Enhanced Gas Uptake in a Microporous Metal-Organic Framework <i>via</i> a Sorbate Induced-Fit Mechanism.
Yu, Mei-Hui; Space, Brian; Franz, Douglas; Zhou, Wei; He, Chaohui; Li, Libo; Krishna, Rajamani; Chang, Ze; Li, Wei; Hu, Tong-Liang; Bu, Xian-He; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b07807

data_4127289
_publ_section_title
;
 Enhanced Gas Uptake in a Microporous Metal-Organic Framework <i>via</i> a
 Sorbate Induced-Fit Mechanism.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b07807
_journal_year                    2019
_chemical_formula_moiety         'C13 H6 Cu F N O4, 3(N2)'
_chemical_formula_sum            'C13 H6 Cu F N7 O4'
_chemical_formula_weight         406.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.254(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5629(2)
_cell_length_b                   11.3332(2)
_cell_length_c                   14.6254(3)
_cell_measurement_reflns_used    5491
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.8310
_cell_measurement_theta_min      5.9130
_cell_volume                     1662.72(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -17.00  10.00   0.50    2.50    --    0.00 -57.00 -60.00   54
  2  \w     11.00 113.00   0.50    5.00    --   94.90 -30.00 150.00  204
  3  \w     89.00 160.00   0.50    5.00    --   94.90  45.00   0.00  142
  4  \w    146.00 174.00   0.50    5.00    --   94.90  77.00 -90.00   56
  5  \w    110.00 142.00   0.50    5.00    --   94.90  77.00 -90.00   64
  6  \w     69.00 132.00   0.50    5.00    --   94.90  61.00  60.00  126
  7  \w     47.00 127.00   0.50    5.00    --   94.90 -82.00 -90.00  160
  8  \w      7.00  95.00   0.50    5.00    --   94.90 -61.00  90.00  176
  9  \w      9.00  34.00   0.50    5.00    --   94.90 -82.00 -90.00   50
 10  \w      6.00 103.00   0.50    5.00    --   94.90 -30.00 -90.00  194
 11  \w    -10.00  18.00   0.50    2.50    --    0.00  82.00   0.00   56
 12  \w    -87.00 -30.00   0.50    2.50    --    0.00 -38.00-120.00  114
 13  \w    -89.00 -24.00   0.50    2.50    --    0.00 -57.00 -60.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1018549000
_diffrn_orient_matrix_UB_12      0.0510945000
_diffrn_orient_matrix_UB_13      0.0450653000
_diffrn_orient_matrix_UB_21      0.1026041000
_diffrn_orient_matrix_UB_22      -0.0122792000
_diffrn_orient_matrix_UB_23      0.1009349000
_diffrn_orient_matrix_UB_31      0.0518516000
_diffrn_orient_matrix_UB_32      0.1253883000
_diffrn_orient_matrix_UB_33      -0.0085201000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9425
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.581
_diffrn_reflns_theta_min         4.408
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.117
_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     235
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+4.1854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2815
_reflns_number_total             3283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NKU-FlexMOF-1a-N2-b.cif
_cod_data_source_block           NKU-FlexMOF-1a-N2-b
_cod_database_code               4127289
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I), C00K(H00K)
;
_shelx_res_checksum              44318
_shelx_hkl_checksum              1564
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.452
_oxdiff_exptl_absorpt_empirical_full_min 0.723