Polyoxometalate-like structure of new potassium triphenylsiloxides: [K~6~(OSiPh~3~)~6~(C~3~H~7~OH)(H~2~O)]·2C~6~H~5~CH~3~ and [K~6~(OSiPh~3~)~6~(H~2~O)~2~]
Wytrych, Patrycja; Utko, Józef; Lis, Tadeusz; John, Łukasz; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621008160

data_2022414
_publ_section_title
;
 Polyoxometalate-like structure of new potassium triphenylsiloxides:
 [K~6~(OSiPh~3~)~6~(C~3~H~7~OH)(H~2~O)]&#x00B7;2C~6~H~5~CH~3~ and
 [K~6~(OSiPh~3~)~6~(H~2~O)~2~]
;
_journal_coeditor_code           JX3064
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621008160
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[K6 (C18 H15 O Si)6 (C3 H8 O) (H2 O)], 2C7 H8'
_chemical_formula_moiety         'C111 H100 K6 O8 Si6, 2(C7 H8)'
_chemical_formula_sum            'C125 H116 K6 O8 Si6'
_chemical_formula_weight         2149.31
_chemical_name_systematic
'(\m~6~-Aqua)(\m~3~-propan-2-ol)pentakis(\m~3~-triphenylsilanolato)(\m~2~-triphenylsilanolato)hexapotassium toluene disolvate'
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                82.52(2)
_cell_angle_beta                 87.24(2)
_cell_angle_gamma                69.51(2)
_cell_formula_units_Z            2
_cell_length_a                   13.081(2)
_cell_length_b                   14.960(3)
_cell_length_c                   31.017(4)
_cell_measurement_reflns_used    43113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2.8
_cell_volume                     5637.4(18)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            97762
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2020), based on
expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.583
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1250
_refine_ls_number_reflns         20072
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0766
_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^)+(0.1182P)^2^+6.1369P], where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2207
_reflns_number_gt                15683
_reflns_number_total             20072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3064sup1.cif
_cod_data_source_block           u777a
_cod_database_code               2022414
_shelx_estimated_absorpt_t_min   0.445
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              11192
_shelx_res_checksum              69961
_shelxl_version_number           20.13
_cod_database_fobs_code 2022414