# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Walter Schuh' _publ_contact_author_email schuh.walter@net4you.at _publ_section_title ; Novel Access to Carbodiphosphoranes in the Coordination Sphere of Group 10 Metals: Template Synthesis and Protonation of PCP Pincer Carbodiphosphorane Complexes of C(dppm)2 ; _publ_author_name W.Schuh # Attachment 'dt-art-10-2011-011949-File002-v1-0.CIF' data_p166 _database_code_depnum_ccdc_archive 'CCDC 849136' #TrackingRef 'dt-art-10-2011-011949-File002-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H60 Cl2 Ni O4 P4' _chemical_formula_weight 1086.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 9.6018(2) _cell_length_b 23.6046(4) _cell_length_c 24.3824(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5526.19(17) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 19263 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15613 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4807 _reflns_number_gt 4328 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.2236P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(12) _refine_ls_number_reflns 4807 _refine_ls_number_parameters 319 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Ni1 Ni 0.5000 1.0000 0.668698(17) 0.03182(11) Uani 1 2 d S . . P1 P 0.62859(6) 0.92263(2) 0.66933(3) 0.03233(14) Uani 1 1 d . . . P2 P 0.54620(7) 0.93921(3) 0.78035(3) 0.03244(14) Uani 1 1 d . . . Cl1 Cl 0.5000 1.0000 0.57880(4) 0.0635(4) Uani 1 2 d S . . Cl2 Cl 1.0000 1.0000 0.76932(5) 0.0583(3) Uani 1 2 d S . . C1 C 0.5000 1.0000 0.74836(15) 0.0321(8) Uani 1 2 d S . . C2 C 0.6881(3) 0.91030(11) 0.73976(10) 0.0368(6) Uani 1 1 d . . . H2A H 0.7009 0.8698 0.7470 0.044 Uiso 1 1 calc . . . H2B H 0.7756 0.9303 0.7471 0.044 Uiso 1 1 calc . . . C101 C 0.5348(3) 0.85886(11) 0.64903(11) 0.0393(6) Uani 1 1 d . . . C102 C 0.4108(3) 0.86276(13) 0.62073(15) 0.0596(8) Uani 1 1 d . . . H102 H 0.3705 0.8985 0.6144 0.071 Uiso 1 1 calc . . . C103 C 0.3453(4) 0.81434(19) 0.60152(19) 0.0863(12) Uani 1 1 d . . . H103 H 0.2615 0.8173 0.5818 0.104 Uiso 1 1 calc . . . C104 C 0.4027(4) 0.76230(17) 0.61125(17) 0.0814(12) Uani 1 1 d . . . H104 H 0.3580 0.7296 0.5981 0.098 Uiso 1 1 calc . . . C105 C 0.5234(4) 0.75748(14) 0.63964(17) 0.0750(11) Uani 1 1 d . . . H105 H 0.5616 0.7215 0.6465 0.090 Uiso 1 1 calc . . . C106 C 0.5907(3) 0.80564(12) 0.65858(15) 0.0598(9) Uani 1 1 d . . . H106 H 0.6748 0.8022 0.6780 0.072 Uiso 1 1 calc . . . C107 C 0.7835(3) 0.91749(11) 0.62639(12) 0.0400(6) Uani 1 1 d . . . C108 C 0.9145(3) 0.93015(18) 0.64578(14) 0.0728(11) Uani 1 1 d . . . H108 H 0.9262 0.9420 0.6823 0.087 Uiso 1 1 calc . . . C109 C 1.0299(4) 0.9254(2) 0.61135(19) 0.0954(15) Uani 1 1 d . . . H109 H 1.1191 0.9341 0.6248 0.114 Uiso 1 1 calc . . . C110 C 1.0143(4) 0.90848(19) 0.55878(19) 0.0833(13) Uani 1 1 d . . . H110 H 1.0925 0.9054 0.5358 0.100 Uiso 1 1 calc . . . C111 C 0.8849(5) 0.89575(19) 0.53910(14) 0.0811(12) Uani 1 1 d . . . H111 H 0.8745 0.8839 0.5025 0.097 Uiso 1 1 calc . . . C112 C 0.7697(3) 0.90018(16) 0.57232(12) 0.0628(9) Uani 1 1 d . . . H112 H 0.6811 0.8914 0.5583 0.075 Uiso 1 1 calc . . . C201 C 0.4142(3) 0.88454(10) 0.77800(11) 0.0411(6) Uani 1 1 d . . . C202 C 0.2826(3) 0.89747(13) 0.75787(13) 0.0539(8) Uani 1 1 d . . . H202 H 0.2605 0.9349 0.7481 0.065 Uiso 1 1 calc . . . C203 C 0.1839(4) 0.85481(17) 0.75222(16) 0.0759(11) Uani 1 1 d . . . H203 H 0.0944 0.8633 0.7389 0.091 Uiso 1 1 calc . . . C204 C 0.2174(5) 0.80057(18) 0.76603(19) 0.0876(13) Uani 1 1 d . . . H204 H 0.1506 0.7718 0.7616 0.105 Uiso 1 1 calc . . . C205 C 0.3458(5) 0.78712(14) 0.78613(19) 0.0812(12) Uani 1 1 d . . . H205 H 0.3666 0.7494 0.7955 0.097 Uiso 1 1 calc . . . C206 C 0.4456(4) 0.82903(12) 0.79270(14) 0.0604(9) Uani 1 1 d . . . H206 H 0.5338 0.8200 0.8070 0.073 Uiso 1 1 calc . . . C207 C 0.6017(3) 0.94477(12) 0.85088(10) 0.0398(6) Uani 1 1 d . . . C208 C 0.7254(3) 0.97289(13) 0.86219(11) 0.0501(7) Uani 1 1 d . . . H208 H 0.7809 0.9870 0.8335 0.060 Uiso 1 1 calc . . . C209 C 0.7663(3) 0.97999(16) 0.91669(14) 0.0671(9) Uani 1 1 d . . . H209 H 0.8495 0.9993 0.9247 0.080 Uiso 1 1 calc . . . C210 C 0.6865(4) 0.95915(18) 0.95879(13) 0.0741(11) Uani 1 1 d . . . H210 H 0.7156 0.9638 0.9953 0.089 Uiso 1 1 calc . . . C211 C 0.5653(4) 0.93176(16) 0.94760(13) 0.0673(10) Uani 1 1 d . . . H211 H 0.5102 0.9181 0.9766 0.081 Uiso 1 1 calc . . . C212 C 0.5217(3) 0.92361(14) 0.89359(12) 0.0527(8) Uani 1 1 d . . . H212 H 0.4387 0.9039 0.8862 0.063 Uiso 1 1 calc . . . O1 O 0.3246(6) 0.66497(16) 0.84668(18) 0.1601(19) Uani 1 1 d . . . O2 O 0.4075(5) 0.6814(2) 0.92995(18) 0.1566(16) Uani 1 1 d . . . C4 C 0.5303(6) 0.6166(2) 0.8784(2) 0.1147(16) Uani 1 1 d . . . H4A H 0.5207 0.5932 0.8459 0.172 Uiso 1 1 calc R . . H4B H 0.5332 0.5926 0.9106 0.172 Uiso 1 1 calc R . . H4C H 0.6157 0.6384 0.8760 0.172 Uiso 1 1 calc R . . C3 C 0.4120(7) 0.6550(2) 0.8822(2) 0.1117(18) Uani 1 1 d . . . C5 C 0.2852(12) 0.7195(5) 0.9386(4) 0.214(4) Uani 1 1 d . . . H5A H 0.2428 0.7293 0.9033 0.257 Uiso 1 1 calc . . . H5B H 0.2150 0.7005 0.9613 0.257 Uiso 1 1 calc . . . C6 C 0.3340(13) 0.7690(5) 0.9652(5) 0.228(5) Uani 1 1 d . . . H6A H 0.2571 0.7950 0.9707 0.342 Uiso 1 1 calc . . . H6B H 0.4047 0.7870 0.9427 0.342 Uiso 1 1 calc . . . H6C H 0.3737 0.7589 1.0005 0.342 Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0416(2) 0.0328(2) 0.02111(19) 0.000 0.000 0.00412(17) P1 0.0357(3) 0.0356(3) 0.0257(3) -0.0009(3) 0.0021(3) 0.0032(2) P2 0.0373(3) 0.0349(3) 0.0251(3) 0.0027(3) 0.0021(3) 0.0022(3) Cl1 0.1074(10) 0.0623(8) 0.0207(5) 0.000 0.000 0.0257(6) Cl2 0.0393(5) 0.0854(8) 0.0502(6) 0.000 0.000 -0.0032(5) C1 0.040(2) 0.034(2) 0.0221(18) 0.000 0.000 0.0034(15) C2 0.0375(13) 0.0420(15) 0.0310(12) 0.0021(11) -0.0009(12) 0.0045(11) C101 0.0431(14) 0.0367(15) 0.0379(13) -0.0062(11) 0.0089(11) 0.0024(11) C102 0.0515(17) 0.0554(19) 0.072(2) -0.0124(17) -0.0073(17) -0.0013(14) C103 0.065(2) 0.084(3) 0.110(3) -0.031(2) -0.017(2) -0.018(2) C104 0.081(3) 0.065(2) 0.098(3) -0.034(2) 0.016(2) -0.027(2) C105 0.096(3) 0.0402(19) 0.088(3) -0.0103(17) 0.019(2) -0.0062(18) C106 0.0672(18) 0.0409(16) 0.071(2) -0.0027(16) -0.0015(17) 0.0037(14) C107 0.0434(14) 0.0404(14) 0.0363(13) 0.0005(12) 0.0089(13) 0.0017(11) C108 0.0468(19) 0.111(3) 0.060(2) -0.027(2) 0.0130(16) -0.0061(18) C109 0.044(2) 0.154(4) 0.088(3) -0.028(3) 0.024(2) -0.011(2) C110 0.074(3) 0.091(3) 0.084(3) -0.008(2) 0.048(2) -0.001(2) C111 0.093(3) 0.103(3) 0.047(2) -0.0103(19) 0.032(2) -0.003(3) C112 0.0578(19) 0.090(3) 0.0403(16) -0.0082(16) 0.0123(16) -0.0016(18) C201 0.0480(15) 0.0384(14) 0.0368(14) 0.0011(12) 0.0102(13) -0.0043(11) C202 0.0504(17) 0.0542(18) 0.0570(18) -0.0038(14) 0.0084(14) -0.0124(14) C203 0.060(2) 0.080(3) 0.087(3) -0.007(2) 0.0088(19) -0.0254(19) C204 0.093(3) 0.069(3) 0.100(3) -0.017(2) 0.035(3) -0.042(2) C205 0.116(3) 0.0387(18) 0.089(3) 0.0035(18) 0.036(3) -0.0122(19) C206 0.074(2) 0.0417(17) 0.066(2) 0.0070(15) 0.0188(18) -0.0012(15) C207 0.0478(16) 0.0459(15) 0.0256(13) 0.0042(11) 0.0003(11) 0.0155(12) C208 0.0424(15) 0.071(2) 0.0367(15) -0.0013(14) -0.0021(13) 0.0069(14) C209 0.0521(17) 0.106(3) 0.0432(16) -0.012(2) -0.0129(17) 0.0145(16) C210 0.074(2) 0.115(3) 0.0331(16) -0.0035(18) -0.0095(16) 0.037(2) C211 0.088(3) 0.081(2) 0.0330(17) 0.0104(16) 0.0131(18) 0.020(2) C212 0.0642(19) 0.063(2) 0.0312(15) 0.0055(14) 0.0092(14) 0.0065(14) O1 0.241(5) 0.104(3) 0.135(4) 0.037(2) -0.074(4) -0.046(3) O2 0.183(4) 0.185(4) 0.102(3) -0.040(3) -0.023(3) 0.046(4) C4 0.140(4) 0.114(4) 0.091(4) -0.014(3) 0.010(3) -0.009(3) C3 0.182(6) 0.086(3) 0.067(3) 0.014(2) -0.033(4) -0.045(4) C5 0.250(11) 0.201(9) 0.192(9) -0.057(7) 0.004(8) 0.080(8) C6 0.269(11) 0.185(10) 0.231(10) -0.046(8) 0.061(9) 0.034(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.942(4) . ? Ni1 Cl1 2.1919(10) . ? Ni1 P1 2.2046(6) 2_675 ? Ni1 P1 2.2046(6) . ? P1 C101 1.822(3) . ? P1 C107 1.823(3) . ? P1 C2 1.833(3) . ? P2 C1 1.6925(18) . ? P2 C207 1.805(2) . ? P2 C201 1.810(3) . ? P2 C2 1.817(3) . ? C1 P2 1.6925(18) 2_675 ? C101 C102 1.379(4) . ? C101 C106 1.386(4) . ? C102 C103 1.386(5) . ? C103 C104 1.367(6) . ? C104 C105 1.355(6) . ? C105 C106 1.387(5) . ? C107 C108 1.377(4) . ? C107 C112 1.387(4) . ? C108 C109 1.394(5) . ? C109 C110 1.351(6) . ? C110 C111 1.365(6) . ? C111 C112 1.375(5) . ? C201 C202 1.389(4) . ? C201 C206 1.391(4) . ? C202 C203 1.390(4) . ? C203 C204 1.362(6) . ? C204 C205 1.364(6) . ? C205 C206 1.387(5) . ? C207 C212 1.387(4) . ? C207 C208 1.389(4) . ? C208 C209 1.396(4) . ? C209 C210 1.372(5) . ? C210 C211 1.359(5) . ? C211 C212 1.395(5) . ? O1 C3 1.229(6) . ? O2 C3 1.321(6) . ? O2 C5 1.493(9) . ? C4 C3 1.457(7) . ? C5 C6 1.417(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 Cl1 180.000(1) . . ? C1 Ni1 P1 89.60(2) . 2_675 ? Cl1 Ni1 P1 90.40(2) . 2_675 ? C1 Ni1 P1 89.60(2) . . ? Cl1 Ni1 P1 90.40(2) . . ? P1 Ni1 P1 179.20(5) 2_675 . ? C101 P1 C107 101.09(12) . . ? C101 P1 C2 106.10(12) . . ? C107 P1 C2 105.84(12) . . ? C101 P1 Ni1 113.92(9) . . ? C107 P1 Ni1 120.54(9) . . ? C2 P1 Ni1 108.22(9) . . ? C1 P2 C207 117.05(14) . . ? C1 P2 C201 113.98(10) . . ? C207 P2 C201 106.79(13) . . ? C1 P2 C2 105.30(12) . . ? C207 P2 C2 108.95(12) . . ? C201 P2 C2 103.90(12) . . ? P2 C1 P2 125.1(2) 2_675 . ? P2 C1 Ni1 117.45(11) 2_675 . ? P2 C1 Ni1 117.45(11) . . ? P2 C2 P1 102.53(12) . . ? C102 C101 C106 118.6(3) . . ? C102 C101 P1 120.5(2) . . ? C106 C101 P1 120.8(2) . . ? C101 C102 C103 120.4(3) . . ? C104 C103 C102 120.0(4) . . ? C105 C104 C103 120.6(3) . . ? C104 C105 C106 120.0(3) . . ? C101 C106 C105 120.5(3) . . ? C108 C107 C112 118.5(3) . . ? C108 C107 P1 122.3(2) . . ? C112 C107 P1 119.2(2) . . ? C107 C108 C109 120.1(3) . . ? C110 C109 C108 120.5(4) . . ? C109 C110 C111 119.9(3) . . ? C110 C111 C112 120.6(3) . . ? C111 C112 C107 120.4(3) . . ? C202 C201 C206 119.7(3) . . ? C202 C201 P2 119.4(2) . . ? C206 C201 P2 120.7(2) . . ? C201 C202 C203 119.7(3) . . ? C204 C203 C202 119.7(4) . . ? C203 C204 C205 121.4(3) . . ? C204 C205 C206 120.0(3) . . ? C205 C206 C201 119.5(3) . . ? C212 C207 C208 119.8(2) . . ? C212 C207 P2 121.7(2) . . ? C208 C207 P2 118.5(2) . . ? C207 C208 C209 119.1(3) . . ? C210 C209 C208 120.8(3) . . ? C211 C210 C209 119.9(3) . . ? C210 C211 C212 120.8(3) . . ? C207 C212 C211 119.5(3) . . ? C3 O2 C5 115.7(6) . . ? O1 C3 O2 120.6(7) . . ? O1 C3 C4 127.3(5) . . ? O2 C3 C4 112.1(5) . . ? C6 C5 O2 107.5(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.253 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.037 # Attachment 'dt-art-10-2011-011949-File006-v1-0.CIF' data_1b _database_code_depnum_ccdc_archive 'CCDC 849137' #TrackingRef 'dt-art-10-2011-011949-File006-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H90 Cl8 Ni3 P8' _chemical_formula_weight 2035.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P31 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 17.4335(2) _cell_length_b 17.4335(2) _cell_length_c 31.0829(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8181.28(17) _cell_formula_units_Z 3 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 116640 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 23.0 _exptl_crystal_description prism _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37849 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 22.00 _reflns_number_total 13390 _reflns_number_gt 11955 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Several crystals were tested in the indexing procedure, because of low diffraction of visible reflections in the two theta range between 30 and 40 degrees. We suggest, that the crystals may lost solvent molecules CH2Cl2 over a period of time in the crystallisation process. In the refinement four positions were found with partial rest-electron densities for CH2Cl2 and the sum of occupation correspond approximately a complete solvent molecule in the asymmetric unit. Solvent molecules CH2Cl2 are partly occupied at four differnt positions with occupation factors of 0.45 (C7, Cl7-8), 0.25 (C8, Cl9-10), 0.15 (C9, Cl11-12) and 0.15 (C10, CL13-14), respectively. All solvent atoms were refined isotropically with bond restraints and hydrogen atoms were omitted. The anion NiCL4 is slightly disorered and one Cl-Position were refined with a 1:1 ratio (CL6:Cl6A). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+1.5001P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(15) _refine_ls_number_reflns 13390 _refine_ls_number_parameters 1129 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.000 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 Ni1 Ni 0.27775(5) 0.65609(5) 0.14821(3) 0.0480(2) Uani 1 1 d . . . Ni2 Ni 0.95120(5) 0.92106(5) 0.03635(3) 0.0491(2) Uani 1 1 d . . . Ni3 Ni 0.66202(13) 0.69316(13) 0.24776(7) 0.1496(9) Uani 1 1 d . . . Cl1 Cl 0.23437(13) 0.73646(13) 0.18430(6) 0.0639(5) Uani 1 1 d . . . Cl2 Cl 0.99761(13) 0.84374(13) -0.00053(6) 0.0662(5) Uani 1 1 d . . . Cl3 Cl 0.5205(3) 0.6079(3) 0.24501(15) 0.1524(15) Uani 1 1 d . . . Cl4 Cl 0.6935(3) 0.7762(3) 0.18680(14) 0.1492(15) Uani 1 1 d . . . Cl5 Cl 0.7206(7) 0.5987(8) 0.2420(5) 0.357(8) Uani 1 1 d . . . Cl6 Cl 0.6940(17) 0.7750(10) 0.3090(5) 0.290(12) Uani 0.50 1 d P . . Cl6A Cl 0.7650(7) 0.7828(13) 0.2868(3) 0.251(11) Uani 0.50 1 d P . . P1 P 0.14196(12) 0.55195(13) 0.13529(6) 0.0523(4) Uani 1 1 d . . . P2 P 0.25119(12) 0.47142(12) 0.13106(6) 0.0506(4) Uani 1 1 d . . . P3 P 0.41382(11) 0.63053(12) 0.09422(6) 0.0496(4) Uani 1 1 d . . . P4 P 0.40998(12) 0.77167(12) 0.14061(6) 0.0505(4) Uani 1 1 d . . . P5 P 1.08784(11) 1.02702(12) 0.04443(6) 0.0496(4) Uani 1 1 d . . . P6 P 0.98342(11) 1.07839(12) 0.09594(6) 0.0488(4) Uani 1 1 d . . . P7 P 0.80067(12) 0.95668(12) 0.06009(6) 0.0525(4) Uani 1 1 d . . . P8 P 0.81887(12) 0.80608(12) 0.04114(6) 0.0555(5) Uani 1 1 d . . . C1 C 0.3204(4) 0.5818(5) 0.1248(2) 0.0494(16) Uani 1 1 d . . . C2 C 0.1422(5) 0.4515(5) 0.1173(3) 0.0627(19) Uani 1 1 d . . . H2A H 0.0964 0.3990 0.1323 0.075 Uiso 1 1 calc . . . H2B H 0.1320 0.4430 0.0863 0.075 Uiso 1 1 calc . . . C3 C 0.4854(5) 0.7367(5) 0.1201(3) 0.0593(18) Uani 1 1 d . . . H3A H 0.5191 0.7300 0.1437 0.071 Uiso 1 1 calc . . . H3B H 0.5270 0.7797 0.0994 0.071 Uiso 1 1 calc . . . C4 C 0.9101(4) 0.9928(4) 0.0646(2) 0.0507(16) Uani 1 1 d . . . C5 C 1.0901(4) 1.1239(5) 0.0693(2) 0.0533(17) Uani 1 1 d . . . H5A H 1.1387 1.1523 0.0900 0.064 Uiso 1 1 calc . . . H5B H 1.0970 1.1674 0.0474 0.064 Uiso 1 1 calc . . . C6 C 0.7467(5) 0.8395(5) 0.0697(2) 0.0592(18) Uani 1 1 d . . . H6A H 0.6866 0.8092 0.0578 0.071 Uiso 1 1 calc . . . H6B H 0.7438 0.8266 0.1005 0.071 Uiso 1 1 calc . . . C101 C 0.0907(5) 0.5807(6) 0.0916(3) 0.064(2) Uani 1 1 d . . . C102 C 0.0615(6) 0.5346(7) 0.0552(3) 0.085(3) Uani 1 1 d . . . H102 H 0.0645 0.4826 0.0518 0.102 Uiso 1 1 calc . . . C103 C 0.0257(8) 0.5620(9) 0.0213(3) 0.109(4) Uani 1 1 d . . . H103 H 0.0072 0.5299 -0.0046 0.131 Uiso 1 1 calc . . . C104 C 0.0187(7) 0.6349(8) 0.0271(4) 0.100(4) Uani 1 1 d . . . H104 H -0.0081 0.6518 0.0058 0.120 Uiso 1 1 calc . . . C105 C 0.0498(8) 0.6840(7) 0.0632(4) 0.097(3) Uani 1 1 d . . . H105 H 0.0455 0.7352 0.0670 0.117 Uiso 1 1 calc . . . C106 C 0.0878(7) 0.6580(7) 0.0943(3) 0.091(3) Uani 1 1 d . . . H106 H 0.1130 0.6945 0.1185 0.109 Uiso 1 1 calc . . . C107 C 0.0640(5) 0.5162(5) 0.1784(2) 0.063(2) Uani 1 1 d . . . C108 C -0.0233(6) 0.4988(8) 0.1740(3) 0.091(3) Uani 1 1 d D . . H108 H -0.0465 0.5027 0.1473 0.109 Uiso 1 1 calc . . . C109 C -0.0748(8) 0.4750(11) 0.2123(5) 0.142(6) Uani 1 1 d D . . H109 H -0.1320 0.4677 0.2109 0.171 Uiso 1 1 calc . . . C110 C -0.0452(10) 0.4617(10) 0.2520(4) 0.136(5) Uani 1 1 d D . . H110 H -0.0833 0.4407 0.2759 0.163 Uiso 1 1 calc . . . C111 C 0.0400(11) 0.4801(11) 0.2551(4) 0.135(5) Uani 1 1 d D . . H111 H 0.0618 0.4725 0.2815 0.162 Uiso 1 1 calc . . . C112 C 0.0954(7) 0.5102(8) 0.2191(3) 0.098(3) Uani 1 1 d . . . H112 H 0.1553 0.5269 0.2222 0.117 Uiso 1 1 calc . . . C201 C 0.2724(5) 0.3981(5) 0.0986(3) 0.062(2) Uani 1 1 d . . . C202 C 0.2491(6) 0.3841(5) 0.0556(2) 0.065(2) Uani 1 1 d . . . H202 H 0.2198 0.4120 0.0437 0.077 Uiso 1 1 calc . . . C203 C 0.2665(7) 0.3319(6) 0.0299(3) 0.080(3) Uani 1 1 d . . . H203 H 0.2469 0.3210 0.0012 0.096 Uiso 1 1 calc . . . C204 C 0.3139(7) 0.2950(6) 0.0470(4) 0.086(3) Uani 1 1 d . . . H204 H 0.3287 0.2607 0.0293 0.104 Uiso 1 1 calc . . . C205 C 0.3392(6) 0.3072(6) 0.0883(4) 0.085(3) Uani 1 1 d . . . H205 H 0.3714 0.2814 0.0991 0.101 Uiso 1 1 calc . . . C206 C 0.3177(6) 0.3591(6) 0.1158(3) 0.073(2) Uani 1 1 d . . . H206 H 0.3339 0.3666 0.1450 0.087 Uiso 1 1 calc . . . C207 C 0.2411(5) 0.4301(5) 0.1851(2) 0.0594(19) Uani 1 1 d . . . C208 C 0.3036(7) 0.4803(6) 0.2160(3) 0.079(2) Uani 1 1 d . . . H208 H 0.3519 0.5362 0.2090 0.095 Uiso 1 1 calc . . . C209 C 0.2939(11) 0.4469(8) 0.2575(4) 0.133(6) Uani 1 1 d . . . H209 H 0.3377 0.4773 0.2785 0.159 Uiso 1 1 calc . . . C210 C 0.2159(11) 0.3652(9) 0.2675(4) 0.116(4) Uani 1 1 d . . . H210 H 0.2056 0.3468 0.2963 0.139 Uiso 1 1 calc . . . C211 C 0.1566(7) 0.3136(7) 0.2381(3) 0.084(3) Uani 1 1 d . . . H211 H 0.1093 0.2571 0.2450 0.101 Uiso 1 1 calc . . . C212 C 0.1691(6) 0.3487(5) 0.1964(3) 0.072(2) Uani 1 1 d . . . H212 H 0.1269 0.3157 0.1752 0.087 Uiso 1 1 calc . . . C301 C 0.4763(5) 0.5744(5) 0.0887(2) 0.0559(18) Uani 1 1 d . . . C302 C 0.4755(5) 0.5313(5) 0.0509(3) 0.064(2) Uani 1 1 d . . . H302 H 0.4412 0.5316 0.0277 0.077 Uiso 1 1 calc . . . C303 C 0.5217(7) 0.4894(6) 0.0464(4) 0.090(3) Uani 1 1 d . . . H303 H 0.5190 0.4597 0.0207 0.108 Uiso 1 1 calc . . . C304 C 0.5731(7) 0.4905(7) 0.0800(6) 0.118(5) Uani 1 1 d . . . H304 H 0.6090 0.4648 0.0764 0.142 Uiso 1 1 calc . . . C305 C 0.5737(7) 0.5307(8) 0.1216(4) 0.103(3) Uani 1 1 d . . . H305 H 0.6063 0.5288 0.1453 0.124 Uiso 1 1 calc . . . C306 C 0.5242(6) 0.5707(6) 0.1236(3) 0.082(3) Uani 1 1 d . . . H306 H 0.5221 0.5969 0.1497 0.098 Uiso 1 1 calc . . . C307 C 0.3963(5) 0.6548(5) 0.0400(2) 0.0545(17) Uani 1 1 d . . . C308 C 0.3118(6) 0.6211(7) 0.0244(3) 0.074(2) Uani 1 1 d . . . H308 H 0.2637 0.5890 0.0430 0.089 Uiso 1 1 calc . . . C309 C 0.2949(8) 0.6331(9) -0.0186(3) 0.101(3) Uani 1 1 d . . . H309 H 0.2365 0.6077 -0.0290 0.121 Uiso 1 1 calc . . . C310 C 0.3633(9) 0.6811(8) -0.0442(3) 0.094(3) Uani 1 1 d . . . H310 H 0.3528 0.6899 -0.0729 0.113 Uiso 1 1 calc . . . C311 C 0.4482(8) 0.7179(7) -0.0300(3) 0.097(3) Uani 1 1 d . . . H311 H 0.4952 0.7535 -0.0486 0.116 Uiso 1 1 calc . . . C312 C 0.4658(6) 0.7034(6) 0.0116(3) 0.078(2) Uani 1 1 d . . . H312 H 0.5247 0.7263 0.0207 0.094 Uiso 1 1 calc . . . C401 C 0.4658(5) 0.8395(5) 0.1870(2) 0.059(2) Uani 1 1 d . . . C402 C 0.4988(6) 0.8066(6) 0.2178(2) 0.072(2) Uani 1 1 d . . . H402 H 0.4925 0.7501 0.2147 0.086 Uiso 1 1 calc . . . C403 C 0.5420(7) 0.8591(8) 0.2539(3) 0.090(3) Uani 1 1 d . . . H403 H 0.5684 0.8387 0.2738 0.108 Uiso 1 1 calc . . . C404 C 0.5468(6) 0.9364(8) 0.2607(3) 0.083(3) Uani 1 1 d . . . H404 H 0.5745 0.9694 0.2856 0.100 Uiso 1 1 calc . . . C405 C 0.5095(6) 0.9686(7) 0.2301(3) 0.085(3) Uani 1 1 d . . . H405 H 0.5125 1.0233 0.2349 0.102 Uiso 1 1 calc . . . C406 C 0.4693(5) 0.9215(6) 0.1936(3) 0.069(2) Uani 1 1 d . . . H406 H 0.4446 0.9431 0.1734 0.082 Uiso 1 1 calc . . . C407 C 0.4111(5) 0.8461(4) 0.1000(2) 0.0540(17) Uani 1 1 d . . . C408 C 0.3325(7) 0.8285(6) 0.0802(3) 0.080(2) Uani 1 1 d . . . H408 H 0.2789 0.7783 0.0883 0.096 Uiso 1 1 calc . . . C409 C 0.3327(9) 0.8861(9) 0.0478(4) 0.104(3) Uani 1 1 d . . . H409 H 0.2797 0.8731 0.0339 0.124 Uiso 1 1 calc . . . C410 C 0.4086(10) 0.9590(7) 0.0371(3) 0.098(3) Uani 1 1 d . . . H410 H 0.4081 0.9979 0.0163 0.117 Uiso 1 1 calc . . . C411 C 0.4864(10) 0.9774(8) 0.0559(4) 0.115(4) Uani 1 1 d . . . H411 H 0.5393 1.0286 0.0480 0.138 Uiso 1 1 calc . . . C412 C 0.4878(6) 0.9204(6) 0.0872(3) 0.084(3) Uani 1 1 d . . . H412 H 0.5421 0.9330 0.0996 0.101 Uiso 1 1 calc . . . C501 C 1.1595(5) 1.0712(5) -0.0025(3) 0.065(2) Uani 1 1 d . . . C502 C 1.1515(7) 1.1320(6) -0.0286(3) 0.081(3) Uani 1 1 d . . . H502 H 1.1094 1.1485 -0.0214 0.097 Uiso 1 1 calc . . . C503 C 1.2044(9) 1.1693(7) -0.0653(4) 0.106(4) Uani 1 1 d . . . H503 H 1.2004 1.2119 -0.0822 0.127 Uiso 1 1 calc . . . C504 C 1.2618(11) 1.1401(11) -0.0749(4) 0.130(6) Uani 1 1 d . . . H504 H 1.2989 1.1646 -0.0990 0.156 Uiso 1 1 calc . . . C505 C 1.2686(9) 1.0785(11) -0.0520(5) 0.124(5) Uani 1 1 d . . . H505 H 1.3084 1.0597 -0.0606 0.148 Uiso 1 1 calc . . . C506 C 1.2154(7) 1.0417(7) -0.0147(3) 0.090(3) Uani 1 1 d . . . H506 H 1.2186 0.9976 0.0013 0.108 Uiso 1 1 calc . . . C507 C 1.1472(5) 0.9952(5) 0.0824(2) 0.0592(19) Uani 1 1 d . . . C508 C 1.1038(7) 0.9166(6) 0.1041(3) 0.083(3) Uani 1 1 d . . . H508 H 1.0430 0.8789 0.0990 0.099 Uiso 1 1 calc . . . C509 C 1.1430(10) 0.8926(8) 0.1312(4) 0.106(4) Uani 1 1 d . . . H509 H 1.1101 0.8401 0.1471 0.128 Uiso 1 1 calc . . . C510 C 1.2308(16) 0.9419(13) 0.1371(4) 0.135(6) Uani 1 1 d . . . H510 H 1.2585 0.9202 0.1555 0.162 Uiso 1 1 calc . . . C511 C 1.2837(9) 1.0250(11) 0.1171(5) 0.127(5) Uani 1 1 d . . . H511 H 1.3450 1.0594 0.1219 0.153 Uiso 1 1 calc . . . C512 C 1.2374(7) 1.0530(7) 0.0890(4) 0.089(3) Uani 1 1 d . . . H512 H 1.2669 1.1086 0.0754 0.107 Uiso 1 1 calc . . . C601 C 0.9605(4) 1.1690(5) 0.1021(2) 0.0536(18) Uani 1 1 d . . . C602 C 0.9613(5) 1.2150(5) 0.0669(2) 0.0573(18) Uani 1 1 d . . . H602 H 0.9773 1.2026 0.0400 0.069 Uiso 1 1 calc . . . C603 C 0.9384(6) 1.2806(5) 0.0703(3) 0.071(2) Uani 1 1 d . . . H603 H 0.9377 1.3110 0.0455 0.085 Uiso 1 1 calc . . . C604 C 0.9180(5) 1.3009(5) 0.1075(4) 0.076(2) Uani 1 1 d . . . H604 H 0.9038 1.3463 0.1090 0.091 Uiso 1 1 calc . . . C605 C 0.9169(6) 1.2553(6) 0.1452(3) 0.074(2) Uani 1 1 d . . . H605 H 0.9012 1.2692 0.1718 0.089 Uiso 1 1 calc . . . C606 C 0.9397(5) 1.1889(5) 0.1421(2) 0.0607(19) Uani 1 1 d . . . H606 H 0.9409 1.1584 0.1668 0.073 Uiso 1 1 calc . . . C607 C 0.9996(5) 1.0479(5) 0.1495(2) 0.0584(19) Uani 1 1 d . . . C608 C 0.9336(5) 0.9670(6) 0.1662(3) 0.071(2) Uani 1 1 d . . . H608 H 0.8853 0.9285 0.1489 0.085 Uiso 1 1 calc . . . C609 C 0.9393(7) 0.9437(9) 0.2078(3) 0.098(3) Uani 1 1 d . . . H609 H 0.8946 0.8894 0.2189 0.118 Uiso 1 1 calc . . . C610 C 1.0093(10) 0.9989(10) 0.2331(4) 0.104(4) Uani 1 1 d . . . H610 H 1.0113 0.9832 0.2618 0.125 Uiso 1 1 calc . . . C611 C 1.0766(10) 1.0771(9) 0.2172(4) 0.104(4) Uani 1 1 d . . . H611 H 1.1260 1.1132 0.2345 0.124 Uiso 1 1 calc . . . C612 C 1.0710(6) 1.1035(7) 0.1740(3) 0.079(2) Uani 1 1 d . . . H612 H 1.1155 1.1579 0.1630 0.095 Uiso 1 1 calc . . . C701 C 0.7535(4) 1.0044(5) 0.0963(3) 0.0556(18) Uani 1 1 d . . . C702 C 0.7414(5) 1.0732(5) 0.0819(3) 0.067(2) Uani 1 1 d . . . H702 H 0.7553 1.0930 0.0533 0.081 Uiso 1 1 calc . . . C703 C 0.7086(6) 1.1131(6) 0.1101(4) 0.083(3) Uani 1 1 d . . . H703 H 0.7016 1.1605 0.1008 0.099 Uiso 1 1 calc . . . C704 C 0.6866(5) 1.0809(6) 0.1521(4) 0.081(3) Uani 1 1 d . . . H704 H 0.6655 1.1071 0.1717 0.097 Uiso 1 1 calc . . . C705 C 0.6962(5) 1.0103(6) 0.1644(3) 0.077(2) Uani 1 1 d . . . H705 H 0.6782 0.9868 0.1922 0.092 Uiso 1 1 calc . . . C706 C 0.7301(5) 0.9741(5) 0.1383(3) 0.066(2) Uani 1 1 d . . . H706 H 0.7382 0.9278 0.1484 0.079 Uiso 1 1 calc . . . C707 C 0.7674(5) 0.9699(5) 0.0065(3) 0.067(2) Uani 1 1 d . . . C708 C 0.8297(7) 1.0249(7) -0.0228(3) 0.083(3) Uani 1 1 d . . . H708 H 0.8906 1.0523 -0.0167 0.100 Uiso 1 1 calc . . . C709 C 0.7996(10) 1.0384(10) -0.0613(4) 0.118(4) Uani 1 1 d . . . H709 H 0.8405 1.0799 -0.0808 0.142 Uiso 1 1 calc . . . C710 C 0.7150(14) 0.9950(15) -0.0718(4) 0.145(6) Uani 1 1 d . . . H710 H 0.6971 1.0027 -0.0992 0.174 Uiso 1 1 calc . . . C711 C 0.6539(9) 0.9395(9) -0.0433(5) 0.123(5) Uani 1 1 d . . . H711 H 0.5937 0.9089 -0.0510 0.148 Uiso 1 1 calc . . . C712 C 0.6780(6) 0.9282(6) -0.0055(4) 0.089(3) Uani 1 1 d . . . H712 H 0.6345 0.8912 0.0143 0.107 Uiso 1 1 calc . . . C801 C 0.7570(5) 0.7616(5) -0.0080(3) 0.068(2) Uani 1 1 d . . . C802 C 0.7935(7) 0.8069(8) -0.0463(3) 0.102(4) Uani 1 1 d . . . H802 H 0.8518 0.8549 -0.0471 0.123 Uiso 1 1 calc . . . C803 C 0.7403(9) 0.7787(12) -0.0839(4) 0.159(8) Uani 1 1 d . . . H803 H 0.7632 0.8089 -0.1100 0.190 Uiso 1 1 calc . . . C804 C 0.6545(9) 0.7068(10) -0.0826(4) 0.136(6) Uani 1 1 d . . . H804 H 0.6208 0.6859 -0.1079 0.163 Uiso 1 1 calc . . . C805 C 0.6205(7) 0.6676(9) -0.0446(4) 0.120(4) Uani 1 1 d . . . H805 H 0.5606 0.6233 -0.0432 0.144 Uiso 1 1 calc . . . C806 C 0.6731(7) 0.6913(6) -0.0064(3) 0.089(3) Uani 1 1 d . . . H806 H 0.6502 0.6591 0.0192 0.107 Uiso 1 1 calc . . . C807 C 0.8165(5) 0.7169(6) 0.0712(4) 0.084(3) Uani 1 1 d . . . C808 C 0.8168(9) 0.7179(8) 0.1159(5) 0.121(5) Uani 1 1 d D . . H808 H 0.8116 0.7622 0.1306 0.146 Uiso 1 1 calc . . . C809 C 0.8246(13) 0.6539(12) 0.1393(8) 0.216(13) Uani 1 1 d D . . H809 H 0.8346 0.6587 0.1691 0.259 Uiso 1 1 calc . . . C810 C 0.8164(12) 0.5813(15) 0.1152(9) 0.30(3) Uani 1 1 d D . . H810 H 0.8116 0.5325 0.1305 0.361 Uiso 1 1 calc . . . C811 C 0.8149(10) 0.5772(8) 0.0701(8) 0.159(8) Uani 1 1 d D . . H811 H 0.8143 0.5293 0.0560 0.191 Uiso 1 1 calc . . . C812 C 0.8144(8) 0.6454(7) 0.0463(5) 0.117(4) Uani 1 1 d . . . H812 H 0.8128 0.6448 0.0161 0.140 Uiso 1 1 calc . . . C7 C -0.288(2) 0.486(4) 0.3178(13) 0.21(2) Uiso 0.45 1 d PD . . Cl7 Cl -0.1840(9) 0.5050(9) 0.3261(4) 0.188(4) Uiso 0.45 1 d PD . . Cl8 Cl -0.3462(13) 0.4348(13) 0.3623(6) 0.231(6) Uiso 0.45 1 d PD . . C8 C -0.398(3) 0.291(4) 0.137(4) 0.22(4) Uiso 0.25 1 d PD . . Cl9 Cl -0.2958(19) 0.3136(18) 0.1553(9) 0.200(9) Uiso 0.25 1 d PD . . Cl10 Cl -0.463(3) 0.183(3) 0.1511(12) 0.255(14) Uiso 0.25 1 d PD . . C9 C 0.429(3) 0.297(3) 0.1860(19) 0.11(2) Uiso 0.15 1 d PD . . Cl11 Cl 0.3261(15) 0.2054(15) 0.1980(7) 0.115(6) Uiso 0.15 1 d PD . . Cl12 Cl 0.446(4) 0.352(4) 0.2331(18) 0.25(2) Uiso 0.15 1 d PD . . C10 C 0.547(5) 0.299(4) -0.012(2) 0.13(3) Uiso 0.15 1 d PD . . Cl13 Cl 0.479(3) 0.207(3) 0.0138(13) 0.185(13) Uiso 0.15 1 d PD . . Cl14 Cl 0.507(4) 0.298(4) -0.0616(17) 0.24(2) Uiso 0.15 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0416(5) 0.0503(5) 0.0441(5) -0.0023(4) -0.0020(4) 0.0171(4) Ni2 0.0429(5) 0.0439(5) 0.0507(5) -0.0013(4) 0.0023(4) 0.0143(4) Ni3 0.1179(13) 0.1234(13) 0.1544(16) 0.0514(12) -0.0484(12) 0.0206(11) Cl1 0.0619(11) 0.0722(12) 0.0593(11) -0.0075(9) -0.0026(8) 0.0348(10) Cl2 0.0648(11) 0.0591(11) 0.0676(12) -0.0092(9) 0.0058(9) 0.0256(9) Cl3 0.114(3) 0.141(3) 0.156(3) 0.001(3) -0.009(2) 0.029(2) Cl4 0.166(3) 0.127(3) 0.132(3) 0.056(2) 0.005(2) 0.056(3) Cl5 0.253(9) 0.350(13) 0.538(19) 0.239(13) 0.080(11) 0.203(9) Cl6 0.53(3) 0.201(12) 0.175(12) -0.088(10) -0.239(18) 0.205(17) Cl6A 0.126(6) 0.38(2) 0.092(6) 0.085(9) -0.019(5) 0.013(9) P1 0.0422(9) 0.0593(11) 0.0473(10) 0.0012(8) -0.0010(8) 0.0193(8) P2 0.0459(10) 0.0477(10) 0.0483(10) -0.0033(8) -0.0004(8) 0.0161(8) P3 0.0444(9) 0.0486(10) 0.0463(10) -0.0029(8) 0.0002(8) 0.0162(8) P4 0.0463(10) 0.0492(10) 0.0469(10) -0.0054(8) -0.0036(8) 0.0171(8) P5 0.0425(9) 0.0468(10) 0.0520(10) -0.0005(8) 0.0043(8) 0.0166(8) P6 0.0461(10) 0.0458(10) 0.0501(10) 0.0006(8) 0.0015(8) 0.0198(8) P7 0.0431(10) 0.0487(10) 0.0576(11) 0.0054(8) 0.0035(8) 0.0168(8) P8 0.0455(10) 0.0464(10) 0.0627(12) -0.0016(8) 0.0002(8) 0.0141(8) C1 0.046(4) 0.054(4) 0.043(4) -0.002(3) 0.002(3) 0.021(3) C2 0.054(4) 0.060(5) 0.061(5) -0.005(4) -0.001(4) 0.019(4) C3 0.048(4) 0.051(4) 0.067(5) -0.007(3) -0.003(3) 0.016(3) C4 0.045(4) 0.048(4) 0.057(4) 0.002(3) 0.006(3) 0.021(3) C5 0.041(4) 0.053(4) 0.059(4) 0.001(3) 0.007(3) 0.018(3) C6 0.041(4) 0.060(5) 0.060(4) 0.010(4) 0.007(3) 0.013(3) C101 0.046(4) 0.077(5) 0.055(5) 0.015(4) -0.001(3) 0.022(4) C102 0.078(6) 0.093(6) 0.060(6) 0.016(5) -0.016(4) 0.024(5) C103 0.108(8) 0.118(10) 0.074(7) 0.017(6) -0.028(6) 0.035(7) C104 0.094(7) 0.086(7) 0.087(7) 0.029(6) -0.026(6) 0.021(6) C105 0.094(7) 0.092(7) 0.106(8) -0.004(6) -0.031(6) 0.048(6) C106 0.097(7) 0.087(7) 0.092(7) -0.003(5) -0.039(6) 0.048(6) C107 0.072(5) 0.055(4) 0.052(5) 0.005(3) 0.012(4) 0.024(4) C108 0.053(5) 0.121(8) 0.085(6) -0.009(6) 0.021(5) 0.034(5) C109 0.073(7) 0.165(14) 0.172(15) -0.005(11) 0.037(9) 0.046(8) C110 0.134(12) 0.140(11) 0.092(9) 0.002(8) 0.058(9) 0.038(9) C111 0.169(14) 0.167(13) 0.084(8) 0.037(8) 0.065(9) 0.095(12) C112 0.094(7) 0.128(9) 0.077(7) 0.020(6) 0.014(5) 0.059(7) C201 0.060(4) 0.044(4) 0.071(5) -0.007(4) -0.003(4) 0.016(4) C202 0.087(6) 0.047(4) 0.052(5) -0.003(3) 0.012(4) 0.028(4) C203 0.095(7) 0.066(5) 0.057(5) 0.003(4) 0.021(5) 0.024(5) C204 0.073(6) 0.061(5) 0.085(7) -0.024(5) 0.028(5) 0.003(5) C205 0.066(5) 0.051(5) 0.130(9) -0.009(5) 0.009(5) 0.024(4) C206 0.071(5) 0.074(5) 0.069(5) -0.007(4) 0.007(4) 0.033(5) C207 0.077(5) 0.060(5) 0.049(4) -0.001(4) -0.001(4) 0.041(4) C208 0.097(6) 0.065(5) 0.054(5) -0.004(4) -0.013(4) 0.025(5) C209 0.203(14) 0.082(7) 0.088(8) -0.013(6) -0.090(9) 0.052(9) C210 0.197(14) 0.093(8) 0.075(7) 0.038(6) 0.035(8) 0.085(10) C211 0.097(7) 0.073(6) 0.073(6) 0.018(5) 0.009(5) 0.035(5) C212 0.066(5) 0.055(5) 0.075(6) 0.008(4) 0.012(4) 0.014(4) C301 0.045(4) 0.048(4) 0.062(4) -0.005(3) -0.002(3) 0.014(3) C302 0.062(5) 0.050(4) 0.074(5) 0.002(4) 0.017(4) 0.023(4) C303 0.073(6) 0.067(6) 0.118(8) -0.004(5) 0.023(6) 0.026(5) C304 0.060(6) 0.062(6) 0.233(17) -0.013(8) 0.028(8) 0.031(5) C305 0.086(7) 0.084(7) 0.136(10) -0.002(7) -0.019(6) 0.040(6) C306 0.074(5) 0.079(6) 0.107(7) -0.020(5) -0.022(5) 0.050(5) C307 0.052(4) 0.047(4) 0.049(4) -0.007(3) -0.002(3) 0.013(3) C308 0.075(6) 0.098(6) 0.047(5) 0.005(4) -0.002(4) 0.041(5) C309 0.111(8) 0.124(9) 0.069(7) 0.001(6) -0.025(6) 0.059(7) C310 0.121(9) 0.115(8) 0.044(5) 0.020(5) 0.011(6) 0.057(7) C311 0.107(9) 0.086(7) 0.076(7) 0.019(5) 0.024(6) 0.032(6) C312 0.071(5) 0.093(6) 0.044(4) 0.009(4) 0.006(4) 0.020(5) C401 0.042(4) 0.062(5) 0.053(5) -0.011(4) 0.004(3) 0.012(3) C402 0.079(5) 0.076(5) 0.044(4) 0.004(4) -0.001(4) 0.026(5) C403 0.078(6) 0.120(9) 0.051(5) -0.003(5) -0.008(4) 0.033(6) C404 0.068(5) 0.096(7) 0.062(6) -0.019(5) 0.011(4) 0.024(5) C405 0.063(5) 0.089(6) 0.090(7) -0.036(5) 0.014(5) 0.029(5) C406 0.067(5) 0.074(5) 0.062(5) -0.029(4) -0.009(4) 0.033(4) C407 0.064(5) 0.045(4) 0.046(4) -0.008(3) -0.008(3) 0.022(4) C408 0.091(6) 0.076(6) 0.066(5) 0.006(4) -0.008(5) 0.035(5) C409 0.117(9) 0.115(9) 0.085(7) 0.007(6) -0.030(6) 0.063(8) C410 0.134(10) 0.077(7) 0.075(7) 0.025(5) 0.020(7) 0.048(7) C411 0.137(11) 0.088(7) 0.082(7) 0.029(6) 0.005(7) 0.027(7) C412 0.083(6) 0.062(5) 0.086(6) 0.006(5) 0.001(5) 0.021(5) C501 0.054(4) 0.051(4) 0.057(5) -0.002(4) 0.007(4) 0.001(4) C502 0.094(6) 0.078(6) 0.043(5) -0.004(4) 0.005(4) 0.021(5) C503 0.113(9) 0.083(7) 0.071(7) 0.003(5) 0.000(6) 0.011(6) C504 0.122(11) 0.109(10) 0.085(9) -0.029(7) 0.048(8) 0.001(9) C505 0.101(9) 0.125(10) 0.128(11) -0.021(9) 0.053(8) 0.043(8) C506 0.094(7) 0.080(6) 0.088(7) -0.007(5) 0.032(6) 0.037(6) C507 0.058(5) 0.056(5) 0.059(5) -0.010(4) -0.003(4) 0.026(4) C508 0.110(7) 0.071(6) 0.063(5) 0.004(4) -0.012(5) 0.043(5) C509 0.131(10) 0.101(8) 0.087(8) -0.005(6) -0.039(7) 0.057(8) C510 0.25(2) 0.162(14) 0.076(7) -0.016(8) -0.038(10) 0.163(16) C511 0.111(9) 0.148(12) 0.157(12) -0.033(11) -0.052(9) 0.090(10) C512 0.078(6) 0.091(7) 0.103(7) -0.009(5) -0.029(5) 0.045(6) C601 0.036(4) 0.046(4) 0.071(5) -0.010(4) -0.005(3) 0.015(3) C602 0.060(4) 0.043(4) 0.066(5) 0.002(3) -0.004(4) 0.024(3) C603 0.063(5) 0.059(5) 0.084(6) 0.006(4) 0.006(4) 0.025(4) C604 0.059(5) 0.053(5) 0.116(8) -0.007(5) -0.005(5) 0.028(4) C605 0.066(5) 0.081(6) 0.080(6) -0.019(5) -0.002(4) 0.038(5) C606 0.062(5) 0.064(5) 0.055(5) -0.005(4) 0.004(4) 0.030(4) C607 0.071(5) 0.077(5) 0.043(4) 0.004(4) 0.010(4) 0.049(4) C608 0.065(5) 0.075(5) 0.069(6) 0.019(4) 0.004(4) 0.032(4) C609 0.086(7) 0.157(10) 0.072(6) 0.042(7) 0.014(6) 0.075(7) C610 0.127(10) 0.155(12) 0.074(7) 0.034(7) 0.014(7) 0.103(10) C611 0.145(10) 0.127(10) 0.071(6) -0.025(6) -0.040(7) 0.092(9) C612 0.082(6) 0.093(6) 0.059(5) -0.005(5) -0.017(4) 0.042(5) C701 0.033(3) 0.045(4) 0.077(5) 0.005(3) 0.004(3) 0.011(3) C702 0.037(4) 0.060(5) 0.092(6) -0.001(4) 0.005(4) 0.014(4) C703 0.052(5) 0.064(5) 0.128(9) -0.004(5) 0.011(5) 0.026(4) C704 0.048(5) 0.073(6) 0.112(8) -0.018(5) 0.007(5) 0.024(4) C705 0.047(4) 0.078(6) 0.081(6) 0.003(5) 0.017(4) 0.012(4) C706 0.051(4) 0.070(5) 0.067(5) -0.007(4) 0.006(4) 0.022(4) C707 0.066(5) 0.056(4) 0.076(6) 0.006(4) -0.016(4) 0.028(4) C708 0.086(6) 0.103(7) 0.062(5) 0.019(5) 0.008(5) 0.048(6) C709 0.121(10) 0.156(12) 0.079(7) 0.047(7) 0.003(7) 0.070(9) C710 0.192(17) 0.228(18) 0.079(8) 0.017(10) -0.032(10) 0.154(16) C711 0.104(8) 0.110(9) 0.117(10) 0.025(7) -0.046(8) 0.026(7) C712 0.073(6) 0.073(6) 0.104(8) 0.014(5) -0.022(5) 0.024(5) C801 0.057(5) 0.059(5) 0.063(5) -0.005(4) 0.006(4) 0.011(4) C802 0.067(6) 0.112(8) 0.075(6) 0.001(6) -0.005(5) 0.005(5) C803 0.102(9) 0.204(16) 0.064(7) 0.007(8) -0.006(6) -0.003(10) C804 0.097(9) 0.150(11) 0.075(7) -0.018(7) -0.023(6) -0.002(8) C805 0.070(6) 0.131(10) 0.112(9) -0.041(8) -0.004(6) 0.015(6) C806 0.080(6) 0.072(6) 0.077(6) -0.021(5) -0.001(5) 0.009(5) C807 0.043(4) 0.057(5) 0.131(9) 0.033(5) 0.000(5) 0.010(4) C808 0.120(9) 0.091(8) 0.127(11) 0.043(7) -0.024(8) 0.034(7) C809 0.137(14) 0.133(14) 0.30(3) 0.130(19) -0.051(16) 0.013(12) C810 0.087(11) 0.23(3) 0.59(7) 0.30(4) 0.13(2) 0.085(16) C811 0.100(10) 0.060(7) 0.31(3) 0.039(11) 0.053(14) 0.038(7) C812 0.087(7) 0.071(7) 0.193(14) 0.030(8) 0.040(8) 0.041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.930(7) . ? Ni1 P1 2.1826(19) . ? Ni1 P4 2.1875(19) . ? Ni1 Cl1 2.203(2) . ? Ni2 C4 1.934(7) . ? Ni2 P8 2.1767(19) . ? Ni2 P5 2.1793(19) . ? Ni2 Cl2 2.208(2) . ? Ni3 Cl6A 2.082(13) . ? Ni3 Cl3 2.153(4) . ? Ni3 Cl6 2.275(12) . ? Ni3 Cl4 2.279(4) . ? Ni3 Cl5 2.338(11) . ? Cl6 Cl6A 1.36(3) . ? P1 C107 1.784(8) . ? P1 C101 1.828(8) . ? P1 C2 1.840(8) . ? P2 C1 1.696(7) . ? P2 C207 1.802(7) . ? P2 C2 1.804(8) . ? P2 C201 1.806(8) . ? P3 C1 1.701(7) . ? P3 C307 1.800(8) . ? P3 C301 1.800(8) . ? P3 C3 1.823(7) . ? P4 C407 1.804(7) . ? P4 C401 1.810(7) . ? P4 C3 1.819(8) . ? P5 C501 1.822(8) . ? P5 C507 1.829(8) . ? P5 C5 1.839(7) . ? P6 C4 1.704(7) . ? P6 C607 1.811(7) . ? P6 C5 1.816(7) . ? P6 C601 1.823(7) . ? P7 C4 1.690(7) . ? P7 C6 1.796(8) . ? P7 C707 1.817(8) . ? P7 C701 1.823(8) . ? P8 C807 1.796(9) . ? P8 C801 1.805(8) . ? P8 C6 1.855(8) . ? C101 C102 1.333(13) . ? C101 C106 1.377(14) . ? C102 C103 1.422(15) . ? C103 C104 1.349(18) . ? C104 C105 1.350(16) . ? C105 C106 1.369(14) . ? C107 C112 1.402(14) . ? C107 C108 1.404(13) . ? C108 C109 1.422(14) . ? C109 C110 1.402(15) . ? C110 C111 1.357(15) . ? C111 C112 1.398(16) . ? C201 C202 1.382(11) . ? C201 C206 1.384(13) . ? C202 C203 1.356(13) . ? C203 C204 1.381(16) . ? C204 C205 1.338(15) . ? C205 C206 1.426(13) . ? C207 C208 1.387(12) . ? C207 C212 1.391(12) . ? C208 C209 1.389(15) . ? C209 C210 1.43(2) . ? C210 C211 1.334(17) . ? C211 C212 1.402(13) . ? C301 C306 1.390(12) . ? C301 C302 1.390(11) . ? C302 C303 1.338(14) . ? C303 C304 1.371(19) . ? C304 C305 1.468(19) . ? C305 C306 1.355(15) . ? C307 C308 1.372(12) . ? C307 C312 1.393(11) . ? C308 C309 1.407(13) . ? C309 C310 1.325(16) . ? C310 C311 1.359(16) . ? C311 C312 1.380(14) . ? C401 C402 1.380(12) . ? C401 C406 1.415(12) . ? C402 C403 1.405(13) . ? C403 C404 1.325(16) . ? C404 C405 1.418(16) . ? C405 C406 1.370(12) . ? C407 C412 1.376(12) . ? C407 C408 1.388(12) . ? C408 C409 1.422(14) . ? C409 C410 1.339(17) . ? C410 C411 1.360(18) . ? C411 C412 1.399(16) . ? C501 C506 1.363(13) . ? C501 C502 1.397(13) . ? C502 C503 1.405(15) . ? C503 C504 1.37(2) . ? C504 C505 1.34(2) . ? C505 C506 1.422(17) . ? C507 C508 1.366(12) . ? C507 C512 1.396(13) . ? C508 C509 1.280(15) . ? C509 C510 1.34(2) . ? C510 C511 1.41(2) . ? C511 C512 1.430(17) . ? C601 C602 1.352(11) . ? C601 C606 1.388(11) . ? C602 C603 1.391(12) . ? C603 C604 1.308(13) . ? C604 C605 1.411(14) . ? C605 C606 1.403(12) . ? C607 C612 1.366(12) . ? C607 C608 1.400(12) . ? C608 C609 1.374(13) . ? C609 C610 1.364(18) . ? C610 C611 1.370(19) . ? C611 C612 1.439(15) . ? C701 C702 1.391(11) . ? C701 C706 1.392(11) . ? C702 C703 1.405(13) . ? C703 C704 1.397(14) . ? C704 C705 1.377(14) . ? C705 C706 1.333(12) . ? C707 C708 1.373(13) . ? C707 C712 1.401(12) . ? C708 C709 1.374(15) . ? C709 C710 1.32(2) . ? C710 C711 1.35(2) . ? C711 C712 1.295(16) . ? C801 C806 1.361(12) . ? C801 C802 1.394(14) . ? C802 C803 1.420(16) . ? C803 C804 1.391(18) . ? C804 C805 1.344(18) . ? C805 C806 1.429(17) . ? C807 C808 1.391(18) . ? C807 C812 1.450(17) . ? C808 C809 1.394(15) . ? C809 C810 1.415(19) . ? C810 C811 1.402(18) . ? C811 C812 1.40(2) . ? C7 Cl8 1.68(3) . ? C7 Cl7 1.69(3) . ? C8 Cl10 1.70(3) . ? C8 Cl9 1.72(3) . ? C9 Cl12 1.70(3) . ? C9 Cl11 1.74(3) . ? C10 Cl13 1.65(3) . ? C10 Cl14 1.69(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 P1 89.7(2) . . ? C1 Ni1 P4 89.7(2) . . ? P1 Ni1 P4 162.08(8) . . ? C1 Ni1 Cl1 171.5(2) . . ? P1 Ni1 Cl1 92.77(8) . . ? P4 Ni1 Cl1 90.45(8) . . ? C4 Ni2 P8 90.0(2) . . ? C4 Ni2 P5 90.0(2) . . ? P8 Ni2 P5 168.15(8) . . ? C4 Ni2 Cl2 175.6(2) . . ? P8 Ni2 Cl2 90.95(8) . . ? P5 Ni2 Cl2 89.91(8) . . ? Cl6A Ni3 Cl3 143.3(4) . . ? Cl6A Ni3 Cl6 36.1(7) . . ? Cl3 Ni3 Cl6 107.7(7) . . ? Cl6A Ni3 Cl4 99.5(4) . . ? Cl3 Ni3 Cl4 103.56(18) . . ? Cl6 Ni3 Cl4 113.1(4) . . ? Cl6A Ni3 Cl5 93.3(7) . . ? Cl3 Ni3 Cl5 105.3(3) . . ? Cl6 Ni3 Cl5 116.7(6) . . ? Cl4 Ni3 Cl5 109.4(4) . . ? Cl6A Cl6 Ni3 64.2(8) . . ? Cl6 Cl6A Ni3 79.7(7) . . ? C107 P1 C101 105.3(4) . . ? C107 P1 C2 105.0(4) . . ? C101 P1 C2 105.6(4) . . ? C107 P1 Ni1 118.2(3) . . ? C101 P1 Ni1 112.6(3) . . ? C2 P1 Ni1 109.3(3) . . ? C1 P2 C207 115.6(3) . . ? C1 P2 C2 105.9(4) . . ? C207 P2 C2 105.1(4) . . ? C1 P2 C201 117.2(3) . . ? C207 P2 C201 104.6(4) . . ? C2 P2 C201 107.5(4) . . ? C1 P3 C307 114.0(3) . . ? C1 P3 C301 118.1(3) . . ? C307 P3 C301 105.0(4) . . ? C1 P3 C3 105.0(3) . . ? C307 P3 C3 106.6(3) . . ? C301 P3 C3 107.5(3) . . ? C407 P4 C401 106.2(3) . . ? C407 P4 C3 104.3(4) . . ? C401 P4 C3 104.8(3) . . ? C407 P4 Ni1 111.4(2) . . ? C401 P4 Ni1 119.4(2) . . ? C3 P4 Ni1 109.5(2) . . ? C501 P5 C507 105.8(4) . . ? C501 P5 C5 104.6(3) . . ? C507 P5 C5 104.6(3) . . ? C501 P5 Ni2 119.6(2) . . ? C507 P5 Ni2 111.2(3) . . ? C5 P5 Ni2 109.8(2) . . ? C4 P6 C607 115.3(4) . . ? C4 P6 C5 106.1(3) . . ? C607 P6 C5 105.8(3) . . ? C4 P6 C601 115.2(3) . . ? C607 P6 C601 107.0(3) . . ? C5 P6 C601 106.8(3) . . ? C4 P7 C6 105.2(3) . . ? C4 P7 C707 113.6(4) . . ? C6 P7 C707 106.1(4) . . ? C4 P7 C701 117.6(3) . . ? C6 P7 C701 108.5(3) . . ? C707 P7 C701 105.3(4) . . ? C807 P8 C801 108.5(5) . . ? C807 P8 C6 107.3(4) . . ? C801 P8 C6 100.7(4) . . ? C807 P8 Ni2 112.8(3) . . ? C801 P8 Ni2 117.9(3) . . ? C6 P8 Ni2 108.5(2) . . ? P2 C1 P3 126.3(4) . . ? P2 C1 Ni1 115.1(4) . . ? P3 C1 Ni1 118.0(4) . . ? P2 C2 P1 104.4(4) . . ? P4 C3 P3 104.6(4) . . ? P7 C4 P6 125.9(4) . . ? P7 C4 Ni2 115.8(4) . . ? P6 C4 Ni2 117.9(4) . . ? P6 C5 P5 104.1(3) . . ? P7 C6 P8 103.1(4) . . ? C102 C101 C106 116.9(8) . . ? C102 C101 P1 123.9(7) . . ? C106 C101 P1 119.0(7) . . ? C101 C102 C103 121.7(11) . . ? C104 C103 C102 118.6(11) . . ? C103 C104 C105 120.8(10) . . ? C104 C105 C106 118.9(11) . . ? C105 C106 C101 122.8(9) . . ? C112 C107 C108 119.6(8) . . ? C112 C107 P1 116.5(7) . . ? C108 C107 P1 123.8(7) . . ? C107 C108 C109 116.1(10) . . ? C110 C109 C108 123.7(11) . . ? C111 C110 C109 118.2(11) . . ? C110 C111 C112 120.1(12) . . ? C111 C112 C107 121.9(11) . . ? C202 C201 C206 118.5(7) . . ? C202 C201 P2 121.3(6) . . ? C206 C201 P2 120.0(6) . . ? C203 C202 C201 122.9(9) . . ? C202 C203 C204 118.2(9) . . ? C205 C204 C203 121.5(9) . . ? C204 C205 C206 120.4(9) . . ? C201 C206 C205 118.3(9) . . ? C208 C207 C212 119.5(7) . . ? C208 C207 P2 120.3(6) . . ? C212 C207 P2 120.1(6) . . ? C207 C208 C209 119.0(9) . . ? C208 C209 C210 118.4(9) . . ? C211 C210 C209 123.7(9) . . ? C210 C211 C212 116.0(9) . . ? C207 C212 C211 122.9(8) . . ? C306 C301 C302 118.5(8) . . ? C306 C301 P3 119.5(6) . . ? C302 C301 P3 122.0(6) . . ? C303 C302 C301 122.6(9) . . ? C302 C303 C304 118.6(10) . . ? C303 C304 C305 121.8(9) . . ? C306 C305 C304 115.5(11) . . ? C305 C306 C301 122.7(10) . . ? C308 C307 C312 117.1(7) . . ? C308 C307 P3 120.2(6) . . ? C312 C307 P3 122.6(6) . . ? C307 C308 C309 122.2(9) . . ? C310 C309 C308 118.3(10) . . ? C309 C310 C311 121.8(9) . . ? C310 C311 C312 120.4(9) . . ? C311 C312 C307 120.0(9) . . ? C402 C401 C406 120.2(7) . . ? C402 C401 P4 118.7(6) . . ? C406 C401 P4 120.8(6) . . ? C401 C402 C403 118.8(9) . . ? C404 C403 C402 122.1(10) . . ? C403 C404 C405 119.1(8) . . ? C406 C405 C404 121.2(9) . . ? C405 C406 C401 118.4(9) . . ? C412 C407 C408 117.9(8) . . ? C412 C407 P4 122.3(6) . . ? C408 C407 P4 119.8(6) . . ? C407 C408 C409 120.2(9) . . ? C410 C409 C408 119.9(10) . . ? C409 C410 C411 120.8(10) . . ? C410 C411 C412 120.1(10) . . ? C407 C412 C411 121.0(10) . . ? C506 C501 C502 119.1(8) . . ? C506 C501 P5 122.1(7) . . ? C502 C501 P5 118.6(7) . . ? C501 C502 C503 122.1(11) . . ? C504 C503 C502 116.0(12) . . ? C505 C504 C503 123.9(11) . . ? C504 C505 C506 119.6(12) . . ? C501 C506 C505 119.0(11) . . ? C508 C507 C512 120.7(8) . . ? C508 C507 P5 120.6(6) . . ? C512 C507 P5 118.7(7) . . ? C509 C508 C507 122.3(11) . . ? C508 C509 C510 120.3(12) . . ? C509 C510 C511 123.1(11) . . ? C510 C511 C512 115.4(12) . . ? C507 C512 C511 117.9(11) . . ? C602 C601 C606 120.2(7) . . ? C602 C601 P6 119.2(6) . . ? C606 C601 P6 120.6(6) . . ? C601 C602 C603 120.2(8) . . ? C604 C603 C602 121.2(9) . . ? C603 C604 C605 120.7(8) . . ? C606 C605 C604 118.6(8) . . ? C601 C606 C605 119.1(8) . . ? C612 C607 C608 120.4(7) . . ? C612 C607 P6 121.7(7) . . ? C608 C607 P6 117.8(6) . . ? C609 C608 C607 120.2(9) . . ? C610 C609 C608 120.4(10) . . ? C609 C610 C611 120.9(10) . . ? C610 C611 C612 119.5(10) . . ? C607 C612 C611 118.6(10) . . ? C702 C701 C706 119.3(7) . . ? C702 C701 P7 119.4(6) . . ? C706 C701 P7 121.3(6) . . ? C701 C702 C703 119.9(8) . . ? C704 C703 C702 118.8(9) . . ? C705 C704 C703 119.1(8) . . ? C706 C705 C704 122.4(9) . . ? C705 C706 C701 120.3(9) . . ? C708 C707 C712 118.2(8) . . ? C708 C707 P7 120.3(6) . . ? C712 C707 P7 121.4(7) . . ? C707 C708 C709 117.4(10) . . ? C710 C709 C708 122.0(12) . . ? C709 C710 C711 120.3(11) . . ? C712 C711 C710 120.3(12) . . ? C711 C712 C707 121.6(11) . . ? C806 C801 C802 121.5(8) . . ? C806 C801 P8 119.9(7) . . ? C802 C801 P8 118.2(6) . . ? C801 C802 C803 118.2(9) . . ? C804 C803 C802 120.6(11) . . ? C805 C804 C803 119.1(10) . . ? C804 C805 C806 121.8(10) . . ? C801 C806 C805 118.4(10) . . ? C808 C807 C812 122.7(10) . . ? C808 C807 P8 120.7(9) . . ? C812 C807 P8 116.6(9) . . ? C807 C808 C809 120.9(17) . . ? C808 C809 C810 115.7(19) . . ? C811 C810 C809 124.4(18) . . ? C810 C811 C812 119.4(16) . . ? C811 C812 C807 116.0(15) . . ? Cl8 C7 Cl7 106(2) . . ? Cl10 C8 Cl9 102(3) . . ? Cl12 C9 Cl11 98(3) . . ? Cl13 C10 Cl14 110(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.159 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.094 # Attachment 'dt-art-10-2011-011949-File007-v1-0.CIF' data_p147 _database_code_depnum_ccdc_archive 'CCDC 849139' #TrackingRef 'dt-art-10-2011-011949-File007-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57.75 H58.50 Cl2 O2.75 P4 Pt' _chemical_formula_weight 1186.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7629(2) _cell_length_b 23.2214(3) _cell_length_c 24.4318(4) _cell_angle_alpha 96.0590(10) _cell_angle_beta 94.7140(10) _cell_angle_gamma 92.4210(10) _cell_volume 5482.07(16) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 88031 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 2.815 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30900 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19002 _reflns_number_gt 15209 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Two molecules lie in the asymmetric unit. Highly disorder of solvent acetone and water, only one acetone molecule is well ordered and was refined anisotropically (O1-C7-C9). All other acetone have a 1:1 position disorder with partial overlying positions (C13=C13A, C16=C16A, C19=C19A). One acetone lies nearby a symmetry center (O5-C19-C21). The two water positions (O6 and O7) were refined with occupancy of 0.5. The disordered parts were refined isotropically and with bond restraints for the acetone molecules. No hydrogen atoms of solvent were found and their positions were not calculated. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+11.6007P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19002 _refine_ls_number_parameters 1202 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.70984(2) 0.316824(8) 0.215226(7) 0.03607(7) Uani 1 1 d . . . Pt2 Pt 0.75699(2) 0.173729(8) 0.707188(8) 0.04153(7) Uani 1 1 d . . . Cl1 Cl 0.7397(2) 0.33301(7) 0.31285(6) 0.0730(5) Uani 1 1 d . . . Cl2 Cl 0.7668(3) 0.18155(8) 0.80461(6) 0.1003(8) Uani 1 1 d . . . Cl3 Cl 0.18274(17) 0.29927(10) 0.09870(9) 0.0843(6) Uani 1 1 d . . . Cl4 Cl 0.23328(16) 0.16551(8) 0.59656(8) 0.0760(5) Uani 1 1 d . . . P1 P 0.56143(14) 0.23828(5) 0.21804(5) 0.0385(3) Uani 1 1 d . . . P2 P 0.63112(14) 0.23315(6) 0.10510(5) 0.0369(3) Uani 1 1 d . . . P3 P 0.72994(13) 0.35737(6) 0.09490(5) 0.0362(3) Uani 1 1 d . . . P4 P 0.85609(13) 0.39405(6) 0.20510(5) 0.0370(3) Uani 1 1 d . . . P5 P 0.61680(15) 0.09138(6) 0.69769(6) 0.0413(3) Uani 1 1 d . . . P6 P 0.68269(12) 0.10544(5) 0.58611(5) 0.0328(3) Uani 1 1 d . . . P7 P 0.78763(13) 0.23122(5) 0.59680(5) 0.0334(3) Uani 1 1 d . . . P8 P 0.90291(14) 0.25415(5) 0.70978(5) 0.0386(3) Uani 1 1 d . . . C1 C 0.6838(5) 0.3018(2) 0.13031(18) 0.0360(11) Uani 1 1 d . . . C2 C 0.4960(5) 0.2129(2) 0.1470(2) 0.0439(12) Uani 1 1 d . . . H2A H 0.4775 0.1708 0.1424 0.053 Uiso 1 1 calc . . . H2B H 0.4109 0.2316 0.1367 0.053 Uiso 1 1 calc . . . C3 C 0.8869(5) 0.3903(2) 0.1319(2) 0.0416(12) Uani 1 1 d . . . H3A H 0.9059 0.4292 0.1213 0.050 Uiso 1 1 calc . . . H3B H 0.9653 0.3666 0.1243 0.050 Uiso 1 1 calc . . . C4 C 0.7439(5) 0.1687(2) 0.62245(18) 0.0330(10) Uani 1 1 d . . . C5 C 0.5497(5) 0.0773(2) 0.6249(2) 0.0370(11) Uani 1 1 d . . . H5A H 0.5315 0.0356 0.6143 0.044 Uiso 1 1 calc . . . H5B H 0.4641 0.0970 0.6183 0.044 Uiso 1 1 calc . . . C6 C 0.9410(5) 0.2608(2) 0.6391(2) 0.0363(11) Uani 1 1 d . . . H6A H 0.9598 0.3015 0.6337 0.044 Uiso 1 1 calc . . . H6B H 1.0211 0.2388 0.6299 0.044 Uiso 1 1 calc . . . C101 C 0.4109(6) 0.2450(2) 0.2572(2) 0.0487(13) Uani 1 1 d . . . C102 C 0.4293(7) 0.2467(3) 0.3139(3) 0.0657(17) Uani 1 1 d . . . H102 H 0.5171 0.2428 0.3316 0.079 Uiso 1 1 calc . . . C103 C 0.3152(10) 0.2544(4) 0.3449(3) 0.090(3) Uani 1 1 d . . . H103 H 0.3277 0.2561 0.3836 0.109 Uiso 1 1 calc . . . C104 C 0.1877(10) 0.2593(4) 0.3201(4) 0.091(3) Uani 1 1 d . . . H104 H 0.1122 0.2640 0.3414 0.110 Uiso 1 1 calc . . . C105 C 0.1697(8) 0.2574(4) 0.2639(4) 0.091(3) Uani 1 1 d . . . H105 H 0.0813 0.2607 0.2464 0.110 Uiso 1 1 calc . . . C106 C 0.2815(7) 0.2507(3) 0.2322(3) 0.0727(19) Uani 1 1 d . . . H106 H 0.2685 0.2501 0.1936 0.087 Uiso 1 1 calc . . . C107 C 0.6465(6) 0.1767(2) 0.2434(2) 0.0449(13) Uani 1 1 d . . . C108 C 0.7810(7) 0.1826(3) 0.2656(3) 0.0584(16) Uani 1 1 d . . . H108 H 0.8279 0.2192 0.2684 0.070 Uiso 1 1 calc . . . C109 C 0.8490(9) 0.1363(3) 0.2837(3) 0.079(2) Uani 1 1 d . . . H109 H 0.9403 0.1417 0.2996 0.095 Uiso 1 1 calc . . . C110 C 0.7846(10) 0.0835(3) 0.2787(3) 0.081(2) Uani 1 1 d . . . H110 H 0.8316 0.0519 0.2905 0.097 Uiso 1 1 calc . . . C111 C 0.6519(10) 0.0754(3) 0.2566(3) 0.083(2) Uani 1 1 d . . . H111 H 0.6079 0.0382 0.2528 0.100 Uiso 1 1 calc . . . C112 C 0.5799(8) 0.1228(3) 0.2392(3) 0.0691(18) Uani 1 1 d . . . H112 H 0.4873 0.1175 0.2249 0.083 Uiso 1 1 calc . . . C201 C 0.5615(6) 0.2198(2) 0.0336(2) 0.0431(12) Uani 1 1 d . . . C202 C 0.6349(7) 0.1906(3) -0.0059(2) 0.0587(16) Uani 1 1 d . . . H202 H 0.7233 0.1782 0.0037 0.070 Uiso 1 1 calc . . . C203 C 0.5757(10) 0.1798(3) -0.0599(3) 0.079(2) Uani 1 1 d . . . H203 H 0.6249 0.1598 -0.0868 0.094 Uiso 1 1 calc . . . C204 C 0.4498(10) 0.1973(3) -0.0746(3) 0.084(2) Uani 1 1 d . . . H204 H 0.4113 0.1895 -0.1113 0.100 Uiso 1 1 calc . . . C205 C 0.3784(8) 0.2266(3) -0.0359(3) 0.078(2) Uani 1 1 d . . . H205 H 0.2901 0.2386 -0.0462 0.094 Uiso 1 1 calc . . . C206 C 0.4340(6) 0.2390(3) 0.0189(3) 0.0604(16) Uani 1 1 d . . . H206 H 0.3850 0.2601 0.0452 0.072 Uiso 1 1 calc . . . C207 C 0.7610(6) 0.1803(2) 0.1132(2) 0.0474(13) Uani 1 1 d . . . C208 C 0.8977(7) 0.1984(3) 0.1216(3) 0.0587(16) Uani 1 1 d . . . H208 H 0.9230 0.2381 0.1240 0.070 Uiso 1 1 calc . . . C209 C 0.9975(7) 0.1589(3) 0.1263(3) 0.082(2) Uani 1 1 d . . . H209 H 1.0909 0.1714 0.1321 0.098 Uiso 1 1 calc . . . C210 C 0.9596(10) 0.1003(4) 0.1226(3) 0.089(3) Uani 1 1 d . . . H210 H 1.0278 0.0732 0.1257 0.107 Uiso 1 1 calc . . . C211 C 0.8231(9) 0.0814(3) 0.1143(3) 0.082(2) Uani 1 1 d . . . H211 H 0.7978 0.0417 0.1120 0.098 Uiso 1 1 calc . . . C212 C 0.7239(7) 0.1215(3) 0.1095(3) 0.0615(16) Uani 1 1 d . . . H212 H 0.6305 0.1090 0.1037 0.074 Uiso 1 1 calc . . . C301 C 0.6138(5) 0.4157(2) 0.0950(2) 0.0423(12) Uani 1 1 d . . . C302 C 0.4851(6) 0.4089(3) 0.1140(3) 0.0564(15) Uani 1 1 d . . . H302 H 0.4571 0.3737 0.1265 0.068 Uiso 1 1 calc . . . C303 C 0.3974(7) 0.4548(3) 0.1146(3) 0.080(2) Uani 1 1 d . . . H303 H 0.3109 0.4506 0.1284 0.096 Uiso 1 1 calc . . . C304 C 0.4354(9) 0.5056(3) 0.0954(4) 0.083(2) Uani 1 1 d . . . H304 H 0.3745 0.5359 0.0956 0.099 Uiso 1 1 calc . . . C305 C 0.5619(9) 0.5127(3) 0.0759(4) 0.082(2) Uani 1 1 d . . . H305 H 0.5884 0.5481 0.0635 0.099 Uiso 1 1 calc . . . C306 C 0.6505(7) 0.4680(3) 0.0745(3) 0.0628(17) Uani 1 1 d . . . H306 H 0.7358 0.4725 0.0598 0.075 Uiso 1 1 calc . . . C307 C 0.7585(6) 0.3387(2) 0.0237(2) 0.0427(12) Uani 1 1 d . . . C308 C 0.8770(7) 0.3126(3) 0.0095(3) 0.0616(16) Uani 1 1 d . . . H308 H 0.9470 0.3070 0.0369 0.074 Uiso 1 1 calc . . . C309 C 0.8917(9) 0.2945(4) -0.0460(3) 0.086(2) Uani 1 1 d . . . H309 H 0.9717 0.2764 -0.0560 0.104 Uiso 1 1 calc . . . C310 C 0.7890(10) 0.3031(4) -0.0864(3) 0.088(2) Uani 1 1 d . . . H310 H 0.7992 0.2905 -0.1236 0.106 Uiso 1 1 calc . . . C311 C 0.6735(9) 0.3296(3) -0.0725(3) 0.075(2) Uani 1 1 d . . . H311 H 0.6050 0.3361 -0.1002 0.090 Uiso 1 1 calc . . . C312 C 0.6562(7) 0.3471(3) -0.0176(2) 0.0602(16) Uani 1 1 d . . . H312 H 0.5752 0.3647 -0.0081 0.072 Uiso 1 1 calc . . . C401 C 0.7822(5) 0.4634(2) 0.2220(2) 0.0442(12) Uani 1 1 d . . . C402 C 0.6708(6) 0.4665(3) 0.2535(3) 0.0617(17) Uani 1 1 d . . . H402 H 0.6308 0.4324 0.2641 0.074 Uiso 1 1 calc . . . C403 C 0.6175(8) 0.5194(3) 0.2695(4) 0.089(2) Uani 1 1 d . . . H403 H 0.5430 0.5210 0.2916 0.107 Uiso 1 1 calc . . . C404 C 0.6729(8) 0.5691(3) 0.2533(4) 0.081(2) Uani 1 1 d . . . H404 H 0.6366 0.6050 0.2642 0.098 Uiso 1 1 calc . . . C405 C 0.7798(9) 0.5666(3) 0.2218(4) 0.081(2) Uani 1 1 d . . . H405 H 0.8167 0.6008 0.2101 0.097 Uiso 1 1 calc . . . C406 C 0.8362(7) 0.5139(3) 0.2063(3) 0.0659(18) Uani 1 1 d . . . H406 H 0.9119 0.5130 0.1849 0.079 Uiso 1 1 calc . . . C407 C 1.0254(6) 0.4033(2) 0.2428(2) 0.0486(13) Uani 1 1 d . . . C408 C 1.0352(7) 0.4203(4) 0.2984(3) 0.077(2) Uani 1 1 d . . . H408 H 0.9550 0.4261 0.3166 0.092 Uiso 1 1 calc . . . C409 C 1.1657(9) 0.4292(4) 0.3283(3) 0.100(3) Uani 1 1 d . . . H409 H 1.1724 0.4415 0.3664 0.120 Uiso 1 1 calc . . . C410 C 1.2815(8) 0.4199(4) 0.3022(4) 0.092(3) Uani 1 1 d . . . H410 H 1.3681 0.4250 0.3224 0.110 Uiso 1 1 calc . . . C411 C 1.2730(7) 0.4035(4) 0.2477(4) 0.085(2) Uani 1 1 d . . . H411 H 1.3537 0.3979 0.2298 0.103 Uiso 1 1 calc . . . C412 C 1.1467(6) 0.3950(3) 0.2177(3) 0.0701(19) Uani 1 1 d . . . H412 H 1.1425 0.3833 0.1795 0.084 Uiso 1 1 calc . . . C501 C 0.4670(7) 0.0874(2) 0.7369(2) 0.0580(16) Uani 1 1 d . . . C502 C 0.4852(9) 0.0769(4) 0.7920(3) 0.090(3) Uani 1 1 d . . . H502 H 0.5734 0.0722 0.8090 0.109 Uiso 1 1 calc . . . C503 C 0.3686(13) 0.0735(4) 0.8216(3) 0.116(4) Uani 1 1 d . . . H503 H 0.3789 0.0655 0.8586 0.140 Uiso 1 1 calc . . . C504 C 0.2414(13) 0.0815(5) 0.7981(5) 0.134(5) Uani 1 1 d . . . H504 H 0.1651 0.0800 0.8191 0.161 Uiso 1 1 calc . . . C505 C 0.2236(9) 0.0914(5) 0.7453(5) 0.113(3) Uani 1 1 d . . . H505 H 0.1346 0.0960 0.7290 0.135 Uiso 1 1 calc . . . C506 C 0.3354(8) 0.0952(3) 0.7143(3) 0.082(2) Uani 1 1 d . . . H506 H 0.3217 0.1031 0.6773 0.098 Uiso 1 1 calc . . . C507 C 0.7108(6) 0.0286(2) 0.7140(2) 0.0454(13) Uani 1 1 d . . . C508 C 0.8288(8) 0.0360(3) 0.7491(3) 0.078(2) Uani 1 1 d . . . H508 H 0.8650 0.0738 0.7612 0.093 Uiso 1 1 calc . . . C509 C 0.8957(8) -0.0108(4) 0.7673(4) 0.097(3) Uani 1 1 d . . . H509 H 0.9736 -0.0047 0.7929 0.117 Uiso 1 1 calc . . . C510 C 0.8482(7) -0.0654(3) 0.7479(3) 0.074(2) Uani 1 1 d . . . H510 H 0.8941 -0.0973 0.7597 0.089 Uiso 1 1 calc . . . C511 C 0.7343(8) -0.0744(3) 0.7112(3) 0.077(2) Uani 1 1 d . . . H511 H 0.7017 -0.1123 0.6975 0.092 Uiso 1 1 calc . . . C512 C 0.6672(7) -0.0272(3) 0.6943(3) 0.0669(18) Uani 1 1 d . . . H512 H 0.5894 -0.0336 0.6687 0.080 Uiso 1 1 calc . . . C601 C 0.6114(5) 0.1116(2) 0.5163(2) 0.0391(12) Uani 1 1 d . . . C602 C 0.6790(6) 0.0905(3) 0.4716(2) 0.0557(15) Uani 1 1 d . . . H602 H 0.7578 0.0692 0.4771 0.067 Uiso 1 1 calc . . . C603 C 0.6308(8) 0.1007(4) 0.4183(3) 0.076(2) Uani 1 1 d . . . H603 H 0.6785 0.0871 0.3880 0.091 Uiso 1 1 calc . . . C604 C 0.5161(9) 0.1301(3) 0.4102(3) 0.077(2) Uani 1 1 d . . . H604 H 0.4834 0.1365 0.3742 0.092 Uiso 1 1 calc . . . C605 C 0.4464(7) 0.1507(3) 0.4544(3) 0.071(2) Uani 1 1 d . . . H605 H 0.3662 0.1710 0.4483 0.085 Uiso 1 1 calc . . . C606 C 0.4940(6) 0.1416(3) 0.5081(2) 0.0527(14) Uani 1 1 d . . . H606 H 0.4466 0.1558 0.5383 0.063 Uiso 1 1 calc . . . C607 C 0.8021(5) 0.0483(2) 0.5801(2) 0.0393(12) Uani 1 1 d . . . C608 C 0.9398(6) 0.0598(2) 0.5991(3) 0.0537(15) Uani 1 1 d . . . H608 H 0.9710 0.0974 0.6144 0.064 Uiso 1 1 calc . . . C609 C 1.0308(6) 0.0155(3) 0.5955(4) 0.078(2) Uani 1 1 d . . . H609 H 1.1238 0.0231 0.6084 0.093 Uiso 1 1 calc . . . C610 C 0.9858(8) -0.0387(3) 0.5734(4) 0.094(3) Uani 1 1 d . . . H610 H 1.0475 -0.0688 0.5725 0.113 Uiso 1 1 calc . . . C611 C 0.8501(7) -0.0505(3) 0.5520(4) 0.081(2) Uani 1 1 d . . . H611 H 0.8212 -0.0877 0.5348 0.097 Uiso 1 1 calc . . . C612 C 0.7587(6) -0.0074(3) 0.5561(3) 0.0599(16) Uani 1 1 d . . . H612 H 0.6661 -0.0154 0.5427 0.072 Uiso 1 1 calc . . . C701 C 0.6646(5) 0.2867(2) 0.6048(2) 0.0421(12) Uani 1 1 d . . . C702 C 0.5330(6) 0.2722(3) 0.6176(3) 0.0566(15) Uani 1 1 d . . . H702 H 0.5078 0.2337 0.6223 0.068 Uiso 1 1 calc . . . C703 C 0.4386(7) 0.3150(3) 0.6234(3) 0.081(2) Uani 1 1 d . . . H703 H 0.3489 0.3054 0.6320 0.097 Uiso 1 1 calc . . . C704 C 0.4766(9) 0.3713(3) 0.6167(4) 0.086(2) Uani 1 1 d . . . H704 H 0.4123 0.4002 0.6208 0.103 Uiso 1 1 calc . . . C705 C 0.6051(9) 0.3858(3) 0.6042(4) 0.083(2) Uani 1 1 d . . . H705 H 0.6297 0.4246 0.6002 0.099 Uiso 1 1 calc . . . C706 C 0.7002(7) 0.3439(3) 0.5974(3) 0.0615(17) Uani 1 1 d . . . H706 H 0.7886 0.3540 0.5877 0.074 Uiso 1 1 calc . . . C707 C 0.8261(5) 0.2274(2) 0.5257(2) 0.0388(11) Uani 1 1 d . . . C708 C 0.9464(6) 0.2014(3) 0.5102(2) 0.0540(14) Uani 1 1 d . . . H708 H 1.0051 0.1853 0.5362 0.065 Uiso 1 1 calc . . . C709 C 0.9770(7) 0.2000(3) 0.4556(3) 0.0714(19) Uani 1 1 d . . . H709 H 1.0570 0.1826 0.4446 0.086 Uiso 1 1 calc . . . C710 C 0.8917(9) 0.2238(4) 0.4174(3) 0.082(2) Uani 1 1 d . . . H710 H 0.9140 0.2230 0.3806 0.098 Uiso 1 1 calc . . . C711 C 0.7751(8) 0.2484(3) 0.4329(3) 0.0702(19) Uani 1 1 d . . . H711 H 0.7171 0.2645 0.4065 0.084 Uiso 1 1 calc . . . C712 C 0.7403(6) 0.2504(3) 0.4862(2) 0.0532(14) Uani 1 1 d . . . H712 H 0.6587 0.2673 0.4960 0.064 Uiso 1 1 calc . . . C801 C 0.8274(6) 0.3218(2) 0.7338(2) 0.0449(13) Uani 1 1 d . . . C802 C 0.7074(6) 0.3212(3) 0.7595(2) 0.0544(15) Uani 1 1 d . . . H802 H 0.6635 0.2854 0.7641 0.065 Uiso 1 1 calc . . . C803 C 0.6502(7) 0.3719(4) 0.7786(3) 0.075(2) Uani 1 1 d . . . H803 H 0.5691 0.3708 0.7967 0.090 Uiso 1 1 calc . . . C804 C 0.7127(9) 0.4240(3) 0.7709(3) 0.077(2) Uani 1 1 d . . . H804 H 0.6738 0.4586 0.7838 0.093 Uiso 1 1 calc . . . C805 C 0.8300(9) 0.4262(3) 0.7450(4) 0.083(2) Uani 1 1 d . . . H805 H 0.8714 0.4623 0.7396 0.099 Uiso 1 1 calc . . . C806 C 0.8894(7) 0.3748(3) 0.7262(3) 0.0682(18) Uani 1 1 d . . . H806 H 0.9712 0.3763 0.7085 0.082 Uiso 1 1 calc . . . C807 C 1.0698(6) 0.2590(2) 0.7498(2) 0.0509(14) Uani 1 1 d . . . C808 C 1.0811(8) 0.2807(3) 0.8053(3) 0.076(2) Uani 1 1 d . . . H808 H 1.0024 0.2918 0.8226 0.092 Uiso 1 1 calc . . . C809 C 1.2098(11) 0.2860(4) 0.8351(3) 0.093(3) Uani 1 1 d . . . H809 H 1.2173 0.3012 0.8725 0.112 Uiso 1 1 calc . . . C810 C 1.3252(9) 0.2694(4) 0.8110(4) 0.097(3) Uani 1 1 d . . . H810 H 1.4115 0.2729 0.8315 0.116 Uiso 1 1 calc . . . C811 C 1.3130(8) 0.2481(4) 0.7580(4) 0.101(3) Uani 1 1 d . . . H811 H 1.3923 0.2367 0.7413 0.121 Uiso 1 1 calc . . . C812 C 1.1857(7) 0.2420(3) 0.7262(3) 0.078(2) Uani 1 1 d . . . H812 H 1.1803 0.2263 0.6889 0.094 Uiso 1 1 calc . . . O1 O 1.423(2) 0.4674(6) 0.4372(6) 0.309(10) Uani 1 1 d . . . C7 C 1.524(3) 0.4384(11) 0.4380(8) 0.30(2) Uani 1 1 d . . . C8 C 1.645(3) 0.4665(15) 0.4297(15) 0.36(2) Uani 1 1 d . . . C9 C 1.517(2) 0.3813(7) 0.4454(7) 0.235(10) Uani 1 1 d . . . O2 O 0.876(3) -0.0680(12) 0.0683(12) 0.259(13) Uiso 0.50 1 d PD A 1 C10 C 0.958(5) -0.1128(16) 0.0648(14) 0.26(2) Uiso 0.50 1 d PD A 1 C11 C 0.965(3) -0.1496(12) 0.1044(12) 0.177(12) Uiso 0.50 1 d PD A 1 C12 C 0.953(4) -0.1384(15) 0.0123(12) 0.227(16) Uiso 0.50 1 d PD A 1 O3 O 1.345(2) 0.0709(10) 0.1014(9) 0.189(8) Uiso 0.50 1 d PD B 1 C13 C 1.347(4) 0.0346(13) 0.0549(11) 0.72(5) Uiso 0.50 1 d PD B 1 C14 C 1.267(4) -0.0141(12) 0.0598(16) 0.257(18) Uiso 0.50 1 d PD B 1 C15 C 1.346(5) 0.0585(19) 0.0079(11) 0.254(19) Uiso 0.50 1 d PD B 1 O4 O 1.105(2) 0.3626(8) 0.5587(10) 0.174(7) Uiso 0.50 1 d PD C 1 C16 C 1.056(5) 0.4084(17) 0.5454(10) 0.84(6) Uiso 0.50 1 d PD C 1 C17 C 0.994(4) 0.4042(16) 0.4958(11) 0.213(15) Uiso 0.50 1 d PD C 1 C18 C 1.022(4) 0.4458(13) 0.5923(13) 0.221(15) Uiso 0.50 1 d PD C 1 O5 O 0.0634(18) 0.4876(7) 0.0355(8) 0.068(5) Uiso 0.25 1 d PD . 1 C19 C -0.001(4) 0.5410(14) 0.0311(9) 0.27(2) Uiso 0.25 1 d PD . 1 C20 C -0.085(2) 0.5438(10) -0.0153(8) 0.052(6) Uiso 0.25 1 d PD . 1 C21 C -0.019(2) 0.5698(9) 0.0760(8) 0.048(5) Uiso 0.25 1 d PD D 1 O6 O -0.2521(16) 0.6368(7) 0.0132(6) 0.141(5) Uiso 0.50 1 d P E 1 O2A O 0.9454(15) -0.0513(6) 0.0951(6) 0.105(4) Uiso 0.50 1 d PD F 2 C10A C 1.024(2) -0.0834(10) 0.0764(11) 0.133(8) Uiso 0.50 1 d PD F 2 C11A C 1.154(3) -0.0669(17) 0.069(2) 0.31(2) Uiso 0.50 1 d PD F 2 C12A C 0.997(4) -0.1427(10) 0.0638(16) 0.183(12) Uiso 0.50 1 d PD F 2 O3A O 1.296(4) 0.0864(17) 0.040(2) 0.38(2) Uiso 0.50 1 d PD G 2 C13A C 1.347(4) 0.0346(13) 0.0549(11) 0.72(5) Uiso 0.50 1 d PD G 2 C14A C 1.445(7) 0.014(3) 0.023(2) 0.44(4) Uiso 0.50 1 d PD . 2 C15A C 1.378(5) 0.029(3) 0.1069(14) 0.30(3) Uiso 0.50 1 d PD G 2 O4A O 1.080(3) 0.3699(13) 0.4996(11) 0.271(13) Uiso 0.50 1 d PD H 2 C16A C 1.056(5) 0.4084(17) 0.5454(10) 0.84(6) Uiso 0.50 1 d PD H 2 C17A C 0.946(3) 0.4394(13) 0.5360(14) 0.190(12) Uiso 0.50 1 d PD H 2 C18A C 1.095(2) 0.3913(12) 0.5941(9) 0.137(8) Uiso 0.50 1 d PD H 2 O5A O 0.0542(19) 0.5309(8) 0.0806(7) 0.079(5) Uiso 0.25 1 d PD I 2 C19A C -0.001(4) 0.5410(14) 0.0311(9) 0.27(2) Uiso 0.25 1 d PD I 2 C20A C -0.100(3) 0.5796(11) 0.0273(11) 0.079(8) Uiso 0.25 1 d PD I 2 C21A C 0.0000 0.5000 0.0000 0.162(14) Uiso 0.50 2 d SPD . 2 O7 O 1.283(3) 0.2598(12) 0.5036(12) 0.265(12) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.05000(13) 0.03070(11) 0.02750(11) 0.00418(8) 0.00568(8) -0.00515(8) Pt2 0.05979(14) 0.03574(12) 0.02746(11) 0.00106(8) 0.00692(9) -0.01628(9) Cl1 0.1301(15) 0.0578(9) 0.0281(7) 0.0043(6) 0.0071(8) -0.0289(9) Cl2 0.190(2) 0.0737(12) 0.0296(8) -0.0022(7) 0.0149(10) -0.0681(13) Cl3 0.0485(9) 0.1130(15) 0.0908(14) 0.0000(11) 0.0098(9) 0.0175(9) Cl4 0.0418(8) 0.0844(12) 0.1013(14) 0.0012(10) 0.0124(8) 0.0097(8) P1 0.0507(8) 0.0310(7) 0.0343(7) 0.0066(5) 0.0070(6) -0.0057(6) P2 0.0449(7) 0.0343(7) 0.0309(7) 0.0017(5) 0.0027(6) 0.0013(6) P3 0.0420(7) 0.0382(7) 0.0295(7) 0.0081(5) 0.0049(5) 0.0001(6) P4 0.0412(7) 0.0351(7) 0.0346(7) 0.0053(5) 0.0031(6) -0.0050(6) P5 0.0522(8) 0.0355(7) 0.0358(7) 0.0015(6) 0.0115(6) -0.0131(6) P6 0.0320(6) 0.0346(7) 0.0307(6) -0.0017(5) 0.0042(5) 0.0003(5) P7 0.0362(7) 0.0332(7) 0.0317(7) 0.0065(5) 0.0043(5) 0.0005(5) P8 0.0496(8) 0.0319(7) 0.0327(7) 0.0043(5) 0.0008(6) -0.0108(6) C1 0.051(3) 0.034(3) 0.022(2) 0.002(2) -0.001(2) 0.000(2) C2 0.051(3) 0.039(3) 0.041(3) 0.005(2) 0.005(2) -0.004(2) C3 0.043(3) 0.045(3) 0.037(3) 0.008(2) 0.005(2) -0.006(2) C4 0.043(3) 0.036(3) 0.021(2) 0.0085(19) 0.006(2) -0.002(2) C5 0.035(3) 0.036(3) 0.039(3) -0.002(2) 0.008(2) -0.003(2) C6 0.039(3) 0.031(3) 0.038(3) 0.004(2) 0.003(2) -0.004(2) C101 0.061(4) 0.041(3) 0.045(3) 0.010(2) 0.014(3) -0.007(3) C102 0.073(4) 0.076(4) 0.051(4) 0.008(3) 0.021(3) 0.001(3) C103 0.118(7) 0.098(6) 0.062(5) 0.010(4) 0.050(5) 0.005(5) C104 0.092(6) 0.092(6) 0.100(7) 0.017(5) 0.061(5) -0.002(5) C105 0.061(5) 0.108(7) 0.110(7) 0.021(5) 0.032(5) 0.000(4) C106 0.061(4) 0.094(5) 0.066(5) 0.015(4) 0.018(3) -0.003(4) C107 0.065(4) 0.037(3) 0.036(3) 0.012(2) 0.016(3) 0.004(3) C108 0.073(4) 0.052(4) 0.051(4) 0.003(3) 0.008(3) 0.011(3) C109 0.104(6) 0.062(5) 0.073(5) 0.004(4) 0.003(4) 0.033(4) C110 0.121(7) 0.066(5) 0.062(5) 0.013(4) 0.022(5) 0.038(5) C111 0.141(8) 0.038(4) 0.075(5) 0.014(3) 0.032(5) -0.007(4) C112 0.092(5) 0.043(4) 0.073(5) 0.017(3) 0.009(4) -0.011(3) C201 0.055(3) 0.040(3) 0.031(3) -0.002(2) -0.003(2) -0.007(2) C202 0.077(4) 0.056(4) 0.041(3) -0.004(3) 0.002(3) 0.007(3) C203 0.134(7) 0.060(4) 0.038(4) -0.005(3) 0.001(4) 0.001(4) C204 0.129(7) 0.071(5) 0.044(4) 0.008(4) -0.026(4) -0.014(5) C205 0.083(5) 0.090(5) 0.056(4) 0.017(4) -0.030(4) -0.008(4) C206 0.060(4) 0.068(4) 0.053(4) 0.009(3) 0.003(3) 0.004(3) C207 0.059(4) 0.044(3) 0.039(3) 0.004(2) 0.000(3) 0.009(3) C208 0.063(4) 0.057(4) 0.054(4) 0.000(3) -0.003(3) 0.014(3) C209 0.062(4) 0.075(5) 0.105(6) -0.001(4) -0.015(4) 0.021(4) C210 0.106(7) 0.076(5) 0.086(6) 0.009(4) -0.004(5) 0.046(5) C211 0.111(6) 0.046(4) 0.092(6) 0.010(4) 0.018(5) 0.020(4) C212 0.076(4) 0.041(3) 0.066(4) 0.002(3) 0.005(3) 0.007(3) C301 0.049(3) 0.040(3) 0.038(3) 0.006(2) 0.001(2) 0.000(2) C302 0.057(4) 0.052(4) 0.064(4) 0.016(3) 0.011(3) 0.011(3) C303 0.068(4) 0.080(5) 0.097(6) 0.015(4) 0.018(4) 0.023(4) C304 0.088(6) 0.055(4) 0.107(6) 0.018(4) 0.001(5) 0.026(4) C305 0.097(6) 0.045(4) 0.106(6) 0.026(4) -0.011(5) 0.011(4) C306 0.067(4) 0.047(4) 0.078(5) 0.022(3) 0.006(3) -0.002(3) C307 0.053(3) 0.046(3) 0.030(3) 0.005(2) 0.009(2) -0.006(2) C308 0.063(4) 0.073(4) 0.048(4) 0.001(3) 0.012(3) -0.003(3) C309 0.090(5) 0.109(6) 0.062(5) -0.008(4) 0.042(4) -0.002(5) C310 0.116(7) 0.105(6) 0.038(4) -0.013(4) 0.020(4) -0.024(5) C311 0.104(6) 0.083(5) 0.034(3) 0.005(3) 0.001(4) -0.014(4) C312 0.077(4) 0.066(4) 0.038(3) 0.011(3) 0.004(3) -0.005(3) C401 0.046(3) 0.037(3) 0.046(3) 0.000(2) -0.001(2) -0.009(2) C402 0.061(4) 0.041(3) 0.083(5) -0.002(3) 0.017(3) 0.000(3) C403 0.081(5) 0.059(5) 0.127(7) -0.010(4) 0.029(5) 0.010(4) C404 0.074(5) 0.052(4) 0.113(7) -0.010(4) -0.007(5) 0.019(4) C405 0.104(6) 0.038(4) 0.097(6) 0.015(4) -0.014(5) -0.016(4) C406 0.081(5) 0.038(3) 0.078(5) 0.006(3) 0.009(4) -0.013(3) C407 0.055(3) 0.047(3) 0.042(3) 0.006(2) -0.007(3) -0.001(3) C408 0.064(4) 0.113(6) 0.049(4) 0.005(4) -0.009(3) -0.012(4) C409 0.088(6) 0.151(9) 0.056(5) 0.022(5) -0.023(4) -0.028(6) C410 0.057(5) 0.124(7) 0.091(6) 0.024(5) -0.023(4) -0.020(4) C411 0.044(4) 0.119(7) 0.091(6) 0.014(5) -0.006(4) -0.006(4) C412 0.045(4) 0.101(5) 0.062(4) 0.002(4) 0.001(3) -0.002(3) C501 0.081(5) 0.047(3) 0.046(3) -0.008(3) 0.032(3) -0.026(3) C502 0.118(6) 0.099(6) 0.047(4) -0.018(4) 0.026(4) -0.059(5) C503 0.166(10) 0.128(8) 0.050(5) -0.021(5) 0.062(6) -0.075(8) C504 0.141(9) 0.126(8) 0.128(10) -0.053(7) 0.093(8) -0.074(8) C505 0.083(6) 0.140(9) 0.118(8) -0.006(6) 0.065(6) -0.015(5) C506 0.068(5) 0.089(5) 0.094(6) 0.012(4) 0.042(4) -0.001(4) C507 0.049(3) 0.045(3) 0.043(3) 0.012(2) 0.010(2) -0.011(2) C508 0.080(5) 0.062(4) 0.086(5) 0.022(4) -0.027(4) -0.023(4) C509 0.080(5) 0.082(6) 0.126(7) 0.039(5) -0.043(5) -0.014(4) C510 0.061(4) 0.074(5) 0.093(6) 0.029(4) 0.010(4) 0.012(4) C511 0.081(5) 0.042(4) 0.101(6) 0.002(4) -0.019(4) -0.001(3) C512 0.068(4) 0.048(4) 0.078(5) 0.002(3) -0.021(4) -0.008(3) C601 0.035(3) 0.044(3) 0.035(3) 0.000(2) -0.004(2) -0.008(2) C602 0.059(4) 0.069(4) 0.037(3) -0.001(3) 0.004(3) -0.002(3) C603 0.093(5) 0.096(6) 0.036(3) -0.002(3) 0.006(3) -0.014(4) C604 0.094(6) 0.085(5) 0.048(4) 0.019(4) -0.017(4) -0.029(4) C605 0.059(4) 0.069(4) 0.080(5) 0.021(4) -0.028(4) -0.011(3) C606 0.049(3) 0.056(4) 0.051(4) 0.009(3) -0.008(3) -0.007(3) C607 0.042(3) 0.033(3) 0.045(3) 0.003(2) 0.013(2) 0.003(2) C608 0.043(3) 0.047(3) 0.070(4) 0.004(3) 0.002(3) 0.001(3) C609 0.040(3) 0.074(5) 0.122(7) 0.016(4) 0.015(4) 0.017(3) C610 0.069(5) 0.050(4) 0.174(9) 0.020(5) 0.049(5) 0.025(4) C611 0.068(5) 0.037(3) 0.141(7) -0.004(4) 0.042(5) 0.004(3) C612 0.049(3) 0.048(3) 0.082(5) -0.007(3) 0.021(3) -0.001(3) C701 0.047(3) 0.036(3) 0.042(3) -0.001(2) -0.001(2) 0.002(2) C702 0.056(4) 0.053(4) 0.061(4) 0.001(3) 0.007(3) 0.010(3) C703 0.060(4) 0.081(5) 0.103(6) 0.002(4) 0.017(4) 0.029(4) C704 0.082(5) 0.060(5) 0.111(7) -0.011(4) -0.001(5) 0.031(4) C705 0.093(6) 0.043(4) 0.107(6) 0.000(4) -0.014(5) 0.019(4) C706 0.066(4) 0.040(3) 0.077(5) 0.004(3) -0.002(3) 0.006(3) C707 0.048(3) 0.037(3) 0.031(3) 0.006(2) 0.006(2) -0.006(2) C708 0.056(3) 0.056(4) 0.051(4) 0.003(3) 0.013(3) 0.002(3) C709 0.077(5) 0.074(5) 0.064(5) -0.009(4) 0.040(4) -0.011(4) C710 0.112(6) 0.092(6) 0.038(4) 0.002(4) 0.020(4) -0.032(5) C711 0.090(5) 0.082(5) 0.039(4) 0.021(3) -0.002(3) -0.014(4) C712 0.057(4) 0.061(4) 0.043(3) 0.015(3) 0.001(3) -0.001(3) C801 0.053(3) 0.042(3) 0.037(3) -0.003(2) -0.001(2) -0.006(2) C802 0.057(4) 0.059(4) 0.046(3) 0.001(3) 0.007(3) -0.001(3) C803 0.067(4) 0.085(5) 0.073(5) 0.003(4) 0.014(4) 0.017(4) C804 0.087(5) 0.068(5) 0.072(5) -0.016(4) 0.000(4) 0.019(4) C805 0.105(6) 0.040(4) 0.099(6) -0.004(4) 0.000(5) -0.007(4) C806 0.071(4) 0.044(4) 0.087(5) -0.010(3) 0.017(4) -0.013(3) C807 0.064(4) 0.036(3) 0.050(3) 0.013(3) -0.016(3) -0.009(3) C808 0.091(5) 0.093(5) 0.041(4) 0.017(4) -0.009(4) -0.028(4) C809 0.115(7) 0.101(6) 0.055(5) 0.026(4) -0.038(5) -0.044(5) C810 0.083(6) 0.091(6) 0.111(8) 0.040(6) -0.051(6) -0.023(5) C811 0.071(5) 0.106(7) 0.114(7) -0.007(6) -0.038(5) 0.009(5) C812 0.059(4) 0.096(6) 0.074(5) -0.006(4) -0.018(4) 0.019(4) O1 0.43(2) 0.185(12) 0.258(16) -0.060(11) -0.190(17) 0.066(15) C7 0.45(4) 0.26(3) 0.141(14) -0.085(15) -0.16(2) 0.25(3) C8 0.33(4) 0.32(4) 0.40(5) -0.05(3) 0.13(3) -0.11(3) C9 0.37(3) 0.135(12) 0.208(18) 0.035(12) -0.002(16) 0.108(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.060(4) . ? Pt1 P1 2.2914(13) . ? Pt1 P4 2.2915(13) . ? Pt1 Cl1 2.3670(14) . ? Pt2 C4 2.054(4) . ? Pt2 P5 2.2841(13) . ? Pt2 P8 2.2927(13) . ? Pt2 Cl2 2.3616(16) . ? P1 C101 1.822(6) . ? P1 C107 1.823(5) . ? P1 C2 1.828(5) . ? P2 C1 1.691(5) . ? P2 C2 1.810(5) . ? P2 C201 1.812(5) . ? P2 C207 1.815(5) . ? P3 C1 1.693(5) . ? P3 C307 1.796(5) . ? P3 C301 1.804(5) . ? P3 C3 1.811(5) . ? P4 C401 1.814(5) . ? P4 C407 1.819(6) . ? P4 C3 1.831(5) . ? P5 C507 1.817(6) . ? P5 C501 1.818(6) . ? P5 C5 1.835(5) . ? P6 C4 1.693(5) . ? P6 C607 1.806(5) . ? P6 C5 1.809(5) . ? P6 C601 1.810(5) . ? P7 C4 1.693(5) . ? P7 C707 1.800(5) . ? P7 C701 1.805(5) . ? P7 C6 1.814(5) . ? P8 C6 1.817(5) . ? P8 C807 1.823(6) . ? P8 C801 1.825(5) . ? C101 C106 1.376(9) . ? C101 C102 1.377(8) . ? C102 C103 1.405(10) . ? C103 C104 1.354(12) . ? C104 C105 1.367(12) . ? C105 C106 1.394(10) . ? C107 C108 1.375(8) . ? C107 C112 1.376(8) . ? C108 C109 1.381(9) . ? C109 C110 1.344(11) . ? C110 C111 1.360(11) . ? C111 C112 1.414(10) . ? C201 C206 1.373(8) . ? C201 C202 1.386(8) . ? C202 C203 1.390(9) . ? C203 C204 1.344(11) . ? C204 C205 1.361(11) . ? C205 C206 1.400(9) . ? C207 C208 1.374(8) . ? C207 C212 1.389(8) . ? C208 C209 1.373(8) . ? C209 C210 1.386(11) . ? C210 C211 1.378(11) . ? C211 C212 1.378(9) . ? C301 C302 1.383(8) . ? C301 C306 1.404(8) . ? C302 C303 1.394(9) . ? C303 C304 1.362(10) . ? C304 C305 1.370(11) . ? C305 C306 1.379(9) . ? C307 C308 1.381(8) . ? C307 C312 1.393(8) . ? C308 C309 1.398(9) . ? C309 C310 1.383(11) . ? C310 C311 1.358(11) . ? C311 C312 1.386(9) . ? C401 C406 1.370(8) . ? C401 C402 1.381(8) . ? C402 C403 1.384(9) . ? C403 C404 1.364(11) . ? C404 C405 1.347(11) . ? C405 C406 1.392(10) . ? C407 C408 1.366(9) . ? C407 C412 1.390(8) . ? C408 C409 1.413(10) . ? C409 C410 1.357(12) . ? C410 C411 1.342(12) . ? C411 C412 1.376(9) . ? C501 C506 1.383(10) . ? C501 C502 1.393(10) . ? C502 C503 1.402(12) . ? C503 C504 1.353(16) . ? C504 C505 1.334(16) . ? C505 C506 1.383(10) . ? C507 C512 1.371(8) . ? C507 C508 1.372(8) . ? C508 C509 1.386(10) . ? C509 C510 1.356(11) . ? C510 C511 1.365(10) . ? C511 C512 1.382(9) . ? C601 C606 1.378(7) . ? C601 C602 1.378(7) . ? C602 C603 1.397(9) . ? C603 C604 1.347(11) . ? C604 C605 1.378(11) . ? C605 C606 1.397(9) . ? C607 C608 1.391(7) . ? C607 C612 1.395(8) . ? C608 C609 1.388(8) . ? C609 C610 1.357(11) . ? C610 C611 1.389(11) . ? C611 C612 1.371(8) . ? C701 C702 1.383(8) . ? C701 C706 1.393(8) . ? C702 C703 1.388(8) . ? C703 C704 1.376(11) . ? C704 C705 1.352(11) . ? C705 C706 1.380(9) . ? C707 C712 1.392(7) . ? C707 C708 1.404(7) . ? C708 C709 1.387(9) . ? C709 C710 1.374(11) . ? C710 C711 1.360(11) . ? C711 C712 1.367(9) . ? C801 C802 1.374(8) . ? C801 C806 1.385(8) . ? C802 C803 1.378(9) . ? C803 C804 1.369(11) . ? C804 C805 1.355(11) . ? C805 C806 1.399(9) . ? C807 C812 1.367(9) . ? C807 C808 1.388(9) . ? C808 C809 1.394(11) . ? C809 C810 1.363(13) . ? C810 C811 1.330(13) . ? C811 C812 1.404(10) . ? O1 C7 1.21(2) . ? C7 C9 1.36(3) . ? C7 C8 1.37(4) . ? O2 C10 1.34(3) . ? C10 C12 1.35(3) . ? C10 C11 1.36(3) . ? O3 C13 1.34(2) . ? C13 C15 1.33(2) . ? C13 C14 1.37(3) . ? O4 C16 1.25(2) . ? C16 C17 1.30(2) . ? C16 C18 1.43(2) . ? O5 C20 0.88(2) 2_565 ? O5 C19 1.42(2) . ? O5 C19 1.74(3) 2_565 ? C19 C21 1.25(2) . ? C19 C20 1.35(2) . ? C19 O5 1.74(3) 2_565 ? C20 O5 0.88(2) 2_565 ? O2A C10A 1.176(18) . ? C10A C11A 1.34(2) . ? C10A C12A 1.39(2) . ? C14A C14A 1.71(6) 2_855 ? C21A C19A 1.15(3) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 87.84(14) . . ? C1 Pt1 P4 87.72(14) . . ? P1 Pt1 P4 175.57(5) . . ? C1 Pt1 Cl1 179.42(14) . . ? P1 Pt1 Cl1 91.68(5) . . ? P4 Pt1 Cl1 92.75(5) . . ? C4 Pt2 P5 87.49(14) . . ? C4 Pt2 P8 88.32(14) . . ? P5 Pt2 P8 175.40(5) . . ? C4 Pt2 Cl2 178.29(15) . . ? P5 Pt2 Cl2 92.74(5) . . ? P8 Pt2 Cl2 91.50(5) . . ? C101 P1 C107 103.9(2) . . ? C101 P1 C2 106.0(3) . . ? C107 P1 C2 104.9(2) . . ? C101 P1 Pt1 120.43(18) . . ? C107 P1 Pt1 112.9(2) . . ? C2 P1 Pt1 107.52(17) . . ? C1 P2 C2 105.4(2) . . ? C1 P2 C201 118.1(2) . . ? C2 P2 C201 107.0(2) . . ? C1 P2 C207 114.4(3) . . ? C2 P2 C207 105.6(3) . . ? C201 P2 C207 105.4(2) . . ? C1 P3 C307 116.3(2) . . ? C1 P3 C301 115.5(2) . . ? C307 P3 C301 105.3(2) . . ? C1 P3 C3 105.5(2) . . ? C307 P3 C3 109.4(2) . . ? C301 P3 C3 104.1(2) . . ? C401 P4 C407 102.9(3) . . ? C401 P4 C3 106.3(2) . . ? C407 P4 C3 105.6(3) . . ? C401 P4 Pt1 112.82(18) . . ? C407 P4 Pt1 120.86(19) . . ? C3 P4 Pt1 107.34(17) . . ? C507 P5 C501 103.8(3) . . ? C507 P5 C5 106.8(2) . . ? C501 P5 C5 105.4(3) . . ? C507 P5 Pt2 111.73(18) . . ? C501 P5 Pt2 120.47(19) . . ? C5 P5 Pt2 107.85(16) . . ? C4 P6 C607 116.3(2) . . ? C4 P6 C5 105.8(2) . . ? C607 P6 C5 104.4(2) . . ? C4 P6 C601 115.0(2) . . ? C607 P6 C601 105.6(2) . . ? C5 P6 C601 109.2(2) . . ? C4 P7 C707 118.1(2) . . ? C4 P7 C701 114.6(2) . . ? C707 P7 C701 105.5(2) . . ? C4 P7 C6 105.4(2) . . ? C707 P7 C6 107.5(2) . . ? C701 P7 C6 104.7(2) . . ? C6 P8 C807 105.3(3) . . ? C6 P8 C801 105.9(2) . . ? C807 P8 C801 102.9(3) . . ? C6 P8 Pt2 106.91(16) . . ? C807 P8 Pt2 120.85(17) . . ? C801 P8 Pt2 113.89(19) . . ? P2 C1 P3 128.3(3) . . ? P2 C1 Pt1 114.9(2) . . ? P3 C1 Pt1 116.6(3) . . ? P2 C2 P1 105.1(3) . . ? P3 C3 P4 105.2(3) . . ? P6 C4 P7 127.1(3) . . ? P6 C4 Pt2 118.0(2) . . ? P7 C4 Pt2 114.8(2) . . ? P6 C5 P5 105.5(2) . . ? P7 C6 P8 105.0(2) . . ? C106 C101 C102 119.5(6) . . ? C106 C101 P1 122.0(5) . . ? C102 C101 P1 118.5(5) . . ? C101 C102 C103 119.2(7) . . ? C104 C103 C102 121.3(7) . . ? C103 C104 C105 119.4(7) . . ? C104 C105 C106 120.5(8) . . ? C101 C106 C105 120.2(7) . . ? C108 C107 C112 118.3(5) . . ? C108 C107 P1 120.5(4) . . ? C112 C107 P1 121.2(5) . . ? C107 C108 C109 121.7(6) . . ? C110 C109 C108 119.9(8) . . ? C109 C110 C111 120.4(7) . . ? C110 C111 C112 120.2(7) . . ? C107 C112 C111 119.4(7) . . ? C206 C201 C202 120.2(5) . . ? C206 C201 P2 118.9(4) . . ? C202 C201 P2 120.9(4) . . ? C201 C202 C203 118.9(6) . . ? C204 C203 C202 121.5(7) . . ? C203 C204 C205 119.5(6) . . ? C204 C205 C206 121.2(7) . . ? C201 C206 C205 118.6(6) . . ? C208 C207 C212 119.6(5) . . ? C208 C207 P2 119.8(4) . . ? C212 C207 P2 120.6(5) . . ? C209 C208 C207 120.6(6) . . ? C208 C209 C210 119.5(7) . . ? C211 C210 C209 120.7(6) . . ? C210 C211 C212 119.2(7) . . ? C211 C212 C207 120.4(6) . . ? C302 C301 C306 119.0(5) . . ? C302 C301 P3 120.1(4) . . ? C306 C301 P3 120.8(4) . . ? C301 C302 C303 119.4(6) . . ? C304 C303 C302 120.9(7) . . ? C303 C304 C305 120.3(6) . . ? C304 C305 C306 120.1(6) . . ? C305 C306 C301 120.2(6) . . ? C308 C307 C312 119.6(5) . . ? C308 C307 P3 120.6(4) . . ? C312 C307 P3 119.7(4) . . ? C307 C308 C309 119.3(6) . . ? C310 C309 C308 120.4(7) . . ? C311 C310 C309 120.2(6) . . ? C310 C311 C312 120.3(7) . . ? C311 C312 C307 120.3(6) . . ? C406 C401 C402 118.0(5) . . ? C406 C401 P4 122.1(5) . . ? C402 C401 P4 119.8(4) . . ? C401 C402 C403 120.8(6) . . ? C404 C403 C402 120.1(7) . . ? C405 C404 C403 119.7(6) . . ? C404 C405 C406 120.8(7) . . ? C401 C406 C405 120.5(7) . . ? C408 C407 C412 117.9(6) . . ? C408 C407 P4 119.0(5) . . ? C412 C407 P4 123.1(4) . . ? C407 C408 C409 120.1(7) . . ? C410 C409 C408 120.0(8) . . ? C411 C410 C409 120.3(7) . . ? C410 C411 C412 120.5(7) . . ? C411 C412 C407 121.2(7) . . ? C506 C501 C502 118.6(6) . . ? C506 C501 P5 122.5(5) . . ? C502 C501 P5 118.9(6) . . ? C501 C502 C503 118.3(9) . . ? C504 C503 C502 121.4(9) . . ? C505 C504 C503 120.4(9) . . ? C504 C505 C506 120.3(10) . . ? C501 C506 C505 120.9(8) . . ? C512 C507 C508 117.2(6) . . ? C512 C507 P5 123.2(4) . . ? C508 C507 P5 119.6(5) . . ? C507 C508 C509 121.6(6) . . ? C510 C509 C508 119.5(7) . . ? C509 C510 C511 120.3(6) . . ? C510 C511 C512 119.3(6) . . ? C507 C512 C511 121.9(6) . . ? C606 C601 C602 119.8(5) . . ? C606 C601 P6 119.4(4) . . ? C602 C601 P6 120.7(4) . . ? C601 C602 C603 120.3(6) . . ? C604 C603 C602 120.0(6) . . ? C603 C604 C605 120.4(6) . . ? C604 C605 C606 120.5(6) . . ? C601 C606 C605 119.1(6) . . ? C608 C607 C612 119.3(5) . . ? C608 C607 P6 119.7(4) . . ? C612 C607 P6 121.0(4) . . ? C609 C608 C607 119.6(6) . . ? C610 C609 C608 120.2(6) . . ? C609 C610 C611 121.0(6) . . ? C612 C611 C610 119.3(6) . . ? C611 C612 C607 120.5(6) . . ? C702 C701 C706 119.6(5) . . ? C702 C701 P7 119.7(4) . . ? C706 C701 P7 120.6(4) . . ? C701 C702 C703 119.6(6) . . ? C704 C703 C702 119.9(7) . . ? C705 C704 C703 120.9(6) . . ? C704 C705 C706 120.3(7) . . ? C705 C706 C701 119.8(6) . . ? C712 C707 C708 119.4(5) . . ? C712 C707 P7 121.4(4) . . ? C708 C707 P7 119.2(4) . . ? C709 C708 C707 118.8(6) . . ? C710 C709 C708 120.8(6) . . ? C711 C710 C709 119.8(6) . . ? C710 C711 C712 121.4(6) . . ? C711 C712 C707 119.8(6) . . ? C802 C801 C806 118.7(5) . . ? C802 C801 P8 120.6(4) . . ? C806 C801 P8 120.7(5) . . ? C801 C802 C803 121.3(6) . . ? C804 C803 C802 119.4(7) . . ? C805 C804 C803 120.9(6) . . ? C804 C805 C806 119.8(7) . . ? C801 C806 C805 119.9(6) . . ? C812 C807 C808 118.7(6) . . ? C812 C807 P8 121.2(5) . . ? C808 C807 P8 120.1(5) . . ? C807 C808 C809 119.7(8) . . ? C810 C809 C808 121.2(8) . . ? C811 C810 C809 118.6(7) . . ? C810 C811 C812 122.3(9) . . ? C807 C812 C811 119.4(7) . . ? O1 C7 C9 123(4) . . ? O1 C7 C8 116(3) . . ? C9 C7 C8 121(3) . . ? O2 C10 C12 111(3) . . ? O2 C10 C11 121(3) . . ? C12 C10 C11 115(3) . . ? C15 C13 O3 117(2) . . ? C15 C13 C14 122(3) . . ? O3 C13 C14 108(2) . . ? O4 C16 C17 114(3) . . ? O4 C16 C18 112(2) . . ? C17 C16 C18 126(3) . . ? C20 O5 C19 142(2) 2_565 . ? C20 O5 C19 49.7(18) 2_565 2_565 ? C19 O5 C19 93.1(17) . 2_565 ? C21 C19 C20 122(2) . . ? C21 C19 O5 115.5(19) . . ? C20 C19 O5 116(2) . . ? C21 C19 O5 150(2) . 2_565 ? C20 C19 O5 29.7(11) . 2_565 ? O5 C19 O5 86.9(17) . 2_565 ? O5 C20 C19 101(2) 2_565 . ? O2A C10A C11A 123(2) . . ? O2A C10A C12A 124(2) . . ? C11A C10A C12A 112(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.930 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.096 # Attachment 'dt-art-10-2011-011949-File003-v1-0.CIF' data_p164c _database_code_depnum_ccdc_archive 'CCDC 849141' #TrackingRef 'dt-art-10-2011-011949-File003-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 Cl P4' _chemical_formula_weight 817.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.9190(4) _cell_length_b 27.1997(6) _cell_length_c 18.7995(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.034(2) _cell_angle_gamma 90.00 _cell_volume 8645.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 65581 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45501 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 24.00 _reflns_number_total 13577 _reflns_number_gt 9328 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+1.8484P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'constr, refined at C1 and C4' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13577 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cl1 Cl 0.53660(5) 0.23716(3) -0.11133(4) 0.0494(2) Uani 1 1 d . . . Cl2 Cl -0.00400(5) 0.24760(3) 0.41237(4) 0.0540(2) Uani 1 1 d . . . P1 P 0.40746(5) 0.11087(3) 0.00169(4) 0.0510(2) Uani 1 1 d . . . P2 P 0.53309(4) 0.15276(3) 0.11087(3) 0.03407(18) Uani 1 1 d . . . P3 P 0.41047(4) 0.15006(3) 0.23107(3) 0.03134(18) Uani 1 1 d . . . P4 P 0.48388(4) 0.09467(3) 0.35624(4) 0.03707(19) Uani 1 1 d . . . P5 P -0.05286(4) 0.09531(3) 0.82451(4) 0.03766(19) Uani 1 1 d . . . P6 P 0.03904(4) 0.14735(3) 0.70893(3) 0.03052(17) Uani 1 1 d . . . P7 P -0.09131(4) 0.13909(3) 0.58804(3) 0.03035(17) Uani 1 1 d . . . P8 P -0.01795(4) 0.07989(3) 0.47216(3) 0.03475(18) Uani 1 1 d . . . C1 C 0.48267(18) 0.12857(13) 0.17936(15) 0.0372(7) Uani 1 1 d . . . H1 H 0.4938(16) 0.1022(10) 0.1857(13) 0.031(9) Uiso 1 1 d . . . C2 C 0.47698(16) 0.16135(11) 0.02802(13) 0.0417(7) Uani 1 1 d . . . H2A H 0.5143 0.1658 -0.0101 0.050 Uiso 1 1 calc . . . H2B H 0.4465 0.1919 0.0315 0.050 Uiso 1 1 calc . . . C3 C 0.44078(16) 0.15391(10) 0.32408(12) 0.0351(7) Uani 1 1 d . . . H3A H 0.3950 0.1622 0.3522 0.042 Uiso 1 1 calc . . . H3B H 0.4801 0.1801 0.3307 0.042 Uiso 1 1 calc . . . C4 C -0.01706(16) 0.11879(12) 0.64445(13) 0.0325(7) Uani 1 1 d . . . H4 H -0.0097(16) 0.0881(11) 0.6420(13) 0.040(9) Uiso 1 1 d . . . C5 C -0.00389(16) 0.15279(10) 0.79551(13) 0.0358(7) Uani 1 1 d . . . H5A H -0.0428 0.1795 0.7940 0.043 Uiso 1 1 calc . . . H5B H 0.0378 0.1616 0.8307 0.043 Uiso 1 1 calc . . . C6 C -0.06556(15) 0.13903(10) 0.49523(13) 0.0350(7) Uani 1 1 d . . . H6A H -0.0293 0.1663 0.4864 0.042 Uiso 1 1 calc . . . H6B H -0.1134 0.1438 0.4650 0.042 Uiso 1 1 calc . . . C101 C 0.32573(17) 0.14837(13) -0.03374(14) 0.0491(8) Uani 1 1 d . . . C102 C 0.33497(18) 0.19148(14) -0.07273(16) 0.0565(9) Uani 1 1 d . . . H102 H 0.3860 0.2020 -0.0836 0.068 Uiso 1 1 calc . . . C103 C 0.2701(2) 0.21894(15) -0.09566(17) 0.0696(11) Uani 1 1 d . . . H103 H 0.2771 0.2476 -0.1227 0.083 Uiso 1 1 calc . . . C104 C 0.1948(2) 0.2041(2) -0.0787(2) 0.0810(14) Uani 1 1 d . . . H104 H 0.1506 0.2230 -0.0931 0.097 Uiso 1 1 calc . . . C105 C 0.1853(2) 0.1618(2) -0.0411(2) 0.0765(13) Uani 1 1 d . . . H105 H 0.1341 0.1514 -0.0305 0.092 Uiso 1 1 calc . . . C106 C 0.2493(2) 0.13428(15) -0.01854(16) 0.0619(10) Uani 1 1 d . . . H106 H 0.2413 0.1054 0.0077 0.074 Uiso 1 1 calc . . . C107 C 0.44806(18) 0.08537(11) -0.07966(16) 0.0484(8) Uani 1 1 d . . . C108 C 0.47407(19) 0.11255(12) -0.13676(16) 0.0537(8) Uani 1 1 d . . . H108 H 0.4735 0.1471 -0.1344 0.064 Uiso 1 1 calc . . . C109 C 0.5009(2) 0.08975(16) -0.19719(17) 0.0682(11) Uani 1 1 d . . . H109 H 0.5185 0.1088 -0.2353 0.082 Uiso 1 1 calc . . . C110 C 0.5019(3) 0.0397(2) -0.2014(3) 0.1019(17) Uani 1 1 d . . . H110 H 0.5202 0.0240 -0.2422 0.122 Uiso 1 1 calc . . . C111 C 0.4763(4) 0.01313(18) -0.1463(4) 0.145(3) Uani 1 1 d . . . H111 H 0.4770 -0.0214 -0.1488 0.175 Uiso 1 1 calc . . . C112 C 0.4493(3) 0.03551(16) -0.0868(3) 0.1044(15) Uani 1 1 d . . . H112 H 0.4310 0.0159 -0.0496 0.125 Uiso 1 1 calc . . . C201 C 0.57481(15) 0.21239(10) 0.12921(13) 0.0358(7) Uani 1 1 d . . . C202 C 0.58127(18) 0.23072(12) 0.19779(15) 0.0500(8) Uani 1 1 d . . . H202 H 0.5637 0.2117 0.2359 0.060 Uiso 1 1 calc . . . C203 C 0.6134(2) 0.27669(14) 0.21086(16) 0.0623(10) Uani 1 1 d . . . H203 H 0.6161 0.2891 0.2576 0.075 Uiso 1 1 calc . . . C204 C 0.6411(2) 0.30422(12) 0.15650(18) 0.0591(9) Uani 1 1 d . . . H204 H 0.6632 0.3354 0.1657 0.071 Uiso 1 1 calc . . . C205 C 0.6363(2) 0.28608(13) 0.08792(17) 0.0585(9) Uani 1 1 d . . . H205 H 0.6556 0.3050 0.0504 0.070 Uiso 1 1 calc . . . C206 C 0.60379(18) 0.24073(12) 0.07390(14) 0.0460(8) Uani 1 1 d . . . H206 H 0.6010 0.2287 0.0270 0.055 Uiso 1 1 calc . . . C207 C 0.61503(17) 0.11218(11) 0.09547(14) 0.0410(7) Uani 1 1 d . . . C208 C 0.66252(19) 0.09750(13) 0.15321(15) 0.0555(9) Uani 1 1 d . . . H208 H 0.6498 0.1076 0.1993 0.067 Uiso 1 1 calc . . . C209 C 0.7278(2) 0.06850(16) 0.14411(18) 0.0763(12) Uani 1 1 d . . . H209 H 0.7589 0.0582 0.1838 0.092 Uiso 1 1 calc . . . C210 C 0.7473(3) 0.0547(2) 0.0776(2) 0.1079(18) Uani 1 1 d . . . H210 H 0.7926 0.0354 0.0712 0.129 Uiso 1 1 calc . . . C211 C 0.7014(3) 0.0687(2) 0.0202(2) 0.132(2) Uani 1 1 d . . . H211 H 0.7147 0.0586 -0.0256 0.158 Uiso 1 1 calc . . . C212 C 0.6352(2) 0.09787(17) 0.02879(17) 0.0879(14) Uani 1 1 d . . . H212 H 0.6042 0.1078 -0.0112 0.105 Uiso 1 1 calc . . . C301 C 0.37376(15) 0.20903(10) 0.20252(13) 0.0337(7) Uani 1 1 d . . . C302 C 0.38633(19) 0.25159(12) 0.24167(15) 0.0486(8) Uani 1 1 d . . . H302 H 0.4174 0.2508 0.2841 0.058 Uiso 1 1 calc . . . C303 C 0.3529(2) 0.29549(12) 0.21800(17) 0.0590(9) Uani 1 1 d . . . H303 H 0.3606 0.3243 0.2450 0.071 Uiso 1 1 calc . . . C304 C 0.3087(2) 0.29707(13) 0.15558(18) 0.0589(9) Uani 1 1 d . . . H304 H 0.2867 0.3270 0.1398 0.071 Uiso 1 1 calc . . . C305 C 0.29631(19) 0.25529(13) 0.11594(16) 0.0556(9) Uani 1 1 d . . . H305 H 0.2665 0.2566 0.0728 0.067 Uiso 1 1 calc . . . C306 C 0.32792(17) 0.21137(11) 0.13986(14) 0.0448(8) Uani 1 1 d . . . H306 H 0.3183 0.1825 0.1134 0.054 Uiso 1 1 calc . . . C307 C 0.32419(15) 0.11072(10) 0.22935(13) 0.0337(7) Uani 1 1 d . . . C308 C 0.26472(17) 0.11667(12) 0.27804(15) 0.0475(8) Uani 1 1 d . . . H308 H 0.2710 0.1404 0.3142 0.057 Uiso 1 1 calc . . . C309 C 0.19707(19) 0.08864(13) 0.27435(18) 0.0572(9) Uani 1 1 d . . . H309 H 0.1580 0.0929 0.3081 0.069 Uiso 1 1 calc . . . C310 C 0.18692(19) 0.05448(13) 0.22123(18) 0.0583(9) Uani 1 1 d . . . H310 H 0.1406 0.0354 0.2186 0.070 Uiso 1 1 calc . . . C311 C 0.2436(2) 0.04796(13) 0.17215(16) 0.0609(9) Uani 1 1 d . . . H311 H 0.2359 0.0248 0.1354 0.073 Uiso 1 1 calc . . . C312 C 0.31306(18) 0.07567(12) 0.17658(14) 0.0488(8) Uani 1 1 d . . . H312 H 0.3526 0.0705 0.1435 0.059 Uiso 1 1 calc . . . C401 C 0.59035(16) 0.10450(11) 0.35046(13) 0.0359(7) Uani 1 1 d . . . C402 C 0.62846(17) 0.14912(12) 0.36034(15) 0.0473(8) Uani 1 1 d . . . H402 H 0.5989 0.1773 0.3707 0.057 Uiso 1 1 calc . . . C403 C 0.70985(19) 0.15255(13) 0.35513(16) 0.0581(9) Uani 1 1 d . . . H403 H 0.7350 0.1832 0.3606 0.070 Uiso 1 1 calc . . . C404 C 0.75375(18) 0.11116(16) 0.34198(16) 0.0591(10) Uani 1 1 d . . . H404 H 0.8089 0.1135 0.3383 0.071 Uiso 1 1 calc . . . C405 C 0.7173(2) 0.06670(15) 0.33425(17) 0.0612(10) Uani 1 1 d . . . H405 H 0.7475 0.0383 0.3268 0.073 Uiso 1 1 calc . . . C406 C 0.63641(19) 0.06326(12) 0.33732(15) 0.0491(8) Uani 1 1 d . . . H406 H 0.6118 0.0326 0.3304 0.059 Uiso 1 1 calc . . . C407 C 0.47107(15) 0.10219(11) 0.45204(13) 0.0361(7) Uani 1 1 d . . . C408 C 0.47539(17) 0.14690(12) 0.48785(14) 0.0476(8) Uani 1 1 d . . . H408 H 0.4866 0.1758 0.4628 0.057 Uiso 1 1 calc . . . C409 C 0.46324(19) 0.14906(14) 0.56037(15) 0.0577(9) Uani 1 1 d . . . H409 H 0.4656 0.1794 0.5843 0.069 Uiso 1 1 calc . . . C410 C 0.4477(2) 0.10665(16) 0.59723(16) 0.0647(10) Uani 1 1 d . . . H410 H 0.4395 0.1082 0.6464 0.078 Uiso 1 1 calc . . . C411 C 0.4441(2) 0.06271(15) 0.56323(17) 0.0634(10) Uani 1 1 d . . . H411 H 0.4339 0.0339 0.5890 0.076 Uiso 1 1 calc . . . C412 C 0.45548(17) 0.06008(12) 0.49036(15) 0.0482(8) Uani 1 1 d . . . H412 H 0.4526 0.0295 0.4671 0.058 Uiso 1 1 calc . . . C501 C -0.15183(16) 0.11866(11) 0.84039(13) 0.0392(7) Uani 1 1 d . . . C502 C -0.16993(17) 0.16508(12) 0.86500(15) 0.0470(8) Uani 1 1 d . . . H502 H -0.1291 0.1877 0.8752 0.056 Uiso 1 1 calc . . . C503 C -0.2484(2) 0.17845(14) 0.87482(17) 0.0614(10) Uani 1 1 d . . . H503 H -0.2603 0.2100 0.8919 0.074 Uiso 1 1 calc . . . C504 C -0.3083(2) 0.14553(18) 0.8594(2) 0.0712(11) Uani 1 1 d . . . H504 H -0.3612 0.1546 0.8659 0.085 Uiso 1 1 calc . . . C505 C -0.2911(2) 0.09998(18) 0.8350(2) 0.0772(12) Uani 1 1 d . . . H505 H -0.3322 0.0776 0.8245 0.093 Uiso 1 1 calc . . . C506 C -0.2140(2) 0.08641(13) 0.82546(16) 0.0566(9) Uani 1 1 d . . . H506 H -0.2031 0.0547 0.8085 0.068 Uiso 1 1 calc . . . C507 C -0.01100(16) 0.08794(11) 0.91550(14) 0.0393(7) Uani 1 1 d . . . C508 C -0.03097(19) 0.11650(13) 0.97335(15) 0.0547(9) Uani 1 1 d . . . H508 H -0.0668 0.1427 0.9668 0.066 Uiso 1 1 calc . . . C509 C 0.0012(2) 0.10695(15) 1.04051(16) 0.0636(10) Uani 1 1 d . . . H509 H -0.0135 0.1264 1.0792 0.076 Uiso 1 1 calc . . . C510 C 0.0536(2) 0.06994(17) 1.05110(18) 0.0770(12) Uani 1 1 d . . . H510 H 0.0747 0.0636 1.0971 0.092 Uiso 1 1 calc . . . C511 C 0.0758(2) 0.04182(16) 0.9951(2) 0.0875(13) Uani 1 1 d . . . H511 H 0.1134 0.0167 1.0022 0.105 Uiso 1 1 calc . . . C512 C 0.0425(2) 0.05045(14) 0.92737(17) 0.0682(10) Uani 1 1 d . . . H512 H 0.0568 0.0304 0.8892 0.082 Uiso 1 1 calc . . . C601 C 0.06620(15) 0.20895(10) 0.68581(13) 0.0324(6) Uani 1 1 d . . . C602 C 0.07286(18) 0.22248(12) 0.61530(14) 0.0483(8) Uani 1 1 d . . . H602 H 0.0619 0.1994 0.5791 0.058 Uiso 1 1 calc . . . C603 C 0.0954(2) 0.26943(14) 0.59760(16) 0.0625(10) Uani 1 1 d . . . H603 H 0.0984 0.2783 0.5495 0.075 Uiso 1 1 calc . . . C604 C 0.11341(19) 0.30320(12) 0.64953(19) 0.0587(9) Uani 1 1 d . . . H604 H 0.1299 0.3350 0.6373 0.070 Uiso 1 1 calc . . . C605 C 0.1072(2) 0.29023(12) 0.71969(17) 0.0566(9) Uani 1 1 d . . . H605 H 0.1198 0.3133 0.7555 0.068 Uiso 1 1 calc . . . C606 C 0.08269(18) 0.24396(11) 0.73810(14) 0.0455(8) Uani 1 1 d . . . H606 H 0.0771 0.2359 0.7863 0.055 Uiso 1 1 calc . . . C607 C 0.12920(15) 0.11204(10) 0.72221(13) 0.0315(6) Uani 1 1 d . . . C608 C 0.16737(17) 0.09344(11) 0.66398(13) 0.0402(7) Uani 1 1 d . . . H608 H 0.1443 0.0972 0.6181 0.048 Uiso 1 1 calc . . . C609 C 0.23845(18) 0.06969(12) 0.67284(15) 0.0505(8) Uani 1 1 d . . . H609 H 0.2636 0.0572 0.6329 0.061 Uiso 1 1 calc . . . C610 C 0.27324(18) 0.06400(12) 0.73940(18) 0.0554(9) Uani 1 1 d . . . H610 H 0.3221 0.0477 0.7450 0.066 Uiso 1 1 calc . . . C611 C 0.2366(2) 0.08215(14) 0.79755(16) 0.0622(10) Uani 1 1 d . . . H611 H 0.2601 0.0783 0.8432 0.075 Uiso 1 1 calc . . . C612 C 0.16502(18) 0.10614(12) 0.78912(15) 0.0524(9) Uani 1 1 d . . . H612 H 0.1402 0.1187 0.8293 0.063 Uiso 1 1 calc . . . C701 C -0.12494(15) 0.19925(10) 0.61166(13) 0.0347(7) Uani 1 1 d . . . C702 C -0.12504(19) 0.23877(12) 0.56483(16) 0.0527(8) Uani 1 1 d . . . H702 H -0.1058 0.2348 0.5189 0.063 Uiso 1 1 calc . . . C703 C -0.1535(2) 0.28397(13) 0.5861(2) 0.0698(11) Uani 1 1 d . . . H703 H -0.1545 0.3105 0.5540 0.084 Uiso 1 1 calc . . . C704 C -0.1803(2) 0.29048(13) 0.6534(2) 0.0659(10) Uani 1 1 d . . . H704 H -0.1980 0.3216 0.6678 0.079 Uiso 1 1 calc . . . C705 C -0.1812(2) 0.25156(14) 0.69981(17) 0.0614(10) Uani 1 1 d . . . H705 H -0.1997 0.2559 0.7459 0.074 Uiso 1 1 calc . . . C706 C -0.15480(18) 0.20588(12) 0.67873(14) 0.0476(8) Uani 1 1 d . . . H706 H -0.1571 0.1791 0.7102 0.057 Uiso 1 1 calc . . . C707 C -0.17779(15) 0.10001(10) 0.59125(12) 0.0306(6) Uani 1 1 d . . . C708 C -0.24165(18) 0.10795(12) 0.54361(15) 0.0457(8) Uani 1 1 d . . . H708 H -0.2374 0.1315 0.5073 0.055 Uiso 1 1 calc . . . C709 C -0.31109(18) 0.08162(13) 0.54911(17) 0.0540(9) Uani 1 1 d . . . H709 H -0.3537 0.0873 0.5167 0.065 Uiso 1 1 calc . . . C710 C -0.31781(18) 0.04744(13) 0.60155(17) 0.0551(9) Uani 1 1 d . . . H710 H -0.3653 0.0300 0.6058 0.066 Uiso 1 1 calc . . . C711 C -0.2555(2) 0.03864(13) 0.64776(17) 0.0635(10) Uani 1 1 d . . . H711 H -0.2601 0.0146 0.6833 0.076 Uiso 1 1 calc . . . C712 C -0.18572(18) 0.06469(12) 0.64282(15) 0.0493(8) Uani 1 1 d . . . H712 H -0.1433 0.0582 0.6750 0.059 Uiso 1 1 calc . . . C801 C 0.08781(16) 0.09449(11) 0.47416(12) 0.0341(7) Uani 1 1 d . . . C802 C 0.12023(16) 0.14087(11) 0.46586(13) 0.0408(7) Uani 1 1 d . . . H802 H 0.0867 0.1681 0.4584 0.049 Uiso 1 1 calc . . . C803 C 0.20135(19) 0.14762(13) 0.46850(15) 0.0516(8) Uani 1 1 d . . . H803 H 0.2224 0.1794 0.4643 0.062 Uiso 1 1 calc . . . C804 C 0.25121(18) 0.10809(16) 0.47727(16) 0.0585(9) Uani 1 1 d . . . H804 H 0.3063 0.1129 0.4792 0.070 Uiso 1 1 calc . . . C805 C 0.2205(2) 0.06147(15) 0.48331(16) 0.0585(9) Uani 1 1 d . . . H805 H 0.2546 0.0343 0.4882 0.070 Uiso 1 1 calc . . . C806 C 0.13932(19) 0.05459(11) 0.48220(14) 0.0470(8) Uani 1 1 d . . . H806 H 0.1187 0.0227 0.4869 0.056 Uiso 1 1 calc . . . C807 C -0.03636(15) 0.07815(11) 0.37528(13) 0.0349(7) Uani 1 1 d . . . C808 C -0.02872(17) 0.11841(12) 0.33061(14) 0.0437(8) Uani 1 1 d . . . H808 H -0.0150 0.1493 0.3498 0.052 Uiso 1 1 calc . . . C809 C -0.04140(18) 0.11309(13) 0.25742(15) 0.0541(9) Uani 1 1 d . . . H809 H -0.0367 0.1404 0.2273 0.065 Uiso 1 1 calc . . . C810 C -0.0607(2) 0.06789(15) 0.22931(15) 0.0606(10) Uani 1 1 d . . . H810 H -0.0683 0.0643 0.1798 0.073 Uiso 1 1 calc . . . C811 C -0.0691(2) 0.02817(14) 0.27248(17) 0.0669(10) Uani 1 1 d . . . H811 H -0.0833 -0.0025 0.2528 0.080 Uiso 1 1 calc . . . C812 C -0.05666(19) 0.03306(12) 0.34570(15) 0.0510(8) Uani 1 1 d . . . H812 H -0.0621 0.0055 0.3753 0.061 Uiso 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0650(5) 0.0422(5) 0.0411(4) 0.0074(3) 0.0037(3) -0.0045(4) Cl2 0.0635(5) 0.0479(5) 0.0516(5) 0.0177(4) 0.0136(4) 0.0054(4) P1 0.0582(6) 0.0540(6) 0.0403(4) 0.0113(4) -0.0051(4) -0.0188(4) P2 0.0359(4) 0.0383(5) 0.0281(4) 0.0045(3) 0.0018(3) 0.0010(3) P3 0.0334(4) 0.0324(4) 0.0283(4) 0.0021(3) 0.0017(3) 0.0034(3) P4 0.0408(5) 0.0374(5) 0.0330(4) 0.0032(3) 0.0002(3) 0.0036(4) P5 0.0440(5) 0.0356(5) 0.0337(4) -0.0025(3) 0.0060(3) -0.0027(4) P6 0.0317(4) 0.0320(4) 0.0280(3) -0.0039(3) 0.0031(3) -0.0009(3) P7 0.0318(4) 0.0323(4) 0.0271(4) -0.0014(3) 0.0032(3) 0.0025(3) P8 0.0383(4) 0.0353(5) 0.0309(4) -0.0008(3) 0.0052(3) 0.0006(3) C1 0.0437(19) 0.030(2) 0.0381(17) 0.0074(14) 0.0080(12) 0.0087(16) C2 0.0437(18) 0.045(2) 0.0365(15) 0.0066(13) -0.0019(12) -0.0032(15) C3 0.0380(16) 0.0381(18) 0.0291(14) 0.0013(12) 0.0014(11) 0.0047(13) C4 0.0352(17) 0.0265(19) 0.0354(15) -0.0042(13) -0.0029(11) 0.0046(14) C5 0.0391(17) 0.0372(18) 0.0314(14) -0.0058(12) 0.0060(12) -0.0040(14) C6 0.0333(16) 0.0404(18) 0.0314(14) 0.0014(12) 0.0036(11) 0.0037(13) C101 0.0415(19) 0.075(3) 0.0312(15) -0.0104(16) 0.0047(13) -0.0104(17) C102 0.042(2) 0.079(3) 0.0486(19) 0.0016(18) 0.0034(14) 0.0062(19) C103 0.058(3) 0.094(3) 0.056(2) -0.0073(19) -0.0019(17) 0.024(2) C104 0.051(3) 0.136(4) 0.055(2) -0.047(3) -0.0119(19) 0.029(3) C105 0.047(2) 0.131(4) 0.051(2) -0.040(2) 0.0059(18) -0.012(3) C106 0.051(2) 0.092(3) 0.0433(18) -0.0217(18) 0.0040(15) -0.021(2) C107 0.0449(19) 0.035(2) 0.064(2) -0.0004(16) -0.0129(15) -0.0022(15) C108 0.062(2) 0.052(2) 0.0464(19) -0.0063(16) -0.0057(15) 0.0053(17) C109 0.052(2) 0.095(3) 0.057(2) -0.025(2) -0.0062(16) 0.005(2) C110 0.068(3) 0.097(4) 0.142(4) -0.078(3) 0.015(3) -0.010(3) C111 0.160(6) 0.045(3) 0.236(7) -0.044(4) 0.077(5) 0.002(3) C112 0.126(4) 0.040(3) 0.150(4) 0.000(3) 0.032(3) -0.002(3) C201 0.0332(16) 0.0397(18) 0.0343(15) 0.0038(13) -0.0012(12) -0.0001(13) C202 0.051(2) 0.060(2) 0.0393(17) -0.0021(15) 0.0036(14) -0.0162(17) C203 0.062(2) 0.078(3) 0.047(2) -0.0135(18) 0.0033(16) -0.018(2) C204 0.061(2) 0.046(2) 0.069(2) -0.0055(18) -0.0041(17) -0.0128(18) C205 0.067(2) 0.053(2) 0.055(2) 0.0130(17) -0.0026(16) -0.0193(19) C206 0.056(2) 0.047(2) 0.0348(16) 0.0039(14) -0.0020(13) -0.0076(16) C207 0.0428(18) 0.046(2) 0.0342(16) 0.0018(13) 0.0076(13) 0.0055(15) C208 0.051(2) 0.070(3) 0.0459(18) 0.0037(16) 0.0061(15) 0.0211(18) C209 0.063(3) 0.104(3) 0.062(2) 0.009(2) 0.0073(18) 0.037(2) C210 0.091(3) 0.154(5) 0.079(3) 0.000(3) 0.021(2) 0.080(3) C211 0.132(4) 0.208(6) 0.056(3) -0.010(3) 0.021(3) 0.105(4) C212 0.084(3) 0.136(4) 0.044(2) 0.002(2) 0.0124(18) 0.058(3) C301 0.0359(16) 0.0338(18) 0.0316(14) 0.0037(12) 0.0031(12) 0.0051(13) C302 0.063(2) 0.043(2) 0.0399(17) 0.0008(15) -0.0008(14) 0.0080(17) C303 0.083(3) 0.033(2) 0.060(2) -0.0022(16) -0.0009(18) 0.0120(18) C304 0.063(2) 0.043(2) 0.070(2) 0.0185(18) 0.0023(18) 0.0195(18) C305 0.057(2) 0.053(2) 0.056(2) 0.0126(17) -0.0124(16) 0.0132(18) C306 0.0487(19) 0.040(2) 0.0456(17) 0.0013(14) -0.0063(14) 0.0061(15) C307 0.0351(16) 0.0345(18) 0.0313(15) 0.0081(13) -0.0003(12) 0.0035(13) C308 0.0403(19) 0.045(2) 0.0573(19) -0.0010(15) 0.0090(14) -0.0006(16) C309 0.044(2) 0.062(3) 0.066(2) 0.0118(19) 0.0121(16) -0.0004(18) C310 0.049(2) 0.059(2) 0.066(2) 0.0272(19) -0.0095(17) -0.0177(18) C311 0.078(3) 0.058(2) 0.0468(19) 0.0051(16) -0.0034(17) -0.029(2) C312 0.057(2) 0.052(2) 0.0384(17) 0.0038(15) 0.0079(14) -0.0130(17) C401 0.0437(18) 0.0365(19) 0.0277(14) 0.0043(12) 0.0050(12) 0.0099(15) C402 0.040(2) 0.049(2) 0.0528(18) -0.0011(15) 0.0033(14) 0.0080(16) C403 0.045(2) 0.068(3) 0.061(2) -0.0009(17) -0.0006(15) -0.0025(19) C404 0.0335(19) 0.090(3) 0.053(2) 0.0060(19) 0.0033(14) 0.010(2) C405 0.048(2) 0.073(3) 0.063(2) 0.0088(19) 0.0103(16) 0.028(2) C406 0.055(2) 0.046(2) 0.0462(18) 0.0063(15) 0.0093(14) 0.0141(17) C407 0.0286(16) 0.045(2) 0.0345(15) 0.0062(14) 0.0003(11) 0.0018(14) C408 0.0487(19) 0.058(2) 0.0366(17) 0.0031(15) 0.0062(13) -0.0090(16) C409 0.056(2) 0.080(3) 0.0379(18) -0.0051(17) 0.0079(14) -0.0059(19) C410 0.063(2) 0.100(3) 0.0318(18) 0.015(2) 0.0066(15) 0.004(2) C411 0.070(2) 0.070(3) 0.050(2) 0.0283(19) 0.0099(17) 0.008(2) C412 0.0484(19) 0.049(2) 0.0480(19) 0.0143(15) 0.0042(14) 0.0056(16) C501 0.0405(18) 0.043(2) 0.0341(15) 0.0083(13) 0.0022(12) -0.0044(15) C502 0.044(2) 0.050(2) 0.0472(18) 0.0059(15) 0.0058(14) 0.0035(16) C503 0.060(2) 0.063(3) 0.062(2) 0.0177(18) 0.0182(17) 0.019(2) C504 0.039(2) 0.092(3) 0.083(3) 0.033(2) 0.0104(18) 0.007(2) C505 0.042(2) 0.091(4) 0.098(3) 0.016(2) -0.004(2) -0.020(2) C506 0.049(2) 0.058(2) 0.063(2) 0.0053(17) 0.0016(16) -0.0167(18) C507 0.0384(17) 0.0399(19) 0.0399(16) 0.0044(14) 0.0059(12) -0.0001(15) C508 0.061(2) 0.063(2) 0.0391(18) -0.0032(16) -0.0017(15) 0.0097(18) C509 0.066(2) 0.084(3) 0.0401(19) -0.0025(17) -0.0017(16) 0.002(2) C510 0.075(3) 0.106(4) 0.049(2) 0.022(2) -0.0122(19) 0.003(3) C511 0.095(3) 0.097(3) 0.070(3) 0.016(2) -0.008(2) 0.042(3) C512 0.083(3) 0.070(3) 0.052(2) 0.0039(18) 0.0054(18) 0.027(2) C601 0.0294(15) 0.0343(17) 0.0338(15) 0.0002(13) 0.0045(11) 0.0009(13) C602 0.057(2) 0.052(2) 0.0366(17) -0.0010(14) 0.0078(14) -0.0156(17) C603 0.076(3) 0.065(3) 0.0468(19) 0.0155(18) 0.0076(16) -0.020(2) C604 0.062(2) 0.040(2) 0.074(2) 0.0123(18) 0.0079(18) -0.0088(17) C605 0.069(2) 0.037(2) 0.064(2) -0.0080(16) 0.0089(17) -0.0104(18) C606 0.063(2) 0.0344(19) 0.0391(16) -0.0022(14) 0.0062(14) -0.0063(16) C607 0.0340(16) 0.0270(16) 0.0335(15) -0.0030(12) 0.0002(12) -0.0040(13) C608 0.0429(18) 0.0426(19) 0.0351(16) 0.0004(13) 0.0025(12) 0.0060(15) C609 0.048(2) 0.053(2) 0.0511(19) 0.0011(15) 0.0088(15) 0.0148(17) C610 0.0403(19) 0.056(2) 0.069(2) -0.0012(17) -0.0117(16) 0.0104(17) C611 0.057(2) 0.077(3) 0.051(2) -0.0135(18) -0.0227(16) 0.011(2) C612 0.049(2) 0.066(2) 0.0409(17) -0.0165(15) -0.0100(14) 0.0109(18) C701 0.0336(16) 0.0341(18) 0.0368(15) -0.0015(13) 0.0061(12) 0.0002(13) C702 0.060(2) 0.043(2) 0.0561(19) 0.0059(16) 0.0222(16) 0.0062(17) C703 0.085(3) 0.036(2) 0.090(3) 0.0126(18) 0.029(2) 0.0099(19) C704 0.069(2) 0.038(2) 0.092(3) -0.017(2) 0.019(2) 0.0098(18) C705 0.068(2) 0.060(3) 0.057(2) -0.0162(18) 0.0128(17) 0.0142(19) C706 0.052(2) 0.047(2) 0.0441(17) -0.0039(14) 0.0098(14) 0.0127(16) C707 0.0323(16) 0.0318(17) 0.0278(14) -0.0037(12) 0.0012(11) 0.0025(13) C708 0.0435(19) 0.049(2) 0.0439(17) 0.0042(14) -0.0037(14) 0.0030(16) C709 0.039(2) 0.062(2) 0.061(2) -0.0039(18) -0.0133(15) -0.0019(17) C710 0.043(2) 0.059(2) 0.063(2) -0.0087(18) 0.0000(16) -0.0192(17) C711 0.066(2) 0.060(2) 0.063(2) 0.0194(18) -0.0089(18) -0.029(2) C712 0.047(2) 0.053(2) 0.0469(18) 0.0098(15) -0.0092(14) -0.0105(17) C801 0.0387(17) 0.0376(19) 0.0260(14) -0.0027(12) 0.0027(11) 0.0027(15) C802 0.0359(18) 0.048(2) 0.0386(16) 0.0001(14) 0.0013(12) 0.0056(15) C803 0.045(2) 0.061(2) 0.0492(18) -0.0011(16) 0.0030(14) -0.0048(18) C804 0.0347(19) 0.088(3) 0.053(2) -0.0064(18) 0.0040(14) 0.001(2) C805 0.046(2) 0.076(3) 0.054(2) -0.0083(18) 0.0029(15) 0.025(2) C806 0.055(2) 0.044(2) 0.0422(17) -0.0066(14) 0.0024(14) 0.0142(17) C807 0.0291(16) 0.0420(19) 0.0338(15) -0.0061(13) 0.0047(11) -0.0012(13) C808 0.0429(18) 0.054(2) 0.0343(16) -0.0032(14) 0.0012(12) -0.0097(15) C809 0.050(2) 0.073(3) 0.0390(18) 0.0071(17) 0.0003(14) -0.0103(18) C810 0.066(2) 0.083(3) 0.0329(17) -0.0145(18) 0.0049(15) -0.015(2) C811 0.085(3) 0.064(3) 0.052(2) -0.0238(19) 0.0071(18) -0.018(2) C812 0.064(2) 0.047(2) 0.0424(18) -0.0110(15) 0.0049(14) -0.0023(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C101 1.825(3) . ? P1 C107 1.835(3) . ? P1 C2 1.864(3) . ? P2 C1 1.702(3) . ? P2 C201 1.797(3) . ? P2 C207 1.803(3) . ? P2 C2 1.810(3) . ? P3 C1 1.692(3) . ? P3 C301 1.795(3) . ? P3 C3 1.808(2) . ? P3 C307 1.809(3) . ? P4 C401 1.828(3) . ? P4 C407 1.833(3) . ? P4 C3 1.861(3) . ? P5 C501 1.825(3) . ? P5 C507 1.839(3) . ? P5 C5 1.860(3) . ? P6 C4 1.701(3) . ? P6 C601 1.795(3) . ? P6 C5 1.812(2) . ? P6 C607 1.812(3) . ? P7 C4 1.707(3) . ? P7 C701 1.793(3) . ? P7 C707 1.811(3) . ? P7 C6 1.813(2) . ? P8 C801 1.832(3) . ? P8 C807 1.837(3) . ? P8 C6 1.857(3) . ? C1 H1 0.75(3) . ? C4 H4 0.84(3) . ? C101 C106 1.388(4) . ? C101 C102 1.395(4) . ? C102 C103 1.384(5) . ? C103 C104 1.384(5) . ? C104 C105 1.362(6) . ? C105 C106 1.372(5) . ? C107 C112 1.363(5) . ? C107 C108 1.388(4) . ? C108 C109 1.385(4) . ? C109 C110 1.363(6) . ? C110 C111 1.347(7) . ? C111 C112 1.366(7) . ? C201 C202 1.383(4) . ? C201 C206 1.397(4) . ? C202 C203 1.382(4) . ? C203 C204 1.363(4) . ? C204 C205 1.380(4) . ? C205 C206 1.372(4) . ? C207 C212 1.367(4) . ? C207 C208 1.386(4) . ? C208 C209 1.373(4) . ? C209 C210 1.357(5) . ? C210 C211 1.362(6) . ? C211 C212 1.386(5) . ? C301 C302 1.384(4) . ? C301 C306 1.389(4) . ? C302 C303 1.388(4) . ? C303 C304 1.370(4) . ? C304 C305 1.371(5) . ? C305 C306 1.378(4) . ? C307 C312 1.384(4) . ? C307 C308 1.393(4) . ? C308 C309 1.375(4) . ? C309 C310 1.370(5) . ? C310 C311 1.366(5) . ? C311 C312 1.396(4) . ? C401 C402 1.384(4) . ? C401 C406 1.393(4) . ? C402 C403 1.387(4) . ? C403 C404 1.376(5) . ? C404 C405 1.363(5) . ? C405 C406 1.375(4) . ? C407 C412 1.384(4) . ? C407 C408 1.391(4) . ? C408 C409 1.387(4) . ? C409 C410 1.376(5) . ? C410 C411 1.356(5) . ? C411 C412 1.392(4) . ? C501 C502 1.383(4) . ? C501 C506 1.391(4) . ? C502 C503 1.395(4) . ? C503 C504 1.376(5) . ? C504 C505 1.357(5) . ? C505 C506 1.373(5) . ? C507 C512 1.376(4) . ? C507 C508 1.388(4) . ? C508 C509 1.382(4) . ? C509 C510 1.351(5) . ? C510 C511 1.365(5) . ? C511 C512 1.394(5) . ? C601 C602 1.384(4) . ? C601 C606 1.390(4) . ? C602 C603 1.377(4) . ? C603 C604 1.367(5) . ? C604 C605 1.373(4) . ? C605 C606 1.373(4) . ? C607 C612 1.386(4) . ? C607 C608 1.386(4) . ? C608 C609 1.370(4) . ? C609 C610 1.373(4) . ? C610 C611 1.368(4) . ? C611 C612 1.379(4) . ? C701 C706 1.387(4) . ? C701 C702 1.389(4) . ? C702 C703 1.385(4) . ? C703 C704 1.370(5) . ? C704 C705 1.372(5) . ? C705 C706 1.383(4) . ? C707 C712 1.375(4) . ? C707 C708 1.395(4) . ? C708 C709 1.383(4) . ? C709 C710 1.363(4) . ? C710 C711 1.363(4) . ? C711 C712 1.383(4) . ? C801 C802 1.387(4) . ? C801 C806 1.397(4) . ? C802 C803 1.384(4) . ? C803 C804 1.373(5) . ? C804 C805 1.376(5) . ? C805 C806 1.386(4) . ? C807 C812 1.385(4) . ? C807 C808 1.389(4) . ? C808 C809 1.393(4) . ? C809 C810 1.373(5) . ? C810 C811 1.362(5) . ? C811 C812 1.392(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C101 P1 C107 102.02(13) . . ? C101 P1 C2 98.51(14) . . ? C107 P1 C2 104.39(13) . . ? C1 P2 C201 114.06(14) . . ? C1 P2 C207 107.08(15) . . ? C201 P2 C207 106.51(13) . . ? C1 P2 C2 116.06(14) . . ? C201 P2 C2 103.83(13) . . ? C207 P2 C2 108.88(13) . . ? C1 P3 C301 112.71(14) . . ? C1 P3 C3 112.94(14) . . ? C301 P3 C3 108.71(12) . . ? C1 P3 C307 112.57(14) . . ? C301 P3 C307 104.64(12) . . ? C3 P3 C307 104.63(12) . . ? C401 P4 C407 101.14(11) . . ? C401 P4 C3 103.28(12) . . ? C407 P4 C3 99.43(12) . . ? C501 P5 C507 102.18(12) . . ? C501 P5 C5 100.15(13) . . ? C507 P5 C5 101.73(12) . . ? C4 P6 C601 113.27(13) . . ? C4 P6 C5 116.50(13) . . ? C601 P6 C5 104.80(12) . . ? C4 P6 C607 107.57(13) . . ? C601 P6 C607 107.86(12) . . ? C5 P6 C607 106.36(12) . . ? C4 P7 C701 111.99(14) . . ? C4 P7 C707 111.54(13) . . ? C701 P7 C707 105.27(12) . . ? C4 P7 C6 113.63(12) . . ? C701 P7 C6 109.17(12) . . ? C707 P7 C6 104.68(12) . . ? C801 P8 C807 99.04(11) . . ? C801 P8 C6 103.81(13) . . ? C807 P8 C6 101.20(12) . . ? H1 C1 P3 115(2) . . ? H1 C1 P2 111(2) . . ? P3 C1 P2 133.8(2) . . ? P2 C2 P1 116.12(15) . . ? P3 C3 P4 111.02(14) . . ? H4 C4 P6 114.2(19) . . ? H4 C4 P7 113.1(19) . . ? P6 C4 P7 132.4(2) . . ? P6 C5 P5 113.05(14) . . ? P7 C6 P8 110.28(14) . . ? C106 C101 C102 117.6(3) . . ? C106 C101 P1 118.0(3) . . ? C102 C101 P1 124.3(2) . . ? C103 C102 C101 121.0(3) . . ? C104 C103 C102 119.8(4) . . ? C105 C104 C103 119.4(4) . . ? C104 C105 C106 121.1(4) . . ? C105 C106 C101 121.1(4) . . ? C112 C107 C108 116.6(3) . . ? C112 C107 P1 117.7(3) . . ? C108 C107 P1 125.6(2) . . ? C109 C108 C107 121.2(3) . . ? C110 C109 C108 119.9(4) . . ? C111 C110 C109 119.1(4) . . ? C110 C111 C112 121.1(4) . . ? C107 C112 C111 122.0(4) . . ? C202 C201 C206 118.5(3) . . ? C202 C201 P2 121.4(2) . . ? C206 C201 P2 120.1(2) . . ? C203 C202 C201 120.6(3) . . ? C204 C203 C202 120.5(3) . . ? C203 C204 C205 119.6(3) . . ? C206 C205 C204 120.7(3) . . ? C205 C206 C201 120.1(3) . . ? C212 C207 C208 118.6(3) . . ? C212 C207 P2 122.7(2) . . ? C208 C207 P2 118.6(2) . . ? C209 C208 C207 121.0(3) . . ? C210 C209 C208 119.8(3) . . ? C209 C210 C211 120.2(3) . . ? C210 C211 C212 120.6(3) . . ? C207 C212 C211 119.9(3) . . ? C302 C301 C306 118.9(3) . . ? C302 C301 P3 122.9(2) . . ? C306 C301 P3 118.1(2) . . ? C301 C302 C303 119.7(3) . . ? C304 C303 C302 120.4(3) . . ? C303 C304 C305 120.5(3) . . ? C304 C305 C306 119.4(3) . . ? C305 C306 C301 121.0(3) . . ? C312 C307 C308 117.9(3) . . ? C312 C307 P3 120.6(2) . . ? C308 C307 P3 121.4(2) . . ? C309 C308 C307 121.4(3) . . ? C310 C309 C308 119.7(3) . . ? C311 C310 C309 120.5(3) . . ? C310 C311 C312 120.0(3) . . ? C307 C312 C311 120.5(3) . . ? C402 C401 C406 118.0(3) . . ? C402 C401 P4 125.1(2) . . ? C406 C401 P4 116.8(2) . . ? C401 C402 C403 120.6(3) . . ? C404 C403 C402 120.1(3) . . ? C405 C404 C403 120.0(3) . . ? C404 C405 C406 120.2(3) . . ? C405 C406 C401 121.1(3) . . ? C412 C407 C408 118.7(2) . . ? C412 C407 P4 116.8(2) . . ? C408 C407 P4 124.6(2) . . ? C409 C408 C407 120.4(3) . . ? C410 C409 C408 119.8(3) . . ? C411 C410 C409 120.5(3) . . ? C410 C411 C412 120.2(3) . . ? C407 C412 C411 120.4(3) . . ? C502 C501 C506 117.9(3) . . ? C502 C501 P5 126.0(2) . . ? C506 C501 P5 116.1(2) . . ? C501 C502 C503 120.4(3) . . ? C504 C503 C502 120.0(3) . . ? C505 C504 C503 120.0(3) . . ? C504 C505 C506 120.4(4) . . ? C505 C506 C501 121.3(3) . . ? C512 C507 C508 117.7(3) . . ? C512 C507 P5 117.4(2) . . ? C508 C507 P5 124.8(2) . . ? C509 C508 C507 120.8(3) . . ? C510 C509 C508 120.6(3) . . ? C509 C510 C511 120.1(3) . . ? C510 C511 C512 119.8(4) . . ? C507 C512 C511 121.0(3) . . ? C602 C601 C606 118.3(3) . . ? C602 C601 P6 120.7(2) . . ? C606 C601 P6 121.0(2) . . ? C603 C602 C601 120.7(3) . . ? C604 C603 C602 120.5(3) . . ? C603 C604 C605 119.4(3) . . ? C604 C605 C606 120.8(3) . . ? C605 C606 C601 120.3(3) . . ? C612 C607 C608 118.3(3) . . ? C612 C607 P6 121.7(2) . . ? C608 C607 P6 119.87(19) . . ? C609 C608 C607 120.5(2) . . ? C608 C609 C610 120.7(3) . . ? C611 C610 C609 119.7(3) . . ? C610 C611 C612 120.0(3) . . ? C611 C612 C607 120.8(3) . . ? C706 C701 C702 118.9(3) . . ? C706 C701 P7 118.2(2) . . ? C702 C701 P7 122.8(2) . . ? C703 C702 C701 119.8(3) . . ? C704 C703 C702 120.8(3) . . ? C703 C704 C705 119.9(3) . . ? C704 C705 C706 120.0(3) . . ? C705 C706 C701 120.6(3) . . ? C712 C707 C708 117.9(3) . . ? C712 C707 P7 122.2(2) . . ? C708 C707 P7 119.7(2) . . ? C709 C708 C707 120.8(3) . . ? C710 C709 C708 120.0(3) . . ? C711 C710 C709 119.9(3) . . ? C710 C711 C712 120.7(3) . . ? C707 C712 C711 120.7(3) . . ? C802 C801 C806 118.1(3) . . ? C802 C801 P8 125.8(2) . . ? C806 C801 P8 116.0(2) . . ? C803 C802 C801 120.8(3) . . ? C804 C803 C802 120.3(3) . . ? C803 C804 C805 120.0(3) . . ? C804 C805 C806 120.0(3) . . ? C805 C806 C801 120.7(3) . . ? C812 C807 C808 118.9(2) . . ? C812 C807 P8 116.9(2) . . ? C808 C807 P8 124.3(2) . . ? C807 C808 C809 120.1(3) . . ? C810 C809 C808 120.0(3) . . ? C811 C810 C809 120.6(3) . . ? C810 C811 C812 119.9(3) . . ? C807 C812 C811 120.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.283 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.047 # Attachment 'dt-art-10-2011-011949-File008-v1-0.CIF' data_7 _database_code_depnum_ccdc_archive 'CCDC 849143' #TrackingRef 'dt-art-10-2011-011949-File008-v1-0.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H47 Cl9 P4 Pt' _chemical_formula_weight 1321.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4233(2) _cell_length_b 15.0455(3) _cell_length_c 19.0383(4) _cell_angle_alpha 90.021(2) _cell_angle_beta 90.644(2) _cell_angle_gamma 96.536(2) _cell_volume 2681.50(10) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 32955 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 3.221 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16937 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9424 _reflns_number_gt 8119 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Hydrogen atom at C1 was found and refined isotropically with bond restraint (d=0.98 angs.). One solvent chloroform was around 2:1 disordered for chlorine atoms (using free varible). The C-Cl (d=1.7 angs.) and Cl-Cl (d=2.75 angs.) were refined with bond restraints and C5=C5A with equal coordinates and displacement factor for hydrogen calculation. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0048P)^2^+6.1925P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'constr, refined at C1' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9424 _refine_ls_number_parameters 636 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.150603(19) -0.206409(11) -0.180336(9) 0.02524(6) Uani 1 1 d . . . Cl1 Cl 0.13552(16) -0.20193(9) -0.05870(6) 0.0501(3) Uani 1 1 d . . . Cl2 Cl -0.44638(14) -0.24571(10) -0.28125(8) 0.0542(4) Uani 1 1 d . . . Cl3 Cl 0.44353(15) 0.17249(10) -0.32444(8) 0.0566(4) Uani 1 1 d . . . P1 P 0.29314(12) -0.07143(7) -0.17713(6) 0.0267(3) Uani 1 1 d . . . P2 P 0.19860(12) -0.09708(7) -0.32186(6) 0.0243(2) Uani 1 1 d . . . P3 P 0.04958(12) -0.29495(7) -0.33606(6) 0.0245(2) Uani 1 1 d . . . P4 P 0.01546(12) -0.34196(7) -0.18694(6) 0.0263(3) Uani 1 1 d . . . C1 C 0.1719(4) -0.2112(3) -0.2902(2) 0.0228(9) Uani 1 1 d D . . H1 H 0.268(3) -0.228(3) -0.295(2) 0.022(11) Uiso 1 1 d D . . C2 C 0.3465(5) -0.0511(3) -0.2681(2) 0.0274(10) Uani 1 1 d . . . H2A H 0.3680 0.0132 -0.2768 0.033 Uiso 1 1 calc . . . H2B H 0.4317 -0.0803 -0.2785 0.033 Uiso 1 1 calc . . . C3 C -0.0790(4) -0.3405(3) -0.2712(2) 0.0282(10) Uani 1 1 d . . . H3A H -0.1188 -0.4013 -0.2844 0.034 Uiso 1 1 calc . . . H3B H -0.1574 -0.3032 -0.2680 0.034 Uiso 1 1 calc . . . C101 C 0.4592(5) -0.0701(3) -0.1277(2) 0.0320(11) Uani 1 1 d . . . C102 C 0.5238(7) -0.1454(4) -0.1219(4) 0.072(2) Uani 1 1 d . . . H102 H 0.4817 -0.1989 -0.1425 0.086 Uiso 1 1 calc . . . C103 C 0.6531(7) -0.1436(4) -0.0853(4) 0.076(2) Uani 1 1 d . . . H103 H 0.6969 -0.1966 -0.0818 0.091 Uiso 1 1 calc . . . C104 C 0.7153(6) -0.0710(4) -0.0556(3) 0.0573(16) Uani 1 1 d . . . H104 H 0.8050 -0.0708 -0.0335 0.069 Uiso 1 1 calc . . . C105 C 0.6488(8) 0.0038(5) -0.0572(5) 0.108(3) Uani 1 1 d . . . H105 H 0.6897 0.0554 -0.0334 0.130 Uiso 1 1 calc . . . C106 C 0.5215(7) 0.0052(4) -0.0934(5) 0.093(3) Uani 1 1 d . . . H106 H 0.4770 0.0580 -0.0947 0.111 Uiso 1 1 calc . . . C107 C 0.2091(5) 0.0255(3) -0.1493(2) 0.0311(11) Uani 1 1 d . . . C108 C 0.0824(5) 0.0142(3) -0.1134(3) 0.0407(12) Uani 1 1 d . . . H108 H 0.0356 -0.0435 -0.1058 0.049 Uiso 1 1 calc . . . C109 C 0.0243(6) 0.0888(4) -0.0885(3) 0.0565(16) Uani 1 1 d . . . H109 H -0.0613 0.0812 -0.0631 0.068 Uiso 1 1 calc . . . C110 C 0.0899(7) 0.1727(4) -0.1003(3) 0.0578(16) Uani 1 1 d . . . H110 H 0.0501 0.2226 -0.0827 0.069 Uiso 1 1 calc . . . C111 C 0.2139(6) 0.1846(3) -0.1379(3) 0.0530(15) Uani 1 1 d . . . H111 H 0.2585 0.2427 -0.1466 0.064 Uiso 1 1 calc . . . C112 C 0.2731(5) 0.1111(3) -0.1630(3) 0.0406(12) Uani 1 1 d . . . H112 H 0.3571 0.1193 -0.1895 0.049 Uiso 1 1 calc . . . C201 C 0.2499(4) -0.0849(3) -0.4120(2) 0.0257(10) Uani 1 1 d . . . C202 C 0.3636(5) -0.1290(3) -0.4356(2) 0.0379(12) Uani 1 1 d . . . H202 H 0.4127 -0.1635 -0.4044 0.046 Uiso 1 1 calc . . . C203 C 0.4027(5) -0.1211(4) -0.5052(3) 0.0463(14) Uani 1 1 d . . . H203 H 0.4779 -0.1513 -0.5216 0.056 Uiso 1 1 calc . . . C204 C 0.3325(6) -0.0696(4) -0.5508(3) 0.0455(13) Uani 1 1 d . . . H204 H 0.3605 -0.0646 -0.5980 0.055 Uiso 1 1 calc . . . C205 C 0.2220(6) -0.0255(4) -0.5277(3) 0.0443(13) Uani 1 1 d . . . H205 H 0.1745 0.0097 -0.5590 0.053 Uiso 1 1 calc . . . C206 C 0.1806(5) -0.0330(3) -0.4585(3) 0.0355(11) Uani 1 1 d . . . H206 H 0.1050 -0.0027 -0.4427 0.043 Uiso 1 1 calc . . . C207 C 0.0478(5) -0.0378(3) -0.3047(2) 0.0270(10) Uani 1 1 d . . . C208 C -0.0831(5) -0.0805(3) -0.2861(3) 0.0346(11) Uani 1 1 d . . . H208 H -0.0968 -0.1433 -0.2835 0.042 Uiso 1 1 calc . . . C209 C -0.1951(5) -0.0315(4) -0.2711(3) 0.0476(14) Uani 1 1 d . . . H209 H -0.2852 -0.0609 -0.2595 0.057 Uiso 1 1 calc . . . C210 C -0.1733(6) 0.0599(4) -0.2732(3) 0.0511(15) Uani 1 1 d . . . H210 H -0.2487 0.0933 -0.2624 0.061 Uiso 1 1 calc . . . C211 C -0.0428(6) 0.1035(3) -0.2910(3) 0.0417(13) Uani 1 1 d . . . H211 H -0.0297 0.1663 -0.2925 0.050 Uiso 1 1 calc . . . C212 C 0.0695(5) 0.0557(3) -0.3066(2) 0.0345(11) Uani 1 1 d . . . H212 H 0.1592 0.0856 -0.3184 0.041 Uiso 1 1 calc . . . C301 C -0.0484(5) -0.2601(3) -0.4110(2) 0.0269(10) Uani 1 1 d . . . C302 C 0.0215(5) -0.2464(3) -0.4746(2) 0.0374(12) Uani 1 1 d . . . H302 H 0.1192 -0.2528 -0.4778 0.045 Uiso 1 1 calc . . . C303 C -0.0548(6) -0.2232(3) -0.5332(3) 0.0461(13) Uani 1 1 d . . . H303 H -0.0071 -0.2117 -0.5760 0.055 Uiso 1 1 calc . . . C304 C -0.1973(7) -0.2168(4) -0.5299(3) 0.0560(16) Uani 1 1 d . . . H304 H -0.2483 -0.2018 -0.5701 0.067 Uiso 1 1 calc . . . C305 C -0.2657(6) -0.2325(5) -0.4672(3) 0.0662(18) Uani 1 1 d . . . H305 H -0.3645 -0.2290 -0.4649 0.079 Uiso 1 1 calc . . . C306 C -0.1924(5) -0.2532(4) -0.4074(3) 0.0486(14) Uani 1 1 d . . . H306 H -0.2405 -0.2626 -0.3646 0.058 Uiso 1 1 calc . . . C307 C 0.1412(5) -0.3858(3) -0.3679(2) 0.0295(10) Uani 1 1 d . . . C308 C 0.2867(6) -0.3858(3) -0.3655(3) 0.0453(13) Uani 1 1 d . . . H308 H 0.3445 -0.3372 -0.3453 0.054 Uiso 1 1 calc . . . C309 C 0.3483(7) -0.4575(4) -0.3927(3) 0.0622(17) Uani 1 1 d . . . H309 H 0.4482 -0.4567 -0.3919 0.075 Uiso 1 1 calc . . . C310 C 0.2656(8) -0.5288(4) -0.4205(3) 0.0624(17) Uani 1 1 d . . . H310 H 0.3081 -0.5780 -0.4374 0.075 Uiso 1 1 calc . . . C311 C 0.1211(8) -0.5294(4) -0.4239(3) 0.0595(17) Uani 1 1 d . . . H311 H 0.0644 -0.5787 -0.4438 0.071 Uiso 1 1 calc . . . C312 C 0.0568(6) -0.4577(3) -0.3982(3) 0.0452(13) Uani 1 1 d . . . H312 H -0.0428 -0.4577 -0.4012 0.054 Uiso 1 1 calc . . . C401 C -0.1183(5) -0.3732(3) -0.1213(2) 0.0312(11) Uani 1 1 d . . . C402 C -0.0696(5) -0.3989(3) -0.0559(3) 0.0403(12) Uani 1 1 d . . . H402 H 0.0282 -0.4033 -0.0483 0.048 Uiso 1 1 calc . . . C403 C -0.1655(7) -0.4180(4) -0.0021(3) 0.0520(15) Uani 1 1 d . . . H403 H -0.1325 -0.4343 0.0423 0.062 Uiso 1 1 calc . . . C404 C -0.3082(7) -0.4134(4) -0.0130(3) 0.0625(17) Uani 1 1 d . . . H404 H -0.3731 -0.4274 0.0236 0.075 Uiso 1 1 calc . . . C405 C -0.3559(6) -0.3883(4) -0.0770(3) 0.0638(17) Uani 1 1 d . . . H405 H -0.4540 -0.3850 -0.0842 0.077 Uiso 1 1 calc . . . C406 C -0.2623(5) -0.3677(4) -0.1320(3) 0.0452(13) Uani 1 1 d . . . H406 H -0.2964 -0.3503 -0.1758 0.054 Uiso 1 1 calc . . . C407 C 0.1209(5) -0.4351(3) -0.1926(2) 0.0310(11) Uani 1 1 d . . . C408 C 0.2672(6) -0.4205(3) -0.1856(3) 0.0478(14) Uani 1 1 d . . . H408 H 0.3119 -0.3630 -0.1748 0.057 Uiso 1 1 calc . . . C409 C 0.3493(6) -0.4910(4) -0.1944(3) 0.0588(16) Uani 1 1 d . . . H409 H 0.4493 -0.4807 -0.1902 0.071 Uiso 1 1 calc . . . C410 C 0.2858(7) -0.5742(4) -0.2091(3) 0.0564(16) Uani 1 1 d . . . H410 H 0.3418 -0.6212 -0.2159 0.068 Uiso 1 1 calc . . . C411 C 0.1401(7) -0.5899(4) -0.2139(4) 0.0618(17) Uani 1 1 d . . . H411 H 0.0960 -0.6482 -0.2224 0.074 Uiso 1 1 calc . . . C412 C 0.0573(6) -0.5199(3) -0.2064(3) 0.0501(15) Uani 1 1 d . . . H412 H -0.0426 -0.5308 -0.2107 0.060 Uiso 1 1 calc . . . C4 C 0.3332(6) -0.3557(4) -0.6490(3) 0.0565(16) Uani 1 1 d . . . H4 H 0.4084 -0.3068 -0.6608 0.068 Uiso 1 1 calc . . . Cl4 Cl 0.3506(2) -0.44878(12) -0.70241(12) 0.0884(6) Uani 1 1 d . . . Cl5 Cl 0.1656(2) -0.32062(13) -0.66469(12) 0.0926(6) Uani 1 1 d . . . Cl6 Cl 0.3497(3) -0.38415(15) -0.56054(11) 0.1025(7) Uani 1 1 d . . . C5 C 0.3107(8) -0.2758(5) 0.0921(4) 0.083(2) Uani 0.67 1 d PD A 1 H5 H 0.2550 -0.2294 0.0727 0.100 Uiso 0.67 1 calc P B 1 Cl7 Cl 0.1992(8) -0.3718(3) 0.0960(3) 0.179(4) Uani 0.669(7) 1 d PD A 1 Cl8 Cl 0.3704(4) -0.2401(2) 0.17564(15) 0.0796(13) Uani 0.669(7) 1 d PD A 1 Cl9 Cl 0.4500(7) -0.2792(8) 0.0415(3) 0.228(5) Uani 0.669(7) 1 d PD A 1 C5A C 0.3107(8) -0.2758(5) 0.0921(4) 0.083(2) Uani 0.33 1 d P A 2 H5A H 0.2391 -0.2698 0.0544 0.100 Uiso 0.33 1 calc P C 2 Cl7A Cl 0.3134(16) -0.3965(5) 0.0939(12) 0.281(12) Uani 0.331(7) 1 d PD A 2 Cl8A Cl 0.2337(19) -0.2457(7) 0.1553(7) 0.191(8) Uani 0.331(7) 1 d PD A 2 Cl9A Cl 0.4581(11) -0.2415(5) 0.0517(8) 0.128(5) Uani 0.331(7) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02978(10) 0.02257(10) 0.02253(10) 0.00151(7) 0.00017(7) -0.00058(7) Cl1 0.0803(10) 0.0429(8) 0.0228(6) 0.0007(6) 0.0035(6) -0.0114(7) Cl2 0.0356(7) 0.0663(9) 0.0597(9) 0.0011(7) -0.0005(6) 0.0013(6) Cl3 0.0569(9) 0.0567(9) 0.0516(9) 0.0125(7) 0.0063(7) -0.0147(7) P1 0.0300(6) 0.0232(6) 0.0261(6) 0.0002(5) 0.0003(5) -0.0010(5) P2 0.0255(6) 0.0236(6) 0.0238(6) 0.0036(5) 0.0024(5) 0.0031(5) P3 0.0256(6) 0.0230(6) 0.0250(6) 0.0010(5) -0.0027(5) 0.0031(5) P4 0.0297(6) 0.0224(6) 0.0259(6) 0.0035(5) -0.0013(5) -0.0009(5) C1 0.022(2) 0.019(2) 0.027(2) 0.0014(18) 0.0011(18) 0.0022(17) C2 0.030(2) 0.023(2) 0.029(3) 0.0005(19) 0.0047(19) 0.0019(19) C3 0.024(2) 0.028(2) 0.033(3) 0.003(2) -0.0001(19) 0.0014(19) C101 0.030(3) 0.034(3) 0.031(3) -0.001(2) -0.001(2) 0.000(2) C102 0.075(4) 0.038(3) 0.102(6) -0.010(3) -0.044(4) 0.012(3) C103 0.060(4) 0.054(4) 0.116(6) -0.005(4) -0.046(4) 0.019(3) C104 0.032(3) 0.068(4) 0.070(4) 0.006(3) -0.014(3) 0.000(3) C105 0.069(5) 0.076(5) 0.176(9) -0.034(6) -0.069(6) 0.004(4) C106 0.064(4) 0.051(4) 0.161(8) -0.020(5) -0.055(5) 0.007(3) C107 0.034(3) 0.028(3) 0.031(3) -0.004(2) 0.000(2) -0.001(2) C108 0.043(3) 0.031(3) 0.047(3) -0.001(2) 0.009(2) -0.003(2) C109 0.054(4) 0.048(4) 0.069(4) -0.007(3) 0.022(3) 0.011(3) C110 0.064(4) 0.040(3) 0.073(4) -0.008(3) 0.010(3) 0.021(3) C111 0.063(4) 0.024(3) 0.072(4) -0.001(3) 0.005(3) 0.005(3) C112 0.040(3) 0.035(3) 0.045(3) -0.001(2) 0.009(2) -0.005(2) C201 0.029(2) 0.025(2) 0.023(2) 0.0011(19) 0.0023(19) 0.0014(19) C202 0.037(3) 0.049(3) 0.030(3) 0.008(2) 0.000(2) 0.011(2) C203 0.039(3) 0.067(4) 0.036(3) 0.004(3) 0.012(2) 0.019(3) C204 0.047(3) 0.067(4) 0.023(3) 0.008(3) 0.005(2) 0.008(3) C205 0.049(3) 0.056(3) 0.030(3) 0.016(2) -0.002(2) 0.014(3) C206 0.039(3) 0.032(3) 0.037(3) 0.004(2) 0.003(2) 0.011(2) C207 0.031(3) 0.024(2) 0.027(2) 0.0013(19) 0.0032(19) 0.0051(19) C208 0.029(3) 0.036(3) 0.039(3) 0.000(2) 0.001(2) 0.003(2) C209 0.030(3) 0.053(4) 0.062(4) -0.005(3) 0.010(3) 0.010(2) C210 0.047(3) 0.056(4) 0.055(4) -0.007(3) 0.003(3) 0.028(3) C211 0.057(3) 0.030(3) 0.041(3) 0.002(2) 0.001(3) 0.016(2) C212 0.039(3) 0.033(3) 0.033(3) 0.004(2) 0.002(2) 0.008(2) C301 0.034(3) 0.022(2) 0.024(2) 0.0008(19) -0.0044(19) 0.0017(19) C302 0.044(3) 0.038(3) 0.030(3) 0.002(2) -0.004(2) 0.002(2) C303 0.071(4) 0.041(3) 0.026(3) 0.002(2) -0.006(3) 0.003(3) C304 0.066(4) 0.058(4) 0.047(4) 0.004(3) -0.022(3) 0.020(3) C305 0.043(3) 0.097(5) 0.062(4) 0.009(4) -0.014(3) 0.028(3) C306 0.039(3) 0.074(4) 0.036(3) 0.010(3) -0.002(2) 0.022(3) C307 0.037(3) 0.028(2) 0.025(2) 0.001(2) 0.000(2) 0.009(2) C308 0.045(3) 0.040(3) 0.053(3) -0.011(3) -0.004(3) 0.013(2) C309 0.058(4) 0.064(4) 0.072(4) -0.016(3) -0.007(3) 0.037(3) C310 0.090(5) 0.040(4) 0.062(4) -0.010(3) 0.001(4) 0.029(3) C311 0.098(5) 0.028(3) 0.051(4) -0.011(3) 0.003(3) 0.001(3) C312 0.046(3) 0.033(3) 0.055(3) -0.013(3) 0.000(3) -0.002(2) C401 0.034(3) 0.025(2) 0.034(3) 0.007(2) 0.005(2) -0.001(2) C402 0.041(3) 0.041(3) 0.039(3) 0.011(2) 0.001(2) 0.003(2) C403 0.071(4) 0.052(4) 0.032(3) 0.013(3) 0.008(3) 0.000(3) C404 0.061(4) 0.076(4) 0.049(4) 0.015(3) 0.021(3) -0.001(3) C405 0.043(3) 0.085(5) 0.064(4) 0.010(4) 0.018(3) 0.008(3) C406 0.041(3) 0.056(3) 0.038(3) 0.006(3) 0.003(2) 0.002(3) C407 0.037(3) 0.028(3) 0.028(3) 0.006(2) -0.002(2) 0.004(2) C408 0.044(3) 0.037(3) 0.062(4) 0.003(3) -0.003(3) 0.005(2) C409 0.045(3) 0.053(4) 0.081(5) 0.011(3) 0.007(3) 0.016(3) C410 0.061(4) 0.041(3) 0.072(4) 0.010(3) 0.010(3) 0.022(3) C411 0.074(4) 0.027(3) 0.084(5) 0.003(3) -0.015(4) 0.007(3) C412 0.041(3) 0.033(3) 0.075(4) 0.004(3) -0.016(3) 0.003(2) C4 0.049(3) 0.043(3) 0.077(4) 0.007(3) 0.011(3) -0.001(3) Cl4 0.0727(12) 0.0701(12) 0.1247(17) -0.0253(11) 0.0106(11) 0.0178(9) Cl5 0.0691(12) 0.0929(14) 0.1237(17) 0.0198(12) 0.0213(11) 0.0410(10) Cl6 0.1228(18) 0.1102(17) 0.0777(14) 0.0258(12) 0.0063(12) 0.0258(14) C5 0.077(5) 0.073(5) 0.100(6) 0.007(4) 0.014(4) 0.007(4) Cl7 0.242(7) 0.102(3) 0.165(5) 0.057(3) -0.120(5) -0.095(4) Cl8 0.100(3) 0.0757(19) 0.0582(17) -0.0025(13) 0.0142(16) -0.0127(17) Cl9 0.122(5) 0.490(14) 0.090(4) -0.070(7) 0.014(3) 0.109(7) C5A 0.077(5) 0.073(5) 0.100(6) 0.007(4) 0.014(4) 0.007(4) Cl7A 0.183(12) 0.061(5) 0.60(3) -0.047(10) 0.206(16) -0.017(6) Cl8A 0.258(19) 0.166(10) 0.166(10) -0.008(8) 0.105(12) 0.085(11) Cl9A 0.074(5) 0.055(4) 0.249(15) -0.012(5) 0.030(7) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.106(4) . ? Pt1 P4 2.2808(11) . ? Pt1 P1 2.3042(12) . ? Pt1 Cl1 2.3231(12) . ? P1 C101 1.815(5) . ? P1 C107 1.819(4) . ? P1 C2 1.826(4) . ? P2 C201 1.792(4) . ? P2 C2 1.793(5) . ? P2 C207 1.794(4) . ? P2 C1 1.811(4) . ? P3 C301 1.801(4) . ? P3 C307 1.806(4) . ? P3 C3 1.819(4) . ? P3 C1 1.823(4) . ? P4 C401 1.809(4) . ? P4 C407 1.811(4) . ? P4 C3 1.826(5) . ? C1 H1 0.971(19) . ? C101 C102 1.349(7) . ? C101 C106 1.375(8) . ? C102 C103 1.395(8) . ? C103 C104 1.305(8) . ? C104 C105 1.348(9) . ? C105 C106 1.379(9) . ? C107 C108 1.376(6) . ? C107 C112 1.385(6) . ? C108 C109 1.388(7) . ? C109 C110 1.361(8) . ? C110 C111 1.372(8) . ? C111 C112 1.381(7) . ? C201 C206 1.386(6) . ? C201 C202 1.401(6) . ? C202 C203 1.380(7) . ? C203 C204 1.378(7) . ? C204 C205 1.373(7) . ? C205 C206 1.380(7) . ? C207 C208 1.375(6) . ? C207 C212 1.400(6) . ? C208 C209 1.387(6) . ? C209 C210 1.368(8) . ? C210 C211 1.372(8) . ? C211 C212 1.380(6) . ? C301 C306 1.375(7) . ? C301 C302 1.389(6) . ? C302 C303 1.388(7) . ? C303 C304 1.360(8) . ? C304 C305 1.371(8) . ? C305 C306 1.379(8) . ? C307 C308 1.372(7) . ? C307 C312 1.387(7) . ? C308 C309 1.384(7) . ? C309 C310 1.356(9) . ? C310 C311 1.362(9) . ? C311 C312 1.388(7) . ? C401 C406 1.381(7) . ? C401 C402 1.393(7) . ? C402 C403 1.382(7) . ? C403 C404 1.367(8) . ? C404 C405 1.364(9) . ? C405 C406 1.388(7) . ? C407 C412 1.372(7) . ? C407 C408 1.376(7) . ? C408 C409 1.393(7) . ? C409 C410 1.352(8) . ? C410 C411 1.369(8) . ? C411 C412 1.387(7) . ? C4 Cl5 1.744(6) . ? C4 Cl6 1.747(7) . ? C4 Cl4 1.754(6) . ? C5 Cl9 1.642(9) . ? C5 Cl7 1.689(8) . ? C5 Cl8 1.746(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P4 88.10(11) . . ? C1 Pt1 P1 90.08(11) . . ? P4 Pt1 P1 177.66(4) . . ? C1 Pt1 Cl1 177.97(12) . . ? P4 Pt1 Cl1 92.55(4) . . ? P1 Pt1 Cl1 89.22(4) . . ? C101 P1 C107 107.1(2) . . ? C101 P1 C2 105.2(2) . . ? C107 P1 C2 106.5(2) . . ? C101 P1 Pt1 115.79(15) . . ? C107 P1 Pt1 116.70(15) . . ? C2 P1 Pt1 104.52(15) . . ? C201 P2 C2 108.1(2) . . ? C201 P2 C207 110.6(2) . . ? C2 P2 C207 109.0(2) . . ? C201 P2 C1 115.2(2) . . ? C2 P2 C1 101.3(2) . . ? C207 P2 C1 112.0(2) . . ? C301 P3 C307 104.9(2) . . ? C301 P3 C3 108.0(2) . . ? C307 P3 C3 107.7(2) . . ? C301 P3 C1 118.3(2) . . ? C307 P3 C1 111.4(2) . . ? C3 P3 C1 106.2(2) . . ? C401 P4 C407 105.8(2) . . ? C401 P4 C3 106.7(2) . . ? C407 P4 C3 105.3(2) . . ? C401 P4 Pt1 120.02(16) . . ? C407 P4 Pt1 113.27(16) . . ? C3 P4 Pt1 104.77(14) . . ? H1 C1 P2 101(2) . . ? H1 C1 P3 107(2) . . ? P2 C1 P3 120.4(2) . . ? H1 C1 Pt1 102(2) . . ? P2 C1 Pt1 107.7(2) . . ? P3 C1 Pt1 115.9(2) . . ? P2 C2 P1 106.4(2) . . ? P3 C3 P4 107.4(2) . . ? C102 C101 C106 117.6(5) . . ? C102 C101 P1 120.0(4) . . ? C106 C101 P1 122.3(4) . . ? C101 C102 C103 119.9(5) . . ? C104 C103 C102 122.2(6) . . ? C103 C104 C105 119.0(6) . . ? C104 C105 C106 120.6(6) . . ? C101 C106 C105 120.5(6) . . ? C108 C107 C112 119.5(4) . . ? C108 C107 P1 120.1(4) . . ? C112 C107 P1 120.4(3) . . ? C107 C108 C109 119.5(5) . . ? C110 C109 C108 120.8(5) . . ? C109 C110 C111 120.2(5) . . ? C110 C111 C112 119.8(5) . . ? C111 C112 C107 120.3(5) . . ? C206 C201 C202 119.5(4) . . ? C206 C201 P2 121.8(3) . . ? C202 C201 P2 118.6(3) . . ? C203 C202 C201 119.1(4) . . ? C204 C203 C202 120.7(4) . . ? C205 C204 C203 120.3(4) . . ? C204 C205 C206 119.9(4) . . ? C205 C206 C201 120.4(4) . . ? C208 C207 C212 119.9(4) . . ? C208 C207 P2 122.6(3) . . ? C212 C207 P2 117.4(3) . . ? C207 C208 C209 120.4(4) . . ? C210 C209 C208 119.4(5) . . ? C209 C210 C211 120.8(4) . . ? C210 C211 C212 120.5(5) . . ? C211 C212 C207 119.0(4) . . ? C306 C301 C302 119.8(4) . . ? C306 C301 P3 121.2(4) . . ? C302 C301 P3 118.9(3) . . ? C303 C302 C301 119.2(5) . . ? C304 C303 C302 121.0(5) . . ? C303 C304 C305 119.1(5) . . ? C304 C305 C306 121.4(5) . . ? C301 C306 C305 119.4(5) . . ? C308 C307 C312 119.6(4) . . ? C308 C307 P3 123.8(4) . . ? C312 C307 P3 116.6(4) . . ? C307 C308 C309 119.9(5) . . ? C310 C309 C308 120.5(6) . . ? C309 C310 C311 120.2(5) . . ? C310 C311 C312 120.4(5) . . ? C307 C312 C311 119.3(5) . . ? C406 C401 C402 119.7(4) . . ? C406 C401 P4 123.3(4) . . ? C402 C401 P4 116.9(4) . . ? C403 C402 C401 119.7(5) . . ? C404 C403 C402 120.6(5) . . ? C405 C404 C403 119.7(5) . . ? C404 C405 C406 121.2(5) . . ? C401 C406 C405 119.1(5) . . ? C412 C407 C408 119.2(4) . . ? C412 C407 P4 120.8(4) . . ? C408 C407 P4 120.0(4) . . ? C407 C408 C409 120.1(5) . . ? C410 C409 C408 120.3(5) . . ? C409 C410 C411 120.1(5) . . ? C410 C411 C412 120.2(5) . . ? C407 C412 C411 120.2(5) . . ? Cl5 C4 Cl6 109.8(3) . . ? Cl5 C4 Cl4 108.6(4) . . ? Cl6 C4 Cl4 110.2(3) . . ? Cl9 C5 Cl7 115.2(6) . . ? Cl9 C5 Cl8 108.6(5) . . ? Cl7 C5 Cl8 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.680 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.099