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_4127291
_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, C1.5 H5'
_chemical_formula_sum            'C29 H22 Cu2 F2 N2 O8'
_chemical_formula_weight         691.59
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.493(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5743(7)
_cell_length_b                   10.6558(7)
_cell_length_c                   15.2273(12)
_cell_measurement_reflns_used    3694
_cell_measurement_temperature    298(20)
_cell_measurement_theta_max      73.6900
_cell_measurement_theta_min      5.1100
_cell_volume                     1627.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298(20)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.963
_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    -27.00  19.00   0.50    6.92    --    0.00  82.00-180.00   92
  2  \w      5.00  48.00   0.50    6.92    --    0.00  77.00   0.00   86
  3  \w      2.00  29.00   0.50    6.92    --    0.00  38.00  90.00   54
  4  \w    -19.00  34.00   0.50    6.92    --    0.00  82.00 -90.00  106
  5  \w    -31.00  32.00   0.50    6.92    --    0.00  82.00  60.00  126
  6  \w    155.00 180.00   0.50   27.67    --   94.30  82.00-120.00   50
  7  \w     11.00  94.00   0.50   27.67    --   94.30 -61.00 -60.00  166
  8  \w    112.00 183.00   0.50   27.67    --   94.30  82.00 120.00  142
  9  \w     77.00 156.00   0.50   27.67    --   94.30  45.00  90.00  158
 10  \w    113.00 160.00   0.50   27.67    --   94.30  82.00  90.00   94
 11  \w     13.00 105.00   0.50   27.67    --   94.30 -61.00-150.00  184
 12  \w    106.00 184.00   0.50   27.67    --   94.30  77.00 -30.00  156
 13  \w     80.00 173.00   0.50   27.67    --   94.30  45.00  60.00  186
;
_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      0.1476279000
_diffrn_orient_matrix_UB_12      -0.0325765000
_diffrn_orient_matrix_UB_13      0.0489599000
_diffrn_orient_matrix_UB_21      0.0425584000
_diffrn_orient_matrix_UB_22      0.1164470000
_diffrn_orient_matrix_UB_23      -0.0435823000
_diffrn_orient_matrix_UB_31      -0.0020351000
_diffrn_orient_matrix_UB_32      0.0793197000
_diffrn_orient_matrix_UB_33      0.0841168000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8741
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.210
_diffrn_reflns_theta_min         4.409
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.131
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.696
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.1033
_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/[\s^2^(Fo^2^)+(0.1510P)^2^+22.0089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3179
_refine_ls_wR_factor_ref         0.3438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2072
_reflns_number_total             3197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NKU-FlexMOF-1a-C3H8.cif
_cod_data_source_block           NKU-FlexMOF-1a-C3H8
_cod_database_code               4127291
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.303
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Others
 Fixed Sof: C00L(0.5) H00A(0.5) H00B(0.5) H00C(0.5) C00M(0.5) H00D(0.5)
 H00E(0.5) H00K(0.5) C1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J)
3.c Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00C), C00M(H00D,H00E,H00K)
;
_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 2.620
_oxdiff_exptl_absorpt_empirical_full_min 0.523