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_7243265
_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_absolute_configuration unk
_chemical_formula_moiety         'C46 H84 O16 Ti4'
_chemical_formula_sum            'C46 H84 O16 Ti4'
_chemical_formula_weight         1084.73
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2020-04-24
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.56(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.216(6)
_cell_length_b                   19.637(5)
_cell_length_c                   23.021(11)
_cell_measurement_reflns_used    21754
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.68
_cell_measurement_wavelength     0.71073
_cell_volume                     5446(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28207
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.9297
_exptl_absorpt_correction_T_min  0.8451
_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    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.169
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0742P)^2^+7.7242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0
_reflns_number_gt                8156
_reflns_number_total             10598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09691a2.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7243265