#------------------------------------------------------------------------------
#$Date: 2019-04-03 01:09:12 +0300 (Wed, 03 Apr 2019) $
#$Revision: 214449 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/32/7123240.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_7123240
loop_
_publ_author_name
'Yang, Lifeng'
'Jin, Anye'
'Ge, Lisha'
'Cui, Xili'
'Xing, Huabin'
_publ_section_title
;
 A novel interpenetrated anion-pillared porous material with high water
 tolerance afforded efficient C2H2/C2H4 separation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00976K
_journal_year                    2019
_chemical_formula_sum            'C24 H16 F5 N4 Nb Ni O'
_chemical_formula_weight         623.03
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-01-29 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8526(6)
_cell_length_b                   13.8526(6)
_cell_length_c                   7.8862(4)
_cell_measurement_reflns_used    6299
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      54.05
_cell_measurement_theta_min      5.62
_cell_volume                     1513.32(12)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9148
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.000
_diffrn_reflns_theta_max         53.000
_diffrn_reflns_theta_min         5.616
_exptl_absorpt_coefficient_mu    5.783
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.216
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         417
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0644
_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)+(0.1350P)²+1.1712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                417
_reflns_number_total             417
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc00976k2.cif
_cod_data_source_block           12_a_sq
_cod_original_cell_volume        1513.32(15)
_cod_database_code               7123240
_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   0.624
_shelx_estimated_absorpt_t_max   0.723
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'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
Nb1 Nb 0.000000 0.000000 1.000000 0.0409(6) Uani 1 16 d S T P . .
Ni1 Ni 0.000000 0.000000 0.500000 0.0168(6) Uani 1 16 d S T P . .
F1 F 0.000000 0.000000 0.7552(5) 0.0263(17) Uani 0.5 8 d S T P A 1
O1 O 0.000000 0.000000 0.7552(5) 0.0263(17) Uani 0.5 8 d S T P A 2
F2 F 0.0971(2) -0.0971(2) 1.000000 0.0639(15) Uani 1 4 d S T P A .
N1 N 0.000000 0.1520(3) 0.500000 0.0245(11) Uani 1 4 d S T P A .
C1B C -0.0252(16) 0.2030(9) 0.3616(19) 0.023(3) Uani 0.34(3) 1 d . U P A 2
H1BA H -0.048187 0.168514 0.265584 0.027 Uiso 0.34(3) 1 d R U P A 2
C2B C -0.0256(16) 0.3022(10) 0.3600(19) 0.031(4) Uani 0.34(3) 1 d . U P A 2
H2BA H -0.048517 0.334840 0.261931 0.038 Uiso 0.34(3) 1 d R U P A 2
C3 C 0.000000 0.3542(4) 0.500000 0.0353(15) Uani 1 4 d S TU P . .
C4 C 0.000000 0.4564(6) 0.500000 0.0380(15) Uani 1 4 d S TU P A .
C1A C 0.056(3) 0.2013(18) 0.380(3) 0.015(6) Uani 0.16(3) 1 d . U P A 1
H1AA H 0.079834 0.166793 0.284294 0.018 Uiso 0.16(3) 1 d R U P A 1
C2A C 0.058(4) 0.300(2) 0.370(4) 0.025(7) Uani 0.16(3) 1 d . U P A 1
H2AA H 0.081820 0.332385 0.272280 0.030 Uiso 0.16(3) 1 d R U P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.2894 1.9494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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
F2 Nb1 F2 180.0(3) 18_557 2
F2 Nb1 F2 90.0 18_557 17_557
F2 Nb1 F2 90.0 2 17_557
F2 Nb1 F2 90.0 18_557 .
F2 Nb1 F2 90.0 2 .
F2 Nb1 F2 180.0 17_557 .
F2 Nb1 F1 90.000(1) 18_557 .
F2 Nb1 F1 90.000(1) 2 .
F2 Nb1 F1 90.0 17_557 .
F2 Nb1 F1 90.0 . .
F2 Nb1 O1 90.000(1) 18_557 .
F2 Nb1 O1 90.000(1) 2 .
F2 Nb1 O1 90.0 17_557 .
F2 Nb1 O1 90.0 . .
F2 Nb1 F1 90.000(1) 18_557 17_557
F2 Nb1 F1 90.000(1) 2 17_557
F2 Nb1 F1 90.0 17_557 17_557
F2 Nb1 F1 90.0 . 17_557
F1 Nb1 F1 180.0 . 17_557
F1 Ni1 F1 180.0 17_556 .
F1 Ni1 N1 90.0 17_556 18_556
F1 Ni1 N1 90.0 . 18_556
F1 Ni1 N1 90.0 17_556 2
F1 Ni1 N1 90.0 . 2
O1 Ni1 N1 90.0 . 2
N1 Ni1 N1 180.0 18_556 2
F1 Ni1 N1 90.0 17_556 17_556
F1 Ni1 N1 90.0 . 17_556
O1 Ni1 N1 90.0 . 17_556
N1 Ni1 N1 90.0 18_556 17_556
N1 Ni1 N1 90.0 2 17_556
F1 Ni1 N1 90.0 17_556 .
F1 Ni1 N1 90.0 . .
O1 Ni1 N1 90.0 . .
N1 Ni1 N1 90.0 18_556 .
N1 Ni1 N1 90.0 2 .
N1 Ni1 N1 180.0 17_556 .
Nb1 F1 Ni1 180.0 . .
Nb1 O1 Ni1 180.0 . .
C1A N1 C1A 85(3) . 19_556
C1A N1 C1A 122(2) . 7_556
C1A N1 C1A 67(3) 19_556 7_556
C1A N1 C1A 67(3) . 21
C1A N1 C1A 122(2) 19_556 21
C1A N1 C1A 85(3) 7_556 21
C1B N1 Ni1 121.7(6) . .
C1B N1 Ni1 121.7(6) 7_556 .
C1B N1 Ni1 121.7(6) 19_556 .
C1B N1 Ni1 121.7(6) 21 .
C1A N1 Ni1 119.1(11) . .
C1A N1 Ni1 119.1(11) 19_556 .
C1A N1 Ni1 119.1(11) 7_556 .
C1A N1 Ni1 119.1(11) 21 .
C1B C1B N1 75.0(10) 21 .
C1B C1B C2B 90.2(7) 21 .
N1 C1B C2B 122.2(11) . .
N1 C1B C2B 110.8(14) . 21
C1B C1B H1BA 109.6 21 .
N1 C1B H1BA 118.0 . .
C2B C1B H1BA 119.6 . .
C2B C1B H1BA 126.4 21 .
C2B C2B C3 74.9(10) 21 .
C2B C2B C1B 89.8(7) 21 .
C3 C2B C1B 121.2(12) . .
C3 C2B C1B 110.1(14) . 21
C2B C2B H2BA 109.5 21 .
C3 C2B H2BA 119.7 . .
C1B C2B H2BA 119.0 . .
C1B C2B H2BA 125.6 21 .
C2B C3 C2B 30.1(19) 21 .
C2B C3 C2B 116.4(12) 7_556 .
C2B C3 C2B 108.0(16) 19_556 .
C2B C3 C4 121.8(6) 21 .
C2B C3 C4 121.8(6) 7_556 .
C2B C3 C4 121.8(6) 19_556 .
C2B C3 C4 121.8(6) . .
C4 C3 C2A 120.0(13) . .
C4 C3 C2A 120.0(13) . 21
C2A C3 C2A 65(3) . 21
C4 C3 C2A 120.0(13) . 19_556
C2A C3 C2A 86(3) . 19_556
C2A C3 C2A 120(3) 21 19_556
C2B C3 C2A 115.2(10) 21 7_556
C2B C3 C2A 48(2) 7_556 7_556
C2B C3 C2A 17.5(11) 19_556 7_556
C2B C3 C2A 98.5(16) . 7_556
C4 C3 C2A 120.0(13) . 7_556
C2A C3 C2A 120(3) . 7_556
C2A C3 C2A 86(3) 21 7_556
C2A C3 C2A 65(3) 19_556 7_556
C4 C4 C3 180.0 17_566 .
C2A C1A N1 122(2) . .
C2A C1A C1A 91.3(17) . 21
N1 C1A C1A 56.4(17) . 21
C2A C1A C1A 93.2(17) . 19_556
N1 C1A C1A 47.5(14) . 19_556
C1A C1A C1A 90.001(5) 21 19_556
C2A C1A C2A 51(3) . 21
N1 C1A C2A 86(2) . 21
C1A C1A C2A 40.8(17) 21 21
C1A C1A C2A 92.1(11) 19_556 21
C2A C1A H1AA 116.7 . .
N1 C1A H1AA 118.8 . .
C1A C1A H1AA 110.3 21 .
C1A C1A H1AA 142.3 19_556 .
C2A C1A H1AA 124.2 21 .
C1A C2A C2A 88.7(17) . 21
C1A C2A C3 117(3) . .
C2A C2A C3 57.6(17) 21 .
C1A C2A C1A 48(2) . 21
C2A C2A C1A 40.8(17) 21 21
C3 C2A C1A 84(3) . 21
C1A C2A C2A 86.8(17) . 19_556
C2A C2A C2A 90.001(4) 21 19_556
C3 C2A C2A 47.1(13) . 19_556
C1A C2A C2A 87.9(11) 21 19_556
C1A C2A H2AA 121.9 . .
C2A C2A H2AA 110.1 21 .
C3 C2A H2AA 119.8 . .
C1A C2A H2AA 126.9 21 .
C2A C2A H2AA 144.1 19_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 F2 1.903(5) 18_557
Nb1 F2 1.903(5) 2
Nb1 F2 1.903(5) 17_557
Nb1 F2 1.903(5) .
Nb1 F1 1.930(4) .
Nb1 O1 1.930(4) .
Nb1 F1 1.930(4) 17_557
Ni1 F1 2.013(4) 17_556
Ni1 F1 2.013(4) .
Ni1 O1 2.013(4) .
Ni1 N1 2.105(4) 18_556
Ni1 N1 2.105(4) 2
Ni1 N1 2.105(4) 17_556
Ni1 N1 2.105(4) .
N1 C1B 1.346(13) .
N1 C1B 1.346(13) 7_556
N1 C1B 1.346(13) 19_556
N1 C1B 1.346(13) 21
N1 C1A 1.40(3) .
N1 C1A 1.40(3) 19_556
N1 C1A 1.40(3) 7_556
N1 C1A 1.40(3) 21
C1B C1B 0.70(4) 21
C1B C2B 1.376(18) .
C1B C2B 1.55(2) 21
C1B H1BA 0.9500 .
C2B C2B 0.71(5) 21
C2B C3 1.365(14) .
C2B H2BA 0.9500 .
C3 C4 1.416(11) .
C3 C2A 1.51(4) .
C3 C2A 1.51(4) 21
C3 C2A 1.51(4) 19_556
C3 C2A 1.51(4) 7_556
C4 C4 1.208(18) 17_566
C1A C2A 1.37(4) .
C1A C1A 1.55(9) 21
C1A C1A 1.90(5) 19_556
C1A C2A 2.09(7) 21
C1A H1AA 0.9500 .
C2A C2A 1.61(10) 21
C2A C2A 2.05(6) 19_556
C2A H2AA 0.9500 .
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_4
C1B N1 C1B C1B 80.5(7) 7_556 21
C1B N1 C1B C1B 111.8(13) 19_556 21
Ni1 N1 C1B C1B -99.5(7) . 21
C1B N1 C1B C2B -0.1(9) 7_556 .
C1B N1 C1B C2B 31(2) 19_556 .
C1B N1 C1B C2B -80.5(13) 21 .
Ni1 N1 C1B C2B 179.9(9) . .
C1B N1 C1B C2B 27.8(11) 7_556 21
C1B N1 C1B C2B 59(3) 19_556 21
C1B N1 C1B C2B -52.6(18) 21 21
Ni1 N1 C1B C2B -152.2(11) . 21
C1B C1B C2B C2B -0.003(1) 21 21
N1 C1B C2B C2B 72.3(14) . 21
C1B C1B C2B C3 -72.2(14) 21 .
N1 C1B C2B C3 0.1(19) . .
C2B C1B C2B C3 -72.1(14) 21 .
N1 C1B C2B C1B 72.3(14) . 21
C2B C1B C2B C1B 0.003(1) 21 21
C1B C2B C3 C2B 80.3(13) . 21
C1B C2B C3 C2B 53.0(17) 21 21
C2B C2B C3 C2B -80.4(7) 21 7_556
C1B C2B C3 C2B -0.1(9) . 7_556
C1B C2B C3 C2B -27.3(11) 21 7_556
C2B C2B C3 C2B -111.7(12) 21 19_556
C1B C2B C3 C2B -31(2) . 19_556
C1B C2B C3 C2B -59(3) 21 19_556
C2B C2B C3 C4 99.6(7) 21 .
C1B C2B C3 C4 179.9(9) . .
C1B C2B C3 C4 152.7(11) 21 .
C1A N1 C1A C2A -60(3) 19_556 .
C1A N1 C1A C2A -1(2) 7_556 .
C1A N1 C1A C2A 67(3) 21 .
Ni1 N1 C1A C2A 179(2) . .
C1A N1 C1A C1A -127.5(16) 19_556 21
C1A N1 C1A C1A -68.3(14) 7_556 21
Ni1 N1 C1A C1A 111.7(14) . 21
C1A N1 C1A C1A 59(2) 7_556 19_556
C1A N1 C1A C1A 127.5(16) 21 19_556
Ni1 N1 C1A C1A -121(2) . 19_556
C1A N1 C1A C2A -97(2) 19_556 21
C1A N1 C1A C2A -37.7(10) 7_556 21
C1A N1 C1A C2A 30.6(19) 21 21
Ni1 N1 C1A C2A 142.3(10) . 21
N1 C1A C2A C2A -50(3) . 21
C1A C1A C2A C2A 0.0 21 21
C1A C1A C2A C2A -90.08(11) 19_556 21
N1 C1A C2A C3 2(4) . .
C1A C1A C2A C3 52(2) 21 .
C1A C1A C2A C3 -38(2) 19_556 .
C2A C1A C2A C3 52(2) 21 .
N1 C1A C2A C1A -50(3) . 21
C1A C1A C2A C1A -90.07(11) 19_556 21
C2A C1A C2A C1A 0.0 21 21
N1 C1A C2A C2A 40(3) . 19_556
C1A C1A C2A C2A 90.07(11) 21 19_556
C1A C1A C2A C2A -0.002(6) 19_556 19_556
C2A C1A C2A C2A 90.07(11) 21 19_556
C4 C3 C2A C1A 178.9(18) . .
C2A C3 C2A C1A -70(3) 21 .
C2A C3 C2A C1A 56(3) 19_556 .
C2A C3 C2A C1A -1.1(18) 7_556 .
C4 C3 C2A C2A -111.5(13) . 21
C2A C3 C2A C2A 126.1(19) 19_556 21
C2A C3 C2A C2A 68.5(13) 7_556 21
C4 C3 C2A C1A -144.9(8) . 21
C2A C3 C2A C1A -33.4(17) 21 21
C2A C3 C2A C1A 93(2) 19_556 21
C2A C3 C2A C1A 35.1(8) 7_556 21
C4 C3 C2A C2A 122(2) . 19_556
C2A C3 C2A C2A -126.1(19) 21 19_556
C2A C3 C2A C2A -58(2) 7_556 19_556
