A new carborane scaffold for assembling metal–organic frameworks
Windsor, Hunter J.; Carraro, Thomas J. C.; Walwyn, Robert J.; Rendina, Louis M.; Kepert, Cameron J.; Chemical Communications 61 (2025) 9634–9637; doi:10.1039/D5CC02620B

data_7134607
_publ_section_title
;
 A new carborane scaffold for assembling metal--organic frameworks
;
_journal_issue                   53
_journal_name_full               'Chemical Communications'
_journal_page_first              9634
_journal_page_last               9637
_journal_paper_doi               10.1039/D5CC02620B
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C7 H15 B10 N'
_chemical_formula_sum            'C7 H15 B10 N'
_chemical_formula_weight         221.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5733(2)
_cell_length_b                   11.9319(2)
_cell_length_c                   7.21180(10)
_cell_measurement_reflns_used    6754
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1700
_cell_measurement_theta_min      4.7340
_cell_volume                     1254.04(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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    -32.00  24.00   0.50    0.20    --   45.00 -38.00-150.00  112
  2  \w     18.00  93.00   0.50    0.20    --   45.00-127.00   4.00  150
  3  \w     18.00  93.00   0.50    0.20    --   45.00-127.00   4.00  150
  4  \w     32.00 122.00   0.50    0.20    --   45.00  38.00   0.00  180
  5  \w     32.00 122.00   0.50    0.20    --   45.00  38.00   0.00  180
  6  \w    -90.00 -12.00   0.50    0.20    --  -41.71 127.00  80.00  156
  7  \w    -92.00 -29.00   0.50    0.80    -- -103.00 101.00  64.25  126
  8  \w    -90.00 -65.00   0.50    0.80    -- -103.00 127.00  80.00   50
  9  \w    -92.00 -30.00   0.50    0.80    -- -103.00  97.00  90.03  124
 10  \w    -93.00 -29.00   0.50    0.80    -- -103.00  93.00  32.52  128
 11  \w    -97.00 -31.00   0.50    0.80    -- -103.00 114.00 -12.56  132
 12  \w    -58.00 -32.00   0.50    0.80    -- -103.00 126.00-120.00   52
 13  \w   -101.00 -53.00   0.50    0.80    -- -103.00 126.00-120.00   96
 14  \w    -93.00 -29.00   0.50    0.80    -- -103.00  91.00  -9.07  128
 15  \w    -93.00 -60.00   0.50    0.80    -- -103.00  91.00 127.02   66
 16  \w    -70.00 -29.00   0.50    0.80    -- -103.00  77.00  60.00   82
 17  \w    -14.00  36.00   0.50    0.20    --  -41.71  38.00-120.00  100
 18  \w    -14.00  36.00   0.50    0.20    --  -41.71  38.00-180.00  100
 19  \w    -70.00 -44.00   0.50    0.80    -- -103.00  77.00 -60.00   52
 20  \w    -70.00 -29.00   0.50    0.80    -- -103.00  77.00 -30.00   82
 21  \w   -129.00 -88.00   0.50    0.80    -- -103.00 -19.00  60.00   82
 22  \w   -172.00 -89.00   0.50    0.80    -- -103.00 -43.00  80.22  166
 23  \w   -172.00 -89.00   0.50    0.80    -- -103.00 -43.00  80.22  166
 24  \w   -144.00 -88.00   0.50    0.80    -- -103.00 -19.00  30.00  112
 25  \w   -144.00 -88.00   0.50    0.80    -- -103.00 -19.00 -60.00  112
 26  \w   -144.00 -99.00   0.50    0.80    -- -103.00 -19.00-120.00   90
 27  \w   -174.00 -87.00   0.50    0.80    -- -103.00-127.00   4.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0046946000
_diffrn_orient_matrix_UB_12      0.0954306000
_diffrn_orient_matrix_UB_13      0.1436681000
_diffrn_orient_matrix_UB_21      -0.0148721000
_diffrn_orient_matrix_UB_22      0.0867331000
_diffrn_orient_matrix_UB_23      -0.1552932000
_diffrn_orient_matrix_UB_31      -0.1045548000
_diffrn_orient_matrix_UB_32      -0.0080050000
_diffrn_orient_matrix_UB_33      0.0284696000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11633
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.350
_diffrn_reflns_theta_min         4.790
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
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            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0640P)^2^+0.2288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.899
_reflns_number_gt                2257
_reflns_number_total             2346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02620b2.cif
_cod_data_source_block           cjk24_scl0355_hw_tjc_p-cb_20240923_2
_cod_depositor_comments
'Adding full bibliography for 7134590--7134613.cif.'
_cod_database_code               7134607
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C7 H15 B10 N1 '
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9(5)
 0.1(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
3.b Boron cage BH refined with riding coordinates:
 C2(H2), B1(H1), B2(H2A), B3(H3), B4(H4A), B5(H5A), B6(H6A), B7(H7A), B8(H8),
 B9(H9), B10(H10)
;
_shelx_res_checksum              60967
_shelx_hkl_checksum              71888
_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 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.328