(4) 0.8783(5) 0.047(2) Uani 1.00 d . . . C(24) C 0.7394(6) -0.2015(4) 0.9167(5) 0.050(2) Uani 1.00 d . . . C(25) C 0.7286(9) -0.2564(4) 0.7872(5) 0.079(3) Uani 1.00 d . . . C(26) C 0.3746(4) 0.2666(3) 0.5637(3) 0.026(1) Uani 1.00 d . . . C(27) C 0.3168(5) 0.2142(3) 0.6086(3) 0.032(2) Uani 1.00 d . . . C(28) C 0.4621(5) 0.2211(4) 0.5323(3) 0.033(2) Uani 1.00 d . . . C(29) C 0.2729(5) 0.2969(4) 0.4930(4) 0.037(2) Uani 1.00 d . . . C(30) C 0.4273(5) 0.5503(3) 0.6262(3) 0.027(1) Uani 1.00 d . . . C(31) C 0.4398(6) 0.5707(4) 0.5473(4) 0.042(2) Uani 1.00 d . . . C(32) C 0.2909(5) 0.5562(4) 0.6168(4) 0.037(2) Uani 1.00 d . . . C(33) C 0.4975(6) 0.6079(4) 0.6851(4) 0.042(2) Uani 1.00 d . . . H(1) H 0.5808 -0.1404 0.7507 0.0383 Uiso 1.00 calc . . . H(2) H 0.9226 -0.0663 0.8704 0.0339 Uiso 1.00 calc . . . H(3) H 0.9781 0.0575 0.8719 0.0303 Uiso 1.00 calc . . . H(4) H 1.0112 0.1830 0.9429 0.0382 Uiso 1.00 calc . . . H(5) H 1.0699 0.1654 0.8805 0.0382 Uiso 1.00 calc . . . H(6) H 1.0787 0.2937 0.9029 0.0410 Uiso 1.00 calc . . . H(7) H 0.9936 0.2784 0.8185 0.0410 Uiso 1.00 calc . . . H(8) H 0.9208 0.3675 0.8952 0.0446 Uiso 1.00 calc . . . H(9) H 0.8905 0.2950 0.9335 0.0446 Uiso 1.00 calc . . . H(10) H 0.7533 0.4120 0.8242 0.0334 Uiso 1.00 calc . . . H(11) H 0.3428 0.4174 0.5585 0.0290 Uiso 1.00 calc . . . H(12) H 0.6146 0.4920 0.7460 0.0287 Uiso 1.00 calc . . . H(13) H 0.4563 0.0882 0.7441 0.0533 Uiso 1.00 calc . . . H(14) H 0.3288 0.0536 0.7016 0.0533 Uiso 1.00 calc . . . H(15) H 0.4122 0.0182 0.7790 0.0533 Uiso 1.00 calc . . . H(16) H 0.5109 0.0662 0.6165 0.0575 Uiso 1.00 calc . . . H(17) H 0.5025 -0.0156 0.5831 0.0575 Uiso 1.00 calc . . . H(18) H 0.3847 0.0292 0.5758 0.0575 Uiso 1.00 calc . . . H(19) H 0.3088 -0.0750 0.6420 0.0692 Uiso 1.00 calc . . . H(20) H 0.4221 -0.1218 0.6431 0.0692 Uiso 1.00 calc . . . H(21) H 0.3954 -0.1082 0.7195 0.0692 Uiso 1.00 calc . . . H(22) H 0.9422 -0.2603 0.8998 0.0564 Uiso 1.00 calc . . . H(23) H 0.9576 -0.2055 0.8373 0.0564 Uiso 1.00 calc . . . H(24) H 0.9644 -0.1741 0.9179 0.0564 Uiso 1.00 calc . . . H(25) H 0.7768 -0.1638 0.9549 0.0589 Uiso 1.00 calc . . . H(26) H 0.6533 -0.1933 0.8985 0.0589 Uiso 1.00 calc . . . H(27) H 0.7557 -0.2505 0.9405 0.0589 Uiso 1.00 calc . . . H(28) H 0.6449 -0.2490 0.7646 0.0973 Uiso 1.00 calc . . . H(29) H 0.7632 -0.2518 0.7440 0.0973 Uiso 1.00 calc . . . H(30) H 0.7473 -0.3062 0.8066 0.0973 Uiso 1.00 calc . . . H(31) H 0.2606 0.2415 0.6252 0.0382 Uiso 1.00 calc . . . H(32) H 0.2770 0.1729 0.5763 0.0382 Uiso 1.00 calc . . . H(33) H 0.3795 0.1939 0.6531 0.0382 Uiso 1.00 calc . . . H(34) H 0.4197 0.1811 0.4996 0.0404 Uiso 1.00 calc . . . H(35) H 0.4951 0.2545 0.5030 0.0404 Uiso 1.00 calc . . . H(36) H 0.5277 0.2006 0.5742 0.0404 Uiso 1.00 calc . . . H(37) H 0.2167 0.3259 0.5089 0.0455 Uiso 1.00 calc . . . H(38) H 0.3078 0.3300 0.4640 0.0455 Uiso 1.00 calc . . . H(39) H 0.2325 0.2565 0.4608 0.0455 Uiso 1.00 calc . . . H(40) H 0.5221 0.5694 0.5503 0.0534 Uiso 1.00 calc . . . H(41) H 0.3951 0.5338 0.5085 0.0534 Uiso 1.00 calc . . . H(42) H 0.4061 0.6195 0.5305 0.0534 Uiso 1.00 calc . . . H(43) H 0.2611 0.6066 0.6018 0.0442 Uiso 1.00 calc . . . H(44) H 0.2435 0.5215 0.5781 0.0442 Uiso 1.00 calc . . . H(45) H 0.2791 0.5443 0.6648 0.0442 Uiso 1.00 calc . . . H(46) H 0.4914 0.5975 0.7348 0.0509 Uiso 1.00 calc . . . H(47) H 0.5817 0.6078 0.6900 0.0509 Uiso 1.00 calc . . . H(48) H 0.4663 0.6585 0.6700 0.0509 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 Sb(1) 0.0301(2) 0.0306(2) 0.0258(2) 0.0005(2) -0.0010(2) 0.0024(2) Pd(1) 0.0161(2) 0.0246(2) 0.0180(2) 0.0015(1) -0.0002(2) -0.0015(2) F(1) 0.046(2) 0.078(3) 0.028(2) 0.000(2) -0.005(2) -0.002(2) F(2) 0.070(3) 0.103(4) 0.062(3) 0.051(3) -0.005(3) -0.016(3) F(3) 0.112(4) 0.056(3) 0.068(3) -0.035(3) -0.004(3) 0.029(3) F(4) 0.052(2) 0.054(2) 0.048(2) 0.012(2) 0.017(2) -0.004(2) F(5) 0.068(3) 0.085(3) 0.052(3) -0.035(3) 0.025(2) 0.003(2) F(6) 0.042(2) 0.066(3) 0.029(2) 0.009(2) -0.001(2) -0.004(2) O(1) 0.020(2) 0.024(2) 0.030(2) 0.000(2) -0.002(2) -0.002(2) O(2) 0.020(2) 0.026(2) 0.024(2) 0.004(1) -0.002(2) 0.003(2) N(1) 0.016(2) 0.031(2) 0.019(2) 0.004(2) 0.002(2) -0.002(2) N(2) 0.024(2) 0.027(2) 0.020(2) -0.001(2) -0.004(2) -0.006(2) C(1) 0.022(2) 0.025(3) 0.022(3) 0.004(2) 0.004(2) 0.001(2) C(2) 0.023(3) 0.028(3) 0.034(3) -0.002(2) 0.003(2) -0.004(2) C(3) 0.023(3) 0.035(3) 0.035(3) -0.003(2) 0.005(2) 0.000(3) C(4) 0.031(3) 0.027(3) 0.030(3) -0.001(2) 0.009(2) -0.003(2) C(5) 0.024(3) 0.029(3) 0.029(3) 0.001(2) 0.004(2) -0.001(2) C(6) 0.021(2) 0.028(3) 0.028(3) -0.003(2) 0.005(2) 0.002(2) C(7) 0.015(2) 0.033(3) 0.024(3) 0.005(2) 0.000(2) 0.002(2) C(8) 0.018(2) 0.035(3) 0.031(3) 0.007(2) -0.004(2) 0.001(2) C(9) 0.023(3) 0.028(3) 0.040(4) -0.004(2) -0.001(2) -0.008(3) C(10) 0.025(3) 0.042(4) 0.031(3) 0.005(3) -0.007(2) -0.013(3) C(11) 0.025(3) 0.025(3) 0.028(3) 0.001(2) 0.002(2) -0.006(2) C(12) 0.024(3) 0.029(3) 0.021(3) 0.000(2) 0.005(2) -0.002(2) C(13) 0.019(2) 0.027(3) 0.026(3) 0.002(2) 0.006(2) -0.005(2) C(14) 0.022(2) 0.030(3) 0.022(3) -0.002(2) 0.003(2) 0.003(2) C(15) 0.019(2) 0.029(3) 0.021(3) 0.005(2) 0.000(2) 0.003(2) C(16) 0.023(3) 0.034(3) 0.020(3) -0.000(2) 0.007(2) 0.001(2) C(17) 0.025(3) 0.025(3) 0.023(3) -0.002(2) 0.007(2) -0.005(2) C(18) 0.022(3) 0.035(3) 0.041(4) -0.000(2) -0.005(3) -0.001(3) C(19) 0.020(3) 0.043(4) 0.061(5) -0.000(3) 0.005(3) -0.000(3) C(20) 0.039(4) 0.047(4) 0.040(4) 0.008(3) -0.010(3) -0.003(3) C(21) 0.029(3) 0.036(4) 0.077(6) -0.009(3) -0.013(3) -0.005(4) C(22) 0.029(3) 0.024(3) 0.047(4) 0.000(2) 0.001(3) 0.003(3) C(23) 0.032(3) 0.031(3) 0.073(5) 0.008(3) 0.013(3) 0.018(3) C(24) 0.043(4) 0.043(4) 0.062(5) -0.005(3) 0.015(3) 0.021(4) C(25) 0.109(7) 0.020(4) 0.067(6) 0.003(4) -0.021(5) -0.013(3) C(26) 0.019(2) 0.031(3) 0.022(3) 0.001(2) -0.001(2) -0.002(2) C(27) 0.024(3) 0.038(3) 0.026(3) -0.004(2) -0.001(2) 0.001(2) C(28) 0.032(3) 0.037(3) 0.026(3) -0.005(2) 0.005(2) -0.006(3) C(29) 0.028(3) 0.043(4) 0.028(3) -0.000(3) -0.006(3) -0.001(3) C(30) 0.030(3) 0.024(3) 0.029(3) 0.006(2) 0.011(2) 0.004(2) C(31) 0.051(4) 0.041(4) 0.043(4) 0.010(3) 0.025(3) 0.008(3) C(32) 0.030(3) 0.046(4) 0.033(3) 0.011(3) 0.008(3) 0.005(3) C(33) 0.037(3) 0.033(3) 0.045(4) 0.001(3) -0.003(3) 0.009(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR97 _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 Sb(1) F(1) 1.874(4) . . yes Sb(1) F(2) 1.884(4) . . yes Sb(1) F(3) 1.859(5) . . yes Sb(1) F(4) 1.862(4) . . yes Sb(1) F(5) 1.873(4) . . yes Sb(1) F(6) 1.865(4) . . yes Pd(1) O(1) 2.022(4) . . yes Pd(1) O(2) 1.982(3) . . yes Pd(1) N(1) 2.004(4) . . yes Pd(1) N(2) 1.981(4) . . yes O(1) C(1) 1.269(6) . . yes O(2) C(13) 1.322(6) . . yes N(1) C(7) 1.286(7) . . yes N(1) C(8) 1.497(7) . . yes N(2) C(10) 1.483(7) . . yes N(2) C(11) 1.291(7) . . yes C(1) C(2) 1.457(7) . . yes C(1) C(6) 1.436(7) . . yes C(2) C(3) 1.375(8) . . yes C(2) C(18) 1.530(7) . . yes C(3) C(4) 1.417(8) . . yes C(4) C(5) 1.403(8) . . yes C(4) C(22) 1.521(8) . . yes C(5) C(6) 1.395(8) . . yes C(6) C(7) 1.450(7) . . yes C(8) C(9) 1.504(8) . . yes C(9) C(10) 1.490(9) . . yes C(11) C(12) 1.419(7) . . yes C(12) C(13) 1.420(7) . . yes C(12) C(17) 1.419(8) . . yes C(13) C(14) 1.436(7) . . yes C(14) C(15) 1.382(8) . . yes C(14) C(26) 1.541(7) . . yes C(15) C(16) 1.414(8) . . yes C(16) C(17) 1.368(8) . . yes C(16) C(30) 1.533(8) . . yes C(18) C(19) 1.547(10) . . yes C(18) C(20) 1.51(1) . . yes C(18) C(21) 1.533(9) . . yes C(22) C(23) 1.511(8) . . yes C(22) C(24) 1.55(1) . . yes C(22) C(25) 1.520(9) . . yes C(26) C(27) 1.535(8) . . yes C(26) C(28) 1.554(8) . . yes C(26) C(29) 1.526(7) . . yes C(30) C(31) 1.541(9) . . yes C(30) C(32) 1.547(8) . . yes C(30) C(33) 1.503(8) . . 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 F(1) Sb(1) F(2) 88.3(2) . . . yes F(1) Sb(1) F(3) 89.8(2) . . . yes F(1) Sb(1) F(4) 90.1(2) . . . yes F(1) Sb(1) F(5) 90.2(2) . . . yes F(1) Sb(1) F(6) 178.6(2) . . . yes F(2) Sb(1) F(3) 91.5(3) . . . yes F(2) Sb(1) F(4) 177.8(2) . . . yes F(2) Sb(1) F(5) 89.5(3) . . . yes F(2) Sb(1) F(6) 90.8(2) . . . yes F(3) Sb(1) F(4) 90.0(3) . . . yes F(3) Sb(1) F(5) 179.0(3) . . . yes F(3) Sb(1) F(6) 91.3(2) . . . yes F(4) Sb(1) F(5) 88.9(2) . . . yes F(4) Sb(1) F(6) 90.8(2) . . . yes F(5) Sb(1) F(6) 88.7(2) . . . yes O(1) Pd(1) O(2) 81.9(1) . . . yes O(1) Pd(1) N(1) 90.5(2) . . . yes O(1) Pd(1) N(2) 170.1(2) . . . yes O(2) Pd(1) N(1) 170.8(2) . . . yes O(2) Pd(1) N(2) 92.0(2) . . . yes N(1) Pd(1) N(2) 96.2(2) . . . yes Pd(1) O(1) C(1) 129.6(3) . . . yes Pd(1) O(2) C(13) 128.3(3) . . . yes Pd(1) N(1) C(7) 123.7(3) . . . yes Pd(1) N(1) C(8) 124.1(3) . . . yes C(7) N(1) C(8) 112.2(4) . . . yes Pd(1) N(2) C(10) 119.7(4) . . . yes Pd(1) N(2) C(11) 123.1(3) . . . yes C(10) N(2) C(11) 117.1(5) . . . yes O(1) C(1) C(2) 120.1(4) . . . yes O(1) C(1) C(6) 122.0(5) . . . yes C(2) C(1) C(6) 117.9(5) . . . yes C(1) C(2) C(3) 117.8(5) . . . yes C(1) C(2) C(18) 120.6(5) . . . yes C(3) C(2) C(18) 121.6(5) . . . yes C(2) C(3) C(4) 124.7(5) . . . yes C(3) C(4) C(5) 117.2(5) . . . yes C(3) C(4) C(22) 120.5(5) . . . yes C(5) C(4) C(22) 122.0(5) . . . yes C(4) C(5) C(6) 121.1(5) . . . yes C(1) C(6) C(5) 121.2(5) . . . yes C(1) C(6) C(7) 122.8(5) . . . yes C(5) C(6) C(7) 116.0(5) . . . yes N(1) C(7) C(6) 129.2(5) . . . yes N(1) C(8) C(9) 113.9(4) . . . yes C(8) C(9) C(10) 113.3(5) . . . yes N(2) C(10) C(9) 110.8(5) . . . yes N(2) C(11) C(12) 130.2(5) . . . yes C(11) C(12) C(13) 122.9(5) . . . yes C(11) C(12) C(17) 116.8(5) . . . yes C(13) C(12) C(17) 120.2(5) . . . yes O(2) C(13) C(12) 122.1(5) . . . yes O(2) C(13) C(14) 119.2(5) . . . yes C(12) C(13) C(14) 118.7(5) . . . yes C(13) C(14) C(15) 117.2(5) . . . yes C(13) C(14) C(26) 120.9(5) . . . yes C(15) C(14) C(26) 121.9(5) . . . yes C(14) C(15) C(16) 125.5(5) . . . yes C(15) C(16) C(17) 116.2(5) . . . yes C(15) C(16) C(30) 120.2(5) . . . yes C(17) C(16) C(30) 123.5(5) . . . yes C(12) C(17) C(16) 122.2(5) . . . yes C(2) C(18) C(19) 107.6(5) . . . yes C(2) C(18) C(20) 110.3(5) . . . yes C(2) C(18) C(21) 112.0(5) . . . yes C(19) C(18) C(20) 112.3(6) . . . yes C(19) C(18) C(21) 106.5(6) . . . yes C(20) C(18) C(21) 108.2(6) . . . yes C(4) C(22) C(23) 112.3(5) . . . yes C(4) C(22) C(24) 105.3(5) . . . yes C(4) C(22) C(25) 110.9(5) . . . yes C(23) C(22) C(24) 109.2(6) . . . yes C(23) C(22) C(25) 108.7(6) . . . yes C(24) C(22) C(25) 110.3(6) . . . yes C(14) C(26) C(27) 109.5(5) . . . yes C(14) C(26) C(28) 109.7(4) . . . yes C(14) C(26) C(29) 112.4(5) . . . yes C(27) C(26) C(28) 110.8(5) . . . yes C(27) C(26) C(29) 107.8(4) . . . yes C(28) C(26) C(29) 106.6(5) . . . yes C(16) C(30) C(31) 109.8(5) . . . yes C(16) C(30) C(32) 109.9(5) . . . yes C(16) C(30) C(33) 112.2(5) . . . yes C(31) C(30) C(32) 107.5(5) . . . yes C(31) C(30) C(33) 108.3(5) . . . yes C(32) C(30) C(33) 108.9(5) . . . yes #--------------------------------------------------------------------------END # Attachment '- PtsalcnOXfin.cif' #============================================================================== data__5 _database_code_depnum_ccdc_archive 'CCDC 801079' #TrackingRef '- PtsalcnOXfin.cif' _audit_creation_date 2009-11-11 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C40 H52 F6 N2 O2 Pt Sb ' _chemical_formula_moiety 'C40 H52 F6 N2 O2 Pt Sb ' _chemical_formula_weight 1023.68 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.7129(5) _cell_length_b 16.7862(5) _cell_length_c 29.5078(8) _cell_angle_alpha 90.0000 _cell_angle_beta 98.5939(9) _cell_angle_gamma 90.0000 _cell_volume 8185.3(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 97919 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 128.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4008.00 _exptl_absorpt_coefficient_mu 4.122 _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 0.476 _exptl_absorpt_correction_T_max 0.884 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_ambient_temperature 133(2) _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 118773 _diffrn_reflns_av_R_equivalents 0.100 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. 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 18708 _reflns_number_gt 16162 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1315 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 18708 _refine_ls_number_parameters 965 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0556P)^2^+43.8339P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0020 _refine_diff_density_max 4.91 _refine_diff_density_min -4.97 _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 0.003 0.002 ; 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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pt Pt -1.703 8.390 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sb Sb -0.587 1.546 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; 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 Pt(1) Pt 0.174086(12) 0.178854(11) 0.106534(7) 0.01987(6) Uani 1.00 1 d . . . Pt(2) Pt 0.247516(12) 0.072787(12) 0.318766(7) 0.02143(6) Uani 1.00 1 d . . . Sb(1) Sb -0.02820(3) -0.13580(3) 0.149177(17) 0.04019(12) Uani 1.00 1 d . . . Sb(2) Sb 0.23081(4) -0.12045(3) 0.00636(2) 0.05456(14) Uani 1.00 1 d . . . F(1) F -0.0092(5) -0.1406(3) 0.09007(19) 0.107(2) Uani 1.00 1 d . . . F(2) F 0.0800(3) -0.1617(3) 0.1701(2) 0.108(2) Uani 1.00 1 d . . . F(3) F -0.0403(6) -0.1340(4) 0.2111(2) 0.150(4) Uani 1.00 1 d . . . F(4) F -0.1348(3) -0.1110(4) 0.1353(3) 0.131(3) Uani 1.00 1 d . . . F(5) F 0.0022(2) -0.0282(2) 0.15282(18) 0.0592(12) Uani 1.00 1 d . . . F(6) F -0.0573(3) -0.2434(2) 0.14609(17) 0.0640(13) Uani 1.00 1 d . . . F(7) F 0.2591(3) -0.0222(3) 0.0343(2) 0.0799(17) Uani 1.00 1 d . . . F(8) F 0.1537(4) -0.1364(5) 0.0435(2) 0.128(3) Uani 1.00 1 d . . . F(9) F 0.2030(5) -0.2173(3) -0.0217(2) 0.102(2) Uani 1.00 1 d . . . F(10) F 0.3015(10) -0.1060(5) -0.0322(5) 0.307(11) Uani 1.00 1 d . . . F(11) F 0.3006(6) -0.1698(4) 0.0509(4) 0.199(6) Uani 1.00 1 d . . . F(12) F 0.1475(9) -0.0712(6) -0.0330(3) 0.216(6) Uani 1.00 1 d . . . O(1) O 0.2661(2) 0.1380(2) 0.15082(13) 0.0222(7) Uani 1.00 1 d . . . O(3) O 0.2196(2) 0.2830(2) 0.12997(13) 0.0237(8) Uani 1.00 1 d . . . O(4) O 0.3392(2) 0.1156(2) 0.36251(13) 0.0262(8) Uani 1.00 1 d . . . O(5) O 0.2915(2) -0.0304(2) 0.34392(13) 0.0248(8) Uani 1.00 1 d . . . N(1) N 0.1329(3) 0.0698(2) 0.09392(18) 0.0291(11) Uani 1.00 1 d . . . N(2) N 0.1679(3) 0.0184(3) 0.27229(17) 0.0291(10) Uani 1.00 1 d . . . N(3) N 0.0960(3) 0.2321(2) 0.05917(19) 0.0346(12) Uani 1.00 1 d . . . N(4) N 0.2067(3) 0.1816(2) 0.30390(18) 0.0295(10) Uani 1.00 1 d . . . C(1) C 0.2880(3) 0.0645(3) 0.16106(18) 0.0203(10) Uani 1.00 1 d . . . C(2) C 0.3639(3) 0.0500(3) 0.19001(18) 0.0209(10) Uani 1.00 1 d . . . C(3) C 0.3823(3) -0.0275(3) 0.20199(18) 0.0215(10) Uani 1.00 1 d . . . C(4) C 0.3327(3) -0.0943(3) 0.18748(18) 0.0211(10) Uani 1.00 1 d . . . C(5) C 0.2616(3) -0.0794(3) 0.15915(19) 0.0239(11) Uani 1.00 1 d . . . C(6) C 0.2385(3) -0.0013(3) 0.14538(18) 0.0222(10) Uani 1.00 1 d . . . C(7) C 0.1652(3) 0.0063(3) 0.1137(2) 0.0284(12) Uani 1.00 1 d . . . C(8) C 0.0559(5) 0.0572(4) 0.0616(3) 0.057(2) Uani 1.00 1 d . . . C(9) C 0.0569(6) 0.1016(4) 0.0193(2) 0.062(2) Uani 1.00 1 d . . . C(10) C 0.0379(5) 0.1887(3) 0.0237(2) 0.055(2) Uani 1.00 1 d . . . C(11) C 0.0919(4) 0.3095(3) 0.0539(2) 0.0336(14) Uani 1.00 1 d . . . C(12) C 0.1350(3) 0.3708(3) 0.08029(19) 0.0243(11) Uani 1.00 1 d . . . C(13) C 0.1966(3) 0.3552(3) 0.11821(18) 0.0206(10) Uani 1.00 1 d . . . C(14) C 0.2334(3) 0.4217(3) 0.14378(18) 0.0200(10) Uani 1.00 1 d . . . C(15) C 0.2095(3) 0.4964(3) 0.12924(19) 0.0245(11) Uani 1.00 1 d . . . C(16) C 0.1501(3) 0.5137(3) 0.0910(2) 0.0240(11) Uani 1.00 1 d . . . C(17) C 0.1138(3) 0.4496(3) 0.0674(2) 0.0234(11) Uani 1.00 1 d . . . C(18) C 0.4230(3) 0.1189(3) 0.20494(19) 0.0236(11) Uani 1.00 1 d . . . C(19) C 0.4456(3) 0.1606(3) 0.1618(2) 0.0253(11) Uani 1.00 1 d . . . C(20) C 0.3844(3) 0.1778(3) 0.2352(2) 0.0263(11) Uani 1.00 1 d . . . C(21) C 0.5020(3) 0.0879(3) 0.2331(2) 0.0308(12) Uani 1.00 1 d . . . C(22) C 0.3631(3) -0.1782(3) 0.20209(19) 0.0230(11) Uani 1.00 1 d . . . C(23) C 0.3819(3) -0.1831(3) 0.25463(19) 0.0275(12) Uani 1.00 1 d . . . C(24) C 0.4405(4) -0.1944(3) 0.1811(2) 0.0322(13) Uani 1.00 1 d . . . C(25) C 0.3000(4) -0.2419(3) 0.1850(2) 0.0360(14) Uani 1.00 1 d . . . C(26) C 0.2979(3) 0.4086(3) 0.18617(19) 0.0234(11) Uani 1.00 1 d . . . C(27) C 0.3711(3) 0.3660(3) 0.1722(2) 0.0314(12) Uani 1.00 1 d . . . C(28) C 0.2608(3) 0.3605(3) 0.2223(2) 0.0290(12) Uani 1.00 1 d . . . C(29) C 0.3284(4) 0.4876(3) 0.2087(2) 0.0389(15) Uani 1.00 1 d . . . C(30) C 0.1319(4) 0.6001(3) 0.0775(2) 0.0358(14) Uani 1.00 1 d . . . C(31) C 0.2094(5) 0.6365(5) 0.0639(3) 0.072(2) Uani 1.00 1 d . . . C(32) C 0.0628(6) 0.6085(4) 0.0392(3) 0.078(3) Uani 1.00 1 d . . . C(33) C 0.1114(6) 0.6487(4) 0.1189(3) 0.070(2) Uani 1.00 1 d . . . C(34) C 0.2636(3) -0.1027(3) 0.33620(19) 0.0250(11) Uani 1.00 1 d . . . C(35) C 0.2995(3) -0.1680(3) 0.3635(2) 0.0252(11) Uani 1.00 1 d . . . C(36) C 0.2676(3) -0.2427(3) 0.3532(2) 0.0308(12) Uani 1.00 1 d . . . C(37) C 0.2037(3) -0.2596(3) 0.3180(2) 0.0326(13) Uani 1.00 1 d . . . C(38) C 0.1696(3) -0.1973(3) 0.2917(2) 0.0311(12) Uani 1.00 1 d . . . C(39) C 0.1976(3) -0.1184(3) 0.3006(2) 0.0265(11) Uani 1.00 1 d . . . C(40) C 0.1581(3) -0.0588(3) 0.2712(2) 0.0291(12) Uani 1.00 1 d . . . C(41) C 0.1159(4) 0.0605(4) 0.2344(2) 0.0376(14) Uani 1.00 1 d . . . C(42) C 0.1340(4) 0.1464(4) 0.2288(2) 0.0400(15) Uani 1.00 1 d . . . C(43) C 0.1304(4) 0.1924(4) 0.2717(2) 0.0374(14) Uani 1.00 1 d . . . C(44) C 0.2393(3) 0.2460(3) 0.3231(2) 0.0316(13) Uani 1.00 1 d . . . C(45) C 0.3113(3) 0.2548(3) 0.3544(2) 0.0262(11) Uani 1.00 1 d . . . C(46) C 0.3611(3) 0.1891(3) 0.37168(19) 0.0236(11) Uani 1.00 1 d . . . C(47) C 0.4375(3) 0.2053(3) 0.40025(18) 0.0246(11) Uani 1.00 1 d . . . C(48) C 0.4538(3) 0.2834(3) 0.41235(19) 0.0278(11) Uani 1.00 1 d . . . C(49) C 0.4035(4) 0.3491(3) 0.3975(2) 0.0316(12) Uani 1.00 1 d . . . C(50) C 0.3337(4) 0.3334(3) 0.3683(2) 0.0325(13) Uani 1.00 1 d . . . C(51) C 0.3703(3) -0.1548(3) 0.4020(2) 0.0275(11) Uani 1.00 1 d . . . C(52) C 0.4419(3) -0.1164(3) 0.3825(2) 0.0309(12) Uani 1.00 1 d . . . C(53) C 0.4028(4) -0.2336(3) 0.4245(2) 0.0343(13) Uani 1.00 1 d . . . C(54) C 0.3427(4) -0.1022(3) 0.4392(2) 0.0321(13) Uani 1.00 1 d . . . C(55) C 0.1750(4) -0.3461(4) 0.3090(2) 0.0433(16) Uani 1.00 1 d . . . C(56) C 0.1066(6) -0.3534(5) 0.2698(4) 0.085(3) Uani 1.00 1 d . . . C(57) C 0.2475(5) -0.3943(4) 0.2964(3) 0.063(2) Uani 1.00 1 d . . . C(58) C 0.1505(8) -0.3814(5) 0.3530(3) 0.093(4) Uani 1.00 1 d . . . C(59) C 0.4971(3) 0.1378(3) 0.41580(19) 0.0257(11) Uani 1.00 1 d . . . C(60) C 0.5176(3) 0.0912(3) 0.3737(2) 0.0299(12) Uani 1.00 1 d . . . C(61) C 0.4599(4) 0.0821(3) 0.4482(2) 0.0325(13) Uani 1.00 1 d . . . C(62) C 0.5774(3) 0.1702(3) 0.4412(2) 0.0344(13) Uani 1.00 1 d . . . C(63) C 0.4273(4) 0.4334(3) 0.4155(2) 0.0350(13) Uani 1.00 1 d . . . C(64) C 0.5158(4) 0.4526(4) 0.4106(2) 0.0442(16) Uani 1.00 1 d . . . C(65) C 0.4163(5) 0.4360(4) 0.4660(2) 0.056(2) Uani 1.00 1 d . . . C(66) C 0.3729(5) 0.4970(4) 0.3895(3) 0.055(2) Uani 1.00 1 d . . . C(67) C 0.3189(5) 0.4286(5) 0.0307(3) 0.072(2) Uani 1.00 1 d . . . C(68) C 0.2897(4) 0.3486(5) 0.0116(2) 0.062(2) Uani 1.00 1 d . . . C(69) C 0.3154(6) 0.2779(6) 0.0343(3) 0.080(2) Uani 1.00 1 d . . . C(70) C 0.2821(9) 0.2024(7) 0.0187(4) 0.129(5) Uani 1.00 1 d . . . C(71) C 0.2358(8) 0.2050(9) -0.0232(4) 0.115(3) Uani 1.00 1 d . . . C(72) C 0.2081(7) 0.2731(8) -0.0470(3) 0.108(3) Uani 1.00 1 d . . . C(73) C 0.2360(6) 0.3472(7) -0.0295(3) 0.089(2) Uani 1.00 1 d . . . C(74) C -0.0383(10) 0.9899(13) 0.3047(6) 0.201(8) Uani 1.00 1 d . . . C(75) C 0.0111(9) 0.9412(11) 0.3413(5) 0.150(6) Uani 0.50 1 d P . . C(75a) C 0.0505(10) 0.8945(13) 0.3716(6) 0.208(9) Uani 0.50 1 d P . . C(76) C -0.0087(8) 0.8598(9) 0.3386(4) 0.172(6) Uani 1.00 1 d . . . C(77) C 0.0340(12) 0.8119(12) 0.3735(6) 0.159(7) Uani 0.50 1 d P . . C(77a) C -0.0501(16) 0.9059(15) 0.3067(8) 0.224(11) Uani 0.50 1 d P . . C(78) C 0.0960(9) 0.8450(12) 0.4061(5) 0.193(7) Uani 1.00 1 d . . . C(79) C 0.1150(10) 0.9271(15) 0.4082(7) 0.177(7) Uani 0.50 1 d P . . C(79a) C 0.0214(14) 1.0163(17) 0.3404(8) 0.201(9) Uani 0.50 1 d P . . C(80) C 0.0707(8) 0.9768(11) 0.3746(5) 0.189(6) Uani 1.00 1 d . . . H(1) H 0.4319 -0.0374 0.2215 0.026 Uiso 1.00 1 c R . . H(2) H 0.2271 -0.1227 0.1486 0.029 Uiso 1.00 1 c R . . H(3) H 0.1364 -0.0418 0.1061 0.034 Uiso 1.00 1 c R . . H(4) H 0.0490 -0.0003 0.0545 0.069 Uiso 1.00 1 c R . . H(5) H 0.0094 0.0748 0.0763 0.069 Uiso 1.00 1 c R . . H(6) H 0.0169 0.0779 -0.0051 0.074 Uiso 1.00 1 c R . . H(7) H 0.1110 0.0963 0.0098 0.074 Uiso 1.00 1 c R . . H(8) H 0.0382 0.2148 -0.0064 0.066 Uiso 1.00 1 c R . . H(9) H -0.0173 0.1938 0.0317 0.066 Uiso 1.00 1 c R . . H(10) H 0.0544 0.3274 0.0285 0.040 Uiso 1.00 1 c R . . H(11) H 0.2347 0.5402 0.1461 0.029 Uiso 1.00 1 c R . . H(12) H 0.0733 0.4586 0.0417 0.028 Uiso 1.00 1 c R . . H(13) H 0.4937 0.1353 0.1529 0.030 Uiso 1.00 1 c R . . H(14) H 0.4568 0.2170 0.1685 0.030 Uiso 1.00 1 c R . . H(15) H 0.4004 0.1560 0.1366 0.030 Uiso 1.00 1 c R . . H(16) H 0.3544 0.2185 0.2158 0.032 Uiso 1.00 1 c R . . H(17) H 0.4269 0.2032 0.2569 0.032 Uiso 1.00 1 c R . . H(18) H 0.3473 0.1491 0.2521 0.032 Uiso 1.00 1 c R . . H(19) H 0.4965 0.0872 0.2657 0.037 Uiso 1.00 1 c R . . H(20) H 0.5469 0.1230 0.2284 0.037 Uiso 1.00 1 c R . . H(21) H 0.5129 0.0338 0.2231 0.037 Uiso 1.00 1 c R . . H(22) H 0.4386 -0.1685 0.2646 0.033 Uiso 1.00 1 c R . . H(23) H 0.3726 -0.2376 0.2645 0.033 Uiso 1.00 1 c R . . H(24) H 0.3466 -0.1463 0.2682 0.033 Uiso 1.00 1 c R . . H(25) H 0.4261 -0.2192 0.1510 0.039 Uiso 1.00 1 c R . . H(26) H 0.4759 -0.2302 0.2013 0.039 Uiso 1.00 1 c R . . H(27) H 0.4687 -0.1440 0.1779 0.039 Uiso 1.00 1 c R . . H(28) H 0.2641 -0.2502 0.2079 0.043 Uiso 1.00 1 c R . . H(29) H 0.3275 -0.2919 0.1799 0.043 Uiso 1.00 1 c R . . H(30) H 0.2682 -0.2242 0.1561 0.043 Uiso 1.00 1 c R . . H(31) H 0.3640 0.3083 0.1745 0.038 Uiso 1.00 1 c R . . H(32) H 0.4202 0.3824 0.1925 0.038 Uiso 1.00 1 c R . . H(33) H 0.3762 0.3800 0.1405 0.038 Uiso 1.00 1 c R . . H(34) H 0.2374 0.3971 0.2426 0.035 Uiso 1.00 1 c R . . H(35) H 0.3030 0.3284 0.2404 0.035 Uiso 1.00 1 c R . . H(36) H 0.2183 0.3254 0.2069 0.035 Uiso 1.00 1 c R . . H(37) H 0.3744 0.5068 0.1947 0.047 Uiso 1.00 1 c R . . H(38) H 0.3454 0.4793 0.2416 0.047 Uiso 1.00 1 c R . . H(39) H 0.2848 0.5272 0.2041 0.047 Uiso 1.00 1 c R . . H(40) H 0.2423 0.6591 0.0911 0.086 Uiso 1.00 1 c R . . H(41) H 0.1949 0.6785 0.0411 0.086 Uiso 1.00 1 c R . . H(42) H 0.2403 0.5949 0.0509 0.086 Uiso 1.00 1 c R . . H(43) H 0.0835 0.6081 0.0098 0.094 Uiso 1.00 1 c R . . H(44) H 0.0346 0.6588 0.0425 0.094 Uiso 1.00 1 c R . . H(45) H 0.0252 0.5640 0.0401 0.094 Uiso 1.00 1 c R . . H(46) H 0.0531 0.6462 0.1196 0.083 Uiso 1.00 1 c R . . H(47) H 0.1277 0.7043 0.1159 0.083 Uiso 1.00 1 c R . . H(48) H 0.1406 0.6263 0.1473 0.083 Uiso 1.00 1 c R . . H(49) H 0.2906 -0.2860 0.3714 0.037 Uiso 1.00 1 c R . . H(50) H 0.1268 -0.2073 0.2673 0.037 Uiso 1.00 1 c R . . H(51) H 0.1186 -0.0780 0.2472 0.035 Uiso 1.00 1 c R . . H(52) H 0.1207 0.0328 0.2053 0.045 Uiso 1.00 1 c R . . H(53) H 0.0589 0.0557 0.2395 0.045 Uiso 1.00 1 c R . . H(54) H 0.0945 0.1689 0.2037 0.048 Uiso 1.00 1 c R . . H(55) H 0.1887 0.1518 0.2200 0.048 Uiso 1.00 1 c R . . H(56) H 0.1224 0.2497 0.2642 0.045 Uiso 1.00 1 c R . . H(57) H 0.0841 0.1739 0.2862 0.045 Uiso 1.00 1 c R . . H(58) H 0.2104 0.2939 0.3149 0.038 Uiso 1.00 1 c R . . H(59) H 0.5028 0.2942 0.4322 0.033 Uiso 1.00 1 c R . . H(60) H 0.2994 0.3764 0.3569 0.039 Uiso 1.00 1 c R . . H(61) H 0.4770 -0.1583 0.3733 0.037 Uiso 1.00 1 c R . . H(62) H 0.4729 -0.0828 0.4060 0.037 Uiso 1.00 1 c R . . H(63) H 0.4212 -0.0837 0.3557 0.037 Uiso 1.00 1 c R . . H(64) H 0.3734 -0.2462 0.4500 0.041 Uiso 1.00 1 c R . . H(65) H 0.4606 -0.2280 0.4361 0.041 Uiso 1.00 1 c R . . H(66) H 0.3950 -0.2766 0.4018 0.041 Uiso 1.00 1 c R . . H(67) H 0.3513 -0.0460 0.4322 0.038 Uiso 1.00 1 c R . . H(68) H 0.3741 -0.1155 0.4690 0.038 Uiso 1.00 1 c R . . H(69) H 0.2851 -0.1114 0.4402 0.038 Uiso 1.00 1 c R . . H(70) H 0.0548 -0.3486 0.2814 0.102 Uiso 1.00 1 c R . . H(71) H 0.1094 -0.4053 0.2550 0.102 Uiso 1.00 1 c R . . H(72) H 0.1110 -0.3110 0.2475 0.102 Uiso 1.00 1 c R . . H(73) H 0.2464 -0.3930 0.2631 0.076 Uiso 1.00 1 c R . . H(74) H 0.2437 -0.4496 0.3065 0.076 Uiso 1.00 1 c R . . H(75) H 0.2981 -0.3707 0.3116 0.076 Uiso 1.00 1 c R . . H(76) H 0.1979 -0.4058 0.3714 0.112 Uiso 1.00 1 c R . . H(77) H 0.1085 -0.4218 0.3450 0.112 Uiso 1.00 1 c R . . H(78) H 0.1296 -0.3389 0.3708 0.112 Uiso 1.00 1 c R . . H(79) H 0.4786 0.0478 0.3664 0.036 Uiso 1.00 1 c R . . H(80) H 0.5723 0.0691 0.3807 0.036 Uiso 1.00 1 c R . . H(81) H 0.5149 0.1273 0.3474 0.036 Uiso 1.00 1 c R . . H(82) H 0.4754 0.1001 0.4799 0.039 Uiso 1.00 1 c R . . H(83) H 0.4798 0.0278 0.4451 0.039 Uiso 1.00 1 c R . . H(84) H 0.4008 0.0829 0.4404 0.039 Uiso 1.00 1 c R . . H(85) H 0.6146 0.1804 0.4191 0.041 Uiso 1.00 1 c R . . H(86) H 0.6014 0.1310 0.4638 0.041 Uiso 1.00 1 c R . . H(87) H 0.5673 0.2200 0.4568 0.041 Uiso 1.00 1 c R . . H(88) H 0.5514 0.4359 0.4385 0.053 Uiso 1.00 1 c R . . H(89) H 0.5215 0.5100 0.4062 0.053 Uiso 1.00 1 c R . . H(90) H 0.5306 0.4240 0.3842 0.053 Uiso 1.00 1 c R . . H(91) H 0.3612 0.4537 0.4685 0.068 Uiso 1.00 1 c R . . H(92) H 0.4554 0.4734 0.4825 0.068 Uiso 1.00 1 c R . . H(93) H 0.4252 0.3828 0.4794 0.068 Uiso 1.00 1 c R . . H(94) H 0.3972 0.5154 0.3631 0.066 Uiso 1.00 1 c R . . H(95) H 0.3674 0.5420 0.4099 0.066 Uiso 1.00 1 c R . . H(96) H 0.3194 0.4742 0.3789 0.066 Uiso 1.00 1 c R . . H(97) H 0.2823 0.4482 0.0513 0.087 Uiso 1.00 1 c R . . H(98) H 0.3196 0.4664 0.0055 0.087 Uiso 1.00 1 c R . . H(99) H 0.3736 0.4231 0.0478 0.087 Uiso 1.00 1 c R . . H(100) H 0.3558 0.2801 0.0606 0.096 Uiso 1.00 1 c R . . H(101) H 0.2914 0.1548 0.0362 0.154 Uiso 1.00 1 c R . . H(102) H 0.2211 0.1554 -0.0376 0.138 Uiso 1.00 1 c R . . H(103) H 0.1709 0.2696 -0.0746 0.129 Uiso 1.00 1 c R . . H(104) H 0.2190 0.3951 -0.0452 0.107 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.01932(11) 0.01479(10) 0.02318(11) 0.00040(7) -0.00437(8) 0.00005(7) Pt(2) 0.01971(12) 0.02500(12) 0.01943(10) 0.00260(8) 0.00247(8) 0.00154(8) Sb(1) 0.0345(2) 0.0416(2) 0.0451(2) -0.01206(19) 0.0077(2) -0.0121(2) Sb(2) 0.0776(4) 0.0365(2) 0.0558(3) 0.0012(2) 0.0305(2) 0.0062(2) F(1) 0.187(7) 0.089(4) 0.053(3) -0.065(4) 0.046(3) -0.021(3) F(2) 0.065(3) 0.077(4) 0.164(6) -0.002(3) -0.041(4) -0.004(4) F(3) 0.264(11) 0.113(5) 0.094(5) -0.109(6) 0.097(6) -0.055(4) F(4) 0.038(3) 0.073(4) 0.276(11) -0.005(2) 0.002(4) -0.007(5) F(5) 0.053(2) 0.043(2) 0.081(3) -0.015(2) 0.009(2) -0.014(2) F(6) 0.080(3) 0.045(2) 0.074(3) -0.027(2) 0.033(2) -0.017(2) F(7) 0.109(4) 0.041(2) 0.101(4) -0.008(2) 0.053(3) -0.006(2) F(8) 0.111(5) 0.141(6) 0.147(6) -0.056(5) 0.073(5) -0.071(5) F(9) 0.176(7) 0.064(3) 0.077(3) -0.036(4) 0.052(4) -0.026(3) F(10) 0.50(2) 0.103(6) 0.432(19) -0.164(10) 0.43(2) -0.139(9) F(11) 0.147(8) 0.074(4) 0.326(14) 0.029(4) -0.135(9) 0.008(6) F(12) 0.344(17) 0.150(9) 0.115(7) 0.094(10) -0.088(9) -0.003(6) O(1) 0.0180(18) 0.0170(17) 0.0284(19) -0.0027(13) -0.0067(15) 0.0015(14) O(3) 0.0243(19) 0.0154(17) 0.0284(19) 0.0002(14) -0.0060(16) -0.0000(14) O(4) 0.026(2) 0.027(2) 0.0239(18) 0.0031(16) -0.0016(16) 0.0035(15) O(5) 0.0231(19) 0.0259(19) 0.0248(18) 0.0025(15) 0.0015(15) -0.0001(15) N(1) 0.029(2) 0.019(2) 0.035(2) -0.0084(18) -0.012(2) 0.0037(19) N(2) 0.024(2) 0.034(2) 0.027(2) 0.005(2) -0.004(2) 0.001(2) N(3) 0.032(2) 0.020(2) 0.044(2) -0.003(2) -0.019(2) -0.005(2) N(4) 0.028(2) 0.028(2) 0.031(2) 0.005(2) 0.001(2) 0.003(2) C(1) 0.016(2) 0.020(2) 0.024(2) 0.0022(18) -0.001(2) 0.003(2) C(2) 0.020(2) 0.021(2) 0.021(2) 0.001(2) 0.002(2) 0.000(2) C(3) 0.021(2) 0.023(2) 0.021(2) 0.002(2) 0.002(2) 0.004(2) C(4) 0.022(2) 0.019(2) 0.023(2) 0.005(2) 0.004(2) 0.003(2) C(5) 0.029(2) 0.017(2) 0.026(2) -0.005(2) 0.006(2) -0.001(2) C(6) 0.019(2) 0.022(2) 0.025(2) -0.000(2) -0.001(2) 0.000(2) C(7) 0.027(2) 0.017(2) 0.039(3) -0.009(2) -0.003(2) -0.000(2) C(8) 0.049(4) 0.033(3) 0.076(5) -0.021(3) -0.038(4) 0.020(3) C(9) 0.079(6) 0.037(4) 0.057(4) -0.009(4) -0.030(4) -0.005(3) C(10) 0.065(5) 0.022(3) 0.064(4) 0.001(3) -0.042(4) -0.008(3) C(11) 0.037(3) 0.022(2) 0.036(3) 0.008(2) -0.013(2) 0.001(2) C(12) 0.022(2) 0.023(2) 0.027(2) 0.001(2) 0.000(2) 0.000(2) C(13) 0.017(2) 0.020(2) 0.025(2) -0.0013(19) 0.003(2) -0.001(2) C(14) 0.016(2) 0.021(2) 0.023(2) -0.0042(18) 0.001(2) -0.003(2) C(15) 0.026(2) 0.018(2) 0.030(2) -0.006(2) 0.006(2) -0.002(2) C(16) 0.019(2) 0.017(2) 0.036(2) 0.0049(19) 0.003(2) 0.003(2) C(17) 0.017(2) 0.020(2) 0.033(2) 0.0016(19) 0.000(2) 0.002(2) C(18) 0.020(2) 0.020(2) 0.029(2) 0.001(2) 0.000(2) 0.004(2) C(19) 0.023(2) 0.021(2) 0.032(2) -0.000(2) 0.006(2) 0.001(2) C(20) 0.029(3) 0.022(2) 0.027(2) 0.001(2) -0.000(2) -0.000(2) C(21) 0.021(2) 0.027(2) 0.041(3) -0.000(2) -0.006(2) 0.003(2) C(22) 0.028(2) 0.018(2) 0.024(2) 0.004(2) 0.006(2) 0.001(2) C(23) 0.031(3) 0.025(2) 0.027(2) 0.009(2) 0.006(2) 0.009(2) C(24) 0.043(3) 0.025(2) 0.031(2) 0.011(2) 0.016(2) 0.005(2) C(25) 0.045(3) 0.017(2) 0.044(3) -0.000(2) -0.001(3) 0.005(2) C(26) 0.022(2) 0.020(2) 0.027(2) -0.003(2) -0.001(2) -0.004(2) C(27) 0.021(2) 0.036(3) 0.037(3) -0.001(2) 0.001(2) 0.006(2) C(28) 0.031(3) 0.031(3) 0.025(2) -0.001(2) 0.004(2) 0.001(2) C(29) 0.043(3) 0.029(3) 0.040(3) -0.011(2) -0.007(3) -0.002(2) C(30) 0.035(3) 0.020(2) 0.051(3) 0.001(2) 0.000(2) 0.007(2) C(31) 0.060(5) 0.053(5) 0.097(7) -0.016(4) -0.008(5) 0.033(5) C(32) 0.091(7) 0.023(3) 0.100(7) 0.001(3) -0.052(6) 0.018(4) C(33) 0.072(6) 0.036(4) 0.092(6) 0.018(4) -0.017(5) -0.015(4) C(34) 0.021(2) 0.030(2) 0.026(2) 0.003(2) 0.008(2) -0.001(2) C(35) 0.023(2) 0.027(2) 0.028(2) 0.002(2) 0.010(2) 0.002(2) C(36) 0.033(3) 0.029(3) 0.033(3) 0.004(2) 0.011(2) 0.002(2) C(37) 0.028(3) 0.035(3) 0.037(3) -0.007(2) 0.014(2) -0.005(2) C(38) 0.025(3) 0.033(3) 0.036(3) -0.002(2) 0.004(2) -0.007(2) C(39) 0.021(2) 0.031(2) 0.028(2) -0.001(2) 0.005(2) -0.004(2) C(40) 0.018(2) 0.036(3) 0.031(2) -0.000(2) -0.002(2) -0.005(2) C(41) 0.033(3) 0.045(3) 0.031(3) 0.005(2) -0.007(2) 0.006(2) C(42) 0.037(3) 0.050(4) 0.031(3) 0.008(3) -0.002(2) 0.009(2) C(43) 0.029(3) 0.036(3) 0.043(3) 0.011(2) -0.006(2) 0.000(2) C(44) 0.031(3) 0.029(3) 0.034(3) 0.007(2) 0.005(2) 0.007(2) C(45) 0.025(2) 0.028(2) 0.027(2) 0.003(2) 0.008(2) 0.001(2) C(46) 0.026(2) 0.025(2) 0.021(2) -0.000(2) 0.005(2) -0.003(2) C(47) 0.028(2) 0.028(2) 0.018(2) 0.002(2) 0.004(2) 0.000(2) C(48) 0.030(3) 0.030(3) 0.023(2) -0.004(2) 0.003(2) -0.001(2) C(49) 0.037(3) 0.032(3) 0.029(2) -0.001(2) 0.012(2) -0.004(2) C(50) 0.038(3) 0.027(2) 0.034(3) 0.006(2) 0.009(2) -0.000(2) C(51) 0.024(2) 0.030(2) 0.028(2) 0.002(2) 0.004(2) 0.005(2) C(52) 0.021(2) 0.036(3) 0.035(3) -0.002(2) 0.001(2) 0.005(2) C(53) 0.034(3) 0.030(3) 0.037(3) 0.003(2) 0.001(2) 0.006(2) C(54) 0.036(3) 0.037(3) 0.024(2) 0.003(2) 0.006(2) 0.002(2) C(55) 0.045(4) 0.030(3) 0.055(4) -0.009(2) 0.010(3) -0.001(3) C(56) 0.071(6) 0.045(4) 0.125(9) -0.025(4) -0.030(6) -0.010(5) C(57) 0.063(5) 0.034(4) 0.093(6) -0.006(3) 0.013(4) -0.017(4) C(58) 0.146(11) 0.052(5) 0.098(8) -0.050(6) 0.069(7) -0.009(5) C(59) 0.024(2) 0.030(2) 0.023(2) 0.001(2) 0.001(2) 0.003(2) C(60) 0.030(3) 0.031(3) 0.028(2) 0.002(2) 0.004(2) 0.002(2) C(61) 0.037(3) 0.035(3) 0.025(2) -0.000(2) 0.006(2) 0.006(2) C(62) 0.029(3) 0.038(3) 0.033(3) -0.005(2) -0.004(2) 0.005(2) C(63) 0.039(3) 0.031(3) 0.036(3) -0.001(2) 0.009(2) -0.004(2) C(64) 0.046(4) 0.033(3) 0.055(4) -0.009(3) 0.013(3) -0.009(3) C(65) 0.079(6) 0.049(4) 0.046(4) -0.011(4) 0.026(4) -0.019(3) C(66) 0.064(5) 0.028(3) 0.070(5) 0.010(3) -0.004(4) -0.009(3) C(67) 0.060(5) 0.094(6) 0.068(5) -0.009(4) 0.025(4) -0.009(4) C(68) 0.045(4) 0.103(5) 0.041(3) -0.004(4) 0.022(3) -0.022(3) C(69) 0.075(6) 0.090(5) 0.085(6) -0.000(4) 0.045(4) -0.012(4) C(70) 0.164(13) 0.086(6) 0.126(9) 0.040(7) -0.009(8) -0.067(6) C(71) 0.095(9) 0.150(9) 0.111(8) -0.022(8) 0.051(6) -0.056(7) C(72) 0.078(7) 0.178(10) 0.068(6) -0.016(7) 0.015(5) -0.062(6) C(73) 0.062(6) 0.151(8) 0.057(5) -0.010(6) 0.020(4) -0.031(5) C(74) 0.158(14) 0.263(16) 0.194(14) 0.109(14) 0.065(9) 0.124(14) C(75) 0.096(10) 0.267(14) 0.118(10) 0.134(11) 0.119(7) 0.147(11) C(75a) 0.164(18) 0.315(16) 0.170(17) 0.116(17) 0.108(10) 0.115(16) C(76) 0.159(10) 0.268(13) 0.120(8) 0.156(10) 0.116(7) 0.110(9) C(77) 0.152(14) 0.240(15) 0.121(13) 0.170(12) 0.133(9) 0.120(11) C(77a) 0.21(2) 0.273(19) 0.20(2) 0.11(2) 0.071(14) 0.140(18) C(78) 0.127(10) 0.325(17) 0.155(11) 0.151(12) 0.117(7) 0.123(12) C(79) 0.073(10) 0.34(2) 0.144(13) 0.119(13) 0.106(8) 0.124(15) C(79a) 0.15(2) 0.322(19) 0.156(19) 0.111(17) 0.090(12) 0.107(17) C(80) 0.121(9) 0.313(14) 0.161(11) 0.113(10) 0.118(7) 0.127(11) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pt(1) O(1) 1.986(3) yes . . Pt(1) O(3) 1.990(3) yes . . Pt(1) N(1) 1.971(4) yes . . Pt(1) N(3) 1.978(5) yes . . Pt(2) O(4) 1.985(3) yes . . Pt(2) O(5) 1.981(3) yes . . Pt(2) N(2) 1.984(4) yes . . Pt(2) N(4) 1.975(4) yes . . Sb(1) F(1) 1.821(6) yes . . Sb(1) F(2) 1.873(6) yes . . Sb(1) F(3) 1.868(7) yes . . Sb(1) F(4) 1.816(5) yes . . Sb(1) F(5) 1.875(4) yes . . Sb(1) F(6) 1.869(4) yes . . Sb(2) F(7) 1.873(5) yes . . Sb(2) F(8) 1.833(8) yes . . Sb(2) F(9) 1.853(6) yes . . Sb(2) F(10) 1.776(17) yes . . Sb(2) F(11) 1.821(10) yes . . Sb(2) F(12) 1.868(12) yes . . O(1) C(1) 1.308(6) yes . . O(3) C(13) 1.303(6) yes . . O(4) C(46) 1.304(6) yes . . O(5) C(34) 1.309(6) yes . . N(1) C(7) 1.294(7) yes . . N(1) C(8) 1.499(9) yes . . N(2) C(40) 1.307(8) yes . . N(2) C(41) 1.488(7) yes . . N(3) C(10) 1.504(9) yes . . N(3) C(11) 1.309(7) yes . . N(4) C(43) 1.483(8) yes . . N(4) C(44) 1.303(7) yes . . C(1) C(2) 1.440(7) yes . . C(1) C(6) 1.416(7) yes . . C(2) C(3) 1.371(7) yes . . C(2) C(18) 1.542(7) yes . . C(3) C(4) 1.421(7) yes . . C(4) C(5) 1.370(7) yes . . C(4) C(22) 1.537(7) yes . . C(5) C(6) 1.411(7) yes . . C(6) C(7) 1.431(7) yes . . C(8) C(9) 1.457(12) yes . . C(9) C(10) 1.506(10) yes . . C(11) C(12) 1.420(8) yes . . C(12) C(13) 1.427(7) yes . . C(12) C(17) 1.406(7) yes . . C(13) C(14) 1.434(7) yes . . C(14) C(15) 1.365(7) yes . . C(14) C(26) 1.540(7) yes . . C(15) C(16) 1.419(7) yes . . C(16) C(17) 1.373(7) yes . . C(16) C(30) 1.522(8) yes . . C(18) C(19) 1.548(8) yes . . C(18) C(20) 1.537(8) yes . . C(18) C(21) 1.541(7) yes . . C(22) C(23) 1.537(7) yes . . C(22) C(24) 1.539(9) yes . . C(22) C(25) 1.533(8) yes . . C(26) C(27) 1.526(8) yes . . C(26) C(28) 1.541(8) yes . . C(26) C(29) 1.535(8) yes . . C(30) C(31) 1.537(12) yes . . C(30) C(32) 1.497(11) yes . . C(30) C(33) 1.549(12) yes . . C(34) C(35) 1.436(7) yes . . C(34) C(39) 1.429(7) yes . . C(35) C(36) 1.379(8) yes . . C(35) C(51) 1.529(7) yes . . C(36) C(37) 1.403(8) yes . . C(37) C(38) 1.374(8) yes . . C(37) C(55) 1.539(9) yes . . C(38) C(39) 1.417(8) yes . . C(39) C(40) 1.420(8) yes . . C(41) C(42) 1.486(10) yes . . C(42) C(43) 1.492(9) yes . . C(44) C(45) 1.412(7) yes . . C(45) C(46) 1.429(7) yes . . C(45) C(50) 1.415(8) yes . . C(46) C(47) 1.447(7) yes . . C(47) C(48) 1.377(8) yes . . C(47) C(59) 1.533(7) yes . . C(48) C(49) 1.416(8) yes . . C(49) C(50) 1.369(8) yes . . C(49) C(63) 1.542(8) yes . . C(51) C(52) 1.544(8) yes . . C(51) C(53) 1.543(8) yes . . C(51) C(54) 1.534(8) yes . . C(55) C(56) 1.507(12) yes . . C(55) C(57) 1.547(12) yes . . C(55) C(58) 1.537(14) yes . . C(59) C(60) 1.549(8) yes . . C(59) C(61) 1.534(8) yes . . C(59) C(62) 1.534(8) yes . . C(63) C(64) 1.541(10) yes . . C(63) C(65) 1.529(10) yes . . C(63) C(66) 1.532(10) yes . . C(67) C(68) 1.509(13) yes . . C(68) C(69) 1.398(13) yes . . C(68) C(73) 1.396(11) yes . . C(69) C(70) 1.434(15) yes . . C(70) C(71) 1.359(18) yes . . C(71) C(72) 1.38(2) yes . . C(72) C(73) 1.399(18) yes . . C(74) C(75) 1.50(2) yes . . C(75) C(75a) 1.29(2) yes . . C(75) C(76) 1.41(2) yes . . C(75) C(80) 1.42(2) yes . . C(75a) C(76) 1.41(2) yes . . C(75a) C(77) 1.42(3) yes . . C(75a) C(78) 1.44(2) yes . . C(75a) C(79) 1.51(2) yes . . C(75a) C(80) 1.42(2) yes . . C(76) C(77) 1.41(2) yes . . C(77) C(78) 1.42(2) yes . . C(78) C(79) 1.41(3) yes . . C(79) C(80) 1.42(2) yes . . C(3) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.990 no . . C(8) H(5) 0.990 no . . C(9) H(6) 0.990 no . . C(9) H(7) 0.990 no . . C(10) H(8) 0.990 no . . C(10) H(9) 0.990 no . . C(11) H(10) 0.950 no . . C(15) H(11) 0.950 no . . C(17) H(12) 0.950 no . . C(19) H(13) 0.980 no . . C(19) H(14) 0.980 no . . C(19) H(15) 0.980 no . . C(20) H(16) 0.980 no . . C(20) H(17) 0.980 no . . C(20) H(18) 0.980 no . . C(21) H(19) 0.980 no . . C(21) H(20) 0.980 no . . C(21) H(21) 0.980 no . . C(23) H(22) 0.980 no . . C(23) H(23) 0.980 no . . C(23) H(24) 0.980 no . . C(24) H(25) 0.980 no . . C(24) H(26) 0.980 no . . C(24) H(27) 0.980 no . . C(25) H(28) 0.980 no . . C(25) H(29) 0.980 no . . C(25) H(30) 0.980 no . . C(27) H(31) 0.980 no . . C(27) H(32) 0.980 no . . C(27) H(33) 0.980 no . . C(28) H(34) 0.980 no . . C(28) H(35) 0.980 no . . C(28) H(36) 0.980 no . . C(29) H(37) 0.980 no . . C(29) H(38) 0.980 no . . C(29) H(39) 0.980 no . . C(31) H(40) 0.980 no . . C(31) H(41) 0.980 no . . C(31) H(42) 0.980 no . . C(32) H(43) 0.980 no . . C(32) H(44) 0.980 no . . C(32) H(45) 0.980 no . . C(33) H(46) 0.980 no . . C(33) H(47) 0.980 no . . C(33) H(48) 0.980 no . . C(36) H(49) 0.950 no . . C(38) H(50) 0.950 no . . C(40) H(51) 0.950 no . . C(41) H(52) 0.990 no . . C(41) H(53) 0.990 no . . C(42) H(54) 0.990 no . . C(42) H(55) 0.990 no . . C(43) H(56) 0.990 no . . C(43) H(57) 0.990 no . . C(44) H(58) 0.950 no . . C(48) H(59) 0.950 no . . C(50) H(60) 0.950 no . . C(52) H(61) 0.980 no . . C(52) H(62) 0.980 no . . C(52) H(63) 0.980 no . . C(53) H(64) 0.980 no . . C(53) H(65) 0.980 no . . C(53) H(66) 0.980 no . . C(54) H(67) 0.980 no . . C(54) H(68) 0.980 no . . C(54) H(69) 0.980 no . . C(56) H(70) 0.980 no . . C(56) H(71) 0.980 no . . C(56) H(72) 0.980 no . . C(57) H(73) 0.980 no . . C(57) H(74) 0.980 no . . C(57) H(75) 0.980 no . . C(58) H(76) 0.980 no . . C(58) H(77) 0.980 no . . C(58) H(78) 0.980 no . . C(60) H(79) 0.980 no . . C(60) H(80) 0.980 no . . C(60) H(81) 0.980 no . . C(61) H(82) 0.980 no . . C(61) H(83) 0.980 no . . C(61) H(84) 0.980 no . . C(62) H(85) 0.980 no . . C(62) H(86) 0.980 no . . C(62) H(87) 0.980 no . . C(64) H(88) 0.980 no . . C(64) H(89) 0.980 no . . C(64) H(90) 0.980 no . . C(65) H(91) 0.980 no . . C(65) H(92) 0.980 no . . C(65) H(93) 0.980 no . . C(66) H(94) 0.980 no . . C(66) H(95) 0.980 no . . C(66) H(96) 0.980 no . . C(67) H(97) 0.980 no . . C(67) H(98) 0.980 no . . C(67) H(99) 0.980 no . . C(69) H(100) 0.950 no . . C(70) H(101) 0.950 no . . C(71) H(102) 0.950 no . . C(72) H(103) 0.950 no . . C(73) H(104) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) Pt(1) O(3) 81.75(14) yes . . . O(1) Pt(1) N(1) 91.00(17) yes . . . O(1) Pt(1) N(3) 170.31(19) yes . . . O(3) Pt(1) N(1) 170.54(18) yes . . . O(3) Pt(1) N(3) 91.50(17) yes . . . N(1) Pt(1) N(3) 96.40(19) yes . . . O(4) Pt(2) O(5) 82.27(15) yes . . . O(4) Pt(2) N(2) 171.33(19) yes . . . O(4) Pt(2) N(4) 91.00(18) yes . . . O(5) Pt(2) N(2) 91.71(18) yes . . . O(5) Pt(2) N(4) 170.88(18) yes . . . N(2) Pt(2) N(4) 95.6(2) yes . . . F(1) Sb(1) F(2) 90.4(3) yes . . . F(1) Sb(1) F(3) 175.9(4) yes . . . F(1) Sb(1) F(4) 95.8(4) yes . . . F(1) Sb(1) F(5) 90.8(2) yes . . . F(1) Sb(1) F(6) 89.5(2) yes . . . F(2) Sb(1) F(3) 85.5(4) yes . . . F(2) Sb(1) F(4) 173.8(4) yes . . . F(2) Sb(1) F(5) 87.9(2) yes . . . F(2) Sb(1) F(6) 91.4(2) yes . . . F(3) Sb(1) F(4) 88.3(4) yes . . . F(3) Sb(1) F(5) 89.8(3) yes . . . F(3) Sb(1) F(6) 89.9(2) yes . . . F(4) Sb(1) F(5) 92.3(2) yes . . . F(4) Sb(1) F(6) 88.3(2) yes . . . F(5) Sb(1) F(6) 179.3(2) yes . . . F(7) Sb(2) F(8) 91.1(3) yes . . . F(7) Sb(2) F(9) 179.6(3) yes . . . F(7) Sb(2) F(10) 90.8(4) yes . . . F(7) Sb(2) F(11) 89.5(3) yes . . . F(7) Sb(2) F(12) 90.0(3) yes . . . F(8) Sb(2) F(9) 89.3(3) yes . . . F(8) Sb(2) F(10) 176.9(5) yes . . . F(8) Sb(2) F(11) 86.2(4) yes . . . F(8) Sb(2) F(12) 84.9(5) yes . . . F(9) Sb(2) F(10) 88.9(4) yes . . . F(9) Sb(2) F(11) 90.8(3) yes . . . F(9) Sb(2) F(12) 89.8(3) yes . . . F(10) Sb(2) F(11) 96.2(6) yes . . . F(10) Sb(2) F(12) 92.6(6) yes . . . F(11) Sb(2) F(12) 171.1(5) yes . . . Pt(1) O(1) C(1) 129.8(3) yes . . . Pt(1) O(3) C(13) 130.0(3) yes . . . Pt(2) O(4) C(46) 130.0(3) yes . . . Pt(2) O(5) C(34) 130.1(3) yes . . . Pt(1) N(1) C(7) 124.7(4) yes . . . Pt(1) N(1) C(8) 119.6(3) yes . . . C(7) N(1) C(8) 115.5(4) yes . . . Pt(2) N(2) C(40) 122.8(3) yes . . . Pt(2) N(2) C(41) 123.8(4) yes . . . C(40) N(2) C(41) 113.3(4) yes . . . Pt(1) N(3) C(10) 124.2(3) yes . . . Pt(1) N(3) C(11) 123.4(4) yes . . . C(10) N(3) C(11) 112.4(5) yes . . . Pt(2) N(4) C(43) 119.4(3) yes . . . Pt(2) N(4) C(44) 124.3(4) yes . . . C(43) N(4) C(44) 116.1(5) yes . . . O(1) C(1) C(2) 119.2(4) yes . . . O(1) C(1) C(6) 122.0(4) yes . . . C(2) C(1) C(6) 118.8(4) yes . . . C(1) C(2) C(3) 117.2(4) yes . . . C(1) C(2) C(18) 120.8(4) yes . . . C(3) C(2) C(18) 122.0(4) yes . . . C(2) C(3) C(4) 124.9(4) yes . . . C(3) C(4) C(5) 117.0(4) yes . . . C(3) C(4) C(22) 119.0(4) yes . . . C(5) C(4) C(22) 123.9(4) yes . . . C(4) C(5) C(6) 121.4(4) yes . . . C(1) C(6) C(5) 120.6(4) yes . . . C(1) C(6) C(7) 123.1(4) yes . . . C(5) C(6) C(7) 116.2(4) yes . . . N(1) C(7) C(6) 128.8(5) yes . . . N(1) C(8) C(9) 110.7(6) yes . . . C(8) C(9) C(10) 113.1(7) yes . . . N(3) C(10) C(9) 114.1(6) yes . . . N(3) C(11) C(12) 129.8(5) yes . . . C(11) C(12) C(13) 123.0(5) yes . . . C(11) C(12) C(17) 116.5(4) yes . . . C(13) C(12) C(17) 120.4(4) yes . . . O(3) C(13) C(12) 122.0(4) yes . . . O(3) C(13) C(14) 119.8(4) yes . . . C(12) C(13) C(14) 118.2(4) yes . . . C(13) C(14) C(15) 117.9(4) yes . . . C(13) C(14) C(26) 120.6(4) yes . . . C(15) C(14) C(26) 121.5(4) yes . . . C(14) C(15) C(16) 125.1(4) yes . . . C(15) C(16) C(17) 116.5(4) yes . . . C(15) C(16) C(30) 119.5(4) yes . . . C(17) C(16) C(30) 124.0(4) yes . . . C(12) C(17) C(16) 121.8(4) yes . . . C(2) C(18) C(19) 109.2(4) yes . . . C(2) C(18) C(20) 110.0(4) yes . . . C(2) C(18) C(21) 111.2(4) yes . . . C(19) C(18) C(20) 111.2(4) yes . . . C(19) C(18) C(21) 107.6(4) yes . . . C(20) C(18) C(21) 107.7(4) yes . . . C(4) C(22) C(23) 110.0(4) yes . . . C(4) C(22) C(24) 108.2(4) yes . . . C(4) C(22) C(25) 111.4(4) yes . . . C(23) C(22) C(24) 109.8(4) yes . . . C(23) C(22) C(25) 108.8(4) yes . . . C(24) C(22) C(25) 108.8(4) yes . . . C(14) C(26) C(27) 109.8(4) yes . . . C(14) C(26) C(28) 109.3(4) yes . . . C(14) C(26) C(29) 112.0(4) yes . . . C(27) C(26) C(28) 111.4(4) yes . . . C(27) C(26) C(29) 107.1(4) yes . . . C(28) C(26) C(29) 107.2(4) yes . . . C(16) C(30) C(31) 107.7(5) yes . . . C(16) C(30) C(32) 112.8(5) yes . . . C(16) C(30) C(33) 110.7(5) yes . . . C(31) C(30) C(32) 110.6(7) yes . . . C(31) C(30) C(33) 106.9(6) yes . . . C(32) C(30) C(33) 108.1(6) yes . . . O(5) C(34) C(35) 120.1(4) yes . . . O(5) C(34) C(39) 120.9(4) yes . . . C(35) C(34) C(39) 118.9(5) yes . . . C(34) C(35) C(36) 117.0(4) yes . . . C(34) C(35) C(51) 121.2(4) yes . . . C(36) C(35) C(51) 121.8(5) yes . . . C(35) C(36) C(37) 125.1(5) yes . . . C(36) C(37) C(38) 118.0(5) yes . . . C(36) C(37) C(55) 120.1(5) yes . . . C(38) C(37) C(55) 121.9(5) yes . . . C(37) C(38) C(39) 120.6(5) yes . . . C(34) C(39) C(38) 120.4(5) yes . . . C(34) C(39) C(40) 123.8(5) yes . . . C(38) C(39) C(40) 115.8(4) yes . . . N(2) C(40) C(39) 129.7(5) yes . . . N(2) C(41) C(42) 116.0(5) yes . . . C(41) C(42) C(43) 111.9(5) yes . . . N(4) C(43) C(42) 109.9(5) yes . . . N(4) C(44) C(45) 129.2(5) yes . . . C(44) C(45) C(46) 123.1(5) yes . . . C(44) C(45) C(50) 116.7(5) yes . . . C(46) C(45) C(50) 120.2(5) yes . . . O(4) C(46) C(45) 121.8(4) yes . . . O(4) C(46) C(47) 119.6(4) yes . . . C(45) C(46) C(47) 118.6(4) yes . . . C(46) C(47) C(48) 117.0(5) yes . . . C(46) C(47) C(59) 120.9(4) yes . . . C(48) C(47) C(59) 122.1(4) yes . . . C(47) C(48) C(49) 125.2(5) yes . . . C(48) C(49) C(50) 117.2(5) yes . . . C(48) C(49) C(63) 119.7(5) yes . . . C(50) C(49) C(63) 123.1(5) yes . . . C(45) C(50) C(49) 121.6(5) yes . . . C(35) C(51) C(52) 109.9(4) yes . . . C(35) C(51) C(53) 112.3(4) yes . . . C(35) C(51) C(54) 109.5(4) yes . . . C(52) C(51) C(53) 106.1(4) yes . . . C(52) C(51) C(54) 111.1(4) yes . . . C(53) C(51) C(54) 107.9(4) yes . . . C(37) C(55) C(56) 112.9(6) yes . . . C(37) C(55) C(57) 107.4(6) yes . . . C(37) C(55) C(58) 109.5(6) yes . . . C(56) C(55) C(57) 107.7(7) yes . . . C(56) C(55) C(58) 110.6(8) yes . . . C(57) C(55) C(58) 108.6(7) yes . . . C(47) C(59) C(60) 110.2(4) yes . . . C(47) C(59) C(61) 109.3(4) yes . . . C(47) C(59) C(62) 111.4(4) yes . . . C(60) C(59) C(61) 110.6(4) yes . . . C(60) C(59) C(62) 106.8(4) yes . . . C(61) C(59) C(62) 108.5(4) yes . . . C(49) C(63) C(64) 111.2(5) yes . . . C(49) C(63) C(65) 107.5(5) yes . . . C(49) C(63) C(66) 111.3(5) yes . . . C(64) C(63) C(65) 110.0(6) yes . . . C(64) C(63) C(66) 108.2(5) yes . . . C(65) C(63) C(66) 108.6(6) yes . . . C(67) C(68) C(69) 121.1(7) yes . . . C(67) C(68) C(73) 118.0(8) yes . . . C(69) C(68) C(73) 121.0(9) yes . . . C(68) C(69) C(70) 121.3(9) yes . . . C(69) C(70) C(71) 113.9(11) yes . . . C(70) C(71) C(72) 126.2(13) yes . . . C(71) C(72) C(73) 118.7(10) yes . . . C(68) C(73) C(72) 118.0(10) yes . . . C(75) C(74) C(77a) 59.7(14) yes . . . C(75) C(74) C(79a) 51.7(14) yes . . . C(77a) C(74) C(79a) 111.4(19) yes . . . C(74) C(75) C(75a) 175.5(19) yes . . . C(74) C(75) C(76) 112.8(13) yes . . . C(74) C(75) C(77a) 57.6(13) yes . . . C(74) C(75) C(79a) 60.5(15) yes . . . C(74) C(75) C(80) 121.5(17) yes . . . C(75a) C(75) C(76) 62.7(13) yes . . . C(75a) C(75) C(77a) 118.0(19) yes . . . C(75a) C(75) C(79a) 123.9(18) yes . . . C(75a) C(75) C(80) 63.0(13) yes . . . C(76) C(75) C(77a) 55.3(13) yes . . . C(76) C(75) C(79a) 173.2(16) yes . . . C(76) C(75) C(80) 125.7(14) yes . . . C(77a) C(75) C(79a) 118.1(18) yes . . . C(77a) C(75) C(80) 179.0(15) yes . . . C(79a) C(75) C(80) 60.9(14) yes . . . C(75) C(75a) C(76) 62.5(12) yes . . . C(75) C(75a) C(77) 122.6(17) yes . . . C(75) C(75a) C(78) 177.9(18) yes . . . C(75) C(75a) C(79) 121(2) yes . . . C(75) C(75a) C(80) 62.9(13) yes . . . C(76) C(75a) C(77) 60.1(12) yes . . . C(76) C(75a) C(78) 119.6(18) yes . . . C(76) C(75a) C(79) 177(2) yes . . . C(76) C(75a) C(80) 125.4(16) yes . . . C(77) C(75a) C(78) 59.5(13) yes . . . C(77) C(75a) C(79) 116.7(17) yes . . . C(77) C(75a) C(80) 174.1(16) yes . . . C(78) C(75a) C(79) 57.2(13) yes . . . C(78) C(75a) C(80) 115.0(15) yes . . . C(79) C(75a) C(80) 57.8(13) yes . . . C(75) C(76) C(75a) 54.8(11) yes . . . C(75) C(76) C(77) 114.9(13) yes . . . C(75) C(76) C(77a) 64.4(14) yes . . . C(75a) C(76) C(77) 60.2(13) yes . . . C(75a) C(76) C(77a) 119.2(18) yes . . . C(77) C(76) C(77a) 178.1(18) yes . . . C(75a) C(77) C(76) 59.7(12) yes . . . C(75a) C(77) C(78) 61.1(13) yes . . . C(76) C(77) C(78) 120.7(18) yes . . . C(74) C(77a) C(75) 62.7(14) yes . . . C(74) C(77a) C(76) 123.1(19) yes . . . C(75) C(77a) C(76) 60.3(13) yes . . . C(75a) C(78) C(77) 59.4(13) yes . . . C(75a) C(78) C(79) 63.9(14) yes . . . C(77) C(78) C(79) 123.3(16) yes . . . C(75a) C(79) C(78) 58.9(13) yes . . . C(75a) C(79) C(80) 58.1(12) yes . . . C(78) C(79) C(80) 117.0(16) yes . . . C(74) C(79a) C(75) 67.7(16) yes . . . C(74) C(79a) C(80) 133(2) yes . . . C(75) C(79a) C(80) 64.9(15) yes . . . C(75) C(80) C(75a) 54.1(11) yes . . . C(75) C(80) C(79) 118.3(17) yes . . . C(75) C(80) C(79a) 54.2(14) yes . . . C(75a) C(80) C(79) 64.2(14) yes . . . C(75a) C(80) C(79a) 108.3(16) yes . . . C(79) C(80) C(79a) 172(2) yes . . . C(2) C(3) H(1) 117.5 no . . . C(4) C(3) H(1) 117.5 no . . . C(4) C(5) H(2) 119.3 no . . . C(6) C(5) H(2) 119.3 no . . . N(1) C(7) H(3) 115.6 no . . . C(6) C(7) H(3) 115.6 no . . . N(1) C(8) H(4) 109.5 no . . . N(1) C(8) H(5) 109.5 no . . . C(9) C(8) H(4) 109.5 no . . . C(9) C(8) H(5) 109.5 no . . . H(4) C(8) H(5) 108.1 no . . . C(8) C(9) H(6) 109.0 no . . . C(8) C(9) H(7) 109.0 no . . . C(10) C(9) H(6) 109.0 no . . . C(10) C(9) H(7) 109.0 no . . . H(6) C(9) H(7) 107.8 no . . . N(3) C(10) H(8) 108.7 no . . . N(3) C(10) H(9) 108.7 no . . . C(9) C(10) H(8) 108.7 no . . . C(9) C(10) H(9) 108.7 no . . . H(8) C(10) H(9) 107.6 no . . . N(3) C(11) H(10) 115.1 no . . . C(12) C(11) H(10) 115.1 no . . . C(14) C(15) H(11) 117.4 no . . . C(16) C(15) H(11) 117.4 no . . . C(12) C(17) H(12) 119.1 no . . . C(16) C(17) H(12) 119.1 no . . . C(18) C(19) H(13) 109.5 no . . . C(18) C(19) H(14) 109.5 no . . . C(18) C(19) H(15) 109.5 no . . . H(13) C(19) H(14) 109.5 no . . . H(13) C(19) H(15) 109.5 no . . . H(14) C(19) H(15) 109.5 no . . . C(18) C(20) H(16) 109.5 no . . . C(18) C(20) H(17) 109.5 no . . . C(18) C(20) H(18) 109.5 no . . . H(16) C(20) H(17) 109.5 no . . . H(16) C(20) H(18) 109.5 no . . . H(17) C(20) H(18) 109.5 no . . . C(18) C(21) H(19) 109.5 no . . . C(18) C(21) H(20) 109.5 no . . . C(18) C(21) H(21) 109.5 no . . . H(19) C(21) H(20) 109.5 no . . . H(19) C(21) H(21) 109.5 no . . . H(20) C(21) H(21) 109.5 no . . . C(22) C(23) H(22) 109.5 no . . . C(22) C(23) H(23) 109.5 no . . . C(22) C(23) H(24) 109.5 no . . . H(22) C(23) H(23) 109.5 no . . . H(22) C(23) H(24) 109.5 no . . . H(23) C(23) H(24) 109.5 no . . . C(22) C(24) H(25) 109.5 no . . . C(22) C(24) H(26) 109.5 no . . . C(22) C(24) H(27) 109.5 no . . . H(25) C(24) H(26) 109.5 no . . . H(25) C(24) H(27) 109.5 no . . . H(26) C(24) H(27) 109.5 no . . . C(22) C(25) H(28) 109.5 no . . . C(22) C(25) H(29) 109.5 no . . . C(22) C(25) H(30) 109.5 no . . . H(28) C(25) H(29) 109.5 no . . . H(28) C(25) H(30) 109.5 no . . . H(29) C(25) H(30) 109.5 no . . . C(26) C(27) H(31) 109.5 no . . . C(26) C(27) H(32) 109.5 no . . . C(26) C(27) H(33) 109.5 no . . . H(31) C(27) H(32) 109.5 no . . . H(31) C(27) H(33) 109.5 no . . . H(32) C(27) H(33) 109.5 no . . . C(26) C(28) H(34) 109.5 no . . . C(26) C(28) H(35) 109.5 no . . . C(26) C(28) H(36) 109.5 no . . . H(34) C(28) H(35) 109.5 no . . . H(34) C(28) H(36) 109.5 no . . . H(35) C(28) H(36) 109.5 no . . . C(26) C(29) H(37) 109.5 no . . . C(26) C(29) H(38) 109.5 no . . . C(26) C(29) H(39) 109.5 no . . . H(37) C(29) H(38) 109.5 no . . . H(37) C(29) H(39) 109.5 no . . . H(38) C(29) H(39) 109.5 no . . . C(30) C(31) H(40) 109.5 no . . . C(30) C(31) H(41) 109.5 no . . . C(30) C(31) H(42) 109.5 no . . . H(40) C(31) H(41) 109.5 no . . . H(40) C(31) H(42) 109.5 no . . . H(41) C(31) H(42) 109.5 no . . . C(30) C(32) H(43) 109.5 no . . . C(30) C(32) H(44) 109.5 no . . . C(30) C(32) H(45) 109.5 no . . . H(43) C(32) H(44) 109.5 no . . . H(43) C(32) H(45) 109.5 no . . . H(44) C(32) H(45) 109.5 no . . . C(30) C(33) H(46) 109.5 no . . . C(30) C(33) H(47) 109.5 no . . . C(30) C(33) H(48) 109.5 no . . . H(46) C(33) H(47) 109.5 no . . . H(46) C(33) H(48) 109.5 no . . . H(47) C(33) H(48) 109.5 no . . . C(35) C(36) H(49) 117.5 no . . . C(37) C(36) H(49) 117.5 no . . . C(37) C(38) H(50) 119.7 no . . . C(39) C(38) H(50) 119.7 no . . . N(2) C(40) H(51) 115.2 no . . . C(39) C(40) H(51) 115.1 no . . . N(2) C(41) H(52) 108.3 no . . . N(2) C(41) H(53) 108.3 no . . . C(42) C(41) H(52) 108.3 no . . . C(42) C(41) H(53) 108.3 no . . . H(52) C(41) H(53) 107.4 no . . . C(41) C(42) H(54) 109.2 no . . . C(41) C(42) H(55) 109.2 no . . . C(43) C(42) H(54) 109.2 no . . . C(43) C(42) H(55) 109.2 no . . . H(54) C(42) H(55) 107.9 no . . . N(4) C(43) H(56) 109.7 no . . . N(4) C(43) H(57) 109.7 no . . . C(42) C(43) H(56) 109.7 no . . . C(42) C(43) H(57) 109.7 no . . . H(56) C(43) H(57) 108.2 no . . . N(4) C(44) H(58) 115.4 no . . . C(45) C(44) H(58) 115.4 no . . . C(47) C(48) H(59) 117.4 no . . . C(49) C(48) H(59) 117.4 no . . . C(45) C(50) H(60) 119.2 no . . . C(49) C(50) H(60) 119.2 no . . . C(51) C(52) H(61) 109.5 no . . . C(51) C(52) H(62) 109.5 no . . . C(51) C(52) H(63) 109.5 no . . . H(61) C(52) H(62) 109.5 no . . . H(61) C(52) H(63) 109.5 no . . . H(62) C(52) H(63) 109.5 no . . . C(51) C(53) H(64) 109.5 no . . . C(51) C(53) H(65) 109.5 no . . . C(51) C(53) H(66) 109.5 no . . . H(64) C(53) H(65) 109.5 no . . . H(64) C(53) H(66) 109.5 no . . . H(65) C(53) H(66) 109.5 no . . . C(51) C(54) H(67) 109.5 no . . . C(51) C(54) H(68) 109.5 no . . . C(51) C(54) H(69) 109.5 no . . . H(67) C(54) H(68) 109.5 no . . . H(67) C(54) H(69) 109.5 no . . . H(68) C(54) H(69) 109.5 no . . . C(55) C(56) H(70) 109.5 no . . . C(55) C(56) H(71) 109.5 no . . . C(55) C(56) H(72) 109.5 no . . . H(70) C(56) H(71) 109.5 no . . . H(70) C(56) H(72) 109.5 no . . . H(71) C(56) H(72) 109.5 no . . . C(55) C(57) H(73) 109.5 no . . . C(55) C(57) H(74) 109.5 no . . . C(55) C(57) H(75) 109.5 no . . . H(73) C(57) H(74) 109.5 no . . . H(73) C(57) H(75) 109.5 no . . . H(74) C(57) H(75) 109.5 no . . . C(55) C(58) H(76) 109.5 no . . . C(55) C(58) H(77) 109.5 no . . . C(55) C(58) H(78) 109.5 no . . . H(76) C(58) H(77) 109.5 no . . . H(76) C(58) H(78) 109.5 no . . . H(77) C(58) H(78) 109.5 no . . . C(59) C(60) H(79) 109.5 no . . . C(59) C(60) H(80) 109.5 no . . . C(59) C(60) H(81) 109.5 no . . . H(79) C(60) H(80) 109.5 no . . . H(79) C(60) H(81) 109.5 no . . . H(80) C(60) H(81) 109.5 no . . . C(59) C(61) H(82) 109.5 no . . . C(59) C(61) H(83) 109.5 no . . . C(59) C(61) H(84) 109.5 no . . . H(82) C(61) H(83) 109.5 no . . . H(82) C(61) H(84) 109.5 no . . . H(83) C(61) H(84) 109.5 no . . . C(59) C(62) H(85) 109.5 no . . . C(59) C(62) H(86) 109.5 no . . . C(59) C(62) H(87) 109.5 no . . . H(85) C(62) H(86) 109.5 no . . . H(85) C(62) H(87) 109.5 no . . . H(86) C(62) H(87) 109.5 no . . . C(63) C(64) H(88) 109.5 no . . . C(63) C(64) H(89) 109.5 no . . . C(63) C(64) H(90) 109.5 no . . . H(88) C(64) H(89) 109.5 no . . . H(88) C(64) H(90) 109.5 no . . . H(89) C(64) H(90) 109.5 no . . . C(63) C(65) H(91) 109.5 no . . . C(63) C(65) H(92) 109.5 no . . . C(63) C(65) H(93) 109.5 no . . . H(91) C(65) H(92) 109.5 no . . . H(91) C(65) H(93) 109.5 no . . . H(92) C(65) H(93) 109.5 no . . . C(63) C(66) H(94) 109.5 no . . . C(63) C(66) H(95) 109.5 no . . . C(63) C(66) H(96) 109.5 no . . . H(94) C(66) H(95) 109.5 no . . . H(94) C(66) H(96) 109.5 no . . . H(95) C(66) H(96) 109.5 no . . . C(68) C(67) H(97) 109.5 no . . . C(68) C(67) H(98) 109.5 no . . . C(68) C(67) H(99) 109.5 no . . . H(97) C(67) H(98) 109.5 no . . . H(97) C(67) H(99) 109.5 no . . . H(98) C(67) H(99) 109.5 no . . . C(68) C(69) H(100) 119.4 no . . . C(70) C(69) H(100) 119.4 no . . . C(69) C(70) H(101) 123.1 no . . . C(71) C(70) H(101) 123.1 no . . . C(70) C(71) H(102) 116.9 no . . . C(72) C(71) H(102) 116.9 no . . . C(71) C(72) H(103) 120.7 no . . . C(73) C(72) H(103) 120.7 no . . . C(68) C(73) H(104) 121.0 no . . . C(72) C(73) H(104) 121.0 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Pt(1) O(3) C(13) 178.1(4) ? . . . . O(3) Pt(1) O(1) C(1) 179.3(4) ? . . . . O(1) Pt(1) N(1) C(7) 1.9(5) ? . . . . O(1) Pt(1) N(1) C(8) 177.7(5) ? . . . . N(1) Pt(1) O(1) C(1) 5.4(4) ? . . . . O(1) Pt(1) N(3) C(10) 131.6(10) ? . . . . O(1) Pt(1) N(3) C(11) -45.0(14) ? . . . . N(3) Pt(1) O(1) C(1) -134.5(10) ? . . . . O(3) Pt(1) N(1) C(7) -37.9(15) ? . . . . O(3) Pt(1) N(1) C(8) 137.9(10) ? . . . . N(1) Pt(1) O(3) C(13) -141.6(10) ? . . . . O(3) Pt(1) N(3) C(10) 177.2(5) ? . . . . O(3) Pt(1) N(3) C(11) 0.6(5) ? . . . . N(3) Pt(1) O(3) C(13) 5.0(5) ? . . . . N(1) Pt(1) N(3) C(10) -8.1(6) ? . . . . N(1) Pt(1) N(3) C(11) 175.4(5) ? . . . . N(3) Pt(1) N(1) C(7) 175.7(5) ? . . . . N(3) Pt(1) N(1) C(8) -8.5(5) ? . . . . O(4) Pt(2) O(5) C(34) 175.1(5) ? . . . . O(5) Pt(2) O(4) C(46) -178.8(5) ? . . . . O(4) Pt(2) N(2) C(40) 51.5(15) ? . . . . O(4) Pt(2) N(2) C(41) -126.2(11) ? . . . . N(2) Pt(2) O(4) C(46) 134.9(12) ? . . . . O(4) Pt(2) N(4) C(43) -177.3(4) ? . . . . O(4) Pt(2) N(4) C(44) -2.5(5) ? . . . . N(4) Pt(2) O(4) C(46) -5.0(5) ? . . . . O(5) Pt(2) N(2) C(40) 5.7(5) ? . . . . O(5) Pt(2) N(2) C(41) -172.0(4) ? . . . . N(2) Pt(2) O(5) C(34) -11.1(5) ? . . . . O(5) Pt(2) N(4) C(43) -135.0(10) ? . . . . O(5) Pt(2) N(4) C(44) 39.8(15) ? . . . . N(4) Pt(2) O(5) C(34) 132.4(11) ? . . . . N(2) Pt(2) N(4) C(43) 8.3(5) ? . . . . N(2) Pt(2) N(4) C(44) -176.9(5) ? . . . . N(4) Pt(2) N(2) C(40) -168.9(5) ? . . . . N(4) Pt(2) N(2) C(41) 13.4(5) ? . . . . Pt(1) O(1) C(1) C(2) 171.6(3) ? . . . . Pt(1) O(1) C(1) C(6) -9.9(7) ? . . . . Pt(1) O(3) C(13) C(12) -7.1(8) ? . . . . Pt(1) O(3) C(13) C(14) 172.8(3) ? . . . . Pt(2) O(4) C(46) C(45) 9.4(8) ? . . . . Pt(2) O(4) C(46) C(47) -170.9(3) ? . . . . Pt(2) O(5) C(34) C(35) -170.9(4) ? . . . . Pt(2) O(5) C(34) C(39) 9.4(8) ? . . . . Pt(1) N(1) C(7) C(6) -5.0(10) ? . . . . Pt(1) N(1) C(8) C(9) 48.7(8) ? . . . . C(7) N(1) C(8) C(9) -135.1(6) ? . . . . C(8) N(1) C(7) C(6) 179.0(6) ? . . . . Pt(2) N(2) C(40) C(39) 0.6(9) ? . . . . Pt(2) N(2) C(41) C(42) 8.1(8) ? . . . . C(40) N(2) C(41) C(42) -169.8(6) ? . . . . C(41) N(2) C(40) C(39) 178.5(6) ? . . . . Pt(1) N(3) C(10) C(9) -14.3(9) ? . . . . Pt(1) N(3) C(11) C(12) -4.3(10) ? . . . . C(10) N(3) C(11) C(12) 178.8(7) ? . . . . C(11) N(3) C(10) C(9) 162.6(7) ? . . . . Pt(2) N(4) C(43) C(42) -51.1(6) ? . . . . Pt(2) N(4) C(44) C(45) 5.9(10) ? . . . . C(43) N(4) C(44) C(45) -179.1(6) ? . . . . C(44) N(4) C(43) C(42) 133.7(6) ? . . . . O(1) C(1) C(2) C(3) 176.4(5) ? . . . . O(1) C(1) C(2) C(18) -6.1(8) ? . . . . O(1) C(1) C(6) C(5) -176.3(5) ? . . . . O(1) C(1) C(6) C(7) 6.5(8) ? . . . . C(2) C(1) C(6) C(5) 2.2(8) ? . . . . C(2) C(1) C(6) C(7) -174.9(5) ? . . . . C(6) C(1) C(2) C(3) -2.2(8) ? . . . . C(6) C(1) C(2) C(18) 175.3(5) ? . . . . C(1) C(2) C(3) C(4) 0.9(8) ? . . . . C(1) C(2) C(18) C(19) -57.8(6) ? . . . . C(1) C(2) C(18) C(20) 64.4(6) ? . . . . C(1) C(2) C(18) C(21) -176.3(5) ? . . . . C(3) C(2) C(18) C(19) 119.5(5) ? . . . . C(3) C(2) C(18) C(20) -118.2(5) ? . . . . C(3) C(2) C(18) C(21) 1.0(7) ? . . . . C(18) C(2) C(3) C(4) -176.5(5) ? . . . . C(2) C(3) C(4) C(5) 0.5(8) ? . . . . C(2) C(3) C(4) C(22) 177.4(5) ? . . . . C(3) C(4) C(5) C(6) -0.5(8) ? . . . . C(3) C(4) C(22) C(23) 56.9(6) ? . . . . C(3) C(4) C(22) C(24) -62.9(6) ? . . . . C(3) C(4) C(22) C(25) 177.6(5) ? . . . . C(5) C(4) C(22) C(23) -126.4(6) ? . . . . C(5) C(4) C(22) C(24) 113.7(6) ? . . . . C(5) C(4) C(22) C(25) -5.7(8) ? . . . . C(22) C(4) C(5) C(6) -177.3(5) ? . . . . C(4) C(5) C(6) C(1) -0.8(8) ? . . . . C(4) C(5) C(6) C(7) 176.5(5) ? . . . . C(1) C(6) C(7) N(1) 1.2(10) ? . . . . C(5) C(6) C(7) N(1) -176.0(6) ? . . . . N(1) C(8) C(9) C(10) -79.3(9) ? . . . . C(8) C(9) C(10) N(3) 60.0(10) ? . . . . N(3) C(11) C(12) C(13) 3.3(11) ? . . . . N(3) C(11) C(12) C(17) -176.5(6) ? . . . . C(11) C(12) C(13) O(3) 2.8(9) ? . . . . C(11) C(12) C(13) C(14) -177.1(5) ? . . . . C(11) C(12) C(17) C(16) 178.7(5) ? . . . . C(13) C(12) C(17) C(16) -1.1(9) ? . . . . C(17) C(12) C(13) O(3) -177.4(5) ? . . . . C(17) C(12) C(13) C(14) 2.7(8) ? . . . . O(3) C(13) C(14) C(15) 177.6(5) ? . . . . O(3) C(13) C(14) C(26) -2.2(8) ? . . . . C(12) C(13) C(14) C(15) -2.5(8) ? . . . . C(12) C(13) C(14) C(26) 177.7(5) ? . . . . C(13) C(14) C(15) C(16) 0.9(9) ? . . . . C(13) C(14) C(26) C(27) 61.9(6) ? . . . . C(13) C(14) C(26) C(28) -60.6(6) ? . . . . C(13) C(14) C(26) C(29) -179.3(5) ? . . . . C(15) C(14) C(26) C(27) -118.0(5) ? . . . . C(15) C(14) C(26) C(28) 119.6(5) ? . . . . C(15) C(14) C(26) C(29) 0.9(8) ? . . . . C(26) C(14) C(15) C(16) -179.3(5) ? . . . . C(14) C(15) C(16) C(17) 0.7(9) ? . . . . C(14) C(15) C(16) C(30) -177.5(5) ? . . . . C(15) C(16) C(17) C(12) -0.6(8) ? . . . . C(15) C(16) C(30) C(31) 62.9(8) ? . . . . C(15) C(16) C(30) C(32) -174.8(6) ? . . . . C(15) C(16) C(30) C(33) -53.6(8) ? . . . . C(17) C(16) C(30) C(31) -115.2(7) ? . . . . C(17) C(16) C(30) C(32) 7.1(9) ? . . . . C(17) C(16) C(30) C(33) 128.4(6) ? . . . . C(30) C(16) C(17) C(12) 177.5(5) ? . . . . O(5) C(34) C(35) C(36) -179.4(5) ? . . . . O(5) C(34) C(35) C(51) 0.1(6) ? . . . . O(5) C(34) C(39) C(38) 178.2(5) ? . . . . O(5) C(34) C(39) C(40) 0.4(8) ? . . . . C(35) C(34) C(39) C(38) -1.5(9) ? . . . . C(35) C(34) C(39) C(40) -179.3(5) ? . . . . C(39) C(34) C(35) C(36) 0.3(7) ? . . . . C(39) C(34) C(35) C(51) 179.8(4) ? . . . . C(34) C(35) C(36) C(37) 0.7(9) ? . . . . C(34) C(35) C(51) C(52) -58.3(7) ? . . . . C(34) C(35) C(51) C(53) -176.2(5) ? . . . . C(34) C(35) C(51) C(54) 63.9(7) ? . . . . C(36) C(35) C(51) C(52) 121.2(6) ? . . . . C(36) C(35) C(51) C(53) 3.3(8) ? . . . . C(36) C(35) C(51) C(54) -116.5(6) ? . . . . C(51) C(35) C(36) C(37) -178.9(6) ? . . . . C(35) C(36) C(37) C(38) -0.3(8) ? . . . . C(35) C(36) C(37) C(55) 178.2(6) ? . . . . C(36) C(37) C(38) C(39) -1.0(9) ? . . . . C(36) C(37) C(55) C(56) -179.4(7) ? . . . . C(36) C(37) C(55) C(57) -60.8(8) ? . . . . C(36) C(37) C(55) C(58) 56.9(9) ? . . . . C(38) C(37) C(55) C(56) -0.9(10) ? . . . . C(38) C(37) C(55) C(57) 117.7(7) ? . . . . C(38) C(37) C(55) C(58) -124.5(8) ? . . . . C(55) C(37) C(38) C(39) -179.5(6) ? . . . . C(37) C(38) C(39) C(34) 1.9(9) ? . . . . C(37) C(38) C(39) C(40) 179.9(4) ? . . . . C(34) C(39) C(40) N(2) -5.7(10) ? . . . . C(38) C(39) C(40) N(2) 176.4(6) ? . . . . N(2) C(41) C(42) C(43) -56.4(8) ? . . . . C(41) C(42) C(43) N(4) 80.2(7) ? . . . . N(4) C(44) C(45) C(46) -2.0(11) ? . . . . N(4) C(44) C(45) C(50) 177.4(6) ? . . . . C(44) C(45) C(46) O(4) -6.0(9) ? . . . . C(44) C(45) C(46) C(47) 174.3(5) ? . . . . C(44) C(45) C(50) C(49) -178.2(6) ? . . . . C(46) C(45) C(50) C(49) 1.2(10) ? . . . . C(50) C(45) C(46) O(4) 174.6(5) ? . . . . C(50) C(45) C(46) C(47) -5.1(9) ? . . . . O(4) C(46) C(47) C(48) -173.9(5) ? . . . . O(4) C(46) C(47) C(59) 6.4(8) ? . . . . C(45) C(46) C(47) C(48) 5.7(8) ? . . . . C(45) C(46) C(47) C(59) -173.9(5) ? . . . . C(46) C(47) C(48) C(49) -2.8(9) ? . . . . C(46) C(47) C(59) C(60) 55.4(7) ? . . . . C(46) C(47) C(59) C(61) -66.3(6) ? . . . . C(46) C(47) C(59) C(62) 173.7(5) ? . . . . C(48) C(47) C(59) C(60) -124.2(5) ? . . . . C(48) C(47) C(59) C(61) 114.1(6) ? . . . . C(48) C(47) C(59) C(62) -5.9(8) ? . . . . C(59) C(47) C(48) C(49) 176.8(5) ? . . . . C(47) C(48) C(49) C(50) -1.1(10) ? . . . . C(47) C(48) C(49) C(63) 177.2(6) ? . . . . C(48) C(49) C(50) C(45) 1.9(10) ? . . . . C(48) C(49) C(63) C(64) 49.9(8) ? . . . . C(48) C(49) C(63) C(65) -70.6(8) ? . . . . C(48) C(49) C(63) C(66) 170.6(6) ? . . . . C(50) C(49) C(63) C(64) -132.0(6) ? . . . . C(50) C(49) C(63) C(65) 107.5(7) ? . . . . C(50) C(49) C(63) C(66) -11.3(9) ? . . . . C(63) C(49) C(50) C(45) -176.3(6) ? . . . . C(67) C(68) C(69) C(70) 174.0(10) ? . . . . C(67) C(68) C(73) C(72) -179.3(9) ? . . . . C(69) C(68) C(73) C(72) 0.7(14) ? . . . . C(73) C(68) C(69) C(70) -6.0(16) ? . . . . C(68) C(69) C(70) C(71) 10.9(18) ? . . . . C(69) C(70) C(71) C(72) -12(2) ? . . . . C(70) C(71) C(72) C(73) 7(2) ? . . . . C(71) C(72) C(73) C(68) -1.0(17) ? . . . . C(75) C(74) C(77a) C(76) 0.5(17) ? . . . . C(77a) C(74) C(75) C(75a) -1(19) ? . . . . C(77a) C(74) C(75) C(76) -0.5(14) ? . . . . C(77a) C(74) C(75) C(79a) -179(2) ? . . . . C(77a) C(74) C(75) C(80) 179.6(16) ? . . . . C(75) C(74) C(79a) C(80) 2(2) ? . . . . C(79a) C(74) C(75) C(75a) 178(17) ? . . . . C(79a) C(74) C(75) C(76) 178(2) ? . . . . C(79a) C(74) C(75) C(77a) 179(2) ? . . . . C(79a) C(74) C(75) C(80) -1.5(19) ? . . . . C(77a) C(74) C(79a) C(75) 1(2) ? . . . . C(77a) C(74) C(79a) C(80) 3(3) ? . . . . C(79a) C(74) C(77a) C(75) -1.0(18) ? . . . . C(79a) C(74) C(77a) C(76) -0(2) ? . . . . C(74) C(75) C(75a) C(76) 0(20) ? . . . . C(74) C(75) C(75a) C(77) -2(18) ? . . . . C(74) C(75) C(75a) C(78) -177(42) ? . . . . C(74) C(75) C(75a) C(79) -180(19) ? . . . . C(74) C(75) C(75a) C(80) -180(20) ? . . . . C(74) C(75) C(76) C(75a) -180.0(18) ? . . . . C(74) C(75) C(76) C(77) -177.6(15) ? . . . . C(74) C(75) C(76) C(77a) 0.5(15) ? . . . . C(74) C(75) C(77a) C(76) -179.5(16) ? . . . . C(74) C(75) C(79a) C(80) -178.5(18) ? . . . . C(74) C(75) C(80) C(75a) 180.0(19) ? . . . . C(74) C(75) C(80) C(79) 180.0(15) ? . . . . C(74) C(75) C(80) C(79a) 1.5(19) ? . . . . C(75a) C(75) C(76) C(77) 2.4(16) ? . . . . C(75a) C(75) C(76) C(77a) -179.6(15) ? . . . . C(76) C(75) C(75a) C(77) -2.6(18) ? . . . . C(76) C(75) C(75a) C(78) -178(55) ? . . . . C(76) C(75) C(75a) C(79) 180(2) ? . . . . C(76) C(75) C(75a) C(80) -180.0(14) ? . . . . C(75a) C(75) C(77a) C(74) 179.9(17) ? . . . . C(75a) C(75) C(77a) C(76) 0.4(15) ? . . . . C(77a) C(75) C(75a) C(76) -0.4(14) ? . . . . C(77a) C(75) C(75a) C(77) -3(2) ? . . . . C(77a) C(75) C(75a) C(78) -178(55) ? . . . . C(77a) C(75) C(75a) C(79) 179.6(14) ? . . . . C(77a) C(75) C(75a) C(80) 179.6(15) ? . . . . C(75a) C(75) C(79a) C(74) -179.8(17) ? . . . . C(75a) C(75) C(79a) C(80) 2(2) ? . . . . C(79a) C(75) C(75a) C(76) 178(2) ? . . . . C(79a) C(75) C(75a) C(77) 176(2) ? . . . . C(79a) C(75) C(75a) C(78) 1(60) ? . . . . C(79a) C(75) C(75a) C(79) -2(3) ? . . . . C(79a) C(75) C(75a) C(80) -2(2) ? . . . . C(75a) C(75) C(80) C(79) 0.0(17) ? . . . . C(75a) C(75) C(80) C(79a) -178(2) ? . . . . C(80) C(75) C(75a) C(76) 180.0(14) ? . . . . C(80) C(75) C(75a) C(77) 177(2) ? . . . . C(80) C(75) C(75a) C(78) 2(55) ? . . . . C(80) C(75) C(75a) C(79) -0.0(16) ? . . . . C(76) C(75) C(77a) C(74) 179.5(16) ? . . . . C(77a) C(75) C(76) C(75a) 179.6(15) ? . . . . C(77a) C(75) C(76) C(77) -178(2) ? . . . . C(76) C(75) C(79a) C(74) -13(16) ? . . . . C(76) C(75) C(79a) C(80) 169(15) ? . . . . C(79a) C(75) C(76) C(75a) -168(16) ? . . . . C(79a) C(75) C(76) C(77) -166(15) ? . . . . C(79a) C(75) C(76) C(77a) 12(16) ? . . . . C(76) C(75) C(80) C(75a) 0.0(16) ? . . . . C(76) C(75) C(80) C(79) 0(2) ? . . . . C(76) C(75) C(80) C(79a) -178(2) ? . . . . C(80) C(75) C(76) C(75a) -0.0(16) ? . . . . C(80) C(75) C(76) C(77) 2(2) ? . . . . C(80) C(75) C(76) C(77a) -179.6(17) ? . . . . C(77a) C(75) C(79a) C(74) -1(2) ? . . . . C(77a) C(75) C(79a) C(80) -179.6(15) ? . . . . C(79a) C(75) C(77a) C(74) 1(2) ? . . . . C(79a) C(75) C(77a) C(76) -178(2) ? . . . . C(77a) C(75) C(80) C(75a) -160(120) ? . . . . C(77a) C(75) C(80) C(79) -160(120) ? . . . . C(77a) C(75) C(80) C(79a) 21(120) ? . . . . C(80) C(75) C(77a) C(74) -20(120) ? . . . . C(80) C(75) C(77a) C(76) 160(120) ? . . . . C(79a) C(75) C(80) C(75a) 178(2) ? . . . . C(79a) C(75) C(80) C(79) 178(2) ? . . . . C(80) C(75) C(79a) C(74) 178.5(18) ? . . . . C(75) C(75a) C(76) C(77) -177.5(17) ? . . . . C(75) C(75a) C(76) C(77a) 0.4(15) ? . . . . C(75) C(75a) C(77) C(76) 2.6(18) ? . . . . C(75) C(75a) C(77) C(78) -179.8(18) ? . . . . C(75) C(75a) C(78) C(77) 175(51) ? . . . . C(75) C(75a) C(78) C(79) -2(55) ? . . . . C(75) C(75a) C(79) C(78) 180(2) ? . . . . C(75) C(75a) C(79) C(80) 0.0(17) ? . . . . C(75) C(75a) C(80) C(79) -180.0(16) ? . . . . C(75) C(75a) C(80) C(79a) 1.4(17) ? . . . . C(76) C(75a) C(77) C(78) 177.6(17) ? . . . . C(77) C(75a) C(76) C(75) 177.5(17) ? . . . . C(77) C(75a) C(76) C(77a) 178(2) ? . . . . C(76) C(75a) C(78) C(77) -2.4(17) ? . . . . C(76) C(75a) C(78) C(79) 180(2) ? . . . . C(78) C(75a) C(76) C(75) 180(2) ? . . . . C(78) C(75a) C(76) C(77) 2.4(16) ? . . . . C(78) C(75a) C(76) C(77a) -179.6(14) ? . . . . C(76) C(75a) C(79) C(78) -0(33) ? . . . . C(76) C(75a) C(79) C(80) 180(34) ? . . . . C(79) C(75a) C(76) C(75) -180(34) ? . . . . C(79) C(75a) C(76) C(77) 3(28) ? . . . . C(79) C(75a) C(76) C(77a) -180(32) ? . . . . C(76) C(75a) C(80) C(75) -0.0(16) ? . . . . C(76) C(75a) C(80) C(79a) 1(2) ? . . . . C(80) C(75a) C(76) C(75) 0.0(16) ? . . . . C(80) C(75a) C(76) C(77) -177(2) ? . . . . C(80) C(75a) C(76) C(77a) 0(2) ? . . . . C(77) C(75a) C(78) C(79) -177.6(18) ? . . . . C(78) C(75a) C(77) C(76) -177.6(17) ? . . . . C(77) C(75a) C(79) C(78) 2.3(17) ? . . . . C(77) C(75a) C(79) C(80) -178(2) ? . . . . C(79) C(75a) C(77) C(76) -179.8(17) ? . . . . C(79) C(75a) C(77) C(78) -2.3(17) ? . . . . C(77) C(75a) C(80) C(75) -158(19) ? . . . . C(77) C(75a) C(80) C(79) 22(18) ? . . . . C(77) C(75a) C(80) C(79a) -157(18) ? . . . . C(80) C(75a) C(77) C(76) 160(19) ? . . . . C(80) C(75a) C(77) C(78) -23(18) ? . . . . C(78) C(75a) C(79) C(80) -179.9(14) ? . . . . C(79) C(75a) C(78) C(77) 177.6(18) ? . . . . C(78) C(75a) C(80) C(75) -179.9(19) ? . . . . C(78) C(75a) C(80) C(79) 0.1(13) ? . . . . C(78) C(75a) C(80) C(79a) -178.6(18) ? . . . . C(80) C(75a) C(78) C(77) 177(2) ? . . . . C(80) C(75a) C(78) C(79) -0.1(13) ? . . . . C(79) C(75a) C(80) C(75) 180.0(16) ? . . . . C(79) C(75a) C(80) C(79a) -179(2) ? . . . . C(80) C(75a) C(79) C(78) 179.9(14) ? . . . . C(75) C(76) C(77) C(75a) -2.3(15) ? . . . . C(75) C(76) C(77) C(78) -5(2) ? . . . . C(75) C(76) C(77a) C(74) -0.5(17) ? . . . . C(75a) C(76) C(77) C(78) -2.5(17) ? . . . . C(75a) C(76) C(77a) C(74) -1(2) ? . . . . C(75a) C(76) C(77a) C(75) -0.4(14) ? . . . . C(77) C(76) C(77a) C(74) 70(63) ? . . . . C(77) C(76) C(77a) C(75) 70(62) ? . . . . C(77a) C(76) C(77) C(75a) -72(62) ? . . . . C(77a) C(76) C(77) C(78) -74(62) ? . . . . C(75a) C(77) C(78) C(79) 2.6(19) ? . . . . C(76) C(77) C(78) C(75a) 2.4(17) ? . . . . C(76) C(77) C(78) C(79) 5(2) ? . . . . C(75a) C(78) C(79) C(80) 0.1(13) ? . . . . C(77) C(78) C(79) C(75a) -2.5(18) ? . . . . C(77) C(78) C(79) C(80) -2(2) ? . . . . C(75a) C(79) C(80) C(75) -0.0(15) ? . . . . C(75a) C(79) C(80) C(79a) 10(14) ? . . . . C(78) C(79) C(80) C(75) -0(2) ? . . . . C(78) C(79) C(80) C(75a) -0.1(14) ? . . . . C(78) C(79) C(80) C(79a) 9(15) ? . . . . C(74) C(79a) C(80) C(75) -2(2) ? . . . . C(74) C(79a) C(80) C(75a) -3(3) ? . . . . C(74) C(79a) C(80) C(79) -12(16) ? . . . . C(75) C(79a) C(80) C(75a) -1.3(17) ? . . . . C(75) C(79a) C(80) C(79) -10(14) ? . . . . #============================================================================== # 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 #============================================================================== # Attachment '- Ptsalpn.cif' #------------------------------------------------------------------------------ data_6 _database_code_depnum_ccdc_archive 'CCDC 801080' #TrackingRef '- Ptsalpn.cif' _audit_creation_date 'Sun Mar 7 00:31:16 2010' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C33 H48 N2 O2 Pt ' _chemical_formula_moiety 'C33 H48 N2 O2 Pt ' _chemical_formula_weight 699.84 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 27.469(7) _cell_length_b 11.691(4) _cell_length_c 9.564(3) _cell_angle_alpha 90 _cell_angle_beta 94.92(1) _cell_angle_gamma 90 _cell_volume 3060.1(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14235 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 133.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.010 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 4.597 _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 0.473 _exptl_absorpt_correction_T_max 0.955 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_ambient_temperature 133(2) _diffrn_reflns_number 15440 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.42 _diffrn_measured_fraction_theta_max 0.9980 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.9980 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. 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 3486 _reflns_number_gt 3313 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1465 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3486 _refine_ls_number_parameters 177 _refine_ls_goodness_of_fit_ref 1.855 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 4.28 _refine_diff_density_min -1.94 _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) ; 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) ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt(1) Pt 0.0000 0.02656(2) 0.2500 0.0232(1) Uani 1.00 2 d S . . O(1) O 0.0373(2) 0.1583(4) 0.3419(4) 0.0255(10) Uani 1.00 1 d . . . N(1) N 0.0369(2) -0.0858(5) 0.3701(6) 0.028(1) Uani 1.00 1 d . . . C(1) C 0.0774(2) 0.1544(5) 0.4308(6) 0.028(1) Uani 1.00 1 d . . . C(2) C 0.1050(2) 0.2531(5) 0.4578(6) 0.029(1) Uani 1.00 1 d . . . C(3) C 0.1437(2) 0.2477(6) 0.5609(6) 0.028(1) Uani 1.00 1 d . . . C(4) C 0.1570(2) 0.1487(6) 0.6395(6) 0.030(1) Uani 1.00 1 d . . . C(5) C 0.1295(2) 0.0520(6) 0.6090(7) 0.030(1) Uani 1.00 1 d . . . C(6) C 0.0911(3) 0.0513(6) 0.5036(8) 0.033(2) Uani 1.00 1 d . . . C(7) C 0.0698(2) -0.0583(6) 0.4747(6) 0.028(1) Uani 1.00 1 d . . . C(8) C 0.0282(3) -0.2121(7) 0.3590(9) 0.050(2) Uani 1.00 1 d . . . C(9) C 0.0181(6) -0.249(1) 0.232(2) 0.045(4) Uani 0.50 2 d P . . C(10) C 0.0938(2) 0.3634(5) 0.3750(6) 0.028(1) Uani 1.00 1 d . . . C(11) C 0.1319(3) 0.4580(6) 0.4099(9) 0.036(2) Uani 1.00 1 d . . . C(12) C 0.0437(2) 0.4102(6) 0.4103(6) 0.032(1) Uani 1.00 1 d . . . C(13) C 0.0926(2) 0.3392(6) 0.2161(7) 0.036(2) Uani 1.00 1 d . . . C(14) C 0.1998(2) 0.1541(6) 0.7570(6) 0.033(2) Uani 1.00 1 d . . . C(15) C 0.2446(2) 0.2052(8) 0.6975(9) 0.047(2) Uani 1.00 1 d . . . C(16) C 0.1854(3) 0.2289(10) 0.8769(8) 0.058(2) Uani 1.00 1 d . . . C(17) C 0.2139(4) 0.0367(8) 0.819(1) 0.054(3) Uani 1.00 1 d . . . H(1) H 0.1628 0.3153 0.5795 0.0343 Uiso 1.00 1 calc . . . H(2) H 0.1365 -0.0162 0.6610 0.0357 Uiso 1.00 1 calc . . . H(3) H 0.0801 -0.1186 0.5377 0.0323 Uiso 1.00 1 calc . . . H(4) H 0.0562 -0.2500 0.4022 0.0622 Uiso 1.00 1 calc . . . H(5) H 0.0009 -0.2295 0.4139 0.0622 Uiso 1.00 1 calc . . . H(6) H 0.1632 0.4337 0.3845 0.0436 Uiso 1.00 1 calc . . . H(7) H 0.1228 0.5256 0.3578 0.0436 Uiso 1.00 1 calc . . . H(8) H 0.1341 0.4750 0.5070 0.0436 Uiso 1.00 1 calc . . . H(9) H 0.0447 0.4288 0.5076 0.0375 Uiso 1.00 1 calc . . . H(10) H 0.0355 0.4766 0.3563 0.0375 Uiso 1.00 1 calc . . . H(11) H 0.0190 0.3534 0.3898 0.0375 Uiso 1.00 1 calc . . . H(12) H 0.0693 0.2805 0.1904 0.0433 Uiso 1.00 1 calc . . . H(13) H 0.0832 0.4069 0.1643 0.0433 Uiso 1.00 1 calc . . . H(14) H 0.1238 0.3155 0.1918 0.0433 Uiso 1.00 1 calc . . . H(15) H 0.2708 0.2125 0.7678 0.0568 Uiso 1.00 1 calc . . . H(16) H 0.2549 0.1563 0.6242 0.0568 Uiso 1.00 1 calc . . . H(17) H 0.2370 0.2783 0.6572 0.0568 Uiso 1.00 1 calc . . . H(18) H 0.2120 0.2384 0.9455 0.0705 Uiso 1.00 1 calc . . . H(19) H 0.1763 0.3043 0.8399 0.0705 Uiso 1.00 1 calc . . . H(20) H 0.1583 0.1981 0.9177 0.0705 Uiso 1.00 1 calc . . . H(21) H 0.1868 0.0037 0.8601 0.0632 Uiso 1.00 1 calc . . . H(22) H 0.2234 -0.0128 0.7468 0.0632 Uiso 1.00 1 calc . . . H(23) H 0.2405 0.0442 0.8891 0.0632 Uiso 1.00 1 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) 0.0251(2) 0.0163(2) 0.0282(2) 0.0000 0.0027(1) 0.0000 O(1) 0.026(2) 0.028(2) 0.019(2) 0.007(2) -0.014(1) -0.003(2) N(1) 0.023(2) 0.019(2) 0.041(3) -0.000(2) 0.002(2) 0.009(2) C(1) 0.032(3) 0.021(3) 0.032(3) -0.006(2) 0.004(2) 0.006(2) C(2) 0.033(3) 0.022(3) 0.034(3) -0.001(2) 0.016(2) 0.000(2) C(3) 0.028(3) 0.032(3) 0.025(3) -0.001(2) 0.000(2) -0.000(2) C(4) 0.025(2) 0.044(4) 0.020(2) 0.004(3) -0.009(2) 0.003(2) C(5) 0.034(3) 0.029(3) 0.025(3) 0.014(3) -0.001(2) 0.004(3) C(6) 0.034(3) 0.024(3) 0.041(4) 0.006(3) 0.012(3) 0.001(3) C(7) 0.031(3) 0.028(3) 0.022(3) 0.002(3) -0.006(2) 0.003(3) C(8) 0.047(4) 0.030(4) 0.066(5) -0.009(3) -0.044(4) 0.011(4) C(9) 0.070(10) 0.020(6) 0.041(8) 0.023(6) -0.013(7) -0.000(5) C(10) 0.029(3) 0.017(3) 0.039(3) -0.002(2) 0.009(2) -0.004(2) C(11) 0.036(4) 0.023(3) 0.050(4) -0.003(3) 0.009(3) 0.006(3) C(12) 0.032(3) 0.031(3) 0.032(3) -0.001(3) -0.000(2) 0.002(3) C(13) 0.043(3) 0.028(3) 0.037(3) 0.001(3) 0.007(3) 0.000(3) C(14) 0.021(2) 0.047(4) 0.028(3) 0.014(3) -0.011(2) -0.006(3) C(15) 0.029(3) 0.064(5) 0.049(4) 0.006(3) 0.004(3) 0.012(4) C(16) 0.039(4) 0.088(7) 0.045(4) 0.009(4) 0.001(3) -0.023(5) C(17) 0.053(5) 0.057(6) 0.047(5) 0.008(4) -0.021(4) 0.004(4) #------------------------------------------------------------------------------ _computing_data_collection . _computing_cell_refinement . _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR97 _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _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) 2.010(5) . . yes Pt(1) O(1) 2.010(5) . 2_555 yes Pt(1) N(1) 1.967(5) . . yes Pt(1) N(1) 1.967(5) . 2_555 yes O(1) C(1) 1.333(7) . . yes N(1) C(7) 1.330(8) . . yes N(1) C(8) 1.497(9) . . yes C(1) C(2) 1.393(9) . . yes C(1) C(6) 1.427(10) . . yes C(2) C(3) 1.389(9) . . yes C(2) C(10) 1.530(9) . . yes C(3) C(4) 1.411(9) . . yes C(4) C(5) 1.38(1) . . yes C(4) C(14) 1.556(8) . . yes C(5) C(6) 1.39(1) . . yes C(6) C(7) 1.43(1) . . yes C(8) C(9) 1.30(2) . . yes C(8) C(9) 1.54(1) . 2_555 yes C(9) C(9) 1.08(3) . 2_555 yes C(10) C(11) 1.540(9) . . yes C(10) C(12) 1.544(8) . . yes C(10) C(13) 1.544(9) . . yes C(14) C(15) 1.522(10) . . yes C(14) C(16) 1.521(10) . . yes C(14) C(17) 1.53(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(1) 79.9(2) . . 2_555 yes O(1) Pt(1) N(1) 92.2(2) . . . yes O(1) Pt(1) N(1) 169.9(2) . . 2_555 yes O(1) Pt(1) N(1) 169.9(2) 2_555 . . yes O(1) Pt(1) N(1) 92.2(2) 2_555 . 2_555 yes N(1) Pt(1) N(1) 96.2(3) . . 2_555 yes Pt(1) O(1) C(1) 127.9(4) . . . yes Pt(1) N(1) C(7) 124.1(5) . . . yes Pt(1) N(1) C(8) 123.1(4) . . . yes C(7) N(1) C(8) 112.7(5) . . . yes O(1) C(1) C(2) 119.8(6) . . . yes O(1) C(1) C(6) 120.7(6) . . . yes C(2) C(1) C(6) 119.5(6) . . . yes C(1) C(2) C(3) 117.8(6) . . . yes C(1) C(2) C(10) 121.4(5) . . . yes C(3) C(2) C(10) 120.8(6) . . . yes C(2) C(3) C(4) 124.3(6) . . . yes C(3) C(4) C(5) 116.6(5) . . . yes C(3) C(4) C(14) 119.7(6) . . . yes C(5) C(4) C(14) 123.6(6) . . . yes C(4) C(5) C(6) 121.7(6) . . . yes C(1) C(6) C(5) 120.0(7) . . . yes C(1) C(6) C(7) 125.2(7) . . . yes C(5) C(6) C(7) 114.8(6) . . . yes N(1) C(7) C(6) 127.3(6) . . . yes N(1) C(8) C(9) 114.5(9) . . . yes N(1) C(8) C(9) 115.8(7) . . 2_555 yes C(9) C(8) C(9) 43(1) . . 2_555 yes C(8) C(9) C(8) 122(1) . . 2_555 yes C(8) C(9) C(9) 80(1) . . 2_555 yes C(8) C(9) C(9) 56(1) 2_555 . 2_555 yes C(2) C(10) C(11) 113.0(5) . . . yes C(2) C(10) C(12) 109.2(5) . . . yes C(2) C(10) C(13) 109.9(5) . . . yes C(11) C(10) C(12) 107.5(5) . . . yes C(11) C(10) C(13) 107.6(5) . . . yes C(12) C(10) C(13) 109.6(5) . . . yes C(4) C(14) C(15) 109.4(5) . . . yes C(4) C(14) C(16) 109.8(5) . . . yes C(4) C(14) C(17) 113.3(7) . . . yes C(15) C(14) C(16) 109.0(7) . . . yes C(15) C(14) C(17) 108.1(7) . . . yes C(16) C(14) C(17) 107.2(7) . . . yes #-------------------------------------------------------------------------END