Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Manuel Almeida' _publ_contact_author_address ; Departmento de Quimica ITN E. N. 10 Sacavem P-2686-953 PORTUGAL ; _publ_contact_author_email MALMEIDA@ITN.PT _publ_section_title ; [Fe(qdt)2]- salts; an undimerised FeIII bisdithiolene complex stabilised by cation interactions ; loop_ _publ_author_name 'Manuel Almeida' 'J. A. Ayllon' 'M. J. Figueira' 'Rui Henriques' 'S. Rabaca' ; I.C.Santos ; 'D. Simao' data_I _database_code_depnum_ccdc_archive 'CCDC 262344' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (tba)(Fe(qdt)2) _chemical_melting_point ? _chemical_formula_moiety '(C16 H36)N, C16 H8 Fe N4 S4' _chemical_formula_sum 'C32 H44 Fe N5 S4' _chemical_formula_weight 682.81 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.290(3) _cell_length_b 8.5089(9) _cell_length_c 19.112(2) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.798(12) _cell_angle_gamma 90.000(5) _cell_volume 3451.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details 'psi-scan (North,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 cad4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 3425 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2916 _reflns_number_gt 1428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction molen _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL(Keller,1989),ORTEP3(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^)+(0.0706P)^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 SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2916 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1572 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.5000 0.0000 0.5000 0.0488(3) Uani 1 2 d S . . S1 S 0.59445(7) 0.0981(2) 0.52971(8) 0.0861(5) Uani 1 1 d . . . S2 S 0.49993(6) -0.05673(18) 0.38890(8) 0.0771(4) Uani 1 1 d . . . C1 C 0.6161(2) 0.0871(6) 0.4498(3) 0.0652(13) Uani 1 1 d . . . C2 C 0.5709(2) 0.0179(6) 0.3838(3) 0.0646(12) Uani 1 1 d . . . N1 N 0.66993(19) 0.1390(5) 0.4493(2) 0.0732(12) Uani 1 1 d . . . N2 N 0.58404(19) 0.0060(5) 0.3221(2) 0.0736(11) Uani 1 1 d . . . C3 C 0.6839(2) 0.1255(6) 0.3848(3) 0.0667(13) Uani 1 1 d . . . C4 C 0.6418(2) 0.0623(6) 0.3222(3) 0.0684(13) Uani 1 1 d . . . C5 C 0.7420(3) 0.1826(7) 0.3811(3) 0.0862(16) Uani 1 1 d . . . H5 H 0.7700 0.2283 0.4225 0.103 Uiso 1 1 calc R . . C6 C 0.6576(3) 0.0553(8) 0.2567(3) 0.100(2) Uani 1 1 d . . . H6 H 0.6293 0.0137 0.2145 0.120 Uiso 1 1 calc R . . C7 C 0.7580(3) 0.1722(8) 0.3183(4) 0.104(2) Uani 1 1 d . . . H7 H 0.7974 0.2065 0.3174 0.125 Uiso 1 1 calc R . . C8 C 0.7154(3) 0.1101(9) 0.2553(4) 0.107(2) Uani 1 1 d . . . H8 H 0.7259 0.1056 0.2119 0.129 Uiso 1 1 calc R . . N3 N 0.5000 0.4980(7) 0.2500 0.0809(17) Uani 1 2 d S . . C10 C 0.5529(3) 0.6042(6) 0.2936(3) 0.0856(17) Uani 1 1 d . . . H10A H 0.5636 0.6743 0.2591 0.103 Uiso 1 1 calc R . . H10B H 0.5366 0.6688 0.3255 0.103 Uiso 1 1 calc R . . C11 C 0.6134(3) 0.5289(8) 0.3405(4) 0.108(2) Uani 1 1 d . . . H11A H 0.6294 0.4587 0.3104 0.129 Uiso 1 1 calc R . . H11B H 0.6047 0.4669 0.3789 0.129 Uiso 1 1 calc R . . C12 C 0.6636(3) 0.6518(9) 0.3756(4) 0.121(2) Uani 1 1 d . . . H12A H 0.6733 0.7102 0.3368 0.145 Uiso 1 1 calc R . . H12B H 0.6463 0.7253 0.4031 0.145 Uiso 1 1 calc R . . C13 C 0.7223(4) 0.5871(11) 0.4247(4) 0.149(3) Uani 1 1 d . . . H13A H 0.7510 0.6712 0.4450 0.223 Uiso 1 1 calc R . . H13B H 0.7408 0.5173 0.3977 0.223 Uiso 1 1 calc R . . H13C H 0.7134 0.5303 0.4639 0.223 Uiso 1 1 calc R . . C20 C 0.5230(3) 0.3919(6) 0.1996(3) 0.0934(19) Uani 1 1 d . . . H20A H 0.5537 0.3195 0.2298 0.112 Uiso 1 1 calc R . . H20B H 0.4876 0.3300 0.1705 0.112 Uiso 1 1 calc R . . C21 C 0.5516(4) 0.4708(7) 0.1491(4) 0.104(2) Uani 1 1 d . . . H21A H 0.5224 0.5482 0.1204 0.125 Uiso 1 1 calc R . . H21B H 0.5894 0.5257 0.1774 0.125 Uiso 1 1 calc R . . C22 C 0.5680(4) 0.3590(9) 0.0992(5) 0.141(3) Uani 1 1 d . . . H22A H 0.5291 0.3125 0.0684 0.170 Uiso 1 1 calc R . . H22B H 0.5926 0.2752 0.1288 0.170 Uiso 1 1 calc R . . C23 C 0.6034(5) 0.4188(11) 0.0501(5) 0.166(4) Uani 1 1 d . . . H23A H 0.6128 0.3331 0.0225 0.249 Uiso 1 1 calc R . . H23B H 0.6420 0.4665 0.0793 0.249 Uiso 1 1 calc R . . H23C H 0.5784 0.4954 0.0170 0.249 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 Fe 0.0399(5) 0.0474(5) 0.0556(5) -0.0071(5) 0.0092(4) 0.0011(5) S1 0.0661(8) 0.1164(13) 0.0719(9) -0.0216(9) 0.0155(7) -0.0245(8) S2 0.0584(8) 0.0909(10) 0.0780(9) -0.0269(7) 0.0151(7) -0.0069(7) C1 0.063(3) 0.060(3) 0.066(3) -0.001(3) 0.010(3) 0.007(3) C2 0.061(3) 0.060(3) 0.069(3) 0.005(3) 0.013(2) 0.006(3) N1 0.054(2) 0.084(3) 0.075(3) -0.006(2) 0.011(2) -0.012(2) N2 0.067(3) 0.083(3) 0.066(2) -0.003(3) 0.014(2) 0.002(3) C3 0.059(3) 0.070(3) 0.067(3) -0.002(3) 0.013(3) 0.000(3) C4 0.066(3) 0.069(3) 0.070(3) 0.002(3) 0.020(3) 0.004(3) C5 0.067(3) 0.098(4) 0.093(4) 0.002(4) 0.023(3) -0.006(3) C6 0.084(4) 0.134(6) 0.079(4) -0.015(4) 0.021(3) -0.008(4) C7 0.085(4) 0.124(5) 0.109(5) 0.006(5) 0.039(4) -0.012(4) C8 0.090(5) 0.150(6) 0.089(4) 0.001(4) 0.037(4) -0.016(5) N3 0.112(5) 0.046(3) 0.078(4) 0.000 0.019(4) 0.000 C10 0.101(4) 0.061(3) 0.091(4) -0.006(3) 0.024(3) 0.008(3) C11 0.124(6) 0.097(5) 0.093(4) -0.004(4) 0.019(4) 0.028(4) C12 0.115(6) 0.101(5) 0.123(6) -0.005(5) 0.000(5) 0.018(5) C13 0.121(6) 0.161(7) 0.143(7) -0.017(6) 0.009(6) 0.033(6) C20 0.132(5) 0.061(4) 0.094(4) -0.009(3) 0.043(4) 0.001(3) C21 0.130(6) 0.090(5) 0.101(4) -0.017(4) 0.048(4) 0.007(4) C22 0.204(9) 0.110(6) 0.139(6) -0.032(5) 0.095(7) -0.019(6) C23 0.226(11) 0.145(7) 0.166(8) -0.028(7) 0.116(8) -0.019(7) _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 S1 2.1729(14) 5_656 ? Fe S1 2.1729(14) . ? Fe S2 2.1770(14) . ? Fe S2 2.1770(14) 5_656 ? S1 C1 1.740(5) . ? S2 C2 1.735(5) . ? C1 N1 1.282(6) . ? C1 C2 1.473(7) . ? C2 N2 1.304(6) . ? N1 C3 1.365(6) . ? N2 C4 1.374(6) . ? C3 C4 1.384(7) . ? C3 C5 1.405(7) . ? C4 C6 1.400(7) . ? C5 C7 1.356(8) . ? C6 C8 1.378(8) . ? C7 C8 1.391(8) . ? N3 C10 1.517(6) . ? N3 C10 1.517(6) 2_655 ? N3 C20 1.520(6) . ? N3 C20 1.520(6) 2_655 ? C10 C11 1.514(8) . ? C11 C12 1.528(9) . ? C12 C13 1.465(9) . ? C20 C21 1.471(8) . ? C21 C22 1.469(8) . ? C22 C23 1.489(9) . ? 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 S1 Fe S1 180.00(4) 5_656 . ? S1 Fe S2 87.03(5) 5_656 . ? S1 Fe S2 92.97(5) . . ? S1 Fe S2 92.97(5) 5_656 5_656 ? S1 Fe S2 87.03(5) . 5_656 ? S2 Fe S2 180.000(1) . 5_656 ? C1 S1 Fe 104.84(18) . . ? C2 S2 Fe 104.15(18) . . ? N1 C1 C2 121.9(5) . . ? N1 C1 S1 119.9(4) . . ? C2 C1 S1 118.2(4) . . ? N2 C2 C1 121.4(4) . . ? N2 C2 S2 118.9(4) . . ? C1 C2 S2 119.7(4) . . ? C1 N1 C3 116.7(4) . . ? C2 N2 C4 116.2(4) . . ? N1 C3 C4 122.2(5) . . ? N1 C3 C5 118.9(5) . . ? C4 C3 C5 118.8(5) . . ? N2 C4 C3 121.6(5) . . ? N2 C4 C6 118.4(5) . . ? C3 C4 C6 120.0(5) . . ? C7 C5 C3 121.2(6) . . ? C8 C6 C4 119.7(6) . . ? C5 C7 C8 119.7(6) . . ? C6 C8 C7 120.5(6) . . ? C10 N3 C10 106.9(5) . 2_655 ? C10 N3 C20 110.2(3) . . ? C10 N3 C20 111.2(3) 2_655 . ? C10 N3 C20 111.2(3) . 2_655 ? C10 N3 C20 110.2(3) 2_655 2_655 ? C20 N3 C20 107.1(6) . 2_655 ? C11 C10 N3 118.4(4) . . ? C10 C11 C12 111.7(5) . . ? C13 C12 C11 114.5(6) . . ? C21 C20 N3 116.3(5) . . ? C22 C21 C20 111.9(6) . . ? C21 C22 C23 118.2(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_publ_flag C10 H10B S2 0.97 2.86 3.789(6) 1_565 159.8 ? C12 H12B N2 0.97 2.95 3.488(8) 1_565 116.0 ? C5 H5 N1 0.93 2.66 3.574(7) 7_656 168.5 ? C13 H13C N1 0.96 2.99 3.426(9) 7_656 108.9 ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.438 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.063 #===END data_II _database_code_depnum_ccdc_archive 'CCDC 298265' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (Ph)4As(Fe(qdt)2) _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 Fe2 N8 S8, 2(C24 H20 As)' _chemical_formula_sum 'C80 H56 As2 Fe2 N8 S8' _chemical_formula_weight 1647.43 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6406(12) _cell_length_b 11.3943(10) _cell_length_c 15.4041(19) _cell_angle_alpha 100.228(9) _cell_angle_beta 91.538(8) _cell_angle_gamma 100.917(8) _cell_volume 1801.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 12 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 838 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7108 _exptl_absorpt_correction_T_max 0.8512 _exptl_absorpt_process_details 'psi-scan (North,1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 cad4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 500 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 7330 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7053 _reflns_number_gt 4077 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1989), Ortep3 (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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7053 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.64210(6) 0.03987(5) 0.47047(4) 0.03358(17) Uani 1 1 d . . . S1 S 0.57752(11) -0.04712(9) 0.58513(7) 0.0322(3) Uani 1 1 d . . . S2 S 0.69417(12) 0.22209(10) 0.56024(8) 0.0424(3) Uani 1 1 d . . . S3 S 0.66889(12) -0.14517(10) 0.40837(8) 0.0413(3) Uani 1 1 d . . . S4 S 0.74436(12) 0.11582(10) 0.36243(8) 0.0436(3) Uani 1 1 d . . . C1 C 0.5994(4) 0.0735(4) 0.6770(3) 0.0320(10) Uani 1 1 d . . . C2 C 0.6516(4) 0.1951(4) 0.6642(3) 0.0344(11) Uani 1 1 d . . . N1 N 0.5682(3) 0.0470(3) 0.7530(2) 0.0376(9) Uani 1 1 d . . . N2 N 0.6676(4) 0.2870(3) 0.7313(2) 0.0399(10) Uani 1 1 d . . . C3 C 0.5843(4) 0.1414(4) 0.8232(3) 0.0383(11) Uani 1 1 d . . . C4 C 0.6316(4) 0.2614(4) 0.8120(3) 0.0403(12) Uani 1 1 d . . . C5 C 0.5489(5) 0.1208(4) 0.9069(3) 0.0547(14) Uani 1 1 d . . . H5 H 0.5189 0.0416 0.9148 0.066 Uiso 1 1 calc R . . C6 C 0.6406(5) 0.3571(4) 0.8846(3) 0.0577(15) Uani 1 1 d . . . H6 H 0.6722 0.4367 0.8781 0.069 Uiso 1 1 calc R . . C7 C 0.5573(6) 0.2143(5) 0.9769(3) 0.0688(17) Uani 1 1 d . . . H7 H 0.5330 0.1993 1.0320 0.083 Uiso 1 1 calc R . . C8 C 0.6031(5) 0.3335(5) 0.9643(4) 0.0664(17) Uani 1 1 d . . . H8 H 0.6080 0.3978 1.0117 0.080 Uiso 1 1 calc R . . C9 C 0.7119(4) -0.1308(4) 0.3021(3) 0.0354(11) Uani 1 1 d . . . C10 C 0.7430(4) -0.0109(4) 0.2799(3) 0.0367(11) Uani 1 1 d . . . N3 N 0.7147(4) -0.2297(3) 0.2450(3) 0.0454(10) Uani 1 1 d . . . N4 N 0.7720(4) 0.0043(3) 0.2005(3) 0.0498(11) Uani 1 1 d . . . C11 C 0.7466(5) -0.2152(4) 0.1617(3) 0.0463(13) Uani 1 1 d . . . C12 C 0.7740(5) -0.0991(4) 0.1389(3) 0.0532(14) Uani 1 1 d . . . C13 C 0.7533(6) -0.3171(5) 0.0979(4) 0.0724(18) Uani 1 1 d . . . H13 H 0.7350 -0.3940 0.1126 0.087 Uiso 1 1 calc R . . C14 C 0.8074(7) -0.0889(5) 0.0530(4) 0.090(2) Uani 1 1 d . . . H14 H 0.8261 -0.0128 0.0371 0.109 Uiso 1 1 calc R . . C15 C 0.7858(7) -0.3061(6) 0.0147(4) 0.095(2) Uani 1 1 d . . . H15 H 0.7902 -0.3748 -0.0270 0.114 Uiso 1 1 calc R . . C16 C 0.8126(8) -0.1917(6) -0.0078(4) 0.111(3) Uani 1 1 d . . . H16 H 0.8345 -0.1844 -0.0650 0.133 Uiso 1 1 calc R . . As As 0.82216(5) 0.71627(4) 0.68734(3) 0.04107(15) Uani 1 1 d . . . C20 C 0.9340(4) 0.6614(4) 0.7648(3) 0.0390(11) Uani 1 1 d . . . C21 C 1.0371(5) 0.7401(4) 0.8104(4) 0.0540(14) Uani 1 1 d . . . H21 H 1.0583 0.8192 0.8000 0.065 Uiso 1 1 calc R . . C22 C 1.1098(5) 0.7029(5) 0.8715(4) 0.0657(16) Uani 1 1 d . . . H22 H 1.1799 0.7568 0.9025 0.079 Uiso 1 1 calc R . . C23 C 1.0787(5) 0.5860(5) 0.8867(4) 0.0642(16) Uani 1 1 d . . . H23 H 1.1252 0.5618 0.9300 0.077 Uiso 1 1 calc R . . C24 C 0.9794(5) 0.5053(5) 0.8382(4) 0.0632(16) Uani 1 1 d . . . H24 H 0.9610 0.4252 0.8467 0.076 Uiso 1 1 calc R . . C25 C 0.9064(5) 0.5418(4) 0.7771(3) 0.0505(13) Uani 1 1 d . . . H25 H 0.8389 0.4866 0.7442 0.061 Uiso 1 1 calc R . . C30 C 0.6511(5) 0.6742(4) 0.7225(3) 0.0430(12) Uani 1 1 d . . . C31 C 0.5832(5) 0.7645(4) 0.7490(3) 0.0486(13) Uani 1 1 d . . . H31 H 0.6200 0.8453 0.7487 0.058 Uiso 1 1 calc R . . C32 C 0.4606(5) 0.7349(4) 0.7761(3) 0.0494(13) Uani 1 1 d . . . H32 H 0.4141 0.7955 0.7934 0.059 Uiso 1 1 calc R . . C33 C 0.4074(5) 0.6158(5) 0.7773(3) 0.0595(15) Uani 1 1 d . . . H33 H 0.3254 0.5964 0.7967 0.071 Uiso 1 1 calc R . . C34 C 0.4738(5) 0.5248(5) 0.7503(4) 0.0614(16) Uani 1 1 d . . . H34 H 0.4364 0.4442 0.7505 0.074 Uiso 1 1 calc R . . C35 C 0.5963(5) 0.5537(4) 0.7229(4) 0.0554(14) Uani 1 1 d . . . H35 H 0.6420 0.4927 0.7047 0.067 Uiso 1 1 calc R . . C40 C 0.8731(4) 0.8896(4) 0.6986(3) 0.0422(12) Uani 1 1 d . . . C41 C 0.8789(5) 0.9640(4) 0.7797(4) 0.0588(15) Uani 1 1 d . . . H41 H 0.8567 0.9310 0.8295 0.071 Uiso 1 1 calc R . . C42 C 0.9181(5) 1.0887(5) 0.7869(4) 0.0687(17) Uani 1 1 d . . . H42 H 0.9217 1.1394 0.8417 0.082 Uiso 1 1 calc R . . C43 C 0.9511(5) 1.1369(5) 0.7149(5) 0.0719(19) Uani 1 1 d . . . H43 H 0.9785 1.2205 0.7204 0.086 Uiso 1 1 calc R . . C44 C 0.9441(5) 1.0628(5) 0.6334(5) 0.0673(17) Uani 1 1 d . . . H44 H 0.9664 1.0967 0.5840 0.081 Uiso 1 1 calc R . . C45 C 0.9044(4) 0.9382(4) 0.6244(4) 0.0510(14) Uani 1 1 d . . . H45 H 0.8989 0.8880 0.5692 0.061 Uiso 1 1 calc R . . C50 C 0.8317(5) 0.6399(4) 0.5683(3) 0.0459(13) Uani 1 1 d . . . C51 C 0.9479(5) 0.6583(4) 0.5286(4) 0.0576(15) Uani 1 1 d . . . H51 H 1.0204 0.7068 0.5607 0.069 Uiso 1 1 calc R . . C52 C 0.9562(6) 0.6053(5) 0.4423(4) 0.0663(16) Uani 1 1 d . . . H52 H 1.0331 0.6201 0.4151 0.080 Uiso 1 1 calc R . . C53 C 0.8516(7) 0.5313(6) 0.3969(4) 0.088(2) Uani 1 1 d . . . H53 H 0.8574 0.4959 0.3382 0.106 Uiso 1 1 calc R . . C54 C 0.7377(7) 0.5077(6) 0.4354(4) 0.101(2) Uani 1 1 d . . . H54 H 0.6679 0.4537 0.4042 0.121 Uiso 1 1 calc R . . C55 C 0.7269(6) 0.5648(6) 0.5214(4) 0.0768(19) Uani 1 1 d . . . H55 H 0.6486 0.5521 0.5472 0.092 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 Fe 0.0377(4) 0.0276(3) 0.0339(4) 0.0044(3) 0.0043(3) 0.0035(3) S1 0.0398(7) 0.0241(5) 0.0313(6) 0.0041(5) 0.0022(5) 0.0038(5) S2 0.0549(8) 0.0288(6) 0.0397(7) 0.0070(5) 0.0066(6) -0.0022(6) S3 0.0542(8) 0.0319(6) 0.0398(7) 0.0077(5) 0.0124(6) 0.0115(6) S4 0.0521(8) 0.0303(6) 0.0439(8) 0.0045(5) 0.0142(6) -0.0025(5) C1 0.033(3) 0.033(2) 0.030(3) 0.005(2) -0.001(2) 0.0070(19) C2 0.032(3) 0.032(2) 0.038(3) 0.005(2) 0.000(2) 0.003(2) N1 0.050(3) 0.029(2) 0.032(2) 0.0043(17) 0.0024(19) 0.0063(18) N2 0.051(3) 0.028(2) 0.035(2) 0.0004(17) -0.001(2) 0.0001(18) C3 0.045(3) 0.034(3) 0.034(3) 0.005(2) -0.002(2) 0.006(2) C4 0.040(3) 0.040(3) 0.036(3) -0.003(2) -0.002(2) 0.006(2) C5 0.081(4) 0.047(3) 0.032(3) 0.006(2) -0.001(3) 0.005(3) C6 0.083(4) 0.038(3) 0.042(3) -0.004(2) -0.003(3) -0.004(3) C7 0.104(5) 0.062(4) 0.035(3) 0.004(3) 0.004(3) 0.005(3) C8 0.091(5) 0.057(4) 0.037(3) -0.012(3) -0.005(3) 0.002(3) C9 0.034(3) 0.034(2) 0.037(3) 0.007(2) 0.003(2) 0.002(2) C10 0.035(3) 0.032(2) 0.039(3) 0.003(2) 0.007(2) 0.001(2) N3 0.053(3) 0.038(2) 0.040(2) -0.0009(19) 0.008(2) 0.0042(19) N4 0.061(3) 0.043(2) 0.039(3) 0.005(2) 0.016(2) -0.005(2) C11 0.048(3) 0.038(3) 0.047(3) 0.000(2) 0.015(3) 0.000(2) C12 0.061(4) 0.049(3) 0.041(3) 0.001(3) 0.013(3) -0.005(3) C13 0.101(5) 0.050(3) 0.060(4) 0.000(3) 0.034(4) 0.006(3) C14 0.152(7) 0.063(4) 0.049(4) 0.009(3) 0.038(4) 0.000(4) C15 0.148(7) 0.063(4) 0.064(5) -0.005(3) 0.038(4) 0.009(4) C16 0.194(8) 0.079(5) 0.049(4) -0.003(4) 0.053(5) 0.005(5) As 0.0474(3) 0.0316(3) 0.0442(3) 0.0119(2) 0.0072(3) 0.0024(2) C20 0.040(3) 0.036(3) 0.041(3) 0.009(2) 0.011(2) 0.006(2) C21 0.044(3) 0.042(3) 0.078(4) 0.017(3) 0.005(3) 0.006(3) C22 0.049(4) 0.058(4) 0.085(5) 0.005(3) -0.010(3) 0.007(3) C23 0.051(4) 0.080(4) 0.070(4) 0.017(3) 0.000(3) 0.032(3) C24 0.064(4) 0.050(3) 0.084(5) 0.031(3) 0.009(4) 0.016(3) C25 0.049(3) 0.041(3) 0.061(4) 0.014(3) 0.004(3) 0.003(2) C30 0.052(3) 0.032(3) 0.047(3) 0.017(2) 0.008(2) 0.005(2) C31 0.061(4) 0.037(3) 0.049(3) 0.009(2) 0.004(3) 0.012(3) C32 0.060(4) 0.051(3) 0.044(3) 0.010(3) 0.010(3) 0.026(3) C33 0.045(3) 0.090(4) 0.051(4) 0.023(3) 0.010(3) 0.022(3) C34 0.050(4) 0.051(3) 0.086(4) 0.025(3) 0.011(3) 0.002(3) C35 0.045(3) 0.040(3) 0.086(4) 0.019(3) 0.015(3) 0.011(2) C40 0.042(3) 0.028(2) 0.056(3) 0.012(2) -0.002(3) 0.002(2) C41 0.074(4) 0.045(3) 0.057(4) 0.013(3) -0.005(3) 0.009(3) C42 0.069(4) 0.042(3) 0.088(5) -0.003(3) -0.010(4) 0.009(3) C43 0.053(4) 0.038(3) 0.124(6) 0.023(4) -0.001(4) 0.001(3) C44 0.054(4) 0.056(4) 0.107(5) 0.051(4) 0.023(4) 0.013(3) C45 0.048(3) 0.052(3) 0.061(4) 0.029(3) 0.008(3) 0.010(3) C50 0.056(3) 0.042(3) 0.040(3) 0.013(2) 0.011(3) 0.006(2) C51 0.053(4) 0.055(3) 0.060(4) 0.004(3) 0.003(3) 0.003(3) C52 0.074(4) 0.064(4) 0.058(4) 0.007(3) 0.019(3) 0.009(3) C53 0.091(6) 0.116(6) 0.048(4) -0.003(4) 0.007(4) 0.013(5) C54 0.079(5) 0.138(7) 0.057(5) -0.018(4) -0.011(4) -0.015(5) C55 0.054(4) 0.105(5) 0.055(4) -0.001(4) 0.005(3) -0.011(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 S4 2.2259(13) . ? Fe S3 2.2289(13) . ? Fe S1 2.2368(12) . ? Fe S2 2.2436(13) . ? Fe S1 2.4884(13) 2_656 ? S1 C1 1.765(4) . ? S1 Fe 2.4884(13) 2_656 ? S2 C2 1.739(4) . ? S3 C9 1.739(4) . ? S4 C10 1.744(4) . ? C1 N1 1.297(5) . ? C1 C2 1.442(5) . ? C2 N2 1.317(5) . ? N1 C3 1.365(5) . ? N2 C4 1.375(5) . ? C3 C5 1.399(6) . ? C3 C4 1.407(6) . ? C4 C6 1.404(6) . ? C5 C7 1.362(6) . ? C6 C8 1.357(7) . ? C7 C8 1.403(7) . ? C9 N3 1.306(5) . ? C9 C10 1.447(5) . ? C10 N4 1.302(5) . ? N3 C11 1.365(6) . ? N4 C12 1.380(6) . ? C11 C13 1.396(6) . ? C11 C12 1.408(6) . ? C12 C14 1.398(7) . ? C13 C15 1.356(7) . ? C14 C16 1.375(7) . ? C15 C16 1.388(8) . ? As C50 1.899(5) . ? As C30 1.911(5) . ? As C40 1.922(4) . ? As C20 1.924(5) . ? C20 C21 1.365(6) . ? C20 C25 1.386(6) . ? C21 C22 1.375(7) . ? C22 C23 1.374(7) . ? C23 C24 1.366(7) . ? C24 C25 1.372(7) . ? C30 C31 1.377(6) . ? C30 C35 1.387(6) . ? C31 C32 1.379(6) . ? C32 C33 1.371(6) . ? C33 C34 1.373(7) . ? C34 C35 1.379(6) . ? C40 C41 1.372(6) . ? C40 C45 1.378(6) . ? C41 C42 1.387(6) . ? C42 C43 1.348(8) . ? C43 C44 1.375(8) . ? C44 C45 1.383(6) . ? C50 C55 1.368(7) . ? C50 C51 1.391(6) . ? C51 C52 1.372(7) . ? C52 C53 1.353(7) . ? C53 C54 1.366(8) . ? C54 C55 1.386(8) . ? 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 S4 Fe S3 89.65(5) . . ? S4 Fe S1 168.26(5) . . ? S3 Fe S1 84.88(4) . . ? S4 Fe S2 90.40(5) . . ? S3 Fe S2 155.75(6) . . ? S1 Fe S2 90.35(5) . . ? S4 Fe S1 96.25(5) . 2_656 ? S3 Fe S1 103.75(5) . 2_656 ? S1 Fe S1 95.14(4) . 2_656 ? S2 Fe S1 100.35(5) . 2_656 ? C1 S1 Fe 105.16(14) . . ? C1 S1 Fe 99.92(14) . 2_656 ? Fe S1 Fe 84.86(4) . 2_656 ? C2 S2 Fe 105.03(14) . . ? C9 S3 Fe 104.43(15) . . ? C10 S4 Fe 104.26(15) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 S1 117.6(3) . . ? C2 C1 S1 118.9(3) . . ? N2 C2 C1 120.2(4) . . ? N2 C2 S2 119.3(3) . . ? C1 C2 S2 120.5(3) . . ? C1 N1 C3 116.9(4) . . ? C2 N2 C4 117.2(4) . . ? N1 C3 C5 120.4(4) . . ? N1 C3 C4 120.7(4) . . ? C5 C3 C4 118.9(4) . . ? N2 C4 C6 119.3(4) . . ? N2 C4 C3 121.4(4) . . ? C6 C4 C3 119.3(4) . . ? C7 C5 C3 121.5(5) . . ? C8 C6 C4 120.0(5) . . ? C5 C7 C8 118.9(5) . . ? C6 C8 C7 121.4(5) . . ? N3 C9 C10 122.4(4) . . ? N3 C9 S3 118.3(3) . . ? C10 C9 S3 119.3(3) . . ? N4 C10 C9 121.6(4) . . ? N4 C10 S4 119.6(3) . . ? C9 C10 S4 118.8(3) . . ? C9 N3 C11 116.8(4) . . ? C10 N4 C12 116.9(4) . . ? N3 C11 C13 119.6(5) . . ? N3 C11 C12 121.3(4) . . ? C13 C11 C12 119.1(5) . . ? N4 C12 C14 119.8(5) . . ? N4 C12 C11 121.1(4) . . ? C14 C12 C11 119.2(5) . . ? C15 C13 C11 121.3(5) . . ? C16 C14 C12 119.8(6) . . ? C13 C15 C16 119.7(6) . . ? C14 C16 C15 121.0(6) . . ? C50 As C30 109.6(2) . . ? C50 As C40 109.8(2) . . ? C30 As C40 110.47(19) . . ? C50 As C20 110.5(2) . . ? C30 As C20 107.82(18) . . ? C40 As C20 108.73(19) . . ? C21 C20 C25 119.7(5) . . ? C21 C20 As 120.7(3) . . ? C25 C20 As 119.5(4) . . ? C20 C21 C22 120.3(5) . . ? C23 C22 C21 119.9(5) . . ? C24 C23 C22 119.9(5) . . ? C23 C24 C25 120.4(5) . . ? C24 C25 C20 119.6(5) . . ? C31 C30 C35 120.2(5) . . ? C31 C30 As 119.5(3) . . ? C35 C30 As 120.3(4) . . ? C30 C31 C32 119.8(4) . . ? C33 C32 C31 119.9(5) . . ? C32 C33 C34 120.8(5) . . ? C33 C34 C35 119.7(5) . . ? C34 C35 C30 119.7(5) . . ? C41 C40 C45 120.5(4) . . ? C41 C40 As 120.3(4) . . ? C45 C40 As 119.2(4) . . ? C40 C41 C42 119.6(5) . . ? C43 C42 C41 120.4(6) . . ? C42 C43 C44 120.2(5) . . ? C43 C44 C45 120.6(5) . . ? C40 C45 C44 118.8(5) . . ? C55 C50 C51 119.3(5) . . ? C55 C50 As 121.2(4) . . ? C51 C50 As 119.5(4) . . ? C52 C51 C50 120.3(5) . . ? C53 C52 C51 119.6(6) . . ? C52 C53 C54 121.3(6) . . ? C53 C54 C55 119.6(6) . . ? C50 C55 C54 119.8(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_publ_flag C25 H25 N2 0.93 2.60 3.430(5) 1_555 148.1 ? C35 H35 N2 0.93 2.51 3.292(6) 1_555 141.5 ? C21 H21 N4 0.93 2.44 3.253(6) 2_766 146.6 ? C31 H31 N1 0.93 2.45 3.243(6) 1_565 142.7 ? C34 H34 N3 0.93 2.67 3.589(6) 2_656 168.5 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.334 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.078 # END of Crystallografic Information File