Oxidation of germanium(II) azides with HN3: a convenient route to six-co-ordinate triazidogermanium(IV) compounds
Filippou, Alexander C.; Portius, Peter; Kociok-Köhn, Gabriele; Albrecht, Volker; Journal of the Chemical Society, Dalton Transactions  (2000) 1759–; doi:10.1039/b001198n

data_7009453
_publ_contact_author
;       Alexander C. Filippou
        Institut f\"ur Anorganische und Allgemeine Chemie der
        Humboldt Universit\"at zu Berlin
        Hessische Strasse 1-2
        10115 Berlin
        Bundesrepublik Deutschland
;
_publ_section_title
;
 Oxidation of germanium(II) azides with HN3: a convenient route to
 six-co-ordinate triazidogermanium(IV) compounds
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1759
_journal_paper_doi               10.1039/b001198n
_journal_year                    2000
_chemical_formula_moiety         'C15 H22 B Ge N15'
_chemical_formula_sum            'C15 H22 B Ge N15'
_chemical_formula_weight         495.90
_chemical_name_systematic
; 
 ? 
;
_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                 101.04(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.378(7)
_cell_length_b                   10.918(13)
_cell_length_c                   17.719(9)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      18.2
_cell_measurement_theta_min      16.8
_cell_volume                     2160(3)
_computing_cell_refinement       'STADI4 (STOE, 1995)'
_computing_data_collection       'STADI4 (STOE, 1995)'
_computing_data_reduction        'X-RED, (STOE, 1995)'
_computing_molecular_graphics
;
 L.Zsolnai, H.Pritzkow, ZORTEP, ORTEP program for PC,
 Universit\"at Heidelberg 1994
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'STOE Stadi4 Diffractometer'
_diffrn_measurement_method       \w-2\q
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6301
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.403
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.1926
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
  6 Psi Scan Reflections used    Mu * R = 0.00
    H   K   L   2Theta   Chi   Imin/Imax
   -1  -1   1     5.9   -83.2    0.182
   -2  -3   2    13.4   -84.5    0.188
   -2  -3   3    14.5   -84.2    0.177
   -3  -3   3    17.8   -83.2    0.201
   -3  -4   3    19.3   -86.6    0.209
   -4  -5   5    26.3   -87.5    0.217 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          1.14
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0258(13)
_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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0647P)^2^+3.4328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                3948
_reflns_number_total             4234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001198n.txt
_cod_data_source_block           peter36a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.4328P] 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^)+(0.0647P)^2^+3.4328P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7009453