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_7244367
_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         'C16 H2.88 F5.12 O8 Zn2'
_chemical_formula_sum            'C16 H2.88 F5.12 O8 Zn2'
_chemical_formula_weight         551.04
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-01
_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                 100.241(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8857(7)
_cell_length_b                   4.77750(10)
_cell_length_c                   25.5982(8)
_cell_measurement_reflns_used    6355
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      30.0820
_cell_measurement_theta_min      2.0210
_cell_volume                     1671.10(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -19.00   6.00   0.50   82.86    --   12.40 -89.00  79.00   50
  2  \w    -40.00  15.00   0.50   82.86    --  -13.03 -89.00  79.00  110
  3  \w    -15.00  60.00   0.50   82.86    --  -13.03  57.00-120.00  150
  4  \w    -53.00   0.00   0.50   82.86    --  -13.03  89.00-164.00  106
  5  \w     55.00  95.00   0.50   82.86    --   12.40 178.00 120.00   80
  6  \w    -93.00 -58.00   0.50   82.86    --  -13.03-178.00-120.00   70
;
_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      0.0386140000
_diffrn_orient_matrix_UB_12      -0.0990998000
_diffrn_orient_matrix_UB_13      0.0029727000
_diffrn_orient_matrix_UB_21      0.0294305000
_diffrn_orient_matrix_UB_22      0.0908606000
_diffrn_orient_matrix_UB_23      0.0181155000
_diffrn_orient_matrix_UB_31      -0.0182254000
_diffrn_orient_matrix_UB_32      -0.0632169000
_diffrn_orient_matrix_UB_33      0.0213555000
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10283
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.975
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.484
_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    2.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.583
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0637P)^2^+5.3940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2922
_reflns_number_total             3382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00060a2.cif
_cod_data_source_block           kuths4-129b_3
_cod_database_code               7244367
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 F48 O20 Zn8 H1 '
_diffrn_oxdiff_digest_frames
;
011fe740f7eb75914938ad6a4490fbcf8b00566bfcf
;
_diffrn_oxdiff_digest_hkl
;
011b8b1639caae29b9a47e86dad3372d8ab6da
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(H00N)=Sof(H00S)=Sof(H00U)=Sof(H00V)=1-FVAR(1)
 Sof(F00M)=Sof(F00Q)=Sof(F00W)=Sof(F00X)=FVAR(1)
 Sof(H00K)=Sof(H00O)=Sof(H00P)=Sof(H00R)=1-FVAR(2)
 Sof(F00I)=Sof(F00J)=Sof(F00T)=Sof(F00Y)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C00O(H00O), C00P(H00P), C00R(H00R), C00S(H00S),
 C00U(H00U), C00V(H00V)
;
_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 1.680
_oxdiff_exptl_absorpt_empirical_full_min 0.585