The Hexacoordinate Silicate Dianions mer-Tris[glycolato(2-)-O1,O2]silicate and fac-Tris[benzilato(2-)-O1,O2]silicate: Syntheses and Structural Characterization
Ingo Richter; Martin Penka; Reinhold Tacke; Inorganic Chemistry 41 (2002) 3950–3955; doi:10.1021/ic025597t

data_4318290
_publ_contact_author
;
        Reinhold Tacke
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland 
        97074 W\"urzburg
        Bundesrepublik Deutschland
;
_publ_contact_author_email       r.tacke@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 888-4609'
_publ_contact_author_phone       '049 931 888-5250'
_publ_section_title
;
 The Hexacoordinate Silicate Dianions
 mer-Tris[glycolato(2-)-O1,O2]silicate and
 fac-Tris[benzilato(2-)-O1,O2]silicate: Syntheses and Structural
 Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3950
_journal_page_last               3955
_journal_paper_doi               10.1021/ic025597t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
'C42 H30 O9 Si(2-); 2 * C6 H16 N(+); 1/2 * C4 H8 O2'
_chemical_formula_sum            'C56 H66 N2 O10 Si'
_chemical_formula_weight         955.20
_chemical_melting_point          436
_chemical_name_common
'Triethylammonium fac-Tris[benzilato(2-)-O1,O2]silicate-Hemi-1,4-dioxane'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 97.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.633(8)
_cell_length_b                   13.055(3)
_cell_length_c                   19.257(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.1
_cell_volume                     10116(4)
_computing_cell_refinement       'Stoe-IPDS cell'
_computing_data_collection       'Stoe-IPDS expose'
_computing_data_reduction        'Stoe-IPDS integrate'
_computing_molecular_graphics    Bruker-Shelxtl
_computing_publication_material  Bruker-Shextl
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.470
_diffrn_measured_fraction_theta_max 0.470
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Phi-Scans
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49031
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         8532
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                6337
_reflns_number_total             8532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025597t_s2_1.cif
_cod_data_source_block           fac-8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0576P)^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^)+(0.0576P)^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 

The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4318290