#------------------------------------------------------------------------------
#$Date: 2014-12-19 10:20:53 +0200 (Fri, 19 Dec 2014) $
#$Revision: 128844 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116052.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_7116052
loop_
_publ_author_name
'P. Steiniger'
'G. Bendt'
'D. Blaser'
'C. Wolper'
'S. Schulz'
_publ_section_title
;
 Germane vs. digermane formation
;
_journal_name_full               Chem.Commun.
_journal_page_first              15461
_journal_paper_doi               10.1039/C4cc07921C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C10 H24 Ge N2 Si'
_chemical_formula_sum            'C10 H24 Ge N2 Si'
_chemical_formula_weight         272.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.704(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9266(18)
_cell_length_b                   6.3714(11)
_cell_length_c                   18.087(2)
_cell_measurement_reflns_used    3357
_cell_measurement_temperature    230(1)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.26
_cell_volume                     1484.6(4)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      230(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 PHI scan 360 deg, kappa 0 deg
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_laue_measured_fraction_full 0.891
_diffrn_reflns_laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13962
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.669
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'sealed X-RAY tube'
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       cylindric
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1358P)^2^+1.3024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2201
_reflns_number_total             3739
_reflns_threshold_expression     'I > 2\s(I)'
_[local]_cod_data_source_file    c4cc07921c2.cif
_[local]_cod_data_source_block   gb_166m
_cod_database_code               7116052
_ccdc_polymorph                  1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.569
_shelxl_version_number           2013-4
_shelx_res_file
;
TITL gb_166m in P2(1)/n  ***Hochtemperatur***
CELL 0.71073  12.9266   6.3714  18.0866  90.000  94.704  90.000
ZERR    4.00   0.0018   0.0011   0.0024   0.000   0.008   0.000
LATT  1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N SI GE
UNIT 40 96 8 4 4
TEMP -43
L.S. 14
SIZE .3 .3 .3
ACTA
FMAP 2
PLAN 10
WGHT    0.135800    1.302400
FVAR       0.11864
GE1   5    0.638750    0.202667    0.246730    11.00000    0.04160    0.10387 =
         0.04032   -0.00888   -0.00010    0.01442
SI1   4    0.482836    0.395136    0.303126    11.00000    0.04257    0.06302 =
         0.04803   -0.00719   -0.00172    0.01064
N1    3    0.508301    0.306073    0.216175    11.00000    0.04353    0.06883 =
         0.03940   -0.00273   -0.00702    0.00023
N2    3    0.602372    0.300771    0.337186    11.00000    0.03989    0.07128 =
         0.03576   -0.00417    0.00166    0.00692
C1    1    0.450746    0.303098    0.143516    11.00000    0.04562    0.07357 =
         0.04949   -0.00140   -0.01187    0.00285
C2    1    0.428730    0.526294    0.116950    11.00000    0.14183    0.10246 =
         0.06167    0.01007   -0.03973   -0.00108
AFIX 137
H2A   2    0.377888    0.589815    0.146591    11.00000   -1.50000
H2B   2    0.401853    0.524002    0.065284    11.00000   -1.50000
H2C   2    0.492402    0.607459    0.122028    11.00000   -1.50000
AFIX   0
C3    1    0.350255    0.188600    0.147541    11.00000    0.09338    0.21047 =
         0.08522    0.02727   -0.04192   -0.08233
AFIX 137
H3A   2    0.363912    0.048358    0.166807    11.00000   -1.50000
H3B   2    0.314611    0.179492    0.098321    11.00000   -1.50000
H3C   2    0.307120    0.263749    0.180105    11.00000   -1.50000
AFIX   0
C4    1    0.514350    0.199247    0.086851    11.00000    0.07584    0.17058 =
         0.04901   -0.02930   -0.01496    0.02570
AFIX 137
H4A   2    0.568998    0.293857    0.074232    11.00000   -1.50000
H4B   2    0.469798    0.166630    0.042560    11.00000   -1.50000
H4C   2    0.544915    0.070867    0.107537    11.00000   -1.50000
AFIX   0
C5    1    0.661713    0.298234    0.409606    11.00000    0.04866    0.07356 =
         0.03620    0.00104   -0.00117    0.00233
C6    1    0.764847    0.195000    0.402553    11.00000    0.05292    0.12929 =
         0.05715   -0.00952   -0.01856    0.02758
AFIX 137
H6A   2    0.754189    0.059084    0.378988    11.00000   -1.50000
H6B   2    0.800459    0.176756    0.451454    11.00000   -1.50000
H6C   2    0.806525    0.282461    0.372659    11.00000   -1.50000
AFIX   0
C7    1    0.601283    0.180016    0.465475    11.00000    0.08671    0.15441 =
         0.05018    0.02942    0.00090   -0.02448
AFIX 137
H7A   2    0.532962    0.242092    0.466924    11.00000   -1.50000
H7B   2    0.638233    0.188815    0.514266    11.00000   -1.50000
H7C   2    0.594239    0.033986    0.450752    11.00000   -1.50000
AFIX   0
C8    1    0.681751    0.523400    0.436451    11.00000    0.07787    0.09455 =
         0.05616   -0.01149   -0.01546    0.00019
AFIX 137
H8A   2    0.716597    0.600650    0.399510    11.00000   -1.50000
H8B   2    0.725169    0.521470    0.482806    11.00000   -1.50000
H8C   2    0.616193    0.590850    0.444057    11.00000   -1.50000
AFIX   0
C9    1    0.369497    0.266442    0.342526    11.00000    0.04806    0.09937 =
         0.08391   -0.00208    0.01830    0.01145
AFIX 137
H9A   2    0.370921    0.116871    0.332657    11.00000   -1.50000
H9B   2    0.305565    0.325844    0.319684    11.00000   -1.50000
H9C   2    0.373222    0.289865    0.395670    11.00000   -1.50000
AFIX   0
C10   1    0.468129    0.679194    0.309591    11.00000    0.10991    0.07766 =
         0.08937   -0.01547   -0.03225    0.02091
AFIX 137
H10A  2    0.455697    0.717083    0.360046    11.00000   -1.50000
H10B  2    0.409886    0.724271    0.276127    11.00000   -1.50000
H10C  2    0.530984    0.747243    0.296038    11.00000   -1.50000
AFIX   0
HKLF 4

REM  gb_166m in P2(1)/n  ***Hochtemperatur***
REM R1 =  0.0802 for    2201 Fo > 4sig(Fo)  and  0.1348 for all    3739 data
REM    135 parameters refined using      0 restraints

END

WGHT      0.1358      1.3028

REM Highest difference peak  1.355,  deepest hole -0.945,  1-sigma level  0.166
Q1    1   0.6176  0.3219  0.2668  11.00000  0.05    1.35
Q2    1   0.6683  0.1090  0.2222  11.00000  0.05    1.31
Q3    1   0.6760  0.3005  0.2162  11.00000  0.05    1.27
Q4    1   0.6071  0.0984  0.2653  11.00000  0.05    1.15
Q5    1   0.5574  0.2876  0.2555  11.00000  0.05    0.85
Q6    1   0.7054 -0.1103  0.3104  11.00000  0.05    0.74
Q7    1   0.5068  0.2811  0.2730  11.00000  0.05    0.71
Q8    1   0.4987  0.3965  0.2486  11.00000  0.05    0.71
Q9    1   0.4502  0.5034  0.3252  11.00000  0.05    0.61
Q10   1   0.5185  0.4951  0.2823  11.00000  0.05    0.59
;
_shelx_res_checksum              44889
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ge1 Ge 0.63875(5) 0.20267(16) 0.24673(3) 0.0621(3) Uani 1 1 d . .
Si1 Si 0.48284(12) 0.3951(3) 0.30313(9) 0.0515(5) Uani 1 1 d . .
N1 N 0.5083(4) 0.3061(9) 0.2162(3) 0.0512(12) Uani 1 1 d . .
N2 N 0.6024(3) 0.3008(9) 0.3372(2) 0.0491(12) Uani 1 1 d . .
C1 C 0.4507(5) 0.3031(12) 0.1435(3) 0.0571(16) Uani 1 1 d . .
C2 C 0.4287(10) 0.5263(17) 0.1170(5) 0.105(3) Uani 1 1 d . .
H2A H 0.3779 0.5898 0.1466 0.157 Uiso 1 1 calc R U
H2B H 0.4019 0.5240 0.0653 0.157 Uiso 1 1 calc R U
H2C H 0.4924 0.6075 0.1220 0.157 Uiso 1 1 calc R U
C3 C 0.3503(9) 0.189(2) 0.1475(6) 0.132(6) Uani 1 1 d . .
H3A H 0.3639 0.0484 0.1668 0.199 Uiso 1 1 calc R U
H3B H 0.3146 0.1795 0.0983 0.199 Uiso 1 1 calc R U
H3C H 0.3071 0.2637 0.1801 0.199 Uiso 1 1 calc R U
C4 C 0.5144(7) 0.199(2) 0.0869(4) 0.100(3) Uani 1 1 d . .
H4A H 0.5690 0.2939 0.0742 0.149 Uiso 1 1 calc R U
H4B H 0.4698 0.1666 0.0426 0.149 Uiso 1 1 calc R U
H4C H 0.5449 0.0709 0.1075 0.149 Uiso 1 1 calc R U
C5 C 0.6617(5) 0.2982(12) 0.4096(3) 0.0531(15) Uani 1 1 d . .
C6 C 0.7648(6) 0.1950(16) 0.4026(4) 0.081(3) Uani 1 1 d . .
H6A H 0.7542 0.0591 0.3790 0.122 Uiso 1 1 calc R U
H6B H 0.8005 0.1768 0.4515 0.122 Uiso 1 1 calc R U
H6C H 0.8065 0.2825 0.3727 0.122 Uiso 1 1 calc R U
C7 C 0.6013(7) 0.1800(19) 0.4655(4) 0.097(3) Uani 1 1 d . .
H7A H 0.5330 0.2421 0.4669 0.146 Uiso 1 1 calc R U
H7B H 0.6382 0.1888 0.5143 0.146 Uiso 1 1 calc R U
H7C H 0.5942 0.0340 0.4508 0.146 Uiso 1 1 calc R U
C8 C 0.6818(7) 0.5234(15) 0.4365(4) 0.077(2) Uani 1 1 d . .
H8A H 0.7166 0.6006 0.3995 0.116 Uiso 1 1 calc R U
H8B H 0.7252 0.5215 0.4828 0.116 Uiso 1 1 calc R U
H8C H 0.6162 0.5908 0.4441 0.116 Uiso 1 1 calc R U
C9 C 0.3695(6) 0.2664(15) 0.3425(5) 0.076(2) Uani 1 1 d . .
H9A H 0.3709 0.1169 0.3327 0.115 Uiso 1 1 calc R U
H9B H 0.3056 0.3258 0.3197 0.115 Uiso 1 1 calc R U
H9C H 0.3732 0.2899 0.3957 0.115 Uiso 1 1 calc R U
C10 C 0.4681(8) 0.6792(16) 0.3096(6) 0.095(3) Uani 1 1 d . .
H10A H 0.4557 0.7171 0.3600 0.142 Uiso 1 1 calc R U
H10B H 0.4099 0.7243 0.2761 0.142 Uiso 1 1 calc R U
H10C H 0.5310 0.7472 0.2960 0.142 Uiso 1 1 calc R U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0416(4) 0.1039(8) 0.0403(4) -0.0089(3) -0.0001(2) 0.0144(3)
Si1 0.0426(8) 0.0630(13) 0.0480(8) -0.0072(8) -0.0017(6) 0.0106(7)
N1 0.044(2) 0.069(4) 0.039(2) -0.003(2) -0.0070(18) 0.000(2)
N2 0.040(2) 0.071(4) 0.036(2) -0.004(2) 0.0017(17) 0.007(2)
C1 0.046(3) 0.074(5) 0.049(3) -0.001(3) -0.012(2) 0.003(3)
C2 0.142(9) 0.102(9) 0.062(5) 0.010(5) -0.040(5) -0.001(6)
C3 0.093(7) 0.210(15) 0.085(7) 0.027(7) -0.042(5) -0.082(8)
C4 0.076(5) 0.171(11) 0.049(4) -0.029(5) -0.015(4) 0.026(6)
C5 0.049(3) 0.074(5) 0.036(2) 0.001(3) -0.001(2) 0.002(3)
C6 0.053(4) 0.129(8) 0.057(4) -0.010(4) -0.019(3) 0.028(4)
C7 0.087(6) 0.154(10) 0.050(4) 0.029(5) 0.001(4) -0.024(6)
C8 0.078(5) 0.095(7) 0.056(4) -0.011(4) -0.015(3) 0.000(4)
C9 0.048(4) 0.099(7) 0.084(5) -0.002(4) 0.018(4) 0.011(3)
C10 0.110(7) 0.078(7) 0.089(6) -0.015(5) -0.032(5) 0.021(5)
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
N2 Ge1 N1 81.5(2)
N2 Ge1 Si1 40.68(15)
N1 Ge1 Si1 40.83(15)
N2 Si1 N1 88.8(2)
N2 Si1 C10 114.7(4)
N1 Si1 C10 114.4(4)
N2 Si1 C9 114.7(3)
N1 Si1 C9 114.6(4)
C10 Si1 C9 108.8(5)
N2 Si1 Ge1 44.31(15)
N1 Si1 Ge1 44.47(16)
C10 Si1 Ge1 125.0(4)
C9 Si1 Ge1 126.3(3)
C1 N1 Si1 134.7(4)
C1 N1 Ge1 130.5(4)
Si1 N1 Ge1 94.7(2)
C5 N2 Si1 135.5(4)
C5 N2 Ge1 129.5(4)
Si1 N2 Ge1 95.0(2)
N1 C1 C3 110.1(6)
N1 C1 C4 110.5(5)
C3 C1 C4 109.9(8)
N1 C1 C2 110.0(6)
C3 C1 C2 109.3(8)
C4 C1 C2 107.0(8)
N2 C5 C6 109.4(5)
N2 C5 C7 109.8(6)
C6 C5 C7 110.3(7)
N2 C5 C8 109.7(5)
C6 C5 C8 108.0(6)
C7 C5 C8 109.6(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 N2 1.848(4)
Ge1 N1 1.852(5)
Ge1 Si1 2.6350(17)
Si1 N2 1.724(5)
Si1 N1 1.729(5)
Si1 C10 1.825(10)
Si1 C9 1.870(8)
N1 C1 1.456(7)
N2 C5 1.463(7)
C1 C3 1.497(11)
C1 C4 1.517(10)
C1 C2 1.520(12)
C5 C6 1.501(9)
C5 C7 1.526(10)
C5 C8 1.530(11)