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_7709910
_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         'C24 H54 O9 Si3'
_chemical_formula_sum            'C24 H54 O9 Si3'
_chemical_formula_weight         570.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                100.242(2)
_cell_angle_beta                 109.429(2)
_cell_angle_gamma                90.071(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6208(6)
_cell_length_b                   11.9586(6)
_cell_length_c                   14.0651(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.00
_cell_measurement_theta_min      3.76
_cell_volume                     1654.32(16)
_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-2019/2 (Sheldrick, 2019)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6116
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.117
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.753298
_exptl_absorpt_correction_T_min  0.593859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1, Sheldrick'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       Prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.562
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0544P)^2^+0.2940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5682
_reflns_number_total             6116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00939k2.cif
_cod_data_source_block           TS
_cod_database_code               7709910
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.453
_shelx_estimated_absorpt_t_max   0.845
_shelx_res_checksum              14443