Investigation of titanium(IV)-oxo complexes stabilized with α-hydroxy carboxylate ligands: structural analysis and DFT studies.
Kubiak, Barbara; Muzioł, Tadeusz; Jabłoński, Mirosław; Radtke, Aleksandra; Piszczek, Piotr; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14457–14468; doi:10.1039/d4dt01710b

data_7716805
_publ_section_title
;
 Investigation of titanium(IV)-oxo complexes stabilized with
 &#x3b1;-hydroxy carboxylate ligands: structural analysis and DFT studies.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14457
_journal_page_last               14468
_journal_paper_doi               10.1039/d4dt01710b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'(Ti 4+)4, (C14 H8 O3 2-)2, (C3 H7 O 1-)10 (O 2-)'
_chemical_formula_sum            'C58 H86 O17 Ti4'
_chemical_formula_weight         1246.86
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0037(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4667(4)
_cell_length_b                   12.6262(2)
_cell_length_c                   23.0730(5)
_cell_measurement_reflns_used    13846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.2820
_cell_measurement_theta_min      3.9750
_cell_volume                     6291.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3, (Dolomanov, 2009)'
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'Olex2 1.3, (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.707
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       'tiny rhombus'
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0593P)^2^+7.5391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5499
_reflns_number_total             6404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01710b7.cif
_cod_data_source_block           nbk19-3Dshape
_cod_depositor_comments
'Adding full bibliography for 7716804--7716805.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7716805
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              40574
_shelx_hkl_checksum              24372