# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bao Li' _publ_contact_author_email libao@mail.hust.edu.cn loop_ _publ_author_name 'Bao Li' 'Fan Yu' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 875827' #TrackingRef '- all-ccdc.cif' _audit_update_record ; 2012-05-31 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_formula_sum 'C31 H46 Fe N8 O8 S2' _chemical_formula_weight 778.71 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' 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 orthorhombic _symmetry_space_group_name_H-M 'C c c m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' _cell_length_a 8.9846(5) _cell_length_b 22.9562(11) _cell_length_c 24.0229(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4954.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2503 _cell_measurement_theta_min 0.856 _cell_measurement_theta_max 0.937 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8128 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 123(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 'Oxford Gemini S Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2503 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2442 _reflns_number_gt 1700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _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. ; _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^)+(0.0842P)^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 2442 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 Fe1 Fe 0.2500 0.2500 0.5000 0.0301(2) Uani 1 4 d S . . S1 S -0.17998(13) 0.37845(6) 0.5000 0.0688(4) Uani 1 2 d S . . N1 N 0.1667(2) 0.19186(8) 0.43323(8) 0.0372(5) Uani 1 1 d . . . N2 N 0.0443(3) 0.29504(12) 0.5000 0.0377(7) Uani 1 2 d S . . C1 C 0.0228(3) 0.18072(11) 0.42660(10) 0.0449(6) Uani 1 1 d . . . H1A H -0.0444 0.2009 0.4488 0.054 Uiso 1 1 calc R . . C2 C -0.0331(3) 0.14138(13) 0.38916(10) 0.0479(7) Uani 1 1 d . . . H2A H -0.1351 0.1348 0.3866 0.057 Uiso 1 1 calc R . . C3 C 0.0652(3) 0.11158(11) 0.35515(8) 0.0373(6) Uani 1 1 d . . . C4 C 0.2151(3) 0.12291(12) 0.36025(10) 0.0446(6) Uani 1 1 d . . . H4A H 0.2845 0.1038 0.3380 0.054 Uiso 1 1 calc R . . C5 C 0.2588(3) 0.16321(12) 0.39914(11) 0.0478(6) Uani 1 1 d . . . H5A H 0.3600 0.1712 0.4020 0.057 Uiso 1 1 calc R . . C6 C 0.1012(2) 0.03800(10) 0.28605(8) 0.0325(5) Uani 1 1 d . . . H6A H 0.1645 0.0140 0.3093 0.039 Uiso 1 1 calc R . . H6B H 0.1636 0.0625 0.2629 0.039 Uiso 1 1 calc R . . C7 C 0.0000 0.0000 0.2500 0.0291(9) Uani 1 4 d S . . C8 C -0.0487(4) 0.32923(15) 0.5000 0.0359(8) Uani 1 2 d S . . O1 O 0.00390(19) 0.07281(8) 0.31961(6) 0.0432(4) Uani 1 1 d . . . O1W O 0.3929(4) -0.04370(19) 0.38803(13) 0.1273(12) Uani 1 1 d . . . C9 C 0.1464(5) 0.0096(2) 0.43822(19) 0.1015(14) Uani 1 1 d . . . N3 N 0.1939(9) 0.0400(3) 0.5000 0.161(3) Uani 1 2 d S . . 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 0.0377(4) 0.0209(3) 0.0317(3) 0.000 0.000 -0.0008(3) S1 0.0480(7) 0.0701(8) 0.0885(8) 0.000 0.000 0.0245(6) N1 0.0389(12) 0.0343(10) 0.0385(10) -0.0076(8) 0.0037(9) -0.0032(9) N2 0.0408(17) 0.0279(14) 0.0445(15) 0.000 0.000 0.0047(14) C1 0.0391(15) 0.0474(15) 0.0481(14) -0.0181(11) 0.0065(11) 0.0009(12) C2 0.0319(14) 0.0573(16) 0.0545(15) -0.0257(13) 0.0025(11) -0.0029(12) C3 0.0406(14) 0.0374(13) 0.0338(12) -0.0089(10) 0.0021(10) -0.0066(11) C4 0.0367(14) 0.0515(15) 0.0457(14) -0.0197(11) 0.0050(10) -0.0015(12) C5 0.0357(14) 0.0556(16) 0.0519(14) -0.0194(12) 0.0036(12) -0.0076(13) C6 0.0349(13) 0.0343(12) 0.0284(11) -0.0045(9) 0.0037(9) -0.0002(11) C7 0.036(2) 0.026(2) 0.025(2) 0.000 0.000 0.000 C8 0.039(2) 0.0367(18) 0.0325(16) 0.000 0.000 -0.0090(17) O1 0.0370(9) 0.0484(10) 0.0441(9) -0.0222(8) 0.0033(7) -0.0036(8) O1W 0.101(2) 0.149(3) 0.132(3) 0.024(2) -0.0068(18) -0.006(2) C9 0.113(4) 0.080(3) 0.112(3) -0.009(2) -0.014(2) 0.016(3) N3 0.172(7) 0.084(4) 0.227(8) 0.000 0.000 0.004(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 Fe1 N2 2.118(3) . ? Fe1 N2 2.118(3) 13_556 ? Fe1 N1 2.2168(19) 13_556 ? Fe1 N1 2.2168(19) . ? Fe1 N1 2.2168(19) 6 ? Fe1 N1 2.2168(19) 10_556 ? S1 C8 1.634(4) . ? N1 C1 1.328(3) . ? N1 C5 1.337(3) . ? N2 C8 1.146(4) . ? C1 C2 1.370(3) . ? C1 H1A 0.9300 . ? C2 C3 1.384(3) . ? C2 H2A 0.9300 . ? C3 O1 1.351(3) . ? C3 C4 1.377(3) . ? C4 C5 1.372(3) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O1 1.433(3) . ? C6 C7 1.529(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C6 1.529(2) 3 ? C7 C6 1.529(2) 2 ? C7 C6 1.529(2) 4 ? C9 N3 1.694(6) . ? N3 C9 1.694(6) 10_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 180.000(1) . 13_556 ? N2 Fe1 N1 90.04(7) . 13_556 ? N2 Fe1 N1 89.96(8) 13_556 13_556 ? N2 Fe1 N1 89.96(8) . . ? N2 Fe1 N1 90.04(7) 13_556 . ? N1 Fe1 N1 180.00(8) 13_556 . ? N2 Fe1 N1 90.04(7) . 6 ? N2 Fe1 N1 89.96(8) 13_556 6 ? N1 Fe1 N1 92.70(10) 13_556 6 ? N1 Fe1 N1 87.30(10) . 6 ? N2 Fe1 N1 89.96(8) . 10_556 ? N2 Fe1 N1 90.04(7) 13_556 10_556 ? N1 Fe1 N1 87.30(10) 13_556 10_556 ? N1 Fe1 N1 92.70(10) . 10_556 ? N1 Fe1 N1 180.00(8) 6 10_556 ? C1 N1 C5 115.7(2) . . ? C1 N1 Fe1 122.12(15) . . ? C5 N1 Fe1 122.03(17) . . ? C8 N2 Fe1 166.0(3) . . ? N1 C1 C2 124.3(2) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? O1 C3 C4 125.4(2) . . ? O1 C3 C2 116.0(2) . . ? C4 C3 C2 118.6(2) . . ? C5 C4 C3 117.9(2) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? N1 C5 C4 124.9(2) . . ? N1 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? O1 C6 C7 105.92(15) . . ? O1 C6 H6A 110.6 . . ? C7 C6 H6A 110.6 . . ? O1 C6 H6B 110.6 . . ? C7 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? C6 C7 C6 110.43(18) . 3 ? C6 C7 C6 110.98(16) . 2 ? C6 C7 C6 107.03(16) 3 2 ? C6 C7 C6 107.03(16) . 4 ? C6 C7 C6 110.98(16) 3 4 ? C6 C7 C6 110.43(18) 2 4 ? N2 C8 S1 179.5(3) . . ? C3 O1 C6 118.32(18) . . ? C9 N3 C9 122.3(6) . 10_556 ? 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 N2 Fe1 N1 C1 -26.9(2) . . . . ? N2 Fe1 N1 C1 153.1(2) 13_556 . . . ? N1 Fe1 N1 C1 164(2) 13_556 . . . ? N1 Fe1 N1 C1 -116.9(2) 6 . . . ? N1 Fe1 N1 C1 63.1(2) 10_556 . . . ? N2 Fe1 N1 C5 157.0(2) . . . . ? N2 Fe1 N1 C5 -23.0(2) 13_556 . . . ? N1 Fe1 N1 C5 -12(2) 13_556 . . . ? N1 Fe1 N1 C5 66.99(19) 6 . . . ? N1 Fe1 N1 C5 -113.01(19) 10_556 . . . ? N2 Fe1 N2 C8 0.0 13_556 . . . ? N1 Fe1 N2 C8 46.35(5) 13_556 . . . ? N1 Fe1 N2 C8 -133.65(5) . . . . ? N1 Fe1 N2 C8 -46.35(5) 6 . . . ? N1 Fe1 N2 C8 133.65(5) 10_556 . . . ? C5 N1 C1 C2 2.1(4) . . . . ? Fe1 N1 C1 C2 -174.2(2) . . . . ? N1 C1 C2 C3 -1.0(4) . . . . ? C1 C2 C3 O1 179.1(2) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? O1 C3 C4 C5 -179.1(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C1 N1 C5 C4 -2.2(4) . . . . ? Fe1 N1 C5 C4 174.1(2) . . . . ? C3 C4 C5 N1 1.1(4) . . . . ? O1 C6 C7 C6 59.46(13) . . . 3 ? O1 C6 C7 C6 -59.07(12) . . . 2 ? O1 C6 C7 C6 -179.6(2) . . . 4 ? Fe1 N2 C8 S1 0.0 . . . . ? C4 C3 O1 C6 3.4(3) . . . . ? C2 C3 O1 C6 -175.9(2) . . . . ? C7 C6 O1 C3 -178.89(16) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.343 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.072 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.124 0.201 0.250 765.4 16.0 2 -0.124 0.201 0.750 765.4 17.1 3 0.000 0.500 0.000 8.3 -1.3 4 0.000 0.500 0.500 8.3 -1.3 5 0.500 0.000 0.000 8.3 -1.3 6 0.500 0.000 0.500 8.3 -1.3 _platon_squeeze_details ; ; #====================================================================== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 875828' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C29 H32 Fe N6 O6 S2' _chemical_formula_weight 680.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 16.5531(9) _cell_length_b 11.7181(7) _cell_length_c 17.4935(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.372(5) _cell_angle_gamma 90.00 _cell_volume 3301.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3248 _cell_measurement_theta_min 0.797 _cell_measurement_theta_max 0.881 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7428 _exptl_absorpt_correction_T_max 0.8840 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 123(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 'Oxford Gemini S Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7466 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3233 _reflns_number_gt 2745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _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. ; _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^)+(0.0507P)^2^+1.5423P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3248 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.0000 1.0000 0.5000 0.01520(11) Uani 1 2 d S . . S2 S -0.20719(5) 1.28960(6) 0.39144(3) 0.0617(2) Uani 1 1 d . . . O1 O -0.03517(7) 0.60798(10) 0.33034(7) 0.0263(3) Uani 1 1 d . . . O2 O 0.09171(8) 0.30819(11) 0.30033(8) 0.0338(3) Uani 1 1 d . . . N2 N -0.07501(8) 0.86675(11) 0.42316(7) 0.0192(3) Uani 1 1 d . . . C13 C 0.0000 0.46152(19) 0.2500 0.0174(4) Uani 1 2 d S . . N3 N -0.09214(9) 1.12405(11) 0.45887(8) 0.0213(3) Uani 1 1 d . . . N1 N 0.06405(8) 0.04937(12) 0.40679(7) 0.0199(3) Uani 1 1 d . . . C6 C -0.07064(10) 0.53528(14) 0.26542(9) 0.0199(3) Uani 1 1 d . . . H6A H -0.0948 0.5805 0.2194 0.024 Uiso 1 1 calc R . . H6B H -0.1137 0.4877 0.2781 0.024 Uiso 1 1 calc R . . C2 C -0.08179(10) 0.69677(14) 0.34560(9) 0.0204(3) Uani 1 1 d . . . C1 C -0.03966(10) 0.77354(14) 0.40131(9) 0.0202(3) Uani 1 1 d . . . H1A H 0.0159 0.7593 0.4245 0.024 Uiso 1 1 calc R . . C9 C 0.12393(11) 0.11857(16) 0.27841(10) 0.0258(4) Uani 1 1 d . . . H9A H 0.1429 0.1415 0.2347 0.031 Uiso 1 1 calc R . . C7 C 0.06230(10) 0.15946(14) 0.38611(9) 0.0192(3) Uani 1 1 d . . . H7A H 0.0407 0.2126 0.4155 0.023 Uiso 1 1 calc R . . C3 C -0.16440(10) 0.71597(15) 0.31111(10) 0.0241(4) Uani 1 1 d . . . H3A H -0.1941 0.6670 0.2729 0.029 Uiso 1 1 calc R . . C8 C 0.09151(10) 0.19702(14) 0.32245(9) 0.0203(3) Uani 1 1 d . . . C5 C -0.15612(11) 0.88385(15) 0.39089(10) 0.0233(4) Uani 1 1 d . . . H5A H -0.1823 0.9470 0.4066 0.028 Uiso 1 1 calc R . . C14 C -0.14029(11) 1.19239(15) 0.43140(9) 0.0249(4) Uani 1 1 d . . . C12 C 0.03363(11) 0.38640(14) 0.32185(10) 0.0237(4) Uani 1 1 d . . . H12A H 0.0611 0.4328 0.3662 0.028 Uiso 1 1 calc R . . H12B H -0.0113 0.3449 0.3363 0.028 Uiso 1 1 calc R . . C4 C -0.20169(11) 0.81137(15) 0.33559(10) 0.0257(4) Uani 1 1 d . . . H4A H -0.2576 0.8261 0.3145 0.031 Uiso 1 1 calc R . . C11 C 0.09724(12) -0.02543(15) 0.36536(11) 0.0282(4) Uani 1 1 d . . . H11A H 0.1003 -0.1018 0.3803 0.034 Uiso 1 1 calc R . . C10 C 0.12736(13) 0.00620(15) 0.30093(11) 0.0309(4) Uani 1 1 d . . . H10A H 0.1497 -0.0483 0.2731 0.037 Uiso 1 1 calc R . . O5 O -0.30915(11) 1.01553(15) 0.45432(10) 0.0557(4) Uani 1 1 d . . . C16 C -0.3089(2) 0.9289(3) 0.51022(18) 0.0658(8) Uani 1 1 d . . . H3 H -0.363(2) 0.965(3) 0.526(2) 0.098(11) Uiso 1 1 d . . . H2 H -0.258(2) 0.928(3) 0.558(2) 0.102(11) Uiso 1 1 d . . . H1 H -0.320(2) 0.847(3) 0.485(2) 0.117(13) 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 0.02282(18) 0.00911(17) 0.01445(16) 0.00061(11) 0.00591(12) 0.00262(12) S2 0.0778(5) 0.0627(4) 0.0379(3) 0.0054(3) -0.0006(3) 0.0504(4) O1 0.0257(6) 0.0186(6) 0.0299(6) -0.0117(5) -0.0031(5) 0.0071(5) O2 0.0351(7) 0.0214(7) 0.0542(8) 0.0211(6) 0.0295(6) 0.0137(5) N2 0.0259(7) 0.0146(7) 0.0182(6) -0.0013(5) 0.0073(5) 0.0008(6) C13 0.0210(11) 0.0103(10) 0.0212(10) 0.000 0.0052(9) 0.000 N3 0.0275(7) 0.0147(7) 0.0220(7) 0.0005(5) 0.0065(6) 0.0045(6) N1 0.0283(7) 0.0133(7) 0.0195(6) 0.0019(5) 0.0085(6) 0.0015(6) C6 0.0225(8) 0.0141(8) 0.0213(8) -0.0046(6) 0.0017(6) -0.0002(6) C2 0.0249(8) 0.0145(8) 0.0224(8) -0.0021(6) 0.0067(7) 0.0023(6) C1 0.0229(8) 0.0171(8) 0.0203(7) -0.0016(6) 0.0040(6) 0.0020(6) C9 0.0272(9) 0.0309(10) 0.0223(8) 0.0056(7) 0.0119(7) 0.0030(7) C7 0.0238(8) 0.0145(8) 0.0203(7) 0.0011(6) 0.0070(6) 0.0026(6) C3 0.0233(8) 0.0203(9) 0.0276(8) -0.0058(7) 0.0035(7) -0.0022(7) C8 0.0187(8) 0.0188(8) 0.0241(8) 0.0079(6) 0.0063(6) 0.0028(6) C5 0.0272(9) 0.0177(9) 0.0280(8) -0.0025(7) 0.0127(7) 0.0031(7) C14 0.0331(9) 0.0243(9) 0.0172(7) -0.0035(7) 0.0059(7) 0.0045(8) C12 0.0270(9) 0.0187(9) 0.0288(8) 0.0071(7) 0.0137(7) 0.0066(7) C4 0.0209(8) 0.0230(9) 0.0341(9) -0.0016(7) 0.0079(7) 0.0014(7) C11 0.0415(11) 0.0136(9) 0.0342(9) 0.0002(7) 0.0185(8) 0.0021(7) C10 0.0437(11) 0.0222(9) 0.0326(9) -0.0035(7) 0.0209(9) 0.0027(8) O5 0.0578(10) 0.0556(11) 0.0551(10) -0.0011(8) 0.0156(8) -0.0030(8) C16 0.0687(19) 0.070(2) 0.0545(16) 0.0067(15) 0.0050(15) -0.0168(16) _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 N3 2.1094(14) . ? Fe1 N3 2.1094(14) 5_576 ? Fe1 N1 2.2175(13) 5_566 ? Fe1 N1 2.2175(13) 1_565 ? Fe1 N2 2.2393(13) . ? Fe1 N2 2.2393(13) 5_576 ? S2 C14 1.6293(18) . ? O1 C2 1.3581(19) . ? O1 C6 1.4324(18) . ? O2 C8 1.359(2) . ? O2 C12 1.440(2) . ? N2 C1 1.336(2) . ? N2 C5 1.346(2) . ? C13 C6 1.527(2) . ? C13 C6 1.527(2) 2 ? C13 C12 1.530(2) 2 ? C13 C12 1.530(2) . ? N3 C14 1.153(2) . ? N1 C11 1.334(2) . ? N1 C7 1.338(2) . ? N1 Fe1 2.2175(13) 1_545 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C2 C3 1.379(2) . ? C2 C1 1.390(2) . ? C1 H1A 0.9300 . ? C9 C10 1.372(3) . ? C9 C8 1.385(2) . ? C9 H9A 0.9300 . ? C7 C8 1.385(2) . ? C7 H7A 0.9300 . ? C3 C4 1.391(2) . ? C3 H3A 0.9300 . ? C5 C4 1.374(2) . ? C5 H5A 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C4 H4A 0.9300 . ? C11 C10 1.384(3) . ? C11 H11A 0.9300 . ? C10 H10A 0.9300 . ? O5 C16 1.409(3) . ? C16 H3 1.09(4) . ? C16 H2 1.04(4) . ? C16 H1 1.05(4) . ? 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 N3 Fe1 N3 180.0 . 5_576 ? N3 Fe1 N1 89.98(5) . 5_566 ? N3 Fe1 N1 90.02(5) 5_576 5_566 ? N3 Fe1 N1 90.02(5) . 1_565 ? N3 Fe1 N1 89.98(5) 5_576 1_565 ? N1 Fe1 N1 180.0 5_566 1_565 ? N3 Fe1 N2 91.09(5) . . ? N3 Fe1 N2 88.91(5) 5_576 . ? N1 Fe1 N2 88.08(5) 5_566 . ? N1 Fe1 N2 91.92(5) 1_565 . ? N3 Fe1 N2 88.91(5) . 5_576 ? N3 Fe1 N2 91.09(5) 5_576 5_576 ? N1 Fe1 N2 91.92(5) 5_566 5_576 ? N1 Fe1 N2 88.08(5) 1_565 5_576 ? N2 Fe1 N2 180.0 . 5_576 ? C2 O1 C6 117.65(12) . . ? C8 O2 C12 119.34(13) . . ? C1 N2 C5 117.53(14) . . ? C1 N2 Fe1 121.54(11) . . ? C5 N2 Fe1 120.59(11) . . ? C6 C13 C6 111.07(19) . 2 ? C6 C13 C12 108.83(9) . 2 ? C6 C13 C12 109.18(9) 2 2 ? C6 C13 C12 109.18(9) . . ? C6 C13 C12 108.83(9) 2 . ? C12 C13 C12 109.8(2) 2 . ? C14 N3 Fe1 174.91(13) . . ? C11 N1 C7 118.20(14) . . ? C11 N1 Fe1 123.72(12) . 1_545 ? C7 N1 Fe1 117.78(10) . 1_545 ? O1 C6 C13 106.65(12) . . ? O1 C6 H6A 110.4 . . ? C13 C6 H6A 110.4 . . ? O1 C6 H6B 110.4 . . ? C13 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O1 C2 C3 126.15(15) . . ? O1 C2 C1 114.71(14) . . ? C3 C2 C1 119.15(15) . . ? N2 C1 C2 123.23(15) . . ? N2 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C10 C9 C8 118.24(15) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N1 C7 C8 122.28(15) . . ? N1 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? C2 C3 C4 117.51(16) . . ? C2 C3 H3A 121.2 . . ? C4 C3 H3A 121.2 . . ? O2 C8 C7 123.91(15) . . ? O2 C8 C9 116.82(14) . . ? C7 C8 C9 119.26(15) . . ? N2 C5 C4 122.36(15) . . ? N2 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? N3 C14 S2 178.90(17) . . ? O2 C12 C13 106.82(12) . . ? O2 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? O2 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C5 C4 C3 120.18(16) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C11 C10 122.52(16) . . ? N1 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? C9 C10 C11 119.47(16) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? O5 C16 H3 91.3(19) . . ? O5 C16 H2 116(2) . . ? H3 C16 H2 111(3) . . ? O5 C16 H1 113(2) . . ? H3 C16 H1 113(3) . . ? H2 C16 H1 111(3) . . ? 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 N3 Fe1 N2 C1 157.25(12) . . . . ? N3 Fe1 N2 C1 -22.75(12) 5_576 . . . ? N1 Fe1 N2 C1 -112.81(12) 5_566 . . . ? N1 Fe1 N2 C1 67.19(12) 1_565 . . . ? N2 Fe1 N2 C1 75(100) 5_576 . . . ? N3 Fe1 N2 C5 -15.85(12) . . . . ? N3 Fe1 N2 C5 164.15(12) 5_576 . . . ? N1 Fe1 N2 C5 74.09(12) 5_566 . . . ? N1 Fe1 N2 C5 -105.91(12) 1_565 . . . ? N2 Fe1 N2 C5 -98(100) 5_576 . . . ? N3 Fe1 N3 C14 82(78) 5_576 . . . ? N1 Fe1 N3 C14 -166.0(16) 5_566 . . . ? N1 Fe1 N3 C14 14.0(16) 1_565 . . . ? N2 Fe1 N3 C14 -77.9(16) . . . . ? N2 Fe1 N3 C14 102.1(16) 5_576 . . . ? C2 O1 C6 C13 167.42(13) . . . . ? C6 C13 C6 O1 -56.79(9) 2 . . . ? C12 C13 C6 O1 -177.00(13) 2 . . . ? C12 C13 C6 O1 63.21(17) . . . . ? C6 O1 C2 C3 9.0(2) . . . . ? C6 O1 C2 C1 -170.76(14) . . . . ? C5 N2 C1 C2 2.2(2) . . . . ? Fe1 N2 C1 C2 -171.13(12) . . . . ? O1 C2 C1 N2 179.15(14) . . . . ? C3 C2 C1 N2 -0.6(2) . . . . ? C11 N1 C7 C8 1.8(2) . . . . ? Fe1 N1 C7 C8 -172.06(12) 1_545 . . . ? O1 C2 C3 C4 179.08(16) . . . . ? C1 C2 C3 C4 -1.2(2) . . . . ? C12 O2 C8 C7 -24.2(2) . . . . ? C12 O2 C8 C9 156.78(16) . . . . ? N1 C7 C8 O2 -179.12(15) . . . . ? N1 C7 C8 C9 -0.1(2) . . . . ? C10 C9 C8 O2 177.71(16) . . . . ? C10 C9 C8 C7 -1.3(3) . . . . ? C1 N2 C5 C4 -2.0(2) . . . . ? Fe1 N2 C5 C4 171.39(13) . . . . ? Fe1 N3 C14 S2 -19(11) . . . . ? C8 O2 C12 C13 -137.90(15) . . . . ? C6 C13 C12 O2 172.32(13) . . . . ? C6 C13 C12 O2 -66.31(18) 2 . . . ? C12 C13 C12 O2 53.11(10) 2 . . . ? N2 C5 C4 C3 0.2(3) . . . . ? C2 C3 C4 C5 1.4(3) . . . . ? C7 N1 C11 C10 -2.0(3) . . . . ? Fe1 N1 C11 C10 171.49(15) 1_545 . . . ? C8 C9 C10 C11 1.2(3) . . . . ? N1 C11 C10 C9 0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.406 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.053 #_eof #End of Crystallographic Information File