# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Munetaka Akita' _publ_contact_author_email MAKITA@RES.TITECH.AC.JP _publ_section_title ; Remarkable Switching Behavior of Bimodally Stimuli-responsive Photochromic Dithienylethenes with Redox-active Organometallic Attachements ; loop_ _publ_author_name 'Munetaka Akita' 'Takashi Koike' 'Keiko Motoyama' # Attachment 'B809318Krev2.CIF' data_compound/1Ru/1013_ _database_code_depnum_ccdc_archive 'CCDC 689366' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H20 Cl2 F6 O4 S2 Ru2 ' _chemical_formula_moiety 'C30 H20 Cl2 F6 O4 S2 Ru2 ' _chemical_formula_weight 895.64 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,1/2+z 1/2+x,1/2-y,-z -x,y,1/2-z -x,-y,-z 1/2+x,1/2+y,1/2-z 1/2-x,1/2+y,z x,-y,1/2+z _cell_length_a 20.883(2) _cell_length_b 13.9416(7) _cell_length_c 11.3024(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3290.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 19559 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.880 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 25860 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 #------------------------------------------------------------------------------ # REFINEMENT DATA _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. ; _reflns_number_total 3770 _reflns_number_gt 2910 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.2187 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2910 _refine_ls_number_parameters 229 _refine_ls_goodness_of_fit_ref 1.678 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0330 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.72 _refine_diff_density_min -1.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru 0.72918(2) 0.19145(3) 0.50074(3) 0.0376(2) Uani 1.00 d . . . Cl(1) Cl 0.4900(5) 0.0628(8) 0.1340(10) 0.36336(7) Uiso 1.00 d . . . S(1) S 0.64213(6) 0.1750(1) 0.7447(1) 0.0456(3) Uani 1.00 d . . . F(1) F 0.5534(5) 0.5181(8) 0.5769(9) 0.051(2) Uani 0.50 d P . . F(1A) F 0.5824(7) 0.5294(8) 0.627(2) 0.114(6) Uani 0.50 d P . . F(2) F 0.6144(4) 0.5213(6) 0.7295(9) 0.054(2) Uani 0.50 d P . . F(2A) F 0.5952(5) 0.5246(6) 0.814(1) 0.100(4) Uani 0.50 d P . . F(3) F 0.4945(5) 0.6512(5) 0.6949(9) 0.077(3) Uani 0.50 d P . . F(4) F 0.5295(5) 0.5986(8) 0.8582(9) 0.083(3) Uani 0.50 d P . . O(31) O 0.8226(2) 0.3169(3) 0.6285(4) 0.068(1) Uani 1.00 d . . . O(32) O 0.6973(2) 0.3528(3) 0.3339(4) 0.065(1) Uani 1.00 d . . . C(1) C 0.5306(2) 0.4045(3) 0.7309(4) 0.038(1) Uani 1.00 d . . . C(2) C 0.5524(6) 0.5017(8) 0.693(1) 0.03309(4) Uiso 0.50 d P . . C(2A) C 0.5542(7) 0.5060(9) 0.730(1) 0.04620(5) Uiso 0.50 d P . . C(3) C 0.5000 0.5687(5) 0.7500 0.053(2) Uani 1.00 d S . . C(11) C 0.5828(2) 0.2506(4) 0.7934(5) 0.041(1) Uani 1.00 d . . . C(12) C 0.5746(2) 0.3252(4) 0.7139(4) 0.037(1) Uani 1.00 d . . . C(13) C 0.6187(2) 0.3171(3) 0.6149(5) 0.038(1) Uani 1.00 d . . . C(14) C 0.6575(2) 0.2398(3) 0.6170(5) 0.039(1) Uani 1.00 d . . . C(15) C 0.5499(3) 0.2333(5) 0.9094(5) 0.056(1) Uani 1.00 d . . . C(21) C 0.6992(3) 0.0665(4) 0.3835(5) 0.055(1) Uani 1.00 d . . . C(22) C 0.7644(3) 0.0861(4) 0.3642(6) 0.054(1) Uani 1.00 d . . . C(23) C 0.7977(4) 0.0697(5) 0.4704(6) 0.058(2) Uani 1.00 d . . . C(24) C 0.7528(4) 0.0419(4) 0.5570(7) 0.064(2) Uani 1.00 d . . . C(25) C 0.6919(4) 0.0386(5) 0.5027(5) 0.061(2) Uani 1.00 d . . . C(31) C 0.7862(3) 0.2713(4) 0.5826(5) 0.044(1) Uani 1.00 d . . . C(32) C 0.7082(3) 0.2933(4) 0.3979(5) 0.049(1) Uani 1.00 d . . . C(41) C 0.541(2) 0.020(2) 0.236(3) 0.1830(2) Uiso 0.50 d P . . H(1) H 0.6205 0.3644 0.5541 0.0456 Uiso 1.00 calc . . . H(2) H 0.5586 0.2880 0.9623 0.0700 Uiso 1.00 calc . . . H(3) H 0.5053 0.2290 0.9003 0.0700 Uiso 1.00 calc . . . H(4) H 0.5664 0.1780 0.9467 0.0700 Uiso 1.00 calc . . . H(5) H 0.6658 0.0695 0.3257 0.0646 Uiso 1.00 calc . . . H(6) H 0.7837 0.1057 0.2899 0.0646 Uiso 1.00 calc . . . H(7) H 0.8429 0.0731 0.4816 0.0728 Uiso 1.00 calc . . . H(8) H 0.7616 0.0222 0.6371 0.0729 Uiso 1.00 calc . . . H(9) H 0.6526 0.0172 0.5398 0.0738 Uiso 1.00 calc . . . H(10) H 0.5437 -0.0490 0.2325 0.2226 Uiso 0.50 calc P . . H(11) H 0.5846 0.0432 0.2203 0.2226 Uiso 0.50 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0410(4) 0.0364(3) 0.0355(4) 0.0079(2) 0.0020(1) 0.0011(1) S(1) 0.0435(7) 0.0498(7) 0.0437(7) 0.0105(6) 0.0044(6) 0.0110(6) F(1) 0.067(6) 0.049(4) 0.039(4) -0.004(4) 0.007(4) 0.008(3) F(1A) 0.12(1) 0.047(5) 0.17(2) 0.014(7) 0.11(1) 0.025(9) F(2) 0.042(4) 0.054(4) 0.065(5) -0.016(3) -0.004(4) 0.004(4) F(2A) 0.052(5) 0.059(5) 0.19(1) -0.016(4) -0.040(7) 0.015(7) F(3) 0.086(6) 0.043(4) 0.103(7) 0.015(4) 0.029(6) 0.017(4) F(4) 0.083(6) 0.090(7) 0.077(6) -0.022(5) 0.017(5) -0.047(5) O(31) 0.065(3) 0.070(3) 0.069(3) -0.017(2) 0.007(2) -0.018(2) O(32) 0.083(3) 0.057(2) 0.056(3) 0.032(2) 0.010(2) 0.021(2) C(1) 0.032(2) 0.043(2) 0.038(3) -0.001(2) 0.003(2) 0.006(2) C(3) 0.061(5) 0.037(4) 0.062(5) 0.0000 0.011(4) 0.0000 C(11) 0.034(2) 0.047(3) 0.042(3) 0.001(2) 0.004(2) 0.007(2) C(12) 0.031(2) 0.042(2) 0.039(3) 0.002(2) 0.001(2) 0.002(2) C(13) 0.034(2) 0.040(2) 0.040(3) 0.001(2) 0.005(2) 0.006(2) C(14) 0.036(2) 0.042(3) 0.039(3) 0.005(2) 0.006(2) -0.001(2) C(15) 0.050(3) 0.072(4) 0.047(3) 0.010(3) 0.010(3) 0.017(3) C(21) 0.069(4) 0.040(3) 0.055(4) 0.001(3) -0.013(3) -0.010(2) C(22) 0.067(4) 0.050(3) 0.044(3) 0.017(3) 0.006(3) -0.012(3) C(23) 0.065(4) 0.047(3) 0.062(4) 0.031(3) -0.007(3) -0.009(3) C(24) 0.106(5) 0.035(3) 0.052(4) 0.017(3) -0.012(4) 0.004(3) C(25) 0.079(5) 0.039(3) 0.066(5) -0.002(3) 0.014(3) -0.001(2) C(31) 0.044(3) 0.044(3) 0.044(3) 0.001(2) 0.010(2) -0.003(2) C(32) 0.050(3) 0.054(3) 0.044(3) 0.015(3) 0.010(3) -0.004(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) C(14) 2.103(5) . . yes Ru(1) C(21) 2.277(6) . . yes Ru(1) C(22) 2.254(6) . . yes Ru(1) C(23) 2.246(7) . . yes Ru(1) C(24) 2.234(6) . . yes Ru(1) C(25) 2.268(7) . . yes Ru(1) C(31) 1.875(6) . . yes Ru(1) C(32) 1.886(6) . . yes Cl(1) C(41) 1.69(4) . . yes Cl(1) C(41) 1.71(3) . 4_655 yes S(1) C(11) 1.718(5) . . yes S(1) C(14) 1.734(5) . . yes F(1) F(1A) 0.85(2) . . yes F(1) C(2) 1.33(2) . . yes F(1) C(2A) 1.74(2) . . yes F(1A) F(2) 1.34(2) . . yes F(1A) C(2) 1.04(2) . . yes F(1A) C(2A) 1.34(2) . . yes F(2) F(2A) 1.04(2) . . yes F(2) C(2) 1.39(1) . . yes F(2) C(2A) 1.27(2) . . yes F(2A) C(2) 1.66(2) . . yes F(2A) C(2A) 1.30(2) . . yes F(3) F(3) 1.27(2) . 4_656 yes F(3) F(4) 1.07(1) . 4_656 yes F(3) C(3) 1.31(1) . . yes F(4) C(3) 1.43(1) . . yes O(31) C(31) 1.117(7) . . yes O(32) C(32) 1.124(7) . . yes C(1) C(1) 1.349(9) . 4_656 yes C(1) C(2) 1.49(1) . . yes C(1) C(2A) 1.50(1) . . yes C(1) C(12) 1.450(7) . . yes C(2) C(2A) 0.42(2) . . yes C(2) C(3) 1.58(1) . . yes C(2A) C(3) 1.45(2) . . yes C(11) C(12) 1.385(7) . . yes C(11) C(15) 1.500(8) . . yes C(12) C(13) 1.454(7) . . yes C(13) C(14) 1.347(7) . . yes C(21) C(22) 1.406(9) . . yes C(21) C(25) 1.410(9) . . yes C(22) C(23) 1.406(10) . . yes C(23) C(24) 1.41(1) . . yes C(24) C(25) 1.41(1) . . yes C(41) C(41) 1.76(8) . 4_655 yes C(13) H(1) 0.953 . . yes C(15) H(2) 0.987 . . yes C(15) H(3) 0.938 . . yes C(15) H(4) 0.943 . . yes C(21) H(5) 0.957 . . yes C(22) H(6) 0.970 . . yes C(23) H(7) 0.953 . . yes C(24) H(8) 0.964 . . yes C(25) H(9) 0.970 . . yes C(41) H(10) 0.964 . . yes C(41) H(11) 0.976 . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(14) Ru(1) C(21) 114.4(2) . . . yes C(14) Ru(1) C(22) 150.4(2) . . . yes C(14) Ru(1) C(23) 142.3(2) . . . yes C(14) Ru(1) C(24) 106.2(2) . . . yes C(14) Ru(1) C(25) 92.9(2) . . . yes C(14) Ru(1) C(31) 87.3(2) . . . yes C(14) Ru(1) C(32) 88.7(2) . . . yes C(21) Ru(1) C(22) 36.2(2) . . . yes C(21) Ru(1) C(23) 60.5(2) . . . yes C(21) Ru(1) C(24) 60.8(2) . . . yes C(21) Ru(1) C(25) 36.2(2) . . . yes C(21) Ru(1) C(31) 156.4(2) . . . yes C(21) Ru(1) C(32) 98.8(2) . . . yes C(22) Ru(1) C(23) 36.4(2) . . . yes C(22) Ru(1) C(24) 61.0(2) . . . yes C(22) Ru(1) C(25) 60.4(2) . . . yes C(22) Ru(1) C(31) 121.1(2) . . . yes C(22) Ru(1) C(32) 98.3(2) . . . yes C(23) Ru(1) C(24) 36.7(3) . . . yes C(23) Ru(1) C(25) 60.7(3) . . . yes C(23) Ru(1) C(31) 96.8(2) . . . yes C(23) Ru(1) C(32) 128.5(3) . . . yes C(24) Ru(1) C(25) 36.5(3) . . . yes C(24) Ru(1) C(31) 105.8(3) . . . yes C(24) Ru(1) C(32) 158.2(3) . . . yes C(25) Ru(1) C(31) 140.4(2) . . . yes C(25) Ru(1) C(32) 129.3(3) . . . yes C(31) Ru(1) C(32) 90.3(2) . . . yes C(41) Cl(1) C(41) 62(2) . . 4_655 yes C(11) S(1) C(14) 94.6(2) . . . yes C(1) C(1) C(2) 112.4(5) 4_656 . . yes C(1) C(1) C(2A) 108.3(6) 4_656 . . yes C(1) C(1) C(12) 130.0(3) 4_656 . . yes C(2) C(1) C(12) 117.5(6) . . . yes C(2A) C(1) C(12) 120.7(7) . . . yes F(1) C(2) F(2) 104(1) . . . yes F(1) C(2) C(1) 116.4(10) . . . yes F(1) C(2) C(3) 108.2(9) . . . yes F(2) C(2) C(1) 112.2(9) . . . yes F(2) C(2) C(3) 114.2(9) . . . yes C(1) C(2) C(3) 102.1(8) . . . yes F(1A) C(2A) F(2A) 107(1) . . . yes F(1A) C(2A) C(3) 109(1) . . . yes F(2A) C(2A) C(1) 113(1) . . . yes F(2A) C(2A) C(3) 106(1) . . . yes C(1) C(2A) C(3) 108(1) . . . yes F(3) C(3) F(4) 100.9(7) . . . yes F(3) C(3) C(2) 112.7(6) . . . yes F(3) C(3) C(2) 130.7(6) . . 4_656 yes F(3) C(3) C(2A) 121.5(7) . . . yes F(3) C(3) C(2A) 122.3(7) . . 4_656 yes F(3) C(3) F(4) 45.7(6) 4_656 . . yes F(3) C(3) F(4) 100.9(7) 4_656 . 4_656 yes F(3) C(3) C(2) 130.7(6) 4_656 . . yes F(3) C(3) C(2) 112.7(6) 4_656 . 4_656 yes F(3) C(3) C(2A) 122.3(7) 4_656 . . yes F(3) C(3) C(2A) 121.5(7) 4_656 . 4_656 yes F(4) C(3) C(2) 102.9(6) . . . yes F(4) C(3) C(2) 97.0(6) . . 4_656 yes F(4) C(3) C(2A) 112.3(7) . . 4_656 yes F(4) C(3) C(2) 97.0(6) 4_656 . . yes F(4) C(3) C(2) 102.9(6) 4_656 . 4_656 yes F(4) C(3) C(2A) 112.3(7) 4_656 . . yes F(4) C(3) C(2A) 88.4(7) 4_656 . 4_656 yes C(2) C(3) C(2) 107.3(9) . . 4_656 yes C(2) C(3) C(2A) 104.4(8) . . 4_656 yes C(2) C(3) C(2A) 104.4(8) 4_656 . . yes S(1) C(11) C(12) 110.0(4) . . . yes S(1) C(11) C(15) 120.8(4) . . . yes C(12) C(11) C(15) 129.2(5) . . . yes C(1) C(12) C(11) 124.4(4) . . . yes C(1) C(12) C(13) 124.3(4) . . . yes C(11) C(12) C(13) 111.2(4) . . . yes C(12) C(13) C(14) 115.4(4) . . . yes Ru(1) C(14) S(1) 119.0(3) . . . yes Ru(1) C(14) C(13) 132.3(4) . . . yes S(1) C(14) C(13) 108.7(4) . . . yes Ru(1) C(21) C(22) 71.0(4) . . . yes Ru(1) C(21) C(25) 71.6(4) . . . yes C(22) C(21) C(25) 107.9(6) . . . yes Ru(1) C(22) C(21) 72.8(3) . . . yes Ru(1) C(22) C(23) 71.5(4) . . . yes C(21) C(22) C(23) 108.3(6) . . . yes Ru(1) C(23) C(22) 72.1(4) . . . yes Ru(1) C(23) C(24) 71.2(4) . . . yes C(22) C(23) C(24) 108.0(6) . . . yes Ru(1) C(24) C(23) 72.1(4) . . . yes Ru(1) C(24) C(25) 73.0(4) . . . yes C(23) C(24) C(25) 107.8(6) . . . yes Ru(1) C(25) C(21) 72.3(4) . . . yes Ru(1) C(25) C(24) 70.4(4) . . . yes C(21) C(25) C(24) 108.0(7) . . . yes Ru(1) C(31) O(31) 176.7(5) . . . yes Ru(1) C(32) O(32) 177.5(5) . . . yes Cl(1) C(41) Cl(1) 102(2) . . 4_655 yes Cl(1) C(41) C(41) 59(1) . . 4_655 yes Cl(1) C(41) C(41) 58(1) 4_655 . 4_655 yes C(12) C(13) H(1) 121.70 . . . yes C(14) C(13) H(1) 122.84 . . . yes C(11) C(15) H(2) 108.69 . . . yes C(11) C(15) H(3) 111.62 . . . yes C(11) C(15) H(4) 110.77 . . . yes H(2) C(15) H(3) 107.44 . . . yes H(2) C(15) H(4) 106.97 . . . yes H(3) C(15) H(4) 111.15 . . . yes Ru(1) C(21) H(5) 124.33 . . . yes C(22) C(21) H(5) 126.20 . . . yes C(25) C(21) H(5) 125.91 . . . yes Ru(1) C(22) H(6) 123.05 . . . yes C(21) C(22) H(6) 126.24 . . . yes C(23) C(22) H(6) 125.46 . . . yes Ru(1) C(23) H(7) 124.92 . . . yes C(22) C(23) H(7) 126.45 . . . yes C(24) C(23) H(7) 125.44 . . . yes Ru(1) C(24) H(8) 125.18 . . . yes C(23) C(24) H(8) 127.13 . . . yes C(25) C(24) H(8) 124.79 . . . yes Ru(1) C(25) H(9) 125.80 . . . yes C(21) C(25) H(9) 126.09 . . . yes C(24) C(25) H(9) 125.80 . . . yes Cl(1) C(41) H(10) 110.70 . . . yes Cl(1) C(41) H(11) 110.04 . . . yes Cl(1) C(41) H(10) 113.96 . . . yes Cl(1) C(41) H(11) 113.42 . . . yes C(41) C(41) H(10) 93.23 . . . yes C(41) C(41) H(11) 160.53 . . . yes H(10) C(41) H(11) 106.13 . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) Cl(1) 3.53(2) . 5_655 ? S(1) C(41) 3.44(4) . 8_555 ? S(1) O(32) 3.523(5) . 2_655 ? F(1) F(1) 2.87(2) . 5_666 ? F(1) F(4) 3.00(1) . 8_564 ? F(1) F(2A) 3.15(2) . 8_564 ? F(1) C(23) 3.41(1) . 7_655 ? F(1A) C(23) 3.12(2) . 7_655 ? F(1A) C(24) 3.54(2) . 7_655 ? F(2) O(32) 2.734(10) . 8_565 ? F(2) C(22) 3.31(1) . 2_655 ? F(2) C(24) 3.40(1) . 7_655 ? F(2) C(23) 3.52(1) . 2_655 ? F(2) C(23) 3.52(1) . 7_655 ? F(2A) O(32) 2.74(1) . 8_565 ? F(2A) C(23) 3.14(1) . 2_655 ? F(2A) C(22) 3.36(1) . 2_655 ? F(2A) C(32) 3.59(1) . 8_565 ? F(4) O(32) 3.58(1) . 8_565 ? O(31) O(32) 3.340(7) . 2_655 ? O(31) C(21) 3.341(8) . 2_655 ? O(31) C(25) 3.417(8) . 7_655 ? O(31) C(32) 3.471(8) . 2_655 ? O(31) C(22) 3.497(8) . 2_655 ? O(32) C(31) 3.343(7) . 2_654 ? O(32) C(22) 3.368(8) . 7_655 ? O(32) C(23) 3.397(8) . 7_655 ? C(11) C(14) 2.537(7) . . ? C(11) C(12) 3.447(7) . 4_656 ? C(11) C(11) 3.592(10) . 4_656 ? C(12) C(12) 3.220(9) . 4_656 ? #------------------------------------------------------------------------------ _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 #------------------------------------------------------------------------------ #===END data_compound/1RuC/1024_ _database_code_depnum_ccdc_archive 'CCDC 689367' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C29 H18 F6 O4 S2 Ru2 ' _chemical_formula_moiety 'C29 H18 F6 O4 S2 Ru2 ' _chemical_formula_weight 810.71 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.026(6) _cell_length_b 11.113(5) _cell_length_c 13.278(7) _cell_angle_alpha 97.04(2) _cell_angle_beta 98.67(2) _cell_angle_gamma 114.02(2) _cell_volume 1438(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9469 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 0.881 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 7214 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _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. ; _reflns_number_total 5194 _reflns_number_gt 4732 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1652 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4732 _refine_ls_number_parameters 390 _refine_ls_goodness_of_fit_ref 1.491 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.23 _refine_diff_density_min -1.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru -0.32747(3) -0.89598(3) -0.19503(3) 0.0307(1) Uani 1.00 d . . . Ru(2) Ru 0.62540(3) -0.47328(3) 0.29311(3) 0.0320(2) Uani 1.00 d . . . S(1) S -0.0096(1) -0.7429(1) -0.05314(8) 0.0312(2) Uani 1.00 d . . . S(2) S 0.3306(1) -0.6008(1) 0.12100(8) 0.0372(3) Uani 1.00 d . . . F(1) F 0.1429(3) -0.7987(4) 0.4573(3) 0.071(1) Uani 1.00 d . . . F(2) F 0.0541(5) -0.6594(4) 0.4600(3) 0.079(1) Uani 1.00 d . . . F(3) F -0.0820(4) -1.0048(4) 0.3724(4) 0.076(1) Uani 1.00 d . . . F(4) F -0.1523(3) -0.8854(5) 0.4643(3) 0.079(1) Uani 1.00 d . . . F(5) F -0.2657(4) -1.0075(4) 0.2309(3) 0.079(1) Uani 1.00 d . . . F(6) F -0.2518(4) -0.8165(5) 0.3009(4) 0.083(1) Uani 1.00 d . . . O(131) O -0.4631(4) -0.7405(4) -0.0952(4) 0.063(1) Uani 1.00 d . . . O(132) O -0.4913(4) -1.1345(4) -0.1077(4) 0.058(1) Uani 1.00 d . . . O(231) O 0.6291(5) -0.6281(6) 0.4634(4) 0.085(2) Uani 1.00 d . . . O(232) O 0.5856(4) -0.2535(5) 0.4211(4) 0.072(1) Uani 1.00 d . . . C(1) C -0.0687(4) -0.8109(5) 0.2243(3) 0.0322(9) Uani 1.00 d . . . C(2) C 0.0654(4) -0.7553(5) 0.2932(3) 0.0333(9) Uani 1.00 d . . . C(3) C 0.0500(4) -0.7728(5) 0.4009(4) 0.040(1) Uani 1.00 d . . . C(4) C -0.0941(6) -0.8856(7) 0.3863(4) 0.055(2) Uani 1.00 d . . . C(5) C -0.1741(4) -0.8817(5) 0.2808(4) 0.040(1) Uani 1.00 d . . . C(111) C 0.0418(4) -0.6983(5) 0.0911(3) 0.0305(8) Uani 1.00 d . . . C(112) C -0.0850(4) -0.7940(4) 0.1238(3) 0.0287(8) Uani 1.00 d . . . C(113) C -0.2050(4) -0.8467(4) 0.0417(4) 0.0341(9) Uani 1.00 d . . . C(114) C -0.1840(4) -0.8298(4) -0.0542(3) 0.0292(8) Uani 1.00 d . . . C(115) C 0.0632(5) -0.5522(4) 0.1278(4) 0.044(1) Uani 1.00 d . . . C(121) C -0.324(1) -1.0182(7) -0.3424(6) 0.087(3) Uani 1.00 d . . . C(122) C -0.1949(6) -0.9251(6) -0.2991(4) 0.053(1) Uani 1.00 d . . . C(123) C -0.1852(5) -0.7957(6) -0.2968(4) 0.046(1) Uani 1.00 d . . . C(124) C -0.3159(7) -0.8094(9) -0.3411(6) 0.071(2) Uani 1.00 d . . . C(125) C -0.4030(7) -0.945(1) -0.3676(5) 0.101(4) Uani 1.00 d . . . C(131) C -0.4118(5) -0.7974(5) -0.1323(4) 0.043(1) Uani 1.00 d . . . C(132) C -0.4288(4) -1.0430(5) -0.1412(4) 0.0389(9) Uani 1.00 d . . . C(211) C 0.1642(4) -0.7228(4) 0.1389(3) 0.0325(8) Uani 1.00 d . . . C(212) C 0.1814(4) -0.7039(5) 0.2563(3) 0.0349(9) Uani 1.00 d . . . C(213) C 0.3232(4) -0.6375(5) 0.3095(3) 0.0368(9) Uani 1.00 d . . . C(214) C 0.4133(4) -0.5817(5) 0.2504(4) 0.0364(9) Uani 1.00 d . . . C(215) C 0.1462(5) -0.8673(5) 0.0949(4) 0.042(1) Uani 1.00 d . . . C(221) C 0.6622(5) -0.5057(8) 0.1309(5) 0.063(2) Uani 1.00 d . . . C(222) C 0.7114(9) -0.3631(9) 0.1708(7) 0.079(2) Uani 1.00 d . . . C(223) C 0.8196(5) -0.3319(5) 0.2584(5) 0.053(1) Uani 1.00 d . . . C(224) C 0.8319(5) -0.4476(7) 0.2715(5) 0.054(1) Uani 1.00 d . . . C(225) C 0.7334(6) -0.5540(6) 0.1907(6) 0.059(2) Uani 1.00 d . . . C(231) C 0.6245(5) -0.5697(6) 0.3990(5) 0.052(1) Uani 1.00 d . . . C(232) C 0.5974(5) -0.3400(6) 0.3758(4) 0.046(1) Uani 1.00 d . . . H(1) H -0.2940 -0.8910 0.0537 0.0407 Uiso 1.00 calc . . . H(2) H 0.0884 -0.5288 0.2025 0.0442 Uiso 1.00 calc . . . H(3) H -0.0197 -0.5448 0.1041 0.0442 Uiso 1.00 calc . . . H(4) H 0.1343 -0.4921 0.0998 0.0442 Uiso 1.00 calc . . . H(5) H -0.3575 -1.1119 -0.3582 0.0961 Uiso 1.00 calc . . . H(6) H -0.1200 -0.9448 -0.2782 0.0626 Uiso 1.00 calc . . . H(7) H -0.1018 -0.7148 -0.2749 0.0561 Uiso 1.00 calc . . . H(8) H -0.3390 -0.7376 -0.3558 0.0892 Uiso 1.00 calc . . . H(9) H -0.4958 -0.9894 -0.4028 0.1232 Uiso 1.00 calc . . . H(10) H 0.3516 -0.6332 0.3820 0.0436 Uiso 1.00 calc . . . H(11) H 0.0667 -0.9326 0.1114 0.0419 Uiso 1.00 calc . . . H(12) H 0.2249 -0.8780 0.1255 0.0419 Uiso 1.00 calc . . . H(13) H 0.1360 -0.8803 0.0207 0.0419 Uiso 1.00 calc . . . H(14) H 0.5938 -0.5587 0.0700 0.0789 Uiso 1.00 calc . . . H(15) H 0.6838 -0.3011 0.1375 0.0961 Uiso 1.00 calc . . . H(16) H 0.8777 -0.2433 0.2981 0.0657 Uiso 1.00 calc . . . H(17) H 0.8995 -0.4545 0.3215 0.0650 Uiso 1.00 calc . . . H(18) H 0.7230 -0.6456 0.1798 0.0688 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0237(2) 0.0393(2) 0.0235(2) 0.0097(2) 0.0020(1) 0.0051(2) Ru(2) 0.0199(2) 0.0436(2) 0.0258(2) 0.0082(2) 0.0046(1) 0.0043(2) S(1) 0.0237(5) 0.0423(5) 0.0230(5) 0.0096(4) 0.0047(4) 0.0085(4) S(2) 0.0220(5) 0.0542(6) 0.0273(5) 0.0076(5) 0.0042(4) 0.0132(5) F(1) 0.049(2) 0.118(3) 0.042(2) 0.028(2) 0.009(1) 0.037(2) F(2) 0.097(3) 0.074(2) 0.042(2) 0.015(2) 0.025(2) -0.007(2) F(3) 0.071(2) 0.069(2) 0.078(3) 0.019(2) 0.004(2) 0.029(2) F(4) 0.049(2) 0.135(3) 0.037(2) 0.019(2) 0.021(1) 0.029(2) F(5) 0.053(2) 0.082(2) 0.051(2) -0.018(2) 0.008(2) 0.013(2) F(6) 0.063(2) 0.149(4) 0.084(3) 0.071(3) 0.050(2) 0.064(3) O(131) 0.066(3) 0.066(2) 0.070(3) 0.042(2) 0.018(2) 0.008(2) O(132) 0.046(2) 0.055(2) 0.069(3) 0.011(2) 0.020(2) 0.024(2) O(231) 0.068(3) 0.123(4) 0.074(3) 0.039(3) 0.020(2) 0.065(3) O(232) 0.054(2) 0.088(3) 0.069(3) 0.039(2) 0.007(2) -0.017(3) C(1) 0.023(2) 0.042(2) 0.024(2) 0.007(2) 0.003(2) 0.007(2) C(2) 0.023(2) 0.048(2) 0.023(2) 0.009(2) 0.004(2) 0.007(2) C(3) 0.029(2) 0.062(3) 0.026(2) 0.015(2) 0.006(2) 0.012(2) C(4) 0.037(3) 0.080(4) 0.035(3) 0.010(3) 0.014(2) 0.020(3) C(5) 0.026(2) 0.057(3) 0.031(2) 0.013(2) 0.006(2) 0.012(2) C(111) 0.024(2) 0.043(2) 0.024(2) 0.013(2) 0.009(1) 0.007(2) C(112) 0.024(2) 0.039(2) 0.022(2) 0.013(2) 0.007(1) 0.006(2) C(113) 0.019(2) 0.044(2) 0.031(2) 0.007(2) 0.007(2) 0.004(2) C(114) 0.021(2) 0.038(2) 0.024(2) 0.010(1) 0.000(1) 0.003(2) C(115) 0.044(3) 0.037(2) 0.051(3) 0.018(2) 0.007(2) 0.009(2) C(121) 0.123(7) 0.057(3) 0.040(3) -0.001(4) 0.036(4) -0.012(3) C(122) 0.063(3) 0.080(4) 0.038(3) 0.048(3) 0.024(2) 0.015(3) C(123) 0.042(3) 0.059(3) 0.037(3) 0.016(2) 0.017(2) 0.017(2) C(124) 0.064(4) 0.123(6) 0.054(4) 0.054(4) 0.024(3) 0.053(4) C(125) 0.052(4) 0.176(9) 0.023(3) 0.001(5) -0.003(2) 0.018(4) C(131) 0.035(2) 0.046(2) 0.040(3) 0.013(2) 0.000(2) 0.011(2) C(132) 0.030(2) 0.047(2) 0.034(2) 0.013(2) 0.006(2) 0.004(2) C(211) 0.023(2) 0.044(2) 0.027(2) 0.011(2) 0.007(1) 0.008(2) C(212) 0.025(2) 0.047(2) 0.027(2) 0.011(2) 0.005(2) 0.009(2) C(213) 0.022(2) 0.055(2) 0.026(2) 0.010(2) 0.004(1) 0.007(2) C(214) 0.023(2) 0.048(2) 0.030(2) 0.010(2) 0.001(2) 0.006(2) C(215) 0.045(2) 0.045(2) 0.042(3) 0.026(2) 0.009(2) 0.009(2) C(221) 0.035(2) 0.101(5) 0.036(3) 0.016(3) 0.012(2) -0.003(3) C(222) 0.094(5) 0.113(6) 0.093(6) 0.074(5) 0.074(5) 0.074(5) C(223) 0.036(2) 0.049(3) 0.059(3) 0.002(2) 0.023(2) 0.001(2) C(224) 0.025(2) 0.086(4) 0.053(3) 0.022(2) 0.014(2) 0.019(3) C(225) 0.048(3) 0.054(3) 0.076(4) 0.019(3) 0.037(3) 0.004(3) C(231) 0.032(2) 0.072(3) 0.048(3) 0.015(2) 0.007(2) 0.020(3) C(232) 0.029(2) 0.066(3) 0.034(2) 0.015(2) 0.008(2) -0.002(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) C(114) 2.089(4) . . yes Ru(1) C(121) 2.254(8) . . yes Ru(1) C(122) 2.244(7) . . yes Ru(1) C(123) 2.261(6) . . yes Ru(1) C(124) 2.267(8) . . yes Ru(1) C(125) 2.234(6) . . yes Ru(1) C(131) 1.897(6) . . yes Ru(1) C(132) 1.863(5) . . yes Ru(2) C(214) 2.093(4) . . yes Ru(2) C(221) 2.265(6) . . yes Ru(2) C(222) 2.246(10) . . yes Ru(2) C(223) 2.237(5) . . yes Ru(2) C(224) 2.244(6) . . yes Ru(2) C(225) 2.265(8) . . yes Ru(2) C(231) 1.868(7) . . yes Ru(2) C(232) 1.890(6) . . yes S(1) C(111) 1.856(4) . . yes S(1) C(114) 1.763(4) . . yes S(2) C(211) 1.856(4) . . yes S(2) C(214) 1.764(5) . . yes F(1) C(3) 1.325(7) . . yes F(2) C(3) 1.381(7) . . yes F(3) C(4) 1.378(9) . . yes F(4) C(4) 1.298(8) . . yes F(5) C(5) 1.355(5) . . yes F(6) C(5) 1.362(8) . . yes O(131) C(131) 1.122(8) . . yes O(132) C(132) 1.157(6) . . yes O(231) C(231) 1.143(10) . . yes O(232) C(232) 1.133(9) . . yes C(1) C(2) 1.454(6) . . yes C(1) C(5) 1.482(7) . . yes C(1) C(112) 1.366(6) . . yes C(2) C(3) 1.492(7) . . yes C(2) C(212) 1.366(6) . . yes C(3) C(4) 1.536(7) . . yes C(4) C(5) 1.554(8) . . yes C(111) C(112) 1.536(6) . . yes C(111) C(115) 1.546(7) . . yes C(111) C(211) 1.543(7) . . yes C(112) C(113) 1.435(5) . . yes C(113) C(114) 1.350(6) . . yes C(121) C(122) 1.358(9) . . yes C(121) C(125) 1.44(2) . . yes C(122) C(123) 1.394(10) . . yes C(123) C(124) 1.41(1) . . yes C(124) C(125) 1.38(1) . . yes C(211) C(212) 1.520(6) . . yes C(211) C(215) 1.561(7) . . yes C(212) C(213) 1.445(5) . . yes C(213) C(214) 1.357(7) . . yes C(221) C(222) 1.45(1) . . yes C(221) C(225) 1.34(1) . . yes C(222) C(223) 1.43(1) . . yes C(223) C(224) 1.38(1) . . yes C(224) C(225) 1.423(7) . . yes C(113) H(1) 0.951 . . yes C(115) H(2) 0.960 . . yes C(115) H(3) 0.960 . . yes C(115) H(4) 0.960 . . yes C(121) H(5) 0.937 . . yes C(122) H(6) 0.949 . . yes C(123) H(7) 0.959 . . yes C(124) H(8) 0.963 . . yes C(125) H(9) 0.948 . . yes C(213) H(10) 0.955 . . yes C(215) H(11) 0.960 . . yes C(215) H(12) 0.960 . . yes C(215) H(13) 0.960 . . yes C(221) H(14) 0.952 . . yes C(222) H(15) 0.983 . . yes C(223) H(16) 0.957 . . yes C(224) H(17) 0.955 . . yes C(225) H(18) 0.967 . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(114) Ru(1) C(121) 126.4(3) . . . yes C(114) Ru(1) C(122) 97.6(2) . . . yes C(114) Ru(1) C(123) 98.1(2) . . . yes C(114) Ru(1) C(124) 129.2(2) . . . yes C(114) Ru(1) C(125) 156.8(2) . . . yes C(114) Ru(1) C(131) 87.1(2) . . . yes C(114) Ru(1) C(132) 86.9(2) . . . yes C(121) Ru(1) C(122) 35.2(3) . . . yes C(121) Ru(1) C(123) 60.0(2) . . . yes C(121) Ru(1) C(124) 60.6(3) . . . yes C(121) Ru(1) C(125) 37.4(4) . . . yes C(121) Ru(1) C(131) 146.2(3) . . . yes C(121) Ru(1) C(132) 95.7(2) . . . yes C(122) Ru(1) C(123) 36.0(2) . . . yes C(122) Ru(1) C(124) 60.1(3) . . . yes C(122) Ru(1) C(125) 60.2(3) . . . yes C(122) Ru(1) C(131) 153.2(2) . . . yes C(122) Ru(1) C(132) 117.1(2) . . . yes C(123) Ru(1) C(124) 36.3(2) . . . yes C(123) Ru(1) C(125) 60.3(2) . . . yes C(123) Ru(1) C(131) 117.2(2) . . . yes C(123) Ru(1) C(132) 153.0(2) . . . yes C(124) Ru(1) C(125) 35.7(3) . . . yes C(124) Ru(1) C(131) 96.6(3) . . . yes C(124) Ru(1) C(132) 143.5(2) . . . yes C(125) Ru(1) C(131) 109.6(4) . . . yes C(125) Ru(1) C(132) 108.6(3) . . . yes C(131) Ru(1) C(132) 89.4(2) . . . yes C(214) Ru(2) C(221) 96.1(2) . . . yes C(214) Ru(2) C(222) 112.3(3) . . . yes C(214) Ru(2) C(223) 149.5(2) . . . yes C(214) Ru(2) C(224) 149.5(2) . . . yes C(214) Ru(2) C(225) 112.9(2) . . . yes C(214) Ru(2) C(231) 88.2(2) . . . yes C(214) Ru(2) C(232) 87.1(2) . . . yes C(221) Ru(2) C(222) 37.4(3) . . . yes C(221) Ru(2) C(223) 60.8(2) . . . yes C(221) Ru(2) C(224) 59.9(2) . . . yes C(221) Ru(2) C(225) 34.4(3) . . . yes C(221) Ru(2) C(231) 131.1(3) . . . yes C(221) Ru(2) C(232) 135.3(3) . . . yes C(222) Ru(2) C(223) 37.2(3) . . . yes C(222) Ru(2) C(224) 61.2(3) . . . yes C(222) Ru(2) C(225) 60.5(3) . . . yes C(222) Ru(2) C(231) 155.4(3) . . . yes C(222) Ru(2) C(232) 100.6(3) . . . yes C(223) Ru(2) C(224) 35.7(3) . . . yes C(223) Ru(2) C(225) 60.1(2) . . . yes C(223) Ru(2) C(231) 121.8(2) . . . yes C(223) Ru(2) C(232) 95.9(2) . . . yes C(224) Ru(2) C(225) 36.8(2) . . . yes C(224) Ru(2) C(231) 94.2(3) . . . yes C(224) Ru(2) C(232) 123.0(2) . . . yes C(225) Ru(2) C(231) 99.9(3) . . . yes C(225) Ru(2) C(232) 156.1(2) . . . yes C(231) Ru(2) C(232) 93.5(3) . . . yes C(111) S(1) C(114) 93.5(2) . . . yes C(211) S(2) C(214) 93.0(2) . . . yes C(2) C(1) C(5) 109.8(4) . . . yes C(2) C(1) C(112) 121.4(4) . . . yes C(5) C(1) C(112) 128.8(4) . . . yes C(1) C(2) C(3) 109.2(4) . . . yes C(1) C(2) C(212) 121.5(4) . . . yes C(3) C(2) C(212) 129.2(4) . . . yes F(1) C(3) F(2) 104.6(4) . . . yes F(1) C(3) C(2) 116.5(5) . . . yes F(1) C(3) C(4) 111.9(5) . . . yes F(2) C(3) C(2) 111.9(5) . . . yes F(2) C(3) C(4) 107.2(5) . . . yes C(2) C(3) C(4) 104.6(3) . . . yes F(3) C(4) F(4) 106.1(6) . . . yes F(3) C(4) C(3) 106.3(5) . . . yes F(3) C(4) C(5) 106.7(4) . . . yes F(4) C(4) C(3) 116.2(4) . . . yes F(4) C(4) C(5) 115.7(5) . . . yes C(3) C(4) C(5) 105.1(5) . . . yes F(5) C(5) F(6) 104.2(4) . . . yes F(5) C(5) C(1) 115.2(4) . . . yes F(5) C(5) C(4) 110.5(5) . . . yes F(6) C(5) C(1) 113.3(5) . . . yes F(6) C(5) C(4) 108.3(5) . . . yes C(1) C(5) C(4) 105.2(4) . . . yes S(1) C(111) C(112) 102.8(2) . . . yes S(1) C(111) C(115) 108.9(4) . . . yes S(1) C(111) C(211) 115.1(3) . . . yes C(112) C(111) C(115) 108.5(4) . . . yes C(112) C(111) C(211) 108.4(4) . . . yes C(115) C(111) C(211) 112.5(3) . . . yes C(1) C(112) C(111) 117.0(3) . . . yes C(1) C(112) C(113) 130.5(4) . . . yes C(111) C(112) C(113) 112.4(4) . . . yes C(112) C(113) C(114) 115.9(4) . . . yes Ru(1) C(114) S(1) 119.5(2) . . . yes Ru(1) C(114) C(113) 128.5(3) . . . yes S(1) C(114) C(113) 112.0(3) . . . yes Ru(1) C(121) C(122) 72.0(4) . . . yes Ru(1) C(121) C(125) 70.6(5) . . . yes C(122) C(121) C(125) 106.8(7) . . . yes Ru(1) C(122) C(121) 72.8(5) . . . yes Ru(1) C(122) C(123) 72.7(4) . . . yes C(121) C(122) C(123) 110.2(7) . . . yes Ru(1) C(123) C(122) 71.3(4) . . . yes Ru(1) C(123) C(124) 72.0(4) . . . yes C(122) C(123) C(124) 107.2(5) . . . yes Ru(1) C(124) C(123) 71.6(4) . . . yes Ru(1) C(124) C(125) 70.9(5) . . . yes C(123) C(124) C(125) 107.9(9) . . . yes Ru(1) C(125) C(121) 72.0(4) . . . yes Ru(1) C(125) C(124) 73.4(4) . . . yes C(121) C(125) C(124) 107.9(7) . . . yes Ru(1) C(131) O(131) 179.1(4) . . . yes Ru(1) C(132) O(132) 179.7(5) . . . yes S(2) C(211) C(111) 114.2(3) . . . yes S(2) C(211) C(212) 103.9(2) . . . yes S(2) C(211) C(215) 107.8(3) . . . yes C(111) C(211) C(212) 109.8(4) . . . yes C(111) C(211) C(215) 112.0(3) . . . yes C(212) C(211) C(215) 108.7(4) . . . yes C(2) C(212) C(211) 116.8(3) . . . yes C(2) C(212) C(213) 131.3(4) . . . yes C(211) C(212) C(213) 111.8(4) . . . yes C(212) C(213) C(214) 116.0(4) . . . yes Ru(2) C(214) S(2) 118.5(2) . . . yes Ru(2) C(214) C(213) 129.7(3) . . . yes S(2) C(214) C(213) 111.7(3) . . . yes Ru(2) C(221) C(222) 70.6(5) . . . yes Ru(2) C(221) C(225) 72.8(4) . . . yes C(222) C(221) C(225) 109.3(6) . . . yes Ru(2) C(222) C(221) 72.0(4) . . . yes Ru(2) C(222) C(223) 71.0(5) . . . yes C(221) C(222) C(223) 104.8(8) . . . yes Ru(2) C(223) C(222) 71.8(4) . . . yes Ru(2) C(223) C(224) 72.4(3) . . . yes C(222) C(223) C(224) 109.2(5) . . . yes Ru(2) C(224) C(223) 71.8(4) . . . yes Ru(2) C(224) C(225) 72.4(4) . . . yes C(223) C(224) C(225) 107.5(5) . . . yes Ru(2) C(225) C(221) 72.8(4) . . . yes Ru(2) C(225) C(224) 70.8(4) . . . yes C(221) C(225) C(224) 109.3(6) . . . yes Ru(2) C(231) O(231) 177.2(6) . . . yes Ru(2) C(232) O(232) 174.8(5) . . . yes C(112) C(113) H(1) 122.38 . . . yes C(114) C(113) H(1) 121.76 . . . yes C(111) C(115) H(2) 109.47 . . . yes C(111) C(115) H(3) 109.47 . . . yes C(111) C(115) H(4) 109.47 . . . yes H(2) C(115) H(3) 109.46 . . . yes H(2) C(115) H(4) 109.47 . . . yes H(3) C(115) H(4) 109.48 . . . yes Ru(1) C(121) H(5) 125.77 . . . yes C(122) C(121) H(5) 127.92 . . . yes C(125) C(121) H(5) 125.15 . . . yes Ru(1) C(122) H(6) 124.93 . . . yes C(121) C(122) H(6) 125.15 . . . yes C(123) C(122) H(6) 124.45 . . . yes Ru(1) C(123) H(7) 126.41 . . . yes C(122) C(123) H(7) 124.60 . . . yes C(124) C(123) H(7) 127.99 . . . yes Ru(1) C(124) H(8) 126.98 . . . yes C(123) C(124) H(8) 126.17 . . . yes C(125) C(124) H(8) 125.76 . . . yes Ru(1) C(125) H(9) 125.02 . . . yes C(121) C(125) H(9) 121.87 . . . yes C(124) C(125) H(9) 129.93 . . . yes C(212) C(213) H(10) 121.88 . . . yes C(214) C(213) H(10) 122.07 . . . yes C(211) C(215) H(11) 109.47 . . . yes C(211) C(215) H(12) 109.47 . . . yes C(211) C(215) H(13) 109.47 . . . yes H(11) C(215) H(12) 109.48 . . . yes H(11) C(215) H(13) 109.47 . . . yes H(12) C(215) H(13) 109.47 . . . yes Ru(2) C(221) H(14) 125.32 . . . yes C(222) C(221) H(14) 127.17 . . . yes C(225) C(221) H(14) 123.50 . . . yes Ru(2) C(222) H(15) 127.70 . . . yes C(221) C(222) H(15) 126.09 . . . yes C(223) C(222) H(15) 128.60 . . . yes Ru(2) C(223) H(16) 125.28 . . . yes C(222) C(223) H(16) 124.80 . . . yes C(224) C(223) H(16) 125.87 . . . yes Ru(2) C(224) H(17) 125.62 . . . yes C(223) C(224) H(17) 126.64 . . . yes C(225) C(224) H(17) 125.62 . . . yes Ru(2) C(225) H(18) 124.55 . . . yes C(221) C(225) H(18) 126.07 . . . yes C(224) C(225) H(18) 124.61 . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(2) O(131) 3.550(5) . 2_545 ? F(1) O(232) 2.967(6) . 2_646 ? F(1) C(232) 3.024(5) . 2_646 ? F(1) F(3) 3.288(7) . 2_536 ? F(2) C(231) 3.470(6) . 2_646 ? F(2) C(224) 3.477(7) . 2_646 ? F(2) O(231) 3.535(6) . 2_646 ? F(3) C(223) 3.410(7) . 1_445 ? F(3) F(3) 3.561(9) . 2_536 ? F(4) C(122) 3.302(7) . 1_556 ? F(4) C(123) 3.325(7) . 1_556 ? F(4) C(121) 3.533(9) . 1_556 ? F(4) C(124) 3.571(10) . 1_556 ? F(5) O(131) 3.218(5) . 2_435 ? F(5) C(131) 3.269(5) . 2_435 ? F(6) O(132) 3.335(6) . 2_435 ? F(6) C(132) 3.436(6) . 2_435 ? F(6) C(225) 3.471(9) . 1_455 ? F(6) O(231) 3.570(9) . 1_455 ? O(131) O(132) 3.193(7) . 2_435 ? O(131) C(221) 3.409(8) . 1_455 ? O(131) C(222) 3.44(1) . 2_545 ? O(132) C(225) 3.314(6) . 2_535 ? O(132) C(113) 3.519(7) . 2_435 ? O(132) C(131) 3.581(8) . 2_435 ? O(231) O(232) 2.957(8) . 2_646 ? O(231) C(232) 3.463(8) . 2_646 ? O(232) C(124) 3.37(1) . 2_545 ? O(232) C(121) 3.553(9) . 1_666 ? C(114) C(215) 3.543(8) . 2_535 ? #------------------------------------------------------------------------------ _diffrn_measured_fraction_theta_max 0.787 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.787 #------------------------------------------------------------------------------ #===END data_compound/2Fe/1034_ _database_code_depnum_ccdc_archive 'CCDC 689368' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C63 H48 F6 Fe2 O2 P2 S2 ' _chemical_formula_moiety 'C63 H48 F6 Fe2 O2 P2 S2 ' _chemical_formula_weight 1188.82 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z _cell_length_a 8.607(6) _cell_length_b 16.521(9) _cell_length_c 20.230(10) _cell_angle_alpha 90 _cell_angle_beta 100.12(2) _cell_angle_gamma 90 _cell_volume 2832(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 16681 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213.2 #------------------------------------------------------------------------------ _exptl_crystal_description cube _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.932 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 22615 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 #------------------------------------------------------------------------------ # REFINEMENT DATA _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. ; _reflns_number_total 6387 _reflns_number_gt 3973 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1225 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1981 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3973 _refine_ls_number_parameters 388 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.72 _refine_diff_density_min -0.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe 0.13520(9) 0.27618(4) 0.01744(3) 0.0325(2) Uani 1.00 d . . . S(1) S 0.2298(2) 0.28500(7) -0.12958(6) 0.0378(3) Uani 1.00 d . . . P(1) P -0.1239(2) 0.28649(7) 0.00501(6) 0.0314(3) Uani 1.00 d . . . F(1) F 0.202(4) -0.020(2) -0.1546(9) 0.066(4) Uani 0.50 d P . . F(1A) F 0.210(4) -0.011(2) -0.173(1) 0.084(6) Uani 0.50 d P . . F(2) F -0.052(5) -0.013(3) -0.148(2) 0.069(7) Uani 0.50 d P . . F(2A) F -0.006(5) -0.011(3) -0.135(2) 0.070(8) Uani 0.50 d P . . F(3) F 0.161(2) -0.0814(8) -0.2670(6) 0.112(6) Uani 0.50 d P . . F(4) F -0.058(3) -0.1183(5) -0.2455(8) 0.13(1) Uani 0.50 d P . . O(31) O 0.1769(8) 0.4431(3) -0.0168(3) 0.094(2) Uani 1.00 d . . . C(1) C 0.0354(6) 0.0860(3) -0.2172(2) 0.035(1) Uani 1.00 d . . . C(2) C 0.041(4) -0.005(2) -0.193(2) 0.040(7) Uani 0.50 d P . . C(2A) C 0.070(5) 0.009(2) -0.189(1) 0.041(7) Uani 0.50 d P . . C(3) C 0.030(6) -0.0533(6) -0.254(3) 0.06(1) Uani 0.50 d P . . C(11) C 0.1850(6) 0.2156(3) -0.1936(2) 0.034(1) Uani 1.00 d . . . C(12) C 0.0940(6) 0.1559(3) -0.1743(2) 0.032(1) Uani 1.00 d . . . C(13) C 0.0621(6) 0.1666(3) -0.1070(2) 0.033(1) Uani 1.00 d . . . C(14) C 0.1263(6) 0.2356(3) -0.0749(2) 0.033(1) Uani 1.00 d . . . C(15) C 0.2489(7) 0.2250(4) -0.2578(3) 0.049(1) Uani 1.00 d . . . C(21) C 0.2052(9) 0.1613(4) 0.0644(3) 0.065(2) Uani 1.00 d . . . C(22) C 0.1542(9) 0.2156(5) 0.1119(3) 0.066(2) Uani 1.00 d . . . C(23) C 0.244(1) 0.2881(4) 0.1187(3) 0.075(2) Uani 1.00 d . . . C(24) C 0.3567(10) 0.2839(6) 0.0800(4) 0.088(3) Uani 1.00 d . . . C(25) C 0.339(1) 0.2033(6) 0.0458(3) 0.084(3) Uani 1.00 d . . . C(31) C 0.1626(9) 0.3763(4) -0.0044(3) 0.062(2) Uani 1.00 d . . . C(41) C -0.1807(7) 0.3196(3) 0.0843(2) 0.043(1) Uani 1.00 d . . . C(42) C -0.141(1) 0.3995(4) 0.1049(3) 0.071(2) Uani 1.00 d . . . C(43) C -0.173(1) 0.4270(5) 0.1658(3) 0.086(3) Uani 1.00 d . . . C(44) C -0.2389(10) 0.3786(5) 0.2066(3) 0.077(2) Uani 1.00 d . . . C(45) C -0.2766(10) 0.3008(6) 0.1883(3) 0.077(2) Uani 1.00 d . . . C(46) C -0.2482(8) 0.2691(4) 0.1265(3) 0.055(2) Uani 1.00 d . . . C(51) C -0.2234(6) 0.3623(3) -0.0541(2) 0.035(1) Uani 1.00 d . . . C(52) C -0.1624(7) 0.3837(3) -0.1096(3) 0.048(1) Uani 1.00 d . . . C(53) C -0.2446(9) 0.4389(4) -0.1558(3) 0.067(2) Uani 1.00 d . . . C(54) C -0.3844(8) 0.4714(4) -0.1469(3) 0.058(2) Uani 1.00 d . . . C(55) C -0.4474(8) 0.4500(3) -0.0906(3) 0.055(2) Uani 1.00 d . . . C(56) C -0.3677(8) 0.3967(3) -0.0454(3) 0.050(1) Uani 1.00 d . . . C(61) C -0.2404(6) 0.1948(3) -0.0198(2) 0.034(1) Uani 1.00 d . . . C(62) C -0.3638(7) 0.1942(3) -0.0746(2) 0.038(1) Uani 1.00 d . . . C(63) C -0.4444(8) 0.1234(4) -0.0939(3) 0.053(2) Uani 1.00 d . . . C(64) C -0.4027(8) 0.0514(3) -0.0605(3) 0.054(2) Uani 1.00 d . . . C(65) C -0.2815(8) 0.0520(3) -0.0055(3) 0.050(1) Uani 1.00 d . . . C(66) C -0.2015(7) 0.1222(3) 0.0131(2) 0.042(1) Uani 1.00 d . . . H(1) H 0.0018 0.1287 -0.0865 0.0400 Uiso 1.00 calc . . . H(2) H 0.3147 0.1798 -0.2637 0.0618 Uiso 1.00 calc . . . H(3) H 0.1642 0.2272 -0.2952 0.0618 Uiso 1.00 calc . . . H(4) H 0.3095 0.2732 -0.2567 0.0618 Uiso 1.00 calc . . . H(5) H 0.1637 0.1077 0.0501 0.0814 Uiso 1.00 calc . . . H(6) H 0.0639 0.2054 0.1336 0.0800 Uiso 1.00 calc . . . H(7) H 0.2278 0.3333 0.1475 0.0885 Uiso 1.00 calc . . . H(8) H 0.4399 0.3226 0.0766 0.1083 Uiso 1.00 calc . . . H(9) H 0.4036 0.1816 0.0150 0.1002 Uiso 1.00 calc . . . H(10) H -0.0935 0.4345 0.0759 0.0872 Uiso 1.00 calc . . . H(11) H -0.1443 0.4820 0.1792 0.1029 Uiso 1.00 calc . . . H(12) H -0.2635 0.3976 0.2484 0.0937 Uiso 1.00 calc . . . H(13) H -0.3241 0.2651 0.2173 0.0906 Uiso 1.00 calc . . . H(14) H -0.2728 0.2137 0.1132 0.0699 Uiso 1.00 calc . . . H(15) H -0.0623 0.3604 -0.1169 0.0594 Uiso 1.00 calc . . . H(16) H -0.2023 0.4525 -0.1964 0.0777 Uiso 1.00 calc . . . H(17) H -0.4375 0.5096 -0.1793 0.0691 Uiso 1.00 calc . . . H(18) H -0.5466 0.4735 -0.0833 0.0700 Uiso 1.00 calc . . . H(19) H -0.4108 0.3818 -0.0056 0.0599 Uiso 1.00 calc . . . H(20) H -0.3931 0.2431 -0.0989 0.0470 Uiso 1.00 calc . . . H(21) H -0.5315 0.1242 -0.1315 0.0632 Uiso 1.00 calc . . . H(22) H -0.4553 0.0013 -0.0747 0.0648 Uiso 1.00 calc . . . H(23) H -0.2546 0.0035 0.0205 0.0578 Uiso 1.00 calc . . . H(24) H -0.1149 0.1210 0.0503 0.0496 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0388(5) 0.0319(4) 0.0251(3) -0.0037(3) 0.0004(3) -0.0009(3) S(1) 0.0401(8) 0.0411(7) 0.0316(6) -0.0087(6) 0.0048(5) 0.0010(5) P(1) 0.0410(8) 0.0275(6) 0.0251(5) 0.0010(5) 0.0037(5) 0.0009(4) F(1) 0.101(10) 0.054(8) 0.035(6) 0.014(7) -0.009(6) 0.030(5) F(1A) 0.09(1) 0.061(7) 0.09(2) 0.037(7) 0.00(1) 0.04(1) F(2) 0.10(2) 0.052(8) 0.06(2) -0.03(1) 0.03(1) 0.00(1) F(2A) 0.11(2) 0.05(1) 0.04(1) 0.00(1) 0.014(9) 0.018(8) F(3) 0.18(2) 0.106(10) 0.040(6) 0.08(1) -0.002(7) -0.006(6) F(4) 0.30(5) 0.048(5) 0.048(7) -0.07(1) 0.04(2) -0.007(8) O(31) 0.122(5) 0.049(3) 0.105(4) -0.029(3) 0.003(3) 0.001(3) C(1) 0.046(3) 0.035(3) 0.024(2) 0.000(2) 0.005(2) 0.005(2) C(2) 0.06(1) 0.012(8) 0.04(1) -0.007(10) -0.007(8) 0.011(8) C(2A) 0.08(2) 0.03(1) 0.014(6) -0.026(9) 0.011(7) -0.013(6) C(3) 0.10(4) 0.034(5) 0.03(1) -0.005(8) 0.01(2) -0.005(7) C(11) 0.036(3) 0.041(3) 0.026(2) 0.000(2) 0.005(2) 0.000(2) C(12) 0.037(3) 0.037(2) 0.021(2) 0.004(2) 0.002(2) 0.005(2) C(13) 0.040(3) 0.033(2) 0.027(2) -0.003(2) 0.008(2) 0.001(2) C(14) 0.041(3) 0.031(2) 0.025(2) 0.001(2) -0.001(2) 0.000(2) C(15) 0.053(4) 0.063(4) 0.035(3) -0.012(3) 0.015(2) 0.001(2) C(21) 0.059(5) 0.094(5) 0.047(3) 0.006(4) 0.020(3) -0.008(3) C(22) 0.064(5) 0.090(5) 0.043(3) 0.003(4) 0.006(3) 0.018(3) C(23) 0.100(7) 0.072(5) 0.041(3) 0.008(4) -0.020(4) -0.016(3) C(24) 0.054(5) 0.122(7) 0.076(5) -0.038(5) -0.020(4) 0.022(5) C(25) 0.072(6) 0.127(7) 0.051(4) 0.041(5) 0.007(4) 0.007(4) C(31) 0.095(6) 0.040(3) 0.053(4) 0.001(3) 0.015(3) 0.002(3) C(41) 0.045(4) 0.051(3) 0.031(2) 0.017(3) 0.001(2) -0.001(2) C(42) 0.124(7) 0.044(3) 0.043(3) 0.018(4) 0.008(4) -0.009(3) C(43) 0.137(8) 0.073(5) 0.047(4) 0.040(5) 0.010(4) -0.015(3) C(44) 0.091(6) 0.103(6) 0.036(3) 0.033(5) 0.010(3) -0.017(4) C(45) 0.072(5) 0.124(6) 0.039(3) 0.006(5) 0.017(3) 0.004(4) C(46) 0.056(4) 0.080(4) 0.032(3) -0.002(3) 0.013(2) -0.002(3) C(51) 0.043(3) 0.027(2) 0.032(2) 0.000(2) 0.000(2) 0.000(2) C(52) 0.055(4) 0.045(3) 0.042(3) 0.006(3) 0.003(2) 0.013(2) C(53) 0.065(5) 0.072(4) 0.064(4) 0.004(4) 0.010(3) 0.035(3) C(54) 0.054(4) 0.047(3) 0.066(4) 0.010(3) -0.005(3) 0.016(3) C(55) 0.055(4) 0.045(3) 0.063(4) 0.014(3) 0.003(3) 0.006(3) C(56) 0.055(4) 0.051(3) 0.041(3) 0.011(3) 0.005(3) 0.005(2) C(61) 0.037(3) 0.035(2) 0.030(2) 0.000(2) 0.008(2) 0.003(2) C(62) 0.040(3) 0.037(2) 0.037(2) -0.001(2) 0.004(2) 0.003(2) C(63) 0.055(4) 0.051(3) 0.049(3) -0.003(3) -0.005(3) -0.001(3) C(64) 0.064(5) 0.040(3) 0.055(3) -0.015(3) 0.005(3) 0.001(3) C(65) 0.062(4) 0.034(3) 0.052(3) -0.007(3) 0.007(3) 0.007(2) C(66) 0.045(3) 0.042(3) 0.036(3) -0.001(2) -0.002(2) 0.007(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe(1) P(1) 2.207(2) . . yes Fe(1) C(14) 1.974(4) . . yes Fe(1) C(21) 2.160(7) . . yes Fe(1) C(22) 2.137(6) . . yes Fe(1) C(23) 2.107(6) . . yes Fe(1) C(24) 2.099(8) . . yes Fe(1) C(25) 2.121(9) . . yes Fe(1) C(31) 1.739(6) . . yes S(1) C(11) 1.722(5) . . yes S(1) C(14) 1.740(5) . . yes P(1) C(41) 1.841(6) . . yes P(1) C(51) 1.837(4) . . yes P(1) C(61) 1.837(5) . . yes F(1) F(1A) 0.41(3) . . yes F(1) C(2) 1.49(5) . . yes F(1) C(2A) 1.32(5) . . yes F(1A) C(2) 1.44(5) . . yes F(1A) C(2A) 1.24(5) . . yes F(2) F(2A) 0.44(6) . . yes F(2) C(2) 1.31(6) . . yes F(2) C(2A) 1.49(6) . . yes F(2A) C(2) 1.31(6) . . yes F(2A) C(2A) 1.41(6) . . yes F(3) F(4) 1.14(3) . 2_554 yes F(3) C(3) 1.29(5) . . yes F(4) F(4) 1.04(5) . 2_554 yes F(4) C(3) 1.34(4) . . yes F(4) C(3) 1.10(2) . 2_554 yes O(31) C(31) 1.142(8) . . yes C(1) C(1) 1.358(8) . 2_554 yes C(1) C(2) 1.58(3) . . yes C(1) C(2A) 1.40(3) . . yes C(1) C(12) 1.479(6) . . yes C(2) C(2A) 0.35(5) . . yes C(2) C(3) 1.46(5) . . yes C(2) C(3) 1.38(5) . 2_554 yes C(2A) C(3) 1.67(5) . . yes C(2A) C(3) 1.67(5) . 2_554 yes C(3) C(3) 0.6(1) . 2_554 yes C(11) C(12) 1.358(7) . . yes C(11) C(15) 1.506(8) . . yes C(12) C(13) 1.445(6) . . yes C(13) C(14) 1.379(6) . . yes C(21) C(22) 1.44(1) . . yes C(21) C(25) 1.45(1) . . yes C(22) C(23) 1.42(1) . . yes C(23) C(24) 1.35(1) . . yes C(24) C(25) 1.50(1) . . yes C(41) C(42) 1.407(8) . . yes C(41) C(46) 1.393(8) . . yes C(42) C(43) 1.38(1) . . yes C(43) C(44) 1.34(1) . . yes C(44) C(45) 1.36(1) . . yes C(45) C(46) 1.415(9) . . yes C(51) C(52) 1.368(8) . . yes C(51) C(56) 1.404(9) . . yes C(52) C(53) 1.403(8) . . yes C(53) C(54) 1.36(1) . . yes C(54) C(55) 1.389(10) . . yes C(55) C(56) 1.364(8) . . yes C(61) C(62) 1.395(7) . . yes C(61) C(66) 1.385(7) . . yes C(62) C(63) 1.381(8) . . yes C(63) C(64) 1.383(8) . . yes C(64) C(65) 1.385(8) . . yes C(65) C(66) 1.367(7) . . yes C(13) H(1) 0.955 . . yes C(15) H(2) 0.958 . . yes C(15) H(3) 0.954 . . yes C(15) H(4) 0.951 . . yes C(21) H(5) 0.980 . . yes C(22) H(6) 0.972 . . yes C(23) H(7) 0.971 . . yes C(24) H(8) 0.972 . . yes C(25) H(9) 0.974 . . yes C(42) H(10) 0.967 . . yes C(43) H(11) 0.969 . . yes C(44) H(12) 0.959 . . yes C(45) H(13) 0.971 . . yes C(46) H(14) 0.967 . . yes C(52) H(15) 0.978 . . yes C(53) H(16) 0.982 . . yes C(54) H(17) 0.965 . . yes C(55) H(18) 0.974 . . yes C(56) H(19) 0.976 . . yes C(62) H(20) 0.957 . . yes C(63) H(21) 0.970 . . yes C(64) H(22) 0.963 . . yes C(65) H(23) 0.965 . . yes C(66) H(24) 0.962 . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Fe(1) C(14) 92.8(2) . . . yes P(1) Fe(1) C(21) 108.4(2) . . . yes P(1) Fe(1) C(22) 93.2(2) . . . yes P(1) Fe(1) C(23) 111.7(3) . . . yes P(1) Fe(1) C(24) 148.9(3) . . . yes P(1) Fe(1) C(25) 147.7(3) . . . yes P(1) Fe(1) C(31) 94.4(3) . . . yes C(14) Fe(1) C(21) 94.6(2) . . . yes C(14) Fe(1) C(22) 132.2(2) . . . yes C(14) Fe(1) C(23) 152.8(3) . . . yes C(14) Fe(1) C(24) 118.1(3) . . . yes C(14) Fe(1) C(25) 87.5(2) . . . yes C(14) Fe(1) C(31) 93.8(2) . . . yes C(21) Fe(1) C(22) 39.1(3) . . . yes C(21) Fe(1) C(23) 67.2(3) . . . yes C(21) Fe(1) C(24) 68.6(3) . . . yes C(21) Fe(1) C(25) 39.6(3) . . . yes C(21) Fe(1) C(31) 155.2(3) . . . yes C(22) Fe(1) C(23) 39.0(3) . . . yes C(22) Fe(1) C(24) 64.6(3) . . . yes C(22) Fe(1) C(25) 64.1(3) . . . yes C(22) Fe(1) C(31) 132.8(3) . . . yes C(23) Fe(1) C(24) 37.5(4) . . . yes C(23) Fe(1) C(25) 65.5(3) . . . yes C(23) Fe(1) C(31) 95.8(3) . . . yes C(24) Fe(1) C(25) 41.5(3) . . . yes C(24) Fe(1) C(31) 86.9(3) . . . yes C(25) Fe(1) C(31) 117.8(4) . . . yes C(11) S(1) C(14) 95.4(2) . . . yes Fe(1) P(1) C(41) 110.0(2) . . . yes Fe(1) P(1) C(51) 118.2(2) . . . yes Fe(1) P(1) C(61) 117.4(2) . . . yes C(41) P(1) C(51) 101.5(2) . . . yes C(41) P(1) C(61) 105.5(2) . . . yes C(51) P(1) C(61) 102.4(2) . . . yes F(1A) F(1) C(2) 75(6) . . . yes F(1A) F(1) C(2A) 70(6) . . . yes C(2) F(1) C(2A) 12(1) . . . yes F(1) F(1A) C(2) 88(7) . . . yes F(1) F(1A) C(2A) 91(7) . . . yes C(2) F(1A) C(2A) 12(1) . . . yes F(2A) F(2) C(2) 80(8) . . . yes F(2A) F(2) C(2A) 71(8) . . . yes C(2) F(2) C(2A) 12(1) . . . yes F(2) F(2A) C(2) 79(7) . . . yes F(2) F(2A) C(2A) 91(8) . . . yes C(2) F(2A) C(2A) 14(1) . . . yes F(4) F(3) C(3) 53(1) 2_554 . . yes F(3) F(4) F(4) 147(1) 2_554 . 2_554 yes F(3) F(4) C(3) 94(2) 2_554 . . yes F(3) F(4) C(3) 70(3) 2_554 . 2_554 yes F(4) F(4) C(3) 53(2) 2_554 . . yes F(4) F(4) C(3) 77(3) 2_554 . 2_554 yes C(3) F(4) C(3) 24(4) . . 2_554 yes C(1) C(1) C(2) 106(1) 2_554 . . yes C(1) C(1) C(2A) 115(1) 2_554 . . yes C(1) C(1) C(12) 128.4(2) 2_554 . . yes C(2) C(1) C(2A) 11(1) . . . yes C(2) C(1) C(12) 124(1) . . . yes C(2A) C(1) C(12) 116(1) . . . yes F(1) C(2) F(1A) 15(1) . . . yes F(1) C(2) F(2) 104(2) . . . yes F(1) C(2) F(2A) 86(2) . . . yes F(1) C(2) C(1) 106(2) . . . yes F(1) C(2) C(2A) 54(7) . . . yes F(1) C(2) C(3) 105(3) . . . yes F(1) C(2) C(3) 123(3) . . 2_554 yes F(1A) C(2) F(2) 120(2) . . . yes F(1A) C(2) F(2A) 101(2) . . . yes F(1A) C(2) C(1) 97(2) . . . yes F(1A) C(2) C(2A) 47(7) . . . yes F(1A) C(2) C(3) 96(3) . . . yes F(1A) C(2) C(3) 117(3) . . 2_554 yes F(2) C(2) F(2A) 19(2) . . . yes F(2) C(2) C(1) 108(2) . . . yes F(2) C(2) C(2A) 114(8) . . . yes F(2) C(2) C(3) 124(3) . . . yes F(2) C(2) C(3) 103(3) . . 2_554 yes F(2A) C(2) C(1) 110(2) . . . yes F(2A) C(2) C(2A) 99(7) . . . yes F(2A) C(2) C(3) 137(3) . . . yes F(2A) C(2) C(3) 119(3) . . 2_554 yes C(1) C(2) C(2A) 52(6) . . . yes C(1) C(2) C(3) 105(2) . . . yes C(1) C(2) C(3) 108(2) . . 2_554 yes C(2A) C(2) C(3) 120(8) . . . yes C(2A) C(2) C(3) 141(8) . . 2_554 yes C(3) C(2) C(3) 23(4) . . 2_554 yes F(1) C(2A) F(1A) 18(1) . . . yes F(1) C(2A) F(2) 104(2) . . . yes F(1) C(2A) F(2A) 89(2) . . . yes F(1) C(2A) C(1) 130(3) . . . yes F(1) C(2A) C(2) 113(7) . . . yes F(1) C(2A) C(3) 103(2) . . . yes F(1) C(2A) C(3) 115(2) . . 2_554 yes F(1A) C(2A) F(2) 121(2) . . . yes F(1A) C(2A) F(2A) 107(2) . . . yes F(1A) C(2A) C(1) 119(3) . . . yes F(1A) C(2A) C(2) 119(8) . . . yes F(1A) C(2A) C(3) 95(2) . . . yes F(1A) C(2A) C(3) 111(2) . . 2_554 yes F(2) C(2A) F(2A) 17(2) . . . yes F(2) C(2A) C(1) 109(3) . . . yes F(2) C(2A) C(2) 53(7) . . . yes F(2) C(2A) C(3) 102(3) . . . yes F(2) C(2A) C(3) 83(3) . . 2_554 yes F(2A) C(2A) C(1) 115(3) . . . yes F(2A) C(2A) C(2) 66(7) . . . yes F(2A) C(2A) C(3) 114(3) . . . yes F(2A) C(2A) C(3) 97(3) . . 2_554 yes C(1) C(2A) C(2) 116(7) . . . yes C(1) C(2A) C(3) 103(1) . . . yes C(1) C(2A) C(3) 103(2) . . 2_554 yes C(2) C(2A) C(3) 49(7) . . . yes C(2) C(2A) C(3) 31(7) . . 2_554 yes C(3) C(2A) C(3) 19(3) . . 2_554 yes F(3) C(3) F(4) 105(1) . . . yes F(3) C(3) F(4) 56(2) . . 2_554 yes F(3) C(3) C(2) 115(3) . . . yes F(3) C(3) C(2) 109(4) . . 2_554 yes F(3) C(3) C(2A) 108(3) . . . yes F(3) C(3) C(2A) 116(3) . . 2_554 yes F(3) C(3) C(3) 158(3) . . 2_554 yes F(4) C(3) F(4) 49(2) . . 2_554 yes F(4) C(3) C(2) 105(3) . . . yes F(4) C(3) C(2) 112(3) . . 2_554 yes F(4) C(3) C(2A) 115(3) . . . yes F(4) C(3) C(2A) 110(3) . . 2_554 yes F(4) C(3) C(3) 53(2) . . 2_554 yes F(4) C(3) C(2) 123(4) 2_554 . . yes F(4) C(3) C(2) 128(4) 2_554 . 2_554 yes F(4) C(3) C(2A) 126(3) 2_554 . . yes F(4) C(3) C(2A) 133(3) 2_554 . 2_554 yes F(4) C(3) C(3) 102(3) 2_554 . 2_554 yes C(2) C(3) C(2) 107(2) . . 2_554 yes C(2) C(3) C(2A) 10(1) . . . yes C(2) C(3) C(2A) 101(2) . . 2_554 yes C(2) C(3) C(3) 70(8) . . 2_554 yes C(2) C(3) C(2A) 104(1) 2_554 . . yes C(2) C(3) C(2A) 7(1) 2_554 . 2_554 yes C(2) C(3) C(3) 86(8) 2_554 . 2_554 yes C(2A) C(3) C(2A) 99(2) . . 2_554 yes C(2A) C(3) C(3) 80(8) . . 2_554 yes C(2A) C(3) C(3) 80(7) 2_554 . 2_554 yes S(1) C(11) C(12) 109.4(3) . . . yes S(1) C(11) C(15) 120.9(4) . . . yes C(12) C(11) C(15) 129.7(4) . . . yes C(1) C(12) C(11) 123.5(4) . . . yes C(1) C(12) C(13) 123.2(4) . . . yes C(11) C(12) C(13) 113.3(4) . . . yes C(12) C(13) C(14) 114.7(4) . . . yes Fe(1) C(14) S(1) 120.2(2) . . . yes Fe(1) C(14) C(13) 132.3(4) . . . yes S(1) C(14) C(13) 107.2(3) . . . yes Fe(1) C(21) C(22) 69.6(4) . . . yes Fe(1) C(21) C(25) 68.8(4) . . . yes C(22) C(21) C(25) 103.0(6) . . . yes Fe(1) C(22) C(21) 71.3(4) . . . yes Fe(1) C(22) C(23) 69.3(4) . . . yes C(21) C(22) C(23) 111.6(7) . . . yes Fe(1) C(23) C(22) 71.6(4) . . . yes Fe(1) C(23) C(24) 70.9(4) . . . yes C(22) C(23) C(24) 109.5(7) . . . yes Fe(1) C(24) C(23) 71.6(5) . . . yes Fe(1) C(24) C(25) 70.0(4) . . . yes C(23) C(24) C(25) 106.7(7) . . . yes Fe(1) C(25) C(21) 71.7(4) . . . yes Fe(1) C(25) C(24) 68.5(5) . . . yes C(21) C(25) C(24) 109.1(7) . . . yes Fe(1) C(31) O(31) 177.2(7) . . . yes P(1) C(41) C(42) 116.7(5) . . . yes P(1) C(41) C(46) 124.0(4) . . . yes C(42) C(41) C(46) 119.0(5) . . . yes C(41) C(42) C(43) 119.8(6) . . . yes C(42) C(43) C(44) 121.4(7) . . . yes C(43) C(44) C(45) 120.0(7) . . . yes C(44) C(45) C(46) 121.4(7) . . . yes C(41) C(46) C(45) 118.3(6) . . . yes P(1) C(51) C(52) 120.6(4) . . . yes P(1) C(51) C(56) 121.0(4) . . . yes C(52) C(51) C(56) 118.3(5) . . . yes C(51) C(52) C(53) 119.5(6) . . . yes C(52) C(53) C(54) 121.6(6) . . . yes C(53) C(54) C(55) 119.3(6) . . . yes C(54) C(55) C(56) 119.4(6) . . . yes C(51) C(56) C(55) 121.9(6) . . . yes P(1) C(61) C(62) 121.7(4) . . . yes P(1) C(61) C(66) 120.6(4) . . . yes C(62) C(61) C(66) 117.6(4) . . . yes C(61) C(62) C(63) 120.3(5) . . . yes C(62) C(63) C(64) 121.1(5) . . . yes C(63) C(64) C(65) 118.7(5) . . . yes C(64) C(65) C(66) 120.0(5) . . . yes C(61) C(66) C(65) 122.3(5) . . . yes C(12) C(13) H(1) 122.50 . . . yes C(14) C(13) H(1) 122.77 . . . yes C(11) C(15) H(2) 109.92 . . . yes C(11) C(15) H(3) 110.09 . . . yes C(11) C(15) H(4) 110.37 . . . yes H(2) C(15) H(3) 108.53 . . . yes H(2) C(15) H(4) 108.79 . . . yes H(3) C(15) H(4) 109.10 . . . yes Fe(1) C(21) H(5) 127.24 . . . yes C(22) C(21) H(5) 128.48 . . . yes C(25) C(21) H(5) 128.46 . . . yes Fe(1) C(22) H(6) 122.89 . . . yes C(21) C(22) H(6) 123.78 . . . yes C(23) C(22) H(6) 124.47 . . . yes Fe(1) C(23) H(7) 124.70 . . . yes C(22) C(23) H(7) 125.21 . . . yes C(24) C(23) H(7) 125.28 . . . yes Fe(1) C(24) H(8) 126.84 . . . yes C(23) C(24) H(8) 128.42 . . . yes C(25) C(24) H(8) 124.69 . . . yes Fe(1) C(25) H(9) 125.16 . . . yes C(21) C(25) H(9) 123.99 . . . yes C(24) C(25) H(9) 126.91 . . . yes C(41) C(42) H(10) 119.27 . . . yes C(43) C(42) H(10) 120.95 . . . yes C(42) C(43) H(11) 118.48 . . . yes C(44) C(43) H(11) 120.09 . . . yes C(43) C(44) H(12) 121.82 . . . yes C(45) C(44) H(12) 118.12 . . . yes C(44) C(45) H(13) 120.97 . . . yes C(46) C(45) H(13) 117.64 . . . yes C(41) C(46) H(14) 119.36 . . . yes C(45) C(46) H(14) 122.31 . . . yes C(51) C(52) H(15) 119.85 . . . yes C(53) C(52) H(15) 120.67 . . . yes C(52) C(53) H(16) 119.20 . . . yes C(54) C(53) H(16) 119.18 . . . yes C(53) C(54) H(17) 119.62 . . . yes C(55) C(54) H(17) 121.03 . . . yes C(54) C(55) H(18) 120.13 . . . yes C(56) C(55) H(18) 120.47 . . . yes C(51) C(56) H(19) 118.30 . . . yes C(55) C(56) H(19) 119.82 . . . yes C(61) C(62) H(20) 119.90 . . . yes C(63) C(62) H(20) 119.80 . . . yes C(62) C(63) H(21) 119.36 . . . yes C(64) C(63) H(21) 119.51 . . . yes C(63) C(64) H(22) 121.71 . . . yes C(65) C(64) H(22) 119.62 . . . yes C(64) C(65) H(23) 120.45 . . . yes C(66) C(65) H(23) 119.54 . . . yes C(61) C(66) H(24) 118.88 . . . yes C(65) C(66) H(24) 118.82 . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(65) 3.24(2) . 3_555 ? F(1) C(66) 3.33(2) . 3_555 ? F(2) C(21) 3.38(5) . 3_555 ? F(2) C(22) 3.57(5) . 3_555 ? F(2A) C(66) 3.33(4) . 3_555 ? F(2A) C(21) 3.47(5) . 3_555 ? F(2A) C(65) 3.49(4) . 3_555 ? F(3) C(22) 3.30(1) . 4_554 ? F(4) C(22) 3.37(2) . 3_555 ? O(31) C(42) 3.138(8) . 3_565 ? O(31) C(56) 3.250(8) . 3_565 ? O(31) C(55) 3.390(8) . 3_565 ? O(31) C(51) 3.515(6) . 3_565 ? C(24) C(46) 3.37(1) . 1_655 ? C(24) C(45) 3.52(1) . 1_655 ? C(11) C(11) 3.578(9) . 2_554 ? #------------------------------------------------------------------------------ _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 #------------------------------------------------------------------------------ #===END data_compound/[2FeC'2+](PF6)2/1070_ _database_code_depnum_ccdc_archive 'CCDC 689369' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C66 H48 F18 Fe2 O3 P4 S2 ' _chemical_formula_moiety 'C66 H48 F18 Fe2 O3 P4 S2 ' _chemical_formula_weight 1530.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 13.983(3) _cell_length_b 15.898(3) _cell_length_c 17.997(3) _cell_angle_alpha 92.44(1) _cell_angle_beta 110.64(1) _cell_angle_gamma 100.416(7) _cell_volume 3657(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5806 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description cube _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.939 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 29754 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _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. ; _reflns_number_total 15210 _reflns_number_gt 7097 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1673 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_ref 0.2652 _refine_ls_wR_factor_gt 0.2425 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7097 _refine_ls_number_parameters 827 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0570 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.00 _refine_diff_density_min -0.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe(1) Fe 0.23221(7) 0.26675(6) 0.20840(6) 0.0538(3) Uani 1.00 d . . . Fe(2) Fe 0.49979(8) 0.88216(6) 0.29581(5) 0.0570(3) Uani 1.00 d . . . S(1) S 0.3327(1) 0.4617(1) 0.2687(1) 0.0608(5) Uani 1.00 d . . . S(2) S 0.4371(1) 0.6818(1) 0.2530(1) 0.0593(5) Uani 1.00 d . . . P(1) P 0.1856(1) 0.2317(1) 0.3119(1) 0.0571(5) Uani 1.00 d . . . P(2) P 0.5111(1) 0.9136(1) 0.1780(1) 0.0520(4) Uani 1.00 d . . . P(3) P 0.6479(2) 0.2242(2) 0.4688(2) 0.1065(9) Uani 1.00 d . . . P(4) P 0.0000 0.0000 0.0000 0.0613(7) Uani 1.00 d S . . P(5) P 0.5000 0.5000 0.0000 0.282(7) Uani 1.00 d S . . F(1) F 0.0442(6) 0.7672(6) 0.1486(6) 0.07527(2) Uiso 0.51 d P . . F(1A) F 0.0354(7) 0.7483(6) 0.1908(6) 0.07527(2) Uiso 0.49 d P . . F(2) F 0.0426(7) 0.7109(6) 0.0406(6) 0.08316(2) Uiso 0.51 d P . . F(2A) F 0.0533(7) 0.7558(7) 0.0829(6) 0.08316(2) Uiso 0.49 d P . . F(3) F -0.1433(8) 0.6463(6) 0.0868(7) 0.09056(3) Uiso 0.51 d P . . F(3A) F -0.1115(8) 0.6505(6) 0.1452(7) 0.09056(3) Uiso 0.49 d P . . F(4) F -0.0733(9) 0.6125(6) 0.0080(6) 0.09742(3) Uiso 0.51 d P . . F(4A) F -0.1306(9) 0.6202(7) 0.0278(7) 0.09742(3) Uiso 0.49 d P . . F(5) F -0.0687(8) 0.5314(7) 0.1902(6) 0.08622(2) Uiso 0.51 d P . . F(5A) F -0.0801(8) 0.4961(7) 0.1593(6) 0.08622(2) Uiso 0.49 d P . . F(6) F -0.0705(6) 0.4759(5) 0.0796(5) 0.06467(2) Uiso 0.51 d P . . F(6A) F -0.0548(6) 0.4893(5) 0.0466(5) 0.06467(2) Uiso 0.49 d P . . F(7) F 0.5875(7) 0.2579(6) 0.5174(5) 0.190(3) Uani 1.00 d . . . F(8) F 0.7447(7) 0.2923(6) 0.5171(5) 0.200(4) Uani 1.00 d . . . F(9) F 0.7039(6) 0.1862(6) 0.4208(6) 0.193(4) Uani 1.00 d . . . F(10) F 0.5475(6) 0.1642(5) 0.4132(5) 0.181(3) Uani 1.00 d . . . F(11) F 0.6143(9) 0.2918(6) 0.4093(6) 0.224(4) Uani 1.00 d . . . F(12) F 0.6752(10) 0.1568(7) 0.5233(6) 0.256(6) Uani 1.00 d . . . F(13) F -0.0290(4) 0.0370(3) 0.0706(2) 0.082(1) Uani 1.00 d . . . F(14) F 0.0511(5) 0.0942(3) -0.0082(3) 0.110(2) Uani 1.00 d . . . F(15) F -0.1063(4) 0.0124(4) -0.0625(3) 0.116(2) Uani 1.00 d . . . F(16) F 0.525(1) 0.587(2) 0.056(2) 0.41(1) Uani 1.00 d . . . F(17) F 0.505(3) 0.456(2) 0.095(2) 0.55(2) Uani 1.00 d . . . F(18) F 0.613(1) 0.493(2) 0.0393(9) 0.38(1) Uani 1.00 d . . . O(131) O 0.0147(4) 0.2230(3) 0.1032(3) 0.091(2) Uani 1.00 d . . . O(231) O 0.3518(5) 0.9910(4) 0.2756(4) 0.085(2) Uani 1.00 d . . . O(301) O 0.583(1) 0.4941(8) 0.2722(8) 0.22939(6) Uiso 1.00 d . . . C(1) C 0.0878(5) 0.5654(4) 0.1627(4) 0.051(2) Uani 1.00 d . . . C(2) C 0.129(1) 0.6503(10) 0.1479(8) 0.04327(3) Uiso 0.51 d P . . C(2A) C 0.125(1) 0.647(1) 0.1683(9) 0.04327(3) Uiso 0.49 d P . . C(3) C 0.036(1) 0.693(1) 0.1054(8) 0.05569(3) Uiso 0.51 d P . . C(3A) C 0.041(1) 0.696(1) 0.1345(9) 0.05569(3) Uiso 0.49 d P . . C(4) C -0.052(1) 0.6309(9) 0.0792(8) 0.05139(3) Uiso 0.51 d P . . C(4A) C -0.056(1) 0.6257(9) 0.1088(9) 0.05139(3) Uiso 0.49 d P . . C(5) C -0.0264(6) 0.5451(5) 0.1247(5) 0.071(2) Uani 1.00 d . . . C(111) C 0.2675(5) 0.5527(4) 0.2503(4) 0.051(2) Uani 1.00 d . . . C(112) C 0.1564(5) 0.5092(4) 0.1992(4) 0.050(2) Uani 1.00 d . . . C(113) C 0.1360(5) 0.4224(4) 0.1904(4) 0.055(2) Uani 1.00 d . . . C(114) C 0.2246(5) 0.3823(4) 0.2223(4) 0.052(2) Uani 1.00 d . . . C(115) C 0.2741(6) 0.5942(4) 0.3311(4) 0.065(2) Uani 1.00 d . . . C(121) C 0.3449(6) 0.2948(5) 0.1541(5) 0.074(2) Uani 1.00 d . . . C(122) C 0.2769(6) 0.2168(5) 0.1177(4) 0.072(2) Uani 1.00 d . . . C(123) C 0.2848(6) 0.1581(5) 0.1767(5) 0.070(2) Uani 1.00 d . . . C(124) C 0.3573(6) 0.2022(5) 0.2480(4) 0.067(2) Uani 1.00 d . . . C(125) C 0.3955(5) 0.2854(5) 0.2350(5) 0.072(2) Uani 1.00 d . . . C(131) C 0.1027(6) 0.2393(4) 0.1444(4) 0.066(2) Uani 1.00 d . . . C(141) C 0.0552(6) 0.2499(5) 0.3003(4) 0.067(2) Uani 1.00 d . . . C(142) C 0.0424(6) 0.3337(5) 0.3112(5) 0.076(2) Uani 1.00 d . . . C(143) C -0.0537(8) 0.3519(6) 0.2990(6) 0.097(3) Uani 1.00 d . . . C(144) C -0.1387(8) 0.2857(10) 0.2723(8) 0.133(4) Uani 1.00 d . . . C(145) C -0.1285(8) 0.2018(8) 0.2639(9) 0.143(5) Uani 1.00 d . . . C(146) C -0.0313(7) 0.1833(6) 0.2776(7) 0.105(3) Uani 1.00 d . . . C(151) C 0.1774(5) 0.1174(4) 0.3239(4) 0.061(2) Uani 1.00 d . . . C(152) C 0.2259(6) 0.0895(5) 0.3975(4) 0.073(2) Uani 1.00 d . . . C(153) C 0.2146(7) 0.0016(5) 0.4045(5) 0.088(3) Uani 1.00 d . . . C(154) C 0.1599(7) -0.0581(5) 0.3383(5) 0.087(3) Uani 1.00 d . . . C(155) C 0.1100(6) -0.0296(5) 0.2639(5) 0.077(2) Uani 1.00 d . . . C(156) C 0.1207(6) 0.0567(5) 0.2585(4) 0.068(2) Uani 1.00 d . . . C(161) C 0.2664(6) 0.2913(5) 0.4077(4) 0.064(2) Uani 1.00 d . . . C(162) C 0.3690(6) 0.3314(5) 0.4243(4) 0.069(2) Uani 1.00 d . . . C(163) C 0.4297(7) 0.3831(5) 0.4954(6) 0.080(2) Uani 1.00 d . . . C(164) C 0.3922(8) 0.3953(6) 0.5508(6) 0.098(3) Uani 1.00 d . . . C(165) C 0.2913(9) 0.3528(7) 0.5395(5) 0.102(3) Uani 1.00 d . . . C(166) C 0.2282(6) 0.3018(6) 0.4668(5) 0.081(2) Uani 1.00 d . . . C(211) C 0.3041(5) 0.6167(4) 0.2004(4) 0.050(1) Uani 1.00 d . . . C(212) C 0.2393(5) 0.6836(4) 0.1868(4) 0.052(2) Uani 1.00 d . . . C(213) C 0.2887(5) 0.7656(4) 0.2093(4) 0.056(2) Uani 1.00 d . . . C(214) C 0.4032(5) 0.7802(4) 0.2492(4) 0.054(2) Uani 1.00 d . . . C(215) C 0.3012(5) 0.5730(4) 0.1208(4) 0.062(2) Uani 1.00 d . . . C(221) C 0.5521(8) 0.9066(6) 0.4223(5) 0.096(3) Uani 1.00 d . . . C(222) C 0.6152(9) 0.9686(5) 0.3920(5) 0.099(3) Uani 1.00 d . . . C(223) C 0.6653(7) 0.9224(6) 0.3532(5) 0.092(3) Uani 1.00 d . . . C(224) C 0.6375(6) 0.8356(6) 0.3591(5) 0.077(2) Uani 1.00 d . . . C(225) C 0.5716(7) 0.8254(5) 0.4009(5) 0.082(3) Uani 1.00 d . . . C(231) C 0.4080(6) 0.9456(5) 0.2827(4) 0.064(2) Uani 1.00 d . . . C(241) C 0.6267(5) 0.8914(5) 0.1616(4) 0.058(2) Uani 1.00 d . . . C(242) C 0.6880(6) 0.9539(5) 0.1373(5) 0.074(2) Uani 1.00 d . . . C(243) C 0.7760(6) 0.9369(7) 0.1203(6) 0.093(3) Uani 1.00 d . . . C(244) C 0.7984(7) 0.8556(8) 0.1310(7) 0.104(3) Uani 1.00 d . . . C(245) C 0.7370(8) 0.7943(7) 0.1556(7) 0.102(3) Uani 1.00 d . . . C(246) C 0.6515(6) 0.8119(5) 0.1713(5) 0.079(2) Uani 1.00 d . . . C(251) C 0.4003(5) 0.8551(4) 0.0925(4) 0.051(2) Uani 1.00 d . . . C(252) C 0.3072(5) 0.8822(5) 0.0706(4) 0.061(2) Uani 1.00 d . . . C(253) C 0.2189(6) 0.8384(5) 0.0067(5) 0.076(2) Uani 1.00 d . . . C(254) C 0.2270(6) 0.7676(5) -0.0358(5) 0.079(2) Uani 1.00 d . . . C(255) C 0.3175(6) 0.7381(5) -0.0138(4) 0.064(2) Uani 1.00 d . . . C(256) C 0.4050(5) 0.7821(4) 0.0501(4) 0.057(2) Uani 1.00 d . . . C(261) C 0.5149(5) 1.0261(4) 0.1614(4) 0.055(2) Uani 1.00 d . . . C(262) C 0.4706(6) 1.0492(5) 0.0843(4) 0.067(2) Uani 1.00 d . . . C(263) C 0.4775(6) 1.1364(5) 0.0722(5) 0.073(2) Uani 1.00 d . . . C(264) C 0.5320(7) 1.1988(5) 0.1365(5) 0.075(2) Uani 1.00 d . . . C(265) C 0.5771(6) 1.1766(5) 0.2125(5) 0.069(2) Uani 1.00 d . . . C(266) C 0.5673(5) 1.0899(5) 0.2250(4) 0.062(2) Uani 1.00 d . . . C(301) C 0.686(1) 0.594(1) 0.2461(10) 0.19002(8) Uiso 1.00 d . . . C(302) C 0.6476(9) 0.5058(8) 0.2308(7) 0.10525(4) Uiso 1.00 d . . . C(303) C 0.672(2) 0.423(1) 0.237(1) 0.2681(1) Uiso 1.00 d . . . H(1) H 0.0657 0.3882 0.1635 0.0671 Uiso 1.00 calc . . . H(2) H 0.3459 0.6179 0.3636 0.0655 Uiso 1.00 calc . . . H(3) H 0.2455 0.5512 0.3579 0.0655 Uiso 1.00 calc . . . H(4) H 0.2351 0.6390 0.3226 0.0655 Uiso 1.00 calc . . . H(5) H 0.3571 0.3458 0.1271 0.0872 Uiso 1.00 calc . . . H(6) H 0.2313 0.2039 0.0615 0.0843 Uiso 1.00 calc . . . H(7) H 0.2458 0.0986 0.1667 0.0827 Uiso 1.00 calc . . . H(8) H 0.3791 0.1775 0.2996 0.0837 Uiso 1.00 calc . . . H(9) H 0.4491 0.3298 0.2741 0.0871 Uiso 1.00 calc . . . H(10) H 0.1045 0.3805 0.3283 0.0936 Uiso 1.00 calc . . . H(11) H -0.0596 0.4102 0.3130 0.1156 Uiso 1.00 calc . . . H(12) H -0.2095 0.2986 0.2567 0.1538 Uiso 1.00 calc . . . H(13) H -0.1893 0.1534 0.2477 0.1670 Uiso 1.00 calc . . . H(14) H -0.0232 0.1228 0.2734 0.1223 Uiso 1.00 calc . . . H(15) H 0.2665 0.1316 0.4439 0.0858 Uiso 1.00 calc . . . H(16) H 0.2435 -0.0174 0.4569 0.1075 Uiso 1.00 calc . . . H(17) H 0.1534 -0.1193 0.3435 0.1009 Uiso 1.00 calc . . . H(18) H 0.0662 -0.0714 0.2178 0.0928 Uiso 1.00 calc . . . H(19) H 0.0890 0.0764 0.2070 0.0844 Uiso 1.00 calc . . . H(20) H 0.4007 0.3213 0.3840 0.0856 Uiso 1.00 calc . . . H(21) H 0.5013 0.4115 0.5029 0.0978 Uiso 1.00 calc . . . H(22) H 0.4349 0.4324 0.5992 0.1165 Uiso 1.00 calc . . . H(23) H 0.2627 0.3600 0.5813 0.1183 Uiso 1.00 calc . . . H(24) H 0.1568 0.2724 0.4601 0.0954 Uiso 1.00 calc . . . H(25) H 0.2525 0.8127 0.1996 0.0656 Uiso 1.00 calc . . . H(26) H 0.2319 0.5386 0.0920 0.0620 Uiso 1.00 calc . . . H(27) H 0.3508 0.5367 0.1316 0.0620 Uiso 1.00 calc . . . H(28) H 0.3169 0.6161 0.0887 0.0620 Uiso 1.00 calc . . . H(29) H 0.5088 0.9181 0.4521 0.1267 Uiso 1.00 calc . . . H(30) H 0.6214 1.0322 0.3972 0.1120 Uiso 1.00 calc . . . H(31) H 0.7105 0.9490 0.3272 0.1139 Uiso 1.00 calc . . . H(32) H 0.6629 0.7905 0.3374 0.0954 Uiso 1.00 calc . . . H(33) H 0.5421 0.7702 0.4126 0.1012 Uiso 1.00 calc . . . H(34) H 0.6694 1.0109 0.1282 0.0889 Uiso 1.00 calc . . . H(35) H 0.8172 0.9799 0.1013 0.1135 Uiso 1.00 calc . . . H(36) H 0.8593 0.8424 0.1234 0.1216 Uiso 1.00 calc . . . H(37) H 0.7555 0.7380 0.1609 0.1184 Uiso 1.00 calc . . . H(38) H 0.6097 0.7681 0.1881 0.0990 Uiso 1.00 calc . . . H(39) H 0.3014 0.9332 0.0999 0.0769 Uiso 1.00 calc . . . H(40) H 0.1530 0.8573 -0.0077 0.0911 Uiso 1.00 calc . . . H(41) H 0.1668 0.7386 -0.0818 0.0930 Uiso 1.00 calc . . . H(42) H 0.3201 0.6851 -0.0426 0.0803 Uiso 1.00 calc . . . H(43) H 0.4708 0.7619 0.0645 0.0700 Uiso 1.00 calc . . . H(44) H 0.4345 1.0052 0.0385 0.0817 Uiso 1.00 calc . . . H(45) H 0.4431 1.1523 0.0192 0.0889 Uiso 1.00 calc . . . H(46) H 0.5370 1.2579 0.1284 0.0895 Uiso 1.00 calc . . . H(47) H 0.6155 1.2207 0.2573 0.0827 Uiso 1.00 calc . . . H(48) H 0.5977 1.0741 0.2786 0.0760 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0482(5) 0.0376(5) 0.0643(6) 0.0124(4) 0.0060(4) -0.0013(4) Fe(2) 0.0637(6) 0.0410(5) 0.0540(5) 0.0071(4) 0.0094(4) -0.0011(4) S(1) 0.0490(10) 0.0390(8) 0.077(1) 0.0121(7) 0.0007(8) -0.0005(8) S(2) 0.0466(9) 0.0404(9) 0.080(1) 0.0115(7) 0.0100(8) -0.0002(8) P(1) 0.0480(10) 0.0477(10) 0.065(1) 0.0103(8) 0.0081(8) 0.0003(8) P(2) 0.0430(9) 0.0493(10) 0.0597(10) 0.0093(7) 0.0149(8) -0.0017(8) P(3) 0.107(2) 0.108(2) 0.088(2) 0.047(2) 0.008(2) -0.026(2) P(4) 0.058(2) 0.053(1) 0.061(1) 0.001(1) 0.015(1) -0.014(1) P(5) 0.185(9) 0.52(2) 0.176(7) 0.17(1) 0.070(7) -0.03(1) F(7) 0.208(8) 0.191(8) 0.185(7) 0.076(7) 0.079(6) -0.062(6) F(8) 0.181(8) 0.179(8) 0.187(7) -0.039(6) 0.053(6) -0.085(6) F(9) 0.148(6) 0.198(8) 0.246(9) 0.015(6) 0.110(7) -0.066(7) F(10) 0.146(6) 0.171(7) 0.157(6) 0.039(5) -0.024(5) -0.043(5) F(11) 0.27(1) 0.176(8) 0.234(10) 0.069(8) 0.083(9) 0.084(8) F(12) 0.36(1) 0.24(1) 0.174(7) 0.20(1) 0.033(9) 0.074(8) F(13) 0.090(3) 0.078(3) 0.078(3) 0.005(2) 0.040(2) -0.021(2) F(14) 0.152(5) 0.060(3) 0.121(4) -0.007(3) 0.072(4) -0.012(3) F(15) 0.089(4) 0.148(5) 0.095(3) 0.049(3) 0.005(3) -0.026(3) F(16) 0.32(2) 0.45(3) 0.50(3) 0.08(2) 0.21(2) -0.15(3) F(17) 0.71(5) 0.39(3) 0.83(7) 0.11(3) 0.60(6) 0.19(3) F(18) 0.19(1) 0.67(3) 0.24(1) 0.15(2) 0.05(1) -0.14(2) O(131) 0.069(4) 0.064(3) 0.100(4) 0.018(3) -0.015(3) -0.019(3) O(231) 0.089(4) 0.066(3) 0.114(4) 0.030(3) 0.048(3) 0.001(3) C(1) 0.042(3) 0.043(3) 0.068(4) 0.013(3) 0.019(3) 0.003(3) C(5) 0.057(4) 0.055(4) 0.106(6) 0.021(4) 0.030(4) 0.009(4) C(111) 0.048(4) 0.033(3) 0.064(4) 0.005(3) 0.015(3) -0.006(3) C(112) 0.044(4) 0.039(3) 0.066(4) 0.008(3) 0.018(3) 0.005(3) C(113) 0.042(4) 0.042(3) 0.072(4) 0.009(3) 0.011(3) -0.001(3) C(114) 0.045(4) 0.042(3) 0.060(4) 0.006(3) 0.012(3) -0.003(3) C(115) 0.087(5) 0.051(4) 0.054(4) 0.015(4) 0.020(4) 0.003(3) C(121) 0.072(5) 0.060(5) 0.089(5) 0.024(4) 0.024(4) 0.011(4) C(122) 0.086(6) 0.059(5) 0.063(4) 0.020(4) 0.019(4) -0.007(4) C(123) 0.057(4) 0.052(4) 0.094(5) 0.017(3) 0.021(4) -0.011(4) C(124) 0.063(5) 0.059(4) 0.078(5) 0.032(4) 0.016(4) 0.001(4) C(125) 0.051(4) 0.052(4) 0.104(6) 0.011(3) 0.021(4) -0.008(4) C(131) 0.064(5) 0.047(4) 0.071(4) 0.020(3) 0.005(4) -0.006(3) C(141) 0.055(4) 0.064(5) 0.077(5) 0.017(4) 0.017(4) 0.006(4) C(142) 0.071(5) 0.078(5) 0.088(5) 0.029(4) 0.034(4) 0.012(4) C(143) 0.082(7) 0.093(7) 0.128(8) 0.033(6) 0.047(6) 0.015(6) C(144) 0.061(6) 0.14(1) 0.19(1) 0.033(7) 0.037(7) 0.007(9) C(145) 0.064(7) 0.105(9) 0.24(1) 0.007(6) 0.035(8) -0.007(9) C(146) 0.051(5) 0.081(6) 0.164(9) 0.015(4) 0.018(5) 0.004(6) C(151) 0.051(4) 0.053(4) 0.069(4) 0.009(3) 0.010(3) 0.003(3) C(152) 0.077(5) 0.055(4) 0.068(5) 0.013(4) 0.006(4) -0.004(4) C(153) 0.109(7) 0.067(5) 0.076(5) 0.020(5) 0.016(5) 0.016(4) C(154) 0.091(6) 0.052(5) 0.098(6) 0.008(4) 0.012(5) 0.006(4) C(155) 0.066(5) 0.056(5) 0.089(5) 0.004(4) 0.010(4) -0.004(4) C(156) 0.065(5) 0.052(4) 0.070(5) 0.009(3) 0.007(4) 0.000(4) C(161) 0.063(5) 0.058(4) 0.066(4) 0.020(4) 0.016(4) -0.001(3) C(162) 0.055(4) 0.055(4) 0.075(5) 0.010(3) -0.001(4) -0.005(4) C(163) 0.081(6) 0.058(5) 0.081(5) 0.010(4) 0.009(5) 0.000(4) C(164) 0.086(7) 0.070(6) 0.100(7) 0.021(5) -0.013(6) -0.019(5) C(165) 0.134(9) 0.107(8) 0.070(5) 0.050(7) 0.034(6) -0.007(5) C(166) 0.077(6) 0.085(6) 0.072(5) 0.018(4) 0.018(4) -0.018(4) C(211) 0.044(3) 0.044(3) 0.057(4) 0.013(3) 0.011(3) -0.004(3) C(212) 0.049(4) 0.038(3) 0.063(4) 0.010(3) 0.015(3) 0.002(3) C(213) 0.055(4) 0.044(4) 0.068(4) 0.018(3) 0.019(3) 0.014(3) C(214) 0.060(4) 0.051(4) 0.051(4) 0.019(3) 0.015(3) 0.003(3) C(215) 0.064(4) 0.054(4) 0.065(4) 0.016(3) 0.021(3) 0.001(3) C(221) 0.127(8) 0.073(6) 0.051(4) 0.011(5) -0.007(4) -0.004(4) C(222) 0.135(9) 0.054(5) 0.064(5) -0.007(5) -0.002(5) -0.006(4) C(223) 0.066(5) 0.085(6) 0.084(6) -0.012(5) -0.009(4) 0.012(5) C(224) 0.058(5) 0.079(6) 0.075(5) 0.007(4) 0.006(4) 0.004(4) C(225) 0.099(7) 0.050(4) 0.063(5) 0.012(4) -0.009(4) -0.001(4) C(231) 0.069(5) 0.051(4) 0.070(5) 0.007(4) 0.027(4) -0.002(3) C(241) 0.039(3) 0.063(4) 0.069(4) 0.009(3) 0.019(3) -0.005(3) C(242) 0.057(5) 0.074(5) 0.084(5) 0.006(4) 0.023(4) -0.004(4) C(243) 0.048(5) 0.123(8) 0.111(7) 0.004(5) 0.040(5) -0.003(6) C(244) 0.065(6) 0.124(9) 0.137(8) 0.030(6) 0.050(6) 0.005(7) C(245) 0.078(6) 0.097(7) 0.140(9) 0.039(6) 0.041(6) -0.003(6) C(246) 0.054(5) 0.081(6) 0.106(6) 0.024(4) 0.031(4) 0.009(5) C(251) 0.044(4) 0.054(4) 0.053(4) 0.005(3) 0.017(3) -0.001(3) C(252) 0.051(4) 0.065(4) 0.058(4) 0.010(3) 0.012(3) 0.000(3) C(253) 0.056(5) 0.073(5) 0.078(5) 0.007(4) 0.003(4) -0.001(4) C(254) 0.061(5) 0.079(6) 0.073(5) 0.008(4) 0.002(4) -0.015(4) C(255) 0.068(5) 0.063(4) 0.055(4) 0.004(4) 0.022(3) -0.006(3) C(256) 0.053(4) 0.055(4) 0.064(4) 0.010(3) 0.023(3) -0.003(3) C(261) 0.046(4) 0.050(4) 0.066(4) 0.009(3) 0.017(3) 0.000(3) C(262) 0.059(4) 0.064(5) 0.074(5) 0.010(4) 0.022(4) 0.003(4) C(263) 0.082(5) 0.062(5) 0.076(5) 0.011(4) 0.031(4) 0.017(4) C(264) 0.088(6) 0.060(5) 0.089(6) 0.014(4) 0.050(5) 0.021(4) C(265) 0.073(5) 0.050(4) 0.086(5) 0.005(4) 0.033(4) -0.001(4) C(266) 0.060(4) 0.059(4) 0.067(4) 0.008(3) 0.024(3) 0.002(4) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement SHELXL97 _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe(1) P(1) 2.240(2) . . yes Fe(1) C(114) 1.872(6) . . yes Fe(1) C(121) 2.122(10) . . yes Fe(1) C(122) 2.115(9) . . yes Fe(1) C(123) 2.126(8) . . yes Fe(1) C(124) 2.110(8) . . yes Fe(1) C(125) 2.121(8) . . yes Fe(1) C(131) 1.732(7) . . yes Fe(2) P(2) 2.250(2) . . yes Fe(2) C(214) 1.858(6) . . yes Fe(2) C(221) 2.125(8) . . yes Fe(2) C(222) 2.125(8) . . yes Fe(2) C(223) 2.134(8) . . yes Fe(2) C(224) 2.143(9) . . yes Fe(2) C(225) 2.129(8) . . yes Fe(2) C(231) 1.731(9) . . yes S(1) C(111) 1.827(7) . . yes S(1) C(114) 1.705(5) . . yes S(2) C(211) 1.845(5) . . yes S(2) C(214) 1.712(7) . . yes P(1) C(141) 1.839(8) . . yes P(1) C(151) 1.827(7) . . yes P(1) C(161) 1.802(6) . . yes P(2) C(241) 1.832(8) . . yes P(2) C(251) 1.819(5) . . yes P(2) C(261) 1.822(7) . . yes P(3) F(7) 1.55(1) . . yes P(3) F(8) 1.523(8) . . yes P(3) F(9) 1.52(1) . . yes P(3) F(10) 1.525(7) . . yes P(3) F(11) 1.56(1) . . yes P(3) F(12) 1.49(1) . . yes P(4) F(13) 1.584(5) . . yes P(4) F(13) 1.584(5) . 2_555 yes P(4) F(14) 1.575(5) . . yes P(4) F(14) 1.575(5) . 2_555 yes P(4) F(15) 1.568(5) . . yes P(4) F(15) 1.568(5) . 2_555 yes P(5) F(16) 1.59(2) . . yes P(5) F(16) 1.59(2) . 2_665 yes P(5) F(17) 1.87(4) . . yes P(5) F(17) 1.87(4) . 2_665 yes P(5) F(18) 1.51(2) . . yes P(5) F(18) 1.51(2) . 2_665 yes F(1) C(3) 1.35(2) . . yes F(1A) C(3A) 1.31(2) . . yes F(2) C(3) 1.24(2) . . yes F(2A) C(3A) 1.39(2) . . yes F(3) C(4) 1.39(2) . . yes F(3) C(4A) 1.25(2) . . yes F(3A) C(4A) 1.28(2) . . yes F(4) C(4) 1.22(2) . . yes F(4A) C(4A) 1.45(2) . . yes F(5) C(5) 1.50(2) . . yes F(5A) C(5) 1.31(2) . . yes F(6) C(5) 1.26(1) . . yes F(6A) C(5) 1.52(1) . . yes O(131) C(131) 1.164(8) . . yes O(231) C(231) 1.14(1) . . yes O(301) C(302) 1.35(2) . . yes C(1) C(2) 1.44(2) . . yes C(1) C(2A) 1.29(2) . . yes C(1) C(5) 1.465(9) . . yes C(1) C(112) 1.438(9) . . yes C(2) C(3) 1.55(2) . . yes C(2) C(3A) 1.50(3) . . yes C(2) C(212) 1.43(1) . . yes C(2A) C(3A) 1.50(2) . . yes C(2A) C(212) 1.51(2) . . yes C(3) C(4) 1.36(2) . . yes C(3A) C(4A) 1.51(2) . . yes C(4) C(5) 1.65(2) . . yes C(4A) C(5) 1.43(2) . . yes C(111) C(112) 1.511(7) . . yes C(111) C(115) 1.54(1) . . yes C(111) C(211) 1.523(10) . . yes C(112) C(113) 1.349(9) . . yes C(113) C(114) 1.443(9) . . yes C(121) C(122) 1.393(9) . . yes C(121) C(125) 1.40(1) . . yes C(122) C(123) 1.43(1) . . yes C(123) C(124) 1.383(9) . . yes C(124) C(125) 1.39(1) . . yes C(141) C(142) 1.39(1) . . yes C(141) C(146) 1.38(1) . . yes C(142) C(143) 1.37(1) . . yes C(143) C(144) 1.36(1) . . yes C(144) C(145) 1.37(2) . . yes C(145) C(146) 1.38(2) . . yes C(151) C(152) 1.39(1) . . yes C(151) C(156) 1.383(9) . . yes C(152) C(153) 1.39(1) . . yes C(153) C(154) 1.38(1) . . yes C(154) C(155) 1.41(1) . . yes C(155) C(156) 1.37(1) . . yes C(161) C(162) 1.38(1) . . yes C(161) C(166) 1.36(1) . . yes C(162) C(163) 1.39(1) . . yes C(163) C(164) 1.30(2) . . yes C(164) C(165) 1.39(2) . . yes C(165) C(166) 1.41(1) . . yes C(211) C(212) 1.491(9) . . yes C(211) C(215) 1.55(1) . . yes C(212) C(213) 1.332(8) . . yes C(213) C(214) 1.474(9) . . yes C(221) C(222) 1.46(1) . . yes C(221) C(225) 1.43(1) . . yes C(222) C(223) 1.41(2) . . yes C(223) C(224) 1.38(1) . . yes C(224) C(225) 1.37(1) . . yes C(241) C(242) 1.38(1) . . yes C(241) C(246) 1.37(1) . . yes C(242) C(243) 1.44(1) . . yes C(243) C(244) 1.39(2) . . yes C(244) C(245) 1.37(2) . . yes C(245) C(246) 1.39(2) . . yes C(251) C(252) 1.38(1) . . yes C(251) C(256) 1.39(1) . . yes C(252) C(253) 1.396(8) . . yes C(253) C(254) 1.38(1) . . yes C(254) C(255) 1.36(1) . . yes C(255) C(256) 1.392(8) . . yes C(261) C(262) 1.401(10) . . yes C(261) C(266) 1.383(9) . . yes C(262) C(263) 1.40(1) . . yes C(263) C(264) 1.38(1) . . yes C(264) C(265) 1.38(1) . . yes C(265) C(266) 1.40(1) . . yes C(301) C(302) 1.39(2) . . yes C(302) C(303) 1.41(3) . . yes C(113) H(1) 0.972 . . yes C(115) H(2) 0.960 . . yes C(115) H(3) 0.963 . . yes C(115) H(4) 0.958 . . yes C(121) H(5) 0.982 . . yes C(122) H(6) 0.975 . . yes C(123) H(7) 0.977 . . yes C(124) H(8) 0.994 . . yes C(125) H(9) 0.974 . . yes C(142) H(10) 0.979 . . yes C(143) H(11) 0.977 . . yes C(144) H(12) 0.993 . . yes C(145) H(13) 0.985 . . yes C(146) H(14) 0.992 . . yes C(152) H(15) 0.973 . . yes C(153) H(16) 0.971 . . yes C(154) H(17) 0.972 . . yes C(155) H(18) 0.975 . . yes C(156) H(19) 0.970 . . yes C(162) H(20) 0.993 . . yes C(163) H(21) 0.980 . . yes C(164) H(22) 0.962 . . yes C(165) H(23) 0.980 . . yes C(166) H(24) 0.986 . . yes C(213) H(25) 0.966 . . yes C(215) H(26) 0.968 . . yes C(215) H(27) 0.955 . . yes C(215) H(28) 0.958 . . yes C(221) H(29) 0.974 . . yes C(222) H(30) 0.997 . . yes C(223) H(31) 0.963 . . yes C(224) H(32) 0.978 . . yes C(225) H(33) 0.966 . . yes C(242) H(34) 0.991 . . yes C(243) H(35) 0.967 . . yes C(244) H(36) 0.966 . . yes C(245) H(37) 0.974 . . yes C(246) H(38) 0.956 . . yes C(252) H(39) 0.979 . . yes C(253) H(40) 0.972 . . yes C(254) H(41) 0.970 . . yes C(255) H(42) 0.984 . . yes C(256) H(43) 0.982 . . yes C(262) H(44) 0.977 . . yes C(263) H(45) 0.972 . . yes C(264) H(46) 0.950 . . yes C(265) H(47) 0.970 . . yes C(266) H(48) 0.972 . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Fe(1) C(114) 94.0(2) . . . yes P(1) Fe(1) C(121) 152.1(2) . . . yes P(1) Fe(1) C(122) 143.3(2) . . . yes P(1) Fe(1) C(123) 104.6(2) . . . yes P(1) Fe(1) C(124) 90.9(2) . . . yes P(1) Fe(1) C(125) 113.5(2) . . . yes P(1) Fe(1) C(131) 90.4(3) . . . yes C(114) Fe(1) C(121) 93.1(3) . . . yes C(114) Fe(1) C(122) 122.7(3) . . . yes C(114) Fe(1) C(123) 158.3(3) . . . yes C(114) Fe(1) C(124) 132.5(2) . . . yes C(114) Fe(1) C(125) 98.1(3) . . . yes C(114) Fe(1) C(131) 91.7(3) . . . yes C(121) Fe(1) C(122) 38.4(3) . . . yes C(121) Fe(1) C(123) 65.3(3) . . . yes C(121) Fe(1) C(124) 64.8(3) . . . yes C(121) Fe(1) C(125) 38.7(3) . . . yes C(121) Fe(1) C(131) 116.4(3) . . . yes C(122) Fe(1) C(123) 39.5(3) . . . yes C(122) Fe(1) C(124) 64.6(3) . . . yes C(122) Fe(1) C(125) 64.3(3) . . . yes C(122) Fe(1) C(131) 89.6(3) . . . yes C(123) Fe(1) C(124) 38.1(3) . . . yes C(123) Fe(1) C(125) 64.5(3) . . . yes C(123) Fe(1) C(131) 99.2(3) . . . yes C(124) Fe(1) C(125) 38.5(3) . . . yes C(124) Fe(1) C(131) 135.6(3) . . . yes C(125) Fe(1) C(131) 153.3(4) . . . yes P(2) Fe(2) C(214) 92.3(2) . . . yes P(2) Fe(2) C(221) 151.1(3) . . . yes P(2) Fe(2) C(222) 111.0(3) . . . yes P(2) Fe(2) C(223) 90.3(3) . . . yes P(2) Fe(2) C(224) 106.2(3) . . . yes P(2) Fe(2) C(225) 143.3(3) . . . yes P(2) Fe(2) C(231) 89.5(3) . . . yes C(214) Fe(2) C(221) 116.3(3) . . . yes C(214) Fe(2) C(222) 155.1(3) . . . yes C(214) Fe(2) C(223) 137.6(4) . . . yes C(214) Fe(2) C(224) 101.7(3) . . . yes C(214) Fe(2) C(225) 91.6(3) . . . yes C(214) Fe(2) C(231) 95.4(3) . . . yes C(221) Fe(2) C(222) 40.0(4) . . . yes C(221) Fe(2) C(223) 66.0(4) . . . yes C(221) Fe(2) C(224) 65.5(4) . . . yes C(221) Fe(2) C(225) 39.3(4) . . . yes C(221) Fe(2) C(231) 92.0(4) . . . yes C(222) Fe(2) C(223) 38.8(4) . . . yes C(222) Fe(2) C(224) 64.5(4) . . . yes C(222) Fe(2) C(225) 64.7(3) . . . yes C(222) Fe(2) C(231) 93.3(4) . . . yes C(223) Fe(2) C(224) 37.8(4) . . . yes C(223) Fe(2) C(225) 63.3(4) . . . yes C(223) Fe(2) C(231) 127.0(4) . . . yes C(224) Fe(2) C(225) 37.5(4) . . . yes C(224) Fe(2) C(231) 156.1(3) . . . yes C(225) Fe(2) C(231) 126.4(4) . . . yes C(111) S(1) C(114) 97.2(3) . . . yes C(211) S(2) C(214) 96.8(3) . . . yes Fe(1) P(1) C(141) 113.0(3) . . . yes Fe(1) P(1) C(151) 112.1(3) . . . yes Fe(1) P(1) C(161) 116.4(3) . . . yes C(141) P(1) C(151) 104.5(3) . . . yes C(141) P(1) C(161) 102.4(4) . . . yes C(151) P(1) C(161) 107.4(3) . . . yes Fe(2) P(2) C(241) 115.4(2) . . . yes Fe(2) P(2) C(251) 113.0(2) . . . yes Fe(2) P(2) C(261) 114.6(3) . . . yes C(241) P(2) C(251) 105.1(3) . . . yes C(241) P(2) C(261) 103.5(3) . . . yes C(251) P(2) C(261) 104.0(3) . . . yes F(7) P(3) F(8) 89.6(5) . . . yes F(7) P(3) F(9) 176.9(5) . . . yes F(7) P(3) F(10) 90.4(5) . . . yes F(7) P(3) F(11) 88.7(6) . . . yes F(7) P(3) F(12) 91.1(7) . . . yes F(8) P(3) F(9) 92.9(5) . . . yes F(8) P(3) F(10) 173.0(5) . . . yes F(8) P(3) F(11) 87.9(5) . . . yes F(8) P(3) F(12) 94.8(5) . . . yes F(9) P(3) F(10) 87.3(5) . . . yes F(9) P(3) F(11) 93.2(6) . . . yes F(9) P(3) F(12) 86.8(7) . . . yes F(10) P(3) F(11) 85.1(5) . . . yes F(10) P(3) F(12) 92.2(5) . . . yes F(11) P(3) F(12) 177.3(5) . . . yes F(13) P(4) F(13) 180.0 . . 2_555 yes F(13) P(4) F(14) 89.5(3) . . . yes F(13) P(4) F(14) 90.5(3) . . 2_555 yes F(13) P(4) F(15) 90.4(3) . . . yes F(13) P(4) F(15) 89.6(3) . . 2_555 yes F(13) P(4) F(14) 90.5(3) 2_555 . . yes F(13) P(4) F(14) 89.5(3) 2_555 . 2_555 yes F(13) P(4) F(15) 89.6(3) 2_555 . . yes F(13) P(4) F(15) 90.4(3) 2_555 . 2_555 yes F(14) P(4) F(14) 180.0 . . 2_555 yes F(14) P(4) F(15) 88.7(3) . . . yes F(14) P(4) F(15) 91.3(3) . . 2_555 yes F(14) P(4) F(15) 91.3(3) 2_555 . . yes F(14) P(4) F(15) 88.7(3) 2_555 . 2_555 yes F(15) P(4) F(15) 180.0 . . 2_555 yes F(16) P(5) F(16) 180.0 . . 2_665 yes F(16) P(5) F(17) 80(1) . . . yes F(16) P(5) F(17) 99(1) . . 2_665 yes F(16) P(5) F(18) 89(1) . . . yes F(16) P(5) F(18) 90(1) . . 2_665 yes F(16) P(5) F(17) 99(1) 2_665 . . yes F(16) P(5) F(17) 80(1) 2_665 . 2_665 yes F(16) P(5) F(18) 90(1) 2_665 . . yes F(16) P(5) F(18) 89(1) 2_665 . 2_665 yes F(17) P(5) F(17) 180.0000(1) . . 2_665 yes F(17) P(5) F(18) 76(1) . . . yes F(17) P(5) F(18) 103(1) . . 2_665 yes F(17) P(5) F(18) 103(1) 2_665 . . yes F(17) P(5) F(18) 76(1) 2_665 . 2_665 yes F(18) P(5) F(18) 180.0000(1) . . 2_665 yes C(2) C(1) C(5) 110.2(8) . . . yes C(2) C(1) C(112) 120.6(8) . . . yes C(2A) C(1) C(5) 111.5(9) . . . yes C(2A) C(1) C(112) 119.6(8) . . . yes C(5) C(1) C(112) 128.5(6) . . . yes C(1) C(2) C(3) 108(1) . . . yes C(1) C(2) C(212) 117(1) . . . yes C(3) C(2) C(212) 132(1) . . . yes C(1) C(2A) C(3A) 112(1) . . . yes C(1) C(2A) C(212) 122(1) . . . yes C(3A) C(2A) C(212) 123(1) . . . yes F(1) C(3) F(2) 108(1) . . . yes F(1) C(3) C(2) 110(1) . . . yes F(1) C(3) C(4) 122(1) . . . yes F(2) C(3) C(2) 106(1) . . . yes F(2) C(3) C(4) 100(1) . . . yes C(2) C(3) C(4) 107(1) . . . yes F(1A) C(3A) F(2A) 98(1) . . . yes F(1A) C(3A) C(2A) 110(1) . . . yes F(1A) C(3A) C(4A) 106(1) . . . yes F(2) C(3A) F(2A) 34.3(7) . . . yes F(2A) C(3A) C(2A) 118(1) . . . yes F(2A) C(3A) C(4A) 119(1) . . . yes C(2A) C(3A) C(4A) 101(1) . . . yes F(3) C(4) F(4) 106(1) . . . yes F(3) C(4) C(3) 120(1) . . . yes F(3) C(4) C(5) 106(1) . . . yes F(4) C(4) C(3) 106(1) . . . yes F(4) C(4) C(5) 108(1) . . . yes C(3) C(4) C(5) 108(1) . . . yes F(3A) C(4A) F(4A) 97(1) . . . yes F(3A) C(4A) C(3A) 104(1) . . . yes F(4A) C(4A) C(3A) 117(1) . . . yes C(3A) C(4A) C(5) 109(1) . . . yes F(5) C(5) F(6) 101.0(8) . . . yes F(5) C(5) C(1) 107.0(7) . . . yes F(5) C(5) C(4) 114.2(9) . . . yes F(5) C(5) C(4A) 95.5(10) . . . yes F(5A) C(5) F(6A) 100.7(7) . . . yes F(5A) C(5) C(1) 118.4(8) . . . yes F(5A) C(5) C(4A) 114(1) . . . yes F(6) C(5) C(1) 119.0(8) . . . yes F(6) C(5) C(4) 112.9(8) . . . yes F(6) C(5) C(4A) 124.4(8) . . . yes F(6A) C(5) C(4A) 109.5(8) . . . yes C(1) C(5) C(4) 103.1(7) . . . yes C(1) C(5) C(4A) 105.7(7) . . . yes S(1) C(111) C(112) 102.2(4) . . . yes S(1) C(111) C(115) 108.1(4) . . . yes S(1) C(111) C(211) 115.1(5) . . . yes C(112) C(111) C(115) 111.3(6) . . . yes C(112) C(111) C(211) 106.0(5) . . . yes C(115) C(111) C(211) 113.5(5) . . . yes C(1) C(112) C(111) 116.0(5) . . . yes C(1) C(112) C(113) 128.2(5) . . . yes C(111) C(112) C(113) 115.6(5) . . . yes C(112) C(113) C(114) 116.4(5) . . . yes Fe(1) C(114) S(1) 122.3(4) . . . yes Fe(1) C(114) C(113) 129.2(4) . . . yes S(1) C(114) C(113) 108.1(4) . . . yes Fe(1) C(121) C(122) 70.5(5) . . . yes Fe(1) C(121) C(125) 70.6(5) . . . yes C(122) C(121) C(125) 107.4(7) . . . yes Fe(1) C(122) C(121) 71.1(5) . . . yes Fe(1) C(122) C(123) 70.7(5) . . . yes C(121) C(122) C(123) 108.5(6) . . . yes Fe(1) C(123) C(122) 69.9(5) . . . yes Fe(1) C(123) C(124) 70.3(5) . . . yes C(122) C(123) C(124) 106.6(6) . . . yes Fe(1) C(124) C(123) 71.6(5) . . . yes Fe(1) C(124) C(125) 71.2(4) . . . yes C(123) C(124) C(125) 109.3(7) . . . yes Fe(1) C(125) C(121) 70.7(5) . . . yes Fe(1) C(125) C(124) 70.3(4) . . . yes C(121) C(125) C(124) 108.3(6) . . . yes Fe(1) C(131) O(131) 177.4(7) . . . yes P(1) C(141) C(142) 119.0(5) . . . yes P(1) C(141) C(146) 122.0(7) . . . yes C(142) C(141) C(146) 119.0(8) . . . yes C(141) C(142) C(143) 121.8(7) . . . yes C(142) C(143) C(144) 118(1) . . . yes C(143) C(144) C(145) 121(1) . . . yes C(144) C(145) C(146) 120.3(10) . . . yes C(141) C(146) C(145) 119.2(9) . . . yes P(1) C(151) C(152) 121.6(5) . . . yes P(1) C(151) C(156) 119.4(5) . . . yes C(152) C(151) C(156) 119.0(6) . . . yes C(151) C(152) C(153) 119.7(6) . . . yes C(152) C(153) C(154) 120.7(8) . . . yes C(153) C(154) C(155) 119.4(7) . . . yes C(154) C(155) C(156) 119.0(6) . . . yes C(151) C(156) C(155) 122.2(7) . . . yes P(1) C(161) C(162) 121.8(7) . . . yes P(1) C(161) C(166) 121.7(6) . . . yes C(162) C(161) C(166) 116.4(6) . . . yes C(161) C(162) C(163) 122.5(9) . . . yes C(162) C(163) C(164) 121.0(8) . . . yes C(163) C(164) C(165) 119.1(8) . . . yes C(164) C(165) C(166) 120(1) . . . yes C(161) C(166) C(165) 120.5(9) . . . yes S(2) C(211) C(111) 113.8(4) . . . yes S(2) C(211) C(212) 102.1(4) . . . yes S(2) C(211) C(215) 107.6(5) . . . yes C(111) C(211) C(212) 108.3(6) . . . yes C(111) C(211) C(215) 112.7(5) . . . yes C(212) C(211) C(215) 111.9(5) . . . yes C(2) C(212) C(2A) 15.1(9) . . . yes C(2) C(212) C(211) 114.4(8) . . . yes C(2) C(212) C(213) 127.8(9) . . . yes C(2A) C(212) C(211) 113.2(8) . . . yes C(2A) C(212) C(213) 127.2(9) . . . yes C(211) C(212) C(213) 117.7(5) . . . yes C(212) C(213) C(214) 115.5(6) . . . yes Fe(2) C(214) S(2) 122.7(4) . . . yes Fe(2) C(214) C(213) 129.5(5) . . . yes S(2) C(214) C(213) 107.7(4) . . . yes Fe(2) C(221) C(222) 70.0(5) . . . yes Fe(2) C(221) C(225) 70.5(5) . . . yes C(222) C(221) C(225) 104.1(9) . . . yes Fe(2) C(222) C(221) 70.0(4) . . . yes Fe(2) C(222) C(223) 71.0(4) . . . yes C(221) C(222) C(223) 107.8(8) . . . yes Fe(2) C(223) C(222) 70.2(5) . . . yes Fe(2) C(223) C(224) 71.5(5) . . . yes C(222) C(223) C(224) 108.8(9) . . . yes Fe(2) C(224) C(223) 70.8(5) . . . yes Fe(2) C(224) C(225) 70.7(5) . . . yes C(223) C(224) C(225) 108.4(9) . . . yes Fe(2) C(225) C(221) 70.2(4) . . . yes Fe(2) C(225) C(224) 71.8(5) . . . yes C(221) C(225) C(224) 110.8(8) . . . yes Fe(2) C(231) O(231) 176.4(6) . . . yes P(2) C(241) C(242) 120.2(6) . . . yes P(2) C(241) C(246) 120.4(6) . . . yes C(242) C(241) C(246) 119.4(8) . . . yes C(241) C(242) C(243) 121.3(8) . . . yes C(242) C(243) C(244) 117.4(9) . . . yes C(243) C(244) C(245) 120(1) . . . yes C(244) C(245) C(246) 121(1) . . . yes C(241) C(246) C(245) 120.1(8) . . . yes P(2) C(251) C(252) 119.1(5) . . . yes P(2) C(251) C(256) 122.4(5) . . . yes C(252) C(251) C(256) 118.5(5) . . . yes C(251) C(252) C(253) 121.5(7) . . . yes C(252) C(253) C(254) 118.6(7) . . . yes C(253) C(254) C(255) 120.9(6) . . . yes C(254) C(255) C(256) 120.0(7) . . . yes C(251) C(256) C(255) 120.5(7) . . . yes P(2) C(261) C(262) 120.8(5) . . . yes P(2) C(261) C(266) 119.6(5) . . . yes C(262) C(261) C(266) 119.5(6) . . . yes C(261) C(262) C(263) 120.0(6) . . . yes C(262) C(263) C(264) 119.3(7) . . . yes C(263) C(264) C(265) 121.0(7) . . . yes C(264) C(265) C(266) 119.7(6) . . . yes C(261) C(266) C(265) 120.5(7) . . . yes O(301) C(302) C(301) 102(1) . . . yes O(301) C(302) C(303) 95(1) . . . yes C(301) C(302) C(303) 146(1) . . . yes C(112) C(113) H(1) 122.20 . . . yes C(114) C(113) H(1) 121.38 . . . yes C(111) C(115) H(2) 109.52 . . . yes C(111) C(115) H(3) 109.33 . . . yes C(111) C(115) H(4) 109.66 . . . yes H(2) C(115) H(3) 109.23 . . . yes H(2) C(115) H(4) 109.67 . . . yes H(3) C(115) H(4) 109.42 . . . yes Fe(1) C(121) H(5) 126.25 . . . yes C(122) C(121) H(5) 125.68 . . . yes C(125) C(121) H(5) 126.89 . . . yes Fe(1) C(122) H(6) 124.00 . . . yes C(121) C(122) H(6) 126.08 . . . yes C(123) C(122) H(6) 125.47 . . . yes Fe(1) C(123) H(7) 124.97 . . . yes C(122) C(123) H(7) 125.12 . . . yes C(124) C(123) H(7) 128.25 . . . yes Fe(1) C(124) H(8) 124.30 . . . yes C(123) C(124) H(8) 124.73 . . . yes C(125) C(124) H(8) 125.97 . . . yes Fe(1) C(125) H(9) 125.92 . . . yes C(121) C(125) H(9) 124.65 . . . yes C(124) C(125) H(9) 127.07 . . . yes C(141) C(142) H(10) 118.43 . . . yes C(143) C(142) H(10) 119.75 . . . yes C(142) C(143) H(11) 120.25 . . . yes C(144) C(143) H(11) 121.40 . . . yes C(143) C(144) H(12) 119.17 . . . yes C(145) C(144) H(12) 119.44 . . . yes C(144) C(145) H(13) 121.76 . . . yes C(146) C(145) H(13) 117.97 . . . yes C(141) C(146) H(14) 120.17 . . . yes C(145) C(146) H(14) 120.59 . . . yes C(151) C(152) H(15) 119.73 . . . yes C(153) C(152) H(15) 120.58 . . . yes C(152) C(153) H(16) 119.27 . . . yes C(154) C(153) H(16) 120.03 . . . yes C(153) C(154) H(17) 120.16 . . . yes C(155) C(154) H(17) 120.39 . . . yes C(154) C(155) H(18) 119.99 . . . yes C(156) C(155) H(18) 120.93 . . . yes C(151) C(156) H(19) 118.63 . . . yes C(155) C(156) H(19) 119.18 . . . yes C(161) C(162) H(20) 118.28 . . . yes C(163) C(162) H(20) 119.19 . . . yes C(162) C(163) H(21) 118.78 . . . yes C(164) C(163) H(21) 120.19 . . . yes C(163) C(164) H(22) 119.90 . . . yes C(165) C(164) H(22) 120.97 . . . yes C(164) C(165) H(23) 120.05 . . . yes C(166) C(165) H(23) 119.68 . . . yes C(161) C(166) H(24) 120.65 . . . yes C(165) C(166) H(24) 118.78 . . . yes C(212) C(213) H(25) 122.53 . . . yes C(214) C(213) H(25) 121.93 . . . yes C(211) C(215) H(26) 109.07 . . . yes C(211) C(215) H(27) 109.79 . . . yes C(211) C(215) H(28) 109.64 . . . yes H(26) C(215) H(27) 109.26 . . . yes H(26) C(215) H(28) 109.00 . . . yes H(27) C(215) H(28) 110.05 . . . yes Fe(2) C(221) H(29) 125.06 . . . yes C(222) C(221) H(29) 127.89 . . . yes C(225) C(221) H(29) 128.00 . . . yes Fe(2) C(222) H(30) 124.19 . . . yes C(221) C(222) H(30) 126.00 . . . yes C(223) C(222) H(30) 126.14 . . . yes Fe(2) C(223) H(31) 123.87 . . . yes C(222) C(223) H(31) 123.87 . . . yes C(224) C(223) H(31) 127.28 . . . yes Fe(2) C(224) H(32) 125.32 . . . yes C(223) C(224) H(32) 124.26 . . . yes C(225) C(224) H(32) 127.31 . . . yes Fe(2) C(225) H(33) 124.00 . . . yes C(221) C(225) H(33) 125.83 . . . yes C(224) C(225) H(33) 123.38 . . . yes C(241) C(242) H(34) 120.20 . . . yes C(243) C(242) H(34) 118.42 . . . yes C(242) C(243) H(35) 121.30 . . . yes C(244) C(243) H(35) 121.34 . . . yes C(243) C(244) H(36) 120.25 . . . yes C(245) C(244) H(36) 119.03 . . . yes C(244) C(245) H(37) 117.15 . . . yes C(246) C(245) H(37) 121.72 . . . yes C(241) C(246) H(38) 120.12 . . . yes C(245) C(246) H(38) 119.75 . . . yes C(251) C(252) H(39) 120.19 . . . yes C(253) C(252) H(39) 118.33 . . . yes C(252) C(253) H(40) 120.95 . . . yes C(254) C(253) H(40) 120.44 . . . yes C(253) C(254) H(41) 118.90 . . . yes C(255) C(254) H(41) 120.22 . . . yes C(254) C(255) H(42) 119.57 . . . yes C(256) C(255) H(42) 120.44 . . . yes C(251) C(256) H(43) 119.83 . . . yes C(255) C(256) H(43) 119.68 . . . yes C(261) C(262) H(44) 120.72 . . . yes C(263) C(262) H(44) 119.25 . . . yes C(262) C(263) H(45) 119.91 . . . yes C(264) C(263) H(45) 120.79 . . . yes C(263) C(264) H(46) 119.43 . . . yes C(265) C(264) H(46) 119.57 . . . yes C(264) C(265) H(47) 120.53 . . . yes C(266) C(265) H(47) 119.79 . . . yes C(261) C(266) H(48) 119.72 . . . yes C(265) C(266) H(48) 119.82 . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) F(14) 3.49(1) . 2_565 ? F(1) C(155) 3.55(1) . 1_565 ? F(1A) C(155) 3.55(1) . 1_565 ? F(2) O(131) 2.74(1) . 2_565 ? F(2) C(131) 3.45(1) . 2_565 ? F(2) F(6A) 3.55(1) . 2_565 ? F(2) F(14) 3.57(1) . 2_565 ? F(2A) F(14) 3.13(1) . 2_565 ? F(2A) O(131) 3.19(1) . 2_565 ? F(3) C(245) 3.54(2) . 1_455 ? F(3A) C(245) 3.43(2) . 1_455 ? F(4) F(6A) 2.99(2) . 2_565 ? F(4) C(113) 3.36(1) . 2_565 ? F(4) F(6) 3.40(2) . 2_565 ? F(4) O(131) 3.51(1) . 2_565 ? F(6) F(6A) 3.33(1) . 2_565 ? F(6A) F(6A) 2.63(2) . 2_565 ? F(7) C(225) 3.20(1) . 2_666 ? F(7) C(115) 3.285(10) . 2_666 ? F(7) C(221) 3.42(1) . 2_666 ? F(8) C(115) 3.32(1) . 2_666 ? F(9) C(222) 3.41(1) . 1_545 ? F(9) C(266) 3.49(1) . 1_545 ? F(9) C(265) 3.52(1) . 1_545 ? F(10) C(222) 3.45(1) . 1_545 ? F(12) C(153) 3.27(2) . 2_656 ? F(12) C(154) 3.40(1) . 2_656 ? F(12) C(222) 3.51(1) . 1_545 ? F(13) C(243) 3.32(1) . 1_445 ? F(13) C(253) 3.528(10) . 2_565 ? F(15) C(253) 3.37(1) . 2_565 ? F(15) C(252) 3.49(1) . 2_565 ? O(131) C(253) 3.108(8) . 2_565 ? O(131) C(254) 3.197(10) . 2_565 ? O(231) C(154) 3.25(1) . 1_565 ? O(231) C(155) 3.27(1) . 1_565 ? O(231) C(123) 3.351(10) . 1_565 ? O(231) C(124) 3.407(9) . 1_565 ? O(231) C(156) 3.49(1) . 1_565 ? O(231) C(153) 3.51(1) . 1_565 ? O(301) C(164) 3.45(2) . 2_666 ? C(121) C(264) 3.36(1) . 1_545 ? C(122) C(264) 3.53(1) . 1_545 ? C(124) C(265) 3.44(1) . 1_545 ? C(125) C(264) 3.44(1) . 1_545 ? C(125) C(265) 3.44(1) . 1_545 ? C(153) C(222) 3.55(1) . 2_666 ? C(256) C(263) 3.35(1) . 2_675 ? #------------------------------------------------------------------------------ _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.907 #------------------------------------------------------------------------------ #===END