#------------------------------------------------------------------------------
#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://crystallography.net/testcod/cif/4/30/00/4300043.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_4300043
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           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 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                 118.667(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2751(13)
_cell_length_b                   7.1940(7)
_cell_length_c                   12.0161(12)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1006.89(17)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4911
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.8248
_exptl_absorpt_correction_T_min  0.7531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0574P)²+1.3860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                1172
_reflns_number_total             1258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202626c_si_002.cif
_cod_data_source_block           CCDC-855741
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4300043
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.5000 0.0262(2) Uani 1 4 d S . .
S1 S -0.40276(9) 0.0000 0.17313(13) 0.0796(4) Uani 1 2 d S . .
N1 N -0.0349(2) 0.0000 0.6617(2) 0.0328(6) Uani 1 2 d S . .
N2 N -0.1450(2) 0.0000 0.6478(3) 0.0531(9) Uani 1 2 d S . .
N3 N -0.0206(2) 0.0000 0.8491(2) 0.0371(6) Uani 1 2 d S . .
N4 N 0.0349(2) 0.0000 0.9803(2) 0.0425(7) Uani 1 2 d S . .
N5 N -0.1778(2) 0.0000 0.3709(3) 0.0380(6) Uani 1 2 d S . .
N6 N 0.0000 0.3065(3) 0.5000 0.0306(5) Uani 1 2 d S . .
C1 C 0.0370(3) 0.0000 0.7823(3) 0.0388(7) Uani 1 2 d S . .
H1A H 0.1165 0.0000 0.8174 0.047 Uiso 1 2 calc SR . .
C2 C -0.1331(3) 0.0000 0.7615(3) 0.0570(11) Uani 1 2 d S . .
H2A H -0.1935 0.0000 0.7801 0.068 Uiso 1 2 calc SR . .
C3 C -0.2709(3) 0.0000 0.2901(3) 0.0400(7) Uani 1 2 d S . .
C4 C 0.08270(18) 0.4042(3) 0.4933(2) 0.0345(5) Uani 1 1 d . . .
H4A H 0.1417 0.3412 0.4886 0.041 Uiso 1 1 calc R . .
O1 O -0.3442(5) 0.0000 0.8264(7) 0.173(3) Uani 1 2 d S . .
H1B H -0.3435 -0.1017 0.8756 0.260 Uiso 1 1 d R . .
O2 O -0.2223(6) -0.2929(14) 0.9757(8) 0.142(3) Uani 0.50 1 d P . .
H2B H -0.2156 -0.3659 0.9224 0.213 Uiso 0.50 1 d PR . .
H2C H -0.1731 -0.1858 0.9937 0.213 Uiso 0.50 1 d PR . .
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 0.0288(3) 0.0260(3) 0.0228(3) 0.000 0.0115(2) 0.000
S1 0.0393(5) 0.0951(10) 0.0674(8) 0.000 -0.0042(5) 0.000
N1 0.0376(13) 0.0384(13) 0.0255(11) 0.000 0.0175(10) 0.000
N2 0.0360(14) 0.096(3) 0.0292(13) 0.000 0.0171(12) 0.000
N3 0.0376(14) 0.0520(16) 0.0236(12) 0.000 0.0162(11) 0.000
N4 0.0437(14) 0.0610(18) 0.0260(12) 0.000 0.0193(11) 0.000
N5 0.0343(13) 0.0435(15) 0.0323(12) 0.000 0.0128(11) 0.000
N6 0.0331(12) 0.0257(11) 0.0329(12) 0.000 0.0157(10) 0.000
C1 0.0327(15) 0.057(2) 0.0278(14) 0.000 0.0150(12) 0.000
C2 0.0397(18) 0.104(4) 0.0339(17) 0.000 0.0224(15) 0.000
C3 0.0377(16) 0.0415(17) 0.0384(16) 0.000 0.0163(14) 0.000
C4 0.0339(10) 0.0287(11) 0.0448(11) -0.0001(9) 0.0219(9) 0.0015(8)
O1 0.112(4) 0.278(10) 0.156(5) 0.000 0.085(4) 0.000
O2 0.125(6) 0.174(8) 0.137(7) -0.060(6) 0.070(5) -0.058(6)
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 180.00(11) 5_556 . ?
N5 Fe1 N1 90.81(10) 5_556 5_556 ?
N5 Fe1 N1 89.19(10) . 5_556 ?
N5 Fe1 N1 89.19(10) 5_556 . ?
N5 Fe1 N1 90.81(10) . . ?
N1 Fe1 N1 180.000(1) 5_556 . ?
N5 Fe1 N6 90.0 5_556 5_556 ?
N5 Fe1 N6 90.000(1) . 5_556 ?
N1 Fe1 N6 90.0 5_556 5_556 ?
N1 Fe1 N6 90.0 . 5_556 ?
N5 Fe1 N6 90.000(1) 5_556 . ?
N5 Fe1 N6 90.0 . . ?
N1 Fe1 N6 90.0 5_556 . ?
N1 Fe1 N6 90.0 . . ?
N6 Fe1 N6 180.0 5_556 . ?
C1 N1 N2 107.6(2) . . ?
C1 N1 Fe1 129.2(2) . . ?
N2 N1 Fe1 123.25(18) . . ?
C2 N2 N1 106.5(3) . . ?
C1 N3 C2 105.5(3) . . ?
C1 N3 N4 122.3(3) . . ?
C2 N3 N4 132.2(3) . . ?
N4 N4 N3 110.7(3) 5_557 . ?
C3 N5 Fe1 172.3(3) . . ?
C4 N6 C4 116.7(2) . 2_556 ?
C4 N6 Fe1 121.67(12) . . ?
C4 N6 Fe1 121.67(12) 2_556 . ?
N1 C1 N3 110.0(3) . . ?
N2 C2 N3 110.5(3) . . ?
N5 C3 S1 178.9(3) . . ?
N6 C4 C4 121.67(12) . 6_565 ?
N1 C1 H1A 125.0 . . ?
N3 C1 H1A 125.0 . . ?
N2 C2 H2A 124.8 . . ?
N3 C2 H2A 124.8 . . ?
N6 C4 H4A 119.2 . . ?
C4 C4 H4A 119.2 6_565 . ?
O2 O2 H2B 154.9 7_447 . ?
O2 O2 H2C 89.4 7_447 . ?
H2B O2 H2C 110.6 . . ?
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 2.113(3) 5_556 ?
Fe1 N5 2.113(3) . ?
Fe1 N1 2.204(2) 5_556 ?
Fe1 N1 2.204(2) . ?
Fe1 N6 2.205(2) 5_556 ?
Fe1 N6 2.205(2) . ?
S1 C3 1.637(3) . ?
N1 C1 1.297(4) . ?
N1 N2 1.389(4) . ?
N2 C2 1.298(4) . ?
N3 C1 1.348(4) . ?
N3 C2 1.353(4) . ?
N3 N4 1.384(3) . ?
N4 N4 1.225(5) 5_557 ?
N5 C3 1.148(4) . ?
N6 C4 1.338(2) . ?
N6 C4 1.338(2) 2_556 ?
C4 C4 1.379(4) 6_565 ?
O2 O2 1.293(14) 7_447 ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C4 H4A 0.9300 . ?
O1 H1B 0.9376 . ?
O2 H2B 0.8654 . ?
O2 H2C 0.9651 . ?
