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#$Date: 2025-07-01 16:04:00 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1351 $
#$URL: svn://crystallography.net/testcod/cif/4/30/00/4300041.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_4300041
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 H12 B2 F8 Fe N24'
_chemical_formula_weight         721.93
_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                 90.061(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1446(4)
_cell_length_b                   20.2603(8)
_cell_length_c                   8.8515(4)
_cell_measurement_temperature    300(2)
_cell_volume                     1460.60(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      300(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17212
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0040(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0725P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                1593
_reflns_number_total             3364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202626c_si_002.cif
_cod_data_source_block           CCDC-855739
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4300041
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
Fe Fe 1.0000 1.0000 1.0000 0.0376(3) Uani 1 2 d S . .
F1 F 0.2278(4) 0.67377(18) 0.7591(4) 0.1282(13) Uani 1 1 d . . .
F2 F 0.2217(7) 0.7587(2) 0.9166(5) 0.189(2) Uani 1 1 d . . .
F3 F 0.3671(5) 0.6726(2) 0.9724(5) 0.1764(18) Uani 1 1 d . . .
F4 F 0.0952(6) 0.6703(3) 0.9736(6) 0.216(2) Uani 1 1 d . . .
B4 B 0.2296(9) 0.6941(4) 0.9034(9) 0.107(2) Uani 1 1 d . . .
N1 N 0.8570(4) 0.91870(12) 0.9045(4) 0.0496(8) Uani 1 1 d . . .
N2 N 0.6880(4) 0.91400(15) 0.9123(4) 0.0686(10) Uani 1 1 d . . .
N3 N 0.7910(5) 0.82140(15) 0.8310(4) 0.0626(9) Uani 1 1 d . . .
N4 N 0.8217(5) 0.75661(17) 0.7745(4) 0.0704(10) Uani 1 1 d . . .
N5 N 0.6920(5) 0.72924(18) 0.7761(4) 0.0708(10) Uani 1 1 d . . .
N6 N 0.7232(4) 0.66446(14) 0.7164(4) 0.0602(9) Uani 1 1 d . . .
N7 N 0.6490(4) 0.57345(13) 0.6143(3) 0.0502(8) Uani 1 1 d . . .
N8 N 0.8191(4) 0.57841(15) 0.6019(4) 0.0618(9) Uani 1 1 d . . .
N9 N 1.1625(3) 0.99635(14) 0.8042(3) 0.0447(6) Uani 1 1 d . . .
N10 N 1.0853(4) 0.99584(18) 0.6640(3) 0.0661(9) Uani 1 1 d . . .
N11 N 1.3490(3) 0.99880(15) 0.6310(3) 0.0502(7) Uani 1 1 d . . .
N12 N 1.5037(3) 1.00117(16) 0.5698(3) 0.0525(7) Uani 1 1 d . . .
C1 C 0.9134(6) 0.8631(2) 0.8543(5) 0.0669(12) Uani 1 1 d . . .
C2 C 0.6526(7) 0.8542(2) 0.8676(6) 0.0820(16) Uani 1 1 d . . .
C3 C 0.8583(6) 0.6343(2) 0.6627(5) 0.0647(12) Uani 1 1 d . . .
C4 C 0.5967(6) 0.6252(2) 0.6836(5) 0.0612(11) Uani 1 1 d . . .
C5 C 1.3195(4) 0.99851(18) 0.7815(4) 0.0469(8) Uani 1 1 d . . .
C6 C 1.1996(5) 0.9980(3) 0.5632(5) 0.0699(12) Uani 1 1 d . . .
H1 H 1.026(6) 0.852(2) 0.834(6) 0.12(2) Uiso 1 1 d . . .
H2 H 0.561(5) 0.8396(19) 0.850(4) 0.062(13) Uiso 1 1 d . . .
H3 H 0.969(5) 0.6468(18) 0.673(4) 0.069(12) Uiso 1 1 d . . .
H4 H 0.497(5) 0.632(2) 0.705(5) 0.081(15) Uiso 1 1 d . . .
H5 H 1.397(5) 0.9993(17) 0.855(4) 0.061(11) Uiso 1 1 d . . .
H6 H 1.182(6) 0.997(2) 0.467(6) 0.086(14) Uiso 1 1 d . . .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N7 Fe N7 180.000(1) 4_676 2_656 ?
N7 Fe N9 90.44(11) 4_676 . ?
N7 Fe N9 89.56(11) 2_656 . ?
N7 Fe N9 89.56(11) 4_676 3_777 ?
N7 Fe N9 90.44(11) 2_656 3_777 ?
N9 Fe N9 180.000(1) . 3_777 ?
N7 Fe N1 87.77(11) 4_676 . ?
N7 Fe N1 92.23(11) 2_656 . ?
N9 Fe N1 89.47(11) . . ?
N9 Fe N1 90.53(11) 3_777 . ?
N7 Fe N1 92.23(11) 4_676 3_777 ?
N7 Fe N1 87.77(11) 2_656 3_777 ?
N9 Fe N1 90.53(11) . 3_777 ?
N9 Fe N1 89.47(11) 3_777 3_777 ?
N1 Fe N1 180.000(1) . 3_777 ?
F2 B4 F1 112.9(7) . . ?
F2 B4 F3 108.8(7) . . ?
F1 B4 F3 109.9(5) . . ?
F2 B4 F4 106.1(6) . . ?
F1 B4 F4 108.7(7) . . ?
F3 B4 F4 110.5(8) . . ?
C1 N1 N2 108.1(3) . . ?
C1 N1 Fe 126.8(3) . . ?
N2 N1 Fe 124.3(2) . . ?
C2 N2 N1 105.6(4) . . ?
C1 N3 C2 106.1(4) . . ?
C1 N3 N4 120.7(4) . . ?
C2 N3 N4 133.2(4) . . ?
N5 N4 N3 105.6(4) . . ?
N4 N5 N6 105.3(4) . . ?
C4 N6 C3 106.5(3) . . ?
C4 N6 N5 119.2(4) . . ?
C3 N6 N5 133.6(4) . . ?
C4 N7 N8 108.0(3) . . ?
C4 N7 Fe 126.5(3) . 2_646 ?
N8 N7 Fe 124.6(2) . 2_646 ?
C3 N8 N7 106.0(3) . . ?
C5 N9 N10 107.9(3) . . ?
C5 N9 Fe 136.2(2) . . ?
N10 N9 Fe 115.78(19) . . ?
C6 N10 N9 106.9(3) . . ?
C5 N11 C6 106.0(3) . . ?
C5 N11 N12 123.5(3) . . ?
C6 N11 N12 130.4(3) . . ?
N12 N12 N11 110.4(3) 3_876 . ?
N1 C1 N3 109.9(4) . . ?
N2 C2 N3 110.2(4) . . ?
N8 C3 N6 110.1(4) . . ?
N7 C4 N6 109.5(4) . . ?
N9 C5 N11 109.2(3) . . ?
N10 C6 N11 110.0(3) . . ?
N1 C1 H1 127(3) . . ?
N3 C1 H1 123(3) . . ?
N2 C2 H2 127(3) . . ?
N3 C2 H2 123(3) . . ?
N8 C3 H3 121(2) . . ?
N6 C3 H3 129(2) . . ?
N7 C4 H4 124(3) . . ?
N6 C4 H4 127(3) . . ?
N9 C5 H5 125(2) . . ?
N11 C5 H5 126(2) . . ?
N10 C6 H6 124(3) . . ?
N11 C6 H6 126(3) . . ?
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
Fe N7 2.170(3) 4_676 ?
Fe N7 2.170(3) 2_656 ?
Fe N9 2.183(2) . ?
Fe N9 2.183(2) 3_777 ?
Fe N1 2.187(3) . ?
Fe N1 2.187(3) 3_777 ?
F1 B4 1.342(7) . ?
F2 B4 1.315(8) . ?
F3 B4 1.348(8) . ?
F4 B4 1.348(9) . ?
N1 C1 1.295(5) . ?
N1 N2 1.381(4) . ?
N2 C2 1.306(5) . ?
N3 C1 1.323(5) . ?
N3 C2 1.349(6) . ?
N3 N4 1.427(4) . ?
N4 N5 1.193(5) . ?
N5 N6 1.437(4) . ?
N6 C4 1.333(5) . ?
N6 C3 1.346(5) . ?
N7 C4 1.287(5) . ?
N7 N8 1.393(4) . ?
N7 Fe 2.170(3) 2_646 ?
N8 C3 1.293(5) . ?
N9 C5 1.296(4) . ?
N9 N10 1.391(4) . ?
N10 C6 1.291(5) . ?
N11 C5 1.354(4) . ?
N11 C6 1.356(5) . ?
N11 N12 1.373(4) . ?
N12 N12 1.237(5) 3_876 ?
C1 H1 0.96(5) . ?
C2 H2 0.82(4) . ?
C3 H3 0.94(4) . ?
C4 H4 0.85(4) . ?
C5 H5 0.91(4) . ?
C6 H6 0.86(5) . ?
