Face-directed assembly of tailored isoreticular MOFs using centring structure-directing agents
Barsukova, Marina; Sapianik, Aleksandr; Guillerm, Vincent; Shkurenko, Aleksander; Shaikh, Aslam C.; Parvatkar, Prakash; Bhatt, Prashant M.; Bonneau, Mickaele; Alhaji, Abdulhadi; Shekhah, Osama; Balestra, Salvador R. G.; Semino, Rocio; Maurin, Guillaume; Eddaoudi, Mohamed; Nature Synthesis  (2023) 1–; doi:10.1038/s44160-023-00401-8

data_1570032
_publ_section_title
;
 Face-directed assembly of tailored isoreticular MOFs using centring
 structure-directing agents
;
_journal_name_full               'Nature Synthesis'
_journal_page_first              1
_journal_paper_doi               10.1038/s44160-023-00401-8
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety
'(In3 O (C24 H12 N3 O6)2 (C51 H36 N4)0.67 Br0.6 (H2 O)0.4 0.4+), 0.4(Br 1-)'
_chemical_formula_sum            'C82 H48.8 Br In3 N8.67 O13.4'
_chemical_formula_weight         1794.20
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   56.942(1)
_cell_length_b                   56.942(1)
_cell_length_c                   56.942(1)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.49
_cell_measurement_theta_min      2.45
_cell_volume                     184628(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            41496
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        29.390
_diffrn_reflns_theta_max         29.390
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  0.0894
_exptl_absorpt_correction_T_min  0.0423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.4732.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.387
_exptl_crystal_description       'rhombic dodecahedron'
_exptl_crystal_F_000             21376
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         4516
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1296P)^2^+604.5647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3347
_reflns_number_total             4516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            44160_2023_401_MOESM12_ESM.cif
_cod_data_source_block           In-sod-ZMOF-307
_cod_original_cell_volume        184630(10)
_cod_original_formula_sum        'C82 H48.80 Br In3 N8.67 O13.40'
_cod_database_code               1570032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.781
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              62055
_shelx_hkl_checksum              23431
_shelx_fab_checksum              31763