Uncommon quadruple stacking topology in a honeycomb-sheet MOF compatible with through-space conduction
Tanabe, Tappei; Qu, Liyuan; Ueno, Kenta; Takaishi, Shinya; Yamashita, Masahiro; Hijikata, Yuh; Matsuda, Ryotaro; Sakamoto, Ryota; Iguchi, Hiroaki; Chemical Communications 61 (2025) 9500–9503; doi:10.1039/D5CC00084J

data_7134584
_publ_section_title
;
 Uncommon quadruple stacking topology in a honeycomb-sheet MOF compatible
 with through-space conduction
;
_journal_issue                   52
_journal_name_full               'Chemical Communications'
_journal_page_first              9500
_journal_page_last               9503
_journal_paper_doi               10.1039/D5CC00084J
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C36 H20.88 Br0.56 Cd N6 O8.44, 2[C4H9NO], 2[H2O], 1[C5H9N]'
_chemical_formula_sum            'C49 H51.88 Br0.56 Cd N9 O12.44'
_chemical_formula_weight         1123.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-17 deposited with the CCDC.	2025-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   9.679(5)
_cell_length_b                   36.891(6)
_cell_length_c                   54.555(13)
_cell_measurement_reflns_used    15655
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.871
_cell_measurement_theta_min      1.688
_cell_volume                     19480(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Hybrid-photon-counting detector'
_diffrn_detector_type            'Dectris Eiger X16M'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'single-axis diffractometer'
_diffrn_measurement_device_type  KEK_PF_BL17A
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.900
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            53196
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        32.684
_diffrn_reflns_theta_max         33.871
_diffrn_reflns_theta_min         2.795
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK PF beamline BL-17A'
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             9216
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.595
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4749
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.604
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.1112
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3577
_refine_ls_wR_factor_ref         0.3635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4081
_reflns_number_total             4749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00084j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7134584.cif.'
_cod_original_cell_volume        19480(11)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7134584
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H,H) groups
2. Restrained distances
 Cd1-O4 \\sim Cd1-O6 \\sim Cd1-O4A
 with sigma of 0.01
 Cd1-O4 \\sim Cd1-O4A
 with sigma of 0.01
 Cd1-O4 \\sim Cd1-O4A \\sim Cd1-O5 \\sim Cd1-O6
 with sigma of 0.01
3. Rigid bond restraints
 C9, C10, Cd1, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O4A) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) = Uanis(O4A)
Uanis(O5) = Uanis(Br1)
Uanis(Br1) = Uanis(O5) = Uanis(O6)
5. Others
 Fixed Sof: Br1(0.28) O4(0.28) O5(0.44) H5A(0.44) O4A(0.22) O6(0.28) H6A(0.28)
 H5B(0.44) H6B(0.28)
6.a Riding coordinates:
 O5(H5A), O6(H6A,H5B,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C7(H7), C2(H2), C1(H1), C9(H9), C11(H11), C12(H12), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47671
_shelx_hkl_checksum              39918
_shelx_fab_checksum              23407
_olex2_submission_special_instructions 'No special instructions were received'