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#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://crystallography.net/testcod/cif/4/30/00/4300045.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_4300045
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            '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                 92.816(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0306(3)
_cell_length_b                   19.4080(4)
_cell_length_c                   8.8862(4)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    264(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1383.31(9)
_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      264(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  0.1397
_diffrn_reflns_av_sigmaI/netI    0.1869
_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            7483
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            orange-ed
_exptl_crystal_density_diffrn    1.880
_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          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.2012
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0401P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                969
_reflns_number_total             2436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202626c_si_002.cif
_cod_data_source_block           CCDC-870070
_cod_original_cell_volume        1383.30(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4300045
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 0.0335(4) Uani 1 2 d S . .
Cl1 Cl -0.7801(3) 0.30841(15) 0.0873(3) 0.0887(8) Uani 1 1 d . . .
O1 O -0.7758(5) 0.3247(3) 0.2414(6) 0.093(2) Uani 1 1 d . . .
O2 O -0.6417(8) 0.3360(3) 0.0206(7) 0.144(3) Uani 1 1 d . . .
O3 O -0.9260(10) 0.3345(5) 0.0218(8) 0.193(4) Uani 1 1 d . . .
O4 O -0.7833(10) 0.2399(4) 0.0660(7) 0.169(4) Uani 1 1 d . . .
N1 N -0.1362(7) 0.0801(3) 0.0840(6) 0.0361(14) Uani 1 1 d . . .
N2 N -0.3056(7) 0.0863(3) 0.0698(6) 0.0553(17) Uani 1 1 d . . .
N3 N -0.2038(8) 0.1783(3) 0.1633(6) 0.0500(16) Uani 1 1 d . . .
N4 N -0.1746(7) 0.2434(4) 0.2239(6) 0.0539(17) Uani 1 1 d . . .
N5 N -0.3067(7) 0.2745(4) 0.2224(6) 0.0577(18) Uani 1 1 d . . .
N6 N -0.2795(8) 0.3381(3) 0.2823(6) 0.0438(15) Uani 1 1 d . . .
N8 N -0.3540(7) 0.4291(3) 0.3956(6) 0.0389(15) Uani 1 1 d . . .
N7 N -0.1835(7) 0.4252(3) 0.4045(6) 0.0480(16) Uani 1 1 d . . .
N9 N 0.1545(5) 0.0036(3) 0.1928(5) 0.0345(11) Uani 1 1 d . . .
N10 N 0.0792(5) 0.0049(3) 0.3317(5) 0.0443(13) Uani 1 1 d . . .
N11 N 0.3444(5) 0.0025(3) 0.3682(5) 0.0356(12) Uani 1 1 d . . .
N12 N 0.5018(5) -0.0001(3) 0.4306(4) 0.0384(12) Uani 1 1 d . . .
C1 C -0.0783(9) 0.1346(4) 0.1412(8) 0.052(2) Uani 1 1 d . . .
H1A H 0.0339 0.1433 0.1646 0.062 Uiso 1 1 calc R . .
C2 C -0.3432(9) 0.1450(5) 0.1187(8) 0.063(2) Uani 1 1 d . . .
H2A H -0.4509 0.1623 0.1230 0.076 Uiso 1 1 calc R . .
C4 C -0.4073(8) 0.3768(4) 0.3214(7) 0.0439(19) Uani 1 1 d . . .
H4A H -0.5190 0.3672 0.2979 0.053 Uiso 1 1 calc R . .
C3 C -0.1435(9) 0.3698(4) 0.3397(8) 0.052(2) Uani 1 1 d . . .
H3A H -0.0351 0.3537 0.3331 0.063 Uiso 1 1 calc R . .
C5 C 0.3138(7) 0.0027(4) 0.2194(6) 0.0353(14) Uani 1 1 d . . .
H5A H 0.3937 0.0022 0.1471 0.042 Uiso 1 1 calc R . .
C6 C 0.1948(7) 0.0037(4) 0.4337(7) 0.0488(17) Uani 1 1 d . . .
H6A H 0.1799 0.0036 0.5369 0.059 Uiso 1 1 calc R . .
O5 O -0.7120(12) 0.1664(5) 0.3479(14) 0.318(7) Uani 1 1 d . . .
H5B H -0.7511 0.1910 0.2660 0.477 Uiso 1 1 d R . .
H5C H -0.6089 0.1790 0.3989 0.477 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'
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
N8 Fe1 N8 180.0(4) 2_445 4_665 ?
N8 Fe1 N1 89.05(18) 2_445 3 ?
N8 Fe1 N1 90.95(18) 4_665 3 ?
N8 Fe1 N1 90.95(18) 2_445 . ?
N8 Fe1 N1 89.05(18) 4_665 . ?
N1 Fe1 N1 180.0(4) 3 . ?
N8 Fe1 N9 91.08(19) 2_445 3 ?
N8 Fe1 N9 88.92(19) 4_665 3 ?
N1 Fe1 N9 89.0(2) 3 3 ?
N1 Fe1 N9 91.0(2) . 3 ?
N8 Fe1 N9 88.92(19) 2_445 . ?
N8 Fe1 N9 91.08(19) 4_665 . ?
N1 Fe1 N9 91.0(2) 3 . ?
N1 Fe1 N9 89.0(2) . . ?
N9 Fe1 N9 180.00(15) 3 . ?
O4 Cl1 O3 107.1(5) . . ?
O4 Cl1 O2 109.3(5) . . ?
O3 Cl1 O2 111.0(5) . . ?
O4 Cl1 O1 111.1(5) . . ?
O3 Cl1 O1 108.0(4) . . ?
O2 Cl1 O1 110.3(4) . . ?
C1 N1 N2 108.1(6) . . ?
C1 N1 Fe1 126.2(5) . . ?
N2 N1 Fe1 125.3(5) . . ?
C2 N2 N1 107.6(6) . . ?
C2 N3 C1 106.0(6) . . ?
C2 N3 N4 132.7(7) . . ?
C1 N3 N4 121.3(7) . . ?
N5 N4 N3 108.4(6) . . ?
N4 N5 N6 108.8(6) . . ?
C4 N6 C3 105.5(6) . . ?
C4 N6 N5 120.3(7) . . ?
C3 N6 N5 133.0(7) . . ?
C4 N8 N7 107.2(5) . . ?
C4 N8 Fe1 125.6(5) . 2_455 ?
N7 N8 Fe1 126.9(5) . 2_455 ?
C3 N7 N8 107.2(6) . . ?
C5 N9 N10 107.8(4) . . ?
C5 N9 Fe1 134.6(4) . . ?
N10 N9 Fe1 117.6(3) . . ?
C6 N10 N9 107.4(4) . . ?
C5 N11 N12 121.9(4) . . ?
C5 N11 C6 107.5(5) . . ?
N12 N11 C6 130.5(5) . . ?
N12 N12 N11 109.9(5) 3_656 . ?
N1 C1 N3 109.1(6) . . ?
N2 C2 N3 109.1(7) . . ?
N8 C4 N6 109.9(6) . . ?
N7 C3 N6 110.1(6) . . ?
N9 C5 N11 108.4(5) . . ?
N10 C6 N11 109.0(5) . . ?
N1 C1 H1A 125.8 . . ?
N3 C1 H1A 125.6 . . ?
N2 C2 H2A 125.3 . . ?
N3 C2 H2A 125.9 . . ?
N8 C4 H4A 125.1 . . ?
N6 C4 H4A 125.0 . . ?
N7 C3 H3A 124.1 . . ?
N6 C3 H3A 124.3 . . ?
N9 C5 H5A 126.3 . . ?
N11 C5 H5A 125.5 . . ?
N10 C6 H6A 124.7 . . ?
N11 C6 H6A 124.6 . . ?
H5B O5 H5C 120.1 . . ?
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 N8 2.058(5) 2_445 ?
Fe1 N8 2.058(5) 4_665 ?
Fe1 N1 2.062(5) 3 ?
Fe1 N1 2.062(5) . ?
Fe1 N9 2.066(4) 3 ?
Fe1 N9 2.066(4) . ?
Cl1 O4 1.343(6) . ?
Cl1 O3 1.379(7) . ?
Cl1 O2 1.392(5) . ?
Cl1 O1 1.404(5) . ?
N1 C1 1.253(7) . ?
N1 N2 1.365(6) . ?
N2 C2 1.260(7) . ?
N3 C2 1.337(7) . ?
N3 C1 1.339(7) . ?
N3 N4 1.389(7) . ?
N4 N5 1.220(6) . ?
N5 N6 1.358(7) . ?
N6 C4 1.332(7) . ?
N6 C3 1.333(7) . ?
N8 C4 1.272(7) . ?
N8 N7 1.369(6) . ?
N8 Fe1 2.058(5) 2_455 ?
N7 C3 1.268(7) . ?
N9 C5 1.290(6) . ?
N9 N10 1.401(5) . ?
N10 C6 1.265(6) . ?
N11 C5 1.332(6) . ?
N11 N12 1.357(5) . ?
N11 C6 1.361(6) . ?
N12 N12 1.235(7) 3_656 ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C4 H4A 0.9300 . ?
C3 H3A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
O5 H5B 0.9130 . ?
O5 H5C 0.9557 . ?
