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_4116125
_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-
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_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         'C56 H40 O13 Si2, 2(C6 H8 N), 2(C2 H3 N)'
_chemical_formula_sum            'C72 H62 N4 O13 Si2'
_chemical_formula_weight         1247.44
_chemical_melting_point          489
_chemical_name_systematic
'Anilinium Tetrakis[benzilato(2-)-O1,O2]-my-oxo-disilicate-Diacetonitrile'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.77(3)
_cell_angle_beta                 61.95(3)
_cell_angle_gamma                60.97(3)
_cell_formula_units_Z            2
_cell_length_a                   15.639(3)
_cell_length_b                   15.996(3)
_cell_length_c                   16.538(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.50
_cell_volume                     3164.3(18)
_computing_cell_refinement       'STOE IPDS'
_computing_data_collection       'STOE IPDS'
_computing_data_reduction        'STOE IPDS'
_computing_molecular_graphics    'Bruker SHELXTL Plus'
_computing_publication_material  'Bruker SHELXTL Plus'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            64209
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         10212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                7065
_reflns_number_total             10212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000637i_1.cif
_cod_data_source_block           sil1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3164.2(11)
_cod_database_code               4116125