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#$Date: 2024-05-05 05:47:28 +0300 (Sun, 05 May 2024) $
#$Revision: 291621 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/54/7715497.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_7715497
loop_
_publ_author_name
'Tołoczko, Aleksandra'
'Kaźmierczak, Marcin'
'Książek, Maria'
'Weselski, Marek'
'Siczek, Miłosz'
'Kusz, Joachim'
'Bronisz, Robert'
_publ_section_title
;
 Expanding the dimensionality of bis(tetrazolyl)alkane-based Fe(II)
 coordination polymers by the application of dinitrile coligands.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7163
_journal_page_last               7174
_journal_paper_doi               10.1039/d4dt00462k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
;
C14 H20 Fe N18, 2(B F4)
;
_chemical_formula_sum            'C14 H20 B2 F8 Fe N18'
_chemical_formula_weight         669.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.886(6)
_cell_angle_beta                 91.310(5)
_cell_angle_gamma                111.316(7)
_cell_formula_units_Z            1
_cell_length_a                   8.0729(6)
_cell_length_b                   8.7297(7)
_cell_length_c                   10.3033(6)
_cell_measurement_reflns_used    2529
_cell_measurement_temperature    250(1)
_cell_measurement_theta_max      35.6040
_cell_measurement_theta_min      3.4000
_cell_volume                     676.25(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      250(1)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5635
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.181
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0506P)²+0.0988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2448
_reflns_number_total             2760
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00462k2.cif
_cod_data_source_block           1_2_rb20_104_1a_3_250k
_cod_depositor_comments
'Adding full bibliography for 7715495--7715502.cif.'
_cod_database_code               7715497
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.974
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.000000 0.500000 0.02463(13) Uani 1 2 d S . P . .
N1 N 0.1826(2) -0.5104(2) 0.41031(17) 0.0397(4) Uani 1 1 d . . . . .
N2 N 0.2295(2) -0.43658(19) 0.29687(15) 0.0309(4) Uani 1 1 d . . . . .
N3 N 0.3235(2) -0.27989(19) 0.30432(15) 0.0307(4) Uani 1 1 d . . . . .
N4 N 0.3411(2) -0.24465(19) 0.42989(15) 0.0304(3) Uani 1 1 d . . . . .
N5 N 0.1188(2) 0.1181(2) 0.25103(19) 0.0436(4) Uani 1 1 d . . . . .
N6 N 0.2723(2) 0.24300(19) 0.24538(15) 0.0301(3) Uani 1 1 d . . . . .
N7 N 0.3956(2) 0.2339(2) 0.32562(15) 0.0320(4) Uani 1 1 d . . . . .
N8 N 0.3215(2) 0.09379(19) 0.38907(15) 0.0317(4) Uani 1 1 d . . . . .
C1 C 0.2546(3) -0.3861(2) 0.49186(19) 0.0372(5) Uani 1 1 d . . . . .
H1 H 0.246360 -0.395417 0.582599 0.045 Uiso 1 1 calc R U . . .
C2 C 0.1547(3) 0.0271(3) 0.3422(2) 0.0416(5) Uani 1 1 d . . . . .
H2 H 0.072159 -0.073428 0.370756 0.050 Uiso 1 1 calc R U . . .
C3 C 0.1858(3) -0.5262(2) 0.17385(18) 0.0348(4) Uani 1 1 d . . . . .
H3A H 0.199452 -0.448428 0.102531 0.042 Uiso 1 1 calc R U . . .
H3B H 0.061518 -0.601728 0.173556 0.042 Uiso 1 1 calc R U . . .
C4 C 0.3054(3) -0.6224(3) 0.15314(18) 0.0355(4) Uani 1 1 d . . . . .
H4A H 0.286338 -0.667289 0.064609 0.043 Uiso 1 1 calc R U . . .
H4B H 0.429839 -0.548094 0.162212 0.043 Uiso 1 1 calc R U . . .
N9 N 0.6558(2) 0.0390(2) 0.32603(15) 0.0329(4) Uani 1 1 d . . . . .
C5 C 0.6935(2) 0.0456(2) 0.22024(18) 0.0298(4) Uani 1 1 d . . . . .
C6 C 0.7358(3) 0.0551(3) 0.08293(18) 0.0373(5) Uani 1 1 d . . . . .
H6A H 0.826778 0.007268 0.069635 0.045 Uiso 0.846(11) 1 calc R U P A 1
H6B H 0.785717 0.170904 0.057614 0.045 Uiso 0.846(11) 1 calc R U P A 1
H6C H 0.757598 -0.043839 0.057234 0.045 Uiso 0.154(11) 1 calc R U P A 2
H6D H 0.844586 0.150460 0.068614 0.045 Uiso 0.154(11) 1 calc R U P A 2
C7 C 0.5734(3) -0.0347(5) -0.0048(2) 0.0335(9) Uani 0.846(11) 1 d . . P A 1
H7A H 0.611284 -0.027444 -0.095085 0.040 Uiso 0.846(11) 1 calc R U P A 1
H7B H 0.525923 -0.151244 0.018652 0.040 Uiso 0.846(11) 1 calc R U P A 1
C7A C 0.583(2) 0.070(3) -0.0018(13) 0.042(6) Uani 0.154(11) 1 d . . P A 2
H7D H 0.559715 0.167896 0.026680 0.051 Uiso 0.154(11) 1 calc R U P A 2
H7C H 0.621063 0.088413 -0.091877 0.051 Uiso 0.154(11) 1 calc R U P A 2
B1 B 0.8316(3) 0.6305(3) 0.1832(2) 0.0384(5) Uani 1 1 d . . . . .
F1 F 0.6923(2) 0.6848(2) 0.16750(16) 0.0643(4) Uani 1 1 d . . . . .
F2 F 0.9000(2) 0.6566(2) 0.30753(14) 0.0672(4) Uani 1 1 d . . . . .
F3 F 0.9641(2) 0.7116(2) 0.09798(15) 0.0688(5) Uani 1 1 d . . . . .
F4 F 0.7695(2) 0.46445(18) 0.15515(17) 0.0672(4) Uani 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'
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'
N N 0.0061 0.0033 '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
N9 Fe1 N4 90.79(6) 2_656 . ?
N9 Fe1 N9 180.0 2_656 . ?
N4 Fe1 N9 89.20(6) . . ?
N9 Fe1 N4 89.21(6) 2_656 2_656 ?
N4 Fe1 N4 180.00(8) . 2_656 ?
N9 Fe1 N4 90.80(6) . 2_656 ?
N9 Fe1 N8 86.53(6) 2_656 2_656 ?
N4 Fe1 N8 91.62(6) . 2_656 ?
N9 Fe1 N8 93.47(6) . 2_656 ?
N4 Fe1 N8 88.38(6) 2_656 2_656 ?
N9 Fe1 N8 93.47(6) 2_656 . ?
N4 Fe1 N8 88.38(6) . . ?
N9 Fe1 N8 86.53(6) . . ?
N4 Fe1 N8 91.62(6) 2_656 . ?
N8 Fe1 N8 180.0 2_656 . ?
C1 N1 N2 101.23(16) . . ?
N3 N2 N1 114.95(16) . . ?
N3 N2 C3 122.67(16) . . ?
N1 N2 C3 122.33(16) . . ?
N2 N3 N4 105.25(14) . . ?
N3 N4 C1 106.46(15) . . ?
N3 N4 Fe1 121.20(12) . . ?
C1 N4 Fe1 132.22(13) . . ?
C2 N5 N6 101.28(17) . . ?
N7 N6 N5 114.68(15) . . ?
N7 N6 C4 122.08(16) . 1_565 ?
N5 N6 C4 123.18(16) . 1_565 ?
N6 N7 N8 105.46(15) . . ?
N7 N8 C2 106.04(16) . . ?
N7 N8 Fe1 117.31(12) . . ?
C2 N8 Fe1 134.53(14) . . ?
N1 C1 N4 112.10(18) . . ?
N1 C1 H1 124.0 . . ?
N4 C1 H1 123.9 . . ?
N5 C2 N8 112.53(19) . . ?
N5 C2 H2 123.7 . . ?
N8 C2 H2 123.7 . . ?
N2 C3 C4 110.79(16) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N6 C4 C3 112.18(16) 1_545 . ?
N6 C4 H4A 109.2 1_545 . ?
C3 C4 H4A 109.2 . . ?
N6 C4 H4B 109.2 1_545 . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C5 N9 Fe1 161.76(15) . . ?
N9 C5 C6 177.8(2) . . ?
C5 C6 C7 112.93(17) . . ?
C5 C6 C7A 111.1(6) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C5 C6 H6C 109.4 . . ?
C7A C6 H6C 109.4 . . ?
C5 C6 H6D 109.4 . . ?
C7A C6 H6D 109.4 . . ?
H6C C6 H6D 108.0 . . ?
C7 C7 C6 113.2(4) 2_655 . ?
C7 C7 H7A 108.9 2_655 . ?
C6 C7 H7A 108.9 . . ?
C7 C7 H7B 108.9 2_655 . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
C7A C7A C6 115(2) 2_655 . ?
C7A C7A H7D 108.6 2_655 . ?
C6 C7A H7D 108.6 . . ?
C7A C7A H7C 108.6 2_655 . ?
C6 C7A H7C 108.6 . . ?
H7D C7A H7C 107.5 . . ?
F2 B1 F1 111.4(2) . . ?
F2 B1 F4 109.50(19) . . ?
F1 B1 F4 108.2(2) . . ?
F2 B1 F3 109.2(2) . . ?
F1 B1 F3 109.67(19) . . ?
F4 B1 F3 108.9(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 N9 2.1680(15) 2_656 ?
Fe1 N4 2.1680(15) . ?
Fe1 N9 2.1681(15) . ?
Fe1 N4 2.1681(15) 2_656 ?
Fe1 N8 2.1983(16) 2_656 ?
Fe1 N8 2.1983(16) . ?
N1 C1 1.320(3) . ?
N1 N2 1.328(2) . ?
N2 N3 1.302(2) . ?
N2 C3 1.458(2) . ?
N3 N4 1.323(2) . ?
N4 C1 1.346(2) . ?
N5 C2 1.323(3) . ?
N5 N6 1.323(2) . ?
N6 N7 1.303(2) . ?
N6 C4 1.461(2) 1_565 ?
N7 N8 1.328(2) . ?
N8 C2 1.337(3) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 C4 1.511(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
N9 C5 1.134(2) . ?
C5 C6 1.458(2) . ?
C6 C7 1.533(3) . ?
C6 C7A 1.543(17) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6D 0.9800 . ?
C7 C7 1.520(6) 2_655 ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7A C7A 1.45(4) 2_655 ?
C7A H7D 0.9800 . ?
C7A H7C 0.9800 . ?
B1 F2 1.369(3) . ?
B1 F1 1.376(3) . ?
B1 F4 1.380(3) . ?
B1 F3 1.381(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.3(2) . . . . ?
C1 N1 N2 C3 177.60(18) . . . . ?
N1 N2 N3 N4 -0.3(2) . . . . ?
C3 N2 N3 N4 -177.56(16) . . . . ?
N2 N3 N4 C1 0.1(2) . . . . ?
N2 N3 N4 Fe1 176.63(11) . . . . ?
C2 N5 N6 N7 -0.3(2) . . . . ?
C2 N5 N6 C4 177.18(18) . . . 1_565 ?
N5 N6 N7 N8 0.4(2) . . . . ?
C4 N6 N7 N8 -177.08(16) 1_565 . . . ?
N6 N7 N8 C2 -0.3(2) . . . . ?
N6 N7 N8 Fe1 165.52(11) . . . . ?
N2 N1 C1 N4 -0.2(2) . . . . ?
N3 N4 C1 N1 0.1(2) . . . . ?
Fe1 N4 C1 N1 -175.92(14) . . . . ?
N6 N5 C2 N8 0.0(2) . . . . ?
N7 N8 C2 N5 0.2(2) . . . . ?
Fe1 N8 C2 N5 -162.07(15) . . . . ?
N3 N2 C3 C4 101.3(2) . . . . ?
N1 N2 C3 C4 -75.8(2) . . . . ?
N2 C3 C4 N6 67.6(2) . . . 1_545 ?
C5 C6 C7 C7 60.8(4) . . . 2_655 ?
C5 C6 C7A C7A -64(2) . . . 2_655 ?
