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_7132100
_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         'C40 H60 Cl4 O4 Ti4 [+ solvent]'
_chemical_formula_sum            'C40 H60 Cl4 O4 Ti4'
_chemical_formula_weight         938.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8466(3)
_cell_length_b                   16.8466(3)
_cell_length_c                   8.9685(3)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      70.54
_cell_measurement_theta_min      3.71
_cell_volume                     2545.33(11)
_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      297(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0721
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23304
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.453
_diffrn_reflns_theta_min         3.710
_exptl_absorpt_coefficient_mu    7.340
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.2566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 482 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0728P)^2^+2.4540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1196
_reflns_number_total             1275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03952h2.cif
_cod_data_source_block           TiY
_cod_original_cell_volume        2545.33(12)
_cod_database_code               7132100
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.206
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              60894
_shelx_hkl_checksum              71345
_shelx_fab_checksum              59263