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_7244365
_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 H14 F4 N2 O6 Zn'
_chemical_formula_sum            'C14 H14 F4 N2 O6 Zn'
_chemical_formula_weight         447.64
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-25
_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                 104.438(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5208(3)
_cell_length_b                   16.3781(5)
_cell_length_c                   12.7517(4)
_cell_measurement_reflns_used    7608
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      29.6460
_cell_measurement_theta_min      2.0670
_cell_volume                     1723.36(10)
_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     18.00  95.00   0.50    2.26    --   12.40  33.00 -58.00  154
  2  \w    -64.00  43.00   0.50    2.26    --   12.40 -33.00 142.00  214
  3  \w     62.00  88.00   0.50    2.26    --   12.40 178.00  60.00   52
  4  \w    -23.00  32.00   0.50    2.26    --  -13.03 -99.00  30.00  110
;
_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      -0.0815486000
_diffrn_orient_matrix_UB_12      -0.0137571000
_diffrn_orient_matrix_UB_13      -0.0149238000
_diffrn_orient_matrix_UB_21      0.0100663000
_diffrn_orient_matrix_UB_22      -0.0118661000
_diffrn_orient_matrix_UB_23      -0.0514243000
_diffrn_orient_matrix_UB_31      0.0251739000
_diffrn_orient_matrix_UB_32      -0.0393178000
_diffrn_orient_matrix_UB_33      0.0207292000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10354
_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         26.372
_diffrn_reflns_theta_min         2.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.267
_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    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.521
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0360P)^2^+0.9552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3159
_reflns_number_total             3511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00060a2.cif
_cod_data_source_block           kuths4-80s_dmf_1
_cod_original_cell_volume        1723.35(10)
_cod_database_code               7244365
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C64 H56 F16 O24 Zn4 '
_diffrn_oxdiff_digest_frames
;
01a6546908cc423f5d4da9c4631c9fc4ba00530abfd
;
_diffrn_oxdiff_digest_hkl
;
013f385fcfcb45a1823cd22bd96338b1df8f4e
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00L(H00L)
2.b Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00P(H00D,H00E,H00F), C00Q(H00G,H00I,H00J)
;
_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 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.742