#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180274 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/60/7116056.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_7116056
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         'C14 H34 Ge N2 S2 Si'
_chemical_formula_sum            'C14 H34 Ge N2 S2 Si'
_chemical_formula_weight         395.23
_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                 105.1850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7422(4)
_cell_length_b                   12.1799(4)
_cell_length_c                   14.9598(5)
_cell_measurement_reflns_used    40476
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.13
_cell_measurement_theta_min      2.56
_cell_volume                     2064.83(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.986
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70543
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.135
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'sealed X-RAY tube'
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.59
_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    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         7162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0244P)²+0.4644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6538
_reflns_number_total             7162
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc07921c2.cif
_cod_data_source_block           pst_048m
_cod_database_code               7116056
#BEGIN Tags that were not found in dictionaries:
_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   0.691
_shelx_estimated_absorpt_t_max   0.780
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
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 0.70981(2) 0.75862(2) 0.01367(2) 0.01137(3) Uani 1 1 d . .
Si1 Si 0.92161(2) 0.76931(2) 0.12787(2) 0.01240(4) Uani 1 1 d . .
S1 S 0.58681(2) 0.89252(2) -0.04632(2) 0.01599(4) Uani 1 1 d . .
S2 S 0.60623(2) 0.61323(2) -0.04755(2) 0.01784(4) Uani 1 1 d . .
N1 N 0.86384(6) 0.77075(6) 0.00770(5) 0.01376(12) Uani 1 1 d . .
N2 N 0.77856(6) 0.75639(5) 0.13928(5) 0.01280(12) Uani 1 1 d . .
C1 C 0.91724(7) 0.75842(6) -0.07011(6) 0.01485(14) Uani 1 1 d . .
C2 C 1.03442(8) 0.82128(8) -0.04613(6) 0.02191(17) Uani 1 1 d . .
H2A H 1.0199 0.8984 -0.0341 0.033 Uiso 1 1 calc R U
H2B H 1.0705 0.8167 -0.0982 0.033 Uiso 1 1 calc R U
H2C H 1.0878 0.7889 0.0091 0.033 Uiso 1 1 calc R U
C3 C 0.94051(9) 0.63750(8) -0.08716(7) 0.02476(18) Uani 1 1 d . .
H3A H 0.9926 0.6059 -0.0309 0.037 Uiso 1 1 calc R U
H3B H 0.9782 0.6319 -0.1382 0.037 Uiso 1 1 calc R U
H3C H 0.8656 0.5973 -0.1033 0.037 Uiso 1 1 calc R U
C4 C 0.83533(8) 0.80665(9) -0.15809(6) 0.02420(18) Uani 1 1 d . .
H4A H 0.7598 0.7674 -0.1727 0.036 Uiso 1 1 calc R U
H4B H 0.8718 0.7988 -0.2096 0.036 Uiso 1 1 calc R U
H4C H 0.8218 0.8846 -0.1483 0.036 Uiso 1 1 calc R U
C5 C 0.72466(7) 0.77310(7) 0.21626(6) 0.01465(14) Uani 1 1 d . .
C6 C 0.60805(7) 0.70974(8) 0.19620(6) 0.02019(16) Uani 1 1 d . .
H6A H 0.5556 0.7357 0.1378 0.030 Uiso 1 1 calc R U
H6B H 0.5705 0.7218 0.2466 0.030 Uiso 1 1 calc R U
H6C H 0.6235 0.6312 0.1913 0.030 Uiso 1 1 calc R U
C7 C 0.70094(8) 0.89543(7) 0.22804(6) 0.02147(16) Uani 1 1 d . .
H7A H 0.7756 0.9360 0.2414 0.032 Uiso 1 1 calc R U
H7B H 0.6644 0.9048 0.2794 0.032 Uiso 1 1 calc R U
H7C H 0.6477 0.9236 0.1708 0.032 Uiso 1 1 calc R U
C8 C 0.80864(8) 0.72882(8) 0.30541(6) 0.02155(17) Uani 1 1 d . .
H8A H 0.8244 0.6509 0.2974 0.032 Uiso 1 1 calc R U
H8B H 0.7722 0.7373 0.3569 0.032 Uiso 1 1 calc R U
H8C H 0.8829 0.7700 0.3188 0.032 Uiso 1 1 calc R U
C9 C 1.02046(8) 0.65104(8) 0.17370(6) 0.02071(16) Uani 1 1 d . .
H9A H 1.0366 0.6489 0.2413 0.031 Uiso 1 1 calc R U
H9B H 1.0948 0.6595 0.1563 0.031 Uiso 1 1 calc R U
H9C H 0.9820 0.5826 0.1476 0.031 Uiso 1 1 calc R U
C10 C 0.99952(8) 0.89758(7) 0.17742(6) 0.02117(16) Uani 1 1 d . .
H10A H 0.9494 0.9611 0.1540 0.032 Uiso 1 1 calc R U
H10B H 1.0736 0.9038 0.1592 0.032 Uiso 1 1 calc R U
H10C H 1.0166 0.8953 0.2451 0.032 Uiso 1 1 calc R U
C11 C 0.68629(8) 1.01129(7) -0.02623(7) 0.02150(17) Uani 1 1 d . .
H11A H 0.6748 1.0546 0.0267 0.026 Uiso 1 1 d R U
H11B H 0.7693 0.9859 -0.0109 0.026 Uiso 1 1 d R U
C12 C 0.66101(9) 1.08251(8) -0.11239(8) 0.0304(2) Uani 1 1 d . .
H12A H 0.6780 1.0410 -0.1635 0.046 Uiso 1 1 calc R U
H12B H 0.7109 1.1482 -0.1001 0.046 Uiso 1 1 calc R U
H12C H 0.5778 1.1044 -0.1292 0.046 Uiso 1 1 calc R U
C13 C 0.69843(8) 0.50375(7) 0.01803(7) 0.02393(18) Uani 1 1 d . .
H13A H 0.7809 0.5298 0.0402 0.029 Uiso 1 1 d R U
H13B H 0.6700 0.4846 0.0728 0.029 Uiso 1 1 d R U
C14 C 0.69437(9) 0.40352(8) -0.04172(8) 0.0313(2) Uani 1 1 d . .
H14A H 0.6127 0.3778 -0.0636 0.047 Uiso 1 1 calc R U
H14B H 0.7431 0.3454 -0.0054 0.047 Uiso 1 1 calc R U
H14C H 0.7246 0.4221 -0.0950 0.047 Uiso 1 1 calc R U
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'
S S 0.1246 0.1234 '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
N1 Ge1 N2 82.93(3)
N1 Ge1 S2 119.09(2)
N2 Ge1 S2 117.28(2)
N1 Ge1 S1 117.89(2)
N2 Ge1 S1 119.42(2)
S2 Ge1 S1 101.148(9)
S2 Ge1 Si1 129.410(8)
S1 Ge1 Si1 129.441(8)
N2 Si1 N1 88.70(3)
N2 Si1 C10 115.02(4)
N1 Si1 C10 114.75(4)
N2 Si1 C9 114.72(4)
N1 Si1 C9 115.00(4)
C10 Si1 C9 107.94(4)
C10 Si1 Ge1 125.66(3)
C9 Si1 Ge1 126.39(3)
C11 S1 Ge1 101.26(3)
C13 S2 Ge1 100.23(3)
C1 N1 Si1 133.14(6)
C1 N1 Ge1 131.30(5)
Si1 N1 Ge1 94.07(4)
C5 N2 Si1 133.72(5)
C5 N2 Ge1 129.46(5)
Si1 N2 Ge1 94.30(4)
N1 C1 C4 109.90(7)
N1 C1 C3 111.25(7)
C4 C1 C3 108.99(8)
N1 C1 C2 107.89(7)
C4 C1 C2 109.46(7)
C3 C1 C2 109.33(7)
N2 C5 C6 108.89(7)
N2 C5 C8 108.82(7)
C6 C5 C8 109.35(7)
N2 C5 C7 110.71(7)
C6 C5 C7 109.39(7)
C8 C5 C7 109.65(7)
C12 C11 S1 109.71(6)
C14 C13 S2 110.47(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 N1 1.8400(7)
Ge1 N2 1.8410(7)
Ge1 S2 2.2070(2)
Ge1 S1 2.2072(2)
Ge1 Si1 2.6258(2)
Si1 N2 1.7394(8)
Si1 N1 1.7474(7)
Si1 C10 1.8634(9)
Si1 C9 1.8642(8)
S1 C11 1.8340(9)
S2 C13 1.8320(9)
N1 C1 1.4674(11)
N2 C5 1.4663(11)
C1 C4 1.5294(12)
C1 C3 1.5315(12)
C1 C2 1.5328(12)
C5 C6 1.5315(12)
C5 C8 1.5340(12)
C5 C7 1.5343(12)
C11 C12 1.5171(14)
C13 C14 1.5064(14)
