# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Elena Lalinde' _publ_contact_author_email ELENA.LALINDE@DQ.UNIRIOJA.ES _publ_section_title ; Complexes of Platinum(II) containing Ferrocenylethynyl ligands: Synthesis, Characterization and Spectroscopic and Electrochemical Properties ; _publ_requested_category FM loop_ _publ_author_name 'Elena Lalinde' 'Alvaro Diez' J.Fernandez 'M. Teresa Moreno' S.Sanchez # Attachment 'B806572A-revised.cif' data_complex1.2CHCl3 _database_code_depnum_ccdc_archive 'CCDC 685381' _audit_creation_date 2007-05-29T11:44:56-00:00 _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 s73 _chemical_formula_sum 'C34 H32 Cl6 Fe2 Pt' _chemical_formula_weight 960.09 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6163(3) _cell_length_b 16.9063(6) _cell_length_c 17.7695(4) _cell_angle_alpha 90 _cell_angle_beta 104.500(2) _cell_angle_gamma 90 _cell_volume 3378.57(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 2981 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.477 _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 0.3985 _exptl_absorpt_correction_T_max 0.5011 #----------------------------------------------------------------------------# # 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 -0.0002081 _diffrn_orient_matrix_ub_12 0.0281309 _diffrn_orient_matrix_ub_13 0.0494701 _diffrn_orient_matrix_ub_21 -0.069031 _diffrn_orient_matrix_ub_22 0.0327449 _diffrn_orient_matrix_ub_23 -0.0282583 _diffrn_orient_matrix_ub_31 -0.0560454 _diffrn_orient_matrix_ub_32 -0.0404363 _diffrn_orient_matrix_ub_33 0.0115323 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_number 50545 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7724 _reflns_number_gt 6099 _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^)+(0.0311P)^2^+13.6825P] 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 7724 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.081 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.515 _refine_diff_density_min -1.72 _refine_diff_density_rms 0.172 #----------------------------------------------------------------------------# # 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.0926(5) 0.9054(5) 0.5199(4) 0.0401(17) Uani 1 1 d . . . H1 H 0.0439 0.9515 0.5249 0.048 Uiso 1 1 calc R . . C2 C 0.0869(5) 0.8459(4) 0.5703(4) 0.0314(15) Uani 1 1 d . . . H2 H 0.035 0.8566 0.605 0.038 Uiso 1 1 calc R . . C3 C 0.1137(8) 0.8959(9) 0.4410(5) 0.114(5) Uani 1 1 d . . . H3A H 0.0494 0.8641 0.4104 0.137 Uiso 1 1 calc R . . H3B H 0.1074 0.9479 0.4171 0.137 Uiso 1 1 calc R . . C4 C 0.2245(7) 0.8611(5) 0.4340(4) 0.049(2) Uani 1 1 d . . . H4A H 0.2584 0.8958 0.4017 0.058 Uiso 1 1 calc R . . H4B H 0.2059 0.8115 0.4063 0.058 Uiso 1 1 calc R . . C5 C 0.3180(5) 0.8453(4) 0.5068(3) 0.0288(14) Uani 1 1 d . . . H5 H 0.3986 0.859 0.5034 0.035 Uiso 1 1 calc R . . C6 C 0.3145(5) 0.7880(4) 0.5597(3) 0.0296(14) Uani 1 1 d . . . H6 H 0.393 0.768 0.5872 0.036 Uiso 1 1 calc R . . C7 C 0.2158(7) 0.7299(4) 0.5544(4) 0.0458(19) Uani 1 1 d . . . H7A H 0.2096 0.6985 0.5079 0.055 Uiso 1 1 calc R . . H7B H 0.2387 0.6943 0.5984 0.055 Uiso 1 1 calc R . . C8 C 0.0996(8) 0.7599(5) 0.5526(8) 0.091(4) Uani 1 1 d . . . H8A H 0.0684 0.7292 0.5892 0.109 Uiso 1 1 calc R . . H8B H 0.049 0.7495 0.5012 0.109 Uiso 1 1 calc R . . C9 C 0.2104(5) 0.9815(3) 0.6720(3) 0.0185(11) Uani 1 1 d . . . C10 C 0.1789(5) 1.0284(3) 0.7127(3) 0.0222(12) Uani 1 1 d . . . C11 C 0.1470(5) 1.0832(3) 0.7656(3) 0.0227(12) Uani 1 1 d . . . C12 C 0.1228(5) 1.1661(4) 0.7522(4) 0.0291(14) Uani 1 1 d . . . H12 H 0.1199 1.1932 0.7063 0.035 Uiso 1 1 calc R . . C13 C 0.1039(5) 1.1995(4) 0.8220(4) 0.0332(15) Uani 1 1 d . . . H13 H 0.0866 1.2522 0.8294 0.04 Uiso 1 1 calc R . . C14 C 0.1160(5) 1.1383(4) 0.8780(4) 0.0312(14) Uani 1 1 d . . . H14 H 0.1078 1.1439 0.9284 0.037 Uiso 1 1 calc R . . C15 C 0.1425(5) 1.0674(4) 0.8441(3) 0.0274(13) Uani 1 1 d . . . H15 H 0.155 1.0184 0.8686 0.033 Uiso 1 1 calc R . . C16 C 0.4111(6) 1.2021(6) 0.8150(4) 0.052(2) Uani 1 1 d . . . H16 H 0.4106 1.2295 0.7695 0.062 Uiso 1 1 calc R . . C17 C 0.3925(6) 1.2351(4) 0.8842(4) 0.0382(16) Uani 1 1 d . . . H17 H 0.3772 1.288 0.892 0.046 Uiso 1 1 calc R . . C18 C 0.4012(6) 1.1744(4) 0.9387(4) 0.0378(16) Uani 1 1 d . . . H18 H 0.3929 1.1801 0.9891 0.045 Uiso 1 1 calc R . . C19 C 0.4245(6) 1.1034(4) 0.9043(5) 0.0463(18) Uani 1 1 d . . . H19 H 0.4343 1.0539 0.9278 0.056 Uiso 1 1 calc R . . C20 C 0.4305(6) 1.1207(6) 0.8274(5) 0.053(2) Uani 1 1 d . . . H20 H 0.4448 1.0844 0.7915 0.064 Uiso 1 1 calc R . . C21 C 0.4319(5) 0.9298(4) 0.6597(3) 0.0249(13) Uani 1 1 d . . . C22 C 0.5315(5) 0.9507(4) 0.6856(3) 0.0264(13) Uani 1 1 d . . . C23 C 0.8578(5) 0.9855(4) 0.7364(3) 0.0362(16) Uani 1 1 d . . . H23 H 0.9368 0.9726 0.7396 0.043 Uiso 1 1 calc R . . C24 C 0.8167(6) 1.0581(4) 0.7587(4) 0.0368(16) Uani 1 1 d . . . H24 H 0.8636 1.1013 0.7794 0.044 Uiso 1 1 calc R . . C25 C 0.6919(5) 1.0537(4) 0.7441(3) 0.0296(14) Uani 1 1 d . . . H25 H 0.6425 1.0937 0.7538 0.036 Uiso 1 1 calc R . . C26 C 0.6535(5) 0.9779(4) 0.7122(3) 0.0260(13) Uani 1 1 d . . . C27 C 0.7581(5) 0.9351(4) 0.7082(3) 0.0347(15) Uani 1 1 d . . . H27 H 0.7605 0.8835 0.6904 0.042 Uiso 1 1 calc R . . C28 C 0.7168(7) 0.9844(6) 0.9199(4) 0.058(2) Uani 1 1 d . . . H28 H 0.6667 1.0243 0.9288 0.069 Uiso 1 1 calc R . . C29 C 0.6813(8) 0.9103(7) 0.8887(5) 0.068(3) Uani 1 1 d . . . H29 H 0.6033 0.8921 0.8731 0.081 Uiso 1 1 calc R . . C30 C 0.7845(10) 0.8669(5) 0.8846(5) 0.071(3) Uani 1 1 d . . . H30 H 0.7869 0.8156 0.8662 0.085 Uiso 1 1 calc R . . C31 C 0.8826(7) 0.9173(5) 0.9140(4) 0.054(2) Uani 1 1 d . . . H31 H 0.962 0.905 0.9184 0.064 Uiso 1 1 calc R . . C32 C 0.8393(7) 0.9887(5) 0.9353(4) 0.0471(19) Uani 1 1 d . . . H32 H 0.8855 1.0321 0.9564 0.057 Uiso 1 1 calc R . . C100 C 0.3354(5) 0.1126(3) 0.5663(3) 0.0272(13) Uani 1 1 d . . . H100 H 0.3281 0.0728 0.6049 0.033 Uiso 1 1 calc R . . C200 C 0.7321(6) 0.1499(4) 0.1849(4) 0.0355(15) Uani 1 1 d . . . H200 H 0.7242 0.1033 0.2161 0.043 Uiso 1 1 calc R . . Fe1 Fe 0.26872(7) 1.14996(5) 0.84257(5) 0.02231(18) Uani 1 1 d . . . Fe2 Fe 0.76819(7) 0.96727(5) 0.82002(4) 0.02332(19) Uani 1 1 d . . . Pt1 Pt 0.265261(17) 0.901796(12) 0.606300(11) 0.01674(7) Uani 1 1 d . . . Cl1 Cl 0.44770(16) 0.17926(11) 0.60945(10) 0.0438(4) Uani 1 1 d . . . Cl2 Cl 0.37225(19) 0.06473(11) 0.48818(10) 0.0488(5) Uani 1 1 d . . . Cl3 Cl 0.19941(17) 0.16242(15) 0.53522(14) 0.0689(6) Uani 1 1 d . . . Cl4 Cl 0.64329(17) 0.13604(13) 0.08997(10) 0.0505(5) Uani 1 1 d . . . Cl5 Cl 0.6826(2) 0.23295(13) 0.22637(12) 0.0700(7) Uani 1 1 d . . . Cl6 Cl 0.88161(17) 0.16077(13) 0.18453(14) 0.0632(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 0.013(3) 0.072(5) 0.027(3) -0.003(3) -0.009(2) 0.000(3) C2 0.010(3) 0.042(4) 0.042(4) -0.014(3) 0.007(3) -0.012(3) C3 0.036(5) 0.274(18) 0.027(4) 0.025(7) -0.002(4) 0.006(8) C4 0.081(6) 0.047(4) 0.018(3) -0.006(3) 0.013(4) 0.002(4) C5 0.027(3) 0.036(4) 0.029(3) -0.016(3) 0.019(3) -0.009(3) C6 0.028(3) 0.033(3) 0.029(3) -0.007(3) 0.010(3) 0.008(3) C7 0.068(5) 0.030(4) 0.051(4) -0.002(3) 0.037(4) -0.006(4) C8 0.044(5) 0.036(5) 0.196(12) -0.027(6) 0.038(6) -0.028(4) C9 0.017(3) 0.020(3) 0.017(3) -0.001(2) 0.001(2) -0.004(2) C10 0.018(3) 0.026(3) 0.020(3) -0.001(2) 0.000(2) -0.007(2) C11 0.015(3) 0.025(3) 0.026(3) -0.007(2) 0.004(2) -0.005(2) C12 0.022(3) 0.036(4) 0.027(3) 0.001(3) 0.002(3) 0.005(3) C13 0.020(3) 0.037(4) 0.041(4) -0.012(3) 0.004(3) 0.010(3) C14 0.019(3) 0.042(4) 0.035(3) -0.007(3) 0.012(3) 0.002(3) C15 0.022(3) 0.029(3) 0.030(3) -0.001(3) 0.005(3) -0.004(3) C16 0.029(4) 0.090(7) 0.035(4) 0.004(4) 0.005(3) -0.025(4) C17 0.032(4) 0.037(4) 0.043(4) -0.013(3) 0.004(3) -0.010(3) C18 0.028(4) 0.056(5) 0.026(3) -0.009(3) 0.000(3) -0.003(3) C19 0.028(4) 0.041(4) 0.063(5) -0.003(4) -0.001(3) 0.004(3) C20 0.018(3) 0.086(6) 0.060(5) -0.036(5) 0.015(3) -0.005(4) C21 0.019(3) 0.032(3) 0.023(3) -0.004(2) 0.003(2) -0.002(2) C22 0.022(3) 0.035(3) 0.020(3) -0.004(2) 0.003(2) -0.008(3) C23 0.016(3) 0.067(5) 0.025(3) 0.012(3) 0.005(3) -0.004(3) C24 0.026(3) 0.044(4) 0.036(4) 0.015(3) 0.000(3) -0.011(3) C25 0.020(3) 0.030(3) 0.034(3) 0.012(3) -0.002(3) -0.005(3) C26 0.013(3) 0.045(4) 0.018(3) 0.000(3) 0.000(2) -0.004(3) C27 0.024(3) 0.056(4) 0.022(3) -0.005(3) 0.002(3) -0.004(3) C28 0.050(5) 0.100(7) 0.025(4) 0.005(4) 0.013(4) 0.026(5) C29 0.056(6) 0.109(8) 0.037(4) 0.033(5) 0.010(4) -0.026(6) C30 0.119(9) 0.045(5) 0.044(5) 0.024(4) 0.011(5) 0.006(6) C31 0.040(4) 0.090(7) 0.028(4) 0.024(4) 0.002(3) 0.020(4) C32 0.049(5) 0.067(5) 0.018(3) -0.005(3) -0.006(3) 0.000(4) C100 0.028(3) 0.026(3) 0.030(3) 0.000(2) 0.012(3) -0.004(2) C200 0.043(4) 0.032(4) 0.030(3) 0.008(3) 0.006(3) 0.009(3) Fe1 0.0185(4) 0.0275(4) 0.0212(4) -0.0067(3) 0.0056(3) -0.0007(3) Fe2 0.0184(4) 0.0315(5) 0.0183(4) 0.0022(3) 0.0013(3) -0.0035(3) Pt1 0.01420(11) 0.01997(11) 0.01573(10) -0.00111(9) 0.00314(7) -0.00203(9) Cl1 0.0408(10) 0.0504(10) 0.0371(9) -0.0037(8) 0.0040(8) -0.0177(8) Cl2 0.0758(13) 0.0390(10) 0.0376(9) -0.0075(8) 0.0253(9) -0.0086(9) Cl3 0.0288(10) 0.0872(17) 0.0876(16) 0.0096(13) 0.0089(10) 0.0133(10) Cl4 0.0487(11) 0.0670(13) 0.0324(9) 0.0034(9) 0.0039(8) -0.0086(9) Cl5 0.1114(19) 0.0555(12) 0.0406(11) 0.0031(9) 0.0144(11) 0.0415(13) Cl6 0.0348(10) 0.0690(14) 0.0797(15) 0.0247(12) 0.0028(10) 0.0001(10) #----------------------------------------------------------------------------# # 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 1.359(9) . ? C1 C3 1.491(11) . ? C1 Pt1 2.201(6) . ? C2 C8 1.504(10) . ? C2 Pt1 2.221(5) . ? C3 C4 1.448(12) . ? C4 C5 1.490(9) . ? C5 C6 1.359(8) . ? C5 Pt1 2.226(5) . ? C6 C7 1.496(9) . ? C6 Pt1 2.225(6) . ? C7 C8 1.434(11) . ? C9 C10 1.190(8) . ? C9 Pt1 1.990(5) . ? C10 C11 1.434(8) . ? C11 C15 1.433(8) . ? C11 C12 1.437(8) . ? C11 Fe1 2.042(5) . ? C12 C13 1.428(8) . ? C12 Fe1 2.040(6) . ? C13 C14 1.417(9) . ? C13 Fe1 2.037(6) . ? C14 C15 1.410(9) . ? C14 Fe1 2.035(6) . ? C15 Fe1 2.030(6) . ? C16 C20 1.404(12) . ? C16 C17 1.414(10) . ? C16 Fe1 2.040(7) . ? C17 C18 1.397(10) . ? C17 Fe1 2.038(6) . ? C18 C19 1.404(10) . ? C18 Fe1 2.034(6) . ? C19 C20 1.415(11) . ? C19 Fe1 2.026(7) . ? C20 Fe1 2.025(7) . ? C21 C22 1.187(8) . ? C21 Pt1 1.988(6) . ? C22 C26 1.452(8) . ? C23 C24 1.409(10) . ? C23 C27 1.424(9) . ? C23 Fe2 2.039(6) . ? C24 C25 1.409(8) . ? C24 Fe2 2.042(6) . ? C25 C26 1.428(9) . ? C25 Fe2 2.035(6) . ? C26 C27 1.431(9) . ? C26 Fe2 2.049(5) . ? C27 Fe2 2.034(6) . ? C28 C32 1.382(11) . ? C28 C29 1.391(13) . ? C28 Fe2 2.029(7) . ? C29 C30 1.423(14) . ? C29 Fe2 2.013(7) . ? C30 C31 1.414(12) . ? C30 Fe2 2.031(8) . ? C31 C32 1.396(11) . ? C31 Fe2 2.039(7) . ? C32 Fe2 2.040(6) . ? C100 Cl1 1.749(6) . ? C100 Cl2 1.750(6) . ? C100 Cl3 1.753(6) . ? C200 Cl5 1.748(7) . ? C200 Cl6 1.749(7) . ? C200 Cl4 1.759(6) . ? 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 C3 126.0(9) . . ? C2 C1 Pt1 72.9(3) . . ? C3 C1 Pt1 108.5(5) . . ? C1 C2 C8 123.6(8) . . ? C1 C2 Pt1 71.3(3) . . ? C8 C2 Pt1 109.8(4) . . ? C4 C3 C1 118.9(7) . . ? C3 C4 C5 118.0(6) . . ? C6 C5 C4 126.0(6) . . ? C6 C5 Pt1 72.2(3) . . ? C4 C5 Pt1 109.1(4) . . ? C5 C6 C7 125.5(6) . . ? C5 C6 Pt1 72.3(3) . . ? C7 C6 Pt1 109.1(4) . . ? C8 C7 C6 118.1(6) . . ? C7 C8 C2 118.6(6) . . ? C10 C9 Pt1 178.5(5) . . ? C9 C10 C11 176.5(6) . . ? C15 C11 C10 126.5(5) . . ? C15 C11 C12 106.9(5) . . ? C10 C11 C12 126.4(5) . . ? C15 C11 Fe1 68.9(3) . . ? C10 C11 Fe1 123.2(4) . . ? C12 C11 Fe1 69.3(3) . . ? C13 C12 C11 107.9(5) . . ? C13 C12 Fe1 69.4(3) . . ? C11 C12 Fe1 69.5(3) . . ? C14 C13 C12 108.1(6) . . ? C14 C13 Fe1 69.6(3) . . ? C12 C13 Fe1 69.6(3) . . ? C15 C14 C13 108.4(5) . . ? C15 C14 Fe1 69.5(3) . . ? C13 C14 Fe1 69.7(3) . . ? C14 C15 C11 108.7(6) . . ? C14 C15 Fe1 69.9(3) . . ? C11 C15 Fe1 69.9(3) . . ? C20 C16 C17 107.6(7) . . ? C20 C16 Fe1 69.2(4) . . ? C17 C16 Fe1 69.6(4) . . ? C18 C17 C16 108.3(7) . . ? C18 C17 Fe1 69.8(4) . . ? C16 C17 Fe1 69.8(4) . . ? C17 C18 C19 108.3(6) . . ? C17 C18 Fe1 70.1(4) . . ? C19 C18 Fe1 69.4(4) . . ? C18 C19 C20 107.7(7) . . ? C18 C19 Fe1 70.1(4) . . ? C20 C19 Fe1 69.5(4) . . ? C16 C20 C19 108.1(7) . . ? C16 C20 Fe1 70.4(4) . . ? C19 C20 Fe1 69.6(4) . . ? C22 C21 Pt1 173.7(5) . . ? C21 C22 C26 176.4(6) . . ? C24 C23 C27 108.4(6) . . ? C24 C23 Fe2 69.9(4) . . ? C27 C23 Fe2 69.3(3) . . ? C25 C24 C23 108.0(6) . . ? C25 C24 Fe2 69.5(3) . . ? C23 C24 Fe2 69.7(4) . . ? C24 C25 C26 108.9(6) . . ? C24 C25 Fe2 70.0(4) . . ? C26 C25 Fe2 70.1(3) . . ? C25 C26 C27 106.8(5) . . ? C25 C26 C22 126.6(6) . . ? C27 C26 C22 126.5(6) . . ? C25 C26 Fe2 69.0(3) . . ? C27 C26 Fe2 68.9(3) . . ? C22 C26 Fe2 129.1(4) . . ? C23 C27 C26 107.8(6) . . ? C23 C27 Fe2 69.7(4) . . ? C26 C27 Fe2 70.1(3) . . ? C32 C28 C29 108.3(8) . . ? C32 C28 Fe2 70.6(4) . . ? C29 C28 Fe2 69.3(5) . . ? C28 C29 C30 108.4(8) . . ? C28 C29 Fe2 70.5(5) . . ? C30 C29 Fe2 70.1(5) . . ? C31 C30 C29 106.4(8) . . ? C31 C30 Fe2 70.0(4) . . ? C29 C30 Fe2 68.8(4) . . ? C32 C31 C30 108.1(7) . . ? C32 C31 Fe2 70.0(4) . . ? C30 C31 Fe2 69.3(4) . . ? C28 C32 C31 108.9(8) . . ? C28 C32 Fe2 69.7(4) . . ? C31 C32 Fe2 70.0(4) . . ? Cl1 C100 Cl2 110.0(3) . . ? Cl1 C100 Cl3 110.0(3) . . ? Cl2 C100 Cl3 110.7(3) . . ? Cl5 C200 Cl6 110.4(4) . . ? Cl5 C200 Cl4 109.6(3) . . ? Cl6 C200 Cl4 110.7(4) . . ? C20 Fe1 C19 40.9(3) . . ? C20 Fe1 C15 122.1(3) . . ? C19 Fe1 C15 106.0(3) . . ? C20 Fe1 C18 68.2(3) . . ? C19 Fe1 C18 40.5(3) . . ? C15 Fe1 C18 121.7(3) . . ? C20 Fe1 C14 158.0(3) . . ? C19 Fe1 C14 121.7(3) . . ? C15 Fe1 C14 40.6(2) . . ? C18 Fe1 C14 107.2(3) . . ? C20 Fe1 C13 159.8(3) . . ? C19 Fe1 C13 158.3(3) . . ? C15 Fe1 C13 68.6(3) . . ? C18 Fe1 C13 123.1(3) . . ? C14 Fe1 C13 40.7(3) . . ? C20 Fe1 C17 68.1(3) . . ? C19 Fe1 C17 67.9(3) . . ? C15 Fe1 C17 158.1(3) . . ? C18 Fe1 C17 40.1(3) . . ? C14 Fe1 C17 123.2(3) . . ? C13 Fe1 C17 108.7(3) . . ? C20 Fe1 C16 40.4(3) . . ? C19 Fe1 C16 68.3(3) . . ? C15 Fe1 C16 158.8(3) . . ? C18 Fe1 C16 68.0(3) . . ? C14 Fe1 C16 159.8(3) . . ? C13 Fe1 C16 124.2(3) . . ? C17 Fe1 C16 40.6(3) . . ? C20 Fe1 C12 123.0(3) . . ? C19 Fe1 C12 158.7(3) . . ? C15 Fe1 C12 69.0(2) . . ? C18 Fe1 C12 159.7(3) . . ? C14 Fe1 C12 68.8(3) . . ? C13 Fe1 C12 41.0(2) . . ? C17 Fe1 C12 124.2(3) . . ? C16 Fe1 C12 108.5(3) . . ? C20 Fe1 C11 106.6(3) . . ? C19 Fe1 C11 121.5(3) . . ? C15 Fe1 C11 41.2(2) . . ? C18 Fe1 C11 157.7(3) . . ? C14 Fe1 C11 69.0(2) . . ? C13 Fe1 C11 69.2(2) . . ? C17 Fe1 C11 160.0(3) . . ? C16 Fe1 C11 123.0(3) . . ? C12 Fe1 C11 41.2(2) . . ? C29 Fe2 C28 40.2(4) . . ? C29 Fe2 C30 41.2(4) . . ? C28 Fe2 C30 68.4(4) . . ? C29 Fe2 C27 123.3(4) . . ? C28 Fe2 C27 159.1(3) . . ? C30 Fe2 C27 107.6(3) . . ? C29 Fe2 C25 122.9(3) . . ? C28 Fe2 C25 107.6(3) . . ? C30 Fe2 C25 159.7(4) . . ? C27 Fe2 C25 68.7(3) . . ? C29 Fe2 C31 68.2(3) . . ? C28 Fe2 C31 67.5(3) . . ? C30 Fe2 C31 40.6(4) . . ? C27 Fe2 C31 123.7(3) . . ? C25 Fe2 C31 157.9(3) . . ? C29 Fe2 C23 159.8(4) . . ? C28 Fe2 C23 158.5(4) . . ? C30 Fe2 C23 123.0(4) . . ? C27 Fe2 C23 40.9(3) . . ? C25 Fe2 C23 68.1(3) . . ? C31 Fe2 C23 108.2(3) . . ? C29 Fe2 C32 67.4(4) . . ? C28 Fe2 C32 39.7(3) . . ? C30 Fe2 C32 67.9(4) . . ? C27 Fe2 C32 159.7(3) . . ? C25 Fe2 C32 122.5(3) . . ? C31 Fe2 C32 40.0(3) . . ? C23 Fe2 C32 123.5(3) . . ? C29 Fe2 C24 158.5(4) . . ? C28 Fe2 C24 122.7(4) . . ? C30 Fe2 C24 158.6(4) . . ? C27 Fe2 C24 68.7(3) . . ? C25 Fe2 C24 40.4(2) . . ? C31 Fe2 C24 122.6(3) . . ? C23 Fe2 C24 40.4(3) . . ? C32 Fe2 C24 107.8(3) . . ? C29 Fe2 C26 107.5(3) . . ? C28 Fe2 C26 122.7(3) . . ? C30 Fe2 C26 123.2(3) . . ? C27 Fe2 C26 41.0(2) . . ? C25 Fe2 C26 40.9(2) . . ? C31 Fe2 C26 160.0(3) . . ? C23 Fe2 C26 68.7(2) . . ? C32 Fe2 C26 158.2(3) . . ? C24 Fe2 C26 68.7(2) . . ? C21 Pt1 C9 88.6(2) . . ? C21 Pt1 C1 159.2(3) . . ? C9 Pt1 C1 91.2(2) . . ? C21 Pt1 C2 164.9(2) . . ? C9 Pt1 C2 92.5(2) . . ? C1 Pt1 C2 35.8(2) . . ? C21 Pt1 C6 94.2(2) . . ? C9 Pt1 C6 162.6(2) . . ? C1 Pt1 C6 92.2(3) . . ? C2 Pt1 C6 80.4(2) . . ? C21 Pt1 C5 93.0(2) . . ? C9 Pt1 C5 161.6(2) . . ? C1 Pt1 C5 80.9(2) . . ? C2 Pt1 C5 90.7(2) . . ? C6 Pt1 C5 35.5(2) . . ? #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 685382' _audit_creation_date 2007-07-13T17:49:18-00:00 _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 s99 _chemical_formula_sum 'C58 H46 Fe3 P2 Pt' _chemical_formula_weight 1167.53 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.04220(10) _cell_length_b 18.2488(5) _cell_length_c 25.2322(7) _cell_angle_alpha 90 _cell_angle_beta 98.312(2) _cell_angle_gamma 90 _cell_volume 4575.43(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 7778 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.09 _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 0.5281 _exptl_absorpt_correction_T_max 0.627 #----------------------------------------------------------------------------# # 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 -0.091341 _diffrn_orient_matrix_ub_12 0.0028272 _diffrn_orient_matrix_ub_13 -0.0217654 _diffrn_orient_matrix_ub_21 0.0204607 _diffrn_orient_matrix_ub_22 -0.0446175 _diffrn_orient_matrix_ub_23 -0.0203745 _diffrn_orient_matrix_ub_31 -0.0369588 _diffrn_orient_matrix_ub_32 -0.0316878 _diffrn_orient_matrix_ub_33 0.0267461 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_number 74239 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10405 _reflns_number_gt 8005 _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^)+(0.0078P)^2^+17.9801P] 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 10405 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.074 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.769 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.159 #----------------------------------------------------------------------------# # 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' 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 0.2903(4) 0.1837(3) 0.09570(17) 0.0148(10) Uani 1 1 d . . . C2 C 0.3411(5) 0.1105(3) 0.10025(18) 0.0206(11) Uani 1 1 d . . . H2 H 0.2949 0.0693 0.1093 0.025 Uiso 1 1 calc R . . C3 C 0.4750(5) 0.1122(3) 0.0885(2) 0.0247(12) Uani 1 1 d . . . H3 H 0.5315 0.0718 0.0885 0.03 Uiso 1 1 calc R . . C4 C 0.5090(5) 0.1847(3) 0.07685(18) 0.0225(11) Uani 1 1 d . . . H4 H 0.5912 0.2004 0.0681 0.027 Uiso 1 1 calc R . . C5 C 0.3954(4) 0.2296(3) 0.08090(17) 0.0163(10) Uani 1 1 d . . . H5 H 0.39 0.2799 0.075 0.02 Uiso 1 1 calc R . . C6 C 0.3944(4) 0.1692(3) 0.22453(17) 0.0162(10) Uani 1 1 d . . . C7 C 0.5083(5) 0.1227(3) 0.22266(19) 0.0231(11) Uani 1 1 d . . . H7 H 0.5101 0.0722 0.2276 0.028 Uiso 1 1 calc R . . C8 C 0.6176(5) 0.1665(3) 0.21204(19) 0.0281(13) Uani 1 1 d . . . H8 H 0.7031 0.1496 0.2083 0.034 Uiso 1 1 calc R . . C9 C 0.5749(5) 0.2401(3) 0.20819(18) 0.0274(13) Uani 1 1 d . . . H9 H 0.6275 0.2801 0.2016 0.033 Uiso 1 1 calc R . . C10 C 0.4387(5) 0.2428(3) 0.21598(18) 0.0185(10) Uani 1 1 d . . . H10 H 0.3864 0.2849 0.2157 0.022 Uiso 1 1 calc R . . C11 C 0.0165(4) 0.1602(3) 0.05650(18) 0.0169(10) Uani 1 1 d . . . C12 C -0.1154(5) 0.1454(3) 0.0628(2) 0.0228(11) Uani 1 1 d . . . H12 H -0.1503 0.1628 0.0927 0.027 Uiso 1 1 calc R . . C13 C -0.1952(5) 0.1045(3) 0.0241(2) 0.0317(13) Uani 1 1 d . . . H13 H -0.2841 0.0947 0.0282 0.038 Uiso 1 1 calc R . . C14 C -0.1458(5) 0.0782(3) -0.0200(2) 0.0307(13) Uani 1 1 d . . . H14 H -0.2006 0.0508 -0.0456 0.037 Uiso 1 1 calc R . . C15 C -0.0152(5) 0.0924(3) -0.0263(2) 0.0295(13) Uani 1 1 d . . . H15 H 0.0191 0.0745 -0.0561 0.035 Uiso 1 1 calc R . . C16 C 0.0664(5) 0.1336(3) 0.01186(19) 0.0237(12) Uani 1 1 d . . . H16 H 0.155 0.1433 0.0074 0.028 Uiso 1 1 calc R . . C17 C 0.1263(4) 0.3079(3) 0.08060(19) 0.0164(10) Uani 1 1 d . . . C18 C 0.1699(5) 0.3641(3) 0.1162(2) 0.0220(11) Uani 1 1 d . . . H18 H 0.1915 0.354 0.1526 0.026 Uiso 1 1 calc R . . C19 C 0.1811(5) 0.4347(3) 0.0980(2) 0.0287(12) Uani 1 1 d . . . H19 H 0.2122 0.4719 0.1218 0.034 Uiso 1 1 calc R . . C20 C 0.1463(5) 0.4500(3) 0.0444(2) 0.0317(13) Uani 1 1 d . . . H20 H 0.1522 0.4979 0.0323 0.038 Uiso 1 1 calc R . . C21 C 0.1031(5) 0.3957(3) 0.0087(2) 0.0323(13) Uani 1 1 d . . . H21 H 0.081 0.4065 -0.0275 0.039 Uiso 1 1 calc R . . C22 C 0.0922(5) 0.3243(3) 0.02667(19) 0.0233(11) Uani 1 1 d . . . H22 H 0.062 0.2874 0.0025 0.028 Uiso 1 1 calc R . . C23 C 0.2451(5) 0.1491(3) 0.30948(18) 0.0178(10) Uani 1 1 d . . . C24 C 0.3462(5) 0.1886(3) 0.3397(2) 0.0345(14) Uani 1 1 d . . . H24 H 0.4101 0.2126 0.3229 0.041 Uiso 1 1 calc R . . C25 C 0.3534(6) 0.1926(4) 0.3948(2) 0.0454(18) Uani 1 1 d . . . H25 H 0.4224 0.2193 0.4145 0.054 Uiso 1 1 calc R . . C26 C 0.2603(6) 0.1579(3) 0.4207(2) 0.0348(14) Uani 1 1 d . . . H26 H 0.2642 0.1622 0.4577 0.042 Uiso 1 1 calc R . . C27 C 0.1610(5) 0.1166(3) 0.3914(2) 0.0257(12) Uani 1 1 d . . . H27 H 0.0989 0.0916 0.4087 0.031 Uiso 1 1 calc R . . C28 C 0.1535(5) 0.1124(3) 0.3367(2) 0.0230(11) Uani 1 1 d . . . H28 H 0.0858 0.0845 0.3173 0.028 Uiso 1 1 calc R . . C29 C 0.2009(5) 0.0498(3) 0.22204(18) 0.0190(10) Uani 1 1 d . . . C30 C 0.2890(5) -0.0031(3) 0.2468(2) 0.0246(12) Uani 1 1 d . . . H30 H 0.3615 0.0111 0.2719 0.03 Uiso 1 1 calc R . . C31 C 0.2695(6) -0.0769(3) 0.2343(2) 0.0332(14) Uani 1 1 d . . . H31 H 0.3302 -0.1117 0.2501 0.04 Uiso 1 1 calc R . . C32 C 0.1592(7) -0.0981(3) 0.1982(2) 0.0429(16) Uani 1 1 d . . . H32 H 0.1462 -0.1473 0.1895 0.051 Uiso 1 1 calc R . . C33 C 0.0693(7) -0.0470(3) 0.1752(2) 0.0406(15) Uani 1 1 d . . . H33 H -0.0068 -0.0619 0.1523 0.049 Uiso 1 1 calc R . . C34 C 0.0910(5) 0.0272(3) 0.1860(2) 0.0292(12) Uani 1 1 d . . . H34 H 0.0317 0.0618 0.1689 0.035 Uiso 1 1 calc R . . C35 C -0.0969(4) 0.2781(3) 0.15315(17) 0.0171(10) Uani 1 1 d . . . C36 C -0.1809(5) 0.3152(3) 0.1297(2) 0.0224(11) Uani 1 1 d . . . C37 C -0.2731(5) 0.3679(3) 0.10185(19) 0.0210(11) Uani 1 1 d . . . C38 C -0.2408(5) 0.4192(3) 0.06247(19) 0.0267(12) Uani 1 1 d . . . H38 H -0.1603 0.4209 0.0483 0.032 Uiso 1 1 calc R . . C39 C -0.3515(5) 0.4667(3) 0.0488(2) 0.0302(13) Uani 1 1 d . . . H39 H -0.3564 0.505 0.0243 0.036 Uiso 1 1 calc R . . C40 C -0.4535(5) 0.4460(3) 0.0791(2) 0.0292(13) Uani 1 1 d . . . H40 H -0.5375 0.468 0.0776 0.035 Uiso 1 1 calc R . . C41 C -0.4063(5) 0.3864(3) 0.1118(2) 0.0265(12) Uani 1 1 d . . . H41 H -0.4535 0.3628 0.1359 0.032 Uiso 1 1 calc R . . C42 C -0.1863(7) 0.5723(4) 0.1473(3) 0.0555(19) Uani 1 1 d . . . H42 H -0.175 0.6101 0.1237 0.067 Uiso 1 1 calc R . . C43 C -0.2941(6) 0.5649(3) 0.1750(3) 0.0426(16) Uani 1 1 d . . . H43 H -0.3662 0.5973 0.1726 0.051 Uiso 1 1 calc R . . C44 C -0.2807(8) 0.5037(4) 0.2064(2) 0.0540(19) Uani 1 1 d . . . H44 H -0.3396 0.4867 0.2289 0.065 Uiso 1 1 calc R . . C45 C -0.1526(10) 0.4704(4) 0.1968(3) 0.082(3) Uani 1 1 d . . . H45 H -0.1133 0.4277 0.212 0.098 Uiso 1 1 calc R . . C46 C -0.1019(7) 0.5177(5) 0.1592(4) 0.071(3) Uani 1 1 d . . . H46 H -0.0218 0.511 0.1453 0.085 Uiso 1 1 calc R . . C47 C -0.0256(4) 0.2339(2) 0.25775(19) 0.0175(10) Uani 1 1 d . . . C48 C -0.0826(5) 0.2463(3) 0.2948(2) 0.0243(11) Uani 1 1 d . . . C49 C -0.1558(5) 0.2577(3) 0.3391(2) 0.0265(12) Uani 1 1 d . . . C50 C -0.1075(6) 0.2418(3) 0.3942(2) 0.0367(14) Uani 1 1 d . . . H50 H -0.0232 0.2232 0.4078 0.044 Uiso 1 1 calc R . . C51 C -0.2123(7) 0.2599(3) 0.4244(2) 0.0391(16) Uani 1 1 d . . . H51 H -0.2087 0.2545 0.4612 0.047 Uiso 1 1 calc R . . C52 C -0.3221(6) 0.2871(3) 0.3891(2) 0.0349(14) Uani 1 1 d . . . H52 H -0.4031 0.3033 0.3988 0.042 Uiso 1 1 calc R . . C53 C -0.2894(5) 0.2861(3) 0.3367(2) 0.0310(13) Uani 1 1 d . . . H53 H -0.3449 0.3012 0.3059 0.037 Uiso 1 1 calc R . . C54 C -0.0780(10) 0.4247(4) 0.4401(3) 0.065(2) Uani 1 1 d . . . H54 H -0.0662 0.4181 0.477 0.078 Uiso 1 1 calc R . . C55 C -0.1890(7) 0.4538(3) 0.4092(3) 0.057(2) Uani 1 1 d . . . H55 H -0.2663 0.4703 0.4218 0.068 Uiso 1 1 calc R . . C56 C -0.1669(8) 0.4547(4) 0.3564(3) 0.057(2) Uani 1 1 d . . . H56 H -0.2258 0.4722 0.3274 0.068 Uiso 1 1 calc R . . C57 C -0.0429(9) 0.4252(4) 0.3548(3) 0.065(2) Uani 1 1 d . . . H57 H -0.0036 0.4188 0.324 0.078 Uiso 1 1 calc R . . C58 C 0.0148(7) 0.4066(4) 0.4052(5) 0.075(3) Uani 1 1 d . . . H58 H 0.0995 0.3858 0.4148 0.09 Uiso 1 1 calc R . . Fe1 Fe 0.45432(6) 0.17773(4) 0.15241(3) 0.01619(15) Uani 1 1 d . . . Fe2 Fe -0.28022(7) 0.47303(4) 0.12877(3) 0.02483(17) Uani 1 1 d . . . Fe3 Fe -0.15697(7) 0.35009(4) 0.38551(3) 0.02155(16) Uani 1 1 d . . . P1 P 0.12479(11) 0.21443(7) 0.10705(4) 0.0134(2) Uani 1 1 d . . . P2 P 0.22654(12) 0.14726(7) 0.23661(5) 0.0149(3) Uani 1 1 d . . . Pt1 Pt 0.057065(17) 0.217454(10) 0.190606(7) 0.01356(5) 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 0.013(2) 0.020(3) 0.011(2) -0.0015(19) 0.0011(18) 0.0025(19) C2 0.026(3) 0.016(3) 0.019(3) -0.005(2) -0.001(2) -0.002(2) C3 0.025(3) 0.024(3) 0.027(3) -0.003(2) 0.009(2) 0.009(2) C4 0.018(3) 0.038(3) 0.012(2) -0.003(2) 0.005(2) 0.000(2) C5 0.018(2) 0.019(3) 0.011(2) 0.0042(19) 0.0002(18) 0.0025(19) C6 0.013(2) 0.023(3) 0.012(2) 0.003(2) -0.0003(18) -0.0011(19) C7 0.017(3) 0.033(3) 0.020(3) 0.010(2) 0.001(2) 0.007(2) C8 0.013(3) 0.053(4) 0.017(3) 0.012(3) -0.005(2) 0.003(2) C9 0.026(3) 0.044(4) 0.010(2) 0.001(2) -0.005(2) -0.016(2) C10 0.024(3) 0.018(3) 0.013(2) -0.0007(19) 0.000(2) -0.001(2) C11 0.017(2) 0.019(3) 0.013(2) 0.001(2) -0.0024(19) 0.002(2) C12 0.019(3) 0.027(3) 0.023(3) -0.007(2) 0.003(2) -0.004(2) C13 0.014(3) 0.039(3) 0.043(3) -0.007(3) 0.007(2) -0.004(2) C14 0.025(3) 0.032(3) 0.032(3) -0.011(3) -0.005(2) -0.002(2) C15 0.035(3) 0.034(3) 0.019(3) -0.010(2) 0.001(2) 0.001(3) C16 0.017(3) 0.032(3) 0.022(3) 0.001(2) 0.002(2) 0.000(2) C17 0.008(2) 0.015(2) 0.027(3) 0.005(2) 0.0046(19) 0.0012(18) C18 0.019(3) 0.028(3) 0.020(3) 0.002(2) 0.002(2) -0.001(2) C19 0.031(3) 0.019(3) 0.036(3) 0.001(2) 0.006(2) -0.002(2) C20 0.033(3) 0.020(3) 0.045(4) 0.015(3) 0.014(3) 0.004(2) C21 0.036(3) 0.035(4) 0.027(3) 0.013(3) 0.007(2) 0.004(3) C22 0.027(3) 0.024(3) 0.017(3) 0.002(2) -0.003(2) 0.002(2) C23 0.018(2) 0.023(3) 0.011(2) 0.002(2) -0.0024(19) 0.004(2) C24 0.032(3) 0.047(4) 0.023(3) 0.009(3) 0.001(2) -0.016(3) C25 0.047(4) 0.072(5) 0.014(3) 0.000(3) -0.006(3) -0.033(3) C26 0.048(4) 0.042(4) 0.015(3) 0.007(3) 0.006(3) -0.003(3) C27 0.032(3) 0.022(3) 0.025(3) 0.006(2) 0.013(2) 0.001(2) C28 0.021(3) 0.023(3) 0.025(3) 0.000(2) 0.005(2) -0.005(2) C29 0.020(3) 0.022(3) 0.016(2) 0.002(2) 0.007(2) -0.001(2) C30 0.022(3) 0.028(3) 0.025(3) 0.005(2) 0.004(2) 0.001(2) C31 0.048(4) 0.017(3) 0.037(3) 0.009(2) 0.015(3) 0.011(3) C32 0.080(5) 0.021(3) 0.029(3) -0.009(3) 0.013(3) -0.005(3) C33 0.059(4) 0.030(3) 0.029(3) 0.001(3) -0.007(3) -0.015(3) C34 0.036(3) 0.025(3) 0.025(3) 0.001(2) 0.001(2) -0.001(2) C35 0.013(2) 0.024(3) 0.014(2) 0.004(2) -0.0002(18) 0.006(2) C36 0.024(3) 0.020(3) 0.024(3) -0.003(2) 0.006(2) -0.003(2) C37 0.025(3) 0.019(3) 0.019(3) -0.002(2) 0.003(2) 0.004(2) C38 0.028(3) 0.031(3) 0.020(3) 0.001(2) -0.002(2) 0.002(2) C39 0.035(3) 0.027(3) 0.025(3) 0.008(2) -0.006(2) 0.002(2) C40 0.017(3) 0.024(3) 0.042(3) 0.000(3) -0.010(2) 0.006(2) C41 0.018(3) 0.023(3) 0.037(3) -0.002(2) -0.001(2) -0.001(2) C42 0.044(4) 0.053(5) 0.070(5) -0.024(4) 0.008(4) -0.021(4) C43 0.039(4) 0.036(4) 0.051(4) -0.019(3) 0.003(3) 0.002(3) C44 0.085(6) 0.052(5) 0.025(3) -0.012(3) 0.007(3) -0.020(4) C45 0.129(8) 0.032(4) 0.059(5) -0.029(4) -0.073(5) 0.036(5) C46 0.024(4) 0.099(7) 0.082(6) -0.060(6) -0.015(4) 0.006(4) C47 0.017(2) 0.015(3) 0.021(3) 0.004(2) 0.004(2) 0.0038(18) C48 0.030(3) 0.020(3) 0.023(3) 0.000(2) 0.001(2) -0.001(2) C49 0.033(3) 0.026(3) 0.023(3) -0.002(2) 0.014(2) -0.004(2) C50 0.053(4) 0.029(3) 0.032(3) -0.001(3) 0.016(3) 0.011(3) C51 0.073(5) 0.020(3) 0.031(3) 0.000(2) 0.032(3) -0.007(3) C52 0.035(3) 0.032(3) 0.043(3) -0.016(3) 0.025(3) -0.014(3) C53 0.027(3) 0.036(3) 0.032(3) -0.016(3) 0.008(2) -0.015(3) C54 0.121(7) 0.048(5) 0.018(3) -0.015(3) -0.012(4) -0.042(5) C55 0.054(4) 0.028(4) 0.100(6) -0.028(4) 0.047(5) -0.015(3) C56 0.081(6) 0.030(4) 0.053(5) 0.014(3) -0.010(4) -0.021(4) C57 0.081(6) 0.053(5) 0.074(6) -0.028(4) 0.055(5) -0.041(4) C58 0.029(4) 0.042(5) 0.142(9) -0.018(5) -0.031(5) -0.008(3) Fe1 0.0125(3) 0.0208(4) 0.0150(3) 0.0025(3) 0.0013(3) 0.0019(3) Fe2 0.0203(4) 0.0233(4) 0.0289(4) -0.0054(3) -0.0034(3) 0.0044(3) Fe3 0.0229(4) 0.0250(4) 0.0176(4) -0.0028(3) 0.0056(3) -0.0036(3) P1 0.0124(5) 0.0158(6) 0.0120(5) 0.0014(5) 0.0022(4) 0.0021(5) P2 0.0139(6) 0.0166(6) 0.0139(6) 0.0031(5) 0.0014(5) 0.0007(5) Pt1 0.01289(9) 0.01563(9) 0.01250(8) 0.00220(8) 0.00303(6) 0.00336(8) #----------------------------------------------------------------------------# # 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 1.429(6) . ? C1 C5 1.438(6) . ? C1 P1 1.816(4) . ? C1 Fe1 2.023(4) . ? C2 C3 1.419(7) . ? C2 Fe1 2.024(5) . ? C3 C4 1.407(7) . ? C3 Fe1 2.042(5) . ? C4 C5 1.419(6) . ? C4 Fe1 2.063(5) . ? C5 Fe1 2.047(4) . ? C6 C7 1.430(6) . ? C6 C10 1.440(7) . ? C6 P2 1.801(4) . ? C6 Fe1 2.003(4) . ? C7 C8 1.414(7) . ? C7 Fe1 2.041(5) . ? C8 C9 1.409(8) . ? C8 Fe1 2.069(5) . ? C9 C10 1.411(7) . ? C9 Fe1 2.062(5) . ? C10 Fe1 2.020(5) . ? C11 C12 1.383(6) . ? C11 C16 1.386(6) . ? C11 P1 1.841(5) . ? C12 C13 1.389(7) . ? C13 C14 1.371(7) . ? C14 C15 1.368(7) . ? C15 C16 1.390(7) . ? C17 C22 1.387(6) . ? C17 C18 1.393(7) . ? C17 P1 1.832(5) . ? C18 C19 1.378(7) . ? C19 C20 1.375(7) . ? C20 C21 1.367(8) . ? C21 C22 1.389(7) . ? C23 C24 1.381(7) . ? C23 C28 1.396(6) . ? C23 P2 1.822(5) . ? C24 C25 1.383(7) . ? C25 C26 1.372(7) . ? C26 C27 1.376(7) . ? C27 C28 1.374(7) . ? C29 C34 1.387(7) . ? C29 C30 1.396(7) . ? C29 P2 1.827(5) . ? C30 C31 1.389(7) . ? C31 C32 1.384(8) . ? C32 C33 1.367(8) . ? C33 C34 1.392(8) . ? C35 C36 1.174(6) . ? C35 Pt1 2.021(4) . ? C36 C37 1.445(7) . ? C37 C41 1.436(7) . ? C37 C38 1.436(7) . ? C37 Fe2 2.040(5) . ? C38 C39 1.413(7) . ? C38 Fe2 2.027(5) . ? C39 C40 1.415(7) . ? C39 Fe2 2.044(5) . ? C40 C41 1.406(7) . ? C40 Fe2 2.053(5) . ? C41 Fe2 2.032(5) . ? C42 C46 1.313(10) . ? C42 C43 1.377(9) . ? C42 Fe2 2.064(7) . ? C43 C44 1.365(9) . ? C43 Fe2 2.059(6) . ? C44 C45 1.473(11) . ? C44 Fe2 2.037(6) . ? C45 C46 1.432(12) . ? C45 Fe2 1.989(6) . ? C46 Fe2 2.016(7) . ? C47 C48 1.187(6) . ? C47 Pt1 2.014(5) . ? C48 C49 1.438(7) . ? C49 C53 1.432(7) . ? C49 C50 1.436(7) . ? C49 Fe3 2.055(5) . ? C50 C51 1.424(7) . ? C50 Fe3 2.042(6) . ? C51 C52 1.404(8) . ? C51 Fe3 2.035(5) . ? C52 C53 1.409(7) . ? C52 Fe3 2.030(5) . ? C53 Fe3 2.044(5) . ? C54 C55 1.371(10) . ? C54 C58 1.411(11) . ? C54 Fe3 2.015(6) . ? C55 C56 1.382(10) . ? C55 Fe3 2.025(6) . ? C56 C57 1.363(10) . ? C56 Fe3 2.043(6) . ? C57 C58 1.362(11) . ? C57 Fe3 2.012(6) . ? C58 Fe3 2.009(6) . ? P1 Pt1 2.3075(11) . ? P2 Pt1 2.3051(12) . ? 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 C5 107.3(4) . . ? C2 C1 P1 126.9(4) . . ? C5 C1 P1 125.8(4) . . ? C2 C1 Fe1 69.4(3) . . ? C5 C1 Fe1 70.2(2) . . ? P1 C1 Fe1 125.1(2) . . ? C3 C2 C1 107.5(4) . . ? C3 C2 Fe1 70.3(3) . . ? C1 C2 Fe1 69.3(3) . . ? C4 C3 C2 109.3(4) . . ? C4 C3 Fe1 70.8(3) . . ? C2 C3 Fe1 68.9(3) . . ? C3 C4 C5 107.8(4) . . ? C3 C4 Fe1 69.1(3) . . ? C5 C4 Fe1 69.2(2) . . ? C4 C5 C1 108.1(4) . . ? C4 C5 Fe1 70.4(3) . . ? C1 C5 Fe1 68.4(2) . . ? C7 C6 C10 106.4(4) . . ? C7 C6 P2 130.2(4) . . ? C10 C6 P2 123.3(4) . . ? C7 C6 Fe1 70.7(3) . . ? C10 C6 Fe1 69.6(2) . . ? P2 C6 Fe1 125.6(2) . . ? C8 C7 C6 108.5(5) . . ? C8 C7 Fe1 71.0(3) . . ? C6 C7 Fe1 67.9(3) . . ? C9 C8 C7 108.3(4) . . ? C9 C8 Fe1 69.8(3) . . ? C7 C8 Fe1 68.8(3) . . ? C8 C9 C10 108.4(4) . . ? C8 C9 Fe1 70.3(3) . . ? C10 C9 Fe1 68.2(3) . . ? C9 C10 C6 108.4(4) . . ? C9 C10 Fe1 71.4(3) . . ? C6 C10 Fe1 68.4(3) . . ? C12 C11 C16 119.4(4) . . ? C12 C11 P1 120.3(4) . . ? C16 C11 P1 120.3(4) . . ? C11 C12 C13 119.2(5) . . ? C14 C13 C12 121.3(5) . . ? C15 C14 C13 119.6(5) . . ? C14 C15 C16 120.1(5) . . ? C11 C16 C15 120.4(5) . . ? C22 C17 C18 119.0(4) . . ? C22 C17 P1 123.0(4) . . ? C18 C17 P1 118.0(4) . . ? C19 C18 C17 120.4(5) . . ? C20 C19 C18 119.8(5) . . ? C21 C20 C19 120.7(5) . . ? C20 C21 C22 119.9(5) . . ? C17 C22 C21 120.2(5) . . ? C24 C23 C28 117.5(4) . . ? C24 C23 P2 121.8(4) . . ? C28 C23 P2 120.6(4) . . ? C23 C24 C25 120.7(5) . . ? C26 C25 C24 121.0(5) . . ? C25 C26 C27 119.2(5) . . ? C28 C27 C26 120.0(5) . . ? C27 C28 C23 121.5(5) . . ? C34 C29 C30 118.8(5) . . ? C34 C29 P2 119.8(4) . . ? C30 C29 P2 121.5(4) . . ? C31 C30 C29 120.6(5) . . ? C32 C31 C30 119.6(5) . . ? C33 C32 C31 120.3(5) . . ? C32 C33 C34 120.4(6) . . ? C29 C34 C33 120.3(5) . . ? C36 C35 Pt1 176.0(4) . . ? C35 C36 C37 173.3(5) . . ? C41 C37 C38 106.1(4) . . ? C41 C37 C36 128.2(5) . . ? C38 C37 C36 125.2(4) . . ? C41 C37 Fe2 69.1(3) . . ? C38 C37 Fe2 68.9(3) . . ? C36 C37 Fe2 121.0(3) . . ? C39 C38 C37 108.7(5) . . ? C39 C38 Fe2 70.3(3) . . ? C37 C38 Fe2 69.8(3) . . ? C38 C39 C40 108.1(5) . . ? C38 C39 Fe2 69.1(3) . . ? C40 C39 Fe2 70.2(3) . . ? C41 C40 C39 108.3(5) . . ? C41 C40 Fe2 69.1(3) . . ? C39 C40 Fe2 69.4(3) . . ? C40 C41 C37 108.8(5) . . ? C40 C41 Fe2 70.7(3) . . ? C37 C41 Fe2 69.6(3) . . ? C46 C42 C43 109.9(8) . . ? C46 C42 Fe2 69.3(4) . . ? C43 C42 Fe2 70.3(4) . . ? C44 C43 C42 110.8(6) . . ? C44 C43 Fe2 69.7(4) . . ? C42 C43 Fe2 70.7(4) . . ? C43 C44 C45 105.0(6) . . ? C43 C44 Fe2 71.4(4) . . ? C45 C44 Fe2 66.8(4) . . ? C46 C45 C44 105.2(6) . . ? C46 C45 Fe2 70.1(4) . . ? C44 C45 Fe2 70.3(4) . . ? C42 C46 C45 109.2(7) . . ? C42 C46 Fe2 73.2(4) . . ? C45 C46 Fe2 68.0(4) . . ? C48 C47 Pt1 174.8(4) . . ? C47 C48 C49 176.8(6) . . ? C53 C49 C50 107.3(4) . . ? C53 C49 C48 126.9(5) . . ? C50 C49 C48 125.8(5) . . ? C53 C49 Fe3 69.1(3) . . ? C50 C49 Fe3 69.0(3) . . ? C48 C49 Fe3 127.4(4) . . ? C51 C50 C49 107.4(5) . . ? C51 C50 Fe3 69.3(3) . . ? C49 C50 Fe3 70.0(3) . . ? C52 C51 C50 108.5(5) . . ? C52 C51 Fe3 69.6(3) . . ? C50 C51 Fe3 69.8(3) . . ? C51 C52 C53 108.8(5) . . ? C51 C52 Fe3 70.0(3) . . ? C53 C52 Fe3 70.3(3) . . ? C52 C53 C49 108.0(5) . . ? C52 C53 Fe3 69.2(3) . . ? C49 C53 Fe3 70.0(3) . . ? C55 C54 C58 107.1(6) . . ? C55 C54 Fe3 70.6(4) . . ? C58 C54 Fe3 69.3(4) . . ? C54 C55 C56 108.7(6) . . ? C54 C55 Fe3 69.8(4) . . ? C56 C55 Fe3 70.8(4) . . ? C57 C56 C55 107.4(7) . . ? C57 C56 Fe3 69.1(4) . . ? C55 C56 Fe3 69.5(4) . . ? C58 C57 C56 109.8(7) . . ? C58 C57 Fe3 70.1(4) . . ? C56 C57 Fe3 71.6(4) . . ? C57 C58 C54 107.0(7) . . ? C57 C58 Fe3 70.3(4) . . ? C54 C58 Fe3 69.7(4) . . ? C6 Fe1 C10 41.94(19) . . ? C6 Fe1 C1 109.03(18) . . ? C10 Fe1 C1 112.40(19) . . ? C6 Fe1 C2 109.25(19) . . ? C10 Fe1 C2 140.52(19) . . ? C1 Fe1 C2 41.36(18) . . ? C6 Fe1 C7 41.40(18) . . ? C10 Fe1 C7 68.9(2) . . ? C1 Fe1 C7 136.71(19) . . ? C2 Fe1 C7 108.7(2) . . ? C6 Fe1 C3 138.6(2) . . ? C10 Fe1 C3 178.6(2) . . ? C1 Fe1 C3 68.81(19) . . ? C2 Fe1 C3 40.84(19) . . ? C7 Fe1 C3 110.7(2) . . ? C6 Fe1 C5 138.58(18) . . ? C10 Fe1 C5 112.49(19) . . ? C1 Fe1 C5 41.38(18) . . ? C2 Fe1 C5 69.11(19) . . ? C7 Fe1 C5 177.8(2) . . ? C3 Fe1 C5 67.90(19) . . ? C6 Fe1 C9 69.29(19) . . ? C10 Fe1 C9 40.42(19) . . ? C1 Fe1 C9 142.3(2) . . ? C2 Fe1 C9 176.2(2) . . ? C7 Fe1 C9 67.8(2) . . ? C3 Fe1 C9 138.2(2) . . ? C5 Fe1 C9 114.4(2) . . ? C6 Fe1 C4 177.77(19) . . ? C10 Fe1 C4 139.4(2) . . ? C1 Fe1 C4 68.96(18) . . ? C2 Fe1 C4 68.6(2) . . ? C7 Fe1 C4 139.5(2) . . ? C3 Fe1 C4 40.1(2) . . ? C5 Fe1 C4 40.40(18) . . ? C9 Fe1 C4 112.9(2) . . ? C6 Fe1 C8 69.04(18) . . ? C10 Fe1 C8 68.0(2) . . ? C1 Fe1 C8 176.9(2) . . ? C2 Fe1 C8 136.4(2) . . ? C7 Fe1 C8 40.24(19) . . ? C3 Fe1 C8 110.8(2) . . ? C5 Fe1 C8 141.64(19) . . ? C9 Fe1 C8 39.9(2) . . ? C4 Fe1 C8 112.92(19) . . ? C45 Fe2 C46 41.9(3) . . ? C45 Fe2 C38 121.5(3) . . ? C46 Fe2 C38 104.0(3) . . ? C45 Fe2 C41 117.8(3) . . ? C46 Fe2 C41 152.5(3) . . ? C38 Fe2 C41 68.9(2) . . ? C45 Fe2 C44 42.9(3) . . ? C46 Fe2 C44 69.4(3) . . ? C38 Fe2 C44 162.5(3) . . ? C41 Fe2 C44 109.2(3) . . ? C45 Fe2 C37 102.4(2) . . ? C46 Fe2 C37 115.8(3) . . ? C38 Fe2 C37 41.4(2) . . ? C41 Fe2 C37 41.29(19) . . ? C44 Fe2 C37 125.7(3) . . ? C45 Fe2 C39 160.2(4) . . ? C46 Fe2 C39 124.3(3) . . ? C38 Fe2 C39 40.6(2) . . ? C41 Fe2 C39 68.3(2) . . ? C44 Fe2 C39 156.2(3) . . ? C37 Fe2 C39 69.1(2) . . ? C45 Fe2 C40 154.8(4) . . ? C46 Fe2 C40 163.3(3) . . ? C38 Fe2 C40 68.2(2) . . ? C41 Fe2 C40 40.3(2) . . ? C44 Fe2 C40 122.3(3) . . ? C37 Fe2 C40 68.8(2) . . ? C39 Fe2 C40 40.4(2) . . ? C45 Fe2 C43 67.6(3) . . ? C46 Fe2 C43 65.4(3) . . ? C38 Fe2 C43 154.0(2) . . ? C41 Fe2 C43 131.5(2) . . ? C44 Fe2 C43 38.9(3) . . ? C37 Fe2 C43 164.4(2) . . ? C39 Fe2 C43 124.2(2) . . ? C40 Fe2 C43 114.9(2) . . ? C45 Fe2 C42 67.0(3) . . ? C46 Fe2 C42 37.5(3) . . ? C38 Fe2 C42 118.3(3) . . ? C41 Fe2 C42 168.7(3) . . ? C44 Fe2 C42 66.8(3) . . ? C37 Fe2 C42 149.8(2) . . ? C39 Fe2 C42 110.9(3) . . ? C40 Fe2 C42 132.0(3) . . ? C43 Fe2 C42 39.0(2) . . ? C58 Fe3 C57 39.6(3) . . ? C58 Fe3 C54 41.0(3) . . ? C57 Fe3 C54 67.2(3) . . ? C58 Fe3 C55 67.3(3) . . ? C57 Fe3 C55 66.4(3) . . ? C54 Fe3 C55 39.7(3) . . ? C58 Fe3 C52 163.1(4) . . ? C57 Fe3 C52 156.5(3) . . ? C54 Fe3 C52 126.5(3) . . ? C55 Fe3 C52 110.5(2) . . ? C58 Fe3 C51 125.5(3) . . ? C57 Fe3 C51 161.3(4) . . ? C54 Fe3 C51 109.0(3) . . ? C55 Fe3 C51 123.2(3) . . ? C52 Fe3 C51 40.4(2) . . ? C58 Fe3 C50 106.4(3) . . ? C57 Fe3 C50 123.9(3) . . ? C54 Fe3 C50 121.0(3) . . ? C55 Fe3 C50 156.9(3) . . ? C52 Fe3 C50 68.6(2) . . ? C51 Fe3 C50 40.9(2) . . ? C58 Fe3 C56 66.7(3) . . ? C57 Fe3 C56 39.3(3) . . ? C54 Fe3 C56 66.9(3) . . ? C55 Fe3 C56 39.7(3) . . ? C52 Fe3 C56 123.2(3) . . ? C51 Fe3 C56 158.0(3) . . ? C50 Fe3 C56 160.4(3) . . ? C58 Fe3 C53 154.5(4) . . ? C57 Fe3 C53 121.0(3) . . ? C54 Fe3 C53 162.8(3) . . ? C55 Fe3 C53 126.5(3) . . ? C52 Fe3 C53 40.5(2) . . ? C51 Fe3 C53 68.2(2) . . ? C50 Fe3 C53 68.8(3) . . ? C56 Fe3 C53 108.9(3) . . ? C58 Fe3 C49 119.1(3) . . ? C57 Fe3 C49 106.8(2) . . ? C54 Fe3 C49 155.5(3) . . ? C55 Fe3 C49 161.8(3) . . ? C52 Fe3 C49 68.5(2) . . ? C51 Fe3 C49 68.6(2) . . ? C50 Fe3 C49 41.0(2) . . ? C56 Fe3 C49 124.5(3) . . ? C53 Fe3 C49 40.9(2) . . ? C1 P1 C17 100.0(2) . . ? C1 P1 C11 100.8(2) . . ? C17 P1 C11 106.5(2) . . ? C1 P1 Pt1 123.30(15) . . ? C17 P1 Pt1 109.25(16) . . ? C11 P1 Pt1 115.03(15) . . ? C6 P2 C23 101.8(2) . . ? C6 P2 C29 106.9(2) . . ? C23 P2 C29 102.3(2) . . ? C6 P2 Pt1 115.59(16) . . ? C23 P2 Pt1 117.27(15) . . ? C29 P2 Pt1 111.55(16) . . ? C47 Pt1 C35 86.06(18) . . ? C47 Pt1 P2 91.35(13) . . ? C35 Pt1 P2 177.23(13) . . ? C47 Pt1 P1 169.69(13) . . ? C35 Pt1 P1 83.82(12) . . ? P2 Pt1 P1 98.81(4) . . ? #===END data_complex6.2CH2Cl2.2H2O _database_code_depnum_ccdc_archive 'CCDC 685383' _audit_creation_date 2008-01-29T10:53:37-00:00 _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 'C82 H116 Cl4 Fe4 N2 O2 Pt' _chemical_formula_weight 1722.06 #----------------------------------------------------------------------------# # 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 12.6320(7) _cell_length_b 13.2780(5) _cell_length_c 13.5760(8) _cell_angle_alpha 81.272(3) _cell_angle_beta 63.866(2) _cell_angle_gamma 70.778(3) _cell_volume 1930.25(17) _cell_formula_units_Z 1 _cell_measurement_temperature 100.0(10) _cell_measurement_reflns_used 2819 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.725 _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 0.7294 _exptl_absorpt_correction_T_max 0.8411 #----------------------------------------------------------------------------# # 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 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0010668 _diffrn_orient_matrix_ub_12 -0.0763119 _diffrn_orient_matrix_ub_13 0.0063065 _diffrn_orient_matrix_ub_21 -0.0797219 _diffrn_orient_matrix_ub_22 0.0219986 _diffrn_orient_matrix_ub_23 -0.0076872 _diffrn_orient_matrix_ub_31 0.0465171 _diffrn_orient_matrix_ub_32 -0.0073485 _diffrn_orient_matrix_ub_33 -0.0814467 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_unetI/netI 0.0775 _diffrn_reflns_number 29742 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8828 _reflns_number_gt 7412 _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^+5.7610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8828 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.067 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.153 #----------------------------------------------------------------------------# # 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 0.0067(4) 0.1228(3) 0.5655(3) 0.0132(8) Uani 1 1 d . . . C2 C 0.0049(4) 0.1980(3) 0.6060(3) 0.0153(9) Uani 1 1 d . . . C3 C -0.0110(4) 0.2937(3) 0.6550(3) 0.0147(9) Uani 1 1 d . . . C4 C -0.0423(4) 0.3999(3) 0.6126(3) 0.0167(9) Uani 1 1 d . . . H4 H -0.0536 0.418 0.5483 0.02 Uiso 1 1 calc R . . C5 C -0.0529(4) 0.4724(3) 0.6858(3) 0.0170(9) Uani 1 1 d . . . H5 H -0.0738 0.5462 0.6781 0.02 Uiso 1 1 calc R . . C6 C -0.0263(4) 0.4129(3) 0.7724(3) 0.0183(9) Uani 1 1 d . . . H6 H -0.0262 0.4411 0.831 0.022 Uiso 1 1 calc R . . C7 C 0.0003(4) 0.3024(3) 0.7543(3) 0.0153(9) Uani 1 1 d . . . H7 H 0.0212 0.2461 0.7986 0.018 Uiso 1 1 calc R . . C8 C 0.2944(4) 0.2878(4) 0.6176(4) 0.0222(10) Uani 1 1 d . . . H8 H 0.3127 0.237 0.6675 0.027 Uiso 1 1 calc R . . C9 C 0.2861(4) 0.2682(4) 0.5221(3) 0.0225(10) Uani 1 1 d . . . H9 H 0.2988 0.2014 0.4982 0.027 Uiso 1 1 calc R . . C10 C 0.2554(4) 0.3663(4) 0.4690(3) 0.0211(10) Uani 1 1 d . . . H10 H 0.2437 0.3755 0.4048 0.025 Uiso 1 1 calc R . . C11 C 0.2458(4) 0.4484(4) 0.5313(3) 0.0215(10) Uani 1 1 d . . . H11 H 0.2272 0.5209 0.5148 0.026 Uiso 1 1 calc R . . C12 C 0.2695(4) 0.4003(4) 0.6230(4) 0.0207(10) Uani 1 1 d . . . H12 H 0.2688 0.4358 0.6774 0.025 Uiso 1 1 calc R . . C13 C -0.0066(4) 0.0923(3) 0.3692(3) 0.0133(9) Uani 1 1 d . . . C14 C -0.0164(4) 0.1514(3) 0.2949(3) 0.0146(9) Uani 1 1 d . . . C15 C -0.0433(4) 0.2319(3) 0.2184(3) 0.0143(9) Uani 1 1 d . . . C16 C -0.0621(4) 0.2187(3) 0.1247(3) 0.0181(9) Uani 1 1 d . . . H16 H -0.0566 0.1546 0.1003 0.022 Uiso 1 1 calc R . . C17 C -0.0904(4) 0.3206(3) 0.0756(3) 0.0182(9) Uani 1 1 d . . . H17 H -0.1072 0.3347 0.0139 0.022 Uiso 1 1 calc R . . C18 C -0.0888(4) 0.3974(3) 0.1373(3) 0.0184(9) Uani 1 1 d . . . H18 H -0.1039 0.4702 0.1228 0.022 Uiso 1 1 calc R . . C19 C -0.0601(4) 0.3435(3) 0.2241(3) 0.0148(9) Uani 1 1 d . . . H19 H -0.0531 0.3751 0.2767 0.018 Uiso 1 1 calc R . . C20 C 0.2391(4) 0.2883(4) 0.0784(4) 0.0251(11) Uani 1 1 d . . . H20 H 0.2477 0.3054 0.1379 0.03 Uiso 1 1 calc R . . C21 C 0.2502(4) 0.1854(4) 0.0513(4) 0.0263(11) Uani 1 1 d . . . H21 H 0.2674 0.1229 0.0902 0.032 Uiso 1 1 calc R . . C22 C 0.2306(4) 0.1941(4) -0.0456(4) 0.0264(11) Uani 1 1 d . . . H22 H 0.233 0.1383 -0.0812 0.032 Uiso 1 1 calc R . . C23 C 0.2067(4) 0.3032(4) -0.0781(3) 0.0228(10) Uani 1 1 d . . . H23 H 0.1903 0.3315 -0.1387 0.027 Uiso 1 1 calc R . . C24 C 0.2124(4) 0.3609(4) -0.0020(3) 0.0209(10) Uani 1 1 d . . . H24 H 0.2006 0.434 -0.0041 0.025 Uiso 1 1 calc R . . C25 C 0.5612(4) 0.1426(4) 0.7624(4) 0.0245(11) Uani 1 1 d . . . H25A H 0.5168 0.1337 0.8408 0.029 Uiso 1 1 calc R . . H25B H 0.5009 0.1674 0.7314 0.029 Uiso 1 1 calc R . . C26 C 0.6470(4) 0.0340(4) 0.7139(4) 0.0302(12) Uani 1 1 d . . . H26A H 0.7001 0.0037 0.7518 0.036 Uiso 1 1 calc R . . H26B H 0.6991 0.043 0.6372 0.036 Uiso 1 1 calc R . . C27 C 0.5760(5) -0.0429(4) 0.7230(4) 0.0385(13) Uani 1 1 d . . . H27A H 0.5199 -0.0104 0.6883 0.046 Uiso 1 1 calc R . . H27B H 0.634 -0.1072 0.6829 0.046 Uiso 1 1 calc R . . C28 C 0.5037(5) -0.0728(4) 0.8380(4) 0.0405(14) Uani 1 1 d . . . H28A H 0.5576 -0.1017 0.8744 0.061 Uiso 1 1 calc R . . H28B H 0.4668 -0.1253 0.8373 0.061 Uiso 1 1 calc R . . H28C H 0.4401 -0.0107 0.8763 0.061 Uiso 1 1 calc R . . C29 C 0.6874(4) 0.2509(3) 0.6220(3) 0.0206(10) Uani 1 1 d . . . H29A H 0.7329 0.3005 0.6127 0.025 Uiso 1 1 calc R . . H29B H 0.747 0.1849 0.5865 0.025 Uiso 1 1 calc R . . C30 C 0.6037(4) 0.2961(4) 0.5633(4) 0.0267(11) Uani 1 1 d . . . H30A H 0.5506 0.3666 0.5911 0.032 Uiso 1 1 calc R . . H30B H 0.5518 0.2509 0.5773 0.032 Uiso 1 1 calc R . . C31 C 0.6801(4) 0.3026(4) 0.4408(4) 0.0244(10) Uani 1 1 d . . . H31A H 0.7327 0.3469 0.4279 0.029 Uiso 1 1 calc R . . H31B H 0.7331 0.2317 0.414 0.029 Uiso 1 1 calc R . . C32 C 0.6029(5) 0.3477(5) 0.3764(4) 0.0471(15) Uani 1 1 d . . . H32A H 0.5511 0.304 0.3881 0.071 Uiso 1 1 calc R . . H32B H 0.6561 0.3489 0.2997 0.071 Uiso 1 1 calc R . . H32C H 0.5525 0.419 0.4004 0.071 Uiso 1 1 calc R . . C33 C 0.7221(4) 0.1920(4) 0.7877(3) 0.0212(10) Uani 1 1 d . . . H33A H 0.7616 0.2476 0.773 0.025 Uiso 1 1 calc R . . H33B H 0.7846 0.1292 0.7477 0.025 Uiso 1 1 calc R . . C34 C 0.6755(4) 0.1659(4) 0.9098(4) 0.0260(11) Uani 1 1 d . . . H34A H 0.6576 0.0982 0.923 0.031 Uiso 1 1 calc R . . H34B H 0.5998 0.2205 0.9498 0.031 Uiso 1 1 calc R . . C35 C 0.7733(4) 0.1597(4) 0.9512(4) 0.0283(11) Uani 1 1 d . . . H35A H 0.7945 0.2261 0.9333 0.034 Uiso 1 1 calc R . . H35B H 0.7379 0.1521 1.0305 0.034 Uiso 1 1 calc R . . C36 C 0.8894(4) 0.0684(4) 0.9027(4) 0.0291(11) Uani 1 1 d . . . H36A H 0.8687 0.0028 0.9157 0.044 Uiso 1 1 calc R . . H36B H 0.9435 0.0646 0.9363 0.044 Uiso 1 1 calc R . . H36C H 0.9301 0.0797 0.8251 0.044 Uiso 1 1 calc R . . C37 C 0.5233(4) 0.3278(3) 0.8016(4) 0.0240(10) Uani 1 1 d . . . H37A H 0.4819 0.3103 0.8784 0.029 Uiso 1 1 calc R . . H37B H 0.4628 0.3477 0.7709 0.029 Uiso 1 1 calc R . . C38 C 0.5665(5) 0.4239(4) 0.7945(4) 0.0316(12) Uani 1 1 d . . . H38A H 0.6304 0.4043 0.8212 0.038 Uiso 1 1 calc R . . H38B H 0.6013 0.4467 0.7186 0.038 Uiso 1 1 calc R . . C39 C 0.4593(5) 0.5149(4) 0.8624(4) 0.0350(13) Uani 1 1 d . . . H39A H 0.4278 0.4931 0.9389 0.042 Uiso 1 1 calc R . . H39B H 0.3933 0.5309 0.8387 0.042 Uiso 1 1 calc R . . C40 C 0.4980(6) 0.6148(4) 0.8514(5) 0.0481(16) Uani 1 1 d . . . H40A H 0.5612 0.5998 0.8773 0.072 Uiso 1 1 calc R . . H40B H 0.4279 0.6711 0.8941 0.072 Uiso 1 1 calc R . . H40C H 0.5292 0.6365 0.7757 0.072 Uiso 1 1 calc R . . C41 C 0.7766(5) 0.0074(5) 0.3349(4) 0.0378(13) Uani 1 1 d . . . H41A H 0.8176 0.0593 0.3303 0.045 Uiso 1 1 calc R . . H41B H 0.8241 -0.0616 0.3512 0.045 Uiso 1 1 calc R . . Fe1 Fe 0.07911(5) 0.28516(5) 0.07694(5) 0.01488(14) Uani 1 1 d . . . Fe2 Fe 0.12161(5) 0.36674(5) 0.62514(5) 0.01458(14) Uani 1 1 d . . . N1 N 0.6238(3) 0.2285(3) 0.7436(3) 0.0199(8) Uani 1 1 d . . . Pt1 Pt 0 0 0.5 0.01087(7) Uani 1 2 d S . . O1 O 0.1434(3) 0.2548(3) 0.3512(3) 0.0286(8) Uani 1 1 d . . . Cl1 Cl 0.62816(13) 0.04236(13) 0.44163(11) 0.0474(4) Uani 1 1 d . . . Cl2 Cl 0.77333(14) 0.00159(16) 0.21048(12) 0.0630(5) Uani 1 1 d . . . H1 H 0.118(5) 0.241(5) 0.417(5) 0.05(2) Uiso 1 1 d . . . H2 H 0.111(6) 0.223(5) 0.328(6) 0.08(2) Uiso 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 0.016(2) 0.015(2) 0.0105(19) 0.0011(16) -0.0064(17) -0.0064(17) C2 0.015(2) 0.016(2) 0.014(2) 0.0012(17) -0.0031(17) -0.0078(17) C3 0.014(2) 0.016(2) 0.014(2) 0.0001(17) -0.0012(17) -0.0093(17) C4 0.016(2) 0.018(2) 0.019(2) 0.0018(18) -0.0077(18) -0.0090(18) C5 0.016(2) 0.012(2) 0.023(2) -0.0005(17) -0.0061(18) -0.0053(17) C6 0.017(2) 0.019(2) 0.017(2) -0.0054(18) -0.0035(18) -0.0066(19) C7 0.013(2) 0.020(2) 0.012(2) 0.0038(17) -0.0041(17) -0.0075(18) C8 0.015(2) 0.024(2) 0.026(2) 0.0036(19) -0.0094(19) -0.0032(19) C9 0.018(2) 0.024(2) 0.020(2) -0.0089(19) 0.0002(19) -0.0062(19) C10 0.016(2) 0.033(3) 0.012(2) 0.0022(19) -0.0005(18) -0.013(2) C11 0.022(2) 0.023(2) 0.022(2) 0.0038(19) -0.0057(19) -0.015(2) C12 0.014(2) 0.030(3) 0.020(2) -0.0020(19) -0.0050(18) -0.012(2) C13 0.011(2) 0.014(2) 0.017(2) -0.0045(17) -0.0056(17) -0.0046(17) C14 0.018(2) 0.015(2) 0.013(2) -0.0018(17) -0.0063(17) -0.0071(18) C15 0.014(2) 0.019(2) 0.010(2) 0.0027(17) -0.0043(17) -0.0065(17) C16 0.024(2) 0.018(2) 0.016(2) 0.0033(17) -0.0095(19) -0.0105(19) C17 0.014(2) 0.027(2) 0.014(2) 0.0084(18) -0.0079(18) -0.0085(19) C18 0.016(2) 0.013(2) 0.022(2) 0.0026(18) -0.0067(19) -0.0018(17) C19 0.015(2) 0.013(2) 0.016(2) -0.0023(17) -0.0045(18) -0.0058(17) C20 0.016(2) 0.037(3) 0.023(2) 0.004(2) -0.008(2) -0.011(2) C21 0.012(2) 0.025(3) 0.033(3) 0.010(2) -0.008(2) -0.0007(19) C22 0.019(2) 0.023(3) 0.025(3) -0.008(2) 0.000(2) -0.001(2) C23 0.019(2) 0.025(3) 0.013(2) 0.0045(18) -0.0015(18) -0.003(2) C24 0.015(2) 0.022(2) 0.022(2) 0.0046(19) -0.0053(19) -0.0067(19) C25 0.022(3) 0.031(3) 0.025(3) 0.013(2) -0.012(2) -0.016(2) C26 0.032(3) 0.029(3) 0.032(3) 0.002(2) -0.012(2) -0.015(2) C27 0.036(3) 0.038(3) 0.043(3) -0.001(3) -0.017(3) -0.010(3) C28 0.034(3) 0.040(3) 0.053(4) 0.010(3) -0.025(3) -0.014(3) C29 0.019(2) 0.021(2) 0.018(2) 0.0016(18) -0.0049(19) -0.0065(19) C30 0.015(2) 0.032(3) 0.026(3) 0.000(2) -0.005(2) -0.002(2) C31 0.020(2) 0.031(3) 0.021(2) 0.004(2) -0.007(2) -0.009(2) C32 0.034(3) 0.074(4) 0.024(3) 0.013(3) -0.014(3) -0.009(3) C33 0.013(2) 0.028(3) 0.020(2) 0.0006(19) -0.0045(18) -0.0062(19) C34 0.020(2) 0.035(3) 0.021(2) 0.003(2) -0.008(2) -0.007(2) C35 0.030(3) 0.032(3) 0.021(2) -0.001(2) -0.010(2) -0.008(2) C36 0.031(3) 0.032(3) 0.027(3) 0.003(2) -0.018(2) -0.007(2) C37 0.016(2) 0.026(3) 0.022(2) 0.0025(19) -0.0037(19) -0.002(2) C38 0.032(3) 0.025(3) 0.033(3) -0.006(2) -0.011(2) -0.003(2) C39 0.041(3) 0.027(3) 0.026(3) -0.001(2) -0.011(2) -0.001(2) C40 0.071(4) 0.026(3) 0.041(3) -0.006(3) -0.024(3) -0.003(3) C41 0.027(3) 0.055(4) 0.037(3) 0.001(3) -0.017(2) -0.014(3) Fe1 0.0157(3) 0.0148(3) 0.0131(3) 0.0027(2) -0.0059(3) -0.0047(3) Fe2 0.0155(3) 0.0149(3) 0.0142(3) -0.0003(2) -0.0053(3) -0.0066(3) N1 0.0157(19) 0.022(2) 0.021(2) 0.0042(16) -0.0074(16) -0.0071(16) Pt1 0.01320(13) 0.01015(12) 0.01010(12) 0.00114(9) -0.00486(10) -0.00503(9) O1 0.038(2) 0.035(2) 0.0212(19) 0.0067(16) -0.0152(17) -0.0197(17) Cl1 0.0390(8) 0.0697(10) 0.0334(7) -0.0056(7) -0.0045(6) -0.0287(8) Cl2 0.0427(9) 0.1219(15) 0.0349(8) -0.0123(9) -0.0179(7) -0.0295(10) #----------------------------------------------------------------------------# # 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 1.200(5) . ? C1 Pt1 2.013(4) . ? C2 C3 1.438(5) . ? C3 C4 1.436(6) . ? C3 C7 1.441(6) . ? C3 Fe2 2.065(4) . ? C4 C5 1.421(5) . ? C4 Fe2 2.048(4) . ? C5 C6 1.419(6) . ? C5 Fe2 2.055(4) . ? C6 C7 1.427(6) . ? C6 Fe2 2.047(4) . ? C7 Fe2 2.048(4) . ? C8 C9 1.414(6) . ? C8 C12 1.427(6) . ? C8 Fe2 2.050(4) . ? C9 C10 1.413(6) . ? C9 Fe2 2.047(4) . ? C10 C11 1.422(6) . ? C10 Fe2 2.047(4) . ? C11 C12 1.418(6) . ? C11 Fe2 2.049(4) . ? C12 Fe2 2.045(4) . ? C13 C14 1.206(6) . ? C13 Pt1 2.016(4) . ? C14 C15 1.440(6) . ? C15 C19 1.435(5) . ? C15 C16 1.438(6) . ? C15 Fe1 2.067(4) . ? C16 C17 1.421(6) . ? C16 Fe1 2.056(4) . ? C17 C18 1.425(6) . ? C17 Fe1 2.043(4) . ? C18 C19 1.408(6) . ? C18 Fe1 2.036(4) . ? C19 Fe1 2.040(4) . ? C20 C21 1.414(6) . ? C20 C24 1.423(6) . ? C20 Fe1 2.044(4) . ? C21 C22 1.424(7) . ? C21 Fe1 2.035(4) . ? C22 C23 1.421(6) . ? C22 Fe1 2.043(4) . ? C23 C24 1.415(6) . ? C23 Fe1 2.049(4) . ? C24 Fe1 2.047(4) . ? C25 C26 1.522(6) . ? C25 N1 1.524(5) . ? C26 C27 1.526(6) . ? C27 C28 1.491(7) . ? C29 C30 1.514(6) . ? C29 N1 1.516(5) . ? C30 C31 1.518(6) . ? C31 C32 1.510(7) . ? C33 N1 1.519(5) . ? C33 C34 1.522(6) . ? C34 C35 1.542(6) . ? C35 C36 1.509(6) . ? C37 N1 1.517(5) . ? C37 C38 1.519(6) . ? C38 C39 1.518(6) . ? C39 C40 1.525(7) . ? C41 Cl2 1.722(5) . ? C41 Cl1 1.752(5) . ? Pt1 C1 2.013(4) 2_556 ? Pt1 C13 2.016(4) 2_556 ? 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 Pt1 177.0(4) . . ? C1 C2 C3 173.5(5) . . ? C4 C3 C2 125.4(4) . . ? C4 C3 C7 107.1(3) . . ? C2 C3 C7 127.5(4) . . ? C4 C3 Fe2 68.9(2) . . ? C2 C3 Fe2 127.5(3) . . ? C7 C3 Fe2 68.8(2) . . ? C5 C4 C3 108.3(4) . . ? C5 C4 Fe2 70.0(2) . . ? C3 C4 Fe2 70.2(2) . . ? C6 C5 C4 108.3(4) . . ? C6 C5 Fe2 69.5(2) . . ? C4 C5 Fe2 69.5(2) . . ? C5 C6 C7 108.3(4) . . ? C5 C6 Fe2 70.0(2) . . ? C7 C6 Fe2 69.6(2) . . ? C6 C7 C3 107.8(4) . . ? C6 C7 Fe2 69.6(2) . . ? C3 C7 Fe2 70.1(2) . . ? C9 C8 C12 107.2(4) . . ? C9 C8 Fe2 69.7(3) . . ? C12 C8 Fe2 69.4(2) . . ? C10 C9 C8 109.0(4) . . ? C10 C9 Fe2 69.8(2) . . ? C8 C9 Fe2 69.9(2) . . ? C9 C10 C11 107.6(4) . . ? C9 C10 Fe2 69.8(2) . . ? C11 C10 Fe2 69.8(2) . . ? C12 C11 C10 108.0(4) . . ? C12 C11 Fe2 69.6(2) . . ? C10 C11 Fe2 69.6(2) . . ? C11 C12 C8 108.2(4) . . ? C11 C12 Fe2 69.9(2) . . ? C8 C12 Fe2 69.8(2) . . ? C14 C13 Pt1 176.4(4) . . ? C13 C14 C15 171.7(4) . . ? C19 C15 C16 106.6(4) . . ? C19 C15 C14 125.5(4) . . ? C16 C15 C14 127.9(4) . . ? C19 C15 Fe1 68.5(2) . . ? C16 C15 Fe1 69.2(2) . . ? C14 C15 Fe1 128.4(3) . . ? C17 C16 C15 108.1(4) . . ? C17 C16 Fe1 69.3(2) . . ? C15 C16 Fe1 70.0(2) . . ? C16 C17 C18 108.3(4) . . ? C16 C17 Fe1 70.2(2) . . ? C18 C17 Fe1 69.3(2) . . ? C19 C18 C17 108.0(4) . . ? C19 C18 Fe1 69.9(2) . . ? C17 C18 Fe1 69.8(2) . . ? C18 C19 C15 109.0(4) . . ? C18 C19 Fe1 69.7(2) . . ? C15 C19 Fe1 70.5(2) . . ? C21 C20 C24 107.6(4) . . ? C21 C20 Fe1 69.4(3) . . ? C24 C20 Fe1 69.8(3) . . ? C20 C21 C22 108.3(4) . . ? C20 C21 Fe1 70.1(3) . . ? C22 C21 Fe1 69.9(3) . . ? C23 C22 C21 107.9(4) . . ? C23 C22 Fe1 69.9(2) . . ? C21 C22 Fe1 69.3(2) . . ? C24 C23 C22 107.8(4) . . ? C24 C23 Fe1 69.7(2) . . ? C22 C23 Fe1 69.4(2) . . ? C23 C24 C20 108.5(4) . . ? C23 C24 Fe1 69.9(2) . . ? C20 C24 Fe1 69.5(2) . . ? C26 C25 N1 115.5(4) . . ? C25 C26 C27 112.1(4) . . ? C28 C27 C26 114.0(4) . . ? C30 C29 N1 115.8(3) . . ? C29 C30 C31 110.1(4) . . ? C32 C31 C30 113.3(4) . . ? N1 C33 C34 115.1(3) . . ? C33 C34 C35 110.3(4) . . ? C36 C35 C34 113.3(4) . . ? N1 C37 C38 115.5(4) . . ? C39 C38 C37 110.3(4) . . ? C38 C39 C40 111.6(4) . . ? Cl2 C41 Cl1 112.0(3) . . ? C21 Fe1 C18 164.61(19) . . ? C21 Fe1 C19 126.58(18) . . ? C18 Fe1 C19 40.40(16) . . ? C21 Fe1 C22 40.87(19) . . ? C18 Fe1 C22 153.46(19) . . ? C19 Fe1 C22 165.05(18) . . ? C21 Fe1 C17 152.50(18) . . ? C18 Fe1 C17 40.87(16) . . ? C19 Fe1 C17 68.24(17) . . ? C22 Fe1 C17 119.43(19) . . ? C21 Fe1 C20 40.59(18) . . ? C18 Fe1 C20 127.33(18) . . ? C19 Fe1 C20 106.89(17) . . ? C22 Fe1 C20 68.52(19) . . ? C17 Fe1 C20 166.33(18) . . ? C21 Fe1 C24 68.22(18) . . ? C18 Fe1 C24 108.66(17) . . ? C19 Fe1 C24 118.35(16) . . ? C22 Fe1 C24 68.13(18) . . ? C17 Fe1 C24 129.17(17) . . ? C20 Fe1 C24 40.71(17) . . ? C21 Fe1 C23 68.53(18) . . ? C18 Fe1 C23 119.60(17) . . ? C19 Fe1 C23 152.50(17) . . ? C22 Fe1 C23 40.63(17) . . ? C17 Fe1 C23 109.52(18) . . ? C20 Fe1 C23 68.50(18) . . ? C24 Fe1 C23 40.41(17) . . ? C21 Fe1 C16 117.89(18) . . ? C18 Fe1 C16 68.61(17) . . ? C19 Fe1 C16 68.46(16) . . ? C22 Fe1 C16 108.24(18) . . ? C17 Fe1 C16 40.57(16) . . ? C20 Fe1 C16 151.10(18) . . ? C24 Fe1 C16 166.93(18) . . ? C23 Fe1 C16 128.81(18) . . ? C21 Fe1 C15 106.40(18) . . ? C18 Fe1 C15 68.69(16) . . ? C19 Fe1 C15 40.91(15) . . ? C22 Fe1 C15 127.19(17) . . ? C17 Fe1 C15 68.55(16) . . ? C20 Fe1 C15 116.78(17) . . ? C24 Fe1 C15 151.38(17) . . ? C23 Fe1 C15 165.99(17) . . ? C16 Fe1 C15 40.83(15) . . ? C12 Fe2 C9 67.95(17) . . ? C12 Fe2 C6 109.09(17) . . ? C9 Fe2 C6 155.13(19) . . ? C12 Fe2 C10 68.28(17) . . ? C9 Fe2 C10 40.37(18) . . ? C6 Fe2 C10 163.64(18) . . ? C12 Fe2 C7 125.94(17) . . ? C9 Fe2 C7 119.45(17) . . ? C6 Fe2 C7 40.80(16) . . ? C10 Fe2 C7 153.90(17) . . ? C12 Fe2 C4 155.94(17) . . ? C9 Fe2 C4 124.69(17) . . ? C6 Fe2 C4 68.40(17) . . ? C10 Fe2 C4 107.02(18) . . ? C7 Fe2 C4 68.84(17) . . ? C12 Fe2 C11 40.52(17) . . ? C9 Fe2 C11 67.89(18) . . ? C6 Fe2 C11 126.99(17) . . ? C10 Fe2 C11 40.61(16) . . ? C7 Fe2 C11 163.68(17) . . ? C4 Fe2 C11 120.56(18) . . ? C12 Fe2 C8 40.79(17) . . ? C9 Fe2 C8 40.38(17) . . ? C6 Fe2 C8 120.99(18) . . ? C10 Fe2 C8 68.35(18) . . ? C7 Fe2 C8 106.98(18) . . ? C4 Fe2 C8 161.49(17) . . ? C11 Fe2 C8 68.40(18) . . ? C12 Fe2 C5 121.93(17) . . ? C9 Fe2 C5 162.34(18) . . ? C6 Fe2 C5 40.48(17) . . ? C10 Fe2 C5 126.05(18) . . ? C7 Fe2 C5 68.47(16) . . ? C4 Fe2 C5 40.52(15) . . ? C11 Fe2 C5 109.11(17) . . ? C8 Fe2 C5 156.41(17) . . ? C12 Fe2 C3 162.49(18) . . ? C9 Fe2 C3 106.38(17) . . ? C6 Fe2 C3 68.64(16) . . ? C10 Fe2 C3 118.92(16) . . ? C7 Fe2 C3 41.03(15) . . ? C4 Fe2 C3 40.87(16) . . ? C11 Fe2 C3 154.54(17) . . ? C8 Fe2 C3 124.30(17) . . ? C5 Fe2 C3 68.41(16) . . ? C29 N1 C37 110.3(3) . . ? C29 N1 C33 107.3(3) . . ? C37 N1 C33 111.5(3) . . ? C29 N1 C25 110.5(3) . . ? C37 N1 C25 106.8(3) . . ? C33 N1 C25 110.4(3) . . ? C1 Pt1 C1 180.00(11) . 2_556 ? C1 Pt1 C13 90.43(15) . 2_556 ? C1 Pt1 C13 89.57(15) 2_556 2_556 ? C1 Pt1 C13 89.57(15) . . ? C1 Pt1 C13 90.43(15) 2_556 . ? C13 Pt1 C13 180.00(15) 2_556 . ? #===END