Unusual ligand substitution of a metal-organic framework with distorted metal–ligand coordination
Sakamoto, Hikaru; Ito, Akitaka; Ohtani, Masataka; CrystEngComm  (2022) –; doi:10.1039/D2CE00060A

data_7244366
_publ_section_title
;
 Unusual ligand substitution of a metal-organic framework with distorted
 metal--ligand coordination
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00060A
_journal_year                    2022
_chemical_formula_moiety         'C14 H18 F4 N2 O8 Zn'
_chemical_formula_sum            'C16 H14 F4 N0.5 O8 Zn'
_chemical_formula_weight         482.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-12-10 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.568(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.2395(3)
_cell_length_b                   10.1581(5)
_cell_length_c                   16.8889(11)
_cell_measurement_reflns_used    2760
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      29.9840
_cell_measurement_theta_min      2.4100
_cell_volume                     894.64(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_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_temperature      93.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -98.00  35.00   0.50   52.74    --  -13.34  -5.00  58.00  266
  2  \w     38.00  68.00   0.50   52.74    --  -13.34  -5.00  58.00   60
  3  \w    -19.00   7.00   0.50   52.74    --   12.72 -99.00-120.00   52
  4  \w     29.00  55.00   0.50   52.74    --   12.72 -99.00-120.00   52
  5  \w    -23.00  31.00   0.50   52.74    --  -13.34 -99.00-180.00  108
  6  \w     47.00  84.00   0.50   52.74    --   12.72 178.00-150.00   74
  7  \w    -91.00 -65.00   0.50   52.74    --  -13.34 178.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0799204000
_diffrn_orient_matrix_UB_12      -0.0039796000
_diffrn_orient_matrix_UB_13      0.0363694000
_diffrn_orient_matrix_UB_21      -0.1097774000
_diffrn_orient_matrix_UB_22      0.0021401000
_diffrn_orient_matrix_UB_23      0.0214054000
_diffrn_orient_matrix_UB_31      -0.0079394000
_diffrn_orient_matrix_UB_32      -0.0696490000
_diffrn_orient_matrix_UB_33      -0.0013424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       plate
_exptl_crystal_F_000             487
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0412P)^2^+1.0166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1527
_reflns_number_total             1832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00060a2.cif
_cod_data_source_block           kuths4-129c_2
_cod_original_formula_sum        'C16 H14 F4 N0.50 O8 Zn'
_cod_database_code               7244366
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H12 F4 O8 Zn1'
_diffrn_oxdiff_digest_frames
;
010819a8df30c456fa1f847062b5666110006644d7e
;
_diffrn_oxdiff_digest_hkl
;
0136a844373cfa2feb0bd80289acd1fa4abc95
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.863