Dianionic Complexes with Hexacoordinate Silicon(IV) or Germanium(IV) and Three Bidentate Ligands of the Hydroximato(2-) Type: Syntheses and Structural Characterization in the Solid State
Andreas Biller; Christian Burschka; Martin Penka; Reinhold Tacke; Inorganic Chemistry 41 (2002) 3901–3908; doi:10.1021/ic0255757

data_4318285
_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
;
 Dianionic Complexes with Hexacoordinate Silicon(IV) or Germanium(IV) and
 Three Bidentate Ligands of the Hydroximato(2-) Type: Syntheses and
 Structural Characterization in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3901
_journal_page_last               3908
_journal_paper_doi               10.1021/ic0255757
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C21 H15 N3 O6 Si(2-), 2 * C4 H11 N2(+) '
_chemical_formula_sum            'C29 H37 N7 O6 Si'
_chemical_formula_weight         607.75
_chemical_melting_point          456
_chemical_name_common
'N,N-Dimethylacetamidinium fac-Tris[benzohydroximato(2-)]silicate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.984(2)
_cell_length_b                   16.883(3)
_cell_length_c                   18.019(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.3
_cell_volume                     3029.1(11)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_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 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       21
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_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27639
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          1
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0648P)^2^+0.1325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                4694
_reflns_number_total             6117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255757_s2_1.cif
_cod_data_source_block           fac8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.1325P] 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^)+(0.0648P)^2^+0.1325P] 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               4318285