Designed additive suppresses interpenetration in IRMOF-10.
Carey, Cassidy A.; Foroughi, Leila M.; Matzger, Adam J.; Chemical communications (Cambridge, England) 60 (2024) 9396–9399; doi:10.1039/d4cc03138e

data_7133497
_publ_section_title
;
 Designed additive suppresses interpenetration in IRMOF-10.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9396
_journal_page_last               9399
_journal_paper_doi               10.1039/d4cc03138e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C42 H24 O13 Zn4'
_chemical_formula_sum            'C42 H24 O13 Zn4'
_chemical_formula_weight         998.09
_chemical_name_common            IRMOF-10
_chemical_name_systematic        IRMOF-10
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-10
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3966(2)
_cell_length_b                   34.3966(2)
_cell_length_c                   34.3966(2)
_cell_measurement_reflns_used    6231
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8300
_cell_measurement_theta_min      2.2150
_cell_volume                     40695.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -116.00 -89.00   0.50   13.08    --  -47.78-128.00 -96.00   54
  2  \w    108.00 144.00   0.50  135.75    --  104.41 129.00  31.00   72
  3  \w    -25.00  26.00   0.50   13.08    --   46.53 -19.00-120.00  102
  4  \w    -67.00 -35.00   0.50  135.75    -- -105.66  61.00-180.00   64
  5  \w    -68.00 -39.00   0.50  135.75    -- -105.66  61.00  30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016457000
_diffrn_orient_matrix_UB_12      0.0445272000
_diffrn_orient_matrix_UB_13      0.0039634000
_diffrn_orient_matrix_UB_21      -0.0327152000
_diffrn_orient_matrix_UB_22      -0.0039354000
_diffrn_orient_matrix_UB_23      0.0303557000
_diffrn_orient_matrix_UB_31      0.0305994000
_diffrn_orient_matrix_UB_32      -0.0018137000
_diffrn_orient_matrix_UB_33      0.0327100000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11527
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.571
_diffrn_reflns_theta_max         66.571
_diffrn_reflns_theta_min         2.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.326
_exptl_crystal_description       'rhombic dodecahedral'
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.026
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1566
_reflns_number_total             1824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03138e3.cif
_cod_data_source_block           cc_163a_161b
_cod_depositor_comments          'Adding full bibliography for 7133497.cif.'
_cod_original_cell_volume        40695.5(7)
_cod_database_code               7133497
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H24 O13 Zn4 '
_chemical_oxdiff_usercomment     'exchanged in hexanes'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C4(0.5) H4(0.5) C3(0.5) H3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
;
_smtbx_masks_special_details
;
    A solvent mask was calculated and 5341 electrons were found in a void volume of 34843 angstroms cubed per unit cell, this is consistent with 13 hexane molecules.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54454
_shelx_hkl_checksum              93003
_shelx_fab_checksum              94982
_olex2_exptl_crystal_mounting_method 'Shard of crystal '
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.889