Preparation and Crystal Structures of a Series of Titanium(III) 9-BBN Hydroborate Complexes Containing Ti...H Agostic Interactions
Errun Ding; Bin Du; Fu-Chen Liu; Shengming Liu; Edward A. Meyers; Sheldon G. Shore; Inorganic Chemistry 44 (2005) 4871–4878; doi:10.1021/ic050422f

data_4309128
_publ_section_title
;
Preparation and Crystal Structures of a Series of Titanium(III) 9-BBN
Hydroborate Complexes Containing Ti...H Agostic Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4871
_journal_page_last               4878
_journal_paper_doi               10.1021/ic050422f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C28 H58 B3 O Ti'
_chemical_formula_weight         491.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3535(10)
_cell_length_b                   13.5503(10)
_cell_length_c                   21.6302(10)
_cell_measurement_temperature    200(2)
_cell_volume                     5965.5(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50239
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9223
_exptl_absorpt_correction_T_min  0.9115
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3492
_reflns_number_total             5242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050422fsi20050321_092335_2.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-09-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C20.36 H42.18 B2.18 O0.73 Ti0.73'
_cod_original_formula_weight         357.14
_cod_original_formula_units_Z            11
_cod_database_code               4309128