Structure of a Hydrated Sulfonatotitanyl(IV) Complex in Aqueous Solution and the Dimethylsulfoxide Solvated Titanyl(IV) Ion in Solution and Solid State
Daniel Lundberg; Ingmar Persson; Journal of Solution Chemistry 46 (2017) 476–487; doi:10.1007/s10953-017-0581-3

data_1548419
_publ_section_title
;
 Structure of a Hydrated Sulfonatotitanyl(IV) Complex in Aqueous Solution
 and the Dimethylsulfoxide Solvated Titanyl(IV) Ion in Solution and Solid
 State
;
_journal_name_full               'Journal of Solution Chemistry'
_journal_page_first              476
_journal_page_last               487
_journal_paper_doi               10.1007/s10953-017-0581-3
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        synthesized
_chemical_formula_moiety         'Ti O6 S5 C10 H30, 2 (C F3 S O3)'
_chemical_formula_sum            'C12 H30 F6 O12 S7 Ti'
_chemical_formula_weight         752.68
_chemical_name_common            'pentakis(dmso)oxotitanium(IV) triflate'
_chemical_name_systematic
'pentakis(dimethylsulfoxide)oxotitanium(IV) trifluoromethanesulfonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                99.002(9)
_cell_angle_beta                 110.814(8)
_cell_angle_gamma                110.231(8)
_cell_formula_units_Z            2
_cell_length_a                   10.198(5)
_cell_length_b                   13.495(6)
_cell_length_c                   13.797(6)
_cell_measurement_reflns_used    4797
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.93
_cell_volume                     1578.6(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond 2.0'
_computing_publication_material  'Diamond 2.0'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5575
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        22.984
_diffrn_reflns_theta_max         22.984
_diffrn_reflns_theta_min         1.666
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART'
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.121029
_exptl_absorpt_correction_T_min  0.054932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_recrystallization_method 'crystallized from dmso'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1597P)^2^+0.5380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3327
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Solution-Chem-2017-46-476-487.cif
_cod_data_source_block           tidmso2m
_cod_original_cell_volume        1578.5(13)
_cod_database_code               1548419
_shelx_res_checksum              41709