Hetero-bimetallic alkali titanosilicates [MOTi{OSi(OtBu)3}3]2 (M = Li–Cs) with terminal Ti–O− groups
Pérez-Pérez, Jovana; Hernández-Balderas, Uvaldo; Martínez-Otero, Diego; Moya-Cabrera, Mónica; Jancik, Vojtech; Dalton Transactions  (2022) –; doi:10.1039/D2DT00939K

data_7709912
_publ_section_title
;
 Hetero-bimetallic alkali titanosilicates [MOTi{OSi(OtBu)3}3]2 (M =
 Li--Cs) with terminal Ti--O&#x2212; groups
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00939K
_journal_year                    2022
_chemical_formula_moiety         'C72 H162 K2 O26 Si6 Ti2'
_chemical_formula_sum            'C72 H162 K2 O26 Si6 Ti2'
_chemical_formula_weight         1786.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmalp
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6892(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9466(4)
_cell_length_b                   22.9279(6)
_cell_length_c                   16.8771(4)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.43
_cell_volume                     5112.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58214
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.655
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         11278
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+3.1650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9788
_reflns_number_total             11278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00939k2.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709912
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              37955