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#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://crystallography.net/testcod/cif/4/30/00/4300040.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(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                 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       '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  0.0944
_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/[σ²(Fo²)+(0.0921P)²+2.3767P] where P=(Fo²+2Fc²)/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_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 . ?
