# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nasser Safari' _publ_contact_author_email n-safari@cc.sbu.ac.ir loop_ _publ_author_name 'A. Abedi' 'N. Safari' 'V. Amani' 'H. R. Khavasi' data_kh161-abs1 _database_code_depnum_ccdc_archive 'CCDC 767148' #TrackingRef 'kh161-abs1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cl8 Fe3 N6 S6' _chemical_formula_weight 1040.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 12.6728(19) _cell_length_b 12.6728(19) _cell_length_c 42.174(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5865.7(16) _cell_formula_units_Z 6 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.994 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.350 _exptl_absorpt_correction_T_max 0.372 _exptl_absorpt_process_details 'shape of crystal determined optically' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean '0.15 mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5060 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.86 _reflns_number_total 1515 _reflns_number_gt 1473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_cell_refinement 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_data_reduction 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Step32 1.07e (Stoe & Cie GmbH, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0319P)^2^+29.7417P] 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 SHELXL _refine_ls_extinction_coef 0.0010(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1515 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 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 0.6667 0.3333 0.0833 0.01399(19) Uani 1 6 d S . . Fe2 Fe 1.0000 1.0000 0.094870(13) 0.02058(18) Uani 1 3 d S . . C1 C 0.70789(18) 0.58900(18) 0.06962(5) 0.0164(4) Uani 1 1 d . . . C2 C 0.7545(2) 0.69751(19) 0.05434(5) 0.0212(4) Uani 1 1 d . . . H2 H 0.7384 0.7594 0.0595 0.025 Uiso 1 1 calc R . . C3 C 0.81918(19) 0.55967(19) 0.03370(5) 0.0182(4) Uani 1 1 d . . . C4 C 0.8793(2) 0.5031(2) 0.01552(5) 0.0246(5) Uani 1 1 d . . . H4A H 0.9662 0.5527 0.0175 0.030 Uiso 1 1 calc R . . H4B H 0.8570 0.4970 -0.0064 0.030 Uiso 1 1 calc R . . H4C H 0.8535 0.4232 0.0238 0.030 Uiso 1 1 calc R . . N1 N 0.74455(15) 0.50994(16) 0.05786(4) 0.0158(3) Uani 1 1 d . . . Cl1 Cl 1.13935(6) 1.18140(5) 0.111798(14) 0.03033(19) Uani 1 1 d . . . Cl2 Cl 1.0000 1.0000 0.04263(2) 0.0223(2) Uani 1 3 d S . . S1 S 0.84766(5) 0.70297(5) 0.024205(13) 0.02358(17) 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 Fe1 0.0126(2) 0.0126(2) 0.0169(3) 0.000 0.000 0.00628(12) Fe2 0.0213(2) 0.0213(2) 0.0191(3) 0.000 0.000 0.01065(11) C1 0.0163(9) 0.0159(9) 0.0175(9) -0.0013(7) 0.0001(7) 0.0083(7) C2 0.0239(10) 0.0171(9) 0.0235(10) 0.0016(8) 0.0060(8) 0.0109(8) C3 0.0169(9) 0.0171(9) 0.0195(9) 0.0007(7) 0.0012(7) 0.0077(8) C4 0.0284(11) 0.0249(11) 0.0253(10) 0.0052(9) 0.0106(9) 0.0168(9) N1 0.0147(8) 0.0153(8) 0.0175(7) 0.0009(6) 0.0010(6) 0.0076(6) Cl1 0.0308(3) 0.0251(3) 0.0307(3) -0.0044(2) -0.0083(2) 0.0107(2) Cl2 0.0235(3) 0.0235(3) 0.0200(4) 0.000 0.000 0.01174(15) S1 0.0283(3) 0.0172(3) 0.0250(3) 0.0057(2) 0.0108(2) 0.0112(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.2198(18) 17_654 ? Fe1 N1 2.2199(18) 18_554 ? Fe1 N1 2.2199(18) 15_544 ? Fe1 N1 2.2199(18) 4_665 ? Fe1 N1 2.2199(18) 2_655 ? Fe1 N1 2.2199(18) . ? Fe2 Cl1 2.2030(7) . ? Fe2 Cl1 2.2030(7) 2_765 ? Fe2 Cl1 2.2030(7) 4_675 ? Fe2 Cl2 2.2032(11) . ? C1 C2 1.357(3) . ? C1 N1 1.390(3) . ? C1 C1 1.469(4) 17_654 ? C2 S1 1.712(2) . ? C2 H2 0.9300 . ? C3 N1 1.317(3) . ? C3 C4 1.493(3) . ? C3 S1 1.713(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 Fe1 N1 98.56(6) 17_654 18_554 ? N1 Fe1 N1 98.56(6) 17_654 15_544 ? N1 Fe1 N1 98.56(6) 18_554 15_544 ? N1 Fe1 N1 173.18(9) 17_654 4_665 ? N1 Fe1 N1 86.83(9) 18_554 4_665 ? N1 Fe1 N1 76.40(9) 15_544 4_665 ? N1 Fe1 N1 86.83(9) 17_654 2_655 ? N1 Fe1 N1 76.40(9) 18_554 2_655 ? N1 Fe1 N1 173.18(9) 15_544 2_655 ? N1 Fe1 N1 98.56(6) 4_665 2_655 ? N1 Fe1 N1 76.40(9) 17_654 . ? N1 Fe1 N1 173.18(9) 18_554 . ? N1 Fe1 N1 86.83(9) 15_544 . ? N1 Fe1 N1 98.56(6) 4_665 . ? N1 Fe1 N1 98.56(6) 2_655 . ? Cl1 Fe2 Cl1 110.03(2) . 2_765 ? Cl1 Fe2 Cl1 110.03(2) . 4_675 ? Cl1 Fe2 Cl1 110.03(2) 2_765 4_675 ? Cl1 Fe2 Cl2 108.91(2) . . ? Cl1 Fe2 Cl2 108.91(2) 2_765 . ? Cl1 Fe2 Cl2 108.91(2) 4_675 . ? C2 C1 N1 115.34(17) . . ? C2 C1 C1 127.32(12) . 17_654 ? N1 C1 C1 117.34(11) . 17_654 ? C1 C2 S1 109.60(16) . . ? C1 C2 H2 125.2 . . ? S1 C2 H2 125.2 . . ? N1 C3 C4 125.77(19) . . ? N1 C3 S1 114.12(16) . . ? C4 C3 S1 120.09(15) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 N1 C1 110.48(17) . . ? C3 N1 Fe1 135.06(14) . . ? C1 N1 Fe1 114.45(13) . . ? C2 S1 C3 90.45(10) . . ? 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 N1 C1 C2 S1 0.0(2) . . . . ? C1 C1 C2 S1 179.1(2) 17_654 . . . ? C4 C3 N1 C1 178.5(2) . . . . ? S1 C3 N1 C1 -0.1(2) . . . . ? C4 C3 N1 Fe1 -1.4(3) . . . . ? S1 C3 N1 Fe1 179.98(11) . . . . ? C2 C1 N1 C3 0.1(3) . . . . ? C1 C1 N1 C3 -179.1(2) 17_654 . . . ? C2 C1 N1 Fe1 -179.98(15) . . . . ? C1 C1 N1 Fe1 0.8(3) 17_654 . . . ? N1 Fe1 N1 C3 179.6(2) 17_654 . . . ? N1 Fe1 N1 C3 -137.6(2) 18_554 . . . ? N1 Fe1 N1 C3 80.0(2) 15_544 . . . ? N1 Fe1 N1 C3 4.3(2) 4_665 . . . ? N1 Fe1 N1 C3 -95.79(17) 2_655 . . . ? N1 Fe1 N1 C1 -0.28(10) 17_654 . . . ? N1 Fe1 N1 C1 42.50(13) 18_554 . . . ? N1 Fe1 N1 C1 -99.88(15) 15_544 . . . ? N1 Fe1 N1 C1 -175.60(13) 4_665 . . . ? N1 Fe1 N1 C1 84.33(17) 2_655 . . . ? C1 C2 S1 C3 -0.04(17) . . . . ? N1 C3 S1 C2 0.10(18) . . . . ? C4 C3 S1 C2 -178.63(19) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.546 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.072 # Attachment 'kh296-lt.cif' data_kh296-lt _database_code_depnum_ccdc_archive 'CCDC 767149' #TrackingRef 'kh296-lt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Fe N6 S6, 2(Br4 Fe)' _chemical_formula_sum 'C24 H24 Br8 Fe3 N6 S6' _chemical_formula_weight 1395.66 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' Br Br -0.2901 2.4595 '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' 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 12.8209(7) _cell_length_b 12.8209(7) _cell_length_c 43.002(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6121.4(6) _cell_formula_units_Z 6 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 29.19 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 9.220 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.118 _exptl_absorpt_correction_T_max 0.178 _exptl_absorpt_process_details 'shape of crystal determined optically' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean '0.15 mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7524 _diffrn_reflns_av_R_equivalents 0.1142 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 29.19 _reflns_number_total 1852 _reflns_number_gt 1657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_cell_refinement 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_data_reduction 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0312P)^2^+28.7401P] 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 1852 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 -0.0426(4) 0.7923(4) 0.18320(9) 0.0228(7) Uani 1 1 d . . . H1A H -0.1075 0.7387 0.1965 0.034 Uiso 1 1 calc R . . H1B H -0.0357 0.7476 0.1662 0.034 Uiso 1 1 calc R . . H1C H -0.0584 0.8530 0.1753 0.034 Uiso 1 1 calc R . . C2 C 0.0721(3) 0.8506(3) 0.20120(8) 0.0179(6) Uani 1 1 d . . . C3 C 0.2102(3) 0.9594(3) 0.23667(8) 0.0162(6) Uani 1 1 d . . . C4 C 0.2719(4) 0.9133(4) 0.22167(9) 0.0226(7) Uani 1 1 d . . . H4 H 0.3488 0.9288 0.2268 0.027 Uiso 1 1 calc R . . Br1 Br 1.0000 1.0000 0.041083(14) 0.01980(15) Uani 1 3 d S . . Br2 Br 0.80980(4) 0.85082(4) 0.112394(9) 0.02596(13) Uani 1 1 d . . . Fe1 Fe 0.0000 1.0000 0.2500 0.0133(2) Uani 1 6 d S . . Fe2 Fe 1.0000 1.0000 0.09530(2) 0.01822(19) Uani 1 3 d S . . N1 N 0.0964(3) 0.9235(3) 0.22502(7) 0.0156(5) Uani 1 1 d . . . S1 S 0.18574(9) 0.82270(10) 0.19201(2) 0.0233(2) 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 0.0230(17) 0.0262(18) 0.0205(17) -0.0068(14) -0.0057(14) 0.0132(15) C2 0.0181(15) 0.0198(15) 0.0188(15) -0.0020(13) -0.0028(13) 0.0116(13) C3 0.0183(15) 0.0158(14) 0.0153(15) -0.0013(12) -0.0027(12) 0.0091(12) C4 0.0210(16) 0.0259(18) 0.0234(17) -0.0049(15) -0.0038(14) 0.0135(15) Br1 0.0226(2) 0.0226(2) 0.0142(3) 0.000 0.000 0.01131(10) Br2 0.0222(2) 0.0274(2) 0.0238(2) 0.00684(15) 0.00254(14) 0.00909(16) Fe1 0.0135(3) 0.0135(3) 0.0128(5) 0.000 0.000 0.00677(15) Fe2 0.0202(3) 0.0202(3) 0.0143(4) 0.000 0.000 0.01008(13) N1 0.0166(13) 0.0156(13) 0.0140(12) -0.0026(11) -0.0024(11) 0.0077(11) S1 0.0257(4) 0.0310(5) 0.0205(4) -0.0113(4) -0.0059(4) 0.0196(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.490(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.315(4) . ? C2 S1 1.711(4) . ? C3 C4 1.363(5) . ? C3 N1 1.385(5) . ? C3 C3 1.459(7) 6_675 ? C4 S1 1.707(4) . ? C4 H4 0.9300 . ? Br1 Fe2 2.3312(11) . ? Br2 Fe2 2.3412(5) . ? Fe1 N1 2.204(3) 4_465 ? Fe1 N1 2.204(3) 2_675 ? Fe1 N1 2.204(3) . ? Fe1 N1 2.204(3) 3_465 ? Fe1 N1 2.204(3) 6_675 ? Fe1 N1 2.204(3) 5 ? Fe2 Br2 2.3412(5) 4_675 ? Fe2 Br2 2.3412(5) 2_765 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 125.8(3) . . ? N1 C2 S1 113.9(3) . . ? C1 C2 S1 120.3(3) . . ? C4 C3 N1 115.3(3) . . ? C4 C3 C3 127.1(2) . 6_675 ? N1 C3 C3 117.51(18) . 6_675 ? C3 C4 S1 109.3(3) . . ? C3 C4 H4 125.4 . . ? S1 C4 H4 125.4 . . ? N1 Fe1 N1 98.26(10) 4_465 2_675 ? N1 Fe1 N1 98.26(10) 4_465 . ? N1 Fe1 N1 98.26(10) 2_675 . ? N1 Fe1 N1 86.98(16) 4_465 3_465 ? N1 Fe1 N1 76.83(15) 2_675 3_465 ? N1 Fe1 N1 173.35(16) . 3_465 ? N1 Fe1 N1 173.35(16) 4_465 6_675 ? N1 Fe1 N1 86.98(16) 2_675 6_675 ? N1 Fe1 N1 76.83(15) . 6_675 ? N1 Fe1 N1 98.26(10) 3_465 6_675 ? N1 Fe1 N1 76.83(15) 4_465 5 ? N1 Fe1 N1 173.35(16) 2_675 5 ? N1 Fe1 N1 86.98(16) . 5 ? N1 Fe1 N1 98.26(10) 3_465 5 ? N1 Fe1 N1 98.26(10) 6_675 5 ? Br1 Fe2 Br2 108.30(2) . . ? Br1 Fe2 Br2 108.30(2) . 4_675 ? Br2 Fe2 Br2 110.61(2) . 4_675 ? Br1 Fe2 Br2 108.30(2) . 2_765 ? Br2 Fe2 Br2 110.61(2) . 2_765 ? Br2 Fe2 Br2 110.61(2) 4_675 2_765 ? C2 N1 C3 110.7(3) . . ? C2 N1 Fe1 135.2(3) . . ? C3 N1 Fe1 114.1(2) . . ? C4 S1 C2 90.80(18) . . ? 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 N1 C3 C4 S1 0.2(4) . . . . ? C3 C3 C4 S1 179.9(4) 6_675 . . . ? C1 C2 N1 C3 178.8(4) . . . . ? S1 C2 N1 C3 0.0(4) . . . . ? C1 C2 N1 Fe1 -1.3(6) . . . . ? S1 C2 N1 Fe1 179.91(19) . . . . ? C4 C3 N1 C2 -0.1(4) . . . . ? C3 C3 N1 C2 -179.8(4) 6_675 . . . ? C4 C3 N1 Fe1 179.9(3) . . . . ? C3 C3 N1 Fe1 0.2(5) 6_675 . . . ? N1 Fe1 N1 C2 4.6(4) 4_465 . . . ? N1 Fe1 N1 C2 -95.1(3) 2_675 . . . ? N1 Fe1 N1 C2 -137.1(3) 3_465 . . . ? N1 Fe1 N1 C2 -180.0(4) 6_675 . . . ? N1 Fe1 N1 C2 80.8(3) 5 . . . ? N1 Fe1 N1 C3 -175.5(2) 4_465 . . . ? N1 Fe1 N1 C3 84.8(3) 2_675 . . . ? N1 Fe1 N1 C3 42.8(2) 3_465 . . . ? N1 Fe1 N1 C3 -0.08(17) 6_675 . . . ? N1 Fe1 N1 C3 -99.3(3) 5 . . . ? C3 C4 S1 C2 -0.1(3) . . . . ? N1 C2 S1 C4 0.1(3) . . . . ? C1 C2 S1 C4 -178.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.669 _refine_diff_density_min -1.555 _refine_diff_density_rms 0.148 # Attachment 'kh296-lt90.cif' data_kh296-lt90 _database_code_depnum_ccdc_archive 'CCDC 767150' #TrackingRef 'kh296-lt90.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Fe N6 S6, 2(Br4 Fe)' _chemical_formula_sum 'C24 H24 Br8 Fe3 N6 S6' _chemical_formula_weight 1395.66 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' Br Br -0.2901 2.4595 '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' 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 12.8035(6) _cell_length_b 12.8035(6) _cell_length_c 43.027(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6108.4(6) _cell_formula_units_Z 6 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 998 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 29.21 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 9.240 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.119 _exptl_absorpt_correction_T_max 0.161 _exptl_absorpt_process_details 'shape of crystal determined optically' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean '0.15 mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7109 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 29.21 _reflns_number_total 1836 _reflns_number_gt 1673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_cell_refinement 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_data_reduction 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0192P)^2^+31.4423P] 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 1836 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.4595(3) 0.2910(3) 0.15027(7) 0.0184(6) Uani 1 1 d . . . H1A H 0.4079 0.2256 0.1368 0.028 Uiso 1 1 calc R . . H1B H 0.4127 0.2968 0.1669 0.028 Uiso 1 1 calc R . . H1C H 0.5207 0.2767 0.1587 0.028 Uiso 1 1 calc R . . C2 C 0.5173(3) 0.4056(3) 0.13231(6) 0.0140(5) Uani 1 1 d . . . C3 C 0.6260(2) 0.5441(3) 0.09665(6) 0.0129(5) Uani 1 1 d . . . C4 C 0.5801(3) 0.6054(3) 0.11184(7) 0.0171(6) Uani 1 1 d . . . H4 H 0.5959 0.6826 0.1068 0.021 Uiso 1 1 calc R . . Br1 Br 0.14953(3) 0.19044(3) 0.112440(7) 0.02011(9) Uani 1 1 d . . . Br2 Br 0.0000 0.0000 0.041037(11) 0.01547(11) Uani 1 3 d S . . Fe1 Fe 0.6667 0.3333 0.0833 0.01069(18) Uani 1 6 d S . . Fe2 Fe 0.0000 0.0000 0.095309(16) 0.01430(15) Uani 1 3 d S . . N1 N 0.5903(2) 0.4301(2) 0.10840(5) 0.0123(4) Uani 1 1 d . . . S1 S 0.48927(7) 0.51941(7) 0.141496(17) 0.01842(15) 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 0.0196(14) 0.0186(14) 0.0180(13) 0.0044(11) 0.0056(11) 0.0103(12) C2 0.0141(12) 0.0151(12) 0.0143(12) 0.0027(10) 0.0011(10) 0.0085(10) C3 0.0121(12) 0.0132(12) 0.0133(12) 0.0005(10) 0.0001(10) 0.0063(10) C4 0.0212(14) 0.0159(13) 0.0172(13) 0.0030(11) 0.0030(11) 0.0115(12) Br1 0.02096(16) 0.01685(15) 0.01911(14) -0.00182(11) -0.00501(12) 0.00689(12) Br2 0.01730(15) 0.01730(15) 0.0118(2) 0.000 0.000 0.00865(7) Fe1 0.0104(2) 0.0104(2) 0.0113(4) 0.000 0.000 0.00518(12) Fe2 0.0155(2) 0.0155(2) 0.0119(3) 0.000 0.000 0.00775(10) N1 0.0114(11) 0.0117(11) 0.0129(10) 0.0003(9) -0.0001(9) 0.0051(9) S1 0.0240(4) 0.0196(3) 0.0172(3) 0.0048(3) 0.0088(3) 0.0151(3) _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 C2 1.487(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.318(4) . ? C2 S1 1.712(3) . ? C3 C4 1.360(4) . ? C3 N1 1.389(4) . ? C3 C3 1.459(5) 17_654 ? C4 S1 1.706(3) . ? C4 H4 0.9300 . ? Br1 Fe2 2.3422(4) . ? Br2 Fe2 2.3351(8) . ? Fe1 N1 2.206(2) 4_665 ? Fe1 N1 2.206(2) 2_655 ? Fe1 N1 2.206(2) . ? Fe1 N1 2.206(2) 17_654 ? Fe1 N1 2.206(2) 18_554 ? Fe1 N1 2.206(2) 15_544 ? Fe2 Br1 2.3422(4) 2 ? Fe2 Br1 2.3422(4) 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 125.8(3) . . ? N1 C2 S1 113.8(2) . . ? C1 C2 S1 120.5(2) . . ? C4 C3 N1 115.0(2) . . ? C4 C3 C3 127.52(17) . 17_654 ? N1 C3 C3 117.53(15) . 17_654 ? C3 C4 S1 109.8(2) . . ? C3 C4 H4 125.1 . . ? S1 C4 H4 125.1 . . ? N1 Fe1 N1 98.13(8) 4_665 2_655 ? N1 Fe1 N1 98.13(8) 4_665 . ? N1 Fe1 N1 98.13(8) 2_655 . ? N1 Fe1 N1 87.21(12) 4_665 17_654 ? N1 Fe1 N1 173.21(12) 2_655 17_654 ? N1 Fe1 N1 76.88(12) . 17_654 ? N1 Fe1 N1 173.21(12) 4_665 18_554 ? N1 Fe1 N1 76.87(12) 2_655 18_554 ? N1 Fe1 N1 87.22(12) . 18_554 ? N1 Fe1 N1 98.13(8) 17_654 18_554 ? N1 Fe1 N1 76.87(12) 4_665 15_544 ? N1 Fe1 N1 87.21(12) 2_655 15_544 ? N1 Fe1 N1 173.21(12) . 15_544 ? N1 Fe1 N1 98.12(8) 17_654 15_544 ? N1 Fe1 N1 98.12(8) 18_554 15_544 ? Br2 Fe2 Br1 108.343(18) . . ? Br2 Fe2 Br1 108.343(18) . 2 ? Br1 Fe2 Br1 110.575(18) . 2 ? Br2 Fe2 Br1 108.343(18) . 4 ? Br1 Fe2 Br1 110.575(18) . 4 ? Br1 Fe2 Br1 110.575(18) 2 4 ? C2 N1 C3 110.8(2) . . ? C2 N1 Fe1 135.1(2) . . ? C3 N1 Fe1 114.03(17) . . ? C4 S1 C2 90.66(14) . . ? 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 N1 C3 C4 S1 -0.3(3) . . . . ? C3 C3 C4 S1 -180.0(3) 17_654 . . . ? C1 C2 N1 C3 178.7(3) . . . . ? S1 C2 N1 C3 -0.1(3) . . . . ? C1 C2 N1 Fe1 -1.2(5) . . . . ? S1 C2 N1 Fe1 -179.95(15) . . . . ? C4 C3 N1 C2 0.3(4) . . . . ? C3 C3 N1 C2 179.9(3) 17_654 . . . ? C4 C3 N1 Fe1 -179.8(2) . . . . ? C3 C3 N1 Fe1 -0.2(4) 17_654 . . . ? N1 Fe1 N1 C2 -94.9(2) 4_665 . . . ? N1 Fe1 N1 C2 4.6(3) 2_655 . . . ? N1 Fe1 N1 C2 179.9(3) 17_654 . . . ? N1 Fe1 N1 C2 80.9(3) 18_554 . . . ? N1 Fe1 N1 C2 -137.0(3) 15_544 . . . ? N1 Fe1 N1 C3 85.3(2) 4_665 . . . ? N1 Fe1 N1 C3 -175.27(19) 2_655 . . . ? N1 Fe1 N1 C3 0.06(14) 17_654 . . . ? N1 Fe1 N1 C3 -99.0(2) 18_554 . . . ? N1 Fe1 N1 C3 43.07(18) 15_544 . . . ? C3 C4 S1 C2 0.3(2) . . . . ? N1 C2 S1 C4 -0.1(2) . . . . ? C1 C2 S1 C4 -178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.628 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.114 # Attachment 'kh296r-abs1.cif' data_kh296r-abs1 _database_code_depnum_ccdc_archive 'CCDC 767151' #TrackingRef 'kh296r-abs1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Fe N6 S6, 2(Br4 Fe)' _chemical_formula_sum 'C24 H24 Br4 Fe3 N6 S6' _chemical_formula_weight 1395.66 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 12.9677(18) _cell_length_b 12.9677(18) _cell_length_c 43.692(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6362.9(18) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 8.870 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.130 _exptl_absorpt_correction_T_max 0.170 _exptl_absorpt_process_details 'shape of crystal determined optically' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean '0.15 mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1922 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.27 _reflns_number_total 1922 _reflns_number_gt 1469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_cell_refinement 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_data_reduction 'X-Area 1.31 (Stoe & Cie GmbH, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0608P)^2^+62.0141P] 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 1922 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.295 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 -0.0413(7) 0.1669(7) 0.18419(17) 0.0556(17) Uani 1 1 d . . . H1C H -0.0566 0.0921 0.1758 0.067 Uiso 1 1 calc R . . H1B H -0.0350 0.2192 0.1678 0.067 Uiso 1 1 calc R . . H1A H -0.1053 0.1543 0.1975 0.067 Uiso 1 1 calc R . . C2 C 0.0719(6) 0.2214(5) 0.20171(14) 0.0400(12) Uani 1 1 d . . . C3 C 0.2679(6) 0.3539(6) 0.22211(16) 0.0543(17) Uani 1 1 d . . . H3 H 0.3444 0.4140 0.2270 0.065 Uiso 1 1 calc R . . C4 C 0.2075(5) 0.2490(5) 0.23703(13) 0.0375(12) Uani 1 1 d . . . N1 N 0.0959(4) 0.1724(4) 0.22532(11) 0.0353(9) Uani 1 1 d . . . S1 S 0.18403(19) 0.36061(15) 0.19302(4) 0.0613(5) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.2500 0.0331(4) Uani 1 6 d S . . Fe2 Fe 0.0000 0.0000 0.09491(4) 0.0477(4) Uani 1 3 d S . . Br1 Br 0.0000 0.0000 0.04141(3) 0.0542(3) Uani 1 3 d S . . Br2 Br 0.14650(8) 0.18763(7) 0.11200(2) 0.0701(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 0.052(4) 0.056(4) 0.060(4) 0.009(3) -0.010(3) 0.027(3) C2 0.043(3) 0.034(3) 0.047(3) 0.003(2) -0.001(2) 0.022(2) C3 0.049(4) 0.039(3) 0.055(4) 0.005(3) -0.007(3) 0.007(3) C4 0.036(3) 0.034(3) 0.044(3) 0.001(2) 0.000(2) 0.018(2) N1 0.030(2) 0.033(2) 0.045(2) 0.0027(18) -0.0008(19) 0.0167(19) S1 0.0637(11) 0.0380(8) 0.0651(10) 0.0151(7) -0.0137(9) 0.0125(8) Fe1 0.0284(5) 0.0284(5) 0.0425(10) 0.000 0.000 0.0142(3) Fe2 0.0482(5) 0.0482(5) 0.0467(8) 0.000 0.000 0.0241(3) Br1 0.0578(4) 0.0578(4) 0.0468(6) 0.000 0.000 0.0289(2) Br2 0.0681(5) 0.0550(5) 0.0748(5) -0.0087(4) -0.0183(4) 0.0214(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.484(9) . ? C1 H1C 0.9600 . ? C1 H1B 0.9600 . ? C1 H1A 0.9600 . ? C2 N1 1.327(7) . ? C2 S1 1.701(6) . ? C3 C4 1.351(8) . ? C3 S1 1.702(7) . ? C3 H3 0.9300 . ? C4 N1 1.381(7) . ? C4 C4 1.468(11) 3 ? N1 Fe1 2.220(4) . ? Fe1 N1 2.220(4) 2 ? Fe1 N1 2.220(4) 5 ? Fe1 N1 2.220(4) 3 ? Fe1 N1 2.220(4) 4 ? Fe1 N1 2.220(4) 6 ? Fe2 Br1 2.337(2) . ? Fe2 Br2 2.3376(10) . ? Fe2 Br2 2.3376(10) 2 ? Fe2 Br2 2.3376(10) 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 C2 C1 H1C 109.4 . . ? C2 C1 H1B 109.4 . . ? H1C C1 H1B 109.5 . . ? C2 C1 H1A 109.6 . . ? H1C C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? N1 C2 C1 125.9(6) . . ? N1 C2 S1 113.6(5) . . ? C1 C2 S1 120.5(5) . . ? C4 C3 S1 110.4(5) . . ? C4 C3 H3 124.8 . . ? S1 C3 H3 124.8 . . ? C3 C4 N1 114.6(5) . . ? C3 C4 C4 127.5(4) . 3 ? N1 C4 C4 117.9(3) . 3 ? C2 N1 C4 110.9(5) . . ? C2 N1 Fe1 135.4(4) . . ? C4 N1 Fe1 113.7(3) . . ? C3 S1 C2 90.5(3) . . ? N1 Fe1 N1 98.40(16) 2 . ? N1 Fe1 N1 76.8(2) 2 5 ? N1 Fe1 N1 86.7(2) . 5 ? N1 Fe1 N1 173.5(2) 2 3 ? N1 Fe1 N1 76.8(2) . 3 ? N1 Fe1 N1 98.40(16) 5 3 ? N1 Fe1 N1 98.40(16) 2 4 ? N1 Fe1 N1 98.40(16) . 4 ? N1 Fe1 N1 173.5(2) 5 4 ? N1 Fe1 N1 86.7(2) 3 4 ? N1 Fe1 N1 86.7(2) 2 6 ? N1 Fe1 N1 173.5(2) . 6 ? N1 Fe1 N1 98.40(16) 5 6 ? N1 Fe1 N1 98.40(16) 3 6 ? N1 Fe1 N1 76.8(2) 4 6 ? Br1 Fe2 Br2 108.62(4) . . ? Br1 Fe2 Br2 108.62(4) . 2 ? Br2 Fe2 Br2 110.30(4) . 2 ? Br1 Fe2 Br2 108.62(4) . 4 ? Br2 Fe2 Br2 110.30(4) . 4 ? Br2 Fe2 Br2 110.30(4) 2 4 ? 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 S1 C3 C4 N1 1.1(8) . . . . ? S1 C3 C4 C4 178.8(7) . . . 3 ? C1 C2 N1 C4 -177.7(6) . . . . ? S1 C2 N1 C4 0.4(6) . . . . ? C1 C2 N1 Fe1 2.0(10) . . . . ? S1 C2 N1 Fe1 -180.0(3) . . . . ? C3 C4 N1 C2 -1.0(8) . . . . ? C4 C4 N1 C2 -178.8(6) 3 . . . ? C3 C4 N1 Fe1 179.3(5) . . . . ? C4 C4 N1 Fe1 1.4(8) 3 . . . ? C4 C3 S1 C2 -0.8(6) . . . . ? N1 C2 S1 C3 0.2(5) . . . . ? C1 C2 S1 C3 178.4(6) . . . . ? C2 N1 Fe1 N1 -4.6(6) . . . 2 ? C4 N1 Fe1 N1 175.1(4) . . . 2 ? C2 N1 Fe1 N1 -80.7(6) . . . 5 ? C4 N1 Fe1 N1 98.9(4) . . . 5 ? C2 N1 Fe1 N1 179.8(7) . . . 3 ? C4 N1 Fe1 N1 -0.5(3) . . . 3 ? C2 N1 Fe1 N1 95.3(5) . . . 4 ? C4 N1 Fe1 N1 -85.1(5) . . . 4 ? C2 N1 Fe1 N1 137.1(6) . . . 6 ? C4 N1 Fe1 N1 -43.2(4) . . . 6 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.427 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.087