#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:36:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179798 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/94/7009453.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009453
loop_
_publ_author_name
'Filippou, Alexander C.'
'Portius, Peter'
'Kociok-Köhn, Gabriele'
'Albrecht, Volker'
_publ_contact_author
;       Alexander C. Filippou
        Institut für Anorganische und Allgemeine Chemie der
        Humboldt Universität 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,
 Universität 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       ω-2θ
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0647P)²+3.4328P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge 0.74477(2) 0.23958(2) 0.599536(15) 0.01648(14) Uani 1 d . . .
B B 0.6909(3) 0.4456(3) 0.71302(16) 0.0190(6) Uani 1 d . . .
H0 H 0.6733 0.5102 0.7493 0.023 Uiso 1 calc R . .
N1 N 0.8179(2) 0.25665(19) 0.71296(14) 0.0196(5) Uani 1 d . . .
C1 C 0.9016(2) 0.1917(3) 0.76099(15) 0.0220(6) Uani 1 d . . .
C11 C 0.9536(3) 0.0730(3) 0.74168(18) 0.0290(6) Uani 1 d . . .
H11A H 0.9206 0.0518 0.6881 0.044 Uiso 1 calc R . .
H11B H 0.9334 0.0086 0.7756 0.044 Uiso 1 calc R . .
H11C H 1.0408 0.0807 0.7487 0.044 Uiso 1 calc R . .
C2 C 0.9258(3) 0.2521(3) 0.83132(17) 0.0252(6) Uani 1 d . . .
H2 H 0.9816 0.2273 0.8756 0.030 Uiso 1 calc R . .
C3 C 0.8540(2) 0.3543(3) 0.82501(14) 0.0223(6) Uani 1 d . . .
C31 C 0.8413(3) 0.4485(3) 0.88449(15) 0.0288(6) Uani 1 d . . .
H31A H 0.7821 0.5099 0.8619 0.043 Uiso 1 calc R . .
H31B H 0.9187 0.4884 0.9026 0.043 Uiso 1 calc R . .
H31C H 0.8147 0.4087 0.9279 0.043 Uiso 1 calc R . .
N2 N 0.78838(19) 0.3565(2) 0.75293(12) 0.0194(5) Uani 1 d . . .
N3 N 0.7646(2) 0.4246(2) 0.58947(12) 0.0183(5) Uani 1 d . . .
C4 C 0.7987(2) 0.4950(3) 0.53475(15) 0.0219(6) Uani 1 d . . .
C41 C 0.8365(3) 0.4469(3) 0.46428(16) 0.0295(6) Uani 1 d . . .
H41A H 0.8332 0.3572 0.4644 0.044 Uiso 1 calc R . .
H41B H 0.9185 0.4736 0.4636 0.044 Uiso 1 calc R . .
H41C H 0.7825 0.4783 0.4186 0.044 Uiso 1 calc R . .
C5 C 0.7914(3) 0.6171(3) 0.55525(16) 0.0243(6) Uani 1 d . . .
H5 H 0.8102 0.6863 0.5273 0.029 Uiso 1 calc R . .
C6 C 0.7514(2) 0.6184(2) 0.62438(15) 0.0215(5) Uani 1 d . . .
C61 C 0.7277(3) 0.7244(3) 0.67267(19) 0.0326(7) Uani 1 d . . .
H61A H 0.7004 0.6941 0.7185 0.049 Uiso 1 calc R . .
H61B H 0.6656 0.7767 0.6429 0.049 Uiso 1 calc R . .
H61C H 0.8013 0.7720 0.6883 0.049 Uiso 1 calc R . .
N4 N 0.7358(2) 0.5019(2) 0.64437(12) 0.0186(5) Uani 1 d . . .
N5 N 0.5864(2) 0.2746(2) 0.63110(13) 0.0200(5) Uani 1 d . . .
C7 C 0.4757(3) 0.2270(3) 0.60917(17) 0.0238(6) Uani 1 d . . .
C71 C 0.4464(3) 0.1215(3) 0.55542(18) 0.0317(7) Uani 1 d . . .
H71A H 0.5192 0.0938 0.5386 0.048 Uiso 1 calc R . .
H71B H 0.3870 0.1470 0.5106 0.048 Uiso 1 calc R . .
H71C H 0.4137 0.0543 0.5817 0.048 Uiso 1 calc R . .
C8 C 0.3976(3) 0.2923(3) 0.64520(17) 0.0283(6) Uani 1 d . . .
H8 H 0.3141 0.2783 0.6405 0.034 Uiso 1 calc R . .
C9 C 0.4644(2) 0.3817(3) 0.68925(16) 0.0249(6) Uani 1 d . . .
C91 C 0.4249(3) 0.4787(3) 0.73829(19) 0.0368(7) Uani 1 d . . .
H91A H 0.4942 0.5277 0.7623 0.055 Uiso 1 calc R . .
H91B H 0.3887 0.4404 0.7783 0.055 Uiso 1 calc R . .
H91C H 0.3659 0.5318 0.7064 0.055 Uiso 1 calc R . .
N6 N 0.5786(2) 0.3695(2) 0.68076(12) 0.0203(5) Uani 1 d . . .
N7 N 0.9011(2) 0.2134(2) 0.57185(14) 0.0239(5) Uani 1 d . . .
N8 N 0.9894(2) 0.2637(2) 0.60760(15) 0.0247(5) Uani 1 d . . .
N9 N 1.0759(3) 0.3072(3) 0.63969(18) 0.0417(7) Uani 1 d . . .
N10 N 0.6691(2) 0.2257(2) 0.49208(14) 0.0255(5) Uani 1 d . . .
N11 N 0.5975(2) 0.3044(3) 0.46444(14) 0.0292(6) Uani 1 d . . .
N12 N 0.5304(3) 0.3754(3) 0.43498(18) 0.0503(8) Uani 1 d . . .
N13 N 0.7235(2) 0.0659(2) 0.61469(14) 0.0244(5) Uani 1 d . . .
N14 N 0.7821(2) -0.0028(2) 0.58189(13) 0.0222(5) Uani 1 d . . .
N15 N 0.8350(2) -0.0727(2) 0.55416(15) 0.0310(6) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N13 Ge N10 90.91(11) . . ?
N13 Ge N7 92.04(11) . . ?
N10 Ge N7 89.79(12) . . ?
N13 Ge N5 90.29(10) . . ?
N10 Ge N5 91.99(11) . . ?
N7 Ge N5 177.05(9) . . ?
N13 Ge N1 89.49(10) . . ?
N10 Ge N1 177.78(10) . . ?
N7 Ge N1 92.38(11) . . ?
N5 Ge N1 85.82(11) . . ?
N13 Ge N3 176.75(9) . . ?
N10 Ge N3 91.55(10) . . ?
N7 Ge N3 90.09(10) . . ?
N5 Ge N3 87.51(10) . . ?
N1 Ge N3 87.97(9) . . ?
N4 B N6 107.5(2) . . ?
N4 B N2 107.3(2) . . ?
N6 B N2 107.6(2) . . ?
C1 N1 N2 107.7(2) . . ?
C1 N1 Ge 132.9(2) . . ?
N2 N1 Ge 119.19(17) . . ?
N1 C1 C2 108.1(3) . . ?
N1 C1 C11 125.1(2) . . ?
C2 C1 C11 126.8(3) . . ?
C3 C2 C1 107.5(3) . . ?
N2 C3 C2 107.6(2) . . ?
N2 C3 C31 122.9(3) . . ?
C2 C3 C31 129.5(3) . . ?
C3 N2 N1 109.1(2) . . ?
C3 N2 B 131.6(2) . . ?
N1 N2 B 119.3(2) . . ?
C4 N3 N4 107.4(2) . . ?
C4 N3 Ge 132.56(19) . . ?
N4 N3 Ge 120.03(17) . . ?
N3 C4 C5 108.6(2) . . ?
N3 C4 C41 124.7(3) . . ?
C5 C4 C41 126.7(3) . . ?
C6 C5 C4 106.7(2) . . ?
N4 C6 C5 107.8(2) . . ?
N4 C6 C61 122.4(3) . . ?
C5 C6 C61 129.8(3) . . ?
C6 N4 N3 109.5(2) . . ?
C6 N4 B 132.1(2) . . ?
N3 N4 B 118.4(2) . . ?
C7 N5 N6 107.7(2) . . ?
C7 N5 Ge 132.8(2) . . ?
N6 N5 Ge 119.33(17) . . ?
N5 C7 C8 108.4(3) . . ?
N5 C7 C71 124.3(3) . . ?
C8 C7 C71 127.3(3) . . ?
C9 C8 C7 106.9(3) . . ?
N6 C9 C8 107.8(3) . . ?
N6 C9 C91 122.8(3) . . ?
C8 C9 C91 129.4(3) . . ?
C9 N6 N5 109.3(2) . . ?
C9 N6 B 131.0(2) . . ?
N5 N6 B 119.6(2) . . ?
N8 N7 Ge 120.4(2) . . ?
N9 N8 N7 176.7(3) . . ?
N11 N10 Ge 118.4(2) . . ?
N12 N11 N10 176.5(3) . . ?
N14 N13 Ge 116.1(2) . . ?
N15 N14 N13 175.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge N13 1.937(3) . ?
Ge N10 1.939(3) . ?
Ge N7 1.954(3) . ?
Ge N5 2.023(3) . ?
Ge N1 2.031(3) . ?
Ge N3 2.044(3) . ?
B N4 1.535(4) . ?
B N6 1.540(4) . ?
B N2 1.542(4) . ?
N1 C1 1.351(4) . ?
N1 N2 1.376(3) . ?
C1 C2 1.390(4) . ?
C1 C11 1.490(4) . ?
C2 C3 1.375(4) . ?
C3 N2 1.351(3) . ?
C3 C31 1.499(4) . ?
N3 C4 1.351(4) . ?
N3 N4 1.374(3) . ?
C4 C5 1.388(4) . ?
C4 C41 1.492(4) . ?
C5 C6 1.386(4) . ?
C6 N4 1.341(4) . ?
C6 C61 1.494(4) . ?
N5 C7 1.349(4) . ?
N5 N6 1.373(3) . ?
C7 C8 1.387(4) . ?
C7 C71 1.492(4) . ?
C8 C9 1.383(4) . ?
C9 N6 1.343(4) . ?
C9 C91 1.493(4) . ?
N7 N8 1.212(4) . ?
N8 N9 1.142(4) . ?
N10 N11 1.220(4) . ?
N11 N12 1.141(4) . ?
N13 N14 1.221(4) . ?
N14 N15 1.141(4) . ?
