#------------------------------------------------------------------------------ #$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1351 $ #$URL: svn://localhost/testcod/cif/4/30/00/4300040.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4300040 loop_ _publ_author_name 'Chuang, Yu-Chun' 'Liu, Chi-Tsun' 'Sheu, Chou-Fu' 'Ho, Wei-Lun' 'Lee, Gene-Hsiang' 'Wang, Chih-Cheh' 'Wang, Yu' _publ_section_title ; New Iron(II) Spin Crossover Coordination Polymers [Fe(\m-atrz)3]X2·2H2O (X = ClO4¯, BF4¯) and [Fe(\m-atrz)(\m-pyz)(NCS)2]·4H2O with an Interesting Solvent Effect ; _journal_issue 8 _journal_name_full 'Inorganic Chemistry' _journal_page_first 4663 _journal_page_last 4671 _journal_paper_doi 10.1021/ic202626c _journal_volume 51 _journal_year 2012 _chemical_formula_sum 'C12 H16 Cl2 Fe N24 O10' _chemical_formula_weight 783.24 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.286(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.0267(4) _cell_length_b 19.4307(9) _cell_length_c 8.9609(4) _cell_measurement_reflns_used all _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 1.00 _cell_volume 1395.28(11) _computing_cell_refinement DENZO-SMN _computing_data_collection 'NONIUS COLLECT' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0944 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12936 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.10 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_T_max 0.8856 _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SORTAV _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_meas not_measured _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.693 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 2456 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0611 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+2.3767P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1531 _refine_ls_wR_factor_ref 0.1793 _reflns_number_gt 1585 _reflns_number_total 2456 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic202626c_si_002.cif _cod_data_source_block CCDC-855738 _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 4300040 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' 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 0.0217(3) Uani 1 2 d S . . Cl1 Cl -0.3253(3) 0.18283(9) 0.58883(19) 0.0585(6) Uani 1 1 d . . . O1 O -0.2858(5) 0.1793(2) 0.7471(5) 0.0500(12) Uani 1 1 d . . . O2 O -0.1979(8) 0.1488(3) 0.5145(6) 0.090(2) Uani 1 1 d . . . O3 O -0.4886(8) 0.1481(3) 0.5610(7) 0.0870(18) Uani 1 1 d . . . O4 O -0.3434(8) 0.2513(3) 0.5443(6) 0.085(2) Uani 1 1 d D . . N1 N -0.1328(5) 0.0764(2) 0.0806(4) 0.0231(10) Uani 1 1 d . . . N2 N -0.3066(5) 0.0808(2) 0.0709(5) 0.0303(11) Uani 1 1 d . . . N3 N -0.2018(5) 0.1748(2) 0.1708(5) 0.0291(11) Uani 1 1 d . . . N4 N -0.1776(6) 0.2402(2) 0.2325(5) 0.0319(11) Uani 1 1 d . . . N5 N -0.3115(6) 0.2723(2) 0.2258(5) 0.0323(11) Uani 1 1 d . . . N6 N -0.2871(5) 0.3370(2) 0.2896(4) 0.0286(11) Uani 1 1 d D . . N8 N -0.3635(5) 0.4289(2) 0.4045(4) 0.0237(10) Uani 1 1 d . . . N7 N -0.1893(6) 0.4240(2) 0.4226(5) 0.0330(11) Uani 1 1 d . . . N9 N 0.1472(5) 0.0033(2) 0.1876(4) 0.0247(9) Uani 1 1 d . . . N10 N 0.0711(5) 0.0068(2) 0.3250(5) 0.0286(10) Uani 1 1 d . . . N11 N 0.3422(5) 0.0037(2) 0.3658(5) 0.0273(10) Uani 1 1 d . . . N12 N 0.5029(5) 0.0008(2) 0.4309(5) 0.0267(10) Uani 1 1 d . . . C1 C -0.0733(7) 0.1325(3) 0.1431(6) 0.0287(12) Uani 1 1 d . . . H1A H 0.0415 0.1421 0.1656 0.034 Uiso 1 1 calc R . . C2 C -0.3447(7) 0.1401(3) 0.1256(6) 0.0330(13) Uani 1 1 d . . . H2A H -0.4550 0.1570 0.1331 0.040 Uiso 1 1 calc R . . C4 C -0.4182(7) 0.3764(3) 0.3254(6) 0.0289(12) Uani 1 1 d . . . H4A H -0.5320 0.3673 0.2974 0.035 Uiso 1 1 calc R . . C3 C -0.1485(7) 0.3681(3) 0.3552(6) 0.0335(13) Uani 1 1 d . . . H3A H -0.0379 0.3511 0.3517 0.040 Uiso 1 1 calc R . . C5 C 0.3093(6) 0.0016(2) 0.2136(5) 0.0248(11) Uani 1 1 d . . . H5A H 0.3899 -0.0008 0.1402 0.030 Uiso 1 1 calc R . . C6 C 0.1902(7) 0.0068(3) 0.4293(6) 0.0327(13) Uani 1 1 d . . . H6A H 0.1748 0.0087 0.5336 0.039 Uiso 1 1 calc R . . O5 O -0.6952(7) 0.1666(3) 0.2988(7) 0.0771(16) Uani 1 1 d . . . H5B H -0.7098 0.1705 0.4088 0.116 Uiso 1 1 d R . . H5C H -0.7154 0.2158 0.2692 0.116 Uiso 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 0.0241(6) 0.0207(6) 0.0202(5) 0.0007(4) 0.0008(4) -0.0010(5) Cl1 0.0865(14) 0.0466(10) 0.0433(9) 0.0087(8) 0.0127(9) 0.0246(10) O1 0.038(3) 0.067(3) 0.044(2) 0.017(2) 0.0019(19) 0.001(2) O2 0.127(5) 0.079(4) 0.069(4) 0.018(3) 0.048(4) 0.052(4) O3 0.081(4) 0.095(5) 0.082(4) -0.021(3) -0.020(3) -0.007(4) O4 0.147(6) 0.048(3) 0.065(3) 0.019(3) 0.046(4) 0.034(3) N1 0.026(3) 0.022(2) 0.021(2) 0.0006(18) -0.0008(18) -0.0010(19) N2 0.024(3) 0.033(3) 0.034(3) -0.006(2) 0.002(2) 0.005(2) N3 0.034(3) 0.022(2) 0.031(2) -0.0050(19) 0.000(2) 0.000(2) N4 0.036(3) 0.027(3) 0.034(3) -0.007(2) 0.004(2) 0.000(2) N5 0.033(3) 0.029(2) 0.035(3) -0.007(2) 0.004(2) 0.003(2) N6 0.030(3) 0.025(2) 0.031(2) -0.0076(19) 0.003(2) 0.004(2) N8 0.026(3) 0.022(2) 0.022(2) 0.0028(18) -0.0008(18) 0.0007(19) N7 0.030(3) 0.033(3) 0.036(3) -0.011(2) 0.000(2) 0.001(2) N9 0.030(2) 0.023(2) 0.021(2) 0.0008(18) 0.0051(17) 0.001(2) N10 0.030(2) 0.032(3) 0.024(2) 0.0032(19) 0.0036(19) -0.001(2) N11 0.025(2) 0.034(3) 0.023(2) 0.0010(19) -0.0007(18) -0.001(2) N12 0.026(2) 0.030(2) 0.0237(19) 0.000(2) -0.0003(18) 0.002(2) C1 0.025(3) 0.027(3) 0.034(3) -0.001(2) 0.001(2) 0.003(2) C2 0.030(3) 0.038(3) 0.031(3) -0.008(2) -0.003(2) 0.007(3) C4 0.032(3) 0.024(3) 0.030(3) -0.003(2) 0.003(2) 0.000(2) C3 0.024(3) 0.035(3) 0.041(3) -0.007(3) 0.001(2) 0.003(3) C5 0.027(3) 0.023(3) 0.024(3) -0.002(2) 0.002(2) 0.001(2) C6 0.031(3) 0.043(3) 0.024(3) -0.002(2) 0.006(2) -0.002(3) O5 0.068(4) 0.067(4) 0.095(4) 0.000(3) -0.007(3) 0.000(3) 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 Fe1 N1 180.0(3) . 3 ? N1 Fe1 N8 87.58(16) . 4_665 ? N1 Fe1 N8 92.42(16) 3 4_665 ? N1 Fe1 N8 92.42(16) . 2_445 ? N1 Fe1 N8 87.58(16) 3 2_445 ? N8 Fe1 N8 180.0(3) 4_665 2_445 ? N1 Fe1 N9 91.52(16) . 3 ? N1 Fe1 N9 88.48(16) 3 3 ? N8 Fe1 N9 88.53(16) 4_665 3 ? N8 Fe1 N9 91.47(16) 2_445 3 ? N1 Fe1 N9 88.48(16) . . ? N1 Fe1 N9 91.52(16) 3 . ? N8 Fe1 N9 91.47(16) 4_665 . ? N8 Fe1 N9 88.53(16) 2_445 . ? N9 Fe1 N9 180.0(3) 3 . ? O4 Cl1 O2 112.2(3) . . ? O4 Cl1 O1 109.9(3) . . ? O2 Cl1 O1 108.5(3) . . ? O4 Cl1 O3 108.0(4) . . ? O2 Cl1 O3 111.3(4) . . ? O1 Cl1 O3 106.7(3) . . ? C1 N1 N2 108.4(4) . . ? C1 N1 Fe1 126.2(4) . . ? N2 N1 Fe1 125.3(3) . . ? C2 N2 N1 106.7(4) . . ? C1 N3 C2 106.2(4) . . ? C1 N3 N4 122.4(4) . . ? C2 N3 N4 131.4(5) . . ? N5 N4 N3 109.7(5) . . ? N4 N5 N6 109.4(4) . . ? C4 N6 C3 105.7(4) . . ? C4 N6 N5 121.1(4) . . ? C3 N6 N5 132.0(5) . . ? C4 N8 N7 108.2(4) . . ? C4 N8 Fe1 126.9(4) . 2_455 ? N7 N8 Fe1 124.6(3) . 2_455 ? C3 N7 N8 106.3(4) . . ? C5 N9 N10 108.8(4) . . ? C5 N9 Fe1 133.0(3) . . ? N10 N9 Fe1 118.1(3) . . ? C6 N10 N9 106.9(4) . . ? C5 N11 C6 106.7(4) . . ? C5 N11 N12 122.5(4) . . ? C6 N11 N12 130.8(4) . . ? N12 N12 N11 109.5(5) 3_656 . ? N1 C1 N3 108.9(5) . . ? N2 C2 N3 109.8(5) . . ? N8 C4 N6 109.2(5) . . ? N7 C3 N6 110.6(5) . . ? N9 C5 N11 107.9(4) . . ? N10 C6 N11 109.6(5) . . ? N1 C1 H1A 125.6 . . ? N3 C1 H1A 125.6 . . ? N2 C2 H2A 125.1 . . ? N3 C2 H2A 125.1 . . ? N8 C4 H4A 125.4 . . ? N6 C4 H4A 125.4 . . ? N7 C3 H3A 124.7 . . ? N6 C3 H3A 124.7 . . ? N9 C5 H5A 126.0 . . ? N11 C5 H5A 126.0 . . ? N10 C6 H6A 125.2 . . ? N11 C6 H6A 125.2 . . ? H5B O5 H5C 99.2 . . ? 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 1.987(4) . ? Fe1 N1 1.987(4) 3 ? Fe1 N8 1.988(4) 4_665 ? Fe1 N8 1.988(4) 2_445 ? Fe1 N9 2.000(4) 3 ? Fe1 N9 2.000(4) . ? Cl1 O4 1.395(5) . ? Cl1 O2 1.416(5) . ? Cl1 O1 1.437(5) . ? Cl1 O3 1.482(6) . ? N1 C1 1.304(6) . ? N1 N2 1.396(6) . ? N2 C2 1.295(7) . ? N3 C1 1.354(7) . ? N3 C2 1.372(7) . ? N3 N4 1.394(6) . ? N4 N5 1.242(6) . ? N5 N6 1.390(6) . ? N6 C4 1.356(7) . ? N6 C3 1.369(7) . ? N8 C4 1.303(6) . ? N8 N7 1.402(6) . ? N8 Fe1 1.988(4) 2_455 ? N7 C3 1.293(7) . ? N9 C5 1.309(7) . ? N9 N10 1.407(6) . ? N10 C6 1.299(7) . ? N11 C5 1.375(6) . ? N11 C6 1.377(7) . ? N11 N12 1.386(6) . ? N12 N12 1.242(8) 3_656 ? C1 H1A 0.9500 . ? C2 H2A 0.9500 . ? C4 H4A 0.9500 . ? C3 H3A 0.9500 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? O5 H5B 1.0026 . ? O5 H5C 1.0040 . ?