#------------------------------------------------------------------------------
#$Date: 2023-05-05 04:16:08 +0300 (Fri, 05 May 2023) $
#$Revision: 283194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/87/1568774.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_1568774
loop_
_publ_author_name
'Duan, Yuefeng'
'Huang, Yuhang'
'Wang, Chongqing'
'Wang, Qian'
'Ge, Kai'
'Lu, Zhiyong'
'Wang, Huijie'
'Duan, Jingui'
'Bai, Junfeng'
'Jin, Wanqin'
_publ_section_title
;
 Formation and fine-tuning of metal--organic frameworks with carboxylic
 pincers for the recognition of a C2H2 tetramer and highly selective
 separation of C2H2/C2H4
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4605
_journal_page_last               4611
_journal_paper_doi               10.1039/D3SC00877K
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C26 H20 Cu F6 N8 O4 Si'
_chemical_formula_weight         714.13
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-10-06 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.228(4)
_cell_length_b                   16.228(4)
_cell_length_c                   32.536(18)
_cell_measurement_reflns_used    1793
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.262
_cell_measurement_theta_min      2.250
_cell_volume                     8568(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker smart CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1537
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            31240
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.402
_exptl_absorpt_coefficient_mu    0.597
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3831
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0804
_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)+(0.0883P)²+9.5003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2001
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2347
_reflns_number_total             3831
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc00877k2.cif
_cod_data_source_block           NTU-71
_cod_depositor_comments
'Adding full bibliography for 1568769--1568774.cif.'
_cod_database_code               1568774
_shelx_shelxl_version_number     2018/3
_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   0.932
_shelx_estimated_absorpt_t_max   0.943
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/4'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x, z+3/4'
'x, -y+1/2, -z+1/4'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y, -z+3/4'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'-x+1, -y+1, z+1'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1, -z+3/4'
'y+1, x+1, -z+1'
'-x+1, y+1/2, -z+5/4'
'-y+1/2, -x+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_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 0.3715(8) 0.5490(7) 0.1839(4) 0.071(3) Uani 1 1 d . U . . .
H1 H 0.370405 0.603800 0.175546 0.085 Uiso 1 1 calc R U . . .
C2 C 0.3309(8) 0.5205(7) 0.2155(4) 0.078(3) Uani 1 1 d . U . . .
H2 H 0.294798 0.549390 0.232416 0.093 Uiso 1 1 calc R U . . .
C3 C 0.4012(6) 0.4227(7) 0.1866(3) 0.050(2) Uani 1 1 d . U . . .
H3 H 0.422671 0.371194 0.180074 0.060 Uiso 1 1 calc R U . . .
C4 C 0.3306(6) 0.3782(6) 0.2493(3) 0.052(2) Uani 1 1 d . U . . .
C5 C 0.3835(7) 0.3126(6) 0.2570(3) 0.054(2) Uani 1 1 d . U . . .
H5 H 0.432927 0.308895 0.242662 0.065 Uiso 1 1 calc R U . . .
C7 C 0.2883(6) 0.2614(7) 0.3070(3) 0.061(3) Uani 1 1 d . U . . .
H7 H 0.271378 0.220726 0.325323 0.074 Uiso 1 1 calc R U . . .
C8 C 0.2384(8) 0.3293(7) 0.3012(4) 0.068(3) Uani 1 1 d . U . . .
C9 C 0.2591(9) 0.3867(7) 0.2712(4) 0.070(3) Uani 1 1 d . U . . .
H9 H 0.224228 0.431022 0.266015 0.084 Uiso 1 1 calc R U . . .
C10 C 0.1574(9) 0.3389(10) 0.3234(5) 0.094(4) Uani 1 1 d . U . . .
C11 C 0.4122(7) 0.1361(7) 0.3262(3) 0.057(2) Uani 1 1 d . U . . .
H11 H 0.368344 0.133522 0.344510 0.068 Uiso 1 1 calc R U . . .
C13 C 0.5263(8) 0.1070(8) 0.2944(4) 0.078(3) Uani 1 1 d . U . . .
H13 H 0.577175 0.084411 0.287534 0.094 Uiso 1 1 calc R U . . .
C6 C 0.3635(6) 0.2516(7) 0.2864(3) 0.049(2) Uani 1 1 d . U . . .
C12 C 0.4871(9) 0.1652(8) 0.2730(4) 0.082(3) Uani 1 1 d . U . . .
H12 H 0.503587 0.186304 0.247744 0.098 Uiso 1 1 calc R U . . .
Cu1 Cu 0.500000 0.500000 0.12021(4) 0.0452(5) Uani 1 2 d S TU P . .
F1 F 0.5847(5) 0.750000 0.125000 0.063(2) Uani 1 2 d S TU P . .
F2 F 0.4804(4) 0.7416(3) 0.17650(15) 0.0616(16) Uani 1 1 d . U . . .
F3 F 0.4781(3) 0.6452(3) 0.12211(15) 0.0439(13) Uani 1 1 d . U . . .
F4 F 0.3758(5) 0.750000 0.125000 0.075(3) Uani 1 2 d S TU P . .
N1 N 0.4155(5) 0.4891(5) 0.1646(2) 0.0411(17) Uani 1 1 d . U . . .
N2 N 0.3536(6) 0.4357(5) 0.2187(3) 0.056(2) Uani 1 1 d . U . . .
N3 N 0.4173(5) 0.1888(5) 0.2950(3) 0.052(2) Uani 1 1 d . U . . .
N4 N 0.4808(5) 0.0858(5) 0.3276(2) 0.051(2) Uani 1 1 d . U . . .
O1 O 0.1214(7) 0.4041(7) 0.3190(3) 0.131(4) Uani 1 1 d . U . . .
O2 O 0.1382(5) 0.2821(5) 0.3492(3) 0.085(3) Uani 1 1 d . U . . .
H2A H 0.091822 0.293464 0.359935 0.127 Uiso 1 1 d R U . . .
Si1 Si 0.4792(2) 0.750000 0.125000 0.0472(10) 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'
Cu Cu 0.3201 1.2651 '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'
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'
Si Si 0.0817 0.0704 '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
C2 C1 N1 112.0(11) . . ?
C2 C1 H1 124.0 . . ?
N1 C1 H1 124.0 . . ?
C1 C2 N2 105.5(11) . . ?
C1 C2 H2 127.2 . . ?
N2 C2 H2 127.2 . . ?
N1 C3 N2 113.8(9) . . ?
N1 C3 H3 123.1 . . ?
N2 C3 H3 123.1 . . ?
C9 C4 C5 120.5(11) . . ?
C9 C4 N2 121.6(10) . . ?
C5 C4 N2 117.9(9) . . ?
C4 C5 C6 121.1(10) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C8 C7 C6 122.4(11) . . ?
C8 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C7 C8 C9 119.3(11) . . ?
C7 C8 C10 121.9(11) . . ?
C9 C8 C10 118.5(12) . . ?
C4 C9 C8 120.1(11) . . ?
C4 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
O1 C10 O2 125.7(13) . . ?
O1 C10 C8 116.9(14) . . ?
O2 C10 C8 116.7(12) . . ?
N3 C11 N4 110.9(9) . . ?
N3 C11 H11 124.6 . . ?
N4 C11 H11 124.6 . . ?
C12 C13 N4 109.6(11) . . ?
C12 C13 H13 125.2 . . ?
N4 C13 H13 125.2 . . ?
N3 C6 C7 122.7(10) . . ?
N3 C6 C5 120.9(9) . . ?
C7 C6 C5 116.3(10) . . ?
C13 C12 N3 108.4(10) . . ?
C13 C12 H12 125.8 . . ?
N3 C12 H12 125.8 . . ?
N4 Cu1 N4 91.6(5) 10_544 4_564 ?
N4 Cu1 N1 175.7(4) 10_544 11_554 ?
N4 Cu1 N1 90.6(3) 4_564 11_554 ?
N4 Cu1 N1 90.6(3) 10_544 . ?
N4 Cu1 N1 175.7(4) 4_564 . ?
N1 Cu1 N1 87.5(4) 11_554 . ?
N4 Cu1 F3 88.1(3) 10_544 11_554 ?
N4 Cu1 F3 94.0(3) 4_564 11_554 ?
N1 Cu1 F3 88.1(3) 11_554 11_554 ?
N1 Cu1 F3 89.7(3) . 11_554 ?
N4 Cu1 F3 94.0(3) 10_544 . ?
N4 Cu1 F3 88.1(3) 4_564 . ?
N1 Cu1 F3 89.7(3) 11_554 . ?
N1 Cu1 F3 88.1(3) . . ?
F3 Cu1 F3 177.0(2) 11_554 . ?
Si1 F3 Cu1 170.7(3) . . ?
C3 N1 C1 104.1(8) . . ?
C3 N1 Cu1 126.0(7) . . ?
C1 N1 Cu1 129.0(7) . . ?
C3 N2 C4 127.4(9) . . ?
C3 N2 C2 104.4(9) . . ?
C4 N2 C2 128.2(9) . . ?
C11 N3 C6 126.5(9) . . ?
C11 N3 C12 105.4(9) . . ?
C6 N3 C12 128.1(9) . . ?
C13 N4 C11 105.2(9) . . ?
C13 N4 Cu1 130.4(8) . 2_645 ?
C11 N4 Cu1 124.3(7) . 2_645 ?
C10 O2 H2A 109.1 . . ?
F4 Si1 F2 90.6(3) . . ?
F4 Si1 F2 90.6(3) . 5_565 ?
F2 Si1 F2 178.7(5) . 5_565 ?
F4 Si1 F3 89.4(2) . . ?
F2 Si1 F3 88.5(3) . . ?
F2 Si1 F3 91.5(3) 5_565 . ?
F4 Si1 F3 89.4(2) . 5_565 ?
F2 Si1 F3 91.5(3) . 5_565 ?
F2 Si1 F3 88.5(3) 5_565 5_565 ?
F3 Si1 F3 178.8(4) . 5_565 ?
F4 Si1 F1 180.0 . . ?
F2 Si1 F1 89.4(3) . . ?
F2 Si1 F1 89.4(3) 5_565 . ?
F3 Si1 F1 90.6(2) . . ?
F3 Si1 F1 90.6(2) 5_565 . ?
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 C2 1.306(15) . ?
C1 N1 1.360(13) . ?
C1 H1 0.9300 . ?
C2 N2 1.428(14) . ?
C2 H2 0.9300 . ?
C3 N1 1.314(12) . ?
C3 N2 1.316(11) . ?
C3 H3 0.9300 . ?
C4 C9 1.369(15) . ?
C4 C5 1.391(13) . ?
C4 N2 1.416(13) . ?
C5 C6 1.413(14) . ?
C5 H5 0.9300 . ?
C7 C8 1.379(15) . ?
C7 C6 1.404(13) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(15) . ?
C8 C10 1.507(17) . ?
C9 H9 0.9300 . ?
C10 O1 1.217(15) . ?
C10 O2 1.284(15) . ?
C11 N3 1.329(13) . ?
C11 N4 1.382(13) . ?
C11 H11 0.9300 . ?
C13 C12 1.334(15) . ?
C13 N4 1.353(13) . ?
C13 H13 0.9300 . ?
C6 N3 1.370(13) . ?
C12 N3 1.394(14) . ?
C12 H12 0.9300 . ?
Cu1 N4 1.989(8) 10_544 ?
Cu1 N4 1.989(8) 4_564 ?
Cu1 N1 2.000(7) 11_554 ?
Cu1 N1 2.000(7) . ?
Cu1 F3 2.384(4) 11_554 ?
Cu1 F3 2.384(4) . ?
F1 Si1 1.711(9) . ?
F2 Si1 1.681(5) . ?
F3 Si1 1.703(4) . ?
F4 Si1 1.678(9) . ?
O2 H2A 0.8500 . ?
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 C1 C2 N2 3.4(15) . . . . ?
C9 C4 C5 C6 2.5(18) . . . . ?
N2 C4 C5 C6 -178.3(9) . . . . ?
C6 C7 C8 C9 5.9(18) . . . . ?
C6 C7 C8 C10 179.7(12) . . . . ?
C5 C4 C9 C8 -0.6(18) . . . . ?
N2 C4 C9 C8 -179.7(10) . . . . ?
C7 C8 C9 C4 -3.6(19) . . . . ?
C10 C8 C9 C4 -177.5(12) . . . . ?
C7 C8 C10 O1 173.7(14) . . . . ?
C9 C8 C10 O1 -13(2) . . . . ?
C7 C8 C10 O2 2(2) . . . . ?
C9 C8 C10 O2 176.0(12) . . . . ?
C8 C7 C6 N3 173.2(11) . . . . ?
C8 C7 C6 C5 -3.9(16) . . . . ?
C4 C5 C6 N3 -177.5(10) . . . . ?
C4 C5 C6 C7 -0.3(15) . . . . ?
N4 C13 C12 N3 5.9(16) . . . . ?
N2 C3 N1 C1 -1.6(12) . . . . ?
N2 C3 N1 Cu1 168.0(7) . . . . ?
C2 C1 N1 C3 -1.3(14) . . . . ?
C2 C1 N1 Cu1 -170.5(8) . . . . ?
N1 C3 N2 C4 -176.4(10) . . . . ?
N1 C3 N2 C2 3.6(12) . . . . ?
C9 C4 N2 C3 -154.1(12) . . . . ?
C5 C4 N2 C3 26.8(17) . . . . ?
C9 C4 N2 C2 25.9(18) . . . . ?
C5 C4 N2 C2 -153.3(12) . . . . ?
C1 C2 N2 C3 -4.1(14) . . . . ?
C1 C2 N2 C4 175.9(11) . . . . ?
N4 C11 N3 C6 -174.6(9) . . . . ?
N4 C11 N3 C12 6.8(13) . . . . ?
C7 C6 N3 C11 -8.8(17) . . . . ?
C5 C6 N3 C11 168.2(10) . . . . ?
C7 C6 N3 C12 169.6(11) . . . . ?
C5 C6 N3 C12 -13.5(17) . . . . ?
C13 C12 N3 C11 -7.7(14) . . . . ?
C13 C12 N3 C6 173.6(11) . . . . ?
C12 C13 N4 C11 -1.8(14) . . . . ?
C12 C13 N4 Cu1 176.5(9) . . . 2_645 ?
N3 C11 N4 C13 -3.3(13) . . . . ?
N3 C11 N4 Cu1 178.3(6) . . . 2_645 ?
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 -0.009 -0.009 -0.001 3788 840 ' '
