#------------------------------------------------------------------------------
#$Date: 2014-12-19 10:20:53 +0200 (Fri, 19 Dec 2014) $
#$Revision: 128844 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116054.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_7116054
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         'C12 H30 Ge N2 Se2 Si'
_chemical_formula_sum            'C12 H30 Ge N2 Se2 Si'
_chemical_formula_weight         460.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 97.731(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3441(8)
_cell_length_b                   9.0775(5)
_cell_length_c                   13.8753(7)
_cell_measurement_reflns_used    15465
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.61
_cell_volume                     1915.07(17)
_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      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31347
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.884
_diffrn_reflns_theta_min         2.613
_exptl_absorpt_coefficient_mu    5.453
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.58
_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    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0159
_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^)+(0.0176P)^2^+1.2813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2653
_reflns_number_total             2949
_reflns_threshold_expression     'I > 2\s(I)'
_[local]_cod_data_source_file    c4cc07921c2.cif
_[local]_cod_data_source_block   pst_022m
_cod_database_code               7116054
_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   0.495
_shelx_estimated_absorpt_t_max   0.670
_shelxl_version_number           2013-4
_shelx_res_file
;
TITL pst_022m in C2/c
CELL 0.71073  15.3441   9.0775  13.8753  90.000  97.731  90.000
ZERR    4.00   0.0008   0.0005   0.0007   0.000   0.002   0.000
LATT  7
SYMM -X, Y, 0.5-Z
SFAC C H N SI GE SE
UNIT 48 120 8 4 4 8
TEMP -173
OMIT     0   4   1
OMIT    -3   3   2
OMIT    -8   0   2
OMIT     8   4   3
OMIT     8   2   2
OMIT     2   2   5
OMIT    -2   4   1
SIZE .08 .12 .15
L.S. 14
ACTA
FMAP 2
PLAN 10
WGHT    0.017600    1.281300
FVAR       0.05752
SE1   6    0.432910    0.025695    0.130667    11.00000    0.02106    0.01215 =
         0.02401   -0.00515    0.00437   -0.00352
GE1   5    0.500000    0.187265    0.250000    10.50000    0.01323    0.00802 =
         0.01664    0.00000    0.00381    0.00000
SI1   4    0.500000    0.476548    0.250000    10.50000    0.01654    0.00871 =
         0.01568    0.00000    0.00234    0.00000
N1    3    0.563808    0.339630    0.206021    11.00000    0.01411    0.00918 =
         0.01840    0.00023    0.00478   -0.00100
C1    1    0.651861    0.341420    0.175241    11.00000    0.01495    0.01596 =
         0.01865    0.00146    0.00528   -0.00159
C2    1    0.660867    0.483134    0.117782    11.00000    0.02454    0.02063 =
         0.02540    0.00446    0.00831   -0.00409
AFIX 137
H2A   2    0.613958    0.487407    0.062447    11.00000   -1.50000
H2B   2    0.718173    0.484371    0.093988    11.00000   -1.50000
H2C   2    0.656242    0.568429    0.160093    11.00000   -1.50000
AFIX   0
C3    1    0.662296    0.208116    0.110381    11.00000    0.02188    0.02114 =
         0.03109   -0.00438    0.01212    0.00047
AFIX 137
H3A   2    0.655798    0.117408    0.147046    11.00000   -1.50000
H3B   2    0.720682    0.210246    0.089183    11.00000   -1.50000
H3C   2    0.617094    0.211269    0.053350    11.00000   -1.50000
AFIX   0
C4    1    0.723466    0.336896    0.263920    11.00000    0.01565    0.03013 =
         0.02670    0.00309    0.00171   -0.00052
AFIX 137
H4A   2    0.715726    0.420345    0.306769    11.00000   -1.50000
H4B   2    0.781522    0.342930    0.242131    11.00000   -1.50000
H4C   2    0.718838    0.244528    0.299440    11.00000   -1.50000
AFIX   0
C5    1    0.439987    0.598259    0.155556    11.00000    0.03119    0.01836 =
         0.02499    0.00746    0.00516    0.00602
AFIX 137
H5A   2    0.407455    0.537737    0.104350    11.00000   -1.50000
H5B   2    0.482166    0.660583    0.127339    11.00000   -1.50000
H5C   2    0.398727    0.660570    0.185231    11.00000   -1.50000
AFIX   0
C6    1    0.398676    0.174627    0.030311    11.00000    0.03194    0.02653 =
         0.02012   -0.00114    0.00125    0.00060
AFIX 137
H6A   2    0.343334    0.220867    0.041971    11.00000   -1.50000
H6B   2    0.390841    0.127622   -0.033855    11.00000   -1.50000
H6C   2    0.444745    0.249818    0.032668    11.00000   -1.50000
AFIX   0
HKLF 4

REM  pst_022m in C2/c
REM R1 =  0.0159 for    2653 Fo > 4sig(Fo)  and  0.0205 for all    2949 data
REM     88 parameters refined using      0 restraints

END

WGHT      0.0176      1.2812

REM Highest difference peak  0.374,  deepest hole -0.290,  1-sigma level  0.061
Q1    1   0.6526  0.4152  0.1424  11.00000  0.05    0.37
Q2    1   0.4758  0.0196  0.1072  11.00000  0.05    0.37
Q3    1   0.3948  0.0212  0.1695  11.00000  0.05    0.37
Q4    1   0.5474  0.4040  0.2305  11.00000  0.05    0.36
Q5    1   0.5376  0.2009  0.2103  11.00000  0.05    0.36
Q6    1   0.4771  0.5448  0.1966  11.00000  0.05    0.33
Q7    1   0.6846  0.3406  0.2165  11.00000  0.05    0.31
Q8    1   0.4578 -0.0196  0.1614  11.00000  0.05    0.31
Q9    1   0.6040  0.3428  0.1794  11.00000  0.05    0.30
Q10   1   0.6583  0.2747  0.1488  11.00000  0.05    0.30
;
_shelx_res_checksum              91672
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_refinement_flags_occupancy
Se1 Se 0.43291(2) 0.02569(2) 0.13067(2) 0.01895(4) Uani 1 1 d . . .
Ge1 Ge 0.5000 0.18727(2) 0.2500 0.01247(4) Uani 1 2 d S T P
Si1 Si 0.5000 0.47655(5) 0.2500 0.01363(9) Uani 1 2 d S T P
N1 N 0.56381(6) 0.33963(10) 0.20602(7) 0.01366(18) Uani 1 1 d . . .
C1 C 0.65186(8) 0.34142(13) 0.17524(9) 0.0162(2) Uani 1 1 d . . .
C2 C 0.66087(9) 0.48313(14) 0.11778(10) 0.0231(3) Uani 1 1 d . . .
H2A H 0.6140 0.4874 0.0624 0.035 Uiso 1 1 calc R U .
H2B H 0.7182 0.4844 0.0940 0.035 Uiso 1 1 calc R U .
H2C H 0.6562 0.5684 0.1601 0.035 Uiso 1 1 calc R U .
C3 C 0.66230(9) 0.20812(15) 0.11038(11) 0.0239(3) Uani 1 1 d . . .
H3A H 0.6558 0.1174 0.1470 0.036 Uiso 1 1 calc R U .
H3B H 0.7207 0.2102 0.0892 0.036 Uiso 1 1 calc R U .
H3C H 0.6171 0.2113 0.0533 0.036 Uiso 1 1 calc R U .
C4 C 0.72347(9) 0.33690(16) 0.26392(10) 0.0243(3) Uani 1 1 d . . .
H4A H 0.7157 0.4203 0.3068 0.036 Uiso 1 1 calc R U .
H4B H 0.7815 0.3429 0.2421 0.036 Uiso 1 1 calc R U .
H4C H 0.7188 0.2445 0.2994 0.036 Uiso 1 1 calc R U .
C5 C 0.43999(9) 0.59826(15) 0.15556(10) 0.0247(3) Uani 1 1 d . . .
H5A H 0.4075 0.5377 0.1043 0.037 Uiso 1 1 calc R U .
H5B H 0.4822 0.6606 0.1273 0.037 Uiso 1 1 calc R U .
H5C H 0.3987 0.6606 0.1852 0.037 Uiso 1 1 calc R U .
C6 C 0.39868(10) 0.17463(15) 0.03031(10) 0.0264(3) Uani 1 1 d . . .
H6A H 0.3433 0.2209 0.0420 0.040 Uiso 1 1 calc R U .
H6B H 0.3908 0.1276 -0.0339 0.040 Uiso 1 1 calc R U .
H6C H 0.4447 0.2498 0.0327 0.040 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
Se1 0.02106(7) 0.01215(6) 0.02401(7) -0.00515(4) 0.00437(5) -0.00352(4)
Ge1 0.01323(8) 0.00802(7) 0.01664(9) 0.000 0.00381(6) 0.000
Si1 0.0165(2) 0.00871(19) 0.0157(2) 0.000 0.00234(16) 0.000
N1 0.0141(4) 0.0092(4) 0.0184(5) 0.0002(3) 0.0048(4) -0.0010(3)
C1 0.0150(5) 0.0160(5) 0.0187(6) 0.0015(4) 0.0053(4) -0.0016(4)
C2 0.0245(6) 0.0206(6) 0.0254(7) 0.0045(5) 0.0083(5) -0.0041(5)
C3 0.0219(6) 0.0211(6) 0.0311(7) -0.0044(5) 0.0121(5) 0.0005(5)
C4 0.0156(6) 0.0301(7) 0.0267(7) 0.0031(5) 0.0017(5) -0.0005(5)
C5 0.0312(7) 0.0184(6) 0.0250(7) 0.0075(5) 0.0052(5) 0.0060(5)
C6 0.0319(7) 0.0265(7) 0.0201(6) -0.0011(5) 0.0012(5) 0.0006(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'
Se Se -0.0929 2.2259 '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
C6 Se1 Ge1 96.92(4) . .
N1 Ge1 N1 82.89(6) 2_655 .
N1 Ge1 Se1 115.95(3) 2_655 2_655
N1 Ge1 Se1 120.03(3) . 2_655
N1 Ge1 Se1 120.03(3) 2_655 .
N1 Ge1 Se1 115.95(3) . .
Se1 Ge1 Se1 102.528(10) 2_655 .
N1 Ge1 Si1 41.44(3) 2_655 .
N1 Ge1 Si1 41.45(3) . .
Se1 Ge1 Si1 128.736(5) 2_655 .
Se1 Ge1 Si1 128.736(5) . .
N1 Si1 N1 89.00(6) 2_655 .
N1 Si1 C5 114.96(6) 2_655 .
N1 Si1 C5 115.16(6) . .
N1 Si1 C5 115.16(6) 2_655 2_655
N1 Si1 C5 114.96(6) . 2_655
C5 Si1 C5 107.14(9) . 2_655
N1 Si1 Ge1 44.50(3) 2_655 .
N1 Si1 Ge1 44.50(3) . .
C5 Si1 Ge1 126.43(5) . .
C5 Si1 Ge1 126.43(5) 2_655 .
C1 N1 Si1 132.47(8) . .
C1 N1 Ge1 130.79(7) . .
Si1 N1 Ge1 94.05(5) . .
N1 C1 C3 109.58(10) . .
N1 C1 C2 108.16(10) . .
C3 C1 C2 109.56(10) . .
N1 C1 C4 110.68(10) . .
C3 C1 C4 109.27(11) . .
C2 C1 C4 109.57(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 C6 1.9611(14) .
Se1 Ge1 2.34390(18) .
Ge1 N1 1.8451(9) 2_655
Ge1 N1 1.8452(9) .
Ge1 Se1 2.34389(18) 2_655
Ge1 Si1 2.6260(5) .
Si1 N1 1.7425(10) 2_655
Si1 N1 1.7425(10) .
Si1 C5 1.8604(13) .
Si1 C5 1.8604(13) 2_655
N1 C1 1.4708(15) .
C1 C3 1.5292(17) .
C1 C2 1.5295(17) .
C1 C4 1.5359(18) .