Crystal structure and computational study of an oxo-bridged bis-titanium(III) complex
Bloomfield, Hannah R.; Hollett, Joshua W.; Ritch, Jamie S.; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621006094

data_2022394
_publ_section_title
;
 Crystal structure and computational study of an oxo-bridged
 bis-titanium(III) complex
;
_journal_coeditor_code           DG3018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621006094
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ti2 Cl4 O (C4 H8 O)6]'
_chemical_formula_moiety         'C24 H48 Cl4 O7 Ti2'
_chemical_formula_sum            'C24 H48 Cl4 O7 Ti2'
_chemical_formula_weight         686.22
_chemical_name_systematic
;
\m-Oxido-bis[dichloridotris(tetrahydrofuran-\k<i>O</i>)titanium(III)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 102.092(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1347(5)
_cell_length_b                   9.1227(3)
_cell_length_c                   18.7937(5)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.48
_cell_volume                     3207.84(16)
_computing_cell_refinement
;
APEX2 (Bruker, 2016)
;
_computing_data_collection
;
SAINT (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.607
_diffrn_reflns_theta_min         2.484
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.6779
_exptl_absorpt_correction_T_min  0.5622
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.277
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.412
_refine_ls_extinction_coef       0.00039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXT2018 (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+30.5697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                3244
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dg3018sup1.cif
_cod_data_source_block           I
_cod_database_code               2022394
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.795
_shelx_hkl_checksum              73502
_shelx_res_checksum              17936
_cod_database_fobs_code 2022394