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#$Date: 2019-11-25 13:50:23 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241018 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/06/4130625.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_4130625
loop_
_publ_author_name
'Bhatt, Prashant M.'
'Belmabkhout, Youssef'
'Cadiau, Amandine'
'Adil, Karim'
'Shekhah, Osama'
'Shkurenko, Aleksander'
'Barbour, Leonard J.'
'Eddaoudi, Mohamed'
_publ_section_title
;
 A Fine-Tuned Fluorinated MOF Addresses the Needs for Trace CO2 Removal
 and Air Capture Using Physisorption.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9301
_journal_page_last               9307
_journal_paper_doi               10.1021/jacs.6b05345
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'Ni Nb O F5 (C4 H4 N2)2, 2(O H2)'
_chemical_formula_sum            'C8 H12 F5 N4 Nb Ni O3'
_chemical_formula_weight         458.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.943(4)
_cell_length_b                   9.943(4)
_cell_length_c                   15.764(6)
_cell_measurement_reflns_used    1674
_cell_measurement_temperature    295.5(1)
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      2.90
_cell_volume                     1558.5(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.5(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3163
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.014
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.6474.
The λ/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0325
_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)+(0.0377P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                225
_reflns_number_total             396
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b05345_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1558(1)
_cod_database_code               4130625
_shelx_shelxl_version_number     2014/7
_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   0.924
_shelx_estimated_absorpt_t_max   0.942
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -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'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, 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'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+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
Nb1 Nb 0.0000 0.0000 0.0000 0.0278(4) Uani 1 8 d S T P . .
Ni1 Ni 0.0000 0.0000 0.2500 0.0113(4) Uani 1 8 d S T P . .
F1 F 0.0000 0.0000 0.1231(4) 0.0225(10) Uani 0.5 4 d S T P A .
O1 O 0.0000 0.0000 0.1231(4) 0.0225(10) Uani 0.5 4 d S T P A .
F2 F 0.0080(7) 0.1908(4) 0.0000 0.0742(17) Uani 1 2 d S T P A 1
N1 N 0.1514(3) 0.1514(3) 0.2500 0.0165(10) Uani 1 2 d S T P A .
C1A C 0.2421(4) 0.1601(5) 0.3120(3) 0.0257(11) Uani 1 1 d . . . A 1
H1A H 0.2392 0.0985 0.3564 0.031 Uiso 1 1 calc R U . A 1
O1W O 0.4171(17) -0.0829(17) 0.4233(14) 0.168(10) Uani 0.5 2 d S T 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'
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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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 . 17
F2 Nb1 F2 90.0 . 18
F2 Nb1 F2 90.0 17 18
F2 Nb1 F2 90.0 . 2
F2 Nb1 F2 90.0 17 2
F2 Nb1 F2 180.000(10) 18 2
F2 Nb1 F1 90.0 . .
F2 Nb1 F1 90.0 17 .
F2 Nb1 F1 90.0 18 .
F2 Nb1 F1 90.0 2 .
F2 Nb1 O1 90.0 . 17
F2 Nb1 O1 90.0 17 17
F2 Nb1 O1 90.0 18 17
F2 Nb1 O1 90.0 2 17
F1 Nb1 O1 180.0 . 17
F2 Nb1 F1 90.0 . 17
F2 Nb1 F1 90.0 17 17
F2 Nb1 F1 90.0 18 17
F2 Nb1 F1 90.0 2 17
F1 Nb1 F1 180.0 . 17
O1 Nb1 F1 0.0 17 17
O1 Ni1 F1 0.0 5 5
O1 Ni1 F1 180.0 5 .
F1 Ni1 F1 180.0 5 .
O1 Ni1 N1 90.0 5 3
F1 Ni1 N1 90.0 5 3
F1 Ni1 N1 90.0 . 3
O1 Ni1 N1 90.0 5 .
F1 Ni1 N1 90.0 5 .
F1 Ni1 N1 90.0 . .
N1 Ni1 N1 180.0(2) 3 .
O1 Ni1 N1 90.0 5 4
F1 Ni1 N1 90.0 5 4
F1 Ni1 N1 90.0 . 4
N1 Ni1 N1 90.0 3 4
N1 Ni1 N1 90.0 . 4
O1 Ni1 N1 90.0 5 2
F1 Ni1 N1 90.0 5 2
F1 Ni1 N1 90.0 . 2
N1 Ni1 N1 90.0 3 2
N1 Ni1 N1 90.0 . 2
N1 Ni1 N1 180.0 4 2
Nb1 F1 Ni1 180.0 . .
C1A N1 C1A 116.7(5) 7 .
C1A N1 Ni1 121.6(2) 7 .
C1A N1 Ni1 121.6(2) . .
N1 C1A C1A 121.6(2) . 31
N1 C1A H1A 119.2 . .
C1A C1A H1A 119.2 31 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 F2 1.899(4) .
Nb1 F2 1.899(4) 17
Nb1 F2 1.899(4) 18
Nb1 F2 1.899(4) 2
Nb1 F1 1.941(6) .
Nb1 O1 1.941(6) 17
Nb1 F1 1.941(6) 17
Ni1 O1 2.000(6) 5
Ni1 F1 2.000(6) 5
Ni1 F1 2.000(6) .
Ni1 N1 2.128(4) 3
Ni1 N1 2.128(4) .
Ni1 N1 2.128(4) 4
Ni1 N1 2.128(4) 2
N1 C1A 1.333(5) 7
N1 C1A 1.333(5) .
C1A C1A 1.375(8) 31
C1A H1A 0.9300 .
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
C1A N1 C1A C1A -0.003(1) 7 31
Ni1 N1 C1A C1A 179.999(1) . 31
