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_4318288
_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 Ge N3 O6(2-); 2 * C2 H8 N(+); CH3OH'
_chemical_formula_sum            'C26 H35 Ge N5 O7'
_chemical_formula_weight         602.18
_chemical_melting_point          431
_chemical_name_common
'Dimethylammonium fac-Tris[benzohydroximato(2-)]germanate-Methanol'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 76.2080(10)
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_cell_length_a                   10.5258(4)
_cell_length_b                   11.5067(5)
_cell_length_c                   12.3019(5)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.8
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_cell_volume                     1436.19(10)
_computing_cell_refinement       'SMART-NT V6'
_computing_data_collection       'SMART-NT V6'
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_computing_molecular_graphics    'XP in Shelxtl-97'
_computing_publication_material  'XP in Shelxtl-97'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.762753
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.35
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_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.628
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0427
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                5463
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255757_s2_4.cif
_cod_data_source_block           fac-7
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Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_database_code               4318288