# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM loop_ _publ_author_name 'Maram Basha' 'Jy Chartres' 'Namfon Pantarat' 'Mohammad Akbar Ali' 'Aminul Mirza' 'Danuta Kalinowski' 'Des Richarson' P.Bernhardt _publ_contact_author_name P.Bernhardt _publ_contact_author_email p.bernhardt@uq.edu.au data_545mb1 _database_code_depnum_ccdc_archive 'CCDC 858720' #TrackingRef '- supdata.cif' _audit_creation_date 2011-12-11T16:48:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C9 H11 N3 S2' _chemical_formula_sum 'C9 H11 N3 S2' _chemical_formula_weight 225.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8633(5) _cell_length_b 8.1483(10) _cell_length_c 11.7569(15) _cell_angle_alpha 81.909(10) _cell_angle_beta 79.334(9) _cell_angle_gamma 84.497(8) _cell_volume 545.09(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1076 _cell_measurement_theta_min 2.8985 _cell_measurement_theta_max 28.8497 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2897 _exptl_crystal_size_mid 0.0873 _exptl_crystal_size_min 0.0445 _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 236 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 -4 0.0209 1 -1 4 0.0235 1 1 -4 0.0806 1 2 2 0.0544 -1 -2 -2 0.0124 -2 1 0 0.13 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.64771 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 0.0251912 _diffrn_orient_matrix_ub_12 0.0676683 _diffrn_orient_matrix_ub_13 -0.0442694 _diffrn_orient_matrix_ub_21 0.0039702 _diffrn_orient_matrix_ub_22 0.0519117 _diffrn_orient_matrix_ub_23 0.0431213 _diffrn_orient_matrix_ub_31 0.1207551 _diffrn_orient_matrix_ub_32 -0.0222913 _diffrn_orient_matrix_ub_33 -0.0031954 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.103 _diffrn_reflns_number 3488 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.9 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1905 _reflns_number_gt 1022 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^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_number_reflns 1905 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.213 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' 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 0.3171(7) 0.2316(5) 0.6722(3) 0.0808(13) Uani 1 1 d . . . H1 H 0.1924 0.2519 0.7313 0.097 Uiso 1 1 calc R . . C2 C 0.5087(8) 0.1372(5) 0.7025(3) 0.0775(13) Uani 1 1 d . . . H2 H 0.5124 0.0927 0.7795 0.093 Uiso 1 1 calc R . . C3 C 0.6925(7) 0.1110(5) 0.6165(4) 0.0733(12) Uani 1 1 d . . . H3 H 0.8268 0.0501 0.6341 0.088 Uiso 1 1 calc R . . C4 C 0.6787(6) 0.1747(4) 0.5039(3) 0.0593(10) Uani 1 1 d . . . H4 H 0.8015 0.1556 0.4437 0.071 Uiso 1 1 calc R . . C5 C 0.4782(6) 0.2684(4) 0.4810(3) 0.0423(8) Uani 1 1 d . . . C6 C 0.4525(5) 0.3374(4) 0.3598(3) 0.0442(9) Uani 1 1 d . . . C7 C 0.2384(5) 0.4440(4) 0.3398(3) 0.0618(11) Uani 1 1 d . . . H7A H 0.2805 0.5529 0.3045 0.093 Uiso 1 1 calc R . . H7B H 0.1363 0.4521 0.4131 0.093 Uiso 1 1 calc R . . H7C H 0.1606 0.3955 0.2891 0.093 Uiso 1 1 calc R . . C8 C 0.7911(5) 0.3050(4) 0.0840(3) 0.0397(8) Uani 1 1 d . . . C9 C 1.2220(5) 0.1460(4) 0.0184(3) 0.0615(10) Uani 1 1 d . . . H9A H 1.1541 0.0951 -0.035 0.092 Uiso 1 1 calc R . . H9B H 1.3509 0.0753 0.0409 0.092 Uiso 1 1 calc R . . H9C H 1.2755 0.2514 -0.0188 0.092 Uiso 1 1 calc R . . N1 N 0.2990(5) 0.2955(4) 0.5641(3) 0.0642(9) Uani 1 1 d . . . N2 N 0.6224(4) 0.2972(3) 0.2808(2) 0.0449(7) Uani 1 1 d . . . N3 N 0.6159(4) 0.3514(3) 0.1653(2) 0.0509(8) Uani 1 1 d . . . H3A H 0.4999 0.4147 0.1457 0.061 Uiso 1 1 calc R . . S1 S 0.79887(14) 0.35774(12) -0.05690(7) 0.0545(3) Uani 1 1 d . . . S2 S 1.00829(14) 0.17669(11) 0.14517(7) 0.0520(3) 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 0.075(3) 0.118(4) 0.036(3) -0.001(2) 0.010(2) 0.010(3) C2 0.094(3) 0.092(3) 0.037(3) 0.009(2) -0.004(2) 0.001(3) C3 0.073(3) 0.080(3) 0.059(3) 0.006(2) -0.015(2) 0.016(2) C4 0.058(2) 0.073(3) 0.039(3) -0.007(2) 0.0032(18) 0.011(2) C5 0.046(2) 0.044(2) 0.036(2) -0.0068(17) -0.0019(16) -0.0025(18) C6 0.050(2) 0.050(2) 0.031(2) -0.0103(18) 0.0003(17) -0.0024(18) C7 0.055(2) 0.079(3) 0.045(2) -0.011(2) 0.0004(18) 0.017(2) C8 0.0377(18) 0.041(2) 0.0384(19) -0.0098(16) 0.0012(15) -0.0030(15) C9 0.043(2) 0.078(3) 0.056(2) -0.010(2) 0.0012(17) 0.0164(18) N1 0.0590(19) 0.091(2) 0.0314(19) -0.0032(17) 0.0074(15) 0.0133(16) N2 0.0514(17) 0.0536(19) 0.0257(17) -0.0046(14) 0.0006(13) 0.0019(13) N3 0.0487(17) 0.062(2) 0.0359(18) -0.0038(15) -0.0004(14) 0.0115(14) S1 0.0517(6) 0.0725(7) 0.0322(5) -0.0019(5) -0.0011(4) 0.0121(5) S2 0.0514(6) 0.0635(6) 0.0361(5) -0.0037(5) -0.0050(4) 0.0115(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.323(4) . ? C1 C2 1.374(5) . ? C1 H1 0.93 . ? C2 C3 1.358(5) . ? C2 H2 0.93 . ? C3 C4 1.366(5) . ? C3 H3 0.93 . ? C4 C5 1.387(4) . ? C4 H4 0.93 . ? C5 N1 1.321(4) . ? C5 C6 1.485(4) . ? C6 N2 1.282(3) . ? C6 C7 1.493(4) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 N3 1.333(3) . ? C8 S1 1.645(3) . ? C8 S2 1.762(3) . ? C9 S2 1.791(3) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? N2 N3 1.374(3) . ? N3 H3A 0.86 . ? 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 N1 C1 C2 124.0(4) . . ? N1 C1 H1 118 . . ? C2 C1 H1 118 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.5(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.1(4) . . ? N1 C5 C6 116.9(3) . . ? C4 C5 C6 120.9(3) . . ? N2 C6 C5 115.0(3) . . ? N2 C6 C7 126.0(3) . . ? C5 C6 C7 119.0(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 S1 123.7(2) . . ? N3 C8 S2 112.0(2) . . ? S1 C8 S2 124.29(18) . . ? S2 C9 H9A 109.5 . . ? S2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 N1 C1 117.6(3) . . ? C6 N2 N3 120.1(3) . . ? C8 N3 N2 119.4(3) . . ? C8 N3 H3A 120.3 . . ? N2 N3 H3A 120.3 . . ? C8 S2 C9 101.65(15) . . ? #===END #\#CIF_1.1 # [Fe(PCSMC)2]ClO4 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-12-11 at 11:58:55 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 717mb11 717 struct data_717mb11 _database_code_depnum_ccdc_archive 'CCDC 858721' #TrackingRef '- supdata.cif' _audit_creation_date 2011-12-11T11:58:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H16 Fe N6 S4, Cl O4 ' _chemical_formula_sum 'C16 H16 Cl Fe N6 O4 S4' _chemical_formula_weight 575.89 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 33.4374(17) _cell_length_b 8.8580(4) _cell_length_c 14.8651(10) _cell_angle_alpha 90 _cell_angle_beta 90.851(5) _cell_angle_gamma 90 _cell_volume 4402.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4268 _cell_measurement_theta_min 2.9316 _cell_measurement_theta_max 29.2181 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.85174 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.0045363 _diffrn_orient_matrix_ub_12 -0.0122443 _diffrn_orient_matrix_ub_13 -0.0462203 _diffrn_orient_matrix_ub_21 -0.0177637 _diffrn_orient_matrix_ub_22 -0.038373 _diffrn_orient_matrix_ub_23 0.0119011 _diffrn_orient_matrix_ub_31 -0.0106537 _diffrn_orient_matrix_ub_32 0.0691999 _diffrn_orient_matrix_ub_33 -0.0016287 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_number 14700 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3881 _reflns_number_gt 3199 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+3.7084P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3881 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.303 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 C1A C 0.68674(10) 0.1715(4) 0.4333(2) 0.0406(8) Uani 1 1 d . . . H1A H 0.6796 0.0707 0.44 0.049 Uiso 1 1 calc R . . C1B C 0.65405(10) 0.3346(3) 0.6716(2) 0.0404(8) Uani 1 1 d . . . H1B H 0.6519 0.4347 0.6533 0.048 Uiso 1 1 calc R . . C2A C 0.72324(10) 0.2058(4) 0.3994(2) 0.0482(9) Uani 1 1 d . . . H2A H 0.7405 0.1294 0.3815 0.058 Uiso 1 1 calc R . . C2B C 0.67536(11) 0.3017(4) 0.7471(2) 0.0496(9) Uani 1 1 d . . . H2B H 0.6885 0.3781 0.7786 0.059 Uiso 1 1 calc R . . C3A C 0.73410(10) 0.3523(4) 0.3922(2) 0.0473(9) Uani 1 1 d . . . H3A H 0.7589 0.3775 0.3689 0.057 Uiso 1 1 calc R . . C3B C 0.67749(10) 0.1569(4) 0.7769(2) 0.0469(9) Uani 1 1 d . . . H3B H 0.6917 0.133 0.8292 0.056 Uiso 1 1 calc R . . C4A C 0.70871(9) 0.4623(4) 0.4190(2) 0.0397(8) Uani 1 1 d . . . H4A H 0.7162 0.5633 0.4171 0.048 Uiso 1 1 calc R . . C4B C 0.65844(9) 0.0478(4) 0.7285(2) 0.0386(8) Uani 1 1 d . . . H4B H 0.6589 -0.0518 0.7482 0.046 Uiso 1 1 calc R . . C5A C 0.67211(8) 0.4214(3) 0.4485(2) 0.0324(7) Uani 1 1 d . . . C5B C 0.63873(8) 0.0856(3) 0.6511(2) 0.0301(7) Uani 1 1 d . . . C6A C 0.64207(9) 0.5244(3) 0.4760(2) 0.0346(7) Uani 1 1 d . . . H6A H 0.6455 0.6284 0.4733 0.041 Uiso 1 1 calc R . . C6B C 0.62031(8) -0.0188(3) 0.5906(2) 0.0328(7) Uani 1 1 d . . . H6B H 0.619 -0.1218 0.6022 0.039 Uiso 1 1 calc R . . C8A C 0.55297(9) 0.4793(3) 0.5725(2) 0.0360(7) Uani 1 1 d . . . C8B C 0.57694(9) 0.0229(3) 0.3863(2) 0.0347(7) Uani 1 1 d . . . C9A C 0.52820(11) 0.7592(4) 0.6182(3) 0.0647(12) Uani 1 1 d . . . H9A1 H 0.5079 0.8207 0.6448 0.097 Uiso 1 1 calc R . . H9A2 H 0.5317 0.7889 0.5567 0.097 Uiso 1 1 calc R . . H9A3 H 0.5529 0.772 0.6509 0.097 Uiso 1 1 calc R . . C9B C 0.55794(13) -0.2593(4) 0.3300(3) 0.0639(11) Uani 1 1 d . . . H9B1 H 0.5459 -0.3218 0.2843 0.096 Uiso 1 1 calc R . . H9B2 H 0.5443 -0.274 0.3857 0.096 Uiso 1 1 calc R . . H9B3 H 0.5856 -0.2861 0.3376 0.096 Uiso 1 1 calc R . . N1A N 0.66136(7) 0.2768(3) 0.45676(17) 0.0323(6) Uani 1 1 d . . . N1B N 0.63627(7) 0.2287(2) 0.62311(17) 0.0309(6) Uani 1 1 d . . . N2A N 0.61000(7) 0.4640(3) 0.50452(16) 0.0315(6) Uani 1 1 d . . . N2B N 0.60574(7) 0.0409(3) 0.51919(17) 0.0321(6) Uani 1 1 d . . . N3A N 0.58116(7) 0.5572(3) 0.53785(17) 0.0353(6) Uani 1 1 d . . . N3B N 0.58882(7) -0.0527(3) 0.45575(18) 0.0364(6) Uani 1 1 d . . . O1 O 0.72736(10) 0.5974(3) 0.6107(3) 0.1041(12) Uani 1 1 d . . . O2 O 0.69765(9) 0.8060(4) 0.5487(2) 0.0854(9) Uani 1 1 d . . . O3 O 0.73106(8) 0.8243(3) 0.6843(2) 0.0730(8) Uani 1 1 d . . . O4 O 0.67136(8) 0.6960(3) 0.6741(2) 0.0772(9) Uani 1 1 d . . . S1A S 0.55090(2) 0.28536(9) 0.57608(6) 0.0395(2) Uani 1 1 d . . . S1B S 0.58243(3) 0.21376(9) 0.37246(6) 0.0410(2) Uani 1 1 d . . . S2A S 0.51360(3) 0.56798(10) 0.62217(7) 0.0497(3) Uani 1 1 d . . . S2B S 0.55422(3) -0.06785(10) 0.29762(6) 0.0494(2) Uani 1 1 d . . . Cl1 Cl 0.70730(3) 0.73021(9) 0.62978(7) 0.0529(3) Uani 1 1 d . . . Fe1 Fe 0.607832(12) 0.25204(4) 0.50800(3) 0.02986(13) 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 C1A 0.045(2) 0.0369(18) 0.040(2) -0.0029(14) -0.0032(16) 0.0064(15) C1B 0.050(2) 0.0334(17) 0.038(2) -0.0013(14) -0.0078(16) -0.0048(14) C2A 0.043(2) 0.055(2) 0.046(2) -0.0046(17) 0.0011(17) 0.0140(16) C2B 0.059(2) 0.048(2) 0.042(2) -0.0071(17) -0.0144(18) -0.0106(17) C3A 0.0351(18) 0.067(2) 0.040(2) 0.0052(17) 0.0043(16) 0.0042(16) C3B 0.050(2) 0.055(2) 0.035(2) 0.0036(16) -0.0157(17) 0.0020(16) C4A 0.0372(18) 0.0468(19) 0.035(2) 0.0068(15) 0.0019(15) -0.0007(14) C4B 0.0387(18) 0.0400(18) 0.037(2) 0.0068(14) -0.0049(15) -0.0003(14) C5A 0.0345(17) 0.0353(17) 0.0272(17) 0.0041(13) -0.0014(13) 0.0035(13) C5B 0.0288(15) 0.0304(16) 0.0311(18) 0.0020(13) -0.0002(13) 0.0001(12) C6A 0.0383(18) 0.0282(16) 0.037(2) 0.0061(13) 0.0018(15) -0.0007(13) C6B 0.0341(17) 0.0276(15) 0.0366(19) 0.0072(13) -0.0045(14) -0.0027(12) C8A 0.0363(17) 0.0383(17) 0.0333(19) -0.0002(14) -0.0042(15) 0.0047(13) C8B 0.0277(16) 0.0422(18) 0.0342(19) -0.0032(14) -0.0035(14) -0.0054(13) C9A 0.050(2) 0.052(2) 0.093(3) -0.025(2) 0.014(2) 0.0041(17) C9B 0.083(3) 0.056(2) 0.053(3) -0.0093(19) -0.005(2) -0.025(2) N1A 0.0340(14) 0.0320(14) 0.0307(15) 0.0007(11) -0.0018(11) 0.0023(11) N1B 0.0332(14) 0.0301(13) 0.0293(15) 0.0008(11) -0.0031(11) -0.0013(10) N2A 0.0305(14) 0.0323(13) 0.0318(15) 0.0046(11) -0.0013(11) 0.0036(10) N2B 0.0310(13) 0.0293(13) 0.0358(16) -0.0008(11) -0.0017(12) -0.0021(10) N3A 0.0329(14) 0.0337(14) 0.0397(17) 0.0021(11) 0.0054(12) 0.0066(11) N3B 0.0376(15) 0.0363(14) 0.0350(17) -0.0027(12) -0.0088(12) -0.0063(11) O1 0.111(3) 0.070(2) 0.131(3) -0.023(2) -0.002(2) 0.0484(19) O2 0.085(2) 0.092(2) 0.078(2) 0.0235(18) -0.0164(18) 0.0050(17) O3 0.0620(18) 0.083(2) 0.074(2) -0.0151(16) -0.0022(16) -0.0272(14) O4 0.0547(17) 0.0530(16) 0.124(3) 0.0060(17) 0.0148(18) -0.0152(13) S1A 0.0354(4) 0.0389(5) 0.0442(5) 0.0056(4) 0.0031(4) -0.0014(3) S1B 0.0465(5) 0.0415(5) 0.0347(5) 0.0048(4) -0.0095(4) -0.0018(4) S2A 0.0383(5) 0.0513(5) 0.0598(6) -0.0079(4) 0.0113(4) 0.0018(4) S2B 0.0503(5) 0.0574(6) 0.0400(6) -0.0049(4) -0.0130(4) -0.0103(4) Cl1 0.0477(5) 0.0411(5) 0.0698(7) -0.0080(4) -0.0041(5) 0.0027(4) Fe1 0.0313(2) 0.0276(2) 0.0305(3) 0.00272(18) -0.00318(19) -0.00057(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1A 1.312(4) . ? C1A C2A 1.361(4) . ? C1A H1A 0.93 . ? C1B N1B 1.319(4) . ? C1B C2B 1.352(5) . ? C1B H1B 0.93 . ? C2A C3A 1.352(5) . ? C2A H2A 0.93 . ? C2B C3B 1.359(5) . ? C2B H2B 0.93 . ? C3A C4A 1.356(4) . ? C3A H3A 0.93 . ? C3B C4B 1.357(4) . ? C3B H3B 0.93 . ? C4A C5A 1.356(4) . ? C4A H4A 0.93 . ? C4B C5B 1.359(4) . ? C4B H4B 0.93 . ? C5A N1A 1.336(4) . ? C5A C6A 1.421(4) . ? C5B N1B 1.336(3) . ? C5B C6B 1.423(4) . ? C6A N2A 1.277(3) . ? C6A H6A 0.93 . ? C6B N2B 1.276(4) . ? C6B H6B 0.93 . ? C8A N3A 1.282(4) . ? C8A S2A 1.710(3) . ? C8A S1A 1.720(3) . ? C8B N3B 1.288(4) . ? C8B S2B 1.713(3) . ? C8B S1B 1.713(3) . ? C9A S2A 1.764(3) . ? C9A H9A1 0.96 . ? C9A H9A2 0.96 . ? C9A H9A3 0.96 . ? C9B S2B 1.767(4) . ? C9B H9B1 0.96 . ? C9B H9B2 0.96 . ? C9B H9B3 0.96 . ? N1A Fe1 1.968(2) . ? N1B Fe1 1.956(3) . ? N2A N3A 1.368(3) . ? N2A Fe1 1.880(2) . ? N2B N3B 1.371(3) . ? N2B Fe1 1.879(2) . ? O1 Cl1 1.386(3) . ? O2 Cl1 1.413(3) . ? O3 Cl1 1.401(3) . ? O4 Cl1 1.412(3) . ? S1A Fe1 2.1891(9) . ? S1B Fe1 2.2012(10) . ? 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 N1A C1A C2A 121.8(3) . . ? N1A C1A H1A 119.1 . . ? C2A C1A H1A 119.1 . . ? N1B C1B C2B 121.9(3) . . ? N1B C1B H1B 119.1 . . ? C2B C1B H1B 119.1 . . ? C3A C2A C1A 119.1(3) . . ? C3A C2A H2A 120.4 . . ? C1A C2A H2A 120.4 . . ? C1B C2B C3B 119.9(3) . . ? C1B C2B H2B 120.1 . . ? C3B C2B H2B 120.1 . . ? C2A C3A C4A 119.7(3) . . ? C2A C3A H3A 120.1 . . ? C4A C3A H3A 120.1 . . ? C4B C3B C2B 118.5(3) . . ? C4B C3B H3B 120.7 . . ? C2B C3B H3B 120.7 . . ? C5A C4A C3A 118.4(3) . . ? C5A C4A H4A 120.8 . . ? C3A C4A H4A 120.8 . . ? C3B C4B C5B 119.4(3) . . ? C3B C4B H4B 120.3 . . ? C5B C4B H4B 120.3 . . ? N1A C5A C4A 122.0(3) . . ? N1A C5A C6A 113.4(2) . . ? C4A C5A C6A 124.5(3) . . ? N1B C5B C4B 121.6(3) . . ? N1B C5B C6B 113.3(3) . . ? C4B C5B C6B 125.1(3) . . ? N2A C6A C5A 115.3(3) . . ? N2A C6A H6A 122.4 . . ? C5A C6A H6A 122.4 . . ? N2B C6B C5B 114.4(3) . . ? N2B C6B H6B 122.8 . . ? C5B C6B H6B 122.8 . . ? N3A C8A S2A 120.1(2) . . ? N3A C8A S1A 125.4(2) . . ? S2A C8A S1A 114.45(18) . . ? N3B C8B S2B 120.0(2) . . ? N3B C8B S1B 125.3(2) . . ? S2B C8B S1B 114.70(19) . . ? S2A C9A H9A1 109.5 . . ? S2A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? S2A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? S2B C9B H9B1 109.5 . . ? S2B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? S2B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C1A N1A C5A 118.8(3) . . ? C1A N1A Fe1 128.3(2) . . ? C5A N1A Fe1 112.92(18) . . ? C1B N1B C5B 118.6(3) . . ? C1B N1B Fe1 127.7(2) . . ? C5B N1B Fe1 113.55(19) . . ? C6A N2A N3A 117.9(2) . . ? C6A N2A Fe1 117.4(2) . . ? N3A N2A Fe1 124.40(18) . . ? C6B N2B N3B 118.1(2) . . ? C6B N2B Fe1 118.1(2) . . ? N3B N2B Fe1 123.8(2) . . ? C8A N3A N2A 110.3(2) . . ? C8B N3B N2B 110.8(2) . . ? C8A S1A Fe1 94.85(11) . . ? C8B S1B Fe1 94.73(12) . . ? C8A S2A C9A 102.21(16) . . ? C8B S2B C9B 102.26(18) . . ? O1 Cl1 O3 110.6(2) . . ? O1 Cl1 O4 109.4(2) . . ? O3 Cl1 O4 109.69(18) . . ? O1 Cl1 O2 109.5(2) . . ? O3 Cl1 O2 109.3(2) . . ? O4 Cl1 O2 108.36(19) . . ? N2B Fe1 N2A 176.51(11) . . ? N2B Fe1 N1B 80.53(10) . . ? N2A Fe1 N1B 96.40(10) . . ? N2B Fe1 N1A 100.39(10) . . ? N2A Fe1 N1A 80.93(10) . . ? N1B Fe1 N1A 85.25(10) . . ? N2B Fe1 S1A 93.42(7) . . ? N2A Fe1 S1A 84.97(7) . . ? N1B Fe1 S1A 91.42(7) . . ? N1A Fe1 S1A 165.04(7) . . ? N2B Fe1 S1B 85.03(8) . . ? N2A Fe1 S1B 98.23(8) . . ? N1B Fe1 S1B 163.80(7) . . ? N1A Fe1 S1B 90.21(8) . . ? S1A Fe1 S1B 96.75(4) . . ? data_614mb4 _database_code_depnum_ccdc_archive 'CCDC 858722' #TrackingRef '- 858722_new.cif' _audit_creation_date 2012-01-08T21:55:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H22 Fe N8 S4, C13 H11 N4 S, 2(Cl O4)' _chemical_formula_sum 'C39 H33 Cl2 Fe N12 O8 S5' _chemical_formula_weight 1084.82 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9883(3) _cell_length_b 14.5465(7) _cell_length_c 20.3055(9) _cell_angle_alpha 89.484(4) _cell_angle_beta 82.777(4) _cell_angle_gamma 84.060(4) _cell_volume 2328.22(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5658 _cell_measurement_theta_min 3.0518 _cell_measurement_theta_max 62.4273 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1110 _exptl_special_details ; Data to only 2\q = 125 were collected due to geometric limitations of the dual source (Mo/Cu) diffractometer. Higher angles would have resulted in a collision between the detector and the Mo collimator. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.58346 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.0370856 _diffrn_orient_matrix_ub_12 -0.0861871 _diffrn_orient_matrix_ub_13 -0.036984 _diffrn_orient_matrix_ub_21 0.0978021 _diffrn_orient_matrix_ub_22 0.033972 _diffrn_orient_matrix_ub_23 -0.0643461 _diffrn_orient_matrix_ub_31 0.1650937 _diffrn_orient_matrix_ub_32 -0.0524913 _diffrn_orient_matrix_ub_33 0.0184507 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_number 21135 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 62.47 _diffrn_reflns_theta_full 62.47 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7365 _reflns_number_gt 5999 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The perchlorate anion including Cl1 was disordered rotationally about Cl1-O1A and the two contributors were refined with complementary occupancies and with restraints to maintain the same geometry (bond lengths and angles). The perchlorate including Cl2 was disordered over three positions and three sets of four O atoms were located. The major contributor (O2A-O2D) defined a tetrahedral geometry and the remaining sets (O2E-O2H and O2I-O2L) were restrained to show the same configuration. The occupancies of O2A-O2D were refined against the sum of O2E-O2H and O2I-O2L. 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^)+(0.0515P)^2^+1.2469P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7365 _refine_ls_number_parameters 653 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.112 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.405 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.0556(4) 0.1404(3) 0.57891(19) 0.0623(9) Uani 1 1 d . . . H1A H 0.0668 0.1911 0.5511 0.075 Uiso 1 1 calc R . . C1B C 0.1384(4) 0.2850(2) 0.74589(16) 0.0535(8) Uani 1 1 d . . . H1B H 0.1548 0.2307 0.7698 0.064 Uiso 1 1 calc R . . C2A C -0.0688(5) 0.0835(3) 0.5719(2) 0.0753(11) Uani 1 1 d . . . H2A H -0.1393 0.0956 0.5391 0.09 Uiso 1 1 calc R . . C2B C 0.0389(5) 0.3592(3) 0.77614(18) 0.0629(9) Uani 1 1 d . . . H2B H -0.0136 0.3548 0.8194 0.076 Uiso 1 1 calc R . . C3A C -0.0893(4) 0.0095(3) 0.6130(2) 0.0720(11) Uani 1 1 d . . . H3A H -0.1736 -0.0287 0.6084 0.086 Uiso 1 1 calc R . . C3B C 0.0185(5) 0.4399(3) 0.74109(19) 0.0661(10) Uani 1 1 d . . . H3B H -0.0471 0.4913 0.7609 0.079 Uiso 1 1 calc R . . C4A C 0.0174(4) -0.0080(2) 0.66172(19) 0.0599(9) Uani 1 1 d . . . H4A H 0.0051 -0.0576 0.6906 0.072 Uiso 1 1 calc R . . C4B C 0.0951(4) 0.4449(2) 0.67683(17) 0.0592(9) Uani 1 1 d . . . H4B H 0.083 0.4996 0.6531 0.071 Uiso 1 1 calc R . . C5A C 0.1428(4) 0.0501(2) 0.66635(15) 0.0458(7) Uani 1 1 d . . . C5B C 0.1902(4) 0.3679(2) 0.64791(15) 0.0475(7) Uani 1 1 d . . . C6A C 0.2729(4) 0.0370(2) 0.71132(15) 0.0455(7) Uani 1 1 d . . . C6B C 0.2716(4) 0.3599(2) 0.57895(15) 0.0469(7) Uani 1 1 d . . . C7A C 0.2817(4) -0.0395(2) 0.75954(16) 0.0512(8) Uani 1 1 d . . . C7B C 0.2562(4) 0.4354(2) 0.52950(16) 0.0513(8) Uani 1 1 d . . . C8A C 0.6081(4) 0.1579(2) 0.72986(15) 0.0467(7) Uani 1 1 d . . . C8B C 0.5127(4) 0.1792(2) 0.49474(16) 0.0519(8) Uani 1 1 d . . . C9A C 0.7458(5) 0.0760(3) 0.8363(2) 0.0761(11) Uani 1 1 d . . . H9A H 0.6354 0.0857 0.8615 0.114 Uiso 1 1 calc R . . H9B H 0.8311 0.0752 0.8657 0.114 Uiso 1 1 calc R . . H9C H 0.757 0.018 0.8131 0.114 Uiso 1 1 calc R . . C9B C 0.6005(6) 0.2467(3) 0.36868(19) 0.0851(13) Uani 1 1 d . . . H9D H 0.4845 0.2547 0.36 0.128 Uiso 1 1 calc R . . H9E H 0.6738 0.2384 0.3275 0.128 Uiso 1 1 calc R . . H9F H 0.6258 0.3004 0.3911 0.128 Uiso 1 1 calc R . . C10A C 0.4294(5) -0.0966(2) 0.76167(18) 0.0648(9) Uani 1 1 d . . . H10A H 0.5272 -0.0871 0.7336 0.078 Uiso 1 1 calc R . . C10B C 0.2276(5) 0.4171(3) 0.46536(18) 0.0630(9) Uani 1 1 d . . . H10B H 0.2151 0.3574 0.4523 0.076 Uiso 1 1 calc R . . C11A C 0.4285(8) -0.1684(3) 0.8067(2) 0.0899(14) Uani 1 1 d . . . H11A H 0.526 -0.2086 0.8089 0.108 Uiso 1 1 calc R . . C11B C 0.2180(5) 0.4892(4) 0.4214(2) 0.0834(13) Uani 1 1 d . . . H11B H 0.2034 0.4785 0.3775 0.1 Uiso 1 1 calc R . . C12A C 0.2870(10) -0.1796(3) 0.8469(2) 0.1045(19) Uani 1 1 d . . . H12A H 0.2854 -0.2268 0.8781 0.125 Uiso 1 1 calc R . . C12B C 0.2298(6) 0.5758(4) 0.4426(3) 0.0896(14) Uani 1 1 d . . . H12B H 0.2216 0.6255 0.4137 0.108 Uiso 1 1 calc R . . C13A C 0.1448(8) -0.1211(4) 0.8417(2) 0.1008(17) Uani 1 1 d . . . H13A H 0.0468 -0.1305 0.8697 0.121 Uiso 1 1 calc R . . C13B C 0.2541(6) 0.5890(3) 0.5069(3) 0.0897(14) Uani 1 1 d . . . H13B H 0.2608 0.6491 0.521 0.108 Uiso 1 1 calc R . . N1A N 0.1605(3) 0.12370(17) 0.62506(13) 0.0490(6) Uani 1 1 d . . . N1B N 0.2127(3) 0.28810(17) 0.68322(12) 0.0456(6) Uani 1 1 d . . . N2A N 0.3831(3) 0.09801(16) 0.70241(12) 0.0431(6) Uani 1 1 d . . . N2B N 0.3537(3) 0.27837(17) 0.56526(12) 0.0447(6) Uani 1 1 d . . . N3A N 0.5101(3) 0.09326(17) 0.74315(13) 0.0477(6) Uani 1 1 d . . . N3B N 0.4401(3) 0.26333(19) 0.50214(12) 0.0519(6) Uani 1 1 d . . . N4A N 0.1373(4) -0.0499(2) 0.79795(16) 0.0750(9) Uani 1 1 d . . . N4B N 0.2690(4) 0.5200(2) 0.55144(16) 0.0697(8) Uani 1 1 d . . . S1A S 0.59057(10) 0.24036(6) 0.66812(4) 0.0517(2) Uani 1 1 d . . . S1B S 0.50287(10) 0.09381(5) 0.55496(4) 0.0513(2) Uani 1 1 d . . . S2A S 0.77167(11) 0.16783(7) 0.77745(5) 0.0625(2) Uani 1 1 d . . . S2B S 0.63311(14) 0.14682(7) 0.41997(5) 0.0749(3) Uani 1 1 d . . . Fe1 Fe 0.36384(6) 0.18798(3) 0.63397(2) 0.04228(14) Uani 1 1 d . . . Cl1 Cl 0.11694(14) 0.27292(7) 0.29645(6) 0.0815(3) Uani 1 1 d . . . O1A O 0.2273(6) 0.3410(3) 0.2819(2) 0.1293(14) Uani 1 1 d . A . O1B O 0.1444(17) 0.2257(7) 0.3532(4) 0.220(6) Uani 0.742(12) 1 d PD A 1 O1C O 0.1538(13) 0.2083(6) 0.2442(4) 0.185(4) Uani 0.742(12) 1 d PD A 1 O1D O -0.0412(9) 0.3115(7) 0.2975(8) 0.285(9) Uani 0.742(12) 1 d PD A 1 O1E O 0.2009(15) 0.1978(10) 0.3213(7) 0.080(5) Uiso 0.258(12) 1 d PD A 2 O1F O 0.008(2) 0.3141(10) 0.3560(7) 0.101(6) Uiso 0.258(12) 1 d PD A 2 O1G O 0.014(3) 0.2561(12) 0.2541(7) 0.119(7) Uiso 0.258(12) 1 d PD A 2 Cl2 Cl -0.19574(13) 0.27714(6) 0.97008(5) 0.0709(3) Uani 1 1 d . . . O2A O -0.0607(8) 0.2234(6) 0.9283(4) 0.179(4) Uani 0.678(8) 1 d PD B 1 O2B O -0.2611(9) 0.3393(4) 0.9222(3) 0.123(2) Uani 0.678(8) 1 d PD B 1 O2C O -0.1243(13) 0.3141(7) 1.0181(4) 0.149(4) Uani 0.678(8) 1 d PD B 1 O2D O -0.3216(8) 0.2178(5) 0.9877(3) 0.124(3) Uani 0.678(8) 1 d PD B 1 O2E O -0.182(3) 0.1842(10) 0.9724(10) 0.083(6) Uiso 0.161(4) 1 d PD B 2 O2F O -0.356(2) 0.3104(15) 1.0005(11) 0.093(7) Uiso 0.161(4) 1 d PD B 2 O2G O -0.126(3) 0.3121(13) 0.9156(9) 0.097(7) Uiso 0.161(4) 1 d PD B 2 O2H O -0.090(3) 0.301(2) 1.0287(13) 0.102(11) Uiso 0.161(4) 1 d PD B 2 O2I O -0.312(2) 0.3279(13) 1.0244(10) 0.082(6) Uiso 0.161(4) 1 d PD B 3 O2J O -0.296(4) 0.267(3) 0.9239(14) 0.37(4) Uiso 0.161(4) 1 d PD B 3 O2K O -0.078(3) 0.3484(17) 0.9553(16) 0.152(11) Uiso 0.161(4) 1 d PD B 3 O2L O -0.126(3) 0.2002(13) 0.9957(16) 0.138(11) Uiso 0.161(4) 1 d PD B 3 C1C C -0.7427(7) 0.5710(3) 0.8281(3) 0.0941(14) Uani 1 1 d . . . H1C H -0.8187 0.6239 0.8353 0.113 Uiso 1 1 calc R . . C2C C -0.6196(8) 0.5687(4) 0.7746(3) 0.1068(17) Uani 1 1 d . . . H2C H -0.6132 0.619 0.7462 0.128 Uiso 1 1 calc R . . C3C C -0.5057(8) 0.4913(4) 0.7634(2) 0.1045(17) Uani 1 1 d . . . H3C H -0.4212 0.4885 0.7273 0.125 Uiso 1 1 calc R . . C4C C -0.5189(6) 0.4184(3) 0.8063(2) 0.0804(12) Uani 1 1 d . . . H4C H -0.4437 0.3651 0.8001 0.096 Uiso 1 1 calc R . . C5C C -0.6469(5) 0.4261(2) 0.85892(17) 0.0605(9) Uani 1 1 d . . . C6C C -0.6698(4) 0.3466(2) 0.90469(17) 0.0548(8) Uani 1 1 d . . . C7C C -0.7054(4) 0.3587(2) 0.97512(17) 0.0557(8) Uani 1 1 d . . . C8C C -0.7003(4) 0.1944(2) 0.97707(18) 0.0563(8) Uani 1 1 d . . . C9C C -0.7423(7) 0.0143(3) 0.9601(3) 0.1069(17) Uani 1 1 d . . . H9G H -0.825 0.0397 0.9327 0.16 Uiso 1 1 calc R . . H9H H -0.7764 -0.0422 0.9797 0.16 Uiso 1 1 calc R . . H9I H -0.6342 0.0021 0.9336 0.16 Uiso 1 1 calc R . . C10C C -0.7221(6) 0.4427(3) 1.0085(2) 0.0789(12) Uani 1 1 d . . . H10C H -0.7146 0.4973 0.9846 0.095 Uiso 1 1 calc R . . C11C C -0.7494(7) 0.4454(3) 1.0761(2) 0.0976(15) Uani 1 1 d . . . H11C H -0.7597 0.5017 1.0983 0.117 Uiso 1 1 calc R . . C12C C -0.7619(7) 0.3645(3) 1.1116(2) 0.0944(15) Uani 1 1 d . . . H12C H -0.7804 0.3663 1.1577 0.113 Uiso 1 1 calc R . . C13C C -0.7471(5) 0.2832(3) 1.07944(19) 0.0731(11) Uani 1 1 d . . . H13C H -0.7566 0.2289 1.1036 0.088 Uiso 1 1 calc R . . N1C N -0.7589(5) 0.5009(2) 0.87059(17) 0.0748(9) Uani 1 1 d . . . N2C N -0.6492(4) 0.26560(19) 0.87593(14) 0.0622(7) Uani 1 1 d . . . N3C N -0.6671(4) 0.18822(19) 0.91391(16) 0.0634(8) Uani 1 1 d . . . N4C N -0.7183(3) 0.27931(19) 1.01164(14) 0.0551(7) Uani 1 1 d . . . S2C S -0.72586(16) 0.09554(7) 1.02465(6) 0.0858(3) 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 C1A 0.050(2) 0.071(2) 0.067(2) 0.0001(18) -0.0172(17) 0.0004(17) C1B 0.061(2) 0.0540(19) 0.0449(18) 0.0000(15) -0.0024(15) -0.0089(15) C2A 0.055(2) 0.091(3) 0.084(3) -0.004(2) -0.024(2) -0.008(2) C2B 0.067(2) 0.071(2) 0.0470(19) -0.0078(17) 0.0077(16) -0.0056(18) C3A 0.045(2) 0.078(3) 0.095(3) -0.016(2) -0.0094(19) -0.0166(18) C3B 0.072(2) 0.061(2) 0.060(2) -0.0117(18) 0.0028(18) 0.0071(18) C4A 0.0492(19) 0.058(2) 0.073(2) -0.0071(17) -0.0004(17) -0.0127(16) C4B 0.069(2) 0.053(2) 0.054(2) 0.0010(16) -0.0059(17) 0.0002(16) C5A 0.0406(16) 0.0437(17) 0.0510(18) -0.0073(14) 0.0024(13) -0.0039(13) C5B 0.0500(18) 0.0467(17) 0.0458(17) -0.0031(14) -0.0061(14) -0.0038(14) C6A 0.0467(17) 0.0416(16) 0.0461(17) -0.0035(13) 0.0036(13) -0.0056(13) C6B 0.0525(18) 0.0450(17) 0.0441(17) 0.0027(13) -0.0079(14) -0.0081(14) C7A 0.065(2) 0.0431(17) 0.0460(18) 0.0000(14) -0.0029(15) -0.0135(15) C7B 0.0501(18) 0.0521(19) 0.0515(19) 0.0096(15) -0.0040(14) -0.0076(14) C8A 0.0470(17) 0.0487(17) 0.0442(17) -0.0065(14) -0.0039(13) -0.0056(14) C8B 0.0495(18) 0.063(2) 0.0432(18) -0.0028(15) -0.0015(14) -0.0084(16) C9A 0.074(3) 0.094(3) 0.063(2) 0.012(2) -0.022(2) -0.003(2) C9B 0.117(4) 0.092(3) 0.045(2) 0.004(2) 0.003(2) -0.019(3) C10A 0.081(3) 0.055(2) 0.059(2) 0.0083(17) -0.0112(18) -0.0066(18) C10B 0.065(2) 0.069(2) 0.055(2) 0.0094(17) -0.0114(17) -0.0022(18) C11A 0.146(5) 0.057(2) 0.072(3) 0.016(2) -0.038(3) -0.011(3) C11B 0.076(3) 0.111(4) 0.062(3) 0.028(2) -0.014(2) -0.003(3) C12A 0.195(6) 0.068(3) 0.059(3) 0.019(2) -0.023(4) -0.048(4) C12B 0.090(3) 0.093(4) 0.091(3) 0.052(3) -0.019(3) -0.025(3) C13A 0.143(5) 0.097(4) 0.065(3) 0.003(3) 0.022(3) -0.063(4) C13B 0.102(3) 0.059(2) 0.116(4) 0.030(3) -0.029(3) -0.032(2) N1A 0.0455(14) 0.0480(15) 0.0531(16) -0.0030(12) -0.0053(12) -0.0034(11) N1B 0.0515(15) 0.0450(14) 0.0407(14) 0.0010(11) -0.0043(11) -0.0085(11) N2A 0.0433(14) 0.0436(14) 0.0419(14) 0.0002(11) -0.0031(11) -0.0055(11) N2B 0.0505(15) 0.0462(14) 0.0370(13) 0.0000(11) -0.0020(11) -0.0072(11) N3A 0.0483(15) 0.0488(15) 0.0474(15) 0.0025(11) -0.0096(12) -0.0072(12) N3B 0.0582(16) 0.0569(17) 0.0395(14) 0.0028(12) 0.0001(12) -0.0084(13) N4A 0.085(2) 0.070(2) 0.068(2) 0.0013(17) 0.0156(17) -0.0306(17) N4B 0.085(2) 0.0546(18) 0.075(2) 0.0160(16) -0.0204(17) -0.0194(15) S1A 0.0544(5) 0.0517(4) 0.0510(5) 0.0060(3) -0.0061(3) -0.0167(4) S1B 0.0538(5) 0.0490(4) 0.0493(4) -0.0037(3) -0.0013(3) -0.0025(3) S2A 0.0555(5) 0.0729(6) 0.0632(5) -0.0011(4) -0.0172(4) -0.0144(4) S2B 0.0865(7) 0.0807(7) 0.0494(5) -0.0062(4) 0.0138(5) 0.0036(5) Fe1 0.0461(3) 0.0409(3) 0.0396(3) 0.00148(19) -0.0031(2) -0.0063(2) Cl1 0.0798(7) 0.0694(6) 0.0980(8) 0.0142(6) -0.0147(6) -0.0166(5) O1A 0.165(4) 0.107(3) 0.126(3) 0.014(2) -0.010(3) -0.072(3) O1B 0.392(15) 0.169(9) 0.128(7) 0.078(7) -0.074(9) -0.122(10) O1C 0.203(9) 0.142(6) 0.213(9) -0.070(5) 0.008(6) -0.068(6) O1D 0.077(5) 0.258(11) 0.50(3) 0.048(14) -0.030(8) 0.047(5) Cl2 0.0889(7) 0.0604(5) 0.0647(6) 0.0086(4) -0.0088(5) -0.0153(5) O2A 0.104(5) 0.228(9) 0.191(8) -0.083(7) -0.011(5) 0.051(5) O2B 0.152(6) 0.103(4) 0.121(5) 0.052(3) -0.047(4) -0.014(4) O2C 0.189(9) 0.173(8) 0.113(6) -0.010(5) -0.074(6) -0.079(6) O2D 0.103(4) 0.156(6) 0.127(5) 0.052(4) -0.024(3) -0.072(4) C1C 0.136(4) 0.056(2) 0.093(4) 0.011(2) -0.021(3) -0.016(3) C2C 0.165(5) 0.079(3) 0.082(3) 0.025(3) -0.015(4) -0.041(4) C3C 0.138(5) 0.100(4) 0.073(3) 0.013(3) 0.020(3) -0.041(3) C4C 0.103(3) 0.075(3) 0.061(2) 0.001(2) 0.007(2) -0.018(2) C5C 0.080(2) 0.051(2) 0.052(2) -0.0015(15) -0.0059(18) -0.0170(18) C6C 0.062(2) 0.0500(19) 0.052(2) -0.0033(15) -0.0036(16) -0.0079(15) C7C 0.062(2) 0.0520(19) 0.052(2) -0.0022(15) -0.0038(16) -0.0045(15) C8C 0.056(2) 0.0481(19) 0.064(2) 0.0020(16) -0.0055(16) -0.0033(15) C9C 0.144(5) 0.056(3) 0.123(4) 0.002(3) -0.013(4) -0.027(3) C10C 0.121(4) 0.056(2) 0.057(2) -0.0062(18) -0.004(2) -0.008(2) C11C 0.158(5) 0.071(3) 0.061(3) -0.019(2) -0.004(3) -0.005(3) C12C 0.146(4) 0.087(3) 0.046(2) -0.004(2) -0.003(2) -0.003(3) C13C 0.093(3) 0.075(3) 0.051(2) 0.0089(19) -0.0063(19) -0.010(2) N1C 0.104(3) 0.0516(18) 0.069(2) 0.0051(15) -0.0094(18) -0.0102(17) N2C 0.078(2) 0.0515(17) 0.0561(18) -0.0040(14) -0.0028(14) -0.0083(14) N3C 0.077(2) 0.0462(16) 0.066(2) -0.0017(14) -0.0038(16) -0.0065(14) N4C 0.0571(17) 0.0551(16) 0.0520(17) 0.0029(13) -0.0034(13) -0.0047(13) S2C 0.1122(9) 0.0580(6) 0.0863(8) 0.0188(5) -0.0086(6) -0.0113(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1A 1.338(4) . ? C1A C2A 1.379(5) . ? C1A H1A 0.93 . ? C1B N1B 1.337(4) . ? C1B C2B 1.373(5) . ? C1B H1B 0.93 . ? C2A C3A 1.366(6) . ? C2A H2A 0.93 . ? C2B C3B 1.374(5) . ? C2B H2B 0.93 . ? C3A C4A 1.391(5) . ? C3A H3A 0.93 . ? C3B C4B 1.374(5) . ? C3B H3B 0.93 . ? C4A C5A 1.388(4) . ? C4A H4A 0.93 . ? C4B C5B 1.378(4) . ? C4B H4B 0.93 . ? C5A N1A 1.362(4) . ? C5A C6A 1.464(4) . ? C5B N1B 1.367(4) . ? C5B C6B 1.468(4) . ? C6A N2A 1.308(4) . ? C6A C7A 1.478(4) . ? C6B N2B 1.309(4) . ? C6B C7B 1.488(4) . ? C7A N4A 1.330(4) . ? C7A C10A 1.375(5) . ? C7B N4B 1.329(4) . ? C7B C10B 1.383(5) . ? C8A N3A 1.291(4) . ? C8A S1A 1.735(3) . ? C8A S2A 1.738(3) . ? C8B N3B 1.301(4) . ? C8B S2B 1.733(3) . ? C8B S1B 1.735(3) . ? C9A S2A 1.794(4) . ? C9A H9A 0.96 . ? C9A H9B 0.96 . ? C9A H9C 0.96 . ? C9B S2B 1.796(4) . ? C9B H9D 0.96 . ? C9B H9E 0.96 . ? C9B H9F 0.96 . ? C10A C11A 1.382(5) . ? C10A H10A 0.93 . ? C10B C11B 1.372(5) . ? C10B H10B 0.93 . ? C11A C12A 1.332(7) . ? C11A H11A 0.93 . ? C11B C12B 1.351(7) . ? C11B H11B 0.93 . ? C12A C13A 1.362(8) . ? C12A H12A 0.93 . ? C12B C13B 1.363(7) . ? C12B H12B 0.93 . ? C13A N4A 1.360(6) . ? C13A H13A 0.93 . ? C13B N4B 1.352(5) . ? C13B H13B 0.93 . ? N1A Fe1 1.984(3) . ? N1B Fe1 1.984(2) . ? N2A N3A 1.384(3) . ? N2A Fe1 1.910(2) . ? N2B N3B 1.385(3) . ? N2B Fe1 1.912(2) . ? S1A Fe1 2.2255(9) . ? S1B Fe1 2.2273(9) . ? Cl1 O1G 1.301(14) . ? Cl1 O1D 1.326(6) . ? Cl1 O1E 1.350(13) . ? Cl1 O1B 1.366(6) . ? Cl1 O1A 1.398(3) . ? Cl1 O1C 1.407(7) . ? Cl1 O1F 1.489(12) . ? Cl2 O2G 1.298(15) . ? Cl2 O2J 1.32(2) . ? Cl2 O2L 1.33(2) . ? Cl2 O2C 1.333(6) . ? Cl2 O2E 1.346(15) . ? Cl2 O2F 1.391(15) . ? Cl2 O2D 1.402(5) . ? Cl2 O2B 1.431(5) . ? Cl2 O2A 1.450(6) . ? Cl2 O2K 1.47(2) . ? Cl2 O2I 1.498(16) . ? Cl2 O2H 1.601(16) . ? C1C N1C 1.336(5) . ? C1C C2C 1.369(7) . ? C1C H1C 0.93 . ? C2C C3C 1.374(8) . ? C2C H2C 0.93 . ? C3C C4C 1.371(6) . ? C3C H3C 0.93 . ? C4C C5C 1.379(5) . ? C4C H4C 0.93 . ? C5C N1C 1.337(5) . ? C5C C6C 1.489(5) . ? C6C N2C 1.306(4) . ? C6C C7C 1.431(5) . ? C7C N4C 1.372(4) . ? C7C C10C 1.389(5) . ? C8C N3C 1.279(4) . ? C8C N4C 1.412(4) . ? C8C S2C 1.740(3) . ? C9C S2C 1.798(5) . ? C9C H9G 0.96 . ? C9C H9H 0.96 . ? C9C H9I 0.96 . ? C10C C11C 1.363(6) . ? C10C H10C 0.93 . ? C11C C12C 1.380(6) . ? C11C H11C 0.93 . ? C12C C13C 1.344(6) . ? C12C H12C 0.93 . ? C13C N4C 1.368(5) . ? C13C H13C 0.93 . ? N2C N3C 1.368(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 N1A C1A C2A 121.0(4) . . ? N1A C1A H1A 119.5 . . ? C2A C1A H1A 119.5 . . ? N1B C1B C2B 122.3(3) . . ? N1B C1B H1B 118.9 . . ? C2B C1B H1B 118.9 . . ? C3A C2A C1A 120.4(4) . . ? C3A C2A H2A 119.8 . . ? C1A C2A H2A 119.8 . . ? C1B C2B C3B 118.6(3) . . ? C1B C2B H2B 120.7 . . ? C3B C2B H2B 120.7 . . ? C2A C3A C4A 119.2(3) . . ? C2A C3A H3A 120.4 . . ? C4A C3A H3A 120.4 . . ? C2B C3B C4B 120.0(3) . . ? C2B C3B H3B 120 . . ? C4B C3B H3B 120 . . ? C5A C4A C3A 118.5(3) . . ? C5A C4A H4A 120.7 . . ? C3A C4A H4A 120.7 . . ? C3B C4B C5B 119.3(3) . . ? C3B C4B H4B 120.3 . . ? C5B C4B H4B 120.3 . . ? N1A C5A C4A 121.3(3) . . ? N1A C5A C6A 113.4(3) . . ? C4A C5A C6A 125.2(3) . . ? N1B C5B C4B 120.5(3) . . ? N1B C5B C6B 113.2(3) . . ? C4B C5B C6B 126.2(3) . . ? N2A C6A C5A 112.8(3) . . ? N2A C6A C7A 124.0(3) . . ? C5A C6A C7A 123.1(3) . . ? N2B C6B C5B 112.7(3) . . ? N2B C6B C7B 123.9(3) . . ? C5B C6B C7B 123.4(3) . . ? N4A C7A C10A 123.8(3) . . ? N4A C7A C6A 115.2(3) . . ? C10A C7A C6A 120.9(3) . . ? N4B C7B C10B 123.2(3) . . ? N4B C7B C6B 115.8(3) . . ? C10B C7B C6B 121.0(3) . . ? N3A C8A S1A 125.7(2) . . ? N3A C8A S2A 119.2(2) . . ? S1A C8A S2A 115.04(18) . . ? N3B C8B S2B 119.2(2) . . ? N3B C8B S1B 125.3(2) . . ? S2B C8B S1B 115.46(19) . . ? S2A C9A H9A 109.5 . . ? S2A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? S2A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? S2B C9B H9D 109.5 . . ? S2B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? S2B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C7A C10A C11A 118.3(4) . . ? C7A C10A H10A 120.9 . . ? C11A C10A H10A 120.9 . . ? C11B C10B C7B 118.5(4) . . ? C11B C10B H10B 120.7 . . ? C7B C10B H10B 120.7 . . ? C12A C11A C10A 119.5(5) . . ? C12A C11A H11A 120.3 . . ? C10A C11A H11A 120.3 . . ? C12B C11B C10B 119.3(4) . . ? C12B C11B H11B 120.3 . . ? C10B C11B H11B 120.3 . . ? C11A C12A C13A 119.2(4) . . ? C11A C12A H12A 120.4 . . ? C13A C12A H12A 120.4 . . ? C11B C12B C13B 119.0(4) . . ? C11B C12B H12B 120.5 . . ? C13B C12B H12B 120.5 . . ? N4A C13A C12A 124.0(5) . . ? N4A C13A H13A 118 . . ? C12A C13A H13A 118 . . ? N4B C13B C12B 123.8(4) . . ? N4B C13B H13B 118.1 . . ? C12B C13B H13B 118.1 . . ? C1A N1A C5A 119.5(3) . . ? C1A N1A Fe1 126.1(2) . . ? C5A N1A Fe1 114.0(2) . . ? C1B N1B C5B 119.2(3) . . ? C1B N1B Fe1 126.8(2) . . ? C5B N1B Fe1 114.1(2) . . ? C6A N2A N3A 117.8(2) . . ? C6A N2A Fe1 119.2(2) . . ? N3A N2A Fe1 123.02(19) . . ? C6B N2B N3B 118.1(2) . . ? C6B N2B Fe1 119.3(2) . . ? N3B N2B Fe1 122.43(19) . . ? C8A N3A N2A 111.5(2) . . ? C8B N3B N2B 111.8(3) . . ? C7A N4A C13A 115.2(4) . . ? C7B N4B C13B 116.1(4) . . ? C8A S1A Fe1 94.38(11) . . ? C8B S1B Fe1 94.31(11) . . ? C8A S2A C9A 102.39(17) . . ? C8B S2B C9B 103.23(19) . . ? N2A Fe1 N2B 177.81(10) . . ? N2A Fe1 N1A 80.41(10) . . ? N2B Fe1 N1A 101.60(11) . . ? N2A Fe1 N1B 100.65(10) . . ? N2B Fe1 N1B 80.35(10) . . ? N1A Fe1 N1B 88.50(10) . . ? N2A Fe1 S1A 85.37(8) . . ? N2B Fe1 S1A 92.67(8) . . ? N1A Fe1 S1A 165.40(8) . . ? N1B Fe1 S1A 90.88(8) . . ? N2A Fe1 S1B 93.69(8) . . ? N2B Fe1 S1B 85.56(8) . . ? N1A Fe1 S1B 87.30(8) . . ? N1B Fe1 S1B 164.17(8) . . ? S1A Fe1 S1B 96.98(4) . . ? O1G Cl1 O1D 54.9(9) . . ? O1G Cl1 O1E 115.6(9) . . ? O1D Cl1 O1E 138.7(8) . . ? O1G Cl1 O1B 127.8(9) . . ? O1D Cl1 O1B 113.1(6) . . ? O1E Cl1 O1B 35.3(7) . . ? O1G Cl1 O1A 119.2(8) . . ? O1D Cl1 O1A 108.7(5) . . ? O1E Cl1 O1A 109.6(7) . . ? O1B Cl1 O1A 112.6(4) . . ? O1G Cl1 O1C 54.6(7) . . ? O1D Cl1 O1C 109.4(7) . . ? O1E Cl1 O1C 74.0(6) . . ? O1B Cl1 O1C 106.5(6) . . ? O1A Cl1 O1C 106.2(4) . . ? O1G Cl1 O1F 106.2(9) . . ? O1D Cl1 O1F 54.5(6) . . ? O1E Cl1 O1F 102.9(7) . . ? O1B Cl1 O1F 67.7(7) . . ? O1A Cl1 O1F 100.8(6) . . ? O1C Cl1 O1F 152.3(7) . . ? O2G Cl2 O2J 72.7(18) . . ? O2G Cl2 O2L 121.5(15) . . ? O2J Cl2 O2L 116.6(15) . . ? O2G Cl2 O2C 104.8(12) . . ? O2J Cl2 O2C 161.4(18) . . ? O2L Cl2 O2C 80.8(16) . . ? O2G Cl2 O2E 115.5(10) . . ? O2J Cl2 O2E 84.3(19) . . ? O2L Cl2 O2E 32.3(14) . . ? O2C Cl2 O2E 112.5(12) . . ? O2G Cl2 O2F 122.4(10) . . ? O2J Cl2 O2F 76.4(16) . . ? O2L Cl2 O2F 115.6(15) . . ? O2C Cl2 O2F 90.4(12) . . ? O2E Cl2 O2F 108.2(10) . . ? O2G Cl2 O2D 136.4(11) . . ? O2J Cl2 O2D 65.4(19) . . ? O2L Cl2 O2D 70.8(13) . . ? O2C Cl2 O2D 118.7(5) . . ? O2E Cl2 O2D 50.5(9) . . ? O2F Cl2 O2D 58.6(9) . . ? O2G Cl2 O2B 47.2(9) . . ? O2J Cl2 O2B 47.6(18) . . ? O2L Cl2 O2B 159.7(14) . . ? O2C Cl2 O2B 116.9(5) . . ? O2E Cl2 O2B 130.3(10) . . ? O2F Cl2 O2B 76.2(9) . . ? O2D Cl2 O2B 105.6(4) . . ? O2G Cl2 O2A 59.8(9) . . ? O2J Cl2 O2A 88.1(15) . . ? O2L Cl2 O2A 62.9(12) . . ? O2C Cl2 O2A 106.8(6) . . ? O2E Cl2 O2A 60.0(9) . . ? O2F Cl2 O2A 161.7(11) . . ? O2D Cl2 O2A 106.3(5) . . ? O2B Cl2 O2A 100.5(4) . . ? O2G Cl2 O2K 46.1(13) . . ? O2J Cl2 O2K 114.7(15) . . ? O2L Cl2 O2K 114.0(14) . . ? O2C Cl2 O2K 58.9(14) . . ? O2E Cl2 O2K 136.1(14) . . ? O2F Cl2 O2K 114.5(13) . . ? O2D Cl2 O2K 173.1(10) . . ? O2B Cl2 O2K 71.6(13) . . ? O2A Cl2 O2K 80.5(11) . . ? O2G Cl2 O2I 126.7(12) . . ? O2J Cl2 O2I 103.2(13) . . ? O2L Cl2 O2I 107.9(13) . . ? O2C Cl2 O2I 62.9(10) . . ? O2E Cl2 O2I 116.9(12) . . ? O2F Cl2 O2I 27.5(10) . . ? O2D Cl2 O2I 75.9(9) . . ? O2B Cl2 O2I 90.0(8) . . ? O2A Cl2 O2I 168.1(10) . . ? O2K Cl2 O2I 97.7(11) . . ? O2G Cl2 O2H 108.1(12) . . ? O2J Cl2 O2H 173.0(16) . . ? O2L Cl2 O2H 69.3(17) . . ? O2C Cl2 O2H 11.8(13) . . ? O2E Cl2 O2H 101.3(10) . . ? O2F Cl2 O2H 97.7(9) . . ? O2D Cl2 O2H 115.0(12) . . ? O2B Cl2 O2H 127.7(12) . . ? O2A Cl2 O2H 98.4(10) . . ? O2K Cl2 O2H 64.1(17) . . ? O2I Cl2 O2H 70.5(12) . . ? N1C C1C C2C 123.1(5) . . ? N1C C1C H1C 118.4 . . ? C2C C1C H1C 118.4 . . ? C1C C2C C3C 119.3(4) . . ? C1C C2C H2C 120.3 . . ? C3C C2C H2C 120.3 . . ? C4C C3C C2C 118.8(5) . . ? C4C C3C H3C 120.6 . . ? C2C C3C H3C 120.6 . . ? C3C C4C C5C 118.2(4) . . ? C3C C4C H4C 120.9 . . ? C5C C4C H4C 120.9 . . ? N1C C5C C4C 123.8(4) . . ? N1C C5C C6C 116.5(3) . . ? C4C C5C C6C 119.6(3) . . ? N2C C6C C7C 123.0(3) . . ? N2C C6C C5C 115.0(3) . . ? C7C C6C C5C 122.0(3) . . ? N4C C7C C10C 118.6(3) . . ? N4C C7C C6C 116.0(3) . . ? C10C C7C C6C 125.4(3) . . ? N3C C8C N4C 123.0(3) . . ? N3C C8C S2C 120.3(3) . . ? N4C C8C S2C 116.8(3) . . ? S2C C9C H9G 109.5 . . ? S2C C9C H9H 109.5 . . ? H9G C9C H9H 109.5 . . ? S2C C9C H9I 109.5 . . ? H9G C9C H9I 109.5 . . ? H9H C9C H9I 109.5 . . ? C11C C10C C7C 120.2(4) . . ? C11C C10C H10C 119.9 . . ? C7C C10C H10C 119.9 . . ? C10C C11C C12C 120.0(4) . . ? C10C C11C H11C 120 . . ? C12C C11C H11C 120 . . ? C13C C12C C11C 119.9(4) . . ? C13C C12C H12C 120 . . ? C11C C12C H12C 120 . . ? C12C C13C N4C 120.8(4) . . ? C12C C13C H13C 119.6 . . ? N4C C13C H13C 119.6 . . ? C1C N1C C5C 116.7(4) . . ? C6C N2C N3C 119.3(3) . . ? C8C N3C N2C 120.8(3) . . ? C13C N4C C7C 120.5(3) . . ? C13C N4C C8C 121.5(3) . . ? C7C N4C C8C 118.0(3) . . ? C8C S2C C9C 99.7(2) . . ? #===END #\#CIF_1.1 # [Fe(PSMC)(PCSMC)].Me2CO # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-11-22 at 15:16:23 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 689mb8 689abs struct data_689mb8 _database_code_depnum_ccdc_archive 'CCDC 858723' #TrackingRef '- supdata.cif' _audit_creation_date 2011-11-22T15:16:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H15 Fe1 N6 O1 S4, C3 H6 O' _chemical_formula_sum 'C19 H21 Fe N6 O2 S4' _chemical_formula_weight 549.51 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting TRIGONAL _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 36.376(5) _cell_length_b 36.376(5) _cell_length_c 9.3420(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 10705(2) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1027 _cell_measurement_theta_min 2.9668 _cell_measurement_theta_max 28.9851 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4184 _exptl_crystal_size_mid 0.1823 _exptl_crystal_size_min 0.1251 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5094 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -2 0 0.0758 -1 2 0 0.0493 2 1 0 0.0551 -2 -1 0 0.076 -3 0 2 0.1814 -1 -1 -2 0.1614 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.000 0.000 6 1 ' ' 2 0.000 0.000 0.500 8 2 ' ' 3 0.000 0.333 0.524 372 96 ' ' 4 0.000 0.667 0.735 372 96 ' ' 5 0.333 1.000 0.514 372 96 ' ' 6 0.333 0.333 0.144 371 96 ' ' 7 0.333 0.667 0.167 8 2 ' ' 8 0.333 0.667 0.667 7 1 ' ' 9 0.667 0.667 0.181 371 96 ' ' 10 0.667 0.000 0.811 372 96 ' ' 11 0.667 0.333 0.333 7 1 ' ' 12 0.667 0.333 0.833 9 2 ' ' _platon_squeeze_details ; A single acetone molecule in the asymmetric unit was modelled as a diffuse contribution to the overall scattering without specific atom positions using SQUEEZE/PLATON. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.987 _exptl_absorpt_correction_T_max 0.994 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.0696 _diffrn_orient_matrix_ub_11 -0.017624 _diffrn_orient_matrix_ub_12 -0.0142778 _diffrn_orient_matrix_ub_13 -0.0421467 _diffrn_orient_matrix_ub_21 -0.0070173 _diffrn_orient_matrix_ub_22 0.0150173 _diffrn_orient_matrix_ub_23 -0.0031015 _diffrn_orient_matrix_ub_31 0.0121256 _diffrn_orient_matrix_ub_32 0.0088153 _diffrn_orient_matrix_ub_33 -0.0630535 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_unetI/netI 0.1472 _diffrn_reflns_number 8404 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 4169 _reflns_number_gt 2072 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1243P)^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_number_reflns 4169 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1707 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2546 _refine_ls_wR_factor_gt 0.216 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.858 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.124 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 C1A C 0.8821(3) 0.0648(3) -0.2140(9) 0.060(3) Uani 1 1 d . . . H1A H 0.8977 0.0831 -0.1403 0.072 Uiso 1 1 calc R . . C1B C 0.7658(3) 0.0382(4) -0.0610(11) 0.072(3) Uani 1 1 d . . . H1B H 0.7514 0.0149 -0.1209 0.086 Uiso 1 1 calc R . . C2A C 0.8951(4) 0.0765(4) -0.3534(11) 0.087(4) Uani 1 1 d . . . H2A H 0.9191 0.1025 -0.3736 0.104 Uiso 1 1 calc R . . C2B C 0.7513(4) 0.0677(4) -0.0449(14) 0.090(4) Uani 1 1 d . . . H2B H 0.728 0.0644 -0.0968 0.108 Uiso 1 1 calc R . . C3A C 0.8722(4) 0.0491(4) -0.4618(10) 0.097(4) Uani 1 1 d . . . H3A H 0.88 0.0566 -0.5568 0.117 Uiso 1 1 calc R . . C3B C 0.7716(4) 0.1007(4) 0.0465(13) 0.086(4) Uani 1 1 d . . . H3B H 0.7616 0.1194 0.0611 0.103 Uiso 1 1 calc R . . C4A C 0.8369(3) 0.0100(4) -0.4278(10) 0.073(3) Uani 1 1 d . . . H4A H 0.8215 -0.0096 -0.4991 0.088 Uiso 1 1 calc R . . C4B C 0.8069(3) 0.1065(3) 0.1173(11) 0.073(3) Uani 1 1 d . . . H4B H 0.8214 0.1295 0.1788 0.087 Uiso 1 1 calc R . . C5A C 0.8257(3) 0.0012(3) -0.2879(8) 0.049(2) Uani 1 1 d . . . C5B C 0.8209(3) 0.0782(3) 0.0970(9) 0.049(2) Uani 1 1 d . . . C6A C 0.7885(3) -0.0398(3) -0.2450(9) 0.057(3) Uani 1 1 d . . . C6B C 0.8569(3) 0.0809(3) 0.1643(8) 0.047(2) Uani 1 1 d . . . H6B H 0.8736 0.1028 0.2269 0.056 Uiso 1 1 calc R . . C8A C 0.7503(3) -0.0737(3) 0.0981(10) 0.059(3) Uani 1 1 d . . . C8B C 0.9045(3) 0.0221(3) 0.1570(9) 0.047(2) Uani 1 1 d . . . C9A C 0.7123(5) -0.1049(4) 0.3582(13) 0.147(7) Uani 1 1 d . . . H9A H 0.6913 -0.1284 0.4129 0.221 Uiso 1 1 calc R . . H9B H 0.7065 -0.0819 0.3623 0.221 Uiso 1 1 calc R . . H9C H 0.7399 -0.0958 0.3972 0.221 Uiso 1 1 calc R . . C9B C 0.9733(3) 0.0608(4) 0.3328(10) 0.082(3) Uani 1 1 d . . . H9D H 0.9969 0.0605 0.3768 0.123 Uiso 1 1 calc R . . H9E H 0.9545 0.0604 0.4057 0.123 Uiso 1 1 calc R . . H9F H 0.9833 0.086 0.2761 0.123 Uiso 1 1 calc R . . N1A N 0.8482(2) 0.0283(2) -0.1819(6) 0.0457(18) Uani 1 1 d . . . N1B N 0.8004(2) 0.0443(2) 0.0109(7) 0.0506(19) Uani 1 1 d . . . N2A N 0.7837(2) -0.0405(2) -0.0985(7) 0.0474(18) Uani 1 1 d . . . N2B N 0.8652(2) 0.0516(2) 0.1350(6) 0.0425(17) Uani 1 1 d . . . N3A N 0.7517(2) -0.0766(2) -0.0391(8) 0.054(2) Uani 1 1 d . . . N3B N 0.8994(2) 0.0523(2) 0.1986(7) 0.0457(18) Uani 1 1 d . . . O1A O 0.7659(2) -0.0683(2) -0.3305(6) 0.071(2) Uani 1 1 d . . . S1A S 0.78570(8) -0.03026(7) 0.1986(2) 0.0558(7) Uani 1 1 d . . . S1B S 0.87266(8) -0.01631(8) 0.0309(2) 0.0571(7) Uani 1 1 d . . . S2A S 0.71056(12) -0.12056(10) 0.1798(3) 0.1054(13) Uani 1 1 d . . . S2B S 0.94566(10) 0.01541(11) 0.2217(3) 0.0842(9) Uani 1 1 d . . . Fe1 Fe 0.82497(4) 0.00620(4) 0.01207(11) 0.0435(4) 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 C1A 0.057(6) 0.056(6) 0.040(5) 0.006(4) 0.010(5) 0.008(5) C1B 0.056(7) 0.086(8) 0.080(7) -0.007(6) -0.003(6) 0.040(6) C2A 0.076(8) 0.079(8) 0.073(8) 0.011(6) 0.035(6) 0.013(7) C2B 0.078(9) 0.103(10) 0.120(10) 0.017(9) -0.009(8) 0.068(8) C3A 0.122(11) 0.108(10) 0.030(5) -0.014(6) 0.000(6) 0.033(9) C3B 0.096(10) 0.073(9) 0.109(10) 0.021(7) 0.031(8) 0.058(8) C4A 0.070(8) 0.079(8) 0.051(6) -0.012(6) -0.002(5) 0.022(7) C4B 0.055(7) 0.075(8) 0.093(8) 0.010(6) 0.009(6) 0.036(6) C5A 0.067(6) 0.058(6) 0.027(4) 0.003(4) 0.001(4) 0.035(5) C5B 0.059(6) 0.042(6) 0.053(5) 0.003(4) 0.010(5) 0.031(5) C6A 0.056(6) 0.073(7) 0.034(5) -0.007(5) -0.007(5) 0.027(6) C6B 0.058(6) 0.040(5) 0.037(5) -0.005(4) 0.001(4) 0.020(5) C8A 0.060(7) 0.040(6) 0.056(6) 0.013(4) 0.016(5) 0.009(5) C8B 0.045(6) 0.038(5) 0.056(5) 0.014(4) 0.010(4) 0.018(5) C9A 0.145(13) 0.081(10) 0.118(11) 0.017(8) 0.076(10) -0.017(9) C9B 0.068(7) 0.119(10) 0.063(6) -0.007(6) -0.020(5) 0.049(7) N1A 0.053(5) 0.052(5) 0.026(4) -0.003(3) 0.004(3) 0.022(4) N1B 0.049(5) 0.051(5) 0.050(4) 0.013(4) 0.005(4) 0.024(4) N2A 0.039(4) 0.048(5) 0.047(4) -0.010(3) -0.001(3) 0.015(4) N2B 0.050(5) 0.039(4) 0.036(4) 0.001(3) 0.010(3) 0.020(4) N3A 0.040(5) 0.052(5) 0.055(5) 0.000(4) 0.005(4) 0.012(4) N3B 0.051(5) 0.044(5) 0.045(4) 0.001(3) 0.004(4) 0.025(4) O1A 0.071(5) 0.071(5) 0.055(4) -0.017(4) -0.023(4) 0.025(4) S1A 0.0690(17) 0.0486(15) 0.0386(12) 0.0037(11) 0.0101(11) 0.0209(13) S1B 0.0659(17) 0.0543(16) 0.0553(14) -0.0091(12) -0.0033(12) 0.0332(14) S2A 0.112(3) 0.064(2) 0.078(2) 0.0071(16) 0.0303(19) -0.0024(19) S2B 0.080(2) 0.094(2) 0.095(2) 0.0048(18) -0.0155(17) 0.0550(19) Fe1 0.0477(8) 0.0416(8) 0.0357(7) -0.0023(5) 0.0027(6) 0.0182(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1A 1.316(10) . ? C1A C2A 1.379(12) . ? C1A H1A 0.93 . ? C1B N1B 1.343(11) . ? C1B C2B 1.421(15) . ? C1B H1B 0.93 . ? C2A C3A 1.372(14) . ? C2A H2A 0.93 . ? C2B C3B 1.352(16) . ? C2B H2B 0.93 . ? C3A C4A 1.395(15) . ? C3A H3A 0.93 . ? C3B C4B 1.363(15) . ? C3B H3B 0.93 . ? C4A C5A 1.359(12) . ? C4A H4A 0.93 . ? C4B C5B 1.372(12) . ? C4B H4B 0.93 . ? C5A N1A 1.348(10) . ? C5A C6A 1.482(13) . ? C5B N1B 1.344(11) . ? C5B C6B 1.409(12) . ? C6A O1A 1.239(10) . ? C6A N2A 1.379(10) . ? C6B N2B 1.273(10) . ? C6B H6B 0.93 . ? C8A N3A 1.289(10) . ? C8A S1A 1.732(10) . ? C8A S2A 1.765(9) . ? C8B N3B 1.261(10) . ? C8B S2B 1.740(9) . ? C8B S1B 1.751(9) . ? C9A S2A 1.753(13) . ? C9A H9A 0.96 . ? C9A H9B 0.96 . ? C9A H9C 0.96 . ? C9B S2B 1.776(10) . ? C9B H9D 0.96 . ? C9B H9E 0.96 . ? C9B H9F 0.96 . ? N1A Fe1 1.992(6) . ? N1B Fe1 1.990(7) . ? N2A N3A 1.365(9) . ? N2A Fe1 1.911(7) . ? N2B N3B 1.369(9) . ? N2B Fe1 1.942(7) . ? S1A Fe1 2.223(2) . ? S1B Fe1 2.265(3) . ? 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 N1A C1A C2A 122.1(9) . . ? N1A C1A H1A 118.9 . . ? C2A C1A H1A 118.9 . . ? N1B C1B C2B 119.6(11) . . ? N1B C1B H1B 120.2 . . ? C2B C1B H1B 120.2 . . ? C3A C2A C1A 118.8(10) . . ? C3A C2A H2A 120.6 . . ? C1A C2A H2A 120.6 . . ? C3B C2B C1B 119.4(11) . . ? C3B C2B H2B 120.3 . . ? C1B C2B H2B 120.3 . . ? C2A C3A C4A 119.2(9) . . ? C2A C3A H3A 120.4 . . ? C4A C3A H3A 120.4 . . ? C2B C3B C4B 120.0(11) . . ? C2B C3B H3B 120 . . ? C4B C3B H3B 120 . . ? C5A C4A C3A 118.3(10) . . ? C5A C4A H4A 120.9 . . ? C3A C4A H4A 120.9 . . ? C3B C4B C5B 119.4(11) . . ? C3B C4B H4B 120.3 . . ? C5B C4B H4B 120.3 . . ? N1A C5A C4A 122.2(9) . . ? N1A C5A C6A 117.0(7) . . ? C4A C5A C6A 120.8(9) . . ? N1B C5B C4B 121.8(9) . . ? N1B C5B C6B 113.7(8) . . ? C4B C5B C6B 124.5(9) . . ? O1A C6A N2A 126.9(9) . . ? O1A C6A C5A 123.9(8) . . ? N2A C6A C5A 109.2(8) . . ? N2B C6B C5B 116.6(8) . . ? N2B C6B H6B 121.7 . . ? C5B C6B H6B 121.7 . . ? N3A C8A S1A 124.9(7) . . ? N3A C8A S2A 113.4(7) . . ? S1A C8A S2A 121.6(5) . . ? N3B C8B S2B 121.7(7) . . ? N3B C8B S1B 125.1(7) . . ? S2B C8B S1B 113.2(5) . . ? S2A C9A H9A 109.5 . . ? S2A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? S2A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? S2B C9B H9D 109.5 . . ? S2B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? S2B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C1A N1A C5A 119.4(7) . . ? C1A N1A Fe1 127.5(6) . . ? C5A N1A Fe1 113.1(6) . . ? C1B N1B C5B 119.7(8) . . ? C1B N1B Fe1 126.8(7) . . ? C5B N1B Fe1 113.4(6) . . ? N3A N2A C6A 117.3(7) . . ? N3A N2A Fe1 123.3(5) . . ? C6A N2A Fe1 119.0(6) . . ? C6B N2B N3B 119.1(7) . . ? C6B N2B Fe1 116.4(6) . . ? N3B N2B Fe1 124.3(5) . . ? C8A N3A N2A 112.0(7) . . ? C8B N3B N2B 112.2(7) . . ? C8A S1A Fe1 94.7(3) . . ? C8B S1B Fe1 94.8(3) . . ? C9A S2A C8A 102.6(5) . . ? C8B S2B C9B 101.5(5) . . ? N2A Fe1 N2B 176.5(3) . . ? N2A Fe1 N1B 100.9(3) . . ? N2B Fe1 N1B 79.7(3) . . ? N2A Fe1 N1A 81.6(3) . . ? N2B Fe1 N1A 102.0(3) . . ? N1B Fe1 N1A 87.8(3) . . ? N2A Fe1 S1A 84.8(2) . . ? N2B Fe1 S1A 91.74(19) . . ? N1B Fe1 S1A 92.4(2) . . ? N1A Fe1 S1A 166.1(2) . . ? N2A Fe1 S1B 97.1(2) . . ? N2B Fe1 S1B 82.8(2) . . ? N1B Fe1 S1B 160.8(2) . . ? N1A Fe1 S1B 88.3(2) . . ? S1A Fe1 S1B 95.93(10) . . ? #===END