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#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://crystallography.net/testcod/cif/4/30/00/4300044.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_4300044
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(μ-atrz)3]X2·2H2O (X = ClO4¯, BF4¯) and
 [Fe(μ-atrz)(μ-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            'C10 H16 Fe N12 O4 S2'
_chemical_formula_weight         488.32
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.562(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.4148(7)
_cell_length_b                   6.7777(3)
_cell_length_c                   13.2311(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1822.11(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8377
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8089
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2086
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0526
_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/[σ²(Fo²)+(0.0825P)²+4.1294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                1408
_reflns_number_total             2086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202626c_si_002.cif
_cod_data_source_block           CCDC-855742
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4300044
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'
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 0.24008(10) 0.2500 0.0130(2) Uani 1 2 d S . .
S1 S -0.15969(5) 0.25433(15) 0.48865(8) 0.0320(3) Uani 1 1 d U . .
N1 N 0.07500(13) 0.2401(4) 0.3581(2) 0.0156(6) Uani 1 1 d . . .
N2 N 0.06738(14) 0.2407(4) 0.4628(2) 0.0230(7) Uani 1 1 d . . .
N3 N 0.17180(14) 0.2440(4) 0.4418(2) 0.0190(6) Uani 1 1 d . . .
N4 N 0.24025(14) 0.2496(4) 0.4544(2) 0.0206(6) Uani 1 1 d . . .
N5 N -0.06309(14) 0.2410(4) 0.3517(2) 0.0169(6) Uani 1 1 d . . .
N6 N 0.0000 -0.0526(6) 0.2500 0.0148(8) Uani 1 2 d S . .
N7 N 0.0000 -0.4665(6) 0.2500 0.0156(8) Uani 1 2 d S . .
C1 C 0.13840(17) 0.2415(5) 0.3487(3) 0.0179(7) Uani 1 1 d . . .
H1 H 0.1577 0.2409 0.2862 0.022 Uiso 1 1 calc R . .
C2 C 0.12597(18) 0.2439(6) 0.5101(3) 0.0264(8) Uani 1 1 d . . .
H2 H 0.1356 0.2458 0.5818 0.032 Uiso 1 1 calc R . .
C3 C 0.00325(16) -0.1582(5) 0.3368(3) 0.0170(7) Uani 1 1 d . . .
H3 H 0.0056 -0.0902 0.3998 0.020 Uiso 1 1 calc R . .
C4 C 0.00332(16) -0.3614(5) 0.3370(3) 0.0169(7) Uani 1 1 d . . .
H4 H 0.0058 -0.4294 0.4001 0.020 Uiso 1 1 calc R . .
C5 C -0.10229(17) 0.2467(5) 0.4097(3) 0.0173(7) Uani 1 1 d U . .
O1 O 0.1631(3) -0.2773(9) 0.2555(4) 0.115(2) Uani 1 1 d . . .
H1A H 0.1907 -0.3742 0.2415 0.173 Uiso 1 1 d R . .
H1B H 0.1191 -0.3274 0.2544 0.173 Uiso 1 1 d R . .
O2 O 0.2578(3) -0.0593(9) 0.2856(3) 0.120(2) Uani 1 1 d . . .
H2A H 0.2248 -0.1354 0.2745 0.181 Uiso 1 1 d R . .
H2B H 0.2802 -0.1084 0.3403 0.181 Uiso 1 1 d R . .
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'
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'
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 179.64(16) . 2 ?
N5 Fe1 N6 90.18(8) . . ?
N5 Fe1 N6 90.18(8) 2 . ?
N5 Fe1 N7 89.82(8) . 1_565 ?
N5 Fe1 N7 89.82(8) 2 1_565 ?
N6 Fe1 N7 180.000(1) . 1_565 ?
N5 Fe1 N1 88.98(11) . 2 ?
N5 Fe1 N1 91.02(11) 2 2 ?
N6 Fe1 N1 90.00(8) . 2 ?
N7 Fe1 N1 90.00(8) 1_565 2 ?
N5 Fe1 N1 91.02(11) . . ?
N5 Fe1 N1 88.98(11) 2 . ?
N6 Fe1 N1 90.00(8) . . ?
N7 Fe1 N1 90.00(8) 1_565 . ?
N1 Fe1 N1 179.99(15) 2 . ?
C1 N1 N2 107.3(3) . . ?
C1 N1 Fe1 129.0(2) . . ?
N2 N1 Fe1 123.8(2) . . ?
C2 N2 N1 106.9(3) . . ?
C1 N3 C2 106.7(3) . . ?
C1 N3 N4 121.5(3) . . ?
C2 N3 N4 131.8(3) . . ?
N4 N4 N3 110.0(4) 7_556 . ?
C5 N5 Fe1 177.2(3) . . ?
C3 N6 C3 115.9(4) 2 . ?
C3 N6 Fe1 122.0(2) 2 . ?
C3 N6 Fe1 122.0(2) . . ?
C4 N7 C4 116.3(4) . 2 ?
C4 N7 Fe1 121.8(2) . 1_545 ?
C4 N7 Fe1 121.8(2) 2 1_545 ?
N1 C1 N3 109.3(3) . . ?
N2 C2 N3 109.9(3) . . ?
N6 C3 C4 122.1(3) . . ?
N7 C4 C3 121.7(3) . . ?
N5 C5 S1 178.1(3) . . ?
N1 C1 H1 125.3 . . ?
N3 C1 H1 125.3 . . ?
N2 C2 H2 125.1 . . ?
N3 C2 H2 125.1 . . ?
N6 C3 H3 119.0 . . ?
C4 C3 H3 118.9 . . ?
N7 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
H1A O1 H1B 110.1 . . ?
H2A O2 H2B 104.6 . . ?
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 1.951(3) . ?
Fe1 N5 1.951(3) 2 ?
Fe1 N6 1.984(4) . ?
Fe1 N7 1.989(4) 1_565 ?
Fe1 N1 1.991(3) 2 ?
Fe1 N1 1.991(3) . ?
S1 C5 1.645(3) . ?
N1 C1 1.312(4) . ?
N1 N2 1.409(4) . ?
N2 C2 1.296(5) . ?
N3 C1 1.349(5) . ?
N3 C2 1.363(5) . ?
N3 N4 1.392(4) . ?
N4 N4 1.234(6) 7_556 ?
N5 C5 1.162(5) . ?
N6 C3 1.350(4) 2 ?
N6 C3 1.350(4) . ?
N7 C4 1.350(4) . ?
N7 C4 1.350(4) 2 ?
N7 Fe1 1.989(4) 1_545 ?
C3 C4 1.377(5) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
O1 H1A 0.8952 . ?
O1 H1B 0.9593 . ?
O2 H2A 0.8501 . ?
O2 H2B 0.8826 . ?
