Crystal structure of a rare trigonal bipyramidal titanium(IV) coordination complex: trichlorido(3,3'-di-<i>tert</i>-butyl-2'-hydroxy-5,5',6,6'-tetramethyl-1,1'-biphenyl-2-olato-κ<i>O</i>^2^)(tetrahydrofuran-κ<i>O</i>)titanium(IV)
Kim, Yun Young; Tanski, Joseph M.; Acta Crystallographica Section E 73 (2017) 88–91; doi:10.1107/S2056989016020156

data_2241994
_publ_section_title
;
 Crystal structure of a rare trigonal bipyramidal titanium(IV)
 coordination complex:
 trichlorido(3,3'-di-<i>tert</i>-butyl-2'-hydroxy-5,5',6,6'-tetramethyl-1,1'-biphenyl-2-olato-\k<i>O</i>^2^)(tetrahydrofuran-\k<i>O</i>)titanium(IV)
;
_journal_coeditor_code           RZ5202
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              88
_journal_page_last               91
_journal_paper_doi               10.1107/S2056989016020156
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ti Cl3 (C24 H33 O2)(C4 H8 O)]'
_chemical_formula_moiety         'C28 H41 Cl3 O3 Ti'
_chemical_formula_sum            'C28 H41 Cl3 O3 Ti'
_chemical_formula_weight         579.86
_chemical_name_systematic
;
trichloro(3,3'-di-<i>t</i>-butyl-2'-hydroxy-5,5',6,6'-tetramethyl-1,1'-\
biphenyl-2-ol)(tetrahydrofuran)titanium(IV)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 95.164(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.289(4)
_cell_length_b                   7.141(3)
_cell_length_c                   40.330(16)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    125.(2)
_cell_measurement_theta_max      28.8923
_cell_measurement_theta_min      2.3111
_cell_volume                     2951(2)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008), <i>OLEX2</i> (Dolomanov <i>et al.</i>,
2009) and
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_structure_refinement
;
<i>SHELXL2014/6</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.1562
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            76791
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.553
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3136 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         17956
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                10069
_reflns_number_total             17956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5202sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2951.(2)
_cod_database_code               2241994
_shelx_hkl_checksum              37465
_shelx_res_checksum              1194
_cod_database_fobs_code 2241994