Hypoelectronic titanaboranes: icosahedral and tetracapped tetrahedral clusters comprising bridging hydrides.
Bairagi, Subhash; Chatterjee, Debipada; Giri, Soumen; Ghosh, Sundargopal; Chemical communications (Cambridge, England) 61 (2025) 3696–3699; doi:10.1039/d4cc06535b

data_7134211
_publ_section_title
;
 Hypoelectronic titanaboranes: icosahedral and tetracapped tetrahedral
 clusters comprising bridging hydrides.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3696
_journal_page_last               3699
_journal_paper_doi               10.1039/d4cc06535b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C30 H53 B9 Cl2 Ti3'
_chemical_formula_weight         725.61
_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   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2436(17)
_cell_length_b                   11.5096(10)
_cell_length_c                   18.5384(16)
_cell_measurement_reflns_used    6884
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      2.8
_cell_volume                     3679.3(6)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      302(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Apex3 CMOS Diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34607
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        20.834
_diffrn_reflns_theta_max         20.834
_diffrn_reflns_theta_min         3.540
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1489 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     335
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+9.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3611
_reflns_number_total             3851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06535b2.cif
_cod_data_source_block           TI3G
_cod_depositor_comments
'Adding full bibliography for 7134210--7134212.cif.'
_cod_database_code               7134211
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              26293
_shelx_hkl_checksum              52081