Pentacoordinate Silicon Compounds with SiO5Skeletons Containing SiOH or SiOSi Groups: Derivatives of the Pentahydroxosilicate(1-) Anion [Si(OH)5]-and Its Anhydride [(HO)4Si-O-Si(OH)4]2-
Reinhold Tacke; Christian Burschka; Ingo Richter; Brigitte Wagner; Reiner Willeke; Journal of the American Chemical Society 122 (2000) 8480–8485; doi:10.1021/ja000637i

data_4116127
_publ_contact_author
;       Reinhold Tacke
    Institut f\"ur Anorganische Chemie
    Bayerische Julius-Maximilians-Universit\"at W\"urzburg
    Am Hubland
    D-97074 W\"urzburg
    Bundesrepublik Deutschland
;
_publ_contact_author_email       r.tacke@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 8884609'
_publ_contact_author_phone       '049 931 8885250'
_publ_section_title
;
 Pentacoordinate Silicon Compounds with SiO5Skeletons Containing SiOH or
 SiOSi Groups: Derivatives of the Pentahydroxosilicate(1-) Anion
 [Si(OH)5]-and Its Anhydride [(HO)4Si-O-Si(OH)4]2-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8480
_journal_page_last               8485
_journal_paper_doi               10.1021/ja000637i
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         '(C28 H21 O7 Si), (C6 H8 N), (C4 H8 O) '
_chemical_formula_sum            'C38 H37 N O8 Si'
_chemical_formula_weight         663.78
_chemical_melting_point          472
_chemical_name_systematic
'Anilinium Bis[benzilato(2-)-O1,O2]hydroxosilicate-Tetrahydrofuran'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.155(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3633(14)
_cell_length_b                   12.5129(13)
_cell_length_c                   11.8372(14)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      4.95
_cell_volume                     1682.8(3)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Bruker-SHELXTL
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Stoe-IPDS
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10398
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       platelet
_exptl_crystal_F_000             700
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                3455
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000637i_3.cif
_cod_data_source_block           ricabul
_cod_database_code               4116127