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#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://localhost/testcod/cif/4/30/00/4300039.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_4300039
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                 90.8456(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1901(3)
_cell_length_b                   20.1869(7)
_cell_length_c                   8.9629(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1481.70(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      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12436
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.756
_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         0.704
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0843
_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^)+(0.1198P)^2^+6.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2613
_refine_ls_wR_factor_ref         0.2798
_reflns_number_gt                1843
_reflns_number_total             2614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202626c_si_002.cif
_cod_data_source_block           CCDC-855737
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4300039
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 0.0255(5) Uani 1 2 d S . .
Cl1 Cl -0.7706(4) 0.30658(16) 0.0921(3) 0.0808(9) Uani 1 1 d . . .
O1 O -0.7691(10) 0.3215(5) 0.2468(10) 0.100(3) Uani 1 1 d . . .
O2 O -0.6306(13) 0.3296(6) 0.0286(12) 0.135(4) Uani 1 1 d . . .
O3 O -0.9099(17) 0.3350(10) 0.0290(17) 0.198(7) Uani 1 1 d . . .
O4 O -0.779(2) 0.2388(5) 0.0709(13) 0.186(7) Uani 1 1 d . . .
N1 N -0.1402(8) 0.0823(3) 0.0919(7) 0.0399(15) Uani 1 1 d . . .
N2 N -0.3063(8) 0.0888(4) 0.0765(9) 0.0537(19) Uani 1 1 d . . .
N3 N -0.2027(9) 0.1799(3) 0.1666(8) 0.0502(18) Uani 1 1 d . . .
N4 N -0.1739(10) 0.2439(4) 0.2248(9) 0.0553(19) Uani 1 1 d . . .
N5 N -0.3020(9) 0.2730(4) 0.2243(8) 0.0518(18) Uani 1 1 d . . .
N6 N -0.2733(8) 0.3367(3) 0.2834(8) 0.0453(17) Uani 1 1 d . . .
N8 N -0.3478(7) 0.4278(3) 0.3879(7) 0.0382(15) Uani 1 1 d . . .
N7 N -0.1792(8) 0.4237(3) 0.4000(8) 0.0493(18) Uani 1 1 d . . .
N9 N 0.1596(7) 0.0034(3) 0.1972(6) 0.0343(14) Uani 1 1 d . . .
N10 N 0.0844(8) 0.0029(3) 0.3332(7) 0.0465(17) Uani 1 1 d . . .
N11 N 0.3468(7) 0.0012(3) 0.3699(7) 0.0374(15) Uani 1 1 d . . .
N12 N 0.5032(7) 0.0000(3) 0.4307(7) 0.0356(14) Uani 1 1 d . . .
C1 C -0.0808(11) 0.1364(4) 0.1491(10) 0.052(2) Uani 1 1 d . . .
H1A H 0.0283 0.1437 0.1739 0.063 Uiso 1 1 calc R . .
C2 C -0.3397(12) 0.1479(5) 0.1227(12) 0.066(3) Uani 1 1 d . . .
H2A H -0.4441 0.1659 0.1253 0.079 Uiso 1 1 calc R . .
C4 C -0.4014(10) 0.3752(4) 0.3206(9) 0.0445(19) Uani 1 1 d . . .
H4A H -0.5106 0.3655 0.3010 0.053 Uiso 1 1 calc R . .
C3 C -0.1393(10) 0.3685(4) 0.3373(10) 0.049(2) Uani 1 1 d . . .
H3A H -0.0329 0.3528 0.3300 0.059 Uiso 1 1 calc R . .
C5 C 0.3170(9) 0.0022(4) 0.2207(8) 0.0360(16) Uani 1 1 d . . .
H5A H 0.3959 0.0019 0.1471 0.043 Uiso 1 1 calc R . .
C6 C 0.1988(9) 0.0016(4) 0.4373(9) 0.0443(19) Uani 1 1 d . . .
H6A H 0.1816 0.0010 0.5396 0.053 Uiso 1 1 calc R . .
O5 O -0.716(3) 0.1650(9) 0.367(3) 0.253(10) Uani 1 1 d . . .
H5B H -0.7182 0.1956 0.2735 0.379 Uiso 1 1 d R . .
H5C H -0.6349 0.1319 0.3879 0.379 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 0.0294(8) 0.0192(7) 0.0276(8) 0.0009(5) -0.0045(5) -0.0006(5)
Cl1 0.0788(19) 0.086(2) 0.0771(19) -0.0278(15) -0.0010(15) -0.0195(16)
O1 0.073(5) 0.141(8) 0.088(6) -0.047(6) 0.011(4) -0.010(5)
O2 0.128(8) 0.181(11) 0.097(7) -0.028(7) 0.025(6) -0.069(8)
O3 0.136(11) 0.30(2) 0.157(12) 0.025(13) -0.060(9) 0.027(12)
O4 0.35(2) 0.085(7) 0.124(9) -0.050(7) 0.082(11) -0.077(10)
N1 0.039(4) 0.037(4) 0.043(4) -0.004(3) -0.004(3) 0.002(3)
N2 0.041(4) 0.048(4) 0.072(5) -0.026(4) -0.006(3) 0.008(3)
N3 0.061(5) 0.030(4) 0.059(5) -0.008(3) -0.006(4) 0.005(3)
N4 0.053(5) 0.047(4) 0.066(5) -0.015(4) 0.002(4) 0.003(3)
N5 0.053(4) 0.045(4) 0.057(5) -0.009(3) -0.007(3) 0.015(3)
N6 0.055(4) 0.028(3) 0.053(4) -0.012(3) -0.005(3) 0.005(3)
N8 0.041(4) 0.030(3) 0.043(4) -0.006(3) -0.004(3) 0.001(3)
N7 0.035(4) 0.042(4) 0.071(5) -0.015(3) -0.002(3) 0.004(3)
N9 0.030(3) 0.045(4) 0.029(3) 0.000(3) -0.002(2) 0.000(3)
N10 0.037(4) 0.069(5) 0.034(4) -0.001(3) -0.003(3) -0.002(3)
N11 0.029(3) 0.049(4) 0.034(3) 0.001(3) -0.007(3) 0.001(3)
N12 0.032(3) 0.048(4) 0.026(3) 0.000(3) -0.009(2) 0.000(3)
C1 0.051(5) 0.036(5) 0.070(6) -0.022(4) -0.003(4) -0.001(4)
C2 0.050(6) 0.061(6) 0.086(7) -0.023(5) -0.015(5) 0.021(5)
C4 0.042(5) 0.035(4) 0.056(5) -0.011(4) -0.007(4) 0.002(3)
C3 0.041(5) 0.039(5) 0.068(6) -0.012(4) -0.001(4) 0.014(4)
C5 0.031(4) 0.047(4) 0.030(4) 0.002(3) -0.005(3) 0.001(3)
C6 0.034(4) 0.068(6) 0.031(4) -0.001(4) -0.001(3) 0.001(4)
O5 0.30(2) 0.144(14) 0.31(3) -0.013(15) -0.10(2) -0.019(14)
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(2) 4_665 2_445 ?
N8 Fe1 N9 90.7(2) 4_665 . ?
N8 Fe1 N9 89.3(2) 2_445 . ?
N8 Fe1 N9 89.3(2) 4_665 3 ?
N8 Fe1 N9 90.7(2) 2_445 3 ?
N9 Fe1 N9 180.00(18) . 3 ?
N8 Fe1 N1 91.6(2) 4_665 3 ?
N8 Fe1 N1 88.4(2) 2_445 3 ?
N9 Fe1 N1 91.0(2) . 3 ?
N9 Fe1 N1 89.0(2) 3 3 ?
N8 Fe1 N1 88.4(2) 4_665 . ?
N8 Fe1 N1 91.6(2) 2_445 . ?
N9 Fe1 N1 89.0(2) . . ?
N9 Fe1 N1 91.0(2) 3 . ?
N1 Fe1 N1 180.0(4) 3 . ?
O2 Cl1 O4 108.6(9) . . ?
O2 Cl1 O3 112.2(10) . . ?
O4 Cl1 O3 108.2(11) . . ?
O2 Cl1 O1 109.8(6) . . ?
O4 Cl1 O1 110.1(7) . . ?
O3 Cl1 O1 107.8(8) . . ?
C1 N1 N2 108.9(7) . . ?
C1 N1 Fe1 126.3(5) . . ?
N2 N1 Fe1 124.1(5) . . ?
C2 N2 N1 105.7(7) . . ?
C1 N3 C2 105.6(7) . . ?
C1 N3 N4 121.5(7) . . ?
C2 N3 N4 132.8(7) . . ?
N5 N4 N3 107.8(7) . . ?
N4 N5 N6 107.7(7) . . ?
C4 N6 C3 105.5(6) . . ?
C4 N6 N5 119.4(7) . . ?
C3 N6 N5 134.2(7) . . ?
C4 N8 N7 108.5(6) . . ?
C4 N8 Fe1 124.9(5) . 2_455 ?
N7 N8 Fe1 125.6(5) . 2_455 ?
C3 N7 N8 106.1(6) . . ?
C5 N9 N10 108.2(6) . . ?
C5 N9 Fe1 135.1(5) . . ?
N10 N9 Fe1 116.6(4) . . ?
C6 N10 N9 107.8(6) . . ?
C5 N11 C6 106.8(6) . . ?
C5 N11 N12 122.7(6) . . ?
C6 N11 N12 130.5(6) . . ?
N12 N12 N11 109.9(7) 3_656 . ?
N1 C1 N3 108.8(7) . . ?
N2 C2 N3 110.9(8) . . ?
N8 C4 N6 109.1(7) . . ?
N7 C3 N6 110.8(7) . . ?
N9 C5 N11 108.8(7) . . ?
N10 C6 N11 108.4(7) . . ?
N1 C1 H1A 125.6 . . ?
N3 C1 H1A 125.6 . . ?
N2 C2 H2A 124.5 . . ?
N3 C2 H2A 124.5 . . ?
N8 C4 H4A 125.4 . . ?
N6 C4 H4A 125.4 . . ?
N7 C3 H3A 124.6 . . ?
N6 C3 H3A 124.6 . . ?
N9 C5 H5A 125.6 . . ?
N11 C5 H5A 125.6 . . ?
N10 C6 H6A 125.8 . . ?
N11 C6 H6A 125.8 . . ?
H5B O5 H5C 124.8 . . ?
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 2.173(6) 4_665 ?
Fe1 N8 2.173(6) 2_445 ?
Fe1 N9 2.184(6) . ?
Fe1 N9 2.184(6) 3 ?
Fe1 N1 2.187(6) 3 ?
Fe1 N1 2.187(6) . ?
Cl1 O2 1.369(10) . ?
Cl1 O4 1.382(10) . ?
Cl1 O3 1.389(13) . ?
Cl1 O1 1.419(9) . ?
N1 C1 1.297(10) . ?
N1 N2 1.372(9) . ?
N2 C2 1.294(11) . ?
N3 C1 1.341(11) . ?
N3 C2 1.348(12) . ?
N3 N4 1.412(9) . ?
N4 N5 1.202(10) . ?
N5 N6 1.408(9) . ?
N6 C4 1.352(10) . ?
N6 C3 1.354(11) . ?
N8 C4 1.296(9) . ?
N8 N7 1.386(9) . ?
N8 Fe1 2.173(6) 2_455 ?
N7 C3 1.292(10) . ?
N9 C5 1.303(10) . ?
N9 N10 1.373(9) . ?
N10 C6 1.313(11) . ?
N11 C5 1.356(10) . ?
N11 C6 1.363(10) . ?
N11 N12 1.385(9) . ?
N12 N12 1.245(12) 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 1.0436 . ?
O5 H5C 0.9590 . ?