# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email makita@res.titech.ac.jp _publ_contact_author_name 'Munetaka Akita' loop_ _publ_author_name 'Keiko Motoyama' 'Huifang Li' 'Takashi Koike' 'Makoto Hatakeyama' 'Satoshi Yokojima' 'Shinichiro Nakamura' 'Munetaka Akita' data_1021_FeCp(CO)2_open _database_code_depnum_ccdc_archive 'CCDC 818896' #TrackingRef 'Akita.CIF' _audit_creation_date 'Tue Oct 31 22:12:38 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H20 Cl2 F6 Fe2 O4 S2 ' _chemical_formula_moiety 'C30 H20 Cl2 F6 Fe2 O4 S2 ' _chemical_formula_weight 805.20 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _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 20.64(1) _cell_length_b 13.514(8) _cell_length_c 11.361(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3169(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15016 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_T_max 0.879 #------------------------------------------------------------------------------ # 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 25803 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3624 _reflns_number_gt 3219 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.2261 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3219 _refine_ls_number_parameters 233 _refine_ls_goodness_of_fit_ref 1.924 _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 1.13 _refine_diff_density_min -1.21 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) ; Cl Cl 0.148 0.159 ;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 0.27217(2) 0.18734(4) -0.00139(3) 0.0353(2) Uani 1.00 d . . . Cl(1) Cl 0.4935(3) 0.0461(6) 0.1230(6) 0.17331(2) Uiso 0.59 d P . . Cl(2) Cl 0.4673(4) 0.1107(8) 0.1369(7) 0.17331(2) Uiso 0.41 d P . . S(1) S 0.35500(4) 0.16572(6) -0.24162(7) 0.0437(3) Uani 1.00 d . . . F(1) F 0.4468(3) 0.5171(5) -0.0763(5) 0.047(1) Uani 0.50 d P . . F(1A) F 0.4192(5) 0.5283(6) -0.123(1) 0.120(5) Uani 0.50 d P . . F(2) F 0.3843(2) 0.5215(4) -0.2260(6) 0.052(1) Uani 0.50 d P . . F(2A) F 0.4017(3) 0.5245(5) -0.305(1) 0.119(3) Uani 0.50 d P . . F(3) F 0.5072(3) 0.6537(4) -0.1919(8) 0.081(2) Uani 0.50 d P . . F(4) F 0.4704(3) 0.6067(6) -0.3543(6) 0.078(2) Uani 0.50 d P . . O(31) O 0.1814(2) 0.3107(3) -0.1293(3) 0.0687(8) Uani 1.00 d . . . O(32) O 0.3046(2) 0.3473(2) 0.1597(3) 0.0678(8) Uani 1.00 d . . . C(1) C 0.4691(1) 0.4008(2) -0.2300(3) 0.0344(6) Uani 1.00 d . . . C(2) C 0.4466(2) 0.5031(3) -0.2051(5) 0.0575(10) Uani 1.00 d . . . C(3) C 0.5000 0.5713(4) -0.2500 0.054(1) Uani 1.00 d S . . C(11) C 0.4154(1) 0.2441(2) -0.2915(3) 0.0392(6) Uani 1.00 d . . . C(12) C 0.4242(1) 0.3178(2) -0.2113(3) 0.0343(6) Uani 1.00 d . . . C(13) C 0.3815(1) 0.3108(2) -0.1118(3) 0.0359(6) Uani 1.00 d . . . C(14) C 0.3409(1) 0.2317(2) -0.1119(3) 0.0368(6) Uani 1.00 d . . . C(15) C 0.4472(2) 0.2272(3) -0.4076(4) 0.0521(8) Uani 1.00 d . . . C(21) C 0.3011(2) 0.0737(3) 0.1142(3) 0.0533(8) Uani 1.00 d . . . C(22) C 0.2344(2) 0.0961(3) 0.1324(3) 0.0502(8) Uani 1.00 d . . . C(23) C 0.2026(2) 0.0769(3) 0.0260(4) 0.0550(9) Uani 1.00 d . . . C(24) C 0.2481(2) 0.0451(3) -0.0594(4) 0.0609(10) Uani 1.00 d . . . C(25) C 0.3099(3) 0.0413(3) -0.0014(3) 0.058(1) Uani 1.00 d . . . C(31) C 0.2166(2) 0.2620(3) -0.0804(3) 0.0454(7) Uani 1.00 d . . . C(32) C 0.2932(2) 0.2846(3) 0.0955(3) 0.0461(7) Uani 1.00 d . . . C(41) C 0.5000 0.105(4) 0.2500 0.3550(3) Uiso 1.00 d S . . H(1) H 0.3813 0.3581 -0.0499 0.0430 Uiso 1.00 calc . . . H(2) H 0.4305 0.1684 -0.4423 0.0629 Uiso 1.00 calc . . . H(3) H 0.4396 0.2816 -0.4579 0.0629 Uiso 1.00 calc . . . H(4) H 0.4928 0.2195 -0.3959 0.0629 Uiso 1.00 calc . . . H(5) H 0.3350 0.0795 0.1717 0.0650 Uiso 1.00 calc . . . H(6) H 0.2148 0.1177 0.2045 0.0600 Uiso 1.00 calc . . . H(7) H 0.1572 0.0845 0.0129 0.0668 Uiso 1.00 calc . . . H(8) H 0.2384 0.0261 -0.1388 0.0731 Uiso 1.00 calc . . . H(9) H 0.3505 0.0208 -0.0365 0.0680 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) 0.0353(4) 0.0356(4) 0.0349(4) -0.0081(2) 0.0010(1) -0.0018(1) S(1) 0.0387(5) 0.0471(5) 0.0452(5) -0.0098(3) 0.0046(3) -0.0130(3) F(1) 0.054(3) 0.046(2) 0.040(2) 0.001(2) 0.007(2) -0.010(2) F(1A) 0.119(8) 0.060(4) 0.18(1) -0.020(5) 0.117(8) -0.043(6) F(2) 0.034(2) 0.053(3) 0.069(3) 0.011(2) -0.002(2) -0.002(2) F(2A) 0.054(4) 0.057(3) 0.24(1) 0.012(3) -0.060(5) 0.015(6) F(3) 0.076(4) 0.049(3) 0.120(6) -0.014(3) 0.028(4) -0.015(3) F(4) 0.079(4) 0.088(4) 0.067(4) 0.024(3) 0.018(3) 0.039(3) O(31) 0.064(2) 0.086(2) 0.056(2) 0.021(1) 0.005(1) 0.015(1) O(32) 0.076(2) 0.070(2) 0.057(2) -0.036(2) 0.012(1) -0.023(1) C(1) 0.030(1) 0.037(1) 0.036(1) 0.000(1) 0.001(1) -0.003(1) C(2) 0.033(1) 0.045(2) 0.094(3) 0.006(1) 0.004(2) -0.007(2) C(3) 0.064(3) 0.039(2) 0.057(3) 0.0000 0.014(2) 0.0000 C(11) 0.030(1) 0.046(2) 0.041(2) -0.004(1) 0.001(1) -0.004(1) C(12) 0.025(1) 0.039(1) 0.038(2) 0.000(1) 0.002(1) -0.004(1) C(13) 0.030(1) 0.040(1) 0.038(2) -0.001(1) 0.004(1) -0.004(1) C(14) 0.032(1) 0.040(2) 0.038(1) -0.002(1) 0.000(1) -0.003(1) C(15) 0.043(2) 0.064(2) 0.050(2) -0.006(2) 0.005(1) -0.016(2) C(21) 0.061(2) 0.046(2) 0.052(2) -0.003(2) -0.008(2) 0.010(2) C(22) 0.060(2) 0.045(2) 0.045(2) -0.013(1) 0.003(1) 0.010(1) C(23) 0.051(2) 0.047(2) 0.067(2) -0.025(2) 0.000(2) 0.003(2) C(24) 0.085(3) 0.041(2) 0.057(2) -0.020(2) -0.008(2) -0.007(2) C(25) 0.073(3) 0.037(2) 0.065(3) 0.003(2) 0.011(2) 0.002(1) C(31) 0.041(1) 0.054(2) 0.041(2) 0.001(1) 0.008(1) 0.003(1) C(32) 0.048(2) 0.047(2) 0.043(2) -0.018(1) 0.010(1) -0.003(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _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) C(14) 1.986(3) . . yes Fe(1) C(21) 2.107(4) . . yes Fe(1) C(22) 2.107(4) . . yes Fe(1) C(23) 2.094(4) . . yes Fe(1) C(24) 2.092(4) . . yes Fe(1) C(25) 2.122(4) . . yes Fe(1) C(31) 1.771(4) . . yes Fe(1) C(32) 1.768(4) . . yes Cl(1) C(41) 1.65(3) . . yes Cl(2) C(41) 1.453(9) . . yes S(1) C(11) 1.732(3) . . yes S(1) C(14) 1.747(3) . . yes F(1) C(2) 1.476(8) . . yes F(1A) C(2) 1.14(1) . . yes F(2) C(2) 1.331(6) . . yes F(2A) C(2) 1.49(1) . . yes F(3) F(3) 1.35(2) . 4_654 yes F(3) F(4) 0.94(1) . 4_654 yes F(3) C(3) 1.304(8) . . yes F(4) C(3) 1.416(7) . . yes O(31) C(31) 1.128(5) . . yes O(32) C(32) 1.143(5) . . yes C(1) C(1) 1.353(6) . 4_654 yes C(1) C(2) 1.486(5) . . yes C(1) C(12) 1.471(4) . . yes C(2) C(3) 1.524(5) . . yes C(11) C(12) 1.361(4) . . yes C(11) C(15) 1.491(5) . . yes C(12) C(13) 1.437(4) . . yes C(13) C(14) 1.359(4) . . yes C(21) C(22) 1.425(5) . . yes C(21) C(25) 1.396(6) . . yes C(22) C(23) 1.400(6) . . yes C(23) C(24) 1.417(6) . . yes C(24) C(25) 1.438(7) . . 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) Fe(1) C(21) 114.3(1) . . . yes C(14) Fe(1) C(22) 153.7(1) . . . yes C(14) Fe(1) C(23) 143.0(1) . . . yes C(14) Fe(1) C(24) 104.3(2) . . . yes C(14) Fe(1) C(25) 91.1(2) . . . yes C(14) Fe(1) C(31) 88.3(1) . . . yes C(14) Fe(1) C(32) 89.7(1) . . . yes C(21) Fe(1) C(22) 39.5(1) . . . yes C(21) Fe(1) C(23) 65.3(2) . . . yes C(21) Fe(1) C(24) 66.1(2) . . . yes C(21) Fe(1) C(25) 38.5(1) . . . yes C(21) Fe(1) C(31) 156.1(2) . . . yes C(21) Fe(1) C(32) 94.8(2) . . . yes C(22) Fe(1) C(23) 38.9(2) . . . yes C(22) Fe(1) C(24) 66.5(2) . . . yes C(22) Fe(1) C(25) 65.9(2) . . . yes C(22) Fe(1) C(31) 117.4(2) . . . yes C(22) Fe(1) C(32) 94.4(2) . . . yes C(23) Fe(1) C(24) 39.6(2) . . . yes C(23) Fe(1) C(25) 65.7(2) . . . yes C(23) Fe(1) C(31) 92.1(2) . . . yes C(23) Fe(1) C(32) 127.2(2) . . . yes C(24) Fe(1) C(25) 39.9(2) . . . yes C(24) Fe(1) C(31) 102.1(2) . . . yes C(24) Fe(1) C(32) 159.6(2) . . . yes C(25) Fe(1) C(31) 140.1(2) . . . yes C(25) Fe(1) C(32) 126.9(2) . . . yes C(31) Fe(1) C(32) 92.9(2) . . . yes C(11) S(1) C(14) 94.8(1) . . . yes C(1) C(1) C(2) 111.0(2) 4_654 . . yes C(1) C(1) C(12) 130.0(2) 4_654 . . yes C(2) C(1) C(12) 119.0(3) . . . yes F(1) C(2) F(2) 99.0(4) . . . yes F(1) C(2) C(1) 107.9(4) . . . yes F(1) C(2) C(3) 104.6(4) . . . yes F(1A) C(2) F(2A) 104.7(7) . . . yes F(1A) C(2) C(1) 126.0(6) . . . yes F(1A) C(2) C(3) 116.8(5) . . . yes F(2) C(2) C(1) 116.2(4) . . . yes F(2) C(2) C(3) 121.8(4) . . . yes F(2A) C(2) C(1) 103.3(4) . . . yes F(2A) C(2) C(3) 94.5(4) . . . yes C(1) C(2) C(3) 105.8(3) . . . yes F(3) C(3) F(4) 100.6(6) . . . yes F(3) C(3) C(2) 115.4(4) . . . yes F(3) C(3) C(2) 127.1(4) . . 4_654 yes F(3) C(3) F(4) 100.6(6) 4_654 . 4_654 yes F(3) C(3) C(2) 127.1(4) 4_654 . . yes F(3) C(3) C(2) 115.4(4) 4_654 . 4_654 yes F(4) C(3) C(2) 99.9(3) . . . yes F(4) C(3) C(2) 103.7(3) . . 4_654 yes F(4) C(3) C(2) 103.7(3) 4_654 . . yes F(4) C(3) C(2) 99.9(3) 4_654 . 4_654 yes C(2) C(3) C(2) 105.7(4) . . 4_654 yes S(1) C(11) C(12) 108.9(2) . . . yes S(1) C(11) C(15) 120.8(2) . . . yes C(12) C(11) C(15) 130.2(3) . . . yes C(1) C(12) C(11) 123.0(3) . . . yes C(1) C(12) C(13) 123.4(3) . . . yes C(11) C(12) C(13) 113.4(3) . . . yes C(12) C(13) C(14) 115.4(3) . . . yes Fe(1) C(14) S(1) 119.9(2) . . . yes Fe(1) C(14) C(13) 132.7(2) . . . yes S(1) C(14) C(13) 107.4(2) . . . yes Fe(1) C(21) C(22) 70.2(2) . . . yes Fe(1) C(21) C(25) 71.3(2) . . . yes C(22) C(21) C(25) 109.2(4) . . . yes Fe(1) C(22) C(21) 70.2(2) . . . yes Fe(1) C(22) C(23) 70.0(2) . . . yes C(21) C(22) C(23) 106.7(3) . . . yes Fe(1) C(23) C(22) 71.0(2) . . . yes Fe(1) C(23) C(24) 70.1(2) . . . yes C(22) C(23) C(24) 109.7(4) . . . yes Fe(1) C(24) C(23) 70.3(2) . . . yes Fe(1) C(24) C(25) 71.2(2) . . . yes C(23) C(24) C(25) 106.6(4) . . . yes Fe(1) C(25) C(21) 70.1(2) . . . yes Fe(1) C(25) C(24) 68.9(2) . . . yes C(21) C(25) C(24) 107.7(4) . . . yes Fe(1) C(31) O(31) 178.8(3) . . . yes Fe(1) C(32) O(32) 177.6(3) . . . yes Cl(1) C(41) Cl(1) 122(3) . . 4_655 yes Cl(2) C(41) Cl(2) 174(4) . . 4_655 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) 2.90(1) . 4_655 ? Cl(1) Cl(2) 2.98(1) . 4_655 ? Cl(1) Cl(1) 3.07(1) . 5_655 ? Cl(2) Cl(2) 2.90(2) . 4_655 ? Cl(2) F(3) 3.29(1) . 5_665 ? S(1) O(32) 3.484(4) . 2_554 ? F(1) F(1) 2.84(1) . 5_665 ? F(1) F(4) 3.066(9) . 8_565 ? F(1) F(2A) 3.27(1) . 8_565 ? F(1) C(23) 3.393(7) . 7_555 ? F(1A) C(23) 3.10(1) . 7_555 ? F(1A) C(24) 3.54(1) . 7_555 ? F(2) O(32) 2.745(6) . 8_564 ? F(2) C(22) 3.333(7) . 2_554 ? F(2) C(24) 3.339(7) . 7_555 ? F(2) C(23) 3.461(7) . 7_555 ? F(2) C(23) 3.595(7) . 2_554 ? F(2A) O(32) 2.680(8) . 8_564 ? F(2A) C(23) 3.19(1) . 2_554 ? F(2A) C(22) 3.324(8) . 2_554 ? F(2A) C(32) 3.600(9) . 8_564 ? F(3) C(41) 3.33(5) . 5_665 ? F(4) O(32) 3.483(7) . 8_564 ? O(31) O(32) 3.222(4) . 2_554 ? O(31) C(21) 3.326(5) . 2_554 ? O(31) C(32) 3.421(5) . 2_554 ? O(31) C(25) 3.443(5) . 7_555 ? O(31) C(22) 3.454(5) . 2_554 ? O(31) C(24) 3.575(5) . 7_555 ? O(32) C(31) 3.330(5) . 2_555 ? O(32) C(23) 3.459(5) . 7_555 ? O(32) C(22) 3.471(5) . 7_555 ? #===END data_1098_FeCp(CO)2_closed _database_code_depnum_ccdc_archive 'CCDC 818897' #TrackingRef 'DT-ART-04-2011-010727CIFrev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H18 F6 Fe2 O4 S2' _chemical_formula_weight 720.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.8074(18) _cell_length_b 11.2063(19) _cell_length_c 12.978(2) _cell_angle_alpha 97.203(8) _cell_angle_beta 98.033(9) _cell_angle_gamma 114.204(6) _cell_volume 1390.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4041 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; Because of the small size of the crystal the data completeness was low. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11277 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5762 _reflns_number_gt 4346 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All fluorine atoms were refined with fixing the C-F distances (~1.35 A). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5762 _refine_ls_number_parameters 388 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0691(4) -0.8170(4) 0.2218(3) 0.0389(8) Uani 1 1 d . . . C2 C 0.0670(4) -0.7603(4) 0.2923(3) 0.0411(8) Uani 1 1 d . . . C3 C 0.0489(4) -0.7786(4) 0.4014(2) 0.0496(10) Uani 1 1 d D . . C4 C -0.0945(4) -0.8965(4) 0.3830(3) 0.0566(12) Uani 1 1 d D . . C5 C -0.1773(3) -0.8909(3) 0.2797(3) 0.0482(10) Uani 1 1 d D . . C111 C 0.0423(4) -0.6997(4) 0.0878(3) 0.0489(10) Uani 1 1 d . . . C112 C -0.0862(4) -0.7999(4) 0.1199(3) 0.0409(8) Uani 1 1 d . . . C113 C -0.2070(4) -0.8534(4) 0.0363(3) 0.0431(9) Uani 1 1 d . . . H113 H -0.2956 -0.8994 0.0485 0.052 Uiso 1 1 calc . . . C114 C -0.1852(4) -0.8333(4) -0.0629(3) 0.0404(8) Uani 1 1 d . . . C115 C 0.0647(5) -0.5549(4) 0.1291(4) 0.0585(11) Uani 1 1 d . . . H11A H -0.0154 -0.5439 0.0992 0.088 Uiso 1 1 calc R . . H11B H 0.1450 -0.4932 0.1085 0.088 Uiso 1 1 calc R . . H11C H 0.0784 -0.5381 0.2051 0.088 Uiso 1 1 calc R . . C121 C -0.1897(5) -0.7986(5) -0.2938(4) 0.0584(12) Uani 1 1 d . . . H121 H -0.1070 -0.7130 -0.2697 0.070 Uiso 1 1 calc . . . C122 C -0.1915(5) -0.9236(6) -0.2935(3) 0.0605(12) Uani 1 1 d . . . H122 H -0.1113 -0.9409 -0.2703 0.073 Uiso 1 1 calc . . . C123 C -0.3268(8) -1.0194(6) -0.3360(4) 0.0847(19) Uani 1 1 d . . . H123 H -0.3592 -1.1165 -0.3480 0.102 Uiso 1 1 calc . . . C124 C -0.4100(6) -0.9502(9) -0.3622(4) 0.096(2) Uani 1 1 d . . . H124 H -0.5091 -0.9915 -0.3954 0.115 Uiso 1 1 calc . . . C125 C -0.3221(6) -0.8138(7) -0.3364(4) 0.0747(16) Uani 1 1 d . . . H125 H -0.3484 -0.7417 -0.3474 0.090 Uiso 1 1 calc . . . C131 C -0.4003(4) -0.8005(5) -0.1388(3) 0.0499(10) Uani 1 1 d . . . C132 C -0.4245(4) -1.0367(4) -0.1501(3) 0.0473(9) Uani 1 1 d . . . C211 C 0.1679(4) -0.7200(5) 0.1342(3) 0.0492(10) Uani 1 1 d . . . C212 C 0.1842(4) -0.7042(4) 0.2556(3) 0.0432(9) Uani 1 1 d . . . C213 C 0.3276(4) -0.6407(4) 0.3078(3) 0.0470(10) Uani 1 1 d . . . H213 H 0.3559 -0.6398 0.3791 0.056 Uiso 1 1 calc . . . C214 C 0.4208(4) -0.5817(4) 0.2477(3) 0.0463(9) Uani 1 1 d . . . C215 C 0.1506(5) -0.8638(5) 0.0875(4) 0.0561(11) Uani 1 1 d . . . H21A H 0.2311 -0.8740 0.1179 0.084 Uiso 1 1 calc R . . H21B H 0.1406 -0.8756 0.0117 0.084 Uiso 1 1 calc R . . H21C H 0.0697 -0.9296 0.1044 0.084 Uiso 1 1 calc R . . C221 C 0.6978(6) -0.3842(7) 0.1688(5) 0.0761(18) Uani 1 1 d . . . H221 H 0.6617 -0.3295 0.1330 0.091 Uiso 1 1 calc . . . C222 C 0.8062(5) -0.3382(5) 0.2601(5) 0.0700(15) Uani 1 1 d . . . H222 H 0.8589 -0.2455 0.2991 0.084 Uiso 1 1 calc . . . C223 C 0.8288(4) -0.4472(6) 0.2815(4) 0.0647(14) Uani 1 1 d . . . H223 H 0.8996 -0.4453 0.3386 0.078 Uiso 1 1 calc . . . C224 C 0.7364(5) -0.5587(5) 0.2031(4) 0.0644(13) Uani 1 1 d . . . H224 H 0.7298 -0.6492 0.1980 0.077 Uiso 1 1 calc . . . C225 C 0.6572(4) -0.5218(6) 0.1357(3) 0.0649(14) Uani 1 1 d . . . H225 H 0.5851 -0.5807 0.0737 0.078 Uiso 1 1 calc . . . C231 C 0.6275(4) -0.5705(5) 0.3928(4) 0.0594(12) Uani 1 1 d . . . C232 C 0.5963(4) -0.3547(5) 0.3642(3) 0.0571(12) Uani 1 1 d . . . F1 F 0.1463(3) -0.8036(4) 0.4591(2) 0.0798(10) Uani 1 1 d D . . F2 F 0.0482(4) -0.6716(3) 0.4621(2) 0.0841(10) Uani 1 1 d D . . F3 F -0.0795(3) -1.0111(3) 0.3689(3) 0.0826(9) Uani 1 1 d D . . F4 F -0.1576(3) -0.9010(4) 0.4657(2) 0.0806(10) Uani 1 1 d D . . F5 F -0.2686(3) -1.0148(3) 0.2270(2) 0.0850(10) Uani 1 1 d D . . F6 F -0.2591(3) -0.8306(4) 0.3017(3) 0.0875(11) Uani 1 1 d D . . S1 S -0.00676(9) -0.74087(10) -0.05922(7) 0.0428(3) Uani 1 1 d . . . S2 S 0.33646(9) -0.59697(12) 0.11764(8) 0.0500(3) Uani 1 1 d . . . O131 O -0.4531(4) -0.7410(4) -0.1016(3) 0.0727(10) Uani 1 1 d . . . O132 O -0.4910(3) -1.1284(3) -0.1181(3) 0.0642(9) Uani 1 1 d . . . O231 O 0.6330(4) -0.6286(5) 0.4583(3) 0.0919(14) Uani 1 1 d . . . O232 O 0.5784(4) -0.2693(4) 0.4084(3) 0.0784(11) Uani 1 1 d . . . Fe1 Fe -0.32371(5) -0.89606(6) -0.19774(4) 0.04058(18) Uani 1 1 d . . . Fe2 Fe 0.62552(5) -0.48028(6) 0.29098(4) 0.04157(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0271(16) 0.052(2) 0.0323(17) 0.0086(16) 0.0072(14) 0.0113(16) C2 0.0288(17) 0.050(2) 0.0361(18) 0.0110(17) 0.0069(14) 0.0087(16) C3 0.037(2) 0.066(3) 0.0349(19) 0.009(2) 0.0074(16) 0.012(2) C4 0.043(2) 0.080(3) 0.038(2) 0.023(2) 0.0112(18) 0.015(2) C5 0.0266(17) 0.068(3) 0.042(2) 0.018(2) 0.0080(15) 0.0112(18) C111 0.0342(19) 0.062(3) 0.039(2) 0.0145(19) 0.0059(16) 0.0088(19) C112 0.0290(17) 0.051(2) 0.0351(18) 0.0057(17) 0.0070(14) 0.0105(17) C113 0.0266(16) 0.061(3) 0.0330(17) 0.0080(18) 0.0062(14) 0.0118(17) C114 0.0293(16) 0.051(2) 0.0363(18) 0.0076(17) 0.0058(14) 0.0136(16) C115 0.063(3) 0.050(3) 0.067(3) 0.013(2) 0.022(2) 0.026(2) C121 0.049(2) 0.078(3) 0.047(2) 0.025(2) 0.0218(19) 0.019(2) C122 0.068(3) 0.083(4) 0.040(2) 0.015(2) 0.023(2) 0.038(3) C123 0.119(5) 0.061(3) 0.043(3) -0.008(2) 0.033(3) 0.010(3) C124 0.046(3) 0.168(7) 0.030(2) 0.014(3) 0.0035(19) 0.008(4) C125 0.066(3) 0.126(5) 0.059(3) 0.046(3) 0.027(3) 0.055(4) C131 0.037(2) 0.058(3) 0.048(2) 0.013(2) 0.0005(18) 0.016(2) C132 0.0337(19) 0.057(3) 0.045(2) 0.0032(19) 0.0113(16) 0.0145(19) C211 0.0314(18) 0.068(3) 0.042(2) 0.017(2) 0.0105(16) 0.0131(19) C212 0.0302(18) 0.058(2) 0.0359(18) 0.0132(18) 0.0060(15) 0.0136(17) C213 0.0284(17) 0.066(3) 0.0355(18) 0.0138(18) 0.0028(15) 0.0098(18) C214 0.0279(17) 0.063(3) 0.0379(19) 0.0117(19) 0.0076(15) 0.0091(18) C215 0.059(3) 0.066(3) 0.055(3) 0.015(2) 0.020(2) 0.036(2) C221 0.075(3) 0.124(5) 0.076(3) 0.063(4) 0.056(3) 0.064(4) C222 0.054(3) 0.055(3) 0.080(4) 0.000(3) 0.043(3) -0.001(2) C223 0.0293(19) 0.101(4) 0.058(3) 0.014(3) 0.0187(19) 0.020(2) C224 0.053(3) 0.064(3) 0.080(3) 0.013(3) 0.034(3) 0.022(2) C225 0.035(2) 0.101(4) 0.040(2) -0.003(2) 0.0161(17) 0.014(2) C231 0.032(2) 0.084(3) 0.059(3) 0.023(3) 0.0097(19) 0.020(2) C232 0.035(2) 0.080(3) 0.042(2) 0.001(2) 0.0075(17) 0.014(2) F1 0.0481(15) 0.131(3) 0.0555(15) 0.0457(18) 0.0110(13) 0.0273(17) F2 0.095(2) 0.084(2) 0.0485(15) -0.0042(15) 0.0231(15) 0.0174(19) F3 0.073(2) 0.077(2) 0.090(2) 0.0346(18) 0.0102(17) 0.0228(17) F4 0.0471(15) 0.134(3) 0.0479(14) 0.0303(17) 0.0228(12) 0.0192(16) F5 0.0612(18) 0.080(2) 0.0637(17) 0.0136(16) 0.0130(14) -0.0178(15) F6 0.0644(18) 0.142(3) 0.096(2) 0.060(2) 0.0503(18) 0.062(2) S1 0.0279(4) 0.0583(6) 0.0350(4) 0.0134(4) 0.0084(3) 0.0101(4) S2 0.0264(4) 0.0714(7) 0.0408(5) 0.0203(5) 0.0081(4) 0.0075(5) O131 0.064(2) 0.076(2) 0.084(3) 0.005(2) 0.0206(19) 0.038(2) O132 0.0498(18) 0.061(2) 0.076(2) 0.0230(18) 0.0230(17) 0.0122(16) O231 0.069(2) 0.140(4) 0.086(3) 0.072(3) 0.031(2) 0.046(3) O232 0.054(2) 0.097(3) 0.080(3) -0.010(2) 0.0135(18) 0.036(2) Fe1 0.0295(3) 0.0514(4) 0.0342(3) 0.0087(2) 0.0062(2) 0.0113(3) Fe2 0.0247(3) 0.0563(4) 0.0355(3) 0.0084(3) 0.0081(2) 0.0093(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C112 1.358(5) . ? C1 C2 1.454(5) . ? C1 C5 1.492(5) . ? C2 C212 1.349(5) . ? C2 C3 1.484(5) . ? C3 F1 1.3500(19) . ? C3 F2 1.3530(19) . ? C3 C4 1.531(5) . ? C4 F4 1.3437(19) . ? C4 F3 1.352(2) . ? C4 C5 1.528(5) . ? C5 F5 1.3488(19) . ? C5 F6 1.3535(19) . ? C111 C211 1.522(6) . ? C111 C112 1.537(5) . ? C111 C115 1.549(6) . ? C111 S1 1.852(4) . ? C112 C113 1.429(5) . ? C113 C114 1.369(5) . ? C114 S1 1.766(4) . ? C114 Fe1 1.974(4) . ? C121 C122 1.393(7) . ? C121 C125 1.392(7) . ? C121 Fe1 2.096(4) . ? C122 C123 1.391(8) . ? C122 Fe1 2.108(5) . ? C123 C124 1.442(10) . ? C123 Fe1 2.111(5) . ? C124 C125 1.394(9) . ? C124 Fe1 2.109(5) . ? C125 Fe1 2.121(5) . ? C131 O131 1.145(5) . ? C131 Fe1 1.765(5) . ? C132 O132 1.153(5) . ? C132 Fe1 1.754(4) . ? C211 C212 1.539(5) . ? C211 C215 1.574(6) . ? C211 S2 1.842(4) . ? C212 C213 1.432(5) . ? C213 C214 1.365(5) . ? C214 S2 1.755(4) . ? C214 Fe2 1.983(4) . ? C221 C225 1.408(8) . ? C221 C222 1.416(8) . ? C221 Fe2 2.090(4) . ? C222 C223 1.393(8) . ? C222 Fe2 2.083(4) . ? C223 C224 1.403(7) . ? C223 Fe2 2.097(4) . ? C224 C225 1.356(7) . ? C224 Fe2 2.122(5) . ? C225 Fe2 2.117(4) . ? C231 O231 1.142(6) . ? C231 Fe2 1.765(5) . ? C232 O232 1.153(6) . ? C232 Fe2 1.759(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C112 C1 C2 122.1(3) . . ? C112 C1 C5 128.4(3) . . ? C2 C1 C5 109.5(3) . . ? C212 C2 C1 121.3(3) . . ? C212 C2 C3 129.8(3) . . ? C1 C2 C3 108.8(3) . . ? F1 C3 F2 104.9(3) . . ? F1 C3 C2 115.4(3) . . ? F2 C3 C2 113.4(3) . . ? F1 C3 C4 110.8(3) . . ? F2 C3 C4 108.8(3) . . ? C2 C3 C4 103.5(3) . . ? F4 C4 F3 105.0(3) . . ? F4 C4 C5 114.2(3) . . ? F3 C4 C5 108.7(3) . . ? F4 C4 C3 114.5(3) . . ? F3 C4 C3 108.5(3) . . ? C5 C4 C3 105.8(2) . . ? F5 C5 F6 103.6(3) . . ? F5 C5 C1 114.7(3) . . ? F6 C5 C1 113.9(3) . . ? F5 C5 C4 110.7(3) . . ? F6 C5 C4 109.9(3) . . ? C1 C5 C4 104.2(3) . . ? C211 C111 C112 108.7(3) . . ? C211 C111 C115 110.5(4) . . ? C112 C111 C115 110.1(4) . . ? C211 C111 S1 114.5(3) . . ? C112 C111 S1 102.8(3) . . ? C115 C111 S1 109.9(3) . . ? C1 C112 C113 131.1(4) . . ? C1 C112 C111 116.4(3) . . ? C113 C112 C111 112.4(3) . . ? C114 C113 C112 116.3(3) . . ? C113 C114 S1 110.8(3) . . ? C113 C114 Fe1 128.2(3) . . ? S1 C114 Fe1 121.0(2) . . ? C122 C121 C125 109.8(5) . . ? C122 C121 Fe1 71.1(3) . . ? C125 C121 Fe1 71.7(3) . . ? C123 C122 C121 107.6(5) . . ? C123 C122 Fe1 70.9(3) . . ? C121 C122 Fe1 70.2(3) . . ? C122 C123 C124 107.6(5) . . ? C122 C123 Fe1 70.6(3) . . ? C124 C123 Fe1 70.0(3) . . ? C125 C124 C123 107.3(5) . . ? C125 C124 Fe1 71.2(3) . . ? C123 C124 Fe1 70.1(3) . . ? C121 C125 C124 107.7(5) . . ? C121 C125 Fe1 69.8(3) . . ? C124 C125 Fe1 70.3(3) . . ? O131 C131 Fe1 178.3(4) . . ? O132 C132 Fe1 179.4(4) . . ? C111 C211 C212 109.6(3) . . ? C111 C211 C215 111.1(3) . . ? C212 C211 C215 108.2(4) . . ? C111 C211 S2 115.6(3) . . ? C212 C211 S2 103.6(3) . . ? C215 C211 S2 108.3(3) . . ? C2 C212 C213 132.0(4) . . ? C2 C212 C211 116.7(3) . . ? C213 C212 C211 111.0(3) . . ? C214 C213 C212 116.6(3) . . ? C213 C214 S2 111.2(3) . . ? C213 C214 Fe2 128.9(3) . . ? S2 C214 Fe2 119.9(2) . . ? C225 C221 C222 107.1(4) . . ? C225 C221 Fe2 71.5(3) . . ? C222 C221 Fe2 69.9(3) . . ? C223 C222 C221 107.6(5) . . ? C223 C222 Fe2 71.1(3) . . ? C221 C222 Fe2 70.4(3) . . ? C222 C223 C224 107.5(5) . . ? C222 C223 Fe2 70.0(3) . . ? C224 C223 Fe2 71.5(3) . . ? C225 C224 C223 109.4(5) . . ? C225 C224 Fe2 71.2(3) . . ? C223 C224 Fe2 69.6(3) . . ? C224 C225 C221 108.5(4) . . ? C224 C225 Fe2 71.5(3) . . ? C221 C225 Fe2 69.4(3) . . ? O231 C231 Fe2 177.7(4) . . ? O232 C232 Fe2 176.9(5) . . ? C114 S1 C111 94.06(18) . . ? C214 S2 C211 93.56(18) . . ? C132 Fe1 C131 92.1(2) . . ? C132 Fe1 C114 89.13(17) . . ? C131 Fe1 C114 87.10(17) . . ? C132 Fe1 C121 153.5(2) . . ? C131 Fe1 C121 113.7(2) . . ? C114 Fe1 C121 97.75(17) . . ? C132 Fe1 C122 115.4(2) . . ? C131 Fe1 C122 152.3(2) . . ? C114 Fe1 C122 95.38(17) . . ? C121 Fe1 C122 38.7(2) . . ? C132 Fe1 C124 103.1(2) . . ? C131 Fe1 C124 107.3(3) . . ? C114 Fe1 C124 160.4(2) . . ? C121 Fe1 C124 64.7(2) . . ? C122 Fe1 C124 65.7(2) . . ? C132 Fe1 C123 90.8(2) . . ? C131 Fe1 C123 146.6(3) . . ? C114 Fe1 C123 126.2(3) . . ? C121 Fe1 C123 64.5(2) . . ? C122 Fe1 C123 38.5(2) . . ? C124 Fe1 C123 40.0(3) . . ? C132 Fe1 C125 140.3(2) . . ? C131 Fe1 C125 92.4(2) . . ? C114 Fe1 C125 130.5(2) . . ? C121 Fe1 C125 38.54(18) . . ? C122 Fe1 C125 65.2(2) . . ? C124 Fe1 C125 38.5(3) . . ? C123 Fe1 C125 65.3(2) . . ? C232 Fe2 C231 96.9(2) . . ? C232 Fe2 C214 86.73(19) . . ? C231 Fe2 C214 90.32(18) . . ? C232 Fe2 C222 91.1(2) . . ? C231 Fe2 C222 122.5(2) . . ? C214 Fe2 C222 147.1(2) . . ? C232 Fe2 C221 98.9(2) . . ? C231 Fe2 C221 156.1(2) . . ? C214 Fe2 C221 108.3(2) . . ? C222 Fe2 C221 39.7(2) . . ? C232 Fe2 C223 119.7(2) . . ? C231 Fe2 C223 91.0(2) . . ? C214 Fe2 C223 153.1(2) . . ? C222 Fe2 C223 38.9(2) . . ? C221 Fe2 C223 65.6(2) . . ? C232 Fe2 C225 135.5(2) . . ? C231 Fe2 C225 127.5(2) . . ? C214 Fe2 C225 93.76(17) . . ? C222 Fe2 C225 65.5(2) . . ? C221 Fe2 C225 39.1(2) . . ? C223 Fe2 C225 64.58(18) . . ? C232 Fe2 C224 155.9(2) . . ? C231 Fe2 C224 94.7(2) . . ? C214 Fe2 C224 114.3(2) . . ? C222 Fe2 C224 64.8(2) . . ? C221 Fe2 C224 64.4(2) . . ? C223 Fe2 C224 38.8(2) . . ? C225 Fe2 C224 37.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C112 C1 C2 C212 -9.6(7) . . . . ? C5 C1 C2 C212 170.8(4) . . . . ? C112 C1 C2 C3 171.4(4) . . . . ? C5 C1 C2 C3 -8.2(4) . . . . ? C212 C2 C3 F1 -34.7(6) . . . . ? C1 C2 C3 F1 144.2(4) . . . . ? C212 C2 C3 F2 86.4(5) . . . . ? C1 C2 C3 F2 -94.7(4) . . . . ? C212 C2 C3 C4 -156.0(4) . . . . ? C1 C2 C3 C4 23.0(4) . . . . ? F1 C3 C4 F4 80.1(4) . . . . ? F2 C3 C4 F4 -34.8(4) . . . . ? C2 C3 C4 F4 -155.6(3) . . . . ? F1 C3 C4 F3 -36.8(4) . . . . ? F2 C3 C4 F3 -151.6(3) . . . . ? C2 C3 C4 F3 87.5(3) . . . . ? F1 C3 C4 C5 -153.2(3) . . . . ? F2 C3 C4 C5 91.9(3) . . . . ? C2 C3 C4 C5 -29.0(3) . . . . ? C112 C1 C5 F5 49.0(5) . . . . ? C2 C1 C5 F5 -131.4(4) . . . . ? C112 C1 C5 F6 -70.1(5) . . . . ? C2 C1 C5 F6 109.5(4) . . . . ? C112 C1 C5 C4 170.2(4) . . . . ? C2 C1 C5 C4 -10.2(4) . . . . ? F4 C4 C5 F5 -85.2(4) . . . . ? F3 C4 C5 F5 31.6(4) . . . . ? C3 C4 C5 F5 148.0(3) . . . . ? F4 C4 C5 F6 28.6(4) . . . . ? F3 C4 C5 F6 145.4(3) . . . . ? C3 C4 C5 F6 -98.2(3) . . . . ? F4 C4 C5 C1 151.0(3) . . . . ? F3 C4 C5 C1 -92.2(3) . . . . ? C3 C4 C5 C1 24.2(3) . . . . ? C2 C1 C112 C113 175.2(4) . . . . ? C5 C1 C112 C113 -5.3(7) . . . . ? C2 C1 C112 C111 -9.2(6) . . . . ? C5 C1 C112 C111 170.3(4) . . . . ? C211 C111 C112 C1 42.4(5) . . . . ? C115 C111 C112 C1 -78.8(5) . . . . ? S1 C111 C112 C1 164.2(3) . . . . ? C211 C111 C112 C113 -141.1(4) . . . . ? C115 C111 C112 C113 97.7(4) . . . . ? S1 C111 C112 C113 -19.4(4) . . . . ? C1 C112 C113 C114 -169.9(4) . . . . ? C111 C112 C113 C114 14.3(6) . . . . ? C112 C113 C114 S1 -0.9(5) . . . . ? C112 C113 C114 Fe1 178.0(3) . . . . ? C125 C121 C122 C123 -0.2(5) . . . . ? Fe1 C121 C122 C123 61.4(3) . . . . ? C125 C121 C122 Fe1 -61.6(3) . . . . ? C121 C122 C123 C124 -0.5(5) . . . . ? Fe1 C122 C123 C124 60.5(4) . . . . ? C121 C122 C123 Fe1 -60.9(3) . . . . ? C122 C123 C124 C125 1.0(6) . . . . ? Fe1 C123 C124 C125 61.9(4) . . . . ? C122 C123 C124 Fe1 -60.9(3) . . . . ? C122 C121 C125 C124 0.9(6) . . . . ? Fe1 C121 C125 C124 -60.4(4) . . . . ? C122 C121 C125 Fe1 61.2(3) . . . . ? C123 C124 C125 C121 -1.1(6) . . . . ? Fe1 C124 C125 C121 60.0(4) . . . . ? C123 C124 C125 Fe1 -61.1(3) . . . . ? C112 C111 C211 C212 -56.8(4) . . . . ? C115 C111 C211 C212 64.1(4) . . . . ? S1 C111 C211 C212 -171.1(3) . . . . ? C112 C111 C211 C215 62.6(4) . . . . ? C115 C111 C211 C215 -176.4(3) . . . . ? S1 C111 C211 C215 -51.7(4) . . . . ? C112 C111 C211 S2 -173.4(3) . . . . ? C115 C111 C211 S2 -52.5(4) . . . . ? S1 C111 C211 S2 72.3(4) . . . . ? C1 C2 C212 C213 178.8(5) . . . . ? C3 C2 C212 C213 -2.4(8) . . . . ? C1 C2 C212 C211 -7.9(6) . . . . ? C3 C2 C212 C211 170.9(4) . . . . ? C111 C211 C212 C2 41.7(5) . . . . ? C215 C211 C212 C2 -79.6(5) . . . . ? S2 C211 C212 C2 165.6(3) . . . . ? C111 C211 C212 C213 -143.7(4) . . . . ? C215 C211 C212 C213 95.0(4) . . . . ? S2 C211 C212 C213 -19.8(4) . . . . ? C2 C212 C213 C214 -173.3(5) . . . . ? C211 C212 C213 C214 13.1(6) . . . . ? C212 C213 C214 S2 1.2(6) . . . . ? C212 C213 C214 Fe2 178.0(3) . . . . ? C225 C221 C222 C223 -0.5(5) . . . . ? Fe2 C221 C222 C223 61.7(3) . . . . ? C225 C221 C222 Fe2 -62.2(3) . . . . ? C221 C222 C223 C224 0.8(5) . . . . ? Fe2 C222 C223 C224 62.1(3) . . . . ? C221 C222 C223 Fe2 -61.3(3) . . . . ? C222 C223 C224 C225 -0.8(5) . . . . ? Fe2 C223 C224 C225 60.3(3) . . . . ? C222 C223 C224 Fe2 -61.1(3) . . . . ? C223 C224 C225 C221 0.5(5) . . . . ? Fe2 C224 C225 C221 59.8(3) . . . . ? C223 C224 C225 Fe2 -59.4(3) . . . . ? C222 C221 C225 C224 0.0(5) . . . . ? Fe2 C221 C225 C224 -61.2(3) . . . . ? C222 C221 C225 Fe2 61.2(3) . . . . ? C113 C114 S1 C111 -9.8(4) . . . . ? Fe1 C114 S1 C111 171.3(2) . . . . ? C211 C111 S1 C114 133.8(3) . . . . ? C112 C111 S1 C114 16.1(3) . . . . ? C115 C111 S1 C114 -101.1(3) . . . . ? C213 C214 S2 C211 -11.9(4) . . . . ? Fe2 C214 S2 C211 171.0(3) . . . . ? C111 C211 S2 C214 137.5(3) . . . . ? C212 C211 S2 C214 17.6(3) . . . . ? C215 C211 S2 C214 -97.1(3) . . . . ? O132 C132 Fe1 C131 -19(41) . . . . ? O132 C132 Fe1 C114 68(41) . . . . ? O132 C132 Fe1 C121 174(100) . . . . ? O132 C132 Fe1 C122 164(41) . . . . ? O132 C132 Fe1 C124 -127(41) . . . . ? O132 C132 Fe1 C123 -165(100) . . . . ? O132 C132 Fe1 C125 -115(41) . . . . ? O131 C131 Fe1 C132 -50(14) . . . . ? O131 C131 Fe1 C114 -139(14) . . . . ? O131 C131 Fe1 C121 124(14) . . . . ? O131 C131 Fe1 C122 125(14) . . . . ? O131 C131 Fe1 C124 55(14) . . . . ? O131 C131 Fe1 C123 45(14) . . . . ? O131 C131 Fe1 C125 91(14) . . . . ? C113 C114 Fe1 C132 -30.9(4) . . . . ? S1 C114 Fe1 C132 147.9(3) . . . . ? C113 C114 Fe1 C131 61.3(4) . . . . ? S1 C114 Fe1 C131 -120.0(3) . . . . ? C113 C114 Fe1 C121 174.8(4) . . . . ? S1 C114 Fe1 C121 -6.5(3) . . . . ? C113 C114 Fe1 C122 -146.3(4) . . . . ? S1 C114 Fe1 C122 32.4(3) . . . . ? C113 C114 Fe1 C124 -160.3(8) . . . . ? S1 C114 Fe1 C124 18.4(10) . . . . ? C113 C114 Fe1 C123 -121.2(4) . . . . ? S1 C114 Fe1 C123 57.5(3) . . . . ? C113 C114 Fe1 C125 151.9(4) . . . . ? S1 C114 Fe1 C125 -29.3(4) . . . . ? C122 C121 Fe1 C132 -14.9(6) . . . . ? C125 C121 Fe1 C132 104.4(5) . . . . ? C122 C121 Fe1 C131 179.2(3) . . . . ? C125 C121 Fe1 C131 -61.5(4) . . . . ? C122 C121 Fe1 C114 88.9(3) . . . . ? C125 C121 Fe1 C114 -151.7(4) . . . . ? C125 C121 Fe1 C122 119.3(5) . . . . ? C122 C121 Fe1 C124 -82.1(4) . . . . ? C125 C121 Fe1 C124 37.3(4) . . . . ? C122 C121 Fe1 C123 -37.6(4) . . . . ? C125 C121 Fe1 C123 81.7(4) . . . . ? C122 C121 Fe1 C125 -119.3(5) . . . . ? C123 C122 Fe1 C132 55.0(4) . . . . ? C121 C122 Fe1 C132 172.7(3) . . . . ? C123 C122 Fe1 C131 -119.4(5) . . . . ? C121 C122 Fe1 C131 -1.7(6) . . . . ? C123 C122 Fe1 C114 146.6(4) . . . . ? C121 C122 Fe1 C114 -95.7(3) . . . . ? C123 C122 Fe1 C121 -117.7(5) . . . . ? C123 C122 Fe1 C124 -38.5(4) . . . . ? C121 C122 Fe1 C124 79.2(4) . . . . ? C121 C122 Fe1 C123 117.7(5) . . . . ? C123 C122 Fe1 C125 -80.9(4) . . . . ? C121 C122 Fe1 C125 36.8(3) . . . . ? C125 C124 Fe1 C132 167.6(3) . . . . ? C123 C124 Fe1 C132 -75.2(4) . . . . ? C125 C124 Fe1 C131 71.2(4) . . . . ? C123 C124 Fe1 C131 -171.6(3) . . . . ? C125 C124 Fe1 C114 -64.9(10) . . . . ? C123 C124 Fe1 C114 52.4(10) . . . . ? C125 C124 Fe1 C121 -37.3(3) . . . . ? C123 C124 Fe1 C121 79.9(4) . . . . ? C125 C124 Fe1 C122 -80.2(3) . . . . ? C123 C124 Fe1 C122 37.1(3) . . . . ? C125 C124 Fe1 C123 -117.2(5) . . . . ? C123 C124 Fe1 C125 117.2(5) . . . . ? C122 C123 Fe1 C132 -132.3(4) . . . . ? C124 C123 Fe1 C132 109.7(4) . . . . ? C122 C123 Fe1 C131 132.7(4) . . . . ? C124 C123 Fe1 C131 14.7(6) . . . . ? C122 C123 Fe1 C114 -42.8(4) . . . . ? C124 C123 Fe1 C114 -160.8(3) . . . . ? C122 C123 Fe1 C121 37.8(3) . . . . ? C124 C123 Fe1 C121 -80.2(4) . . . . ? C124 C123 Fe1 C122 -118.0(5) . . . . ? C122 C123 Fe1 C124 118.0(5) . . . . ? C122 C123 Fe1 C125 80.6(4) . . . . ? C124 C123 Fe1 C125 -37.5(3) . . . . ? C121 C125 Fe1 C132 -137.5(4) . . . . ? C124 C125 Fe1 C132 -19.1(5) . . . . ? C121 C125 Fe1 C131 126.3(4) . . . . ? C124 C125 Fe1 C131 -115.3(4) . . . . ? C121 C125 Fe1 C114 38.1(5) . . . . ? C124 C125 Fe1 C114 156.5(4) . . . . ? C124 C125 Fe1 C121 118.4(5) . . . . ? C121 C125 Fe1 C122 -36.9(3) . . . . ? C124 C125 Fe1 C122 81.5(4) . . . . ? C121 C125 Fe1 C124 -118.4(5) . . . . ? C121 C125 Fe1 C123 -79.5(4) . . . . ? C124 C125 Fe1 C123 38.9(4) . . . . ? O232 C232 Fe2 C231 169(7) . . . . ? O232 C232 Fe2 C214 -101(7) . . . . ? O232 C232 Fe2 C222 47(7) . . . . ? O232 C232 Fe2 C221 7(7) . . . . ? O232 C232 Fe2 C223 74(7) . . . . ? O232 C232 Fe2 C225 -9(7) . . . . ? O232 C232 Fe2 C224 51(7) . . . . ? O231 C231 Fe2 C232 -126(13) . . . . ? O231 C231 Fe2 C214 147(13) . . . . ? O231 C231 Fe2 C222 -30(13) . . . . ? O231 C231 Fe2 C221 5(14) . . . . ? O231 C231 Fe2 C223 -6(13) . . . . ? O231 C231 Fe2 C225 52(13) . . . . ? O231 C231 Fe2 C224 33(13) . . . . ? C213 C214 Fe2 C232 -69.7(5) . . . . ? S2 C214 Fe2 C232 106.9(3) . . . . ? C213 C214 Fe2 C231 27.2(5) . . . . ? S2 C214 Fe2 C231 -156.2(3) . . . . ? C213 C214 Fe2 C222 -156.8(4) . . . . ? S2 C214 Fe2 C222 19.8(5) . . . . ? C213 C214 Fe2 C221 -168.0(4) . . . . ? S2 C214 Fe2 C221 8.5(4) . . . . ? C213 C214 Fe2 C223 120.1(5) . . . . ? S2 C214 Fe2 C223 -63.3(5) . . . . ? C213 C214 Fe2 C225 154.8(5) . . . . ? S2 C214 Fe2 C225 -28.6(3) . . . . ? C213 C214 Fe2 C224 122.5(4) . . . . ? S2 C214 Fe2 C224 -60.9(3) . . . . ? C223 C222 Fe2 C232 139.8(3) . . . . ? C221 C222 Fe2 C232 -102.7(4) . . . . ? C223 C222 Fe2 C231 40.9(4) . . . . ? C221 C222 Fe2 C231 158.4(4) . . . . ? C223 C222 Fe2 C214 -134.4(4) . . . . ? C221 C222 Fe2 C214 -16.9(5) . . . . ? C223 C222 Fe2 C221 -117.5(5) . . . . ? C221 C222 Fe2 C223 117.5(5) . . . . ? C223 C222 Fe2 C225 -79.3(3) . . . . ? C221 C222 Fe2 C225 38.2(3) . . . . ? C223 C222 Fe2 C224 -38.0(3) . . . . ? C221 C222 Fe2 C224 79.5(4) . . . . ? C225 C221 Fe2 C232 -162.2(3) . . . . ? C222 C221 Fe2 C232 80.9(3) . . . . ? C225 C221 Fe2 C231 66.8(8) . . . . ? C222 C221 Fe2 C231 -50.1(8) . . . . ? C225 C221 Fe2 C214 -72.7(3) . . . . ? C222 C221 Fe2 C214 170.4(3) . . . . ? C225 C221 Fe2 C222 116.9(4) . . . . ? C225 C221 Fe2 C223 79.1(3) . . . . ? C222 C221 Fe2 C223 -37.7(3) . . . . ? C222 C221 Fe2 C225 -116.9(4) . . . . ? C225 C221 Fe2 C224 36.1(3) . . . . ? C222 C221 Fe2 C224 -80.8(3) . . . . ? C222 C223 Fe2 C232 -47.9(4) . . . . ? C224 C223 Fe2 C232 -165.2(3) . . . . ? C222 C223 Fe2 C231 -146.5(3) . . . . ? C224 C223 Fe2 C231 96.2(4) . . . . ? C222 C223 Fe2 C214 120.8(5) . . . . ? C224 C223 Fe2 C214 3.5(6) . . . . ? C224 C223 Fe2 C222 -117.3(4) . . . . ? C222 C223 Fe2 C221 38.5(3) . . . . ? C224 C223 Fe2 C221 -78.8(4) . . . . ? C222 C223 Fe2 C225 81.8(4) . . . . ? C224 C223 Fe2 C225 -35.5(3) . . . . ? C222 C223 Fe2 C224 117.3(4) . . . . ? C224 C225 Fe2 C232 144.4(3) . . . . ? C221 C225 Fe2 C232 25.5(4) . . . . ? C224 C225 Fe2 C231 -33.2(4) . . . . ? C221 C225 Fe2 C231 -152.0(3) . . . . ? C224 C225 Fe2 C214 -126.5(3) . . . . ? C221 C225 Fe2 C214 114.7(3) . . . . ? C224 C225 Fe2 C222 80.1(3) . . . . ? C221 C225 Fe2 C222 -38.8(3) . . . . ? C224 C225 Fe2 C221 118.8(4) . . . . ? C224 C225 Fe2 C223 37.0(3) . . . . ? C221 C225 Fe2 C223 -81.9(3) . . . . ? C221 C225 Fe2 C224 -118.8(4) . . . . ? C225 C224 Fe2 C232 -87.2(6) . . . . ? C223 C224 Fe2 C232 32.8(7) . . . . ? C225 C224 Fe2 C231 154.2(3) . . . . ? C223 C224 Fe2 C231 -85.8(3) . . . . ? C225 C224 Fe2 C214 61.7(4) . . . . ? C223 C224 Fe2 C214 -178.3(3) . . . . ? C225 C224 Fe2 C222 -81.9(4) . . . . ? C223 C224 Fe2 C222 38.1(3) . . . . ? C225 C224 Fe2 C221 -37.8(3) . . . . ? C223 C224 Fe2 C221 82.2(4) . . . . ? C225 C224 Fe2 C223 -120.0(5) . . . . ? C223 C224 Fe2 C225 120.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.909 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.097 #===END #------------------------------------------------------------------------------ data_1027_FeCp'dppe_open _database_code_depnum_ccdc_archive 'CCDC 818898' #TrackingRef 'Akita.CIF' #TrackingRef 'Akita.CIF' #TrackingRef 'Akita.CIF' _audit_creation_date 'Thu Dec 14 16:27:18 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C79 H70 F6 Fe2 P4 S2 ' _chemical_formula_moiety 'C79 H70 F6 Fe2 P4 S2 ' _chemical_formula_weight 1433.12 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.566(9) _cell_length_b 8.579(3) _cell_length_c 38.08(2) _cell_angle_alpha 90 _cell_angle_beta 102.99(2) _cell_angle_gamma 90 _cell_volume 6865(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16578 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # 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 25083 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 48 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7123 _reflns_number_gt 4204 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1471 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4204 _refine_ls_number_parameters 452 _refine_ls_goodness_of_fit_ref 0.765 _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 0.43 _refine_diff_density_min -0.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 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) ; 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 0.83561(3) 0.09879(6) 0.61759(1) 0.0241(1) Uani 1.00 d . . . S(1) S 0.86965(5) 0.1147(1) 0.70406(2) 0.0347(2) Uani 1.00 d . . . P(1) P 0.88122(5) -0.0678(1) 0.58868(3) 0.0271(2) Uani 1.00 d . . . P(2) P 0.76654(5) -0.0828(1) 0.62000(2) 0.0271(2) Uani 1.00 d . . . F(1) F 0.963(1) -0.445(2) 0.6878(5) 0.088(7) Uani 0.50 d P . . F(1A) F 0.9825(9) -0.446(2) 0.6911(4) 0.045(3) Uani 0.50 d P . . F(2) F 0.896(1) -0.454(2) 0.7238(5) 0.086(6) Uani 0.50 d P . . F(2A) F 0.900(1) -0.453(2) 0.7121(4) 0.047(3) Uani 0.50 d P . . F(3) F 0.9734(7) -0.638(2) 0.7640(6) 0.057(3) Uani 0.50 d P . . F(4) F 1.0462(7) -0.602(2) 0.7341(6) 0.066(5) Uani 0.50 d P . . C(1) C 0.9757(2) -0.2585(4) 0.73512(9) 0.0270(8) Uani 1.00 d . . . C(2) C 0.9595(2) -0.4206(5) 0.7220(1) 0.0349(9) Uani 1.00 d . . . C(3) C 1.0000 -0.5291(6) 0.7500 0.033(1) Uani 1.00 d S . . C(11) C 0.9147(2) -0.0114(4) 0.73501(9) 0.0312(9) Uani 1.00 d . . . C(12) C 0.9381(2) -0.1287(4) 0.71693(9) 0.0258(8) Uani 1.00 d . . . C(13) C 0.9175(2) -0.1131(4) 0.67836(9) 0.0267(8) Uani 1.00 d . . . C(14) C 0.8804(2) 0.0136(4) 0.66598(9) 0.0259(8) Uani 1.00 d . . . C(15) C 0.9209(2) 0.0113(5) 0.7746(1) 0.044(1) Uani 1.00 d . . . C(21) C 0.8459(2) -0.2659(5) 0.5891(1) 0.044(1) Uani 1.00 d . . . C(22) C 0.8027(2) -0.2746(4) 0.6154(1) 0.0305(8) Uani 1.00 d . . . C(31) C 0.9679(2) -0.1005(5) 0.6022(1) 0.0365(9) Uani 1.00 d . . . C(32) C 1.0058(2) 0.0044(5) 0.6252(1) 0.039(1) Uani 1.00 d . . . C(33) C 1.0720(2) -0.0145(7) 0.6346(1) 0.054(1) Uani 1.00 d . . . C(34) C 1.0997(3) -0.1406(8) 0.6218(2) 0.066(2) Uani 1.00 d . . . C(35) C 1.0630(3) -0.2449(7) 0.5991(2) 0.066(2) Uani 1.00 d . . . C(36) C 0.9968(2) -0.2269(6) 0.5888(1) 0.050(1) Uani 1.00 d . . . C(41) C 0.8741(2) -0.0327(5) 0.5400(1) 0.0310(8) Uani 1.00 d . . . C(42) C 0.9225(2) 0.0370(6) 0.5273(1) 0.048(1) Uani 1.00 d . . . C(43) C 0.9146(3) 0.0774(7) 0.4915(1) 0.061(1) Uani 1.00 d . . . C(44) C 0.8590(3) 0.0455(7) 0.4673(1) 0.057(1) Uani 1.00 d . . . C(45) C 0.8103(2) -0.0243(6) 0.4791(1) 0.054(1) Uani 1.00 d . . . C(46) C 0.8177(2) -0.0636(6) 0.5152(1) 0.044(1) Uani 1.00 d . . . C(51) C 0.7355(2) -0.1013(5) 0.6609(1) 0.0357(9) Uani 1.00 d . . . C(52) C 0.6865(3) -0.0048(6) 0.6653(1) 0.056(1) Uani 1.00 d . . . C(53) C 0.6640(3) -0.0061(7) 0.6965(2) 0.071(2) Uani 1.00 d . . . C(54) C 0.6897(3) -0.1091(7) 0.7240(1) 0.066(2) Uani 1.00 d . . . C(55) C 0.7383(3) -0.2042(7) 0.7203(1) 0.059(1) Uani 1.00 d . . . C(56) C 0.7615(2) -0.2008(6) 0.6893(1) 0.047(1) Uani 1.00 d . . . C(61) C 0.6912(2) -0.0955(5) 0.5848(1) 0.0369(9) Uani 1.00 d . . . C(62) C 0.6425(2) -0.1932(6) 0.5893(1) 0.051(1) Uani 1.00 d . . . C(63) C 0.5869(3) -0.2076(7) 0.5627(2) 0.071(2) Uani 1.00 d . . . C(64) C 0.5794(3) -0.1247(7) 0.5313(2) 0.071(2) Uani 1.00 d . . . C(65) C 0.6275(3) -0.0278(6) 0.5263(1) 0.061(1) Uani 1.00 d . . . C(66) C 0.6831(2) -0.0121(5) 0.5529(1) 0.043(1) Uani 1.00 d . . . C(71) C 0.8027(2) 0.3116(4) 0.6354(1) 0.0363(9) Uani 1.00 d . . . C(72) C 0.8670(2) 0.3267(4) 0.6333(1) 0.0357(10) Uani 1.00 d . . . C(73) C 0.8735(2) 0.3004(5) 0.5976(1) 0.0376(10) Uani 1.00 d . . . C(74) C 0.8112(2) 0.2674(4) 0.5765(1) 0.0342(9) Uani 1.00 d . . . C(75) C 0.7687(2) 0.2744(4) 0.5997(1) 0.0338(9) Uani 1.00 d . . . C(76) C 0.7720(5) 0.362(1) 0.6638(3) 0.049(2) Uani 0.51 d P . . C(76A) C 0.9295(5) 0.339(1) 0.5837(3) 0.049(2) Uani 0.49 d P . . H(1) H 0.9239 -0.0882 0.7864 0.0440 Uiso 1.00 calc . . . H(2) H 0.8843 0.0662 0.7787 0.0440 Uiso 1.00 calc . . . H(3) H 0.9586 0.0711 0.7843 0.0440 Uiso 1.00 calc . . . H(4) H 0.9294 -0.1878 0.6621 0.0318 Uiso 1.00 calc . . . H(5) H 0.8229 -0.2934 0.5657 0.0546 Uiso 1.00 calc . . . H(6) H 0.8801 -0.3413 0.5963 0.0546 Uiso 1.00 calc . . . H(7) H 0.8263 -0.3081 0.6386 0.0373 Uiso 1.00 calc . . . H(8) H 0.7695 -0.3492 0.6071 0.0373 Uiso 1.00 calc . . . H(9) H 0.9859 0.0917 0.6348 0.0496 Uiso 1.00 calc . . . H(10) H 1.0989 0.0625 0.6500 0.0658 Uiso 1.00 calc . . . H(11) H 1.1451 -0.1534 0.6288 0.0774 Uiso 1.00 calc . . . H(12) H 1.0831 -0.3333 0.5904 0.0827 Uiso 1.00 calc . . . H(13) H 0.9704 -0.3006 0.5721 0.0611 Uiso 1.00 calc . . . H(14) H 0.9624 0.0588 0.5439 0.0578 Uiso 1.00 calc . . . H(15) H 0.9488 0.1303 0.4836 0.0733 Uiso 1.00 calc . . . H(16) H 0.8542 0.0749 0.4424 0.0684 Uiso 1.00 calc . . . H(17) H 0.7707 -0.0481 0.4621 0.0639 Uiso 1.00 calc . . . H(18) H 0.7831 -0.1129 0.5232 0.0550 Uiso 1.00 calc . . . H(19) H 0.6681 0.0669 0.6462 0.0664 Uiso 1.00 calc . . . H(20) H 0.6302 0.0648 0.6990 0.0843 Uiso 1.00 calc . . . H(21) H 0.6734 -0.1130 0.7458 0.0770 Uiso 1.00 calc . . . H(22) H 0.7564 -0.2750 0.7396 0.0698 Uiso 1.00 calc . . . H(23) H 0.7963 -0.2706 0.6870 0.0567 Uiso 1.00 calc . . . H(24) H 0.6478 -0.2536 0.6114 0.0633 Uiso 1.00 calc . . . H(25) H 0.5532 -0.2760 0.5663 0.0882 Uiso 1.00 calc . . . H(26) H 0.5404 -0.1334 0.5125 0.0852 Uiso 1.00 calc . . . H(27) H 0.6226 0.0304 0.5041 0.0729 Uiso 1.00 calc . . . H(28) H 0.7168 0.0575 0.5491 0.0525 Uiso 1.00 calc . . . H(29) H 0.9016 0.3512 0.6533 0.0425 Uiso 1.00 calc . . . H(30) H 0.8004 0.2472 0.5510 0.0421 Uiso 1.00 calc . . . H(31) H 0.7232 0.2588 0.5925 0.0417 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) 0.0264(3) 0.0221(3) 0.0211(3) 0.0021(2) -0.0002(2) 0.0015(2) S(1) 0.0451(6) 0.0322(5) 0.0233(5) 0.0107(5) 0.0003(4) -0.0013(4) P(1) 0.0293(5) 0.0264(5) 0.0251(5) 0.0022(4) 0.0052(4) 0.0010(4) P(2) 0.0262(5) 0.0287(5) 0.0249(5) 0.0004(4) 0.0023(4) 0.0029(4) F(1) 0.17(2) 0.037(5) 0.029(4) 0.022(8) -0.039(7) -0.013(3) F(1A) 0.080(7) 0.038(5) 0.014(4) 0.014(4) 0.006(5) -0.002(4) F(2) 0.029(5) 0.056(7) 0.16(2) -0.010(5) -0.01(1) 0.040(9) F(2A) 0.041(6) 0.027(5) 0.062(5) -0.008(4) -0.011(4) -0.006(4) F(3) 0.048(8) 0.047(5) 0.063(5) -0.019(6) -0.014(6) 0.025(4) F(4) 0.043(8) 0.09(1) 0.056(5) 0.018(6) -0.010(6) -0.035(7) C(1) 0.032(2) 0.027(2) 0.021(2) -0.003(2) 0.004(1) -0.002(1) C(2) 0.037(2) 0.029(2) 0.033(2) -0.001(2) -0.006(2) -0.004(2) C(3) 0.041(3) 0.023(3) 0.034(3) 0.0000 0.004(2) 0.0000 C(11) 0.036(2) 0.032(2) 0.022(2) 0.003(2) -0.001(2) 0.001(1) C(12) 0.029(2) 0.026(2) 0.020(2) 0.000(2) 0.001(1) -0.001(1) C(13) 0.030(2) 0.027(2) 0.020(2) 0.000(2) -0.001(1) -0.001(1) C(14) 0.022(2) 0.029(2) 0.022(2) 0.002(2) -0.002(1) 0.002(1) C(15) 0.061(3) 0.046(3) 0.023(2) 0.018(2) 0.004(2) -0.001(2) C(21) 0.059(3) 0.034(2) 0.045(3) -0.001(2) 0.021(2) -0.004(2) C(22) 0.032(2) 0.026(2) 0.033(2) -0.005(2) 0.005(2) 0.003(1) C(31) 0.036(2) 0.045(2) 0.028(2) 0.011(2) 0.008(2) 0.013(2) C(32) 0.029(2) 0.056(3) 0.033(2) 0.004(2) 0.007(2) 0.010(2) C(33) 0.040(3) 0.091(4) 0.031(2) 0.001(3) 0.008(2) 0.019(2) C(34) 0.040(3) 0.113(5) 0.048(3) 0.029(3) 0.017(2) 0.032(3) C(35) 0.064(4) 0.082(4) 0.062(4) 0.039(3) 0.033(3) 0.024(3) C(36) 0.057(3) 0.056(3) 0.041(3) 0.016(3) 0.019(2) 0.011(2) C(41) 0.030(2) 0.032(2) 0.029(2) 0.005(2) 0.003(2) -0.001(1) C(42) 0.039(3) 0.070(3) 0.032(2) -0.003(2) 0.000(2) 0.017(2) C(43) 0.056(3) 0.083(4) 0.046(3) 0.004(3) 0.015(2) 0.027(3) C(44) 0.064(3) 0.081(4) 0.023(2) 0.024(3) 0.004(2) 0.015(2) C(45) 0.050(3) 0.072(3) 0.033(2) 0.004(3) -0.005(2) -0.005(2) C(46) 0.041(3) 0.055(3) 0.035(2) -0.006(2) 0.005(2) -0.005(2) C(51) 0.033(2) 0.036(2) 0.037(2) -0.002(2) 0.007(2) 0.004(2) C(52) 0.064(3) 0.062(3) 0.048(3) 0.023(3) 0.026(3) 0.018(2) C(53) 0.072(4) 0.083(4) 0.071(4) 0.027(3) 0.045(3) 0.013(3) C(54) 0.073(4) 0.088(4) 0.044(3) -0.001(3) 0.029(3) 0.006(3) C(55) 0.067(4) 0.073(4) 0.042(3) 0.003(3) 0.021(2) 0.018(2) C(56) 0.047(3) 0.056(3) 0.038(2) 0.007(2) 0.013(2) 0.015(2) C(61) 0.034(2) 0.039(2) 0.035(2) -0.001(2) 0.002(2) -0.002(2) C(62) 0.035(3) 0.055(3) 0.060(3) -0.014(2) 0.002(2) 0.003(2) C(63) 0.040(3) 0.076(4) 0.087(4) -0.021(3) -0.004(3) -0.006(3) C(64) 0.046(3) 0.073(4) 0.075(4) -0.010(3) -0.025(3) -0.008(3) C(65) 0.059(3) 0.066(3) 0.044(3) 0.005(3) -0.014(2) 0.003(2) C(66) 0.037(2) 0.047(3) 0.038(2) -0.002(2) -0.006(2) 0.000(2) C(71) 0.046(3) 0.025(2) 0.036(2) 0.011(2) 0.005(2) -0.002(2) C(72) 0.044(3) 0.019(2) 0.037(2) -0.001(2) -0.005(2) -0.004(1) C(73) 0.047(3) 0.023(2) 0.044(2) -0.006(2) 0.012(2) 0.007(2) C(74) 0.047(3) 0.024(2) 0.027(2) 0.007(2) -0.001(2) 0.012(1) C(75) 0.035(2) 0.026(2) 0.035(2) 0.012(2) -0.003(2) 0.004(2) C(76) 0.054(4) 0.043(4) 0.047(4) 0.001(3) 0.009(3) 0.004(3) C(76A) 0.054(4) 0.043(4) 0.047(4) 0.001(3) 0.009(3) 0.004(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS _computing_cell_refinement PROCESS _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) 2.170(1) . . yes Fe(1) P(2) 2.172(1) . . yes Fe(1) C(14) 2.016(3) . . yes Fe(1) C(71) 2.125(4) . . yes Fe(1) C(72) 2.111(4) . . yes Fe(1) C(73) 2.126(4) . . yes Fe(1) C(74) 2.108(4) . . yes Fe(1) C(75) 2.091(4) . . yes S(1) C(11) 1.728(4) . . yes S(1) C(14) 1.750(4) . . yes P(1) C(21) 1.864(4) . . yes P(1) C(31) 1.844(4) . . yes P(1) C(41) 1.851(4) . . yes P(2) C(22) 1.845(4) . . yes P(2) C(51) 1.834(5) . . yes P(2) C(61) 1.862(4) . . yes F(1) F(1A) 0.40(3) . . yes F(1) C(2) 1.34(2) . . yes F(1A) C(2) 1.39(2) . . yes F(2) F(2A) 0.47(3) . . yes F(2) C(2) 1.42(2) . . yes F(2A) C(2) 1.29(2) . . yes F(3) F(4) 0.54(2) . 2_756 yes F(3) C(3) 1.27(2) . . yes F(4) C(3) 1.42(2) . . yes C(1) C(1) 1.360(6) . 2_756 yes C(1) C(2) 1.492(5) . . yes C(1) C(12) 1.458(5) . . yes C(2) C(3) 1.533(5) . . yes C(11) C(12) 1.378(5) . . yes C(11) C(15) 1.497(5) . . yes C(12) C(13) 1.442(5) . . yes C(13) C(14) 1.368(5) . . yes C(21) C(22) 1.517(7) . . yes C(31) C(32) 1.388(6) . . yes C(31) C(36) 1.403(7) . . yes C(32) C(33) 1.400(6) . . yes C(33) C(34) 1.377(9) . . yes C(34) C(35) 1.366(8) . . yes C(35) C(36) 1.401(8) . . yes C(41) C(42) 1.380(7) . . yes C(41) C(46) 1.387(6) . . yes C(42) C(43) 1.382(7) . . yes C(43) C(44) 1.364(7) . . yes C(44) C(45) 1.368(8) . . yes C(45) C(46) 1.390(7) . . yes C(51) C(52) 1.383(7) . . yes C(51) C(56) 1.394(6) . . yes C(52) C(53) 1.378(9) . . yes C(53) C(54) 1.388(8) . . yes C(54) C(55) 1.360(9) . . yes C(55) C(56) 1.381(8) . . yes C(61) C(62) 1.383(7) . . yes C(61) C(66) 1.389(6) . . yes C(62) C(63) 1.392(7) . . yes C(63) C(64) 1.368(9) . . yes C(64) C(65) 1.377(8) . . yes C(65) C(66) 1.393(6) . . yes C(71) C(72) 1.413(7) . . yes C(71) C(75) 1.429(5) . . yes C(71) C(76) 1.45(1) . . yes C(72) C(73) 1.417(6) . . yes C(73) C(74) 1.429(6) . . yes C(73) C(76A) 1.46(1) . . yes C(74) C(75) 1.410(6) . . 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) P(2) 86.69(5) . . . yes P(1) Fe(1) C(14) 92.6(1) . . . yes P(1) Fe(1) C(71) 161.8(1) . . . yes P(1) Fe(1) C(72) 126.9(1) . . . yes P(1) Fe(1) C(73) 95.7(1) . . . yes P(1) Fe(1) C(74) 98.1(1) . . . yes P(1) Fe(1) C(75) 131.9(1) . . . yes P(2) Fe(1) C(14) 83.9(1) . . . yes P(2) Fe(1) C(71) 108.8(1) . . . yes P(2) Fe(1) C(72) 146.3(1) . . . yes P(2) Fe(1) C(73) 157.1(1) . . . yes P(2) Fe(1) C(74) 117.7(1) . . . yes P(2) Fe(1) C(75) 95.8(1) . . . yes C(14) Fe(1) C(71) 98.4(1) . . . yes C(14) Fe(1) C(72) 91.1(1) . . . yes C(14) Fe(1) C(73) 118.6(1) . . . yes C(14) Fe(1) C(74) 156.3(1) . . . yes C(14) Fe(1) C(75) 135.5(2) . . . yes C(71) Fe(1) C(72) 39.0(2) . . . yes C(71) Fe(1) C(73) 66.3(2) . . . yes C(71) Fe(1) C(74) 66.5(2) . . . yes C(71) Fe(1) C(75) 39.6(1) . . . yes C(72) Fe(1) C(73) 39.1(2) . . . yes C(72) Fe(1) C(74) 65.5(1) . . . yes C(72) Fe(1) C(75) 65.1(2) . . . yes C(73) Fe(1) C(74) 39.4(2) . . . yes C(73) Fe(1) C(75) 65.8(2) . . . yes C(74) Fe(1) C(75) 39.2(2) . . . yes C(11) S(1) C(14) 95.5(2) . . . yes Fe(1) P(1) C(21) 111.3(2) . . . yes Fe(1) P(1) C(31) 120.3(1) . . . yes Fe(1) P(1) C(41) 117.1(1) . . . yes C(21) P(1) C(31) 104.4(2) . . . yes C(21) P(1) C(41) 102.4(2) . . . yes C(31) P(1) C(41) 98.9(2) . . . yes Fe(1) P(2) C(22) 109.1(1) . . . yes Fe(1) P(2) C(51) 118.8(1) . . . yes Fe(1) P(2) C(61) 120.5(1) . . . yes C(22) P(2) C(51) 104.2(2) . . . yes C(22) P(2) C(61) 101.5(2) . . . yes C(51) P(2) C(61) 100.3(2) . . . yes F(1A) F(1) C(2) 88(3) . . . yes F(1) F(1A) C(2) 74(3) . . . yes F(2A) F(2) C(2) 65(3) . . . yes F(2) F(2A) C(2) 95(3) . . . yes F(4) F(3) C(3) 94(3) 2_756 . . yes F(3) F(4) C(3) 63(2) 2_756 . . yes C(1) C(1) C(2) 111.0(2) 2_756 . . yes C(1) C(1) C(12) 129.7(2) 2_756 . . yes C(2) C(1) C(12) 119.3(3) . . . yes F(1) C(2) F(1A) 16(1) . . . yes F(1) C(2) F(2) 106(1) . . . yes F(1) C(2) F(2A) 87(1) . . . yes F(1) C(2) C(1) 114.2(10) . . . yes F(1) C(2) C(3) 115.6(9) . . . yes F(1A) C(2) F(2) 122(1) . . . yes F(1A) C(2) F(2A) 104(1) . . . yes F(1A) C(2) C(1) 109.2(8) . . . yes F(1A) C(2) C(3) 103.7(8) . . . yes F(2) C(2) F(2A) 19(1) . . . yes F(2) C(2) C(1) 109.3(9) . . . yes F(2) C(2) C(3) 104.4(8) . . . yes F(2A) C(2) C(1) 116.0(8) . . . yes F(2A) C(2) C(3) 116.7(8) . . . yes C(1) C(2) C(3) 106.2(3) . . . yes F(3) C(3) F(3) 85(1) . . 2_756 yes F(3) C(3) F(4) 106(1) . . . yes F(3) C(3) F(4) 22(1) . . 2_756 yes F(3) C(3) C(2) 119.7(7) . . . yes F(3) C(3) C(2) 113.2(9) . . 2_756 yes F(3) C(3) F(4) 22(1) 2_756 . . yes F(3) C(3) F(4) 106(1) 2_756 . 2_756 yes F(3) C(3) C(2) 113.2(9) 2_756 . . yes F(3) C(3) C(2) 119.7(7) 2_756 . 2_756 yes F(4) C(3) F(4) 128(1) . . 2_756 yes F(4) C(3) C(2) 108.3(8) . . . yes F(4) C(3) C(2) 102.5(7) . . 2_756 yes F(4) C(3) C(2) 102.5(7) 2_756 . . yes F(4) C(3) C(2) 108.3(8) 2_756 . 2_756 yes C(2) C(3) C(2) 105.2(4) . . 2_756 yes S(1) C(11) C(12) 109.2(2) . . . yes S(1) C(11) C(15) 121.0(3) . . . yes C(12) C(11) C(15) 129.7(3) . . . yes C(1) C(12) C(11) 123.2(3) . . . yes C(1) C(12) C(13) 124.5(3) . . . yes C(11) C(12) C(13) 112.2(3) . . . yes C(12) C(13) C(14) 116.6(3) . . . yes Fe(1) C(14) S(1) 116.9(2) . . . yes Fe(1) C(14) C(13) 136.5(3) . . . yes S(1) C(14) C(13) 106.5(2) . . . yes P(1) C(21) C(22) 111.3(3) . . . yes P(2) C(22) C(21) 110.7(3) . . . yes P(1) C(31) C(32) 119.6(3) . . . yes P(1) C(31) C(36) 121.5(3) . . . yes C(32) C(31) C(36) 118.9(4) . . . yes C(31) C(32) C(33) 120.6(4) . . . yes C(32) C(33) C(34) 119.9(5) . . . yes C(33) C(34) C(35) 120.3(5) . . . yes C(34) C(35) C(36) 120.9(6) . . . yes C(31) C(36) C(35) 119.5(4) . . . yes P(1) C(41) C(42) 121.4(3) . . . yes P(1) C(41) C(46) 120.9(3) . . . yes C(42) C(41) C(46) 117.4(4) . . . yes C(41) C(42) C(43) 121.2(4) . . . yes C(42) C(43) C(44) 120.7(5) . . . yes C(43) C(44) C(45) 119.3(5) . . . yes C(44) C(45) C(46) 120.3(4) . . . yes C(41) C(46) C(45) 121.0(5) . . . yes P(2) C(51) C(52) 119.2(3) . . . yes P(2) C(51) C(56) 123.5(3) . . . yes C(52) C(51) C(56) 117.1(4) . . . yes C(51) C(52) C(53) 121.8(5) . . . yes C(52) C(53) C(54) 119.9(6) . . . yes C(53) C(54) C(55) 119.2(6) . . . yes C(54) C(55) C(56) 120.8(5) . . . yes C(51) C(56) C(55) 121.1(5) . . . yes P(2) C(61) C(62) 120.7(3) . . . yes P(2) C(61) C(66) 121.1(3) . . . yes C(62) C(61) C(66) 118.1(4) . . . yes C(61) C(62) C(63) 121.2(5) . . . yes C(62) C(63) C(64) 120.2(5) . . . yes C(63) C(64) C(65) 119.4(5) . . . yes C(64) C(65) C(66) 120.7(5) . . . yes C(61) C(66) C(65) 120.4(4) . . . yes Fe(1) C(71) C(72) 70.0(2) . . . yes Fe(1) C(71) C(75) 68.9(2) . . . yes Fe(1) C(71) C(76) 137.1(4) . . . yes C(72) C(71) C(75) 105.4(4) . . . yes C(72) C(71) C(76) 129.3(5) . . . yes C(75) C(71) C(76) 123.4(5) . . . yes Fe(1) C(72) C(71) 71.0(2) . . . yes Fe(1) C(72) C(73) 71.1(2) . . . yes C(71) C(72) C(73) 110.6(3) . . . yes Fe(1) C(73) C(72) 69.9(2) . . . yes Fe(1) C(73) C(74) 69.6(2) . . . yes Fe(1) C(73) C(76A) 136.9(5) . . . yes C(72) C(73) C(74) 106.6(4) . . . yes C(72) C(73) C(76A) 125.4(5) . . . yes C(74) C(73) C(76A) 126.3(5) . . . yes Fe(1) C(74) C(73) 71.0(2) . . . yes Fe(1) C(74) C(75) 69.7(2) . . . yes C(73) C(74) C(75) 107.6(3) . . . yes Fe(1) C(75) C(71) 71.5(2) . . . yes Fe(1) C(75) C(74) 71.0(2) . . . yes C(71) C(75) C(74) 109.8(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . 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(1) F(3) 3.53(2) . 1_565 ? S(1) F(4) 3.58(2) . 2_766 ? F(1) C(72) 3.24(2) . 1_545 ? F(1A) C(72) 3.52(2) . 1_545 ? F(2) C(54) 3.28(2) . 6_646 ? F(2) C(76) 3.48(2) . 1_545 ? F(2) C(53) 3.59(2) . 6_646 ? F(2A) C(76) 3.35(2) . 1_545 ? F(2A) C(72) 3.49(2) . 1_545 ? F(3) C(15) 3.27(2) . 1_545 ? F(3) C(11) 3.53(2) . 1_545 ? F(4) C(54) 3.20(2) . 5_545 ? F(4) C(53) 3.29(2) . 5_545 ? F(4) C(15) 3.43(2) . 2_746 ? C(44) C(63) 3.417(9) . 7_646 ? #===END data_1091_FeCp*(CO)2_open _database_code_depnum_ccdc_archive 'CCDC 818899' #TrackingRef 'DT-ART-04-2011-010727CIFrev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cl2 F6 Fe2 O4 S2' _chemical_formula_weight 945.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1297(12) _cell_length_b 13.572(3) _cell_length_c 18.309(4) _cell_angle_alpha 101.002(5) _cell_angle_beta 103.323(11) _cell_angle_gamma 98.326(12) _cell_volume 2124.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5599 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.907 _exptl_special_details ; Because of the small size of the crystal the completeness was low. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 17161 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8830 _reflns_number_gt 6061 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All fluorine atoms were refined with fixing the C-F distances (~1.35 A). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8830 _refine_ls_number_parameters 533 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1537 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12384(6) 0.52774(4) 0.68695(3) 0.03011(15) Uani 1 1 d . . . Fe2 Fe 0.45560(5) 0.90146(4) 1.31042(3) 0.02846(15) Uani 1 1 d . . . Cl1 Cl -0.00410(15) 0.07296(12) 0.22458(8) 0.0661(4) Uani 1 1 d . . . Cl2 Cl 0.0790(3) 0.1728(2) 0.38717(11) 0.1319(10) Uani 1 1 d . . . S1 S 0.29018(10) 0.72372(8) 0.82970(5) 0.0339(2) Uani 1 1 d . . . S2 S 0.37162(11) 0.70609(8) 1.16650(5) 0.0348(2) Uani 1 1 d . . . F1 F -0.1048(4) 0.8852(3) 1.0914(2) 0.119(2) Uani 1 1 d D . . F2 F -0.1800(4) 0.7289(4) 1.0923(2) 0.129(2) Uani 1 1 d D . . F3 F -0.2799(7) 0.8673(4) 0.9665(2) 0.163(3) Uani 1 1 d D . . F4 F -0.3872(4) 0.7272(5) 0.9773(2) 0.157(3) Uani 1 1 d D . . F5 F -0.2279(4) 0.7593(4) 0.84862(18) 0.0918(14) Uani 1 1 d D . . F6 F -0.2673(3) 0.6257(3) 0.8878(2) 0.0848(11) Uani 1 1 d D . . O131 O -0.1984(4) 0.5342(3) 0.6335(2) 0.0659(11) Uani 1 1 d . . . O132 O 0.2447(4) 0.6854(3) 0.6165(2) 0.0646(10) Uani 1 1 d . . . O231 O 0.1777(3) 0.9338(3) 1.35561(19) 0.0520(8) Uani 1 1 d . . . O232 O 0.4734(4) 0.7244(3) 1.3772(2) 0.0624(10) Uani 1 1 d . . . C1 C -0.0235(4) 0.7348(3) 0.9473(2) 0.0314(8) Uani 1 1 d . . . C2 C 0.0081(4) 0.7620(3) 1.0259(2) 0.0304(8) Uani 1 1 d . . . C3 C -0.1290(5) 0.7889(3) 1.0490(2) 0.0481(12) Uani 1 1 d D . . C4 C -0.2489(4) 0.7762(3) 0.9767(3) 0.0538(13) Uani 1 1 d D . . C5 C -0.1918(4) 0.7244(3) 0.91302(18) 0.0481(12) Uani 1 1 d D . . C111 C 0.2170(4) 0.7708(3) 0.9058(2) 0.0313(8) Uani 1 1 d . . . C112 C 0.0754(4) 0.7132(3) 0.8963(2) 0.0305(8) Uani 1 1 d . . . C113 C 0.0276(4) 0.6318(3) 0.8270(2) 0.0325(8) Uani 1 1 d . . . C114 C 0.1320(4) 0.6256(3) 0.7841(2) 0.0324(8) Uani 1 1 d . . . C115 C 0.3041(5) 0.8626(3) 0.9671(2) 0.0420(10) Uani 1 1 d . . . H2 H 0.3529 0.8415 1.0122 0.042 Uiso 1 1 calc R . . H3 H 0.2350 0.9060 0.9796 0.042 Uiso 1 1 calc R . . H4 H 0.3808 0.8996 0.9489 0.042 Uiso 1 1 calc R . . C120 C 0.2483(4) 0.4420(3) 0.7567(2) 0.0350(9) Uani 1 1 d . . . C121 C 0.0969(5) 0.3869(3) 0.7190(2) 0.0374(9) Uani 1 1 d . . . C122 C 0.0805(5) 0.3703(3) 0.6370(2) 0.0379(9) Uani 1 1 d . . . C123 C 0.2194(5) 0.4178(3) 0.6259(2) 0.0369(9) Uani 1 1 d . . . C124 C 0.3232(4) 0.4630(3) 0.6999(2) 0.0361(9) Uani 1 1 d . . . C125 C 0.3210(5) 0.4678(4) 0.8418(2) 0.0451(10) Uani 1 1 d . . . H5 H 0.3724 0.4142 0.8552 0.045 Uiso 1 1 calc R . . H6 H 0.2432 0.4744 0.8689 0.045 Uiso 1 1 calc R . . H7 H 0.3940 0.5312 0.8560 0.045 Uiso 1 1 calc R . . C126 C -0.0201(5) 0.3461(4) 0.7566(3) 0.0526(12) Uani 1 1 d . . . H8 H -0.0051 0.3899 0.8066 0.053 Uiso 1 1 calc R . . H9 H -0.0093 0.2783 0.7620 0.053 Uiso 1 1 calc R . . H10 H -0.1212 0.3437 0.7253 0.053 Uiso 1 1 calc R . . C127 C -0.0573(6) 0.3054(4) 0.5756(3) 0.0584(13) Uani 1 1 d . . . H11 H -0.1494 0.3207 0.5878 0.058 Uiso 1 1 calc R . . H12 H -0.0555 0.2343 0.5732 0.058 Uiso 1 1 calc R . . H13 H -0.0545 0.3198 0.5265 0.058 Uiso 1 1 calc R . . C128 C 0.2551(6) 0.4148(4) 0.5493(3) 0.0575(13) Uani 1 1 d . . . H14 H 0.2989 0.3560 0.5357 0.057 Uiso 1 1 calc R . . H15 H 0.3270 0.4758 0.5529 0.057 Uiso 1 1 calc R . . H16 H 0.1623 0.4108 0.5104 0.057 Uiso 1 1 calc R . . C129 C 0.4870(5) 0.5176(4) 0.7149(3) 0.0547(12) Uani 1 1 d . . . H17 H 0.5545 0.4704 0.7232 0.055 Uiso 1 1 calc R . . H18 H 0.5120 0.5729 0.7599 0.055 Uiso 1 1 calc R . . H19 H 0.4988 0.5442 0.6712 0.055 Uiso 1 1 calc R . . C131 C -0.0713(5) 0.5329(4) 0.6545(2) 0.0437(10) Uani 1 1 d . . . C132 C 0.1960(5) 0.6243(4) 0.6455(2) 0.0420(10) Uani 1 1 d . . . C211 C 0.2280(4) 0.6831(3) 1.0820(2) 0.0305(8) Uani 1 1 d . . . C212 C 0.1455(4) 0.7605(3) 1.0853(2) 0.0285(8) Uani 1 1 d . . . C213 C 0.2026(4) 0.8365(3) 1.1572(2) 0.0288(8) Uani 1 1 d . . . C214 C 0.3280(4) 0.8201(3) 1.2080(2) 0.0298(8) Uani 1 1 d . . . C215 C 0.2070(5) 0.5883(4) 1.0204(2) 0.0469(11) Uani 1 1 d . . . H21 H 0.1004 0.5666 0.9931 0.047 Uiso 1 1 calc R . . H22 H 0.2413 0.5351 1.0436 0.047 Uiso 1 1 calc R . . H23 H 0.2659 0.6024 0.9851 0.047 Uiso 1 1 calc R . . C220 C 0.5875(4) 1.0457(3) 1.3739(2) 0.0372(9) Uani 1 1 d . . . C221 C 0.6805(4) 0.9718(4) 1.3763(2) 0.0404(10) Uani 1 1 d . . . C222 C 0.6810(4) 0.9275(3) 1.2984(2) 0.0360(9) Uani 1 1 d . . . C223 C 0.5919(4) 0.9779(3) 1.2493(2) 0.0348(9) Uani 1 1 d . . . C224 C 0.5284(4) 1.0486(3) 1.2941(2) 0.0366(9) Uani 1 1 d . . . C225 C 0.5619(6) 1.1152(4) 1.4422(3) 0.0533(12) Uani 1 1 d . . . H24 H 0.6388 1.1769 1.4579 0.053 Uiso 1 1 calc R . . H25 H 0.5686 1.0814 1.4840 0.053 Uiso 1 1 calc R . . H26 H 0.4621 1.1318 1.4283 0.053 Uiso 1 1 calc R . . C226 C 0.7746(5) 0.9483(5) 1.4472(3) 0.0582(14) Uani 1 1 d . . . H27 H 0.7335 0.9699 1.4900 0.058 Uiso 1 1 calc R . . H28 H 0.8789 0.9841 1.4583 0.058 Uiso 1 1 calc R . . H29 H 0.7718 0.8760 1.4385 0.058 Uiso 1 1 calc R . . C227 C 0.7721(5) 0.8495(4) 1.2754(3) 0.0523(12) Uani 1 1 d . . . H30 H 0.7216 0.8098 1.2241 0.052 Uiso 1 1 calc R . . H31 H 0.7803 0.8051 1.3106 0.052 Uiso 1 1 calc R . . H32 H 0.8729 0.8834 1.2769 0.052 Uiso 1 1 calc R . . C228 C 0.5730(5) 0.9620(4) 1.1635(2) 0.0470(11) Uani 1 1 d . . . H33 H 0.4773 0.9784 1.1397 0.047 Uiso 1 1 calc R . . H34 H 0.5735 0.8918 1.1421 0.047 Uiso 1 1 calc R . . H35 H 0.6561 1.0056 1.1543 0.047 Uiso 1 1 calc R . . C229 C 0.4330(5) 1.1212(4) 1.2654(3) 0.0534(12) Uani 1 1 d . . . H36 H 0.3711 1.1393 1.2998 0.053 Uiso 1 1 calc R . . H37 H 0.3676 1.0890 1.2147 0.053 Uiso 1 1 calc R . . H38 H 0.4990 1.1818 1.2632 0.053 Uiso 1 1 calc R . . C231 C 0.2878(4) 0.9224(3) 1.3364(2) 0.0351(9) Uani 1 1 d . . . C232 C 0.4648(5) 0.7925(4) 1.3492(2) 0.0401(10) Uani 1 1 d . . . C300 C -0.003(2) 0.1729(9) 0.2952(6) 0.155(6) Uani 1 1 d . . . H1 H -0.070(5) 0.574(3) 0.816(2) 0.035(11) Uiso 1 1 d . . . H20 H 0.166(4) 0.894(3) 1.1669(19) 0.015(8) Uiso 1 1 d . . . H39 H 0.042(8) 0.221(5) 0.289(4) 0.052(19) Uiso 1 1 d . . . H40 H -0.068(9) 0.206(7) 0.287(4) 0.10(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0322(3) 0.0354(3) 0.0208(3) 0.0048(2) 0.00695(19) 0.0029(2) Fe2 0.0257(3) 0.0367(3) 0.0203(3) 0.0071(2) 0.00263(18) 0.0024(2) Cl1 0.0611(8) 0.0663(9) 0.0635(9) 0.0058(7) 0.0101(6) 0.0117(6) Cl2 0.198(3) 0.125(2) 0.0602(11) -0.0042(11) -0.0012(13) 0.0864(18) S1 0.0333(5) 0.0396(6) 0.0272(5) 0.0053(4) 0.0096(3) 0.0023(4) S2 0.0352(5) 0.0407(6) 0.0265(5) 0.0059(4) 0.0031(3) 0.0122(4) F1 0.060(2) 0.150(4) 0.096(3) -0.074(3) -0.0201(18) 0.060(2) F2 0.071(2) 0.279(7) 0.114(3) 0.136(4) 0.066(2) 0.090(3) F3 0.246(6) 0.154(5) 0.072(3) -0.016(3) -0.031(3) 0.160(5) F4 0.073(2) 0.287(8) 0.058(2) -0.028(3) 0.0241(19) -0.057(3) F5 0.065(2) 0.184(4) 0.060(2) 0.070(2) 0.0222(15) 0.066(2) F6 0.0456(17) 0.087(3) 0.089(3) -0.027(2) 0.0026(15) -0.0053(16) O131 0.040(2) 0.104(3) 0.053(2) 0.019(2) 0.0051(15) 0.0201(18) O132 0.089(3) 0.058(2) 0.053(2) 0.0279(19) 0.0274(19) 0.0008(19) O231 0.0417(17) 0.064(2) 0.051(2) 0.0066(17) 0.0192(14) 0.0098(15) O232 0.081(3) 0.053(2) 0.058(2) 0.0306(19) 0.0118(18) 0.0163(18) C1 0.0258(18) 0.040(2) 0.0243(18) 0.0049(16) 0.0027(13) 0.0053(15) C2 0.0283(18) 0.038(2) 0.0219(18) 0.0034(16) 0.0046(13) 0.0050(15) C3 0.048(3) 0.074(4) 0.024(2) 0.007(2) 0.0105(17) 0.023(2) C4 0.039(2) 0.080(4) 0.040(3) 0.002(2) 0.0086(18) 0.022(2) C5 0.031(2) 0.082(4) 0.025(2) 0.007(2) -0.0030(15) 0.015(2) C111 0.0358(19) 0.035(2) 0.0213(18) 0.0068(16) 0.0042(14) 0.0061(15) C112 0.0320(18) 0.036(2) 0.0196(17) 0.0033(15) 0.0019(13) 0.0074(15) C113 0.0337(19) 0.042(2) 0.0178(17) 0.0039(16) 0.0041(13) 0.0042(16) C114 0.0349(19) 0.036(2) 0.0247(19) 0.0082(16) 0.0039(14) 0.0068(15) C115 0.045(2) 0.041(3) 0.032(2) 0.0007(19) 0.0081(17) -0.0064(18) C120 0.041(2) 0.037(2) 0.0255(19) 0.0054(17) 0.0072(15) 0.0093(17) C121 0.045(2) 0.035(2) 0.033(2) 0.0087(18) 0.0111(16) 0.0053(17) C122 0.039(2) 0.038(2) 0.030(2) 0.0008(17) 0.0043(15) 0.0011(16) C123 0.044(2) 0.038(2) 0.029(2) 0.0024(17) 0.0142(16) 0.0071(17) C124 0.035(2) 0.038(2) 0.032(2) 0.0005(18) 0.0108(15) 0.0059(16) C125 0.054(3) 0.052(3) 0.027(2) 0.008(2) 0.0030(17) 0.018(2) C126 0.051(3) 0.065(3) 0.049(3) 0.027(3) 0.021(2) 0.006(2) C127 0.056(3) 0.050(3) 0.048(3) -0.002(2) -0.005(2) -0.006(2) C128 0.077(3) 0.064(4) 0.037(3) 0.008(2) 0.028(2) 0.018(3) C129 0.037(2) 0.058(3) 0.063(3) 0.006(3) 0.013(2) 0.003(2) C131 0.048(3) 0.055(3) 0.024(2) 0.0060(19) 0.0077(17) 0.006(2) C132 0.048(2) 0.048(3) 0.030(2) 0.007(2) 0.0113(17) 0.0102(19) C211 0.0349(19) 0.036(2) 0.0213(18) 0.0073(16) 0.0075(14) 0.0081(15) C212 0.0294(18) 0.035(2) 0.0210(17) 0.0073(15) 0.0072(13) 0.0042(14) C213 0.0284(18) 0.034(2) 0.0220(18) 0.0035(15) 0.0064(13) 0.0054(15) C214 0.0298(17) 0.037(2) 0.0212(17) 0.0086(16) 0.0059(13) 0.0017(15) C215 0.059(3) 0.044(3) 0.033(2) 0.005(2) 0.0036(19) 0.017(2) C220 0.034(2) 0.039(2) 0.030(2) 0.0033(18) 0.0047(15) -0.0083(16) C221 0.0250(19) 0.053(3) 0.034(2) 0.0086(19) -0.0027(14) -0.0028(16) C222 0.0228(18) 0.050(3) 0.035(2) 0.0139(19) 0.0058(14) 0.0047(16) C223 0.0247(17) 0.048(3) 0.029(2) 0.0135(18) 0.0052(13) -0.0050(15) C224 0.033(2) 0.039(2) 0.034(2) 0.0126(18) 0.0052(15) -0.0034(16) C225 0.063(3) 0.044(3) 0.041(3) -0.005(2) 0.015(2) -0.008(2) C226 0.041(2) 0.087(4) 0.038(3) 0.024(3) -0.0036(18) -0.001(2) C227 0.036(2) 0.065(3) 0.062(3) 0.020(3) 0.015(2) 0.015(2) C228 0.038(2) 0.070(3) 0.029(2) 0.016(2) 0.0068(16) -0.003(2) C229 0.047(3) 0.054(3) 0.064(3) 0.027(3) 0.012(2) 0.010(2) C231 0.037(2) 0.037(2) 0.0246(19) 0.0059(17) 0.0008(15) -0.0009(16) C232 0.041(2) 0.046(3) 0.028(2) 0.0065(19) 0.0042(16) 0.0049(18) C300 0.265(15) 0.071(7) 0.087(6) -0.013(5) -0.046(8) 0.091(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C132 1.758(5) . ? Fe1 C131 1.760(5) . ? Fe1 C114 1.986(4) . ? Fe1 C122 2.097(4) . ? Fe1 C121 2.101(4) . ? Fe1 C123 2.104(4) . ? Fe1 C124 2.118(4) . ? Fe1 C120 2.135(4) . ? Fe2 C231 1.750(4) . ? Fe2 C232 1.763(5) . ? Fe2 C214 1.980(4) . ? Fe2 C220 2.106(4) . ? Fe2 C221 2.106(4) . ? Fe2 C222 2.106(4) . ? Fe2 C224 2.111(4) . ? Fe2 C223 2.143(4) . ? Cl1 C300 1.682(10) . ? Cl2 C300 1.679(10) . ? S1 C111 1.734(4) . ? S1 C114 1.737(4) . ? S2 C211 1.724(4) . ? S2 C214 1.732(4) . ? F1 C3 1.345(2) . ? F2 C3 1.347(2) . ? F3 C4 1.345(2) . ? F4 C4 1.342(2) . ? F5 C5 1.3429(19) . ? F6 C5 1.353(2) . ? O131 C131 1.139(5) . ? O132 C132 1.155(5) . ? O231 C231 1.161(5) . ? O232 C232 1.143(5) . ? C1 C2 1.365(5) . ? C1 C112 1.461(5) . ? C1 C5 1.495(5) . ? C2 C212 1.465(5) . ? C2 C3 1.482(5) . ? C3 C4 1.473(6) . ? C4 C5 1.484(6) . ? C111 C112 1.365(5) . ? C111 C115 1.487(5) . ? C112 C113 1.446(5) . ? C113 C114 1.369(5) . ? C120 C121 1.418(6) . ? C120 C124 1.420(5) . ? C120 C125 1.496(5) . ? C121 C122 1.444(6) . ? C121 C126 1.495(6) . ? C122 C123 1.413(6) . ? C122 C127 1.508(6) . ? C123 C124 1.426(5) . ? C123 C128 1.506(6) . ? C124 C129 1.508(6) . ? C211 C212 1.378(5) . ? C211 C215 1.496(6) . ? C212 C213 1.442(5) . ? C213 C214 1.374(5) . ? C220 C221 1.405(6) . ? C220 C224 1.447(5) . ? C220 C225 1.502(6) . ? C221 C222 1.439(6) . ? C221 C226 1.499(5) . ? C222 C223 1.414(5) . ? C222 C227 1.496(6) . ? C223 C224 1.417(6) . ? C223 C228 1.508(5) . ? C224 C229 1.497(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C132 Fe1 C131 96.7(2) . . ? C132 Fe1 C114 93.48(19) . . ? C131 Fe1 C114 88.15(18) . . ? C132 Fe1 C122 124.69(19) . . ? C131 Fe1 C122 91.7(2) . . ? C114 Fe1 C122 141.52(17) . . ? C132 Fe1 C121 158.64(18) . . ? C131 Fe1 C121 98.6(2) . . ? C114 Fe1 C121 101.81(16) . . ? C122 Fe1 C121 40.24(16) . . ? C132 Fe1 C123 92.62(18) . . ? C131 Fe1 C123 120.54(19) . . ? C114 Fe1 C123 149.68(15) . . ? C122 Fe1 C123 39.29(16) . . ? C121 Fe1 C123 66.74(16) . . ? C132 Fe1 C124 94.59(18) . . ? C131 Fe1 C124 157.6(2) . . ? C114 Fe1 C124 110.36(15) . . ? C122 Fe1 C124 66.07(16) . . ? C121 Fe1 C124 66.22(16) . . ? C123 Fe1 C124 39.49(15) . . ? C132 Fe1 C120 128.46(18) . . ? C131 Fe1 C120 134.76(19) . . ? C114 Fe1 C120 87.45(15) . . ? C122 Fe1 C120 65.94(15) . . ? C121 Fe1 C120 39.11(15) . . ? C123 Fe1 C120 65.78(15) . . ? C124 Fe1 C120 39.00(15) . . ? C231 Fe2 C232 93.83(19) . . ? C231 Fe2 C214 89.16(17) . . ? C232 Fe2 C214 93.04(18) . . ? C231 Fe2 C220 94.90(18) . . ? C232 Fe2 C220 120.61(18) . . ? C214 Fe2 C220 145.63(16) . . ? C231 Fe2 C221 125.22(18) . . ? C232 Fe2 C221 91.59(18) . . ? C214 Fe2 C221 144.88(16) . . ? C220 Fe2 C221 38.96(17) . . ? C231 Fe2 C222 161.03(19) . . ? C232 Fe2 C222 97.91(18) . . ? C214 Fe2 C222 104.96(16) . . ? C220 Fe2 C222 66.28(17) . . ? C221 Fe2 C222 39.95(16) . . ? C231 Fe2 C224 98.12(18) . . ? C232 Fe2 C224 158.00(17) . . ? C214 Fe2 C224 105.50(15) . . ? C220 Fe2 C224 40.14(15) . . ? C221 Fe2 C224 66.43(16) . . ? C222 Fe2 C224 66.25(16) . . ? C231 Fe2 C223 132.42(18) . . ? C232 Fe2 C223 133.70(18) . . ? C214 Fe2 C223 86.62(15) . . ? C220 Fe2 C223 65.65(16) . . ? C221 Fe2 C223 65.59(15) . . ? C222 Fe2 C223 38.86(15) . . ? C224 Fe2 C223 38.92(16) . . ? C111 S1 C114 94.79(19) . . ? C211 S2 C214 95.22(18) . . ? C2 C1 C112 131.4(3) . . ? C2 C1 C5 109.4(3) . . ? C112 C1 C5 119.2(3) . . ? C1 C2 C212 130.3(3) . . ? C1 C2 C3 110.0(3) . . ? C212 C2 C3 119.5(3) . . ? F1 C3 F2 105.1(4) . . ? F1 C3 C4 109.5(3) . . ? F2 C3 C4 109.5(3) . . ? F1 C3 C2 113.6(3) . . ? F2 C3 C2 113.1(3) . . ? C4 C3 C2 106.1(3) . . ? F4 C4 F3 101.1(5) . . ? F4 C4 C3 113.8(4) . . ? F3 C4 C3 110.9(4) . . ? F4 C4 C5 112.7(4) . . ? F3 C4 C5 111.3(4) . . ? C3 C4 C5 107.2(3) . . ? F5 C5 F6 101.5(4) . . ? F5 C5 C4 113.7(4) . . ? F6 C5 C4 109.3(3) . . ? F5 C5 C1 114.7(3) . . ? F6 C5 C1 113.0(3) . . ? C4 C5 C1 104.8(3) . . ? C112 C111 C115 129.7(4) . . ? C112 C111 S1 109.4(3) . . ? C115 C111 S1 120.9(3) . . ? C111 C112 C113 112.9(3) . . ? C111 C112 C1 124.2(4) . . ? C113 C112 C1 122.7(3) . . ? C114 C113 C112 114.9(4) . . ? C113 C114 S1 108.0(3) . . ? C113 C114 Fe1 130.6(3) . . ? S1 C114 Fe1 121.4(2) . . ? C121 C120 C124 108.6(3) . . ? C121 C120 C125 125.8(4) . . ? C124 C120 C125 125.4(4) . . ? C121 C120 Fe1 69.2(2) . . ? C124 C120 Fe1 69.8(2) . . ? C125 C120 Fe1 129.9(3) . . ? C120 C121 C122 107.2(3) . . ? C120 C121 C126 126.6(4) . . ? C122 C121 C126 126.1(4) . . ? C120 C121 Fe1 71.7(2) . . ? C122 C121 Fe1 69.7(2) . . ? C126 C121 Fe1 127.4(3) . . ? C123 C122 C121 108.1(3) . . ? C123 C122 C127 127.0(4) . . ? C121 C122 C127 124.7(4) . . ? C123 C122 Fe1 70.6(2) . . ? C121 C122 Fe1 70.0(2) . . ? C127 C122 Fe1 129.0(3) . . ? C122 C123 C124 108.1(3) . . ? C122 C123 C128 125.9(4) . . ? C124 C123 C128 125.9(4) . . ? C122 C123 Fe1 70.1(2) . . ? C124 C123 Fe1 70.8(2) . . ? C128 C123 Fe1 127.9(3) . . ? C120 C124 C123 108.0(3) . . ? C120 C124 C129 126.1(4) . . ? C123 C124 C129 125.8(4) . . ? C120 C124 Fe1 71.2(2) . . ? C123 C124 Fe1 69.8(2) . . ? C129 C124 Fe1 127.6(3) . . ? O131 C131 Fe1 178.7(5) . . ? O132 C132 Fe1 177.7(4) . . ? C212 C211 C215 130.5(3) . . ? C212 C211 S2 109.5(3) . . ? C215 C211 S2 119.9(3) . . ? C211 C212 C213 112.2(3) . . ? C211 C212 C2 124.4(3) . . ? C213 C212 C2 123.3(3) . . ? C214 C213 C212 115.4(4) . . ? C213 C214 S2 107.6(3) . . ? C213 C214 Fe2 132.1(3) . . ? S2 C214 Fe2 120.23(19) . . ? C221 C220 C224 108.2(4) . . ? C221 C220 C225 126.4(4) . . ? C224 C220 C225 125.4(4) . . ? C221 C220 Fe2 70.5(2) . . ? C224 C220 Fe2 70.1(2) . . ? C225 C220 Fe2 128.3(3) . . ? C220 C221 C222 108.2(3) . . ? C220 C221 C226 126.7(4) . . ? C222 C221 C226 125.0(4) . . ? C220 C221 Fe2 70.5(2) . . ? C222 C221 Fe2 70.0(2) . . ? C226 C221 Fe2 129.0(3) . . ? C223 C222 C221 107.6(4) . . ? C223 C222 C227 126.7(4) . . ? C221 C222 C227 125.5(4) . . ? C223 C222 Fe2 72.0(2) . . ? C221 C222 Fe2 70.0(2) . . ? C227 C222 Fe2 127.7(3) . . ? C222 C223 C224 108.9(3) . . ? C222 C223 C228 125.4(4) . . ? C224 C223 C228 125.6(4) . . ? C222 C223 Fe2 69.2(2) . . ? C224 C223 Fe2 69.3(2) . . ? C228 C223 Fe2 129.4(3) . . ? C223 C224 C220 107.1(4) . . ? C223 C224 C229 126.4(4) . . ? C220 C224 C229 126.2(4) . . ? C223 C224 Fe2 71.8(2) . . ? C220 C224 Fe2 69.8(2) . . ? C229 C224 Fe2 128.8(3) . . ? O231 C231 Fe2 177.3(4) . . ? O232 C232 Fe2 177.3(4) . . ? Cl2 C300 Cl1 119.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C112 C1 C2 C212 -12.7(8) . . . . ? C5 C1 C2 C212 165.4(4) . . . . ? C112 C1 C2 C3 172.2(4) . . . . ? C5 C1 C2 C3 -9.7(5) . . . . ? C1 C2 C3 F1 -120.6(4) . . . . ? C212 C2 C3 F1 63.7(5) . . . . ? C1 C2 C3 F2 119.7(4) . . . . ? C212 C2 C3 F2 -56.0(5) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C212 C2 C3 C4 -176.0(3) . . . . ? F1 C3 C4 F4 -101.7(5) . . . . ? F2 C3 C4 F4 13.0(6) . . . . ? C2 C3 C4 F4 135.4(4) . . . . ? F1 C3 C4 F3 11.5(5) . . . . ? F2 C3 C4 F3 126.2(4) . . . . ? C2 C3 C4 F3 -111.5(4) . . . . ? F1 C3 C4 C5 133.1(4) . . . . ? F2 C3 C4 C5 -112.2(4) . . . . ? C2 C3 C4 C5 10.2(4) . . . . ? F4 C4 C5 F5 92.6(5) . . . . ? F3 C4 C5 F5 -20.2(5) . . . . ? C3 C4 C5 F5 -141.5(3) . . . . ? F4 C4 C5 F6 -20.0(5) . . . . ? F3 C4 C5 F6 -132.8(4) . . . . ? C3 C4 C5 F6 105.9(3) . . . . ? F4 C4 C5 C1 -141.4(4) . . . . ? F3 C4 C5 C1 105.9(4) . . . . ? C3 C4 C5 C1 -15.5(4) . . . . ? C2 C1 C5 F5 141.2(4) . . . . ? C112 C1 C5 F5 -40.5(5) . . . . ? C2 C1 C5 F6 -103.2(4) . . . . ? C112 C1 C5 F6 75.2(4) . . . . ? C2 C1 C5 C4 15.7(4) . . . . ? C112 C1 C5 C4 -165.9(3) . . . . ? C114 S1 C111 C112 -0.2(3) . . . . ? C114 S1 C111 C115 -178.4(3) . . . . ? C115 C111 C112 C113 177.6(4) . . . . ? S1 C111 C112 C113 -0.4(4) . . . . ? C115 C111 C112 C1 1.6(6) . . . . ? S1 C111 C112 C1 -176.4(3) . . . . ? C2 C1 C112 C111 -43.8(7) . . . . ? C5 C1 C112 C111 138.2(4) . . . . ? C2 C1 C112 C113 140.5(5) . . . . ? C5 C1 C112 C113 -37.4(6) . . . . ? C111 C112 C113 C114 0.9(5) . . . . ? C1 C112 C113 C114 177.0(3) . . . . ? C112 C113 C114 S1 -1.0(4) . . . . ? C112 C113 C114 Fe1 178.7(3) . . . . ? C111 S1 C114 C113 0.7(3) . . . . ? C111 S1 C114 Fe1 -179.0(2) . . . . ? C132 Fe1 C114 C113 136.2(4) . . . . ? C131 Fe1 C114 C113 39.6(4) . . . . ? C122 Fe1 C114 C113 -50.8(5) . . . . ? C121 Fe1 C114 C113 -58.8(4) . . . . ? C123 Fe1 C114 C113 -122.6(4) . . . . ? C124 Fe1 C114 C113 -127.6(4) . . . . ? C120 Fe1 C114 C113 -95.4(4) . . . . ? C132 Fe1 C114 S1 -44.1(3) . . . . ? C131 Fe1 C114 S1 -140.7(3) . . . . ? C122 Fe1 C114 S1 128.9(3) . . . . ? C121 Fe1 C114 S1 120.9(2) . . . . ? C123 Fe1 C114 S1 57.1(4) . . . . ? C124 Fe1 C114 S1 52.1(3) . . . . ? C120 Fe1 C114 S1 84.3(2) . . . . ? C132 Fe1 C120 C121 -155.3(3) . . . . ? C131 Fe1 C120 C121 27.5(4) . . . . ? C114 Fe1 C120 C121 112.3(2) . . . . ? C122 Fe1 C120 C121 -39.1(2) . . . . ? C123 Fe1 C120 C121 -82.3(3) . . . . ? C124 Fe1 C120 C121 -120.2(3) . . . . ? C132 Fe1 C120 C124 -35.1(3) . . . . ? C131 Fe1 C120 C124 147.7(3) . . . . ? C114 Fe1 C120 C124 -127.5(3) . . . . ? C122 Fe1 C120 C124 81.1(3) . . . . ? C121 Fe1 C120 C124 120.2(3) . . . . ? C123 Fe1 C120 C124 37.9(2) . . . . ? C132 Fe1 C120 C125 84.8(4) . . . . ? C131 Fe1 C120 C125 -92.4(5) . . . . ? C114 Fe1 C120 C125 -7.6(4) . . . . ? C122 Fe1 C120 C125 -159.0(5) . . . . ? C121 Fe1 C120 C125 -119.9(5) . . . . ? C123 Fe1 C120 C125 157.8(5) . . . . ? C124 Fe1 C120 C125 119.9(5) . . . . ? C124 C120 C121 C122 2.2(5) . . . . ? C125 C120 C121 C122 -174.0(4) . . . . ? Fe1 C120 C121 C122 61.1(3) . . . . ? C124 C120 C121 C126 177.7(4) . . . . ? C125 C120 C121 C126 1.4(7) . . . . ? Fe1 C120 C121 C126 -123.5(5) . . . . ? C124 C120 C121 Fe1 -58.9(3) . . . . ? C125 C120 C121 Fe1 124.9(4) . . . . ? C132 Fe1 C121 C120 64.0(6) . . . . ? C131 Fe1 C121 C120 -160.7(2) . . . . ? C114 Fe1 C121 C120 -70.8(2) . . . . ? C122 Fe1 C121 C120 116.9(3) . . . . ? C123 Fe1 C121 C120 79.7(2) . . . . ? C124 Fe1 C121 C120 36.5(2) . . . . ? C132 Fe1 C121 C122 -52.9(6) . . . . ? C131 Fe1 C121 C122 82.4(3) . . . . ? C114 Fe1 C121 C122 172.3(2) . . . . ? C123 Fe1 C121 C122 -37.2(2) . . . . ? C124 Fe1 C121 C122 -80.5(2) . . . . ? C120 Fe1 C121 C122 -116.9(3) . . . . ? C132 Fe1 C121 C126 -173.4(5) . . . . ? C131 Fe1 C121 C126 -38.1(4) . . . . ? C114 Fe1 C121 C126 51.8(4) . . . . ? C122 Fe1 C121 C126 -120.5(5) . . . . ? C123 Fe1 C121 C126 -157.8(4) . . . . ? C124 Fe1 C121 C126 159.0(4) . . . . ? C120 Fe1 C121 C126 122.5(5) . . . . ? C120 C121 C122 C123 -1.7(5) . . . . ? C126 C121 C122 C123 -177.2(4) . . . . ? Fe1 C121 C122 C123 60.6(3) . . . . ? C120 C121 C122 C127 173.4(4) . . . . ? C126 C121 C122 C127 -2.1(7) . . . . ? Fe1 C121 C122 C127 -124.2(5) . . . . ? C120 C121 C122 Fe1 -62.4(3) . . . . ? C126 C121 C122 Fe1 122.2(5) . . . . ? C132 Fe1 C122 C123 40.7(3) . . . . ? C131 Fe1 C122 C123 140.1(3) . . . . ? C114 Fe1 C122 C123 -130.8(3) . . . . ? C121 Fe1 C122 C123 -118.6(3) . . . . ? C124 Fe1 C122 C123 -37.7(2) . . . . ? C120 Fe1 C122 C123 -80.6(2) . . . . ? C132 Fe1 C122 C121 159.3(3) . . . . ? C131 Fe1 C122 C121 -101.3(2) . . . . ? C114 Fe1 C122 C121 -12.2(4) . . . . ? C123 Fe1 C122 C121 118.6(3) . . . . ? C124 Fe1 C122 C121 80.9(2) . . . . ? C120 Fe1 C122 C121 38.0(2) . . . . ? C132 Fe1 C122 C127 -81.6(5) . . . . ? C131 Fe1 C122 C127 17.7(4) . . . . ? C114 Fe1 C122 C127 106.9(4) . . . . ? C121 Fe1 C122 C127 119.0(5) . . . . ? C123 Fe1 C122 C127 -122.4(5) . . . . ? C124 Fe1 C122 C127 -160.1(5) . . . . ? C120 Fe1 C122 C127 157.1(5) . . . . ? C121 C122 C123 C124 0.6(5) . . . . ? C127 C122 C123 C124 -174.4(5) . . . . ? Fe1 C122 C123 C124 60.9(3) . . . . ? C121 C122 C123 C128 176.8(4) . . . . ? C127 C122 C123 C128 1.8(8) . . . . ? Fe1 C122 C123 C128 -123.0(5) . . . . ? C121 C122 C123 Fe1 -60.2(3) . . . . ? C127 C122 C123 Fe1 124.8(5) . . . . ? C132 Fe1 C123 C122 -147.5(3) . . . . ? C131 Fe1 C123 C122 -48.1(3) . . . . ? C114 Fe1 C123 C122 111.0(4) . . . . ? C121 Fe1 C123 C122 38.1(2) . . . . ? C124 Fe1 C123 C122 118.4(3) . . . . ? C120 Fe1 C123 C122 81.0(3) . . . . ? C132 Fe1 C123 C124 94.0(3) . . . . ? C131 Fe1 C123 C124 -166.5(3) . . . . ? C114 Fe1 C123 C124 -7.4(4) . . . . ? C122 Fe1 C123 C124 -118.4(3) . . . . ? C121 Fe1 C123 C124 -80.3(3) . . . . ? C120 Fe1 C123 C124 -37.4(2) . . . . ? C132 Fe1 C123 C128 -27.0(4) . . . . ? C131 Fe1 C123 C128 72.4(5) . . . . ? C114 Fe1 C123 C128 -128.5(4) . . . . ? C122 Fe1 C123 C128 120.5(5) . . . . ? C121 Fe1 C123 C128 158.6(4) . . . . ? C124 Fe1 C123 C128 -121.1(5) . . . . ? C120 Fe1 C123 C128 -158.5(5) . . . . ? C121 C120 C124 C123 -1.9(5) . . . . ? C125 C120 C124 C123 174.4(4) . . . . ? Fe1 C120 C124 C123 -60.3(3) . . . . ? C121 C120 C124 C129 -178.3(4) . . . . ? C125 C120 C124 C129 -2.0(7) . . . . ? Fe1 C120 C124 C129 123.3(5) . . . . ? C121 C120 C124 Fe1 58.4(3) . . . . ? C125 C120 C124 Fe1 -125.3(4) . . . . ? C122 C123 C124 C120 0.8(5) . . . . ? C128 C123 C124 C120 -175.4(4) . . . . ? Fe1 C123 C124 C120 61.2(3) . . . . ? C122 C123 C124 C129 177.2(4) . . . . ? C128 C123 C124 C129 1.0(7) . . . . ? Fe1 C123 C124 C129 -122.4(5) . . . . ? C122 C123 C124 Fe1 -60.4(3) . . . . ? C128 C123 C124 Fe1 123.4(5) . . . . ? C132 Fe1 C124 C120 153.2(3) . . . . ? C131 Fe1 C124 C120 -86.5(5) . . . . ? C114 Fe1 C124 C120 57.7(3) . . . . ? C122 Fe1 C124 C120 -80.7(3) . . . . ? C121 Fe1 C124 C120 -36.6(2) . . . . ? C123 Fe1 C124 C120 -118.3(3) . . . . ? C132 Fe1 C124 C123 -88.5(3) . . . . ? C131 Fe1 C124 C123 31.8(6) . . . . ? C114 Fe1 C124 C123 176.0(2) . . . . ? C122 Fe1 C124 C123 37.5(2) . . . . ? C121 Fe1 C124 C123 81.7(3) . . . . ? C120 Fe1 C124 C123 118.3(3) . . . . ? C132 Fe1 C124 C129 31.7(4) . . . . ? C131 Fe1 C124 C129 152.0(5) . . . . ? C114 Fe1 C124 C129 -63.7(4) . . . . ? C122 Fe1 C124 C129 157.8(4) . . . . ? C121 Fe1 C124 C129 -158.1(4) . . . . ? C123 Fe1 C124 C129 120.2(5) . . . . ? C120 Fe1 C124 C129 -121.5(5) . . . . ? C132 Fe1 C131 O131 152(18) . . . . ? C114 Fe1 C131 O131 -115(18) . . . . ? C122 Fe1 C131 O131 27(18) . . . . ? C121 Fe1 C131 O131 -13(18) . . . . ? C123 Fe1 C131 O131 55(18) . . . . ? C124 Fe1 C131 O131 32(18) . . . . ? C120 Fe1 C131 O131 -30(18) . . . . ? C131 Fe1 C132 O132 -110(10) . . . . ? C114 Fe1 C132 O132 161(10) . . . . ? C122 Fe1 C132 O132 -13(11) . . . . ? C121 Fe1 C132 O132 26(11) . . . . ? C123 Fe1 C132 O132 11(10) . . . . ? C124 Fe1 C132 O132 51(10) . . . . ? C120 Fe1 C132 O132 72(11) . . . . ? C214 S2 C211 C212 -0.8(3) . . . . ? C214 S2 C211 C215 -179.2(3) . . . . ? C215 C211 C212 C213 178.1(4) . . . . ? S2 C211 C212 C213 0.0(4) . . . . ? C215 C211 C212 C2 2.7(7) . . . . ? S2 C211 C212 C2 -175.4(3) . . . . ? C1 C2 C212 C211 -40.9(7) . . . . ? C3 C2 C212 C211 133.8(4) . . . . ? C1 C2 C212 C213 144.3(4) . . . . ? C3 C2 C212 C213 -41.0(5) . . . . ? C211 C212 C213 C214 1.2(5) . . . . ? C2 C212 C213 C214 176.6(3) . . . . ? C212 C213 C214 S2 -1.7(4) . . . . ? C212 C213 C214 Fe2 176.8(3) . . . . ? C211 S2 C214 C213 1.5(3) . . . . ? C211 S2 C214 Fe2 -177.3(2) . . . . ? C231 Fe2 C214 C213 44.3(4) . . . . ? C232 Fe2 C214 C213 138.1(4) . . . . ? C220 Fe2 C214 C213 -53.1(5) . . . . ? C221 Fe2 C214 C213 -124.8(4) . . . . ? C222 Fe2 C214 C213 -122.8(4) . . . . ? C224 Fe2 C214 C213 -53.9(4) . . . . ? C223 Fe2 C214 C213 -88.2(4) . . . . ? C231 Fe2 C214 S2 -137.2(2) . . . . ? C232 Fe2 C214 S2 -43.4(2) . . . . ? C220 Fe2 C214 S2 125.3(3) . . . . ? C221 Fe2 C214 S2 53.7(4) . . . . ? C222 Fe2 C214 S2 55.6(3) . . . . ? C224 Fe2 C214 S2 124.6(2) . . . . ? C223 Fe2 C214 S2 90.2(2) . . . . ? C231 Fe2 C220 C221 144.5(3) . . . . ? C232 Fe2 C220 C221 47.1(3) . . . . ? C214 Fe2 C220 C221 -119.8(3) . . . . ? C222 Fe2 C220 C221 -38.0(2) . . . . ? C224 Fe2 C220 C221 -118.7(3) . . . . ? C223 Fe2 C220 C221 -80.7(3) . . . . ? C231 Fe2 C220 C224 -96.8(3) . . . . ? C232 Fe2 C220 C224 165.8(3) . . . . ? C214 Fe2 C220 C224 -1.1(4) . . . . ? C221 Fe2 C220 C224 118.7(3) . . . . ? C222 Fe2 C220 C224 80.7(3) . . . . ? C223 Fe2 C220 C224 38.0(2) . . . . ? C231 Fe2 C220 C225 23.1(4) . . . . ? C232 Fe2 C220 C225 -74.3(5) . . . . ? C214 Fe2 C220 C225 118.8(4) . . . . ? C221 Fe2 C220 C225 -121.4(5) . . . . ? C222 Fe2 C220 C225 -159.4(4) . . . . ? C224 Fe2 C220 C225 119.9(5) . . . . ? C223 Fe2 C220 C225 157.9(5) . . . . ? C224 C220 C221 C222 0.0(4) . . . . ? C225 C220 C221 C222 -176.1(4) . . . . ? Fe2 C220 C221 C222 60.2(3) . . . . ? C224 C220 C221 C226 175.1(4) . . . . ? C225 C220 C221 C226 -0.9(7) . . . . ? Fe2 C220 C221 C226 -124.7(4) . . . . ? C224 C220 C221 Fe2 -60.2(3) . . . . ? C225 C220 C221 Fe2 123.7(4) . . . . ? C231 Fe2 C221 C220 -45.0(3) . . . . ? C232 Fe2 C221 C220 -140.9(3) . . . . ? C214 Fe2 C221 C220 121.6(3) . . . . ? C222 Fe2 C221 C220 118.7(4) . . . . ? C224 Fe2 C221 C220 38.1(2) . . . . ? C223 Fe2 C221 C220 80.9(3) . . . . ? C231 Fe2 C221 C222 -163.7(3) . . . . ? C232 Fe2 C221 C222 100.4(3) . . . . ? C214 Fe2 C221 C222 2.9(4) . . . . ? C220 Fe2 C221 C222 -118.7(4) . . . . ? C224 Fe2 C221 C222 -80.6(3) . . . . ? C223 Fe2 C221 C222 -37.8(2) . . . . ? C231 Fe2 C221 C226 76.9(5) . . . . ? C232 Fe2 C221 C226 -18.9(5) . . . . ? C214 Fe2 C221 C226 -116.5(5) . . . . ? C220 Fe2 C221 C226 122.0(6) . . . . ? C222 Fe2 C221 C226 -119.4(6) . . . . ? C224 Fe2 C221 C226 160.1(5) . . . . ? C223 Fe2 C221 C226 -157.2(5) . . . . ? C220 C221 C222 C223 2.1(4) . . . . ? C226 C221 C222 C223 -173.2(4) . . . . ? Fe2 C221 C222 C223 62.6(3) . . . . ? C220 C221 C222 C227 176.8(4) . . . . ? C226 C221 C222 C227 1.5(7) . . . . ? Fe2 C221 C222 C227 -122.7(4) . . . . ? C220 C221 C222 Fe2 -60.5(3) . . . . ? C226 C221 C222 Fe2 124.2(4) . . . . ? C231 Fe2 C222 C223 -72.4(6) . . . . ? C232 Fe2 C222 C223 159.9(3) . . . . ? C214 Fe2 C222 C223 64.6(3) . . . . ? C220 Fe2 C222 C223 -80.1(3) . . . . ? C221 Fe2 C222 C223 -117.1(4) . . . . ? C224 Fe2 C222 C223 -36.0(2) . . . . ? C231 Fe2 C222 C221 44.8(6) . . . . ? C232 Fe2 C222 C221 -83.0(3) . . . . ? C214 Fe2 C222 C221 -178.3(3) . . . . ? C220 Fe2 C222 C221 37.1(3) . . . . ? C224 Fe2 C222 C221 81.1(3) . . . . ? C223 Fe2 C222 C221 117.1(4) . . . . ? C231 Fe2 C222 C227 164.8(5) . . . . ? C232 Fe2 C222 C227 37.1(4) . . . . ? C214 Fe2 C222 C227 -58.2(4) . . . . ? C220 Fe2 C222 C227 157.1(4) . . . . ? C221 Fe2 C222 C227 120.1(5) . . . . ? C224 Fe2 C222 C227 -158.9(4) . . . . ? C223 Fe2 C222 C227 -122.8(5) . . . . ? C221 C222 C223 C224 -3.4(4) . . . . ? C227 C222 C223 C224 -178.0(4) . . . . ? Fe2 C222 C223 C224 58.0(3) . . . . ? C221 C222 C223 C228 174.4(4) . . . . ? C227 C222 C223 C228 -0.2(6) . . . . ? Fe2 C222 C223 C228 -124.3(4) . . . . ? C221 C222 C223 Fe2 -61.3(3) . . . . ? C227 C222 C223 Fe2 124.1(4) . . . . ? C231 Fe2 C223 C222 155.2(3) . . . . ? C232 Fe2 C223 C222 -28.1(4) . . . . ? C214 Fe2 C223 C222 -119.0(3) . . . . ? C220 Fe2 C223 C222 81.8(3) . . . . ? C221 Fe2 C223 C222 38.9(3) . . . . ? C224 Fe2 C223 C222 121.0(3) . . . . ? C231 Fe2 C223 C224 34.2(3) . . . . ? C232 Fe2 C223 C224 -149.1(3) . . . . ? C214 Fe2 C223 C224 119.9(2) . . . . ? C220 Fe2 C223 C224 -39.2(2) . . . . ? C221 Fe2 C223 C224 -82.1(3) . . . . ? C222 Fe2 C223 C224 -121.0(3) . . . . ? C231 Fe2 C223 C228 -85.5(5) . . . . ? C232 Fe2 C223 C228 91.2(4) . . . . ? C214 Fe2 C223 C228 0.2(4) . . . . ? C220 Fe2 C223 C228 -158.9(5) . . . . ? C221 Fe2 C223 C228 158.1(5) . . . . ? C222 Fe2 C223 C228 119.3(5) . . . . ? C224 Fe2 C223 C228 -119.7(5) . . . . ? C222 C223 C224 C220 3.3(4) . . . . ? C228 C223 C224 C220 -174.4(4) . . . . ? Fe2 C223 C224 C220 61.2(3) . . . . ? C222 C223 C224 C229 176.9(4) . . . . ? C228 C223 C224 C229 -0.8(7) . . . . ? Fe2 C223 C224 C229 -125.2(4) . . . . ? C222 C223 C224 Fe2 -57.9(3) . . . . ? C228 C223 C224 Fe2 124.4(4) . . . . ? C221 C220 C224 C223 -2.0(4) . . . . ? C225 C220 C224 C223 174.1(4) . . . . ? Fe2 C220 C224 C223 -62.5(3) . . . . ? C221 C220 C224 C229 -175.6(4) . . . . ? C225 C220 C224 C229 0.5(7) . . . . ? Fe2 C220 C224 C229 123.9(4) . . . . ? C221 C220 C224 Fe2 60.5(3) . . . . ? C225 C220 C224 Fe2 -123.4(4) . . . . ? C231 Fe2 C224 C223 -155.2(2) . . . . ? C232 Fe2 C224 C223 82.5(5) . . . . ? C214 Fe2 C224 C223 -63.8(2) . . . . ? C220 Fe2 C224 C223 116.8(3) . . . . ? C221 Fe2 C224 C223 79.8(2) . . . . ? C222 Fe2 C224 C223 36.0(2) . . . . ? C231 Fe2 C224 C220 88.0(3) . . . . ? C232 Fe2 C224 C220 -34.2(6) . . . . ? C214 Fe2 C224 C220 179.4(2) . . . . ? C221 Fe2 C224 C220 -37.0(2) . . . . ? C222 Fe2 C224 C220 -80.8(3) . . . . ? C223 Fe2 C224 C220 -116.8(3) . . . . ? C231 Fe2 C224 C229 -32.8(4) . . . . ? C232 Fe2 C224 C229 -155.0(5) . . . . ? C214 Fe2 C224 C229 58.6(4) . . . . ? C220 Fe2 C224 C229 -120.8(5) . . . . ? C221 Fe2 C224 C229 -157.8(5) . . . . ? C222 Fe2 C224 C229 158.4(4) . . . . ? C223 Fe2 C224 C229 122.5(5) . . . . ? C232 Fe2 C231 O231 18(8) . . . . ? C214 Fe2 C231 O231 111(8) . . . . ? C220 Fe2 C231 O231 -103(8) . . . . ? C221 Fe2 C231 O231 -76(8) . . . . ? C222 Fe2 C231 O231 -110(8) . . . . ? C224 Fe2 C231 O231 -143(8) . . . . ? C223 Fe2 C231 O231 -164(8) . . . . ? C231 Fe2 C232 O232 -81(9) . . . . ? C214 Fe2 C232 O232 -171(9) . . . . ? C220 Fe2 C232 O232 17(9) . . . . ? C221 Fe2 C232 O232 44(9) . . . . ? C222 Fe2 C232 O232 84(9) . . . . ? C224 Fe2 C232 O232 42(9) . . . . ? C223 Fe2 C232 O232 101(9) . . . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.377 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.082 #===END data_1051_RuCp(dppe)_open _database_code_depnum_ccdc_archive 'CCDC 820900' #TrackingRef 'DT-ART-04-2011-010727CIFrev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 Cl2 F6 O2 P2 Ru2 S2' _chemical_formula_weight 1237.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.8045(19) _cell_length_b 14.196(3) _cell_length_c 16.925(2) _cell_angle_alpha 97.361(7) _cell_angle_beta 105.434(8) _cell_angle_gamma 93.453(5) _cell_volume 2698.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5475 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.1 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; Because of the small size of the crystal the data completeness was low. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 21298 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.1593 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11168 _reflns_number_gt 5492 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A part of the cyclopentene ring was disordered and refined taking into account two components (C4-F3-6 : C4A-F3A-6A= 0.717 : 0.283). All fluorine atoms were refined with fixing the C-F distances (-1.35 A). The disordered CH2Cl2 molecules was refined isotropically with fixing the C401-Cl1 distance (1.78 A). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11168 _refine_ls_number_parameters 637 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1570 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2244 _refine_ls_wR_factor_gt 0.2013 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.04995(7) 0.67054(6) 0.19472(4) 0.0373(2) Uani 1 1 d . A . Ru2 Ru -0.47028(6) 0.39194(5) 0.15145(4) 0.0339(2) Uani 1 1 d . A . Cl1 Cl 0.3337(10) 0.0219(8) 0.4473(7) 0.289(5) Uiso 1 1 d D . . Cl2 Cl 0.2715(9) 0.1254(9) 0.3219(6) 0.271(5) Uiso 1 1 d . . . S1 S -0.0184(2) 0.8772(2) 0.27891(17) 0.0515(7) Uani 1 1 d . A . S2 S -0.4715(2) 0.57816(18) 0.29474(14) 0.0406(6) Uani 1 1 d . A . P1 P -0.0043(2) 0.59992(18) 0.29467(14) 0.0342(5) Uani 1 1 d . . . P2 P -0.3052(2) 0.37002(17) 0.25157(13) 0.0340(5) Uani 1 1 d . . . F1 F -0.6352(5) 0.7673(5) 0.0661(4) 0.0684(19) Uani 1 1 d . A . F2 F -0.6419(6) 0.8449(5) 0.1807(4) 0.075(2) Uani 1 1 d . A . F3 F -0.6103(10) 0.9848(7) 0.0915(7) 0.063(3) Uani 0.717(7) 1 d PD A 1 F3A F -0.5483(19) 0.9953(15) 0.1968(14) 0.063(3) Uani 0.283(7) 1 d PD A 2 F4 F -0.5345(8) 0.8905(6) 0.0134(5) 0.068(3) Uani 0.717(7) 1 d PD A 1 F4A F -0.607(3) 0.966(2) 0.0588(15) 0.068(3) Uani 0.283(7) 1 d PD A 2 F5 F -0.4176(10) 1.0178(7) 0.2062(7) 0.098(5) Uani 0.717(7) 1 d PD A 3 F5A F -0.345(2) 1.0310(13) 0.162(2) 0.098(5) Uani 0.283(7) 1 d PD A 4 F6 F -0.3430(9) 0.9930(9) 0.1081(9) 0.122(5) Uani 0.717(7) 1 d PD A 3 F6A F -0.397(2) 0.9308(17) 0.0685(9) 0.122(5) Uani 0.283(7) 1 d PD A 4 O131 O 0.2485(6) 0.7839(6) 0.3284(5) 0.067(2) Uani 1 1 d . A . O231 O -0.3236(7) 0.4461(6) 0.0406(4) 0.059(2) Uani 1 1 d . A . C1 C -0.3642(8) 0.8599(7) 0.1790(5) 0.038(2) Uani 1 1 d . A . C2 C -0.4550(8) 0.7963(6) 0.1741(5) 0.036(2) Uani 1 1 d . A . C3 C -0.5692(8) 0.8300(7) 0.1317(6) 0.044(2) Uani 1 1 d . . . C4 C -0.5354(13) 0.9164(10) 0.0931(6) 0.045(4) Uani 0.717(7) 1 d PD A 1 C4A C -0.547(4) 0.935(3) 0.1289(14) 0.045(4) Uani 0.283(7) 1 d PD A 2 C5 C -0.4126(9) 0.9471(6) 0.1452(6) 0.054(3) Uani 1 1 d D . . C111 C -0.1538(9) 0.9179(7) 0.2633(7) 0.051(3) Uani 1 1 d . A . C112 C -0.2376(8) 0.8503(6) 0.2084(6) 0.039(2) Uani 1 1 d . . . C113 C -0.1859(8) 0.7682(6) 0.1802(5) 0.036(2) Uani 1 1 d . A . C114 C -0.0649(8) 0.7698(7) 0.2131(5) 0.038(2) Uani 1 1 d . . . C115 C -0.1693(11) 1.0084(9) 0.3124(8) 0.075(4) Uani 1 1 d . . . C121 C 0.1012(9) 0.6822(9) 0.0762(6) 0.052(3) Uani 1 1 d . . . C122 C 0.1524(10) 0.6051(9) 0.1104(6) 0.057(3) Uani 1 1 d . A . C123 C 0.0625(10) 0.5367(8) 0.1108(6) 0.054(3) Uani 1 1 d . . . C124 C -0.0487(10) 0.5724(8) 0.0780(6) 0.054(3) Uani 1 1 d . A . C125 C -0.0228(10) 0.6620(9) 0.0555(6) 0.058(3) Uani 1 1 d . A . C131 C 0.1706(9) 0.7403(8) 0.2757(6) 0.051(3) Uani 1 1 d . . . C211 C -0.4648(8) 0.6973(7) 0.2825(5) 0.038(2) Uani 1 1 d . A . C212 C -0.4535(8) 0.7054(7) 0.2048(5) 0.038(2) Uani 1 1 d . . . C213 C -0.4513(8) 0.6146(7) 0.1573(5) 0.039(2) Uani 1 1 d . A . C214 C -0.4591(8) 0.5351(7) 0.1953(5) 0.039(2) Uani 1 1 d . . . C215 C -0.4687(9) 0.7755(8) 0.3499(6) 0.051(3) Uani 1 1 d . . . C221 C -0.6615(8) 0.3762(8) 0.1544(7) 0.050(3) Uani 1 1 d . . . C222 C -0.6041(9) 0.3035(7) 0.1923(6) 0.045(2) Uani 1 1 d . A . C223 C -0.5672(9) 0.2444(7) 0.1318(7) 0.052(3) Uani 1 1 d . . . C224 C -0.5982(9) 0.2842(8) 0.0561(6) 0.051(3) Uani 1 1 d . A . C225 C -0.6576(9) 0.3657(8) 0.0699(6) 0.053(3) Uani 1 1 d . A . C231 C -0.3807(9) 0.4264(7) 0.0852(6) 0.042(2) Uani 1 1 d . . . C311 C -0.1424(8) 0.5210(6) 0.2504(5) 0.037(2) Uani 1 1 d . . . C312 C -0.2018(8) 0.4741(6) 0.3069(5) 0.036(2) Uani 1 1 d . . . C321 C 0.1003(8) 0.5235(7) 0.3487(5) 0.036(2) Uani 1 1 d . . . C322 C 0.0862(8) 0.4859(7) 0.4186(5) 0.040(2) Uani 1 1 d . . . C323 C 0.1611(9) 0.4247(8) 0.4560(6) 0.047(3) Uani 1 1 d . . . C324 C 0.2572(11) 0.4015(8) 0.4287(7) 0.059(3) Uani 1 1 d . . . C325 C 0.2781(10) 0.4417(9) 0.3618(7) 0.057(3) Uani 1 1 d . . . C326 C 0.1988(9) 0.5020(8) 0.3220(5) 0.046(2) Uani 1 1 d . . . C331 C -0.0288(7) 0.6799(7) 0.3802(5) 0.035(2) Uani 1 1 d . . . C332 C 0.0643(8) 0.7180(7) 0.4475(6) 0.045(2) Uani 1 1 d . . . C333 C 0.0534(10) 0.7858(8) 0.5076(6) 0.057(3) Uani 1 1 d . . . C334 C -0.0547(10) 0.8219(8) 0.5024(6) 0.059(3) Uani 1 1 d . . . C335 C -0.1506(8) 0.7841(8) 0.4369(6) 0.046(2) Uani 1 1 d . . . C336 C -0.1384(8) 0.7159(7) 0.3749(5) 0.038(2) Uani 1 1 d . . . C341 C -0.2062(8) 0.2899(7) 0.2202(5) 0.039(2) Uani 1 1 d . . . C342 C -0.2298(9) 0.2421(8) 0.1403(6) 0.051(3) Uani 1 1 d . . . C343 C -0.1513(13) 0.1865(10) 0.1157(7) 0.078(4) Uani 1 1 d . . . C344 C -0.0434(13) 0.1783(12) 0.1730(9) 0.088(5) Uani 1 1 d . . . C345 C -0.0185(12) 0.2246(11) 0.2503(9) 0.084(4) Uani 1 1 d . . . C346 C -0.0969(9) 0.2806(8) 0.2772(7) 0.056(3) Uani 1 1 d . . . C351 C -0.3389(7) 0.3172(7) 0.3362(5) 0.035(2) Uani 1 1 d . . . C352 C -0.3582(9) 0.3738(7) 0.4049(5) 0.042(2) Uani 1 1 d . . . C353 C -0.3922(10) 0.3308(8) 0.4647(6) 0.051(3) Uani 1 1 d . . . C354 C -0.4062(10) 0.2324(9) 0.4589(6) 0.057(3) Uani 1 1 d . . . C355 C -0.3887(10) 0.1775(8) 0.3919(7) 0.052(3) Uani 1 1 d . . . C356 C -0.3552(9) 0.2187(7) 0.3290(6) 0.043(2) Uani 1 1 d . . . C401 C 0.291(3) 0.008(3) 0.3373(8) 0.237(14) Uiso 1 1 d D . . H1 H -0.2333 0.7159 0.1412 0.044 Uiso 1 1 d . . . H2 H -0.0955 1.0393 0.3453 0.089 Uiso 1 1 d . . . H3 H -0.2094 1.0498 0.2771 0.089 Uiso 1 1 d . . . H4 H -0.2166 0.9946 0.3493 0.089 Uiso 1 1 d . . . H5 H 0.1421 0.7391 0.0649 0.063 Uiso 1 1 d . . . H6 H 0.2359 0.5999 0.1280 0.070 Uiso 1 1 d . . . H7 H 0.0744 0.4742 0.1286 0.066 Uiso 1 1 d . . . H8 H -0.1273 0.5395 0.0689 0.068 Uiso 1 1 d . . . H9 H -0.0805 0.7027 0.0289 0.069 Uiso 1 1 d . . . H10 H -0.4464 0.6086 0.1007 0.047 Uiso 1 1 d . . . H11 H -0.3980 0.8177 0.3658 0.062 Uiso 1 1 d . . . H12 H -0.5343 0.8113 0.3316 0.062 Uiso 1 1 d . . . H13 H -0.4772 0.7490 0.3975 0.062 Uiso 1 1 d . . . H14 H -0.7013 0.4234 0.1805 0.060 Uiso 1 1 d . . . H15 H -0.5970 0.2914 0.2487 0.056 Uiso 1 1 d . . . H16 H -0.5299 0.1861 0.1391 0.061 Uiso 1 1 d . . . H17 H -0.5874 0.2561 0.0042 0.059 Uiso 1 1 d . . . H18 H -0.6935 0.4035 0.0288 0.063 Uiso 1 1 d . . . H19 H -0.1994 0.5583 0.2187 0.045 Uiso 1 1 d . . . H20 H -0.1275 0.4713 0.2110 0.045 Uiso 1 1 d . . . H21 H -0.2423 0.5194 0.3325 0.044 Uiso 1 1 d . . . H22 H -0.1409 0.4537 0.3501 0.044 Uiso 1 1 d . . . H23 H 0.0210 0.5050 0.4408 0.048 Uiso 1 1 d . . . H24 H 0.1473 0.3980 0.5028 0.057 Uiso 1 1 d . . . H25 H 0.3099 0.3584 0.4556 0.071 Uiso 1 1 d . . . H26 H 0.3486 0.4287 0.3446 0.067 Uiso 1 1 d . . . H27 H 0.2121 0.5282 0.2753 0.055 Uiso 1 1 d . . . H28 H 0.1411 0.6945 0.4526 0.054 Uiso 1 1 d . . . H29 H 0.1206 0.8092 0.5540 0.068 Uiso 1 1 d . . . H30 H -0.0623 0.8712 0.5448 0.069 Uiso 1 1 d . . . H31 H -0.2265 0.8057 0.4340 0.056 Uiso 1 1 d . . . H32 H -0.2044 0.6919 0.3280 0.045 Uiso 1 1 d . . . H33 H -0.3032 0.2486 0.1008 0.060 Uiso 1 1 d . . . H34 H -0.1718 0.1543 0.0593 0.090 Uiso 1 1 d . . . H35 H 0.0120 0.1385 0.1558 0.100 Uiso 1 1 d . . . H36 H 0.0590 0.2194 0.2883 0.097 Uiso 1 1 d . . . H37 H -0.0780 0.3130 0.3335 0.068 Uiso 1 1 d . . . H38 H -0.3482 0.4434 0.4088 0.051 Uiso 1 1 d . . . H39 H -0.4026 0.3700 0.5145 0.061 Uiso 1 1 d . . . H40 H -0.4268 0.2037 0.5026 0.069 Uiso 1 1 d . . . H41 H -0.4015 0.1078 0.3869 0.064 Uiso 1 1 d . . . H42 H -0.3441 0.1789 0.2806 0.051 Uiso 1 1 d . . . H43 H 0.3527 -0.0127 0.3215 0.203 Uiso 1 1 d . . . H44 H 0.2217 -0.0281 0.3220 0.203 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0350(4) 0.0424(5) 0.0351(4) 0.0059(3) 0.0111(3) 0.0000(3) Ru2 0.0384(4) 0.0285(4) 0.0328(4) 0.0051(3) 0.0064(3) 0.0017(3) S1 0.0428(14) 0.0412(16) 0.0607(16) -0.0025(12) 0.0037(13) -0.0029(11) S2 0.0457(13) 0.0386(14) 0.0422(13) 0.0092(10) 0.0186(11) 0.0049(11) P1 0.0359(12) 0.0355(14) 0.0303(11) 0.0034(9) 0.0087(10) 0.0022(10) P2 0.0371(12) 0.0334(14) 0.0299(11) 0.0046(9) 0.0072(10) 0.0019(10) F1 0.058(4) 0.073(5) 0.057(4) 0.004(3) -0.012(3) 0.009(3) F2 0.058(4) 0.093(6) 0.083(5) 0.016(4) 0.029(4) 0.036(4) F3 0.059(5) 0.039(5) 0.090(7) 0.007(5) 0.017(6) 0.021(4) F3A 0.059(5) 0.039(5) 0.090(7) 0.007(5) 0.017(6) 0.021(4) F4 0.086(7) 0.054(6) 0.052(5) 0.014(4) -0.002(5) 0.002(5) F4A 0.086(7) 0.054(6) 0.052(5) 0.014(4) -0.002(5) 0.002(5) F5 0.090(9) 0.048(6) 0.108(9) -0.033(6) -0.038(7) 0.030(6) F5A 0.090(9) 0.048(6) 0.108(9) -0.033(6) -0.038(7) 0.030(6) F6 0.069(7) 0.086(10) 0.214(14) 0.120(10) 0.006(8) -0.021(6) F6A 0.069(7) 0.086(10) 0.214(14) 0.120(10) 0.006(8) -0.021(6) O131 0.047(4) 0.075(6) 0.066(5) -0.001(4) 0.003(4) -0.011(4) O231 0.069(5) 0.067(6) 0.046(4) 0.011(4) 0.024(4) -0.006(4) C1 0.040(5) 0.034(6) 0.034(5) 0.002(4) -0.001(4) 0.007(4) C2 0.050(5) 0.023(5) 0.037(5) 0.004(4) 0.015(4) 0.005(4) C3 0.036(5) 0.043(6) 0.052(6) 0.010(5) 0.011(5) 0.009(4) C4 0.044(7) 0.031(8) 0.067(11) 0.014(9) 0.021(9) 0.016(6) C4A 0.044(7) 0.031(8) 0.067(11) 0.014(9) 0.021(9) 0.016(6) C5 0.059(7) 0.043(7) 0.060(7) 0.019(5) 0.012(6) 0.007(5) C111 0.053(6) 0.028(6) 0.067(7) -0.003(5) 0.016(5) -0.004(5) C112 0.043(5) 0.025(5) 0.047(5) 0.000(4) 0.013(4) 0.000(4) C113 0.044(5) 0.029(5) 0.035(5) 0.004(4) 0.009(4) 0.003(4) C114 0.039(5) 0.039(6) 0.040(5) 0.012(4) 0.017(4) -0.007(4) C115 0.067(8) 0.046(7) 0.087(9) -0.025(6) -0.006(7) 0.003(6) C121 0.053(6) 0.077(8) 0.030(5) 0.011(5) 0.021(5) 0.000(6) C122 0.051(6) 0.076(9) 0.048(6) 0.009(6) 0.018(5) 0.019(6) C123 0.066(7) 0.056(7) 0.034(5) -0.005(5) 0.009(5) 0.004(6) C124 0.066(7) 0.060(8) 0.034(5) -0.001(5) 0.018(5) -0.006(6) C125 0.065(7) 0.079(9) 0.032(5) 0.008(5) 0.017(5) 0.008(6) C131 0.046(6) 0.054(7) 0.050(6) 0.003(5) 0.011(5) 0.003(5) C211 0.038(5) 0.038(6) 0.041(5) 0.002(4) 0.016(4) 0.010(4) C212 0.035(5) 0.033(5) 0.040(5) 0.006(4) 0.003(4) -0.001(4) C213 0.044(5) 0.031(5) 0.038(5) 0.007(4) 0.007(4) -0.001(4) C214 0.032(5) 0.052(6) 0.032(5) 0.016(4) 0.004(4) 0.003(4) C215 0.054(6) 0.047(7) 0.053(6) -0.001(5) 0.020(5) 0.018(5) C221 0.033(5) 0.050(7) 0.062(7) 0.007(5) 0.008(5) 0.001(5) C222 0.043(5) 0.044(6) 0.052(6) 0.008(5) 0.019(5) -0.002(5) C223 0.043(5) 0.025(5) 0.080(8) 0.008(5) 0.008(5) -0.013(4) C224 0.043(6) 0.053(7) 0.041(6) -0.017(5) 0.003(5) -0.021(5) C225 0.038(5) 0.061(8) 0.044(6) 0.012(5) -0.013(5) -0.003(5) C231 0.054(6) 0.028(5) 0.041(5) 0.002(4) 0.010(5) 0.002(4) C311 0.045(5) 0.030(5) 0.038(5) 0.002(4) 0.015(4) -0.001(4) C312 0.045(5) 0.033(5) 0.026(4) 0.003(3) 0.006(4) 0.003(4) C321 0.032(4) 0.039(6) 0.035(5) -0.001(4) 0.009(4) 0.000(4) C322 0.036(5) 0.045(6) 0.037(5) 0.015(4) 0.001(4) 0.004(4) C323 0.050(6) 0.051(7) 0.042(6) 0.016(5) 0.011(5) 0.003(5) C324 0.070(7) 0.057(8) 0.056(7) 0.023(5) 0.013(6) 0.027(6) C325 0.055(7) 0.068(8) 0.057(7) 0.015(6) 0.024(6) 0.025(6) C326 0.049(6) 0.059(7) 0.035(5) 0.008(4) 0.020(5) 0.006(5) C331 0.028(4) 0.043(6) 0.034(5) 0.007(4) 0.005(4) 0.004(4) C332 0.036(5) 0.050(7) 0.039(5) -0.010(4) 0.001(4) 0.002(4) C333 0.056(6) 0.053(7) 0.045(6) -0.017(5) -0.002(5) 0.005(5) C334 0.061(7) 0.058(8) 0.044(6) -0.013(5) 0.003(5) 0.006(6) C335 0.034(5) 0.051(7) 0.052(6) 0.000(5) 0.009(5) 0.010(4) C336 0.036(5) 0.037(6) 0.036(5) -0.003(4) 0.006(4) 0.007(4) C341 0.043(5) 0.040(6) 0.036(5) 0.005(4) 0.011(4) 0.005(4) C342 0.055(6) 0.056(7) 0.042(6) -0.002(5) 0.016(5) 0.015(5) C343 0.098(10) 0.087(11) 0.055(7) 0.002(6) 0.022(7) 0.052(8) C344 0.081(10) 0.108(13) 0.091(10) 0.009(9) 0.047(9) 0.043(9) C345 0.072(9) 0.079(11) 0.094(11) 0.004(8) 0.008(8) 0.034(8) C346 0.036(5) 0.061(8) 0.063(7) 0.005(5) 0.003(5) 0.010(5) C351 0.032(4) 0.040(6) 0.029(4) 0.005(4) 0.001(4) 0.001(4) C352 0.049(6) 0.050(6) 0.027(4) 0.005(4) 0.011(4) 0.002(5) C353 0.068(7) 0.052(7) 0.033(5) 0.001(4) 0.015(5) 0.010(6) C354 0.061(7) 0.076(9) 0.041(6) 0.017(5) 0.024(5) 0.000(6) C355 0.064(7) 0.039(6) 0.064(7) 0.027(5) 0.025(6) 0.012(5) C356 0.050(6) 0.038(6) 0.040(5) 0.009(4) 0.012(5) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C131 1.825(10) . ? Ru1 C114 2.064(10) . ? Ru1 C122 2.252(11) . ? Ru1 C124 2.254(10) . ? Ru1 C123 2.260(11) . ? Ru1 C121 2.267(9) . ? Ru1 C125 2.267(10) . ? Ru1 P1 2.283(2) . ? Ru2 C231 1.824(11) . ? Ru2 C214 2.057(10) . ? Ru2 C224 2.240(8) . ? Ru2 C225 2.254(9) . ? Ru2 C222 2.262(10) . ? Ru2 C223 2.267(9) . ? Ru2 C221 2.269(10) . ? Ru2 P2 2.284(2) . ? Cl1 C401 1.776(5) . ? Cl2 C401 1.74(3) . ? S1 C111 1.698(11) . ? S1 C114 1.734(10) . ? S2 C211 1.730(10) . ? S2 C214 1.762(9) . ? P1 C331 1.820(9) . ? P1 C321 1.830(9) . ? P1 C311 1.841(9) . ? P2 C341 1.810(10) . ? P2 C351 1.820(9) . ? P2 C312 1.836(9) . ? F1 C3 1.355(11) . ? F2 C3 1.350(11) . ? F3 C4 1.351(5) . ? F3A C4A 1.350(5) . ? F4 C4 1.354(5) . ? F4A C4A 1.351(5) . ? F5 C5 1.360(5) . ? F5A C5 1.349(5) . ? F6 C5 1.345(5) . ? F6A C5 1.355(5) . ? O131 C131 1.174(11) . ? O231 C231 1.184(11) . ? C1 C2 1.336(12) . ? C1 C112 1.464(12) . ? C1 C5 1.510(12) . ? C2 C212 1.451(12) . ? C2 C3 1.487(12) . ? C3 C4A 1.50(4) . ? C3 C4 1.542(18) . ? C4 C5 1.488(18) . ? C4A C5 1.53(5) . ? C111 C112 1.389(12) . ? C111 C115 1.488(14) . ? C112 C113 1.435(12) . ? C113 C114 1.386(12) . ? C121 C122 1.399(15) . ? C121 C125 1.413(15) . ? C122 C123 1.397(16) . ? C123 C124 1.433(16) . ? C124 C125 1.413(16) . ? C211 C212 1.376(12) . ? C211 C215 1.498(13) . ? C212 C213 1.435(13) . ? C213 C214 1.379(12) . ? C221 C222 1.400(14) . ? C221 C225 1.431(14) . ? C222 C223 1.415(15) . ? C223 C224 1.435(14) . ? C224 C225 1.414(15) . ? C311 C312 1.522(12) . ? C321 C326 1.391(13) . ? C321 C322 1.404(12) . ? C322 C323 1.368(13) . ? C323 C324 1.377(15) . ? C324 C325 1.403(15) . ? C325 C326 1.403(14) . ? C331 C332 1.379(11) . ? C331 C336 1.404(12) . ? C332 C333 1.347(13) . ? C333 C334 1.388(15) . ? C334 C335 1.379(13) . ? C335 C336 1.377(13) . ? C341 C342 1.382(12) . ? C341 C346 1.415(13) . ? C342 C343 1.365(15) . ? C343 C344 1.402(18) . ? C344 C345 1.335(18) . ? C345 C346 1.384(16) . ? C351 C356 1.385(13) . ? C351 C352 1.406(12) . ? C352 C353 1.378(13) . ? C353 C354 1.385(16) . ? C354 C355 1.361(15) . ? C355 C356 1.409(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C131 Ru1 C114 90.9(4) . . ? C131 Ru1 C122 99.8(4) . . ? C114 Ru1 C122 146.8(4) . . ? C131 Ru1 C124 161.0(4) . . ? C114 Ru1 C124 105.2(4) . . ? C122 Ru1 C124 61.2(4) . . ? C131 Ru1 C123 126.7(5) . . ? C114 Ru1 C123 142.1(4) . . ? C122 Ru1 C123 36.1(4) . . ? C124 Ru1 C123 37.0(4) . . ? C131 Ru1 C121 104.1(4) . . ? C114 Ru1 C121 110.9(4) . . ? C122 Ru1 C121 36.1(4) . . ? C124 Ru1 C121 61.1(4) . . ? C123 Ru1 C121 60.3(4) . . ? C131 Ru1 C125 136.2(5) . . ? C114 Ru1 C125 90.3(4) . . ? C122 Ru1 C125 60.3(4) . . ? C124 Ru1 C125 36.4(4) . . ? C123 Ru1 C125 60.5(4) . . ? C121 Ru1 C125 36.3(4) . . ? C131 Ru1 P1 88.7(3) . . ? C114 Ru1 P1 85.7(2) . . ? C122 Ru1 P1 125.5(3) . . ? C124 Ru1 P1 102.2(3) . . ? C123 Ru1 P1 98.2(3) . . ? C121 Ru1 P1 158.5(3) . . ? C125 Ru1 P1 135.0(3) . . ? C231 Ru2 C214 86.3(4) . . ? C231 Ru2 C224 97.1(4) . . ? C214 Ru2 C224 137.4(4) . . ? C231 Ru2 C225 105.8(4) . . ? C214 Ru2 C225 101.5(4) . . ? C224 Ru2 C225 36.7(4) . . ? C231 Ru2 C222 158.0(4) . . ? C214 Ru2 C222 113.0(4) . . ? C224 Ru2 C222 61.7(4) . . ? C225 Ru2 C222 61.4(4) . . ? C231 Ru2 C223 122.5(4) . . ? C214 Ru2 C223 148.5(4) . . ? C224 Ru2 C223 37.1(4) . . ? C225 Ru2 C223 61.2(4) . . ? C222 Ru2 C223 36.4(4) . . ? C231 Ru2 C221 140.5(4) . . ? C214 Ru2 C221 89.8(4) . . ? C224 Ru2 C221 61.1(4) . . ? C225 Ru2 C221 36.9(4) . . ? C222 Ru2 C221 36.0(4) . . ? C223 Ru2 C221 60.2(4) . . ? C231 Ru2 P2 91.1(3) . . ? C214 Ru2 P2 92.5(2) . . ? C224 Ru2 P2 129.7(3) . . ? C225 Ru2 P2 158.6(3) . . ? C222 Ru2 P2 98.3(3) . . ? C223 Ru2 P2 98.7(3) . . ? C221 Ru2 P2 128.4(3) . . ? C111 S1 C114 96.2(5) . . ? C211 S2 C214 95.5(4) . . ? C331 P1 C321 102.2(4) . . ? C331 P1 C311 105.7(4) . . ? C321 P1 C311 104.4(4) . . ? C331 P1 Ru1 116.3(3) . . ? C321 P1 Ru1 115.9(3) . . ? C311 P1 Ru1 111.1(3) . . ? C341 P2 C351 102.1(4) . . ? C341 P2 C312 101.3(4) . . ? C351 P2 C312 102.2(4) . . ? C341 P2 Ru2 116.8(3) . . ? C351 P2 Ru2 113.0(3) . . ? C312 P2 Ru2 119.1(3) . . ? C2 C1 C112 128.4(9) . . ? C2 C1 C5 108.4(8) . . ? C112 C1 C5 123.2(8) . . ? C1 C2 C212 128.8(9) . . ? C1 C2 C3 111.2(8) . . ? C212 C2 C3 120.0(8) . . ? F2 C3 F1 103.8(8) . . ? F2 C3 C2 113.8(8) . . ? F1 C3 C2 113.7(8) . . ? F2 C3 C4A 93.0(16) . . ? F1 C3 C4A 123.2(12) . . ? C2 C3 C4A 107.5(17) . . ? F2 C3 C4 116.1(8) . . ? F1 C3 C4 104.2(8) . . ? C2 C3 C4 105.1(8) . . ? C4A C3 C4 25.7(10) . . ? F3 C4 F4 105.9(9) . . ? F3 C4 C5 114.5(12) . . ? F4 C4 C5 109.4(10) . . ? F3 C4 C3 113.5(11) . . ? F4 C4 C3 111.6(11) . . ? C5 C4 C3 102.0(8) . . ? F3A C4A F4A 111(2) . . ? F3A C4A C3 117(3) . . ? F4A C4A C3 116(3) . . ? F3A C4A C5 95(3) . . ? F4A C4A C5 114(4) . . ? C3 C4A C5 101.9(18) . . ? F6 C5 F5A 43.6(15) . . ? F6 C5 F6A 47.6(11) . . ? F5A C5 F6A 90.7(18) . . ? F6 C5 F5 100.4(11) . . ? F5A C5 F5 57.5(15) . . ? F6A C5 F5 142.9(14) . . ? F6 C5 C4 115.2(10) . . ? F5A C5 C4 132.5(17) . . ? F6A C5 C4 78.5(13) . . ? F5 C5 C4 107.9(8) . . ? F6 C5 C1 114.2(9) . . ? F5A C5 C1 120.9(17) . . ? F6A C5 C1 99.7(13) . . ? F5 C5 C1 112.5(9) . . ? C4 C5 C1 106.5(8) . . ? F6 C5 C4A 131.7(15) . . ? F5A C5 C4A 126(2) . . ? F6A C5 C4A 103.7(16) . . ? F5 C5 C4A 84.1(11) . . ? C4 C5 C4A 25.9(8) . . ? C1 C5 C4A 107.8(15) . . ? C112 C111 C115 130.0(10) . . ? C112 C111 S1 109.5(8) . . ? C115 C111 S1 120.1(8) . . ? C111 C112 C113 112.2(8) . . ? C111 C112 C1 125.7(9) . . ? C113 C112 C1 122.1(8) . . ? C114 C113 C112 115.4(8) . . ? C113 C114 S1 106.7(7) . . ? C113 C114 Ru1 130.8(7) . . ? S1 C114 Ru1 122.5(5) . . ? C122 C121 C125 107.8(10) . . ? C122 C121 Ru1 71.4(6) . . ? C125 C121 Ru1 71.9(6) . . ? C123 C122 C121 108.7(10) . . ? C123 C122 Ru1 72.3(6) . . ? C121 C122 Ru1 72.5(6) . . ? C122 C123 C124 108.3(10) . . ? C122 C123 Ru1 71.7(6) . . ? C124 C123 Ru1 71.3(6) . . ? C125 C124 C123 106.4(10) . . ? C125 C124 Ru1 72.3(6) . . ? C123 C124 Ru1 71.7(6) . . ? C124 C125 C121 108.7(11) . . ? C124 C125 Ru1 71.3(6) . . ? C121 C125 Ru1 71.8(6) . . ? O131 C131 Ru1 179.0(10) . . ? C212 C211 C215 128.2(9) . . ? C212 C211 S2 109.3(7) . . ? C215 C211 S2 122.5(7) . . ? C211 C212 C213 112.5(8) . . ? C211 C212 C2 122.0(9) . . ? C213 C212 C2 125.3(8) . . ? C214 C213 C212 116.9(9) . . ? C213 C214 S2 105.8(7) . . ? C213 C214 Ru2 131.3(7) . . ? S2 C214 Ru2 122.7(5) . . ? C222 C221 C225 109.0(10) . . ? C222 C221 Ru2 71.7(6) . . ? C225 C221 Ru2 71.0(6) . . ? C221 C222 C223 107.8(9) . . ? C221 C222 Ru2 72.2(6) . . ? C223 C222 Ru2 72.0(5) . . ? C222 C223 C224 108.1(9) . . ? C222 C223 Ru2 71.6(6) . . ? C224 C223 Ru2 70.4(5) . . ? C225 C224 C223 107.7(9) . . ? C225 C224 Ru2 72.2(5) . . ? C223 C224 Ru2 72.5(5) . . ? C224 C225 C221 107.3(9) . . ? C224 C225 Ru2 71.1(5) . . ? C221 C225 Ru2 72.1(5) . . ? O231 C231 Ru2 178.0(9) . . ? C312 C311 P1 120.2(6) . . ? C311 C312 P2 112.5(6) . . ? C326 C321 C322 117.4(8) . . ? C326 C321 P1 120.5(7) . . ? C322 C321 P1 122.1(7) . . ? C323 C322 C321 121.7(9) . . ? C322 C323 C324 120.9(9) . . ? C323 C324 C325 119.1(9) . . ? C324 C325 C326 119.7(10) . . ? C321 C326 C325 121.0(9) . . ? C332 C331 C336 117.4(9) . . ? C332 C331 P1 120.6(7) . . ? C336 C331 P1 121.4(7) . . ? C333 C332 C331 122.9(10) . . ? C332 C333 C334 119.9(9) . . ? C335 C334 C333 118.9(10) . . ? C336 C335 C334 120.8(9) . . ? C335 C336 C331 120.0(8) . . ? C342 C341 C346 118.2(9) . . ? C342 C341 P2 122.2(7) . . ? C346 C341 P2 119.4(7) . . ? C343 C342 C341 121.9(10) . . ? C342 C343 C344 119.0(11) . . ? C345 C344 C343 120.0(12) . . ? C344 C345 C346 122.2(12) . . ? C345 C346 C341 118.6(10) . . ? C356 C351 C352 119.4(8) . . ? C356 C351 P2 118.8(7) . . ? C352 C351 P2 121.5(7) . . ? C353 C352 C351 119.8(9) . . ? C352 C353 C354 121.1(9) . . ? C355 C354 C353 119.1(9) . . ? C354 C355 C356 121.5(10) . . ? C351 C356 C355 119.1(9) . . ? Cl2 C401 Cl1 100.2(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C131 Ru1 P1 C331 53.8(5) . . . . ? C114 Ru1 P1 C331 -37.2(4) . . . . ? C122 Ru1 P1 C331 155.0(5) . . . . ? C124 Ru1 P1 C331 -141.8(4) . . . . ? C123 Ru1 P1 C331 -179.3(4) . . . . ? C121 Ru1 P1 C331 -178.7(8) . . . . ? C125 Ru1 P1 C331 -123.4(5) . . . . ? C131 Ru1 P1 C321 -66.4(5) . . . . ? C114 Ru1 P1 C321 -157.4(4) . . . . ? C122 Ru1 P1 C321 34.8(5) . . . . ? C124 Ru1 P1 C321 98.0(5) . . . . ? C123 Ru1 P1 C321 60.5(4) . . . . ? C121 Ru1 P1 C321 61.1(8) . . . . ? C125 Ru1 P1 C321 116.4(5) . . . . ? C131 Ru1 P1 C311 174.7(5) . . . . ? C114 Ru1 P1 C311 83.7(4) . . . . ? C122 Ru1 P1 C311 -84.1(5) . . . . ? C124 Ru1 P1 C311 -20.9(5) . . . . ? C123 Ru1 P1 C311 -58.4(4) . . . . ? C121 Ru1 P1 C311 -57.8(8) . . . . ? C125 Ru1 P1 C311 -2.5(6) . . . . ? C231 Ru2 P2 C341 -54.6(5) . . . . ? C214 Ru2 P2 C341 -140.9(4) . . . . ? C224 Ru2 P2 C341 45.6(5) . . . . ? C225 Ru2 P2 C341 88.0(9) . . . . ? C222 Ru2 P2 C341 105.5(5) . . . . ? C223 Ru2 P2 C341 68.6(5) . . . . ? C221 Ru2 P2 C341 127.3(5) . . . . ? C231 Ru2 P2 C351 -172.5(4) . . . . ? C214 Ru2 P2 C351 101.2(4) . . . . ? C224 Ru2 P2 C351 -72.3(5) . . . . ? C225 Ru2 P2 C351 -29.9(9) . . . . ? C222 Ru2 P2 C351 -12.5(4) . . . . ? C223 Ru2 P2 C351 -49.3(5) . . . . ? C221 Ru2 P2 C351 9.4(5) . . . . ? C231 Ru2 P2 C312 67.5(4) . . . . ? C214 Ru2 P2 C312 -18.8(4) . . . . ? C224 Ru2 P2 C312 167.7(5) . . . . ? C225 Ru2 P2 C312 -149.9(9) . . . . ? C222 Ru2 P2 C312 -132.5(4) . . . . ? C223 Ru2 P2 C312 -169.3(5) . . . . ? C221 Ru2 P2 C312 -110.6(5) . . . . ? C112 C1 C2 C212 7.6(17) . . . . ? C5 C1 C2 C212 -174.5(9) . . . . ? C112 C1 C2 C3 -173.5(9) . . . . ? C5 C1 C2 C3 4.4(11) . . . . ? C1 C2 C3 F2 -116.2(10) . . . . ? C212 C2 C3 F2 62.9(12) . . . . ? C1 C2 C3 F1 125.3(9) . . . . ? C212 C2 C3 F1 -55.6(12) . . . . ? C1 C2 C3 C4A -14.7(15) . . . . ? C212 C2 C3 C4A 164.4(13) . . . . ? C1 C2 C3 C4 12.0(11) . . . . ? C212 C2 C3 C4 -169.0(8) . . . . ? F2 C3 C4 F3 -19.9(15) . . . . ? F1 C3 C4 F3 93.5(11) . . . . ? C2 C3 C4 F3 -146.6(10) . . . . ? C4A C3 C4 F3 -48(4) . . . . ? F2 C3 C4 F4 -139.5(9) . . . . ? F1 C3 C4 F4 -26.1(12) . . . . ? C2 C3 C4 F4 93.8(11) . . . . ? C4A C3 C4 F4 -167(5) . . . . ? F2 C3 C4 C5 103.8(9) . . . . ? F1 C3 C4 C5 -142.8(7) . . . . ? C2 C3 C4 C5 -22.9(9) . . . . ? C4A C3 C4 C5 76(4) . . . . ? F2 C3 C4A F3A 32(3) . . . . ? F1 C3 C4A F3A 140(2) . . . . ? C2 C3 C4A F3A -84(3) . . . . ? C4 C3 C4A F3A -173(7) . . . . ? F2 C3 C4A F4A -102(3) . . . . ? F1 C3 C4A F4A 7(4) . . . . ? C2 C3 C4A F4A 142(3) . . . . ? C4 C3 C4A F4A 53(3) . . . . ? F2 C3 C4A C5 133.7(12) . . . . ? F1 C3 C4A C5 -117.7(14) . . . . ? C2 C3 C4A C5 17.6(16) . . . . ? C4 C3 C4A C5 -71(4) . . . . ? F3 C4 C5 F6 -83.5(13) . . . . ? F4 C4 C5 F6 35.2(14) . . . . ? C3 C4 C5 F6 153.5(10) . . . . ? F3 C4 C5 F5A -34(3) . . . . ? F4 C4 C5 F5A 84(2) . . . . ? C3 C4 C5 F5A -157(2) . . . . ? F3 C4 C5 F6A -114.5(15) . . . . ? F4 C4 C5 F6A 4.2(14) . . . . ? C3 C4 C5 F6A 122.5(13) . . . . ? F3 C4 C5 F5 27.7(14) . . . . ? F4 C4 C5 F5 146.4(10) . . . . ? C3 C4 C5 F5 -95.3(10) . . . . ? F3 C4 C5 C1 148.7(10) . . . . ? F4 C4 C5 C1 -92.7(11) . . . . ? C3 C4 C5 C1 25.6(9) . . . . ? F3 C4 C5 C4A 52(4) . . . . ? F4 C4 C5 C4A 171(4) . . . . ? C3 C4 C5 C4A -71(4) . . . . ? C2 C1 C5 F6 -148.3(11) . . . . ? C112 C1 C5 F6 29.8(14) . . . . ? C2 C1 C5 F5A 162.6(19) . . . . ? C112 C1 C5 F5A -19(2) . . . . ? C2 C1 C5 F6A -100.7(14) . . . . ? C112 C1 C5 F6A 77.4(15) . . . . ? C2 C1 C5 F5 98.1(11) . . . . ? C112 C1 C5 F5 -83.8(12) . . . . ? C2 C1 C5 C4 -19.9(10) . . . . ? C112 C1 C5 C4 158.2(8) . . . . ? C2 C1 C5 C4A 7.2(13) . . . . ? C112 C1 C5 C4A -174.7(11) . . . . ? F3A C4A C5 F6 -107(2) . . . . ? F4A C4A C5 F6 9(3) . . . . ? C3 C4A C5 F6 134.4(17) . . . . ? F3A C4A C5 F5A -50(3) . . . . ? F4A C4A C5 F5A 65(3) . . . . ? C3 C4A C5 F5A -169(2) . . . . ? F3A C4A C5 F6A -151(2) . . . . ? F4A C4A C5 F6A -36(3) . . . . ? C3 C4A C5 F6A 89.9(17) . . . . ? F3A C4A C5 F5 -8(2) . . . . ? F4A C4A C5 F5 107(2) . . . . ? C3 C4A C5 F5 -126.9(14) . . . . ? F3A C4A C5 C4 -165(5) . . . . ? F4A C4A C5 C4 -49(3) . . . . ? C3 C4A C5 C4 76(3) . . . . ? F3A C4A C5 C1 103(2) . . . . ? F4A C4A C5 C1 -141(2) . . . . ? C3 C4A C5 C1 -15.2(15) . . . . ? C114 S1 C111 C112 0.6(8) . . . . ? C114 S1 C111 C115 174.4(10) . . . . ? C115 C111 C112 C113 -174.1(12) . . . . ? S1 C111 C112 C113 -1.1(11) . . . . ? C115 C111 C112 C1 7.7(19) . . . . ? S1 C111 C112 C1 -179.3(8) . . . . ? C2 C1 C112 C111 -133.3(11) . . . . ? C5 C1 C112 C111 49.1(14) . . . . ? C2 C1 C112 C113 48.7(15) . . . . ? C5 C1 C112 C113 -128.9(10) . . . . ? C111 C112 C113 C114 1.3(12) . . . . ? C1 C112 C113 C114 179.5(8) . . . . ? C112 C113 C114 S1 -0.8(10) . . . . ? C112 C113 C114 Ru1 179.0(6) . . . . ? C111 S1 C114 C113 0.1(7) . . . . ? C111 S1 C114 Ru1 -179.7(6) . . . . ? C131 Ru1 C114 C113 -173.1(9) . . . . ? C122 Ru1 C114 C113 77.3(11) . . . . ? C124 Ru1 C114 C113 17.1(9) . . . . ? C123 Ru1 C114 C113 13.4(12) . . . . ? C121 Ru1 C114 C113 81.4(9) . . . . ? C125 Ru1 C114 C113 50.7(9) . . . . ? P1 Ru1 C114 C113 -84.4(8) . . . . ? C131 Ru1 C114 S1 6.7(6) . . . . ? C122 Ru1 C114 S1 -102.9(8) . . . . ? C124 Ru1 C114 S1 -163.1(5) . . . . ? C123 Ru1 C114 S1 -166.8(5) . . . . ? C121 Ru1 C114 S1 -98.8(6) . . . . ? C125 Ru1 C114 S1 -129.5(6) . . . . ? P1 Ru1 C114 S1 95.4(5) . . . . ? C131 Ru1 C121 C122 87.3(8) . . . . ? C114 Ru1 C121 C122 -176.2(7) . . . . ? C124 Ru1 C121 C122 -79.9(8) . . . . ? C123 Ru1 C121 C122 -37.2(7) . . . . ? C125 Ru1 C121 C122 -116.7(11) . . . . ? P1 Ru1 C121 C122 -37.9(12) . . . . ? C131 Ru1 C121 C125 -156.0(7) . . . . ? C114 Ru1 C121 C125 -59.5(8) . . . . ? C122 Ru1 C121 C125 116.7(11) . . . . ? C124 Ru1 C121 C125 36.8(7) . . . . ? C123 Ru1 C121 C125 79.5(8) . . . . ? P1 Ru1 C121 C125 78.9(11) . . . . ? C125 C121 C122 C123 0.6(12) . . . . ? Ru1 C121 C122 C123 63.6(8) . . . . ? C125 C121 C122 Ru1 -63.1(7) . . . . ? C131 Ru1 C122 C123 142.4(7) . . . . ? C114 Ru1 C122 C123 -110.5(9) . . . . ? C124 Ru1 C122 C123 -37.5(6) . . . . ? C121 Ru1 C122 C123 -117.0(9) . . . . ? C125 Ru1 C122 C123 -79.5(7) . . . . ? P1 Ru1 C122 C123 46.9(7) . . . . ? C131 Ru1 C122 C121 -100.6(7) . . . . ? C114 Ru1 C122 C121 6.5(11) . . . . ? C124 Ru1 C122 C121 79.4(7) . . . . ? C123 Ru1 C122 C121 117.0(9) . . . . ? C125 Ru1 C122 C121 37.5(7) . . . . ? P1 Ru1 C122 C121 163.9(5) . . . . ? C121 C122 C123 C124 -1.6(12) . . . . ? Ru1 C122 C123 C124 62.2(7) . . . . ? C121 C122 C123 Ru1 -63.8(8) . . . . ? C131 Ru1 C123 C122 -48.5(8) . . . . ? C114 Ru1 C123 C122 123.4(7) . . . . ? C124 Ru1 C123 C122 117.5(9) . . . . ? C121 Ru1 C123 C122 37.2(6) . . . . ? C125 Ru1 C123 C122 79.2(7) . . . . ? P1 Ru1 C123 C122 -143.1(6) . . . . ? C131 Ru1 C123 C124 -166.0(7) . . . . ? C114 Ru1 C123 C124 5.9(10) . . . . ? C122 Ru1 C123 C124 -117.5(9) . . . . ? C121 Ru1 C123 C124 -80.3(7) . . . . ? C125 Ru1 C123 C124 -38.3(6) . . . . ? P1 Ru1 C123 C124 99.4(6) . . . . ? C122 C123 C124 C125 2.0(12) . . . . ? Ru1 C123 C124 C125 64.5(7) . . . . ? C122 C123 C124 Ru1 -62.5(7) . . . . ? C131 Ru1 C124 C125 -78.1(16) . . . . ? C114 Ru1 C124 C125 69.0(7) . . . . ? C122 Ru1 C124 C125 -78.1(7) . . . . ? C123 Ru1 C124 C125 -114.7(10) . . . . ? C121 Ru1 C124 C125 -36.7(7) . . . . ? P1 Ru1 C124 C125 157.8(6) . . . . ? C131 Ru1 C124 C123 36.6(17) . . . . ? C114 Ru1 C124 C123 -176.3(6) . . . . ? C122 Ru1 C124 C123 36.6(6) . . . . ? C121 Ru1 C124 C123 78.0(7) . . . . ? C125 Ru1 C124 C123 114.7(10) . . . . ? P1 Ru1 C124 C123 -87.5(6) . . . . ? C123 C124 C125 C121 -1.6(12) . . . . ? Ru1 C124 C125 C121 62.4(7) . . . . ? C123 C124 C125 Ru1 -64.1(7) . . . . ? C122 C121 C125 C124 0.7(12) . . . . ? Ru1 C121 C125 C124 -62.1(7) . . . . ? C122 C121 C125 Ru1 62.8(7) . . . . ? C131 Ru1 C125 C124 152.6(7) . . . . ? C114 Ru1 C125 C124 -115.7(7) . . . . ? C122 Ru1 C125 C124 80.7(8) . . . . ? C123 Ru1 C125 C124 38.9(7) . . . . ? C121 Ru1 C125 C124 117.9(10) . . . . ? P1 Ru1 C125 C124 -31.5(9) . . . . ? C131 Ru1 C125 C121 34.7(10) . . . . ? C114 Ru1 C125 C121 126.4(7) . . . . ? C122 Ru1 C125 C121 -37.2(7) . . . . ? C124 Ru1 C125 C121 -117.9(10) . . . . ? C123 Ru1 C125 C121 -78.9(8) . . . . ? P1 Ru1 C125 C121 -149.4(6) . . . . ? C114 Ru1 C131 O131 128(58) . . . . ? C122 Ru1 C131 O131 -84(58) . . . . ? C124 Ru1 C131 O131 -84(58) . . . . ? C123 Ru1 C131 O131 -57(58) . . . . ? C121 Ru1 C131 O131 -120(58) . . . . ? C125 Ru1 C131 O131 -141(57) . . . . ? P1 Ru1 C131 O131 42(58) . . . . ? C214 S2 C211 C212 0.1(7) . . . . ? C214 S2 C211 C215 -178.8(8) . . . . ? C215 C211 C212 C213 179.1(9) . . . . ? S2 C211 C212 C213 0.3(10) . . . . ? C215 C211 C212 C2 -6.2(16) . . . . ? S2 C211 C212 C2 175.1(7) . . . . ? C1 C2 C212 C211 91.7(13) . . . . ? C3 C2 C212 C211 -87.2(11) . . . . ? C1 C2 C212 C213 -94.3(13) . . . . ? C3 C2 C212 C213 86.9(12) . . . . ? C211 C212 C213 C214 -0.8(12) . . . . ? C2 C212 C213 C214 -175.3(9) . . . . ? C212 C213 C214 S2 0.8(10) . . . . ? C212 C213 C214 Ru2 175.5(7) . . . . ? C211 S2 C214 C213 -0.5(7) . . . . ? C211 S2 C214 Ru2 -175.8(5) . . . . ? C231 Ru2 C214 C213 31.9(9) . . . . ? C224 Ru2 C214 C213 -64.5(11) . . . . ? C225 Ru2 C214 C213 -73.5(9) . . . . ? C222 Ru2 C214 C213 -137.1(9) . . . . ? C223 Ru2 C214 C213 -125.8(9) . . . . ? C221 Ru2 C214 C213 -108.8(9) . . . . ? P2 Ru2 C214 C213 122.8(9) . . . . ? C231 Ru2 C214 S2 -154.1(6) . . . . ? C224 Ru2 C214 S2 109.4(6) . . . . ? C225 Ru2 C214 S2 100.5(6) . . . . ? C222 Ru2 C214 S2 36.9(6) . . . . ? C223 Ru2 C214 S2 48.2(9) . . . . ? C221 Ru2 C214 S2 65.2(5) . . . . ? P2 Ru2 C214 S2 -63.2(5) . . . . ? C231 Ru2 C221 C222 144.1(7) . . . . ? C214 Ru2 C221 C222 -132.0(6) . . . . ? C224 Ru2 C221 C222 80.7(7) . . . . ? C225 Ru2 C221 C222 118.5(9) . . . . ? C223 Ru2 C221 C222 37.8(6) . . . . ? P2 Ru2 C221 C222 -38.9(7) . . . . ? C231 Ru2 C221 C225 25.7(9) . . . . ? C214 Ru2 C221 C225 109.6(7) . . . . ? C224 Ru2 C221 C225 -37.8(6) . . . . ? C222 Ru2 C221 C225 -118.5(9) . . . . ? C223 Ru2 C221 C225 -80.6(7) . . . . ? P2 Ru2 C221 C225 -157.3(5) . . . . ? C225 C221 C222 C223 -2.1(11) . . . . ? Ru2 C221 C222 C223 -63.6(7) . . . . ? C225 C221 C222 Ru2 61.5(7) . . . . ? C231 Ru2 C222 C221 -95.6(12) . . . . ? C214 Ru2 C222 C221 53.9(7) . . . . ? C224 Ru2 C222 C221 -78.9(7) . . . . ? C225 Ru2 C222 C221 -37.0(6) . . . . ? C223 Ru2 C222 C221 -116.3(9) . . . . ? P2 Ru2 C222 C221 150.2(6) . . . . ? C231 Ru2 C222 C223 20.6(14) . . . . ? C214 Ru2 C222 C223 170.1(6) . . . . ? C224 Ru2 C222 C223 37.3(6) . . . . ? C225 Ru2 C222 C223 79.3(7) . . . . ? C221 Ru2 C222 C223 116.3(9) . . . . ? P2 Ru2 C222 C223 -93.5(6) . . . . ? C221 C222 C223 C224 2.5(11) . . . . ? Ru2 C222 C223 C224 -61.3(6) . . . . ? C221 C222 C223 Ru2 63.8(7) . . . . ? C231 Ru2 C223 C222 -171.0(6) . . . . ? C214 Ru2 C223 C222 -17.6(10) . . . . ? C224 Ru2 C223 C222 -117.8(9) . . . . ? C225 Ru2 C223 C222 -79.9(7) . . . . ? C221 Ru2 C223 C222 -37.4(6) . . . . ? P2 Ru2 C223 C222 92.1(6) . . . . ? C231 Ru2 C223 C224 -53.2(8) . . . . ? C214 Ru2 C223 C224 100.2(9) . . . . ? C225 Ru2 C223 C224 37.9(6) . . . . ? C222 Ru2 C223 C224 117.8(9) . . . . ? C221 Ru2 C223 C224 80.4(7) . . . . ? P2 Ru2 C223 C224 -150.1(6) . . . . ? C222 C223 C224 C225 -2.0(11) . . . . ? Ru2 C223 C224 C225 -64.1(6) . . . . ? C222 C223 C224 Ru2 62.0(7) . . . . ? C231 Ru2 C224 C225 -107.0(7) . . . . ? C214 Ru2 C224 C225 -14.8(9) . . . . ? C222 Ru2 C224 C225 79.2(7) . . . . ? C223 Ru2 C224 C225 115.9(9) . . . . ? C221 Ru2 C224 C225 38.0(6) . . . . ? P2 Ru2 C224 C225 155.6(5) . . . . ? C231 Ru2 C224 C223 137.1(7) . . . . ? C214 Ru2 C224 C223 -130.6(7) . . . . ? C225 Ru2 C224 C223 -115.9(9) . . . . ? C222 Ru2 C224 C223 -36.6(6) . . . . ? C221 Ru2 C224 C223 -77.8(7) . . . . ? P2 Ru2 C224 C223 39.8(8) . . . . ? C223 C224 C225 C221 0.8(10) . . . . ? Ru2 C224 C225 C221 -63.5(7) . . . . ? C223 C224 C225 Ru2 64.2(6) . . . . ? C222 C221 C225 C224 0.8(11) . . . . ? Ru2 C221 C225 C224 62.8(7) . . . . ? C222 C221 C225 Ru2 -62.0(7) . . . . ? C231 Ru2 C225 C224 80.5(7) . . . . ? C214 Ru2 C225 C224 169.8(6) . . . . ? C222 Ru2 C225 C224 -80.1(7) . . . . ? C223 Ru2 C225 C224 -38.3(6) . . . . ? C221 Ru2 C225 C224 -116.1(9) . . . . ? P2 Ru2 C225 C224 -60.3(12) . . . . ? C231 Ru2 C225 C221 -163.4(6) . . . . ? C214 Ru2 C225 C221 -74.0(7) . . . . ? C224 Ru2 C225 C221 116.1(9) . . . . ? C222 Ru2 C225 C221 36.1(6) . . . . ? C223 Ru2 C225 C221 77.8(7) . . . . ? P2 Ru2 C225 C221 55.8(12) . . . . ? C214 Ru2 C231 O231 -162(26) . . . . ? C224 Ru2 C231 O231 -25(26) . . . . ? C225 Ru2 C231 O231 -61(26) . . . . ? C222 Ru2 C231 O231 -10(26) . . . . ? C223 Ru2 C231 O231 4(26) . . . . ? C221 Ru2 C231 O231 -77(26) . . . . ? P2 Ru2 C231 O231 105(26) . . . . ? C331 P1 C311 C312 -47.0(8) . . . . ? C321 P1 C311 C312 60.4(8) . . . . ? Ru1 P1 C311 C312 -173.9(6) . . . . ? P1 C311 C312 P2 -160.5(5) . . . . ? C341 P2 C312 C311 64.4(7) . . . . ? C351 P2 C312 C311 169.5(7) . . . . ? Ru2 P2 C312 C311 -65.2(7) . . . . ? C331 P1 C321 C326 -135.1(8) . . . . ? C311 P1 C321 C326 114.9(8) . . . . ? Ru1 P1 C321 C326 -7.6(9) . . . . ? C331 P1 C321 C322 43.8(9) . . . . ? C311 P1 C321 C322 -66.1(8) . . . . ? Ru1 P1 C321 C322 171.4(7) . . . . ? C326 C321 C322 C323 -4.6(14) . . . . ? P1 C321 C322 C323 176.4(8) . . . . ? C321 C322 C323 C324 3.3(16) . . . . ? C322 C323 C324 C325 0.3(18) . . . . ? C323 C324 C325 C326 -2.3(18) . . . . ? C322 C321 C326 C325 2.5(15) . . . . ? P1 C321 C326 C325 -178.5(9) . . . . ? C324 C325 C326 C321 0.9(17) . . . . ? C321 P1 C331 C332 42.4(9) . . . . ? C311 P1 C331 C332 151.4(8) . . . . ? Ru1 P1 C331 C332 -84.9(8) . . . . ? C321 P1 C331 C336 -147.1(8) . . . . ? C311 P1 C331 C336 -38.2(9) . . . . ? Ru1 P1 C331 C336 85.5(8) . . . . ? C336 C331 C332 C333 1.2(16) . . . . ? P1 C331 C332 C333 172.0(9) . . . . ? C331 C332 C333 C334 -1.5(19) . . . . ? C332 C333 C334 C335 2.8(19) . . . . ? C333 C334 C335 C336 -3.9(18) . . . . ? C334 C335 C336 C331 3.7(17) . . . . ? C332 C331 C336 C335 -2.3(15) . . . . ? P1 C331 C336 C335 -173.0(8) . . . . ? C351 P2 C341 C342 122.1(9) . . . . ? C312 P2 C341 C342 -132.6(9) . . . . ? Ru2 P2 C341 C342 -1.6(10) . . . . ? C351 P2 C341 C346 -62.4(9) . . . . ? C312 P2 C341 C346 42.9(9) . . . . ? Ru2 P2 C341 C346 173.8(7) . . . . ? C346 C341 C342 C343 0.3(18) . . . . ? P2 C341 C342 C343 175.8(10) . . . . ? C341 C342 C343 C344 0(2) . . . . ? C342 C343 C344 C345 0(2) . . . . ? C343 C344 C345 C346 1(3) . . . . ? C344 C345 C346 C341 -1(2) . . . . ? C342 C341 C346 C345 0.4(17) . . . . ? P2 C341 C346 C345 -175.2(10) . . . . ? C341 P2 C351 C356 -39.2(8) . . . . ? C312 P2 C351 C356 -143.8(7) . . . . ? Ru2 P2 C351 C356 87.0(7) . . . . ? C341 P2 C351 C352 146.1(8) . . . . ? C312 P2 C351 C352 41.6(8) . . . . ? Ru2 P2 C351 C352 -87.6(8) . . . . ? C356 C351 C352 C353 0.5(14) . . . . ? P2 C351 C352 C353 175.1(8) . . . . ? C351 C352 C353 C354 0.9(16) . . . . ? C352 C353 C354 C355 -1.5(17) . . . . ? C353 C354 C355 C356 0.8(18) . . . . ? C352 C351 C356 C355 -1.2(14) . . . . ? P2 C351 C356 C355 -176.0(8) . . . . ? C354 C355 C356 C351 0.5(17) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.139 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.155 #===END