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_7134599
_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_formula_moiety         'C14 H13 B5 N O4 Zn, C3 H7 N O'
_chemical_formula_sum            'C17 H20 B5 N2 O5 Zn'
_chemical_formula_weight         451.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.925(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7584(4)
_cell_length_b                   13.3728(4)
_cell_length_c                   17.1991(4)
_cell_measurement_reflns_used    4792
_cell_measurement_temperature    310.00(10)
_cell_measurement_theta_max      72.2510
_cell_measurement_theta_min      4.6700
_cell_volume                     4312.00(19)
_computing_cell_refinement       'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.91a (Rigaku OD, 2025)'
_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      air
_diffrn_ambient_temperature      310.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_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    -86.00  -8.00   0.50    0.12    --  -42.10 121.00  94.00  156
  2  \w     14.00  86.00   0.50    0.12    --   42.10-121.00  12.00  144
  3  \w     14.00  89.00   0.50    0.12    --   45.00-121.00  12.00  150
  4  \w    -98.00 -31.00   0.50    0.12    -- -103.00 121.00  94.00  134
  5  \w   -174.00 -90.00   0.50    0.12    -- -103.00-121.00  12.00  168
  6  \w    -56.00 -27.00   0.50    0.12    --  -42.10 -57.00 127.19   58
  7  \w    -14.00  35.00   0.50    0.12    --  -42.10  38.00 -90.00   98
  8  \w    -14.00  35.00   0.50    0.12    --  -42.10  38.00-120.00   98
  9  \w    -14.00  35.00   0.50    0.12    --  -42.10  38.00-150.00   98
 10  \w    -14.00  35.00   0.50    0.12    --  -42.10  38.00-180.00   98
 11  \w    -14.00  35.00   0.50    0.12    --  -42.10  38.00 -30.00   98
 12  \w   -174.00 -89.00   0.50    0.12    -- -103.00 -48.00 103.54  170
 13  \w    -70.00 -29.00   0.50    0.12    -- -103.00  77.00 -30.00   82
 14  \w    -70.00 -29.00   0.50    0.12    -- -103.00  77.00-120.00   82
 15  \w    -93.00 -29.00   0.50    0.12    -- -103.00  93.00  82.91  128
 16  \w   -144.00 -88.00   0.50    0.12    -- -103.00 -19.00 -60.00  112
 17  \w   -167.00 -89.00   0.50    0.12    -- -103.00 -36.00  21.06  156
 18  \w    -93.00 -29.00   0.50    0.12    -- -103.00  93.00 -14.87  128
 19  \w    -93.00 -29.00   0.50    0.12    -- -103.00  91.00  63.80  128
 20  \w    -92.00 -30.00   0.50    0.12    -- -103.00  98.00  -5.92  124
 21  \w   -102.00 -31.00   0.50    0.12    -- -103.00 130.00   4.67  142
 22  \w    -92.00 -30.00   0.50    0.12    -- -103.00  96.00 105.53  124
 23  \w    -93.00 -29.00   0.50    0.12    -- -103.00  93.00  13.80  128
 24  \w   -144.00 -88.00   0.50    0.12    -- -103.00 -19.00 -30.00  112
 25  \w   -171.00 -99.00   0.50    0.12    -- -103.00 -77.00 120.00  144
 26  \w    -93.00 -65.00   0.50    0.12    -- -103.00  91.00  44.26   56
 27  \w   -167.00-142.00   0.50    0.12    -- -103.00 -77.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, SynergyCustom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0189545000
_diffrn_orient_matrix_UB_12      -0.0832121000
_diffrn_orient_matrix_UB_13      -0.0591021000
_diffrn_orient_matrix_UB_21      0.0034195000
_diffrn_orient_matrix_UB_22      -0.0778165000
_diffrn_orient_matrix_UB_23      0.0660713000
_diffrn_orient_matrix_UB_31      -0.0799007000
_diffrn_orient_matrix_UB_32      0.0162456000
_diffrn_orient_matrix_UB_33      0.0137017000
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20156
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.365
_diffrn_reflns_theta_min         4.061
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.91a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4172
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+1.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3180
_reflns_number_total             4172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02620b2.cif
_cod_data_source_block           scl0470_tjc_mof_vt_2_17_310_00
_cod_depositor_comments
'Adding full bibliography for 7134590--7134613.cif.'
_cod_database_code               7134599
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C16 H13 B5 N1 O4 Zn1'
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2B-C16B \\sim N2A-C16A \\sim N2A-C17A \\sim N2B-C17B
 with sigma of 0.02
 N2A-C15A \\sim N2B-C15B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, B1A, B1B, B2A, B2B, B3A, B3B, B4A, B4B, B5A, B5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N2A, N2B, C15A, C15B, C16A, C16B, C17A, C17B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N2B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(N2A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(B1B)=Sof(H1B)=Sof(B2B)=Sof(H2B)=Sof(B3B)=Sof(H3B)=Sof(B4B)=Sof(H4B)=
 Sof(B5B)=Sof(H5B)=1-FVAR(2)
 Sof(B1A)=Sof(H1A)=Sof(B2A)=Sof(H2A)=Sof(B3A)=Sof(H3A)=Sof(B4A)=Sof(H4A)=
 Sof(B5A)=Sof(H5A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14),
 C15A(H15A), C15B(H15B)
5.b Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F)
5.c Boron cage BH refined with riding coordinates:
 B1A(H1A), B1B(H1B), B2A(H2A), B2B(H2B), B3A(H3A), B3B(H3B), B4A(H4A),
 B4B(H4B), B5A(H5A), B5B(H5B)
;
_shelx_res_checksum              63486
_shelx_hkl_checksum              37824
_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 1.864
_oxdiff_exptl_absorpt_empirical_full_min 0.708