Solvothermal synthesis and structural characterization of three polyoxotitanium-organic acid clusters
Kazimierczuk, Katarzyna; Milanesio, Marco; Dołęga, Anna; Palin, Luca; Walencik, Maja; Jurkowski, Michał; Conterosito, Eleonora; RSC Advances 11 (2021) 25068–25078; doi:10.1039/D0RA09691A

data_7243266
_publ_section_title
;
 Solvothermal synthesis and structural characterization of three
 polyoxotitanium-organic acid clusters
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              25068
_journal_page_last               25078
_journal_paper_doi               10.1039/D0RA09691A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C96 H96 O24 Ti6'
_chemical_formula_sum            'C96 H96 O24 Ti6'
_chemical_formula_weight         1921.12
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                107.574(13)
_cell_angle_beta                 92.097(13)
_cell_angle_gamma                105.434(11)
_cell_formula_units_Z            1
_cell_length_a                   12.1900(15)
_cell_length_b                   13.515(2)
_cell_length_c                   15.260(3)
_cell_measurement_reflns_used    20777
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.5
_cell_measurement_wavelength     0.71073
_cell_volume                     2291.5(7)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.98
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16107
_diffrn_reflns_point_group_measured_fraction_full 0.98
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9317
_exptl_absorpt_correction_T_min  0.8644
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
        Numerical  absorption  correction was  performed
        after the  optimization of  the  crystal-shape
        description due to Herrendorf?s method
        [Herrendorf, 1994]
        Herrendorf,  W. (1994).HABITUS, a program for the
        optimization  of  the  crystal description for
 the numerical absorption correction by means of
        suitable, psi scanned reflections;dissertation
        1994,Karlsruhe;extension 1998,Gie\&sen
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         8379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+2.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0
_reflns_number_gt                7358
_reflns_number_total             8379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09691a2.cif
_cod_data_source_block           III
_cod_original_cell_volume        2291.4(7)
_cod_database_code               7243266