# cm010688u.cif #============================================================================ _publ_contact_author_name 'Xiao-Zeng You' _publ_contact_author_address ; Coordination Chemistry Institute Nanjing University Nanjing, 210093 P.R. China ; _publ_contact_author_email 'sklc@netra.nju.edu.cn' _publ_contact_author_fax '+86-25-3314502' _publ_requested_journal 'Chem. Mater.' #============================================================================ _publ_section_title ; A Novel Bis(trans-thiocyanate)iron(II) Spin Transition Molecular Material with Bidentate Triaryltriazole Ligands and its Bis(cis-thiocyanate)iron(II) High-spin Isomer ; loop_ _publ_author_name _publ_author_address ; 'Dunru Zhu, Yan Xu, Zhi Yu, Zijian Guo, Xiaozeng You*' Coordination Chemistry Institute Nanjing University Nanjing, 210093 P. R. China ; 'Hai Sang' ; National Laboratory of Solid State Microstructures Nanjing University Nanjing, 210093 P.R. China ; #============================================================================ data_Complex 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Fe N12 S2' _chemical_formula_weight 798.73 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 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.120(3) _cell_length_b 9.2563(18) _cell_length_c 11.576(2) _cell_angle_alpha 76.256(15) _cell_angle_beta 76.405(18) _cell_angle_gamma 84.983(19) _cell_volume 922.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 4.82 _cell_measurement_theta_max 10.01 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3276 _exptl_absorpt_correction_T_max 0.3632 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 10.63 _diffrn_reflns_number 3902 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3226 _reflns_number_gt 2492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97' _computing_structure_refinement 'SHELXTL-97' _computing_molecular_graphics 'SHELXTL-97' _computing_publication_material 'SHELXTL-97' _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^)+(0.0843P)^2^+0.2973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3226 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.0000 0.0000 0.0336(2) Uani 1 2 d S . . S1 S 0.05497(13) 0.39405(14) -0.34840(11) 0.0654(4) Uani 1 1 d . . . N1 N 0.0188(3) 0.0752(3) 0.1636(3) 0.0381(7) Uani 1 1 d . . . N2 N 0.2291(3) -0.0658(3) 0.0253(2) 0.0344(6) Uani 1 1 d . . . N3 N 0.3412(3) -0.1555(3) -0.0262(2) 0.0336(6) Uani 1 1 d . . . N4 N 0.3678(3) -0.1536(3) 0.1585(2) 0.0311(6) Uani 1 1 d . . . N5 N 0.6095(3) -0.3823(3) 0.1290(3) 0.0445(7) Uani 1 1 d . . . N6 N 0.0639(4) 0.2037(4) -0.1241(3) 0.0505(8) Uani 1 1 d . . . C1 C -0.0841(4) 0.1593(4) 0.2229(4) 0.0488(9) Uani 1 1 d . . . H1A H -0.1685 0.1947 0.1913 0.059 Uiso 1 1 calc R . . C2 C -0.0714(5) 0.1959(5) 0.3278(4) 0.0578(11) Uani 1 1 d . . . H2A H -0.1456 0.2552 0.3661 0.069 Uiso 1 1 calc R . . C3 C 0.0522(5) 0.1441(5) 0.3759(4) 0.0524(10) Uani 1 1 d . . . H3A H 0.0638 0.1687 0.4465 0.063 Uiso 1 1 calc R . . C4 C 0.1597(4) 0.0540(4) 0.3171(3) 0.0434(8) Uani 1 1 d . . . H4A H 0.2436 0.0156 0.3485 0.052 Uiso 1 1 calc R . . C5 C 0.1396(3) 0.0228(4) 0.2117(3) 0.0337(7) Uani 1 1 d . . . C6 C 0.2456(3) -0.0649(3) 0.1342(3) 0.0317(7) Uani 1 1 d . . . C7 C 0.4239(3) -0.2078(3) 0.0552(3) 0.0309(7) Uani 1 1 d . . . C8 C 0.5562(3) -0.3094(3) 0.0332(3) 0.0318(7) Uani 1 1 d . . . C9 C 0.6160(4) -0.3252(4) -0.0848(3) 0.0456(9) Uani 1 1 d . . . H9A H 0.5754 -0.2712 -0.1493 0.055 Uiso 1 1 calc R . . C10 C 0.7378(4) -0.4232(5) -0.1042(4) 0.0544(10) Uani 1 1 d . . . H10A H 0.7800 -0.4373 -0.1822 0.065 Uiso 1 1 calc R . . C11 C 0.7951(4) -0.4986(4) -0.0078(4) 0.0490(9) Uani 1 1 d . . . H11A H 0.8770 -0.5651 -0.0188 0.059 Uiso 1 1 calc R . . C12 C 0.7302(4) -0.4751(4) 0.1063(4) 0.0517(10) Uani 1 1 d . . . H12A H 0.7717 -0.5257 0.1713 0.062 Uiso 1 1 calc R . . C13 C 0.4193(3) -0.1903(3) 0.2722(3) 0.0305(7) Uani 1 1 d . . . C14 C 0.3471(3) -0.2990(4) 0.3662(3) 0.0348(7) Uani 1 1 d . . . H14A H 0.2673 -0.3480 0.3568 0.042 Uiso 1 1 calc R . . C15 C 0.3945(4) -0.3347(4) 0.4751(3) 0.0382(8) Uani 1 1 d . . . H15A H 0.3477 -0.4098 0.5384 0.046 Uiso 1 1 calc R . . C16 C 0.5117(4) -0.2592(4) 0.4906(3) 0.0398(8) Uani 1 1 d . . . C17 C 0.5812(4) -0.1501(4) 0.3935(3) 0.0465(9) Uani 1 1 d . . . H17A H 0.6601 -0.0993 0.4023 0.056 Uiso 1 1 calc R . . C18 C 0.5361(4) -0.1149(4) 0.2839(3) 0.0393(8) Uani 1 1 d . . . H18A H 0.5839 -0.0417 0.2195 0.047 Uiso 1 1 calc R . . C19 C 0.5622(3) -0.2969(3) 0.6095(3) 0.0648(12) Uani 1 1 d . . . H19A H 0.5013 -0.3742 0.6657 0.097 Uiso 1 1 calc R . . H19B H 0.5512 -0.2101 0.6429 0.097 Uiso 1 1 calc R . . H19C H 0.6661 -0.3305 0.5956 0.097 Uiso 1 1 calc R . . C20 C 0.0610(3) 0.2835(3) -0.2177(3) 0.0427(8) Uani 1 1 d 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 Fe1 0.0281(4) 0.0364(4) 0.0358(4) -0.0061(3) -0.0118(3) 0.0084(3) S1 0.0574(7) 0.0708(7) 0.0572(7) 0.0111(5) -0.0162(5) -0.0052(5) N1 0.0322(14) 0.0396(15) 0.0424(16) -0.0115(12) -0.0099(12) 0.0100(12) N2 0.0289(14) 0.0405(15) 0.0352(15) -0.0106(12) -0.0120(11) 0.0115(12) N3 0.0294(14) 0.0398(15) 0.0307(14) -0.0084(11) -0.0074(11) 0.0075(11) N4 0.0248(13) 0.0380(14) 0.0316(14) -0.0080(11) -0.0109(11) 0.0068(11) N5 0.0428(17) 0.0503(18) 0.0429(17) -0.0156(14) -0.0162(13) 0.0178(14) N6 0.0475(18) 0.0453(18) 0.055(2) -0.0013(16) -0.0137(15) -0.0020(14) C1 0.041(2) 0.050(2) 0.052(2) -0.0147(18) -0.0085(17) 0.0183(16) C2 0.050(2) 0.063(3) 0.060(3) -0.028(2) -0.0067(19) 0.024(2) C3 0.060(3) 0.058(2) 0.044(2) -0.0236(19) -0.0097(18) 0.0052(19) C4 0.044(2) 0.047(2) 0.043(2) -0.0157(16) -0.0130(16) 0.0083(16) C5 0.0292(16) 0.0342(16) 0.0364(17) -0.0077(13) -0.0074(13) 0.0046(13) C6 0.0248(15) 0.0357(17) 0.0352(17) -0.0069(13) -0.0106(13) 0.0036(13) C7 0.0267(15) 0.0360(16) 0.0292(16) -0.0068(13) -0.0066(13) 0.0028(13) C8 0.0253(15) 0.0337(17) 0.0383(18) -0.0094(14) -0.0106(13) 0.0024(13) C9 0.0393(19) 0.058(2) 0.0377(19) -0.0140(17) -0.0069(15) 0.0109(17) C10 0.044(2) 0.066(3) 0.051(2) -0.025(2) 0.0036(18) 0.0076(19) C11 0.0306(18) 0.046(2) 0.072(3) -0.0222(19) -0.0109(18) 0.0140(16) C12 0.049(2) 0.050(2) 0.063(3) -0.0174(19) -0.0285(19) 0.0211(18) C13 0.0245(15) 0.0380(17) 0.0301(16) -0.0102(13) -0.0092(12) 0.0084(13) C14 0.0266(16) 0.0396(18) 0.0393(18) -0.0121(14) -0.0077(13) 0.0025(13) C15 0.0408(19) 0.0370(18) 0.0320(17) -0.0052(14) -0.0036(14) 0.0049(14) C16 0.0436(19) 0.047(2) 0.0329(18) -0.0127(15) -0.0147(15) 0.0055(16) C17 0.045(2) 0.055(2) 0.046(2) -0.0112(17) -0.0206(17) -0.0078(17) C18 0.0388(19) 0.0432(19) 0.0339(18) -0.0017(14) -0.0088(14) -0.0078(15) C19 0.094(3) 0.062(3) 0.045(2) -0.003(2) -0.037(2) -0.006(2) C20 0.0319(18) 0.0418(19) 0.052(2) -0.0087(17) -0.0074(16) -0.0003(15) _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 N6 2.114(3) . ? Fe1 N6 2.114(3) 2 ? Fe1 N2 2.192(2) . ? Fe1 N2 2.192(2) 2 ? Fe1 N1 2.213(3) . ? Fe1 N1 2.213(3) 2 ? S1 C20 1.622(3) . ? N1 C1 1.335(4) . ? N1 C5 1.351(4) . ? N2 C6 1.306(4) . ? N2 N3 1.374(4) . ? N3 C7 1.321(4) . ? N4 C6 1.368(4) . ? N4 C7 1.376(4) . ? N4 C13 1.456(4) . ? N5 C8 1.328(4) . ? N5 C12 1.350(5) . ? N6 C20 1.162(4) . ? C1 C2 1.368(6) . ? C2 C3 1.373(6) . ? C3 C4 1.390(5) . ? C4 C5 1.374(5) . ? C5 C6 1.483(4) . ? C7 C8 1.476(4) . ? C8 C9 1.384(5) . ? C9 C10 1.382(5) . ? C10 C11 1.358(6) . ? C11 C12 1.374(6) . ? C13 C18 1.372(5) . ? C13 C14 1.375(5) . ? C14 C15 1.384(5) . ? C15 C16 1.395(5) . ? C16 C17 1.387(5) . ? C16 C19 1.506(4) . ? C17 C18 1.382(5) . ? 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 N6 Fe1 N6 180.0(2) . 2 ? N6 Fe1 N2 94.52(11) . . ? N6 Fe1 N2 85.48(11) 2 . ? N6 Fe1 N2 85.48(11) . 2 ? N6 Fe1 N2 94.52(11) 2 2 ? N2 Fe1 N2 180.00(13) . 2 ? N6 Fe1 N1 95.30(12) . . ? N6 Fe1 N1 84.70(12) 2 . ? N2 Fe1 N1 74.17(10) . . ? N2 Fe1 N1 105.83(10) 2 . ? N6 Fe1 N1 84.70(12) . 2 ? N6 Fe1 N1 95.30(12) 2 2 ? N2 Fe1 N1 105.83(10) . 2 ? N2 Fe1 N1 74.17(10) 2 2 ? N1 Fe1 N1 180.00(12) . 2 ? C1 N1 C5 117.6(3) . . ? C1 N1 Fe1 125.4(2) . . ? C5 N1 Fe1 116.9(2) . . ? C6 N2 N3 109.0(2) . . ? C6 N2 Fe1 113.0(2) . . ? N3 N2 Fe1 133.3(2) . . ? C7 N3 N2 106.5(2) . . ? C6 N4 C7 104.8(2) . . ? C6 N4 C13 127.1(3) . . ? C7 N4 C13 128.0(2) . . ? C8 N5 C12 116.3(3) . . ? C20 N6 Fe1 148.3(3) . . ? N1 C1 C2 123.2(3) . . ? C1 C2 C3 119.1(3) . . ? C2 C3 C4 118.8(3) . . ? C5 C4 C3 118.7(3) . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 111.3(3) . . ? C4 C5 C6 126.1(3) . . ? N2 C6 N4 109.6(3) . . ? N2 C6 C5 120.9(3) . . ? N4 C6 C5 129.5(3) . . ? N3 C7 N4 110.1(3) . . ? N3 C7 C8 122.7(3) . . ? N4 C7 C8 127.2(3) . . ? N5 C8 C9 123.8(3) . . ? N5 C8 C7 117.5(3) . . ? C9 C8 C7 118.6(3) . . ? C10 C9 C8 118.2(3) . . ? C11 C10 C9 119.2(4) . . ? C10 C11 C12 118.9(3) . . ? N5 C12 C11 123.5(3) . . ? C18 C13 C14 121.7(3) . . ? C18 C13 N4 119.7(3) . . ? C14 C13 N4 118.6(3) . . ? C13 C14 C15 119.2(3) . . ? C14 C15 C16 120.6(3) . . ? C17 C16 C15 118.2(3) . . ? C17 C16 C19 121.1(3) . . ? C15 C16 C19 120.6(3) . . ? C18 C17 C16 121.6(3) . . ? C13 C18 C17 118.6(3) . . ? N6 C20 S1 179.3(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.575 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.084 #============================================================================ data_Complex 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Fe N12 S2' _chemical_formula_weight 798.73 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 21.851(3) _cell_length_b 13.4113(15) _cell_length_c 16.859(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.153(9) _cell_angle_gamma 90.00 _cell_volume 3885.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 7.27 _cell_measurement_theta_max 12.38 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6634 _exptl_absorpt_correction_T_max 0.7113 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 7.08 _diffrn_reflns_number 4052 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3412 _reflns_number_gt 1865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXTL' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _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^)+(0.1129P)^2^+3.5619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXTL _refine_ls_extinction_coef 0.0116(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3412 _refine_ls_number_parameters 250 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.010 _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 Fe1 Fe 0.0000 0.20979(5) 0.2500 0.07773(19) Uani 1 2 d S . . S1 S 0.13642(6) 0.03561(12) 0.15769(9) 0.1629(5) Uani 1 1 d . . . N1 N 0.10203(11) 0.23388(18) 0.40983(16) 0.0776(7) Uani 1 1 d . . . N2 N 0.06482(13) 0.3421(2) 0.25363(16) 0.0863(8) Uani 1 1 d . . . N3 N 0.04217(13) 0.4161(2) 0.18399(17) 0.0922(9) Uani 1 1 d . . . N4 N 0.12574(12) 0.47818(19) 0.33767(16) 0.0805(8) Uani 1 1 d . A . N5 N 0.05223(14) 0.1137(2) 0.21357(19) 0.1032(10) Uani 1 1 d . . . N6 N 0.06713(17) 0.6768(3) 0.23209(19) 0.1152(12) Uani 1 1 d . . . C1 C 0.12535(16) 0.1699(3) 0.4841(2) 0.0893(11) Uani 1 1 d . . . H1A H 0.0977 0.1108 0.4681 0.107 Uiso 1 1 calc R . . C2 C 0.18878(17) 0.1869(3) 0.5843(2) 0.0989(13) Uani 1 1 d . . . H2A H 0.2026 0.1410 0.6342 0.119 Uiso 1 1 calc R . . C3 C 0.23048(18) 0.2734(3) 0.6074(2) 0.0979(13) Uani 1 1 d . . . H3A H 0.2728 0.2874 0.6738 0.118 Uiso 1 1 calc R . . C4 C 0.20903(17) 0.3387(3) 0.5317(2) 0.0946(12) Uani 1 1 d . . . H4A H 0.2378 0.3964 0.5459 0.114 Uiso 1 1 calc R . . C5 C 0.14423(15) 0.3183(2) 0.43403(19) 0.0773(9) Uani 1 1 d . . . C6 C 0.11396(15) 0.3795(2) 0.34422(19) 0.0791(9) Uani 1 1 d . . . C7 C 0.07905(15) 0.4977(3) 0.23499(19) 0.0844(10) Uani 1 1 d . . . C8 C 0.06682(16) 0.5939(3) 0.1869(2) 0.0883(10) Uani 1 1 d . . . C9 C 0.04962(18) 0.5946(3) 0.0955(2) 0.1104(12) Uani 1 1 d . . . H9A H 0.0524 0.5363 0.0679 0.132 Uiso 1 1 calc R . . C10 C 0.0278(2) 0.6835(4) 0.0430(3) 0.1375(17) Uani 1 1 d . . . H10A H 0.0132 0.6849 -0.0218 0.165 Uiso 1 1 calc R . . C11 C 0.0276(2) 0.7670(3) 0.0853(3) 0.1215(15) Uani 1 1 d . . . H11A H 0.0144 0.8275 0.0515 0.146 Uiso 1 1 calc R . . C12 C 0.0471(2) 0.7622(3) 0.1786(3) 0.1248(16) Uani 1 1 d . . . H12A H 0.0466 0.8209 0.2076 0.150 Uiso 1 1 calc R . . C13 C 0.15534(19) 0.5753(3) 0.4786(2) 0.1015(13) Uani 1 1 d . A . H13A H 0.1065 0.5595 0.4598 0.122 Uiso 1 1 calc R . . C14 C 0.2073(2) 0.6307(4) 0.5640(3) 0.1353(18) Uani 1 1 d . . . H14A H 0.1939 0.6526 0.6038 0.162 Uiso 0.274(6) 1 calc PR A 2 C15 C 0.2769(3) 0.6530(4) 0.5898(4) 0.175(3) Uani 1 1 d U A . H15A H 0.3115 0.6903 0.6478 0.209 Uiso 1 1 calc R . . C16 C 0.2990(2) 0.6226(4) 0.5335(4) 0.159(2) Uani 1 1 d U . . H16A H 0.3480 0.6393 0.5531 0.191 Uiso 0.726(6) 1 calc PR A 1 C17 C 0.24752(19) 0.5663(3) 0.4458(3) 0.1152(15) Uani 1 1 d . A . H17A H 0.2609 0.5450 0.4057 0.138 Uiso 1 1 calc R . . C18 C 0.17707(16) 0.5441(2) 0.4220(2) 0.0837(11) Uani 1 1 d . . . C19 C 0.08752(17) 0.0794(2) 0.1904(2) 0.0879(11) Uani 1 1 d . . . C20 C 0.1882(4) 0.6644(7) 0.6273(6) 0.187(3) Uiso 0.726(6) 1 d P A 1 H20A H 0.2310 0.7016 0.6830 0.280 Uiso 0.726(6) 1 calc PR A 1 H20B H 0.1777 0.6079 0.6523 0.280 Uiso 0.726(6) 1 calc PR A 1 H20C H 0.1429 0.7063 0.5888 0.280 Uiso 0.726(6) 1 calc PR A 1 C20A C 0.3827(7) 0.6237(12) 0.5864(10) 0.115(5) Uiso 0.274(6) 1 d P A 2 H20D H 0.4074 0.6666 0.6442 0.172 Uiso 0.274(6) 1 calc PR A 2 H20E H 0.3929 0.6478 0.5420 0.172 Uiso 0.274(6) 1 calc PR A 2 H20F H 0.4029 0.5573 0.6080 0.172 Uiso 0.274(6) 1 calc PR A 2 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 0.0834(2) 0.0665(3) 0.0910(3) 0.000 0.05771(19) 0.000 S1 0.1940(5) 0.1498(11) 0.2243(7) -0.0167(7) 0.1689(4) 0.0208(7) N1 0.0825(9) 0.0688(14) 0.0925(11) 0.0032(10) 0.0596(8) 0.0022(11) N2 0.0985(11) 0.0846(16) 0.0757(10) -0.0089(12) 0.0538(9) -0.0137(13) N3 0.1141(12) 0.0858(17) 0.0821(11) -0.0075(12) 0.0633(9) -0.0253(13) N4 0.0876(10) 0.0763(15) 0.0775(10) -0.0089(11) 0.0510(8) -0.0150(11) N5 0.0999(12) 0.095(2) 0.1190(15) -0.0162(14) 0.0695(11) -0.0038(14) N6 0.1461(18) 0.098(2) 0.0957(14) 0.0010(14) 0.0717(13) -0.0129(17) C1 0.0920(14) 0.0786(19) 0.0967(15) 0.0056(15) 0.0579(11) 0.0053(15) C2 0.0983(16) 0.090(2) 0.0945(17) 0.0135(16) 0.0527(13) 0.0099(17) C3 0.0967(16) 0.097(3) 0.0848(16) 0.0020(17) 0.0485(13) 0.0009(18) C4 0.0935(15) 0.090(2) 0.0897(16) -0.0031(17) 0.0512(13) -0.0065(17) C5 0.0793(12) 0.0755(18) 0.0763(13) -0.0036(13) 0.0476(10) -0.0024(14) C6 0.0900(12) 0.0762(19) 0.0837(12) -0.0076(13) 0.0599(9) -0.0116(14) C7 0.0973(13) 0.084(2) 0.0780(12) -0.0086(14) 0.0572(10) -0.0208(15) C8 0.1029(14) 0.089(2) 0.0783(13) -0.0140(14) 0.0585(10) -0.0308(15) C9 0.1583(18) 0.095(2) 0.1001(15) -0.0194(16) 0.0912(13) -0.0443(19) C10 0.187(3) 0.135(3) 0.0899(17) -0.0115(19) 0.0852(16) -0.062(3) C11 0.134(2) 0.119(3) 0.0955(18) 0.011(2) 0.0630(16) -0.033(2) C12 0.162(2) 0.102(3) 0.115(2) 0.005(2) 0.0877(17) -0.001(2) C13 0.1092(18) 0.102(2) 0.0784(15) -0.0165(16) 0.0504(13) -0.0040(19) C14 0.148(3) 0.132(3) 0.0966(19) -0.030(2) 0.0609(18) 0.018(3) C15 0.134(3) 0.152(4) 0.177(4) -0.076(3) 0.065(3) -0.029(3) C16 0.096(2) 0.147(4) 0.190(4) -0.053(3) 0.067(2) -0.042(3) C17 0.0983(18) 0.096(3) 0.133(2) -0.015(2) 0.0627(16) -0.0189(19) C18 0.0828(14) 0.0759(19) 0.0745(14) -0.0087(14) 0.0396(11) -0.0105(15) C19 0.0897(14) 0.075(2) 0.0984(16) -0.0099(15) 0.0577(12) 0.0035(15) _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 N5 2.051(3) 2 ? Fe1 N5 2.051(3) . ? Fe1 N1 2.2166(19) 2 ? Fe1 N1 2.2166(19) . ? Fe1 N2 2.248(3) . ? Fe1 N2 2.248(3) 2 ? S1 C19 1.586(4) . ? N1 C1 1.332(4) . ? N1 C5 1.354(4) . ? N2 C6 1.308(3) . ? N2 N3 1.375(4) . ? N3 C7 1.315(4) . ? N4 C6 1.365(4) . ? N4 C7 1.387(3) . ? N4 C18 1.446(3) . ? N5 C19 1.154(5) . ? N6 C8 1.346(5) . ? N6 C12 1.351(5) . ? C1 C2 1.390(4) . ? C2 C3 1.374(5) . ? C3 C4 1.370(5) . ? C4 C5 1.382(3) . ? C5 C6 1.472(4) . ? C7 C8 1.458(5) . ? C8 C9 1.343(5) . ? C9 C10 1.381(5) . ? C10 C11 1.329(6) . ? C11 C12 1.354(6) . ? C13 C18 1.368(6) . ? C13 C14 1.377(5) . ? C14 C15 1.332(7) . ? C14 C20 1.439(10) . ? C15 C16 1.366(9) . ? C16 C17 1.403(6) . ? C16 C20A 1.457(13) . ? C17 C18 1.362(5) . ? 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 N5 Fe1 N5 102.13(18) 2 . ? N5 Fe1 N1 97.34(9) 2 2 ? N5 Fe1 N1 93.17(9) . 2 ? N5 Fe1 N1 93.17(9) 2 . ? N5 Fe1 N1 97.34(9) . . ? N1 Fe1 N1 163.24(13) 2 . ? N5 Fe1 N2 161.05(11) 2 . ? N5 Fe1 N2 92.66(12) . . ? N1 Fe1 N2 93.54(8) 2 . ? N1 Fe1 N2 73.03(9) . . ? N5 Fe1 N2 92.66(12) 2 2 ? N5 Fe1 N2 161.05(11) . 2 ? N1 Fe1 N2 73.03(9) 2 2 ? N1 Fe1 N2 93.54(8) . 2 ? N2 Fe1 N2 75.72(15) . 2 ? C1 N1 C5 117.5(2) . . ? C1 N1 Fe1 124.21(19) . . ? C5 N1 Fe1 118.32(18) . . ? C6 N2 N3 108.8(3) . . ? C6 N2 Fe1 112.6(2) . . ? N3 N2 Fe1 131.17(16) . . ? C7 N3 N2 106.9(2) . . ? C6 N4 C7 104.7(2) . . ? C6 N4 C18 125.7(2) . . ? C7 N4 C18 129.6(3) . . ? C19 N5 Fe1 164.5(3) . . ? C8 N6 C12 115.9(3) . . ? N1 C1 C2 123.5(3) . . ? C3 C2 C1 118.2(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 119.5(3) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 111.5(2) . . ? C4 C5 C6 126.4(3) . . ? N2 C6 N4 109.7(3) . . ? N2 C6 C5 120.7(3) . . ? N4 C6 C5 129.5(2) . . ? N3 C7 N4 109.9(3) . . ? N3 C7 C8 123.0(2) . . ? N4 C7 C8 127.0(3) . . ? C9 C8 N6 122.9(3) . . ? C9 C8 C7 118.0(3) . . ? N6 C8 C7 118.9(3) . . ? C8 C9 C10 118.8(4) . . ? C11 C10 C9 119.8(4) . . ? C10 C11 C12 118.7(4) . . ? N6 C12 C11 123.7(4) . . ? C18 C13 C14 118.5(4) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 C20 119.0(5) . . ? C13 C14 C20 121.0(5) . . ? C14 C15 C16 122.0(5) . . ? C15 C16 C17 119.7(5) . . ? C15 C16 C20A 114.8(8) . . ? C17 C16 C20A 122.5(8) . . ? C18 C17 C16 116.9(5) . . ? C17 C18 C13 122.9(3) . . ? C17 C18 N4 118.2(4) . . ? C13 C18 N4 118.7(3) . . ? N5 C19 S1 178.2(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.315 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.061 #===END