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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/7/71/55/7715500.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_7715500
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
;
C22 H36 Fe N18, 2(B F4)
;
_chemical_formula_sum            'C22 H36 B2 F8 Fe N18'
_chemical_formula_weight         782.16
_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                109.557(18)
_cell_angle_beta                 99.300(16)
_cell_angle_gamma                112.580(17)
_cell_formula_units_Z            1
_cell_length_a                   8.7981(15)
_cell_length_b                   9.9945(19)
_cell_length_c                   11.413(2)
_cell_measurement_reflns_used    3685
_cell_measurement_temperature    80(1)
_cell_measurement_theta_max      35.7280
_cell_measurement_theta_min      3.6540
_cell_volume                     823.2(3)
_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      80(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  0.0275
_diffrn_reflns_av_unetI/netI     0.0410
_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       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6790
_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         26.369
_diffrn_reflns_theta_min         3.202
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93957
_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    1.578
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0456
_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)+(0.0413P)²+0.4398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2848
_reflns_number_total             3363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00462k2.cif
_cod_data_source_block           2_1_rb20_143_1a_80k
_cod_depositor_comments
'Adding full bibliography for 7715495--7715502.cif.'
_cod_database_code               7715500
_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   0.922
_shelx_estimated_absorpt_t_max   0.973
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 0.000000 0.000000 0.500000 0.00919(12) Uani 1 2 d S . P . .
N1 N -0.3241(2) -0.3066(2) 0.11532(18) 0.0181(4) Uani 1 1 d . . . . .
N2 N -0.2808(2) -0.1596(2) 0.12532(17) 0.0142(4) Uani 1 1 d . . . . .
N3 N -0.1809(2) -0.0441(2) 0.24251(17) 0.0149(4) Uani 1 1 d . . . . .
N4 N -0.1564(2) -0.11612(19) 0.31579(16) 0.0120(3) Uani 1 1 d . . . . .
C1 C -0.2454(3) -0.2758(2) 0.2366(2) 0.0161(4) Uani 1 1 d . . . . .
H1 H -0.250489 -0.356111 0.264996 0.019 Uiso 1 1 calc R U . . .
C2 C -0.3311(3) -0.1290(3) 0.0122(2) 0.0179(4) Uani 1 1 d . . . . .
H2A H -0.298733 -0.013593 0.042596 0.021 Uiso 1 1 calc R U . . .
H2B H -0.459117 -0.192706 -0.032317 0.021 Uiso 1 1 calc R U . . .
C3 C -0.2393(3) -0.1750(3) -0.0840(2) 0.0193(5) Uani 1 1 d . . . . .
H3A H -0.271180 -0.149701 -0.158201 0.023 Uiso 1 1 calc R U . . .
H3B H -0.282355 -0.292751 -0.120626 0.023 Uiso 1 1 calc R U . . .
C4 C -0.0416(3) -0.0905(2) -0.0240(2) 0.0187(5) Uani 1 1 d . . . . .
H4A H -0.009508 -0.114185 0.051201 0.022 Uiso 1 1 calc R U . . .
H4B H 0.006739 -0.134961 -0.090616 0.022 Uiso 1 1 calc R U . . .
N5 N 0.3291(2) -0.1956(2) 0.41473(18) 0.0167(4) Uani 1 1 d . . . . .
N6 N 0.2967(2) -0.15099(19) 0.32047(17) 0.0130(3) Uani 1 1 d . . . . .
N7 N 0.1975(2) -0.08124(19) 0.33245(17) 0.0126(3) Uani 1 1 d . . . . .
N8 N 0.1615(2) -0.07921(19) 0.44081(16) 0.0112(3) Uani 1 1 d . . . . .
C5 C 0.2424(3) -0.1490(2) 0.4891(2) 0.0154(4) Uani 1 1 d . . . . .
H5 H 0.237593 -0.162940 0.567031 0.019 Uiso 1 1 calc R U . . .
C6 C 0.3534(3) -0.1904(2) 0.2054(2) 0.0172(4) Uani 1 1 d . . . . .
H6A H 0.477356 -0.165148 0.234783 0.021 Uiso 1 1 calc R U . . .
H6B H 0.343978 -0.123328 0.160329 0.021 Uiso 1 1 calc R U . . .
C7 C 0.2431(3) -0.3674(2) 0.1091(2) 0.0162(4) Uani 1 1 d . . . . .
H7A H 0.288679 -0.390743 0.035016 0.019 Uiso 1 1 calc R U . . .
H7B H 0.254239 -0.433784 0.154406 0.019 Uiso 1 1 calc R U . . .
C8 C 0.0518(3) -0.4148(2) 0.0547(2) 0.0161(4) Uani 1 1 d . . . . .
H8A H 0.041293 -0.339013 0.020002 0.019 Uiso 1 1 calc R U . . .
H8B H 0.001669 -0.406006 0.126873 0.019 Uiso 1 1 calc R U . . .
N9 N 0.1135(2) 0.1880(2) 0.47204(16) 0.0120(3) Uani 1 1 d . . . . .
C9 C 0.1728(2) 0.2960(2) 0.4498(2) 0.0129(4) Uani 1 1 d . . . . .
C10 C 0.2542(3) 0.4332(2) 0.4212(2) 0.0159(4) Uani 1 1 d . . . . .
H10A H 0.249923 0.527065 0.483921 0.019 Uiso 1 1 calc R U . . .
H10B H 0.187821 0.407546 0.331058 0.019 Uiso 1 1 calc R U . . .
C11 C 0.4440(3) 0.4765(3) 0.4317(2) 0.0184(5) Uani 1 1 d . . . . .
H11A H 0.447542 0.383063 0.367716 0.022 Uiso 1 1 calc R U . . .
H11B H 0.492880 0.566934 0.407915 0.022 Uiso 1 1 calc R U . . .
B1 B 0.7375(3) 0.2968(3) 0.2418(3) 0.0186(5) Uani 1 1 d . . . . .
F1 F 0.7793(2) 0.25677(18) 0.12885(14) 0.0324(4) Uani 1 1 d . . . . .
F2 F 0.87993(18) 0.35732(18) 0.35220(15) 0.0333(4) Uani 1 1 d . . . . .
F3 F 0.60335(16) 0.16293(16) 0.23804(14) 0.0245(3) Uani 1 1 d . . . . .
F4 F 0.68278(18) 0.41267(16) 0.25351(14) 0.0274(3) 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'
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
N9 Fe1 N9 180.0 2_556 . ?
N9 Fe1 N4 90.31(7) 2_556 . ?
N9 Fe1 N4 89.69(7) . . ?
N9 Fe1 N4 89.69(7) 2_556 2_556 ?
N9 Fe1 N4 90.31(7) . 2_556 ?
N4 Fe1 N4 180.00(10) . 2_556 ?
N9 Fe1 N8 89.23(7) 2_556 . ?
N9 Fe1 N8 90.77(7) . . ?
N4 Fe1 N8 88.35(7) . . ?
N4 Fe1 N8 91.65(7) 2_556 . ?
N9 Fe1 N8 90.77(7) 2_556 2_556 ?
N9 Fe1 N8 89.23(7) . 2_556 ?
N4 Fe1 N8 91.65(7) . 2_556 ?
N4 Fe1 N8 88.35(7) 2_556 2_556 ?
N8 Fe1 N8 180.00(4) . 2_556 ?
C1 N1 N2 101.62(17) . . ?
N3 N2 N1 114.52(17) . . ?
N3 N2 C2 122.62(17) . . ?
N1 N2 C2 122.73(17) . . ?
N2 N3 N4 105.50(16) . . ?
N3 N4 C1 106.57(17) . . ?
N3 N4 Fe1 123.50(13) . . ?
C1 N4 Fe1 129.72(14) . . ?
N1 C1 N4 111.78(18) . . ?
N1 C1 H1 124.1 . . ?
N4 C1 H1 124.1 . . ?
N2 C2 C3 109.78(17) . . ?
N2 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 C3 C4 114.16(18) . . ?
C2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C4 C4 C3 113.7(2) 2 . ?
C4 C4 H4A 108.8 2 . ?
C3 C4 H4A 108.8 . . ?
C4 C4 H4B 108.8 2 . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 N5 N6 101.83(16) . . ?
N7 N6 N5 114.70(17) . . ?
N7 N6 C6 122.42(17) . . ?
N5 N6 C6 122.63(16) . . ?
N6 N7 N8 104.87(16) . . ?
N7 N8 C5 107.12(16) . . ?
N7 N8 Fe1 122.25(13) . . ?
C5 N8 Fe1 130.45(14) . . ?
N5 C5 N8 111.48(18) . . ?
N5 C5 H5 124.3 . . ?
N8 C5 H5 124.3 . . ?
N6 C6 C7 111.26(16) . . ?
N6 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
N6 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 112.84(16) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 C8 112.1(2) . 2_545 ?
C7 C8 H8A 109.2 . . ?
C8 C8 H8A 109.2 2_545 . ?
C7 C8 H8B 109.2 . . ?
C8 C8 H8B 109.2 2_545 . ?
H8A C8 H8B 107.9 . . ?
C9 N9 Fe1 176.26(16) . . ?
N9 C9 C10 177.8(2) . . ?
C9 C10 C11 111.59(17) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C11 C11 C10 112.6(2) 2_666 . ?
C11 C11 H11A 109.1 2_666 . ?
C10 C11 H11A 109.1 . . ?
C11 C11 H11B 109.1 2_666 . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
F1 B1 F3 110.4(2) . . ?
F1 B1 F2 111.09(19) . . ?
F3 B1 F2 108.29(18) . . ?
F1 B1 F4 109.63(19) . . ?
F3 B1 F4 108.46(18) . . ?
F2 B1 F4 108.89(19) . . ?
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 1.9216(17) 2_556 ?
Fe1 N9 1.9216(17) . ?
Fe1 N4 1.9660(18) . ?
Fe1 N4 1.9661(18) 2_556 ?
Fe1 N8 1.9796(16) . ?
Fe1 N8 1.9796(16) 2_556 ?
N1 C1 1.316(3) . ?
N1 N2 1.327(2) . ?
N2 N3 1.305(2) . ?
N2 C2 1.463(3) . ?
N3 N4 1.314(2) . ?
N4 C1 1.350(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.517(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.519(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C4 1.517(4) 2 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N5 C5 1.318(3) . ?
N5 N6 1.326(2) . ?
N6 N7 1.307(2) . ?
N6 C6 1.464(3) . ?
N7 N8 1.321(2) . ?
N8 C5 1.345(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.522(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.516(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C8 1.519(4) 2_545 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N9 C9 1.138(3) . ?
C9 C10 1.457(3) . ?
C10 C11 1.528(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C11 1.509(4) 2_666 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
B1 F1 1.370(3) . ?
B1 F3 1.385(3) . ?
B1 F2 1.386(3) . ?
B1 F4 1.392(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 0.9(2) . . . . ?
C1 N1 N2 C2 176.82(18) . . . . ?
N1 N2 N3 N4 -0.6(2) . . . . ?
C2 N2 N3 N4 -176.56(17) . . . . ?
N2 N3 N4 C1 0.0(2) . . . . ?
N2 N3 N4 Fe1 175.14(12) . . . . ?
N2 N1 C1 N4 -0.8(2) . . . . ?
N3 N4 C1 N1 0.5(2) . . . . ?
Fe1 N4 C1 N1 -174.18(13) . . . . ?
N3 N2 C2 C3 109.3(2) . . . . ?
N1 N2 C2 C3 -66.3(2) . . . . ?
N2 C2 C3 C4 -56.3(2) . . . . ?
C2 C3 C4 C4 -64.0(3) . . . 2 ?
C5 N5 N6 N7 0.0(2) . . . . ?
C5 N5 N6 C6 -174.39(17) . . . . ?
N5 N6 N7 N8 0.0(2) . . . . ?
C6 N6 N7 N8 174.40(16) . . . . ?
N6 N7 N8 C5 0.0(2) . . . . ?
N6 N7 N8 Fe1 -175.55(12) . . . . ?
N6 N5 C5 N8 0.0(2) . . . . ?
N7 N8 C5 N5 0.0(2) . . . . ?
Fe1 N8 C5 N5 175.08(13) . . . . ?
N7 N6 C6 C7 -100.3(2) . . . . ?
N5 N6 C6 C7 73.7(2) . . . . ?
N6 C6 C7 C8 61.5(2) . . . . ?
C6 C7 C8 C8 172.3(2) . . . 2_545 ?
C9 C10 C11 C11 -61.2(3) . . . 2_666 ?
