Carborane isothiocyanates: synthesis, characterization and conjugation with N-nucleophiles
Alpatova, Victoria M.; Rys, Evgeny G.; Smol’yakov, Alexander F.; Kononova, Elena G.; Ol'shevskaya, Valentina A.; New Journal of Chemistry  (2026) –; doi:10.1039/D6NJ00718J

data_7064359
_publ_section_title
;
 Carborane isothiocyanates: synthesis, characterization and conjugation
 with N-nucleophiles
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6197
_journal_page_last               6204
_journal_paper_doi               10.1039/D6NJ00718J
_journal_volume                  50
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H24 B10 N2 O3 S'
_chemical_formula_sum            'C9 H24 B10 N2 O3 S'
_chemical_formula_weight         348.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-04 deposited with the CCDC.	2026-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.084(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6763(3)
_cell_length_b                   23.3782(9)
_cell_length_c                   10.1930(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.65
_cell_volume                     1828.01(12)
_computing_cell_refinement       'SAINT V8.30A (22 Oct 2012)'
_computing_data_reduction        'SAINT V8.30A (22 Oct 2012)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26505
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.999
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9547
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1360 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.9547.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7158
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0639P)^2^+0.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                6595
_reflns_number_total             7158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6nj00718j2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7064358--7064360.cif.'
_cod_database_code               7064359
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7A(H7A), C17B(H17B)
2.b Secondary CH2 refined with riding coordinates:
 C8A(H8AB,H8AA), C18B(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 N10A(H10A), N12A(H12A), N20B(H20B), N22B(H22B)
2.d Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C13B(H13A,
 H13B,H13C), C24B(H24A,H24B,H24C), C25B(H25A,H25B,H25C)
2.e Idealised tetrahedral OH refined as rotating group:
 O9A(H9A), O19B(H19B)
2.f Boron cage BH refined with riding coordinates:
 B4A(H4A), B5A(H5A), B6A(H6A), B7A(H7AA), B8A(H8A), B9A(H9AA), B10A(H10C),
 B11A(H11A), B12A(H12C), B4B(H4B), B5B(H5B), B6B(H6B), B7B(H7B), B8B(H8B),
 B9B(H9B), B10B(H10B), B11B(H11B), B12B(H12B)
;
_shelx_res_checksum              2919
_olex2_submission_special_instructions 'No special instructions were received'