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#$Date: 2024-05-05 04:31:51 +0300 (Sun, 05 May 2024) $
#$Revision: 291557 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/13/1571326.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_1571326
loop_
_publ_author_name
'Liu, Shuang'
'Huang, Yuhang'
'Wan, Jingmeng'
'Zheng, Jia-Jia'
'Krishna, Rajamani'
'Li, Yi'
'Ge, Kai'
'Tang, Jie'
'Duan, Jingui'
_publ_section_title
;
 Fine-regulation of gradient gate-opening in nanoporous crystals for
 sieving separation of ternary C3 hydrocarbons.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              6583
_journal_page_last               6588
_journal_paper_doi               10.1039/d3sc05489f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C24 H20 F6 Fe N8 Ti'
_chemical_formula_weight         638.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2gpjqf
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.756(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.599(6)
_cell_length_b                   25.838(11)
_cell_length_c                   13.639(6)
_cell_measurement_reflns_used    3710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.011
_cell_measurement_theta_min      2.983
_cell_volume                     3965(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.1297
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11793
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.367
_diffrn_reflns_theta_min         2.979
_exptl_absorpt_coefficient_mu    0.616
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       rod
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.602
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4959
_refine_ls_number_restraints     293
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0835
_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)+(0.1182P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2630
_reflns_number_total             4959
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05489f2.cif
_cod_data_source_block           as
_cod_depositor_comments
'Adding full bibliography for 1571326--1571329.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               1571326
_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   0.887
_shelx_estimated_absorpt_t_max   0.913
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
C1 C 0.7342(4) 0.75095(18) 0.2684(4) 0.0402(11) Uani 1 1 d . U . . .
H1 H 0.7708 0.7187 0.2824 0.048 Uiso 1 1 calc R U . . .
C2 C 0.6485(4) 0.82028(18) 0.2816(4) 0.0431(11) Uani 1 1 d . U . . .
H2 H 0.6151 0.8452 0.3085 0.052 Uiso 1 1 calc R U . . .
C3 C 0.6505(4) 0.82257(19) 0.1856(4) 0.0444(11) Uani 1 1 d . U . . .
H3 H 0.6198 0.8490 0.1341 0.053 Uiso 1 1 calc R U . . .
C4 C 0.7274(4) 0.76394(19) 0.0864(4) 0.0415(11) Uani 1 1 d . U . . .
C5 C 0.6650(5) 0.7853(2) -0.0149(4) 0.0557(14) Uani 1 1 d . U . . .
H5 H 0.6072 0.8100 -0.0254 0.067 Uiso 1 1 calc R U . . .
C6 C 0.8146(5) 0.7287(2) 0.1013(4) 0.0527(13) Uani 1 1 d . U . . .
H6 H 0.8597 0.7143 0.1703 0.063 Uiso 1 1 calc R U . . .
C7 C 0.5057(5) 0.6890(2) 0.3764(5) 0.0686(18) Uani 1 1 d . U . . .
H7 H 0.4608 0.7192 0.3576 0.082 Uiso 1 1 calc R U . . .
C8 C 0.4613(5) 0.64113(19) 0.3528(6) 0.071(2) Uani 1 1 d . U . . .
H8 H 0.3815 0.6319 0.3174 0.086 Uiso 1 1 calc R U . . .
C9 C 0.6521(4) 0.63741(15) 0.4397(4) 0.0398(11) Uani 1 1 d . U . . .
H9 H 0.7287 0.6240 0.4753 0.048 Uiso 1 1 calc R U . . .
C10 C 0.5528(4) 0.55289(15) 0.3871(4) 0.0394(11) Uani 1 1 d . U . . .
C11 C 0.4537(5) 0.5271(2) 0.3424(8) 0.102(3) Uani 1 1 d . U . . .
H11 H 0.3819 0.5448 0.3100 0.122 Uiso 1 1 calc R U . . .
C12 C 0.6544(5) 0.5272(2) 0.4279(9) 0.133(4) Uani 1 1 d . U . . .
H12 H 0.7260 0.5452 0.4566 0.160 Uiso 1 1 calc R U . . .
F1 F 0.6075(2) 0.79462(9) 0.4983(2) 0.0438(7) Uani 1 1 d . U . . .
F2 F 0.5960(2) 0.89590(10) 0.4901(3) 0.0666(10) Uani 1 1 d . U . . .
F3 F 0.4195(3) 0.84137(12) 0.3501(3) 0.0636(9) Uani 1 1 d . U . . .
Fe1 Fe 0.7500 0.7500 0.5000 0.0306(3) Uani 1 2 d S U P . .
N1 N 0.7023(3) 0.77602(14) 0.3356(3) 0.0405(9) Uani 1 1 d . U . . .
N2 N 0.7057(3) 0.77920(15) 0.1762(3) 0.0379(9) Uani 1 1 d . U . . .
N3 N 0.6275(3) 0.68693(13) 0.4325(3) 0.0413(10) Uani 1 1 d . U . . .
N4 N 0.5556(3) 0.60867(13) 0.3907(3) 0.0412(10) Uani 1 1 d . U . . .
Ti2 Ti 0.5000 0.84585(4) 0.5000 0.0347(3) Uani 1 2 d S TU P . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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 C1 N2 110.0(4) . . ?
N1 C1 H1 125.0 . . ?
N2 C1 H1 125.0 . . ?
C3 C2 N1 110.2(4) . . ?
C3 C2 H2 124.9 . . ?
N1 C2 H2 124.9 . . ?
C2 C3 N2 107.2(4) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
C5 C4 C6 118.6(5) . . ?
C5 C4 N2 120.8(4) . . ?
C6 C4 N2 120.5(4) . . ?
C4 C5 C6 121.4(5) . 7_665 ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 7_665 . ?
C5 C6 C4 119.9(4) 7_665 . ?
C5 C6 H6 120.0 7_665 . ?
C4 C6 H6 120.0 . . ?
C8 C7 N3 109.8(4) . . ?
C8 C7 H7 125.1 . . ?
N3 C7 H7 125.1 . . ?
C7 C8 N4 106.4(5) . . ?
C7 C8 H8 126.8 . . ?
N4 C8 H8 126.8 . . ?
N3 C9 N4 112.2(4) . . ?
N3 C9 H9 123.9 . . ?
N4 C9 H9 123.9 . . ?
C11 C10 C12 118.9(5) . . ?
C11 C10 N4 122.2(4) . . ?
C12 C10 N4 118.9(4) . . ?
C10 C11 C11 120.9(3) . 6_565 ?
C10 C11 H11 119.6 . . ?
C11 C11 H11 119.6 6_565 . ?
C10 C12 C12 120.1(3) . 6_565 ?
C10 C12 H12 120.0 . . ?
C12 C12 H12 120.0 6_565 . ?
Ti2 F1 Fe1 168.64(15) . . ?
F1 Fe1 F1 180.0 7_666 . ?
F1 Fe1 N3 88.05(12) 7_666 7_666 ?
F1 Fe1 N3 91.95(12) . 7_666 ?
F1 Fe1 N3 91.95(12) 7_666 . ?
F1 Fe1 N3 88.05(12) . . ?
N3 Fe1 N3 180.0 7_666 . ?
F1 Fe1 N1 91.08(13) 7_666 . ?
F1 Fe1 N1 88.93(13) . . ?
N3 Fe1 N1 91.12(15) 7_666 . ?
N3 Fe1 N1 88.88(15) . . ?
F1 Fe1 N1 88.92(13) 7_666 7_666 ?
F1 Fe1 N1 91.07(13) . 7_666 ?
N3 Fe1 N1 88.88(15) 7_666 7_666 ?
N3 Fe1 N1 91.12(15) . 7_666 ?
N1 Fe1 N1 180.0(2) . 7_666 ?
C1 N1 C2 105.6(4) . . ?
C1 N1 Fe1 122.6(3) . . ?
C2 N1 Fe1 131.5(3) . . ?
C3 N2 C1 106.9(4) . . ?
C3 N2 C4 128.0(4) . . ?
C1 N2 C4 125.1(4) . . ?
C9 N3 C7 104.3(4) . . ?
C9 N3 Fe1 127.5(3) . . ?
C7 N3 Fe1 128.1(3) . . ?
C9 N4 C8 107.1(4) . . ?
C9 N4 C10 125.6(4) . . ?
C8 N4 C10 127.1(4) . . ?
F2 Ti2 F2 89.21(19) . 2_656 ?
F2 Ti2 F3 94.30(16) . 2_656 ?
F2 Ti2 F3 90.86(15) 2_656 2_656 ?
F2 Ti2 F3 90.85(15) . . ?
F2 Ti2 F3 94.30(16) 2_656 . ?
F3 Ti2 F3 172.8(2) 2_656 . ?
F2 Ti2 F1 176.53(14) . 2_656 ?
F2 Ti2 F1 89.62(13) 2_656 2_656 ?
F3 Ti2 F1 88.98(13) 2_656 2_656 ?
F3 Ti2 F1 85.98(13) . 2_656 ?
F2 Ti2 F1 89.62(13) . . ?
F2 Ti2 F1 176.53(14) 2_656 . ?
F3 Ti2 F1 85.98(13) 2_656 . ?
F3 Ti2 F1 88.98(13) . . ?
F1 Ti2 F1 91.73(17) 2_656 . ?
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
C1 N1 1.324(6) . ?
C1 N2 1.355(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.323(7) . ?
C2 N1 1.364(5) . ?
C2 H2 0.9300 . ?
C3 N2 1.355(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(6) . ?
C4 C6 1.370(7) . ?
C4 N2 1.426(6) . ?
C5 C6 1.363(7) 7_665 ?
C5 H5 0.9300 . ?
C6 C5 1.363(7) 7_665 ?
C6 H6 0.9300 . ?
C7 C8 1.336(7) . ?
C7 N3 1.373(6) . ?
C7 H7 0.9300 . ?
C8 N4 1.352(6) . ?
C8 H8 0.9300 . ?
C9 N3 1.310(5) . ?
C9 N4 1.321(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.300(7) . ?
C10 C12 1.322(7) . ?
C10 N4 1.442(5) . ?
C11 C11 1.399(11) 6_565 ?
C11 H11 0.9300 . ?
C12 C12 1.407(10) 6_565 ?
C12 H12 0.9300 . ?
F1 Ti2 1.901(2) . ?
F1 Fe1 2.126(2) . ?
F2 Ti2 1.816(3) . ?
F3 Ti2 1.832(3) . ?
Fe1 F1 2.126(2) 7_666 ?
Fe1 N3 2.146(4) 7_666 ?
Fe1 N3 2.146(4) . ?
Fe1 N1 2.151(4) . ?
Fe1 N1 2.151(4) 7_666 ?
Ti2 F2 1.816(3) 2_656 ?
Ti2 F3 1.832(3) 2_656 ?
Ti2 F1 1.901(2) 2_656 ?
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
N1 C2 C3 N2 0.4(6) . . . . ?
C6 C4 C5 C6 1.8(10) . . . 7_665 ?
N2 C4 C5 C6 179.6(5) . . . 7_665 ?
C5 C4 C6 C5 -1.7(9) . . . 7_665 ?
N2 C4 C6 C5 -179.5(5) . . . 7_665 ?
N3 C7 C8 N4 -2.1(8) . . . . ?
C12 C10 C11 C11 3.4(9) . . . 6_565 ?
N4 C10 C11 C11 -178.5(3) . . . 6_565 ?
C11 C10 C12 C12 -3.4(9) . . . 6_565 ?
N4 C10 C12 C12 178.5(3) . . . 6_565 ?
N2 C1 N1 C2 2.2(5) . . . . ?
N2 C1 N1 Fe1 -172.2(3) . . . . ?
C3 C2 N1 C1 -1.6(6) . . . . ?
C3 C2 N1 Fe1 172.1(4) . . . . ?
C2 C3 N2 C1 1.0(5) . . . . ?
C2 C3 N2 C4 179.0(5) . . . . ?
N1 C1 N2 C3 -2.0(5) . . . . ?
N1 C1 N2 C4 179.9(4) . . . . ?
C5 C4 N2 C3 -18.5(8) . . . . ?
C6 C4 N2 C3 159.2(5) . . . . ?
C5 C4 N2 C1 159.1(5) . . . . ?
C6 C4 N2 C1 -23.2(7) . . . . ?
N4 C9 N3 C7 1.3(6) . . . . ?
N4 C9 N3 Fe1 178.7(3) . . . . ?
C8 C7 N3 C9 0.6(7) . . . . ?
C8 C7 N3 Fe1 -176.8(4) . . . . ?
N3 C9 N4 C8 -2.6(6) . . . . ?
N3 C9 N4 C10 -178.0(4) . . . . ?
C7 C8 N4 C9 2.9(7) . . . . ?
C7 C8 N4 C10 178.2(5) . . . . ?
C11 C10 N4 C9 176.1(7) . . . . ?
C12 C10 N4 C9 -5.8(10) . . . . ?
C11 C10 N4 C8 1.6(10) . . . . ?
C12 C10 N4 C8 179.7(8) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.021 0.000 -0.004 911 223 ' '
2 -0.021 0.500 0.000 911 223 ' '
