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_7709917
_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 Cs2 O26 Si6 Ti2'
_chemical_formula_sum            'C72 H162 Cs2 O26 Si6 Ti2'
_chemical_formula_weight         1974.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 101.1948(6)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   35.3441(14)
_cell_length_b                   17.2885(8)
_cell_length_c                   26.0710(14)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.44
_cell_volume                     15627.5(13)
_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 0.997
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            231333
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.087
_diffrn_reflns_theta_min         1.592
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6223
_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    1.259
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6240
_exptl_crystal_size_max          0.611
_exptl_crystal_size_mid          0.526
_exptl_crystal_size_min          0.270
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2226
_refine_ls_number_reflns         30915
_refine_ls_number_restraints     2686
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+21.7863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28220
_reflns_number_total             30915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00939k2.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7709917
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.779
_shelx_res_checksum              39153