# 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 'Elena Lalinde' _publ_contact_author_email ELENA.LALINDE@UNIRIOJA.ES _publ_section_title ; Platinum complexes having redox-active PPh2C?CFc and/or C?CFc as terminal or bridging ligands ; _publ_requested_category FM loop_ _publ_author_name 'Elena Lalinde' 'Alvaro Diez' 'M Teresa Moreno' 'Sergio Sanchez' # Attachment 'B822171E_revised.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 713069' _audit_creation_date 2007-06-04T17:31:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common s42 _chemical_formula_sum 'C61 H39 Cl3 F10 Fe2 P2 Pt' _chemical_formula_weight 1437 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 20.3213(3) _cell_length_b 13.3744(2) _cell_length_c 21.9589(3) _cell_angle_alpha 90 _cell_angle_beta 110.0390(10) _cell_angle_gamma 90 _cell_volume 5606.79(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 13336 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.49 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.309 _exptl_absorpt_correction_T_max 0.612 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0137082 _diffrn_orient_matrix_ub_12 -0.0652196 _diffrn_orient_matrix_ub_13 0.0144655 _diffrn_orient_matrix_ub_21 -0.049317 _diffrn_orient_matrix_ub_22 0.0242905 _diffrn_orient_matrix_ub_23 -0.0115621 _diffrn_orient_matrix_ub_31 -0.0111198 _diffrn_orient_matrix_ub_32 -0.0273292 _diffrn_orient_matrix_ub_33 -0.0447976 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_number 12763 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 12763 _reflns_number_gt 10267 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+30.7097P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12763 _refine_ls_number_parameters 742 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.072 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.681 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.13 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0116(3) 0.0471(4) 0.8651(2) 0.0280(11) Uani 1 1 d . . . C2 C -0.0650(3) 0.0220(4) 0.8080(3) 0.0365(13) Uani 1 1 d . . . H2 H -0.0738 0.0614 0.7712 0.044 Uiso 1 1 calc R . . C3 C -0.1052(3) -0.0630(4) 0.8065(3) 0.0430(14) Uani 1 1 d . . . H3 H -0.1414 -0.0798 0.7687 0.052 Uiso 1 1 calc R . . C4 C -0.0916(3) -0.1221(5) 0.8606(3) 0.0463(15) Uani 1 1 d . . . H4 H -0.1186 -0.1787 0.859 0.056 Uiso 1 1 calc R . . C5 C -0.0385(3) -0.0984(4) 0.9170(3) 0.0435(15) Uani 1 1 d . . . H5 H -0.0294 -0.1389 0.9534 0.052 Uiso 1 1 calc R . . C6 C 0.0017(3) -0.0136(4) 0.9194(3) 0.0353(12) Uani 1 1 d . . . H6 H 0.0377 0.0027 0.9575 0.042 Uiso 1 1 calc R . . C7 C 0.0087(3) 0.2428(4) 0.9217(2) 0.0337(12) Uani 1 1 d . . . C8 C 0.0564(4) 0.3019(4) 0.9681(3) 0.0486(16) Uani 1 1 d . . . H8 H 0.1039 0.2992 0.9739 0.058 Uiso 1 1 calc R . . C9 C 0.0321(6) 0.3653(5) 1.0059(4) 0.073(2) Uani 1 1 d . . . H9 H 0.0637 0.405 1.0373 0.088 Uiso 1 1 calc R . . C10 C -0.0377(6) 0.3702(6) 0.9975(4) 0.080(3) Uani 1 1 d . . . H10 H -0.0532 0.4127 1.0233 0.096 Uiso 1 1 calc R . . C11 C -0.0853(5) 0.3121(5) 0.9507(4) 0.068(2) Uani 1 1 d . . . H11 H -0.1328 0.3159 0.9447 0.081 Uiso 1 1 calc R . . C12 C -0.0617(4) 0.2483(4) 0.9129(3) 0.0453(15) Uani 1 1 d . . . H12 H -0.0936 0.2089 0.8815 0.054 Uiso 1 1 calc R . . C13 C 0.1236(3) 0.1310(4) 0.9206(2) 0.0346(13) Uani 1 1 d . . . C14 C 0.1818(3) 0.1099(4) 0.9548(3) 0.0380(13) Uani 1 1 d . . . C15 C 0.2503(3) 0.0818(5) 0.9954(3) 0.0408(14) Uani 1 1 d . . . C16 C 0.2821(3) 0.1082(5) 1.0616(3) 0.0508(17) Uani 1 1 d . . . H16 H 0.2622 0.1493 1.0847 0.061 Uiso 1 1 calc R . . C17 C 0.3480(3) 0.0628(5) 1.0867(3) 0.0547(18) Uani 1 1 d . . . H17 H 0.3786 0.067 1.1292 0.066 Uiso 1 1 calc R . . C18 C 0.3596(3) 0.0091(6) 1.0353(4) 0.060(2) Uani 1 1 d . . . H18 H 0.3997 -0.0268 1.0381 0.073 Uiso 1 1 calc R . . C19 C 0.2993(3) 0.0199(5) 0.9790(3) 0.0507(16) Uani 1 1 d . . . H19 H 0.2928 -0.0083 0.9386 0.061 Uiso 1 1 calc R . . C20 C 0.2901(4) -0.1892(5) 1.0803(4) 0.060(2) Uani 1 1 d . . . H20 H 0.3317 -0.2243 1.0887 0.072 Uiso 1 1 calc R . . C21 C 0.2355(4) -0.1838(5) 1.0199(4) 0.0592(18) Uani 1 1 d . . . H21 H 0.2348 -0.2147 0.9818 0.071 Uiso 1 1 calc R . . C22 C 0.1824(3) -0.1237(5) 1.0275(4) 0.0585(19) Uani 1 1 d . . . H22 H 0.1403 -0.1073 0.9953 0.07 Uiso 1 1 calc R . . C23 C 0.2043(4) -0.0923(6) 1.0933(4) 0.068(2) Uani 1 1 d . . . H23 H 0.1792 -0.052 1.112 0.082 Uiso 1 1 calc R . . C24 C 0.2717(4) -0.1339(6) 1.1250(4) 0.063(2) Uani 1 1 d . . . H24 H 0.2988 -0.1254 1.1684 0.075 Uiso 1 1 calc R . . C25 C 0.2008(3) 0.1907(4) 0.8067(2) 0.0337(12) Uani 1 1 d . . . C26 C 0.2025(3) 0.2914(6) 0.8199(3) 0.0546(18) Uani 1 1 d . . . H26 H 0.1609 0.3274 0.8071 0.066 Uiso 1 1 calc R . . C27 C 0.2651(4) 0.3402(7) 0.8520(4) 0.072(2) Uani 1 1 d . . . H27 H 0.266 0.4091 0.858 0.086 Uiso 1 1 calc R . . C28 C 0.3247(4) 0.2863(8) 0.8745(3) 0.078(3) Uani 1 1 d . . . H28 H 0.3664 0.3184 0.8975 0.093 Uiso 1 1 calc R . . C29 C 0.3254(4) 0.1862(8) 0.8643(4) 0.077(3) Uani 1 1 d . . . H29 H 0.367 0.1506 0.8809 0.092 Uiso 1 1 calc R . . C30 C 0.2624(3) 0.1355(6) 0.8284(3) 0.0518(18) Uani 1 1 d . . . H30 H 0.2625 0.0675 0.8197 0.062 Uiso 1 1 calc R . . C31 C 0.1214(3) 0.1150(5) 0.6801(3) 0.0418(15) Uani 1 1 d . . . C32 C 0.1551(3) 0.1829(7) 0.6546(3) 0.065(2) Uani 1 1 d . . . H32 H 0.1794 0.2361 0.6796 0.078 Uiso 1 1 calc R . . C33 C 0.1528(5) 0.1719(10) 0.5907(4) 0.102(4) Uani 1 1 d . . . H33 H 0.1768 0.2166 0.5735 0.122 Uiso 1 1 calc R . . C34 C 0.1149(6) 0.0946(12) 0.5531(4) 0.123(6) Uani 1 1 d . . . H34 H 0.1123 0.0882 0.5101 0.148 Uiso 1 1 calc R . . C35 C 0.0815(6) 0.0281(8) 0.5789(4) 0.107(5) Uani 1 1 d . . . H35 H 0.0561 -0.0239 0.5533 0.128 Uiso 1 1 calc R . . C36 C 0.0844(4) 0.0362(5) 0.6422(3) 0.070(2) Uani 1 1 d . . . H36 H 0.062 -0.0106 0.6595 0.083 Uiso 1 1 calc R . . C37 C 0.1243(3) 0.0090(4) 0.7900(3) 0.0379(13) Uani 1 1 d . . . C38 C 0.1224(3) -0.0782(4) 0.8017(3) 0.0370(13) Uani 1 1 d . . . C39 C 0.1232(3) -0.1832(4) 0.8138(3) 0.0354(13) Uani 1 1 d . . . C40 C 0.0879(3) -0.2351(5) 0.8504(3) 0.0447(15) Uani 1 1 d . . . H40 H 0.0621 -0.2061 0.8736 0.054 Uiso 1 1 calc R . . C41 C 0.0992(4) -0.3384(5) 0.8450(3) 0.0539(18) Uani 1 1 d . . . H41 H 0.0823 -0.3893 0.8645 0.065 Uiso 1 1 calc R . . C42 C 0.1400(4) -0.3515(5) 0.8053(3) 0.0523(18) Uani 1 1 d . . . H42 H 0.1546 -0.4124 0.7939 0.063 Uiso 1 1 calc R . . C43 C 0.1550(3) -0.2562(4) 0.7856(3) 0.0416(14) Uani 1 1 d . . . H43 H 0.181 -0.2434 0.759 0.05 Uiso 1 1 calc R . . C44 C 0.0032(3) -0.2349(5) 0.6601(3) 0.0482(15) Uani 1 1 d . . . H44 H 0.024 -0.1985 0.6355 0.058 Uiso 1 1 calc R . . C45 C -0.0338(3) -0.1951(5) 0.6989(3) 0.0514(17) Uani 1 1 d . . . H45 H -0.0411 -0.1276 0.7045 0.062 Uiso 1 1 calc R . . C46 C -0.0576(3) -0.2749(6) 0.7272(3) 0.0549(17) Uani 1 1 d . . . H46 H -0.0839 -0.2693 0.7544 0.066 Uiso 1 1 calc R . . C47 C -0.0345(3) -0.3661(5) 0.7072(3) 0.0505(17) Uani 1 1 d . . . H47 H -0.0427 -0.4303 0.7194 0.061 Uiso 1 1 calc R . . C48 C 0.0027(3) -0.3416(5) 0.6660(3) 0.0476(16) Uani 1 1 d . . . H48 H 0.0234 -0.3868 0.6459 0.057 Uiso 1 1 calc R . . C49 C -0.0542(3) 0.3165(4) 0.7713(3) 0.0344(12) Uani 1 1 d . . . C50 C -0.0408(3) 0.4060(4) 0.8044(3) 0.0392(14) Uani 1 1 d . . . C51 C -0.0931(5) 0.4706(5) 0.8070(3) 0.058(2) Uani 1 1 d . . . C52 C -0.1620(5) 0.4444(7) 0.7756(4) 0.074(2) Uani 1 1 d . . . C53 C -0.1777(4) 0.3562(7) 0.7431(4) 0.068(2) Uani 1 1 d . . . C54 C -0.1246(3) 0.2938(5) 0.7405(3) 0.0466(16) Uani 1 1 d . . . C55 C 0.0076(3) 0.2740(4) 0.6755(2) 0.0273(10) Uani 1 1 d . . . C56 C 0.0360(3) 0.3594(4) 0.6601(3) 0.0369(13) Uani 1 1 d . . . C57 C 0.0302(4) 0.3845(5) 0.5972(3) 0.0536(18) Uani 1 1 d . . . C58 C -0.0058(4) 0.3225(5) 0.5474(3) 0.0544(19) Uani 1 1 d . . . C59 C -0.0359(3) 0.2389(5) 0.5605(3) 0.0482(17) Uani 1 1 d . . . C60 C -0.0288(3) 0.2153(4) 0.6238(3) 0.0380(13) Uani 1 1 d . . . F1 F 0.0263(2) 0.4340(2) 0.83633(18) 0.0511(9) Uani 1 1 d . . . F2 F -0.0767(3) 0.5572(3) 0.8397(2) 0.0826(14) Uani 1 1 d . . . F3 F -0.2133(3) 0.5071(5) 0.7776(3) 0.116(2) Uani 1 1 d . . . F4 F -0.2450(2) 0.3305(5) 0.7124(3) 0.109(2) Uani 1 1 d . . . F5 F -0.14335(18) 0.2089(3) 0.70691(18) 0.0630(11) Uani 1 1 d . . . F6 F 0.0731(2) 0.4226(2) 0.70754(18) 0.0594(11) Uani 1 1 d . . . F7 F 0.0609(3) 0.4673(3) 0.5854(2) 0.0893(16) Uani 1 1 d . . . F8 F -0.0106(3) 0.3450(4) 0.48643(18) 0.0854(15) Uani 1 1 d . . . F9 F -0.0707(2) 0.1767(4) 0.51184(17) 0.0829(14) Uani 1 1 d . . . F10 F -0.05874(19) 0.1288(3) 0.63286(16) 0.0546(10) Uani 1 1 d . . . Fe1 Fe 0.27260(4) -0.04322(6) 1.05061(4) 0.0393(2) Uani 1 1 d . . . Fe2 Fe 0.04925(4) -0.27695(6) 0.75560(4) 0.03770(18) Uani 1 1 d . . . P1 P 0.03843(7) 0.16207(10) 0.86951(6) 0.0263(3) Uani 1 1 d . . . P2 P 0.11820(7) 0.13193(10) 0.76170(6) 0.0275(3) Uani 1 1 d . . . Pt1 Pt 0.026146(10) 0.223331(14) 0.768940(9) 0.02186(5) Uani 1 1 d . . . C99A C 0.7739(8) 1.0658(12) 0.5700(7) 0.096(6) Uani 0.6 1 d PD A 1 H99A H 0.8119 1.1151 0.5835 0.115 Uiso 0.6 1 calc PR A 1 Cl1A Cl 0.8157(5) 0.9557(5) 0.6004(4) 0.103(2) Uani 0.6 1 d PD A 1 Cl2A Cl 0.7131(3) 1.1158(4) 0.5962(2) 0.1058(14) Uani 0.6 1 d PD A 1 Cl3A Cl 0.7449(8) 1.0753(15) 0.4891(5) 0.391(12) Uani 0.6 1 d PD A 1 C99B C 0.7866(10) 1.0306(13) 0.5347(10) 0.096(6) Uani 0.4 1 d PD B 2 H99B H 0.8299 1.0265 0.5246 0.115 Uiso 0.4 1 calc PR B 2 Cl1B Cl 0.7863(11) 0.9577(16) 0.6000(11) 0.227(11) Uani 0.4 1 d PD B 2 Cl2B Cl 0.7623(5) 1.1485(7) 0.5460(8) 0.206(7) Uani 0.4 1 d PD B 2 Cl3B Cl 0.7146(3) 0.9766(5) 0.4774(3) 0.0794(18) Uani 0.4 1 d PD B 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 C1 0.026(3) 0.028(3) 0.033(3) 0.001(2) 0.014(2) -0.001(2) C2 0.033(3) 0.041(3) 0.036(3) 0.003(3) 0.013(2) -0.002(3) C3 0.039(3) 0.044(3) 0.044(3) -0.009(3) 0.013(3) -0.016(3) C4 0.049(4) 0.036(3) 0.062(4) -0.003(3) 0.030(3) -0.013(3) C5 0.055(4) 0.033(3) 0.050(4) 0.013(3) 0.027(3) -0.002(3) C6 0.044(3) 0.029(3) 0.033(3) 0.004(2) 0.013(3) -0.003(2) C7 0.047(3) 0.029(3) 0.028(3) 0.005(2) 0.016(2) -0.001(2) C8 0.076(5) 0.032(3) 0.036(3) -0.004(3) 0.018(3) -0.011(3) C9 0.132(8) 0.040(4) 0.055(5) -0.011(3) 0.041(5) -0.016(5) C10 0.160(10) 0.041(4) 0.075(6) -0.007(4) 0.086(6) -0.005(5) C11 0.099(6) 0.044(4) 0.090(6) 0.007(4) 0.072(5) 0.004(4) C12 0.065(4) 0.037(3) 0.046(3) 0.000(3) 0.035(3) -0.003(3) C13 0.037(3) 0.038(3) 0.024(3) 0.003(2) 0.004(2) -0.009(2) C14 0.035(3) 0.042(3) 0.031(3) 0.005(3) 0.003(2) -0.009(3) C15 0.033(3) 0.046(3) 0.037(3) 0.013(3) 0.004(3) -0.010(3) C16 0.038(4) 0.042(4) 0.058(4) 0.003(3) -0.001(3) -0.004(3) C17 0.040(4) 0.058(4) 0.049(4) 0.007(3) -0.007(3) -0.014(3) C18 0.033(3) 0.068(5) 0.074(5) 0.029(4) 0.010(3) -0.003(3) C19 0.043(4) 0.059(4) 0.050(4) 0.014(3) 0.016(3) -0.006(3) C20 0.046(4) 0.043(4) 0.084(5) 0.021(4) 0.013(4) 0.006(3) C21 0.063(5) 0.048(4) 0.064(5) -0.003(3) 0.018(4) -0.003(4) C22 0.038(4) 0.052(4) 0.075(5) 0.019(4) 0.006(3) -0.008(3) C23 0.080(6) 0.052(4) 0.100(6) 0.008(4) 0.064(5) -0.009(4) C24 0.071(5) 0.062(5) 0.053(4) 0.023(4) 0.018(4) -0.002(4) C25 0.024(3) 0.052(3) 0.025(3) 0.001(2) 0.009(2) -0.006(2) C26 0.037(3) 0.074(5) 0.050(4) -0.023(4) 0.011(3) -0.018(3) C27 0.053(5) 0.109(7) 0.056(5) -0.031(5) 0.022(4) -0.034(5) C28 0.057(5) 0.125(8) 0.042(4) 0.005(5) 0.005(4) -0.042(6) C29 0.028(4) 0.134(8) 0.063(5) 0.051(5) 0.008(3) 0.002(4) C30 0.030(3) 0.071(5) 0.053(4) 0.029(3) 0.011(3) 0.003(3) C31 0.038(3) 0.054(4) 0.028(3) -0.004(3) 0.004(2) 0.025(3) C32 0.036(4) 0.125(7) 0.039(4) 0.005(4) 0.018(3) 0.006(4) C33 0.066(6) 0.201(12) 0.048(5) 0.014(6) 0.033(4) 0.029(7) C34 0.128(10) 0.204(14) 0.036(5) -0.012(7) 0.025(6) 0.102(10) C35 0.160(11) 0.098(7) 0.031(4) -0.031(5) -0.007(5) 0.075(7) C36 0.105(6) 0.043(4) 0.042(4) -0.013(3) 0.002(4) 0.031(4) C37 0.035(3) 0.034(3) 0.037(3) -0.004(3) 0.003(2) 0.004(2) C38 0.033(3) 0.041(3) 0.029(3) -0.005(2) 0.000(2) -0.002(3) C39 0.038(3) 0.029(3) 0.031(3) -0.001(2) 0.001(2) -0.002(2) C40 0.050(4) 0.045(3) 0.032(3) -0.001(3) 0.004(3) -0.005(3) C41 0.068(5) 0.038(3) 0.043(4) 0.008(3) 0.003(3) -0.008(3) C42 0.054(4) 0.033(3) 0.056(4) -0.007(3) 0.001(3) 0.007(3) C43 0.036(3) 0.041(3) 0.041(3) -0.007(3) 0.003(3) 0.005(3) C44 0.044(3) 0.054(4) 0.038(3) 0.001(3) 0.003(3) -0.008(3) C45 0.040(4) 0.051(4) 0.049(4) -0.005(3) -0.004(3) 0.003(3) C46 0.039(3) 0.076(5) 0.047(4) -0.009(4) 0.011(3) -0.008(4) C47 0.047(4) 0.052(4) 0.039(3) -0.005(3) -0.001(3) -0.025(3) C48 0.051(4) 0.050(4) 0.033(3) -0.012(3) 0.003(3) -0.008(3) C49 0.036(3) 0.037(3) 0.031(3) 0.006(2) 0.012(2) 0.009(2) C50 0.051(4) 0.039(3) 0.033(3) 0.014(3) 0.021(3) 0.013(3) C51 0.096(6) 0.046(4) 0.050(4) 0.006(3) 0.047(4) 0.025(4) C52 0.068(5) 0.095(6) 0.068(5) 0.010(5) 0.034(4) 0.046(5) C53 0.039(4) 0.109(7) 0.056(4) 0.003(5) 0.015(3) 0.031(4) C54 0.033(3) 0.070(5) 0.038(3) 0.005(3) 0.014(3) 0.016(3) C55 0.031(3) 0.030(3) 0.021(2) 0.004(2) 0.011(2) 0.014(2) C56 0.062(4) 0.023(3) 0.033(3) 0.001(2) 0.026(3) 0.008(3) C57 0.093(5) 0.035(3) 0.050(4) 0.017(3) 0.045(4) 0.017(3) C58 0.082(5) 0.061(4) 0.027(3) 0.015(3) 0.028(3) 0.037(4) C59 0.053(4) 0.060(4) 0.022(3) -0.004(3) -0.001(3) 0.021(3) C60 0.037(3) 0.042(3) 0.030(3) -0.001(3) 0.006(2) 0.012(3) F1 0.069(3) 0.0303(17) 0.060(2) -0.0066(16) 0.030(2) -0.0054(17) F2 0.134(4) 0.051(2) 0.086(3) -0.003(2) 0.067(3) 0.028(3) F3 0.102(4) 0.146(5) 0.113(4) 0.003(4) 0.055(3) 0.083(4) F4 0.037(2) 0.182(6) 0.099(4) -0.016(4) 0.010(2) 0.038(3) F5 0.0322(19) 0.089(3) 0.058(2) -0.021(2) 0.0025(17) 0.003(2) F6 0.104(3) 0.0334(19) 0.053(2) -0.0070(17) 0.043(2) -0.020(2) F7 0.178(5) 0.043(2) 0.080(3) 0.018(2) 0.086(3) -0.001(3) F8 0.137(4) 0.096(3) 0.033(2) 0.026(2) 0.042(3) 0.044(3) F9 0.094(3) 0.107(4) 0.028(2) -0.017(2) -0.005(2) 0.007(3) F10 0.053(2) 0.061(2) 0.041(2) -0.0113(18) 0.0051(17) -0.0216(19) Fe1 0.0294(4) 0.0427(5) 0.0388(5) 0.0073(4) 0.0026(4) -0.0017(4) Fe2 0.0392(4) 0.0327(4) 0.0356(4) -0.0046(4) 0.0055(3) -0.0028(4) P1 0.0290(7) 0.0271(7) 0.0215(6) 0.0036(5) 0.0068(5) -0.0037(5) P2 0.0241(7) 0.0282(7) 0.0257(7) -0.0015(5) 0.0027(5) 0.0032(5) Pt1 0.02178(9) 0.02236(9) 0.01992(8) 0.00216(8) 0.00516(6) -0.00025(8) C99A 0.063(8) 0.101(13) 0.128(16) 0.060(11) 0.038(9) 0.032(8) Cl1A 0.127(6) 0.059(3) 0.106(4) 0.024(3) 0.021(3) 0.011(3) Cl2A 0.107(4) 0.108(3) 0.082(3) 0.007(2) 0.007(3) 0.009(3) Cl3A 0.45(2) 0.62(3) 0.219(11) 0.258(15) 0.267(14) 0.39(2) C99B 0.063(8) 0.101(13) 0.128(16) 0.060(11) 0.038(9) 0.032(8) Cl1B 0.21(2) 0.198(15) 0.251(18) 0.082(13) 0.055(15) -0.061(13) Cl2B 0.117(8) 0.090(6) 0.302(17) -0.043(8) -0.068(9) 0.027(5) Cl3B 0.075(4) 0.085(4) 0.064(3) -0.017(3) 0.006(3) -0.023(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.389(7) . ? C1 C6 1.390(7) . ? C1 P1 1.828(5) . ? C2 C3 1.393(8) . ? C3 C4 1.373(8) . ? C4 C5 1.372(9) . ? C5 C6 1.387(8) . ? C7 C12 1.380(8) . ? C7 C8 1.388(8) . ? C7 P1 1.821(6) . ? C8 C9 1.390(10) . ? C9 C10 1.369(12) . ? C10 C11 1.383(12) . ? C11 C12 1.385(9) . ? C13 C14 1.197(7) . ? C13 P1 1.760(6) . ? C14 C15 1.422(8) . ? C15 C16 1.417(8) . ? C15 C19 1.433(9) . ? C15 Fe1 2.024(6) . ? C16 C17 1.400(9) . ? C16 Fe1 2.041(6) . ? C17 C18 1.424(10) . ? C17 Fe1 2.038(6) . ? C18 C19 1.418(9) . ? C18 Fe1 2.034(7) . ? C19 Fe1 2.017(6) . ? C20 C24 1.377(10) . ? C20 C21 1.410(10) . ? C20 Fe1 2.050(7) . ? C21 C22 1.400(10) . ? C21 Fe1 2.052(7) . ? C22 C23 1.420(11) . ? C22 Fe1 2.034(6) . ? C23 C24 1.421(10) . ? C23 Fe1 2.031(7) . ? C24 Fe1 2.040(7) . ? C25 C26 1.376(9) . ? C25 C30 1.389(8) . ? C25 P2 1.810(5) . ? C26 C27 1.388(9) . ? C27 C28 1.350(12) . ? C28 C29 1.358(12) . ? C29 C30 1.423(10) . ? C31 C32 1.368(10) . ? C31 C36 1.393(9) . ? C31 P2 1.830(6) . ? C32 C33 1.395(10) . ? C33 C34 1.382(16) . ? C34 C35 1.355(17) . ? C35 C36 1.375(11) . ? C37 C38 1.197(8) . ? C37 P2 1.747(6) . ? C38 C39 1.428(8) . ? C39 C43 1.422(8) . ? C39 C40 1.429(8) . ? C39 Fe2 2.037(5) . ? C40 C41 1.412(9) . ? C40 Fe2 2.036(6) . ? C41 C42 1.405(10) . ? C41 Fe2 2.047(6) . ? C42 C43 1.412(9) . ? C42 Fe2 2.051(6) . ? C43 Fe2 2.038(6) . ? C44 C45 1.418(9) . ? C44 C48 1.433(9) . ? C44 Fe2 2.059(6) . ? C45 C46 1.401(9) . ? C45 Fe2 2.039(6) . ? C46 C47 1.429(10) . ? C46 Fe2 2.044(6) . ? C47 C48 1.403(9) . ? C47 Fe2 2.052(6) . ? C48 Fe2 2.058(6) . ? C49 C50 1.378(8) . ? C49 C54 1.392(8) . ? C49 Pt1 2.068(5) . ? C50 F1 1.354(7) . ? C50 C51 1.387(9) . ? C51 F2 1.343(8) . ? C51 C52 1.377(11) . ? C52 F3 1.348(8) . ? C52 C53 1.360(12) . ? C53 F4 1.346(9) . ? C53 C54 1.379(9) . ? C54 F5 1.336(8) . ? C55 C60 1.370(7) . ? C55 C56 1.373(7) . ? C55 Pt1 2.069(5) . ? C56 F6 1.353(6) . ? C56 C57 1.386(8) . ? C57 F7 1.340(7) . ? C57 C58 1.367(10) . ? C58 F8 1.344(7) . ? C58 C59 1.351(10) . ? C59 F9 1.348(7) . ? C59 C60 1.384(8) . ? C60 F10 1.352(7) . ? P1 Pt1 2.2876(13) . ? P2 Pt1 2.2854(13) . ? C99A Cl2A 1.672(13) . ? C99A Cl3A 1.673(14) . ? C99A Cl1A 1.717(13) . ? C99B Cl2B 1.695(16) . ? C99B Cl3B 1.727(17) . ? C99B Cl1B 1.737(18) . ? 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 C2 C1 C6 119.7(5) . . ? C2 C1 P1 120.0(4) . . ? C6 C1 P1 120.3(4) . . ? C1 C2 C3 119.2(5) . . ? C4 C3 C2 120.4(6) . . ? C5 C4 C3 120.7(5) . . ? C4 C5 C6 119.6(5) . . ? C5 C6 C1 120.4(5) . . ? C12 C7 C8 120.1(6) . . ? C12 C7 P1 119.7(4) . . ? C8 C7 P1 120.1(5) . . ? C7 C8 C9 119.0(7) . . ? C10 C9 C8 120.9(8) . . ? C9 C10 C11 120.1(7) . . ? C10 C11 C12 119.7(8) . . ? C7 C12 C11 120.3(7) . . ? C14 C13 P1 179.4(5) . . ? C13 C14 C15 178.3(6) . . ? C16 C15 C14 125.5(6) . . ? C16 C15 C19 106.8(5) . . ? C14 C15 C19 127.6(6) . . ? C16 C15 Fe1 70.2(3) . . ? C14 C15 Fe1 124.3(4) . . ? C19 C15 Fe1 68.9(3) . . ? C17 C16 C15 109.5(6) . . ? C17 C16 Fe1 69.8(4) . . ? C15 C16 Fe1 69.0(4) . . ? C16 C17 C18 107.6(6) . . ? C16 C17 Fe1 70.0(4) . . ? C18 C17 Fe1 69.4(4) . . ? C19 C18 C17 108.2(6) . . ? C19 C18 Fe1 68.9(4) . . ? C17 C18 Fe1 69.7(4) . . ? C18 C19 C15 107.9(6) . . ? C18 C19 Fe1 70.2(4) . . ? C15 C19 Fe1 69.5(3) . . ? C24 C20 C21 109.0(7) . . ? C24 C20 Fe1 69.9(4) . . ? C21 C20 Fe1 69.9(4) . . ? C22 C21 C20 107.9(7) . . ? C22 C21 Fe1 69.3(4) . . ? C20 C21 Fe1 69.8(4) . . ? C21 C22 C23 107.8(6) . . ? C21 C22 Fe1 70.6(4) . . ? C23 C22 Fe1 69.4(4) . . ? C22 C23 C24 107.2(7) . . ? C22 C23 Fe1 69.7(4) . . ? C24 C23 Fe1 69.9(4) . . ? C20 C24 C23 108.2(7) . . ? C20 C24 Fe1 70.7(4) . . ? C23 C24 Fe1 69.2(4) . . ? C26 C25 C30 119.5(6) . . ? C26 C25 P2 119.4(4) . . ? C30 C25 P2 121.0(5) . . ? C25 C26 C27 121.3(7) . . ? C28 C27 C26 119.0(9) . . ? C27 C28 C29 121.7(7) . . ? C28 C29 C30 120.2(7) . . ? C25 C30 C29 118.1(7) . . ? C32 C31 C36 120.1(6) . . ? C32 C31 P2 120.7(5) . . ? C36 C31 P2 119.1(6) . . ? C31 C32 C33 119.5(9) . . ? C34 C33 C32 120.0(10) . . ? C35 C34 C33 119.9(9) . . ? C34 C35 C36 121.1(10) . . ? C35 C36 C31 119.5(9) . . ? C38 C37 P2 171.6(5) . . ? C37 C38 C39 176.4(7) . . ? C43 C39 C38 125.0(6) . . ? C43 C39 C40 107.5(5) . . ? C38 C39 C40 127.3(6) . . ? C43 C39 Fe2 69.6(3) . . ? C38 C39 Fe2 122.0(4) . . ? C40 C39 Fe2 69.4(3) . . ? C41 C40 C39 107.4(6) . . ? C41 C40 Fe2 70.2(4) . . ? C39 C40 Fe2 69.5(3) . . ? C42 C41 C40 108.8(6) . . ? C42 C41 Fe2 70.1(4) . . ? C40 C41 Fe2 69.3(3) . . ? C41 C42 C43 108.1(6) . . ? C41 C42 Fe2 69.8(4) . . ? C43 C42 Fe2 69.3(3) . . ? C42 C43 C39 108.1(6) . . ? C42 C43 Fe2 70.3(4) . . ? C39 C43 Fe2 69.5(3) . . ? C45 C44 C48 107.3(6) . . ? C45 C44 Fe2 69.0(4) . . ? C48 C44 Fe2 69.6(4) . . ? C46 C45 C44 108.4(6) . . ? C46 C45 Fe2 70.1(4) . . ? C44 C45 Fe2 70.5(4) . . ? C45 C46 C47 108.3(6) . . ? C45 C46 Fe2 69.7(4) . . ? C47 C46 Fe2 69.9(4) . . ? C48 C47 C46 107.7(6) . . ? C48 C47 Fe2 70.3(3) . . ? C46 C47 Fe2 69.3(3) . . ? C47 C48 C44 108.3(6) . . ? C47 C48 Fe2 69.8(3) . . ? C44 C48 Fe2 69.7(3) . . ? C50 C49 C54 115.5(5) . . ? C50 C49 Pt1 121.4(4) . . ? C54 C49 Pt1 123.1(4) . . ? F1 C50 C49 119.7(5) . . ? F1 C50 C51 117.1(6) . . ? C49 C50 C51 123.2(6) . . ? F2 C51 C52 120.7(7) . . ? F2 C51 C50 120.4(7) . . ? C52 C51 C50 118.9(7) . . ? F3 C52 C53 120.8(8) . . ? F3 C52 C51 119.3(8) . . ? C53 C52 C51 119.9(7) . . ? F4 C53 C52 119.9(7) . . ? F4 C53 C54 119.9(8) . . ? C52 C53 C54 120.1(7) . . ? F5 C54 C53 117.3(6) . . ? F5 C54 C49 120.3(5) . . ? C53 C54 C49 122.4(7) . . ? C60 C55 C56 115.2(5) . . ? C60 C55 Pt1 119.8(4) . . ? C56 C55 Pt1 124.6(4) . . ? F6 C56 C55 120.0(5) . . ? F6 C56 C57 116.8(5) . . ? C55 C56 C57 123.2(6) . . ? F7 C57 C58 120.3(6) . . ? F7 C57 C56 120.4(6) . . ? C58 C57 C56 119.3(6) . . ? F8 C58 C59 121.0(7) . . ? F8 C58 C57 119.8(7) . . ? C59 C58 C57 119.3(5) . . ? F9 C59 C58 119.6(6) . . ? F9 C59 C60 120.1(6) . . ? C58 C59 C60 120.3(6) . . ? F10 C60 C55 120.7(5) . . ? F10 C60 C59 116.5(5) . . ? C55 C60 C59 122.8(6) . . ? C19 Fe1 C15 41.6(3) . . ? C19 Fe1 C23 154.7(3) . . ? C15 Fe1 C23 119.7(3) . . ? C19 Fe1 C18 41.0(3) . . ? C15 Fe1 C18 69.2(3) . . ? C23 Fe1 C18 163.3(3) . . ? C19 Fe1 C22 119.2(3) . . ? C15 Fe1 C22 106.9(3) . . ? C23 Fe1 C22 40.9(3) . . ? C18 Fe1 C22 154.3(3) . . ? C19 Fe1 C17 69.2(3) . . ? C15 Fe1 C17 69.0(2) . . ? C23 Fe1 C17 126.0(3) . . ? C18 Fe1 C17 40.9(3) . . ? C22 Fe1 C17 163.4(3) . . ? C19 Fe1 C24 162.2(3) . . ? C15 Fe1 C24 155.5(3) . . ? C23 Fe1 C24 40.8(3) . . ? C18 Fe1 C24 125.7(3) . . ? C22 Fe1 C24 68.3(3) . . ? C17 Fe1 C24 108.3(3) . . ? C19 Fe1 C16 68.7(3) . . ? C15 Fe1 C16 40.8(2) . . ? C23 Fe1 C16 108.6(3) . . ? C18 Fe1 C16 68.0(3) . . ? C22 Fe1 C16 126.5(3) . . ? C17 Fe1 C16 40.1(3) . . ? C24 Fe1 C16 121.5(3) . . ? C19 Fe1 C20 125.7(3) . . ? C15 Fe1 C20 163.0(3) . . ? C23 Fe1 C20 67.4(3) . . ? C18 Fe1 C20 108.4(3) . . ? C22 Fe1 C20 67.6(3) . . ? C17 Fe1 C20 120.9(3) . . ? C24 Fe1 C20 39.4(3) . . ? C16 Fe1 C20 155.3(3) . . ? C19 Fe1 C21 107.1(3) . . ? C15 Fe1 C21 125.4(3) . . ? C23 Fe1 C21 67.8(3) . . ? C18 Fe1 C21 120.2(3) . . ? C22 Fe1 C21 40.1(3) . . ? C17 Fe1 C21 155.2(3) . . ? C24 Fe1 C21 67.4(3) . . ? C16 Fe1 C21 163.2(3) . . ? C20 Fe1 C21 40.2(3) . . ? C40 Fe2 C39 41.1(2) . . ? C40 Fe2 C43 68.7(3) . . ? C39 Fe2 C43 40.9(2) . . ? C40 Fe2 C45 115.2(3) . . ? C39 Fe2 C45 109.4(2) . . ? C43 Fe2 C45 133.2(3) . . ? C40 Fe2 C46 107.8(3) . . ? C39 Fe2 C46 131.4(3) . . ? C43 Fe2 C46 171.3(3) . . ? C45 Fe2 C46 40.1(3) . . ? C40 Fe2 C41 40.5(2) . . ? C39 Fe2 C41 68.2(2) . . ? C43 Fe2 C41 67.9(3) . . ? C45 Fe2 C41 146.7(3) . . ? C46 Fe2 C41 115.1(3) . . ? C40 Fe2 C42 68.2(3) . . ? C39 Fe2 C42 68.3(2) . . ? C43 Fe2 C42 40.4(2) . . ? C45 Fe2 C42 172.4(3) . . ? C46 Fe2 C42 146.8(3) . . ? C41 Fe2 C42 40.1(3) . . ? C40 Fe2 C47 130.5(3) . . ? C39 Fe2 C47 170.3(3) . . ? C43 Fe2 C47 147.4(3) . . ? C45 Fe2 C47 68.2(3) . . ? C46 Fe2 C47 40.9(3) . . ? C41 Fe2 C47 108.3(3) . . ? C42 Fe2 C47 115.3(3) . . ? C40 Fe2 C48 169.3(3) . . ? C39 Fe2 C48 149.0(3) . . ? C43 Fe2 C48 117.1(3) . . ? C45 Fe2 C48 68.2(3) . . ? C46 Fe2 C48 67.8(3) . . ? C41 Fe2 C48 131.5(3) . . ? C42 Fe2 C48 109.8(3) . . ? C47 Fe2 C48 39.9(3) . . ? C40 Fe2 C44 147.9(3) . . ? C39 Fe2 C44 116.8(2) . . ? C43 Fe2 C44 110.7(3) . . ? C45 Fe2 C44 40.5(3) . . ? C46 Fe2 C44 67.7(3) . . ? C41 Fe2 C44 171.2(3) . . ? C42 Fe2 C44 133.3(3) . . ? C47 Fe2 C44 68.0(3) . . ? C48 Fe2 C44 40.7(2) . . ? C13 P1 C7 101.9(3) . . ? C13 P1 C1 104.1(2) . . ? C7 P1 C1 103.5(2) . . ? C13 P1 Pt1 117.23(19) . . ? C7 P1 Pt1 116.40(17) . . ? C1 P1 Pt1 112.05(17) . . ? C37 P2 C25 106.0(3) . . ? C37 P2 C31 102.1(3) . . ? C25 P2 C31 104.5(3) . . ? C37 P2 Pt1 116.0(2) . . ? C25 P2 Pt1 110.99(19) . . ? C31 P2 Pt1 116.06(17) . . ? C49 Pt1 C55 87.2(2) . . ? C49 Pt1 P2 174.77(16) . . ? C55 Pt1 P2 88.95(13) . . ? C49 Pt1 P1 91.00(15) . . ? C55 Pt1 P1 175.68(15) . . ? P2 Pt1 P1 93.12(5) . . ? Cl2A C99A Cl3A 107.6(7) . . ? Cl2A C99A Cl1A 122.3(9) . . ? Cl3A C99A Cl1A 115.2(11) . . ? Cl2B C99B Cl3B 106.2(10) . . ? Cl2B C99B Cl1B 108.5(15) . . ? Cl3B C99B Cl1B 97.2(13) . . ? #===END data_complex9 _database_code_depnum_ccdc_archive 'CCDC 713070' _audit_creation_date 2009-02-02T11:46:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common s50 _chemical_formula_sum 'C74 H42 Cl4 F20 Fe2 P2 Pt2' _chemical_formula_weight 2016.7 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 22.5130(7) _cell_length_b 12.8900(3) _cell_length_c 25.7752(8) _cell_angle_alpha 90 _cell_angle_beta 112.4820(10) _cell_angle_gamma 90 _cell_volume 6911.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 16348 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 26.02 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.375 _exptl_crystal_size_min 0.175 _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_T_max 0.436 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0136553 _diffrn_orient_matrix_ub_12 0.0640309 _diffrn_orient_matrix_ub_13 -0.0143701 _diffrn_orient_matrix_ub_21 0.0431759 _diffrn_orient_matrix_ub_22 -0.0039492 _diffrn_orient_matrix_ub_23 0.0313651 _diffrn_orient_matrix_ub_31 0.0161346 _diffrn_orient_matrix_ub_32 -0.0436237 _diffrn_orient_matrix_ub_33 -0.0239319 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_number 13582 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 13582 _reflns_number_gt 11771 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+43.9723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13582 _refine_ls_number_parameters 946 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.273 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8621(3) 0.8562(4) 0.6556(2) 0.0270(13) Uani 1 1 d . . . C2 C 0.8158(3) 0.9176(5) 0.6159(2) 0.0275(13) Uani 1 1 d . . . C3 C 0.8239(3) 0.9617(5) 0.5704(3) 0.0350(15) Uani 1 1 d . . . C4 C 0.8798(3) 0.9435(5) 0.5622(3) 0.0391(16) Uani 1 1 d . . . C5 C 0.9271(3) 0.8847(5) 0.6003(3) 0.0379(16) Uani 1 1 d . . . C6 C 0.9180(3) 0.8450(5) 0.6467(3) 0.0318(14) Uani 1 1 d . . . C7 C 0.9070(3) 0.9081(4) 0.7725(2) 0.0261(12) Uani 1 1 d . . . C8 C 0.8941(3) 1.0104(5) 0.7773(3) 0.0320(14) Uani 1 1 d . . . C9 C 0.9356(3) 1.0780(5) 0.8155(3) 0.0397(16) Uani 1 1 d . . . C10 C 0.9942(3) 1.0420(6) 0.8513(3) 0.0404(17) Uani 1 1 d . . . C11 C 1.0105(3) 0.9405(6) 0.8476(3) 0.0411(17) Uani 1 1 d . . . C12 C 0.9678(3) 0.8764(5) 0.8079(3) 0.0305(14) Uani 1 1 d . . . C13 C 0.8211(3) 0.5800(5) 0.6387(2) 0.0270(13) Uani 1 1 d . . . C14 C 0.8861(3) 0.5919(5) 0.6496(3) 0.0358(15) Uani 1 1 d . . . H14 H 0.9098 0.643 0.6743 0.043 Uiso 1 1 calc R . . C15 C 0.9159(3) 0.5270(6) 0.6234(3) 0.0456(18) Uani 1 1 d . . . H15 H 0.9591 0.5361 0.6298 0.055 Uiso 1 1 calc R . . C16 C 0.8809(4) 0.4494(6) 0.5880(3) 0.0464(18) Uani 1 1 d . . . H16 H 0.9007 0.4062 0.5706 0.056 Uiso 1 1 calc R . . C17 C 0.8169(3) 0.4355(5) 0.5784(3) 0.0404(16) Uani 1 1 d . . . H17 H 0.7939 0.3821 0.5551 0.049 Uiso 1 1 calc R . . C18 C 0.7867(3) 0.5005(5) 0.6032(3) 0.0343(14) Uani 1 1 d . . . H18 H 0.7434 0.4912 0.5962 0.041 Uiso 1 1 calc R . . C19 C 0.7069(3) 0.7035(4) 0.6095(3) 0.0278(13) Uani 1 1 d . . . C20 C 0.7064(3) 0.7080(5) 0.5551(3) 0.0341(14) Uani 1 1 d . . . H20 H 0.7434 0.6932 0.5487 0.041 Uiso 1 1 calc R . . C21 C 0.6501(3) 0.7348(5) 0.5111(3) 0.0411(17) Uani 1 1 d . . . H21 H 0.6493 0.7364 0.4748 0.049 Uiso 1 1 calc R . . C22 C 0.5963(3) 0.7571(6) 0.5737(3) 0.0417(17) Uani 1 1 d . . . H22 H 0.5596 0.7751 0.58 0.05 Uiso 1 1 calc R . . C23 C 0.5955(3) 0.7589(6) 0.5199(3) 0.0456(18) Uani 1 1 d . . . H23 H 0.558 0.7764 0.4898 0.055 Uiso 1 1 calc R . . C24 C 0.6516(3) 0.7286(5) 0.6182(3) 0.0354(15) Uani 1 1 d . . . H24 H 0.6518 0.7262 0.6543 0.043 Uiso 1 1 calc R . . C25 C 0.8409(3) 0.8587(4) 0.8564(2) 0.0254(12) Uani 1 1 d . . . C26 C 0.8178(3) 0.9582(5) 0.8597(3) 0.0317(14) Uani 1 1 d . . . H26 H 0.7829 0.9844 0.8297 0.038 Uiso 1 1 calc R . . C27 C 0.8467(3) 1.0178(5) 0.9075(3) 0.0390(16) Uani 1 1 d . . . H27 H 0.8309 1.0837 0.9097 0.047 Uiso 1 1 calc R . . C28 C 0.8990(3) 0.9796(5) 0.9520(3) 0.0426(17) Uani 1 1 d . . . H28 H 0.9185 1.0198 0.984 0.051 Uiso 1 1 calc R . . C29 C 0.9223(3) 0.8813(5) 0.9490(3) 0.0394(16) Uani 1 1 d . . . H29 H 0.9573 0.8555 0.979 0.047 Uiso 1 1 calc R . . C30 C 0.8936(3) 0.8214(5) 0.9012(3) 0.0341(15) Uani 1 1 d . . . H30 H 0.9098 0.7557 0.8992 0.041 Uiso 1 1 calc R . . C31 C 0.7194(3) 0.8230(4) 0.7657(2) 0.0269(13) Uani 1 1 d . . . C32 C 0.7013(3) 0.9027(5) 0.7261(3) 0.0365(15) Uani 1 1 d . . . H32 H 0.7313 0.9319 0.7137 0.044 Uiso 1 1 calc R . . C33 C 0.6381(3) 0.9381(6) 0.7054(3) 0.0471(18) Uani 1 1 d . . . H33 H 0.6261 0.992 0.6794 0.057 Uiso 1 1 calc R . . C34 C 0.5931(3) 0.8941(6) 0.7230(3) 0.0481(19) Uani 1 1 d . . . H34 H 0.5508 0.9179 0.7088 0.058 Uiso 1 1 calc R . . C35 C 0.6112(3) 0.8147(6) 0.7619(3) 0.0431(17) Uani 1 1 d . . . H35 H 0.5809 0.7847 0.7736 0.052 Uiso 1 1 calc R . . C36 C 0.6740(3) 0.7792(5) 0.7835(3) 0.0311(14) Uani 1 1 d . . . H36 H 0.6859 0.726 0.8099 0.037 Uiso 1 1 calc R . . C37 C 0.7482(3) 0.5825(4) 0.7055(2) 0.0246(12) Uani 1 1 d . . . C38 C 0.7119(3) 0.5333(4) 0.7225(2) 0.0230(12) Uani 1 1 d . . . C39 C 0.8870(3) 0.4574(4) 0.8552(3) 0.0273(13) Uani 1 1 d . . . C40 C 0.9438(3) 0.5138(5) 0.8803(2) 0.0277(13) Uani 1 1 d . . . C41 C 0.9936(3) 0.4779(5) 0.9268(3) 0.0318(14) Uani 1 1 d . . . C42 C 0.9886(3) 0.3861(5) 0.9507(3) 0.0353(15) Uani 1 1 d . . . C43 C 0.9331(3) 0.3291(5) 0.9279(3) 0.0327(14) Uani 1 1 d . . . C44 C 0.8835(3) 0.3658(5) 0.8807(3) 0.0296(13) Uani 1 1 d . . . C45 C 0.8410(3) 0.3975(4) 0.7434(3) 0.0289(13) Uani 1 1 d . . . C46 C 0.8027(3) 0.3167(5) 0.7146(3) 0.0329(14) Uani 1 1 d . . . C47 C 0.8202(4) 0.2448(5) 0.6836(3) 0.0437(18) Uani 1 1 d . . . C48 C 0.8809(4) 0.2488(6) 0.6831(3) 0.050(2) Uani 1 1 d . . . C49 C 0.9219(4) 0.3261(6) 0.7125(3) 0.0470(18) Uani 1 1 d . . . C50 C 0.9013(3) 0.3991(5) 0.7412(3) 0.0342(15) Uani 1 1 d . . . C51 C 0.7998(3) 0.6560(4) 0.8214(2) 0.0220(12) Uani 1 1 d . . . C52 C 0.7846(3) 0.6015(4) 0.8530(2) 0.0225(12) Uani 1 1 d . . . C53 C 0.6571(3) 0.4942(4) 0.7308(2) 0.0249(12) Uani 1 1 d . . . C54 C 0.6521(3) 0.3997(5) 0.7584(2) 0.0315(14) Uani 1 1 d . . . H54 H 0.6848 0.3517 0.7749 0.038 Uiso 1 1 calc R . . C55 C 0.5881(3) 0.3932(5) 0.7559(3) 0.0369(15) Uani 1 1 d . . . H55 H 0.5715 0.3402 0.7708 0.044 Uiso 1 1 calc R . . C56 C 0.5541(3) 0.4818(5) 0.7269(3) 0.0381(16) Uani 1 1 d . . . H56 H 0.5112 0.4964 0.7194 0.046 Uiso 1 1 calc R . . C57 C 0.5955(3) 0.5435(5) 0.7111(3) 0.0318(14) Uani 1 1 d . . . H57 H 0.5848 0.6057 0.6914 0.038 Uiso 1 1 calc R . . C58 C 0.6065(3) 0.2716(5) 0.6380(3) 0.0426(17) Uani 1 1 d . . . H58 H 0.6357 0.2192 0.6554 0.051 Uiso 1 1 calc R . . C59 C 0.6190(4) 0.3618(6) 0.6133(3) 0.0461(18) Uani 1 1 d . . . H59 H 0.6582 0.3797 0.6115 0.055 Uiso 1 1 calc R . . C60 C 0.5617(4) 0.4208(7) 0.5915(3) 0.051(2) Uani 1 1 d . . . H60 H 0.5567 0.4842 0.5731 0.062 Uiso 1 1 calc R . . C61 C 0.5140(4) 0.3672(7) 0.6026(3) 0.054(2) Uani 1 1 d . . . H61 H 0.4716 0.3884 0.5926 0.064 Uiso 1 1 calc R . . C62 C 0.5413(4) 0.2752(6) 0.6315(3) 0.050(2) Uani 1 1 d . . . H62 H 0.52 0.2255 0.6442 0.06 Uiso 1 1 calc R . . C63 C 0.7680(3) 0.5459(4) 0.8932(2) 0.0253(12) Uani 1 1 d . . . C64 C 0.8103(3) 0.5193(5) 0.9493(3) 0.0330(14) Uani 1 1 d . . . H64 H 0.8545 0.5296 0.965 0.04 Uiso 1 1 calc R . . C65 C 0.7726(3) 0.4747(5) 0.9761(3) 0.0386(16) Uani 1 1 d . . . H65 H 0.7879 0.4495 1.0127 0.046 Uiso 1 1 calc R . . C66 C 0.7074(3) 0.4745(5) 0.9382(3) 0.0362(15) Uani 1 1 d . . . H66 H 0.6728 0.4494 0.9458 0.043 Uiso 1 1 calc R . . C67 C 0.7037(3) 0.5187(4) 0.8871(3) 0.0296(13) Uani 1 1 d . . . H67 H 0.6665 0.5284 0.8553 0.036 Uiso 1 1 calc R . . C68 C 0.7910(4) 0.7492(5) 0.9948(3) 0.0462(18) Uani 1 1 d . . . H68 H 0.8355 0.7566 1.0105 0.055 Uiso 1 1 calc R . . C69 C 0.7522(4) 0.7045(6) 1.0214(3) 0.0452(17) Uani 1 1 d . . . H69 H 0.7666 0.6782 1.0578 0.054 Uiso 1 1 calc R . . C70 C 0.6879(4) 0.7074(5) 0.9824(3) 0.0410(16) Uani 1 1 d . . . H70 H 0.6524 0.6826 0.9886 0.049 Uiso 1 1 calc R . . C71 C 0.6866(4) 0.7541(5) 0.9328(3) 0.0392(16) Uani 1 1 d . . . H71 H 0.6502 0.7657 0.9005 0.047 Uiso 1 1 calc R . . C72 C 0.7501(4) 0.7802(5) 0.9406(3) 0.0397(16) Uani 1 1 d . . . H72 H 0.7628 0.8125 0.9142 0.048 Uiso 1 1 calc R . . F1 F 0.75924(16) 0.9377(3) 0.62102(15) 0.0345(8) Uani 1 1 d . . . F2 F 0.7785(2) 1.0227(3) 0.53439(16) 0.0509(11) Uani 1 1 d . . . F3 F 0.8880(2) 0.9832(4) 0.51699(18) 0.0595(12) Uani 1 1 d . . . F4 F 0.98211(19) 0.8663(4) 0.59275(19) 0.0538(11) Uani 1 1 d . . . F5 F 0.96819(16) 0.7915(3) 0.68376(16) 0.0400(9) Uani 1 1 d . . . F6 F 0.83517(18) 1.0487(3) 0.74548(18) 0.0480(10) Uani 1 1 d . . . F7 F 0.9191(2) 1.1766(3) 0.8199(2) 0.0633(13) Uani 1 1 d . . . F8 F 1.0354(2) 1.1048(4) 0.8907(2) 0.0690(14) Uani 1 1 d . . . F9 F 1.06783(19) 0.9043(4) 0.8827(2) 0.0678(14) Uani 1 1 d . . . F10 F 0.98618(17) 0.7764(3) 0.80708(18) 0.0457(10) Uani 1 1 d . . . F11 F 0.95154(16) 0.6056(3) 0.85812(15) 0.0349(8) Uani 1 1 d . . . F12 F 1.04861(18) 0.5342(3) 0.94891(17) 0.0477(10) Uani 1 1 d . . . F14 F 0.9277(2) 0.2385(3) 0.95169(17) 0.0482(10) Uani 1 1 d . . . F15 F 0.82962(17) 0.3062(3) 0.85973(16) 0.0389(9) Uani 1 1 d . . . F16 F 0.94360(17) 0.4759(3) 0.76666(16) 0.0415(9) Uani 1 1 d . . . F17 F 0.9819(2) 0.3335(4) 0.7119(2) 0.0685(14) Uani 1 1 d . . . F19 F 0.7786(2) 0.1717(3) 0.65355(18) 0.0598(13) Uani 1 1 d . . . F20 F 0.74362(18) 0.3049(3) 0.71550(18) 0.0474(10) Uani 1 1 d . . . Fe1 Fe 0.58929(4) 0.40091(7) 0.67621(4) 0.0307(2) Uani 1 1 d . . . Fe2 Fe 0.74289(4) 0.62348(7) 0.95032(4) 0.02780(19) Uani 1 1 d . . . P1 P 0.78012(7) 0.66838(11) 0.66882(6) 0.0232(3) Uani 1 1 d . . . P2 P 0.80351(7) 0.78133(11) 0.79272(6) 0.0216(3) Uani 1 1 d . . . Pt1 Pt 0.841757(10) 0.800896(16) 0.722894(9) 0.02133(6) Uani 1 1 d . . . Pt2 Pt 0.814073(10) 0.509726(16) 0.785377(9) 0.02184(6) Uani 1 1 d . . . Cl1 Cl 0.84190(19) 0.7124(3) 0.49398(14) 0.1104(11) Uani 1 1 d . . . Cl2 Cl 0.93330(15) 0.5751(3) 0.47454(18) 0.1289(14) Uani 1 1 d . . . C100 C 0.8540(5) 0.6032(8) 0.4586(4) 0.080(3) Uani 1 1 d . . . H10A H 0.8336 0.5438 0.468 0.096 Uiso 1 1 calc R . . H10B H 0.8331 0.6148 0.4185 0.096 Uiso 1 1 calc R . . F18 F 0.8995(3) 0.1797(4) 0.6527(2) 0.0766(16) Uani 1 1 d . . . F13 F 1.03767(19) 0.3509(3) 0.99636(16) 0.0493(11) Uani 1 1 d . . . Cl3 Cl 0.07137(13) 0.3234(2) 0.85968(11) 0.0770(7) Uani 1 1 d . . . C99A C 0.0987(3) 0.4112(8) 0.8258(5) 0.178(9) Uani 0.4 1 d PD A 1 H99A H 0.0656 0.4637 0.8115 0.214 Uiso 0.4 1 calc PR A 1 H99B H 0.1012 0.3762 0.7934 0.214 Uiso 0.4 1 calc PR A 1 Cl4A Cl 0.1701(3) 0.4757(6) 0.8578(3) 0.093(2) Uani 0.4 1 d PD A 1 C99B C 0.0987(3) 0.4112(8) 0.8258(5) 0.178(9) Uani 0.6 1 d PD A 2 H99C H 0.1067 0.4761 0.8464 0.214 Uiso 0.6 1 calc PR A 2 H99D H 0.0656 0.4237 0.789 0.214 Uiso 0.6 1 calc PR A 2 Cl4B Cl 0.1682(2) 0.3733(4) 0.8179(2) 0.0933(15) Uani 0.6 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 C1 0.032(3) 0.022(3) 0.027(3) 0.001(2) 0.012(3) -0.008(2) C2 0.029(3) 0.031(3) 0.024(3) 0.001(3) 0.011(3) -0.001(3) C3 0.036(3) 0.040(4) 0.027(3) 0.003(3) 0.010(3) -0.001(3) C4 0.050(4) 0.043(4) 0.026(3) 0.006(3) 0.017(3) -0.009(3) C5 0.038(4) 0.046(4) 0.041(4) -0.002(3) 0.026(3) -0.005(3) C6 0.025(3) 0.037(4) 0.029(3) -0.002(3) 0.006(3) 0.000(3) C7 0.026(3) 0.028(3) 0.029(3) -0.002(3) 0.014(3) -0.006(2) C8 0.029(3) 0.034(3) 0.030(3) 0.001(3) 0.008(3) -0.002(3) C9 0.046(4) 0.030(4) 0.040(4) -0.009(3) 0.013(3) -0.011(3) C10 0.042(4) 0.044(4) 0.031(4) -0.011(3) 0.009(3) -0.025(3) C11 0.028(3) 0.050(4) 0.037(4) 0.005(3) 0.003(3) -0.012(3) C12 0.021(3) 0.030(3) 0.040(4) 0.001(3) 0.010(3) -0.006(2) C13 0.031(3) 0.033(3) 0.018(3) 0.000(2) 0.010(2) -0.001(3) C14 0.033(3) 0.038(4) 0.036(4) -0.012(3) 0.012(3) -0.007(3) C15 0.033(4) 0.053(4) 0.051(5) -0.009(4) 0.017(3) -0.001(3) C16 0.049(4) 0.048(4) 0.045(4) -0.015(3) 0.021(4) 0.007(3) C17 0.046(4) 0.034(4) 0.033(4) -0.013(3) 0.007(3) -0.004(3) C18 0.035(3) 0.032(3) 0.034(3) -0.005(3) 0.010(3) -0.002(3) C19 0.025(3) 0.023(3) 0.030(3) 0.001(3) 0.005(2) -0.006(2) C20 0.043(4) 0.032(3) 0.026(3) 0.005(3) 0.011(3) 0.000(3) C21 0.051(4) 0.042(4) 0.018(3) 0.004(3) 0.000(3) -0.001(3) C22 0.029(3) 0.049(4) 0.040(4) 0.012(3) 0.005(3) 0.000(3) C23 0.036(4) 0.045(4) 0.038(4) 0.010(3) -0.006(3) -0.006(3) C24 0.029(3) 0.040(4) 0.034(4) 0.008(3) 0.008(3) -0.002(3) C25 0.027(3) 0.025(3) 0.025(3) 0.000(2) 0.011(2) -0.006(2) C26 0.033(3) 0.028(3) 0.032(3) 0.001(3) 0.009(3) 0.002(3) C27 0.046(4) 0.026(3) 0.042(4) -0.011(3) 0.014(3) 0.000(3) C28 0.049(4) 0.041(4) 0.031(4) -0.016(3) 0.007(3) -0.013(3) C29 0.038(4) 0.035(4) 0.033(4) -0.004(3) -0.001(3) -0.004(3) C30 0.028(3) 0.029(3) 0.038(4) -0.002(3) 0.004(3) 0.000(3) C31 0.022(3) 0.026(3) 0.029(3) -0.004(2) 0.006(2) 0.003(2) C32 0.032(3) 0.041(4) 0.036(4) 0.008(3) 0.012(3) 0.009(3) C33 0.040(4) 0.050(4) 0.041(4) 0.011(3) 0.005(3) 0.017(3) C34 0.025(3) 0.057(5) 0.051(5) 0.002(4) 0.002(3) 0.010(3) C35 0.028(3) 0.050(4) 0.052(4) -0.002(4) 0.016(3) -0.002(3) C36 0.027(3) 0.032(3) 0.033(3) -0.002(3) 0.011(3) 0.001(3) C37 0.026(3) 0.023(3) 0.019(3) 0.001(2) 0.003(2) 0.002(2) C38 0.019(3) 0.024(3) 0.021(3) -0.004(2) 0.002(2) 0.001(2) C39 0.022(3) 0.023(3) 0.029(3) 0.003(2) 0.002(2) 0.007(2) C40 0.029(3) 0.029(3) 0.023(3) -0.001(2) 0.007(2) 0.001(2) C41 0.024(3) 0.034(3) 0.028(3) -0.004(3) -0.001(3) 0.000(3) C42 0.032(3) 0.040(4) 0.022(3) 0.003(3) -0.003(3) 0.015(3) C43 0.040(4) 0.023(3) 0.031(3) 0.003(3) 0.009(3) 0.007(3) C44 0.029(3) 0.026(3) 0.031(3) -0.002(3) 0.009(3) -0.001(2) C45 0.035(3) 0.021(3) 0.029(3) -0.001(2) 0.009(3) 0.010(2) C46 0.035(3) 0.028(3) 0.031(3) -0.005(3) 0.008(3) 0.004(3) C47 0.053(4) 0.032(4) 0.035(4) -0.010(3) 0.004(3) 0.007(3) C48 0.064(5) 0.044(4) 0.037(4) -0.009(3) 0.016(4) 0.021(4) C49 0.046(4) 0.063(5) 0.033(4) -0.002(4) 0.016(3) 0.016(4) C50 0.034(3) 0.038(4) 0.029(3) -0.005(3) 0.011(3) 0.010(3) C51 0.026(3) 0.021(3) 0.020(3) -0.005(2) 0.009(2) -0.001(2) C52 0.023(3) 0.021(3) 0.020(3) -0.003(2) 0.005(2) 0.002(2) C53 0.027(3) 0.029(3) 0.015(3) -0.007(2) 0.004(2) -0.008(2) C54 0.039(3) 0.033(3) 0.024(3) -0.003(3) 0.013(3) -0.006(3) C55 0.043(4) 0.039(4) 0.034(4) -0.004(3) 0.021(3) -0.012(3) C56 0.032(3) 0.045(4) 0.044(4) -0.013(3) 0.021(3) -0.007(3) C57 0.029(3) 0.035(3) 0.030(3) -0.006(3) 0.010(3) -0.001(3) C58 0.048(4) 0.037(4) 0.046(4) -0.023(3) 0.021(3) -0.009(3) C59 0.052(4) 0.051(4) 0.047(4) -0.018(4) 0.032(4) -0.017(4) C60 0.061(5) 0.061(5) 0.035(4) -0.012(4) 0.021(4) -0.008(4) C61 0.040(4) 0.069(6) 0.040(4) -0.027(4) 0.002(3) -0.008(4) C62 0.053(5) 0.056(5) 0.048(4) -0.030(4) 0.027(4) -0.035(4) C63 0.029(3) 0.019(3) 0.026(3) 0.002(2) 0.009(3) 0.006(2) C64 0.033(3) 0.027(3) 0.033(3) 0.006(3) 0.005(3) 0.003(3) C65 0.056(4) 0.027(3) 0.033(4) 0.010(3) 0.018(3) 0.001(3) C66 0.046(4) 0.026(3) 0.043(4) 0.000(3) 0.024(3) -0.004(3) C67 0.032(3) 0.022(3) 0.032(3) -0.002(3) 0.010(3) -0.003(2) C68 0.045(4) 0.037(4) 0.057(5) -0.021(4) 0.021(4) -0.010(3) C69 0.063(5) 0.044(4) 0.033(4) -0.004(3) 0.023(4) 0.001(4) C70 0.051(4) 0.037(4) 0.049(4) -0.005(3) 0.034(4) 0.001(3) C71 0.054(4) 0.029(3) 0.036(4) 0.002(3) 0.017(3) 0.007(3) C72 0.065(5) 0.022(3) 0.046(4) 0.001(3) 0.037(4) 0.001(3) F1 0.0272(18) 0.039(2) 0.037(2) 0.0080(16) 0.0114(16) 0.0041(15) F2 0.051(2) 0.059(3) 0.037(2) 0.023(2) 0.0106(19) 0.011(2) F3 0.069(3) 0.078(3) 0.042(2) 0.015(2) 0.034(2) -0.007(2) F4 0.044(2) 0.071(3) 0.062(3) 0.004(2) 0.037(2) 0.001(2) F5 0.0276(19) 0.044(2) 0.048(2) 0.0053(18) 0.0149(17) 0.0036(16) F6 0.038(2) 0.030(2) 0.062(3) 0.0003(19) 0.005(2) 0.0044(17) F7 0.074(3) 0.030(2) 0.077(3) -0.020(2) 0.019(3) -0.007(2) F8 0.064(3) 0.060(3) 0.060(3) -0.015(2) -0.003(2) -0.030(2) F9 0.032(2) 0.070(3) 0.071(3) 0.009(3) -0.014(2) -0.007(2) F10 0.0278(19) 0.037(2) 0.063(3) 0.0047(19) 0.0082(18) 0.0037(16) F11 0.0354(19) 0.0274(18) 0.034(2) 0.0068(15) 0.0050(16) -0.0028(15) F12 0.032(2) 0.047(2) 0.047(2) 0.0037(19) -0.0034(18) -0.0069(18) F14 0.054(3) 0.035(2) 0.046(2) 0.0144(18) 0.008(2) -0.0005(18) F15 0.036(2) 0.0291(19) 0.043(2) 0.0042(17) 0.0054(17) -0.0054(16) F16 0.0315(19) 0.051(2) 0.044(2) -0.0099(19) 0.0164(17) -0.0008(17) F17 0.045(3) 0.098(4) 0.068(3) -0.022(3) 0.028(2) 0.018(3) F19 0.070(3) 0.039(2) 0.049(3) -0.020(2) -0.001(2) 0.007(2) F20 0.038(2) 0.038(2) 0.059(3) -0.0155(19) 0.0097(19) -0.0024(17) Fe1 0.0280(4) 0.0359(5) 0.0291(5) -0.0075(4) 0.0118(4) -0.0101(4) Fe2 0.0346(5) 0.0264(4) 0.0243(4) 0.0002(4) 0.0133(4) -0.0016(4) P1 0.0224(7) 0.0238(7) 0.0214(7) -0.0013(6) 0.0060(6) -0.0020(6) P2 0.0219(7) 0.0195(7) 0.0229(7) 0.0013(6) 0.0082(6) 0.0000(6) Pt1 0.01995(11) 0.02153(11) 0.02126(11) 0.00060(9) 0.00649(8) -0.00105(8) Pt2 0.02151(11) 0.01931(11) 0.02162(11) -0.00050(9) 0.00482(8) 0.00185(8) Cl1 0.153(3) 0.096(2) 0.104(2) -0.0187(18) 0.073(2) -0.030(2) Cl2 0.0737(19) 0.148(3) 0.169(4) 0.076(3) 0.051(2) 0.017(2) C100 0.070(6) 0.091(8) 0.073(7) -0.005(6) 0.021(5) -0.019(6) F18 0.082(4) 0.078(3) 0.069(3) -0.037(3) 0.028(3) 0.025(3) F13 0.042(2) 0.048(2) 0.038(2) 0.0109(19) -0.0079(18) 0.0059(18) Cl3 0.0840(17) 0.0754(16) 0.0810(17) -0.0025(13) 0.0419(14) -0.0051(13) C99A 0.093(10) 0.195(17) 0.23(2) 0.121(15) 0.045(12) -0.032(11) Cl4A 0.060(4) 0.108(5) 0.086(5) 0.043(4) 0.001(3) -0.020(3) C99B 0.093(10) 0.195(17) 0.23(2) 0.121(15) 0.045(12) -0.032(11) Cl4B 0.077(3) 0.102(4) 0.099(3) 0.021(3) 0.033(3) -0.028(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.369(8) . ? C1 C2 1.394(8) . ? C1 Pt1 2.082(6) . ? C2 F1 1.354(7) . ? C2 C3 1.377(9) . ? C3 F2 1.342(7) . ? C3 C4 1.372(9) . ? C4 F3 1.348(7) . ? C4 C5 1.370(10) . ? C5 F4 1.346(7) . ? C5 C6 1.387(9) . ? C6 F5 1.356(7) . ? C7 C8 1.365(8) . ? C7 C12 1.385(8) . ? C7 Pt1 2.065(6) . ? C8 F6 1.358(7) . ? C8 C9 1.378(9) . ? C9 F7 1.341(8) . ? C9 C10 1.369(10) . ? C10 F8 1.351(7) . ? C10 C11 1.372(10) . ? C11 F9 1.345(8) . ? C11 C12 1.379(9) . ? C12 F10 1.356(7) . ? C13 C14 1.389(8) . ? C13 C18 1.396(8) . ? C13 P1 1.817(6) . ? C14 C15 1.394(9) . ? C15 C16 1.380(10) . ? C16 C17 1.377(10) . ? C17 C18 1.379(9) . ? C19 C24 1.385(9) . ? C19 C20 1.399(8) . ? C19 P1 1.825(6) . ? C20 C21 1.384(9) . ? C21 C23 1.369(10) . ? C22 C23 1.380(10) . ? C22 C24 1.382(9) . ? C25 C30 1.388(8) . ? C25 C26 1.399(8) . ? C25 P2 1.827(6) . ? C26 C27 1.385(9) . ? C27 C28 1.382(10) . ? C28 C29 1.385(10) . ? C29 C30 1.386(9) . ? C31 C36 1.389(8) . ? C31 C32 1.395(9) . ? C31 P2 1.830(6) . ? C32 C33 1.392(9) . ? C33 C34 1.382(11) . ? C34 C35 1.381(10) . ? C35 C36 1.386(9) . ? C37 C38 1.240(8) . ? C37 P1 1.776(6) . ? C37 Pt2 2.232(5) . ? C38 C53 1.421(8) . ? C38 Pt2 2.272(5) . ? C39 C44 1.368(8) . ? C39 C40 1.395(8) . ? C39 Pt2 2.033(5) . ? C40 F11 1.354(7) . ? C40 C41 1.371(8) . ? C41 F12 1.359(7) . ? C41 C42 1.359(9) . ? C42 F13 1.348(7) . ? C42 C43 1.371(9) . ? C43 F14 1.346(7) . ? C43 C44 1.385(8) . ? C44 F15 1.360(7) . ? C45 C46 1.375(8) . ? C45 C50 1.381(9) . ? C45 Pt2 2.032(6) . ? C46 F20 1.348(7) . ? C46 C47 1.377(9) . ? C47 F19 1.344(8) . ? C47 C48 1.373(11) . ? C48 F18 1.353(8) . ? C48 C49 1.372(11) . ? C49 F17 1.362(8) . ? C49 C50 1.382(9) . ? C50 F16 1.356(7) . ? C51 C52 1.218(8) . ? C51 P2 1.792(6) . ? C51 Pt2 2.179(5) . ? C52 C63 1.424(8) . ? C52 Pt2 2.399(5) . ? C53 C57 1.432(8) . ? C53 C54 1.436(8) . ? C53 Fe1 2.028(5) . ? C54 C55 1.420(9) . ? C54 Fe1 2.049(6) . ? C55 C56 1.419(10) . ? C55 Fe1 2.068(6) . ? C56 C57 1.399(9) . ? C56 Fe1 2.051(6) . ? C57 Fe1 2.028(6) . ? C58 C59 1.406(10) . ? C58 C62 1.413(10) . ? C58 Fe1 2.047(6) . ? C59 C60 1.414(11) . ? C59 Fe1 2.040(7) . ? C60 C61 1.394(11) . ? C60 Fe1 2.044(8) . ? C61 C62 1.410(12) . ? C61 Fe1 2.050(7) . ? C62 Fe1 2.041(7) . ? C63 C64 1.437(8) . ? C63 C67 1.438(8) . ? C63 Fe2 2.030(6) . ? C64 C65 1.405(9) . ? C64 Fe2 2.033(6) . ? C65 C66 1.419(10) . ? C65 Fe2 2.056(6) . ? C66 C67 1.406(9) . ? C66 Fe2 2.057(6) . ? C67 Fe2 2.039(6) . ? C68 C72 1.407(10) . ? C68 C69 1.423(10) . ? C68 Fe2 2.041(7) . ? C69 C70 1.413(10) . ? C69 Fe2 2.049(7) . ? C70 C71 1.403(9) . ? C70 Fe2 2.043(6) . ? C71 C72 1.405(10) . ? C71 Fe2 2.051(7) . ? C72 Fe2 2.049(6) . ? P1 Pt1 2.3037(14) . ? P2 Pt1 2.2869(15) . ? Cl1 C100 1.752(11) . ? Cl2 C100 1.712(10) . ? Cl3 C99A 1.682(12) . ? C99A Cl4A 1.715(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 C6 C1 C2 114.5(5) . . ? C6 C1 Pt1 127.7(5) . . ? C2 C1 Pt1 117.7(4) . . ? F1 C2 C3 116.1(5) . . ? F1 C2 C1 120.3(5) . . ? C3 C2 C1 123.6(6) . . ? F2 C3 C4 119.6(6) . . ? F2 C3 C2 121.1(6) . . ? C4 C3 C2 119.3(6) . . ? F3 C4 C5 120.2(6) . . ? F3 C4 C3 120.3(6) . . ? C5 C4 C3 119.4(6) . . ? F4 C5 C4 120.0(6) . . ? F4 C5 C6 120.6(6) . . ? C4 C5 C6 119.4(6) . . ? F5 C6 C1 120.6(6) . . ? F5 C6 C5 115.8(5) . . ? C1 C6 C5 123.6(6) . . ? C8 C7 C12 114.6(5) . . ? C8 C7 Pt1 125.2(4) . . ? C12 C7 Pt1 120.0(4) . . ? F6 C8 C7 119.3(5) . . ? F6 C8 C9 116.1(6) . . ? C7 C8 C9 124.4(6) . . ? F7 C9 C10 119.3(6) . . ? F7 C9 C8 121.8(6) . . ? C10 C9 C8 118.9(6) . . ? F8 C10 C9 120.8(7) . . ? F8 C10 C11 119.8(6) . . ? C9 C10 C11 119.3(6) . . ? F9 C11 C10 119.9(6) . . ? F9 C11 C12 120.6(7) . . ? C10 C11 C12 119.6(6) . . ? F10 C12 C11 116.8(6) . . ? F10 C12 C7 120.1(5) . . ? C11 C12 C7 123.0(6) . . ? C14 C13 C18 119.3(6) . . ? C14 C13 P1 120.9(5) . . ? C18 C13 P1 119.7(5) . . ? C13 C14 C15 120.0(6) . . ? C16 C15 C14 119.7(6) . . ? C17 C16 C15 120.4(6) . . ? C16 C17 C18 120.3(6) . . ? C17 C18 C13 120.1(6) . . ? C24 C19 C20 119.4(6) . . ? C24 C19 P1 120.1(5) . . ? C20 C19 P1 120.5(5) . . ? C21 C20 C19 119.1(6) . . ? C23 C21 C20 121.3(6) . . ? C23 C22 C24 120.0(7) . . ? C21 C23 C22 119.7(6) . . ? C22 C24 C19 120.5(6) . . ? C30 C25 C26 119.1(6) . . ? C30 C25 P2 120.8(5) . . ? C26 C25 P2 120.1(5) . . ? C27 C26 C25 120.3(6) . . ? C28 C27 C26 120.0(6) . . ? C27 C28 C29 120.1(6) . . ? C28 C29 C30 120.1(6) . . ? C29 C30 C25 120.4(6) . . ? C36 C31 C32 119.7(5) . . ? C36 C31 P2 122.7(5) . . ? C32 C31 P2 117.7(5) . . ? C33 C32 C31 119.5(6) . . ? C34 C33 C32 120.7(7) . . ? C35 C34 C33 119.5(6) . . ? C34 C35 C36 120.6(7) . . ? C35 C36 C31 120.0(6) . . ? C38 C37 P1 164.3(5) . . ? C38 C37 Pt2 75.8(4) . . ? P1 C37 Pt2 119.5(3) . . ? C37 C38 C53 164.1(6) . . ? C37 C38 Pt2 72.3(3) . . ? C53 C38 Pt2 123.1(4) . . ? C44 C39 C40 116.0(5) . . ? C44 C39 Pt2 122.4(4) . . ? C40 C39 Pt2 121.6(4) . . ? F11 C40 C41 118.0(5) . . ? F11 C40 C39 120.2(5) . . ? C41 C40 C39 121.8(6) . . ? F12 C41 C42 119.6(5) . . ? F12 C41 C40 119.8(6) . . ? C42 C41 C40 120.6(6) . . ? F13 C42 C41 120.4(6) . . ? F13 C42 C43 120.1(6) . . ? C41 C42 C43 119.4(5) . . ? F14 C43 C42 119.8(5) . . ? F14 C43 C44 120.8(6) . . ? C42 C43 C44 119.4(6) . . ? F15 C44 C39 120.3(5) . . ? F15 C44 C43 117.0(5) . . ? C39 C44 C43 122.7(6) . . ? C46 C45 C50 114.3(5) . . ? C46 C45 Pt2 125.0(5) . . ? C50 C45 Pt2 120.6(5) . . ? F20 C46 C45 119.7(5) . . ? F20 C46 C47 115.9(6) . . ? C45 C46 C47 124.4(6) . . ? F19 C47 C48 119.9(6) . . ? F19 C47 C46 121.0(7) . . ? C48 C47 C46 119.1(6) . . ? F18 C48 C49 120.5(7) . . ? F18 C48 C47 120.6(7) . . ? C49 C48 C47 118.9(6) . . ? F17 C49 C48 120.3(6) . . ? F17 C49 C50 119.7(7) . . ? C48 C49 C50 119.9(7) . . ? F16 C50 C45 120.7(5) . . ? F16 C50 C49 116.1(6) . . ? C45 C50 C49 123.2(6) . . ? C52 C51 P2 149.9(5) . . ? C52 C51 Pt2 84.8(4) . . ? P2 C51 Pt2 124.5(3) . . ? C51 C52 C63 174.6(6) . . ? C51 C52 Pt2 64.8(3) . . ? C63 C52 Pt2 120.3(4) . . ? C38 C53 C57 124.6(5) . . ? C38 C53 C54 127.7(5) . . ? C57 C53 C54 107.6(5) . . ? C38 C53 Fe1 125.0(4) . . ? C57 C53 Fe1 69.3(3) . . ? C54 C53 Fe1 70.2(3) . . ? C55 C54 C53 107.4(6) . . ? C55 C54 Fe1 70.5(4) . . ? C53 C54 Fe1 68.6(3) . . ? C56 C55 C54 108.1(6) . . ? C56 C55 Fe1 69.2(4) . . ? C54 C55 Fe1 69.1(4) . . ? C57 C56 C55 109.0(6) . . ? C57 C56 Fe1 69.0(4) . . ? C55 C56 Fe1 70.5(4) . . ? C56 C57 C53 107.9(6) . . ? C56 C57 Fe1 70.9(4) . . ? C53 C57 Fe1 69.3(3) . . ? C59 C58 C62 107.4(7) . . ? C59 C58 Fe1 69.6(4) . . ? C62 C58 Fe1 69.6(4) . . ? C58 C59 C60 108.3(7) . . ? C58 C59 Fe1 70.1(4) . . ? C60 C59 Fe1 69.9(4) . . ? C61 C60 C59 108.0(8) . . ? C61 C60 Fe1 70.3(4) . . ? C59 C60 Fe1 69.6(4) . . ? C60 C61 C62 108.2(7) . . ? C60 C61 Fe1 69.9(4) . . ? C62 C61 Fe1 69.5(4) . . ? C61 C62 C58 108.2(7) . . ? C61 C62 Fe1 70.2(4) . . ? C58 C62 Fe1 70.0(4) . . ? C52 C63 C64 126.6(5) . . ? C52 C63 C67 125.3(5) . . ? C64 C63 C67 107.6(5) . . ? C52 C63 Fe2 120.3(4) . . ? C64 C63 Fe2 69.4(3) . . ? C67 C63 Fe2 69.6(3) . . ? C65 C64 C63 107.5(6) . . ? C65 C64 Fe2 70.8(4) . . ? C63 C64 Fe2 69.2(3) . . ? C64 C65 C66 108.8(6) . . ? C64 C65 Fe2 69.1(4) . . ? C66 C65 Fe2 69.9(4) . . ? C67 C66 C65 108.6(6) . . ? C67 C66 Fe2 69.2(3) . . ? C65 C66 Fe2 69.7(4) . . ? C66 C67 C63 107.5(5) . . ? C66 C67 Fe2 70.6(4) . . ? C63 C67 Fe2 69.0(3) . . ? C72 C68 C69 107.7(7) . . ? C72 C68 Fe2 70.2(4) . . ? C69 C68 Fe2 70.0(4) . . ? C70 C69 C68 107.3(6) . . ? C70 C69 Fe2 69.5(4) . . ? C68 C69 Fe2 69.3(4) . . ? C71 C70 C69 108.5(6) . . ? C71 C70 Fe2 70.3(4) . . ? C69 C70 Fe2 70.1(4) . . ? C70 C71 C72 107.9(6) . . ? C70 C71 Fe2 69.6(4) . . ? C72 C71 Fe2 69.9(4) . . ? C71 C72 C68 108.5(6) . . ? C71 C72 Fe2 70.0(4) . . ? C68 C72 Fe2 69.6(4) . . ? C53 Fe1 C57 41.3(2) . . ? C53 Fe1 C59 108.0(3) . . ? C57 Fe1 C59 126.1(3) . . ? C53 Fe1 C62 163.2(3) . . ? C57 Fe1 C62 154.4(3) . . ? C59 Fe1 C62 67.6(3) . . ? C53 Fe1 C60 120.4(3) . . ? C57 Fe1 C60 107.5(3) . . ? C59 Fe1 C60 40.5(3) . . ? C62 Fe1 C60 67.5(3) . . ? C53 Fe1 C58 125.9(3) . . ? C57 Fe1 C58 163.4(3) . . ? C59 Fe1 C58 40.2(3) . . ? C62 Fe1 C58 40.4(3) . . ? C60 Fe1 C58 67.9(3) . . ? C53 Fe1 C54 41.3(2) . . ? C57 Fe1 C54 69.2(3) . . ? C59 Fe1 C54 120.9(3) . . ? C62 Fe1 C54 125.8(3) . . ? C60 Fe1 C54 155.9(3) . . ? C58 Fe1 C54 108.0(3) . . ? C53 Fe1 C61 154.7(3) . . ? C57 Fe1 C61 119.7(3) . . ? C59 Fe1 C61 67.5(3) . . ? C62 Fe1 C61 40.3(3) . . ? C60 Fe1 C61 39.8(3) . . ? C58 Fe1 C61 67.9(3) . . ? C54 Fe1 C61 162.8(3) . . ? C53 Fe1 C56 68.2(2) . . ? C57 Fe1 C56 40.1(3) . . ? C59 Fe1 C56 162.8(3) . . ? C62 Fe1 C56 120.8(3) . . ? C60 Fe1 C56 125.6(3) . . ? C58 Fe1 C56 155.5(3) . . ? C54 Fe1 C56 68.2(3) . . ? C61 Fe1 C56 108.3(3) . . ? C53 Fe1 C55 68.4(2) . . ? C57 Fe1 C55 68.1(3) . . ? C59 Fe1 C55 155.7(3) . . ? C62 Fe1 C55 108.5(3) . . ? C60 Fe1 C55 162.4(3) . . ? C58 Fe1 C55 121.1(3) . . ? C54 Fe1 C55 40.4(2) . . ? C61 Fe1 C55 126.2(3) . . ? C56 Fe1 C55 40.3(3) . . ? C63 Fe2 C64 41.4(2) . . ? C63 Fe2 C67 41.4(2) . . ? C64 Fe2 C67 69.5(2) . . ? C63 Fe2 C68 124.3(3) . . ? C64 Fe2 C68 107.0(3) . . ? C67 Fe2 C68 161.7(3) . . ? C63 Fe2 C70 159.1(3) . . ? C64 Fe2 C70 157.8(3) . . ? C67 Fe2 C70 122.1(3) . . ? C68 Fe2 C70 68.0(3) . . ? C63 Fe2 C69 159.7(3) . . ? C64 Fe2 C69 121.7(3) . . ? C67 Fe2 C69 156.5(3) . . ? C68 Fe2 C69 40.7(3) . . ? C70 Fe2 C69 40.4(3) . . ? C63 Fe2 C72 109.8(3) . . ? C64 Fe2 C72 123.7(3) . . ? C67 Fe2 C72 125.8(3) . . ? C68 Fe2 C72 40.2(3) . . ? C70 Fe2 C72 67.4(3) . . ? C69 Fe2 C72 67.8(3) . . ? C63 Fe2 C71 124.4(2) . . ? C64 Fe2 C71 160.1(3) . . ? C67 Fe2 C71 109.0(3) . . ? C68 Fe2 C71 67.8(3) . . ? C70 Fe2 C71 40.1(3) . . ? C69 Fe2 C71 67.8(3) . . ? C72 Fe2 C71 40.1(3) . . ? C63 Fe2 C65 68.2(2) . . ? C64 Fe2 C65 40.2(3) . . ? C67 Fe2 C65 68.2(3) . . ? C68 Fe2 C65 121.4(3) . . ? C70 Fe2 C65 122.4(3) . . ? C69 Fe2 C65 106.0(3) . . ? C72 Fe2 C65 158.1(3) . . ? C71 Fe2 C65 159.1(3) . . ? C63 Fe2 C66 68.3(3) . . ? C64 Fe2 C66 68.3(3) . . ? C67 Fe2 C66 40.2(2) . . ? C68 Fe2 C66 156.7(3) . . ? C70 Fe2 C66 107.2(3) . . ? C69 Fe2 C66 120.8(3) . . ? C72 Fe2 C66 161.0(3) . . ? C71 Fe2 C66 124.1(3) . . ? C65 Fe2 C66 40.4(3) . . ? C37 P1 C13 102.2(3) . . ? C37 P1 C19 100.5(3) . . ? C13 P1 C19 104.0(3) . . ? C37 P1 Pt1 114.35(19) . . ? C13 P1 Pt1 115.9(2) . . ? C19 P1 Pt1 117.70(19) . . ? C51 P2 C25 101.5(3) . . ? C51 P2 C31 102.5(3) . . ? C25 P2 C31 103.7(3) . . ? C51 P2 Pt1 121.03(18) . . ? C25 P2 Pt1 117.61(19) . . ? C31 P2 Pt1 108.3(2) . . ? C7 Pt1 C1 87.5(2) . . ? C7 Pt1 P2 88.76(16) . . ? C1 Pt1 P2 164.26(17) . . ? C7 Pt1 P1 172.76(17) . . ? C1 Pt1 P1 91.30(16) . . ? P2 Pt1 P1 94.21(5) . . ? C45 Pt2 C39 86.0(2) . . ? C45 Pt2 C51 164.9(2) . . ? C39 Pt2 C51 96.3(2) . . ? C45 Pt2 C37 92.1(2) . . ? C39 Pt2 C37 169.4(2) . . ? C51 Pt2 C37 82.8(2) . . ? C45 Pt2 C38 98.2(2) . . ? C39 Pt2 C38 158.6(2) . . ? C51 Pt2 C38 85.1(2) . . ? C37 Pt2 C38 32.0(2) . . ? C45 Pt2 C52 163.5(2) . . ? C39 Pt2 C52 82.8(2) . . ? C51 Pt2 C52 30.36(19) . . ? C37 Pt2 C52 101.1(2) . . ? C38 Pt2 C52 88.08(19) . . ? Cl2 C100 Cl1 113.6(6) . . ? Cl3 C99A Cl4A 122.6(8) . . ? #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 713071' _audit_creation_date 2008-02-21T16:37:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common s51 _chemical_formula_sum 'C61.50 H44 Cl3 F10 Fe2 P2 Pt' _chemical_formula_weight 1448.05 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 23.2877(6) _cell_length_b 11.0269(2) _cell_length_c 23.3719(7) _cell_angle_alpha 90 _cell_angle_beta 93.8790(10) _cell_angle_gamma 90 _cell_volume 5987.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 9296 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 25.68 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.928 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.4911 _exptl_absorpt_correction_T_max 0.8598 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0302708 _diffrn_orient_matrix_ub_12 -0.020273 _diffrn_orient_matrix_ub_13 -0.0309132 _diffrn_orient_matrix_ub_21 -0.0305661 _diffrn_orient_matrix_ub_22 0.0162472 _diffrn_orient_matrix_ub_23 0.0270702 _diffrn_orient_matrix_ub_31 -0.0013473 _diffrn_orient_matrix_ub_32 0.0868863 _diffrn_orient_matrix_ub_33 -0.0122749 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0437 _diffrn_reflns_number 5667 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5667 _reflns_number_gt 4555 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+54.6989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5667 _refine_ls_number_parameters 381 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.789 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3508(2) 0.4806(5) 0.4756(2) 0.0223(12) Uani 1 1 d . . . C2 C 0.3250(3) 0.5930(5) 0.4669(3) 0.0349(14) Uani 1 1 d . . . H2 H 0.2904 0.5993 0.4447 0.042 Uiso 1 1 calc R . . C3 C 0.3506(3) 0.6965(6) 0.4913(3) 0.0432(17) Uani 1 1 d . . . H3 H 0.3331 0.7717 0.4856 0.052 Uiso 1 1 calc R . . C4 C 0.4020(3) 0.6875(6) 0.5239(3) 0.0427(17) Uani 1 1 d . . . H4 H 0.4192 0.7568 0.5399 0.051 Uiso 1 1 calc R . . C5 C 0.4279(3) 0.5764(7) 0.5329(3) 0.0454(18) Uani 1 1 d . . . H5 H 0.4624 0.5707 0.5552 0.054 Uiso 1 1 calc R . . C6 C 0.4027(3) 0.4727(6) 0.5087(3) 0.0337(14) Uani 1 1 d . . . H6 H 0.4206 0.3978 0.5146 0.04 Uiso 1 1 calc R . . C7 C 0.3753(2) 0.2448(5) 0.4306(2) 0.0253(11) Uani 1 1 d . . . C8 C 0.3881(3) 0.1458(6) 0.4653(3) 0.0356(15) Uani 1 1 d . . . H8 H 0.3656 0.1286 0.4957 0.043 Uiso 1 1 calc R . . C9 C 0.4346(3) 0.0718(7) 0.4549(3) 0.0478(18) Uani 1 1 d . . . H9 H 0.4432 0.0055 0.4785 0.057 Uiso 1 1 calc R . . C10 C 0.4676(3) 0.0957(7) 0.4105(3) 0.0483(19) Uani 1 1 d . . . H10 H 0.4984 0.0452 0.4035 0.058 Uiso 1 1 calc R . . C11 C 0.4555(3) 0.1944(7) 0.3760(3) 0.0470(18) Uani 1 1 d . . . H11 H 0.4786 0.2109 0.346 0.056 Uiso 1 1 calc R . . C12 C 0.4091(3) 0.2705(6) 0.3851(3) 0.0345(15) Uani 1 1 d . . . H12 H 0.401 0.3368 0.3613 0.041 Uiso 1 1 calc R . . C13 C 0.2869(2) 0.3955(5) 0.3802(2) 0.0261(13) Uani 1 1 d . . . C14 C 0.2625(2) 0.4397(5) 0.3385(2) 0.0241(12) Uani 1 1 d . . . C15 C 0.2350(2) 0.4934(5) 0.2884(2) 0.0252(12) Uani 1 1 d . . . C16 C 0.1993(2) 0.4332(6) 0.2446(2) 0.0305(13) Uani 1 1 d . . . H16 H 0.1904 0.351 0.243 0.037 Uiso 1 1 calc R . . C17 C 0.1803(3) 0.5227(6) 0.2043(3) 0.0373(16) Uani 1 1 d . . . H17 H 0.1565 0.5087 0.1714 0.045 Uiso 1 1 calc R . . C18 C 0.2029(3) 0.6360(6) 0.2216(3) 0.0337(14) Uani 1 1 d . . . H18 H 0.1966 0.7091 0.2024 0.04 Uiso 1 1 calc R . . C19 C 0.2372(2) 0.6192(5) 0.2736(2) 0.0261(12) Uani 1 1 d . . . H19 H 0.2575 0.6793 0.2943 0.031 Uiso 1 1 calc R . . C20 C 0.0875(3) 0.4798(7) 0.3182(3) 0.0408(16) Uani 1 1 d . . . H20 H 0.0806 0.3967 0.3187 0.049 Uiso 1 1 calc R . . C21 C 0.1197(3) 0.5460(6) 0.3607(3) 0.0366(15) Uani 1 1 d . . . H21 H 0.138 0.5149 0.3941 0.044 Uiso 1 1 calc R . . C22 C 0.1189(3) 0.6693(6) 0.3429(3) 0.0419(17) Uani 1 1 d . . . H22 H 0.1366 0.7334 0.363 0.05 Uiso 1 1 calc R . . C23 C 0.0872(3) 0.6782(7) 0.2903(3) 0.052(2) Uani 1 1 d . . . H23 H 0.0803 0.7491 0.2693 0.062 Uiso 1 1 calc R . . C24 C 0.0673(3) 0.5614(8) 0.2744(3) 0.054(2) Uani 1 1 d . . . H24 H 0.045 0.5415 0.2412 0.065 Uiso 1 1 calc R . . C25 C 0.2247(2) 0.1401(5) 0.4312(2) 0.0215(12) Uani 1 1 d . . . C26 C 0.2439(3) 0.0230(5) 0.4248(2) 0.0302(13) Uani 1 1 d . . . C27 C 0.2253(3) -0.0533(5) 0.3810(3) 0.0365(15) Uani 1 1 d . . . C28 C 0.1855(3) -0.0110(6) 0.3390(3) 0.0385(16) Uani 1 1 d . . . C29 C 0.1650(3) 0.1051(6) 0.3428(2) 0.0321(14) Uani 1 1 d . . . C30 C 0.1844(2) 0.1760(5) 0.3884(2) 0.0268(13) Uani 1 1 d . . . F1 F 0.28295(15) -0.0244(3) 0.46475(15) 0.0347(8) Uani 1 1 d . . . F2 F 0.24588(18) -0.1669(3) 0.37798(16) 0.0484(10) Uani 1 1 d . . . F3 F 0.16749(19) -0.0830(4) 0.29481(16) 0.0542(11) Uani 1 1 d . . . F4 F 0.12632(17) 0.1469(4) 0.30205(16) 0.0506(10) Uani 1 1 d . . . F5 F 0.16004(14) 0.2883(3) 0.39119(15) 0.0337(8) Uani 1 1 d . . . Fe1 Fe 0.15435(4) 0.56400(8) 0.28304(4) 0.0278(2) Uani 1 1 d . . . P1 P 0.31596(6) 0.34345(13) 0.44642(6) 0.0212(3) Uani 1 1 d . . . Pt1 Pt 0.25 0.25 0.5 0.01900(10) Uani 1 2 d S . . Cl1 Cl 0.49015(18) 0.2424(5) 0.5911(3) 0.0898(18) Uani 0.5 1 d P . . Cl2 Cl 0.5770(3) 0.2130(6) 0.6780(2) 0.127(3) Uani 0.5 1 d PD . . C100 C 0.5548(8) 0.294(3) 0.6215(10) 0.178(17) Uani 0.5 1 d PD . . H10A H 0.5834 0.2908 0.5933 0.213 Uiso 1 1 calc R . . H10B H 0.5506 0.3781 0.6329 0.213 Uiso 1 1 calc R . . Cl3 Cl 0.5022(4) 0.5330(7) 0.6907(4) 0.143(3) Uani 0.5 1 d PD . . C200 C 0.5 0.463(3) 0.75 0.113(13) Uani 0.5 2 d SPD . . H20A H 0.4665 0.4101 0.7465 0.136 Uiso 0.5 1 calc PR . . H20B H 0.5335 0.4101 0.7535 0.136 Uiso 0.5 1 calc PR . . 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 C1 0.021(3) 0.025(3) 0.021(3) 0.000(2) 0.002(2) -0.004(2) C2 0.037(4) 0.030(3) 0.037(4) 0.001(3) 0.000(3) 0.003(3) C3 0.053(5) 0.028(3) 0.049(4) -0.006(3) 0.005(4) -0.005(3) C4 0.055(5) 0.034(4) 0.040(4) -0.011(3) 0.007(3) -0.018(3) C5 0.044(4) 0.054(4) 0.037(4) -0.008(3) -0.008(3) -0.016(3) C6 0.033(3) 0.034(3) 0.034(3) -0.004(3) 0.000(3) 0.000(3) C7 0.020(2) 0.030(3) 0.026(3) -0.008(3) -0.005(2) 0.003(3) C8 0.029(3) 0.035(3) 0.042(4) -0.003(3) 0.000(3) 0.004(3) C9 0.028(4) 0.047(4) 0.068(5) -0.005(4) -0.002(3) 0.018(3) C10 0.024(3) 0.052(4) 0.069(5) -0.020(4) -0.002(3) 0.010(3) C11 0.027(4) 0.071(5) 0.043(4) -0.024(4) 0.007(3) 0.002(3) C12 0.030(3) 0.046(4) 0.027(3) -0.007(3) 0.000(2) 0.003(3) C13 0.023(3) 0.030(3) 0.025(3) 0.000(3) 0.003(2) -0.004(2) C14 0.020(3) 0.026(3) 0.026(3) 0.000(2) 0.002(2) -0.004(2) C15 0.023(3) 0.031(3) 0.022(3) 0.000(2) 0.004(2) 0.001(2) C16 0.028(3) 0.037(3) 0.027(3) -0.006(3) 0.002(3) 0.006(3) C17 0.032(3) 0.060(4) 0.019(3) 0.003(3) -0.002(3) 0.008(3) C18 0.032(3) 0.040(4) 0.030(3) 0.012(3) 0.004(3) 0.008(3) C19 0.022(3) 0.030(3) 0.027(3) 0.004(2) 0.005(2) -0.002(2) C20 0.021(3) 0.049(4) 0.053(4) 0.003(3) 0.008(3) -0.004(3) C21 0.037(4) 0.040(4) 0.035(4) 0.008(3) 0.016(3) 0.003(3) C22 0.047(4) 0.041(4) 0.040(4) 0.003(3) 0.021(3) 0.015(3) C23 0.039(4) 0.058(5) 0.062(5) 0.026(4) 0.020(4) 0.022(4) C24 0.018(3) 0.091(6) 0.052(5) 0.016(4) -0.001(3) 0.009(4) C25 0.024(3) 0.020(3) 0.021(3) 0.000(2) 0.003(2) -0.005(2) C26 0.034(3) 0.029(3) 0.028(3) 0.002(3) 0.006(3) 0.001(3) C27 0.049(4) 0.028(3) 0.034(4) -0.005(3) 0.021(3) -0.006(3) C28 0.056(4) 0.040(4) 0.019(3) -0.003(3) 0.001(3) -0.023(3) C29 0.039(4) 0.035(3) 0.022(3) 0.008(3) -0.005(3) -0.014(3) C30 0.030(3) 0.025(3) 0.026(3) 0.003(2) 0.006(3) -0.003(2) F1 0.038(2) 0.0264(17) 0.039(2) 0.0000(15) -0.0015(16) 0.0086(15) F2 0.069(3) 0.0288(19) 0.049(2) -0.0141(17) 0.015(2) 0.0010(19) F3 0.075(3) 0.055(3) 0.031(2) -0.0136(19) 0.001(2) -0.024(2) F4 0.055(3) 0.060(3) 0.034(2) 0.0081(19) -0.0176(19) -0.017(2) F5 0.0292(19) 0.0299(17) 0.041(2) 0.0065(15) -0.0086(16) -0.0011(14) Fe1 0.0237(4) 0.0346(5) 0.0252(4) 0.0052(4) 0.0021(3) 0.0051(4) P1 0.0212(7) 0.0231(7) 0.0194(7) 0.0004(6) 0.0009(6) 0.0015(6) Pt1 0.01944(15) 0.01836(14) 0.01920(15) 0.00128(14) 0.00135(10) 0.00301(14) Cl1 0.045(2) 0.083(3) 0.138(5) 0.069(3) -0.019(3) -0.007(2) Cl2 0.158(6) 0.128(5) 0.085(4) -0.036(3) -0.068(4) 0.103(5) C100 0.049(12) 0.37(5) 0.12(2) 0.14(3) 0.010(12) -0.04(2) Cl3 0.161(7) 0.117(5) 0.155(7) 0.034(5) 0.048(6) -0.014(5) C200 0.044(16) 0.19(4) 0.10(2) 0 -0.048(16) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(8) . ? C1 C6 1.395(8) . ? C1 P1 1.826(5) . ? C2 C3 1.392(9) . ? C3 C4 1.379(10) . ? C4 C5 1.376(10) . ? C5 C6 1.388(9) . ? C7 C8 1.382(8) . ? C7 C12 1.394(8) . ? C7 P1 1.817(6) . ? C8 C9 1.390(8) . ? C9 C10 1.357(10) . ? C10 C11 1.373(11) . ? C11 C12 1.395(9) . ? C13 C14 1.199(8) . ? C13 P1 1.743(6) . ? C14 C15 1.425(8) . ? C15 C19 1.433(8) . ? C15 C16 1.437(8) . ? C15 Fe1 2.028(6) . ? C16 C17 1.414(8) . ? C16 Fe1 2.028(6) . ? C17 C18 1.406(9) . ? C17 Fe1 2.028(6) . ? C18 C19 1.419(8) . ? C18 Fe1 2.047(6) . ? C19 Fe1 2.050(6) . ? C20 C21 1.407(9) . ? C20 C24 1.418(10) . ? C20 Fe1 2.033(6) . ? C21 C22 1.422(9) . ? C21 Fe1 2.044(6) . ? C22 C23 1.393(10) . ? C22 Fe1 2.035(6) . ? C23 C24 1.410(11) . ? C23 Fe1 2.025(7) . ? C24 Fe1 2.023(7) . ? C25 C26 1.377(8) . ? C25 C30 1.383(8) . ? C25 Pt1 2.068(5) . ? C26 F1 1.362(7) . ? C26 C27 1.374(8) . ? C27 F2 1.345(7) . ? C27 C28 1.383(9) . ? C28 F3 1.347(7) . ? C28 C29 1.372(9) . ? C29 F4 1.347(7) . ? C29 C30 1.372(8) . ? C30 F5 1.365(6) . ? P1 Pt1 2.2912(14) . ? Pt1 C25 2.068(5) 7_556 ? Pt1 P1 2.2912(14) 7_556 ? Cl1 C100 1.72(2) . ? Cl2 C100 1.649(15) . ? Cl3 C200 1.591(14) . ? C200 Cl3 1.591(14) 2_656 ? 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 C2 C1 C6 119.2(5) . . ? C2 C1 P1 120.6(4) . . ? C6 C1 P1 120.1(4) . . ? C1 C2 C3 120.3(6) . . ? C4 C3 C2 120.0(6) . . ? C5 C4 C3 120.3(6) . . ? C4 C5 C6 120.2(6) . . ? C5 C6 C1 120.1(6) . . ? C8 C7 C12 119.9(5) . . ? C8 C7 P1 119.3(4) . . ? C12 C7 P1 120.7(5) . . ? C7 C8 C9 120.0(6) . . ? C10 C9 C8 120.6(7) . . ? C9 C10 C11 119.9(6) . . ? C10 C11 C12 121.2(7) . . ? C7 C12 C11 118.5(6) . . ? C14 C13 P1 171.9(5) . . ? C13 C14 C15 178.4(6) . . ? C14 C15 C19 125.4(5) . . ? C14 C15 C16 126.9(5) . . ? C19 C15 C16 107.7(5) . . ? C14 C15 Fe1 125.0(4) . . ? C19 C15 Fe1 70.2(3) . . ? C16 C15 Fe1 69.2(3) . . ? C17 C16 C15 107.0(5) . . ? C17 C16 Fe1 69.6(3) . . ? C15 C16 Fe1 69.3(3) . . ? C18 C17 C16 109.5(5) . . ? C18 C17 Fe1 70.6(4) . . ? C16 C17 Fe1 69.6(3) . . ? C17 C18 C19 108.0(5) . . ? C17 C18 Fe1 69.1(3) . . ? C19 C18 Fe1 69.8(3) . . ? C18 C19 C15 107.8(5) . . ? C18 C19 Fe1 69.6(3) . . ? C15 C19 Fe1 68.6(3) . . ? C21 C20 C24 108.3(7) . . ? C21 C20 Fe1 70.2(4) . . ? C24 C20 Fe1 69.2(4) . . ? C20 C21 C22 107.1(6) . . ? C20 C21 Fe1 69.4(4) . . ? C22 C21 Fe1 69.2(3) . . ? C23 C22 C21 108.7(7) . . ? C23 C22 Fe1 69.5(4) . . ? C21 C22 Fe1 70.0(4) . . ? C22 C23 C24 108.2(6) . . ? C22 C23 Fe1 70.3(4) . . ? C24 C23 Fe1 69.6(4) . . ? C23 C24 C20 107.7(7) . . ? C23 C24 Fe1 69.7(4) . . ? C20 C24 Fe1 69.9(4) . . ? C26 C25 C30 113.6(5) . . ? C26 C25 Pt1 123.7(4) . . ? C30 C25 Pt1 122.6(4) . . ? F1 C26 C27 116.0(5) . . ? F1 C26 C25 119.5(5) . . ? C27 C26 C25 124.4(6) . . ? F2 C27 C26 120.8(6) . . ? F2 C27 C28 120.1(6) . . ? C26 C27 C28 119.0(6) . . ? F3 C28 C29 120.6(6) . . ? F3 C28 C27 120.2(6) . . ? C29 C28 C27 119.2(6) . . ? F4 C29 C30 121.5(6) . . ? F4 C29 C28 119.5(5) . . ? C30 C29 C28 119.0(6) . . ? F5 C30 C29 116.0(5) . . ? F5 C30 C25 119.3(5) . . ? C29 C30 C25 124.7(5) . . ? C24 Fe1 C23 40.8(3) . . ? C24 Fe1 C17 105.3(3) . . ? C23 Fe1 C17 119.7(3) . . ? C24 Fe1 C16 119.3(3) . . ? C23 Fe1 C16 154.8(3) . . ? C17 Fe1 C16 40.8(2) . . ? C24 Fe1 C15 156.5(3) . . ? C23 Fe1 C15 162.0(3) . . ? C17 Fe1 C15 68.8(2) . . ? C16 Fe1 C15 41.5(2) . . ? C24 Fe1 C20 40.9(3) . . ? C23 Fe1 C20 68.5(3) . . ? C17 Fe1 C20 123.2(3) . . ? C16 Fe1 C20 106.6(3) . . ? C15 Fe1 C20 122.0(3) . . ? C24 Fe1 C22 68.1(3) . . ? C23 Fe1 C22 40.2(3) . . ? C17 Fe1 C22 155.7(3) . . ? C16 Fe1 C22 163.0(3) . . ? C15 Fe1 C22 126.4(3) . . ? C20 Fe1 C22 68.0(3) . . ? C24 Fe1 C21 68.5(3) . . ? C23 Fe1 C21 68.4(3) . . ? C17 Fe1 C21 160.6(3) . . ? C16 Fe1 C21 124.8(3) . . ? C15 Fe1 C21 109.1(2) . . ? C20 Fe1 C21 40.4(3) . . ? C22 Fe1 C21 40.8(3) . . ? C24 Fe1 C18 122.2(3) . . ? C23 Fe1 C18 106.5(3) . . ? C17 Fe1 C18 40.4(3) . . ? C16 Fe1 C18 68.8(3) . . ? C15 Fe1 C18 68.8(2) . . ? C20 Fe1 C18 159.2(3) . . ? C22 Fe1 C18 122.0(3) . . ? C21 Fe1 C18 158.4(3) . . ? C24 Fe1 C19 159.6(3) . . ? C23 Fe1 C19 124.2(3) . . ? C17 Fe1 C19 68.2(2) . . ? C16 Fe1 C19 69.3(2) . . ? C15 Fe1 C19 41.1(2) . . ? C20 Fe1 C19 158.7(2) . . ? C22 Fe1 C19 109.5(3) . . ? C21 Fe1 C19 123.7(3) . . ? C18 Fe1 C19 40.5(2) . . ? C13 P1 C7 105.7(3) . . ? C13 P1 C1 101.2(3) . . ? C7 P1 C1 104.3(3) . . ? C13 P1 Pt1 113.49(19) . . ? C7 P1 Pt1 112.9(2) . . ? C1 P1 Pt1 117.73(18) . . ? C25 Pt1 C25 180.0000(10) 7_556 . ? C25 Pt1 P1 90.24(15) 7_556 7_556 ? C25 Pt1 P1 89.76(15) . 7_556 ? C25 Pt1 P1 89.76(15) 7_556 . ? C25 Pt1 P1 90.24(15) . . ? P1 Pt1 P1 180.00(5) 7_556 . ? Cl2 C100 Cl1 111.7(13) . . ? Cl3 C200 Cl3 122(2) 2_656 . ? #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 713072' _audit_creation_date 2009-01-22T18:24:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_sum 'C40 H27 F10 Fe P Pt S' _chemical_formula_weight 1011.59 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7286(3) _cell_length_b 11.8603(5) _cell_length_c 17.0124(7) _cell_angle_alpha 78.501(2) _cell_angle_beta 81.325(2) _cell_angle_gamma 69.772(2) _cell_volume 1797.75(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 5745 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 26.02 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_special_details ; This crystal was the only adequately for its study by X-ray diffraction. Unfortunately, the poor quality of the crystal showed a low diffraction profile, especially at two theta angles. ACTA 50 instruction has been also tried, following the indications of the iUCR, obtaining the same low completeless value. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.475 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.2221 _exptl_absorpt_correction_T_max 0.4745 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0725198 _diffrn_orient_matrix_ub_12 0.0363372 _diffrn_orient_matrix_ub_13 -0.0414743 _diffrn_orient_matrix_ub_21 0.0795962 _diffrn_orient_matrix_ub_22 -0.029804 _diffrn_orient_matrix_ub_23 -0.0428859 _diffrn_orient_matrix_ub_31 -0.022397 _diffrn_orient_matrix_ub_32 -0.077937 _diffrn_orient_matrix_ub_33 0.0082238 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_number 6511 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.921 _diffrn_measured_fraction_theta_max 0.921 _reflns_number_total 6511 _reflns_number_gt 5733 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+4.7288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6511 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.101 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8712(6) 0.7581(5) 0.6197(3) 0.0320(12) Uani 1 1 d . . . C2 C 0.9038(8) 0.6378(6) 0.6131(4) 0.0437(14) Uani 1 1 d . . . C3 C 0.8379(8) 0.5994(6) 0.5613(4) 0.0458(15) Uani 1 1 d . . . C4 C 0.7357(8) 0.6848(6) 0.5134(4) 0.0495(16) Uani 1 1 d . . . C5 C 0.7009(7) 0.8047(6) 0.5187(4) 0.0481(16) Uani 1 1 d . . . C6 C 0.7673(7) 0.8399(5) 0.5713(4) 0.0402(13) Uani 1 1 d . . . C7 C 0.8366(6) 0.7706(5) 0.7883(3) 0.0321(12) Uani 1 1 d . . . C8 C 0.8666(7) 0.6651(5) 0.8426(4) 0.0377(13) Uani 1 1 d . . . C9 C 0.7738(8) 0.6468(6) 0.9099(4) 0.0465(15) Uani 1 1 d . . . C10 C 0.6432(8) 0.7362(6) 0.9240(4) 0.0462(15) Uani 1 1 d . . . C11 C 0.6083(7) 0.8421(6) 0.8708(4) 0.0460(15) Uani 1 1 d . . . C12 C 0.7020(7) 0.8589(5) 0.8054(4) 0.0409(14) Uani 1 1 d . . . C14 C 1.0005(7) 0.8787(5) 0.8852(4) 0.0385(13) Uani 1 1 d . . . C15 C 0.8891(8) 0.9844(6) 0.9021(4) 0.0506(16) Uani 1 1 d . . . H15 H 0.8643 1.0521 0.862 0.061 Uiso 1 1 calc R . . C16 C 0.8150(9) 0.9894(7) 0.9781(4) 0.061(2) Uani 1 1 d . . . H16 H 0.7428 1.061 0.9894 0.073 Uiso 1 1 calc R . . C17 C 0.8482(9) 0.8883(8) 1.0369(4) 0.0597(19) Uani 1 1 d . . . H17 H 0.7965 0.8913 1.0875 0.072 Uiso 1 1 calc R . . C18 C 0.9576(9) 0.7829(7) 1.0210(4) 0.0554(18) Uani 1 1 d . . . H18 H 0.9801 0.715 1.0611 0.066 Uiso 1 1 calc R . . C19 C 1.0343(7) 0.7777(6) 0.9455(4) 0.0459(15) Uani 1 1 d . . . H19 H 1.1085 0.7065 0.9351 0.055 Uiso 1 1 calc R . . C20 C 1.1152(7) 1.0145(5) 0.7454(3) 0.0366(13) Uani 1 1 d . . . C21 C 1.2424(7) 1.0366(6) 0.7510(4) 0.0445(15) Uani 1 1 d . . . H21 H 1.3209 0.975 0.7743 0.053 Uiso 1 1 calc R . . C22 C 1.2534(9) 1.1513(7) 0.7219(5) 0.0585(19) Uani 1 1 d . . . H22 H 1.3397 1.166 0.726 0.07 Uiso 1 1 calc R . . C23 C 1.1397(10) 1.2428(6) 0.6873(4) 0.0578(19) Uani 1 1 d . . . H23 H 1.148 1.3196 0.6686 0.069 Uiso 1 1 calc R . . C24 C 1.0134(9) 1.2209(6) 0.6803(4) 0.0546(18) Uani 1 1 d . . . H24 H 0.9356 1.2831 0.6568 0.066 Uiso 1 1 calc R . . C25 C 1.0003(7) 1.1066(5) 0.7080(4) 0.0443(15) Uani 1 1 d . . . H25 H 0.9153 1.0915 0.7017 0.053 Uiso 1 1 calc R . . C26 C 1.2632(7) 0.7667(5) 0.8001(3) 0.0384(13) Uani 1 1 d . . . C27 C 1.3753(7) 0.6818(5) 0.8093(3) 0.0356(12) Uani 1 1 d . . . C28 C 1.5050(7) 0.5796(5) 0.8221(4) 0.0374(13) Uani 1 1 d . . . C29 C 1.6296(7) 0.5424(6) 0.7662(4) 0.0486(16) Uani 1 1 d . . . H29 H 1.644 0.582 0.7143 0.058 Uiso 1 1 calc R . . C30 C 1.7278(8) 0.4335(7) 0.8047(5) 0.060(2) Uani 1 1 d . . . H30 H 1.8193 0.39 0.7821 0.072 Uiso 1 1 calc R . . C31 C 1.6652(8) 0.4017(6) 0.8821(5) 0.0567(19) Uani 1 1 d . . . H31 H 1.707 0.3335 0.9192 0.068 Uiso 1 1 calc R . . C32 C 1.5279(8) 0.4915(6) 0.8935(4) 0.0450(15) Uani 1 1 d . . . H32 H 1.4631 0.4931 0.9398 0.054 Uiso 1 1 calc R . . C33 C 1.5597(8) 0.2718(6) 0.7388(5) 0.059(2) Uani 1 1 d . . . H33 H 1.6502 0.2242 0.7177 0.071 Uiso 1 1 calc R . . C34 C 1.4931(9) 0.2486(6) 0.8172(5) 0.060(2) Uani 1 1 d . . . H34 H 1.5305 0.1824 0.8567 0.073 Uiso 1 1 calc R . . C35 C 1.3606(8) 0.3434(6) 0.8245(5) 0.0519(17) Uani 1 1 d . . . H35 H 1.2949 0.3518 0.8704 0.062 Uiso 1 1 calc R . . C36 C 1.3424(8) 0.4241(6) 0.7514(4) 0.0502(16) Uani 1 1 d . . . H36 H 1.2627 0.4944 0.7407 0.06 Uiso 1 1 calc R . . C37 C 1.4644(8) 0.3808(6) 0.6973(4) 0.0515(17) Uani 1 1 d . . . H37 H 1.4804 0.4164 0.6444 0.062 Uiso 1 1 calc R . . C38 C 1.1429(11) 0.8010(9) 0.5000(6) 0.0785(13) Uani 1 1 d . . . H38A H 1.0557 0.7811 0.4961 0.094 Uiso 1 1 calc R . . H38B H 1.1673 0.8475 0.4495 0.094 Uiso 1 1 calc R . . C39 C 1.2841(11) 0.6764(9) 0.5271(6) 0.0785(13) Uani 1 1 d . . . H39A H 1.2498 0.6074 0.5473 0.094 Uiso 1 1 calc R . . H39B H 1.3556 0.6574 0.4813 0.094 Uiso 1 1 calc R . . C40 C 1.3518(11) 0.7027(9) 0.5914(6) 0.0785(13) Uani 1 1 d . . . H40A H 1.3252 0.6594 0.6428 0.094 Uiso 1 1 calc R . . H40B H 1.4579 0.6721 0.5811 0.094 Uiso 1 1 calc R . . C41 C 1.3087(10) 0.8263(9) 0.5966(6) 0.0785(13) Uani 1 1 d . . . H41A H 1.3619 0.8678 0.5548 0.094 Uiso 1 1 calc R . . H41B H 1.3255 0.8381 0.6487 0.094 Uiso 1 1 calc R . . F1 F 1.0043(5) 0.5495(3) 0.6574(3) 0.0645(12) Uani 1 1 d . . . F2 F 0.8739(6) 0.4810(4) 0.5566(3) 0.0712(13) Uani 1 1 d . . . F3 F 0.6729(5) 0.6486(4) 0.4628(3) 0.0696(12) Uani 1 1 d . . . F4 F 0.6028(5) 0.8890(4) 0.4712(3) 0.0710(13) Uani 1 1 d . . . F5 F 0.7289(5) 0.9606(3) 0.5735(2) 0.0548(10) Uani 1 1 d . . . F6 F 0.9966(4) 0.5751(3) 0.8328(2) 0.0579(10) Uani 1 1 d . . . F7 F 0.8134(5) 0.5416(4) 0.9629(2) 0.0658(12) Uani 1 1 d . . . F8 F 0.5521(5) 0.7204(4) 0.9894(2) 0.0660(12) Uani 1 1 d . . . F9 F 0.4818(4) 0.9325(4) 0.8874(3) 0.0696(13) Uani 1 1 d . . . F10 F 0.6623(4) 0.9680(3) 0.7566(2) 0.0588(11) Uani 1 1 d . . . Fe1 Fe 1.52980(10) 0.41231(8) 0.79765(6) 0.0411(2) Uani 1 1 d . . . P1 P 1.08824(17) 0.86863(13) 0.78274(9) 0.0330(3) Uani 1 1 d . . . Pt1 Pt 0.97797(2) 0.811647(19) 0.694966(13) 0.03362(9) Uani 1 1 d . . . S1 S 1.1208(2) 0.87937(17) 0.58336(10) 0.0522(4) 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 C1 0.035(3) 0.032(3) 0.031(3) -0.008(2) 0.007(2) -0.016(2) C2 0.053(4) 0.040(3) 0.036(3) 0.000(3) -0.008(3) -0.014(3) C3 0.065(5) 0.043(3) 0.038(3) -0.007(3) -0.002(3) -0.029(3) C4 0.055(4) 0.059(4) 0.044(4) -0.012(3) 0.000(3) -0.031(3) C5 0.041(4) 0.060(4) 0.040(3) 0.000(3) -0.013(3) -0.012(3) C6 0.039(3) 0.042(3) 0.039(3) -0.006(3) -0.004(3) -0.012(3) C7 0.029(3) 0.034(3) 0.035(3) -0.010(2) -0.004(2) -0.008(2) C8 0.034(3) 0.036(3) 0.044(3) -0.003(2) -0.010(3) -0.012(2) C9 0.060(4) 0.049(4) 0.036(3) 0.004(3) -0.011(3) -0.027(3) C10 0.049(4) 0.063(4) 0.034(3) -0.008(3) 0.001(3) -0.028(3) C11 0.033(3) 0.060(4) 0.041(3) -0.013(3) 0.000(3) -0.010(3) C12 0.041(4) 0.037(3) 0.039(3) -0.003(2) -0.006(3) -0.007(3) C14 0.039(3) 0.043(3) 0.035(3) -0.011(2) 0.000(2) -0.015(3) C15 0.054(4) 0.049(4) 0.044(4) -0.013(3) 0.004(3) -0.011(3) C16 0.061(5) 0.070(5) 0.052(4) -0.026(4) 0.013(4) -0.021(4) C17 0.063(5) 0.083(5) 0.042(4) -0.019(4) 0.007(3) -0.034(4) C18 0.065(5) 0.073(5) 0.032(3) -0.001(3) -0.007(3) -0.030(4) C19 0.044(4) 0.049(4) 0.042(3) -0.004(3) -0.008(3) -0.014(3) C20 0.037(3) 0.035(3) 0.038(3) -0.007(2) -0.004(2) -0.011(2) C21 0.046(4) 0.046(3) 0.044(3) -0.009(3) -0.010(3) -0.016(3) C22 0.068(5) 0.063(5) 0.058(4) -0.014(4) -0.001(4) -0.037(4) C23 0.087(6) 0.039(4) 0.052(4) -0.006(3) 0.004(4) -0.031(4) C24 0.073(5) 0.031(3) 0.049(4) 0.001(3) -0.008(3) -0.006(3) C25 0.045(4) 0.038(3) 0.047(4) -0.007(3) -0.007(3) -0.009(3) C26 0.041(3) 0.040(3) 0.033(3) -0.004(2) -0.004(2) -0.012(3) C27 0.038(3) 0.033(3) 0.036(3) -0.003(2) -0.007(2) -0.011(3) C28 0.038(3) 0.040(3) 0.038(3) -0.012(2) -0.006(3) -0.013(3) C29 0.038(4) 0.064(4) 0.052(4) -0.016(3) -0.003(3) -0.023(3) C30 0.028(4) 0.063(5) 0.091(6) -0.031(4) -0.015(4) -0.003(3) C31 0.046(4) 0.050(4) 0.074(5) -0.008(4) -0.032(4) -0.005(3) C32 0.047(4) 0.041(3) 0.044(3) -0.007(3) -0.013(3) -0.008(3) C33 0.047(4) 0.045(4) 0.086(6) -0.029(4) -0.021(4) 0.001(3) C34 0.076(5) 0.041(4) 0.072(5) -0.003(3) -0.030(4) -0.022(4) C35 0.042(4) 0.058(4) 0.066(5) -0.018(3) -0.007(3) -0.023(3) C36 0.046(4) 0.047(4) 0.062(4) -0.016(3) -0.015(3) -0.013(3) C37 0.051(4) 0.057(4) 0.053(4) -0.021(3) -0.015(3) -0.014(3) C38 0.082(3) 0.091(3) 0.072(3) -0.027(2) 0.004(2) -0.037(3) C39 0.082(3) 0.091(3) 0.072(3) -0.027(2) 0.004(2) -0.037(3) C40 0.082(3) 0.091(3) 0.072(3) -0.027(2) 0.004(2) -0.037(3) C41 0.082(3) 0.091(3) 0.072(3) -0.027(2) 0.004(2) -0.037(3) F1 0.095(3) 0.037(2) 0.060(3) -0.0016(18) -0.033(2) -0.012(2) F2 0.119(4) 0.048(2) 0.063(3) -0.0095(19) -0.016(3) -0.044(2) F3 0.084(3) 0.095(3) 0.054(3) -0.021(2) -0.012(2) -0.053(3) F4 0.063(3) 0.078(3) 0.067(3) -0.015(2) -0.032(2) -0.004(2) F5 0.060(3) 0.040(2) 0.058(2) -0.0068(17) -0.0167(19) -0.0044(18) F6 0.054(2) 0.041(2) 0.062(3) 0.0030(18) -0.0089(19) 0.0005(18) F7 0.089(3) 0.060(2) 0.049(2) 0.0158(19) -0.011(2) -0.037(2) F8 0.066(3) 0.089(3) 0.043(2) -0.001(2) 0.011(2) -0.037(2) F9 0.046(2) 0.083(3) 0.057(3) -0.014(2) 0.0089(19) 0.004(2) F10 0.058(3) 0.041(2) 0.053(2) 0.0039(17) -0.0010(19) 0.0056(18) Fe1 0.0341(5) 0.0392(5) 0.0494(5) -0.0118(4) -0.0107(4) -0.0055(4) P1 0.0333(8) 0.0323(7) 0.0329(7) -0.0056(6) -0.0028(6) -0.0100(6) Pt1 0.03343(14) 0.03384(13) 0.03387(13) -0.00520(9) -0.00297(9) -0.01145(9) S1 0.0636(12) 0.0635(11) 0.0401(9) -0.0127(8) 0.0081(8) -0.0366(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.374(8) . ? C1 C6 1.377(8) . ? C1 Pt1 2.075(6) . ? C2 F1 1.348(7) . ? C2 C3 1.389(9) . ? C3 F2 1.341(7) . ? C3 C4 1.378(10) . ? C4 F3 1.337(7) . ? C4 C5 1.362(9) . ? C5 F4 1.347(7) . ? C5 C6 1.379(9) . ? C6 F5 1.356(7) . ? C7 C8 1.368(8) . ? C7 C12 1.398(8) . ? C7 Pt1 2.036(5) . ? C8 F6 1.357(7) . ? C8 C9 1.377(9) . ? C9 F7 1.357(7) . ? C9 C10 1.369(10) . ? C10 F8 1.338(7) . ? C10 C11 1.363(9) . ? C11 C12 1.356(9) . ? C11 F9 1.359(7) . ? C12 F10 1.355(7) . ? C14 C19 1.391(9) . ? C14 C15 1.392(9) . ? C14 P1 1.829(6) . ? C15 C16 1.384(9) . ? C16 C17 1.376(11) . ? C17 C18 1.377(11) . ? C18 C19 1.386(9) . ? C20 C21 1.370(9) . ? C20 C25 1.393(9) . ? C20 P1 1.815(6) . ? C21 C22 1.387(9) . ? C22 C23 1.364(11) . ? C23 C24 1.367(11) . ? C24 C25 1.386(9) . ? C26 C27 1.207(8) . ? C26 P1 1.742(6) . ? C27 C28 1.424(8) . ? C28 C29 1.420(9) . ? C28 C32 1.426(9) . ? C28 Fe1 2.034(6) . ? C29 C30 1.416(10) . ? C29 Fe1 2.039(7) . ? C30 C31 1.402(11) . ? C30 Fe1 2.050(7) . ? C31 C32 1.406(10) . ? C31 Fe1 2.049(7) . ? C32 Fe1 2.032(6) . ? C33 C34 1.412(11) . ? C33 C37 1.425(10) . ? C33 Fe1 2.027(7) . ? C34 C35 1.395(10) . ? C34 Fe1 2.048(7) . ? C35 C36 1.402(10) . ? C35 Fe1 2.035(7) . ? C36 C37 1.398(10) . ? C36 Fe1 2.044(7) . ? C37 Fe1 2.050(6) . ? C38 C39 1.673(13) . ? C38 S1 1.794(9) . ? C39 C40 1.490(12) . ? C40 C41 1.396(12) . ? C41 S1 1.749(10) . ? P1 Pt1 2.2856(15) . ? Pt1 S1 2.3558(16) . ? 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 C2 C1 C6 115.6(5) . . ? C2 C1 Pt1 121.7(5) . . ? C6 C1 Pt1 122.7(4) . . ? F1 C2 C1 120.9(6) . . ? F1 C2 C3 116.1(5) . . ? C1 C2 C3 123.0(6) . . ? F2 C3 C4 119.8(6) . . ? F2 C3 C2 120.9(6) . . ? C4 C3 C2 119.2(6) . . ? F3 C4 C5 121.4(7) . . ? F3 C4 C3 119.6(6) . . ? C5 C4 C3 119.0(6) . . ? F4 C5 C4 119.5(6) . . ? F4 C5 C6 120.2(6) . . ? C4 C5 C6 120.4(6) . . ? F5 C6 C1 119.6(5) . . ? F5 C6 C5 117.6(5) . . ? C1 C6 C5 122.7(6) . . ? C8 C7 C12 114.8(5) . . ? C8 C7 Pt1 125.4(4) . . ? C12 C7 Pt1 119.6(4) . . ? F6 C8 C7 119.4(5) . . ? F6 C8 C9 117.3(5) . . ? C7 C8 C9 123.3(6) . . ? F7 C9 C10 120.2(6) . . ? F7 C9 C8 120.0(6) . . ? C10 C9 C8 119.7(6) . . ? F8 C10 C11 120.6(6) . . ? F8 C10 C9 120.6(6) . . ? C11 C10 C9 118.8(6) . . ? C12 C11 F9 121.1(6) . . ? C12 C11 C10 120.5(6) . . ? F9 C11 C10 118.3(6) . . ? F10 C12 C11 117.3(6) . . ? F10 C12 C7 119.8(5) . . ? C11 C12 C7 122.9(6) . . ? C19 C14 C15 119.0(6) . . ? C19 C14 P1 120.5(5) . . ? C15 C14 P1 120.2(5) . . ? C16 C15 C14 120.4(7) . . ? C17 C16 C15 120.0(7) . . ? C16 C17 C18 120.3(7) . . ? C17 C18 C19 120.1(7) . . ? C18 C19 C14 120.1(6) . . ? C21 C20 C25 119.5(6) . . ? C21 C20 P1 123.3(5) . . ? C25 C20 P1 117.2(5) . . ? C20 C21 C22 119.7(7) . . ? C23 C22 C21 121.1(7) . . ? C22 C23 C24 119.5(6) . . ? C23 C24 C25 120.5(7) . . ? C24 C25 C20 119.6(7) . . ? C27 C26 P1 168.9(6) . . ? C26 C27 C28 178.2(7) . . ? C29 C28 C27 127.4(6) . . ? C29 C28 C32 107.6(6) . . ? C27 C28 C32 124.9(6) . . ? C29 C28 Fe1 69.8(4) . . ? C27 C28 Fe1 123.4(4) . . ? C32 C28 Fe1 69.4(3) . . ? C30 C29 C28 107.0(6) . . ? C30 C29 Fe1 70.2(4) . . ? C28 C29 Fe1 69.4(4) . . ? C31 C30 C29 109.3(6) . . ? C31 C30 Fe1 69.9(4) . . ? C29 C30 Fe1 69.3(4) . . ? C30 C31 C32 107.7(6) . . ? C30 C31 Fe1 70.1(4) . . ? C32 C31 Fe1 69.2(4) . . ? C31 C32 C28 108.3(6) . . ? C31 C32 Fe1 70.5(4) . . ? C28 C32 Fe1 69.5(3) . . ? C34 C33 C37 108.3(7) . . ? C34 C33 Fe1 70.6(4) . . ? C37 C33 Fe1 70.4(4) . . ? C35 C34 C33 107.1(7) . . ? C35 C34 Fe1 69.5(4) . . ? C33 C34 Fe1 68.9(4) . . ? C34 C35 C36 109.1(7) . . ? C34 C35 Fe1 70.6(4) . . ? C36 C35 Fe1 70.2(4) . . ? C37 C36 C35 108.4(6) . . ? C37 C36 Fe1 70.3(4) . . ? C35 C36 Fe1 69.5(4) . . ? C36 C37 C33 107.0(7) . . ? C36 C37 Fe1 69.8(4) . . ? C33 C37 Fe1 68.7(4) . . ? C39 C38 S1 99.9(6) . . ? C40 C39 C38 107.2(7) . . ? C41 C40 C39 113.6(9) . . ? C40 C41 S1 103.9(7) . . ? C33 Fe1 C32 155.7(3) . . ? C33 Fe1 C28 162.6(3) . . ? C32 Fe1 C28 41.1(2) . . ? C33 Fe1 C35 67.6(3) . . ? C32 Fe1 C35 105.5(3) . . ? C28 Fe1 C35 120.5(3) . . ? C33 Fe1 C29 126.5(3) . . ? C32 Fe1 C29 68.7(3) . . ? C28 Fe1 C29 40.8(2) . . ? C35 Fe1 C29 157.3(3) . . ? C33 Fe1 C36 67.8(3) . . ? C32 Fe1 C36 123.0(3) . . ? C28 Fe1 C36 107.6(3) . . ? C35 Fe1 C36 40.2(3) . . ? C29 Fe1 C36 123.2(3) . . ? C33 Fe1 C34 40.5(3) . . ? C32 Fe1 C34 119.3(3) . . ? C28 Fe1 C34 155.0(3) . . ? C35 Fe1 C34 40.0(3) . . ? C29 Fe1 C34 162.2(3) . . ? C36 Fe1 C34 67.7(3) . . ? C33 Fe1 C31 122.1(3) . . ? C32 Fe1 C31 40.3(3) . . ? C28 Fe1 C31 68.4(3) . . ? C35 Fe1 C31 122.2(3) . . ? C29 Fe1 C31 68.4(3) . . ? C36 Fe1 C31 158.6(3) . . ? C34 Fe1 C31 106.5(3) . . ? C33 Fe1 C37 40.9(3) . . ? C32 Fe1 C37 160.1(3) . . ? C28 Fe1 C37 124.9(3) . . ? C35 Fe1 C37 67.6(3) . . ? C29 Fe1 C37 110.0(3) . . ? C36 Fe1 C37 40.0(3) . . ? C34 Fe1 C37 68.3(3) . . ? C31 Fe1 C37 159.2(3) . . ? C33 Fe1 C30 110.3(3) . . ? C32 Fe1 C30 67.5(3) . . ? C28 Fe1 C30 67.9(3) . . ? C35 Fe1 C30 159.3(3) . . ? C29 Fe1 C30 40.5(3) . . ? C36 Fe1 C30 159.9(3) . . ? C34 Fe1 C30 124.9(3) . . ? C31 Fe1 C30 40.0(3) . . ? C37 Fe1 C30 125.3(3) . . ? C26 P1 C20 105.0(3) . . ? C26 P1 C14 101.9(3) . . ? C20 P1 C14 105.5(3) . . ? C26 P1 Pt1 112.3(2) . . ? C20 P1 Pt1 112.6(2) . . ? C14 P1 Pt1 118.2(2) . . ? C7 Pt1 C1 88.3(2) . . ? C7 Pt1 P1 89.02(16) . . ? C1 Pt1 P1 177.35(14) . . ? C7 Pt1 S1 173.72(16) . . ? C1 Pt1 S1 90.62(15) . . ? P1 Pt1 S1 92.02(6) . . ? C41 S1 C38 94.1(4) . . ? C41 S1 Pt1 113.0(3) . . ? C38 S1 Pt1 112.6(3) . . ? #===END data_complex10c _database_code_depnum_ccdc_archive 'CCDC 713073' _audit_creation_date 2009-01-27T17:11:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C72 H56 F10 Fe2 P2 Pt2' _chemical_formula_weight 1674.99 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 14.0670(2) _cell_length_b 29.7506(5) _cell_length_c 15.0209(3) _cell_angle_alpha 90 _cell_angle_beta 93.731(2) _cell_angle_gamma 90 _cell_volume 6272.95(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(10) _cell_measurement_reflns_used 10954 _cell_measurement_theta_min 2.7128 _cell_measurement_theta_max 27.5504 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET) (compiled Feb 28 2008,12:10:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.9335 _exptl_absorpt_correction_T_max 1.0583 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.399 _diffrn_orient_matrix_ub_11 0.0195187809 _diffrn_orient_matrix_ub_12 -0.016622172 _diffrn_orient_matrix_ub_13 -0.0271483126 _diffrn_orient_matrix_ub_21 -0.0435905254 _diffrn_orient_matrix_ub_22 -0.0010971507 _diffrn_orient_matrix_ub_23 -0.0263247737 _diffrn_orient_matrix_ub_31 0.0162764601 _diffrn_orient_matrix_ub_32 0.0169874079 _diffrn_orient_matrix_ub_33 -0.028282945 _diffrn_measurement_device '90-92 mm CCD Sapphire on k-goniometer' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_unetI/netI 0.1341 _diffrn_reflns_number 52667 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 12354 _reflns_number_gt 7348 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET) (compiled Feb 28 2008,12:10:31) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET) (compiled Feb 28 2008,12:10:31) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET) (compiled Feb 28 2008,12:10:31) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12354 _refine_ls_number_parameters 763 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.042 _refine_ls_goodness_of_fit_ref 0.739 _refine_ls_restrained_S_all 0.739 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.373 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.147 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' 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 C1 C 0.1895(4) -0.00935(18) 0.1595(3) 0.0175(14) Uani 1 1 d . . . C2 C 0.1349(4) -0.0397(2) 0.1449(3) 0.0219(15) Uani 1 1 d . . . C3 C 0.0686(4) -0.07669(19) 0.1212(4) 0.0224(15) Uani 1 1 d . . . C4 C 0.0222(4) -0.0931(2) 0.2031(4) 0.056(2) Uani 1 1 d . . . H4A H -0.021 -0.1171 0.1868 0.084 Uiso 1 1 calc R . . H4B H -0.0123 -0.0688 0.2282 0.084 Uiso 1 1 calc R . . H4C H 0.0703 -0.1037 0.2462 0.084 Uiso 1 1 calc R . . C5 C 0.1251(4) -0.11460(18) 0.0826(4) 0.0414(18) Uani 1 1 d . . . H5A H 0.0832 -0.1392 0.0666 0.062 Uiso 1 1 calc R . . H5B H 0.1735 -0.1245 0.1262 0.062 Uiso 1 1 calc R . . H5C H 0.1544 -0.1041 0.0305 0.062 Uiso 1 1 calc R . . C6 C -0.0064(4) -0.0602(2) 0.0521(4) 0.056(2) Uani 1 1 d . . . H6A H -0.0501 -0.0841 0.0364 0.084 Uiso 1 1 calc R . . H6B H 0.0237 -0.0504 -0.0001 0.084 Uiso 1 1 calc R . . H6C H -0.0405 -0.0355 0.0762 0.084 Uiso 1 1 calc R . . C7 C 0.1655(4) 0.00569(19) 0.3825(3) 0.0156(13) Uani 1 1 d . . . C8 C 0.2039(4) -0.0265(2) 0.4126(4) 0.0229(15) Uani 1 1 d . . . C9 C 0.2558(4) -0.06554(19) 0.4527(4) 0.0257(15) Uani 1 1 d . . . C10 C 0.2438(4) -0.10576(19) 0.3886(4) 0.0410(18) Uani 1 1 d . . . H10A H 0.2776 -0.1312 0.414 0.061 Uiso 1 1 calc R . . H10B H 0.269 -0.0982 0.3326 0.061 Uiso 1 1 calc R . . H10C H 0.1774 -0.113 0.3791 0.061 Uiso 1 1 calc R . . C11 C 0.2163(4) -0.0772(2) 0.5405(4) 0.047(2) Uani 1 1 d . . . H11A H 0.2502 -0.1025 0.5663 0.07 Uiso 1 1 calc R . . H11B H 0.15 -0.0846 0.531 0.07 Uiso 1 1 calc R . . H11C H 0.2235 -0.052 0.5802 0.07 Uiso 1 1 calc R . . C12 C 0.3606(4) -0.0518(2) 0.4672(4) 0.0379(18) Uani 1 1 d . . . H12A H 0.3967 -0.0765 0.4931 0.057 Uiso 1 1 calc R . . H12B H 0.3659 -0.0264 0.5067 0.057 Uiso 1 1 calc R . . H12C H 0.3848 -0.0439 0.411 0.057 Uiso 1 1 calc R . . C13 C 0.2942(4) 0.04819(18) 0.0607(3) 0.0188(14) Uani 1 1 d . . . C14 C 0.3547(4) 0.02092(19) 0.0143(3) 0.0250(15) Uani 1 1 d . . . H14 H 0.3846 -0.0036 0.0425 0.03 Uiso 1 1 calc R . . C15 C 0.3700(4) 0.0303(2) -0.0731(4) 0.0334(17) Uani 1 1 d . . . H15 H 0.4095 0.0119 -0.1045 0.04 Uiso 1 1 calc R . . C16 C 0.3268(4) 0.06724(19) -0.1146(3) 0.0268(16) Uani 1 1 d . . . H16 H 0.3388 0.074 -0.1732 0.032 Uiso 1 1 calc R . . C17 C 0.2664(4) 0.0938(2) -0.0698(3) 0.0247(14) Uani 1 1 d . . . H17 H 0.2362 0.1182 -0.0982 0.03 Uiso 1 1 calc R . . C18 C 0.2509(4) 0.08409(18) 0.0176(3) 0.0226(15) Uani 1 1 d . . . H18 H 0.2102 0.1023 0.0482 0.027 Uiso 1 1 calc R . . C19 C 0.3760(4) 0.01057(17) 0.2246(3) 0.0134(13) Uani 1 1 d . . . C20 C 0.3972(4) -0.03467(18) 0.2202(3) 0.0209(14) Uani 1 1 d . . . H20 H 0.3538 -0.054 0.1908 0.025 Uiso 1 1 calc R . . C21 C 0.4812(4) -0.0518(2) 0.2583(4) 0.0260(15) Uani 1 1 d . . . H21 H 0.4939 -0.0825 0.2555 0.031 Uiso 1 1 calc R . . C22 C 0.5458(4) -0.0232(2) 0.3006(4) 0.0278(16) Uani 1 1 d . . . H22 H 0.6027 -0.0347 0.3261 0.033 Uiso 1 1 calc R . . C23 C 0.5286(4) 0.0212(2) 0.3058(3) 0.0292(16) Uani 1 1 d . . . H23 H 0.5733 0.0402 0.3346 0.035 Uiso 1 1 calc R . . C24 C 0.4436(4) 0.0385(2) 0.2679(3) 0.0258(15) Uani 1 1 d . . . H24 H 0.4317 0.0691 0.2716 0.031 Uiso 1 1 calc R . . C25 C 0.0101(4) 0.04910(19) 0.2872(3) 0.0207(14) Uani 1 1 d . . . C26 C -0.0503(4) 0.0150(2) 0.3110(4) 0.0316(16) Uani 1 1 d . . . H26 H -0.0309 -0.005 0.3561 0.038 Uiso 1 1 calc R . . C27 C -0.1396(4) 0.0109(2) 0.2671(4) 0.0414(18) Uani 1 1 d . . . H27 H -0.179 -0.0126 0.2825 0.05 Uiso 1 1 calc R . . C28 C -0.1714(5) 0.0402(2) 0.2023(4) 0.0407(18) Uani 1 1 d . . . H28 H -0.2322 0.0373 0.1747 0.049 Uiso 1 1 calc R . . C29 C -0.1124(4) 0.0736(2) 0.1789(4) 0.0389(18) Uani 1 1 d . . . H29 H -0.133 0.0938 0.1344 0.047 Uiso 1 1 calc R . . C30 C -0.0231(4) 0.0781(2) 0.2198(4) 0.0327(17) Uani 1 1 d . . . H30 H 0.0162 0.1011 0.202 0.039 Uiso 1 1 calc R . . C31 C 0.1015(4) 0.08783(17) 0.4452(3) 0.0155(13) Uani 1 1 d . . . C32 C 0.1449(4) 0.07597(19) 0.5276(4) 0.0314(16) Uani 1 1 d . . . H32 H 0.1854 0.0513 0.5323 0.038 Uiso 1 1 calc R . . C33 C 0.1278(5) 0.1009(2) 0.6025(4) 0.0364(18) Uani 1 1 d . . . H33 H 0.1581 0.093 0.6572 0.044 Uiso 1 1 calc R . . C34 C 0.0678(4) 0.1365(2) 0.5976(4) 0.0352(18) Uani 1 1 d . . . H34 H 0.0559 0.1526 0.6488 0.042 Uiso 1 1 calc R . . C35 C 0.0246(4) 0.1487(2) 0.5168(4) 0.0304(17) Uani 1 1 d . . . H35 H -0.016 0.1734 0.5129 0.036 Uiso 1 1 calc R . . C36 C 0.0410(4) 0.12441(19) 0.4410(4) 0.0257(15) Uani 1 1 d . . . H36 H 0.0111 0.1328 0.3865 0.031 Uiso 1 1 calc R . . C37 C 0.3108(4) 0.13609(18) 0.1935(3) 0.0177(14) Uani 1 1 d . . . C38 C 0.3651(4) 0.16532(18) 0.1693(3) 0.0177(14) Uani 1 1 d . . . C39 C 0.4420(4) 0.19245(18) 0.1356(3) 0.0173(13) Uani 1 1 d . . . C40 C 0.2173(4) 0.15297(18) 0.3248(3) 0.0156(14) Uani 1 1 d . . . C41 C 0.2479(3) 0.18678(18) 0.3625(3) 0.0133(13) Uani 1 1 d . . . C42 C 0.2861(4) 0.21708(16) 0.4312(3) 0.0127(13) Uani 1 1 d . . . C43 C 0.4630(4) 0.19854(19) 0.0461(3) 0.0208(14) Uani 1 1 d . . . H43 H 0.4313 0.1852 -0.0034 0.025 Uiso 1 1 calc R . . C44 C 0.5391(4) 0.22795(18) 0.0446(4) 0.0211(14) Uani 1 1 d . . . H44 H 0.567 0.2378 -0.0064 0.025 Uiso 1 1 calc R . . C45 C 0.5673(4) 0.24036(19) 0.1317(3) 0.0233(15) Uani 1 1 d . . . H45 H 0.6166 0.2599 0.1491 0.028 Uiso 1 1 calc R . . C46 C 0.5074(4) 0.21785(17) 0.1888(3) 0.0160(13) Uani 1 1 d . . . H46 H 0.5107 0.2196 0.2507 0.019 Uiso 1 1 calc R . . C47 C 0.3598(4) 0.24893(17) 0.4258(3) 0.0181(14) Uani 1 1 d . . . H47 H 0.3868 0.2581 0.3739 0.022 Uiso 1 1 calc R . . C48 C 0.3854(4) 0.26458(18) 0.5129(4) 0.0226(15) Uani 1 1 d . . . H48 H 0.4325 0.2856 0.5283 0.027 Uiso 1 1 calc R . . C49 C 0.3276(4) 0.24284(19) 0.5720(4) 0.0253(15) Uani 1 1 d . . . H49 H 0.3291 0.2472 0.6333 0.03 Uiso 1 1 calc R . . C50 C 0.2670(4) 0.21326(18) 0.5224(3) 0.0210(14) Uani 1 1 d . . . H50 H 0.222 0.1944 0.5454 0.025 Uiso 1 1 calc R . . C51 C 0.5878(4) 0.1055(2) 0.1298(4) 0.0344(17) Uani 1 1 d . . . H51 H 0.5378 0.0856 0.1364 0.041 Uiso 1 1 calc R . . C52 C 0.6237(5) 0.1190(2) 0.0490(4) 0.0416(19) Uani 1 1 d . . . H52 H 0.6015 0.1098 -0.0078 0.05 Uiso 1 1 calc R . . C53 C 0.6981(5) 0.1486(2) 0.0690(5) 0.045(2) Uani 1 1 d . . . H53 H 0.735 0.1626 0.0279 0.055 Uiso 1 1 calc R . . C54 C 0.7079(4) 0.1539(2) 0.1607(5) 0.0431(19) Uani 1 1 d . . . H54 H 0.752 0.1723 0.1919 0.052 Uiso 1 1 calc R . . C55 C 0.6405(5) 0.1271(2) 0.1977(4) 0.0385(18) Uani 1 1 d . . . H55 H 0.632 0.1242 0.2583 0.046 Uiso 1 1 calc R . . C56 C 0.4521(4) 0.1417(2) 0.4411(4) 0.0353(18) Uani 1 1 d . . . H56 H 0.4323 0.1323 0.3838 0.042 Uiso 1 1 calc R . . C57 C 0.5276(4) 0.1709(2) 0.4644(5) 0.0359(17) Uani 1 1 d . . . H57 H 0.5677 0.1842 0.4253 0.043 Uiso 1 1 calc R . . C58 C 0.5318(5) 0.1765(2) 0.5545(5) 0.044(2) Uani 1 1 d . . . H58 H 0.5747 0.1949 0.5871 0.053 Uiso 1 1 calc R . . C59 C 0.4627(5) 0.1506(2) 0.5897(4) 0.0420(19) Uani 1 1 d . . . H59 H 0.4515 0.1479 0.6498 0.05 Uiso 1 1 calc R . . C60 C 0.4127(4) 0.12939(19) 0.5190(4) 0.0356(17) Uani 1 1 d . . . H60 H 0.3612 0.1101 0.5235 0.043 Uiso 1 1 calc R . . C61 C 0.2193(4) 0.22479(18) 0.0892(3) 0.0171(14) Uani 1 1 d . . . C62 C 0.1580(4) 0.20566(19) 0.0247(4) 0.0178(13) Uani 1 1 d . . . C63 C 0.1488(4) 0.21686(19) -0.0635(4) 0.0194(14) Uani 1 1 d . . . C64 C 0.2034(4) 0.2511(2) -0.0926(3) 0.0220(15) Uani 1 1 d . . . C65 C 0.2652(4) 0.27310(18) -0.0342(4) 0.0181(14) Uani 1 1 d . . . C66 C 0.2726(4) 0.25996(19) 0.0546(3) 0.0184(14) Uani 1 1 d . . . C67 C 0.1384(4) 0.24740(18) 0.2504(3) 0.0210(6) Uani 1 1 d . . . C68 C 0.0421(4) 0.23782(19) 0.2593(3) 0.0210(6) Uani 1 1 d . . . C69 C -0.0225(4) 0.26842(19) 0.2889(3) 0.0210(6) Uani 1 1 d . . . C70 C 0.0074(4) 0.31075(19) 0.3126(3) 0.0210(6) Uani 1 1 d . . . C71 C 0.1007(4) 0.32223(19) 0.3070(3) 0.0210(6) Uani 1 1 d . . . C72 C 0.1625(4) 0.29122(19) 0.2755(3) 0.0210(6) Uani 1 1 d . . . F1 F 0.1010(2) 0.17104(10) 0.04977(18) 0.0260(8) Uani 1 1 d . . . F2 F 0.0866(2) 0.19612(11) -0.12081(19) 0.0371(9) Uani 1 1 d . . . F3 F 0.1942(2) 0.26425(11) -0.17902(19) 0.0368(9) Uani 1 1 d . . . F4 F 0.3180(2) 0.30717(11) -0.06264(18) 0.0328(9) Uani 1 1 d . . . F5 F 0.3357(2) 0.28310(9) 0.10874(18) 0.0238(8) Uani 1 1 d . . . F6 F 0.0081(2) 0.19675(10) 0.23598(18) 0.0272(8) Uani 1 1 d . . . F7 F -0.1140(2) 0.25673(11) 0.29504(19) 0.0380(9) Uani 1 1 d . . . F8 F -0.0552(2) 0.34138(11) 0.33858(19) 0.0429(10) Uani 1 1 d . . . F9 F 0.1311(2) 0.36380(10) 0.32910(19) 0.0377(10) Uani 1 1 d . . . F10 F 0.2543(2) 0.30488(10) 0.27103(17) 0.0271(8) Uani 1 1 d . . . Fe1 Fe 0.57639(6) 0.17296(3) 0.11568(5) 0.0213(2) Uani 1 1 d . . . Fe2 Fe 0.40250(5) 0.19633(3) 0.50439(5) 0.01833(19) Uani 1 1 d . . . P1 P 0.26778(10) 0.03549(5) 0.17551(9) 0.0177(4) Uani 1 1 d . . . P2 P 0.12532(11) 0.05812(5) 0.34325(9) 0.0176(4) Uani 1 1 d . . . Pt1 Pt 0.226381(16) 0.095737(8) 0.257211(14) 0.01498(6) Uani 1 1 d . . . Pt2 Pt 0.231848(15) 0.201857(8) 0.214480(13) 0.01423(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 C1 0.015(3) 0.018(4) 0.020(3) 0.003(3) 0.007(3) 0.004(3) C2 0.017(3) 0.028(4) 0.021(3) -0.005(3) 0.011(3) -0.001(3) C3 0.021(4) 0.019(4) 0.028(4) -0.010(3) 0.005(3) -0.010(3) C4 0.066(5) 0.051(5) 0.055(4) -0.017(4) 0.028(4) -0.044(5) C5 0.046(5) 0.022(4) 0.056(4) -0.008(3) 0.001(4) -0.008(4) C6 0.038(4) 0.056(5) 0.072(6) -0.004(4) -0.016(4) -0.002(4) C7 0.011(3) 0.017(4) 0.018(3) -0.004(3) 0.003(3) -0.002(3) C8 0.021(4) 0.021(4) 0.027(4) -0.003(3) 0.006(3) -0.002(3) C9 0.033(4) 0.020(4) 0.025(4) 0.000(3) 0.010(3) 0.006(3) C10 0.049(5) 0.021(4) 0.051(4) 0.004(3) -0.008(4) 0.010(4) C11 0.060(5) 0.032(4) 0.050(4) 0.012(3) 0.017(4) 0.005(4) C12 0.036(4) 0.042(5) 0.036(4) 0.011(3) 0.003(3) 0.018(4) C13 0.015(3) 0.016(4) 0.026(3) 0.000(3) 0.002(3) -0.009(3) C14 0.027(4) 0.023(4) 0.025(4) 0.004(3) 0.005(3) 0.011(3) C15 0.037(4) 0.026(4) 0.039(4) 0.005(3) 0.017(4) 0.012(3) C16 0.037(4) 0.027(4) 0.017(3) 0.004(3) 0.006(3) -0.005(3) C17 0.029(4) 0.022(4) 0.022(3) 0.003(3) -0.001(3) 0.003(3) C18 0.023(4) 0.017(4) 0.029(4) -0.007(3) 0.004(3) 0.001(3) C19 0.017(3) 0.009(3) 0.015(3) 0.005(2) 0.008(3) 0.003(3) C20 0.023(4) 0.018(4) 0.023(3) -0.004(3) 0.008(3) 0.001(3) C21 0.029(4) 0.017(4) 0.032(4) 0.004(3) 0.009(3) 0.008(3) C22 0.018(4) 0.033(4) 0.032(4) 0.001(3) 0.000(3) 0.000(3) C23 0.032(4) 0.030(4) 0.025(4) -0.005(3) -0.003(3) 0.002(4) C24 0.022(4) 0.024(4) 0.032(4) -0.002(3) 0.002(3) 0.002(3) C25 0.022(4) 0.017(4) 0.024(3) -0.006(3) 0.006(3) 0.004(3) C26 0.026(4) 0.030(4) 0.038(4) -0.005(3) 0.000(3) 0.000(3) C27 0.025(4) 0.043(5) 0.055(5) -0.004(4) -0.005(4) -0.009(4) C28 0.024(4) 0.055(5) 0.041(4) -0.008(4) -0.009(4) 0.016(4) C29 0.031(4) 0.053(5) 0.032(4) 0.003(4) -0.006(4) 0.015(4) C30 0.027(4) 0.036(4) 0.036(4) 0.014(3) 0.007(3) 0.003(3) C31 0.016(3) 0.011(3) 0.022(3) 0.001(3) 0.012(3) -0.003(3) C32 0.039(4) 0.020(4) 0.036(4) 0.004(3) 0.014(4) -0.001(3) C33 0.067(5) 0.026(4) 0.017(3) 0.003(3) 0.006(4) -0.002(4) C34 0.053(5) 0.024(4) 0.032(4) -0.005(3) 0.025(4) -0.008(4) C35 0.020(4) 0.026(4) 0.048(5) -0.012(3) 0.020(4) 0.000(3) C36 0.013(3) 0.034(4) 0.031(4) 0.000(3) 0.005(3) 0.003(3) C37 0.024(4) 0.017(3) 0.011(3) -0.003(3) -0.007(3) -0.002(3) C38 0.018(3) 0.015(3) 0.019(3) -0.006(3) -0.007(3) 0.003(3) C39 0.022(3) 0.010(3) 0.020(3) -0.002(3) 0.004(3) -0.003(3) C40 0.018(3) 0.012(3) 0.017(3) 0.007(3) 0.007(3) -0.003(3) C41 0.008(3) 0.017(3) 0.015(3) 0.008(3) 0.000(3) 0.005(3) C42 0.011(3) 0.006(3) 0.021(3) 0.001(2) 0.003(3) 0.002(3) C43 0.022(3) 0.025(4) 0.016(3) -0.002(3) 0.006(3) -0.008(3) C44 0.016(3) 0.025(4) 0.022(3) 0.004(3) 0.007(3) 0.003(3) C45 0.016(4) 0.025(4) 0.029(4) 0.001(3) 0.004(3) -0.002(3) C46 0.018(3) 0.015(3) 0.015(3) 0.003(3) 0.000(3) -0.002(3) C47 0.021(4) 0.012(3) 0.021(3) 0.000(3) 0.001(3) 0.003(3) C48 0.019(4) 0.006(3) 0.042(4) -0.002(3) -0.005(3) 0.007(3) C49 0.026(4) 0.023(4) 0.025(3) -0.009(3) -0.007(3) 0.009(3) C50 0.016(3) 0.020(4) 0.027(3) 0.000(3) 0.005(3) 0.005(3) C51 0.029(4) 0.024(4) 0.052(5) 0.004(4) 0.013(4) 0.005(3) C52 0.057(5) 0.023(4) 0.047(5) -0.002(3) 0.018(4) 0.010(4) C53 0.038(5) 0.027(4) 0.075(6) 0.003(4) 0.032(5) 0.003(4) C54 0.022(4) 0.033(4) 0.074(6) -0.010(4) -0.002(4) 0.011(4) C55 0.031(4) 0.040(5) 0.045(5) 0.013(4) 0.007(4) 0.016(4) C56 0.040(4) 0.036(5) 0.028(4) -0.012(3) -0.010(4) 0.020(4) C57 0.023(4) 0.026(4) 0.058(5) 0.006(4) 0.003(4) 0.008(3) C58 0.036(5) 0.022(4) 0.069(5) -0.021(4) -0.034(4) 0.010(4) C59 0.061(5) 0.033(4) 0.030(4) 0.001(3) -0.014(4) 0.012(4) C60 0.031(4) 0.015(4) 0.061(5) 0.002(4) 0.000(4) 0.000(3) C61 0.011(3) 0.020(4) 0.020(3) -0.005(3) -0.003(3) 0.003(3) C62 0.013(3) 0.012(3) 0.029(3) 0.002(3) 0.004(3) 0.001(3) C63 0.007(3) 0.028(4) 0.023(3) -0.006(3) -0.003(3) 0.000(3) C64 0.018(4) 0.040(4) 0.008(3) 0.002(3) -0.003(3) 0.006(3) C65 0.017(3) 0.015(3) 0.023(3) 0.014(3) 0.009(3) 0.002(3) C66 0.020(3) 0.015(3) 0.019(3) -0.002(3) -0.009(3) 0.004(3) C67 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) C68 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) C69 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) C70 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) C71 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) C72 0.0262(15) 0.0239(16) 0.0132(12) 0.0026(12) 0.0023(12) 0.0076(14) F1 0.0214(19) 0.023(2) 0.0329(19) 0.0016(15) -0.0011(16) -0.0075(17) F2 0.034(2) 0.044(2) 0.0314(19) -0.0047(18) -0.0111(17) -0.007(2) F3 0.035(2) 0.052(2) 0.0238(19) 0.0096(17) -0.0019(18) 0.002(2) F4 0.037(2) 0.029(2) 0.0324(19) 0.0116(16) 0.0049(17) -0.0027(19) F5 0.0235(19) 0.022(2) 0.0261(18) 0.0025(15) -0.0014(16) -0.0084(16) F6 0.0221(18) 0.022(2) 0.0376(19) -0.0065(16) 0.0044(16) 0.0020(17) F7 0.019(2) 0.058(3) 0.038(2) 0.0072(18) 0.0075(18) 0.0108(19) F8 0.059(3) 0.038(2) 0.034(2) -0.0005(18) 0.018(2) 0.028(2) F9 0.061(3) 0.016(2) 0.036(2) -0.0079(16) 0.005(2) 0.0084(19) F10 0.038(2) 0.0140(18) 0.0294(18) -0.0024(15) 0.0035(17) -0.0008(17) Fe1 0.0187(5) 0.0175(5) 0.0286(5) 0.0005(4) 0.0079(4) 0.0005(4) Fe2 0.0183(5) 0.0134(5) 0.0227(4) -0.0023(4) -0.0036(4) 0.0036(4) P1 0.0188(9) 0.0120(8) 0.0226(9) -0.0005(7) 0.0038(7) -0.0028(7) P2 0.0182(9) 0.0123(9) 0.0225(9) -0.0015(7) 0.0034(7) 0.0006(7) Pt1 0.01623(13) 0.00998(12) 0.01912(12) -0.00072(11) 0.00404(10) -0.00075(12) Pt2 0.01486(12) 0.01061(12) 0.01719(12) -0.00014(11) 0.00083(10) 0.00034(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.195(7) . ? C1 P1 1.737(6) . ? C2 C3 1.472(7) . ? C3 C4 1.510(6) . ? C3 C6 1.512(8) . ? C3 C5 1.517(7) . ? C7 C8 1.175(7) . ? C7 P2 1.748(6) . ? C8 C9 1.479(8) . ? C9 C11 1.504(6) . ? C9 C12 1.532(7) . ? C9 C10 1.539(7) . ? C13 C18 1.371(7) . ? C13 C14 1.395(6) . ? C13 P1 1.827(5) . ? C14 C15 1.373(6) . ? C15 C16 1.384(7) . ? C16 C17 1.369(7) . ? C17 C18 1.377(6) . ? C19 C20 1.381(7) . ? C19 C24 1.392(7) . ? C19 P1 1.806(5) . ? C20 C21 1.377(7) . ? C21 C22 1.371(7) . ? C22 C23 1.348(7) . ? C23 C24 1.389(7) . ? C25 C26 1.384(7) . ? C25 C30 1.389(7) . ? C25 P2 1.797(6) . ? C26 C27 1.386(7) . ? C27 C28 1.360(8) . ? C28 C29 1.356(8) . ? C29 C30 1.368(7) . ? C31 C36 1.380(7) . ? C31 C32 1.390(7) . ? C31 P2 1.818(5) . ? C32 C33 1.381(7) . ? C33 C34 1.355(8) . ? C34 C35 1.371(7) . ? C35 C36 1.381(7) . ? C37 C38 1.228(6) . ? C37 Pt1 1.979(6) . ? C37 Pt2 2.282(5) . ? C38 C39 1.465(7) . ? C38 Pt2 2.307(5) . ? C39 C46 1.400(7) . ? C39 C43 1.407(6) . ? C39 Fe1 2.019(5) . ? C40 C41 1.219(7) . ? C40 Pt1 1.991(5) . ? C40 Pt2 2.225(5) . ? C41 C42 1.447(7) . ? C41 Pt2 2.264(5) . ? C42 C47 1.411(7) . ? C42 C50 1.417(6) . ? C42 Fe2 2.009(5) . ? C43 C44 1.384(7) . ? C43 Fe1 2.000(5) . ? C44 C45 1.392(7) . ? C44 Fe1 2.005(5) . ? C45 C46 1.410(6) . ? C45 Fe1 2.025(6) . ? C46 Fe1 2.017(5) . ? C47 C48 1.413(7) . ? C47 Fe2 2.027(5) . ? C48 C49 1.400(7) . ? C48 Fe2 2.049(5) . ? C49 C50 1.405(7) . ? C49 Fe2 2.048(5) . ? C50 Fe2 2.007(5) . ? C51 C55 1.380(8) . ? C51 C52 1.404(7) . ? C51 Fe1 2.024(6) . ? C52 C53 1.386(8) . ? C52 Fe1 2.027(6) . ? C53 C54 1.384(8) . ? C53 Fe1 2.025(6) . ? C54 C55 1.384(7) . ? C54 Fe1 2.009(6) . ? C55 Fe1 2.012(6) . ? C56 C60 1.377(7) . ? C56 C57 1.399(8) . ? C56 Fe2 2.029(6) . ? C57 C58 1.361(7) . ? C57 Fe2 2.040(6) . ? C58 C59 1.371(8) . ? C58 Fe2 2.011(6) . ? C59 C60 1.387(8) . ? C59 Fe2 2.017(6) . ? C60 Fe2 2.008(6) . ? C61 C62 1.377(7) . ? C61 C66 1.406(7) . ? C61 Pt2 1.998(5) . ? C62 C63 1.365(7) . ? C62 F1 1.372(5) . ? C63 F2 1.338(6) . ? C63 C64 1.365(7) . ? C64 F3 1.354(5) . ? C64 C65 1.361(7) . ? C65 F4 1.343(5) . ? C65 C66 1.387(7) . ? C66 F5 1.352(6) . ? C67 C68 1.399(7) . ? C67 C72 1.393(7) . ? C67 Pt2 1.987(5) . ? C68 F6 1.350(6) . ? C68 C69 1.380(7) . ? C69 F7 1.343(6) . ? C69 C70 1.367(7) . ? C70 F8 1.343(6) . ? C70 C71 1.364(7) . ? C71 F9 1.343(6) . ? C71 C72 1.373(7) . ? C72 F10 1.360(6) . ? P1 Pt1 2.2697(14) . ? P2 Pt1 2.2766(14) . ? Pt1 Pt2 3.2236(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 C2 C1 P1 177.3(5) . . ? C1 C2 C3 176.5(6) . . ? C2 C3 C4 110.2(4) . . ? C2 C3 C6 109.0(5) . . ? C4 C3 C6 110.2(5) . . ? C2 C3 C5 108.0(4) . . ? C4 C3 C5 109.6(5) . . ? C6 C3 C5 109.8(5) . . ? C8 C7 P2 170.8(5) . . ? C7 C8 C9 177.1(7) . . ? C8 C9 C11 109.8(5) . . ? C8 C9 C12 107.1(5) . . ? C11 C9 C12 110.1(5) . . ? C8 C9 C10 108.9(5) . . ? C11 C9 C10 109.7(5) . . ? C12 C9 C10 111.2(5) . . ? C18 C13 C14 119.0(5) . . ? C18 C13 P1 119.7(4) . . ? C14 C13 P1 121.3(4) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 120.0(5) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 119.2(5) . . ? C13 C18 C17 121.4(5) . . ? C20 C19 C24 117.4(5) . . ? C20 C19 P1 124.0(4) . . ? C24 C19 P1 118.6(4) . . ? C21 C20 C19 121.6(6) . . ? C22 C21 C20 119.2(6) . . ? C23 C22 C21 121.3(6) . . ? C22 C23 C24 119.5(6) . . ? C23 C24 C19 121.0(6) . . ? C26 C25 C30 117.5(6) . . ? C26 C25 P2 122.6(5) . . ? C30 C25 P2 119.9(5) . . ? C25 C26 C27 119.7(6) . . ? C28 C27 C26 121.9(6) . . ? C29 C28 C27 118.5(6) . . ? C28 C29 C30 121.0(6) . . ? C29 C30 C25 121.4(6) . . ? C36 C31 C32 118.3(5) . . ? C36 C31 P2 119.4(4) . . ? C32 C31 P2 122.2(4) . . ? C33 C32 C31 120.0(6) . . ? C34 C33 C32 121.1(6) . . ? C33 C34 C35 119.6(6) . . ? C34 C35 C36 120.2(6) . . ? C35 C36 C31 120.7(6) . . ? C38 C37 Pt1 167.8(5) . . ? C38 C37 Pt2 75.6(4) . . ? Pt1 C37 Pt2 98.1(2) . . ? C37 C38 C39 168.3(5) . . ? C37 C38 Pt2 73.4(4) . . ? C39 C38 Pt2 118.3(4) . . ? C46 C39 C43 107.8(5) . . ? C46 C39 C38 124.9(4) . . ? C43 C39 C38 127.3(5) . . ? C46 C39 Fe1 69.7(3) . . ? C43 C39 Fe1 68.8(3) . . ? C38 C39 Fe1 127.7(4) . . ? C41 C40 Pt1 155.5(5) . . ? C41 C40 Pt2 76.1(3) . . ? Pt1 C40 Pt2 99.6(2) . . ? C40 C41 C42 161.5(5) . . ? C40 C41 Pt2 72.5(3) . . ? C42 C41 Pt2 125.9(4) . . ? C47 C42 C50 107.2(5) . . ? C47 C42 C41 128.1(5) . . ? C50 C42 C41 123.7(5) . . ? C47 C42 Fe2 70.2(3) . . ? C50 C42 Fe2 69.3(3) . . ? C41 C42 Fe2 116.8(4) . . ? C44 C43 C39 107.9(5) . . ? C44 C43 Fe1 69.9(3) . . ? C39 C43 Fe1 70.2(3) . . ? C43 C44 C45 109.0(5) . . ? C43 C44 Fe1 69.6(3) . . ? C45 C44 Fe1 70.6(3) . . ? C44 C45 C46 107.5(5) . . ? C44 C45 Fe1 69.0(3) . . ? C46 C45 Fe1 69.3(3) . . ? C39 C46 C45 107.8(4) . . ? C39 C46 Fe1 69.7(3) . . ? C45 C46 Fe1 69.9(3) . . ? C42 C47 C48 108.2(5) . . ? C42 C47 Fe2 68.9(3) . . ? C48 C47 Fe2 70.6(3) . . ? C49 C48 C47 108.1(5) . . ? C49 C48 Fe2 70.0(3) . . ? C47 C48 Fe2 68.9(3) . . ? C48 C49 C50 108.1(5) . . ? C48 C49 Fe2 70.1(3) . . ? C50 C49 Fe2 68.2(3) . . ? C49 C50 C42 108.4(5) . . ? C49 C50 Fe2 71.3(3) . . ? C42 C50 Fe2 69.4(3) . . ? C55 C51 C52 107.4(6) . . ? C55 C51 Fe1 69.5(4) . . ? C52 C51 Fe1 69.8(3) . . ? C53 C52 C51 107.6(6) . . ? C53 C52 Fe1 69.9(4) . . ? C51 C52 Fe1 69.6(3) . . ? C54 C53 C52 108.3(6) . . ? C54 C53 Fe1 69.3(4) . . ? C52 C53 Fe1 70.1(3) . . ? C53 C54 C55 107.9(6) . . ? C53 C54 Fe1 70.5(4) . . ? C55 C54 Fe1 70.0(3) . . ? C51 C55 C54 108.7(6) . . ? C51 C55 Fe1 70.5(4) . . ? C54 C55 Fe1 69.8(3) . . ? C60 C56 C57 107.1(6) . . ? C60 C56 Fe2 69.2(3) . . ? C57 C56 Fe2 70.3(3) . . ? C58 C57 C56 107.9(6) . . ? C58 C57 Fe2 69.2(4) . . ? C56 C57 Fe2 69.5(3) . . ? C57 C58 C59 109.2(6) . . ? C57 C58 Fe2 71.5(4) . . ? C59 C58 Fe2 70.3(4) . . ? C58 C59 C60 107.3(6) . . ? C58 C59 Fe2 69.9(4) . . ? C60 C59 Fe2 69.5(3) . . ? C56 C60 C59 108.5(6) . . ? C56 C60 Fe2 70.9(4) . . ? C59 C60 Fe2 70.2(4) . . ? C62 C61 C66 111.8(5) . . ? C62 C61 Pt2 122.3(4) . . ? C66 C61 Pt2 125.8(4) . . ? C63 C62 F1 115.4(5) . . ? C63 C62 C61 126.7(5) . . ? F1 C62 C61 117.9(5) . . ? F2 C63 C64 119.8(5) . . ? F2 C63 C62 121.9(5) . . ? C64 C63 C62 118.3(5) . . ? F3 C64 C65 119.8(5) . . ? F3 C64 C63 120.1(5) . . ? C65 C64 C63 120.1(5) . . ? F4 C65 C64 120.0(5) . . ? F4 C65 C66 120.7(5) . . ? C64 C65 C66 119.3(5) . . ? F5 C66 C65 116.1(5) . . ? F5 C66 C61 120.1(5) . . ? C65 C66 C61 123.8(5) . . ? C68 C67 C72 112.6(5) . . ? C68 C67 Pt2 123.3(4) . . ? C72 C67 Pt2 123.9(4) . . ? F6 C68 C69 116.8(5) . . ? F6 C68 C67 119.2(5) . . ? C69 C68 C67 123.9(6) . . ? F7 C69 C70 120.0(5) . . ? F7 C69 C68 120.4(5) . . ? C70 C69 C68 119.6(6) . . ? F8 C70 C71 120.0(5) . . ? F8 C70 C69 120.3(5) . . ? C71 C70 C69 119.7(6) . . ? F9 C71 C70 120.5(5) . . ? F9 C71 C72 120.3(5) . . ? C70 C71 C72 119.1(6) . . ? F10 C72 C71 116.2(5) . . ? F10 C72 C67 118.8(5) . . ? C71 C72 C67 125.0(5) . . ? C43 Fe1 C44 40.4(2) . . ? C43 Fe1 C54 165.6(3) . . ? C44 Fe1 C54 127.8(3) . . ? C43 Fe1 C55 152.7(3) . . ? C44 Fe1 C55 166.1(3) . . ? C54 Fe1 C55 40.3(2) . . ? C43 Fe1 C46 68.7(2) . . ? C44 Fe1 C46 68.4(2) . . ? C54 Fe1 C46 117.9(3) . . ? C55 Fe1 C46 109.1(2) . . ? C43 Fe1 C39 40.99(17) . . ? C44 Fe1 C39 68.3(2) . . ? C54 Fe1 C39 151.9(3) . . ? C55 Fe1 C39 119.4(2) . . ? C46 Fe1 C39 40.60(19) . . ? C43 Fe1 C51 119.2(3) . . ? C44 Fe1 C51 151.8(3) . . ? C54 Fe1 C51 67.7(3) . . ? C55 Fe1 C51 40.0(2) . . ? C46 Fe1 C51 129.6(2) . . ? C39 Fe1 C51 109.8(2) . . ? C43 Fe1 C45 68.3(2) . . ? C44 Fe1 C45 40.43(19) . . ? C54 Fe1 C45 107.6(3) . . ? C55 Fe1 C45 128.9(3) . . ? C46 Fe1 C45 40.82(18) . . ? C39 Fe1 C45 68.3(2) . . ? C51 Fe1 C45 167.2(2) . . ? C43 Fe1 C53 128.2(3) . . ? C44 Fe1 C53 107.8(2) . . ? C54 Fe1 C53 40.1(2) . . ? C55 Fe1 C53 67.3(2) . . ? C46 Fe1 C53 150.7(3) . . ? C39 Fe1 C53 167.2(3) . . ? C51 Fe1 C53 67.6(2) . . ? C45 Fe1 C53 117.2(3) . . ? C43 Fe1 C52 108.6(3) . . ? C44 Fe1 C52 117.7(2) . . ? C54 Fe1 C52 67.6(3) . . ? C55 Fe1 C52 67.5(3) . . ? C46 Fe1 C52 168.0(2) . . ? C39 Fe1 C52 129.9(3) . . ? C51 Fe1 C52 40.6(2) . . ? C45 Fe1 C52 150.3(2) . . ? C53 Fe1 C52 40.0(2) . . ? C50 Fe2 C60 107.2(2) . . ? C50 Fe2 C42 41.33(18) . . ? C60 Fe2 C42 114.5(2) . . ? C50 Fe2 C58 150.1(3) . . ? C60 Fe2 C58 67.1(2) . . ? C42 Fe2 C58 168.5(3) . . ? C50 Fe2 C59 116.5(3) . . ? C60 Fe2 C59 40.3(2) . . ? C42 Fe2 C59 148.0(3) . . ? C58 Fe2 C59 39.8(2) . . ? C50 Fe2 C47 68.7(2) . . ? C60 Fe2 C47 147.8(2) . . ? C42 Fe2 C47 40.90(19) . . ? C58 Fe2 C47 132.2(3) . . ? C59 Fe2 C47 170.6(3) . . ? C50 Fe2 C56 128.5(2) . . ? C60 Fe2 C56 39.9(2) . . ? C42 Fe2 C56 106.4(2) . . ? C58 Fe2 C56 67.0(2) . . ? C59 Fe2 C56 67.3(2) . . ? C47 Fe2 C56 116.3(2) . . ? C50 Fe2 C57 167.8(3) . . ? C60 Fe2 C57 66.9(2) . . ? C42 Fe2 C57 129.8(2) . . ? C58 Fe2 C57 39.2(2) . . ? C59 Fe2 C57 66.6(2) . . ? C47 Fe2 C57 110.1(2) . . ? C56 Fe2 C57 40.2(2) . . ? C50 Fe2 C49 40.5(2) . . ? C60 Fe2 C49 130.6(2) . . ? C42 Fe2 C49 68.7(2) . . ? C58 Fe2 C49 119.6(2) . . ? C59 Fe2 C49 110.4(2) . . ? C47 Fe2 C49 67.9(2) . . ? C56 Fe2 C49 167.7(3) . . ? C57 Fe2 C49 151.3(3) . . ? C50 Fe2 C48 68.1(2) . . ? C60 Fe2 C48 169.6(2) . . ? C42 Fe2 C48 68.6(2) . . ? C58 Fe2 C48 112.0(2) . . ? C59 Fe2 C48 132.4(2) . . ? C47 Fe2 C48 40.56(19) . . ? C56 Fe2 C48 150.2(2) . . ? C57 Fe2 C48 119.5(2) . . ? C49 Fe2 C48 39.96(19) . . ? C1 P1 C19 104.6(3) . . ? C1 P1 C13 101.2(2) . . ? C19 P1 C13 104.6(2) . . ? C1 P1 Pt1 119.92(17) . . ? C19 P1 Pt1 110.03(18) . . ? C13 P1 Pt1 114.96(18) . . ? C7 P2 C25 106.7(3) . . ? C7 P2 C31 102.9(2) . . ? C25 P2 C31 104.9(2) . . ? C7 P2 Pt1 115.46(17) . . ? C25 P2 Pt1 112.65(19) . . ? C31 P2 Pt1 113.28(17) . . ? C37 Pt1 C40 77.8(2) . . ? C37 Pt1 P1 91.96(15) . . ? C40 Pt1 P1 168.08(15) . . ? C37 Pt1 P2 171.67(15) . . ? C40 Pt1 P2 93.88(14) . . ? P1 Pt1 P2 96.34(5) . . ? C37 Pt1 Pt2 44.51(15) . . ? C40 Pt1 Pt2 42.88(14) . . ? P1 Pt1 Pt2 130.96(4) . . ? P2 Pt1 Pt2 128.20(4) . . ? C67 Pt2 C61 90.2(2) . . ? C67 Pt2 C40 98.58(19) . . ? C61 Pt2 C40 156.6(2) . . ? C67 Pt2 C41 83.94(19) . . ? C61 Pt2 C41 171.4(2) . . ? C40 Pt2 C41 31.48(17) . . ? C67 Pt2 C37 163.5(2) . . ? C61 Pt2 C37 100.17(19) . . ? C40 Pt2 C37 67.14(18) . . ? C41 Pt2 C37 86.98(18) . . ? C67 Pt2 C38 165.0(2) . . ? C61 Pt2 C38 84.68(19) . . ? C40 Pt2 C38 91.55(19) . . ? C41 Pt2 C38 99.46(18) . . ? C37 Pt2 C38 31.04(16) . . ? C67 Pt2 Pt1 126.09(15) . . ? C61 Pt2 Pt1 121.34(15) . . ? C40 Pt2 Pt1 37.52(14) . . ? C41 Pt2 Pt1 67.22(14) . . ? C37 Pt2 Pt1 37.44(14) . . ? C38 Pt2 Pt1 68.14(14) . . ? #===END