# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tzi Sum Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Na+ and Ca2+ Ion Selective Pyridylcarboxylate Rings of Pd(II) and Pt(II) ; loop_ _publ_author_name 'Tzi Sum Andy Hor' 'L L Koh' 'Peili Teo' # Attachment 'complex4_new.cif' data_7461 _database_code_depnum_ccdc_archive 'CCDC 711710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H86 Cl12 F9 Fe2 N2 Na O14 P4 Pt2 S3' _chemical_formula_weight 2820.99 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 12.4821(17) _cell_length_b 20.550(3) _cell_length_c 21.713(3) _cell_angle_alpha 94.943(2) _cell_angle_beta 94.756(2) _cell_angle_gamma 100.886(2) _cell_volume 5420.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6917 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 22.70 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2788 _exptl_absorpt_coefficient_mu 3.327 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4352 _exptl_absorpt_correction_T_max 0.7767 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66108 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.50 _reflns_number_total 24861 _reflns_number_gt 16166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The free Otf is disordered, so is one of the CHCL3. The disorder of the two appeared to be linked as the ratios of the two disorder sets are almost the same. Restraints in Bond length and thermal parameters were applied to the disordered otf, CHCL3 and ether. Minors parts of the disordered otf and CHCL3 were kept isotropic. ; _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^)+(0.0787P)^2^+12.8846P] 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 24861 _refine_ls_number_parameters 1346 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1758 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.006 _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 0.24951(3) 0.483439(15) 0.712049(15) 0.02711(9) Uani 1 1 d . . . Pt2 Pt 0.25965(3) 0.900756(15) 0.770657(16) 0.02927(10) Uani 1 1 d . . . Fe1 Fe 0.44887(10) 0.35398(6) 0.63940(6) 0.0329(3) Uani 1 1 d . . . Fe2 Fe 0.34314(11) 1.07387(6) 0.67757(6) 0.0356(3) Uani 1 1 d . . . Na1 Na 0.3867(2) 0.71450(13) 0.66719(13) 0.0219(6) Uani 1 1 d . . . P1 P 0.35972(17) 0.42836(10) 0.76394(10) 0.0275(5) Uani 1 1 d . . . P2 P 0.22022(18) 0.41910(10) 0.61998(10) 0.0281(5) Uani 1 1 d . . . P3 P 0.39659(19) 0.99017(10) 0.80013(10) 0.0301(5) Uani 1 1 d . . . P4 P 0.14814(19) 0.95068(11) 0.71320(12) 0.0357(5) Uani 1 1 d . . . N1 N 0.2627(5) 0.5567(3) 0.7855(3) 0.0295(15) Uani 1 1 d . . . N2 N 0.1506(6) 0.8108(3) 0.7536(3) 0.0302(16) Uani 1 1 d . . . O1 O 0.3515(5) 0.8548(3) 0.8297(3) 0.0341(14) Uani 1 1 d . . . O2 O 0.3779(5) 0.7769(3) 0.7577(3) 0.0387(15) Uani 1 1 d . . . O3 O 0.2416(5) 0.6276(3) 0.6657(3) 0.0389(15) Uani 1 1 d . . . O4 O 0.1331(5) 0.5292(3) 0.6699(3) 0.0350(14) Uani 1 1 d . . . C1 C 0.3529(7) 0.6045(4) 0.7948(4) 0.0316(19) Uani 1 1 d . . . H1 H 0.4091 0.6019 0.7697 0.038 Uiso 1 1 calc R . . C2 C 0.3665(7) 0.6581(4) 0.8404(4) 0.0297(18) Uani 1 1 d . . . C3 C 0.2803(8) 0.6609(5) 0.8761(4) 0.042(2) Uani 1 1 d . . . H3 H 0.2853 0.6959 0.9070 0.051 Uiso 1 1 calc R . . C4 C 0.1865(8) 0.6115(5) 0.8658(5) 0.049(3) Uani 1 1 d . . . H4 H 0.1282 0.6131 0.8895 0.058 Uiso 1 1 calc R . . C5 C 0.1811(7) 0.5604(5) 0.8200(4) 0.039(2) Uani 1 1 d . . . H5 H 0.1182 0.5272 0.8130 0.047 Uiso 1 1 calc R . . C6 C 0.4722(7) 0.7083(4) 0.8490(4) 0.033(2) Uani 1 1 d . . . H6A H 0.5095 0.7046 0.8118 0.040 Uiso 1 1 calc R . . H6B H 0.5188 0.6976 0.8832 0.040 Uiso 1 1 calc R . . C7 C 0.4582(8) 0.7804(4) 0.8623(4) 0.038(2) Uani 1 1 d . . . H7A H 0.4240 0.7846 0.9006 0.045 Uiso 1 1 calc R . . H7B H 0.5300 0.8093 0.8684 0.045 Uiso 1 1 calc R . . C8 C 0.3898(7) 0.8034(4) 0.8111(4) 0.0295(18) Uani 1 1 d . . . C9 C 0.1389(7) 0.7761(4) 0.6970(4) 0.034(2) Uani 1 1 d . . . H9 H 0.1811 0.7934 0.6666 0.041 Uiso 1 1 calc R . . C10 C 0.0661(7) 0.7155(4) 0.6824(4) 0.0331(19) Uani 1 1 d . . . C11 C 0.0078(8) 0.6915(5) 0.7289(5) 0.046(2) Uani 1 1 d . . . H11 H -0.0418 0.6511 0.7213 0.056 Uiso 1 1 calc R . . C12 C 0.0215(9) 0.7260(5) 0.7858(5) 0.051(3) Uani 1 1 d . . . H12 H -0.0193 0.7091 0.8169 0.061 Uiso 1 1 calc R . . C13 C 0.0945(8) 0.7851(5) 0.7983(5) 0.042(2) Uani 1 1 d . . . H13 H 0.1050 0.8075 0.8381 0.051 Uiso 1 1 calc R . . C14 C 0.0608(8) 0.6799(4) 0.6184(4) 0.038(2) Uani 1 1 d . . . H14A H 0.1247 0.6994 0.5989 0.046 Uiso 1 1 calc R . . H14B H -0.0036 0.6870 0.5937 0.046 Uiso 1 1 calc R . . C15 C 0.0564(7) 0.6060(4) 0.6177(4) 0.035(2) Uani 1 1 d . . . H15A H 0.0542 0.5868 0.5751 0.043 Uiso 1 1 calc R . . H15B H -0.0107 0.5857 0.6340 0.043 Uiso 1 1 calc R . . C16 C 0.1533(7) 0.5895(4) 0.6557(4) 0.0320(19) Uani 1 1 d . . . C17 C 0.4684(7) 0.4042(4) 0.7234(4) 0.0332(19) Uani 1 1 d . . . C18 C 0.5104(7) 0.3450(4) 0.7273(4) 0.035(2) Uani 1 1 d . . . H18 H 0.4851 0.3089 0.7526 0.042 Uiso 1 1 calc R . . C19 C 0.5937(8) 0.3474(5) 0.6880(5) 0.047(2) Uani 1 1 d . . . H19 H 0.6358 0.3124 0.6801 0.057 Uiso 1 1 calc R . . C20 C 0.6060(8) 0.4085(5) 0.6602(5) 0.045(2) Uani 1 1 d . . . H20 H 0.6580 0.4231 0.6303 0.054 Uiso 1 1 calc R . . C21 C 0.5291(8) 0.4432(5) 0.6828(4) 0.041(2) Uani 1 1 d . . . H21 H 0.5181 0.4869 0.6719 0.049 Uiso 1 1 calc R . . C22 C 0.3008(7) 0.3593(4) 0.5972(4) 0.0305(19) Uani 1 1 d . . . C23 C 0.2981(7) 0.2952(4) 0.6190(4) 0.034(2) Uani 1 1 d . . . H23 H 0.2507 0.2759 0.6493 0.041 Uiso 1 1 calc R . . C24 C 0.3760(8) 0.2641(4) 0.5893(4) 0.043(2) Uani 1 1 d . . . H24 H 0.3925 0.2204 0.5961 0.051 Uiso 1 1 calc R . . C25 C 0.4266(8) 0.3085(5) 0.5491(5) 0.043(2) Uani 1 1 d . . . H25 H 0.4851 0.3010 0.5236 0.052 Uiso 1 1 calc R . . C26 C 0.3814(8) 0.3673(4) 0.5543(4) 0.037(2) Uani 1 1 d . . . H26 H 0.4021 0.4064 0.5319 0.045 Uiso 1 1 calc R . . C27 C 0.4119(7) 1.0646(4) 0.7637(4) 0.035(2) Uani 1 1 d . . . C28 C 0.4956(8) 1.0891(5) 0.7241(5) 0.044(2) Uani 1 1 d . . . H28 H 0.5544 1.0662 0.7126 0.053 Uiso 1 1 calc R . . C29 C 0.4775(9) 1.1498(5) 0.7030(5) 0.051(3) Uani 1 1 d . . . H29 H 0.5209 1.1759 0.6748 0.062 Uiso 1 1 calc R . . C30 C 0.3859(9) 1.1660(5) 0.7301(5) 0.050(3) Uani 1 1 d . . . H30 H 0.3538 1.2049 0.7226 0.060 Uiso 1 1 calc R . . C31 C 0.3409(8) 1.1135(4) 0.7655(4) 0.040(2) Uani 1 1 d . . . H31 H 0.2761 1.1118 0.7884 0.048 Uiso 1 1 calc R . . C32 C 0.2134(7) 0.9995(4) 0.6572(4) 0.037(2) Uani 1 1 d . . . C33 C 0.1898(8) 1.0576(5) 0.6323(5) 0.050(3) Uani 1 1 d . . . H33 H 0.1309 1.0806 0.6431 0.060 Uiso 1 1 calc R . . C34 C 0.2652(9) 1.0766(5) 0.5905(5) 0.056(3) Uani 1 1 d . . . H34 H 0.2696 1.1163 0.5681 0.067 Uiso 1 1 calc R . . C35 C 0.3358(10) 1.0325(5) 0.5869(5) 0.053(3) Uani 1 1 d . . . H35 H 0.3974 1.0353 0.5614 0.063 Uiso 1 1 calc R . . C36 C 0.3050(8) 0.9828(5) 0.6280(4) 0.041(2) Uani 1 1 d . . . H36 H 0.3396 0.9446 0.6346 0.049 Uiso 1 1 calc R . . C1A C 0.4314(7) 0.4780(4) 0.8333(4) 0.034(2) Uani 1 1 d . . . C2A C 0.3782(8) 0.4835(4) 0.8860(4) 0.040(2) Uani 1 1 d . . . H2A H 0.3082 0.4584 0.8870 0.048 Uiso 1 1 calc R . . C3A C 0.4281(10) 0.5260(5) 0.9374(5) 0.053(3) Uani 1 1 d . . . H3A H 0.3913 0.5297 0.9727 0.064 Uiso 1 1 calc R . . C4A C 0.5318(10) 0.5630(5) 0.9367(5) 0.057(3) Uani 1 1 d . . . H4A H 0.5651 0.5918 0.9712 0.068 Uiso 1 1 calc R . . C5A C 0.5860(9) 0.5572(5) 0.8845(6) 0.057(3) Uani 1 1 d . . . H5A H 0.6562 0.5822 0.8839 0.068 Uiso 1 1 calc R . . C6A C 0.5375(7) 0.5148(4) 0.8333(5) 0.040(2) Uani 1 1 d . . . H6A1 H 0.5754 0.5106 0.7985 0.048 Uiso 1 1 calc R . . C1B C 0.2870(7) 0.3524(4) 0.7906(4) 0.0310(18) Uani 1 1 d . . . C2B C 0.3356(8) 0.3216(5) 0.8369(4) 0.044(2) Uani 1 1 d . . . H2B H 0.4057 0.3411 0.8551 0.053 Uiso 1 1 calc R . . C3B C 0.2845(9) 0.2645(5) 0.8563(5) 0.053(3) Uani 1 1 d . . . H3B H 0.3183 0.2459 0.8882 0.063 Uiso 1 1 calc R . . C4B C 0.1812(9) 0.2334(5) 0.8287(6) 0.059(3) Uani 1 1 d . . . H4B H 0.1461 0.1934 0.8412 0.070 Uiso 1 1 calc R . . C5B C 0.1318(9) 0.2624(5) 0.7829(6) 0.059(3) Uani 1 1 d . . . H5B H 0.0627 0.2419 0.7639 0.071 Uiso 1 1 calc R . . C6B C 0.1848(8) 0.3229(5) 0.7644(5) 0.047(2) Uani 1 1 d . . . H6B1 H 0.1498 0.3430 0.7341 0.057 Uiso 1 1 calc R . . C1C C 0.0807(7) 0.3710(4) 0.6059(4) 0.033(2) Uani 1 1 d . . . C2C C 0.0509(8) 0.3222(4) 0.5566(4) 0.041(2) Uani 1 1 d . . . H2C H 0.1023 0.3132 0.5302 0.049 Uiso 1 1 calc R . . C3C C -0.0563(9) 0.2866(5) 0.5466(5) 0.055(3) Uani 1 1 d . . . H3C H -0.0767 0.2543 0.5129 0.067 Uiso 1 1 calc R . . C4C C -0.1320(8) 0.2985(5) 0.5856(5) 0.050(3) Uani 1 1 d . . . H4C H -0.2032 0.2737 0.5789 0.060 Uiso 1 1 calc R . . C5C C -0.1033(8) 0.3470(5) 0.6349(5) 0.049(3) Uani 1 1 d . . . H5C H -0.1555 0.3556 0.6610 0.058 Uiso 1 1 calc R . . C6C C 0.0034(7) 0.3832(4) 0.6458(4) 0.037(2) Uani 1 1 d . . . H6C H 0.0231 0.4155 0.6797 0.044 Uiso 1 1 calc R . . C1D C 0.2376(7) 0.4769(4) 0.5616(4) 0.0304(18) Uani 1 1 d . . . C2D C 0.1589(8) 0.4772(4) 0.5131(4) 0.042(2) Uani 1 1 d . . . H2D H 0.0966 0.4436 0.5063 0.050 Uiso 1 1 calc R . . C3D C 0.1731(9) 0.5277(5) 0.4749(5) 0.051(3) Uani 1 1 d . . . H3D H 0.1206 0.5276 0.4419 0.061 Uiso 1 1 calc R . . C4D C 0.2639(8) 0.5782(4) 0.4850(4) 0.042(2) Uani 1 1 d . . . H4D H 0.2714 0.6127 0.4596 0.050 Uiso 1 1 calc R . . C5D C 0.3421(8) 0.5780(5) 0.5314(4) 0.039(2) Uani 1 1 d . . . H5D H 0.4046 0.6115 0.5368 0.046 Uiso 1 1 calc R . . C6D C 0.3308(8) 0.5284(4) 0.5712(4) 0.039(2) Uani 1 1 d . . . H6D H 0.3842 0.5293 0.6039 0.047 Uiso 1 1 calc R . . C1E C 0.5248(7) 0.9634(4) 0.7914(5) 0.038(2) Uani 1 1 d . . . C2E C 0.5330(8) 0.9200(5) 0.7411(5) 0.049(3) Uani 1 1 d . . . H2E H 0.4723 0.9046 0.7122 0.058 Uiso 1 1 calc R . . C3E C 0.6268(11) 0.8993(7) 0.7330(6) 0.071(4) Uani 1 1 d . . . H3E H 0.6301 0.8687 0.6994 0.086 Uiso 1 1 calc R . . C4E C 0.7175(11) 0.9231(9) 0.7738(8) 0.096(5) Uani 1 1 d . . . H4E H 0.7831 0.9097 0.7673 0.115 Uiso 1 1 calc R . . C5E C 0.7127(10) 0.9666(9) 0.8243(7) 0.087(5) Uani 1 1 d . . . H5E H 0.7746 0.9823 0.8523 0.105 Uiso 1 1 calc R . . C6E C 0.6166(8) 0.9868(6) 0.8336(5) 0.055(3) Uani 1 1 d . . . H6E H 0.6127 1.0161 0.8681 0.066 Uiso 1 1 calc R . . C1F C 0.3983(8) 1.0186(5) 0.8819(4) 0.042(2) Uani 1 1 d . . . C2F C 0.4569(12) 1.0816(5) 0.9040(5) 0.068(4) Uani 1 1 d . . . H2F H 0.4927 1.1084 0.8767 0.082 Uiso 1 1 calc R . . C3F C 0.4633(14) 1.1055(6) 0.9669(6) 0.086(5) Uani 1 1 d . . . H3F H 0.5035 1.1476 0.9818 0.103 Uiso 1 1 calc R . . C4F C 0.4081(15) 1.0648(7) 1.0058(6) 0.097(6) Uani 1 1 d . . . H4F H 0.4095 1.0800 1.0475 0.117 Uiso 1 1 calc R . . C5F C 0.3506(11) 1.0017(6) 0.9841(6) 0.069(3) Uani 1 1 d . . . H5F H 0.3149 0.9743 1.0111 0.082 Uiso 1 1 calc R . . C6F C 0.3465(9) 0.9796(5) 0.9217(5) 0.049(3) Uani 1 1 d . . . H6F H 0.3075 0.9371 0.9069 0.058 Uiso 1 1 calc R . . C1G C 0.0353(7) 0.8947(5) 0.6651(5) 0.047(3) Uani 1 1 d . . . C2G C -0.0536(8) 0.8635(5) 0.6927(6) 0.057(3) Uani 1 1 d . . . H2G H -0.0544 0.8704 0.7356 0.068 Uiso 1 1 calc R . . C3G C -0.1408(9) 0.8223(6) 0.6575(8) 0.073(4) Uani 1 1 d . . . H3G H -0.2002 0.8008 0.6761 0.088 Uiso 1 1 calc R . . C4G C -0.1384(11) 0.8136(6) 0.5941(8) 0.079(4) Uani 1 1 d . . . H4G H -0.1975 0.7867 0.5695 0.095 Uiso 1 1 calc R . . C5G C -0.0517(11) 0.8434(6) 0.5672(7) 0.075(4) Uani 1 1 d . . . H5G H -0.0511 0.8368 0.5243 0.089 Uiso 1 1 calc R . . C6G C 0.0354(10) 0.8833(5) 0.6023(6) 0.060(3) Uani 1 1 d . . . H6G H 0.0956 0.9030 0.5832 0.072 Uiso 1 1 calc R . . C1H C 0.0789(8) 1.0030(5) 0.7605(5) 0.045(2) Uani 1 1 d . . . C2H C -0.0030(9) 1.0311(6) 0.7336(7) 0.072(4) Uani 1 1 d . . . H2H H -0.0214 1.0227 0.6909 0.086 Uiso 1 1 calc R . . C3H C -0.0576(12) 1.0706(7) 0.7669(10) 0.094(5) Uani 1 1 d . . . H3H H -0.1123 1.0890 0.7475 0.113 Uiso 1 1 calc R . . C4H C -0.0300(12) 1.0830(6) 0.8309(10) 0.093(6) Uani 1 1 d . . . H4H H -0.0654 1.1106 0.8547 0.111 Uiso 1 1 calc R . . C5H C 0.0507(11) 1.0539(6) 0.8593(7) 0.072(4) Uani 1 1 d . . . H5H H 0.0681 1.0611 0.9021 0.086 Uiso 1 1 calc R . . C6H C 0.1049(8) 1.0143(5) 0.8233(5) 0.049(3) Uani 1 1 d . . . H6H H 0.1595 0.9952 0.8421 0.059 Uiso 1 1 calc R . . C37 C 0.6809(9) 0.6179(6) 0.6242(5) 0.057(3) Uani 1 1 d . . . C38 C 0.4798(12) 0.8544(6) 0.5324(7) 0.071(4) Uani 1 1 d . . . S1 S 0.6185(2) 0.65432(13) 0.68587(15) 0.0527(7) Uani 1 1 d . . . S2 S 0.3539(2) 0.80452(12) 0.55035(12) 0.0434(6) Uani 1 1 d . . . F1 F 0.7450(9) 0.6556(4) 0.5950(5) 0.144(5) Uani 1 1 d . . . F2 F 0.6168(7) 0.5718(4) 0.5862(4) 0.087(2) Uani 1 1 d . . . F3 F 0.7492(9) 0.5803(6) 0.6470(5) 0.140(4) Uani 1 1 d . . . O5 O 0.5497(12) 0.6041(6) 0.7039(6) 0.166(7) Uani 1 1 d . . . O6 O 0.6989(11) 0.6972(7) 0.7207(5) 0.153(6) Uani 1 1 d . . . O7 O 0.5567(12) 0.6939(7) 0.6505(7) 0.153(6) Uani 1 1 d . . . F4 F 0.5658(6) 0.8339(4) 0.5511(5) 0.115(3) Uani 1 1 d . . . F5 F 0.4803(11) 0.8516(6) 0.4715(5) 0.154(5) Uani 1 1 d . . . F6 F 0.4887(8) 0.9163(4) 0.5514(7) 0.154(5) Uani 1 1 d . . . O8 O 0.3572(7) 0.7418(4) 0.5247(6) 0.096(3) Uani 1 1 d . . . O9 O 0.3681(8) 0.8140(6) 0.6167(4) 0.095(3) Uani 1 1 d . . . O10 O 0.2701(6) 0.8356(4) 0.5252(4) 0.068(2) Uani 1 1 d . . . C1S C 0.8440(12) 0.8077(9) 0.9223(7) 0.096(5) Uani 1 1 d . . . H1S H 0.8957 0.7815 0.9387 0.116 Uiso 1 1 calc R . . C2S C 0.6261(10) 0.3057(6) 0.9228(6) 0.070(4) Uani 1 1 d . . . H2S H 0.6975 0.3004 0.9419 0.083 Uiso 1 1 calc R . . C3S C 0.9071(14) 0.5945(8) 0.9981(9) 0.114(6) Uani 1 1 d . . . H3S H 0.9835 0.6125 1.0146 0.137 Uiso 1 1 calc R . . C5S C 0.1388(14) 0.4833(9) 0.2437(9) 0.138(9) Uani 1 1 d D . . H5S1 H 0.0902 0.4884 0.2750 0.207 Uiso 1 1 calc R . . H5S2 H 0.2085 0.4784 0.2630 0.207 Uiso 1 1 calc R . . H5S3 H 0.1079 0.4444 0.2155 0.207 Uiso 1 1 calc R . . C6S C 0.1540(13) 0.5429(8) 0.2090(8) 0.116(7) Uani 1 1 d D . . H6S1 H 0.2129 0.5770 0.2303 0.140 Uiso 1 1 calc R . . H6S2 H 0.1735 0.5312 0.1677 0.140 Uiso 1 1 calc R . . C7S C 0.058(2) 0.6161(11) 0.1647(10) 0.167(9) Uani 1 1 d DU . . H7S1 H -0.0164 0.6216 0.1552 0.200 Uiso 1 1 calc R . . H7S2 H 0.0854 0.6020 0.1261 0.200 Uiso 1 1 calc R . . C8S C 0.1290(18) 0.6834(11) 0.1922(10) 0.168(10) Uani 1 1 d DU . . H8S1 H 0.1001 0.6989 0.2291 0.253 Uiso 1 1 calc R . . H8S2 H 0.1279 0.7151 0.1623 0.253 Uiso 1 1 calc R . . H8S3 H 0.2030 0.6782 0.2023 0.253 Uiso 1 1 calc R . . Cl1A Cl 0.9175(5) 0.8854(3) 0.9100(4) 0.182(3) Uani 1 1 d . . . Cl2A Cl 0.6368(3) 0.38809(16) 0.90216(18) 0.0793(10) Uani 1 1 d . . . Cl3A Cl 0.8664(5) 0.5140(3) 1.0180(4) 0.183(3) Uani 1 1 d . . . Cl1B Cl 0.7477(5) 0.8135(5) 0.9758(3) 0.195(4) Uani 1 1 d . . . Cl2B Cl 0.5870(3) 0.24862(15) 0.85721(15) 0.0695(8) Uani 1 1 d . . . Cl3B Cl 0.8940(4) 0.5911(4) 0.9178(3) 0.171(3) Uani 1 1 d . . . Cl1C Cl 0.7771(3) 0.7662(2) 0.8534(2) 0.1055(14) Uani 1 1 d . . . Cl2C Cl 0.5291(3) 0.29293(18) 0.97691(16) 0.0820(10) Uani 1 1 d . . . Cl3C Cl 0.8221(4) 0.6445(3) 1.0277(3) 0.147(2) Uani 1 1 d . . . O1S O 0.0590(10) 0.5661(6) 0.2049(6) 0.112(4) Uani 1 1 d DU . . C4SA C 0.8062(11) 0.0711(7) 0.5644(8) 0.107(9) Uiso 0.630(8) 1 d PD A 1 H4SA H 0.7771 0.0874 0.5266 0.129 Uiso 0.630(8) 1 calc PR A 1 Cl4A Cl 0.8961(10) 0.1348(4) 0.6122(5) 0.186(6) Uani 0.630(8) 1 d PD A 1 Cl4B Cl 0.7022(10) 0.0367(8) 0.6070(7) 0.206(7) Uani 0.630(8) 1 d PD A 1 Cl4C Cl 0.8870(12) 0.0135(7) 0.5475(5) 0.258(9) Uani 0.630(8) 1 d PD A 1 C4SB C 0.7792(15) 0.0845(10) 0.5817(11) 0.14(2) Uiso 0.370(8) 1 d PD A 2 H4SB H 0.7383 0.0950 0.5446 0.167 Uiso 0.370(8) 1 calc PR A 2 Cl4D Cl 0.9186(13) 0.0912(9) 0.5726(8) 0.149(7) Uiso 0.370(8) 1 d PD A 2 Cl4E Cl 0.7355(18) 0.0022(9) 0.5967(14) 0.177(11) Uiso 0.370(8) 1 d PD A 2 Cl4F Cl 0.7700(15) 0.1378(8) 0.6471(9) 0.170(8) Uiso 0.370(8) 1 d PD A 2 S3 S 0.8539(5) 0.2413(3) 1.0137(2) 0.0587(16) Uani 0.630(8) 1 d PD A 1 C39 C 0.8798(14) 0.1822(9) 0.9533(8) 0.096(9) Uani 0.630(8) 1 d PD A 1 F7 F 0.8723(16) 0.1219(7) 0.9706(8) 0.114(6) Uani 0.630(8) 1 d PD A 1 F8 F 0.8043(14) 0.1743(8) 0.9050(6) 0.104(6) Uani 0.630(8) 1 d PD A 1 F9 F 0.9774(12) 0.2066(11) 0.9376(10) 0.114(7) Uani 0.630(8) 1 d PD A 1 O11 O 0.853(3) 0.2979(13) 0.9789(16) 0.088(12) Uani 0.630(8) 1 d PDU A 1 O12 O 0.936(3) 0.2398(19) 1.0631(8) 0.082(10) Uani 0.630(8) 1 d PDU A 1 O13 O 0.7412(11) 0.2089(10) 1.0251(9) 0.102(7) Uani 0.630(8) 1 d PDU A 1 S3A S 0.9111(7) 0.2438(4) 0.9945(4) 0.041(2) Uani 0.370(8) 1 d PD A 2 C39A C 0.8042(18) 0.1723(10) 0.9893(13) 0.055(8) Uiso 0.370(8) 1 d PD A 2 F7A F 0.835(2) 0.1166(12) 1.0039(13) 0.091(8) Uiso 0.370(8) 1 d PD A 2 F8A F 0.752(2) 0.1582(15) 0.9333(13) 0.112(11) Uiso 0.370(8) 1 d PD A 2 F9A F 0.712(3) 0.1768(17) 1.0150(17) 0.124(13) Uiso 0.370(8) 1 d PD A 2 O11A O 0.863(4) 0.3022(19) 0.987(2) 0.047(10) Uiso 0.370(8) 1 d PD A 2 O12A O 0.941(4) 0.254(3) 1.0601(11) 0.058(11) Uiso 0.370(8) 1 d PD A 2 O13A O 0.994(3) 0.227(2) 0.9600(18) 0.099(16) Uiso 0.370(8) 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 0.02894(18) 0.02086(16) 0.02944(18) 0.00228(12) -0.00295(13) 0.00233(12) Pt2 0.03084(18) 0.02204(16) 0.0353(2) 0.00402(13) 0.00283(14) 0.00600(13) Fe1 0.0369(7) 0.0277(6) 0.0339(7) 0.0034(5) 0.0047(6) 0.0056(5) Fe2 0.0403(7) 0.0263(6) 0.0373(7) 0.0072(5) -0.0026(6) 0.0003(5) Na1 0.0255(15) 0.0111(13) 0.0263(16) -0.0053(11) 0.0037(12) -0.0004(11) P1 0.0293(11) 0.0247(10) 0.0281(11) 0.0049(9) 0.0004(9) 0.0044(9) P2 0.0319(11) 0.0202(10) 0.0298(12) 0.0022(8) -0.0020(9) 0.0012(8) P3 0.0367(12) 0.0229(10) 0.0303(12) 0.0019(9) 0.0021(10) 0.0059(9) P4 0.0320(12) 0.0274(11) 0.0491(15) 0.0096(10) 0.0003(11) 0.0085(9) N1 0.030(4) 0.024(3) 0.033(4) 0.004(3) 0.002(3) 0.002(3) N2 0.033(4) 0.018(3) 0.036(4) 0.003(3) 0.002(3) -0.003(3) O1 0.040(3) 0.026(3) 0.037(3) 0.004(3) 0.001(3) 0.010(3) O2 0.048(4) 0.033(3) 0.036(4) -0.002(3) 0.001(3) 0.016(3) O3 0.038(4) 0.033(3) 0.045(4) 0.003(3) -0.003(3) 0.007(3) O4 0.044(4) 0.019(3) 0.040(4) -0.002(2) -0.009(3) 0.008(2) C1 0.035(5) 0.026(4) 0.038(5) 0.006(4) 0.002(4) 0.013(4) C2 0.028(4) 0.031(4) 0.030(5) 0.004(4) -0.006(4) 0.011(3) C3 0.053(6) 0.037(5) 0.034(5) -0.014(4) -0.001(4) 0.012(4) C4 0.042(6) 0.057(7) 0.046(6) 0.003(5) 0.012(5) 0.004(5) C5 0.032(5) 0.039(5) 0.040(5) 0.004(4) 0.000(4) -0.006(4) C6 0.030(4) 0.026(4) 0.043(5) -0.005(4) -0.009(4) 0.011(3) C7 0.045(5) 0.028(4) 0.037(5) -0.002(4) -0.010(4) 0.007(4) C8 0.028(4) 0.020(4) 0.039(5) -0.001(4) 0.000(4) 0.003(3) C9 0.037(5) 0.027(4) 0.041(5) 0.006(4) -0.001(4) 0.015(4) C10 0.032(5) 0.030(4) 0.040(5) 0.008(4) 0.000(4) 0.012(4) C11 0.049(6) 0.033(5) 0.051(6) 0.004(4) 0.006(5) -0.007(4) C12 0.060(7) 0.039(6) 0.053(7) 0.008(5) 0.013(5) 0.000(5) C13 0.045(6) 0.039(5) 0.041(6) 0.005(4) 0.001(4) 0.006(4) C14 0.041(5) 0.039(5) 0.037(5) 0.010(4) 0.000(4) 0.012(4) C15 0.037(5) 0.024(4) 0.043(5) -0.008(4) -0.016(4) 0.013(4) C16 0.032(5) 0.033(5) 0.032(5) 0.004(4) 0.007(4) 0.007(4) C17 0.033(5) 0.038(5) 0.024(4) -0.002(4) 0.001(4) 0.000(4) C18 0.035(5) 0.030(4) 0.038(5) 0.001(4) -0.002(4) 0.005(4) C19 0.036(5) 0.064(7) 0.046(6) 0.000(5) 0.007(4) 0.021(5) C20 0.043(6) 0.048(6) 0.040(6) 0.003(5) 0.013(4) -0.004(4) C21 0.044(5) 0.034(5) 0.041(5) 0.002(4) -0.001(4) 0.005(4) C22 0.052(5) 0.018(4) 0.021(4) 0.001(3) 0.004(4) 0.007(4) C23 0.038(5) 0.025(4) 0.036(5) -0.001(4) 0.004(4) 0.000(4) C24 0.058(6) 0.027(5) 0.041(5) 0.001(4) 0.001(5) 0.008(4) C25 0.048(6) 0.039(5) 0.043(6) 0.003(4) 0.011(5) 0.008(4) C26 0.057(6) 0.028(4) 0.027(5) 0.009(4) 0.004(4) 0.007(4) C27 0.041(5) 0.031(5) 0.032(5) -0.001(4) 0.000(4) 0.004(4) C28 0.043(6) 0.038(5) 0.048(6) 0.009(4) 0.004(5) 0.002(4) C29 0.048(6) 0.045(6) 0.051(6) 0.019(5) -0.008(5) -0.018(5) C30 0.062(7) 0.031(5) 0.052(6) 0.005(4) -0.012(5) 0.007(5) C31 0.050(6) 0.025(4) 0.041(5) -0.006(4) -0.001(4) 0.004(4) C32 0.028(5) 0.037(5) 0.039(5) 0.003(4) -0.002(4) -0.006(4) C33 0.043(6) 0.032(5) 0.075(8) 0.023(5) -0.008(5) 0.007(4) C34 0.067(7) 0.047(6) 0.043(6) 0.022(5) -0.025(5) -0.011(5) C35 0.066(7) 0.045(6) 0.040(6) 0.011(5) -0.003(5) -0.007(5) C36 0.041(5) 0.051(6) 0.029(5) 0.002(4) -0.002(4) 0.005(4) C1A 0.032(5) 0.028(4) 0.039(5) 0.004(4) -0.006(4) 0.005(4) C2A 0.047(6) 0.034(5) 0.039(5) 0.008(4) -0.002(4) 0.013(4) C3A 0.080(8) 0.055(6) 0.028(5) 0.003(5) -0.005(5) 0.029(6) C4A 0.074(8) 0.041(6) 0.048(7) -0.013(5) -0.030(6) 0.018(5) C5A 0.048(6) 0.040(6) 0.076(8) 0.000(6) -0.021(6) 0.008(5) C6A 0.037(5) 0.037(5) 0.045(6) 0.000(4) -0.004(4) 0.010(4) C1B 0.031(4) 0.030(4) 0.031(5) 0.004(4) 0.006(4) 0.003(4) C2B 0.050(6) 0.047(6) 0.040(6) 0.016(5) 0.013(5) 0.011(5) C3B 0.060(7) 0.050(6) 0.055(7) 0.029(5) 0.016(6) 0.015(5) C4B 0.055(7) 0.043(6) 0.086(9) 0.033(6) 0.031(6) 0.008(5) C5B 0.043(6) 0.044(6) 0.084(9) 0.006(6) 0.006(6) -0.009(5) C6B 0.043(6) 0.046(6) 0.053(6) 0.023(5) 0.003(5) -0.001(4) C1C 0.031(5) 0.024(4) 0.038(5) 0.006(4) -0.011(4) -0.006(3) C2C 0.044(5) 0.032(5) 0.038(5) -0.003(4) -0.004(4) -0.008(4) C3C 0.061(7) 0.035(5) 0.057(7) 0.002(5) -0.023(6) -0.010(5) C4C 0.035(5) 0.046(6) 0.064(7) 0.015(5) -0.006(5) -0.006(4) C5C 0.030(5) 0.055(6) 0.058(7) 0.011(5) -0.002(5) 0.002(4) C6C 0.042(5) 0.026(4) 0.040(5) 0.004(4) -0.005(4) 0.003(4) C1D 0.037(5) 0.021(4) 0.032(5) -0.002(3) -0.001(4) 0.005(3) C2D 0.052(6) 0.030(5) 0.040(5) 0.007(4) -0.005(5) 0.003(4) C3D 0.069(7) 0.051(6) 0.032(5) 0.005(5) -0.015(5) 0.016(5) C4D 0.064(7) 0.029(5) 0.037(5) 0.012(4) 0.018(5) 0.012(4) C5D 0.044(5) 0.038(5) 0.033(5) 0.011(4) 0.001(4) 0.003(4) C6D 0.041(5) 0.039(5) 0.033(5) 0.005(4) -0.001(4) 0.000(4) C1E 0.032(5) 0.033(5) 0.053(6) 0.021(4) 0.007(4) 0.006(4) C2E 0.044(6) 0.047(6) 0.057(7) -0.002(5) 0.012(5) 0.014(5) C3E 0.063(8) 0.090(10) 0.069(9) 0.008(7) 0.015(7) 0.035(7) C4E 0.043(8) 0.155(16) 0.112(13) 0.045(12) 0.032(8) 0.050(9) C5E 0.028(6) 0.142(14) 0.092(11) 0.031(10) -0.004(7) 0.015(7) C6E 0.034(5) 0.079(8) 0.046(6) 0.007(6) -0.009(5) 0.000(5) C1F 0.056(6) 0.037(5) 0.033(5) -0.001(4) -0.005(4) 0.015(4) C2F 0.118(11) 0.041(6) 0.038(6) 0.002(5) -0.005(7) 0.002(6) C3F 0.170(15) 0.041(7) 0.043(7) -0.007(5) -0.007(8) 0.024(8) C4F 0.202(18) 0.055(8) 0.041(7) -0.011(6) -0.001(9) 0.053(10) C5F 0.098(10) 0.062(8) 0.055(7) 0.011(6) 0.025(7) 0.032(7) C6F 0.064(7) 0.046(6) 0.038(6) 0.006(5) 0.011(5) 0.015(5) C1G 0.024(5) 0.046(6) 0.074(8) 0.019(5) -0.006(5) 0.011(4) C2G 0.031(5) 0.040(6) 0.097(9) 0.016(6) -0.003(6) 0.004(4) C3G 0.027(6) 0.047(7) 0.147(14) 0.025(8) 0.009(7) 0.003(5) C4G 0.066(9) 0.046(7) 0.115(13) 0.004(8) -0.032(9) 0.001(6) C5G 0.082(9) 0.038(6) 0.090(10) 0.001(6) -0.028(8) -0.003(6) C6G 0.059(7) 0.044(6) 0.070(8) 0.014(6) -0.009(6) -0.006(5) C1H 0.032(5) 0.037(5) 0.070(7) 0.014(5) 0.010(5) 0.009(4) C2H 0.041(6) 0.058(7) 0.128(12) 0.034(8) 0.016(7) 0.021(5) C3H 0.067(9) 0.078(10) 0.159(17) 0.041(11) 0.032(11) 0.049(8) C4H 0.070(10) 0.047(7) 0.177(18) 0.022(10) 0.068(11) 0.024(7) C5H 0.075(9) 0.056(7) 0.087(10) 0.012(7) 0.037(8) 0.007(7) C6H 0.045(6) 0.043(6) 0.062(7) 0.001(5) 0.015(5) 0.013(5) C37 0.033(6) 0.083(8) 0.050(7) 0.008(6) 0.004(5) -0.001(6) C38 0.076(9) 0.047(7) 0.095(11) 0.005(7) 0.051(8) 0.008(6) S1 0.0425(15) 0.0400(14) 0.0726(19) 0.0000(13) 0.0117(13) 0.0009(11) S2 0.0418(13) 0.0359(13) 0.0489(15) 0.0071(11) -0.0024(11) 0.0002(10) F1 0.179(10) 0.076(6) 0.176(10) 0.007(6) 0.131(9) -0.023(6) F2 0.092(6) 0.080(5) 0.080(5) -0.011(4) 0.020(5) -0.001(4) F3 0.150(9) 0.187(11) 0.112(8) 0.004(7) 0.009(7) 0.112(9) O5 0.225(15) 0.104(9) 0.151(11) -0.037(8) 0.157(11) -0.053(9) O6 0.139(10) 0.173(12) 0.089(8) -0.064(8) 0.029(8) -0.088(9) O7 0.176(13) 0.157(12) 0.167(13) 0.031(10) 0.047(11) 0.119(11) F4 0.049(5) 0.101(7) 0.189(11) -0.013(6) 0.024(6) 0.009(4) F5 0.209(12) 0.152(10) 0.125(9) 0.058(8) 0.113(9) 0.037(9) F6 0.103(7) 0.048(5) 0.305(16) -0.020(7) 0.100(9) -0.017(4) O8 0.066(6) 0.042(5) 0.171(10) -0.018(6) -0.007(6) 0.005(4) O9 0.075(6) 0.164(10) 0.055(6) 0.045(6) 0.016(5) 0.029(6) O10 0.058(5) 0.070(5) 0.075(6) 0.006(4) -0.016(4) 0.018(4) C1S 0.072(10) 0.126(14) 0.091(11) 0.002(10) -0.014(8) 0.033(9) C2S 0.068(8) 0.060(7) 0.070(8) 0.001(6) -0.024(7) 0.003(6) C3S 0.095(12) 0.096(12) 0.145(17) 0.003(12) 0.042(12) -0.003(10) C5S 0.106(14) 0.132(16) 0.163(19) 0.091(15) -0.048(13) -0.016(11) C6S 0.088(12) 0.128(16) 0.116(15) -0.049(13) -0.018(11) 0.017(11) C7S 0.185(17) 0.150(16) 0.169(16) 0.043(14) 0.037(14) 0.022(14) C8S 0.17(2) 0.19(2) 0.18(2) 0.111(18) 0.085(17) 0.067(17) Cl1A 0.154(5) 0.104(4) 0.265(8) 0.010(4) -0.111(5) 0.024(4) Cl2A 0.078(2) 0.0533(18) 0.103(3) 0.0146(17) -0.0048(19) 0.0074(15) Cl3A 0.122(4) 0.133(5) 0.306(10) 0.017(5) 0.094(5) 0.023(4) Cl1B 0.162(6) 0.354(10) 0.100(4) -0.025(5) 0.007(4) 0.155(7) Cl2B 0.085(2) 0.0565(17) 0.070(2) 0.0064(15) 0.0010(17) 0.0240(16) Cl3B 0.079(3) 0.279(8) 0.128(5) -0.027(5) 0.016(3) -0.016(4) Cl1C 0.064(2) 0.146(4) 0.103(3) -0.012(3) -0.008(2) 0.029(2) Cl2C 0.107(3) 0.078(2) 0.063(2) 0.0145(17) 0.0035(19) 0.020(2) Cl3C 0.116(4) 0.116(4) 0.196(6) -0.045(4) 0.050(4) 0.005(3) O1S 0.116(9) 0.101(8) 0.118(9) 0.028(7) 0.011(7) 0.013(7) Cl4A 0.293(15) 0.081(6) 0.180(10) 0.061(6) -0.039(10) 0.031(7) Cl4B 0.149(11) 0.275(18) 0.188(13) 0.067(13) 0.050(9) -0.011(12) Cl4C 0.354(19) 0.293(17) 0.138(9) -0.074(10) -0.135(11) 0.205(15) S3 0.057(4) 0.067(3) 0.050(3) -0.010(2) -0.002(3) 0.019(3) C39 0.074(16) 0.13(2) 0.078(17) -0.044(16) 0.010(13) 0.041(16) F7 0.189(17) 0.053(8) 0.112(13) -0.003(8) 0.023(12) 0.057(9) F8 0.110(11) 0.130(12) 0.063(8) -0.061(9) -0.030(9) 0.049(10) F9 0.068(10) 0.158(18) 0.113(15) -0.015(13) 0.049(10) 0.011(10) O11 0.080(15) 0.048(10) 0.13(2) 0.022(11) -0.034(12) 0.008(9) O12 0.108(16) 0.11(2) 0.035(8) -0.012(8) -0.028(8) 0.057(15) O13 0.049(9) 0.132(16) 0.120(14) -0.039(12) 0.051(9) 0.014(10) S3A 0.029(4) 0.053(4) 0.042(4) 0.009(3) 0.009(3) 0.010(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 O4 2.069(6) . ? Pt1 N1 2.070(7) . ? Pt1 P1 2.235(2) . ? Pt1 P2 2.262(2) . ? Pt2 O1 2.055(6) . ? Pt2 N2 2.063(6) . ? Pt2 P4 2.240(2) . ? Pt2 P3 2.267(2) . ? Fe1 C17 1.989(8) . ? Fe1 C22 2.020(9) . ? Fe1 C21 2.025(9) . ? Fe1 C23 2.027(9) . ? Fe1 C26 2.029(9) . ? Fe1 C18 2.034(9) . ? Fe1 C19 2.050(10) . ? Fe1 C20 2.060(10) . ? Fe1 C24 2.068(9) . ? Fe1 C25 2.070(10) . ? Fe2 C32 1.996(8) . ? Fe2 C31 2.015(9) . ? Fe2 C36 2.029(10) . ? Fe2 C27 2.032(9) . ? Fe2 C33 2.032(10) . ? Fe2 C28 2.036(10) . ? Fe2 C35 2.063(11) . ? Fe2 C34 2.064(9) . ? Fe2 C29 2.064(9) . ? Fe2 C30 2.077(10) . ? Na1 O2 2.274(6) . ? Na1 O3 2.285(7) . ? Na1 O7 2.293(13) . ? Na1 O9 2.441(11) . ? Na1 S2 3.309(4) . ? Na1 S1 3.363(4) . ? P1 C17 1.799(9) . ? P1 C1A 1.810(9) . ? P1 C1B 1.818(8) . ? P2 C22 1.792(8) . ? P2 C1D 1.809(9) . ? P2 C1C 1.820(8) . ? P3 C27 1.768(9) . ? P3 C1E 1.807(9) . ? P3 C1F 1.817(9) . ? P4 C32 1.793(9) . ? P4 C1H 1.808(10) . ? P4 C1G 1.826(10) . ? N1 C5 1.323(11) . ? N1 C1 1.336(10) . ? N2 C13 1.331(11) . ? N2 C9 1.350(11) . ? O1 C8 1.289(9) . ? O2 C8 1.223(10) . ? O3 C16 1.217(10) . ? O4 C16 1.286(10) . ? C1 C2 1.391(11) . ? C2 C3 1.384(12) . ? C2 C6 1.501(11) . ? C3 C4 1.385(13) . ? C4 C5 1.371(13) . ? C6 C7 1.529(11) . ? C7 C8 1.506(12) . ? C9 C10 1.392(12) . ? C10 C11 1.364(13) . ? C10 C14 1.505(12) . ? C11 C12 1.351(14) . ? C12 C13 1.366(13) . ? C14 C15 1.508(11) . ? C15 C16 1.515(11) . ? C17 C21 1.413(12) . ? C17 C18 1.418(12) . ? C18 C19 1.395(13) . ? C19 C20 1.428(14) . ? C20 C21 1.395(13) . ? C22 C26 1.424(12) . ? C22 C23 1.435(11) . ? C23 C24 1.427(13) . ? C24 C25 1.415(13) . ? C25 C26 1.426(13) . ? C27 C28 1.451(13) . ? C27 C31 1.460(12) . ? C28 C29 1.417(13) . ? C29 C30 1.408(15) . ? C30 C31 1.434(13) . ? C32 C33 1.422(12) . ? C32 C36 1.434(13) . ? C33 C34 1.388(15) . ? C34 C35 1.380(16) . ? C35 C36 1.431(13) . ? C1A C2A 1.376(13) . ? C1A C6A 1.396(12) . ? C2A C3A 1.382(13) . ? C3A C4A 1.374(16) . ? C4A C5A 1.375(16) . ? C5A C6A 1.373(14) . ? C1B C6B 1.358(12) . ? C1B C2B 1.391(12) . ? C2B C3B 1.344(13) . ? C3B C4B 1.387(16) . ? C4B C5B 1.365(16) . ? C5B C6B 1.401(13) . ? C1C C2C 1.376(12) . ? C1C C6C 1.393(13) . ? C2C C3C 1.389(13) . ? C3C C4C 1.361(15) . ? C4C C5C 1.373(15) . ? C5C C6C 1.388(12) . ? C1D C2D 1.380(12) . ? C1D C6D 1.405(12) . ? C2D C3D 1.379(13) . ? C3D C4D 1.372(14) . ? C4D C5D 1.344(13) . ? C5D C6D 1.387(12) . ? C1E C2E 1.373(14) . ? C1E C6E 1.387(13) . ? C2E C3E 1.338(15) . ? C3E C4E 1.36(2) . ? C4E C5E 1.37(2) . ? C5E C6E 1.366(17) . ? C1F C6F 1.351(13) . ? C1F C2F 1.385(14) . ? C2F C3F 1.402(15) . ? C3F C4F 1.375(19) . ? C4F C5F 1.381(18) . ? C5F C6F 1.385(15) . ? C1G C6G 1.365(16) . ? C1G C2G 1.382(14) . ? C2G C3G 1.374(16) . ? C3G C4G 1.377(19) . ? C4G C5G 1.343(19) . ? C5G C6G 1.360(15) . ? C1H C6H 1.363(15) . ? C1H C2H 1.380(14) . ? C2H C3H 1.355(19) . ? C3H C4H 1.39(2) . ? C4H C5H 1.39(2) . ? C5H C6H 1.385(15) . ? C37 F1 1.254(13) . ? C37 F2 1.298(13) . ? C37 F3 1.346(14) . ? C37 S1 1.785(12) . ? C38 F4 1.274(16) . ? C38 F6 1.284(13) . ? C38 F5 1.320(17) . ? C38 S2 1.799(12) . ? S1 O5 1.321(10) . ? S1 O6 1.335(10) . ? S1 O7 1.446(13) . ? S2 O8 1.370(8) . ? S2 O10 1.420(8) . ? S2 O9 1.428(9) . ? C1S Cl1C 1.722(15) . ? C1S Cl1A 1.740(18) . ? C1S Cl1B 1.752(16) . ? C2S Cl2B 1.739(12) . ? C2S Cl2C 1.756(14) . ? C2S Cl2A 1.771(13) . ? C3S Cl3B 1.73(2) . ? C3S Cl3C 1.734(18) . ? C3S Cl3A 1.740(17) . ? C5S C6S 1.483(15) . ? C6S O1S 1.358(14) . ? C7S O1S 1.405(15) . ? C7S C8S 1.534(17) . ? C4SA Cl4C 1.728(10) . ? C4SA Cl4B 1.734(10) . ? C4SA Cl4A 1.752(10) . ? C4SB Cl4F 1.742(10) . ? C4SB Cl4E 1.743(10) . ? C4SB Cl4D 1.748(10) . ? S3 O12 1.424(16) . ? S3 O11 1.443(16) . ? S3 O13 1.489(14) . ? S3 C39 1.801(14) . ? C39 F9 1.311(16) . ? C39 F7 1.314(16) . ? C39 F8 1.326(16) . ? S3A O13A 1.402(19) . ? S3A O12A 1.430(19) . ? S3A O11A 1.452(19) . ? S3A C39A 1.778(17) . ? C39A F8A 1.311(18) . ? C39A F7A 1.326(18) . ? C39A F9A 1.331(19) . ? 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 O4 Pt1 N1 86.1(2) . . ? O4 Pt1 P1 173.28(18) . . ? N1 Pt1 P1 92.80(19) . . ? O4 Pt1 P2 82.50(17) . . ? N1 Pt1 P2 167.72(19) . . ? P1 Pt1 P2 99.08(8) . . ? O1 Pt2 N2 87.0(3) . . ? O1 Pt2 P4 174.48(18) . . ? N2 Pt2 P4 91.4(2) . . ? O1 Pt2 P3 83.10(17) . . ? N2 Pt2 P3 170.1(2) . . ? P4 Pt2 P3 98.48(8) . . ? C17 Fe1 C22 108.7(3) . . ? C17 Fe1 C21 41.2(4) . . ? C22 Fe1 C21 112.1(3) . . ? C17 Fe1 C23 112.9(4) . . ? C22 Fe1 C23 41.5(3) . . ? C21 Fe1 C23 143.1(4) . . ? C17 Fe1 C26 135.1(4) . . ? C22 Fe1 C26 41.2(3) . . ? C21 Fe1 C26 109.3(4) . . ? C23 Fe1 C26 69.0(4) . . ? C17 Fe1 C18 41.3(3) . . ? C22 Fe1 C18 135.9(3) . . ? C21 Fe1 C18 68.7(4) . . ? C23 Fe1 C18 110.4(4) . . ? C26 Fe1 C18 176.1(4) . . ? C17 Fe1 C19 68.2(4) . . ? C22 Fe1 C19 175.8(4) . . ? C21 Fe1 C19 67.7(4) . . ? C23 Fe1 C19 136.3(4) . . ? C26 Fe1 C19 143.0(4) . . ? C18 Fe1 C19 39.9(4) . . ? C17 Fe1 C20 68.5(4) . . ? C22 Fe1 C20 141.6(4) . . ? C21 Fe1 C20 39.9(4) . . ? C23 Fe1 C20 176.5(4) . . ? C26 Fe1 C20 112.5(4) . . ? C18 Fe1 C20 68.3(4) . . ? C19 Fe1 C20 40.7(4) . . ? C17 Fe1 C24 143.4(4) . . ? C22 Fe1 C24 69.3(4) . . ? C21 Fe1 C24 175.1(4) . . ? C23 Fe1 C24 40.8(4) . . ? C26 Fe1 C24 68.4(4) . . ? C18 Fe1 C24 113.8(4) . . ? C19 Fe1 C24 111.3(4) . . ? C20 Fe1 C24 136.3(4) . . ? C17 Fe1 C25 175.5(4) . . ? C22 Fe1 C25 68.8(4) . . ? C21 Fe1 C25 135.6(4) . . ? C23 Fe1 C25 68.1(4) . . ? C26 Fe1 C25 40.7(4) . . ? C18 Fe1 C25 143.0(4) . . ? C19 Fe1 C25 114.4(4) . . ? C20 Fe1 C25 110.8(4) . . ? C24 Fe1 C25 40.0(4) . . ? C32 Fe2 C31 108.4(4) . . ? C32 Fe2 C36 41.7(4) . . ? C31 Fe2 C36 138.2(4) . . ? C32 Fe2 C27 107.5(4) . . ? C31 Fe2 C27 42.3(4) . . ? C36 Fe2 C27 109.1(4) . . ? C32 Fe2 C33 41.3(4) . . ? C31 Fe2 C33 109.7(4) . . ? C36 Fe2 C33 68.8(4) . . ? C27 Fe2 C33 137.2(4) . . ? C32 Fe2 C28 137.8(4) . . ? C31 Fe2 C28 69.8(4) . . ? C36 Fe2 C28 110.9(4) . . ? C27 Fe2 C28 41.8(4) . . ? C33 Fe2 C28 178.9(4) . . ? C32 Fe2 C35 69.0(4) . . ? C31 Fe2 C35 176.7(4) . . ? C36 Fe2 C35 40.9(4) . . ? C27 Fe2 C35 139.8(4) . . ? C33 Fe2 C35 67.1(5) . . ? C28 Fe2 C35 113.5(5) . . ? C32 Fe2 C34 68.2(4) . . ? C31 Fe2 C34 138.5(5) . . ? C36 Fe2 C34 67.6(4) . . ? C27 Fe2 C34 175.7(4) . . ? C33 Fe2 C34 39.6(4) . . ? C28 Fe2 C34 141.4(4) . . ? C35 Fe2 C34 39.1(4) . . ? C32 Fe2 C29 177.3(4) . . ? C31 Fe2 C29 69.3(4) . . ? C36 Fe2 C29 139.3(4) . . ? C27 Fe2 C29 69.9(4) . . ? C33 Fe2 C29 140.4(4) . . ? C28 Fe2 C29 40.4(4) . . ? C35 Fe2 C29 113.4(4) . . ? C34 Fe2 C29 114.4(4) . . ? C32 Fe2 C30 139.1(4) . . ? C31 Fe2 C30 41.0(4) . . ? C36 Fe2 C30 178.2(4) . . ? C27 Fe2 C30 69.3(4) . . ? C33 Fe2 C30 112.9(4) . . ? C28 Fe2 C30 67.4(4) . . ? C35 Fe2 C30 140.0(4) . . ? C34 Fe2 C30 114.1(4) . . ? C29 Fe2 C30 39.8(4) . . ? O2 Na1 O3 102.8(3) . . ? O2 Na1 O7 115.5(4) . . ? O3 Na1 O7 119.8(4) . . ? O2 Na1 O9 86.0(3) . . ? O3 Na1 O9 121.3(3) . . ? O7 Na1 O9 106.5(4) . . ? O2 Na1 S2 108.77(18) . . ? O3 Na1 S2 111.31(19) . . ? O7 Na1 S2 98.4(4) . . ? O9 Na1 S2 23.0(2) . . ? O2 Na1 S1 106.21(19) . . ? O3 Na1 S1 107.91(18) . . ? O7 Na1 S1 20.2(4) . . ? O9 Na1 S1 125.2(2) . . ? S2 Na1 S1 118.57(11) . . ? C17 P1 C1A 103.5(4) . . ? C17 P1 C1B 105.5(4) . . ? C1A P1 C1B 105.4(4) . . ? C17 P1 Pt1 116.5(3) . . ? C1A P1 Pt1 111.6(3) . . ? C1B P1 Pt1 113.3(3) . . ? C22 P2 C1D 103.5(4) . . ? C22 P2 C1C 102.8(4) . . ? C1D P2 C1C 107.4(4) . . ? C22 P2 Pt1 124.5(3) . . ? C1D P2 Pt1 105.3(3) . . ? C1C P2 Pt1 112.1(3) . . ? C27 P3 C1E 103.3(4) . . ? C27 P3 C1F 103.6(4) . . ? C1E P3 C1F 106.6(5) . . ? C27 P3 Pt2 123.6(3) . . ? C1E P3 Pt2 107.5(3) . . ? C1F P3 Pt2 111.1(3) . . ? C32 P4 C1H 108.2(4) . . ? C32 P4 C1G 102.1(5) . . ? C1H P4 C1G 103.1(5) . . ? C32 P4 Pt2 114.7(3) . . ? C1H P4 Pt2 112.2(4) . . ? C1G P4 Pt2 115.4(3) . . ? C5 N1 C1 119.3(7) . . ? C5 N1 Pt1 121.8(6) . . ? C1 N1 Pt1 118.7(6) . . ? C13 N2 C9 119.3(7) . . ? C13 N2 Pt2 121.0(6) . . ? C9 N2 Pt2 119.6(6) . . ? C8 O1 Pt2 122.3(5) . . ? C8 O2 Na1 166.3(6) . . ? C16 O3 Na1 165.4(6) . . ? C16 O4 Pt1 123.8(5) . . ? N1 C1 C2 122.9(8) . . ? C3 C2 C1 116.8(8) . . ? C3 C2 C6 123.9(8) . . ? C1 C2 C6 119.3(8) . . ? C2 C3 C4 120.0(8) . . ? C5 C4 C3 118.9(9) . . ? N1 C5 C4 122.0(8) . . ? C2 C6 C7 114.1(7) . . ? C8 C7 C6 113.5(7) . . ? O2 C8 O1 125.2(8) . . ? O2 C8 C7 122.3(7) . . ? O1 C8 C7 112.5(7) . . ? N2 C9 C10 122.3(8) . . ? C11 C10 C9 116.7(9) . . ? C11 C10 C14 125.0(8) . . ? C9 C10 C14 118.3(8) . . ? C12 C11 C10 120.6(9) . . ? C11 C12 C13 120.9(10) . . ? N2 C13 C12 120.1(9) . . ? C10 C14 C15 113.8(7) . . ? C14 C15 C16 113.0(7) . . ? O3 C16 O4 125.5(8) . . ? O3 C16 C15 122.5(8) . . ? O4 C16 C15 111.6(7) . . ? C21 C17 C18 108.1(8) . . ? C21 C17 P1 124.7(7) . . ? C18 C17 P1 127.2(7) . . ? C21 C17 Fe1 70.8(5) . . ? C18 C17 Fe1 71.1(5) . . ? P1 C17 Fe1 125.1(5) . . ? C19 C18 C17 107.3(8) . . ? C19 C18 Fe1 70.6(6) . . ? C17 C18 Fe1 67.7(5) . . ? C18 C19 C20 109.0(8) . . ? C18 C19 Fe1 69.4(5) . . ? C20 C19 Fe1 70.0(6) . . ? C21 C20 C19 107.1(8) . . ? C21 C20 Fe1 68.7(5) . . ? C19 C20 Fe1 69.3(5) . . ? C20 C21 C17 108.6(8) . . ? C20 C21 Fe1 71.4(6) . . ? C17 C21 Fe1 68.0(5) . . ? C26 C22 C23 106.9(7) . . ? C26 C22 P2 126.1(6) . . ? C23 C22 P2 127.0(7) . . ? C26 C22 Fe1 69.7(5) . . ? C23 C22 Fe1 69.5(5) . . ? P2 C22 Fe1 125.1(4) . . ? C24 C23 C22 108.6(8) . . ? C24 C23 Fe1 71.2(5) . . ? C22 C23 Fe1 69.0(5) . . ? C25 C24 C23 107.6(8) . . ? C25 C24 Fe1 70.1(5) . . ? C23 C24 Fe1 68.1(5) . . ? C24 C25 C26 108.4(8) . . ? C24 C25 Fe1 69.9(5) . . ? C26 C25 Fe1 68.1(5) . . ? C22 C26 C25 108.5(8) . . ? C22 C26 Fe1 69.1(5) . . ? C25 C26 Fe1 71.2(5) . . ? C28 C27 C31 105.4(8) . . ? C28 C27 P3 127.4(7) . . ? C31 C27 P3 127.2(7) . . ? C28 C27 Fe2 69.2(5) . . ? C31 C27 Fe2 68.2(5) . . ? P3 C27 Fe2 125.4(5) . . ? C29 C28 C27 109.7(9) . . ? C29 C28 Fe2 70.9(6) . . ? C27 C28 Fe2 68.9(5) . . ? C30 C29 C28 107.7(9) . . ? C30 C29 Fe2 70.6(6) . . ? C28 C29 Fe2 68.7(5) . . ? C29 C30 C31 109.4(9) . . ? C29 C30 Fe2 69.6(6) . . ? C31 C30 Fe2 67.2(5) . . ? C30 C31 C27 107.6(9) . . ? C30 C31 Fe2 71.8(6) . . ? C27 C31 Fe2 69.5(5) . . ? C33 C32 C36 107.0(8) . . ? C33 C32 P4 130.8(8) . . ? C36 C32 P4 122.2(7) . . ? C33 C32 Fe2 70.7(5) . . ? C36 C32 Fe2 70.4(5) . . ? P4 C32 Fe2 124.5(5) . . ? C34 C33 C32 108.3(9) . . ? C34 C33 Fe2 71.4(6) . . ? C32 C33 Fe2 68.0(5) . . ? C35 C34 C33 109.7(9) . . ? C35 C34 Fe2 70.4(6) . . ? C33 C34 Fe2 69.0(6) . . ? C34 C35 C36 108.2(10) . . ? C34 C35 Fe2 70.5(6) . . ? C36 C35 Fe2 68.3(6) . . ? C35 C36 C32 106.8(9) . . ? C35 C36 Fe2 70.8(6) . . ? C32 C36 Fe2 67.9(5) . . ? C2A C1A C6A 118.9(9) . . ? C2A C1A P1 119.8(7) . . ? C6A C1A P1 121.2(7) . . ? C1A C2A C3A 120.5(10) . . ? C4A C3A C2A 120.3(10) . . ? C3A C4A C5A 119.5(10) . . ? C6A C5A C4A 120.6(10) . . ? C5A C6A C1A 120.1(10) . . ? C6B C1B C2B 118.0(8) . . ? C6B C1B P1 120.9(7) . . ? C2B C1B P1 121.1(7) . . ? C3B C2B C1B 122.1(10) . . ? C2B C3B C4B 120.0(10) . . ? C5B C4B C3B 119.1(9) . . ? C4B C5B C6B 120.2(10) . . ? C1B C6B C5B 120.5(10) . . ? C2C C1C C6C 119.6(8) . . ? C2C C1C P2 120.9(7) . . ? C6C C1C P2 119.5(6) . . ? C1C C2C C3C 119.7(10) . . ? C4C C3C C2C 120.8(10) . . ? C3C C4C C5C 120.0(9) . . ? C4C C5C C6C 120.2(10) . . ? C5C C6C C1C 119.7(9) . . ? C2D C1D C6D 119.2(8) . . ? C2D C1D P2 123.4(7) . . ? C6D C1D P2 117.0(6) . . ? C3D C2D C1D 119.6(9) . . ? C4D C3D C2D 120.7(9) . . ? C5D C4D C3D 120.3(9) . . ? C4D C5D C6D 120.8(9) . . ? C5D C6D C1D 119.3(8) . . ? C2E C1E C6E 118.7(9) . . ? C2E C1E P3 119.5(8) . . ? C6E C1E P3 121.7(8) . . ? C3E C2E C1E 121.1(11) . . ? C2E C3E C4E 120.1(13) . . ? C3E C4E C5E 120.5(12) . . ? C4E C5E C6E 119.7(12) . . ? C5E C6E C1E 119.8(12) . . ? C6F C1F C2F 119.3(10) . . ? C6F C1F P3 121.9(8) . . ? C2F C1F P3 118.7(8) . . ? C1F C2F C3F 121.2(12) . . ? C4F C3F C2F 117.8(12) . . ? C3F C4F C5F 121.2(11) . . ? C4F C5F C6F 119.4(12) . . ? C1F C6F C5F 121.1(11) . . ? C6G C1G C2G 118.8(10) . . ? C6G C1G P4 121.9(8) . . ? C2G C1G P4 119.4(9) . . ? C3G C2G C1G 120.6(13) . . ? C2G C3G C4G 118.6(12) . . ? C5G C4G C3G 120.9(12) . . ? C4G C5G C6G 120.4(14) . . ? C5G C6G C1G 120.7(12) . . ? C6H C1H C2H 119.0(11) . . ? C6H C1H P4 120.8(8) . . ? C2H C1H P4 120.2(10) . . ? C3H C2H C1H 122.6(15) . . ? C2H C3H C4H 118.5(14) . . ? C5H C4H C3H 119.9(13) . . ? C6H C5H C4H 119.6(14) . . ? C1H C6H C5H 120.4(11) . . ? F1 C37 F2 110.7(11) . . ? F1 C37 F3 100.3(11) . . ? F2 C37 F3 98.2(11) . . ? F1 C37 S1 118.5(10) . . ? F2 C37 S1 116.0(8) . . ? F3 C37 S1 109.9(8) . . ? F4 C38 F6 110.4(13) . . ? F4 C38 F5 104.5(11) . . ? F6 C38 F5 105.7(13) . . ? F4 C38 S2 114.4(10) . . ? F6 C38 S2 112.2(9) . . ? F5 C38 S2 108.9(11) . . ? O5 S1 O6 127.7(9) . . ? O5 S1 O7 109.0(10) . . ? O6 S1 O7 106.5(10) . . ? O5 S1 C37 104.9(6) . . ? O6 S1 C37 106.2(7) . . ? O7 S1 C37 98.9(7) . . ? O5 S1 Na1 81.3(8) . . ? O6 S1 Na1 112.4(7) . . ? O7 S1 Na1 33.2(6) . . ? C37 S1 Na1 124.6(4) . . ? O8 S2 O10 117.5(6) . . ? O8 S2 O9 115.2(7) . . ? O10 S2 O9 112.3(6) . . ? O8 S2 C38 103.7(6) . . ? O10 S2 C38 104.9(6) . . ? O9 S2 C38 100.7(7) . . ? O8 S2 Na1 73.2(5) . . ? O10 S2 Na1 136.3(4) . . ? O9 S2 Na1 42.0(5) . . ? C38 S2 Na1 113.5(5) . . ? S1 O7 Na1 126.7(9) . . ? S2 O9 Na1 115.0(7) . . ? Cl1C C1S Cl1A 110.4(9) . . ? Cl1C C1S Cl1B 108.9(8) . . ? Cl1A C1S Cl1B 112.2(10) . . ? Cl2B C2S Cl2C 110.6(7) . . ? Cl2B C2S Cl2A 110.3(7) . . ? Cl2C C2S Cl2A 108.3(7) . . ? Cl3B C3S Cl3C 109.2(12) . . ? Cl3B C3S Cl3A 107.9(10) . . ? Cl3C C3S Cl3A 109.3(9) . . ? O1S C6S C5S 108.8(15) . . ? O1S C7S C8S 113.0(18) . . ? C6S O1S C7S 113.6(17) . . ? Cl4C C4SA Cl4B 109.8(10) . . ? Cl4C C4SA Cl4A 103.4(8) . . ? Cl4B C4SA Cl4A 108.5(9) . . ? Cl4F C4SB Cl4E 109.3(11) . . ? Cl4F C4SB Cl4D 107.0(10) . . ? Cl4E C4SB Cl4D 104.5(10) . . ? O12 S3 O11 123(2) . . ? O12 S3 O13 114.0(18) . . ? O11 S3 O13 111.5(17) . . ? O12 S3 C39 103.9(14) . . ? O11 S3 C39 99.5(15) . . ? O13 S3 C39 99.9(9) . . ? F9 C39 F7 112.6(19) . . ? F9 C39 F8 111.1(19) . . ? F7 C39 F8 103.7(16) . . ? F9 C39 S3 105.8(14) . . ? F7 C39 S3 112.7(13) . . ? F8 C39 S3 111.1(12) . . ? O13A S3A O12A 114(3) . . ? O13A S3A O11A 124(3) . . ? O12A S3A O11A 99(3) . . ? O13A S3A C39A 108(2) . . ? O12A S3A C39A 101(2) . . ? O11A S3A C39A 109(2) . . ? F8A C39A F7A 106(2) . . ? F8A C39A F9A 93(3) . . ? F7A C39A F9A 108(3) . . ? F8A C39A S3A 112(2) . . ? F7A C39A S3A 115.7(19) . . ? F9A C39A S3A 119(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.753 _refine_diff_density_min -1.668 _refine_diff_density_rms 0.177 # Attachment 'complex3_new.cif' data_7494 _database_code_depnum_ccdc_archive 'CCDC 711711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H76 F12 N2 O6 P6 Pt2' _chemical_formula_weight 2037.49 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.180(3) _cell_length_b 13.867(2) _cell_length_c 31.879(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.178(3) _cell_angle_gamma 90.00 _cell_volume 8915(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2915 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 19.57 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4016 _exptl_absorpt_coefficient_mu 3.318 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4360 _exptl_absorpt_correction_T_max 0.6188 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30945 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10219 _reflns_number_gt 6342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The PF6 is disordered into two sets). There are two residual peaks assigned as half water (H not assigned). They are so assigned because they are at H bonding distances to some of the O s and F. The H atoms of these water cold not be located. There are also some residual peaks in the voids in the lattice, but their peaks heights are too low to be assigned as solvent. ; _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^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10219 _refine_ls_number_parameters 540 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.175 _refine_ls_shift/su_mean 0.008 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 0.385066(7) 0.407624(12) 0.149564(4) 0.03991(4) Uani 1 1 d . . . P1 P 0.28410(5) 0.47373(9) 0.13558(3) 0.0449(3) Uani 1 1 d . . . P2 P 0.43036(5) 0.43410(8) 0.08735(3) 0.0417(3) Uani 1 1 d . . . O1 O 0.59193(15) 0.5041(2) 0.26809(9) 0.0660(10) Uani 1 1 d . . . O2 O 0.65182(12) 0.3782(2) 0.29162(8) 0.0472(8) Uani 1 1 d . . . N1 N 0.46969(15) 0.3391(2) 0.17353(9) 0.0435(9) Uani 1 1 d . . . C1 C 0.52355(19) 0.3868(3) 0.18682(12) 0.0491(13) Uani 1 1 d . . . H1 H 0.5233 0.4544 0.1850 0.059 Uiso 1 1 calc R . . C2 C 0.57970(18) 0.3420(4) 0.20316(11) 0.0519(13) Uani 1 1 d . . . C3 C 0.5784(2) 0.2429(4) 0.20622(14) 0.0765(17) Uani 1 1 d . . . H3 H 0.6160 0.2098 0.2169 0.092 Uiso 1 1 calc R . . C4 C 0.5221(2) 0.1916(4) 0.19367(17) 0.0799(18) Uani 1 1 d . . . H4 H 0.5204 0.1241 0.1962 0.096 Uiso 1 1 calc R . . C5 C 0.4678(2) 0.2438(4) 0.17713(13) 0.0608(14) Uani 1 1 d . . . H5 H 0.4291 0.2106 0.1684 0.073 Uiso 1 1 calc R . . C6 C 0.6382(2) 0.3991(4) 0.21831(13) 0.0671(16) Uani 1 1 d . . . H6A H 0.6443 0.4550 0.2001 0.081 Uiso 1 1 calc R . . H6B H 0.6783 0.3593 0.2180 0.081 Uiso 1 1 calc R . . C7 C 0.62582(18) 0.4319(3) 0.26262(12) 0.0482(12) Uani 1 1 d . . . C1A C 0.2699(2) 0.5623(4) 0.17630(14) 0.0616(15) Uani 1 1 d . . . C2A C 0.2314(2) 0.5398(4) 0.20958(12) 0.0726(16) Uani 1 1 d . . . H2A H 0.2082 0.4811 0.2097 0.087 Uiso 1 1 calc R . . C3A C 0.2267(3) 0.6028(5) 0.24293(17) 0.102(2) Uani 1 1 d . . . H3A H 0.2012 0.5864 0.2660 0.122 Uiso 1 1 calc R . . C4A C 0.2592(3) 0.6890(5) 0.24217(16) 0.108(2) Uani 1 1 d . . . H4A H 0.2545 0.7327 0.2644 0.129 Uiso 1 1 calc R . . C5A C 0.2987(3) 0.7133(5) 0.20958(18) 0.107(2) Uani 1 1 d . . . H5A H 0.3212 0.7726 0.2093 0.128 Uiso 1 1 calc R . . C6A C 0.3043(2) 0.6480(4) 0.17746(15) 0.0720(16) Uani 1 1 d . . . H6A1 H 0.3326 0.6624 0.1555 0.086 Uiso 1 1 calc R . . C1B C 0.2197(2) 0.3830(3) 0.13865(12) 0.0547(14) Uani 1 1 d . . . C2B C 0.1532(2) 0.4141(4) 0.13273(16) 0.0783(18) Uani 1 1 d . . . H2B H 0.1426 0.4787 0.1266 0.094 Uiso 1 1 calc R . . C3B C 0.1042(2) 0.3447(5) 0.13634(17) 0.092(2) Uani 1 1 d . . . H3B H 0.0597 0.3639 0.1330 0.111 Uiso 1 1 calc R . . C4B C 0.1175(3) 0.2514(5) 0.14442(16) 0.096(2) Uani 1 1 d . . . H4B H 0.0828 0.2068 0.1466 0.116 Uiso 1 1 calc R . . C5B C 0.1822(3) 0.2221(4) 0.14937(15) 0.0875(19) Uani 1 1 d . . . H5B H 0.1921 0.1568 0.1544 0.105 Uiso 1 1 calc R . . C6B C 0.2333(2) 0.2889(4) 0.14691(12) 0.0642(15) Uani 1 1 d . . . H6B1 H 0.2776 0.2688 0.1510 0.077 Uiso 1 1 calc R . . C1C C 0.26197(16) 0.5298(3) 0.08515(11) 0.0470(12) Uani 1 1 d . . . C2C C 0.2568(2) 0.4719(4) 0.05046(12) 0.0595(14) Uani 1 1 d . . . H2C H 0.2655 0.4056 0.0534 0.071 Uiso 1 1 calc R . . C3C C 0.2396(2) 0.5075(4) 0.01190(14) 0.0783(18) Uani 1 1 d . . . H3C H 0.2375 0.4665 -0.0116 0.094 Uiso 1 1 calc R . . C4C C 0.2250(3) 0.6050(4) 0.00743(16) 0.085(2) Uani 1 1 d . . . H4C H 0.2111 0.6301 -0.0188 0.102 Uiso 1 1 calc R . . C5C C 0.2311(3) 0.6622(4) 0.04081(14) 0.0822(17) Uani 1 1 d . . . H5C H 0.2235 0.7287 0.0374 0.099 Uiso 1 1 calc R . . C6C C 0.2480(2) 0.6278(4) 0.07982(15) 0.0635(14) Uani 1 1 d . . . H6C H 0.2502 0.6698 0.1030 0.076 Uiso 1 1 calc R . . C1D C 0.42256(18) 0.5587(3) 0.07216(11) 0.0394(10) Uani 1 1 d . . . C2D C 0.4060(2) 0.5910(3) 0.03207(14) 0.0562(13) Uani 1 1 d . . . H2D H 0.3966 0.5465 0.0104 0.067 Uiso 1 1 calc R . . C3D C 0.4032(2) 0.6905(4) 0.02392(16) 0.0701(16) Uani 1 1 d . . . H3D H 0.3918 0.7120 -0.0034 0.084 Uiso 1 1 calc R . . C4D C 0.4163(2) 0.7550(4) 0.05405(16) 0.0792(18) Uani 1 1 d . . . H4D H 0.4147 0.8213 0.0480 0.095 Uiso 1 1 calc R . . C5D C 0.4325(2) 0.7234(4) 0.09469(16) 0.0706(16) Uani 1 1 d . . . H5D H 0.4408 0.7686 0.1162 0.085 Uiso 1 1 calc R . . C6D C 0.4365(2) 0.6248(3) 0.10361(15) 0.0562(13) Uani 1 1 d . . . H6D H 0.4487 0.6037 0.1309 0.067 Uiso 1 1 calc R . . C1E C 0.40231(19) 0.3533(3) 0.04614(12) 0.0469(12) Uani 1 1 d . . . C2E C 0.4261(2) 0.3597(3) 0.00568(12) 0.0548(13) Uani 1 1 d . . . H2E H 0.4547 0.4104 -0.0011 0.066 Uiso 1 1 calc R . . C3E C 0.4083(2) 0.2935(4) -0.02392(14) 0.0758(17) Uani 1 1 d . . . H3E H 0.4240 0.2999 -0.0512 0.091 Uiso 1 1 calc R . . C4E C 0.3683(3) 0.2184(4) -0.01502(16) 0.105(2) Uani 1 1 d . . . H4E H 0.3568 0.1728 -0.0359 0.126 Uiso 1 1 calc R . . C5E C 0.3444(4) 0.2091(5) 0.02481(17) 0.127(2) Uani 1 1 d . . . H5E H 0.3158 0.1580 0.0311 0.153 Uiso 1 1 calc R . . C6E C 0.3632(3) 0.2765(4) 0.05578(15) 0.0853(17) Uani 1 1 d . . . H6E H 0.3488 0.2689 0.0833 0.102 Uiso 1 1 calc R . . C1F C 0.51922(19) 0.4102(3) 0.08935(11) 0.0484(12) Uani 1 1 d . . . C2F C 0.5404(2) 0.3155(3) 0.09042(13) 0.0542(13) Uani 1 1 d . . . H2F H 0.5096 0.2649 0.0874 0.065 Uiso 1 1 calc R . . C3F C 0.6065(2) 0.2959(4) 0.09587(14) 0.0701(16) Uani 1 1 d . . . H3F H 0.6199 0.2311 0.0975 0.084 Uiso 1 1 calc R . . C4F C 0.6535(2) 0.3653(4) 0.09907(15) 0.0779(18) Uani 1 1 d . . . H4F H 0.6986 0.3489 0.1023 0.093 Uiso 1 1 calc R . . C5F C 0.6337(2) 0.4613(4) 0.09748(14) 0.0728(17) Uani 1 1 d . . . H5F H 0.6654 0.5110 0.0994 0.087 Uiso 1 1 calc R . . C6F C 0.5655(2) 0.4836(4) 0.09300(14) 0.0610(14) Uani 1 1 d . . . H6F H 0.5516 0.5483 0.0925 0.073 Uiso 1 1 calc R . . O1S O 0.5364(6) 0.0629(9) 0.0799(4) 0.174(5) Uiso 0.50 1 d P . . O2S O 0.4911(5) 0.6295(7) 0.2935(3) 0.142(4) Uani 0.50 1 d P . . P3 P 0.34547(12) 1.00179(17) 0.13111(7) 0.1018(7) Uani 0.616(4) 1 d PD A 1 F1 F 0.28388(16) 1.0019(3) 0.15795(10) 0.332(6) Uani 0.616(4) 1 d PD A 1 F2 F 0.40376(16) 1.0001(3) 0.10434(11) 0.332(6) Uani 0.616(4) 1 d PD A 1 F3 F 0.29909(17) 1.0136(4) 0.09213(10) 0.259(3) Uani 0.616(4) 1 d PD A 1 F4 F 0.3374(2) 0.8922(2) 0.12668(16) 0.240(4) Uani 0.616(4) 1 d PD A 1 F6 F 0.3496(2) 1.1098(2) 0.13559(16) 0.240(4) Uani 0.616(4) 1 d PD A 1 F5 F 0.38855(17) 0.9886(4) 0.17033(10) 0.259(3) Uani 0.616(4) 1 d PD A 1 P3A P 0.34251(15) 0.9884(2) 0.13060(9) 0.1018(7) Uani 0.384(4) 1 d PD A 2 F1A F 0.28337(18) 0.9802(3) 0.15922(11) 0.243(5) Uani 0.384(4) 1 d PD A 2 F2A F 0.39908(17) 0.9939(3) 0.10150(11) 0.243(5) Uani 0.384(4) 1 d PD A 2 F4A F 0.31090(19) 0.9077(3) 0.10308(13) 0.204(4) Uani 0.384(4) 1 d PD A 2 F6A F 0.3734(3) 1.0665(3) 0.15834(13) 0.204(4) Uani 0.384(4) 1 d PD A 2 F5A F 0.37854(19) 0.9107(3) 0.15643(13) 0.192(5) Uani 0.384(4) 1 d PD A 2 F3A F 0.30383(19) 1.0631(3) 0.10428(13) 0.192(5) Uani 0.384(4) 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 0.03695(7) 0.04813(8) 0.03425(7) 0.00030(8) -0.00381(5) 0.00037(8) P1 0.0361(5) 0.0620(7) 0.0366(5) 0.0058(5) -0.0004(4) 0.0009(5) P2 0.0403(5) 0.0468(6) 0.0377(5) -0.0050(5) -0.0020(4) -0.0013(5) O1 0.0564(17) 0.084(2) 0.0570(16) 0.0024(17) -0.0054(14) -0.0001(17) O2 0.0406(14) 0.0643(18) 0.0366(13) -0.0034(13) -0.0019(11) -0.0003(13) N1 0.0449(17) 0.0486(19) 0.0364(15) 0.0008(16) -0.0068(13) 0.0035(16) C1 0.044(2) 0.061(3) 0.041(2) -0.005(2) -0.0004(17) 0.001(2) C2 0.0346(19) 0.084(3) 0.0375(19) 0.002(2) 0.0020(16) 0.010(2) C3 0.062(3) 0.095(4) 0.071(3) 0.011(3) -0.011(2) 0.027(3) C4 0.082(3) 0.051(3) 0.106(4) 0.001(3) -0.010(3) 0.015(3) C5 0.056(2) 0.072(3) 0.055(2) -0.001(2) -0.002(2) -0.002(2) C6 0.047(2) 0.115(4) 0.039(2) -0.004(3) -0.0018(18) -0.002(3) C7 0.0273(17) 0.069(3) 0.048(2) -0.003(2) -0.0044(16) -0.0127(18) C1A 0.047(2) 0.084(3) 0.053(2) -0.004(2) -0.002(2) 0.015(2) C2A 0.076(3) 0.105(4) 0.038(2) 0.002(3) 0.007(2) 0.032(3) C3A 0.100(4) 0.143(5) 0.064(3) 0.010(3) 0.016(3) 0.059(4) C4A 0.127(5) 0.129(5) 0.065(3) -0.033(3) -0.014(3) 0.059(4) C5A 0.124(5) 0.103(4) 0.093(4) -0.030(4) -0.015(4) 0.037(4) C6A 0.058(3) 0.088(4) 0.069(3) -0.021(3) -0.011(2) 0.021(3) C1B 0.053(2) 0.080(3) 0.0305(18) 0.007(2) 0.0012(17) -0.013(2) C2B 0.046(2) 0.103(4) 0.086(3) 0.010(3) -0.006(2) -0.006(3) C3B 0.046(3) 0.125(5) 0.106(4) 0.005(4) -0.014(3) -0.024(3) C4B 0.085(3) 0.125(5) 0.080(3) -0.010(4) 0.001(3) -0.048(3) C5B 0.098(4) 0.096(4) 0.067(3) 0.008(3) -0.008(3) -0.041(3) C6B 0.065(3) 0.077(3) 0.049(2) 0.010(2) -0.013(2) -0.021(3) C1C 0.0231(17) 0.082(3) 0.0353(18) 0.008(2) -0.0027(14) -0.0017(19) C2C 0.068(3) 0.070(3) 0.040(2) 0.003(2) -0.0082(19) -0.019(2) C3C 0.072(3) 0.106(4) 0.057(3) 0.003(3) -0.003(2) -0.027(3) C4C 0.068(3) 0.124(5) 0.062(3) 0.026(3) -0.012(2) -0.006(3) C5C 0.096(4) 0.091(4) 0.060(3) 0.035(3) 0.008(3) 0.033(3) C6C 0.062(3) 0.064(3) 0.065(3) 0.008(2) 0.010(2) 0.020(2) C1D 0.0358(18) 0.041(2) 0.0414(19) 0.0020(18) 0.0065(16) -0.0027(17) C2D 0.044(2) 0.065(3) 0.059(2) 0.000(2) 0.0014(19) 0.004(2) C3D 0.066(3) 0.067(3) 0.077(3) 0.017(3) 0.008(2) 0.016(3) C4D 0.071(3) 0.066(3) 0.101(4) 0.016(3) 0.011(3) 0.012(3) C5D 0.063(3) 0.054(3) 0.095(3) -0.024(3) 0.006(3) -0.002(2) C6D 0.051(2) 0.052(3) 0.066(3) -0.002(2) -0.005(2) -0.001(2) C1E 0.050(2) 0.048(2) 0.042(2) 0.000(2) -0.0004(18) 0.000(2) C2E 0.060(2) 0.057(3) 0.047(2) -0.011(2) 0.005(2) -0.020(2) C3E 0.078(3) 0.097(4) 0.054(2) -0.023(3) 0.016(2) -0.016(3) C4E 0.145(5) 0.101(4) 0.070(3) -0.037(3) 0.014(3) -0.061(4) C5E 0.198(5) 0.108(4) 0.079(3) -0.046(3) 0.052(4) -0.091(4) C6E 0.109(4) 0.089(3) 0.060(3) -0.010(3) 0.019(3) -0.056(3) C1F 0.041(2) 0.071(3) 0.0332(18) -0.001(2) 0.0045(16) -0.006(2) C2F 0.043(2) 0.061(3) 0.059(2) -0.007(2) 0.0077(19) 0.010(2) C3F 0.068(3) 0.082(3) 0.062(3) -0.005(3) 0.018(2) 0.024(3) C4F 0.045(2) 0.109(4) 0.079(3) -0.023(3) -0.001(2) 0.016(3) C5F 0.049(2) 0.104(4) 0.066(3) -0.010(3) 0.010(2) -0.007(3) C6F 0.043(2) 0.068(3) 0.071(3) 0.001(3) 0.002(2) 0.006(2) O2S 0.174(8) 0.111(6) 0.141(7) -0.057(6) 0.020(7) 0.045(6) P3 0.1016(12) 0.0922(13) 0.1111(12) -0.0099(12) 0.0002(11) 0.0067(11) F1 0.256(7) 0.524(15) 0.224(6) -0.075(9) 0.105(5) 0.086(10) F2 0.256(7) 0.524(15) 0.224(6) -0.075(9) 0.105(5) 0.086(10) F3 0.275(6) 0.300(7) 0.193(5) 0.064(5) -0.121(4) -0.159(5) F4 0.216(6) 0.099(4) 0.396(9) -0.028(5) -0.121(6) -0.007(4) F6 0.216(6) 0.099(4) 0.396(9) -0.028(5) -0.121(6) -0.007(4) F5 0.275(6) 0.300(7) 0.193(5) 0.064(5) -0.121(4) -0.159(5) P3A 0.1016(12) 0.0922(13) 0.1111(12) -0.0099(12) 0.0002(11) 0.0067(11) F1A 0.151(5) 0.180(8) 0.408(14) -0.006(9) 0.156(7) -0.079(6) F2A 0.151(5) 0.180(8) 0.408(14) -0.006(9) 0.156(7) -0.079(6) F4A 0.128(7) 0.152(5) 0.331(10) -0.169(5) -0.020(7) -0.013(5) F6A 0.128(7) 0.152(5) 0.331(10) -0.169(5) -0.020(7) -0.013(5) F5A 0.187(9) 0.184(9) 0.204(10) -0.004(8) -0.020(8) 0.054(7) F3A 0.187(9) 0.184(9) 0.204(10) -0.004(8) -0.020(8) 0.054(7) _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 N1 2.074(3) . ? Pt1 O2 2.084(2) 2_655 ? Pt1 P2 2.2452(10) . ? Pt1 P1 2.2631(11) . ? P1 C1B 1.814(5) . ? P1 C1A 1.818(5) . ? P1 C1C 1.826(4) . ? P2 C1D 1.799(4) . ? P2 C1E 1.802(4) . ? P2 C1F 1.822(4) . ? O1 C7 1.228(5) . ? O2 C7 1.284(5) . ? O2 Pt1 2.084(2) 2_655 ? N1 C5 1.327(6) . ? N1 C1 1.327(5) . ? C1 C2 1.377(5) . ? C2 C3 1.378(7) . ? C2 C6 1.486(6) . ? C3 C4 1.387(7) . ? C4 C5 1.400(7) . ? C6 C7 1.514(6) . ? C1A C2A 1.374(6) . ? C1A C6A 1.377(7) . ? C2A C3A 1.382(7) . ? C3A C4A 1.364(9) . ? C4A C5A 1.376(8) . ? C5A C6A 1.374(8) . ? C1B C6B 1.357(7) . ? C1B C2B 1.416(6) . ? C2B C3B 1.386(8) . ? C3B C4B 1.344(9) . ? C4B C5B 1.372(8) . ? C5B C6B 1.390(7) . ? C1C C2C 1.367(6) . ? C1C C6C 1.397(7) . ? C2C C3C 1.358(6) . ? C3C C4C 1.389(8) . ? C4C C5C 1.330(7) . ? C5C C6C 1.363(6) . ? C1D C6D 1.380(6) . ? C1D C2D 1.383(6) . ? C2D C3D 1.405(7) . ? C3D C4D 1.331(7) . ? C4D C5D 1.395(7) . ? C5D C6D 1.398(7) . ? C1E C6E 1.367(7) . ? C1E C2E 1.396(5) . ? C2E C3E 1.355(6) . ? C3E C4E 1.354(8) . ? C4E C5E 1.381(8) . ? C5E C6E 1.401(7) . ? C1F C2F 1.381(6) . ? C1F C6F 1.383(6) . ? C2F C3F 1.364(6) . ? C3F C4F 1.353(7) . ? C4F C5F 1.391(8) . ? C5F C6F 1.413(6) . ? P3 F2 1.479(4) . ? P3 F6 1.506(4) . ? P3 F5 1.507(4) . ? P3 F4 1.534(4) . ? P3 F1 1.535(4) . ? P3 F3 1.536(4) . ? P3A F2A 1.500(4) . ? P3A F6A 1.517(5) . ? P3A F5A 1.523(5) . ? P3A F3A 1.529(5) . ? P3A F1A 1.534(4) . ? P3A F4A 1.545(5) . ? 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 N1 Pt1 O2 84.04(11) . 2_655 ? N1 Pt1 P2 92.47(8) . . ? O2 Pt1 P2 176.50(8) 2_655 . ? N1 Pt1 P1 168.65(8) . . ? O2 Pt1 P1 84.65(7) 2_655 . ? P2 Pt1 P1 98.82(4) . . ? C1B P1 C1A 107.3(2) . . ? C1B P1 C1C 101.01(18) . . ? C1A P1 C1C 107.5(2) . . ? C1B P1 Pt1 110.48(15) . . ? C1A P1 Pt1 107.35(14) . . ? C1C P1 Pt1 122.29(12) . . ? C1D P2 C1E 112.28(18) . . ? C1D P2 C1F 105.05(19) . . ? C1E P2 C1F 101.18(18) . . ? C1D P2 Pt1 111.13(13) . . ? C1E P2 Pt1 114.53(14) . . ? C1F P2 Pt1 111.87(12) . . ? C7 O2 Pt1 112.6(2) . 2_655 ? C5 N1 C1 119.6(3) . . ? C5 N1 Pt1 117.5(3) . . ? C1 N1 Pt1 122.8(3) . . ? N1 C1 C2 123.3(4) . . ? C1 C2 C3 117.3(4) . . ? C1 C2 C6 121.0(4) . . ? C3 C2 C6 121.6(4) . . ? C2 C3 C4 120.6(4) . . ? C3 C4 C5 117.6(5) . . ? N1 C5 C4 121.6(4) . . ? C2 C6 C7 107.9(3) . . ? O1 C7 O2 125.8(4) . . ? O1 C7 C6 119.3(4) . . ? O2 C7 C6 114.8(4) . . ? C2A C1A C6A 118.3(5) . . ? C2A C1A P1 120.5(4) . . ? C6A C1A P1 120.6(3) . . ? C1A C2A C3A 120.6(5) . . ? C4A C3A C2A 119.5(5) . . ? C3A C4A C5A 121.4(6) . . ? C6A C5A C4A 117.9(6) . . ? C5A C6A C1A 122.2(5) . . ? C6B C1B C2B 120.1(4) . . ? C6B C1B P1 122.5(3) . . ? C2B C1B P1 117.4(4) . . ? C3B C2B C1B 116.9(5) . . ? C4B C3B C2B 123.1(5) . . ? C3B C4B C5B 119.3(5) . . ? C4B C5B C6B 120.0(6) . . ? C1B C6B C5B 120.5(5) . . ? C2C C1C C6C 117.6(4) . . ? C2C C1C P1 118.1(4) . . ? C6C C1C P1 124.2(3) . . ? C3C C2C C1C 121.9(5) . . ? C2C C3C C4C 119.5(5) . . ? C5C C4C C3C 119.1(5) . . ? C4C C5C C6C 122.2(5) . . ? C5C C6C C1C 119.6(5) . . ? C6D C1D C2D 119.5(4) . . ? C6D C1D P2 115.4(3) . . ? C2D C1D P2 125.1(3) . . ? C1D C2D C3D 119.7(4) . . ? C4D C3D C2D 121.4(5) . . ? C3D C4D C5D 119.5(5) . . ? C4D C5D C6D 120.4(5) . . ? C1D C6D C5D 119.5(4) . . ? C6E C1E C2E 118.7(4) . . ? C6E C1E P2 119.2(3) . . ? C2E C1E P2 121.6(3) . . ? C3E C2E C1E 120.5(4) . . ? C4E C3E C2E 121.3(4) . . ? C3E C4E C5E 119.7(5) . . ? C4E C5E C6E 119.4(6) . . ? C1E C6E C5E 120.3(5) . . ? C2F C1F C6F 119.3(4) . . ? C2F C1F P2 118.5(3) . . ? C6F C1F P2 122.0(3) . . ? C3F C2F C1F 119.5(4) . . ? C4F C3F C2F 123.2(5) . . ? C3F C4F C5F 118.6(4) . . ? C4F C5F C6F 119.4(5) . . ? C1F C6F C5F 120.0(5) . . ? F2 P3 F6 91.6(2) . . ? F2 P3 F5 91.7(2) . . ? F6 P3 F5 90.8(3) . . ? F2 P3 F4 90.9(2) . . ? F6 P3 F4 177.1(3) . . ? F5 P3 F4 90.7(3) . . ? F2 P3 F1 178.4(3) . . ? F6 P3 F1 89.4(2) . . ? F5 P3 F1 89.5(2) . . ? F4 P3 F1 88.1(2) . . ? F2 P3 F3 90.5(2) . . ? F6 P3 F3 90.0(3) . . ? F5 P3 F3 177.6(3) . . ? F4 P3 F3 88.4(3) . . ? F1 P3 F3 88.2(2) . . ? F2A P3A F6A 91.1(3) . . ? F2A P3A F5A 90.7(2) . . ? F6A P3A F5A 90.7(3) . . ? F2A P3A F3A 90.6(2) . . ? F6A P3A F3A 91.5(3) . . ? F5A P3A F3A 177.4(3) . . ? F2A P3A F1A 177.9(3) . . ? F6A P3A F1A 91.0(3) . . ? F5A P3A F1A 89.6(2) . . ? F3A P3A F1A 89.1(2) . . ? F2A P3A F4A 89.6(2) . . ? F6A P3A F4A 178.9(3) . . ? F5A P3A F4A 88.5(3) . . ? F3A P3A F4A 89.3(3) . . ? F1A P3A F4A 88.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.780 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.149 # Attachment 'complex6_new.cif' data_7511b _database_code_depnum_ccdc_archive 'CCDC 711712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H74 Ca Cl6 F12 Fe2 N2 O16 P4 Pd2 S4' _chemical_formula_weight 2496.91 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.533(17) _cell_length_b 19.872(13) _cell_length_c 21.352(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10834(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 169 _cell_measurement_theta_min 5.74 _cell_measurement_theta_max 16.30 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5016 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8251 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74964 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9545 _reflns_number_gt 7206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Both the free Otf and the CHCl3 have very large thermal parameters. Restraints in bond lengths and thermal parameters were applied. ; _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^)+(0.1363P)^2^+304.3844P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9545 _refine_ls_number_parameters 587 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1864 _refine_ls_R_factor_gt 0.1573 _refine_ls_wR_factor_ref 0.3872 _refine_ls_wR_factor_gt 0.3712 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.002 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 C21 C 0.2200(12) 0.3526(13) 0.8738(15) 0.26(3) Uiso 1 1 d D . . H21 H 0.2467 0.3576 0.9065 0.308 Uiso 1 1 calc R . . Cl3 Cl 0.1882(12) 0.2743(12) 0.8692(12) 0.44(2) Uani 1 1 d D . . Cl2 Cl 0.2404(7) 0.3640(16) 0.7964(9) 0.44(2) Uani 1 1 d D . . Cl1 Cl 0.1660(6) 0.4061(16) 0.8781(10) 0.397(17) Uani 1 1 d D . . S2 S 0.3146(4) 0.3432(7) 0.0379(6) 0.160(4) Uani 1 1 d DU . . O6 O 0.3557(8) 0.3895(13) 0.0567(12) 0.192(7) Uani 1 1 d D . . O7 O 0.3060(10) 0.3410(15) -0.0287(8) 0.192(7) Uani 1 1 d D . . O8 O 0.3141(11) 0.2871(11) 0.0789(13) 0.192(7) Uani 1 1 d DU . . C20 C 0.2573(8) 0.3892(11) 0.0632(11) 0.355(14) Uiso 1 1 d D . . F4 F 0.2606(14) 0.4027(19) 0.1231(12) 0.355(14) Uiso 1 1 d D . . F5 F 0.2542(14) 0.4463(13) 0.0303(18) 0.355(14) Uiso 1 1 d D . . F6 F 0.2148(8) 0.3527(19) 0.0516(19) 0.355(14) Uiso 1 1 d D . . Pd1 Pd 0.60018(4) 0.22873(5) 0.14948(6) 0.0378(4) Uani 1 1 d . . . Fe2 Fe 0.44176(8) 0.25165(11) 0.22139(11) 0.0422(6) Uani 1 1 d . . . Ca1 Ca 0.7500 0.2500 0.3166(3) 0.0535(13) Uani 1 2 d S . . P1 P 0.54448(14) 0.14492(18) 0.18725(19) 0.0359(9) Uani 1 1 d . . . P2 P 0.54126(14) 0.31472(18) 0.13015(17) 0.0323(8) Uani 1 1 d . . . N1 N 0.8406(5) 0.2093(6) 0.1062(7) 0.048(4) Uani 1 1 d . . . O1 O 0.6540(4) 0.1499(5) 0.1610(6) 0.054(3) Uani 1 1 d . . . O2 O 0.6896(5) 0.2120(7) 0.2416(7) 0.070(4) Uani 1 1 d . . . C1 C 0.8307(8) 0.2185(9) 0.0440(10) 0.063(5) Uani 1 1 d . . . H1 H 0.8499 0.2494 0.0207 0.076 Uiso 1 1 calc R . . C2 C 0.7898(8) 0.1791(11) 0.0152(14) 0.091(9) Uani 1 1 d . . . H2 H 0.7813 0.1860 -0.0267 0.110 Uiso 1 1 calc R . . C3 C 0.7632(7) 0.1310(11) 0.0497(14) 0.080(7) Uani 1 1 d . . . H3 H 0.7378 0.1046 0.0305 0.096 Uiso 1 1 calc R . . C4 C 0.8128(5) 0.1624(8) 0.1409(10) 0.052(4) Uani 1 1 d . . . H4 H 0.8202 0.1583 0.1833 0.062 Uiso 1 1 calc R . . C5 C 0.7746(6) 0.1215(8) 0.1153(14) 0.077(8) Uani 1 1 d . . . C6 C 0.7451(8) 0.0674(9) 0.1557(15) 0.095(9) Uani 1 1 d . . . H6A H 0.7686 0.0301 0.1642 0.113 Uiso 1 1 calc R . . H6B H 0.7155 0.0502 0.1322 0.113 Uiso 1 1 calc R . . C7 C 0.7245(8) 0.0984(11) 0.2214(14) 0.094(9) Uani 1 1 d . . . H7A H 0.7059 0.0639 0.2444 0.113 Uiso 1 1 calc R . . H7B H 0.7543 0.1123 0.2464 0.113 Uiso 1 1 calc R . . C8 C 0.6877(5) 0.1598(9) 0.2108(11) 0.061(6) Uani 1 1 d . . . C9 C 0.4757(6) 0.1583(7) 0.2020(7) 0.036(3) Uani 1 1 d . . . C10 C 0.4372(6) 0.1755(8) 0.1504(10) 0.056(5) Uani 1 1 d . . . H10 H 0.4440 0.1800 0.1054 0.067 Uiso 1 1 calc R . . C11 C 0.3880(6) 0.1820(10) 0.1832(12) 0.068(6) Uani 1 1 d . . . H11 H 0.3549 0.1945 0.1632 0.082 Uiso 1 1 calc R . . C12 C 0.3942(7) 0.1708(9) 0.2493(13) 0.078(7) Uani 1 1 d . . . H12 H 0.3661 0.1733 0.2805 0.094 Uiso 1 1 calc R . . C13 C 0.4500(6) 0.1559(8) 0.2631(8) 0.048(4) Uani 1 1 d . . . H13 H 0.4658 0.1450 0.3037 0.057 Uiso 1 1 calc R . . C14 C 0.4888(6) 0.3281(7) 0.1893(8) 0.041(4) Uani 1 1 d . . . C15 C 0.4935(6) 0.3221(8) 0.2566(8) 0.046(4) Uani 1 1 d . . . H15 H 0.5259 0.3117 0.2792 0.055 Uiso 1 1 calc R . . C16 C 0.4426(7) 0.3354(8) 0.2859(8) 0.048(4) Uani 1 1 d . . . H16 H 0.4339 0.3350 0.3306 0.058 Uiso 1 1 calc R . . C17 C 0.4092(6) 0.3486(8) 0.2354(8) 0.052(4) Uani 1 1 d . . . H17 H 0.3715 0.3563 0.2404 0.062 Uiso 1 1 calc R . . C18 C 0.4348(6) 0.3438(8) 0.1735(8) 0.046(4) Uani 1 1 d . . . H18 H 0.4196 0.3523 0.1321 0.055 Uiso 1 1 calc R . . C1A C 0.5432(6) 0.0700(7) 0.1334(7) 0.039(3) Uani 1 1 d . . . C2A C 0.5796(6) 0.0612(8) 0.0820(9) 0.054(4) Uani 1 1 d . . . H2A H 0.6045 0.0942 0.0740 0.065 Uiso 1 1 calc R . . C3A C 0.5779(7) 0.0037(9) 0.0442(10) 0.063(5) Uani 1 1 d . . . H3A H 0.6025 -0.0014 0.0124 0.075 Uiso 1 1 calc R . . C4A C 0.5395(8) -0.0470(9) 0.0533(11) 0.067(5) Uani 1 1 d . . . H4A H 0.5386 -0.0849 0.0279 0.080 Uiso 1 1 calc R . . C5A C 0.5037(7) -0.0384(9) 0.1008(9) 0.054(4) Uani 1 1 d . . . H5A H 0.4782 -0.0710 0.1077 0.064 Uiso 1 1 calc R . . C6A C 0.5052(6) 0.0201(8) 0.1396(8) 0.045(4) Uani 1 1 d . . . H6A1 H 0.4797 0.0252 0.1704 0.054 Uiso 1 1 calc R . . C1B C 0.5700(6) 0.1158(8) 0.2642(7) 0.041(4) Uani 1 1 d . . . C2B C 0.5849(7) 0.1649(8) 0.3138(7) 0.050(4) Uani 1 1 d . . . H2B H 0.5807 0.2106 0.3058 0.060 Uiso 1 1 calc R . . C3B C 0.6049(7) 0.1452(10) 0.3711(8) 0.059(5) Uani 1 1 d . . . H3B H 0.6127 0.1774 0.4013 0.071 Uiso 1 1 calc R . . C4B C 0.6132(9) 0.0775(11) 0.3836(9) 0.077(6) Uani 1 1 d . . . H4B H 0.6258 0.0648 0.4227 0.092 Uiso 1 1 calc R . . C5B C 0.6030(11) 0.0273(10) 0.3381(9) 0.091(9) Uani 1 1 d . . . H5B H 0.6107 -0.0175 0.3464 0.109 Uiso 1 1 calc R . . C6B C 0.5808(10) 0.0463(10) 0.2792(10) 0.076(6) Uani 1 1 d . . . H6B1 H 0.5731 0.0131 0.2499 0.091 Uiso 1 1 calc R . . C1C C 0.5119(5) 0.3029(7) 0.0486(7) 0.034(3) Uani 1 1 d . . . C2C C 0.4785(6) 0.3536(7) 0.0238(7) 0.042(4) Uani 1 1 d . . . H2C H 0.4723 0.3934 0.0455 0.050 Uiso 1 1 calc R . . C3C C 0.4556(8) 0.3416(10) -0.0340(9) 0.065(5) Uani 1 1 d . . . H3C H 0.4325 0.3737 -0.0497 0.078 Uiso 1 1 calc R . . C4C C 0.4656(8) 0.2820(10) -0.0715(9) 0.064(5) Uani 1 1 d . . . H4C H 0.4501 0.2759 -0.1106 0.077 Uiso 1 1 calc R . . C5C C 0.5003(9) 0.2334(10) -0.0453(10) 0.072(6) Uani 1 1 d . . . H5C H 0.5079 0.1942 -0.0673 0.087 Uiso 1 1 calc R . . C6C C 0.5230(6) 0.2443(8) 0.0136(8) 0.049(4) Uani 1 1 d . . . H6C H 0.5458 0.2123 0.0299 0.059 Uiso 1 1 calc R . . C1D C 0.5714(5) 0.4016(7) 0.1276(7) 0.036(3) Uani 1 1 d . . . C2D C 0.5917(6) 0.4281(8) 0.0686(9) 0.049(4) Uani 1 1 d . . . H2D H 0.5869 0.4047 0.0314 0.058 Uiso 1 1 calc R . . C3D C 0.6193(7) 0.4907(8) 0.0694(9) 0.057(5) Uani 1 1 d . . . H3D H 0.6315 0.5094 0.0323 0.068 Uiso 1 1 calc R . . C4D C 0.6279(6) 0.5234(8) 0.1266(10) 0.057(5) Uani 1 1 d . . . H4D H 0.6461 0.5640 0.1266 0.068 Uiso 1 1 calc R . . C5D C 0.6099(6) 0.4972(8) 0.1844(9) 0.049(4) Uani 1 1 d . . . H5D H 0.6155 0.5206 0.2216 0.059 Uiso 1 1 calc R . . C6D C 0.5832(6) 0.4348(8) 0.1847(8) 0.045(4) Uani 1 1 d . . . H6D H 0.5733 0.4155 0.2226 0.054 Uiso 1 1 calc R . . S1 S 0.64769(18) 0.3507(3) 0.3799(3) 0.0737(16) Uani 1 1 d . . . O3 O 0.6965(5) 0.3160(7) 0.3813(7) 0.078(4) Uani 1 1 d . . . O4 O 0.6185(8) 0.3414(10) 0.3231(13) 0.154(10) Uani 1 1 d . . . O5 O 0.6202(9) 0.3463(10) 0.4414(13) 0.159(11) Uani 1 1 d . . . C19 C 0.6659(9) 0.4434(11) 0.3805(12) 0.075(6) Uani 1 1 d . . . F1 F 0.6243(6) 0.4828(6) 0.3765(9) 0.120(6) Uani 1 1 d . . . F2 F 0.6925(6) 0.4579(7) 0.3271(9) 0.125(6) Uani 1 1 d . . . F3 F 0.6907(8) 0.4604(9) 0.4318(8) 0.135(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.56(4) 0.38(3) 0.37(3) 0.08(3) -0.25(3) -0.27(4) Cl2 0.182(16) 0.94(7) 0.210(17) -0.06(3) -0.032(14) 0.08(3) Cl1 0.120(11) 0.73(5) 0.35(3) -0.14(3) -0.076(14) 0.05(2) S2 0.124(7) 0.213(12) 0.144(9) 0.008(8) -0.036(7) -0.037(8) O6 0.185(15) 0.234(18) 0.157(13) 0.054(13) -0.070(12) -0.037(13) O7 0.185(15) 0.234(18) 0.157(13) 0.054(13) -0.070(12) -0.037(13) O8 0.185(15) 0.234(18) 0.157(13) 0.054(13) -0.070(12) -0.037(13) Pd1 0.0231(5) 0.0291(6) 0.0613(8) 0.0082(5) -0.0030(5) 0.0001(4) Fe2 0.0282(10) 0.0390(11) 0.0594(15) 0.0098(10) 0.0028(10) 0.0008(9) Ca1 0.025(2) 0.071(3) 0.064(3) 0.000 0.000 -0.006(2) P1 0.0273(18) 0.0325(19) 0.048(2) 0.0081(17) -0.0081(17) -0.0041(15) P2 0.0305(18) 0.0302(18) 0.036(2) 0.0051(15) 0.0006(15) 0.0028(14) N1 0.027(6) 0.029(7) 0.089(11) -0.016(7) -0.011(7) -0.002(5) O1 0.029(5) 0.034(6) 0.099(10) 0.010(6) -0.014(6) 0.005(4) O2 0.047(7) 0.052(8) 0.112(12) 0.014(8) -0.017(7) -0.009(6) C1 0.067(12) 0.036(9) 0.086(15) 0.001(9) -0.020(11) 0.003(8) C2 0.058(13) 0.054(12) 0.16(2) -0.034(14) -0.047(15) 0.021(10) C3 0.035(10) 0.057(12) 0.15(2) -0.031(14) -0.027(12) -0.005(9) C4 0.018(7) 0.045(9) 0.092(14) -0.015(9) -0.008(8) 0.001(6) C5 0.021(8) 0.028(9) 0.18(3) -0.023(12) -0.003(12) 0.008(6) C6 0.040(10) 0.037(10) 0.21(3) 0.004(14) -0.021(15) -0.001(8) C7 0.044(11) 0.063(13) 0.18(3) 0.047(16) -0.041(14) -0.008(10) C8 0.013(7) 0.049(11) 0.120(17) 0.029(11) 0.007(9) -0.003(7) C9 0.035(7) 0.030(7) 0.042(9) 0.006(6) -0.002(6) -0.003(6) C10 0.040(9) 0.048(10) 0.081(13) 0.017(9) -0.013(9) 0.004(7) C11 0.022(8) 0.065(12) 0.118(19) 0.011(12) 0.006(10) -0.006(8) C12 0.043(10) 0.043(10) 0.15(2) 0.010(12) 0.043(13) -0.009(8) C13 0.048(9) 0.044(9) 0.051(10) 0.015(7) 0.002(8) -0.006(7) C14 0.031(8) 0.034(8) 0.059(10) 0.007(7) 0.011(7) 0.007(6) C15 0.046(9) 0.047(9) 0.044(10) 0.007(7) 0.002(7) 0.010(7) C16 0.060(10) 0.051(10) 0.035(9) 0.006(7) 0.008(8) -0.001(8) C17 0.042(9) 0.049(10) 0.065(12) 0.014(8) 0.027(8) 0.016(7) C18 0.045(9) 0.040(8) 0.053(10) 0.017(7) 0.000(7) 0.011(7) C1A 0.033(8) 0.039(8) 0.045(9) 0.006(7) -0.008(7) -0.003(6) C2A 0.039(9) 0.038(9) 0.086(14) 0.007(9) 0.002(9) -0.004(7) C3A 0.055(11) 0.059(12) 0.074(14) -0.009(10) 0.012(10) -0.006(9) C4A 0.067(12) 0.038(9) 0.096(16) -0.003(9) -0.020(12) -0.001(8) C5A 0.045(10) 0.051(10) 0.066(12) 0.001(9) -0.002(9) -0.014(8) C6A 0.036(8) 0.053(10) 0.046(10) 0.004(7) -0.010(7) -0.011(7) C1B 0.042(9) 0.045(9) 0.036(9) 0.010(7) -0.010(7) -0.005(7) C2B 0.067(11) 0.046(9) 0.037(9) 0.005(7) -0.032(8) 0.005(8) C3B 0.067(12) 0.065(12) 0.045(10) -0.018(8) -0.009(9) 0.014(9) C4B 0.101(17) 0.084(15) 0.047(11) 0.008(11) -0.035(11) 0.020(12) C5B 0.17(3) 0.051(11) 0.046(12) 0.010(9) -0.053(14) 0.003(14) C6B 0.115(18) 0.047(11) 0.067(13) 0.003(9) -0.022(13) -0.007(11) C1C 0.018(6) 0.038(8) 0.047(9) 0.005(6) -0.006(6) -0.004(5) C2C 0.053(9) 0.035(8) 0.037(9) -0.008(7) 0.002(7) 0.008(7) C3C 0.070(12) 0.073(13) 0.052(11) -0.003(10) -0.022(10) 0.017(10) C4C 0.076(13) 0.075(13) 0.043(10) -0.002(9) -0.011(9) -0.006(10) C5C 0.088(15) 0.050(11) 0.079(15) -0.018(10) 0.009(12) -0.008(10) C6C 0.048(9) 0.037(8) 0.063(11) -0.001(8) -0.004(8) 0.006(7) C1D 0.027(7) 0.028(7) 0.053(9) -0.001(6) -0.006(6) 0.000(6) C2D 0.037(8) 0.044(9) 0.066(11) 0.001(8) 0.018(8) 0.000(7) C3D 0.063(11) 0.035(9) 0.072(13) 0.004(8) 0.016(10) 0.004(8) C4D 0.031(8) 0.028(8) 0.112(16) 0.001(9) -0.003(9) 0.001(6) C5D 0.048(10) 0.031(8) 0.068(12) -0.004(8) -0.002(8) 0.007(7) C6D 0.032(8) 0.045(9) 0.057(10) 0.009(8) -0.007(7) -0.002(7) S1 0.041(2) 0.056(3) 0.124(5) 0.020(3) 0.010(3) 0.007(2) O3 0.066(9) 0.089(10) 0.078(9) -0.007(8) -0.007(7) 0.037(8) O4 0.114(15) 0.091(13) 0.26(3) -0.013(15) -0.124(18) 0.004(11) O5 0.129(16) 0.101(14) 0.25(3) 0.100(17) 0.086(18) 0.053(13) C19 0.064(13) 0.069(13) 0.091(17) 0.003(12) 0.013(13) 0.020(11) F1 0.108(11) 0.058(8) 0.196(17) 0.024(9) 0.045(11) 0.027(8) F2 0.121(12) 0.083(10) 0.172(15) 0.013(10) 0.083(12) -0.006(9) F3 0.181(18) 0.111(13) 0.113(13) -0.027(10) -0.043(13) 0.008(12) _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 C21 Cl1 1.74(2) . ? C21 Cl2 1.75(2) . ? C21 Cl3 1.76(2) . ? S2 O8 1.417(16) . ? S2 O7 1.441(16) . ? S2 O6 1.451(17) . ? S2 C20 1.808(10) . ? C20 F4 1.310(19) . ? C20 F6 1.331(19) . ? C20 F5 1.336(19) . ? Pd1 O1 2.098(10) . ? Pd1 N1 2.157(12) 2_655 ? Pd1 P2 2.314(4) . ? Pd1 P1 2.334(4) . ? Fe2 C14 2.055(15) . ? Fe2 C15 2.067(17) . ? Fe2 C9 2.088(14) . ? Fe2 C12 2.100(17) . ? Fe2 C18 2.105(15) . ? Fe2 C13 2.111(15) . ? Fe2 C11 2.113(19) . ? Fe2 C17 2.120(16) . ? Fe2 C10 2.14(2) . ? Fe2 C16 2.160(17) . ? Ca1 O3 2.345(14) . ? Ca1 O3 2.345(14) 2_655 ? Ca1 O2 2.348(14) . ? Ca1 O2 2.348(14) 2_655 ? P1 C9 1.805(15) . ? P1 C1B 1.859(15) . ? P1 C1A 1.881(16) . ? P2 C14 1.859(15) . ? P2 C1D 1.891(14) . ? P2 C1C 1.910(15) . ? N1 C1 1.36(2) . ? N1 C4 1.39(2) . ? N1 Pd1 2.157(12) 2_655 ? O1 C8 1.38(2) . ? O2 C8 1.23(2) . ? C1 C2 1.44(3) . ? C2 C3 1.38(3) . ? C3 C5 1.44(3) . ? C4 C5 1.38(2) . ? C5 C6 1.57(3) . ? C6 C7 1.62(4) . ? C7 C8 1.56(2) . ? C9 C13 1.46(2) . ? C9 C10 1.51(2) . ? C10 C11 1.45(3) . ? C11 C12 1.44(3) . ? C12 C13 1.49(3) . ? C14 C15 1.45(2) . ? C14 C18 1.45(2) . ? C15 C16 1.47(2) . ? C16 C17 1.40(2) . ? C17 C18 1.48(2) . ? C1A C6A 1.39(2) . ? C1A C2A 1.45(2) . ? C2A C3A 1.40(2) . ? C3A C4A 1.42(3) . ? C4A C5A 1.38(3) . ? C5A C6A 1.43(2) . ? C1B C6B 1.44(2) . ? C1B C2B 1.49(2) . ? C2B C3B 1.38(2) . ? C3B C4B 1.39(3) . ? C4B C5B 1.42(3) . ? C5B C6B 1.43(3) . ? C1C C6C 1.41(2) . ? C1C C2C 1.42(2) . ? C2C C3C 1.39(2) . ? C3C C4C 1.45(3) . ? C4C C5C 1.43(3) . ? C5C C6C 1.40(3) . ? C1D C6D 1.42(2) . ? C1D C2D 1.46(2) . ? C2D C3D 1.43(2) . ? C3D C4D 1.40(3) . ? C4D C5D 1.42(3) . ? C5D C6D 1.41(2) . ? S1 O3 1.424(13) . ? S1 O4 1.43(2) . ? S1 O5 1.49(2) . ? S1 C19 1.90(2) . ? C19 F3 1.31(3) . ? C19 F1 1.32(2) . ? C19 F2 1.36(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 Cl1 C21 Cl2 101.9(17) . . ? Cl1 C21 Cl3 100.2(17) . . ? Cl2 C21 Cl3 101.5(17) . . ? O8 S2 O7 126(2) . . ? O8 S2 O6 109.6(17) . . ? O7 S2 O6 113.8(18) . . ? O8 S2 C20 101.9(12) . . ? O7 S2 C20 100.8(11) . . ? O6 S2 C20 100.4(12) . . ? F4 C20 F6 110.3(18) . . ? F4 C20 F5 110.1(17) . . ? F6 C20 F5 108.4(17) . . ? F4 C20 S2 110.1(16) . . ? F6 C20 S2 109.2(16) . . ? F5 C20 S2 108.7(16) . . ? O1 Pd1 N1 91.0(4) . 2_655 ? O1 Pd1 P2 176.5(4) . . ? N1 Pd1 P2 87.6(3) 2_655 . ? O1 Pd1 P1 80.0(3) . . ? N1 Pd1 P1 169.2(4) 2_655 . ? P2 Pd1 P1 101.10(14) . . ? C14 Fe2 C15 41.1(6) . . ? C14 Fe2 C9 110.3(6) . . ? C15 Fe2 C9 114.1(6) . . ? C14 Fe2 C12 176.8(9) . . ? C15 Fe2 C12 141.7(9) . . ? C9 Fe2 C12 67.5(6) . . ? C14 Fe2 C18 40.9(6) . . ? C15 Fe2 C18 69.0(6) . . ? C9 Fe2 C18 135.3(6) . . ? C12 Fe2 C18 139.0(8) . . ? C14 Fe2 C13 138.5(6) . . ? C15 Fe2 C13 113.1(6) . . ? C9 Fe2 C13 40.7(6) . . ? C12 Fe2 C13 41.3(7) . . ? C18 Fe2 C13 175.8(7) . . ? C14 Fe2 C11 137.3(8) . . ? C15 Fe2 C11 178.1(8) . . ? C9 Fe2 C11 67.1(6) . . ? C12 Fe2 C11 39.9(9) . . ? C18 Fe2 C11 109.1(8) . . ? C13 Fe2 C11 68.7(8) . . ? C14 Fe2 C17 66.7(6) . . ? C15 Fe2 C17 65.4(7) . . ? C9 Fe2 C17 176.3(6) . . ? C12 Fe2 C17 115.3(7) . . ? C18 Fe2 C17 40.9(6) . . ? C13 Fe2 C17 143.0(6) . . ? C11 Fe2 C17 113.3(7) . . ? C14 Fe2 C10 108.5(7) . . ? C15 Fe2 C10 140.3(6) . . ? C9 Fe2 C10 41.9(6) . . ? C12 Fe2 C10 68.3(9) . . ? C18 Fe2 C10 105.4(7) . . ? C13 Fe2 C10 70.6(7) . . ? C11 Fe2 C10 39.7(7) . . ? C17 Fe2 C10 136.0(7) . . ? C14 Fe2 C16 68.8(6) . . ? C15 Fe2 C16 40.6(6) . . ? C9 Fe2 C16 143.8(6) . . ? C12 Fe2 C16 114.4(8) . . ? C18 Fe2 C16 68.9(6) . . ? C13 Fe2 C16 115.1(6) . . ? C11 Fe2 C16 139.2(7) . . ? C17 Fe2 C16 38.2(7) . . ? C10 Fe2 C16 174.0(6) . . ? O3 Ca1 O3 107.7(7) . 2_655 ? O3 Ca1 O2 101.5(5) . . ? O3 Ca1 O2 127.2(5) 2_655 . ? O3 Ca1 O2 127.2(5) . 2_655 ? O3 Ca1 O2 101.5(5) 2_655 2_655 ? O2 Ca1 O2 94.1(7) . 2_655 ? C9 P1 C1B 103.4(7) . . ? C9 P1 C1A 101.9(7) . . ? C1B P1 C1A 107.5(7) . . ? C9 P1 Pd1 123.2(5) . . ? C1B P1 Pd1 108.3(5) . . ? C1A P1 Pd1 111.4(5) . . ? C14 P2 C1D 100.5(6) . . ? C14 P2 C1C 110.7(7) . . ? C1D P2 C1C 104.2(6) . . ? C14 P2 Pd1 116.9(5) . . ? C1D P2 Pd1 114.5(4) . . ? C1C P2 Pd1 109.1(4) . . ? C1 N1 C4 121.0(14) . . ? C1 N1 Pd1 118.1(12) . 2_655 ? C4 N1 Pd1 121.0(12) . 2_655 ? C8 O1 Pd1 113.1(10) . . ? C8 O2 Ca1 131.5(11) . . ? N1 C1 C2 118(2) . . ? C3 C2 C1 120(2) . . ? C2 C3 C5 120.5(18) . . ? C5 C4 N1 123(2) . . ? C4 C5 C3 117(2) . . ? C4 C5 C6 122(2) . . ? C3 C5 C6 121.7(19) . . ? C5 C6 C7 111.8(16) . . ? C8 C7 C6 111.6(19) . . ? O2 C8 O1 123.8(15) . . ? O2 C8 C7 124.0(19) . . ? O1 C8 C7 112.1(18) . . ? C13 C9 C10 111.5(14) . . ? C13 C9 P1 126.0(11) . . ? C10 C9 P1 122.5(12) . . ? C13 C9 Fe2 70.5(9) . . ? C10 C9 Fe2 71.1(9) . . ? P1 C9 Fe2 124.7(7) . . ? C11 C10 C9 103.4(17) . . ? C11 C10 Fe2 69.0(12) . . ? C9 C10 Fe2 67.0(9) . . ? C12 C11 C10 111.5(17) . . ? C12 C11 Fe2 69.6(11) . . ? C10 C11 Fe2 71.3(10) . . ? C11 C12 C13 109.3(16) . . ? C11 C12 Fe2 70.5(11) . . ? C13 C12 Fe2 69.7(9) . . ? C9 C13 C12 104.3(16) . . ? C9 C13 Fe2 68.8(8) . . ? C12 C13 Fe2 69.0(9) . . ? C15 C14 C18 109.0(13) . . ? C15 C14 P2 127.1(11) . . ? C18 C14 P2 123.8(13) . . ? C15 C14 Fe2 69.9(9) . . ? C18 C14 Fe2 71.4(8) . . ? P2 C14 Fe2 122.8(8) . . ? C14 C15 C16 109.6(14) . . ? C14 C15 Fe2 69.0(9) . . ? C16 C15 Fe2 73.1(10) . . ? C17 C16 C15 104.2(13) . . ? C17 C16 Fe2 69.4(10) . . ? C15 C16 Fe2 66.3(9) . . ? C16 C17 C18 114.1(14) . . ? C16 C17 Fe2 72.5(9) . . ? C18 C17 Fe2 69.0(8) . . ? C14 C18 C17 103.1(14) . . ? C14 C18 Fe2 67.7(8) . . ? C17 C18 Fe2 70.1(8) . . ? C6A C1A C2A 115.6(14) . . ? C6A C1A P1 121.1(12) . . ? C2A C1A P1 123.2(11) . . ? C3A C2A C1A 121.0(15) . . ? C2A C3A C4A 121.5(18) . . ? C5A C4A C3A 118.2(17) . . ? C4A C5A C6A 120.7(15) . . ? C1A C6A C5A 122.9(15) . . ? C6B C1B C2B 114.8(14) . . ? C6B C1B P1 124.1(13) . . ? C2B C1B P1 121.0(11) . . ? C3B C2B C1B 122.6(15) . . ? C2B C3B C4B 120.1(16) . . ? C3B C4B C5B 121.5(17) . . ? C4B C5B C6B 119.4(18) . . ? C5B C6B C1B 121.5(18) . . ? C6C C1C C2C 120.4(14) . . ? C6C C1C P2 120.4(11) . . ? C2C C1C P2 119.3(11) . . ? C3C C2C C1C 117.6(14) . . ? C2C C3C C4C 123.9(17) . . ? C5C C4C C3C 116.4(17) . . ? C6C C5C C4C 120.3(17) . . ? C5C C6C C1C 121.3(16) . . ? C6D C1D C2D 119.9(13) . . ? C6D C1D P2 119.1(11) . . ? C2D C1D P2 119.9(11) . . ? C3D C2D C1D 118.6(16) . . ? C4D C3D C2D 119.4(17) . . ? C3D C4D C5D 122.5(15) . . ? C6D C5D C4D 118.9(16) . . ? C5D C6D C1D 120.4(16) . . ? O3 S1 O4 114.2(12) . . ? O3 S1 O5 111.4(11) . . ? O4 S1 O5 119.5(16) . . ? O3 S1 C19 104.7(10) . . ? O4 S1 C19 104.9(12) . . ? O5 S1 C19 99.6(12) . . ? S1 O3 Ca1 140.1(9) . . ? F3 C19 F1 107(2) . . ? F3 C19 F2 114(2) . . ? F1 C19 F2 102.7(19) . . ? F3 C19 S1 112.1(17) . . ? F1 C19 S1 112.1(16) . . ? F2 C19 S1 108.9(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.338 _refine_diff_density_min -1.951 _refine_diff_density_rms 0.205 # Attachment 'complex5_new.cif' data_7519 _database_code_depnum_ccdc_archive 'CCDC 711713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H79 Cl9 F9 N2 Na O13 P4 Pt2 S3' _chemical_formula_weight 2567.87 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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' Na Na 0.0362 0.0249 '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 Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 49.267(4) _cell_length_b 11.0373(10) _cell_length_c 19.4584(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.375(2) _cell_angle_gamma 90.00 _cell_volume 10407.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3414 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.46 _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 3.117 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5216 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26480 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.1493 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.00 _reflns_number_total 15046 _reflns_number_gt 12229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Data quality was bad, probably a result of poor formation of the crystal. Anisotropic refinement led to poor thermal ellipsoids for the lighter atoms. In order to have reasonable results as well as good data to parameter ratio max 2-theta were capped at 48 degrees in final refinement cycles. All C atoms were kept isotropic and phenyl rings were treated as hexagons using AFIX 66. Restraints in bond length and thermal parameters were applied to the otf and chloroform. Twin refinement was done assuming a model of racemic twins. ; _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^)+(0.0652P)^2^+134.2917P] 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 0.000(18) _refine_ls_number_reflns 15046 _refine_ls_number_parameters 555 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.008 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 0.227248(16) 0.41872(6) 0.29224(3) 0.0233(2) Uani 1 1 d . . . Pt2 Pt 0.403978(16) 0.51598(5) 0.30747(3) 0.01738(18) Uani 1 1 d . . . Na1 Na 0.32211(15) 0.4824(7) 0.4171(4) 0.0314(18) Uani 1 1 d . . . P1 P 0.20189(11) 0.2873(5) 0.3443(3) 0.0292(12) Uani 1 1 d . . . P2 P 0.19866(11) 0.5787(5) 0.2910(3) 0.0314(13) Uani 1 1 d . . . P3 P 0.43102(10) 0.3515(5) 0.3138(3) 0.0203(11) Uani 1 1 d . . . P4 P 0.43875(10) 0.6464(4) 0.3501(2) 0.0200(11) Uani 1 1 d . . . N1 N 0.2536(3) 0.5151(13) 0.2427(8) 0.026(4) Uani 1 1 d . . . N2 N 0.3693(3) 0.4155(13) 0.2640(8) 0.023(4) Uani 1 1 d . . . O1 O 0.2537(3) 0.2706(12) 0.2873(7) 0.033(4) Uani 1 1 d . . . O2 O 0.2896(3) 0.3574(12) 0.3544(6) 0.028(3) Uani 1 1 d . . . O3 O 0.3784(3) 0.6666(12) 0.2935(7) 0.028(3) Uani 1 1 d . . . O4 O 0.3453(3) 0.5926(11) 0.3494(7) 0.034(3) Uani 1 1 d . . . C1 C 0.2712(4) 0.6027(17) 0.2740(10) 0.022(4) Uiso 1 1 d . . . H1 H 0.2701 0.6236 0.3202 0.027 Uiso 1 1 calc R . . C2 C 0.2898(4) 0.6609(18) 0.2449(10) 0.025(5) Uiso 1 1 d . . . C3 C 0.2912(5) 0.633(2) 0.1756(11) 0.044(6) Uiso 1 1 d . . . H3 H 0.3027 0.6786 0.1519 0.052 Uiso 1 1 calc R . . C4 C 0.2761(4) 0.5420(17) 0.1423(10) 0.025(5) Uiso 1 1 d . . . H4 H 0.2783 0.5189 0.0971 0.030 Uiso 1 1 calc R . . C5 C 0.2569(4) 0.482(2) 0.1759(10) 0.036(5) Uiso 1 1 d . . . H5 H 0.2462 0.4182 0.1528 0.043 Uiso 1 1 calc R . . C6 C 0.3063(4) 0.7631(18) 0.2838(10) 0.029(5) Uiso 1 1 d . . . H6A H 0.3055 0.7549 0.3335 0.035 Uiso 1 1 calc R . . H6B H 0.2973 0.8397 0.2677 0.035 Uiso 1 1 calc R . . C7 C 0.3365(4) 0.7715(18) 0.2765(10) 0.029(5) Uiso 1 1 d . . . H7A H 0.3444 0.8465 0.2986 0.035 Uiso 1 1 calc R . . H7B H 0.3377 0.7753 0.2268 0.035 Uiso 1 1 calc R . . C8 C 0.3540(4) 0.6612(19) 0.3107(10) 0.030(5) Uiso 1 1 d . . . C9 C 0.3575(4) 0.3339(17) 0.2999(9) 0.022(4) Uiso 1 1 d . . . H9 H 0.3656 0.3212 0.3468 0.026 Uiso 1 1 calc R . . C10 C 0.3350(4) 0.2688(16) 0.2744(9) 0.018(4) Uiso 1 1 d . . . C11 C 0.3236(4) 0.2890(17) 0.2055(9) 0.028(5) Uiso 1 1 d . . . H11 H 0.3085 0.2414 0.1844 0.033 Uiso 1 1 calc R . . C12 C 0.3339(4) 0.3796(18) 0.1654(11) 0.034(5) Uiso 1 1 d . . . H12 H 0.3254 0.3986 0.1195 0.041 Uiso 1 1 calc R . . C13 C 0.3584(4) 0.4401(19) 0.1999(10) 0.032(5) Uiso 1 1 d . . . H13 H 0.3668 0.4987 0.1755 0.038 Uiso 1 1 calc R . . C14 C 0.3241(4) 0.171(2) 0.3215(11) 0.036(5) Uiso 1 1 d . . . H14A H 0.3326 0.0926 0.3141 0.043 Uiso 1 1 calc R . . H14B H 0.3301 0.1930 0.3706 0.043 Uiso 1 1 calc R . . C15 C 0.2937(4) 0.1567(19) 0.3071(11) 0.033(5) Uiso 1 1 d . . . H15A H 0.2883 0.0958 0.3387 0.040 Uiso 1 1 calc R . . H15B H 0.2877 0.1281 0.2591 0.040 Uiso 1 1 calc R . . C16 C 0.2793(4) 0.2772(18) 0.3170(10) 0.025(5) Uiso 1 1 d . . . C17 C 0.3233(8) 0.818(3) 0.498(2) 0.086(10) Uiso 1 1 d . . . C18 C 0.3549(6) 0.182(3) 0.5417(14) 0.054(7) Uiso 1 1 d . . . C19 C 0.0618(7) 0.319(3) 0.8860(10) 0.123(15) Uiso 1 1 d D . . C1A C 0.22584(6) 0.2086(3) 0.4124(2) 0.037(5) Uiso 1 1 d G . . C2A C 0.22081(7) 0.0884(3) 0.4274(2) 0.046(6) Uiso 1 1 d G . . H2A H 0.2053 0.0482 0.4023 0.056 Uiso 1 1 calc R . . C3A C 0.23868(7) 0.0277(3) 0.4795(2) 0.069(8) Uiso 1 1 d G . . H3A H 0.2353 -0.0535 0.4897 0.083 Uiso 1 1 calc R . . C4A C 0.26158(7) 0.0872(4) 0.5167(2) 0.061(7) Uiso 1 1 d G . . H4A H 0.2737 0.0461 0.5519 0.073 Uiso 1 1 calc R . . C5A C 0.26661(7) 0.2073(3) 0.50164(18) 0.085(10) Uiso 1 1 d G . . H5A H 0.2821 0.2475 0.5268 0.102 Uiso 1 1 calc R . . C6A C 0.24874(6) 0.2681(3) 0.44949(18) 0.036(5) Uiso 1 1 d G . . H6A1 H 0.2521 0.3493 0.4393 0.043 Uiso 1 1 calc R . . C1B C 0.18575(6) 0.1749(3) 0.2813(2) 0.033(5) Uiso 1 1 d G . . C2B C 0.16484(6) 0.1007(4) 0.2966(2) 0.059(7) Uiso 1 1 d G . . H2B H 0.1594 0.1061 0.3404 0.071 Uiso 1 1 calc R . . C3B C 0.15198(7) 0.0184(4) 0.2471(3) 0.064(7) Uiso 1 1 d G . . H3B H 0.1378 -0.0318 0.2575 0.077 Uiso 1 1 calc R . . C4B C 0.16002(7) 0.0104(4) 0.1824(3) 0.054(6) Uiso 1 1 d G . . H4B H 0.1513 -0.0452 0.1489 0.064 Uiso 1 1 calc R . . C5B C 0.18093(6) 0.0847(4) 0.1671(2) 0.032(5) Uiso 1 1 d G . . H5B H 0.1864 0.0793 0.1233 0.038 Uiso 1 1 calc R . . C6B C 0.19380(6) 0.1669(3) 0.2165(2) 0.036(5) Uiso 1 1 d G . . H6B1 H 0.2079 0.2171 0.2062 0.043 Uiso 1 1 calc R . . C1C C 0.17407(6) 0.3386(4) 0.3882(2) 0.036(5) Uiso 1 1 d G . . C2C C 0.17946(6) 0.3549(4) 0.4602(2) 0.042(6) Uiso 1 1 d G . . H2C H 0.1974 0.3422 0.4855 0.051 Uiso 1 1 calc R . . C3C C 0.15838(7) 0.3900(4) 0.4947(2) 0.070(8) Uiso 1 1 d G . . H3C H 0.1620 0.4011 0.5434 0.084 Uiso 1 1 calc R . . C4C C 0.13192(6) 0.4088(4) 0.4573(2) 0.063(7) Uiso 1 1 d G . . H4C H 0.1177 0.4325 0.4806 0.076 Uiso 1 1 calc R . . C5C C 0.12653(6) 0.3924(4) 0.3853(2) 0.043(6) Uiso 1 1 d G . . H5C H 0.1086 0.4051 0.3599 0.052 Uiso 1 1 calc R . . C6C C 0.14760(6) 0.3573(4) 0.3507(2) 0.034(5) Uiso 1 1 d G . . H6C H 0.1440 0.3463 0.3020 0.041 Uiso 1 1 calc R . . C1D C 0.16655(6) 0.5637(4) 0.2319(2) 0.032(5) Uiso 1 1 d G . . C2D C 0.14778(6) 0.6589(4) 0.2252(2) 0.048(6) Uiso 1 1 d G . . H2D H 0.1519 0.7294 0.2521 0.058 Uiso 1 1 calc R . . C3D C 0.12289(6) 0.6496(4) 0.1788(2) 0.067(8) Uiso 1 1 d G . . H3D H 0.1102 0.7140 0.1743 0.080 Uiso 1 1 calc R . . C4D C 0.11677(6) 0.5453(5) 0.1390(2) 0.061(7) Uiso 1 1 d G . . H4D H 0.0999 0.5391 0.1076 0.073 Uiso 1 1 calc R . . C5D C 0.13555(6) 0.4501(4) 0.1457(2) 0.055(7) Uiso 1 1 d G . . H5D H 0.1314 0.3796 0.1188 0.066 Uiso 1 1 calc R . . C6D C 0.16044(6) 0.4594(4) 0.1922(2) 0.038(5) Uiso 1 1 d G . . H6D H 0.1731 0.3950 0.1967 0.045 Uiso 1 1 calc R . . C1E C 0.21328(6) 0.7133(3) 0.2564(2) 0.020(4) Uiso 1 1 d G . . C2E C 0.22491(6) 0.8085(3) 0.2983(2) 0.060(7) Uiso 1 1 d G . . H2E H 0.2252 0.8064 0.3468 0.072 Uiso 1 1 calc R . . C3E C 0.23610(7) 0.9070(3) 0.2687(2) 0.041(6) Uiso 1 1 d G . . H3E H 0.2440 0.9714 0.2971 0.049 Uiso 1 1 calc R . . C4E C 0.23568(7) 0.9102(3) 0.1971(2) 0.047(6) Uiso 1 1 d G . . H4E H 0.2432 0.9768 0.1771 0.056 Uiso 1 1 calc R . . C5E C 0.22405(6) 0.8150(4) 0.1551(2) 0.044(6) Uiso 1 1 d G . . H5E H 0.2238 0.8171 0.1067 0.053 Uiso 1 1 calc R . . C6E C 0.21286(6) 0.7165(3) 0.1848(2) 0.038(5) Uiso 1 1 d G . . H6E H 0.2050 0.6521 0.1564 0.046 Uiso 1 1 calc R . . C1F C 0.19407(6) 0.6228(3) 0.3778(2) 0.027(4) Uiso 1 1 d G . . C2F C 0.16855(6) 0.6527(4) 0.3940(2) 0.041(6) Uiso 1 1 d G . . H2F H 0.1526 0.6496 0.3593 0.049 Uiso 1 1 calc R . . C3F C 0.16660(7) 0.6871(4) 0.4617(2) 0.060(7) Uiso 1 1 d G . . H3F H 0.1493 0.7073 0.4727 0.072 Uiso 1 1 calc R . . C4F C 0.19016(7) 0.6916(4) 0.5131(2) 0.064(8) Uiso 1 1 d G . . H4F H 0.1888 0.7149 0.5588 0.077 Uiso 1 1 calc R . . C5F C 0.21568(7) 0.6618(4) 0.4968(2) 0.059(7) Uiso 1 1 d G . . H5F H 0.2316 0.6649 0.5316 0.070 Uiso 1 1 calc R . . C6F C 0.21763(6) 0.6274(3) 0.42915(19) 0.031(5) Uiso 1 1 d G . . H6F H 0.2349 0.6072 0.4182 0.037 Uiso 1 1 calc R . . C1G C 0.41126(6) 0.2136(3) 0.28547(19) 0.029(5) Uiso 1 1 d G . . C2G C 0.40855(6) 0.1207(3) 0.3320(2) 0.029(5) Uiso 1 1 d G . . H2G H 0.4169 0.1278 0.3792 0.035 Uiso 1 1 calc R . . C3G C 0.39356(7) 0.0174(3) 0.3086(2) 0.043(6) Uiso 1 1 d G . . H3G H 0.3917 -0.0454 0.3401 0.052 Uiso 1 1 calc R . . C4G C 0.38126(7) 0.0070(3) 0.2388(2) 0.049(6) Uiso 1 1 d G . . H4G H 0.3711 -0.0629 0.2230 0.058 Uiso 1 1 calc R . . C5G C 0.38397(7) 0.0999(3) 0.1922(2) 0.034(5) Uiso 1 1 d G . . H5G H 0.3757 0.0929 0.1450 0.040 Uiso 1 1 calc R . . C6G C 0.39896(6) 0.2032(3) 0.21560(19) 0.032(5) Uiso 1 1 d G . . H6G H 0.4008 0.2661 0.1841 0.038 Uiso 1 1 calc R . . C1H C 0.44797(6) 0.3189(3) 0.40125(19) 0.021(4) Uiso 1 1 d G . . C2H C 0.47493(6) 0.2770(3) 0.4190(2) 0.035(5) Uiso 1 1 d G . . H2H H 0.4858 0.2682 0.3844 0.041 Uiso 1 1 calc R . . C3H C 0.48576(6) 0.2482(4) 0.4881(2) 0.044(6) Uiso 1 1 d G . . H3H H 0.5040 0.2199 0.5001 0.053 Uiso 1 1 calc R . . C4H C 0.46964(6) 0.2613(4) 0.5393(2) 0.042(6) Uiso 1 1 d G . . H4H H 0.4770 0.2418 0.5860 0.050 Uiso 1 1 calc R . . C5H C 0.44268(6) 0.3032(4) 0.52154(18) 0.033(5) Uiso 1 1 d G . . H5H H 0.4318 0.3120 0.5562 0.040 Uiso 1 1 calc R . . C6H C 0.43184(6) 0.3320(3) 0.45251(17) 0.034(5) Uiso 1 1 d G . . H6H H 0.4136 0.3603 0.4405 0.040 Uiso 1 1 calc R . . C1I C 0.45451(6) 0.3500(3) 0.25129(19) 0.022(4) Uiso 1 1 d G . . C2I C 0.47246(6) 0.2533(4) 0.2496(2) 0.035(5) Uiso 1 1 d G . . H2I H 0.4733 0.1905 0.2825 0.041 Uiso 1 1 calc R . . C3I C 0.48916(7) 0.2495(4) 0.1992(2) 0.053(6) Uiso 1 1 d G . . H3I H 0.5013 0.1841 0.1980 0.064 Uiso 1 1 calc R . . C4I C 0.48792(7) 0.3423(4) 0.1505(2) 0.051(6) Uiso 1 1 d G . . H4I H 0.4992 0.3398 0.1164 0.061 Uiso 1 1 calc R . . C5I C 0.46998(7) 0.4390(4) 0.1522(2) 0.049(6) Uiso 1 1 d G . . H5I H 0.4691 0.5019 0.1192 0.059 Uiso 1 1 calc R . . C6I C 0.45328(6) 0.4429(4) 0.20258(19) 0.032(5) Uiso 1 1 d G . . H6I H 0.4411 0.5083 0.2037 0.039 Uiso 1 1 calc R . . C1K C 0.47331(6) 0.5912(3) 0.38921(19) 0.025(4) Uiso 1 1 d G . . C2K C 0.49170(6) 0.5671(3) 0.3445(2) 0.028(5) Uiso 1 1 d G . . H2K H 0.4862 0.5786 0.2961 0.034 Uiso 1 1 calc R . . C3K C 0.51816(6) 0.5261(4) 0.3713(2) 0.038(5) Uiso 1 1 d G . . H3K H 0.5306 0.5098 0.3411 0.046 Uiso 1 1 calc R . . C4K C 0.52624(6) 0.5091(4) 0.4429(2) 0.039(5) Uiso 1 1 d G . . H4K H 0.5441 0.4813 0.4610 0.046 Uiso 1 1 calc R . . C5K C 0.50785(6) 0.5332(4) 0.4876(2) 0.039(5) Uiso 1 1 d G . . H5K H 0.5133 0.5217 0.5360 0.047 Uiso 1 1 calc R . . C6K C 0.48139(6) 0.5742(4) 0.46075(19) 0.038(5) Uiso 1 1 d G . . H6K H 0.4690 0.5905 0.4910 0.045 Uiso 1 1 calc R . . C1L C 0.44558(6) 0.7550(3) 0.2852(2) 0.018(4) Uiso 1 1 d G . . C2L C 0.46918(6) 0.8264(3) 0.2989(2) 0.030(5) Uiso 1 1 d G . . H2L H 0.4818 0.8165 0.3409 0.036 Uiso 1 1 calc R . . C3L C 0.47416(7) 0.9123(4) 0.2504(3) 0.045(6) Uiso 1 1 d G . . H3L H 0.4901 0.9605 0.2597 0.054 Uiso 1 1 calc R . . C4L C 0.45553(7) 0.9268(4) 0.1882(3) 0.042(6) Uiso 1 1 d G . . H4L H 0.4589 0.9849 0.1555 0.050 Uiso 1 1 calc R . . C5L C 0.43192(7) 0.8555(4) 0.1745(2) 0.029(5) Uiso 1 1 d G . . H5L H 0.4193 0.8653 0.1325 0.035 Uiso 1 1 calc R . . C6L C 0.42694(6) 0.7696(3) 0.2230(2) 0.028(5) Uiso 1 1 d G . . H6L H 0.4110 0.7214 0.2138 0.033 Uiso 1 1 calc R . . C1M C 0.42798(6) 0.7304(3) 0.42301(19) 0.031(5) Uiso 1 1 d G . . C2M C 0.43745(6) 0.8478(3) 0.4381(2) 0.029(5) Uiso 1 1 d G . . H2M H 0.4482 0.8864 0.4092 0.035 Uiso 1 1 calc R . . C3M C 0.43105(7) 0.9080(3) 0.4958(2) 0.042(6) Uiso 1 1 d G . . H3M H 0.4375 0.9874 0.5060 0.051 Uiso 1 1 calc R . . C4M C 0.41517(7) 0.8510(4) 0.5385(2) 0.058(7) Uiso 1 1 d G . . H4M H 0.4108 0.8917 0.5775 0.070 Uiso 1 1 calc R . . C5M C 0.40569(6) 0.7336(3) 0.52341(18) 0.065(8) Uiso 1 1 d G . . H5M H 0.3950 0.6950 0.5523 0.078 Uiso 1 1 calc R . . C6M C 0.41209(6) 0.6734(3) 0.46568(17) 0.045(6) Uiso 1 1 d G . . H6M H 0.4057 0.5940 0.4555 0.053 Uiso 1 1 calc R . . Cl7 Cl 0.0010(2) 0.4083(12) 0.5204(9) 0.165(6) Uani 1 1 d D . . Cl8 Cl 0.0359(5) 0.5056(17) 0.6445(11) 0.269(12) Uani 1 1 d D . . Cl9 Cl 0.0496(2) 0.2886(10) 0.5835(8) 0.143(5) Uani 1 1 d D . . F1 F 0.3328(4) 0.851(2) 0.4457(9) 0.109(7) Uani 1 1 d U . . F2 F 0.3431(4) 0.752(3) 0.5335(12) 0.143(10) Uani 1 1 d U . . F3 F 0.3253(6) 0.900(2) 0.5443(11) 0.149(10) Uani 1 1 d U . . F4 F 0.3338(4) 0.1531(15) 0.4945(9) 0.085(5) Uani 1 1 d U . . F5 F 0.3750(5) 0.1239(17) 0.5255(11) 0.116(8) Uani 1 1 d U . . F6 F 0.3524(5) 0.1464(17) 0.5998(8) 0.119(8) Uani 1 1 d U . . F7 F 0.0760(8) 0.379(3) 0.8466(17) 0.24(2) Uani 1 1 d D . . F8 F 0.0367(6) 0.363(3) 0.8748(13) 0.159(11) Uani 1 1 d D . . F9 F 0.0582(7) 0.209(2) 0.8602(11) 0.185(15) Uani 1 1 d D . . O5 O 0.2739(4) 0.809(2) 0.4360(9) 0.089(7) Uani 1 1 d . . . O6 O 0.2972(5) 0.6230(16) 0.4569(15) 0.109(9) Uani 1 1 d . . . O7 O 0.2833(4) 0.737(2) 0.5486(9) 0.087(8) Uani 1 1 d . . . O8 O 0.3344(4) 0.3946(17) 0.5538(11) 0.074(6) Uani 1 1 d . . . O9 O 0.3632(3) 0.3697(15) 0.4698(8) 0.051(4) Uani 1 1 d . . . O10 O 0.3834(3) 0.3753(18) 0.5887(8) 0.064(6) Uani 1 1 d . . . O11 O 0.0784(5) 0.4372(16) 0.9966(13) 0.110(9) Uani 1 1 d DU . . O12 O 0.1017(4) 0.258(2) 0.9816(19) 0.148(11) Uani 1 1 d DU . . O13 O 0.0555(5) 0.252(3) 1.0072(15) 0.149(11) Uani 1 1 d DU . . S1 S 0.29090(12) 0.7390(5) 0.4841(3) 0.0390(14) Uani 1 1 d . . . S2 S 0.35940(12) 0.3472(5) 0.5395(3) 0.0373(14) Uani 1 1 d . . . S3 S 0.07567(18) 0.3123(8) 0.9779(5) 0.081(3) Uani 1 1 d D . . C1S C 0.1155(4) 0.014(2) 0.4694(9) 0.073(9) Uiso 1 1 d D . . H1S H 0.1105 -0.0712 0.4780 0.088 Uiso 1 1 calc R . . C2S C 0.0595(4) 0.158(2) 0.1553(15) 0.137(16) Uiso 1 1 d D . . H2S H 0.0572 0.1816 0.1055 0.164 Uiso 1 1 calc R . . C3S C 0.0355(5) 0.433(2) 0.5614(13) 0.137(16) Uiso 1 1 d D . . H3S H 0.0461 0.4790 0.5314 0.165 Uiso 1 1 calc R . . Cl1 Cl 0.1005(2) 0.0600(11) 0.3830(5) 0.126(4) Uani 1 1 d D . . Cl2 Cl 0.1024(3) 0.1156(14) 0.5272(8) 0.163(6) Uani 1 1 d D . . Cl3 Cl 0.15166(18) 0.0323(10) 0.4850(5) 0.103(3) Uani 1 1 d D . . Cl4 Cl 0.0302(3) 0.179(2) 0.1943(10) 0.234(10) Uani 1 1 d D . . Cl5 Cl 0.0879(3) 0.2214(14) 0.2101(9) 0.191(8) Uani 1 1 d D . . Cl6 Cl 0.0651(7) -0.0023(18) 0.1730(14) 0.314(14) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0157(4) 0.0237(5) 0.0301(4) -0.0017(4) 0.0031(3) -0.0012(4) Pt2 0.0183(4) 0.0127(4) 0.0210(3) 0.0005(4) 0.0032(3) -0.0004(4) Na1 0.026(4) 0.030(4) 0.037(4) 0.001(4) 0.002(3) -0.002(4) P1 0.026(3) 0.017(3) 0.045(3) 0.000(2) 0.004(3) 0.004(2) P2 0.023(3) 0.023(3) 0.046(3) -0.006(3) 0.000(3) -0.002(3) P3 0.020(3) 0.016(3) 0.025(3) 0.004(2) 0.005(2) 0.001(2) P4 0.021(3) 0.018(3) 0.018(2) 0.001(2) -0.003(2) 0.001(2) N1 0.032(10) 0.015(8) 0.026(8) -0.004(7) -0.007(7) 0.002(7) N2 0.019(8) 0.009(8) 0.034(9) -0.002(7) -0.011(7) -0.001(7) O1 0.046(10) 0.017(7) 0.041(8) 0.004(7) 0.022(7) 0.003(7) O2 0.033(8) 0.028(8) 0.021(7) -0.004(6) 0.004(6) -0.001(6) O3 0.018(8) 0.017(7) 0.048(9) -0.019(7) 0.007(7) -0.002(6) O4 0.046(9) 0.007(7) 0.052(9) 0.010(7) 0.022(7) 0.002(6) Cl7 0.065(6) 0.141(11) 0.265(16) 0.063(11) -0.032(9) -0.009(7) Cl8 0.40(3) 0.191(17) 0.26(2) -0.107(15) 0.18(2) -0.176(19) Cl9 0.072(6) 0.081(7) 0.263(15) 0.012(9) -0.003(8) 0.004(5) F1 0.111(14) 0.139(17) 0.067(10) 0.010(11) -0.008(10) -0.067(13) F2 0.059(12) 0.24(3) 0.119(15) 0.079(17) -0.005(12) -0.041(15) F3 0.22(3) 0.14(2) 0.091(13) -0.071(14) 0.037(15) -0.093(19) F4 0.096(12) 0.067(11) 0.096(12) -0.002(10) 0.028(10) -0.020(10) F5 0.137(17) 0.073(12) 0.122(15) -0.023(11) -0.016(13) 0.052(12) F6 0.22(2) 0.085(13) 0.043(9) 0.029(9) 0.005(12) -0.015(14) F7 0.28(4) 0.28(4) 0.20(3) -0.09(3) 0.09(3) -0.22(4) F8 0.17(3) 0.16(2) 0.122(18) 0.003(18) -0.035(18) -0.05(2) F9 0.32(4) 0.13(2) 0.100(16) -0.042(15) 0.03(2) -0.16(3) O5 0.059(12) 0.15(2) 0.046(10) 0.024(12) -0.020(10) 0.019(13) O6 0.113(18) 0.034(11) 0.21(3) -0.044(14) 0.108(19) -0.031(11) O7 0.064(14) 0.14(2) 0.043(11) -0.022(12) -0.023(10) 0.028(14) O8 0.048(11) 0.074(14) 0.105(15) 0.026(12) 0.025(11) 0.016(10) O9 0.039(9) 0.051(10) 0.059(10) -0.008(9) -0.002(8) 0.001(8) O10 0.045(10) 0.095(15) 0.044(9) -0.015(10) -0.014(8) 0.032(10) O11 0.115(19) 0.093(17) 0.119(18) -0.051(15) 0.017(15) -0.025(14) O12 0.072(15) 0.13(2) 0.26(3) -0.07(2) 0.063(18) -0.011(15) O13 0.12(2) 0.19(2) 0.14(2) 0.002(19) 0.029(17) -0.07(2) S1 0.045(4) 0.029(3) 0.041(3) -0.004(3) 0.002(3) 0.006(3) S2 0.037(3) 0.047(4) 0.027(3) 0.001(3) 0.004(2) 0.011(3) S3 0.062(5) 0.067(5) 0.116(7) -0.020(5) 0.024(5) -0.025(4) Cl1 0.109(8) 0.166(11) 0.110(7) 0.045(7) 0.035(6) -0.012(8) Cl2 0.110(9) 0.178(13) 0.207(14) -0.056(11) 0.043(10) 0.024(9) Cl3 0.075(6) 0.150(9) 0.088(6) 0.035(6) 0.022(5) 0.006(6) Cl4 0.125(11) 0.33(2) 0.267(19) 0.148(19) 0.080(13) 0.037(14) Cl5 0.120(10) 0.163(13) 0.253(17) 0.046(12) -0.067(11) -0.067(9) Cl6 0.45(4) 0.176(19) 0.31(3) -0.075(19) 0.04(3) -0.08(2) _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 N1 2.049(16) . ? Pt1 O1 2.104(14) . ? Pt1 P2 2.256(6) . ? Pt1 P1 2.269(6) . ? Pt2 O3 2.075(13) . ? Pt2 N2 2.086(14) . ? Pt2 P3 2.242(5) . ? Pt2 P4 2.277(5) . ? Na1 O6 2.20(2) . ? Na1 O4 2.251(15) . ? Na1 O2 2.291(15) . ? Na1 O9 2.438(17) . ? Na1 O8 2.79(2) . ? Na1 S2 3.114(9) . ? P1 C1B 1.823(6) . ? P1 C1A 1.827(6) . ? P1 C1C 1.829(6) . ? P2 C1D 1.788(6) . ? P2 C1F 1.809(7) . ? P2 C1E 1.832(7) . ? P3 C1H 1.792(6) . ? P3 C1I 1.823(6) . ? P3 C1G 1.837(6) . ? P4 C1L 1.816(6) . ? P4 C1K 1.840(6) . ? P4 C1M 1.851(6) . ? N1 C1 1.37(2) . ? N1 C5 1.39(3) . ? N2 C13 1.29(2) . ? N2 C9 1.34(2) . ? O1 C16 1.29(2) . ? O2 C16 1.20(2) . ? O3 C8 1.31(2) . ? O4 C8 1.20(2) . ? C1 C2 1.33(3) . ? C2 C3 1.39(3) . ? C2 C6 1.51(3) . ? C3 C4 1.34(3) . ? C4 C5 1.41(3) . ? C6 C7 1.52(3) . ? C7 C8 1.57(3) . ? C9 C10 1.34(2) . ? C10 C11 1.38(2) . ? C10 C14 1.57(3) . ? C11 C12 1.42(3) . ? C12 C13 1.44(3) . ? C14 C15 1.48(3) . ? C15 C16 1.54(3) . ? C17 F1 1.25(4) . ? C17 F3 1.26(4) . ? C17 F2 1.30(4) . ? C17 S1 1.80(4) . ? C18 F6 1.23(3) . ? C18 F5 1.27(3) . ? C18 F4 1.30(3) . ? C18 S2 1.84(3) . ? C19 F8 1.306(18) . ? C19 F7 1.307(18) . ? C19 F9 1.312(19) . ? C19 S3 1.798(18) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C1B C2B 1.3899 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C3B C4B 1.3900 . ? C4B C5B 1.3899 . ? C5B C6B 1.3900 . ? C1C C2C 1.3900 . ? C1C C6C 1.3901 . ? C2C C3C 1.3901 . ? C3C C4C 1.3900 . ? C4C C5C 1.3900 . ? C5C C6C 1.3899 . ? C1D C6D 1.3900 . ? C1D C2D 1.3900 . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C2E C3E 1.3900 . ? C3E C4E 1.3900 . ? C4E C5E 1.3900 . ? C5E C6E 1.3900 . ? C1F C6F 1.3900 . ? C1F C2F 1.3901 . ? C2F C3F 1.3900 . ? C3F C4F 1.3899 . ? C4F C5F 1.3901 . ? C5F C6F 1.3900 . ? C1G C2G 1.3900 . ? C1G C6G 1.3900 . ? C2G C3G 1.3900 . ? C3G C4G 1.3900 . ? C4G C5G 1.3900 . ? C5G C6G 1.3900 . ? C1H C2H 1.3900 . ? C1H C6H 1.3900 . ? C2H C3H 1.3900 . ? C3H C4H 1.3900 . ? C4H C5H 1.3900 . ? C5H C6H 1.3899 . ? C1I C6I 1.3900 . ? C1I C2I 1.3900 . ? C2I C3I 1.3900 . ? C3I C4I 1.3900 . ? C4I C5I 1.3900 . ? C5I C6I 1.3899 . ? C1K C2K 1.3900 . ? C1K C6K 1.3900 . ? C2K C3K 1.3900 . ? C3K C4K 1.3900 . ? C4K C5K 1.3900 . ? C5K C6K 1.3901 . ? C1L C2L 1.3900 . ? C1L C6L 1.3901 . ? C2L C3L 1.3900 . ? C3L C4L 1.3900 . ? C4L C5L 1.3900 . ? C5L C6L 1.3900 . ? C1M C2M 1.3900 . ? C1M C6M 1.3901 . ? C2M C3M 1.3900 . ? C3M C4M 1.3901 . ? C4M C5M 1.3900 . ? C5M C6M 1.3899 . ? Cl7 C3S 1.762(19) . ? Cl8 C3S 1.803(19) . ? Cl9 C3S 1.762(19) . ? O5 S1 1.376(18) . ? O6 S1 1.440(18) . ? O7 S1 1.37(2) . ? O8 S2 1.414(19) . ? O9 S2 1.423(17) . ? O10 S2 1.415(16) . ? O11 S3 1.425(15) . ? O12 S3 1.407(16) . ? O13 S3 1.398(16) . ? C1S Cl3 1.764(17) . ? C1S Cl1 1.784(17) . ? C1S Cl2 1.793(17) . ? C2S Cl5 1.746(18) . ? C2S Cl4 1.762(19) . ? C2S Cl6 1.813(19) . ? 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 N1 Pt1 O1 86.1(6) . . ? N1 Pt1 P2 92.1(4) . . ? O1 Pt1 P2 176.8(4) . . ? N1 Pt1 P1 171.4(4) . . ? O1 Pt1 P1 85.4(4) . . ? P2 Pt1 P1 96.4(2) . . ? O3 Pt2 N2 86.5(5) . . ? O3 Pt2 P3 175.7(4) . . ? N2 Pt2 P3 91.6(4) . . ? O3 Pt2 P4 86.6(4) . . ? N2 Pt2 P4 172.9(4) . . ? P3 Pt2 P4 95.25(18) . . ? O6 Na1 O4 101.5(7) . . ? O6 Na1 O2 103.4(8) . . ? O4 Na1 O2 113.2(6) . . ? O6 Na1 O9 133.1(9) . . ? O4 Na1 O9 92.9(6) . . ? O2 Na1 O9 111.3(6) . . ? O6 Na1 O8 87.0(9) . . ? O4 Na1 O8 134.4(6) . . ? O2 Na1 O8 108.0(6) . . ? O9 Na1 O8 53.3(6) . . ? O6 Na1 S2 110.9(8) . . ? O4 Na1 S2 114.5(5) . . ? O2 Na1 S2 112.2(4) . . ? O9 Na1 S2 26.3(4) . . ? O8 Na1 S2 27.0(4) . . ? C1B P1 C1A 108.1(3) . . ? C1B P1 C1C 104.6(3) . . ? C1A P1 C1C 104.5(3) . . ? C1B P1 Pt1 110.0(3) . . ? C1A P1 Pt1 107.0(3) . . ? C1C P1 Pt1 122.0(3) . . ? C1D P2 C1F 112.3(3) . . ? C1D P2 C1E 101.5(3) . . ? C1F P2 C1E 104.4(3) . . ? C1D P2 Pt1 114.4(3) . . ? C1F P2 Pt1 112.6(3) . . ? C1E P2 Pt1 110.6(3) . . ? C1H P3 C1I 112.9(3) . . ? C1H P3 C1G 104.4(3) . . ? C1I P3 C1G 99.1(3) . . ? C1H P3 Pt2 112.6(3) . . ? C1I P3 Pt2 114.4(3) . . ? C1G P3 Pt2 112.1(3) . . ? C1L P4 C1K 103.5(3) . . ? C1L P4 C1M 108.5(3) . . ? C1K P4 C1M 102.8(3) . . ? C1L P4 Pt2 112.7(2) . . ? C1K P4 Pt2 121.4(3) . . ? C1M P4 Pt2 107.2(2) . . ? C1 N1 C5 115.7(17) . . ? C1 N1 Pt1 124.2(12) . . ? C5 N1 Pt1 119.5(13) . . ? C13 N2 C9 120.2(16) . . ? C13 N2 Pt2 116.4(13) . . ? C9 N2 Pt2 123.3(12) . . ? C16 O1 Pt1 119.9(13) . . ? C16 O2 Na1 161.4(13) . . ? C8 O3 Pt2 119.7(13) . . ? C8 O4 Na1 169.8(15) . . ? C2 C1 N1 125.7(17) . . ? C1 C2 C3 117.6(19) . . ? C1 C2 C6 119.8(17) . . ? C3 C2 C6 122.3(19) . . ? C4 C3 C2 121(2) . . ? C3 C4 C5 119.2(19) . . ? N1 C5 C4 120.6(19) . . ? C2 C6 C7 116.4(17) . . ? C6 C7 C8 112.6(16) . . ? O4 C8 O3 130(2) . . ? O4 C8 C7 121.8(19) . . ? O3 C8 C7 108.4(17) . . ? N2 C9 C10 125.3(17) . . ? C9 C10 C11 116.0(17) . . ? C9 C10 C14 120.0(16) . . ? C11 C10 C14 123.9(16) . . ? C10 C11 C12 121.8(18) . . ? C11 C12 C13 115.3(18) . . ? N2 C13 C12 121.2(19) . . ? C15 C14 C10 113.6(17) . . ? C14 C15 C16 111.1(18) . . ? O2 C16 O1 126.0(19) . . ? O2 C16 C15 124.0(18) . . ? O1 C16 C15 109.3(17) . . ? F1 C17 F3 112(3) . . ? F1 C17 F2 104(3) . . ? F3 C17 F2 94(3) . . ? F1 C17 S1 118(3) . . ? F3 C17 S1 114(3) . . ? F2 C17 S1 112(3) . . ? F6 C18 F5 106(3) . . ? F6 C18 F4 112(3) . . ? F5 C18 F4 105(2) . . ? F6 C18 S2 112(2) . . ? F5 C18 S2 113(2) . . ? F4 C18 S2 108.2(19) . . ? F8 C19 F7 108(3) . . ? F8 C19 F9 103(3) . . ? F7 C19 F9 107(3) . . ? F8 C19 S3 111.2(19) . . ? F7 C19 S3 117(3) . . ? F9 C19 S3 110.1(19) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 119.32(19) . . ? C6A C1A P1 120.67(19) . . ? C1A C2A C3A 120.0 . . ? C2A C3A C4A 120.0 . . ? C5A C4A C3A 120.0 . . ? C4A C5A C6A 120.0 . . ? C5A C6A C1A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 120.5(2) . . ? C6B C1B P1 119.5(2) . . ? C1B C2B C3B 120.0 . . ? C2B C3B C4B 120.0 . . ? C5B C4B C3B 120.0 . . ? C4B C5B C6B 120.0 . . ? C5B C6B C1B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C P1 119.1(2) . . ? C6C C1C P1 120.8(2) . . ? C1C C2C C3C 120.0 . . ? C4C C3C C2C 120.0 . . ? C3C C4C C5C 120.0 . . ? C6C C5C C4C 120.0 . . ? C5C C6C C1C 120.0 . . ? C6D C1D C2D 120.0 . . ? C6D C1D P2 120.8(2) . . ? C2D C1D P2 119.2(2) . . ? C3D C2D C1D 120.0 . . ? C2D C3D C4D 120.0 . . ? C3D C4D C5D 120.0 . . ? C6D C5D C4D 120.0 . . ? C5D C6D C1D 120.0 . . ? C2E C1E C6E 120.0 . . ? C2E C1E P2 123.0(2) . . ? C6E C1E P2 117.0(2) . . ? C3E C2E C1E 120.0 . . ? C4E C3E C2E 120.0 . . ? C3E C4E C5E 120.0 . . ? C6E C5E C4E 120.0 . . ? C5E C6E C1E 120.0 . . ? C6F C1F C2F 120.0 . . ? C6F C1F P2 116.89(19) . . ? C2F C1F P2 123.11(19) . . ? C3F C2F C1F 120.0 . . ? C4F C3F C2F 120.0 . . ? C3F C4F C5F 120.0 . . ? C6F C5F C4F 120.0 . . ? C1F C6F C5F 120.0 . . ? C2G C1G C6G 120.0 . . ? C2G C1G P3 121.60(19) . . ? C6G C1G P3 118.40(19) . . ? C3G C2G C1G 120.0 . . ? C2G C3G C4G 120.0 . . ? C3G C4G C5G 120.0 . . ? C6G C5G C4G 120.0 . . ? C5G C6G C1G 120.0 . . ? C2H C1H C6H 120.0 . . ? C2H C1H P3 124.32(19) . . ? C6H C1H P3 115.60(19) . . ? C1H C2H C3H 120.0 . . ? C2H C3H C4H 120.0 . . ? C5H C4H C3H 120.0 . . ? C6H C5H C4H 120.0 . . ? C5H C6H C1H 120.0 . . ? C6I C1I C2I 120.0 . . ? C6I C1I P3 119.52(18) . . ? C2I C1I P3 120.38(18) . . ? C3I C2I C1I 120.0 . . ? C2I C3I C4I 120.0 . . ? C3I C4I C5I 120.0 . . ? C6I C5I C4I 120.0 . . ? C5I C6I C1I 120.0 . . ? C2K C1K C6K 120.0 . . ? C2K C1K P4 117.61(19) . . ? C6K C1K P4 122.39(19) . . ? C3K C2K C1K 120.0 . . ? C2K C3K C4K 120.0 . . ? C5K C4K C3K 120.0 . . ? C4K C5K C6K 120.0 . . ? C1K C6K C5K 120.0 . . ? C2L C1L C6L 120.0 . . ? C2L C1L P4 119.60(17) . . ? C6L C1L P4 120.37(17) . . ? C1L C2L C3L 120.0 . . ? C4L C3L C2L 120.0 . . ? C3L C4L C5L 120.0 . . ? C4L C5L C6L 120.0 . . ? C5L C6L C1L 120.0 . . ? C2M C1M C6M 120.0 . . ? C2M C1M P4 119.78(18) . . ? C6M C1M P4 120.06(18) . . ? C1M C2M C3M 120.0 . . ? C2M C3M C4M 120.0 . . ? C5M C4M C3M 120.0 . . ? C6M C5M C4M 120.0 . . ? C5M C6M C1M 120.0 . . ? S1 O6 Na1 157.7(14) . . ? S2 O8 Na1 89.2(9) . . ? S2 O9 Na1 104.4(9) . . ? O7 S1 O5 113.5(13) . . ? O7 S1 O6 115.7(15) . . ? O5 S1 O6 113.2(16) . . ? O7 S1 C17 104.2(15) . . ? O5 S1 C17 104.5(16) . . ? O6 S1 C17 104.1(15) . . ? O10 S2 O8 115.9(11) . . ? O10 S2 O9 111.8(11) . . ? O8 S2 O9 113.1(11) . . ? O10 S2 C18 106.9(12) . . ? O8 S2 C18 104.4(12) . . ? O9 S2 C18 103.4(11) . . ? O10 S2 Na1 135.9(9) . . ? O8 S2 Na1 63.8(8) . . ? O9 S2 Na1 49.3(7) . . ? C18 S2 Na1 115.9(9) . . ? O13 S3 O12 119(2) . . ? O13 S3 O11 113.3(19) . . ? O12 S3 O11 110.7(16) . . ? O13 S3 C19 104.7(16) . . ? O12 S3 C19 104.4(19) . . ? O11 S3 C19 102.5(15) . . ? Cl3 C1S Cl1 111.2(12) . . ? Cl3 C1S Cl2 106.5(12) . . ? Cl1 C1S Cl2 106.1(13) . . ? Cl5 C2S Cl4 108.3(16) . . ? Cl5 C2S Cl6 101.4(15) . . ? Cl4 C2S Cl6 98.8(19) . . ? Cl9 C3S Cl7 106.1(13) . . ? Cl9 C3S Cl8 104.1(15) . . ? Cl7 C3S Cl8 109.2(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.102 _refine_diff_density_min -4.242 _refine_diff_density_rms 0.198 # Attachment 'complex2_new.cif' data_8007 _database_code_depnum_ccdc_archive 'CCDC 711714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.5 H82.5 F12 Fe2 N2 O8.75 P6 Pt2' _chemical_formula_weight 2181.72 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.3878(8) _cell_length_b 13.2026(5) _cell_length_c 32.0746(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.5460(10) _cell_angle_gamma 90.00 _cell_volume 8625.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8514 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.18 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4292 _exptl_absorpt_coefficient_mu 3.757 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3149 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30060 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9869 _reflns_number_gt 8453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. During final anisotropic refinement, the thermal parameters of the F atoms became quite large. Splitting the F atoms into disordered pair did not improve the refinement. EADP instruction was used to make the opposite F atoms having the same thermal parameter. There is one solvent methanol. Another group of solvent peaks were assigned as partially occupied by methanol and water. H atoms were not located for the water and the disordered methanol. ; _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^)+(0.0511P)^2^+38.3902P] 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 9869 _refine_ls_number_parameters 516 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 O1W O 0.4752(3) 0.3635(6) 0.6803(2) 0.0671(18) Uani 0.75 1 d P A 1 O2W O 0.5000 0.1926(14) 0.7500 0.150 Uiso 0.75 2 d SP B 1 O2S O 0.5089(9) 0.3695(14) 0.7050(6) 0.048(4) Uiso 0.25 1 d P C 2 C2S C 0.4782(15) 0.271(2) 0.7001(10) 0.065(7) Uiso 0.25 1 d P C 2 Pt1 Pt 0.384750(8) 0.594759(13) 0.648644(5) 0.02333(7) Uani 1 1 d . . . Fe2 Fe 0.32803(3) 0.38480(5) 0.55329(2) 0.02683(15) Uani 1 1 d . . . P1 P 0.42594(6) 0.57461(9) 0.58534(4) 0.0237(2) Uani 1 1 d . . . P2 P 0.28511(6) 0.52287(10) 0.63678(4) 0.0250(2) Uani 1 1 d . . . N1 N 0.53057(19) 0.6684(3) 0.82816(12) 0.0291(9) Uani 1 1 d . . . O1 O 0.35207(16) 0.6246(3) 0.70803(10) 0.0307(7) Uani 1 1 d . . . O2 O 0.41163(19) 0.4939(3) 0.73252(12) 0.0446(9) Uani 1 1 d . . . C1 C 0.3774(2) 0.5681(4) 0.73726(15) 0.0318(11) Uani 1 1 d . . . C2 C 0.3638(3) 0.6037(5) 0.78149(16) 0.0403(13) Uani 1 1 d . . . H2A H 0.3237 0.6448 0.7811 0.048 Uiso 1 1 calc R . . H2B H 0.3578 0.5453 0.7998 0.048 Uiso 1 1 calc R . . C3 C 0.4769(2) 0.6178(4) 0.81478(15) 0.0314(11) Uani 1 1 d . . . H3 H 0.4764 0.5469 0.8173 0.038 Uiso 1 1 calc R . . C4 C 0.4221(2) 0.6660(4) 0.79728(15) 0.0345(11) Uani 1 1 d . . . C5 C 0.4240(3) 0.7708(5) 0.79366(19) 0.0500(15) Uani 1 1 d . . . H5 H 0.3877 0.8060 0.7818 0.060 Uiso 1 1 calc R . . C6 C 0.4795(3) 0.8229(5) 0.8075(2) 0.0530(16) Uani 1 1 d . . . H6 H 0.4811 0.8939 0.8054 0.064 Uiso 1 1 calc R . . C7 C 0.5329(3) 0.7693(4) 0.82438(17) 0.0394(12) Uani 1 1 d . . . H7 H 0.5711 0.8043 0.8333 0.047 Uiso 1 1 calc R . . C8 C 0.4153(2) 0.4516(4) 0.56250(15) 0.0256(9) Uani 1 1 d . . . C9 C 0.4053(2) 0.4245(4) 0.51949(16) 0.0333(11) Uani 1 1 d . . . H9 H 0.4042 0.4717 0.4955 0.040 Uiso 1 1 calc R . . C10 C 0.3974(2) 0.3175(4) 0.51738(18) 0.0411(13) Uani 1 1 d . . . H10 H 0.3879 0.2780 0.4916 0.049 Uiso 1 1 calc R . . C11 C 0.4023(3) 0.2776(4) 0.55782(19) 0.0411(13) Uani 1 1 d . . . H11 H 0.3970 0.2055 0.5654 0.049 Uiso 1 1 calc R . . C12 C 0.4137(2) 0.3590(4) 0.58619(17) 0.0330(11) Uani 1 1 d . . . H12 H 0.4192 0.3531 0.6169 0.040 Uiso 1 1 calc R . . C13 C 0.2639(2) 0.4521(4) 0.59039(15) 0.0285(10) Uani 1 1 d . . . C14 C 0.2487(2) 0.3466(4) 0.58679(16) 0.0345(11) Uani 1 1 d . . . H14 H 0.2484 0.2973 0.6100 0.041 Uiso 1 1 calc R . . C15 C 0.2350(2) 0.3248(5) 0.54382(17) 0.0398(13) Uani 1 1 d . . . H15 H 0.2244 0.2573 0.5319 0.048 Uiso 1 1 calc R . . C16 C 0.2407(3) 0.4153(5) 0.52104(17) 0.0409(13) Uani 1 1 d . . . H16 H 0.2346 0.4221 0.4904 0.049 Uiso 1 1 calc R . . C17 C 0.2583(2) 0.4942(4) 0.54916(15) 0.0324(11) Uani 1 1 d . . . H17 H 0.2655 0.5659 0.5417 0.039 Uiso 1 1 calc R . . C1A C 0.2196(2) 0.6156(4) 0.63739(16) 0.0342(11) Uani 1 1 d . . . C2A C 0.1548(3) 0.5839(5) 0.6305(2) 0.0476(15) Uani 1 1 d . . . H2A1 H 0.1452 0.5159 0.6240 0.057 Uiso 1 1 calc R . . C3A C 0.1048(3) 0.6543(6) 0.6334(2) 0.0569(17) Uani 1 1 d . . . H3A H 0.0609 0.6334 0.6292 0.068 Uiso 1 1 calc R . . C4A C 0.1184(3) 0.7543(6) 0.6422(2) 0.0594(19) Uani 1 1 d . . . H4A H 0.0839 0.8010 0.6442 0.071 Uiso 1 1 calc R . . C5A C 0.1813(3) 0.7857(5) 0.64804(19) 0.0510(15) Uani 1 1 d . . . H5A H 0.1903 0.8543 0.6537 0.061 Uiso 1 1 calc R . . C6A C 0.2326(3) 0.7168(4) 0.64575(16) 0.0394(12) Uani 1 1 d . . . H6A H 0.2762 0.7390 0.6499 0.047 Uiso 1 1 calc R . . C1B C 0.2711(2) 0.4374(4) 0.67982(16) 0.0349(11) Uani 1 1 d . . . C2B C 0.2331(3) 0.4669(5) 0.71237(16) 0.0482(16) Uani 1 1 d . . . H2B1 H 0.2113 0.5296 0.7115 0.058 Uiso 1 1 calc R . . C3B C 0.2277(4) 0.4033(7) 0.7461(2) 0.069(3) Uani 1 1 d . . . H3B H 0.2026 0.4237 0.7685 0.083 Uiso 1 1 calc R . . C4B C 0.2582(4) 0.3107(7) 0.7476(2) 0.078(3) Uani 1 1 d . . . H4B H 0.2533 0.2677 0.7706 0.093 Uiso 1 1 calc R . . C5B C 0.2961(4) 0.2810(6) 0.7154(2) 0.068(2) Uani 1 1 d . . . H5B H 0.3166 0.2172 0.7161 0.082 Uiso 1 1 calc R . . C6B C 0.3040(3) 0.3454(5) 0.68213(19) 0.0477(15) Uani 1 1 d . . . H6B H 0.3318 0.3267 0.6608 0.057 Uiso 1 1 calc R . . C1C C 0.3984(2) 0.6659(4) 0.54618(14) 0.0275(10) Uani 1 1 d . . . C2C C 0.3484(3) 0.7340(4) 0.55320(17) 0.0385(12) Uani 1 1 d . . . H2C H 0.3272 0.7325 0.5786 0.046 Uiso 1 1 calc R . . C3C C 0.3296(3) 0.8039(5) 0.5231(2) 0.0523(16) Uani 1 1 d . . . H3C H 0.2960 0.8505 0.5280 0.063 Uiso 1 1 calc R . . C4C C 0.3603(3) 0.8051(5) 0.4857(2) 0.0552(17) Uani 1 1 d . . . H4C H 0.3468 0.8518 0.4650 0.066 Uiso 1 1 calc R . . C5C C 0.4097(3) 0.7397(5) 0.47849(18) 0.0468(15) Uani 1 1 d . . . H5C H 0.4306 0.7423 0.4530 0.056 Uiso 1 1 calc R . . C6C C 0.4297(3) 0.6695(4) 0.50826(16) 0.0360(12) Uani 1 1 d . . . H6C H 0.4640 0.6243 0.5031 0.043 Uiso 1 1 calc R . . C1D C 0.5145(2) 0.5914(4) 0.58764(15) 0.0279(10) Uani 1 1 d . . . C2D C 0.5396(2) 0.6903(4) 0.58997(16) 0.0320(11) Uani 1 1 d . . . H2D H 0.5112 0.7463 0.5876 0.038 Uiso 1 1 calc R . . C3D C 0.6073(3) 0.7047(5) 0.59588(17) 0.0408(13) Uani 1 1 d . . . H3D H 0.6246 0.7706 0.5981 0.049 Uiso 1 1 calc R . . C4D C 0.6488(3) 0.6223(5) 0.59852(19) 0.0444(14) Uani 1 1 d . . . H4D H 0.6943 0.6324 0.6023 0.053 Uiso 1 1 calc R . . C5D C 0.6244(2) 0.5265(5) 0.59577(18) 0.0413(13) Uani 1 1 d . . . H5D H 0.6533 0.4709 0.5972 0.050 Uiso 1 1 calc R . . C6D C 0.5570(2) 0.5099(4) 0.59081(16) 0.0339(11) Uani 1 1 d . . . H6D H 0.5404 0.4434 0.5896 0.041 Uiso 1 1 calc R . . P3 P 0.84324(11) 0.51851(16) 0.62889(8) 0.0731(6) Uani 1 1 d D . . F1 F 0.8356(6) 0.6308(5) 0.6326(3) 0.210(3) Uani 1 1 d D . . F2 F 0.8024(5) 0.5249(9) 0.5884(2) 0.205(3) Uani 1 1 d D . . F3 F 0.8461(7) 0.4044(5) 0.6268(4) 0.210(3) Uani 1 1 d D . . F4 F 0.8794(5) 0.5035(9) 0.6724(2) 0.205(3) Uani 1 1 d D . . F5 F 0.9036(4) 0.5237(10) 0.6062(4) 0.233(4) Uani 1 1 d D . . F6 F 0.7800(4) 0.5179(10) 0.6539(3) 0.233(4) Uani 1 1 d D . . C1S C 0.5302(8) 0.9568(11) 0.5484(4) 0.155(6) Uani 1 1 d . . . H1S1 H 0.5114 1.0229 0.5422 0.233 Uiso 1 1 calc R . . H1S2 H 0.5044 0.9050 0.5339 0.233 Uiso 1 1 calc R . . H1S3 H 0.5750 0.9546 0.5394 0.233 Uiso 1 1 calc R . . O1S O 0.5300(4) 0.9391(7) 0.5923(3) 0.123(3) Uani 1 1 d . . . H1S H 0.4916 0.9341 0.5995 0.184 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.066(4) 0.084(5) 0.052(4) -0.003(4) 0.006(3) 0.006(4) Pt1 0.02211(10) 0.02929(10) 0.01843(10) -0.00076(7) -0.00080(6) -0.00402(7) Fe2 0.0244(3) 0.0315(4) 0.0250(3) -0.0051(3) 0.0051(3) -0.0065(3) P1 0.0208(5) 0.0296(6) 0.0205(6) 0.0025(4) 0.0003(4) -0.0041(4) P2 0.0224(5) 0.0323(6) 0.0203(6) -0.0036(5) 0.0028(4) -0.0031(5) N1 0.028(2) 0.038(2) 0.022(2) -0.0019(16) -0.0039(16) 0.0064(17) O1 0.0304(17) 0.043(2) 0.0186(16) -0.0060(14) -0.0003(13) -0.0026(15) O2 0.039(2) 0.053(2) 0.042(2) 0.0006(18) 0.0017(17) 0.0078(19) C1 0.026(2) 0.046(3) 0.023(2) -0.003(2) 0.0015(19) -0.005(2) C2 0.030(3) 0.070(4) 0.021(2) -0.002(2) 0.002(2) 0.003(2) C3 0.031(2) 0.042(3) 0.021(2) -0.004(2) 0.0019(19) 0.005(2) C4 0.031(2) 0.053(3) 0.020(2) -0.005(2) -0.0001(19) 0.009(2) C5 0.043(3) 0.060(4) 0.046(3) 0.004(3) -0.010(3) 0.022(3) C6 0.053(4) 0.040(3) 0.065(4) 0.003(3) -0.012(3) 0.013(3) C7 0.039(3) 0.040(3) 0.039(3) -0.001(2) -0.007(2) 0.002(2) C8 0.020(2) 0.029(2) 0.028(2) -0.0017(19) 0.0020(18) -0.0017(18) C9 0.023(2) 0.048(3) 0.030(3) -0.007(2) 0.0086(19) -0.006(2) C10 0.031(3) 0.052(3) 0.041(3) -0.020(3) 0.012(2) -0.006(2) C11 0.037(3) 0.029(3) 0.057(4) -0.004(2) 0.011(3) -0.001(2) C12 0.032(3) 0.030(3) 0.037(3) 0.004(2) 0.003(2) -0.002(2) C13 0.019(2) 0.041(3) 0.026(2) -0.007(2) 0.0019(18) -0.0036(19) C14 0.029(2) 0.043(3) 0.033(3) -0.009(2) 0.011(2) -0.012(2) C15 0.029(3) 0.052(3) 0.039(3) -0.018(3) 0.009(2) -0.017(2) C16 0.027(3) 0.067(4) 0.028(3) -0.010(3) -0.002(2) -0.005(2) C17 0.022(2) 0.046(3) 0.028(3) -0.003(2) -0.0014(18) 0.003(2) C1A 0.028(2) 0.047(3) 0.027(3) -0.004(2) 0.003(2) 0.002(2) C2A 0.030(3) 0.064(4) 0.049(4) -0.010(3) 0.001(2) 0.001(3) C3A 0.030(3) 0.084(5) 0.056(4) -0.006(4) 0.003(3) 0.011(3) C4A 0.058(4) 0.075(5) 0.045(4) 0.004(3) 0.006(3) 0.037(4) C5A 0.061(4) 0.053(4) 0.040(3) 0.001(3) 0.000(3) 0.017(3) C6A 0.046(3) 0.046(3) 0.026(3) -0.002(2) 0.005(2) 0.005(3) C1B 0.030(2) 0.048(3) 0.027(3) 0.000(2) 0.002(2) -0.016(2) C2B 0.049(3) 0.072(4) 0.024(3) -0.008(3) 0.008(2) -0.027(3) C3B 0.069(5) 0.114(7) 0.025(3) -0.003(4) 0.011(3) -0.051(5) C4B 0.100(6) 0.095(6) 0.036(4) 0.024(4) -0.010(4) -0.059(5) C5B 0.089(5) 0.060(4) 0.055(4) 0.022(3) -0.013(4) -0.026(4) C6B 0.051(3) 0.052(4) 0.040(3) 0.014(3) 0.001(3) -0.016(3) C1C 0.027(2) 0.030(2) 0.025(2) 0.0052(19) -0.0025(18) -0.0048(19) C2C 0.038(3) 0.045(3) 0.033(3) 0.003(2) 0.009(2) 0.000(2) C3C 0.050(3) 0.054(4) 0.054(4) 0.017(3) 0.010(3) 0.021(3) C4C 0.060(4) 0.061(4) 0.045(4) 0.028(3) 0.001(3) 0.012(3) C5C 0.045(3) 0.062(4) 0.034(3) 0.021(3) 0.010(2) 0.004(3) C6C 0.034(3) 0.043(3) 0.032(3) 0.010(2) 0.004(2) 0.004(2) C1D 0.021(2) 0.038(3) 0.025(2) 0.0041(19) 0.0024(17) -0.0074(19) C2D 0.028(2) 0.036(3) 0.032(3) 0.006(2) 0.002(2) -0.006(2) C3D 0.033(3) 0.048(3) 0.041(3) 0.009(2) 0.000(2) -0.016(2) C4D 0.021(2) 0.065(4) 0.047(3) 0.006(3) 0.000(2) -0.009(2) C5D 0.024(2) 0.055(4) 0.044(3) 0.012(3) -0.001(2) 0.005(2) C6D 0.026(2) 0.037(3) 0.038(3) 0.006(2) 0.000(2) -0.003(2) P3 0.0757(14) 0.0525(11) 0.0908(16) 0.0175(11) -0.0013(12) 0.0066(10) F1 0.342(10) 0.067(3) 0.221(7) 0.000(4) 0.002(7) 0.006(5) F2 0.227(7) 0.270(9) 0.112(4) -0.009(5) -0.052(4) 0.107(6) F3 0.342(10) 0.067(3) 0.221(7) 0.000(4) 0.002(7) 0.006(5) F4 0.227(7) 0.270(9) 0.112(4) -0.009(5) -0.052(4) 0.107(6) F5 0.136(5) 0.312(10) 0.261(8) 0.110(8) 0.103(5) 0.039(6) F6 0.136(5) 0.312(10) 0.261(8) 0.110(8) 0.103(5) 0.039(6) C1S 0.225(18) 0.129(12) 0.112(11) 0.042(9) 0.015(11) -0.030(11) O1S 0.105(6) 0.092(5) 0.170(9) 0.001(6) 0.004(6) 0.002(5) _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 O2S C2S 1.45(4) . ? Pt1 O1 2.083(3) . ? Pt1 N1 2.089(4) 2_656 ? Pt1 P1 2.2473(12) . ? Pt1 P2 2.2592(12) . ? Fe2 C8 1.997(4) . ? Fe2 C13 2.013(5) . ? Fe2 C9 2.021(5) . ? Fe2 C17 2.026(5) . ? Fe2 C12 2.029(5) . ? Fe2 C14 2.045(5) . ? Fe2 C16 2.059(5) . ? Fe2 C10 2.064(5) . ? Fe2 C15 2.065(5) . ? Fe2 C11 2.073(5) . ? P1 C8 1.790(5) . ? P1 C1C 1.812(5) . ? P1 C1D 1.818(5) . ? P2 C13 1.793(5) . ? P2 C1A 1.812(5) . ? P2 C1B 1.815(5) . ? N1 C3 1.336(6) . ? N1 C7 1.339(7) . ? N1 Pt1 2.089(4) 2_656 ? O1 C1 1.288(6) . ? O2 C1 1.216(6) . ? C1 C2 1.532(7) . ? C2 C4 1.514(8) . ? C3 C4 1.384(7) . ? C4 C5 1.389(9) . ? C5 C6 1.380(9) . ? C6 C7 1.388(8) . ? C8 C9 1.431(7) . ? C8 C12 1.441(7) . ? C9 C10 1.423(8) . ? C10 C11 1.399(8) . ? C11 C12 1.420(8) . ? C13 C14 1.431(7) . ? C13 C17 1.434(7) . ? C14 C15 1.423(7) . ? C15 C16 1.407(8) . ? C16 C17 1.414(7) . ? C1A C6A 1.386(8) . ? C1A C2A 1.395(8) . ? C2A C3A 1.386(9) . ? C3A C4A 1.377(11) . ? C4A C5A 1.352(10) . ? C5A C6A 1.391(8) . ? C1B C2B 1.383(8) . ? C1B C6B 1.388(9) . ? C2B C3B 1.377(10) . ? C3B C4B 1.371(12) . ? C4B C5B 1.375(12) . ? C5B C6B 1.379(8) . ? C1C C2C 1.384(7) . ? C1C C6C 1.399(7) . ? C2C C3C 1.379(8) . ? C3C C4C 1.375(9) . ? C4C C5C 1.354(9) . ? C5C C6C 1.380(7) . ? C1D C6D 1.382(7) . ? C1D C2D 1.403(7) . ? C2D C3D 1.398(7) . ? C3D C4D 1.377(8) . ? C4D C5D 1.361(9) . ? C5D C6D 1.395(7) . ? P3 F5 1.459(7) . ? P3 F1 1.495(7) . ? P3 F3 1.509(6) . ? P3 F2 1.514(7) . ? P3 F6 1.548(7) . ? P3 F4 1.561(7) . ? C1S O1S 1.425(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 O1 Pt1 N1 83.06(14) . 2_656 ? O1 Pt1 P1 174.88(10) . . ? N1 Pt1 P1 92.34(11) 2_656 . ? O1 Pt1 P2 84.94(10) . . ? N1 Pt1 P2 167.99(11) 2_656 . ? P1 Pt1 P2 99.63(4) . . ? C8 Fe2 C13 108.38(19) . . ? C8 Fe2 C9 41.72(19) . . ? C13 Fe2 C9 138.1(2) . . ? C8 Fe2 C17 108.2(2) . . ? C13 Fe2 C17 41.6(2) . . ? C9 Fe2 C17 110.0(2) . . ? C8 Fe2 C12 41.94(19) . . ? C13 Fe2 C12 109.5(2) . . ? C9 Fe2 C12 69.4(2) . . ? C17 Fe2 C12 137.6(2) . . ? C8 Fe2 C14 138.8(2) . . ? C13 Fe2 C14 41.3(2) . . ? C9 Fe2 C14 178.9(2) . . ? C17 Fe2 C14 69.0(2) . . ? C12 Fe2 C14 111.6(2) . . ? C8 Fe2 C16 137.2(2) . . ? C13 Fe2 C16 68.9(2) . . ? C9 Fe2 C16 111.0(2) . . ? C17 Fe2 C16 40.5(2) . . ? C12 Fe2 C16 178.1(2) . . ? C14 Fe2 C16 68.0(2) . . ? C8 Fe2 C10 69.2(2) . . ? C13 Fe2 C10 177.2(2) . . ? C9 Fe2 C10 40.8(2) . . ? C17 Fe2 C10 140.0(2) . . ? C12 Fe2 C10 67.8(2) . . ? C14 Fe2 C10 139.9(2) . . ? C16 Fe2 C10 113.7(2) . . ? C8 Fe2 C15 176.3(2) . . ? C13 Fe2 C15 68.9(2) . . ? C9 Fe2 C15 138.9(2) . . ? C17 Fe2 C15 68.1(2) . . ? C12 Fe2 C15 140.9(2) . . ? C14 Fe2 C15 40.5(2) . . ? C16 Fe2 C15 39.9(2) . . ? C10 Fe2 C15 113.6(2) . . ? C8 Fe2 C11 69.4(2) . . ? C13 Fe2 C11 138.7(2) . . ? C9 Fe2 C11 68.3(2) . . ? C17 Fe2 C11 177.6(2) . . ? C12 Fe2 C11 40.5(2) . . ? C14 Fe2 C11 112.8(2) . . ? C16 Fe2 C11 141.4(2) . . ? C10 Fe2 C11 39.5(2) . . ? C15 Fe2 C11 114.3(2) . . ? C8 P1 C1C 107.0(2) . . ? C8 P1 C1D 103.2(2) . . ? C1C P1 C1D 102.9(2) . . ? C8 P1 Pt1 115.71(15) . . ? C1C P1 Pt1 115.52(16) . . ? C1D P1 Pt1 111.06(16) . . ? C13 P2 C1A 102.1(2) . . ? C13 P2 C1B 105.5(2) . . ? C1A P2 C1B 105.7(3) . . ? C13 P2 Pt1 122.71(15) . . ? C1A P2 Pt1 111.82(18) . . ? C1B P2 Pt1 107.65(16) . . ? C3 N1 C7 119.9(4) . . ? C3 N1 Pt1 122.3(3) . 2_656 ? C7 N1 Pt1 117.6(3) . 2_656 ? C1 O1 Pt1 115.0(3) . . ? O2 C1 O1 126.1(5) . . ? O2 C1 C2 119.5(5) . . ? O1 C1 C2 114.4(5) . . ? C4 C2 C1 107.8(4) . . ? N1 C3 C4 122.4(5) . . ? C3 C4 C5 117.8(5) . . ? C3 C4 C2 119.6(5) . . ? C5 C4 C2 122.6(5) . . ? C6 C5 C4 119.8(5) . . ? C5 C6 C7 119.2(6) . . ? N1 C7 C6 120.9(5) . . ? C9 C8 C12 106.9(4) . . ? C9 C8 P1 129.1(4) . . ? C12 C8 P1 124.0(4) . . ? C9 C8 Fe2 70.1(3) . . ? C12 C8 Fe2 70.2(3) . . ? P1 C8 Fe2 123.5(2) . . ? C10 C9 C8 107.8(5) . . ? C10 C9 Fe2 71.2(3) . . ? C8 C9 Fe2 68.2(3) . . ? C11 C10 C9 109.0(5) . . ? C11 C10 Fe2 70.6(3) . . ? C9 C10 Fe2 68.0(3) . . ? C10 C11 C12 108.2(5) . . ? C10 C11 Fe2 69.9(3) . . ? C12 C11 Fe2 68.1(3) . . ? C11 C12 C8 108.1(5) . . ? C11 C12 Fe2 71.4(3) . . ? C8 C12 Fe2 67.8(3) . . ? C14 C13 C17 107.1(4) . . ? C14 C13 P2 128.1(4) . . ? C17 C13 P2 124.8(4) . . ? C14 C13 Fe2 70.5(3) . . ? C17 C13 Fe2 69.7(3) . . ? P2 C13 Fe2 125.6(2) . . ? C15 C14 C13 107.9(5) . . ? C15 C14 Fe2 70.5(3) . . ? C13 C14 Fe2 68.2(3) . . ? C16 C15 C14 108.3(5) . . ? C16 C15 Fe2 69.8(3) . . ? C14 C15 Fe2 69.0(3) . . ? C15 C16 C17 108.5(5) . . ? C15 C16 Fe2 70.3(3) . . ? C17 C16 Fe2 68.5(3) . . ? C16 C17 C13 108.1(5) . . ? C16 C17 Fe2 71.0(3) . . ? C13 C17 Fe2 68.7(3) . . ? C6A C1A C2A 119.4(5) . . ? C6A C1A P2 121.3(4) . . ? C2A C1A P2 119.3(4) . . ? C3A C2A C1A 118.9(6) . . ? C4A C3A C2A 121.0(6) . . ? C5A C4A C3A 120.2(6) . . ? C4A C5A C6A 120.2(6) . . ? C1A C6A C5A 120.2(6) . . ? C2B C1B C6B 119.4(5) . . ? C2B C1B P2 120.8(5) . . ? C6B C1B P2 119.6(4) . . ? C3B C2B C1B 119.3(7) . . ? C4B C3B C2B 121.3(7) . . ? C3B C4B C5B 119.7(7) . . ? C4B C5B C6B 119.7(8) . . ? C5B C6B C1B 120.6(7) . . ? C2C C1C C6C 119.1(5) . . ? C2C C1C P1 121.8(4) . . ? C6C C1C P1 119.1(4) . . ? C3C C2C C1C 120.3(5) . . ? C4C C3C C2C 119.6(6) . . ? C5C C4C C3C 120.9(5) . . ? C4C C5C C6C 120.5(5) . . ? C5C C6C C1C 119.5(5) . . ? C6D C1D C2D 119.7(4) . . ? C6D C1D P1 121.7(4) . . ? C2D C1D P1 118.4(4) . . ? C3D C2D C1D 119.3(5) . . ? C4D C3D C2D 120.0(5) . . ? C5D C4D C3D 120.6(5) . . ? C4D C5D C6D 120.5(5) . . ? C1D C6D C5D 119.8(5) . . ? F5 P3 F1 95.0(7) . . ? F5 P3 F3 89.4(7) . . ? F1 P3 F3 175.6(7) . . ? F5 P3 F2 90.8(6) . . ? F1 P3 F2 87.5(6) . . ? F3 P3 F2 92.3(7) . . ? F5 P3 F6 177.3(8) . . ? F1 P3 F6 82.6(7) . . ? F3 P3 F6 93.0(7) . . ? F2 P3 F6 90.3(6) . . ? F5 P3 F4 94.4(6) . . ? F1 P3 F4 95.8(6) . . ? F3 P3 F4 84.0(6) . . ? F2 P3 F4 173.6(7) . . ? F6 P3 F4 84.7(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.609 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.139 # Attachment 'complex1_new.cif' data_8048 _database_code_depnum_ccdc_archive 'CCDC 711715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H76 Ca Cl6 F12 Fe2 N2 O19 P4 Pd2 S4' _chemical_formula_weight 2522.91 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.4811(9) _cell_length_b 21.8543(11) _cell_length_c 25.3431(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.479(2) _cell_angle_gamma 90.00 _cell_volume 10204.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3468 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 21.07 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5048 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7005 _exptl_absorpt_correction_T_max 0.9389 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58893 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17928 _reflns_number_gt 11105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One of the CHCl3 is disordered with one of the Cl atoms and the C atom disordered into two positions with occupancy ratio 50:50. Restriants in bond length and thermal parameters were applied to the disordered CHCl3. H atoms of the three water molecules were not located because the data quality is poor. ; _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^)+(0.0816P)^2^+44.6500P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17928 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2067 _refine_ls_wR_factor_gt 0.1822 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.68950(3) 0.18986(3) 0.64175(3) 0.02640(17) Uani 1 1 d . . . Pd2 Pd 0.28436(3) 0.30432(3) 0.64852(3) 0.02545(17) Uani 1 1 d . . . Fe3 Fe 0.12246(7) 0.37335(6) 0.73937(5) 0.0353(3) Uani 1 1 d . . . Fe4 Fe 0.86269(7) 0.11790(6) 0.73737(5) 0.0328(3) Uani 1 1 d . . . Ca1 Ca 0.50457(9) 0.24141(8) 0.77424(7) 0.0325(4) Uani 1 1 d . . . P1 P 0.72912(11) 0.09200(10) 0.64436(9) 0.0278(5) Uani 1 1 d . . . P2 P 0.79881(11) 0.23601(10) 0.66498(9) 0.0279(5) Uani 1 1 d . . . P3 P 0.18162(11) 0.25578(10) 0.67115(9) 0.0271(5) Uani 1 1 d . . . P4 P 0.24574(12) 0.40199(10) 0.65435(9) 0.0290(5) Uani 1 1 d . . . O1 O 0.6488(3) 0.2788(3) 0.6390(2) 0.0320(14) Uani 1 1 d . . . O2 O 0.5818(3) 0.2623(3) 0.7078(2) 0.0335(14) Uani 1 1 d . . . O3 O 0.3232(3) 0.2154(2) 0.6412(2) 0.0308(13) Uani 1 1 d . . . O4 O 0.4065(3) 0.2273(3) 0.7104(2) 0.0374(15) Uani 1 1 d . . . N1 N 0.5868(3) 0.1624(3) 0.6111(3) 0.0292(16) Uani 1 1 d . . . N2 N 0.3796(3) 0.3334(3) 0.6171(3) 0.0286(16) Uani 1 1 d . . . C1 C 0.5339(4) 0.1480(3) 0.6423(3) 0.0245(18) Uani 1 1 d . . . H1 H 0.5460 0.1415 0.6786 0.029 Uiso 1 1 calc R . . C2 C 0.4615(4) 0.1425(4) 0.6228(3) 0.030(2) Uani 1 1 d . . . C3 C 0.4467(5) 0.1490(4) 0.5687(4) 0.046(3) Uani 1 1 d . . . H3 H 0.3987 0.1451 0.5538 0.055 Uiso 1 1 calc R . . C4 C 0.5020(5) 0.1611(5) 0.5364(4) 0.045(2) Uani 1 1 d . . . H4 H 0.4922 0.1644 0.4996 0.054 Uiso 1 1 calc R . . C5 C 0.5712(5) 0.1681(4) 0.5591(4) 0.037(2) Uani 1 1 d . . . H5 H 0.6088 0.1773 0.5375 0.045 Uiso 1 1 calc R . . C6 C 0.4034(4) 0.1343(4) 0.6600(4) 0.030(2) Uani 1 1 d . . . H6A H 0.4230 0.1137 0.6924 0.037 Uiso 1 1 calc R . . H6B H 0.3637 0.1094 0.6435 0.037 Uiso 1 1 calc R . . C7 C 0.3761(4) 0.1977(4) 0.6728(4) 0.029(2) Uani 1 1 d . . . C8 C 0.4407(4) 0.3445(3) 0.6461(4) 0.029(2) Uani 1 1 d . . . H8 H 0.4390 0.3456 0.6831 0.035 Uiso 1 1 calc R . . C9 C 0.5065(4) 0.3545(4) 0.6260(4) 0.030(2) Uani 1 1 d . . . C10 C 0.5084(5) 0.3541(5) 0.5720(4) 0.052(3) Uani 1 1 d . . . H10 H 0.5524 0.3606 0.5565 0.063 Uiso 1 1 calc R . . C11 C 0.4455(5) 0.3439(6) 0.5408(4) 0.058(3) Uani 1 1 d . . . H11 H 0.4458 0.3442 0.5037 0.070 Uiso 1 1 calc R . . C12 C 0.3821(5) 0.3332(5) 0.5642(4) 0.044(2) Uani 1 1 d . . . H12 H 0.3393 0.3255 0.5427 0.053 Uiso 1 1 calc R . . C13 C 0.5742(4) 0.3595(4) 0.6635(4) 0.033(2) Uani 1 1 d . . . H13A H 0.5624 0.3771 0.6974 0.039 Uiso 1 1 calc R . . H13B H 0.6102 0.3858 0.6483 0.039 Uiso 1 1 calc R . . C14 C 0.6039(4) 0.2945(4) 0.6716(4) 0.031(2) Uani 1 1 d . . . C15 C 0.7723(4) 0.0740(4) 0.7087(4) 0.032(2) Uani 1 1 d . . . C16 C 0.8279(5) 0.0312(4) 0.7246(4) 0.034(2) Uani 1 1 d . . . H16 H 0.8495 0.0012 0.7011 0.041 Uiso 1 1 calc R . . C17 C 0.8469(5) 0.0378(4) 0.7786(4) 0.045(2) Uani 1 1 d . . . H17 H 0.8845 0.0143 0.7999 0.054 Uiso 1 1 calc R . . C18 C 0.8040(5) 0.0854(4) 0.7969(4) 0.045(2) Uani 1 1 d . . . H18 H 0.8068 0.1012 0.8336 0.054 Uiso 1 1 calc R . . C19 C 0.7588(5) 0.1078(4) 0.7551(4) 0.036(2) Uani 1 1 d . . . H19 H 0.7228 0.1411 0.7573 0.043 Uiso 1 1 calc R . . C20 C 0.8758(4) 0.1971(4) 0.6977(3) 0.0278(19) Uani 1 1 d . . . C21 C 0.9021(5) 0.2044(4) 0.7521(4) 0.044(2) Uani 1 1 d . . . H21 H 0.8845 0.2342 0.7776 0.053 Uiso 1 1 calc R . . C22 C 0.9597(5) 0.1605(5) 0.7625(5) 0.057(3) Uani 1 1 d . . . H22 H 0.9878 0.1539 0.7970 0.068 Uiso 1 1 calc R . . C23 C 0.9682(5) 0.1276(5) 0.7154(4) 0.049(3) Uani 1 1 d . . . H23 H 1.0030 0.0938 0.7114 0.059 Uiso 1 1 calc R . . C24 C 0.9153(4) 0.1485(4) 0.6757(4) 0.035(2) Uani 1 1 d . . . H24 H 0.9087 0.1333 0.6388 0.042 Uiso 1 1 calc R . . C25 C 0.1079(4) 0.2936(4) 0.6996(4) 0.036(2) Uani 1 1 d . . . C26 C 0.0838(5) 0.2871(4) 0.7519(4) 0.046(3) Uani 1 1 d . . . H26 H 0.1034 0.2579 0.7793 0.055 Uiso 1 1 calc R . . C27 C 0.0284(5) 0.3301(5) 0.7576(5) 0.055(3) Uani 1 1 d . . . H27 H 0.0031 0.3367 0.7901 0.066 Uiso 1 1 calc R . . C28 C 0.0161(5) 0.3637(5) 0.7095(5) 0.056(3) Uani 1 1 d . . . H28 H -0.0194 0.3972 0.7027 0.068 Uiso 1 1 calc R . . C29 C 0.0651(4) 0.3420(4) 0.6740(4) 0.039(2) Uani 1 1 d . . . H29 H 0.0690 0.3569 0.6375 0.047 Uiso 1 1 calc R . . C30 C 0.2090(5) 0.4178(4) 0.7159(3) 0.034(2) Uani 1 1 d . . . C31 C 0.1531(5) 0.4610(4) 0.7293(4) 0.042(2) Uani 1 1 d . . . H31 H 0.1283 0.4912 0.7050 0.050 Uiso 1 1 calc R . . C32 C 0.1414(6) 0.4525(4) 0.7825(4) 0.049(3) Uani 1 1 d . . . H32 H 0.1046 0.4746 0.8016 0.059 Uiso 1 1 calc R . . C33 C 0.1865(6) 0.4059(5) 0.8042(4) 0.049(3) Uani 1 1 d . . . H33 H 0.1877 0.3899 0.8408 0.059 Uiso 1 1 calc R . . C34 C 0.2294(5) 0.3847(4) 0.7635(4) 0.040(2) Uani 1 1 d . . . H34 H 0.2661 0.3517 0.7673 0.048 Uiso 1 1 calc R . . C35 C 0.5793(7) 0.0630(6) 0.8524(5) 0.068(3) Uani 1 1 d . . . C36 C 0.4489(7) 0.4238(7) 0.8599(6) 0.075(4) Uani 1 1 d . . . C37 C 0.6020(9) 0.2868(7) 0.4220(7) 0.091(4) Uani 1 1 d . . . C1A C 0.6554(4) 0.0363(4) 0.6341(4) 0.031(2) Uani 1 1 d . . . C2A C 0.6341(5) 0.0167(5) 0.5834(4) 0.053(3) Uani 1 1 d . . . H2A H 0.6579 0.0315 0.5546 0.064 Uiso 1 1 calc R . . C3A C 0.5783(6) -0.0244(6) 0.5753(5) 0.072(4) Uani 1 1 d . . . H3A H 0.5640 -0.0373 0.5407 0.086 Uiso 1 1 calc R . . C4A C 0.5427(6) -0.0469(5) 0.6167(6) 0.066(3) Uani 1 1 d . . . H4A H 0.5056 -0.0762 0.6111 0.079 Uiso 1 1 calc R . . C5A C 0.5632(6) -0.0254(5) 0.6672(5) 0.058(3) Uani 1 1 d . . . H5A H 0.5387 -0.0391 0.6961 0.070 Uiso 1 1 calc R . . C6A C 0.6188(5) 0.0157(4) 0.6750(4) 0.046(2) Uani 1 1 d . . . H6A1 H 0.6321 0.0300 0.7094 0.055 Uiso 1 1 calc R . . C1B C 0.7899(4) 0.0734(4) 0.5940(3) 0.032(2) Uani 1 1 d . . . C2B C 0.8024(5) 0.1166(4) 0.5547(3) 0.038(2) Uani 1 1 d . . . H2B H 0.7781 0.1544 0.5541 0.046 Uiso 1 1 calc R . . C3B C 0.8499(5) 0.1037(5) 0.5173(4) 0.049(3) Uani 1 1 d . . . H3B H 0.8583 0.1329 0.4912 0.059 Uiso 1 1 calc R . . C4B C 0.8857(5) 0.0477(6) 0.5178(4) 0.058(3) Uani 1 1 d . . . H4B H 0.9192 0.0396 0.4926 0.069 Uiso 1 1 calc R . . C5B C 0.8723(5) 0.0039(5) 0.5551(4) 0.048(3) Uani 1 1 d . . . H5B H 0.8960 -0.0341 0.5549 0.057 Uiso 1 1 calc R . . C6B C 0.8245(5) 0.0161(4) 0.5925(4) 0.039(2) Uani 1 1 d . . . H6B1 H 0.8147 -0.0141 0.6174 0.047 Uiso 1 1 calc R . . C1C C 0.7849(4) 0.3001(4) 0.7085(4) 0.033(2) Uani 1 1 d . . . C2C C 0.8109(6) 0.3575(4) 0.6985(5) 0.058(3) Uani 1 1 d . . . H2C H 0.8343 0.3647 0.6675 0.069 Uiso 1 1 calc R . . C3C C 0.8032(7) 0.4037(5) 0.7330(5) 0.073(4) Uani 1 1 d . . . H3C H 0.8221 0.4424 0.7256 0.088 Uiso 1 1 calc R . . C4C C 0.7685(6) 0.3961(5) 0.7785(5) 0.067(3) Uani 1 1 d . . . H4C H 0.7634 0.4288 0.8020 0.080 Uiso 1 1 calc R . . C5C C 0.7417(5) 0.3396(5) 0.7884(4) 0.051(3) Uani 1 1 d . . . H5C H 0.7172 0.3332 0.8191 0.061 Uiso 1 1 calc R . . C6C C 0.7500(5) 0.2914(4) 0.7538(4) 0.040(2) Uani 1 1 d . . . H6C H 0.7316 0.2525 0.7614 0.048 Uiso 1 1 calc R . . C1D C 0.8338(5) 0.2680(4) 0.6059(4) 0.036(2) Uani 1 1 d . . . C2D C 0.9070(5) 0.2797(5) 0.6041(4) 0.050(3) Uani 1 1 d . . . H2D H 0.9395 0.2709 0.6335 0.060 Uiso 1 1 calc R . . C3D C 0.9321(6) 0.3040(6) 0.5594(5) 0.077(4) Uani 1 1 d . . . H3D H 0.9824 0.3099 0.5584 0.092 Uiso 1 1 calc R . . C4D C 0.8872(8) 0.3203(8) 0.5160(5) 0.097(5) Uani 1 1 d . . . H4D H 0.9055 0.3374 0.4857 0.117 Uiso 1 1 calc R . . C5D C 0.8135(7) 0.3101(7) 0.5190(5) 0.093(5) Uani 1 1 d . . . H5D H 0.7810 0.3210 0.4902 0.111 Uiso 1 1 calc R . . C6D C 0.7865(5) 0.2843(5) 0.5632(4) 0.054(3) Uani 1 1 d . . . H6D H 0.7364 0.2779 0.5643 0.065 Uiso 1 1 calc R . . C1E C 0.2060(4) 0.1941(4) 0.7171(4) 0.033(2) Uani 1 1 d . . . C2E C 0.2036(6) 0.1326(4) 0.7009(4) 0.055(3) Uani 1 1 d . . . H2E H 0.1894 0.1229 0.6655 0.066 Uiso 1 1 calc R . . C3E C 0.2216(7) 0.0871(5) 0.7362(5) 0.069(4) Uani 1 1 d . . . H3E H 0.2192 0.0460 0.7250 0.083 Uiso 1 1 calc R . . C4E C 0.2428(7) 0.1002(5) 0.7866(5) 0.065(3) Uani 1 1 d . . . H4E H 0.2534 0.0681 0.8106 0.078 Uiso 1 1 calc R . . C5E C 0.2494(6) 0.1601(5) 0.8042(4) 0.057(3) Uani 1 1 d . . . H5E H 0.2658 0.1691 0.8394 0.068 Uiso 1 1 calc R . . C6E C 0.2313(5) 0.2059(4) 0.7684(4) 0.049(3) Uani 1 1 d . . . H6E H 0.2364 0.2468 0.7795 0.059 Uiso 1 1 calc R . . C1F C 0.1390(4) 0.2207(4) 0.6115(4) 0.035(2) Uani 1 1 d . . . C2F C 0.0724(5) 0.1915(5) 0.6133(4) 0.057(3) Uani 1 1 d . . . H2F H 0.0500 0.1905 0.6453 0.068 Uiso 1 1 calc R . . C3F C 0.0393(7) 0.1645(7) 0.5695(5) 0.091(5) Uani 1 1 d . . . H3F H -0.0054 0.1444 0.5712 0.109 Uiso 1 1 calc R . . C4F C 0.0720(6) 0.1671(6) 0.5226(5) 0.068(4) Uani 1 1 d . . . H4F H 0.0481 0.1504 0.4918 0.081 Uiso 1 1 calc R . . C5F C 0.1374(6) 0.1929(5) 0.5199(4) 0.049(3) Uani 1 1 d . . . H5F H 0.1598 0.1930 0.4878 0.059 Uiso 1 1 calc R . . C6F C 0.1717(5) 0.2195(4) 0.5644(4) 0.042(2) Uani 1 1 d . . . H6F H 0.2179 0.2370 0.5627 0.050 Uiso 1 1 calc R . . C1G C 0.3205(5) 0.4553(4) 0.6510(4) 0.040(2) Uani 1 1 d . . . C2G C 0.3346(6) 0.4841(5) 0.6050(5) 0.062(3) Uani 1 1 d . . . H2G H 0.3039 0.4775 0.5742 0.074 Uiso 1 1 calc R . . C3G C 0.3951(7) 0.5238(6) 0.6033(7) 0.085(4) Uani 1 1 d . . . H3G H 0.4047 0.5433 0.5716 0.102 Uiso 1 1 calc R . . C4G C 0.4390(8) 0.5332(7) 0.6480(9) 0.105(6) Uani 1 1 d . . . H4G H 0.4789 0.5598 0.6467 0.126 Uiso 1 1 calc R . . C5G C 0.4270(7) 0.5053(6) 0.6949(7) 0.081(4) Uani 1 1 d . . . H5G H 0.4579 0.5125 0.7255 0.098 Uiso 1 1 calc R . . C6G C 0.3669(5) 0.4654(5) 0.6963(5) 0.052(3) Uani 1 1 d . . . H6G H 0.3581 0.4454 0.7280 0.062 Uiso 1 1 calc R . . C1H C 0.1814(5) 0.4249(4) 0.5996(4) 0.037(2) Uani 1 1 d . . . C2H C 0.1481(6) 0.4820(5) 0.5982(4) 0.050(3) Uani 1 1 d . . . H2H H 0.1580 0.5105 0.6256 0.060 Uiso 1 1 calc R . . C3H C 0.1003(8) 0.4955(7) 0.5556(6) 0.098(5) Uani 1 1 d . . . H3H H 0.0771 0.5338 0.5544 0.118 Uiso 1 1 calc R . . C4H C 0.0852(8) 0.4556(8) 0.5149(5) 0.108(6) Uani 1 1 d . . . H4H H 0.0522 0.4662 0.4863 0.130 Uiso 1 1 calc R . . C5H C 0.1194(7) 0.3990(7) 0.5164(5) 0.077(4) Uani 1 1 d . . . H5H H 0.1097 0.3708 0.4887 0.093 Uiso 1 1 calc R . . C6H C 0.1677(5) 0.3844(5) 0.5588(4) 0.049(3) Uani 1 1 d . . . H6H H 0.1914 0.3463 0.5598 0.059 Uiso 1 1 calc R . . S1 S 0.50599(14) 0.08092(11) 0.80408(11) 0.0459(6) Uani 1 1 d . . . O5 O 0.5319(3) 0.1360(3) 0.7799(3) 0.0431(16) Uani 1 1 d . . . O6 O 0.4455(4) 0.0894(3) 0.8346(4) 0.076(3) Uani 1 1 d . . . O7 O 0.5026(5) 0.0288(3) 0.7704(3) 0.085(3) Uani 1 1 d . . . F1 F 0.5896(6) 0.1055(5) 0.8874(3) 0.131(4) Uani 1 1 d . . . F2 F 0.6407(4) 0.0550(4) 0.8294(4) 0.116(3) Uani 1 1 d . . . F3 F 0.5653(5) 0.0114(4) 0.8784(3) 0.106(3) Uani 1 1 d . . . S2 S 0.52046(15) 0.39578(13) 0.82297(13) 0.0590(8) Uani 1 1 d . . . O8 O 0.4862(4) 0.3452(3) 0.7929(3) 0.0517(18) Uani 1 1 d . . . O9 O 0.5753(5) 0.3774(4) 0.8624(4) 0.100(4) Uani 1 1 d . . . F4 F 0.4316(6) 0.3850(6) 0.8951(4) 0.144(4) Uani 1 1 d . . . F5 F 0.3898(4) 0.4357(5) 0.8294(3) 0.113(3) Uani 1 1 d . . . F6 F 0.4675(4) 0.4734(4) 0.8878(4) 0.121(4) Uani 1 1 d . . . S3 S 0.64245(17) 0.21226(14) 0.42266(12) 0.0601(8) Uani 1 1 d . . . O10 O 0.5365(5) 0.4477(4) 0.7911(4) 0.104(4) Uani 1 1 d . . . O11 O 0.6868(5) 0.2165(4) 0.3791(3) 0.087(3) Uani 1 1 d . . . O12 O 0.6835(5) 0.2100(4) 0.4728(3) 0.083(3) Uani 1 1 d . . . O13 O 0.5817(6) 0.1722(5) 0.4156(5) 0.113(4) Uani 1 1 d . . . F7 F 0.6520(7) 0.3297(4) 0.4290(5) 0.143(4) Uani 1 1 d . . . F8 F 0.5640(6) 0.2991(5) 0.3777(5) 0.153(4) Uani 1 1 d . . . F9 F 0.5591(7) 0.2919(6) 0.4615(5) 0.171(5) Uani 1 1 d . . . O1W O 0.4252(4) 0.2191(3) 0.8391(3) 0.061(2) Uani 1 1 d . . . O2W O 0.6005(3) 0.2524(3) 0.8400(3) 0.0517(18) Uani 1 1 d . . . S4A S 0.77726(18) 0.20070(17) 0.92078(13) 0.0708(9) Uani 1 1 d . . . O14A O 0.7439(5) 0.2068(4) 0.9674(3) 0.091(3) Uani 1 1 d . . . O15A O 0.7344(4) 0.2031(4) 0.8711(3) 0.064(2) Uani 1 1 d . . . O16A O 0.8329(7) 0.1537(6) 0.9225(5) 0.152(6) Uani 1 1 d . . . C38A C 0.8327(12) 0.2656(10) 0.9185(7) 0.119(6) Uani 1 1 d . . . F10A F 0.7839(9) 0.3175(5) 0.9183(4) 0.166(5) Uani 1 1 d . . . F11A F 0.8764(6) 0.2734(6) 0.9625(4) 0.167(5) Uani 1 1 d . . . F12A F 0.8701(5) 0.2731(7) 0.8783(5) 0.166(5) Uani 1 1 d . . . O3W O 0.3330(7) 0.2734(7) 0.9013(7) 0.188(8) Uani 1 1 d . . . C1SA C 0.2247(6) 0.5095(5) 0.9517(5) 0.058(3) Uiso 1 1 d . . . H1SA H 0.249(5) 0.481(5) 0.984(4) 0.069 Uiso 1 1 d . . . Cl1A Cl 0.2784(2) 0.5087(3) 0.89937(17) 0.142(2) Uani 1 1 d . . . Cl2A Cl 0.13558(19) 0.49070(17) 0.93283(14) 0.0821(10) Uani 1 1 d . . . Cl3A Cl 0.2286(2) 0.58013(17) 0.9848(2) 0.1159(16) Uani 1 1 d . . . C2SA C 0.6988(7) 0.5004(9) 0.5611(6) 0.250 Uiso 0.50 1 d PD A 1 H2SA H 0.7229 0.5402 0.5561 0.300 Uiso 0.50 1 calc PR A 1 Cl6 Cl 0.7108(14) 0.4442(11) 0.5127(7) 0.404(17) Uani 0.50 1 d PDU A 1 C2SB C 0.6895(7) 0.4692(9) 0.5529(6) 0.250 Uiso 0.50 1 d PD A 2 H2SB H 0.6853 0.4304 0.5328 0.300 Uiso 0.50 1 calc PR A 2 Cl6A Cl 0.7540(8) 0.5185(12) 0.5285(6) 0.319(13) Uani 0.50 1 d PDU A 2 Cl4 Cl 0.7298(4) 0.4584(4) 0.6172(3) 0.237(4) Uani 1 1 d DU . . Cl5 Cl 0.6047(4) 0.5018(4) 0.5605(4) 0.242(4) Uani 1 1 d DU . . 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 Pd1 0.0209(3) 0.0223(3) 0.0362(4) -0.0005(3) 0.0039(3) 0.0002(3) Pd2 0.0204(3) 0.0193(3) 0.0365(4) -0.0003(3) 0.0010(3) 0.0011(3) Fe3 0.0362(7) 0.0277(7) 0.0424(8) -0.0041(6) 0.0059(6) 0.0047(6) Fe4 0.0322(7) 0.0276(7) 0.0381(8) 0.0032(5) 0.0001(6) 0.0002(6) Ca1 0.0295(9) 0.0287(10) 0.0391(11) -0.0014(8) 0.0011(8) -0.0035(8) P1 0.0248(11) 0.0237(12) 0.0354(13) -0.0002(9) 0.0063(9) -0.0014(9) P2 0.0227(11) 0.0219(12) 0.0392(14) 0.0011(9) 0.0034(9) -0.0021(9) P3 0.0238(11) 0.0213(12) 0.0362(13) -0.0008(9) 0.0018(9) -0.0005(9) P4 0.0283(12) 0.0222(12) 0.0359(13) 0.0020(9) -0.0014(10) 0.0013(9) O1 0.022(3) 0.030(3) 0.043(4) 0.004(3) 0.005(3) 0.004(3) O2 0.035(3) 0.028(3) 0.038(4) 0.000(3) 0.005(3) -0.004(3) O3 0.025(3) 0.023(3) 0.044(4) -0.001(3) 0.004(3) 0.004(3) O4 0.038(3) 0.032(4) 0.041(4) 0.001(3) -0.001(3) -0.005(3) N1 0.025(4) 0.020(4) 0.041(5) -0.005(3) -0.003(3) 0.004(3) N2 0.025(4) 0.020(4) 0.041(5) -0.003(3) 0.002(3) -0.003(3) C1 0.023(4) 0.017(4) 0.033(5) -0.004(3) 0.002(4) -0.001(3) C2 0.029(5) 0.017(4) 0.044(6) -0.006(4) 0.003(4) 0.000(4) C3 0.034(5) 0.041(6) 0.060(7) 0.000(5) -0.011(5) -0.003(5) C4 0.042(6) 0.060(7) 0.033(6) 0.000(5) -0.002(4) -0.005(5) C5 0.031(5) 0.048(6) 0.034(6) -0.005(4) 0.006(4) -0.005(4) C6 0.021(4) 0.023(5) 0.048(6) -0.002(4) 0.005(4) -0.005(4) C7 0.011(4) 0.021(4) 0.055(6) 0.003(4) 0.011(4) -0.003(4) C8 0.032(5) 0.011(4) 0.044(5) 0.009(3) -0.002(4) 0.006(4) C9 0.025(4) 0.019(4) 0.046(6) -0.004(4) 0.009(4) 0.001(4) C10 0.034(5) 0.058(7) 0.065(8) -0.004(6) 0.010(5) -0.010(5) C11 0.047(6) 0.095(9) 0.033(6) 0.006(6) 0.005(5) -0.020(6) C12 0.045(6) 0.055(6) 0.031(6) 0.008(4) 0.004(4) -0.002(5) C13 0.029(5) 0.019(5) 0.052(6) -0.002(4) 0.014(4) -0.003(4) C14 0.020(4) 0.026(5) 0.046(6) -0.005(4) -0.008(4) -0.002(4) C15 0.033(5) 0.018(4) 0.046(6) -0.002(4) 0.009(4) -0.009(4) C16 0.038(5) 0.020(5) 0.044(6) 0.007(4) 0.003(4) -0.001(4) C17 0.054(6) 0.031(6) 0.050(6) 0.016(4) 0.000(5) 0.001(5) C18 0.056(6) 0.043(6) 0.039(6) 0.006(4) 0.015(5) -0.001(5) C19 0.040(5) 0.028(5) 0.040(6) -0.004(4) 0.005(4) 0.007(4) C20 0.017(4) 0.023(4) 0.043(5) 0.006(4) 0.001(4) 0.000(4) C21 0.044(6) 0.037(6) 0.050(6) -0.003(4) -0.007(5) -0.009(5) C22 0.047(6) 0.055(7) 0.062(8) 0.022(6) -0.032(5) -0.022(5) C23 0.034(5) 0.044(6) 0.069(8) 0.008(5) 0.011(5) -0.005(5) C24 0.021(4) 0.044(6) 0.041(6) 0.003(4) 0.007(4) 0.004(4) C25 0.023(4) 0.029(5) 0.057(6) -0.006(4) 0.007(4) -0.003(4) C26 0.053(6) 0.028(5) 0.059(7) -0.005(4) 0.022(5) -0.003(5) C27 0.046(6) 0.047(7) 0.076(8) -0.014(6) 0.029(6) 0.000(5) C28 0.035(6) 0.043(6) 0.093(9) -0.004(6) 0.010(6) 0.007(5) C29 0.022(4) 0.041(6) 0.052(6) -0.003(4) -0.010(4) -0.001(4) C30 0.042(5) 0.023(5) 0.035(5) 0.001(4) -0.005(4) 0.004(4) C31 0.042(5) 0.027(5) 0.056(7) -0.005(4) 0.007(5) 0.007(4) C32 0.068(7) 0.029(5) 0.054(7) -0.011(5) 0.017(6) 0.001(5) C33 0.066(7) 0.049(6) 0.031(6) -0.010(5) -0.006(5) -0.004(6) C34 0.053(6) 0.025(5) 0.039(6) -0.002(4) -0.016(5) 0.000(4) C35 0.062(8) 0.081(10) 0.062(9) 0.019(7) 0.007(7) -0.009(7) C36 0.058(8) 0.091(11) 0.076(10) -0.030(8) -0.002(7) -0.011(7) C37 0.096(11) 0.084(11) 0.095(12) -0.014(9) 0.008(10) 0.008(10) C1A 0.029(5) 0.020(5) 0.044(6) -0.003(4) 0.009(4) 0.000(4) C2A 0.043(6) 0.059(7) 0.056(7) -0.010(5) 0.000(5) -0.026(5) C3A 0.066(8) 0.086(10) 0.065(8) -0.031(7) 0.021(7) -0.027(7) C4A 0.040(6) 0.049(7) 0.108(11) -0.016(7) 0.006(7) -0.013(5) C5A 0.048(6) 0.039(6) 0.087(9) 0.019(6) 0.008(6) -0.013(5) C6A 0.045(6) 0.027(5) 0.065(7) 0.010(5) 0.004(5) -0.005(5) C1B 0.029(4) 0.034(5) 0.033(5) 0.001(4) 0.003(4) -0.006(4) C2B 0.045(6) 0.033(5) 0.036(5) -0.004(4) -0.001(4) -0.009(4) C3B 0.051(6) 0.054(7) 0.043(6) -0.002(5) 0.015(5) -0.017(5) C4B 0.043(6) 0.085(9) 0.046(7) -0.025(6) 0.009(5) -0.001(6) C5B 0.044(6) 0.058(7) 0.041(6) -0.007(5) 0.000(5) 0.017(5) C6B 0.041(5) 0.041(6) 0.035(5) -0.001(4) -0.002(4) 0.013(5) C1C 0.026(4) 0.020(5) 0.053(6) -0.008(4) -0.001(4) 0.003(4) C2C 0.077(8) 0.032(6) 0.067(8) -0.003(5) 0.025(6) -0.016(6) C3C 0.111(11) 0.018(6) 0.094(10) -0.016(6) 0.024(8) -0.015(6) C4C 0.069(8) 0.033(7) 0.097(10) -0.031(6) 0.001(7) 0.005(6) C5C 0.048(6) 0.046(7) 0.058(7) -0.011(5) 0.004(5) -0.001(5) C6C 0.039(5) 0.028(5) 0.055(6) -0.005(4) 0.006(5) -0.011(4) C1D 0.032(5) 0.036(5) 0.040(6) -0.003(4) 0.005(4) -0.005(4) C2D 0.034(5) 0.069(7) 0.047(6) 0.012(5) 0.000(5) -0.012(5) C3D 0.051(7) 0.112(11) 0.068(9) 0.021(8) 0.012(6) -0.034(7) C4D 0.091(11) 0.144(15) 0.056(9) 0.030(9) 0.004(8) -0.039(10) C5D 0.070(9) 0.135(14) 0.071(9) 0.054(9) -0.009(7) -0.016(9) C6D 0.036(6) 0.064(7) 0.062(7) 0.019(6) 0.002(5) -0.011(5) C1E 0.027(4) 0.020(5) 0.052(6) 0.002(4) 0.009(4) -0.001(4) C2E 0.092(8) 0.032(6) 0.038(6) -0.003(4) -0.007(6) -0.014(6) C3E 0.118(11) 0.036(6) 0.052(8) -0.001(5) 0.004(7) 0.008(7) C4E 0.089(9) 0.039(7) 0.066(8) 0.018(6) 0.008(7) 0.011(6) C5E 0.072(8) 0.045(7) 0.051(7) 0.011(5) -0.012(6) 0.005(6) C6E 0.059(7) 0.031(6) 0.056(7) 0.011(5) -0.008(5) -0.006(5) C1F 0.027(5) 0.036(5) 0.041(6) -0.009(4) 0.000(4) 0.005(4) C2F 0.037(6) 0.092(9) 0.043(6) -0.021(6) 0.016(5) -0.033(6) C3F 0.058(8) 0.133(13) 0.084(10) -0.054(9) 0.021(7) -0.041(8) C4F 0.051(7) 0.091(9) 0.059(8) -0.035(7) -0.008(6) -0.001(7) C5F 0.053(6) 0.055(7) 0.042(6) -0.011(5) 0.012(5) -0.013(5) C6F 0.043(6) 0.031(5) 0.053(6) -0.013(4) 0.012(5) -0.005(4) C1G 0.034(5) 0.018(5) 0.067(7) -0.001(4) 0.005(5) -0.005(4) C2G 0.065(7) 0.047(7) 0.074(9) 0.005(6) 0.005(6) -0.016(6) C3G 0.084(10) 0.052(8) 0.122(13) 0.006(8) 0.027(9) -0.042(7) C4G 0.082(11) 0.061(10) 0.176(19) -0.035(11) 0.031(12) -0.049(8) C5G 0.052(8) 0.070(9) 0.121(13) -0.035(9) -0.007(8) -0.014(7) C6G 0.047(6) 0.038(6) 0.069(8) -0.014(5) -0.002(5) 0.004(5) C1H 0.033(5) 0.043(6) 0.036(5) 0.000(4) -0.004(4) 0.013(4) C2H 0.062(7) 0.040(6) 0.046(6) 0.011(5) -0.006(5) 0.016(5) C3H 0.113(12) 0.100(11) 0.078(10) -0.003(8) -0.016(9) 0.082(10) C4H 0.108(11) 0.166(16) 0.045(8) -0.025(9) -0.034(8) 0.079(12) C5H 0.078(9) 0.107(11) 0.043(7) -0.024(7) -0.026(6) 0.030(8) C6H 0.045(6) 0.059(7) 0.043(6) -0.007(5) -0.002(5) 0.016(5) S1 0.0472(15) 0.0349(14) 0.0556(17) 0.0065(12) 0.0027(12) -0.0094(12) O5 0.048(4) 0.029(4) 0.051(4) 0.009(3) 0.002(3) -0.002(3) O6 0.058(5) 0.051(5) 0.124(8) 0.017(5) 0.035(5) 0.001(4) O7 0.125(8) 0.042(5) 0.086(6) -0.009(4) 0.007(6) -0.036(5) F1 0.182(10) 0.139(8) 0.063(6) 0.010(5) -0.047(6) -0.045(7) F2 0.065(5) 0.145(8) 0.140(8) 0.067(6) 0.018(5) 0.032(5) F3 0.118(6) 0.098(6) 0.104(6) 0.068(5) 0.012(5) 0.007(5) S2 0.0472(16) 0.0416(16) 0.089(2) -0.0233(15) 0.0073(15) -0.0050(13) O8 0.050(4) 0.035(4) 0.070(5) -0.013(3) -0.001(4) -0.005(3) O9 0.067(6) 0.085(7) 0.139(9) -0.061(6) -0.045(6) 0.025(5) F4 0.181(10) 0.171(11) 0.090(7) -0.002(7) 0.063(7) -0.021(8) F5 0.062(5) 0.177(9) 0.099(6) -0.059(6) -0.010(4) 0.042(5) F6 0.087(6) 0.126(7) 0.146(8) -0.092(7) -0.011(5) 0.018(5) S3 0.075(2) 0.0595(19) 0.0476(17) -0.0010(13) 0.0166(15) -0.0076(16) O10 0.112(8) 0.053(6) 0.158(10) -0.001(6) 0.067(7) -0.026(5) O11 0.115(7) 0.083(6) 0.068(6) -0.005(5) 0.041(5) -0.008(6) O12 0.080(6) 0.111(7) 0.057(6) 0.023(5) 0.008(4) -0.003(5) O13 0.105(8) 0.097(8) 0.139(10) -0.017(7) 0.026(7) -0.050(6) F7 0.176(10) 0.065(6) 0.182(11) -0.010(6) -0.022(9) 0.002(7) F8 0.163(10) 0.160(10) 0.128(9) 0.035(7) -0.048(8) 0.048(8) F9 0.183(11) 0.168(11) 0.171(11) -0.033(8) 0.073(9) 0.073(9) O1W 0.056(5) 0.063(5) 0.068(5) 0.003(4) 0.025(4) -0.011(4) O2W 0.046(4) 0.048(4) 0.059(5) -0.002(3) -0.012(3) 0.001(3) S4A 0.066(2) 0.093(3) 0.0523(19) -0.0084(17) -0.0052(15) 0.0116(19) O14A 0.121(8) 0.094(7) 0.061(6) -0.001(5) 0.022(5) 0.018(6) O15A 0.055(5) 0.072(5) 0.062(5) -0.006(4) -0.021(4) 0.011(4) O16A 0.168(11) 0.164(11) 0.112(9) -0.036(8) -0.066(8) 0.124(10) C38A 0.150(17) 0.142(18) 0.061(11) 0.008(11) -0.023(11) -0.042(15) F10A 0.295(17) 0.083(7) 0.117(9) -0.011(6) -0.001(10) -0.025(9) F11A 0.172(10) 0.206(12) 0.109(8) -0.006(8) -0.073(7) -0.085(9) F12A 0.095(7) 0.289(16) 0.114(9) -0.012(9) 0.014(6) -0.077(9) O3W 0.121(10) 0.170(13) 0.288(19) -0.127(13) 0.119(11) -0.036(9) Cl1A 0.092(3) 0.254(7) 0.082(3) 0.027(3) 0.024(2) -0.003(4) Cl2A 0.080(2) 0.086(2) 0.079(2) -0.0019(18) -0.0013(18) -0.0172(19) Cl3A 0.094(3) 0.062(2) 0.180(5) -0.005(2) -0.061(3) 0.008(2) Cl6 0.56(4) 0.24(2) 0.43(3) -0.12(2) 0.18(3) 0.10(2) Cl6A 0.235(16) 0.52(3) 0.192(15) 0.164(18) -0.031(12) -0.202(19) Cl4 0.211(7) 0.257(9) 0.242(9) -0.027(7) 0.013(7) -0.010(7) Cl5 0.201(7) 0.200(7) 0.311(10) 0.073(7) -0.059(7) -0.069(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 Pd1 O1 2.083(6) . ? Pd1 N1 2.083(6) . ? Pd1 P1 2.260(2) . ? Pd1 P2 2.293(2) . ? Pd2 O3 2.086(5) . ? Pd2 N2 2.087(7) . ? Pd2 P4 2.259(2) . ? Pd2 P3 2.287(2) . ? Fe3 C30 2.001(9) . ? Fe3 C29 2.016(9) . ? Fe3 C25 2.020(9) . ? Fe3 C31 2.021(9) . ? Fe3 C34 2.038(9) . ? Fe3 C26 2.049(9) . ? Fe3 C28 2.060(10) . ? Fe3 C27 2.062(10) . ? Fe3 C32 2.063(9) . ? Fe3 C33 2.074(9) . ? Fe4 C15 2.013(8) . ? Fe4 C19 2.018(9) . ? Fe4 C24 2.018(9) . ? Fe4 C16 2.019(8) . ? Fe4 C20 2.026(8) . ? Fe4 C21 2.050(9) . ? Fe4 C18 2.052(9) . ? Fe4 C17 2.071(9) . ? Fe4 C22 2.076(9) . ? Fe4 C23 2.079(9) . ? Ca1 O2 2.337(6) . ? Ca1 O1W 2.338(7) . ? Ca1 O8 2.348(7) . ? Ca1 O2W 2.349(6) . ? Ca1 O4 2.355(6) . ? Ca1 O5 2.360(6) . ? P1 C15 1.801(9) . ? P1 C1B 1.811(9) . ? P1 C1A 1.831(8) . ? P2 C20 1.803(8) . ? P2 C1C 1.813(9) . ? P2 C1D 1.815(9) . ? P3 C25 1.793(9) . ? P3 C1E 1.816(9) . ? P3 C1F 1.819(9) . ? P4 C30 1.783(9) . ? P4 C1G 1.815(9) . ? P4 C1H 1.825(9) . ? O1 C14 1.265(10) . ? O2 C14 1.250(10) . ? O3 C7 1.274(10) . ? O4 C7 1.247(10) . ? N1 C5 1.333(11) . ? N1 C1 1.342(10) . ? N2 C8 1.322(10) . ? N2 C12 1.344(11) . ? C1 C2 1.394(11) . ? C2 C3 1.384(13) . ? C2 C6 1.494(11) . ? C3 C4 1.385(13) . ? C4 C5 1.370(12) . ? C6 C7 1.520(11) . ? C8 C9 1.372(11) . ? C9 C10 1.373(13) . ? C9 C13 1.515(12) . ? C10 C11 1.373(13) . ? C11 C12 1.376(13) . ? C13 C14 1.531(11) . ? C15 C16 1.424(12) . ? C15 C19 1.430(12) . ? C16 C17 1.394(13) . ? C17 C18 1.406(13) . ? C18 C19 1.386(13) . ? C20 C24 1.427(12) . ? C20 C21 1.435(12) . ? C21 C22 1.441(14) . ? C22 C23 1.412(15) . ? C23 C24 1.423(13) . ? C25 C26 1.436(13) . ? C25 C29 1.444(12) . ? C26 C27 1.405(13) . ? C27 C28 1.426(15) . ? C28 C29 1.407(14) . ? C30 C34 1.432(12) . ? C30 C31 1.459(12) . ? C31 C32 1.397(13) . ? C32 C33 1.402(14) . ? C33 C34 1.426(13) . ? C35 F1 1.287(15) . ? C35 F2 1.327(14) . ? C35 F3 1.342(13) . ? C35 S1 1.797(13) . ? C36 F4 1.289(16) . ? C36 F5 1.314(14) . ? C36 F6 1.325(14) . ? C36 S2 1.787(13) . ? C37 F8 1.305(17) . ? C37 F7 1.318(17) . ? C37 F9 1.331(17) . ? C37 S3 1.791(16) . ? C1A C6A 1.358(12) . ? C1A C2A 1.380(13) . ? C2A C3A 1.372(14) . ? C3A C4A 1.374(16) . ? C4A C5A 1.387(16) . ? C5A C6A 1.369(13) . ? C1B C2B 1.403(12) . ? C1B C6B 1.407(12) . ? C2B C3B 1.370(13) . ? C3B C4B 1.392(15) . ? C4B C5B 1.381(15) . ? C5B C6B 1.371(13) . ? C1C C2C 1.374(12) . ? C1C C6C 1.374(13) . ? C2C C3C 1.351(14) . ? C3C C4C 1.372(16) . ? C4C C5C 1.360(15) . ? C5C C6C 1.389(13) . ? C1D C2D 1.382(12) . ? C1D C6D 1.383(13) . ? C2D C3D 1.364(14) . ? C3D C4D 1.372(17) . ? C4D C5D 1.390(17) . ? C5D C6D 1.380(15) . ? C1E C6E 1.370(13) . ? C1E C2E 1.404(12) . ? C2E C3E 1.362(14) . ? C3E C4E 1.339(15) . ? C4E C5E 1.384(15) . ? C5E C6E 1.374(13) . ? C1F C6F 1.379(12) . ? C1F C2F 1.389(12) . ? C2F C3F 1.362(15) . ? C3F C4F 1.376(17) . ? C4F C5F 1.341(14) . ? C5F C6F 1.378(13) . ? C1G C2G 1.367(14) . ? C1G C6G 1.395(14) . ? C2G C3G 1.418(15) . ? C3G C4G 1.36(2) . ? C4G C5G 1.37(2) . ? C5G C6G 1.415(16) . ? C1H C6H 1.370(13) . ? C1H C2H 1.390(12) . ? C2H C3H 1.373(15) . ? C3H C4H 1.364(19) . ? C4H C5H 1.388(18) . ? C5H C6H 1.380(14) . ? S1 O6 1.420(8) . ? S1 O7 1.421(8) . ? S1 O5 1.450(6) . ? S2 O9 1.425(9) . ? S2 O10 1.437(9) . ? S2 O8 1.458(7) . ? S3 O13 1.424(9) . ? S3 O11 1.428(8) . ? S3 O12 1.429(9) . ? S4A O14A 1.380(9) . ? S4A O15A 1.434(7) . ? S4A O16A 1.451(9) . ? S4A C38A 1.753(19) . ? C38A F12A 1.286(19) . ? C38A F11A 1.334(17) . ? C38A F10A 1.45(2) . ? C1SA Cl1A 1.717(12) . ? C1SA Cl2A 1.729(12) . ? C1SA Cl3A 1.756(12) . ? C2SA Cl5 1.739(10) . ? C2SA Cl4 1.752(10) . ? C2SA Cl6 1.761(10) . ? C2SB Cl5 1.745(10) . ? C2SB Cl6A 1.754(10) . ? C2SB Cl4 1.755(10) . ? 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 O1 Pd1 N1 86.6(2) . . ? O1 Pd1 P1 177.75(16) . . ? N1 Pd1 P1 91.24(19) . . ? O1 Pd1 P2 84.65(16) . . ? N1 Pd1 P2 169.0(2) . . ? P1 Pd1 P2 97.57(8) . . ? O3 Pd2 N2 86.8(2) . . ? O3 Pd2 P4 177.70(17) . . ? N2 Pd2 P4 91.00(19) . . ? O3 Pd2 P3 83.58(16) . . ? N2 Pd2 P3 168.10(19) . . ? P4 Pd2 P3 98.58(8) . . ? C30 Fe3 C29 107.6(4) . . ? C30 Fe3 C25 110.4(3) . . ? C29 Fe3 C25 41.9(4) . . ? C30 Fe3 C31 42.5(3) . . ? C29 Fe3 C31 110.7(4) . . ? C25 Fe3 C31 141.5(4) . . ? C30 Fe3 C34 41.5(3) . . ? C29 Fe3 C34 136.4(4) . . ? C25 Fe3 C34 110.0(4) . . ? C31 Fe3 C34 69.4(4) . . ? C30 Fe3 C26 142.1(4) . . ? C29 Fe3 C26 69.3(4) . . ? C25 Fe3 C26 41.3(4) . . ? C31 Fe3 C26 175.4(4) . . ? C34 Fe3 C26 114.0(4) . . ? C30 Fe3 C28 134.6(4) . . ? C29 Fe3 C28 40.4(4) . . ? C25 Fe3 C28 69.1(4) . . ? C31 Fe3 C28 108.6(4) . . ? C34 Fe3 C28 175.9(4) . . ? C26 Fe3 C28 68.2(4) . . ? C30 Fe3 C27 175.1(4) . . ? C29 Fe3 C27 68.3(4) . . ? C25 Fe3 C27 68.5(4) . . ? C31 Fe3 C27 135.5(4) . . ? C34 Fe3 C27 143.4(4) . . ? C26 Fe3 C27 40.0(4) . . ? C28 Fe3 C27 40.5(4) . . ? C30 Fe3 C32 69.1(4) . . ? C29 Fe3 C32 141.1(4) . . ? C25 Fe3 C32 177.0(4) . . ? C31 Fe3 C32 40.0(4) . . ? C34 Fe3 C32 67.6(4) . . ? C26 Fe3 C32 137.5(4) . . ? C28 Fe3 C32 113.5(4) . . ? C27 Fe3 C32 112.2(4) . . ? C30 Fe3 C33 69.5(4) . . ? C29 Fe3 C33 176.8(4) . . ? C25 Fe3 C33 137.4(4) . . ? C31 Fe3 C33 68.1(4) . . ? C34 Fe3 C33 40.6(4) . . ? C26 Fe3 C33 112.2(4) . . ? C28 Fe3 C33 142.6(4) . . ? C27 Fe3 C33 114.7(4) . . ? C32 Fe3 C33 39.6(4) . . ? C15 Fe4 C19 41.5(3) . . ? C15 Fe4 C24 108.3(4) . . ? C19 Fe4 C24 137.2(4) . . ? C15 Fe4 C16 41.4(3) . . ? C19 Fe4 C16 68.7(4) . . ? C24 Fe4 C16 110.7(4) . . ? C15 Fe4 C20 110.9(3) . . ? C19 Fe4 C20 110.9(3) . . ? C24 Fe4 C20 41.3(3) . . ? C16 Fe4 C20 140.5(4) . . ? C15 Fe4 C21 141.2(4) . . ? C19 Fe4 C21 113.0(4) . . ? C24 Fe4 C21 69.5(4) . . ? C16 Fe4 C21 177.4(4) . . ? C20 Fe4 C21 41.2(4) . . ? C15 Fe4 C18 68.2(4) . . ? C19 Fe4 C18 39.8(4) . . ? C24 Fe4 C18 176.5(4) . . ? C16 Fe4 C18 67.2(4) . . ? C20 Fe4 C18 138.7(4) . . ? C21 Fe4 C18 112.7(4) . . ? C15 Fe4 C17 68.5(4) . . ? C19 Fe4 C17 67.7(4) . . ? C24 Fe4 C17 140.0(4) . . ? C16 Fe4 C17 39.8(4) . . ? C20 Fe4 C17 178.5(4) . . ? C21 Fe4 C17 138.5(4) . . ? C18 Fe4 C17 39.9(4) . . ? C15 Fe4 C22 175.9(4) . . ? C19 Fe4 C22 142.6(4) . . ? C24 Fe4 C22 68.5(4) . . ? C16 Fe4 C22 136.6(4) . . ? C20 Fe4 C22 68.6(4) . . ? C21 Fe4 C22 40.9(4) . . ? C18 Fe4 C22 115.0(4) . . ? C17 Fe4 C22 112.1(4) . . ? C15 Fe4 C23 136.1(4) . . ? C19 Fe4 C23 177.4(4) . . ? C24 Fe4 C23 40.6(4) . . ? C16 Fe4 C23 110.3(4) . . ? C20 Fe4 C23 68.2(4) . . ? C21 Fe4 C23 68.1(4) . . ? C18 Fe4 C23 142.4(4) . . ? C17 Fe4 C23 113.2(4) . . ? C22 Fe4 C23 39.7(4) . . ? O2 Ca1 O1W 178.4(3) . . ? O2 Ca1 O8 93.6(2) . . ? O1W Ca1 O8 87.2(3) . . ? O2 Ca1 O2W 91.3(2) . . ? O1W Ca1 O2W 90.2(3) . . ? O8 Ca1 O2W 82.6(2) . . ? O2 Ca1 O4 90.6(2) . . ? O1W Ca1 O4 87.9(2) . . ? O8 Ca1 O4 98.6(2) . . ? O2W Ca1 O4 177.7(2) . . ? O2 Ca1 O5 95.4(2) . . ? O1W Ca1 O5 84.1(2) . . ? O8 Ca1 O5 164.7(2) . . ? O2W Ca1 O5 84.9(2) . . ? O4 Ca1 O5 93.6(2) . . ? C15 P1 C1B 109.5(4) . . ? C15 P1 C1A 104.8(4) . . ? C1B P1 C1A 104.2(4) . . ? C15 P1 Pd1 110.7(3) . . ? C1B P1 Pd1 114.2(3) . . ? C1A P1 Pd1 112.9(3) . . ? C20 P2 C1C 103.2(4) . . ? C20 P2 C1D 104.0(4) . . ? C1C P2 C1D 106.3(4) . . ? C20 P2 Pd1 123.9(3) . . ? C1C P2 Pd1 109.4(3) . . ? C1D P2 Pd1 108.7(3) . . ? C25 P3 C1E 104.0(4) . . ? C25 P3 C1F 103.6(4) . . ? C1E P3 C1F 106.8(4) . . ? C25 P3 Pd2 124.0(3) . . ? C1E P3 Pd2 109.6(3) . . ? C1F P3 Pd2 107.5(3) . . ? C30 P4 C1G 105.1(4) . . ? C30 P4 C1H 110.0(4) . . ? C1G P4 C1H 104.0(4) . . ? C30 P4 Pd2 112.6(3) . . ? C1G P4 Pd2 111.0(3) . . ? C1H P4 Pd2 113.6(3) . . ? C14 O1 Pd1 119.0(5) . . ? C14 O2 Ca1 153.1(6) . . ? C7 O3 Pd2 118.6(5) . . ? C7 O4 Ca1 150.4(6) . . ? C5 N1 C1 119.6(7) . . ? C5 N1 Pd1 117.5(6) . . ? C1 N1 Pd1 122.2(6) . . ? C8 N2 C12 117.5(7) . . ? C8 N2 Pd2 123.6(6) . . ? C12 N2 Pd2 118.3(6) . . ? N1 C1 C2 122.2(8) . . ? C3 C2 C1 117.0(8) . . ? C3 C2 C6 122.7(8) . . ? C1 C2 C6 120.2(8) . . ? C2 C3 C4 120.5(8) . . ? C5 C4 C3 118.7(9) . . ? N1 C5 C4 121.9(8) . . ? C2 C6 C7 107.0(6) . . ? O4 C7 O3 126.9(8) . . ? O4 C7 C6 119.9(7) . . ? O3 C7 C6 113.2(7) . . ? N2 C8 C9 124.5(8) . . ? C8 C9 C10 117.5(8) . . ? C8 C9 C13 119.4(8) . . ? C10 C9 C13 122.8(8) . . ? C11 C10 C9 119.3(9) . . ? C10 C11 C12 119.4(10) . . ? N2 C12 C11 121.8(9) . . ? C9 C13 C14 106.7(7) . . ? O2 C14 O1 126.5(8) . . ? O2 C14 C13 119.2(8) . . ? O1 C14 C13 114.3(8) . . ? C16 C15 C19 105.9(8) . . ? C16 C15 P1 131.3(7) . . ? C19 C15 P1 122.6(7) . . ? C16 C15 Fe4 69.5(5) . . ? C19 C15 Fe4 69.4(5) . . ? P1 C15 Fe4 121.3(4) . . ? C17 C16 C15 109.3(8) . . ? C17 C16 Fe4 72.1(5) . . ? C15 C16 Fe4 69.1(5) . . ? C16 C17 C18 107.2(8) . . ? C16 C17 Fe4 68.1(5) . . ? C18 C17 Fe4 69.3(5) . . ? C19 C18 C17 109.4(9) . . ? C19 C18 Fe4 68.8(5) . . ? C17 C18 Fe4 70.8(5) . . ? C18 C19 C15 108.2(8) . . ? C18 C19 Fe4 71.4(5) . . ? C15 C19 Fe4 69.1(5) . . ? C24 C20 C21 108.2(7) . . ? C24 C20 P2 125.5(7) . . ? C21 C20 P2 125.8(7) . . ? C24 C20 Fe4 69.0(5) . . ? C21 C20 Fe4 70.3(5) . . ? P2 C20 Fe4 120.7(4) . . ? C20 C21 C22 107.0(9) . . ? C20 C21 Fe4 68.5(5) . . ? C22 C21 Fe4 70.5(5) . . ? C23 C22 C21 108.2(9) . . ? C23 C22 Fe4 70.3(5) . . ? C21 C22 Fe4 68.6(5) . . ? C22 C23 C24 108.7(9) . . ? C22 C23 Fe4 70.0(6) . . ? C24 C23 Fe4 67.4(5) . . ? C23 C24 C20 107.8(8) . . ? C23 C24 Fe4 72.0(5) . . ? C20 C24 Fe4 69.6(5) . . ? C26 C25 C29 106.8(8) . . ? C26 C25 P3 128.7(7) . . ? C29 C25 P3 124.3(7) . . ? C26 C25 Fe3 70.4(5) . . ? C29 C25 Fe3 68.9(5) . . ? P3 C25 Fe3 121.5(4) . . ? C27 C26 C25 108.1(9) . . ? C27 C26 Fe3 70.5(6) . . ? C25 C26 Fe3 68.3(5) . . ? C26 C27 C28 109.0(9) . . ? C26 C27 Fe3 69.5(5) . . ? C28 C27 Fe3 69.7(6) . . ? C29 C28 C27 107.8(9) . . ? C29 C28 Fe3 68.1(5) . . ? C27 C28 Fe3 69.8(6) . . ? C28 C29 C25 108.4(9) . . ? C28 C29 Fe3 71.5(6) . . ? C25 C29 Fe3 69.2(5) . . ? C34 C30 C31 106.1(8) . . ? C34 C30 P4 123.1(7) . . ? C31 C30 P4 130.7(7) . . ? C34 C30 Fe3 70.6(5) . . ? C31 C30 Fe3 69.5(5) . . ? P4 C30 Fe3 122.3(5) . . ? C32 C31 C30 107.7(8) . . ? C32 C31 Fe3 71.6(6) . . ? C30 C31 Fe3 68.0(5) . . ? C31 C32 C33 110.1(9) . . ? C31 C32 Fe3 68.4(5) . . ? C33 C32 Fe3 70.6(5) . . ? C32 C33 C34 107.5(9) . . ? C32 C33 Fe3 69.7(6) . . ? C34 C33 Fe3 68.3(5) . . ? C33 C34 C30 108.7(8) . . ? C33 C34 Fe3 71.1(6) . . ? C30 C34 Fe3 67.9(5) . . ? F1 C35 F2 108.2(12) . . ? F1 C35 F3 107.0(11) . . ? F2 C35 F3 108.0(11) . . ? F1 C35 S1 112.1(10) . . ? F2 C35 S1 110.7(9) . . ? F3 C35 S1 110.7(9) . . ? F4 C36 F5 107.3(12) . . ? F4 C36 F6 103.8(12) . . ? F5 C36 F6 108.7(12) . . ? F4 C36 S2 111.8(11) . . ? F5 C36 S2 112.0(10) . . ? F6 C36 S2 112.8(9) . . ? F8 C37 F7 107.1(15) . . ? F8 C37 F9 108.5(15) . . ? F7 C37 F9 106.9(14) . . ? F8 C37 S3 113.1(12) . . ? F7 C37 S3 111.0(11) . . ? F9 C37 S3 110.0(12) . . ? C6A C1A C2A 119.1(9) . . ? C6A C1A P1 121.3(7) . . ? C2A C1A P1 119.5(7) . . ? C3A C2A C1A 119.9(10) . . ? C2A C3A C4A 121.3(11) . . ? C3A C4A C5A 118.1(10) . . ? C6A C5A C4A 120.3(11) . . ? C1A C6A C5A 121.3(10) . . ? C2B C1B C6B 118.6(8) . . ? C2B C1B P1 119.6(7) . . ? C6B C1B P1 121.8(7) . . ? C3B C2B C1B 120.2(9) . . ? C2B C3B C4B 120.3(10) . . ? C5B C4B C3B 120.3(9) . . ? C6B C5B C4B 119.9(10) . . ? C5B C6B C1B 120.7(9) . . ? C2C C1C C6C 118.3(8) . . ? C2C C1C P2 121.7(8) . . ? C6C C1C P2 119.9(7) . . ? C3C C2C C1C 120.5(11) . . ? C2C C3C C4C 122.2(11) . . ? C5C C4C C3C 117.9(10) . . ? C4C C5C C6C 120.8(11) . . ? C1C C6C C5C 120.3(9) . . ? C2D C1D C6D 119.1(9) . . ? C2D C1D P2 120.8(7) . . ? C6D C1D P2 120.1(7) . . ? C3D C2D C1D 119.8(10) . . ? C2D C3D C4D 122.9(11) . . ? C3D C4D C5D 116.7(12) . . ? C6D C5D C4D 121.8(12) . . ? C5D C6D C1D 119.7(10) . . ? C6E C1E C2E 117.3(8) . . ? C6E C1E P3 121.2(7) . . ? C2E C1E P3 121.4(7) . . ? C3E C2E C1E 120.4(10) . . ? C4E C3E C2E 120.5(11) . . ? C3E C4E C5E 121.5(10) . . ? C6E C5E C4E 117.7(11) . . ? C1E C6E C5E 122.4(10) . . ? C6F C1F C2F 117.9(8) . . ? C6F C1F P3 122.5(7) . . ? C2F C1F P3 119.6(7) . . ? C3F C2F C1F 121.0(10) . . ? C2F C3F C4F 119.1(11) . . ? C5F C4F C3F 121.3(10) . . ? C4F C5F C6F 119.6(10) . . ? C5F C6F C1F 120.9(9) . . ? C2G C1G C6G 118.9(9) . . ? C2G C1G P4 122.1(8) . . ? C6G C1G P4 118.9(8) . . ? C1G C2G C3G 120.7(12) . . ? C4G C3G C2G 119.3(14) . . ? C3G C4G C5G 122.0(13) . . ? C4G C5G C6G 118.4(13) . . ? C1G C6G C5G 120.7(12) . . ? C6H C1H C2H 120.4(9) . . ? C6H C1H P4 117.8(7) . . ? C2H C1H P4 121.8(7) . . ? C3H C2H C1H 118.0(11) . . ? C4H C3H C2H 122.6(12) . . ? C3H C4H C5H 119.0(11) . . ? C6H C5H C4H 119.5(11) . . ? C1H C6H C5H 120.6(10) . . ? O6 S1 O7 115.6(5) . . ? O6 S1 O5 115.0(4) . . ? O7 S1 O5 114.4(5) . . ? O6 S1 C35 103.9(6) . . ? O7 S1 C35 103.3(6) . . ? O5 S1 C35 102.3(5) . . ? S1 O5 Ca1 139.4(4) . . ? O9 S2 O10 116.8(6) . . ? O9 S2 O8 114.1(5) . . ? O10 S2 O8 113.9(6) . . ? O9 S2 C36 104.1(6) . . ? O10 S2 C36 102.6(7) . . ? O8 S2 C36 102.9(5) . . ? S2 O8 Ca1 140.7(4) . . ? O13 S3 O11 115.9(6) . . ? O13 S3 O12 116.6(6) . . ? O11 S3 O12 113.2(6) . . ? O13 S3 C37 103.5(8) . . ? O11 S3 C37 101.4(7) . . ? O12 S3 C37 103.4(7) . . ? O14A S4A O15A 119.6(6) . . ? O14A S4A O16A 113.9(7) . . ? O15A S4A O16A 113.2(6) . . ? O14A S4A C38A 104.5(8) . . ? O15A S4A C38A 103.1(7) . . ? O16A S4A C38A 99.1(11) . . ? F12A C38A F11A 108.6(17) . . ? F12A C38A F10A 105.6(16) . . ? F11A C38A F10A 103.8(17) . . ? F12A C38A S4A 118.7(15) . . ? F11A C38A S4A 113.2(13) . . ? F10A C38A S4A 105.5(14) . . ? Cl1A C1SA Cl2A 112.3(7) . . ? Cl1A C1SA Cl3A 112.0(7) . . ? Cl2A C1SA Cl3A 110.1(6) . . ? Cl5 C2SA Cl4 106.2(9) . . ? Cl5 C2SA Cl6 100.8(10) . . ? Cl4 C2SA Cl6 98.6(10) . . ? Cl5 C2SB Cl6A 115.4(12) . . ? Cl5 C2SB Cl4 105.8(9) . . ? Cl6A C2SB Cl4 99.2(9) . . ? C2SA Cl4 C2SB 24.0(9) . . ? C2SA Cl5 C2SB 24.2(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.350 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.132 # Attachment 'complex8_new.cif' data_8167a _database_code_depnum_ccdc_archive 'CCDC 711716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Cl4 F3 Fe N O5 P2 Pt S' _chemical_formula_weight 1204.49 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.4057(9) _cell_length_b 39.184(3) _cell_length_c 9.2855(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.127(2) _cell_angle_gamma 90.00 _cell_volume 5159.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5880 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.74 _exptl_crystal_description PLATE _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 3.351 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3197 _exptl_absorpt_correction_T_max 0.5095 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29771 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9044 _reflns_number_gt 7036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The Otf and CHCl3 are badly disordered. A model was assigned in which the otf and the CHCl3 are disordered into two sets (50:50). Instructions PART -1 and PART -2 were used because one of the otf was located near a symmetry point. Restraints in bond length and thermal parameters were applied to the otf and CHCl3. Attempt to solve the structure in lower symmetry space group did not resolve the disorder. There also some solvent residual peaks within voids of the crystal. But the peak heights were too low to fit the known solvents. ; _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^)+(0.1192P)^2^+42.3437P] 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 9044 _refine_ls_number_parameters 635 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2332 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 0.57254(4) 0.377237(10) 0.87613(5) 0.0395(2) Uani 1 1 d . . . Cl1 Cl 0.5734(3) 0.35440(7) 1.1088(3) 0.0506(8) Uani 1 1 d . . . P1 P 0.5894(3) 0.40090(7) 0.6614(3) 0.0405(7) Uani 1 1 d . . . P2 P 0.5035(3) 0.32778(7) 0.7864(3) 0.0410(7) Uani 1 1 d . . . Fe1 Fe 0.40827(14) 0.36194(4) 0.45731(18) 0.0441(4) Uani 1 1 d . . . N1 N 0.6275(9) 0.4201(3) 0.9914(11) 0.053(3) Uani 1 1 d . . . O1 O 0.6405(11) 0.5566(4) 1.1203(19) 0.115(6) Uani 1 1 d . . . O2 O 0.7597(11) 0.5712(3) 1.0188(16) 0.092(4) Uani 1 1 d . . . H2O H 0.8078 0.5616 1.0012 0.138 Uiso 1 1 calc R . . C1 C 0.5706(13) 0.4444(3) 1.0261(16) 0.066(4) Uani 1 1 d . . . H1 H 0.5058 0.4436 0.9871 0.079 Uiso 1 1 calc R . . C2 C 0.606(2) 0.4711(5) 1.120(2) 0.103(8) Uani 1 1 d . . . H2 H 0.5642 0.4880 1.1414 0.124 Uiso 1 1 calc R . . C3 C 0.699(2) 0.4735(5) 1.1810(19) 0.104(9) Uani 1 1 d . . . C4 C 0.7572(19) 0.4488(6) 1.143(2) 0.100(8) Uani 1 1 d . . . H4 H 0.8224 0.4497 1.1787 0.120 Uiso 1 1 calc R . . C5 C 0.7179(14) 0.4214(5) 1.0478(18) 0.081(5) Uani 1 1 d . . . H5 H 0.7579 0.4040 1.0254 0.098 Uiso 1 1 calc R . . C6 C 0.737(2) 0.5028(5) 1.281(2) 0.140(12) Uani 1 1 d . . . H6A H 0.6842 0.5143 1.3157 0.168 Uiso 1 1 calc R . . H6B H 0.7796 0.4940 1.3668 0.168 Uiso 1 1 calc R . . C7 C 0.7881(19) 0.5279(5) 1.200(3) 0.148(13) Uani 1 1 d . . . H7A H 0.8339 0.5406 1.2712 0.178 Uiso 1 1 calc R . . H7B H 0.8230 0.5154 1.1357 0.178 Uiso 1 1 calc R . . C8 C 0.7220(18) 0.5526(4) 1.111(2) 0.085(6) Uani 1 1 d . . . C9 C 0.4812(11) 0.4032(3) 0.5261(13) 0.048(3) Uani 1 1 d . . . C10 C 0.4745(11) 0.4008(3) 0.3702(13) 0.049(3) Uani 1 1 d . . . H10 H 0.5270 0.3989 0.3148 0.059 Uiso 1 1 calc R . . C11 C 0.3787(11) 0.4018(3) 0.3137(15) 0.056(4) Uani 1 1 d . . . H11 H 0.3502 0.3998 0.2090 0.067 Uiso 1 1 calc R . . C12 C 0.3276(12) 0.4052(4) 0.4321(18) 0.068(4) Uani 1 1 d . . . H12 H 0.2581 0.4061 0.4231 0.081 Uiso 1 1 calc R . . C13 C 0.3918(11) 0.4068(3) 0.5606(14) 0.052(3) Uani 1 1 d . . . H13 H 0.3768 0.4093 0.6601 0.062 Uiso 1 1 calc R . . C14 C 0.4456(9) 0.3238(3) 0.5984(12) 0.041(3) Uani 1 1 d . . . C15 C 0.3462(10) 0.3222(3) 0.5476(14) 0.049(3) Uani 1 1 d . . . H15 H 0.2968 0.3241 0.6090 0.059 Uiso 1 1 calc R . . C16 C 0.3305(11) 0.3182(3) 0.3933(14) 0.052(3) Uani 1 1 d . . . H16 H 0.2679 0.3177 0.3289 0.062 Uiso 1 1 calc R . . C17 C 0.4173(11) 0.3166(3) 0.3456(15) 0.055(4) Uani 1 1 d . . . H17 H 0.4261 0.3145 0.2426 0.066 Uiso 1 1 calc R . . C18 C 0.4916(11) 0.3198(3) 0.4706(12) 0.046(3) Uani 1 1 d . . . H18 H 0.5603 0.3193 0.4704 0.056 Uiso 1 1 calc R . . C1A C 0.6804(9) 0.3797(3) 0.5808(14) 0.044(3) Uani 1 1 d . . . C2A C 0.7079(11) 0.3922(4) 0.4545(15) 0.058(4) Uani 1 1 d . . . H2A H 0.6774 0.4112 0.4057 0.070 Uiso 1 1 calc R . . C3A C 0.7815(13) 0.3761(5) 0.4013(16) 0.080(5) Uani 1 1 d . . . H3A H 0.8011 0.3846 0.3168 0.096 Uiso 1 1 calc R . . C4A C 0.8243(11) 0.3490(4) 0.4687(18) 0.067(4) Uani 1 1 d . . . H4A H 0.8730 0.3384 0.4300 0.081 Uiso 1 1 calc R . . C5A C 0.7987(12) 0.3362(4) 0.5935(19) 0.074(5) Uani 1 1 d . . . H5A H 0.8304 0.3173 0.6417 0.089 Uiso 1 1 calc R . . C6A C 0.7253(11) 0.3516(4) 0.6470(16) 0.059(4) Uani 1 1 d . . . H6A1 H 0.7059 0.3426 0.7307 0.071 Uiso 1 1 calc R . . C1B C 0.6325(11) 0.4445(3) 0.6807(13) 0.050(3) Uani 1 1 d . . . C2B C 0.7271(12) 0.4510(4) 0.7293(18) 0.070(4) Uani 1 1 d . . . H2B H 0.7692 0.4325 0.7482 0.083 Uiso 1 1 calc R . . C3B C 0.7617(15) 0.4841(4) 0.751(2) 0.089(6) Uani 1 1 d . . . H3B H 0.8264 0.4881 0.7826 0.107 Uiso 1 1 calc R . . C4B C 0.6998(16) 0.5106(4) 0.7252(19) 0.085(6) Uani 1 1 d . . . H4B H 0.7223 0.5331 0.7389 0.102 Uiso 1 1 calc R . . C5B C 0.6080(16) 0.5053(4) 0.681(2) 0.081(5) Uani 1 1 d . . . H5B H 0.5674 0.5242 0.6640 0.097 Uiso 1 1 calc R . . C6B C 0.5697(13) 0.4722(3) 0.6593(16) 0.067(4) Uani 1 1 d . . . H6B1 H 0.5044 0.4687 0.6313 0.081 Uiso 1 1 calc R . . C1C C 0.4046(10) 0.3184(3) 0.8788(12) 0.045(3) Uani 1 1 d . . . C2C C 0.3839(11) 0.2848(3) 0.9184(14) 0.051(3) Uani 1 1 d . . . H2C H 0.4232 0.2668 0.9006 0.062 Uiso 1 1 calc R . . C3C C 0.3094(12) 0.2786(4) 0.9805(17) 0.064(4) Uani 1 1 d . . . H3C H 0.2954 0.2560 1.0035 0.077 Uiso 1 1 calc R . . C4C C 0.2525(11) 0.3047(4) 1.0114(16) 0.064(4) Uani 1 1 d . . . H4C H 0.2004 0.3001 1.0565 0.077 Uiso 1 1 calc R . . C5C C 0.2721(10) 0.3384(4) 0.9759(15) 0.057(4) Uani 1 1 d . . . H5C H 0.2326 0.3564 0.9941 0.069 Uiso 1 1 calc R . . C6C C 0.3484(10) 0.3444(3) 0.9153(14) 0.051(3) Uani 1 1 d . . . H6C H 0.3641 0.3671 0.8970 0.061 Uiso 1 1 calc R . . C1D C 0.5817(10) 0.2911(3) 0.8097(13) 0.045(3) Uani 1 1 d . . . C2D C 0.5586(11) 0.2614(3) 0.7296(15) 0.055(4) Uani 1 1 d . . . H2D H 0.5021 0.2606 0.6613 0.066 Uiso 1 1 calc R . . C3D C 0.6137(14) 0.2341(3) 0.7466(18) 0.068(4) Uani 1 1 d . . . H3D H 0.5945 0.2139 0.6954 0.081 Uiso 1 1 calc R . . C4D C 0.6995(16) 0.2355(4) 0.840(2) 0.082(6) Uani 1 1 d . . . H4D H 0.7407 0.2167 0.8490 0.098 Uiso 1 1 calc R . . C5D C 0.7235(12) 0.2648(4) 0.919(2) 0.074(5) Uani 1 1 d . . . H5D H 0.7817 0.2656 0.9838 0.089 Uiso 1 1 calc R . . C6D C 0.6671(10) 0.2923(3) 0.9085(14) 0.052(3) Uani 1 1 d . . . H6D H 0.6844 0.3118 0.9657 0.062 Uiso 1 1 calc R . . C3S C 0.033(2) 0.4130(10) 0.545(5) 0.115(15) Uiso 0.50 1 d PD A -1 H3S H -0.0048 0.3977 0.4721 0.138 Uiso 0.50 1 calc PR A -1 Cl2 Cl 0.1291(15) 0.3892(4) 0.6331(16) 0.158(7) Uani 0.50 1 d PD A -1 Cl3 Cl 0.067(2) 0.4477(7) 0.449(2) 0.211(12) Uani 0.50 1 d PD A -1 Cl4 Cl -0.0411(12) 0.4277(8) 0.652(3) 0.271(17) Uani 0.50 1 d P A -1 S1 S 0.0066(8) 0.3701(3) 0.1520(14) 0.105(4) Uani 0.50 1 d PD B -1 O3 O 0.016(3) 0.3572(10) 0.297(2) 0.168(16) Uani 0.50 1 d PDU B -1 O4 O 0.0917(16) 0.3719(9) 0.105(4) 0.178(18) Uani 0.50 1 d PDU B -1 O5 O -0.036(2) 0.4032(6) 0.152(4) 0.177(17) Uani 0.50 1 d PDU B -1 C1S C -0.076(2) 0.3444(8) 0.037(3) 0.150 Uiso 0.50 1 d PD B -1 F1 F -0.043(4) 0.3145(8) 0.028(7) 0.38(3) Uani 0.50 1 d PDU B -1 F2 F -0.097(4) 0.3590(15) -0.088(4) 0.38(3) Uani 0.50 1 d PDU B -1 F3 F -0.152(3) 0.343(2) 0.095(7) 0.38(3) Uani 0.50 1 d PDU B -1 S2 S 0.0165(10) 0.4532(4) 0.1023(17) 0.151(7) Uani 0.50 1 d PD C -2 O6 O 0.0910(18) 0.4357(8) 0.058(3) 0.173(16) Uani 0.50 1 d PDU C -2 O7 O -0.0704(18) 0.4408(10) 0.026(3) 0.25(3) Uani 0.50 1 d PDU C -2 O8 O 0.025(2) 0.4885(5) 0.066(3) 0.159(15) Uani 0.50 1 d PDU C -2 C2S C 0.0199(18) 0.4495(7) 0.292(2) 0.130(18) Uiso 0.50 1 d PD C -2 F4 F 0.1030(18) 0.4558(11) 0.363(3) 0.190(19) Uani 0.50 1 d PDU C -2 F5 F -0.004(3) 0.4188(7) 0.324(3) 0.207(17) Uani 0.50 1 d PDU C -2 F6 F -0.038(2) 0.4709(9) 0.336(3) 0.199(16) Uani 0.50 1 d PDU C -2 C4S C -0.0275(14) 0.3554(8) 0.048(2) 0.093(12) Uiso 0.50 1 d PD D -2 H4S H -0.0248 0.3803 0.0324 0.112 Uiso 0.50 1 calc PR D -2 Cl5 Cl 0.0066(11) 0.3346(6) -0.0961(17) 0.162(7) Uani 0.50 1 d PD D -2 Cl6 Cl -0.1422(8) 0.3437(4) 0.0595(19) 0.123(5) Uani 0.50 1 d PD D -2 Cl7 Cl 0.0548(16) 0.3439(6) 0.208(2) 0.187(10) Uani 0.50 1 d PD D -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 0.0710(4) 0.0218(3) 0.0271(3) -0.00148(16) 0.0123(2) -0.0010(2) Cl1 0.094(2) 0.0307(14) 0.0288(14) -0.0002(11) 0.0163(15) -0.0045(14) P1 0.069(2) 0.0237(14) 0.0296(15) 0.0007(11) 0.0119(14) -0.0048(13) P2 0.072(2) 0.0192(13) 0.0340(15) -0.0016(11) 0.0164(14) 0.0015(13) Fe1 0.0679(12) 0.0283(9) 0.0351(9) -0.0015(7) 0.0062(8) -0.0001(8) N1 0.092(9) 0.031(6) 0.034(5) 0.003(4) 0.005(6) -0.010(5) O1 0.093(10) 0.115(12) 0.143(14) -0.054(10) 0.039(10) -0.001(9) O2 0.120(11) 0.069(8) 0.085(9) -0.001(7) 0.013(8) -0.008(7) C1 0.117(13) 0.032(7) 0.052(8) -0.019(6) 0.024(9) -0.004(8) C2 0.21(3) 0.050(10) 0.062(11) -0.008(8) 0.046(15) -0.003(13) C3 0.19(2) 0.064(13) 0.043(9) 0.010(8) -0.015(13) -0.057(15) C4 0.15(2) 0.071(13) 0.066(12) 0.007(10) -0.015(12) -0.054(14) C5 0.101(14) 0.076(12) 0.060(10) 0.003(8) -0.007(10) -0.029(10) C6 0.28(3) 0.061(12) 0.061(12) -0.013(9) -0.022(16) -0.048(17) C7 0.17(2) 0.050(11) 0.17(2) 0.018(13) -0.10(2) -0.034(13) C8 0.129(18) 0.046(9) 0.072(12) -0.028(8) -0.001(12) -0.016(10) C9 0.092(10) 0.018(5) 0.035(6) 0.004(4) 0.018(7) -0.005(6) C10 0.088(10) 0.019(5) 0.036(6) 0.002(5) 0.001(7) -0.013(6) C11 0.095(12) 0.026(6) 0.041(7) -0.002(5) -0.007(8) 0.003(6) C12 0.075(10) 0.056(9) 0.069(10) 0.004(7) 0.003(9) 0.027(8) C13 0.079(10) 0.042(7) 0.038(7) -0.012(5) 0.022(7) 0.012(6) C14 0.066(9) 0.023(5) 0.035(6) -0.001(4) 0.014(6) -0.002(5) C15 0.068(9) 0.040(7) 0.043(7) 0.001(5) 0.020(7) -0.003(6) C16 0.068(9) 0.039(7) 0.044(7) -0.004(6) 0.000(7) -0.014(6) C17 0.087(11) 0.032(7) 0.046(7) -0.009(5) 0.014(7) 0.002(6) C18 0.085(10) 0.030(6) 0.025(6) -0.009(5) 0.012(6) 0.002(6) C1A 0.057(8) 0.038(7) 0.040(7) -0.006(5) 0.013(6) -0.008(5) C2A 0.065(9) 0.062(9) 0.049(8) 0.015(7) 0.012(7) 0.003(7) C3A 0.086(12) 0.127(17) 0.028(7) 0.007(8) 0.018(8) 0.006(11) C4A 0.067(10) 0.070(10) 0.071(10) -0.001(8) 0.025(8) 0.006(8) C5A 0.085(12) 0.062(10) 0.079(11) 0.020(8) 0.023(9) 0.013(8) C6A 0.077(10) 0.048(8) 0.054(8) 0.008(6) 0.019(7) 0.007(7) C1B 0.085(10) 0.030(6) 0.036(6) 0.004(5) 0.011(7) -0.015(6) C2B 0.087(12) 0.044(8) 0.073(10) 0.011(7) 0.002(9) -0.011(8) C3B 0.116(15) 0.049(10) 0.094(14) 0.007(9) -0.004(12) -0.030(10) C4B 0.138(17) 0.026(8) 0.079(12) 0.008(7) -0.011(11) -0.029(9) C5B 0.127(16) 0.030(8) 0.080(12) 0.002(7) 0.004(11) -0.002(9) C6B 0.108(13) 0.033(7) 0.057(9) -0.008(6) 0.005(9) -0.005(7) C1C 0.066(8) 0.039(7) 0.030(6) -0.004(5) 0.011(6) -0.004(6) C2C 0.079(10) 0.033(7) 0.044(7) 0.004(5) 0.015(7) 0.003(6) C3C 0.088(11) 0.045(8) 0.061(9) 0.003(7) 0.021(8) -0.011(8) C4C 0.063(9) 0.077(11) 0.055(9) -0.006(8) 0.020(7) -0.015(8) C5C 0.062(9) 0.066(9) 0.047(8) -0.007(7) 0.018(7) 0.004(7) C6C 0.082(10) 0.028(6) 0.044(7) -0.003(5) 0.017(7) -0.003(6) C1D 0.077(9) 0.027(6) 0.036(6) 0.003(5) 0.021(6) 0.007(6) C2D 0.091(11) 0.025(6) 0.053(8) -0.001(5) 0.025(7) 0.005(6) C3D 0.118(14) 0.029(7) 0.064(10) 0.001(6) 0.038(10) 0.001(8) C4D 0.135(17) 0.050(9) 0.072(11) 0.011(8) 0.048(12) 0.042(10) C5D 0.068(10) 0.076(12) 0.078(11) 0.005(9) 0.011(9) 0.029(9) C6D 0.076(10) 0.044(7) 0.037(7) 0.000(5) 0.015(7) 0.005(7) Cl2 0.26(2) 0.119(11) 0.093(9) -0.025(8) 0.043(11) -0.048(12) Cl3 0.28(3) 0.21(2) 0.120(15) -0.039(15) -0.039(16) 0.02(2) Cl4 0.116(12) 0.43(4) 0.29(3) -0.25(3) 0.102(14) -0.121(18) S1 0.095(8) 0.130(10) 0.097(8) -0.023(7) 0.033(7) 0.017(7) O3 0.21(3) 0.19(3) 0.12(2) 0.01(2) 0.05(3) -0.05(3) O4 0.14(3) 0.20(3) 0.20(3) 0.05(3) 0.06(2) -0.08(2) O5 0.17(3) 0.16(3) 0.20(3) -0.06(3) 0.04(3) 0.03(3) F1 0.38(3) 0.39(3) 0.37(3) -0.01(2) 0.08(2) 0.02(2) F2 0.38(3) 0.39(3) 0.37(3) -0.01(2) 0.08(2) 0.02(2) F3 0.38(3) 0.39(3) 0.37(3) -0.01(2) 0.08(2) 0.02(2) S2 0.114(11) 0.100(10) 0.218(19) 0.018(11) -0.025(11) -0.018(8) O6 0.084(19) 0.22(3) 0.23(3) -0.09(3) 0.09(2) -0.01(2) O7 0.25(4) 0.26(4) 0.21(4) -0.05(3) 0.00(3) -0.03(3) O8 0.18(3) 0.11(2) 0.17(3) 0.05(2) -0.02(2) -0.04(2) F4 0.13(2) 0.22(3) 0.19(3) -0.01(3) -0.04(2) -0.02(2) F5 0.22(3) 0.21(3) 0.19(3) 0.00(3) 0.05(3) -0.04(3) F6 0.20(3) 0.20(3) 0.19(3) -0.08(2) 0.00(2) 0.06(2) Cl5 0.115(10) 0.25(2) 0.121(11) -0.026(12) 0.025(9) 0.028(12) Cl6 0.089(7) 0.100(8) 0.179(14) -0.032(9) 0.025(8) 0.002(6) Cl7 0.21(2) 0.22(2) 0.111(12) -0.013(13) -0.015(12) 0.102(18) _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 N1 2.072(10) . ? Pt1 P1 2.251(3) . ? Pt1 P2 2.269(3) . ? Pt1 Cl1 2.336(3) . ? P1 C1B 1.816(12) . ? P1 C1A 1.820(13) . ? P1 C9 1.824(15) . ? P2 C14 1.805(12) . ? P2 C1D 1.817(12) . ? P2 C1C 1.824(13) . ? Fe1 C9 1.971(12) . ? Fe1 C14 1.998(11) . ? Fe1 C18 2.032(13) . ? Fe1 C13 2.035(12) . ? Fe1 C10 2.038(12) . ? Fe1 C12 2.045(14) . ? Fe1 C15 2.048(13) . ? Fe1 C11 2.051(13) . ? Fe1 C17 2.074(12) . ? Fe1 C16 2.078(12) . ? N1 C5 1.32(2) . ? N1 C1 1.333(19) . ? O1 C8 1.20(2) . ? O2 C8 1.31(2) . ? C1 C2 1.40(2) . ? C2 C3 1.37(3) . ? C3 C4 1.36(3) . ? C3 C6 1.52(2) . ? C4 C5 1.44(2) . ? C6 C7 1.51(4) . ? C7 C8 1.50(3) . ? C9 C13 1.39(2) . ? C9 C10 1.436(17) . ? C10 C11 1.39(2) . ? C11 C12 1.43(2) . ? C12 C13 1.38(2) . ? C14 C15 1.428(19) . ? C14 C18 1.466(17) . ? C15 C16 1.420(18) . ? C16 C17 1.40(2) . ? C17 C18 1.440(19) . ? C1A C6A 1.366(19) . ? C1A C2A 1.391(19) . ? C2A C3A 1.40(2) . ? C3A C4A 1.33(2) . ? C4A C5A 1.37(2) . ? C5A C6A 1.38(2) . ? C1B C2B 1.38(2) . ? C1B C6B 1.40(2) . ? C2B C3B 1.39(2) . ? C3B C4B 1.36(3) . ? C4B C5B 1.33(3) . ? C5B C6B 1.41(2) . ? C1C C6C 1.380(18) . ? C1C C2C 1.412(17) . ? C2C C3C 1.33(2) . ? C3C C4C 1.37(2) . ? C4C C5C 1.40(2) . ? C5C C6C 1.340(19) . ? C1D C2D 1.390(17) . ? C1D C6D 1.400(19) . ? C2D C3D 1.32(2) . ? C3D C4D 1.38(3) . ? C4D C5D 1.38(2) . ? C5D C6D 1.34(2) . ? C3S Cl4 1.67(5) . ? C3S Cl3 1.746(14) . ? C3S Cl2 1.752(19) . ? S1 O4 1.372(15) . ? S1 O3 1.424(16) . ? S1 O5 1.432(16) . ? S1 C1S 1.768(15) . ? C1S F1 1.274(18) . ? C1S F2 1.283(18) . ? C1S F3 1.307(18) . ? S2 O6 1.396(15) . ? S2 O7 1.412(16) . ? S2 O8 1.435(16) . ? S2 C2S 1.756(15) . ? C2S F4 1.286(18) . ? C2S F5 1.298(17) . ? C2S F6 1.302(17) . ? C4S Cl5 1.710(19) . ? C4S Cl6 1.735(18) . ? C4S Cl7 1.789(19) . ? 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 N1 Pt1 P1 91.9(3) . . ? N1 Pt1 P2 170.0(3) . . ? P1 Pt1 P2 97.77(11) . . ? N1 Pt1 Cl1 83.9(3) . . ? P1 Pt1 Cl1 173.31(13) . . ? P2 Pt1 Cl1 86.74(11) . . ? C1B P1 C1A 102.2(6) . . ? C1B P1 C9 105.0(6) . . ? C1A P1 C9 109.2(6) . . ? C1B P1 Pt1 112.8(4) . . ? C1A P1 Pt1 112.0(4) . . ? C9 P1 Pt1 114.7(4) . . ? C14 P2 C1D 102.6(6) . . ? C14 P2 C1C 99.9(6) . . ? C1D P2 C1C 107.7(6) . . ? C14 P2 Pt1 121.8(4) . . ? C1D P2 Pt1 114.2(5) . . ? C1C P2 Pt1 109.1(4) . . ? C9 Fe1 C14 109.5(5) . . ? C9 Fe1 C18 111.7(6) . . ? C14 Fe1 C18 42.7(5) . . ? C9 Fe1 C13 40.5(6) . . ? C14 Fe1 C13 112.1(5) . . ? C18 Fe1 C13 142.1(5) . . ? C9 Fe1 C10 42.0(5) . . ? C14 Fe1 C10 136.8(6) . . ? C18 Fe1 C10 108.5(6) . . ? C13 Fe1 C10 69.1(6) . . ? C9 Fe1 C12 67.5(6) . . ? C14 Fe1 C12 141.0(6) . . ? C18 Fe1 C12 176.3(6) . . ? C13 Fe1 C12 39.4(6) . . ? C10 Fe1 C12 68.4(7) . . ? C9 Fe1 C15 137.5(5) . . ? C14 Fe1 C15 41.3(5) . . ? C18 Fe1 C15 69.7(6) . . ? C13 Fe1 C15 111.6(5) . . ? C10 Fe1 C15 178.0(6) . . ? C12 Fe1 C15 113.4(7) . . ? C9 Fe1 C11 67.9(5) . . ? C14 Fe1 C11 176.4(6) . . ? C18 Fe1 C11 135.4(6) . . ? C13 Fe1 C11 67.7(5) . . ? C10 Fe1 C11 39.7(6) . . ? C12 Fe1 C11 40.9(6) . . ? C15 Fe1 C11 142.2(6) . . ? C9 Fe1 C17 142.0(6) . . ? C14 Fe1 C17 69.7(5) . . ? C18 Fe1 C17 41.0(5) . . ? C13 Fe1 C17 176.7(6) . . ? C10 Fe1 C17 111.5(6) . . ? C12 Fe1 C17 137.5(6) . . ? C15 Fe1 C17 67.9(6) . . ? C11 Fe1 C17 110.6(5) . . ? C9 Fe1 C16 177.7(5) . . ? C14 Fe1 C16 68.9(5) . . ? C18 Fe1 C16 68.3(6) . . ? C13 Fe1 C16 138.2(6) . . ? C10 Fe1 C16 140.3(5) . . ? C12 Fe1 C16 112.6(7) . . ? C15 Fe1 C16 40.3(5) . . ? C11 Fe1 C16 113.8(5) . . ? C17 Fe1 C16 39.4(6) . . ? C5 N1 C1 118.9(14) . . ? C5 N1 Pt1 120.0(11) . . ? C1 N1 Pt1 120.5(11) . . ? N1 C1 C2 120.8(19) . . ? C3 C2 C1 122(2) . . ? C4 C3 C2 116.5(18) . . ? C4 C3 C6 122(3) . . ? C2 C3 C6 122(3) . . ? C3 C4 C5 120(2) . . ? N1 C5 C4 122(2) . . ? C7 C6 C3 110.0(19) . . ? C8 C7 C6 112(2) . . ? O1 C8 O2 120(2) . . ? O1 C8 C7 125(2) . . ? O2 C8 C7 115(2) . . ? C13 C9 C10 109.8(13) . . ? C13 C9 P1 124.1(9) . . ? C10 C9 P1 126.1(11) . . ? C13 C9 Fe1 72.2(8) . . ? C10 C9 Fe1 71.5(7) . . ? P1 C9 Fe1 121.7(6) . . ? C11 C10 C9 105.4(13) . . ? C11 C10 Fe1 70.7(8) . . ? C9 C10 Fe1 66.5(7) . . ? C10 C11 C12 108.9(12) . . ? C10 C11 Fe1 69.6(7) . . ? C12 C11 Fe1 69.3(8) . . ? C13 C12 C11 108.1(14) . . ? C13 C12 Fe1 69.9(8) . . ? C11 C12 Fe1 69.7(8) . . ? C12 C13 C9 107.7(12) . . ? C12 C13 Fe1 70.7(8) . . ? C9 C13 Fe1 67.3(7) . . ? C15 C14 C18 107.4(11) . . ? C15 C14 P2 126.1(9) . . ? C18 C14 P2 126.5(10) . . ? C15 C14 Fe1 71.2(7) . . ? C18 C14 Fe1 69.9(7) . . ? P2 C14 Fe1 126.5(6) . . ? C16 C15 C14 108.1(12) . . ? C16 C15 Fe1 71.0(7) . . ? C14 C15 Fe1 67.4(7) . . ? C17 C16 C15 109.4(12) . . ? C17 C16 Fe1 70.2(7) . . ? C15 C16 Fe1 68.8(7) . . ? C16 C17 C18 108.7(12) . . ? C16 C17 Fe1 70.4(7) . . ? C18 C17 Fe1 67.9(7) . . ? C17 C18 C14 106.5(12) . . ? C17 C18 Fe1 71.0(7) . . ? C14 C18 Fe1 67.4(7) . . ? C6A C1A C2A 118.7(13) . . ? C6A C1A P1 120.1(10) . . ? C2A C1A P1 121.2(11) . . ? C1A C2A C3A 119.1(14) . . ? C4A C3A C2A 120.8(15) . . ? C3A C4A C5A 121.3(16) . . ? C4A C5A C6A 118.6(15) . . ? C1A C6A C5A 121.5(14) . . ? C2B C1B C6B 118.6(13) . . ? C2B C1B P1 120.4(11) . . ? C6B C1B P1 120.8(12) . . ? C1B C2B C3B 121.8(16) . . ? C4B C3B C2B 118.5(18) . . ? C5B C4B C3B 121.4(15) . . ? C4B C5B C6B 122.0(17) . . ? C1B C6B C5B 117.6(17) . . ? C6C C1C C2C 117.6(12) . . ? C6C C1C P2 120.5(10) . . ? C2C C1C P2 121.9(10) . . ? C3C C2C C1C 120.7(13) . . ? C2C C3C C4C 120.6(14) . . ? C3C C4C C5C 120.1(14) . . ? C6C C5C C4C 118.6(14) . . ? C5C C6C C1C 122.3(13) . . ? C2D C1D C6D 118.6(12) . . ? C2D C1D P2 120.9(11) . . ? C6D C1D P2 120.5(9) . . ? C3D C2D C1D 122.0(16) . . ? C2D C3D C4D 119.7(15) . . ? C5D C4D C3D 118.8(14) . . ? C6D C5D C4D 122.5(17) . . ? C5D C6D C1D 118.3(14) . . ? Cl4 C3S Cl3 108(3) . . ? Cl4 C3S Cl2 116(3) . . ? Cl3 C3S Cl2 112(2) . . ? O4 S1 O3 111.9(15) . . ? O4 S1 O5 110.9(15) . . ? O3 S1 O5 107.0(14) . . ? O4 S1 C1S 112.5(14) . . ? O3 S1 C1S 108.3(13) . . ? O5 S1 C1S 106.0(13) . . ? F1 C1S F2 112.2(19) . . ? F1 C1S F3 109.5(18) . . ? F2 C1S F3 108.7(18) . . ? F1 C1S S1 110.1(16) . . ? F2 C1S S1 108.6(16) . . ? F3 C1S S1 107.6(16) . . ? O6 S2 O7 110.0(15) . . ? O6 S2 O8 107.7(14) . . ? O7 S2 O8 108.6(15) . . ? O6 S2 C2S 111.4(13) . . ? O7 S2 C2S 110.0(13) . . ? O8 S2 C2S 109.2(13) . . ? F4 C2S F5 108.5(18) . . ? F4 C2S F6 107.6(17) . . ? F5 C2S F6 108.5(17) . . ? F4 C2S S2 111.0(15) . . ? F5 C2S S2 110.1(15) . . ? F6 C2S S2 111.0(15) . . ? Cl5 C4S Cl6 109.3(16) . . ? Cl5 C4S Cl7 106.8(16) . . ? Cl6 C4S Cl7 112.4(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.971 _refine_diff_density_min -2.723 _refine_diff_density_rms 0.210 # Attachment 'complex7_new.cif' data_8175a _database_code_depnum_ccdc_archive 'CCDC 711717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H78 Cl3 F6 Fe2 N2 O10.50 P4 Pd2 S2' _chemical_formula_weight 2076.38 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 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' _cell_length_a 27.515(5) _cell_length_b 34.233(5) _cell_length_c 19.337(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 18214(5) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3878 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 16.00 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8408 _exptl_absorpt_coefficient_mu 0.975 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5923 _exptl_absorpt_correction_T_max 0.7585 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 197123 _diffrn_reflns_av_R_equivalents 0.2051 _diffrn_reflns_av_sigmaI/netI 0.1377 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 32073 _reflns_number_gt 21259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The anions and the solvents have large thermal parameters. Restraints in bond distances and thermal parameters were applied to them. One of the CHCl3 was disordered into two parts with 50:50 occupancy ratio. As the disordered CHCL3 and the ether had very bad thermal parameters and were kept isotropic. Twin refinement was applied resulting in BASF value of 0.34 for racemic twins. ; _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^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.35(2) _refine_ls_number_reflns 32073 _refine_ls_number_parameters 2138 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1696 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 O1S O 0.9182(7) 0.4906(7) 0.3142(12) 0.237(10) Uiso 1 1 d D . . C3S C 0.9180(14) 0.5115(10) 0.1976(14) 0.326(17) Uiso 1 1 d D . . H3S1 H 0.8866 0.5098 0.1751 0.489 Uiso 1 1 calc R . . H3S2 H 0.9435 0.5118 0.1629 0.489 Uiso 1 1 calc R . . H3S3 H 0.9196 0.5353 0.2247 0.489 Uiso 1 1 calc R . . C4S C 0.9250(15) 0.4755(8) 0.2461(17) 0.352(19) Uiso 1 1 d D . . H4S1 H 0.9010 0.4552 0.2358 0.422 Uiso 1 1 calc R . . H4S2 H 0.9577 0.4645 0.2408 0.422 Uiso 1 1 calc R . . C5S C 0.9221(14) 0.4629(8) 0.3689(18) 0.352(19) Uiso 1 1 d D . . H5S1 H 0.9542 0.4506 0.3686 0.422 Uiso 1 1 calc R . . H5S2 H 0.8973 0.4426 0.3643 0.422 Uiso 1 1 calc R . . C6S C 0.9145(14) 0.4863(12) 0.4357(14) 0.326(17) Uiso 1 1 d D . . H6S1 H 0.8929 0.5081 0.4266 0.489 Uiso 1 1 calc R . . H6S2 H 0.9455 0.4961 0.4520 0.489 Uiso 1 1 calc R . . H6S3 H 0.9002 0.4696 0.4707 0.489 Uiso 1 1 calc R . . C1S C 0.9604(11) 0.3629(9) 0.8526(13) 0.300 Uiso 0.50 1 d PD A 1 H1S H 0.9716 0.3642 0.9012 0.360 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.9010(10) 0.3481(9) 0.834(2) 0.43(2) Uiso 0.50 1 d PD A 1 Cl2 Cl 0.9874(10) 0.3299(8) 0.7952(17) 0.371(17) Uiso 0.50 1 d PD A 1 Cl3 Cl 0.9623(11) 0.4049(7) 0.801(2) 0.386(19) Uiso 0.50 1 d PD A 1 C1SA C 0.9261(6) 0.3803(6) 0.8620(11) 0.300 Uiso 0.50 1 d PD B 2 H1SA H 0.9483 0.3705 0.8984 0.360 Uiso 0.50 1 calc PR B 2 Cl1A Cl 0.8676(5) 0.3611(3) 0.8560(7) 0.132(4) Uiso 0.50 1 d PD B 2 Cl2A Cl 0.9422(7) 0.3743(6) 0.7750(10) 0.226(8) Uiso 0.50 1 d PD B 2 Cl3A Cl 0.9100(7) 0.4295(5) 0.8613(10) 0.240(9) Uiso 0.50 1 d PD B 2 Pd1 Pd 0.81392(3) 0.15834(2) -0.12105(4) 0.0291(2) Uani 1 1 d . . . Pd2 Pd 0.78362(3) 0.14880(2) 0.26806(4) 0.0297(2) Uani 1 1 d . . . Pd3 Pd 0.20470(3) 0.15241(2) 0.73689(4) 0.02682(19) Uani 1 1 d . . . Pd4 Pd 0.17506(3) 0.16298(2) 0.34838(4) 0.0290(2) Uani 1 1 d . . . Fe1 Fe 0.90166(6) 0.08669(5) -0.25328(8) 0.0356(4) Uani 1 1 d . . . Fe2 Fe 0.87249(6) 0.07532(5) 0.39503(9) 0.0392(4) Uani 1 1 d . . . Fe3 Fe 0.11922(5) 0.08189(5) 0.87663(8) 0.0322(4) Uani 1 1 d . . . Fe4 Fe 0.08520(6) 0.08536(5) 0.23726(8) 0.0366(4) Uani 1 1 d . . . P1 P 0.87938(11) 0.17608(8) -0.18717(15) 0.0323(7) Uani 1 1 d . . . P2 P 0.79233(11) 0.10318(8) -0.17772(16) 0.0348(7) Uani 1 1 d . . . P3 P 0.85276(10) 0.16442(9) 0.32670(15) 0.0334(7) Uani 1 1 d . . . P4 P 0.75859(10) 0.09760(8) 0.33460(15) 0.0314(7) Uani 1 1 d . . . P5 P 0.23010(10) 0.10189(8) 0.80397(15) 0.0303(7) Uani 1 1 d . . . P6 P 0.13414(10) 0.16791(8) 0.79285(15) 0.0293(7) Uani 1 1 d . . . P7 P 0.19744(11) 0.10870(8) 0.28866(15) 0.0332(7) Uani 1 1 d . . . P8 P 0.10844(11) 0.17878(8) 0.28330(15) 0.0322(7) Uani 1 1 d . . . N1 N 0.8047(3) 0.1860(2) 0.1887(4) 0.034(2) Uani 1 1 d . . . N2 N 0.7590(3) 0.1485(3) -0.0473(4) 0.030(2) Uani 1 1 d . . . N3 N 0.1845(3) 0.1902(2) 0.6575(4) 0.030(2) Uani 1 1 d . . . N4 N 0.2280(3) 0.1537(3) 0.4244(4) 0.035(2) Uani 1 1 d . . . O1 O 0.8364(3) 0.2069(2) -0.0692(4) 0.0334(18) Uani 1 1 d . . . O2 O 0.7684(3) 0.2428(2) -0.0829(4) 0.042(2) Uani 1 1 d . . . O3 O 0.7208(3) 0.1377(2) 0.2120(4) 0.0371(19) Uani 1 1 d . . . O4 O 0.6963(3) 0.1979(2) 0.2412(4) 0.049(2) Uani 1 1 d . . . O5 O 0.2676(3) 0.1407(2) 0.6834(4) 0.0329(18) Uani 1 1 d . . . O6 O 0.2936(3) 0.2008(2) 0.7080(4) 0.042(2) Uani 1 1 d . . . O7 O 0.1536(3) 0.2114(2) 0.4027(4) 0.0378(19) Uani 1 1 d . . . O8 O 0.2186(3) 0.2482(2) 0.3805(4) 0.044(2) Uani 1 1 d . . . C1 C 0.8098(4) 0.2383(3) -0.0600(5) 0.032(3) Uani 1 1 d . . . C2 C 0.8373(4) 0.2708(3) -0.0240(6) 0.034(3) Uani 1 1 d . . . H2A H 0.8140 0.2883 -0.0016 0.041 Uiso 1 1 calc R . . H2B H 0.8551 0.2861 -0.0588 0.041 Uiso 1 1 calc R . . C3 C 0.8733(4) 0.2559(3) 0.0303(5) 0.030(3) Uani 1 1 d . . . H3A H 0.8894 0.2782 0.0524 0.036 Uiso 1 1 calc R . . H3B H 0.8983 0.2401 0.0076 0.036 Uiso 1 1 calc R . . C4 C 0.8002(4) 0.2248(3) 0.1871(6) 0.044(3) Uani 1 1 d . . . H4 H 0.7825 0.2369 0.2228 0.053 Uiso 1 1 calc R . . C5 C 0.8196(5) 0.2479(3) 0.1373(6) 0.039(3) Uani 1 1 d . . . H5 H 0.8141 0.2750 0.1378 0.047 Uiso 1 1 calc R . . C6 C 0.8477(4) 0.2313(3) 0.0855(6) 0.031(3) Uani 1 1 d . . . C7 C 0.8512(4) 0.1903(3) 0.0846(6) 0.035(3) Uani 1 1 d . . . H7 H 0.8678 0.1775 0.0485 0.042 Uiso 1 1 calc R . . C8 C 0.8305(4) 0.1694(3) 0.1362(6) 0.035(3) Uani 1 1 d . . . H8 H 0.8341 0.1421 0.1359 0.042 Uiso 1 1 calc R . . C9 C 0.6917(4) 0.1677(4) 0.2072(6) 0.040(3) Uani 1 1 d . . . C10 C 0.6476(4) 0.1610(4) 0.1596(6) 0.040(3) Uani 1 1 d . . . H10A H 0.6190 0.1566 0.1889 0.048 Uiso 1 1 calc R . . H10B H 0.6419 0.1850 0.1334 0.048 Uiso 1 1 calc R . . C11 C 0.6510(4) 0.1275(3) 0.1088(6) 0.042(3) Uani 1 1 d . . . H11A H 0.6195 0.1242 0.0857 0.050 Uiso 1 1 calc R . . H11B H 0.6581 0.1033 0.1340 0.050 Uiso 1 1 calc R . . C12 C 0.7162(4) 0.1663(3) -0.0485(5) 0.033(3) Uani 1 1 d . . . H12 H 0.7097 0.1843 -0.0841 0.039 Uiso 1 1 calc R . . C13 C 0.6812(4) 0.1596(3) -0.0003(6) 0.036(3) Uani 1 1 d . . . H13 H 0.6509 0.1721 -0.0037 0.043 Uiso 1 1 calc R . . C14 C 0.6904(4) 0.1341(3) 0.0541(6) 0.034(3) Uani 1 1 d . . . C15 C 0.7351(4) 0.1168(3) 0.0572(6) 0.036(3) Uani 1 1 d . . . H15 H 0.7430 0.1000 0.0939 0.043 Uiso 1 1 calc R . . C16 C 0.7683(4) 0.1242(3) 0.0059(6) 0.037(3) Uani 1 1 d . . . H16 H 0.7988 0.1119 0.0080 0.044 Uiso 1 1 calc R . . C17 C 0.9078(4) 0.1448(3) -0.2499(5) 0.033(3) Uani 1 1 d . . . C18 C 0.9551(4) 0.1272(3) -0.2426(6) 0.034(3) Uani 1 1 d . . . H18 H 0.9774 0.1300 -0.2028 0.041 Uiso 1 1 calc R . . C19 C 0.9634(5) 0.1053(3) -0.3027(6) 0.046(3) Uani 1 1 d . . . H19 H 0.9925 0.0892 -0.3123 0.055 Uiso 1 1 calc R . . C20 C 0.9231(5) 0.1093(4) -0.3460(6) 0.049(3) Uani 1 1 d . . . H20 H 0.9189 0.0966 -0.3916 0.059 Uiso 1 1 calc R . . C21 C 0.8890(4) 0.1336(3) -0.3133(6) 0.039(3) Uani 1 1 d . . . H21 H 0.8571 0.1415 -0.3324 0.047 Uiso 1 1 calc R . . C22 C 0.8415(4) 0.0714(3) -0.2011(6) 0.032(3) Uani 1 1 d . . . C23 C 0.8461(5) 0.0472(3) -0.2615(6) 0.043(3) Uani 1 1 d . . . H23 H 0.8225 0.0453 -0.3000 0.051 Uiso 1 1 calc R . . C24 C 0.8912(5) 0.0282(3) -0.2573(7) 0.051(4) Uani 1 1 d . . . H24 H 0.9045 0.0109 -0.2938 0.061 Uiso 1 1 calc R . . C25 C 0.9158(4) 0.0376(4) -0.1951(7) 0.052(4) Uani 1 1 d . . . H25 H 0.9480 0.0280 -0.1799 0.063 Uiso 1 1 calc R . . C26 C 0.8848(4) 0.0641(3) -0.1591(6) 0.036(3) Uani 1 1 d . . . H26 H 0.8920 0.0764 -0.1140 0.043 Uiso 1 1 calc R . . C27 C 0.8931(4) 0.1246(3) 0.3478(6) 0.035(3) Uani 1 1 d . . . C28 C 0.9209(5) 0.1191(4) 0.4085(7) 0.049(3) Uani 1 1 d . . . H28 H 0.9217 0.1371 0.4485 0.058 Uiso 1 1 calc R . . C29 C 0.9461(5) 0.0844(4) 0.4040(8) 0.062(4) Uani 1 1 d . . . H29 H 0.9674 0.0733 0.4401 0.074 Uiso 1 1 calc R . . C30 C 0.9342(5) 0.0662(4) 0.3382(9) 0.067(4) Uani 1 1 d . . . H30 H 0.9463 0.0407 0.3214 0.080 Uiso 1 1 calc R . . C31 C 0.9001(4) 0.0920(3) 0.3023(6) 0.038(3) Uani 1 1 d . . . H31 H 0.8855 0.0880 0.2560 0.045 Uiso 1 1 calc R . . C32 C 0.7991(4) 0.0703(3) 0.3914(6) 0.036(3) Uani 1 1 d . . . C33 C 0.8204(4) 0.0332(3) 0.3769(6) 0.032(3) Uani 1 1 d . . . H33 H 0.8162 0.0171 0.3347 0.038 Uiso 1 1 calc R . . C34 C 0.8474(4) 0.0240(4) 0.4358(8) 0.056(4) Uani 1 1 d . . . H34 H 0.8673 0.0001 0.4410 0.067 Uiso 1 1 calc R . . C35 C 0.8439(5) 0.0542(4) 0.4872(7) 0.052(4) Uani 1 1 d . . . H35 H 0.8598 0.0544 0.5332 0.062 Uiso 1 1 calc R . . C36 C 0.8140(4) 0.0837(4) 0.4589(6) 0.044(3) Uani 1 1 d . . . H36 H 0.8043 0.1085 0.4816 0.052 Uiso 1 1 calc R . . C37 C 0.2972(4) 0.1698(4) 0.6780(6) 0.038(3) Uani 1 1 d . . . C38 C 0.3423(4) 0.1617(4) 0.6309(6) 0.048(3) Uani 1 1 d . . . H38A H 0.3502 0.1857 0.6058 0.058 Uiso 1 1 calc R . . H38B H 0.3701 0.1555 0.6606 0.058 Uiso 1 1 calc R . . C39 C 0.3361(4) 0.1292(3) 0.5791(6) 0.039(3) Uani 1 1 d . . . H39A H 0.3673 0.1247 0.5558 0.047 Uiso 1 1 calc R . . H39B H 0.3277 0.1051 0.6039 0.047 Uiso 1 1 calc R . . C40 C 0.2188(4) 0.1279(3) 0.4752(6) 0.034(3) Uani 1 1 d . . . H40 H 0.1885 0.1151 0.4764 0.041 Uiso 1 1 calc R . . C41 C 0.2529(4) 0.1200(3) 0.5256(5) 0.033(3) Uani 1 1 d . . . H41 H 0.2448 0.1023 0.5609 0.040 Uiso 1 1 calc R . . C42 C 0.2983(4) 0.1369(3) 0.5261(6) 0.031(3) Uani 1 1 d . . . C43 C 0.3064(4) 0.1637(4) 0.4734(6) 0.047(3) Uani 1 1 d . . . H43 H 0.3362 0.1771 0.4712 0.057 Uiso 1 1 calc R . . C44 C 0.2705(4) 0.1711(4) 0.4235(6) 0.044(3) Uani 1 1 d . . . H44 H 0.2772 0.1891 0.3881 0.052 Uiso 1 1 calc R . . C45 C 0.1786(5) 0.2427(3) 0.4060(5) 0.037(3) Uani 1 1 d . . . C46 C 0.1543(4) 0.2750(3) 0.4450(6) 0.040(3) Uani 1 1 d . . . H46A H 0.1362 0.2913 0.4123 0.049 Uiso 1 1 calc R . . H46B H 0.1793 0.2914 0.4665 0.049 Uiso 1 1 calc R . . C47 C 0.1189(4) 0.2605(3) 0.5021(6) 0.040(3) Uani 1 1 d . . . H47A H 0.1037 0.2831 0.5244 0.048 Uiso 1 1 calc R . . H47B H 0.0930 0.2449 0.4806 0.048 Uiso 1 1 calc R . . C48 C 0.1943(4) 0.2289(3) 0.6545(6) 0.039(3) Uani 1 1 d . . . H48 H 0.2157 0.2400 0.6869 0.046 Uiso 1 1 calc R . . C49 C 0.1737(4) 0.2522(3) 0.6055(6) 0.035(3) Uani 1 1 d . . . H49 H 0.1800 0.2792 0.6057 0.041 Uiso 1 1 calc R . . C50 C 0.1437(4) 0.2364(3) 0.5553(5) 0.026(2) Uani 1 1 d . . . C51 C 0.1370(4) 0.1954(3) 0.5569(6) 0.032(3) Uani 1 1 d . . . H51 H 0.1188 0.1830 0.5221 0.039 Uiso 1 1 calc R . . C52 C 0.1567(4) 0.1745(3) 0.6082(6) 0.033(3) Uani 1 1 d . . . H52 H 0.1508 0.1475 0.6095 0.039 Uiso 1 1 calc R . . C53 C 0.1929(4) 0.0797(3) 0.8678(5) 0.031(3) Uani 1 1 d . . . C54 C 0.1712(4) 0.0404(3) 0.8630(6) 0.039(3) Uani 1 1 d . . . H54 H 0.1738 0.0224 0.8232 0.047 Uiso 1 1 calc R . . C55 C 0.1447(5) 0.0332(4) 0.9258(7) 0.048(3) Uani 1 1 d . . . H55 H 0.1257 0.0095 0.9365 0.058 Uiso 1 1 calc R . . C56 C 0.1507(4) 0.0660(4) 0.9696(6) 0.055(4) Uani 1 1 d . . . H56 H 0.1358 0.0693 1.0159 0.066 Uiso 1 1 calc R . . C57 C 0.1786(4) 0.0951(3) 0.9335(6) 0.036(3) Uani 1 1 d . . . H57 H 0.1869 0.1214 0.9514 0.043 Uiso 1 1 calc R . . C58 C 0.0962(4) 0.1286(3) 0.8218(5) 0.029(3) Uani 1 1 d . . . C59 C 0.0691(4) 0.1268(3) 0.8867(6) 0.038(3) Uani 1 1 d . . . H59 H 0.0690 0.1470 0.9234 0.046 Uiso 1 1 calc R . . C60 C 0.0438(4) 0.0893(4) 0.8892(7) 0.049(3) Uani 1 1 d . . . H60 H 0.0236 0.0793 0.9276 0.059 Uiso 1 1 calc R . . C61 C 0.0554(4) 0.0698(3) 0.8277(6) 0.041(3) Uani 1 1 d . . . H61 H 0.0440 0.0432 0.8157 0.049 Uiso 1 1 calc R . . C62 C 0.0865(4) 0.0932(3) 0.7852(6) 0.037(3) Uani 1 1 d . . . H62 H 0.0989 0.0861 0.7388 0.045 Uiso 1 1 calc R . . C63 C 0.1497(4) 0.0729(3) 0.2829(6) 0.033(3) Uani 1 1 d . . . C64 C 0.1387(5) 0.0454(3) 0.2287(6) 0.044(3) Uani 1 1 d . . . H64 H 0.1587 0.0409 0.1869 0.053 Uiso 1 1 calc R . . C65 C 0.0963(4) 0.0256(3) 0.2451(7) 0.050(3) Uani 1 1 d . . . H65 H 0.0803 0.0051 0.2171 0.060 Uiso 1 1 calc R . . C66 C 0.0801(5) 0.0405(3) 0.3084(7) 0.048(3) Uani 1 1 d . . . H66 H 0.0497 0.0324 0.3317 0.058 Uiso 1 1 calc R . . C67 C 0.1111(4) 0.0697(3) 0.3322(5) 0.037(3) Uani 1 1 d . . . H67 H 0.1077 0.0846 0.3758 0.044 Uiso 1 1 calc R . . C68 C 0.0767(4) 0.1445(3) 0.2300(5) 0.031(2) Uani 1 1 d . . . C69 C 0.0313(4) 0.1257(3) 0.2464(6) 0.037(3) Uani 1 1 d . . . H69 H 0.0114 0.1305 0.2882 0.044 Uiso 1 1 calc R . . C70 C 0.0205(5) 0.0988(4) 0.1932(6) 0.053(4) Uani 1 1 d . . . H70 H -0.0083 0.0815 0.1918 0.064 Uiso 1 1 calc R . . C71 C 0.0565(5) 0.1007(4) 0.1426(6) 0.051(4) Uani 1 1 d . . . H71 H 0.0579 0.0849 0.0997 0.062 Uiso 1 1 calc R . . C72 C 0.0930(4) 0.1286(3) 0.1662(6) 0.040(3) Uani 1 1 d . . . H72 H 0.1233 0.1356 0.1416 0.048 Uiso 1 1 calc R . . C1A C 0.9257(4) 0.1876(3) -0.1244(6) 0.040(3) Uani 1 1 d . . . C2A C 0.9507(4) 0.2229(4) -0.1227(7) 0.052(4) Uani 1 1 d . . . H2A1 H 0.9447 0.2418 -0.1568 0.062 Uiso 1 1 calc R . . C3A C 0.9844(5) 0.2303(5) -0.0710(8) 0.064(4) Uani 1 1 d . . . H3A1 H 1.0019 0.2539 -0.0716 0.077 Uiso 1 1 calc R . . C4A C 0.9925(5) 0.2043(5) -0.0202(8) 0.062(4) Uani 1 1 d . . . H4A H 1.0141 0.2100 0.0161 0.074 Uiso 1 1 calc R . . C5A C 0.9684(5) 0.1695(5) -0.0229(7) 0.060(4) Uani 1 1 d . . . H5A H 0.9744 0.1507 0.0115 0.072 Uiso 1 1 calc R . . C6A C 0.9359(4) 0.1611(4) -0.0737(6) 0.041(3) Uani 1 1 d . . . H6A H 0.9202 0.1367 -0.0739 0.049 Uiso 1 1 calc R . . C1B C 0.8692(4) 0.2198(3) -0.2362(6) 0.038(3) Uani 1 1 d . . . C2B C 0.9052(4) 0.2329(3) -0.2816(6) 0.039(3) Uani 1 1 d . . . H2B1 H 0.9332 0.2178 -0.2890 0.047 Uiso 1 1 calc R . . C3B C 0.8995(5) 0.2682(4) -0.3156(7) 0.055(4) Uani 1 1 d . . . H3B1 H 0.9241 0.2768 -0.3458 0.066 Uiso 1 1 calc R . . C4B C 0.8597(4) 0.2906(4) -0.3067(6) 0.046(3) Uani 1 1 d . . . H4B H 0.8566 0.3145 -0.3302 0.055 Uiso 1 1 calc R . . C5B C 0.8226(4) 0.2776(4) -0.2614(6) 0.047(3) Uani 1 1 d . . . H5B H 0.7948 0.2931 -0.2547 0.056 Uiso 1 1 calc R . . C6B C 0.8271(4) 0.2423(3) -0.2267(6) 0.040(3) Uani 1 1 d . . . H6B H 0.8022 0.2336 -0.1972 0.048 Uiso 1 1 calc R . . C1C C 0.7513(4) 0.0726(4) -0.1295(8) 0.054(4) Uani 1 1 d . . . C2C C 0.7019(5) 0.0784(4) -0.1284(9) 0.073(5) Uani 1 1 d . . . H2C H 0.6877 0.0972 -0.1576 0.087 Uiso 1 1 calc R . . C3C C 0.6717(6) 0.0557(5) -0.0821(10) 0.086(6) Uani 1 1 d . . . H3C H 0.6383 0.0612 -0.0791 0.103 Uiso 1 1 calc R . . C4C C 0.6903(6) 0.0276(5) -0.0445(10) 0.089(6) Uani 1 1 d . . . H4C H 0.6693 0.0113 -0.0192 0.107 Uiso 1 1 calc R . . C5C C 0.7401(6) 0.0214(4) -0.0411(8) 0.069(5) Uani 1 1 d . . . H5C H 0.7536 0.0029 -0.0106 0.083 Uiso 1 1 calc R . . C6C C 0.7693(5) 0.0437(4) -0.0849(7) 0.052(4) Uani 1 1 d . . . H6C H 0.8030 0.0390 -0.0845 0.062 Uiso 1 1 calc R . . C1D C 0.7606(4) 0.1138(3) -0.2558(7) 0.051(4) Uani 1 1 d . . . C2D C 0.7358(6) 0.0844(4) -0.2912(8) 0.078(5) Uani 1 1 d . . . H2D H 0.7348 0.0587 -0.2738 0.093 Uiso 1 1 calc R . . C3D C 0.7118(8) 0.0941(5) -0.3549(11) 0.125(9) Uani 1 1 d . . . H3D H 0.6949 0.0745 -0.3792 0.150 Uiso 1 1 calc R . . C4D C 0.7130(8) 0.1307(5) -0.3805(11) 0.133(10) Uani 1 1 d . . . H4D H 0.6978 0.1359 -0.4231 0.159 Uiso 1 1 calc R . . C5D C 0.7353(5) 0.1598(4) -0.3468(8) 0.075(5) Uani 1 1 d . . . H5D H 0.7344 0.1853 -0.3649 0.090 Uiso 1 1 calc R . . C6D C 0.7607(4) 0.1526(3) -0.2833(7) 0.052(4) Uani 1 1 d . . . H6D H 0.7771 0.1729 -0.2602 0.062 Uiso 1 1 calc R . . C1E C 0.8924(4) 0.1983(3) 0.2791(6) 0.036(3) Uani 1 1 d . . . C2E C 0.8897(5) 0.2388(3) 0.2905(8) 0.059(4) Uani 1 1 d . . . H2E H 0.8687 0.2486 0.3246 0.071 Uiso 1 1 calc R . . C3E C 0.9170(5) 0.2634(5) 0.2529(10) 0.075(5) Uani 1 1 d . . . H3E H 0.9136 0.2905 0.2595 0.090 Uiso 1 1 calc R . . C4E C 0.9487(6) 0.2501(5) 0.2062(9) 0.082(6) Uani 1 1 d . . . H4E H 0.9687 0.2677 0.1822 0.099 Uiso 1 1 calc R . . C5E C 0.9522(5) 0.2101(6) 0.1931(7) 0.070(5) Uani 1 1 d . . . H5E H 0.9733 0.2007 0.1586 0.084 Uiso 1 1 calc R . . C6E C 0.9246(4) 0.1849(4) 0.2309(6) 0.045(3) Uani 1 1 d . . . H6E H 0.9278 0.1579 0.2236 0.054 Uiso 1 1 calc R . . C1F C 0.8396(4) 0.1888(3) 0.4089(6) 0.036(3) Uani 1 1 d . . . C2F C 0.8763(5) 0.2051(4) 0.4470(8) 0.072(5) Uani 1 1 d . . . H2F H 0.9083 0.2039 0.4298 0.087 Uiso 1 1 calc R . . C3F C 0.8679(5) 0.2235(5) 0.5110(9) 0.086(6) Uani 1 1 d . . . H3F H 0.8933 0.2350 0.5364 0.103 Uiso 1 1 calc R . . C4F C 0.8210(5) 0.2239(4) 0.5346(8) 0.070(5) Uani 1 1 d . . . H4F H 0.8144 0.2347 0.5783 0.084 Uiso 1 1 calc R . . C5F C 0.7832(5) 0.2089(5) 0.4959(8) 0.087(6) Uani 1 1 d . . . H5F H 0.7510 0.2105 0.5120 0.104 Uiso 1 1 calc R . . C6F C 0.7936(5) 0.1913(4) 0.4327(7) 0.061(4) Uani 1 1 d . . . H6F H 0.7681 0.1811 0.4060 0.073 Uiso 1 1 calc R . . C1G C 0.7062(4) 0.1046(3) 0.3871(6) 0.037(3) Uani 1 1 d . . . C2G C 0.6929(4) 0.0783(4) 0.4379(6) 0.045(3) Uani 1 1 d . . . H2G H 0.7139 0.0573 0.4473 0.054 Uiso 1 1 calc R . . C3G C 0.6514(5) 0.0811(4) 0.4746(7) 0.061(4) Uani 1 1 d . . . H3G H 0.6440 0.0627 0.5092 0.073 Uiso 1 1 calc R . . C4G C 0.6192(5) 0.1124(4) 0.4599(7) 0.058(4) Uani 1 1 d . . . H4G H 0.5901 0.1144 0.4850 0.069 Uiso 1 1 calc R . . C5G C 0.6291(4) 0.1395(4) 0.4110(7) 0.051(4) Uani 1 1 d . . . H5G H 0.6074 0.1600 0.4015 0.061 Uiso 1 1 calc R . . C6G C 0.6732(4) 0.1356(3) 0.3750(6) 0.040(3) Uani 1 1 d . . . H6G H 0.6811 0.1544 0.3414 0.048 Uiso 1 1 calc R . . C1H C 0.7421(4) 0.0608(3) 0.2707(6) 0.036(3) Uani 1 1 d . . . C2H C 0.6969(4) 0.0427(3) 0.2717(6) 0.045(3) Uani 1 1 d . . . H2H H 0.6752 0.0481 0.3080 0.054 Uiso 1 1 calc R . . C3H C 0.6833(6) 0.0165(4) 0.2191(7) 0.067(4) Uani 1 1 d . . . H3H H 0.6526 0.0044 0.2197 0.080 Uiso 1 1 calc R . . C4H C 0.7146(6) 0.0091(4) 0.1688(7) 0.060(4) Uani 1 1 d . . . H4H H 0.7056 -0.0085 0.1338 0.073 Uiso 1 1 calc R . . C5H C 0.7596(5) 0.0261(4) 0.1656(7) 0.051(3) Uani 1 1 d . . . H5H H 0.7811 0.0205 0.1292 0.061 Uiso 1 1 calc R . . C6H C 0.7727(4) 0.0524(3) 0.2187(6) 0.044(3) Uani 1 1 d . . . H6H H 0.8035 0.0643 0.2177 0.052 Uiso 1 1 calc R . . C1I C 0.2426(4) 0.0637(3) 0.7404(6) 0.039(3) Uani 1 1 d . . . C2I C 0.2865(5) 0.0457(4) 0.7375(8) 0.063(4) Uani 1 1 d . . . H2I H 0.3106 0.0506 0.7709 0.075 Uiso 1 1 calc R . . C3I C 0.2948(6) 0.0186(4) 0.6806(10) 0.081(5) Uani 1 1 d . . . H3I H 0.3246 0.0053 0.6777 0.097 Uiso 1 1 calc R . . C4I C 0.2604(7) 0.0122(4) 0.6315(8) 0.071(5) Uani 1 1 d . . . H4I H 0.2673 -0.0050 0.5948 0.085 Uiso 1 1 calc R . . C5I C 0.2167(6) 0.0297(4) 0.6341(6) 0.060(4) Uani 1 1 d . . . H5I H 0.1927 0.0246 0.6007 0.072 Uiso 1 1 calc R . . C6I C 0.2081(5) 0.0562(3) 0.6895(7) 0.048(3) Uani 1 1 d . . . H6I H 0.1780 0.0692 0.6918 0.058 Uiso 1 1 calc R . . C1J C 0.2857(4) 0.1095(3) 0.8523(6) 0.038(3) Uani 1 1 d . . . C2J C 0.3005(4) 0.0814(4) 0.9005(7) 0.059(4) Uani 1 1 d . . . H2J H 0.2810 0.0594 0.9090 0.070 Uiso 1 1 calc R . . C3J C 0.3433(5) 0.0861(4) 0.9352(9) 0.075(5) Uani 1 1 d . . . H3J H 0.3528 0.0670 0.9674 0.090 Uiso 1 1 calc R . . C4J C 0.3723(5) 0.1169(5) 0.9249(8) 0.065(4) Uani 1 1 d . . . H4J H 0.4008 0.1198 0.9511 0.078 Uiso 1 1 calc R . . C5J C 0.3604(4) 0.1440(4) 0.8764(7) 0.051(3) Uani 1 1 d . . . H5J H 0.3815 0.1649 0.8668 0.061 Uiso 1 1 calc R . . C6J C 0.3161(4) 0.1404(3) 0.8407(6) 0.039(3) Uani 1 1 d . . . H6J H 0.3071 0.1596 0.8083 0.047 Uiso 1 1 calc R . . C1K C 0.0928(4) 0.1974(3) 0.7431(6) 0.038(3) Uani 1 1 d . . . C2K C 0.0583(4) 0.1792(4) 0.7003(6) 0.043(3) Uani 1 1 d . . . H2K H 0.0560 0.1518 0.6993 0.051 Uiso 1 1 calc R . . C3K C 0.0281(5) 0.2012(4) 0.6603(7) 0.059(4) Uani 1 1 d . . . H3K H 0.0048 0.1887 0.6324 0.071 Uiso 1 1 calc R . . C4K C 0.0306(5) 0.2408(5) 0.6597(9) 0.079(5) Uani 1 1 d . . . H4K H 0.0097 0.2553 0.6311 0.095 Uiso 1 1 calc R . . C5K C 0.0639(5) 0.2596(4) 0.7010(8) 0.068(4) Uani 1 1 d . . . H5K H 0.0653 0.2871 0.7010 0.082 Uiso 1 1 calc R . . C6K C 0.0959(5) 0.2381(4) 0.7433(8) 0.058(4) Uani 1 1 d . . . H6K H 0.1189 0.2509 0.7711 0.070 Uiso 1 1 calc R . . C1L C 0.1480(4) 0.1971(3) 0.8692(6) 0.035(3) Uani 1 1 d . . . C2L C 0.1105(5) 0.2156(3) 0.9037(7) 0.049(3) Uani 1 1 d . . . H2L H 0.0785 0.2142 0.8870 0.059 Uiso 1 1 calc R . . C3L C 0.1214(5) 0.2365(4) 0.9642(7) 0.060(4) Uani 1 1 d . . . H3L H 0.0967 0.2499 0.9879 0.072 Uiso 1 1 calc R . . C4L C 0.1686(5) 0.2373(4) 0.9890(7) 0.050(3) Uani 1 1 d . . . H4L H 0.1754 0.2496 1.0314 0.059 Uiso 1 1 calc R . . C5L C 0.2048(4) 0.2207(3) 0.9528(7) 0.048(3) Uani 1 1 d . . . H5L H 0.2371 0.2229 0.9685 0.057 Uiso 1 1 calc R . . C6L C 0.1949(4) 0.2001(3) 0.8922(7) 0.045(3) Uani 1 1 d . . . H6L H 0.2204 0.1883 0.8673 0.054 Uiso 1 1 calc R . . C1M C 0.2478(4) 0.0825(3) 0.3281(6) 0.035(3) Uani 1 1 d . . . C2M C 0.2951(5) 0.0905(4) 0.3109(8) 0.064(4) Uani 1 1 d . . . H2M H 0.3022 0.1088 0.2760 0.076 Uiso 1 1 calc R . . C3M C 0.3315(6) 0.0719(5) 0.3447(10) 0.088(6) Uani 1 1 d . . . H3M H 0.3640 0.0783 0.3357 0.106 Uiso 1 1 calc R . . C4M C 0.3202(9) 0.0430(5) 0.3930(11) 0.105(8) Uani 1 1 d . . . H4M H 0.3454 0.0289 0.4142 0.127 Uiso 1 1 calc R . . C5M C 0.2748(7) 0.0353(5) 0.4091(9) 0.083(5) Uani 1 1 d . . . H5M H 0.2680 0.0168 0.4436 0.099 Uiso 1 1 calc R . . C6M C 0.2383(5) 0.0537(4) 0.3769(7) 0.055(4) Uani 1 1 d . . . H6M H 0.2060 0.0470 0.3873 0.066 Uiso 1 1 calc R . . C1N C 0.2190(4) 0.1190(3) 0.2025(6) 0.036(3) Uani 1 1 d . . . C2N C 0.2363(4) 0.0897(3) 0.1594(6) 0.046(3) Uani 1 1 d . . . H2N H 0.2359 0.0637 0.1747 0.055 Uiso 1 1 calc R . . C3N C 0.2534(5) 0.0980(4) 0.0965(7) 0.063(4) Uani 1 1 d . . . H3N H 0.2661 0.0778 0.0688 0.075 Uiso 1 1 calc R . . C4N C 0.2529(5) 0.1365(4) 0.0713(6) 0.055(4) Uani 1 1 d . . . H4N H 0.2628 0.1417 0.0257 0.066 Uiso 1 1 calc R . . C5N C 0.2380(5) 0.1659(4) 0.1126(7) 0.054(4) Uani 1 1 d . . . H5N H 0.2396 0.1919 0.0973 0.065 Uiso 1 1 calc R . . C6N C 0.2206(4) 0.1572(3) 0.1771(6) 0.038(3) Uani 1 1 d . . . H6N H 0.2093 0.1777 0.2053 0.046 Uiso 1 1 calc R . . C1O C 0.1173(4) 0.2207(3) 0.2278(5) 0.031(3) Uani 1 1 d . . . C2O C 0.0836(4) 0.2292(4) 0.1757(7) 0.054(4) Uani 1 1 d . . . H2O H 0.0588 0.2113 0.1650 0.064 Uiso 1 1 calc R . . C3O C 0.0868(5) 0.2645(4) 0.1395(6) 0.050(4) Uani 1 1 d . . . H3O H 0.0633 0.2707 0.1060 0.060 Uiso 1 1 calc R . . C4O C 0.1234(5) 0.2899(4) 0.1525(7) 0.058(4) Uani 1 1 d . . . H4O H 0.1249 0.3139 0.1289 0.070 Uiso 1 1 calc R . . C5O C 0.1572(5) 0.2806(4) 0.1986(6) 0.049(3) Uani 1 1 d . . . H5O H 0.1831 0.2981 0.2051 0.059 Uiso 1 1 calc R . . C6O C 0.1568(4) 0.2467(3) 0.2379(6) 0.040(3) Uani 1 1 d . . . H6O H 0.1816 0.2412 0.2698 0.047 Uiso 1 1 calc R . . C1P C 0.0622(4) 0.1940(4) 0.3457(6) 0.038(3) Uani 1 1 d . . . C2P C 0.0399(4) 0.2304(4) 0.3397(7) 0.049(3) Uani 1 1 d . . . H2P H 0.0459 0.2464 0.3011 0.058 Uiso 1 1 calc R . . C3P C 0.0090(4) 0.2425(4) 0.3916(7) 0.045(3) Uani 1 1 d . . . H3P H -0.0062 0.2670 0.3884 0.054 Uiso 1 1 calc R . . C4P C 0.0002(4) 0.2193(5) 0.4474(7) 0.058(4) Uani 1 1 d . . . H4P H -0.0199 0.2288 0.4828 0.070 Uiso 1 1 calc R . . C5P C 0.0204(4) 0.1815(4) 0.4541(7) 0.048(3) Uani 1 1 d . . . H5P H 0.0128 0.1650 0.4915 0.058 Uiso 1 1 calc R . . C6P C 0.0522(4) 0.1702(3) 0.4014(5) 0.033(3) Uani 1 1 d . . . H6P H 0.0673 0.1456 0.4040 0.039 Uiso 1 1 calc R . . S1 S 0.00865(17) 0.33681(16) 0.0220(3) 0.1001(17) Uani 1 1 d D . . O9 O -0.0144(5) 0.3202(5) 0.0936(11) 0.192(9) Uani 1 1 d D . . O10 O 0.0502(4) 0.3160(3) 0.0014(7) 0.106(4) Uani 1 1 d D . . O11 O -0.0268(6) 0.3474(5) -0.0194(7) 0.193(9) Uani 1 1 d D . . C73 C 0.0311(6) 0.3794(5) 0.0609(12) 0.131(9) Uani 1 1 d D . . F1 F 0.0511(6) 0.3987(4) 0.0037(14) 0.295(15) Uani 1 1 d D . . F2 F -0.0018(5) 0.4000(4) 0.0888(9) 0.166(6) Uani 1 1 d D . . F3 F 0.0640(6) 0.3731(4) 0.1067(10) 0.199(8) Uani 1 1 d D . . S2 S 0.97600(14) 0.33021(12) 0.5125(2) 0.0676(11) Uani 1 1 d D . . O12 O 1.0246(4) 0.3304(4) 0.4992(8) 0.128(6) Uani 1 1 d D . . O13 O 0.9496(7) 0.3005(4) 0.5350(8) 0.182(9) Uani 1 1 d D . . O14 O 0.9531(6) 0.3438(6) 0.4500(7) 0.179(8) Uani 1 1 d D . . C74 C 0.9645(7) 0.3685(5) 0.5693(10) 0.103(7) Uani 1 1 d D . . F4 F 0.9910(9) 0.3656(8) 0.6209(10) 0.281(13) Uani 1 1 d D . . F5 F 0.9858(8) 0.4001(4) 0.5475(14) 0.261(13) Uani 1 1 d D . . F6 F 0.9227(5) 0.3749(5) 0.5816(10) 0.233(10) Uani 1 1 d D . . C75 C 0.9405(4) 0.0347(5) 0.0478(7) 0.070(5) Uani 1 1 d D . . F7 F 0.9493(6) 0.0091(5) 0.0914(10) 0.242(9) Uani 1 1 d DU . . F8 F 0.9464(4) 0.0211(4) -0.0083(7) 0.163(6) Uani 1 1 d DU . . F9 F 0.9775(4) 0.0575(5) 0.0544(8) 0.192(7) Uani 1 1 d DU . . S3 S 0.88639(14) 0.05996(13) 0.06859(19) 0.0652(12) Uani 1 1 d D . . O15 O 0.8775(6) 0.0841(6) 0.0186(8) 0.185(8) Uani 1 1 d DU . . O16 O 0.8527(5) 0.0264(5) 0.0615(10) 0.189(8) Uani 1 1 d DU . . O17 O 0.8885(4) 0.0715(4) 0.1351(6) 0.116(5) Uani 1 1 d DU . . S4 S 0.0888(2) 0.07899(13) 0.5507(2) 0.0816(15) Uani 1 1 d D . . O18 O 0.1003(4) 0.0868(3) 0.6186(5) 0.095(4) Uani 1 1 d DU . . O19 O 0.1287(6) 0.0692(5) 0.5082(7) 0.166(7) Uani 1 1 d DU . . O20 O 0.0629(10) 0.1058(5) 0.5169(12) 0.240(10) Uani 1 1 d DU . . C76 C 0.0534(5) 0.0371(4) 0.5509(8) 0.072(5) Uani 1 1 d D . . F10 F 0.0413(4) 0.0265(3) 0.4857(6) 0.116(4) Uani 1 1 d DU . . F11 F 0.0161(4) 0.0395(4) 0.5873(8) 0.198(8) Uani 1 1 d D . . F12 F 0.0795(6) 0.0066(3) 0.5738(6) 0.148(5) Uani 1 1 d D . . C2S C 0.5331(9) 0.1339(6) 0.6683(13) 0.132(8) Uani 1 1 d . . . H2S H 0.5216 0.1443 0.6234 0.159 Uiso 1 1 calc R . . Cl4 Cl 0.5791(4) 0.1624(3) 0.6974(5) 0.258(6) Uani 1 1 d . . . Cl5 Cl 0.5547(3) 0.0860(2) 0.6558(5) 0.186(3) Uani 1 1 d . . . Cl6 Cl 0.4851(4) 0.1317(3) 0.7239(6) 0.270(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0270(4) 0.0281(5) 0.0322(5) -0.0040(4) -0.0015(4) 0.0019(4) Pd2 0.0308(5) 0.0280(5) 0.0304(5) -0.0021(4) -0.0007(4) 0.0026(4) Pd3 0.0258(4) 0.0274(4) 0.0273(4) -0.0012(4) 0.0020(4) -0.0029(3) Pd4 0.0291(4) 0.0316(5) 0.0263(4) -0.0023(4) -0.0016(4) -0.0049(4) Fe1 0.0398(10) 0.0324(9) 0.0347(10) -0.0070(7) 0.0028(8) 0.0026(7) Fe2 0.0364(10) 0.0368(10) 0.0445(10) 0.0023(8) -0.0087(8) -0.0009(8) Fe3 0.0290(9) 0.0346(9) 0.0330(9) 0.0025(8) 0.0053(7) 0.0000(7) Fe4 0.0380(9) 0.0395(10) 0.0322(9) -0.0095(8) -0.0017(8) -0.0094(8) P1 0.0316(16) 0.0304(16) 0.0348(17) -0.0059(13) 0.0003(14) 0.0014(13) P2 0.0288(16) 0.0313(16) 0.0444(18) -0.0083(14) -0.0022(14) 0.0023(13) P3 0.0249(15) 0.0355(17) 0.0397(18) -0.0044(14) 0.0007(13) 0.0006(13) P4 0.0300(16) 0.0315(16) 0.0326(17) 0.0021(13) -0.0026(13) -0.0010(13) P5 0.0302(16) 0.0268(16) 0.0339(16) 0.0023(13) 0.0043(13) -0.0007(12) P6 0.0262(15) 0.0279(16) 0.0338(16) -0.0005(13) 0.0019(12) -0.0012(12) P7 0.0339(17) 0.0317(16) 0.0340(17) -0.0024(13) -0.0016(13) -0.0005(13) P8 0.0328(17) 0.0351(17) 0.0288(16) -0.0032(13) -0.0051(13) -0.0036(13) N1 0.046(6) 0.032(5) 0.024(5) -0.003(4) -0.007(4) 0.012(4) N2 0.032(5) 0.028(5) 0.029(5) -0.004(4) -0.004(4) -0.001(4) N3 0.026(5) 0.036(5) 0.029(5) 0.002(4) -0.002(4) -0.008(4) N4 0.034(5) 0.043(6) 0.028(5) 0.007(5) 0.002(4) -0.013(5) O1 0.031(4) 0.037(5) 0.032(4) -0.008(3) 0.002(3) 0.006(4) O2 0.044(5) 0.044(5) 0.038(5) 0.001(4) 0.003(4) 0.006(4) O3 0.035(4) 0.042(5) 0.035(4) 0.001(4) -0.011(4) 0.005(4) O4 0.046(5) 0.039(5) 0.061(6) -0.013(4) 0.010(4) 0.004(4) O5 0.031(4) 0.027(4) 0.041(5) -0.003(3) 0.011(4) -0.002(3) O6 0.034(5) 0.041(5) 0.051(5) -0.003(4) 0.008(4) -0.013(4) O7 0.028(4) 0.037(5) 0.048(5) -0.013(4) -0.002(4) -0.011(4) O8 0.033(5) 0.056(5) 0.044(5) -0.006(4) 0.012(4) -0.010(4) C1 0.042(8) 0.034(7) 0.021(6) -0.005(5) 0.018(6) -0.002(6) C2 0.045(7) 0.016(6) 0.041(7) -0.015(5) 0.000(6) -0.002(5) C3 0.021(6) 0.041(7) 0.029(6) -0.008(5) 0.006(5) -0.007(5) C4 0.058(8) 0.041(7) 0.034(7) -0.011(6) 0.009(6) 0.020(6) C5 0.063(8) 0.023(6) 0.031(7) -0.004(5) -0.010(6) 0.005(6) C6 0.026(6) 0.031(7) 0.037(7) 0.003(5) -0.009(5) -0.003(5) C7 0.039(7) 0.038(7) 0.028(6) -0.005(5) -0.006(5) 0.010(6) C8 0.033(6) 0.020(6) 0.051(8) -0.003(5) -0.003(6) 0.002(5) C9 0.040(7) 0.047(8) 0.034(7) 0.007(6) 0.007(5) 0.006(6) C10 0.028(6) 0.061(8) 0.031(6) -0.009(6) 0.003(5) 0.012(6) C11 0.044(7) 0.036(7) 0.045(7) 0.010(6) 0.007(6) -0.006(6) C12 0.031(6) 0.035(6) 0.032(6) 0.006(5) -0.011(5) 0.014(5) C13 0.024(6) 0.043(7) 0.041(7) 0.001(6) -0.005(5) 0.013(5) C14 0.027(6) 0.041(7) 0.033(7) -0.007(5) 0.004(5) -0.001(5) C15 0.039(7) 0.035(7) 0.034(7) -0.001(5) -0.003(6) -0.003(6) C16 0.036(7) 0.033(7) 0.041(7) -0.011(6) -0.011(6) 0.006(5) C17 0.035(6) 0.027(6) 0.038(7) -0.006(5) -0.008(5) -0.006(5) C18 0.034(6) 0.039(7) 0.029(6) 0.000(5) -0.005(5) -0.009(5) C19 0.055(8) 0.041(7) 0.043(8) -0.008(6) 0.012(7) -0.003(6) C20 0.056(8) 0.062(9) 0.029(7) 0.002(6) -0.002(7) -0.008(7) C21 0.037(7) 0.042(7) 0.038(7) -0.004(6) 0.003(6) -0.005(6) C22 0.043(7) 0.018(6) 0.035(6) 0.000(5) -0.017(5) -0.004(5) C23 0.056(8) 0.034(7) 0.039(7) -0.003(6) 0.005(6) -0.011(6) C24 0.068(9) 0.026(6) 0.058(9) 0.003(6) 0.026(8) 0.005(6) C25 0.037(7) 0.048(8) 0.072(10) -0.006(7) -0.010(7) 0.022(6) C26 0.029(6) 0.047(7) 0.031(6) 0.011(6) -0.001(5) 0.006(5) C27 0.036(7) 0.025(6) 0.043(7) -0.006(5) -0.003(6) 0.000(5) C28 0.055(8) 0.042(8) 0.049(8) 0.000(6) -0.021(7) 0.002(6) C29 0.045(8) 0.045(8) 0.095(12) 0.001(8) -0.024(8) 0.018(7) C30 0.056(9) 0.038(8) 0.106(13) -0.002(9) 0.026(9) 0.001(7) C31 0.032(7) 0.030(7) 0.051(8) -0.007(6) 0.000(6) 0.000(5) C32 0.033(6) 0.038(7) 0.036(7) 0.011(5) -0.005(5) -0.001(5) C33 0.033(6) 0.025(6) 0.038(7) -0.002(5) -0.006(6) 0.009(5) C34 0.034(8) 0.043(8) 0.091(11) 0.013(8) -0.009(8) -0.004(6) C35 0.057(9) 0.056(9) 0.043(8) 0.010(7) -0.017(7) -0.010(7) C36 0.056(8) 0.048(8) 0.028(6) -0.003(6) -0.006(6) -0.013(7) C37 0.022(6) 0.057(8) 0.036(7) 0.001(6) 0.003(5) 0.000(6) C38 0.056(8) 0.058(8) 0.029(7) 0.002(6) 0.003(6) -0.020(7) C39 0.035(7) 0.045(7) 0.039(7) 0.011(6) 0.006(6) 0.004(6) C40 0.034(7) 0.025(6) 0.042(7) -0.006(5) 0.014(6) -0.017(5) C41 0.040(7) 0.039(7) 0.021(6) 0.008(5) 0.003(5) -0.005(6) C42 0.029(6) 0.030(6) 0.033(6) 0.000(5) -0.001(5) 0.003(5) C43 0.034(7) 0.063(9) 0.045(8) 0.005(7) 0.004(6) -0.007(6) C44 0.039(7) 0.048(8) 0.045(8) 0.011(6) -0.010(6) -0.006(6) C45 0.045(8) 0.042(7) 0.022(6) 0.001(5) -0.013(6) 0.005(6) C46 0.033(7) 0.053(8) 0.035(7) -0.006(6) -0.010(6) 0.009(6) C47 0.046(7) 0.041(7) 0.033(7) -0.014(6) 0.012(6) 0.001(6) C48 0.035(7) 0.039(7) 0.042(7) -0.013(6) -0.009(6) -0.013(5) C49 0.051(7) 0.015(5) 0.038(7) -0.001(5) 0.002(6) -0.005(5) C50 0.026(6) 0.025(6) 0.028(6) -0.011(5) 0.004(5) 0.016(5) C51 0.031(6) 0.032(7) 0.035(7) -0.006(5) -0.003(5) -0.002(5) C52 0.028(6) 0.034(6) 0.037(7) -0.009(5) 0.007(5) -0.005(5) C53 0.021(6) 0.034(6) 0.038(7) 0.005(5) -0.004(5) 0.003(5) C54 0.047(7) 0.034(7) 0.036(7) -0.005(5) 0.001(6) 0.016(6) C55 0.054(8) 0.036(8) 0.054(9) 0.015(7) 0.005(7) -0.006(6) C56 0.034(7) 0.105(12) 0.024(7) 0.014(7) 0.015(6) 0.019(7) C57 0.036(7) 0.041(7) 0.032(6) 0.000(5) -0.001(5) 0.000(6) C58 0.021(6) 0.039(7) 0.028(6) 0.000(5) 0.007(5) 0.008(5) C59 0.034(7) 0.032(7) 0.048(8) 0.000(6) 0.016(6) 0.008(5) C60 0.038(7) 0.053(8) 0.056(9) 0.015(7) -0.003(6) 0.015(6) C61 0.030(7) 0.032(7) 0.061(9) 0.001(6) -0.005(6) -0.021(5) C62 0.038(7) 0.047(7) 0.027(6) -0.006(5) 0.001(5) -0.004(6) C63 0.032(6) 0.033(6) 0.034(7) -0.006(5) -0.005(5) 0.005(5) C64 0.059(8) 0.039(7) 0.034(7) -0.011(6) 0.002(6) 0.003(6) C65 0.048(8) 0.035(7) 0.068(10) -0.021(7) 0.004(7) -0.005(6) C66 0.049(8) 0.036(7) 0.059(9) 0.008(6) 0.006(7) -0.009(6) C67 0.054(8) 0.043(7) 0.014(5) -0.004(5) 0.014(5) -0.018(6) C68 0.043(6) 0.029(6) 0.022(5) -0.002(5) 0.001(5) -0.003(5) C69 0.023(6) 0.048(7) 0.041(7) -0.005(6) 0.014(5) -0.009(5) C70 0.047(8) 0.076(10) 0.037(8) -0.024(7) -0.011(6) -0.018(7) C71 0.062(9) 0.066(9) 0.027(7) -0.021(6) -0.001(6) -0.022(7) C72 0.035(7) 0.054(8) 0.031(7) -0.001(6) -0.006(6) -0.006(6) C1A 0.028(7) 0.044(8) 0.049(8) -0.013(7) -0.003(6) 0.002(6) C2A 0.034(7) 0.062(9) 0.060(9) -0.022(7) -0.002(7) 0.003(6) C3A 0.040(9) 0.084(12) 0.068(11) -0.023(9) 0.001(8) -0.016(8) C4A 0.028(7) 0.090(12) 0.067(11) -0.033(10) -0.002(7) 0.008(8) C5A 0.051(9) 0.082(11) 0.047(9) -0.023(8) 0.000(7) 0.013(8) C6A 0.024(6) 0.047(8) 0.051(8) -0.027(7) 0.008(5) 0.000(6) C1B 0.031(6) 0.049(7) 0.035(7) -0.004(6) 0.000(6) 0.002(5) C2B 0.040(7) 0.024(6) 0.053(8) 0.004(6) 0.018(6) 0.002(5) C3B 0.043(8) 0.061(9) 0.061(9) -0.001(8) -0.001(7) -0.010(7) C4B 0.030(7) 0.066(9) 0.041(8) 0.008(7) -0.002(6) 0.010(6) C5B 0.036(7) 0.053(8) 0.052(8) -0.006(7) 0.004(7) 0.011(6) C6B 0.036(7) 0.050(7) 0.032(7) 0.001(6) -0.006(6) -0.015(6) C1C 0.037(8) 0.047(8) 0.079(10) -0.022(8) 0.012(7) -0.007(6) C2C 0.027(8) 0.070(10) 0.121(14) -0.005(10) 0.003(8) 0.006(7) C3C 0.046(10) 0.071(12) 0.141(17) 0.005(11) 0.024(11) 0.017(9) C4C 0.074(13) 0.047(10) 0.146(17) -0.006(11) 0.033(12) -0.014(9) C5C 0.078(11) 0.040(8) 0.089(12) -0.021(8) 0.039(10) -0.020(8) C6C 0.045(8) 0.048(8) 0.063(9) -0.026(7) 0.017(7) -0.013(7) C1D 0.036(7) 0.040(7) 0.077(10) -0.008(7) -0.023(7) 0.013(6) C2D 0.096(12) 0.030(7) 0.108(13) -0.021(8) -0.074(10) 0.001(7) C3D 0.159(19) 0.058(11) 0.159(19) -0.049(12) -0.114(17) 0.045(12) C4D 0.19(2) 0.054(11) 0.156(19) -0.025(12) -0.149(18) 0.036(12) C5D 0.095(12) 0.046(9) 0.084(11) 0.013(9) -0.046(10) 0.017(8) C6D 0.054(8) 0.031(7) 0.071(9) -0.022(7) -0.029(7) 0.013(6) C1E 0.022(6) 0.049(7) 0.036(7) 0.005(6) -0.010(5) -0.004(5) C2E 0.038(8) 0.037(8) 0.103(12) 0.009(8) 0.017(8) -0.004(6) C3E 0.033(8) 0.068(10) 0.125(15) 0.040(10) -0.010(10) -0.003(7) C4E 0.059(11) 0.094(14) 0.094(14) 0.058(11) -0.035(10) -0.023(10) C5E 0.036(8) 0.136(16) 0.038(8) 0.011(9) 0.006(7) -0.027(9) C6E 0.017(6) 0.076(9) 0.042(7) 0.001(7) -0.006(6) -0.004(6) C1F 0.041(7) 0.036(7) 0.031(6) -0.017(5) -0.003(6) 0.007(5) C2F 0.034(8) 0.109(13) 0.074(10) -0.059(10) 0.003(7) -0.006(8) C3F 0.047(9) 0.106(13) 0.103(13) -0.077(11) -0.001(9) 0.012(9) C4F 0.044(9) 0.095(12) 0.070(10) -0.046(9) 0.003(8) 0.010(8) C5F 0.037(8) 0.134(16) 0.090(12) -0.058(11) 0.014(9) 0.002(9) C6F 0.038(8) 0.081(11) 0.063(9) -0.045(8) 0.001(7) -0.003(7) C1G 0.036(7) 0.031(6) 0.042(7) -0.009(6) 0.000(6) 0.000(5) C2G 0.036(7) 0.043(8) 0.055(8) 0.012(6) 0.010(6) 0.005(6) C3G 0.074(11) 0.061(10) 0.048(8) 0.012(7) 0.010(8) -0.022(8) C4G 0.053(9) 0.058(10) 0.062(9) -0.009(8) 0.015(7) -0.026(8) C5G 0.031(7) 0.067(10) 0.056(9) -0.009(7) 0.007(6) 0.020(6) C6G 0.041(7) 0.036(7) 0.043(7) -0.006(6) 0.002(6) -0.004(6) C1H 0.043(7) 0.027(6) 0.039(7) 0.002(5) 0.012(6) 0.002(5) C2H 0.049(8) 0.043(7) 0.043(7) -0.004(6) 0.003(6) -0.011(6) C3H 0.074(11) 0.072(10) 0.055(9) -0.007(8) -0.019(9) -0.022(8) C4H 0.095(12) 0.043(8) 0.044(9) -0.012(7) -0.015(9) 0.011(8) C5H 0.053(9) 0.048(8) 0.051(8) -0.017(7) -0.018(7) 0.008(7) C6H 0.037(7) 0.044(7) 0.049(8) -0.007(6) -0.006(6) 0.002(6) C1I 0.045(7) 0.041(7) 0.033(7) -0.002(6) 0.021(6) 0.003(6) C2I 0.061(9) 0.047(8) 0.080(11) -0.014(8) 0.013(9) -0.005(7) C3I 0.073(12) 0.062(10) 0.108(14) 0.010(10) 0.054(11) 0.032(9) C4I 0.101(14) 0.052(10) 0.060(11) 0.011(8) 0.025(10) 0.002(10) C5I 0.108(13) 0.036(8) 0.037(8) 0.003(6) 0.007(8) -0.015(8) C6I 0.060(9) 0.030(7) 0.055(8) 0.011(6) 0.000(7) 0.000(6) C1J 0.033(7) 0.043(7) 0.038(7) -0.004(6) 0.002(6) 0.016(6) C2J 0.034(7) 0.076(10) 0.066(9) 0.025(8) -0.022(7) -0.012(7) C3J 0.055(10) 0.068(11) 0.102(13) 0.032(10) -0.017(9) -0.011(8) C4J 0.029(8) 0.087(12) 0.078(11) -0.002(9) -0.019(7) -0.011(8) C5J 0.039(7) 0.062(9) 0.052(8) 0.005(7) -0.011(6) -0.015(6) C6J 0.036(7) 0.027(6) 0.054(8) 0.000(6) 0.000(6) -0.008(5) C1K 0.045(7) 0.028(6) 0.040(7) 0.012(5) 0.015(6) 0.007(5) C2K 0.025(6) 0.050(8) 0.053(8) 0.012(6) -0.010(6) 0.001(5) C3K 0.049(9) 0.079(11) 0.050(9) 0.026(8) -0.004(7) -0.012(8) C4K 0.025(8) 0.118(15) 0.095(13) 0.054(12) 0.006(8) 0.012(8) C5K 0.055(10) 0.069(10) 0.080(11) 0.019(9) 0.000(9) 0.022(8) C6K 0.047(8) 0.044(8) 0.083(11) -0.008(7) 0.000(8) 0.013(6) C1L 0.040(7) 0.025(6) 0.038(7) -0.001(5) 0.001(6) -0.011(5) C2L 0.042(8) 0.038(7) 0.067(9) -0.019(7) 0.006(7) -0.001(6) C3L 0.052(9) 0.058(9) 0.069(10) -0.040(8) 0.015(8) -0.003(7) C4L 0.043(8) 0.056(9) 0.050(8) -0.021(7) -0.001(7) -0.014(7) C5L 0.034(7) 0.044(8) 0.065(9) -0.022(7) -0.012(7) -0.011(6) C6L 0.041(8) 0.037(7) 0.058(8) -0.016(6) 0.005(6) -0.003(6) C1M 0.033(7) 0.035(7) 0.035(7) -0.014(6) -0.019(5) 0.008(5) C2M 0.033(8) 0.073(10) 0.084(11) 0.015(8) -0.015(8) 0.010(7) C3M 0.053(10) 0.098(14) 0.113(15) -0.052(13) -0.025(11) 0.005(10) C4M 0.15(2) 0.056(12) 0.113(17) -0.035(11) -0.075(16) 0.048(13) C5M 0.082(13) 0.082(13) 0.083(13) 0.006(10) -0.032(12) 0.018(11) C6M 0.061(9) 0.051(8) 0.053(9) -0.004(7) -0.015(8) -0.004(7) C1N 0.031(6) 0.036(7) 0.041(7) -0.002(6) -0.008(5) -0.014(5) C2N 0.060(8) 0.036(7) 0.043(7) 0.011(6) 0.020(7) 0.005(6) C3N 0.092(11) 0.044(9) 0.051(8) -0.010(7) 0.035(8) 0.004(8) C4N 0.067(10) 0.067(10) 0.031(7) -0.015(7) 0.008(7) -0.018(8) C5N 0.077(10) 0.035(7) 0.050(8) 0.003(7) 0.018(7) -0.019(7) C6N 0.039(7) 0.042(7) 0.034(6) 0.000(6) -0.004(5) -0.013(6) C1O 0.045(7) 0.024(6) 0.024(6) -0.002(5) -0.004(5) 0.007(5) C2O 0.033(7) 0.065(9) 0.063(9) 0.019(8) 0.005(7) 0.002(6) C3O 0.053(9) 0.057(9) 0.039(8) 0.014(7) 0.019(7) 0.026(7) C4O 0.061(9) 0.056(9) 0.056(9) 0.023(8) 0.019(8) 0.012(8) C5O 0.058(9) 0.048(8) 0.042(8) 0.008(7) 0.011(7) -0.021(7) C6O 0.044(7) 0.046(7) 0.029(6) 0.002(6) 0.006(6) 0.008(6) C1P 0.027(6) 0.055(8) 0.033(7) -0.007(6) -0.002(5) -0.007(6) C2P 0.052(8) 0.056(9) 0.038(7) -0.008(7) -0.004(6) 0.017(7) C3P 0.028(7) 0.055(8) 0.051(8) -0.008(7) -0.020(6) 0.016(6) C4P 0.020(7) 0.103(13) 0.052(9) -0.028(9) -0.017(6) 0.004(7) C5P 0.044(8) 0.057(9) 0.044(8) -0.005(7) -0.015(6) -0.016(7) C6P 0.028(6) 0.038(7) 0.032(6) -0.008(5) 0.010(5) -0.021(5) S1 0.069(3) 0.107(4) 0.125(4) -0.023(3) -0.029(3) 0.036(3) O9 0.117(12) 0.195(17) 0.26(2) 0.132(16) 0.082(14) 0.005(11) O10 0.091(9) 0.102(9) 0.125(11) -0.002(8) 0.003(8) 0.040(7) O11 0.193(16) 0.28(2) 0.108(11) -0.038(13) -0.079(11) 0.160(17) C73 0.057(14) 0.13(2) 0.20(3) 0.00(2) 0.002(16) 0.012(14) F1 0.203(18) 0.195(17) 0.49(4) 0.17(2) 0.19(2) 0.029(14) F2 0.109(10) 0.109(10) 0.281(18) -0.069(11) 0.032(11) 0.015(8) F3 0.157(13) 0.143(12) 0.30(2) -0.102(14) -0.095(15) 0.013(10) S2 0.050(2) 0.071(3) 0.082(3) 0.006(2) 0.011(2) 0.003(2) O12 0.055(7) 0.133(12) 0.195(14) -0.089(11) 0.009(8) -0.004(7) O13 0.233(19) 0.175(15) 0.138(13) -0.073(12) 0.126(13) -0.126(15) O14 0.178(16) 0.26(2) 0.096(11) 0.036(13) -0.029(11) 0.089(16) C74 0.090(16) 0.100(17) 0.120(18) -0.046(14) -0.006(14) 0.018(13) F4 0.27(3) 0.38(3) 0.193(19) -0.17(2) -0.072(19) 0.01(2) F5 0.29(2) 0.061(10) 0.43(4) 0.003(14) 0.13(2) 0.012(12) F6 0.078(9) 0.28(2) 0.34(2) -0.186(18) 0.066(12) 0.032(10) C75 0.055(10) 0.101(14) 0.055(10) -0.009(10) -0.030(8) 0.029(9) F7 0.223(15) 0.224(14) 0.278(17) 0.184(14) 0.141(13) 0.163(12) F8 0.082(7) 0.233(13) 0.173(11) -0.162(11) 0.011(8) 0.004(8) F9 0.062(7) 0.294(17) 0.221(14) -0.181(13) 0.000(8) -0.032(9) S3 0.063(3) 0.093(3) 0.039(2) -0.009(2) -0.0069(18) 0.035(2) O15 0.163(13) 0.266(18) 0.126(11) 0.063(12) 0.060(10) 0.160(13) O16 0.134(12) 0.210(15) 0.222(16) -0.130(14) 0.070(12) -0.092(12) O17 0.107(9) 0.162(12) 0.079(8) -0.055(8) 0.003(7) 0.021(8) S4 0.119(4) 0.077(3) 0.048(2) -0.003(2) -0.003(3) -0.053(3) O18 0.115(9) 0.118(9) 0.053(6) -0.027(6) -0.015(6) -0.048(7) O19 0.168(13) 0.222(15) 0.110(10) -0.056(10) 0.081(10) -0.150(12) O20 0.37(2) 0.132(14) 0.214(18) 0.055(14) -0.100(18) 0.018(16) C76 0.063(11) 0.074(12) 0.080(12) -0.020(10) 0.014(9) -0.010(9) F10 0.106(8) 0.121(8) 0.120(8) -0.045(7) -0.017(7) -0.026(6) F11 0.135(10) 0.166(12) 0.293(18) -0.147(13) 0.156(12) -0.079(9) F12 0.243(16) 0.072(7) 0.129(10) 0.033(7) -0.010(10) 0.024(9) C2S 0.17(2) 0.095(16) 0.13(2) -0.003(14) -0.043(18) 0.000(15) Cl4 0.400(15) 0.182(8) 0.193(8) 0.055(7) -0.132(10) -0.132(9) Cl5 0.175(7) 0.157(6) 0.226(9) -0.018(6) 0.002(7) 0.013(5) Cl6 0.318(14) 0.279(12) 0.213(10) 0.020(9) 0.080(10) 0.132(11) _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 O1S C5S 1.422(19) . ? O1S C4S 1.427(19) . ? C3S C4S 1.560(19) . ? C5S C6S 1.534(19) . ? C1S Cl2 1.749(10) . ? C1S Cl1 1.750(10) . ? C1S Cl3 1.754(10) . ? C1SA Cl3A 1.743(10) . ? C1SA Cl1A 1.744(10) . ? C1SA Cl2A 1.751(10) . ? Pd1 O1 2.037(7) . ? Pd1 N2 2.105(8) . ? Pd1 P2 2.263(3) . ? Pd1 P1 2.291(3) . ? Pd2 O3 2.076(7) . ? Pd2 N1 2.077(9) . ? Pd2 P3 2.278(3) . ? Pd2 P4 2.281(3) . ? Pd3 O5 2.057(7) . ? Pd3 N3 2.083(8) . ? Pd3 P5 2.272(3) . ? Pd3 P6 2.285(3) . ? Pd4 O7 2.050(7) . ? Pd4 N4 2.094(9) . ? Pd4 P7 2.273(3) . ? Pd4 P8 2.288(3) . ? Fe1 C17 1.998(10) . ? Fe1 C22 2.007(11) . ? Fe1 C21 2.012(12) . ? Fe1 C24 2.026(11) . ? Fe1 C18 2.030(10) . ? Fe1 C26 2.033(11) . ? Fe1 C20 2.040(12) . ? Fe1 C23 2.047(11) . ? Fe1 C19 2.050(12) . ? Fe1 C25 2.058(13) . ? Fe2 C27 2.001(11) . ? Fe2 C28 2.021(12) . ? Fe2 C32 2.027(11) . ? Fe2 C31 2.030(12) . ? Fe2 C34 2.045(13) . ? Fe2 C30 2.045(14) . ? Fe2 C36 2.050(12) . ? Fe2 C29 2.055(13) . ? Fe2 C33 2.064(10) . ? Fe2 C35 2.080(13) . ? Fe3 C58 2.020(10) . ? Fe3 C57 2.020(11) . ? Fe3 C62 2.023(11) . ? Fe3 C54 2.031(10) . ? Fe3 C53 2.037(10) . ? Fe3 C61 2.038(11) . ? Fe3 C55 2.042(12) . ? Fe3 C56 2.069(12) . ? Fe3 C59 2.074(10) . ? Fe3 C60 2.104(12) . ? Fe4 C64 2.016(12) . ? Fe4 C63 2.028(11) . ? Fe4 C70 2.027(12) . ? Fe4 C72 2.032(12) . ? Fe4 C69 2.034(11) . ? Fe4 C67 2.041(11) . ? Fe4 C68 2.043(10) . ? Fe4 C71 2.062(12) . ? Fe4 C66 2.068(12) . ? Fe4 C65 2.073(12) . ? P1 C1B 1.792(12) . ? P1 C17 1.797(11) . ? P1 C1A 1.804(12) . ? P2 C1D 1.781(13) . ? P2 C22 1.795(11) . ? P2 C1C 1.799(13) . ? P3 C27 1.804(11) . ? P3 C1F 1.831(11) . ? P3 C1E 1.840(11) . ? P4 C1G 1.779(11) . ? P4 C1H 1.821(12) . ? P4 C32 1.822(11) . ? P5 C53 1.774(11) . ? P5 C1J 1.812(12) . ? P5 C1I 1.828(11) . ? P6 C58 1.793(11) . ? P6 C1K 1.799(11) . ? P6 C1L 1.824(11) . ? P7 C63 1.801(11) . ? P7 C1N 1.804(12) . ? P7 C1M 1.818(11) . ? P8 C68 1.789(10) . ? P8 C1O 1.807(11) . ? P8 C1P 1.830(11) . ? N1 C4 1.336(13) . ? N1 C8 1.362(13) . ? N2 C12 1.328(12) . ? N2 C16 1.345(14) . ? N3 C52 1.335(13) . ? N3 C48 1.353(13) . ? N4 C44 1.312(13) . ? N4 C40 1.345(13) . ? O1 C1 1.312(12) . ? O2 C1 1.231(13) . ? O3 C9 1.306(13) . ? O4 C9 1.230(13) . ? O5 C37 1.291(13) . ? O6 C37 1.215(13) . ? O7 C45 1.275(13) . ? O8 C45 1.221(13) . ? C1 C2 1.516(14) . ? C2 C3 1.531(14) . ? C3 C6 1.534(14) . ? C4 C5 1.356(15) . ? C5 C6 1.385(15) . ? C6 C7 1.408(15) . ? C7 C8 1.353(15) . ? C9 C10 1.540(15) . ? C10 C11 1.514(15) . ? C11 C14 1.530(15) . ? C12 C13 1.359(15) . ? C13 C14 1.389(15) . ? C14 C15 1.367(15) . ? C15 C16 1.373(15) . ? C17 C21 1.385(15) . ? C17 C18 1.440(15) . ? C18 C19 1.401(15) . ? C19 C20 1.396(17) . ? C20 C21 1.405(16) . ? C22 C23 1.437(15) . ? C22 C26 1.462(14) . ? C23 C24 1.403(16) . ? C24 C25 1.418(17) . ? C25 C26 1.425(15) . ? C27 C28 1.413(16) . ? C27 C31 1.436(15) . ? C28 C29 1.376(17) . ? C29 C30 1.45(2) . ? C30 C31 1.462(18) . ? C32 C33 1.429(14) . ? C32 C36 1.443(15) . ? C33 C34 1.397(16) . ? C34 C35 1.436(18) . ? C35 C36 1.414(17) . ? C37 C38 1.563(15) . ? C38 C39 1.507(15) . ? C39 C42 1.484(15) . ? C40 C41 1.380(15) . ? C41 C42 1.377(15) . ? C42 C43 1.389(15) . ? C43 C44 1.403(15) . ? C45 C46 1.495(15) . ? C46 C47 1.554(15) . ? C47 C50 1.483(15) . ? C48 C49 1.362(15) . ? C49 C50 1.384(15) . ? C50 C51 1.417(14) . ? C51 C52 1.338(14) . ? C53 C57 1.432(15) . ? C53 C54 1.473(15) . ? C54 C55 1.436(16) . ? C55 C56 1.416(18) . ? C56 C57 1.439(16) . ? C58 C62 1.428(14) . ? C58 C59 1.462(15) . ? C59 C60 1.459(16) . ? C60 C61 1.402(17) . ? C61 C62 1.432(15) . ? C63 C67 1.433(14) . ? C63 C64 1.440(15) . ? C64 C65 1.387(16) . ? C65 C66 1.398(17) . ? C66 C67 1.391(15) . ? C68 C72 1.421(15) . ? C68 C69 1.441(14) . ? C69 C70 1.412(15) . ? C70 C71 1.393(17) . ? C71 C72 1.460(15) . ? C1A C6A 1.364(16) . ? C1A C2A 1.390(16) . ? C2A C3A 1.387(18) . ? C3A C4A 1.35(2) . ? C4A C5A 1.367(19) . ? C5A C6A 1.359(16) . ? C1B C2B 1.397(15) . ? C1B C6B 1.404(15) . ? C2B C3B 1.383(16) . ? C3B C4B 1.348(16) . ? C4B C5B 1.415(16) . ? C5B C6B 1.388(16) . ? C1C C2C 1.374(17) . ? C1C C6C 1.404(18) . ? C2C C3C 1.45(2) . ? C3C C4C 1.31(2) . ? C4C C5C 1.39(2) . ? C5C C6C 1.395(18) . ? C1D C2D 1.398(16) . ? C1D C6D 1.430(16) . ? C2D C3D 1.44(2) . ? C3D C4D 1.35(2) . ? C4D C5D 1.342(19) . ? C5D C6D 1.434(17) . ? C1E C6E 1.366(16) . ? C1E C2E 1.404(16) . ? C2E C3E 1.343(18) . ? C3E C4E 1.34(2) . ? C4E C5E 1.40(2) . ? C5E C6E 1.361(17) . ? C1F C6F 1.348(16) . ? C1F C2F 1.370(16) . ? C2F C3F 1.410(18) . ? C3F C4F 1.367(19) . ? C4F C5F 1.381(18) . ? C5F C6F 1.393(18) . ? C1G C2G 1.383(16) . ? C1G C6G 1.416(15) . ? C2G C3G 1.347(17) . ? C3G C4G 1.420(19) . ? C4G C5G 1.351(17) . ? C5G C6G 1.406(16) . ? C1H C6H 1.342(15) . ? C1H C2H 1.388(15) . ? C2H C3H 1.410(17) . ? C3H C4H 1.322(19) . ? C4H C5H 1.370(19) . ? C5H C6H 1.412(16) . ? C1I C2I 1.357(17) . ? C1I C6I 1.391(17) . ? C2I C3I 1.46(2) . ? C3I C4I 1.36(2) . ? C4I C5I 1.35(2) . ? C5I C6I 1.424(17) . ? C1J C6J 1.368(15) . ? C1J C2J 1.399(16) . ? C2J C3J 1.366(17) . ? C3J C4J 1.336(18) . ? C4J C5J 1.359(18) . ? C5J C6J 1.406(15) . ? C1K C6K 1.395(16) . ? C1K C2K 1.407(16) . ? C2K C3K 1.364(16) . ? C3K C4K 1.36(2) . ? C4K C5K 1.38(2) . ? C5K C6K 1.409(18) . ? C1L C6L 1.369(15) . ? C1L C2L 1.383(15) . ? C2L C3L 1.405(17) . ? C3L C4L 1.386(17) . ? C4L C5L 1.344(16) . ? C5L C6L 1.394(16) . ? C1M C2M 1.372(17) . ? C1M C6M 1.389(17) . ? C2M C3M 1.36(2) . ? C3M C4M 1.39(3) . ? C4M C5M 1.31(3) . ? C5M C6M 1.338(19) . ? C1N C2N 1.388(15) . ? C1N C6N 1.398(15) . ? C2N C3N 1.336(16) . ? C3N C4N 1.404(18) . ? C4N C5N 1.349(17) . ? C5N C6N 1.369(16) . ? C1O C2O 1.402(16) . ? C1O C6O 1.419(15) . ? C2O C3O 1.399(16) . ? C3O C4O 1.353(18) . ? C4O C5O 1.329(17) . ? C5O C6O 1.386(16) . ? C1P C6P 1.380(15) . ? C1P C2P 1.392(16) . ? C2P C3P 1.379(16) . ? C3P C4P 1.360(18) . ? C4P C5P 1.414(19) . ? C5P C6P 1.399(16) . ? S1 O11 1.314(12) . ? S1 O10 1.403(11) . ? S1 O9 1.626(15) . ? S1 C73 1.754(13) . ? C73 F2 1.268(19) . ? C73 F3 1.29(2) . ? C73 F1 1.40(3) . ? S2 O13 1.324(12) . ? S2 O12 1.361(11) . ? S2 O14 1.440(13) . ? S2 C74 1.738(11) . ? C74 F6 1.195(19) . ? C74 F4 1.24(2) . ? C74 F5 1.30(2) . ? C75 F8 1.192(15) . ? C75 F7 1.240(17) . ? C75 F9 1.288(18) . ? C75 S3 1.768(10) . ? S3 O15 1.295(14) . ? S3 O17 1.346(11) . ? S3 O16 1.482(14) . ? S4 O20 1.332(18) . ? S4 O18 1.376(10) . ? S4 O19 1.411(14) . ? S4 C76 1.733(10) . ? C76 F11 1.249(15) . ? C76 F12 1.341(18) . ? C76 F10 1.354(17) . ? C2S Cl4 1.69(2) . ? C2S Cl6 1.70(3) . ? C2S Cl5 1.76(2) . ? 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 C5S O1S C4S 116(2) . . ? O1S C4S C3S 104.7(17) . . ? O1S C5S C6S 105.5(18) . . ? Cl2 C1S Cl1 94.6(11) . . ? Cl2 C1S Cl3 98.7(11) . . ? Cl1 C1S Cl3 98.6(11) . . ? Cl3A C1SA Cl1A 97.4(10) . . ? Cl3A C1SA Cl2A 99.8(11) . . ? Cl1A C1SA Cl2A 97.2(10) . . ? O1 Pd1 N2 90.8(3) . . ? O1 Pd1 P2 177.4(2) . . ? N2 Pd1 P2 90.3(2) . . ? O1 Pd1 P1 79.7(2) . . ? N2 Pd1 P1 170.1(2) . . ? P2 Pd1 P1 99.05(11) . . ? O3 Pd2 N1 87.7(3) . . ? O3 Pd2 P3 176.8(2) . . ? N1 Pd2 P3 89.5(3) . . ? O3 Pd2 P4 84.4(2) . . ? N1 Pd2 P4 166.5(2) . . ? P3 Pd2 P4 98.72(11) . . ? O5 Pd3 N3 88.6(3) . . ? O5 Pd3 P5 83.1(2) . . ? N3 Pd3 P5 167.3(3) . . ? O5 Pd3 P6 177.2(2) . . ? N3 Pd3 P6 88.7(2) . . ? P5 Pd3 P6 99.65(10) . . ? O7 Pd4 N4 87.9(3) . . ? O7 Pd4 P7 178.9(2) . . ? N4 Pd4 P7 92.5(3) . . ? O7 Pd4 P8 81.9(2) . . ? N4 Pd4 P8 168.3(3) . . ? P7 Pd4 P8 97.52(11) . . ? C17 Fe1 C22 108.2(4) . . ? C17 Fe1 C21 40.4(4) . . ? C22 Fe1 C21 110.8(4) . . ? C17 Fe1 C24 176.6(5) . . ? C22 Fe1 C24 69.1(4) . . ? C21 Fe1 C24 138.0(5) . . ? C17 Fe1 C18 41.9(4) . . ? C22 Fe1 C18 136.4(4) . . ? C21 Fe1 C18 68.8(4) . . ? C24 Fe1 C18 141.5(5) . . ? C17 Fe1 C26 111.7(5) . . ? C22 Fe1 C26 42.4(4) . . ? C21 Fe1 C26 141.4(4) . . ? C24 Fe1 C26 68.0(5) . . ? C18 Fe1 C26 109.5(5) . . ? C17 Fe1 C20 68.1(5) . . ? C22 Fe1 C20 141.2(5) . . ? C21 Fe1 C20 40.6(5) . . ? C24 Fe1 C20 112.5(5) . . ? C18 Fe1 C20 67.8(5) . . ? C26 Fe1 C20 176.4(5) . . ? C17 Fe1 C23 136.4(5) . . ? C22 Fe1 C23 41.5(4) . . ? C21 Fe1 C23 110.7(5) . . ? C24 Fe1 C23 40.3(5) . . ? C18 Fe1 C23 177.7(5) . . ? C26 Fe1 C23 69.3(5) . . ? C20 Fe1 C23 113.4(5) . . ? C17 Fe1 C19 68.6(5) . . ? C22 Fe1 C19 176.5(4) . . ? C21 Fe1 C19 68.1(5) . . ? C24 Fe1 C19 114.0(5) . . ? C18 Fe1 C19 40.2(4) . . ? C26 Fe1 C19 136.5(5) . . ? C20 Fe1 C19 39.9(5) . . ? C23 Fe1 C19 142.0(5) . . ? C17 Fe1 C25 141.1(5) . . ? C22 Fe1 C25 70.6(5) . . ? C21 Fe1 C25 177.8(5) . . ? C24 Fe1 C25 40.6(5) . . ? C18 Fe1 C25 111.4(5) . . ? C26 Fe1 C25 40.8(4) . . ? C20 Fe1 C25 137.3(5) . . ? C23 Fe1 C25 69.2(5) . . ? C19 Fe1 C25 110.6(5) . . ? C27 Fe2 C28 41.1(4) . . ? C27 Fe2 C32 109.7(4) . . ? C28 Fe2 C32 136.3(5) . . ? C27 Fe2 C31 41.7(4) . . ? C28 Fe2 C31 70.0(5) . . ? C32 Fe2 C31 111.5(4) . . ? C27 Fe2 C34 174.8(5) . . ? C28 Fe2 C34 144.0(5) . . ? C32 Fe2 C34 66.8(5) . . ? C31 Fe2 C34 135.1(5) . . ? C27 Fe2 C30 69.4(5) . . ? C28 Fe2 C30 68.6(5) . . ? C32 Fe2 C30 142.7(6) . . ? C31 Fe2 C30 42.0(5) . . ? C34 Fe2 C30 110.9(5) . . ? C27 Fe2 C36 112.3(5) . . ? C28 Fe2 C36 109.7(5) . . ? C32 Fe2 C36 41.4(4) . . ? C31 Fe2 C36 142.0(5) . . ? C34 Fe2 C36 67.8(5) . . ? C30 Fe2 C36 175.4(6) . . ? C27 Fe2 C29 68.4(5) . . ? C28 Fe2 C29 39.4(5) . . ? C32 Fe2 C29 175.2(5) . . ? C31 Fe2 C29 70.3(5) . . ? C34 Fe2 C29 115.5(5) . . ? C30 Fe2 C29 41.5(6) . . ? C36 Fe2 C29 134.6(6) . . ? C27 Fe2 C33 135.2(4) . . ? C28 Fe2 C33 176.1(4) . . ? C32 Fe2 C33 40.9(4) . . ? C31 Fe2 C33 107.8(4) . . ? C34 Fe2 C33 39.7(4) . . ? C30 Fe2 C33 112.3(5) . . ? C36 Fe2 C33 69.8(4) . . ? C29 Fe2 C33 143.6(5) . . ? C27 Fe2 C35 142.4(5) . . ? C28 Fe2 C35 113.4(5) . . ? C32 Fe2 C35 67.9(5) . . ? C31 Fe2 C35 175.8(5) . . ? C34 Fe2 C35 40.7(5) . . ? C30 Fe2 C35 136.2(6) . . ? C36 Fe2 C35 40.0(5) . . ? C29 Fe2 C35 110.7(6) . . ? C33 Fe2 C35 68.9(5) . . ? C58 Fe3 C57 111.2(5) . . ? C58 Fe3 C62 41.4(4) . . ? C57 Fe3 C62 142.5(4) . . ? C58 Fe3 C54 134.9(4) . . ? C57 Fe3 C54 70.0(5) . . ? C62 Fe3 C54 109.5(5) . . ? C58 Fe3 C53 107.3(4) . . ? C57 Fe3 C53 41.3(4) . . ? C62 Fe3 C53 112.2(4) . . ? C54 Fe3 C53 42.5(4) . . ? C58 Fe3 C61 69.3(4) . . ? C57 Fe3 C61 174.4(5) . . ? C62 Fe3 C61 41.3(4) . . ? C54 Fe3 C61 113.8(5) . . ? C53 Fe3 C61 144.2(5) . . ? C58 Fe3 C55 175.9(5) . . ? C57 Fe3 C55 69.7(5) . . ? C62 Fe3 C55 135.7(5) . . ? C54 Fe3 C55 41.3(5) . . ? C53 Fe3 C55 70.5(5) . . ? C61 Fe3 C55 110.2(5) . . ? C58 Fe3 C56 142.7(5) . . ? C57 Fe3 C56 41.2(5) . . ? C62 Fe3 C56 175.6(5) . . ? C54 Fe3 C56 68.5(5) . . ? C53 Fe3 C56 69.3(4) . . ? C61 Fe3 C56 135.3(5) . . ? C55 Fe3 C56 40.3(5) . . ? C58 Fe3 C59 41.8(4) . . ? C57 Fe3 C59 108.6(5) . . ? C62 Fe3 C59 69.2(5) . . ? C54 Fe3 C59 176.1(5) . . ? C53 Fe3 C59 134.2(4) . . ? C61 Fe3 C59 67.8(5) . . ? C55 Fe3 C59 142.1(5) . . ? C56 Fe3 C59 113.0(5) . . ? C58 Fe3 C60 69.9(4) . . ? C57 Fe3 C60 135.0(5) . . ? C62 Fe3 C60 68.8(5) . . ? C54 Fe3 C60 142.5(5) . . ? C53 Fe3 C60 174.8(5) . . ? C61 Fe3 C60 39.5(5) . . ? C55 Fe3 C60 112.6(5) . . ? C56 Fe3 C60 110.1(5) . . ? C59 Fe3 C60 40.9(4) . . ? C64 Fe4 C63 41.7(4) . . ? C64 Fe4 C70 139.5(5) . . ? C63 Fe4 C70 178.8(5) . . ? C64 Fe4 C72 111.2(5) . . ? C63 Fe4 C72 110.9(4) . . ? C70 Fe4 C72 69.0(5) . . ? C64 Fe4 C69 179.7(5) . . ? C63 Fe4 C69 138.1(4) . . ? C70 Fe4 C69 40.7(4) . . ? C72 Fe4 C69 68.9(4) . . ? C64 Fe4 C67 69.0(5) . . ? C63 Fe4 C67 41.2(4) . . ? C70 Fe4 C67 138.1(5) . . ? C72 Fe4 C67 139.8(4) . . ? C69 Fe4 C67 110.8(5) . . ? C64 Fe4 C68 138.5(5) . . ? C63 Fe4 C68 109.8(4) . . ? C70 Fe4 C68 69.3(5) . . ? C72 Fe4 C68 40.8(4) . . ? C69 Fe4 C68 41.4(4) . . ? C67 Fe4 C68 111.3(4) . . ? C64 Fe4 C71 112.3(5) . . ? C63 Fe4 C71 140.8(5) . . ? C70 Fe4 C71 39.8(5) . . ? C72 Fe4 C71 41.8(4) . . ? C69 Fe4 C71 68.0(5) . . ? C67 Fe4 C71 177.8(5) . . ? C68 Fe4 C71 69.1(5) . . ? C64 Fe4 C66 66.4(5) . . ? C63 Fe4 C66 67.2(5) . . ? C70 Fe4 C66 112.9(5) . . ? C72 Fe4 C66 177.6(5) . . ? C69 Fe4 C66 113.5(5) . . ? C67 Fe4 C66 39.6(4) . . ? C68 Fe4 C66 140.8(5) . . ? C71 Fe4 C66 138.9(5) . . ? C64 Fe4 C65 39.6(4) . . ? C63 Fe4 C65 68.4(5) . . ? C70 Fe4 C65 112.6(5) . . ? C72 Fe4 C65 138.8(5) . . ? C69 Fe4 C65 140.4(4) . . ? C67 Fe4 C65 67.9(5) . . ? C68 Fe4 C65 178.1(5) . . ? C71 Fe4 C65 111.8(5) . . ? C66 Fe4 C65 39.5(5) . . ? C1B P1 C17 102.0(5) . . ? C1B P1 C1A 106.5(6) . . ? C17 P1 C1A 106.0(5) . . ? C1B P1 Pd1 113.2(4) . . ? C17 P1 Pd1 124.1(3) . . ? C1A P1 Pd1 103.8(4) . . ? C1D P2 C22 106.2(5) . . ? C1D P2 C1C 104.5(6) . . ? C22 P2 C1C 104.5(5) . . ? C1D P2 Pd1 111.6(4) . . ? C22 P2 Pd1 115.5(3) . . ? C1C P2 Pd1 113.5(4) . . ? C27 P3 C1F 105.6(5) . . ? C27 P3 C1E 103.0(5) . . ? C1F P3 C1E 105.3(5) . . ? C27 P3 Pd2 116.7(4) . . ? C1F P3 Pd2 111.9(4) . . ? C1E P3 Pd2 113.2(3) . . ? C1G P4 C1H 106.2(5) . . ? C1G P4 C32 102.8(5) . . ? C1H P4 C32 102.0(5) . . ? C1G P4 Pd2 117.5(4) . . ? C1H P4 Pd2 102.9(4) . . ? C32 P4 Pd2 123.3(4) . . ? C53 P5 C1J 100.9(5) . . ? C53 P5 C1I 105.6(5) . . ? C1J P5 C1I 106.9(5) . . ? C53 P5 Pd3 123.1(3) . . ? C1J P5 Pd3 116.4(4) . . ? C1I P5 Pd3 102.6(4) . . ? C58 P6 C1K 102.7(5) . . ? C58 P6 C1L 106.3(5) . . ? C1K P6 C1L 104.9(5) . . ? C58 P6 Pd3 117.9(3) . . ? C1K P6 Pd3 114.4(4) . . ? C1L P6 Pd3 109.4(4) . . ? C63 P7 C1N 108.4(5) . . ? C63 P7 C1M 104.2(5) . . ? C1N P7 C1M 103.6(5) . . ? C63 P7 Pd4 113.0(4) . . ? C1N P7 Pd4 113.5(4) . . ? C1M P7 Pd4 113.4(3) . . ? C68 P8 C1O 104.2(5) . . ? C68 P8 C1P 103.2(5) . . ? C1O P8 C1P 105.0(5) . . ? C68 P8 Pd4 123.5(4) . . ? C1O P8 Pd4 113.9(4) . . ? C1P P8 Pd4 105.2(4) . . ? C4 N1 C8 116.5(10) . . ? C4 N1 Pd2 126.9(8) . . ? C8 N1 Pd2 116.1(7) . . ? C12 N2 C16 117.7(9) . . ? C12 N2 Pd1 123.5(7) . . ? C16 N2 Pd1 118.7(7) . . ? C52 N3 C48 118.5(9) . . ? C52 N3 Pd3 115.4(7) . . ? C48 N3 Pd3 126.0(7) . . ? C44 N4 C40 118.4(10) . . ? C44 N4 Pd4 122.9(8) . . ? C40 N4 Pd4 118.7(7) . . ? C1 O1 Pd1 124.5(7) . . ? C9 O3 Pd2 113.8(7) . . ? C37 O5 Pd3 114.9(7) . . ? C45 O7 Pd4 123.3(7) . . ? O2 C1 O1 124.7(10) . . ? O2 C1 C2 122.3(10) . . ? O1 C1 C2 112.7(10) . . ? C1 C2 C3 113.1(9) . . ? C2 C3 C6 111.3(8) . . ? N1 C4 C5 124.0(11) . . ? C4 C5 C6 119.6(10) . . ? C5 C6 C7 117.2(10) . . ? C5 C6 C3 122.3(10) . . ? C7 C6 C3 120.5(10) . . ? C8 C7 C6 119.2(10) . . ? C7 C8 N1 123.2(10) . . ? O4 C9 O3 124.0(11) . . ? O4 C9 C10 121.8(11) . . ? O3 C9 C10 114.0(10) . . ? C11 C10 C9 117.0(9) . . ? C10 C11 C14 112.3(9) . . ? N2 C12 C13 122.6(10) . . ? C12 C13 C14 119.9(10) . . ? C15 C14 C13 117.9(10) . . ? C15 C14 C11 122.9(10) . . ? C13 C14 C11 119.2(10) . . ? C14 C15 C16 119.2(11) . . ? N2 C16 C15 122.7(11) . . ? C21 C17 C18 107.9(10) . . ? C21 C17 P1 126.8(9) . . ? C18 C17 P1 125.2(8) . . ? C21 C17 Fe1 70.4(6) . . ? C18 C17 Fe1 70.3(6) . . ? P1 C17 Fe1 125.4(6) . . ? C19 C18 C17 106.9(10) . . ? C19 C18 Fe1 70.7(7) . . ? C17 C18 Fe1 67.8(6) . . ? C20 C19 C18 108.4(11) . . ? C20 C19 Fe1 69.6(7) . . ? C18 C19 Fe1 69.1(7) . . ? C19 C20 C21 108.5(11) . . ? C19 C20 Fe1 70.5(7) . . ? C21 C20 Fe1 68.7(7) . . ? C17 C21 C20 108.3(11) . . ? C17 C21 Fe1 69.2(7) . . ? C20 C21 Fe1 70.8(7) . . ? C23 C22 C26 106.4(10) . . ? C23 C22 P2 128.3(9) . . ? C26 C22 P2 125.3(8) . . ? C23 C22 Fe1 70.8(7) . . ? C26 C22 Fe1 69.7(6) . . ? P2 C22 Fe1 126.2(5) . . ? C24 C23 C22 107.3(11) . . ? C24 C23 Fe1 69.0(7) . . ? C22 C23 Fe1 67.7(6) . . ? C23 C24 C25 111.4(11) . . ? C23 C24 Fe1 70.7(6) . . ? C25 C24 Fe1 70.9(7) . . ? C24 C25 C26 105.8(10) . . ? C24 C25 Fe1 68.5(7) . . ? C26 C25 Fe1 68.7(6) . . ? C25 C26 C22 109.0(10) . . ? C25 C26 Fe1 70.6(7) . . ? C22 C26 Fe1 67.8(6) . . ? C28 C27 C31 109.4(10) . . ? C28 C27 P3 128.5(9) . . ? C31 C27 P3 122.1(9) . . ? C28 C27 Fe2 70.2(7) . . ? C31 C27 Fe2 70.2(6) . . ? P3 C27 Fe2 124.5(6) . . ? C29 C28 C27 109.6(12) . . ? C29 C28 Fe2 71.6(8) . . ? C27 C28 Fe2 68.6(7) . . ? C28 C29 C30 108.2(12) . . ? C28 C29 Fe2 69.0(7) . . ? C30 C29 Fe2 68.9(8) . . ? C29 C30 C31 107.6(11) . . ? C29 C30 Fe2 69.6(8) . . ? C31 C30 Fe2 68.4(7) . . ? C27 C31 C30 105.3(11) . . ? C27 C31 Fe2 68.0(6) . . ? C30 C31 Fe2 69.5(7) . . ? C33 C32 C36 110.1(10) . . ? C33 C32 P4 126.1(9) . . ? C36 C32 P4 123.8(9) . . ? C33 C32 Fe2 71.0(6) . . ? C36 C32 Fe2 70.1(7) . . ? P4 C32 Fe2 126.0(6) . . ? C34 C33 C32 104.9(10) . . ? C34 C33 Fe2 69.4(7) . . ? C32 C33 Fe2 68.2(6) . . ? C33 C34 C35 111.6(11) . . ? C33 C34 Fe2 70.9(7) . . ? C35 C34 Fe2 70.9(7) . . ? C36 C35 C34 106.6(11) . . ? C36 C35 Fe2 68.9(7) . . ? C34 C35 Fe2 68.3(7) . . ? C35 C36 C32 106.8(11) . . ? C35 C36 Fe2 71.1(8) . . ? C32 C36 Fe2 68.4(6) . . ? O6 C37 O5 125.8(10) . . ? O6 C37 C38 119.9(10) . . ? O5 C37 C38 114.2(10) . . ? C39 C38 C37 115.4(10) . . ? C42 C39 C38 113.9(10) . . ? N4 C40 C41 121.0(10) . . ? C42 C41 C40 122.7(10) . . ? C41 C42 C43 114.7(10) . . ? C41 C42 C39 124.5(10) . . ? C43 C42 C39 120.8(10) . . ? C42 C43 C44 120.7(11) . . ? N4 C44 C43 122.5(11) . . ? O8 C45 O7 126.6(11) . . ? O8 C45 C46 119.5(11) . . ? O7 C45 C46 113.9(11) . . ? C45 C46 C47 113.7(10) . . ? C50 C47 C46 112.5(9) . . ? N3 C48 C49 121.4(10) . . ? C48 C49 C50 120.5(10) . . ? C49 C50 C51 116.7(10) . . ? C49 C50 C47 123.0(10) . . ? C51 C50 C47 120.3(10) . . ? C52 C51 C50 119.5(10) . . ? N3 C52 C51 123.2(10) . . ? C57 C53 C54 106.3(9) . . ? C57 C53 P5 128.1(8) . . ? C54 C53 P5 125.6(8) . . ? C57 C53 Fe3 68.7(6) . . ? C54 C53 Fe3 68.5(6) . . ? P5 C53 Fe3 128.0(5) . . ? C55 C54 C53 108.1(10) . . ? C55 C54 Fe3 69.7(7) . . ? C53 C54 Fe3 69.0(6) . . ? C56 C55 C54 108.1(10) . . ? C56 C55 Fe3 70.9(7) . . ? C54 C55 Fe3 69.0(6) . . ? C55 C56 C57 108.7(10) . . ? C55 C56 Fe3 68.8(7) . . ? C57 C56 Fe3 67.6(6) . . ? C53 C57 C56 108.8(10) . . ? C53 C57 Fe3 70.0(6) . . ? C56 C57 Fe3 71.2(7) . . ? C62 C58 C59 107.1(9) . . ? C62 C58 P6 126.3(8) . . ? C59 C58 P6 126.6(8) . . ? C62 C58 Fe3 69.4(6) . . ? C59 C58 Fe3 71.1(6) . . ? P6 C58 Fe3 125.1(5) . . ? C60 C59 C58 107.9(10) . . ? C60 C59 Fe3 70.7(6) . . ? C58 C59 Fe3 67.1(6) . . ? C61 C60 C59 106.5(11) . . ? C61 C60 Fe3 67.7(7) . . ? C59 C60 Fe3 68.5(6) . . ? C60 C61 C62 110.8(10) . . ? C60 C61 Fe3 72.8(7) . . ? C62 C61 Fe3 68.8(6) . . ? C58 C62 C61 107.6(10) . . ? C58 C62 Fe3 69.2(6) . . ? C61 C62 Fe3 69.9(6) . . ? C67 C63 C64 106.2(10) . . ? C67 C63 P7 123.5(8) . . ? C64 C63 P7 130.0(9) . . ? C67 C63 Fe4 69.9(6) . . ? C64 C63 Fe4 68.7(6) . . ? P7 C63 Fe4 121.4(6) . . ? C65 C64 C63 109.2(11) . . ? C65 C64 Fe4 72.4(7) . . ? C63 C64 Fe4 69.6(6) . . ? C64 C65 C66 106.9(11) . . ? C64 C65 Fe4 68.0(7) . . ? C66 C65 Fe4 70.1(7) . . ? C67 C66 C65 110.9(11) . . ? C67 C66 Fe4 69.2(6) . . ? C65 C66 Fe4 70.5(7) . . ? C66 C67 C63 106.8(10) . . ? C66 C67 Fe4 71.2(7) . . ? C63 C67 Fe4 68.9(6) . . ? C72 C68 C69 107.0(9) . . ? C72 C68 P8 126.8(8) . . ? C69 C68 P8 126.1(8) . . ? C72 C68 Fe4 69.2(6) . . ? C69 C68 Fe4 69.0(6) . . ? P8 C68 Fe4 123.7(6) . . ? C70 C69 C68 108.3(10) . . ? C70 C69 Fe4 69.4(7) . . ? C68 C69 Fe4 69.6(6) . . ? C71 C70 C69 109.4(10) . . ? C71 C70 Fe4 71.4(7) . . ? C69 C70 Fe4 69.9(6) . . ? C70 C71 C72 107.4(10) . . ? C70 C71 Fe4 68.7(7) . . ? C72 C71 Fe4 68.0(6) . . ? C68 C72 C71 107.8(10) . . ? C68 C72 Fe4 70.0(6) . . ? C71 C72 Fe4 70.2(7) . . ? C6A C1A C2A 117.3(11) . . ? C6A C1A P1 118.9(9) . . ? C2A C1A P1 123.7(10) . . ? C3A C2A C1A 120.6(14) . . ? C4A C3A C2A 121.0(15) . . ? C3A C4A C5A 118.0(14) . . ? C6A C5A C4A 122.1(15) . . ? C5A C6A C1A 121.0(13) . . ? C2B C1B C6B 119.3(11) . . ? C2B C1B P1 119.4(8) . . ? C6B C1B P1 121.2(9) . . ? C3B C2B C1B 120.0(11) . . ? C4B C3B C2B 121.7(13) . . ? C3B C4B C5B 119.2(12) . . ? C6B C5B C4B 120.5(11) . . ? C5B C6B C1B 119.3(11) . . ? C2C C1C C6C 116.1(13) . . ? C2C C1C P2 123.0(12) . . ? C6C C1C P2 120.6(10) . . ? C1C C2C C3C 120.0(15) . . ? C4C C3C C2C 121.0(15) . . ? C3C C4C C5C 121.6(16) . . ? C4C C5C C6C 117.1(16) . . ? C5C C6C C1C 123.9(14) . . ? C2D C1D C6D 119.2(12) . . ? C2D C1D P2 120.5(10) . . ? C6D C1D P2 120.3(9) . . ? C1D C2D C3D 118.5(13) . . ? C4D C3D C2D 121.3(15) . . ? C5D C4D C3D 121.6(15) . . ? C4D C5D C6D 120.7(13) . . ? C1D C6D C5D 118.6(11) . . ? C6E C1E C2E 118.2(11) . . ? C6E C1E P3 120.9(9) . . ? C2E C1E P3 120.8(9) . . ? C3E C2E C1E 120.3(14) . . ? C4E C3E C2E 121.1(16) . . ? C3E C4E C5E 120.2(15) . . ? C6E C5E C4E 119.1(15) . . ? C5E C6E C1E 120.9(13) . . ? C6F C1F C2F 118.8(11) . . ? C6F C1F P3 120.8(9) . . ? C2F C1F P3 120.4(9) . . ? C1F C2F C3F 122.2(13) . . ? C4F C3F C2F 116.9(13) . . ? C3F C4F C5F 121.9(13) . . ? C4F C5F C6F 118.7(13) . . ? C1F C6F C5F 121.5(12) . . ? C2G C1G C6G 115.9(11) . . ? C2G C1G P4 122.1(9) . . ? C6G C1G P4 121.8(9) . . ? C3G C2G C1G 123.6(12) . . ? C2G C3G C4G 118.4(12) . . ? C5G C4G C3G 122.2(13) . . ? C4G C5G C6G 117.1(12) . . ? C5G C6G C1G 122.8(11) . . ? C6H C1H C2H 118.4(11) . . ? C6H C1H P4 120.0(9) . . ? C2H C1H P4 121.4(9) . . ? C1H C2H C3H 120.8(12) . . ? C4H C3H C2H 118.6(14) . . ? C3H C4H C5H 122.8(13) . . ? C4H C5H C6H 117.8(13) . . ? C1H C6H C5H 121.5(12) . . ? C2I C1I C6I 119.8(12) . . ? C2I C1I P5 121.3(11) . . ? C6I C1I P5 118.6(9) . . ? C1I C2I C3I 117.3(14) . . ? C4I C3I C2I 121.4(14) . . ? C5I C4I C3I 121.7(15) . . ? C4I C5I C6I 117.5(15) . . ? C1I C6I C5I 122.4(13) . . ? C6J C1J C2J 117.6(11) . . ? C6J C1J P5 122.8(9) . . ? C2J C1J P5 119.4(9) . . ? C3J C2J C1J 119.8(13) . . ? C4J C3J C2J 122.3(14) . . ? C3J C4J C5J 119.9(13) . . ? C4J C5J C6J 119.2(12) . . ? C1J C6J C5J 121.1(11) . . ? C6K C1K C2K 119.0(11) . . ? C6K C1K P6 121.4(10) . . ? C2K C1K P6 119.5(8) . . ? C3K C2K C1K 120.0(12) . . ? C4K C3K C2K 121.7(14) . . ? C3K C4K C5K 119.9(14) . . ? C4K C5K C6K 120.4(15) . . ? C1K C6K C5K 119.0(13) . . ? C6L C1L C2L 120.9(11) . . ? C6L C1L P6 120.1(9) . . ? C2L C1L P6 119.0(9) . . ? C1L C2L C3L 118.4(12) . . ? C4L C3L C2L 119.9(12) . . ? C5L C4L C3L 120.5(12) . . ? C4L C5L C6L 120.5(11) . . ? C1L C6L C5L 119.7(11) . . ? C2M C1M C6M 119.0(11) . . ? C2M C1M P7 121.4(10) . . ? C6M C1M P7 119.6(10) . . ? C3M C2M C1M 119.2(15) . . ? C2M C3M C4M 119.5(17) . . ? C5M C4M C3M 120.8(18) . . ? C4M C5M C6M 120.6(19) . . ? C5M C6M C1M 120.6(15) . . ? C2N C1N C6N 117.0(11) . . ? C2N C1N P7 121.7(9) . . ? C6N C1N P7 121.2(9) . . ? C3N C2N C1N 121.0(11) . . ? C2N C3N C4N 120.8(12) . . ? C5N C4N C3N 119.8(12) . . ? C4N C5N C6N 119.0(12) . . ? C5N C6N C1N 122.3(12) . . ? C2O C1O C6O 118.3(10) . . ? C2O C1O P8 120.2(9) . . ? C6O C1O P8 121.4(8) . . ? C3O C2O C1O 119.9(12) . . ? C4O C3O C2O 120.6(13) . . ? C5O C4O C3O 119.5(13) . . ? C4O C5O C6O 124.2(12) . . ? C5O C6O C1O 117.2(11) . . ? C6P C1P C2P 120.5(11) . . ? C6P C1P P8 118.9(9) . . ? C2P C1P P8 120.4(9) . . ? C3P C2P C1P 118.6(12) . . ? C4P C3P C2P 120.8(12) . . ? C3P C4P C5P 122.5(13) . . ? C6P C5P C4P 115.6(13) . . ? C1P C6P C5P 121.9(12) . . ? O11 S1 O10 124.9(10) . . ? O11 S1 O9 109.1(11) . . ? O10 S1 O9 112.4(9) . . ? O11 S1 C73 107.1(9) . . ? O10 S1 C73 104.9(8) . . ? O9 S1 C73 93.5(9) . . ? F2 C73 F3 107.7(19) . . ? F2 C73 F1 110.7(19) . . ? F3 C73 F1 110.2(18) . . ? F2 C73 S1 113.2(12) . . ? F3 C73 S1 113.8(13) . . ? F1 C73 S1 101.0(15) . . ? O13 S2 O12 127.1(11) . . ? O13 S2 O14 106.6(12) . . ? O12 S2 O14 105.6(10) . . ? O13 S2 C74 105.8(8) . . ? O12 S2 C74 107.1(8) . . ? O14 S2 C74 102.0(9) . . ? F6 C74 F4 115(2) . . ? F6 C74 F5 110(2) . . ? F4 C74 F5 94(2) . . ? F6 C74 S2 116.0(13) . . ? F4 C74 S2 110.1(15) . . ? F5 C74 S2 109.9(15) . . ? F8 C75 F7 108.4(16) . . ? F8 C75 F9 102.7(14) . . ? F7 C75 F9 101.9(15) . . ? F8 C75 S3 120.8(10) . . ? F7 C75 S3 110.8(11) . . ? F9 C75 S3 110.3(11) . . ? O15 S3 O17 122.3(11) . . ? O15 S3 O16 107.9(13) . . ? O17 S3 O16 110.0(10) . . ? O15 S3 C75 107.5(7) . . ? O17 S3 C75 109.0(7) . . ? O16 S3 C75 97.3(8) . . ? O20 S4 O18 117.2(12) . . ? O20 S4 O19 107.1(13) . . ? O18 S4 O19 115.0(9) . . ? O20 S4 C76 105.6(11) . . ? O18 S4 C76 106.7(7) . . ? O19 S4 C76 104.1(7) . . ? F11 C76 F12 107.7(15) . . ? F11 C76 F10 109.8(14) . . ? F12 C76 F10 103.4(12) . . ? F11 C76 S4 114.3(10) . . ? F12 C76 S4 110.1(11) . . ? F10 C76 S4 110.9(10) . . ? Cl4 C2S Cl6 113.3(16) . . ? Cl4 C2S Cl5 109.2(14) . . ? Cl6 C2S Cl5 107.9(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.701 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.119