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_7709916
_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         'C40 H91 N O12 Si3 Ti'
_chemical_formula_sum            'C40 H91 N O12 Si3 Ti'
_chemical_formula_weight         910.30
_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   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                90
_cell_angle_beta                 105.4661(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5226(8)
_cell_length_b                   21.9475(13)
_cell_length_c                   19.2826(12)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.38
_cell_volume                     5515.6(6)
_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 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82469
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.099
_diffrn_reflns_theta_min         1.652
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6256
_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            Yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.356
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10935
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0438P)^2^+2.8132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9517
_reflns_number_total             10935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00939k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709916
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              23198