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_4318287
_publ_contact_author
;
        Reinhold Tacke
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland 
        97074 W\"urzburg
        Bundesrepublik Deutschland
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_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 * C2 H8 N(+); CH3OH'
_chemical_formula_sum            'C26 H35 N5 O7 Si'
_chemical_formula_weight         557.68
_chemical_melting_point          442
_chemical_name_common
'Dimethylammonium fac-Tris[benzohydroximato(2-)]silicate-Methanol'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                89.555(18)
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_cell_angle_gamma                83.275(18)
_cell_formula_units_Z            2
_cell_length_a                   10.4703(13)
_cell_length_b                   11.404(2)
_cell_length_c                   12.3215(16)
_cell_measurement_reflns_used    3452
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      6.7
_cell_volume                     1422.7(4)
_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 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0302
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18620
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             592
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.259
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6343
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_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.0910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                4636
_reflns_number_total             6343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255757_s2_3.cif
_cod_data_source_block           fac-6
_cod_depositor_comments
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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 
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_cod_database_code               4318287