# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2093 data_global _publ_contact_author_name 'Raubenheimer, Helgard G.' _publ_contact_author_address ; Department of Chemistry Stellenbosch University Private Bag X1 Matieland, 7602 South Africa ; _publ_contact_author_email hgr@land.sun.ac.za _publ_requested_journal ; Journal of the Chemical Society, Dalton Transactions ; _publ_section_title ; Synthesis and crystallographic characterization of thiazole-2-carbodithiomethylester complexes of chromium, tungsten and iron carbonyls ; _publ_section_references ; Farrugia, L.J. (1997). J. Appl. Cryst. 30, 565. Hall, S.R., King, G.S.D. & Stewart, J.M. (1995) Eds. Xtal3.4 Reference Manual. University of Western Australia: Lamb, Perth. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta. Cryst. A24, 351-359. Sheldrick, G.M. (1997). SHELX-97. Program for crystal structure analysis. Univ. of G\"ottingen, Germany. ; _publ_section_exptl_refinement ; The structures were solved using XTAL3.4, by interpretation of a Patterson synthesis which yielded the position of the metal atoms, while the remaining non-metal atoms were found from the difference Fourier maps. All non-hydrogen atoms were allowed anisotropic displacement parameters. The H atoms could be located by difference Fourier, but were refined in ideal positions with bond lengths of 0.93 \%A for aromatic C-H bonds and 0.96 \%A for the rest, and displacement parameters 1.2 times that of the aromatic atoms (or 1.5 times for the non-aromatic atoms) they were bonded to. ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetracarbonyl(4-methylthiazole-2-carbodithiomethylester)Cr(0) ; _chemical_name_common ? _chemical_formula_moiety 'C10 H7 Cr N O4 S3' _chemical_formula_sum 'C10 H7 Cr1 N1 O4 S3' _chemical_formula_weight 353.35 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' 'S' 'S' 0.1246 0.1234 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2~1~/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.948(2) _cell_length_b 16.647(3) _cell_length_c 9.4732(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.854(19) _cell_angle_gamma 90.00 _cell_volume 1397.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 17 _exptl_crystal_description needle _exptl_crystal_colour 'blue-green' _exptl_crystal_size_max 0.96 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.27 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.79 _exptl_absorpt_process_details 'via psi scan (North et al.,1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ENRAF-NONIUS CAD4F' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 2535 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.009 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 22.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 1941 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'XTAL3.4 (Hall, King & Stewart,1995)' _computing_structure_refinement 'XTAL3.4 (Hall, King & Stewart,1995)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.7200P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 1941 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.050 _refine_ls_R_factor_obs 0.037 _refine_ls_wR_factor_all 0.036 _refine_ls_wR_factor_obs 0.036 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.27806(5) 0.34655(3) 0.31414(5) 0.0415(2) Uani 1 1 d . . . S1 S 0.05724(9) 0.39446(6) 0.17785(10) 0.0543(3) Uani 1 1 d . . . S2 S -0.10308(11) 0.39693(6) 0.58109(11) 0.0632(3) Uani 1 1 d . . . S3 S -0.23864(10) 0.44590(7) 0.26990(14) 0.0743(4) Uani 1 1 d . . . N N 0.1394(3) 0.36122(15) 0.4790(3) 0.0419(6) Uani 1 1 d . . . O1 O 0.5729(3) 0.28691(18) 0.4658(3) 0.0706(7) Uani 1 1 d . . . O2 O 0.4239(3) 0.3279(2) 0.0505(3) 0.0809(9) Uani 1 1 d . . . O3 O 0.1985(3) 0.17976(17) 0.3079(3) 0.0745(8) Uani 1 1 d . . . O4 O 0.4264(3) 0.5108(2) 0.3347(4) 0.090(1) Uani 1 1 d . . . C1 C 0.4573(4) 0.3111(2) 0.4144(4) 0.0486(8) Uani 1 1 d . . . C2 C 0.3656(4) 0.3347(2) 0.1518(4) 0.0539(9) Uani 1 1 d . . . C3 C 0.2218(4) 0.2368(2) 0.3066(4) 0.0490(8) Uani 1 1 d . . . C4 C 0.3650(4) 0.4510(2) 0.3308(4) 0.0557(9) Uani 1 1 d . . . C5 C 0.0003(4) 0.38944(18) 0.4418(4) 0.0450(8) Uani 1 1 d . . . C6 C 0.0461(4) 0.3608(2) 0.6922(4) 0.0611(10) Uani 1 1 d . . . H6 H 0.04643 0.3532 0.7905 0.07337 Uiso 1 1 calc R . . C7 C 0.1649(4) 0.3443(2) 0.6226(4) 0.0507(9) Uani 1 1 d . . . C8 C 0.3111(5) 0.3107(3) 0.691(10) 0.0755(12) Uani 1 1 d . . . H8A H 0.3776 0.3040 0.6201 0.075 Uiso 1 1 calc R . . H8B H 0.2941 0.2596 0.7326 0.075 Uiso 1 1 calc R . . H8C H 0.3561 0.3468 0.7634 0.075 Uiso 1 1 calc R . . C9 C -0.0567(3) 0.4093(2) 0.2987(4) 0.0300(16) Uani 1 1 d . . . C10 C -0.2650(5) 0.4708(3) 0.0866(5) 0.053(2) Uani 1 1 d . . . H10A H -0.3646 0.4920 0.0605 0.135 Uiso 1 1 calc R . . H10B H -0.2528 0.4235 0.0313 0.135 Uiso 1 1 calc R . . H10C H -0.1918 0.5103 0.0684 0.135 Uiso 1 1 calc R . . 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 Cr 0.0299(3) 0.0501(4) 0.0450(3) -0.0012(2) 0.0062(2) 0.0029(2) S1 0.0375(5) 0.0704(6) 0.0546(5) 0.0045(4) 0.0040(4) 0.0073(4) S2 0.0487(6) 0.0672(6) 0.0804(7) -0.0040(5) 0.0327(5) -0.0033(4) S3 0.0337(5) 0.0821(8) 0.1080(9) 0.0195(6) 0.0138(5) 0.0139(5) N 0.0340(14) 0.0424(14) 0.0506(17) -0.0041(12) 0.0101(12) -0.0029(11) O1 0.0421(15) 0.0901(19) 0.0760(18) 0.0086(15) -0.0047(13) 0.0118(14) O2 0.076(2) 0.116(2) 0.0549(17) 0.0033(16) 0.0273(16) 0.0090(17) O3 0.078(2) 0.0579(18) 0.091(2) -0.0131(15) 0.0230(16) -0.0124(15) O4 0.0565(17) 0.0542(17) 0.163(3) 0.0067(19) 0.0238(19) -0.0034(15) C1 0.040(2) 0.056(2) 0.050(2) 0.0012(16) 0.0066(16) -0.0001(16) C2 0.043(2) 0.067(2) 0.051(2) 0.0040(18) 0.0039(17) 0.0047(17) C3 0.0359(17) 0.063(2) 0.050(2) -0.0068(17) 0.0109(14) 0.0012(17) C4 0.0352(19) 0.057(2) 0.076(2) 0.0053(19) 0.0141(17) 0.0104(17) C5 0.0353(18) 0.0372(17) 0.065(2) -0.0027(16) 0.0157(16) -0.0037(14) C6 0.064(2) 0.066(2) 0.058(2) -0.0063(18) 0.0226(19) -0.0149(19) C7 0.051(2) 0.053(2) 0.049(2) -0.0047(16) 0.0117(17) -0.0091(16) C8 0.066(3) 0.111(4) 0.048(2) 0.008(2) 0.002(2) 0.010(2) C9 0.0300(16) 0.0412(18) 0.073(2) 0.0018(16) 0.0091(16) -0.0002(14) C10 0.053(3) 0.101(4) 0.109(4) 0.022(3) -0.010(2) 0.015(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 Cr C2 1.830(4) . ? Cr C1 1.845(4) . ? Cr C3 1.895(4) . ? Cr C4 1.902(4) . ? Cr N 2.137(3) . ? Cr S1 2.3474(11) . ? S1 C9 1.652(4) . ? S2 C6 1.694(4) . ? S2 C5 1.716(3) . ? S3 C9 1.725(3) . ? S3 C10 1.770(5) . ? N C5 1.333(4) . ? N C7 1.377(4) . ? O1 C1 1.154(4) . ? O2 C2 1.158(4) . ? O3 C3 1.135(4) . ? O4 C4 1.136(4) . ? C5 C9 1.421(5) . ? C6 C7 1.353(5) . ? C6 H6 0.9300 . ? C7 C8 1.487(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 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 C2 Cr C1 87.49(15) . . ? C2 Cr C3 90.34(15) . . ? C1 Cr C3 85.35(15) . . ? C2 Cr C4 87.22(16) . . ? C1 Cr C4 86.11(15) . . ? C3 Cr C4 171.21(14) . . ? C2 Cr N 169.96(13) . . ? C1 Cr N 102.19(13) . . ? C3 Cr N 87.72(12) . . ? C4 Cr N 96.11(13) . . ? C2 Cr S1 89.95(11) . . ? C1 Cr S1 177.02(11) . . ? C3 Cr S1 96.19(11) . . ? C4 Cr S1 92.25(11) . . ? N Cr S1 80.45(8) . . ? C9 S1 Cr 102.85(13) . . ? C6 S2 C5 89.44(17) . . ? C9 S3 C10 103.5(2) . . ? C5 N C7 110.8(3) . . ? C5 N Cr 117.5(2) . . ? C7 N Cr 131.6(2) . . ? O1 C1 Cr 174.0(3) . . ? O2 C2 Cr 178.5(3) . . ? O3 C3 Cr 174.8(3) . . ? O4 C4 Cr 174.11(3) . . ? N C5 C9 122.3(3) . . ? N C5 S2 113.9(3) . . ? C9 C5 S2 123.8(2) . . ? C7 C6 S2 112.0(3) . . ? C7 C6 H6 124.02 . . ? S2 C6 H6 124.02 . . ? C6 C7 N 113.9(3) . . ? C6 C7 C8 124.59(4) . . ? N C7 C8 121.5(3) . . ? C7 C8 H8A 109.47 . . ? C7 C8 H8B 109.47 . . ? H8A C8 H8B 109.47 . . ? C7 C8 H8C 109.47 . . ? H8A C8 H8C 109.47 . . ? H8B C8 H8C 109.47 . . ? C5 C9 S1 116.9(2) . . ? C5 C9 S3 116.1(3) . . ? S1 C9 S3 127.0(2) . . ? S3 C10 H10A 109.47 . . ? S3 C10 H10B 109.47 . . ? H10A C10 H10B 109.47 . . ? S3 C10 H10C 109.47 . . ? H10A C10 H10C 109.47 . . ? H10B C10 H10C 109.47 . . ? _refine_diff_density_max 0.37 _refine_diff_density_min -0.44 _refine_diff_density_rms 0.07 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tricarbonyl(benzothiazole-2-carbodithiomethylester)Fe(0) ; _chemical_name_common ? _chemical_formula_moiety 'C12 H7 Fe N O3 S3' _chemical_formula_sum 'C12 H7 Fe1 N1 O3 S3' _chemical_formula_weight 365.23 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' 'S' 'S' 0.1246 0.1234 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2~1~' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.312(2) _cell_length_b 7.317(3) _cell_length_c 10.741(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.38(2) _cell_angle_gamma 90.00 _cell_volume 729.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 17 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.448 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details 'via psi scan (North et al.,1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ENRAF-NONIUS CAD4F' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 2752 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.014 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 30 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 1845 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'XTAL3.4 (Hall, King & Stewart,1995)' _computing_structure_refinement 'XTAL3.4 (Hall, King & Stewart,1995)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.72P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment calc _refine_ls_number_reflns 1845 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.034 _refine_ls_wR_factor_obs 0.031 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.7510(1) 0.2449(1) 0.7534(1) 0.07328 Uani 1 d . . . S1 S 0.9358(1) 0.2473(2) 0.8925(1) 0.08489 Uani 1 d . . . S2 S 1.1580(1) 0.2452(2) 0.5605(1) 0.06561 Uani 1 d . . . S3 S 1.2553(2) 0.2383(1) 0.8571(1) 0.09193 Uani 1 d . . . O1 O 0.5797(4) -0.0542(3) 0.6337(4) 0.13060 Uani 1 d . . . O2 O 0.5884(3) 0.2794(3) 0.9718(3) 0.14476 Uani 1 d . . . O3 O 0.5897(3) 0.5545(3) 0.6546(4) 0.10467 Uani 1 d . . . N N 0.8980(4) 0.2540(4) 0.6326(4) 0.05604 Uani 1 d . . . C1 C 0.6504(4) 0.0548(3) 0.6802(4) 0.08135 Uani 1 d . . . C2 C 0.6481(4) 0.2635(4) 0.8835(5) 0.11202 Uani 1 d . . . C3 C 0.6521(5) 0.4304(4) 0.6899(5) 0.09206 Uani 1 d . . . C4 C 1.0370(4) 0.2511(4) 0.6744(4) 0.05545 Uani 1 d . . . C5 C 1.0145(4) 0.2452(3) 0.4480(5) 0.06283 Uani 1 d . . . C6 C 0.8834(5) 0.2448(4) 0.5018(5) 0.05444 Uani 1 d . . . C7 C 0.7553(4) 0.2544(4) 0.4263(4) 0.06472 Uani 1 d . . . H7 H 0.6676 0.2689 0.4611 0.07767 Uiso 1 calc R . . C8 C 0.7615(4) 0.2421(3) 0.2999(4) 0.08008 Uani 1 d . . . H8 H 0.6781 0.2185 0.2492 0.09609 Uiso 1 calc R . . C9 C 0.8924(5) 0.2648(4) 0.2462(5) 0.04930 Uani 1 d . . . H9 H 0.8931 0.2823 0.1605 0.05916 Uiso 1 calc R . . C10 C 1.0204(4) 0.2614(3) 0.3195(5) 0.06989 Uani 1 d . . . H10 H 1.1082 0.2697 0.2841 0.08386 Uiso 1 calc R . . C11 C 1.0750(5) 0.2470(3) 0.8020(5) 0.06499 Uani 1 d . . . C12 C 1.2462(4) 0.2585(4) 1.0184(5) 0.10961 Uani 1 d . . . H12A H 1.3366 0.2227 1.0602 0.16442 Uiso 1 calc R . . H12B H 1.1711 0.1809 1.0447 0.16442 Uiso 1 calc R . . H12C H 1.2259 0.3831 1.0389 0.16442 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.048(1) 0.114(1) 0.058(1) -0.013(1) 0.005(1) 0.000(1) S1 0.052(1) 0.154(1) 0.049(1) -0.010(2) 0.006(1) -0.022(1) S2 0.055(1) 0.085(2) 0.058(1) -0.009(2) 0.012(1) -0.019(1) S3 0.047(1) 0.166(1) 0.062(1) -0.020(1) -0.001(2) 0.005(1) O1 0.104(2) 0.137(2) 0.149(1) 0.007(2) -0.002(2) -0.044(2) O2 0.064(1) 0.298(2) 0.075(2) -0.024(3) 0.023(2) -0.034(1) O3 0.042(2) 0.102(2) 0.188(2) 0.029(3) 0.008(2) 0.043(2) N 0.050(2) 0.069(1) 0.049(2) 0.005(2) 0.003(1) 0.008(1) C1 0.044(4) 0.121(2) 0.082(3) 0.020(4) 0.024(2) -0.012(2) C2 0.044(3) 0.220(2) 0.072(3) 0.029(3) 0.004(2) -0.007(2) C3 0.088(3) 0.084(3) 0.100(4) 0.009(3) -0.020(3) 0.003(3) C4 0.049(3) 0.068(3) 0.050(3) -0.004(3) 0.008(2) -0.017(2) C5 0.070(4) 0.067(3) 0.052(2) -0.0013(19) 0.008(3) 0.033(2) C6 0.062(3) 0.057(4) 0.044(3) 0.000(3) 0.002(2) -0.010(2) C7 0.066(3) 0.073(3) 0.054(2) 0.001(3) -0.003(3) 0.013(2) C8 0.089(2) 0.093(2) 0.056(4) 0.013(2) -0.009(2) -0.025(4) C9 0.017(3) 0.085(2) 0.046(3) -0.013(2) 0.003(1) 0.005(2) C10 0.089(3) 0.073(2) 0.049(3) 0.007(2) 0.014(2) 0.005(3) C11 0.044(3) 0.094(2) 0.057(3) 0.024(2) 0.004(14) 0.025(2) C12 0.059(4) 0.198(2) 0.070(2) -0.036(3) -0.007(2) 0.006(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 Fe C3 1.750(2) . ? Fe C2 1.759(8) . ? Fe C1 1.820(2) . ? Fe N 1.958(4) . ? Fe S1 2.191(1) . ? S1 C11 1.678(5) . ? S3 C11 1.738(4) . ? S3 C12 1.747(6) . ? S2 C4 1.726(5) . ? S2 C5 1.732(5) . ? O2 C2 1.141(6) . ? O1 C1 1.126(5) . ? O3 C3 1.128(6) . ? N C4 1.337(5) . ? N C6 1.402(6) . ? C11 C4 1.389(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C5 C6 1.390(6) . ? C5 C10 1.391(5) . ? C6 C7 1.392(6) . ? C7 C8 1.366(5) . ? C7 H7 0.9300 . ? C8 C9 1.398(8) . ? C8 H8 0.9300 . ? C9 C10 1.378(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 C3 Fe C2 87.0(5) . . ? C3 Fe C1 100.8(3) . . ? C1 Fe C2 96.2(5) . . ? C3 Fe N 95.1(4) . . ? C2 Fe N 167.1(9) . . ? C1 Fe N 95.9(3) . . ? C3 Fe S1 128.5(8) . . ? C2 Fe S1 84.5(2) . . ? C1 Fe S1 130.7(7) . . ? N Fe S1 84.2(1) . . ? C11 S1 Fe 101.9(2) . . ? C11 S3 C12 102.5(3) . . ? C4 S2 C5 89.08(18) . . ? C4 N C6 110.7(3) . . ? C4 N Fe 119.0(3) . . ? C6 N Fe 130.0(3) . . ? C4 C11 S1 114.9(3) . . ? C4 C11 S3 120.2(3) . . ? S1 C11 S3 124.9(2) . . ? S3 C12 H12A 109.47 . . ? S3 C12 H12B 109.47 . . ? H1 C12 H12B 109.47 . . ? S3 C12 H12C 109.47 . . ? H12A C12 H12C 109.47 . . ? H12B C12 H12C 109.47 . . ? N C4 C11 119.9(4) . . ? N C4 S3 115.5(3) . . ? C11 C4 S3 124.6(3) . . ? C6 C5 C10 121.0(4) . . ? C6 C5 S3 111.4(2) . . ? C10 C5 S3 127.3(5) . . ? C5 C6 C7 119.9(3) . . ? C5 C6 N 113.3(3) . . ? C7 C6 N 126.5(4) . . ? C8 C7 C6 118.4(5) . . ? C8 C7 H7 120.78 . . ? C6 C7 H7 120.78 . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.78 . . ? C9 C8 H8 119.78 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.81 . . ? C8 C9 H9 119.81 . . ? C9 C10 C5 118.1(5) . . ? C9 C10 H10 120.96 . . ? C5 C10 H10 120.96 . . ? O1 C1 Fe 174.9(7) . . ? O2 C2 Fe 176.0(10) . . ? O3 C3 Fe 176.5(7) . . ? _refine_diff_density_max 0.28 _refine_diff_density_min -0.53 _refine_diff_density_rms 0.07