16-vertex Oblato-Hypho-Titanaborane [(Cp*Ti)2B14H18]
Kar, Sourav; Bairagi, Subhash; Halet, Jean-François; Ghosh, Sundargopal; Chemical Communications  (2023) –; doi:10.1039/D3CC03952H

data_7132101
_publ_section_title
;
 16-vertex Oblato-Hypho-Titanaborane [(Cp*Ti)2B14H18]
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03952H
_journal_year                    2023
_chemical_formula_moiety         'C21 H50 B14 Ti2'
_chemical_formula_sum            'C21 H50 B14 Ti2'
_chemical_formula_weight         549.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.344(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4697(7)
_cell_length_b                   15.0305(11)
_cell_length_c                   20.0992(15)
_cell_measurement_reflns_used    7979
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      69.21
_cell_measurement_theta_min      2.94
_cell_volume                     3077.5(4)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Bruker D8 VENTURE diffractometer with PHOTON II detector'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34523
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.688
_diffrn_reflns_theta_min         3.709
_exptl_absorpt_coefficient_mu    4.458
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.4452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1132P)^2^+1.1140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.2229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3082
_reflns_number_total             5704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03952h2.cif
_cod_data_source_block           Ti
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.825
_shelx_res_checksum              45594
_shelx_hkl_checksum              66617