A 14-Vertex Bud-Shaped [(Cp*Ti)2B12H18] Cluster
Bairagi, Subhash; Chatterjee, Debipada; Patel, Deepak Kumar; Acharya, Swetashree; Ghosh, Sundargopal; Dalton Transactions  (2026) –; doi:10.1039/D5DT03098F

data_7720692
_publ_section_title
;
 A 14-vertex bud-shaped [(Cp*Ti)<sub>2</sub>B<sub>12</sub>H<sub>18</sub>]
 cluster.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5437
_journal_page_last               5442
_journal_paper_doi               10.1039/d5dt03098f
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'(C20 H46 B15 S Ti2) + (C6 H14) + 0.5(C H2 Cl2)'
_chemical_formula_sum            'C26.5 H51 B15 Cl S Ti2'
_chemical_formula_weight         695.13
_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
;
2026-02-05 deposited with the CCDC.	2026-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.441(3)
_cell_length_b                   9.5780(9)
_cell_length_c                   14.6840(13)
_cell_measurement_reflns_used    6484
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      2.8
_cell_volume                     4000.0(7)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Axs Kappa Apex3 CMOS Diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27503
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.998
_diffrn_reflns_theta_max         22.998
_diffrn_reflns_theta_min         2.638
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
The solvents used for crystallisation were hexane and DCM. 
The difference Fourier Map after the refinement of the main molecule 
showed a lot of peaks above 1 electrons per angstrom^3. 
However, the peaks could not be modelled to meaningful solvent 
molecules. Hence, it was decided to squeeze the data using the 
program PLATON. The squeeze results show removal of 71 electrons 
per asymmetric unit. This amounts to the number of electrons 
of 1 hexane +1/2 DCM. The squeezed solvent content is added 
to the formula unit.
;
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.59(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     955
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+22.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.2713
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4285
_reflns_number_total             5561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03098f2.cif
_cod_data_source_block           TIB84
_cod_depositor_comments
'Adding full bibliography for 7720692--7720694.cif.'
_cod_original_cell_volume        4000.0(6)
_cod_original_formula_sum        'C26.50 H51 B15 Cl S Ti2'
_cod_database_code               7720692
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.979
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              28822
_shelx_hkl_checksum              76802
_shelx_fab_checksum              7533