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_2022415
_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 (H2 O)2]'
_chemical_formula_moiety         'C108 H94 K6 O8 Si6'
_chemical_formula_sum            'C108 H94 K6 O8 Si6'
_chemical_formula_weight         1922.97
_chemical_name_systematic
(\m~4~-Aqua)(\m~3~-aqua)pentakis(\m~3~-triphenylsilanolato)(\m~2~-triphenylsilanolato)hexapotassium
_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-2018/1
_cell_angle_alpha                89.61(2)
_cell_angle_beta                 78.98(2)
_cell_angle_gamma                73.26(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7633(7)
_cell_length_b                   14.7076(8)
_cell_length_c                   28.183(3)
_cell_measurement_reflns_used    144636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3.1
_cell_volume                     4966.3(9)
_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_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            243068
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         75.852
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.480
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.715
_refine_diff_density_min         -1.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         20415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0459P)^2^+6.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                19325
_reflns_number_total             20415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3064sup1.cif
_cod_data_source_block           u777bba
_cod_database_code               2022415
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.745
_shelx_hkl_checksum              37353
_shelx_res_checksum              98333
_cod_database_fobs_code 2022415