Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'George Britovsek' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Technology & Medicine Building RCS1, room 314 Frankland Road South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email G.BRITOVSEK@IMPERIAL.AC.UK _publ_section_title ; Iron(II), Manganese(II) and Cobalt(II) Complexes Containing Tetradentate Biphenyl-Bridged Ligands and their Application in Alkane Oxidation Catalysis ; loop_ _publ_author_name 'George Britovsek' 'Jason England' 'Andrew J. P. White' data_Compound_Fe(1)OTf2 _database_code_depnum_ccdc_archive 'CCDC 270626' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H22 F6 Fe N4 O6 S2' _chemical_formula_weight 744.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.7167(13) _cell_length_b 11.4815(8) _cell_length_c 16.6129(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.470(5) _cell_angle_gamma 90.00 _cell_volume 3174.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.15 _cell_measurement_theta_max 12.48 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method ? _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.5989 _exptl_absorpt_correction_T_max 0.6520 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.29 _diffrn_reflns_number 2887 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2787 _reflns_number_observed 2119 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 188 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.3697P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2599 _refine_ls_number_parameters 242 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_all 0.1121 _refine_ls_wR_factor_obs 0.0993 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.0000 0.26725(5) 0.2500 0.0357(2) Uani 1 d S . N1 N 0.09590(14) 0.2475(2) 0.16917(15) 0.0412(6) Uani 1 d . . C2 C 0.1041(2) 0.1623(3) 0.1170(2) 0.0550(8) Uani 1 d . . H2A H 0.0604(2) 0.1138(3) 0.1031(2) 0.066 Uiso 1 calc R . C3 C 0.1753(3) 0.1423(4) 0.0821(3) 0.0698(11) Uani 1 d . . H3A H 0.1787(3) 0.0825(4) 0.0447(3) 0.084 Uiso 1 calc R . C4 C 0.2399(2) 0.2116(4) 0.1036(3) 0.0679(11) Uani 1 d . . H4A H 0.2885(2) 0.1984(4) 0.0822(3) 0.081 Uiso 1 calc R . C5 C 0.2325(2) 0.3014(3) 0.1573(3) 0.0560(9) Uani 1 d . . H5A H 0.2756(2) 0.3505(3) 0.1720(3) 0.067 Uiso 1 calc R . C6 C 0.1600(2) 0.3171(3) 0.1890(2) 0.0410(6) Uani 1 d . . C7 C 0.1465(2) 0.4117(3) 0.2451(2) 0.0420(7) Uani 1 d . . H7A H 0.1849(2) 0.4697(3) 0.2558(2) 0.050 Uiso 1 calc R . N7 N 0.08199(14) 0.4134(2) 0.2789(2) 0.0376(5) Uani 1 d . . C8 C 0.0625(2) 0.5089(3) 0.3290(2) 0.0377(6) Uani 1 d . . C9 C 0.0125(2) 0.5973(3) 0.2946(2) 0.0410(6) Uani 1 d . . C10 C -0.0133(2) 0.6845(3) 0.3460(2) 0.0506(8) Uani 1 d . . C11 C 0.0138(2) 0.6814(3) 0.4277(2) 0.0579(9) Uani 1 d . . H11A H -0.0023(2) 0.7395(3) 0.4616(2) 0.069 Uiso 1 calc R . C12 C 0.0638(2) 0.5951(4) 0.4595(2) 0.0587(9) Uani 1 d . . H12A H 0.0816(2) 0.5961(4) 0.5142(2) 0.070 Uiso 1 calc R . C13 C 0.0881(2) 0.5064(3) 0.4110(2) 0.0503(8) Uani 1 d . . H13A H 0.1207(2) 0.4464(3) 0.4328(2) 0.060 Uiso 1 calc R . C14 C -0.0712(3) 0.7788(4) 0.3156(3) 0.0733(11) Uani 1 d . . H14A H -0.0943(17) 0.7596(17) 0.2621(10) 0.110 Uiso 1 calc R . H14B H -0.0430(5) 0.8516(8) 0.3142(22) 0.110 Uiso 1 calc R . H14C H -0.1130(13) 0.7855(23) 0.3511(13) 0.110 Uiso 1 calc R . O1 O 0.0649(2) 0.1543(3) 0.3312(2) 0.0645(7) Uani 1 d D . S S 0.12734(6) 0.06707(8) 0.34587(7) 0.0493(3) Uani 0.90 d PDU 1 O2 O 0.1722(2) 0.0452(3) 0.2792(2) 0.0808(11) Uani 0.90 d PDU 1 O3 O 0.1035(4) -0.0305(4) 0.3916(4) 0.093(2) Uani 0.90 d PDU 1 C15 C 0.1969(3) 0.1428(5) 0.4183(3) 0.0723(13) Uani 0.90 d PDU 1 F1 F 0.2599(3) 0.0779(5) 0.4405(4) 0.121(2) Uani 0.90 d PDU 1 F2 F 0.1641(3) 0.1713(5) 0.4832(2) 0.129(2) Uani 0.90 d PDU 1 F3 F 0.2232(3) 0.2397(4) 0.3839(3) 0.1112(15) Uani 0.90 d PDU 1 S' S 0.1056(8) 0.0761(12) 0.3874(9) 0.084(3) Uiso 0.10 d PDU 2 O2' O 0.0926(21) 0.1019(32) 0.4722(12) 0.119(12) Uiso 0.10 d PDU 2 O3' O 0.1066(24) -0.0431(16) 0.3710(22) 0.052(8) Uiso 0.10 d PDU 2 C15' C 0.2094(12) 0.1238(28) 0.3887(18) 0.086(11) Uiso 0.10 d PDU 2 F1' F 0.2554(18) 0.0549(46) 0.4363(30) 0.127(11) Uiso 0.10 d PDU 2 F2' F 0.2320(18) 0.1217(36) 0.3155(19) 0.130(10) Uiso 0.10 d PDU 2 F3' F 0.2128(24) 0.2309(33) 0.4187(27) 0.125(11) Uiso 0.10 d PDU 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0277(3) 0.0316(3) 0.0476(3) 0.000 0.0026(2) 0.000 N1 0.0376(12) 0.0430(14) 0.0431(13) -0.0017(11) 0.0041(10) 0.0002(10) C2 0.061(2) 0.051(2) 0.053(2) -0.015(2) 0.005(2) -0.002(2) C3 0.079(3) 0.066(2) 0.068(3) -0.019(2) 0.024(2) 0.008(2) C4 0.062(2) 0.072(3) 0.074(3) -0.002(2) 0.034(2) 0.013(2) C5 0.045(2) 0.055(2) 0.071(2) 0.001(2) 0.021(2) -0.0043(14) C6 0.0381(15) 0.0398(15) 0.046(2) 0.0060(13) 0.0075(12) 0.0014(12) C7 0.0353(14) 0.0365(15) 0.054(2) -0.0007(13) 0.0022(12) -0.0074(12) N7 0.0346(12) 0.0340(12) 0.0437(13) -0.0014(10) 0.0013(10) -0.0001(9) C8 0.0352(14) 0.0347(14) 0.044(2) -0.0016(12) 0.0056(11) -0.0045(11) C9 0.0451(15) 0.0333(14) 0.045(2) -0.0008(13) 0.0069(12) -0.0018(12) C10 0.053(2) 0.040(2) 0.059(2) -0.0081(15) 0.009(2) 0.0011(14) C11 0.067(2) 0.056(2) 0.052(2) -0.017(2) 0.013(2) -0.002(2) C12 0.067(2) 0.067(2) 0.042(2) -0.010(2) 0.006(2) -0.012(2) C13 0.054(2) 0.047(2) 0.048(2) -0.0006(14) -0.0047(15) -0.0040(14) C14 0.076(3) 0.058(2) 0.087(3) -0.010(2) 0.010(2) 0.022(2) O1 0.0506(14) 0.071(2) 0.071(2) 0.0211(14) -0.0007(12) 0.0230(13) S 0.0461(5) 0.0454(5) 0.0545(6) 0.0085(4) -0.0051(4) 0.0102(4) O2 0.091(2) 0.086(2) 0.066(2) 0.003(2) 0.010(2) 0.044(2) O3 0.098(3) 0.062(2) 0.114(5) 0.034(3) -0.008(3) -0.007(2) C15 0.070(3) 0.066(3) 0.076(3) 0.006(3) -0.017(3) 0.001(2) F1 0.080(2) 0.123(4) 0.144(4) 0.016(3) -0.064(2) 0.019(2) F2 0.152(4) 0.161(4) 0.072(2) -0.040(3) -0.006(2) 0.006(3) F3 0.104(3) 0.091(3) 0.131(3) 0.024(2) -0.030(2) -0.036(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 Fe O1 2.097(2) . ? Fe O1 2.097(2) 2 ? Fe N7 2.190(2) . ? Fe N7 2.190(2) 2 ? Fe N1 2.199(2) 2 ? Fe N1 2.199(2) . ? N1 C2 1.322(4) . ? N1 C6 1.352(4) . ? C2 C3 1.394(6) . ? C3 C4 1.360(6) . ? C4 C5 1.377(6) . ? C5 C6 1.378(5) . ? C6 C7 1.463(4) . ? C7 N7 1.262(4) . ? N7 C8 1.432(4) . ? C8 C13 1.388(5) . ? C8 C9 1.402(4) . ? C9 C10 1.410(4) . ? C9 C9 1.501(6) 2 ? C10 C11 1.390(5) . ? C10 C14 1.507(5) . ? C11 C12 1.369(6) . ? C12 C13 1.383(5) . ? O1 S' 1.422(14) . ? O1 S 1.450(2) . ? S O2 1.418(4) . ? S O3 1.431(5) . ? S C15 1.814(5) . ? C15 F2 1.296(7) . ? C15 F1 1.314(6) . ? C15 F3 1.345(6) . ? S' O3' 1.40(2) . ? S' O2' 1.48(2) . ? S' C15' 1.82(2) . ? C15' F2' 1.31(2) . ? C15' F1' 1.31(2) . ? C15' F3' 1.33(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 103.6(2) . 2 ? O1 Fe N7 93.33(11) . . ? O1 Fe N7 152.77(11) 2 . ? O1 Fe N7 152.77(11) . 2 ? O1 Fe N7 93.33(11) 2 2 ? N7 Fe N7 80.03(13) . 2 ? O1 Fe N1 84.62(10) . 2 ? O1 Fe N1 88.07(10) 2 2 ? N7 Fe N1 114.98(10) . 2 ? N7 Fe N1 74.67(9) 2 2 ? O1 Fe N1 88.07(10) . . ? O1 Fe N1 84.62(10) 2 . ? N7 Fe N1 74.67(9) . . ? N7 Fe N1 114.98(10) 2 . ? N1 Fe N1 168.17(14) 2 . ? C2 N1 C6 117.9(3) . . ? C2 N1 Fe 127.1(2) . . ? C6 N1 Fe 113.4(2) . . ? N1 C2 C3 122.7(4) . . ? C4 C3 C2 118.8(4) . . ? C3 C4 C5 119.4(3) . . ? C4 C5 C6 118.8(4) . . ? N1 C6 C5 122.3(3) . . ? N1 C6 C7 115.3(3) . . ? C5 C6 C7 122.4(3) . . ? N7 C7 C6 119.0(3) . . ? C7 N7 C8 121.4(3) . . ? C7 N7 Fe 115.7(2) . . ? C8 N7 Fe 122.8(2) . . ? C13 C8 C9 122.0(3) . . ? C13 C8 N7 119.2(3) . . ? C9 C8 N7 118.5(3) . . ? C8 C9 C10 118.2(3) . . ? C8 C9 C9 120.1(2) . 2 ? C10 C9 C9 121.7(3) . 2 ? C11 C10 C9 118.9(3) . . ? C11 C10 C14 119.0(3) . . ? C9 C10 C14 122.1(3) . . ? C12 C11 C10 121.7(3) . . ? C11 C12 C13 120.7(3) . . ? C12 C13 C8 118.4(3) . . ? S' O1 Fe 177.5(6) . . ? S O1 Fe 148.8(2) . . ? O2 S O3 118.1(3) . . ? O2 S O1 114.6(2) . . ? O3 S O1 113.4(3) . . ? O2 S C15 104.5(3) . . ? O3 S C15 102.5(3) . . ? O1 S C15 100.7(2) . . ? F2 C15 F1 107.5(5) . . ? F2 C15 F3 109.1(5) . . ? F1 C15 F3 107.6(5) . . ? F2 C15 S 112.2(4) . . ? F1 C15 S 111.1(5) . . ? F3 C15 S 109.3(4) . . ? O3' S' O1 120.3(16) . . ? O3' S' O2' 112.8(16) . . ? O1 S' O2' 113.3(14) . . ? O3' S' C15' 105.6(15) . . ? O1 S' C15' 102.4(11) . . ? O2' S' C15' 99.0(13) . . ? F2' C15' F1' 110.2(20) . . ? F2' C15' F3' 111.2(20) . . ? F1' C15' F3' 109.2(20) . . ? F2' C15' S' 110.1(17) . . ? F1' C15' S' 109.2(19) . . ? F3' C15' S' 106.9(17) . . ? _refine_diff_density_max 0.282 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.055 #===END data_Compound_Fe(9)OTf2 _database_code_depnum_ccdc_archive 'CCDC 270627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 F6 Fe N4 O6 S2' _chemical_formula_weight 776.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2990(17) _cell_length_b 11.717(4) _cell_length_c 15.587(2) _cell_angle_alpha 94.10(3) _cell_angle_beta 102.471(18) _cell_angle_gamma 115.10(2) _cell_volume 1634.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.19 _cell_measurement_theta_max 12.52 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.67 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4186 _exptl_absorpt_correction_T_max 0.8044 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5994 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5645 _reflns_number_gt 4137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5645 _refine_ls_number_parameters 503 _refine_ls_number_restraints 426 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.172 _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 Fe Fe 0.19964(7) 0.15435(6) 1.29618(4) 0.0270(3) Uani 1 1 d . A . N1 N 0.3482(5) 0.1653(4) 1.4205(3) 0.0343(10) Uani 1 1 d . . . C2 C 0.3125(7) 0.1019(6) 1.4877(4) 0.0461(15) Uani 1 1 d . . . H2A H 0.2147 0.0372 1.4784 0.055 Uiso 1 1 calc R . . C3 C 0.4141(8) 0.1286(7) 1.5693(4) 0.0553(17) Uani 1 1 d . . . H3A H 0.3864 0.0818 1.6143 0.066 Uiso 1 1 calc R . . C4 C 0.5570(7) 0.2250(7) 1.5839(4) 0.0502(15) Uani 1 1 d . . . H4A H 0.6283 0.2444 1.6389 0.060 Uiso 1 1 calc R . . C5 C 0.5940(6) 0.2930(6) 1.5162(4) 0.0426(13) Uani 1 1 d . . . H5A H 0.6893 0.3617 1.5254 0.051 Uiso 1 1 calc R . . C6 C 0.4886(6) 0.2579(5) 1.4355(3) 0.0318(11) Uani 1 1 d . . . C7 C 0.5270(5) 0.3157(5) 1.3549(3) 0.0329(11) Uani 1 1 d . . . H7A H 0.6193 0.3962 1.3751 0.039 Uiso 1 1 calc R . . H7B H 0.5446 0.2568 1.3165 0.039 Uiso 1 1 calc R . . N8 N 0.4071(4) 0.3409(4) 1.3025(3) 0.0275(9) Uani 1 1 d . . . C9 C 0.4163(5) 0.3547(4) 1.2105(3) 0.0261(10) Uani 1 1 d . . . C10 C 0.5388(5) 0.3564(5) 1.1845(4) 0.0337(11) Uani 1 1 d . . . H10A H 0.6196 0.3578 1.2272 0.040 Uiso 1 1 calc R . . C11 C 0.5412(6) 0.3560(5) 1.0955(4) 0.0378(12) Uani 1 1 d . . . H11A H 0.6242 0.3577 1.0786 0.045 Uiso 1 1 calc R . . C12 C 0.4240(6) 0.3532(5) 1.0321(4) 0.0363(12) Uani 1 1 d . . . H12A H 0.4247 0.3482 0.9717 0.044 Uiso 1 1 calc R . . C13 C 0.3037(6) 0.3579(5) 1.0571(4) 0.0355(12) Uani 1 1 d . . . C14 C 0.2987(5) 0.3594(5) 1.1470(3) 0.0298(11) Uani 1 1 d . . . C15 C 0.1753(5) 0.3821(5) 1.1689(3) 0.0316(11) Uani 1 1 d . . . C16 C 0.1945(6) 0.5089(5) 1.1729(4) 0.0354(12) Uani 1 1 d . . . C17 C 0.0815(6) 0.5394(5) 1.1839(4) 0.0425(14) Uani 1 1 d . . . H17A H 0.0957 0.6245 1.1881 0.051 Uiso 1 1 calc R . . C18 C -0.0517(6) 0.4426(6) 1.1887(4) 0.0466(15) Uani 1 1 d . . . H18A H -0.1291 0.4624 1.1948 0.056 Uiso 1 1 calc R . . C19 C -0.0737(6) 0.3171(5) 1.1846(4) 0.0398(13) Uani 1 1 d . . . H19A H -0.1656 0.2526 1.1872 0.048 Uiso 1 1 calc R . . C20 C 0.0405(5) 0.2862(5) 1.1765(3) 0.0310(11) Uani 1 1 d . . . N21 N 0.0217(4) 0.1542(4) 1.1798(3) 0.0286(9) Uani 1 1 d . . . C22 C -0.1181(5) 0.0718(5) 1.2022(4) 0.0342(12) Uani 1 1 d . . . H22A H -0.2032 0.0474 1.1498 0.041 Uiso 1 1 calc R . . H22B H -0.1313 0.1204 1.2506 0.041 Uiso 1 1 calc R . . C23 C -0.1149(6) -0.0465(5) 1.2304(4) 0.0336(11) Uani 1 1 d . . . C24 C -0.2427(7) -0.1624(6) 1.2128(4) 0.0479(15) Uani 1 1 d . . . H24A H -0.3347 -0.1701 1.1794 0.058 Uiso 1 1 calc R . . C25 C -0.2331(7) -0.2668(6) 1.2450(5) 0.0505(16) Uani 1 1 d . . . H25A H -0.3192 -0.3454 1.2346 0.061 Uiso 1 1 calc R . . C26 C -0.0978(7) -0.2549(5) 1.2921(4) 0.0430(14) Uani 1 1 d . . . H26A H -0.0890 -0.3253 1.3131 0.052 Uiso 1 1 calc R . . C27 C 0.0254(7) -0.1367(5) 1.3081(4) 0.0396(13) Uani 1 1 d . . . H27A H 0.1182 -0.1278 1.3409 0.047 Uiso 1 1 calc R . . N28 N 0.0180(5) -0.0341(4) 1.2786(3) 0.0344(10) Uani 1 1 d . . . C29 C 0.4138(6) 0.4571(5) 1.3539(3) 0.0323(11) Uani 1 1 d . . . H29A H 0.5042 0.5319 1.3541 0.048 Uiso 1 1 calc R . . H29B H 0.4138 0.4456 1.4149 0.048 Uiso 1 1 calc R . . H29C H 0.3278 0.4691 1.3261 0.048 Uiso 1 1 calc R . . C30 C 0.1796(7) 0.3608(6) 0.9857(4) 0.0469(15) Uani 1 1 d . . . H30A H 0.0847 0.2925 0.9868 0.070 Uiso 1 1 calc R . . H30B H 0.1960 0.3488 0.9275 0.070 Uiso 1 1 calc R . . H30C H 0.1786 0.4428 0.9972 0.070 Uiso 1 1 calc R . . C31 C 0.3388(6) 0.6174(5) 1.1669(5) 0.0443(14) Uani 1 1 d . . . H31A H 0.3525 0.6031 1.1081 0.066 Uiso 1 1 calc R . . H31B H 0.4218 0.6202 1.2121 0.066 Uiso 1 1 calc R . . H31C H 0.3343 0.6982 1.1766 0.066 Uiso 1 1 calc R . . C32 C 0.0179(6) 0.0913(5) 1.0921(3) 0.0349(12) Uani 1 1 d . . . H32A H -0.0592 0.0942 1.0452 0.052 Uiso 1 1 calc R . . H32B H -0.0033 0.0027 1.0940 0.052 Uiso 1 1 calc R . . H32C H 0.1138 0.1361 1.0800 0.052 Uiso 1 1 calc R . . S1A S 0.2949(2) -0.04417(15) 1.18874(11) 0.0317(5) Uani 0.800(5) 1 d PD A 1 O1A O 0.2941(4) 0.0755(3) 1.2134(2) 0.0364(9) Uani 1 1 d D . . O1B O 0.3748(10) -0.0800(8) 1.2607(4) 0.066(2) Uani 0.800(5) 1 d PD A 1 O1C O 0.1581(5) -0.1419(5) 1.1316(4) 0.0559(16) Uani 0.800(5) 1 d PD A 1 C1A C 0.4172(8) -0.0018(7) 1.1148(5) 0.050(2) Uani 0.800(5) 1 d PD A 1 F1A F 0.4309(11) -0.1042(9) 1.0832(7) 0.094(5) Uani 0.800(5) 1 d PD A 1 F1B F 0.3639(12) 0.0414(10) 1.0462(5) 0.083(6) Uani 0.800(5) 1 d PD A 1 F1C F 0.5522(5) 0.0898(5) 1.1586(5) 0.083(2) Uani 0.800(5) 1 d PD A 1 S1A' S 0.3884(9) 0.0001(7) 1.2146(5) 0.040(2) Uiso 0.200(5) 1 d PD A 2 O1B' O 0.324(2) -0.1125(15) 1.2517(14) 0.035(7) Uiso 0.200(5) 1 d PD A 2 O1C' O 0.5438(12) 0.0787(17) 1.2416(13) 0.061(6) Uiso 0.200(5) 1 d PD A 2 C1A' C 0.3477(19) -0.0588(16) 1.0978(9) 0.050(9) Uiso 0.200(5) 1 d PD A 2 F1A' F 0.441(3) -0.107(3) 1.0828(15) 0.053(11) Uiso 0.200(5) 1 d PD A 2 F1B' F 0.362(3) 0.033(2) 1.0488(13) 0.053(15) Uiso 0.200(5) 1 d PD A 2 F1C' F 0.2093(18) -0.1542(17) 1.0653(11) 0.075(7) Uiso 0.200(5) 1 d PD A 2 S2A S 0.08961(17) 0.26220(17) 1.45927(10) 0.0405(6) Uani 0.901(6) 1 d PD A 1 O2A O 0.1098(4) 0.2476(4) 1.3691(2) 0.0391(9) Uani 1 1 d D . . O2B O 0.0263(8) 0.1428(5) 1.4892(4) 0.086(2) Uani 0.901(6) 1 d PD A 1 O2C O 0.2114(7) 0.3695(7) 1.5200(4) 0.080(3) Uani 0.901(6) 1 d PD A 1 C2A C -0.0587(10) 0.3089(11) 1.4402(6) 0.109(5) Uani 0.901(6) 1 d PDU A 1 F2A F -0.0891(9) 0.3269(10) 1.5184(5) 0.134(4) Uani 0.901(6) 1 d PDU A 1 F2B F -0.0178(12) 0.4185(9) 1.4100(5) 0.153(4) Uani 0.901(6) 1 d PDU A 1 F2C F -0.1816(6) 0.2182(11) 1.3830(5) 0.139(4) Uani 0.901(6) 1 d PDU A 1 S2A' S 0.1038(18) 0.3335(16) 1.4376(11) 0.068(7) Uiso 0.099(6) 1 d PD A 2 O2B' O 0.119(4) 0.4552(18) 1.415(3) 0.18(5) Uiso 0.099(6) 1 d PD A 2 O2C' O 0.185(3) 0.340(4) 1.5274(11) 0.039(15) Uiso 0.099(6) 1 d PD A 2 C2A' C -0.089(2) 0.254(2) 1.4396(15) 0.016(10) Uiso 0.099(6) 1 d PD A 2 F2A' F -0.104(3) 0.276(3) 1.5209(17) 0.026(8) Uiso 0.099(6) 1 d PD A 2 F2B' F -0.146(4) 0.127(2) 1.414(3) 0.13(3) Uiso 0.099(6) 1 d PD A 2 F2C' F -0.170(3) 0.295(5) 1.383(2) 0.082(19) Uiso 0.099(6) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0228(4) 0.0242(4) 0.0252(4) 0.0024(3) 0.0044(3) 0.0039(3) N1 0.035(2) 0.031(2) 0.030(2) 0.0080(18) 0.0062(18) 0.0087(19) C2 0.053(4) 0.040(3) 0.035(3) 0.012(2) 0.013(3) 0.010(3) C3 0.071(5) 0.056(4) 0.038(3) 0.019(3) 0.012(3) 0.028(4) C4 0.053(4) 0.063(4) 0.034(3) 0.007(3) -0.003(3) 0.032(3) C5 0.035(3) 0.049(3) 0.033(3) 0.001(2) -0.003(2) 0.016(3) C6 0.029(3) 0.034(3) 0.025(2) 0.002(2) -0.002(2) 0.012(2) C7 0.023(2) 0.039(3) 0.030(3) 0.004(2) 0.004(2) 0.009(2) N8 0.023(2) 0.023(2) 0.028(2) -0.0018(16) 0.0062(16) 0.0046(16) C9 0.028(2) 0.014(2) 0.029(2) 0.0052(18) 0.0106(19) 0.0016(18) C10 0.022(2) 0.029(3) 0.041(3) 0.007(2) 0.007(2) 0.004(2) C11 0.032(3) 0.036(3) 0.045(3) 0.010(2) 0.020(2) 0.010(2) C12 0.039(3) 0.033(3) 0.038(3) 0.010(2) 0.021(2) 0.011(2) C13 0.033(3) 0.031(3) 0.036(3) 0.011(2) 0.009(2) 0.008(2) C14 0.026(2) 0.024(2) 0.032(3) 0.004(2) 0.009(2) 0.004(2) C15 0.026(2) 0.034(3) 0.025(2) 0.006(2) 0.0030(19) 0.006(2) C16 0.032(3) 0.025(3) 0.043(3) 0.011(2) 0.009(2) 0.007(2) C17 0.037(3) 0.029(3) 0.057(4) 0.015(3) 0.009(3) 0.013(2) C18 0.030(3) 0.051(4) 0.064(4) 0.015(3) 0.013(3) 0.022(3) C19 0.021(2) 0.035(3) 0.054(3) 0.007(3) 0.006(2) 0.006(2) C20 0.026(2) 0.027(3) 0.028(2) 0.003(2) 0.002(2) 0.004(2) N21 0.022(2) 0.027(2) 0.029(2) 0.0023(17) 0.0055(16) 0.0048(17) C22 0.024(2) 0.029(3) 0.036(3) 0.000(2) 0.005(2) 0.002(2) C23 0.030(3) 0.028(3) 0.034(3) 0.002(2) 0.013(2) 0.004(2) C24 0.032(3) 0.040(3) 0.053(4) 0.006(3) 0.007(3) 0.002(3) C25 0.044(3) 0.029(3) 0.062(4) 0.008(3) 0.017(3) 0.000(3) C26 0.058(4) 0.024(3) 0.038(3) 0.009(2) 0.019(3) 0.008(3) C27 0.047(3) 0.029(3) 0.031(3) 0.004(2) 0.010(2) 0.008(2) N28 0.030(2) 0.029(2) 0.035(2) 0.0085(18) 0.0109(19) 0.0041(18) C29 0.028(3) 0.028(3) 0.034(3) -0.001(2) 0.005(2) 0.010(2) C30 0.045(3) 0.054(4) 0.035(3) 0.016(3) 0.008(3) 0.015(3) C31 0.036(3) 0.028(3) 0.067(4) 0.015(3) 0.018(3) 0.010(2) C32 0.029(3) 0.030(3) 0.031(3) 0.000(2) 0.003(2) 0.005(2) S1A 0.0347(11) 0.0259(9) 0.0319(9) 0.0051(6) 0.0093(7) 0.0114(8) O1A 0.035(2) 0.0307(19) 0.041(2) 0.0059(16) 0.0161(17) 0.0099(16) O1B 0.089(7) 0.071(5) 0.053(4) 0.025(4) 0.010(4) 0.051(5) O1C 0.041(3) 0.036(3) 0.064(4) -0.011(3) 0.013(3) -0.003(2) C1A 0.044(5) 0.048(5) 0.055(5) 0.003(4) 0.023(4) 0.015(4) F1A 0.119(8) 0.063(5) 0.136(9) 0.017(4) 0.097(7) 0.045(4) F1B 0.113(9) 0.086(7) 0.056(5) 0.036(4) 0.045(4) 0.036(5) F1C 0.035(3) 0.054(3) 0.158(6) 0.015(3) 0.038(3) 0.014(2) S2A 0.0361(9) 0.0439(11) 0.0349(9) 0.0022(7) 0.0163(7) 0.0096(7) O2A 0.0321(19) 0.046(2) 0.032(2) 0.0007(16) 0.0130(16) 0.0096(17) O2B 0.127(6) 0.058(4) 0.079(4) 0.030(3) 0.067(4) 0.025(4) O2C 0.049(3) 0.091(5) 0.046(3) -0.023(3) 0.017(3) -0.014(3) C2A 0.073(7) 0.150(12) 0.098(8) -0.026(8) 0.039(6) 0.046(8) F2A 0.130(6) 0.236(10) 0.096(5) 0.007(6) 0.055(4) 0.130(7) F2B 0.240(10) 0.180(8) 0.120(6) 0.033(6) 0.053(6) 0.167(8) F2C 0.056(4) 0.254(11) 0.100(5) -0.024(6) 0.010(3) 0.077(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2A 2.116(4) . ? Fe O1A 2.144(4) . ? Fe N1 2.151(4) . ? Fe N28 2.153(4) . ? Fe N21 2.282(4) . ? Fe N8 2.295(4) . ? N1 C6 1.345(7) . ? N1 C2 1.352(7) . ? C2 C3 1.380(9) . ? C3 C4 1.379(10) . ? C4 C5 1.390(9) . ? C5 C6 1.374(7) . ? C6 C7 1.518(7) . ? C7 N8 1.480(6) . ? N8 C9 1.473(6) . ? N8 C29 1.498(6) . ? C9 C10 1.398(7) . ? C9 C14 1.413(7) . ? C10 C11 1.393(8) . ? C11 C12 1.371(8) . ? C12 C13 1.398(8) . ? C13 C14 1.412(7) . ? C13 C30 1.517(8) . ? C14 C15 1.504(7) . ? C15 C20 1.404(7) . ? C15 C16 1.407(7) . ? C16 C17 1.394(8) . ? C16 C31 1.520(7) . ? C17 C18 1.382(8) . ? C18 C19 1.384(8) . ? C19 C20 1.395(8) . ? C20 N21 1.482(6) . ? N21 C22 1.487(6) . ? N21 C32 1.491(6) . ? C22 C23 1.495(8) . ? C23 N28 1.353(7) . ? C23 C24 1.388(8) . ? C24 C25 1.389(9) . ? C25 C26 1.371(9) . ? C26 C27 1.384(8) . ? C27 N28 1.343(7) . ? S1A O1C 1.425(5) . ? S1A O1A 1.432(4) . ? S1A O1B 1.440(6) . ? S1A C1A 1.829(7) . ? O1A S1A' 1.565(7) . ? C1A F1B 1.327(9) . ? C1A F1C 1.331(8) . ? C1A F1A 1.338(9) . ? S1A' O1C' 1.411(12) . ? S1A' O1B' 1.430(11) . ? S1A' C1A' 1.793(13) . ? C1A' F1B' 1.337(14) . ? C1A' F1C' 1.339(13) . ? C1A' F1A' 1.353(13) . ? S2A O2C 1.424(6) . ? S2A O2B 1.432(5) . ? S2A O2A 1.473(4) . ? S2A C2A 1.805(9) . ? O2A S2A' 1.444(12) . ? C2A F2B 1.327(11) . ? C2A F2C 1.327(10) . ? C2A F2A 1.346(9) . ? S2A' O2C' 1.446(13) . ? S2A' O2B' 1.447(14) . ? S2A' C2A' 1.809(15) . ? C2A' F2A' 1.329(14) . ? C2A' F2B' 1.335(14) . ? C2A' F2C' 1.339(14) . ? 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 O2A Fe O1A 173.75(15) . . ? O2A Fe N1 88.50(16) . . ? O1A Fe N1 95.30(16) . . ? O2A Fe N28 94.89(16) . . ? O1A Fe N28 89.17(16) . . ? N1 Fe N28 101.96(17) . . ? O2A Fe N21 81.51(15) . . ? O1A Fe N21 94.80(15) . . ? N1 Fe N21 169.85(16) . . ? N28 Fe N21 77.26(16) . . ? O2A Fe N8 93.54(15) . . ? O1A Fe N8 82.39(14) . . ? N1 Fe N8 78.63(16) . . ? N28 Fe N8 171.56(16) . . ? N21 Fe N8 103.66(15) . . ? C6 N1 C2 117.7(5) . . ? C6 N1 Fe 114.2(3) . . ? C2 N1 Fe 127.6(4) . . ? N1 C2 C3 122.5(6) . . ? C4 C3 C2 119.0(6) . . ? C3 C4 C5 119.0(5) . . ? C6 C5 C4 118.7(6) . . ? N1 C6 C5 123.0(5) . . ? N1 C6 C7 115.3(4) . . ? C5 C6 C7 121.5(5) . . ? N8 C7 C6 112.1(4) . . ? C9 N8 C7 112.9(4) . . ? C9 N8 C29 112.6(4) . . ? C7 N8 C29 107.2(4) . . ? C9 N8 Fe 108.3(3) . . ? C7 N8 Fe 101.3(3) . . ? C29 N8 Fe 114.0(3) . . ? C10 C9 C14 119.7(4) . . ? C10 C9 N8 119.7(4) . . ? C14 C9 N8 120.4(4) . . ? C11 C10 C9 120.1(5) . . ? C12 C11 C10 120.9(5) . . ? C11 C12 C13 120.1(5) . . ? C12 C13 C14 120.3(5) . . ? C12 C13 C30 118.6(5) . . ? C14 C13 C30 121.2(5) . . ? C13 C14 C9 118.8(5) . . ? C13 C14 C15 115.8(5) . . ? C9 C14 C15 125.0(4) . . ? C20 C15 C16 119.1(5) . . ? C20 C15 C14 125.2(5) . . ? C16 C15 C14 115.4(4) . . ? C17 C16 C15 120.8(5) . . ? C17 C16 C31 117.6(5) . . ? C15 C16 C31 121.6(5) . . ? C18 C17 C16 119.0(5) . . ? C17 C18 C19 121.4(5) . . ? C18 C19 C20 120.1(5) . . ? C19 C20 C15 119.6(5) . . ? C19 C20 N21 120.1(4) . . ? C15 C20 N21 120.3(5) . . ? C20 N21 C22 112.4(4) . . ? C20 N21 C32 110.8(4) . . ? C22 N21 C32 107.7(4) . . ? C20 N21 Fe 110.7(3) . . ? C22 N21 Fe 102.0(3) . . ? C32 N21 Fe 112.9(3) . . ? N21 C22 C23 111.3(4) . . ? N28 C23 C24 120.9(5) . . ? N28 C23 C22 116.8(4) . . ? C24 C23 C22 122.2(5) . . ? C23 C24 C25 119.2(6) . . ? C26 C25 C24 119.8(5) . . ? C25 C26 C27 118.2(6) . . ? N28 C27 C26 122.8(6) . . ? C27 N28 C23 118.9(5) . . ? C27 N28 Fe 127.1(4) . . ? C23 N28 Fe 114.0(3) . . ? O1C S1A O1A 115.1(3) . . ? O1C S1A O1B 118.0(4) . . ? O1A S1A O1B 113.6(4) . . ? O1C S1A C1A 102.9(3) . . ? O1A S1A C1A 101.3(3) . . ? O1B S1A C1A 102.9(4) . . ? S1A O1A S1A' 32.9(3) . . ? S1A O1A Fe 138.8(2) . . ? S1A' O1A Fe 142.7(3) . . ? F1B C1A F1C 107.8(7) . . ? F1B C1A F1A 108.7(7) . . ? F1C C1A F1A 108.4(7) . . ? F1B C1A S1A 111.0(6) . . ? F1C C1A S1A 110.6(5) . . ? F1A C1A S1A 110.3(6) . . ? O1C' S1A' O1B' 120.2(10) . . ? O1C' S1A' O1A 114.1(8) . . ? O1B' S1A' O1A 109.5(9) . . ? O1C' S1A' C1A' 104.4(9) . . ? O1B' S1A' C1A' 104.6(9) . . ? O1A S1A' C1A' 101.6(6) . . ? F1B' C1A' F1C' 107.7(13) . . ? F1B' C1A' F1A' 107.2(13) . . ? F1C' C1A' F1A' 106.4(13) . . ? F1B' C1A' S1A' 112.4(12) . . ? F1C' C1A' S1A' 112.0(11) . . ? F1A' C1A' S1A' 110.9(11) . . ? O2C S2A O2B 118.8(4) . . ? O2C S2A O2A 113.3(3) . . ? O2B S2A O2A 113.2(3) . . ? O2C S2A C2A 103.6(5) . . ? O2B S2A C2A 103.4(5) . . ? O2A S2A C2A 102.0(3) . . ? S2A' O2A S2A 35.5(8) . . ? S2A' O2A Fe 159.3(7) . . ? S2A O2A Fe 138.9(3) . . ? F2B C2A F2C 109.9(10) . . ? F2B C2A F2A 107.9(9) . . ? F2C C2A F2A 108.4(8) . . ? F2B C2A S2A 110.8(7) . . ? F2C C2A S2A 111.0(7) . . ? F2A C2A S2A 108.7(7) . . ? O2A S2A' O2C' 115.1(12) . . ? O2A S2A' O2B' 115.3(13) . . ? O2C' S2A' O2B' 115.3(13) . . ? O2A S2A' C2A' 102.5(9) . . ? O2C' S2A' C2A' 103.4(11) . . ? O2B' S2A' C2A' 102.6(11) . . ? F2A' C2A' F2B' 108.2(14) . . ? F2A' C2A' F2C' 108.6(14) . . ? F2B' C2A' F2C' 107.7(14) . . ? F2A' C2A' S2A' 111.7(12) . . ? F2B' C2A' S2A' 110.9(13) . . ? F2C' C2A' S2A' 109.7(13) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.680 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.121 #===END