# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gb_166lt

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009920'


_ccdc_polymorph                  2


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H24 Ge N2 Si'
_chemical_formula_sum            'C10 H24 Ge N2 Si'
_chemical_formula_weight         272.99

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   11.4041(7)
_cell_length_b                   6.2297(4)
_cell_length_c                   20.3921(13)
_cell_angle_alpha                90
_cell_angle_beta                 102.231(2)
_cell_angle_gamma                90
_cell_volume                     1415.85(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    18660
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      30.69

_exptl_crystal_description       cylindric
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    2.220
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 The crystallization was performed on the diffractometer at a temperature of 
 230 K with a miniature zone melting procedure using focussed infrared-laser- 
 radiation according to: R. Boese, M. Nussbaumer, "In Situ Crystallization 
 Techniques", in: "Organic Crystal Chemistry", 
 Ed. D.W. Jones, Oxford University Press, Oxford, England, (1994) 20-37 
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            31948
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.895
_diffrn_reflns_theta_max         30.706
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4122
_reflns_number_gt                3618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+1.0274P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4122
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0701
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.29988(2) 0.20618(4) 0.19413(2) 0.01940(7) Uani 1 1 d . . . . .
Si1 Si 0.46251(4) 0.40735(8) 0.14168(2) 0.01566(10) Uani 1 1 d . . . . .
N1 N 0.45546(12) 0.3102(2) 0.22009(6) 0.0158(3) Uani 1 1 d . . . . .
N2 N 0.31879(12) 0.3103(2) 0.11160(6) 0.0170(3) Uani 1 1 d . . . . .
C1 C 0.53560(13) 0.3116(3) 0.28620(8) 0.0172(3) Uani 1 1 d . . . . .
C2 C 0.56605(16) 0.5427(3) 0.30886(8) 0.0249(4) Uani 1 1 d . . . . .
H2A H 0.6082 0.6127 0.2775 0.037 Uiso 1 1 calc R U . . .
H2B H 0.6176 0.5422 0.3539 0.037 Uiso 1 1 calc R U . . .
H2C H 0.4919 0.6212 0.3097 0.037 Uiso 1 1 calc R U . . .
C3 C 0.65157(16) 0.1913(4) 0.28336(10) 0.0292(4) Uani 1 1 d . . . . .
H3A H 0.6324 0.0432 0.2687 0.044 Uiso 1 1 calc R U . . .
H3B H 0.7045 0.1908 0.3280 0.044 Uiso 1 1 calc R U . . .
H3C H 0.6920 0.2629 0.2515 0.044 Uiso 1 1 calc R U . . .
C4 C 0.47339(16) 0.2020(3) 0.33648(8) 0.0245(4) Uani 1 1 d . . . . .
H4A H 0.3989 0.2784 0.3380 0.037 Uiso 1 1 calc R U . . .
H4B H 0.5265 0.2041 0.3811 0.037 Uiso 1 1 calc R U . . .
H4C H 0.4548 0.0530 0.3226 0.037 Uiso 1 1 calc R U . . .
C5 C 0.23685(14) 0.3059(3) 0.04576(8) 0.0183(3) Uani 1 1 d . . . . .
C6 C 0.12369(17) 0.1843(4) 0.05085(9) 0.0289(4) Uani 1 1 d . . . . .
H6A H 0.1444 0.0359 0.0646 0.043 Uiso 1 1 calc R U . . .
H6B H 0.0679 0.1847 0.0071 0.043 Uiso 1 1 calc R U . . .
H6C H 0.0858 0.2537 0.0842 0.043 Uiso 1 1 calc R U . . .
C7 C 0.29771(19) 0.1945(4) -0.00488(9) 0.0300(4) Uani 1 1 d . . . . .
H7A H 0.3681 0.2778 -0.0101 0.045 Uiso 1 1 calc R U . . .
H7B H 0.2412 0.1843 -0.0483 0.045 Uiso 1 1 calc R U . . .
H7C H 0.3229 0.0501 0.0112 0.045 Uiso 1 1 calc R U . . .
C8 C 0.20229(17) 0.5343(3) 0.02233(9) 0.0255(4) Uani 1 1 d . . . . .
H8A H 0.1636 0.6056 0.0550 0.038 Uiso 1 1 calc R U . . .
H8B H 0.1466 0.5298 -0.0214 0.038 Uiso 1 1 calc R U . . .
H8C H 0.2745 0.6142 0.0184 0.038 Uiso 1 1 calc R U . . .
C9 C 0.58185(16) 0.2862(4) 0.10358(10) 0.0262(4) Uani 1 1 d . . . . .
H9A H 0.6605 0.3382 0.1273 0.039 Uiso 1 1 calc R U . . .
H9B H 0.5687 0.3271 0.0562 0.039 Uiso 1 1 calc R U . . .
H9C H 0.5791 0.1295 0.1072 0.039 Uiso 1 1 calc R U . . .
C10 C 0.47567(19) 0.7036(3) 0.13661(10) 0.0279(4) Uani 1 1 d . . . . .
H10A H 0.4166 0.7717 0.1585 0.042 Uiso 1 1 calc R U . . .
H10B H 0.4608 0.7476 0.0894 0.042 Uiso 1 1 calc R U . . .
H10C H 0.5566 0.7479 0.1592 0.042 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ge1 N1 1.8574(13) . ?
Ge1 N2 1.8584(13) . ?
Ge1 Si1 2.6447(5) . ?
Si1 N1 1.7275(14) . ?
Si1 N2 1.7325(14) . ?
Si1 C10 1.856(2) . ?
Si1 C9 1.8639(19) . ?
N1 C1 1.4598(19) . ?
N2 C5 1.4645(19) . ?
C1 C4 1.526(2) . ?
C1 C2 1.529(3) . ?
C1 C3 1.532(2) . ?
C5 C6 1.519(2) . ?
C5 C8 1.526(3) . ?
C5 C7 1.527(2) . ?

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
N1 Ge1 N2 81.33(6) . . ?
N1 Si1 N2 88.82(6) . . ?
N1 Si1 C10 114.84(8) . . ?
N2 Si1 C10 114.12(9) . . ?
N1 Si1 C9 115.16(8) . . ?
N2 Si1 C9 115.52(8) . . ?
C10 Si1 C9 107.74(10) . . ?
C10 Si1 Ge1 124.44(7) . . ?
C9 Si1 Ge1 127.82(7) . . ?
C1 N1 Si1 135.23(11) . . ?
C1 N1 Ge1 129.70(11) . . ?
Si1 N1 Ge1 95.01(6) . . ?
C5 N2 Si1 134.68(11) . . ?
C5 N2 Ge1 130.51(11) . . ?
Si1 N2 Ge1 94.80(6) . . ?
N1 C1 C4 109.18(13) . . ?
N1 C1 C2 110.04(14) . . ?
C4 C1 C2 109.05(14) . . ?
N1 C1 C3 109.79(13) . . ?
C4 C1 C3 109.53(16) . . ?
C2 C1 C3 109.24(15) . . ?
N2 C5 C6 109.47(13) . . ?
N2 C5 C8 109.97(14) . . ?
C6 C5 C8 108.64(15) . . ?
N2 C5 C7 109.60(14) . . ?
C6 C5 C7 109.52(16) . . ?
C8 C5 C7 109.63(15) . . ?

_refine_diff_density_max         0.838
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gb_166m

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009921'


_ccdc_polymorph                  1

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H24 Ge N2 Si'
_chemical_formula_sum            'C10 H24 Ge N2 Si'
_chemical_formula_weight         272.99

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   12.9266(18)
_cell_length_b                   6.3714(11)
_cell_length_c                   18.087(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.704(8)
_cell_angle_gamma                90
_cell_volume                     1484.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(1)
_cell_measurement_reflns_used    3357
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.87

_exptl_crystal_description       cylindric
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    2.118
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 The crystallization was performed on the diffractometer at a temperature of 
 230 K with a miniature zone melting procedure using focussed infrared-laser- 
 radiation according to: R. Boese, M. Nussbaumer, "In Situ Crystallization 
 Techniques", in: "Organic Crystal Chemistry", 
 Ed. D.W. Jones, Oxford University Press, Oxford, England, (1994) 20-37 
;

_diffrn_ambient_temperature      230(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            13962
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.866
_diffrn_reflns_theta_max         30.669
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measured_fraction_theta_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_point_group_measured_fraction_full 0.891
_reflns_number_total             3739
_reflns_number_gt                2201
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1358P)²+1.3024P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3739
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2562
_refine_ls_wR_factor_gt          0.1985
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_vrf_PLAT029_gb_166m             
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......       0.82      
RESPONSE:
 The low coverage resulted from the orientation
 of the cylindric crystal and the chosen scan mode,
 both due to the in situ crystal growing technique.
 Any other mounting of the crystal / scan mode
 would lead to a melting of the crystal.
;

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
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) . ?

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
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) . . ?

_refine_diff_density_max         1.355
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.166

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_014s

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009922'

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H58 Ge2 N4 S2 Si2'
_chemical_formula_sum            'C24 H58 Ge2 N4 S2 Si2'
_chemical_formula_weight         668.22

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'
Ge Ge 0.1547 1.8001 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9171(8)
_cell_length_b                   17.7348(12)
_cell_length_c                   17.6945(10)
_cell_angle_alpha                90
_cell_angle_beta                 109.874(4)
_cell_angle_gamma                90
_cell_volume                     3517.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(1)
_cell_measurement_reflns_used    40556
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    1.915
_shelx_estimated_absorpt_T_min   0.530
_shelx_estimated_absorpt_T_max   0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      180(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            81721
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.817
_diffrn_reflns_theta_max         32.890
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             13009
_reflns_number_gt                10491
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Refined as a 2-component twin.
 The structure is pseudo orthorhombic twinned
 by the twin law 1 0 0 0 -1 0 -1 0 -1
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 Disorder
 t-butyl carbon atoms C(12-14) disordered over 
 two sites with occupancies factor 0.5 
 together with the riding hydrogen atoms.
 t-butyl carbon atoms C(6-8) disordered over 
 two sites with occupancies factor 0.75 and 0.25
 together with the riding hydrogen atoms.
 ethyl carbon atoms C(21, 22) disordered over 
 two sites with occupancies factor 0.5 
 together with the riding hydrogen atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+14.8765P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13009
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_vrf_PLAT201_pst_014s            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s)
RESPONSE:
  some carbon atoms disordered over two sites with SOF 0.5
;

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.29426(4) 0.32966(2) 0.23351(3) 0.02044(8) Uani 1 1 d . . . . .
Ge2 Ge 0.13528(4) 0.39147(2) 0.27161(3) 0.02286(9) Uani 1 1 d . . . . .
Si1 Si 0.52622(11) 0.34867(7) 0.27021(10) 0.0330(3) Uani 1 1 d . . . . .
Si2 Si 0.00933(13) 0.51612(7) 0.22805(9) 0.0335(3) Uani 1 1 d . . . . .
S1 S 0.19549(11) 0.24210(7) 0.14589(8) 0.0361(3) Uani 1 1 d . . . . .
S2 S 0.11054(12) 0.31169(8) 0.36202(8) 0.0384(3) Uani 1 1 d . . . . .
N1 N 0.4354(3) 0.2956(2) 0.3086(2) 0.0255(7) Uani 1 1 d . . . . .
N2 N 0.3985(3) 0.3866(2) 0.2002(3) 0.0310(8) Uani 1 1 d . . . . .
N3 N 0.1477(4) 0.4926(2) 0.2984(2) 0.0329(8) Uani 1 1 d . . . . .
N4 N -0.0063(3) 0.4227(2) 0.1958(2) 0.0247(7) Uani 1 1 d . . . . .
C1 C 0.4617(4) 0.2457(3) 0.3781(3) 0.0328(9) Uani 1 1 d . . . . .
C2 C 0.4627(6) 0.2894(4) 0.4527(3) 0.0506(14) Uani 1 1 d . . . . .
H2A H 0.5231 0.3292 0.4641 0.076 Uiso 1 1 calc R U . . .
H2B H 0.4815 0.2549 0.4986 0.076 Uiso 1 1 calc R U . . .
H2C H 0.3840 0.3120 0.4432 0.076 Uiso 1 1 calc R U . . .
C3 C 0.3659(5) 0.1838(3) 0.3615(3) 0.0401(11) Uani 1 1 d . . . . .
H3A H 0.2871 0.2071 0.3491 0.060 Uiso 1 1 calc R U . . .
H3B H 0.3823 0.1516 0.4091 0.060 Uiso 1 1 calc R U . . .
H3C H 0.3673 0.1531 0.3158 0.060 Uiso 1 1 calc R U . . .
C4 C 0.5840(5) 0.2087(4) 0.3941(4) 0.0556(16) Uani 1 1 d . . . . .
H4A H 0.5836 0.1802 0.3466 0.083 Uiso 1 1 calc R U . . .
H4B H 0.6010 0.1744 0.4401 0.083 Uiso 1 1 calc R U . . .
H4C H 0.6457 0.2478 0.4060 0.083 Uiso 1 1 calc R U . . .
C5 C 0.3764(5) 0.4401(3) 0.1334(3) 0.0365(11) Uani 1 1 d . . . . .
C6 C 0.4870(8) 0.4950(5) 0.1561(6) 0.057(2) Uiso 0.75 1 d . . P A 1
H6A H 0.4817 0.5270 0.1099 0.086 Uiso 0.75 1 calc R U P A 1
H6B H 0.5607 0.4653 0.1710 0.086 Uiso 0.75 1 calc R U P A 1
H6C H 0.4874 0.5267 0.2016 0.086 Uiso 0.75 1 calc R U P A 1
C7 C 0.2710(7) 0.4871(4) 0.1246(5) 0.0415(15) Uiso 0.75 1 d . . P A 1
H7A H 0.2650 0.5267 0.0848 0.062 Uiso 0.75 1 calc R U P A 1
H7B H 0.2787 0.5102 0.1764 0.062 Uiso 0.75 1 calc R U P A 1
H7C H 0.1992 0.4556 0.1068 0.062 Uiso 0.75 1 calc R U P A 1
C8 C 0.3714(10) 0.3996(6) 0.0601(6) 0.066(3) Uiso 0.75 1 d . . P A 1
H8A H 0.4445 0.3700 0.0703 0.100 Uiso 0.75 1 calc R U P A 1
H8B H 0.3641 0.4359 0.0169 0.100 Uiso 0.75 1 calc R U P A 1
H8C H 0.3022 0.3657 0.0440 0.100 Uiso 0.75 1 calc R U P A 1
C6A C 0.344(3) 0.5120(15) 0.1616(17) 0.054(6) Uiso 0.25 1 d . . P A 2
H6A1 H 0.2734 0.5049 0.1771 0.081 Uiso 0.25 1 calc R U P A 2
H6A2 H 0.3270 0.5495 0.1184 0.081 Uiso 0.25 1 calc R U P A 2
H6A3 H 0.4107 0.5297 0.2081 0.081 Uiso 0.25 1 calc R U P A 2
C7A C 0.253(3) 0.4152(18) 0.0582(18) 0.063(7) Uiso 0.25 1 d . . P A 2
H7A1 H 0.1904 0.4020 0.0798 0.094 Uiso 0.25 1 calc R U P A 2
H7A2 H 0.2709 0.3716 0.0301 0.094 Uiso 0.25 1 calc R U P A 2
H7A3 H 0.2268 0.4574 0.0205 0.094 Uiso 0.25 1 calc R U P A 2
C8A C 0.470(2) 0.4457(14) 0.0990(15) 0.047(5) Uiso 0.25 1 d . . P A 2
H8A1 H 0.4555 0.4899 0.0638 0.071 Uiso 0.25 1 calc R U P A 2
H8A2 H 0.4699 0.4001 0.0678 0.071 Uiso 0.25 1 calc R U P A 2
H8A3 H 0.5469 0.4508 0.1421 0.071 Uiso 0.25 1 calc R U P A 2
C9 C 0.6204(5) 0.2922(3) 0.2258(4) 0.0505(15) Uani 1 1 d . . . . .
H9A H 0.5783 0.2457 0.2025 0.076 Uiso 1 1 calc R U . . .
H9B H 0.6960 0.2795 0.2678 0.076 Uiso 1 1 calc R U . . .
H9C H 0.6363 0.3217 0.1837 0.076 Uiso 1 1 calc R U . . .
C10 C 0.6267(5) 0.4172(4) 0.3404(5) 0.064(2) Uani 1 1 d . . . . .
H10A H 0.6700 0.4463 0.3120 0.096 Uiso 1 1 calc R U . . .
H10B H 0.6839 0.3901 0.3854 0.096 Uiso 1 1 calc R U . . .
H10C H 0.5794 0.4516 0.3609 0.096 Uiso 1 1 calc R U . . .
C11 C 0.2329(6) 0.5335(3) 0.3649(4) 0.0525(16) Uani 1 1 d . . . . .
C12 C 0.2560(14) 0.6146(8) 0.3297(9) 0.056(3) Uiso 0.5 1 d . . P B 1
H12A H 0.3102 0.6447 0.3734 0.084 Uiso 0.5 1 calc R U P B 1
H12B H 0.1799 0.6412 0.3067 0.084 Uiso 0.5 1 calc R U P B 1
H12C H 0.2918 0.6066 0.2880 0.084 Uiso 0.5 1 calc R U P B 1
C13 C 0.1864(17) 0.5496(11) 0.4289(11) 0.073(5) Uiso 0.5 1 d . . P B 1
H13A H 0.1403 0.5062 0.4365 0.110 Uiso 0.5 1 calc R U P B 1
H13B H 0.1347 0.5941 0.4148 0.110 Uiso 0.5 1 calc R U P B 1
H13C H 0.2528 0.5593 0.4788 0.110 Uiso 0.5 1 calc R U P B 1
C14 C 0.3390(15) 0.4909(9) 0.4014(10) 0.061(4) Uiso 0.5 1 d . . P B 1
H14A H 0.3189 0.4435 0.4221 0.091 Uiso 0.5 1 calc R U P B 1
H14B H 0.3940 0.5200 0.4457 0.091 Uiso 0.5 1 calc R U P B 1
H14C H 0.3770 0.4801 0.3614 0.091 Uiso 0.5 1 calc R U P B 1
C12A C 0.2211(17) 0.6134(10) 0.3561(12) 0.076(5) Uiso 0.5 1 d . . P B 2
H12D H 0.1661 0.6255 0.3022 0.114 Uiso 0.5 1 calc R U P B 2
H12E H 0.2994 0.6357 0.3636 0.114 Uiso 0.5 1 calc R U P B 2
H12F H 0.1898 0.6337 0.3964 0.114 Uiso 0.5 1 calc R U P B 2
C13A C 0.195(2) 0.5116(14) 0.4445(13) 0.095(7) Uiso 0.5 1 d . . P B 2
H13D H 0.1293 0.5438 0.4458 0.143 Uiso 0.5 1 calc R U P B 2
H13E H 0.2642 0.5194 0.4936 0.143 Uiso 0.5 1 calc R U P B 2
H13F H 0.1708 0.4586 0.4411 0.143 Uiso 0.5 1 calc R U P B 2
C14A C 0.3601(11) 0.5023(7) 0.3792(8) 0.042(2) Uiso 0.5 1 d . . P B 2
H14D H 0.3621 0.4484 0.3916 0.063 Uiso 0.5 1 calc R U P B 2
H14E H 0.4176 0.5291 0.4242 0.063 Uiso 0.5 1 calc R U P B 2
H14F H 0.3808 0.5096 0.3306 0.063 Uiso 0.5 1 calc R U P B 2
C15 C -0.0947(4) 0.3847(3) 0.1274(3) 0.0306(9) Uani 1 1 d . . . . .
C16 C -0.2157(4) 0.4239(4) 0.1109(4) 0.0461(13) Uani 1 1 d . . . . .
H16A H -0.2390 0.4206 0.1588 0.069 Uiso 1 1 calc R U . . .
H16B H -0.2761 0.3990 0.0657 0.069 Uiso 1 1 calc R U . . .
H16C H -0.2091 0.4769 0.0976 0.069 Uiso 1 1 calc R U . . .
C17 C -0.0593(5) 0.3897(3) 0.0524(3) 0.0416(11) Uani 1 1 d . . . . .
H17A H -0.0513 0.4428 0.0396 0.062 Uiso 1 1 calc R U . . .
H17B H -0.1207 0.3656 0.0072 0.062 Uiso 1 1 calc R U . . .
H17C H 0.0171 0.3639 0.0623 0.062 Uiso 1 1 calc R U . . .
C18 C -0.1063(5) 0.3019(3) 0.1478(4) 0.0397(11) Uani 1 1 d . . . . .
H18A H -0.0298 0.2763 0.1576 0.060 Uiso 1 1 calc R U . . .
H18B H -0.1678 0.2776 0.1028 0.060 Uiso 1 1 calc R U . . .
H18C H -0.1288 0.2988 0.1961 0.060 Uiso 1 1 calc R U . . .
C19 C -0.1050(6) 0.5489(4) 0.2715(5) 0.0601(18) Uani 1 1 d . . . . .
H19A H -0.1146 0.5109 0.3090 0.090 Uiso 1 1 calc R U . . .
H19B H -0.1814 0.5565 0.2282 0.090 Uiso 1 1 calc R U . . .
H19C H -0.0790 0.5966 0.3002 0.090 Uiso 1 1 calc R U . . .
C20 C 0.0111(6) 0.5878(3) 0.1509(4) 0.0533(15) Uani 1 1 d . . . . .
H20A H 0.0218 0.6382 0.1750 0.080 Uiso 1 1 calc R U . . .
H20B H -0.0646 0.5859 0.1059 0.080 Uiso 1 1 calc R U . . .
H20C H 0.0771 0.5769 0.1313 0.080 Uiso 1 1 calc R U . . .
C23 C -0.0183(6) 0.3522(4) 0.3813(4) 0.0514(16) Uani 1 1 d . . . . .
H23A H 0.0033 0.4021 0.4072 0.062 Uiso 1 1 calc R U . . .
H23B H -0.0845 0.3594 0.3298 0.062 Uiso 1 1 calc R U . . .
C24 C -0.0575(6) 0.3014(5) 0.4344(4) 0.064(2) Uani 1 1 d . . . . .
H24A H -0.0828 0.2530 0.4073 0.096 Uiso 1 1 calc R U . . .
H24B H -0.1243 0.3246 0.4462 0.096 Uiso 1 1 calc R U . . .
H24C H 0.0090 0.2932 0.4846 0.096 Uiso 1 1 calc R U . . .
C21A C 0.3291(13) 0.1958(8) 0.1319(9) 0.052(3) Uiso 0.5 1 d . . P C 1
H21A H 0.3590 0.2273 0.0966 0.062 Uiso 0.5 1 calc R U P C 1
H21B H 0.3937 0.1907 0.1845 0.062 Uiso 0.5 1 calc R U P C 1
C22A C 0.2948(14) 0.1208(8) 0.0954(9) 0.059(3) Uiso 0.5 1 d . . P C 1
H22A H 0.2170 0.1241 0.0525 0.088 Uiso 0.5 1 calc R U P C 1
H22B H 0.2898 0.0853 0.1366 0.088 Uiso 0.5 1 calc R U P C 1
H22C H 0.3548 0.1032 0.0730 0.088 Uiso 0.5 1 calc R U P C 1
C21 C 0.3000(9) 0.2077(5) 0.1006(6) 0.0265(16) Uiso 0.5 1 d . . P C 2
H21C H 0.2591 0.2029 0.0418 0.032 Uiso 0.5 1 calc R U P C 2
H21D H 0.3654 0.2448 0.1097 0.032 Uiso 0.5 1 calc R U P C 2
C22 C 0.3527(12) 0.1314(7) 0.1347(8) 0.050(3) Uiso 0.5 1 d . . P C 2
H22D H 0.4100 0.1154 0.1092 0.074 Uiso 0.5 1 calc R U P C 2
H22E H 0.2886 0.0940 0.1239 0.074 Uiso 0.5 1 calc R U P C 2
H22F H 0.3934 0.1359 0.1928 0.074 Uiso 0.5 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ge1 N2 1.845(4) . ?
Ge1 N1 1.855(3) . ?
Ge1 S1 2.2271(13) . ?
Ge1 Ge2 2.4727(6) . ?
Ge1 Si1 2.6374(13) . ?
Ge2 N3 1.847(4) . ?
Ge2 N4 1.847(4) . ?
Ge2 S2 2.2290(12) . ?
Ge2 Si2 2.6358(13) . ?
Si1 N1 1.737(4) . ?
Si1 N2 1.738(4) . ?
Si1 C10 1.856(7) . ?
Si1 C9 1.866(6) . ?
Si2 N4 1.741(4) . ?
Si2 N3 1.746(4) . ?
Si2 C20 1.871(6) . ?
Si2 C19 1.871(6) . ?
S1 C21 1.801(9) . ?
S1 C21A 1.881(14) . ?
S2 C23 1.829(5) . ?
N1 C1 1.460(6) . ?
N2 C5 1.469(6) . ?
N3 C11 1.460(7) . ?
N4 C15 1.471(6) . ?
C1 C2 1.527(7) . ?
C1 C4 1.535(7) . ?
C1 C3 1.539(7) . ?
C5 C8A 1.44(2) . ?
C5 C6A 1.47(3) . ?
C5 C8 1.468(11) . ?
C5 C7 1.470(9) . ?
C5 C6 1.577(11) . ?
C5 C7A 1.67(3) . ?
C11 C14 1.425(17) . ?
C11 C12A 1.426(19) . ?
C11 C13 1.449(19) . ?
C11 C14A 1.551(14) . ?
C11 C12 1.626(16) . ?
C11 C13A 1.66(2) . ?
C15 C17 1.525(7) . ?
C15 C18 1.530(7) . ?
C15 C16 1.535(6) . ?
C23 C24 1.487(8) . ?
C21A C22A 1.47(2) . ?
C21 C22 1.528(16) . ?

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
N2 Ge1 N1 82.05(16) . . ?
N2 Ge1 S1 114.39(14) . . ?
N1 Ge1 S1 114.03(12) . . ?
N2 Ge1 Ge2 120.39(12) . . ?
N1 Ge1 Ge2 122.81(12) . . ?
S1 Ge1 Ge2 103.08(4) . . ?
N2 Ge1 Si1 41.04(12) . . ?
N1 Ge1 Si1 41.05(12) . . ?
S1 Ge1 Si1 121.48(5) . . ?
Ge2 Ge1 Si1 135.42(4) . . ?
N3 Ge2 N4 82.47(17) . . ?
N3 Ge2 S2 116.80(13) . . ?
N4 Ge2 S2 113.60(12) . . ?
N3 Ge2 Ge1 119.85(14) . . ?
N4 Ge2 Ge1 122.02(11) . . ?
S2 Ge2 Ge1 102.41(4) . . ?
N3 Ge2 Si2 41.33(14) . . ?
N4 Ge2 Si2 41.20(12) . . ?
S2 Ge2 Si2 122.76(5) . . ?
Ge1 Ge2 Si2 134.83(4) . . ?
N1 Si1 N2 88.69(17) . . ?
N1 Si1 C10 116.1(3) . . ?
N2 Si1 C10 115.7(3) . . ?
N1 Si1 C9 114.7(2) . . ?
N2 Si1 C9 114.5(3) . . ?
C10 Si1 C9 106.8(3) . . ?
N1 Si1 Ge1 44.53(12) . . ?
N2 Si1 Ge1 44.21(12) . . ?
C10 Si1 Ge1 129.2(2) . . ?
C9 Si1 Ge1 123.9(2) . . ?
N4 Si2 N3 88.59(18) . . ?
N4 Si2 C20 115.7(3) . . ?
N3 Si2 C20 116.1(3) . . ?
N4 Si2 C19 114.8(3) . . ?
N3 Si2 C19 115.2(3) . . ?
C20 Si2 C19 106.2(3) . . ?
N4 Si2 Ge2 44.33(12) . . ?
N3 Si2 Ge2 44.33(13) . . ?
C20 Si2 Ge2 129.5(2) . . ?
C19 Si2 Ge2 124.2(2) . . ?
C21 S1 Ge1 105.3(3) . . ?
C21A S1 Ge1 97.2(4) . . ?
C23 S2 Ge2 102.02(19) . . ?
C1 N1 Si1 132.4(3) . . ?
C1 N1 Ge1 133.1(3) . . ?
Si1 N1 Ge1 94.43(18) . . ?
C5 N2 Si1 134.2(3) . . ?
C5 N2 Ge1 130.9(3) . . ?
Si1 N2 Ge1 94.75(18) . . ?
C11 N3 Si2 133.2(3) . . ?
C11 N3 Ge2 131.5(3) . . ?
Si2 N3 Ge2 94.3(2) . . ?
C15 N4 Si2 132.2(3) . . ?
C15 N4 Ge2 133.0(3) . . ?
Si2 N4 Ge2 94.48(18) . . ?
N1 C1 C2 110.9(4) . . ?
N1 C1 C4 109.5(4) . . ?
C2 C1 C4 109.2(5) . . ?
N1 C1 C3 109.8(4) . . ?
C2 C1 C3 108.3(5) . . ?
C4 C1 C3 109.1(4) . . ?
C8A C5 C6A 114.4(16) . . ?
C8A C5 N2 115.5(11) . . ?
C6A C5 N2 106.5(11) . . ?
C8 C5 N2 109.7(5) . . ?
C8 C5 C7 114.0(7) . . ?
N2 C5 C7 111.4(5) . . ?
C8 C5 C6 107.9(6) . . ?
N2 C5 C6 106.8(5) . . ?
C7 C5 C6 106.7(5) . . ?
C8A C5 C7A 106.0(15) . . ?
C6A C5 C7A 104.0(16) . . ?
N2 C5 C7A 109.8(11) . . ?
C14 C11 C13 105.4(11) . . ?
C14 C11 N3 111.6(8) . . ?
C12A C11 N3 113.0(9) . . ?
C13 C11 N3 112.5(9) . . ?
C12A C11 C14A 115.3(10) . . ?
N3 C11 C14A 109.1(6) . . ?
C14 C11 C12 113.7(10) . . ?
C13 C11 C12 106.5(10) . . ?
N3 C11 C12 107.1(7) . . ?
C12A C11 C13A 106.2(12) . . ?
N3 C11 C13A 104.7(10) . . ?
C14A C11 C13A 107.9(10) . . ?
N4 C15 C17 110.9(4) . . ?
N4 C15 C18 110.0(4) . . ?
C17 C15 C18 109.6(4) . . ?
N4 C15 C16 108.2(4) . . ?
C17 C15 C16 109.2(4) . . ?
C18 C15 C16 108.9(4) . . ?
C24 C23 S2 110.1(4) . . ?
C22A C21A S1 109.3(10) . . ?
C22 C21 S1 112.2(7) . . ?

_refine_diff_density_max         0.779
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.105

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_022m

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009923'

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H30 Ge N2 Se2 Si'
_chemical_formula_sum            'C12 H30 Ge N2 Se2 Si'
_chemical_formula_weight         460.98

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   15.3441(8)
_cell_length_b                   9.0775(5)
_cell_length_c                   13.8753(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.731(2)
_cell_angle_gamma                90
_cell_volume                     1915.07(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    15465
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      30.63

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    5.453
_shelx_estimated_absorpt_T_min   0.495
_shelx_estimated_absorpt_T_max   0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            31347
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.613
_diffrn_reflns_theta_max         30.884
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2949
_reflns_number_gt                2653
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0176P)²+1.2813P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2949
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0385
_refine_ls_wR_factor_gt          0.0372
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
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) . ?

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
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) . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_034m

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009924'

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H34 Ge N2 Se2 Si'
_chemical_formula_sum            'C14 H34 Ge N2 Se2 Si'
_chemical_formula_weight         489.03

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   11.8560(15)
_cell_length_b                   12.2706(16)
_cell_length_c                   15.0579(19)
_cell_angle_alpha                90
_cell_angle_beta                 104.574(3)
_cell_angle_gamma                90
_cell_volume                     2120.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      30.07

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    4.930
_shelx_estimated_absorpt_T_min   0.339
_shelx_estimated_absorpt_T_max   0.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            29485
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.170
_diffrn_reflns_theta_max         30.758
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6538
_reflns_number_gt                5153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+2.0978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6538
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.89837(2) 0.40010(2) 0.55395(2) 0.01750(6) Uani 1 1 d . . . . .
Se2 Se 0.92207(2) 0.10502(2) 0.55184(2) 0.01502(6) Uani 1 1 d . . . . .
Ge1 Ge 0.79290(2) 0.24575(2) 0.49091(2) 0.01085(6) Uani 1 1 d . . . . .
Si1 Si 0.58423(5) 0.23215(5) 0.37874(4) 0.01243(12) Uani 1 1 d . . . . .
N1 N 0.72510(16) 0.24809(14) 0.36644(13) 0.0123(4) Uani 1 1 d . . . . .
N2 N 0.64066(16) 0.23114(15) 0.49747(13) 0.0133(4) Uani 1 1 d . . . . .
C1 C 0.77895(19) 0.23248(19) 0.28941(15) 0.0150(4) Uani 1 1 d . . . . .
C2 C 0.8941(2) 0.2951(2) 0.30922(17) 0.0216(5) Uani 1 1 d . . . . .
H2A H 0.8790 0.3729 0.3151 0.032 Uiso 1 1 calc R U . . .
H2B H 0.9313 0.2840 0.2587 0.032 Uiso 1 1 calc R U . . .
H2C H 0.9457 0.2684 0.3665 0.032 Uiso 1 1 calc R U . . .
C3 C 0.8020(2) 0.1114(2) 0.27640(18) 0.0231(5) Uani 1 1 d . . . . .
H3A H 0.8564 0.0833 0.3318 0.035 Uiso 1 1 calc R U . . .
H3B H 0.8357 0.1025 0.2238 0.035 Uiso 1 1 calc R U . . .
H3C H 0.7285 0.0710 0.2654 0.035 Uiso 1 1 calc R U . . .
C4 C 0.6958(2) 0.2771(2) 0.20230(17) 0.0220(5) Uani 1 1 d . . . . .
H4A H 0.6225 0.2361 0.1895 0.033 Uiso 1 1 calc R U . . .
H4B H 0.7315 0.2694 0.1506 0.033 Uiso 1 1 calc R U . . .
H4C H 0.6802 0.3542 0.2110 0.033 Uiso 1 1 calc R U . . .
C5 C 0.5868(2) 0.24320(18) 0.57448(16) 0.0148(4) Uani 1 1 d . . . . .
C6 C 0.6682(2) 0.1972(2) 0.66236(16) 0.0239(5) Uani 1 1 d . . . . .
H6A H 0.6831 0.1199 0.6534 0.036 Uiso 1 1 calc R U . . .
H6B H 0.6315 0.2050 0.7135 0.036 Uiso 1 1 calc R U . . .
H6C H 0.7421 0.2373 0.6763 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5616(2) 0.3627(2) 0.59062(18) 0.0236(5) Uani 1 1 d . . . . .
H7A H 0.6351 0.4033 0.6077 0.035 Uiso 1 1 calc R U . . .
H7B H 0.5219 0.3678 0.6402 0.035 Uiso 1 1 calc R U . . .
H7C H 0.5117 0.3936 0.5343 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4727(2) 0.1788(2) 0.55177(17) 0.0216(5) Uani 1 1 d . . . . .
H8A H 0.4190 0.2107 0.4977 0.032 Uiso 1 1 calc R U . . .
H8B H 0.4375 0.1817 0.6040 0.032 Uiso 1 1 calc R U . . .
H8C H 0.4886 0.1028 0.5390 0.032 Uiso 1 1 calc R U . . .
C9 C 0.5104(2) 0.1037(2) 0.33056(17) 0.0220(5) Uani 1 1 d . . . . .
H9A H 0.4932 0.1060 0.2634 0.033 Uiso 1 1 calc R U . . .
H9B H 0.4376 0.0957 0.3495 0.033 Uiso 1 1 calc R U . . .
H9C H 0.5615 0.0416 0.3534 0.033 Uiso 1 1 calc R U . . .
C10 C 0.4834(2) 0.3467(2) 0.33340(17) 0.0213(5) Uani 1 1 d . . . . .
H10A H 0.5184 0.4154 0.3601 0.032 Uiso 1 1 calc R U . . .
H10B H 0.4094 0.3353 0.3498 0.032 Uiso 1 1 calc R U . . .
H10C H 0.4694 0.3498 0.2665 0.032 Uiso 1 1 calc R U . . .
C11 C 0.7945(2) 0.5097(2) 0.47902(18) 0.0236(5) Uani 1 1 d . . . . .
H11A H 0.8202 0.5248 0.4226 0.028 Uiso 1 1 calc R U . . .
H11B H 0.7140 0.4809 0.4607 0.028 Uiso 1 1 calc R U . . .
C12 C 0.7962(2) 0.6130(2) 0.5320(2) 0.0315(6) Uani 1 1 d . . . . .
H12A H 0.7667 0.5988 0.5862 0.047 Uiso 1 1 calc R U . . .
H12B H 0.7467 0.6675 0.4931 0.047 Uiso 1 1 calc R U . . .
H12C H 0.8762 0.6405 0.5515 0.047 Uiso 1 1 calc R U . . .
C13 C 0.8099(2) -0.01665(19) 0.53233(18) 0.0208(5) Uani 1 1 d . . . . .
H13A H 0.7294 0.0124 0.5178 0.025 Uiso 1 1 calc R U . . .
H13B H 0.8186 -0.0614 0.4797 0.025 Uiso 1 1 calc R U . . .
C14 C 0.8308(2) -0.0865(2) 0.6173(2) 0.0303(6) Uani 1 1 d . . . . .
H14A H 0.9107 -0.1147 0.6318 0.045 Uiso 1 1 calc R U . . .
H14B H 0.7758 -0.1475 0.6066 0.045 Uiso 1 1 calc R U . . .
H14C H 0.8197 -0.0426 0.6688 0.045 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Se1 C11 1.975(2) . ?
Se1 Ge1 2.3355(4) . ?
Se2 C13 1.972(2) . ?
Se2 Ge1 2.3371(4) . ?
Ge1 N2 1.8411(18) . ?
Ge1 N1 1.8444(19) . ?
Ge1 Si1 2.6264(7) . ?
Si1 N1 1.7372(19) . ?
Si1 N2 1.744(2) . ?
Si1 C9 1.860(2) . ?
Si1 C10 1.860(2) . ?
N1 C1 1.470(3) . ?
N2 C5 1.465(3) . ?
C1 C2 1.529(3) . ?
C1 C4 1.530(3) . ?
C1 C3 1.532(3) . ?
C5 C7 1.528(3) . ?
C5 C8 1.529(3) . ?
C5 C6 1.536(3) . ?
C11 C12 1.495(4) . ?
C13 C14 1.508(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
C11 Se1 Ge1 97.30(7) . . ?
C13 Se2 Ge1 98.64(7) . . ?
N2 Ge1 N1 82.74(8) . . ?
N2 Ge1 Se1 119.28(6) . . ?
N1 Ge1 Se1 116.89(6) . . ?
N2 Ge1 Se2 117.48(6) . . ?
N1 Ge1 Se2 119.04(6) . . ?
Se1 Ge1 Se2 102.047(15) . . ?
Se1 Ge1 Si1 129.366(18) . . ?
Se2 Ge1 Si1 128.582(18) . . ?
N1 Si1 N2 88.80(9) . . ?
N1 Si1 C9 115.12(10) . . ?
N2 Si1 C9 114.54(11) . . ?
N1 Si1 C10 114.96(10) . . ?
N2 Si1 C10 115.27(10) . . ?
C9 Si1 C10 107.56(12) . . ?
C9 Si1 Ge1 125.41(9) . . ?
C10 Si1 Ge1 127.03(9) . . ?
C1 N1 Si1 133.58(15) . . ?
C1 N1 Ge1 129.41(14) . . ?
Si1 N1 Ge1 94.29(9) . . ?
C5 N2 Si1 132.80(15) . . ?
C5 N2 Ge1 131.37(15) . . ?
Si1 N2 Ge1 94.16(9) . . ?
N1 C1 C2 108.91(18) . . ?
N1 C1 C4 108.42(18) . . ?
C2 C1 C4 109.8(2) . . ?
N1 C1 C3 110.72(18) . . ?
C2 C1 C3 109.47(19) . . ?
C4 C1 C3 109.5(2) . . ?
N2 C5 C7 111.37(18) . . ?
N2 C5 C8 107.93(19) . . ?
C7 C5 C8 109.51(19) . . ?
N2 C5 C6 109.89(18) . . ?
C7 C5 C6 108.8(2) . . ?
C8 C5 C6 109.36(19) . . ?
C12 C11 Se1 110.47(18) . . ?
C14 C13 Se2 110.05(17) . . ?

_refine_diff_density_max         1.072
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.112

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_048m

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1009925'

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H34 Ge N2 S2 Si'
_chemical_formula_sum            'C14 H34 Ge N2 S2 Si'
_chemical_formula_weight         395.23

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   11.7422(4)
_cell_length_b                   12.1799(4)
_cell_length_c                   14.9598(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.1850(10)
_cell_angle_gamma                90
_cell_volume                     2064.83(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    40476
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      32.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.739
_shelx_estimated_absorpt_T_min   0.691
_shelx_estimated_absorpt_T_max   0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            70543
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.188
_diffrn_reflns_theta_max         32.135
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7162
_reflns_number_gt                6538
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+0.4644P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7162
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0486
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
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) . ?

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
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) . . ?

_refine_diff_density_max         0.426
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-4

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_074m

_database_code_CSD               ?
_database_code_depnum_ccdc_archive 'CCDC 1019789'

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H58 Ge2 N4 Se2 Si2'
_chemical_formula_sum            'C24 H58 Ge2 N4 Se2 Si2'
_chemical_formula_weight         762.02

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.9600(7)
_cell_length_b                   18.0926(11)
_cell_length_c                   18.1839(11)
_cell_angle_alpha                113.426(3)
_cell_angle_beta                 90.896(3)
_cell_angle_gamma                99.856(3)
_cell_volume                     3541.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    23513
_cell_measurement_theta_min      2.297
_cell_measurement_theta_max      28.114

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.839
_shelx_estimated_absorpt_T_min   0.413
_shelx_estimated_absorpt_T_max   0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            101681
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.349
_diffrn_reflns_theta_max         28.178
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             17182
_reflns_number_gt                12899
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'SHELXL-2014/5 (Sheldrick, 2014)'
_refine_special_details          
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²+7.4020P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17182
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.20649(3) 0.60449(2) 0.16401(2) 0.01668(8) Uani 1 1 d . . . . .
Ge1 Ge 0.17353(3) 0.72053(2) 0.27596(2) 0.01197(8) Uani 1 1 d . . . . .
Si1 Si 0.33514(8) 0.81791(6) 0.39067(6) 0.0191(2) Uani 1 1 d . . . . .
N1 N 0.2800(2) 0.81582(17) 0.30095(18) 0.0165(6) Uani 1 1 d . . . . .
N2 N 0.2367(2) 0.72889(18) 0.37318(17) 0.0179(6) Uani 1 1 d . . . . .
C1 C 0.4898(3) 0.8114(3) 0.3942(3) 0.0296(9) Uani 1 1 d . . . . .
H1A H 0.5030 0.7647 0.3463 0.044 Uiso 1 1 calc R U . . .
H1B H 0.5112 0.8039 0.4426 0.044 Uiso 1 1 calc R U . . .
H1C H 0.5360 0.8622 0.3953 0.044 Uiso 1 1 calc R U . . .
C2 C 0.3224(4) 0.9089(3) 0.4842(2) 0.0319(10) Uani 1 1 d . . . . .
H2A H 0.3713 0.9581 0.4839 0.048 Uiso 1 1 calc R U . . .
H2B H 0.3461 0.9000 0.5314 0.048 Uiso 1 1 calc R U . . .
H2C H 0.2430 0.9162 0.4863 0.048 Uiso 1 1 calc R U . . .
C3 C 0.3180(3) 0.8592(2) 0.2500(2) 0.0216(8) Uani 1 1 d . . . . .
C4 C 0.3652(4) 0.9488(2) 0.3034(3) 0.0340(10) Uani 1 1 d . . . . .
H4A H 0.3069 0.9725 0.3377 0.051 Uiso 1 1 calc R U . . .
H4B H 0.3866 0.9790 0.2698 0.051 Uiso 1 1 calc R U . . .
H4C H 0.4324 0.9528 0.3373 0.051 Uiso 1 1 calc R U . . .
C5 C 0.2158(3) 0.8547(3) 0.1953(3) 0.0281(9) Uani 1 1 d . . . . .
H5A H 0.1844 0.7971 0.1604 0.042 Uiso 1 1 calc R U . . .
H5B H 0.2406 0.8847 0.1620 0.042 Uiso 1 1 calc R U . . .
H5C H 0.1572 0.8793 0.2284 0.042 Uiso 1 1 calc R U . . .
C6 C 0.4088(3) 0.8206(3) 0.1971(3) 0.0306(10) Uani 1 1 d . . . . .
H6A H 0.4751 0.8239 0.2315 0.046 Uiso 1 1 calc R U . . .
H6B H 0.4321 0.8502 0.1633 0.046 Uiso 1 1 calc R U . . .
H6C H 0.3773 0.7629 0.1629 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2050(3) 0.6827(2) 0.4232(2) 0.0230(8) Uani 1 1 d . . . . .
C8 C 0.1207(3) 0.7222(3) 0.4826(2) 0.0279(9) Uani 1 1 d . . . . .
H8A H 0.1553 0.7793 0.5167 0.042 Uiso 1 1 calc R U . . .
H8B H 0.1021 0.6918 0.5164 0.042 Uiso 1 1 calc R U . . .
H8C H 0.0509 0.7206 0.4526 0.042 Uiso 1 1 calc R U . . .
C9 C 0.1534(3) 0.5936(2) 0.3704(2) 0.0276(9) Uani 1 1 d . . . . .
H9A H 0.0845 0.5911 0.3390 0.041 Uiso 1 1 calc R U . . .
H9B H 0.1337 0.5636 0.4044 0.041 Uiso 1 1 calc R U . . .
H9C H 0.2087 0.5687 0.3339 0.041 Uiso 1 1 calc R U . . .
C10 C 0.3143(4) 0.6860(3) 0.4714(3) 0.0338(10) Uani 1 1 d . . . . .
H10A H 0.3686 0.6606 0.4341 0.051 Uiso 1 1 calc R U . . .
H10B H 0.2954 0.6561 0.5056 0.051 Uiso 1 1 calc R U . . .
H10C H 0.3485 0.7433 0.5051 0.051 Uiso 1 1 calc R U . . .
C11 C 0.3612(3) 0.6026(3) 0.2007(2) 0.0236(8) Uani 1 1 d . . . . .
H11A H 0.3947 0.6567 0.2439 0.028 Uiso 1 1 calc R U . . .
H11B H 0.3573 0.5607 0.2232 0.028 Uiso 1 1 calc R U . . .
C12 C 0.4363(3) 0.5833(3) 0.1324(3) 0.0338(10) Uani 1 1 d . . . . .
H12A H 0.3992 0.5328 0.0873 0.051 Uiso 1 1 calc R U . . .
H12B H 0.5097 0.5760 0.1505 0.051 Uiso 1 1 calc R U . . .
H12C H 0.4489 0.6287 0.1151 0.051 Uiso 1 1 calc R U . . .
Ge21 Ge -0.03120(3) 0.72391(2) 0.25315(2) 0.01297(8) Uani 1 1 d . . . . .
Se21 Se -0.13127(3) 0.64476(3) 0.31674(2) 0.02301(9) Uani 1 1 d . . . . .
Si21 Si -0.13646(8) 0.79689(6) 0.18032(6) 0.0178(2) Uani 1 1 d . . . . .
N21 N -0.1015(2) 0.70055(18) 0.15288(17) 0.0153(6) Uani 1 1 d . . . . .
N22 N -0.0715(2) 0.82489(18) 0.27629(18) 0.0178(6) Uani 1 1 d . . . . .
C21 C -0.2925(3) 0.7990(3) 0.1760(3) 0.0274(9) Uani 1 1 d . . . . .
H21A H -0.3320 0.7647 0.2016 0.041 Uiso 1 1 calc R U . . .
H21B H -0.3235 0.7778 0.1197 0.041 Uiso 1 1 calc R U . . .
H21C H -0.3036 0.8556 0.2045 0.041 Uiso 1 1 calc R U . . .
C22 C -0.0733(3) 0.8567(3) 0.1221(3) 0.0318(10) Uani 1 1 d . . . . .
H22A H -0.0880 0.9127 0.1468 0.048 Uiso 1 1 calc R U . . .
H22B H -0.1080 0.8301 0.0664 0.048 Uiso 1 1 calc R U . . .
H22C H 0.0091 0.8587 0.1226 0.048 Uiso 1 1 calc R U . . .
C23 C -0.1070(3) 0.6317(2) 0.0744(2) 0.0208(8) Uani 1 1 d . . . . .
C24 C -0.2160(3) 0.6241(3) 0.0239(2) 0.0337(10) Uani 1 1 d . . . . .
H24A H -0.2825 0.6164 0.0527 0.051 Uiso 1 1 calc R U . . .
H24B H -0.2221 0.5769 -0.0280 0.051 Uiso 1 1 calc R U . . .
H24C H -0.2128 0.6742 0.0147 0.051 Uiso 1 1 calc R U . . .
C25 C -0.1119(3) 0.5519(2) 0.0859(2) 0.0255(8) Uani 1 1 d . . . . .
H25A H -0.0428 0.5560 0.1182 0.038 Uiso 1 1 calc R U . . .
H25B H -0.1171 0.5058 0.0333 0.038 Uiso 1 1 calc R U . . .
H25C H -0.1789 0.5427 0.1138 0.038 Uiso 1 1 calc R U . . .
C26 C -0.0030(3) 0.6452(3) 0.0300(2) 0.0275(9) Uani 1 1 d . . . . .
H26A H -0.0009 0.6954 0.0212 0.041 Uiso 1 1 calc R U . . .
H26B H -0.0080 0.5983 -0.0219 0.041 Uiso 1 1 calc R U . . .
H26C H 0.0665 0.6506 0.0625 0.041 Uiso 1 1 calc R U . . .
C27 C -0.0702(3) 0.8931(2) 0.3539(2) 0.0243(8) Uani 1 1 d . . . . .
C28 C -0.1772(4) 0.8789(3) 0.3955(3) 0.0363(11) Uani 1 1 d . . . . .
H28A H -0.2450 0.8744 0.3618 0.054 Uiso 1 1 calc R U . . .
H28B H -0.1738 0.9252 0.4478 0.054 Uiso 1 1 calc R U . . .
H28C H -0.1813 0.8281 0.4035 0.054 Uiso 1 1 calc R U . . .
C29 C -0.0649(4) 0.9721(3) 0.3402(3) 0.0369(11) Uani 1 1 d . . . . .
H29A H 0.0014 0.9798 0.3112 0.055 Uiso 1 1 calc R U . . .
H29B H -0.0581 1.0192 0.3923 0.055 Uiso 1 1 calc R U . . .
H29C H -0.1345 0.9678 0.3084 0.055 Uiso 1 1 calc R U . . .
C30 C 0.0358(3) 0.9020(3) 0.4068(2) 0.0301(10) Uani 1 1 d . . . . .
H30A H 0.0325 0.8521 0.4163 0.045 Uiso 1 1 calc R U . . .
H30B H 0.0391 0.9492 0.4584 0.045 Uiso 1 1 calc R U . . .
H30C H 0.1039 0.9106 0.3797 0.045 Uiso 1 1 calc R U . . .
C31 C -0.2853(3) 0.6452(2) 0.2775(2) 0.0204(8) Uani 1 1 d . . . . .
H31A H -0.2912 0.7014 0.2844 0.025 Uiso 1 1 calc R U . . .
H31B H -0.3007 0.6087 0.2196 0.025 Uiso 1 1 calc R U . . .
C32 C -0.3718(3) 0.6156(3) 0.3249(2) 0.0258(9) Uani 1 1 d . . . . .
H32A H -0.3607 0.5621 0.3221 0.039 Uiso 1 1 calc R U . . .
H32B H -0.4490 0.6102 0.3020 0.039 Uiso 1 1 calc R U . . .
H32C H -0.3616 0.6552 0.3812 0.039 Uiso 1 1 calc R U . . .
Se41 Se 0.65126(3) 0.39595(2) 0.34152(2) 0.01675(8) Uani 1 1 d . . . . .
Ge41 Ge 0.55373(3) 0.28501(2) 0.22479(2) 0.01231(8) Uani 1 1 d . . . . .
Si41 Si 0.66008(8) 0.19089(6) 0.10787(6) 0.0159(2) Uani 1 1 d . . . . .
N41 N 0.6050(2) 0.18689(17) 0.19452(17) 0.0148(6) Uani 1 1 d . . . . .
N42 N 0.6144(2) 0.28262(18) 0.13050(17) 0.0160(6) Uani 1 1 d . . . . .
C41 C 0.5955(3) 0.1065(2) 0.0101(2) 0.0234(8) Uani 1 1 d . . . . .
H41A H 0.5131 0.1040 0.0053 0.035 Uiso 1 1 calc R U . . .
H41B H 0.6103 0.0541 0.0081 0.035 Uiso 1 1 calc R U . . .
H41C H 0.6292 0.1171 -0.0343 0.035 Uiso 1 1 calc R U . . .
C42 C 0.8171(3) 0.1946(3) 0.1069(3) 0.0269(9) Uani 1 1 d . . . . .
H42A H 0.8440 0.2060 0.0612 0.040 Uiso 1 1 calc R U . . .
H42B H 0.8335 0.1417 0.1020 0.040 Uiso 1 1 calc R U . . .
H42C H 0.8561 0.2381 0.1572 0.040 Uiso 1 1 calc R U . . .
C43 C 0.6177(3) 0.1383(2) 0.2412(2) 0.0186(7) Uani 1 1 d . . . . .
C44 C 0.6039(4) 0.0480(2) 0.1835(3) 0.0292(9) Uani 1 1 d . . . . .
H44A H 0.5304 0.0304 0.1511 0.044 Uiso 1 1 calc R U . . .
H44B H 0.6068 0.0146 0.2144 0.044 Uiso 1 1 calc R U . . .
H44C H 0.6656 0.0413 0.1479 0.044 Uiso 1 1 calc R U . . .
C45 C 0.5246(3) 0.1474(2) 0.2991(2) 0.0234(8) Uani 1 1 d . . . . .
H45A H 0.5323 0.2053 0.3359 0.035 Uiso 1 1 calc R U . . .
H45B H 0.5322 0.1147 0.3302 0.035 Uiso 1 1 calc R U . . .
H45C H 0.4496 0.1281 0.2684 0.035 Uiso 1 1 calc R U . . .
C46 C 0.7348(3) 0.1678(3) 0.2903(3) 0.0303(9) Uani 1 1 d . . . . .
H46A H 0.7952 0.1609 0.2536 0.045 Uiso 1 1 calc R U . . .
H46B H 0.7406 0.1355 0.3220 0.045 Uiso 1 1 calc R U . . .
H46C H 0.7434 0.2259 0.3265 0.045 Uiso 1 1 calc R U . . .
C47 C 0.6083(3) 0.3325(2) 0.0842(2) 0.0187(7) Uani 1 1 d . . . . .
C48 C 0.6074(3) 0.4210(2) 0.1411(2) 0.0228(8) Uani 1 1 d . . . . .
H48A H 0.5399 0.4227 0.1712 0.034 Uiso 1 1 calc R U . . .
H48B H 0.6052 0.4542 0.1098 0.034 Uiso 1 1 calc R U . . .
H48C H 0.6763 0.4430 0.1787 0.034 Uiso 1 1 calc R U . . .
C49 C 0.5009(3) 0.2979(2) 0.0244(2) 0.0222(8) Uani 1 1 d . . . . .
H49A H 0.5045 0.2424 -0.0145 0.033 Uiso 1 1 calc R U . . .
H49B H 0.4966 0.3334 -0.0041 0.033 Uiso 1 1 calc R U . . .
H49C H 0.4332 0.2958 0.0537 0.033 Uiso 1 1 calc R U . . .
C50 C 0.7145(3) 0.3314(2) 0.0375(2) 0.0240(8) Uani 1 1 d . . . . .
H50A H 0.7831 0.3542 0.0755 0.036 Uiso 1 1 calc R U . . .
H50B H 0.7114 0.3644 0.0062 0.036 Uiso 1 1 calc R U . . .
H50C H 0.7166 0.2747 0.0010 0.036 Uiso 1 1 calc R U . . .
C51 C 0.8065(3) 0.4023(3) 0.3063(2) 0.0281(9) Uani 1 1 d . . . . .
H51A H 0.8112 0.3501 0.2607 0.034 Uiso 1 1 calc R U . . .
H51B H 0.8226 0.4469 0.2871 0.034 Uiso 1 1 calc R U . . .
C52 C 0.8936(3) 0.4182(3) 0.3729(3) 0.0376(11) Uani 1 1 d . . . . .
H52A H 0.8856 0.4679 0.4194 0.056 Uiso 1 1 calc R U . . .
H52B H 0.9699 0.4258 0.3550 0.056 Uiso 1 1 calc R U . . .
H52C H 0.8826 0.3714 0.3881 0.056 Uiso 1 1 calc R U . . .
Ge61 Ge 0.34721(3) 0.28273(2) 0.24397(2) 0.01333(8) Uani 1 1 d . . . . .
Se61 Se 0.28799(3) 0.36769(2) 0.18646(2) 0.02193(9) Uani 1 1 d . . . . .
Si61 Si 0.20372(8) 0.20412(6) 0.30981(6) 0.0172(2) Uani 1 1 d . . . . .
N61 N 0.2897(2) 0.30099(18) 0.34249(17) 0.0167(6) Uani 1 1 d . . . . .
N62 N 0.2522(2) 0.18154(17) 0.21492(17) 0.0150(6) Uani 1 1 d . . . . .
C61 C 0.0466(3) 0.2007(3) 0.3124(2) 0.0254(8) Uani 1 1 d . . . . .
H61A H 0.0238 0.2349 0.2866 0.038 Uiso 1 1 calc R U . . .
H61B H 0.0280 0.2215 0.3684 0.038 Uiso 1 1 calc R U . . .
H61C H 0.0058 0.1439 0.2835 0.038 Uiso 1 1 calc R U . . .
C62 C 0.2361(3) 0.1407(3) 0.3639(3) 0.0275(9) Uani 1 1 d . . . . .
H62A H 0.1943 0.0842 0.3351 0.041 Uiso 1 1 calc R U . . .
H62B H 0.2129 0.1635 0.4186 0.041 Uiso 1 1 calc R U . . .
H62C H 0.3181 0.1411 0.3662 0.041 Uiso 1 1 calc R U . . .
C63 C 0.3221(3) 0.3675(2) 0.4232(2) 0.0216(8) Uani 1 1 d . . . . .
C64 C 0.2173(3) 0.3722(3) 0.4714(2) 0.0302(9) Uani 1 1 d . . . . .
H64A H 0.1558 0.3838 0.4439 0.045 Uiso 1 1 calc R U . . .
H64B H 0.2374 0.4161 0.5255 0.045 Uiso 1 1 calc R U . . .
H64C H 0.1920 0.3197 0.4757 0.045 Uiso 1 1 calc R U . . .
C65 C 0.4183(3) 0.3501(3) 0.4670(2) 0.0244(8) Uani 1 1 d . . . . .
H65A H 0.3930 0.2979 0.4718 0.037 Uiso 1 1 calc R U . . .
H65B H 0.4381 0.3945 0.5208 0.037 Uiso 1 1 calc R U . . .
H65C H 0.4853 0.3469 0.4364 0.037 Uiso 1 1 calc R U . . .
C66 C 0.3596(3) 0.4491(2) 0.4160(2) 0.0251(8) Uani 1 1 d . . . . .
H66A H 0.4262 0.4465 0.3850 0.038 Uiso 1 1 calc R U . . .
H66B H 0.3796 0.4933 0.4699 0.038 Uiso 1 1 calc R U . . .
H66C H 0.2972 0.4600 0.3886 0.038 Uiso 1 1 calc R U . . .
C67 C 0.2131(3) 0.1166(2) 0.1346(2) 0.0198(8) Uani 1 1 d . . . . .
C68 C 0.1048(3) 0.1307(3) 0.1000(3) 0.0355(11) Uani 1 1 d . . . . .
H68A H 0.0436 0.1291 0.1349 0.053 Uiso 1 1 calc R U . . .
H68B H 0.0815 0.0877 0.0459 0.053 Uiso 1 1 calc R U . . .
H68C H 0.1201 0.1845 0.0972 0.053 Uiso 1 1 calc R U . . .
C69 C 0.1886(4) 0.0339(3) 0.1411(3) 0.0356(10) Uani 1 1 d . . . . .
H69A H 0.2580 0.0247 0.1627 0.053 Uiso 1 1 calc R U . . .
H69B H 0.1635 -0.0100 0.0877 0.053 Uiso 1 1 calc R U . . .
H69C H 0.1286 0.0339 0.1772 0.053 Uiso 1 1 calc R U . . .
C70 C 0.3064(3) 0.1161(3) 0.0784(2) 0.0272(9) Uani 1 1 d . . . . .
H70A H 0.3210 0.1686 0.0729 0.041 Uiso 1 1 calc R U . . .
H70B H 0.2820 0.0713 0.0255 0.041 Uiso 1 1 calc R U . . .
H70C H 0.3763 0.1083 0.1008 0.041 Uiso 1 1 calc R U . . .
C71 C 0.1365(3) 0.3679(3) 0.2281(2) 0.0227(8) Uani 1 1 d . . . . .
H71A H 0.1034 0.3123 0.2244 0.027 Uiso 1 1 calc R U . . .
H71B H 0.1443 0.4065 0.2854 0.027 Uiso 1 1 calc R U . . .
C72 C 0.0587(3) 0.3929(3) 0.1805(2) 0.0265(9) Uani 1 1 d . . . . .
H72A H 0.0925 0.4474 0.1831 0.040 Uiso 1 1 calc R U . . .
H72B H -0.0152 0.3948 0.2029 0.040 Uiso 1 1 calc R U . . .
H72C H 0.0481 0.3530 0.1242 0.040 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Se1 C11 1.968(4) . ?
Se1 Ge1 2.3700(5) . ?
Ge1 N1 1.846(3) . ?
Ge1 N2 1.851(3) . ?
Ge1 Ge21 2.4921(5) . ?
Ge1 Si1 2.6414(11) . ?
Si1 N1 1.734(3) . ?
Si1 N2 1.736(3) . ?
Si1 C2 1.869(4) . ?
Si1 C1 1.875(4) . ?
N1 C3 1.467(5) . ?
N2 C7 1.476(5) . ?
C3 C4 1.519(6) . ?
C3 C6 1.533(5) . ?
C3 C5 1.534(5) . ?
C7 C9 1.520(6) . ?
C7 C8 1.536(5) . ?
C7 C10 1.542(5) . ?
C11 C12 1.506(5) . ?
Ge21 N21 1.851(3) . ?
Ge21 N22 1.856(3) . ?
Ge21 Se21 2.3650(5) . ?
Ge21 Si21 2.6438(10) . ?
Se21 C31 1.967(3) . ?
Si21 N22 1.740(3) . ?
Si21 N21 1.740(3) . ?
Si21 C21 1.874(4) . ?
Si21 C22 1.877(4) . ?
N21 C23 1.466(4) . ?
N22 C27 1.458(5) . ?
C23 C26 1.531(5) . ?
C23 C25 1.531(5) . ?
C23 C24 1.537(5) . ?
C27 C30 1.525(5) . ?
C27 C28 1.532(6) . ?
C27 C29 1.537(6) . ?
C31 C32 1.518(5) . ?
Se41 C51 1.974(4) . ?
Se41 Ge41 2.3725(5) . ?
Ge41 N41 1.854(3) . ?
Ge41 N42 1.859(3) . ?
Ge41 Ge61 2.4955(5) . ?
Ge41 Si41 2.6430(10) . ?
Si41 N42 1.731(3) . ?
Si41 N41 1.740(3) . ?
Si41 C41 1.866(4) . ?
Si41 C42 1.868(4) . ?
N41 C43 1.467(4) . ?
N42 C47 1.467(4) . ?
C43 C44 1.528(5) . ?
C43 C45 1.529(5) . ?
C43 C46 1.540(5) . ?
C47 C48 1.524(5) . ?
C47 C50 1.537(5) . ?
C47 C49 1.538(5) . ?
C51 C52 1.488(5) . ?
Ge61 N62 1.850(3) . ?
Ge61 N61 1.854(3) . ?
Ge61 Se61 2.3634(5) . ?
Ge61 Si61 2.6428(10) . ?
Se61 C71 1.974(3) . ?
Si61 N61 1.737(3) . ?
Si61 N62 1.742(3) . ?
Si61 C62 1.863(4) . ?
Si61 C61 1.871(4) . ?
N61 C63 1.473(5) . ?
N62 C67 1.470(4) . ?
C63 C66 1.526(5) . ?
C63 C65 1.534(5) . ?
C63 C64 1.536(5) . ?
C67 C70 1.523(5) . ?
C67 C69 1.527(6) . ?
C67 C68 1.534(5) . ?
C71 C72 1.501(5) . ?

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
C11 Se1 Ge1 98.55(11) . . ?
N1 Ge1 N2 81.75(13) . . ?
N1 Ge1 Se1 115.59(9) . . ?
N2 Ge1 Se1 113.45(10) . . ?
N1 Ge1 Ge21 118.46(9) . . ?
N2 Ge1 Ge21 122.29(9) . . ?
Se1 Ge1 Ge21 104.764(18) . . ?
Se1 Ge1 Si1 122.81(3) . . ?
Ge21 Ge1 Si1 132.41(3) . . ?
N1 Si1 N2 88.40(14) . . ?
N1 Si1 C2 116.47(18) . . ?
N2 Si1 C2 115.46(18) . . ?
N1 Si1 C1 114.50(18) . . ?
N2 Si1 C1 117.16(17) . . ?
C2 Si1 C1 104.94(19) . . ?
C2 Si1 Ge1 128.17(13) . . ?
C1 Si1 Ge1 126.88(14) . . ?
C3 N1 Si1 134.1(2) . . ?
C3 N1 Ge1 129.3(2) . . ?
Si1 N1 Ge1 95.04(14) . . ?
C7 N2 Si1 132.2(2) . . ?
C7 N2 Ge1 132.5(2) . . ?
Si1 N2 Ge1 94.81(14) . . ?
N1 C3 C4 108.9(3) . . ?
N1 C3 C6 111.1(3) . . ?
C4 C3 C6 110.3(3) . . ?
N1 C3 C5 109.2(3) . . ?
C4 C3 C5 108.6(3) . . ?
C6 C3 C5 108.7(3) . . ?
N2 C7 C9 110.4(3) . . ?
N2 C7 C8 110.4(3) . . ?
C9 C7 C8 110.3(3) . . ?
N2 C7 C10 107.9(3) . . ?
C9 C7 C10 109.0(3) . . ?
C8 C7 C10 108.8(3) . . ?
C12 C11 Se1 111.0(3) . . ?
N21 Ge21 N22 81.97(13) . . ?
N21 Ge21 Se21 112.17(9) . . ?
N22 Ge21 Se21 115.38(9) . . ?
N21 Ge21 Ge1 123.10(9) . . ?
N22 Ge21 Ge1 118.28(9) . . ?
Se21 Ge21 Ge1 105.228(18) . . ?
Se21 Ge21 Si21 122.03(3) . . ?
Ge1 Ge21 Si21 132.72(3) . . ?
C31 Se21 Ge21 96.55(10) . . ?
N22 Si21 N21 88.64(14) . . ?
N22 Si21 C21 114.86(17) . . ?
N21 Si21 C21 115.97(17) . . ?
N22 Si21 C22 116.71(18) . . ?
N21 Si21 C22 115.41(17) . . ?
C21 Si21 C22 105.25(19) . . ?
C21 Si21 Ge21 126.61(14) . . ?
C22 Si21 Ge21 128.15(13) . . ?
C23 N21 Si21 131.8(2) . . ?
C23 N21 Ge21 132.6(2) . . ?
Si21 N21 Ge21 94.77(14) . . ?
C27 N22 Si21 134.5(2) . . ?
C27 N22 Ge21 129.4(3) . . ?
Si21 N22 Ge21 94.62(14) . . ?
N21 C23 C26 110.8(3) . . ?
N21 C23 C25 109.7(3) . . ?
C26 C23 C25 109.3(3) . . ?
N21 C23 C24 108.8(3) . . ?
C26 C23 C24 109.4(3) . . ?
C25 C23 C24 108.7(3) . . ?
N22 C27 C30 108.8(3) . . ?
N22 C27 C28 111.1(3) . . ?
C30 C27 C28 109.8(4) . . ?
N22 C27 C29 108.6(3) . . ?
C30 C27 C29 109.1(3) . . ?
C28 C27 C29 109.4(3) . . ?
C32 C31 Se21 109.1(2) . . ?
C51 Se41 Ge41 99.09(12) . . ?
N41 Ge41 N42 81.78(12) . . ?
N41 Ge41 Se41 116.26(9) . . ?
N42 Ge41 Se41 112.79(9) . . ?
N41 Ge41 Ge61 117.93(9) . . ?
N42 Ge41 Ge61 122.49(9) . . ?
Se41 Ge41 Ge61 105.022(18) . . ?
Se41 Ge41 Si41 122.99(3) . . ?
Ge61 Ge41 Si41 131.98(3) . . ?
N42 Si41 N41 88.87(13) . . ?
N42 Si41 C41 114.78(16) . . ?
N41 Si41 C41 116.66(16) . . ?
N42 Si41 C42 116.86(17) . . ?
N41 Si41 C42 114.09(17) . . ?
C41 Si41 C42 105.54(18) . . ?
C41 Si41 Ge41 127.75(12) . . ?
C42 Si41 Ge41 126.70(14) . . ?
C43 N41 Si41 134.3(2) . . ?
C43 N41 Ge41 129.4(2) . . ?
Si41 N41 Ge41 94.62(13) . . ?
C47 N42 Si41 131.9(2) . . ?
C47 N42 Ge41 132.6(2) . . ?
Si41 N42 Ge41 94.72(14) . . ?
N41 C43 C44 108.9(3) . . ?
N41 C43 C45 109.1(3) . . ?
C44 C43 C45 109.0(3) . . ?
N41 C43 C46 111.0(3) . . ?
C44 C43 C46 110.1(3) . . ?
C45 C43 C46 108.8(3) . . ?
N42 C47 C48 110.0(3) . . ?
N42 C47 C50 108.7(3) . . ?
C48 C47 C50 108.6(3) . . ?
N42 C47 C49 110.7(3) . . ?
C48 C47 C49 109.7(3) . . ?
C50 C47 C49 109.2(3) . . ?
C52 C51 Se41 111.4(3) . . ?
N62 Ge61 N61 81.98(13) . . ?
N62 Ge61 Se61 114.94(9) . . ?
N61 Ge61 Se61 111.50(9) . . ?
N62 Ge61 Ge41 117.70(9) . . ?
N61 Ge61 Ge41 122.74(9) . . ?
Se61 Ge61 Ge41 106.745(18) . . ?
Se61 Ge61 Si61 121.69(3) . . ?
Ge41 Ge61 Si61 131.55(3) . . ?
C71 Se61 Ge61 96.03(11) . . ?
N61 Si61 N62 88.59(14) . . ?
N61 Si61 C62 115.18(17) . . ?
N62 Si61 C62 117.29(17) . . ?
N61 Si61 C61 116.27(17) . . ?
N62 Si61 C61 114.63(16) . . ?
C62 Si61 C61 104.97(17) . . ?
C62 Si61 Ge61 127.88(12) . . ?
C61 Si61 Ge61 127.14(13) . . ?
C63 N61 Si61 132.2(2) . . ?
C63 N61 Ge61 132.2(2) . . ?
Si61 N61 Ge61 94.70(14) . . ?
C67 N62 Si61 133.8(2) . . ?
C67 N62 Ge61 129.8(2) . . ?
Si61 N62 Ge61 94.72(14) . . ?
N61 C63 C66 109.8(3) . . ?
N61 C63 C65 110.5(3) . . ?
C66 C63 C65 110.1(3) . . ?
N61 C63 C64 108.3(3) . . ?
C66 C63 C64 108.9(3) . . ?
C65 C63 C64 109.1(3) . . ?
N62 C67 C70 109.2(3) . . ?
N62 C67 C69 108.8(3) . . ?
C70 C67 C69 109.2(3) . . ?
N62 C67 C68 110.9(3) . . ?
C70 C67 C68 109.1(3) . . ?
C69 C67 C68 109.5(3) . . ?
C72 C71 Se61 110.2(2) . . ?

_refine_diff_density_max         2.720
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.118

_shelxl_version_number           2014/5

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pst_013m

_database_code_CSD               WIDFOE
_database_code_depnum_ccdc_archive 'CCDC 1010028'

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H48 Ge2 N4 Si2 Te2'
_chemical_formula_sum            'C20 H48 Ge2 N4 Si2 Te2'
_chemical_formula_weight         801.18

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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5756(4)
_cell_length_b                   10.2876(7)
_cell_length_c                   13.1762(9)
_cell_angle_alpha                110.256(2)
_cell_angle_beta                 93.937(2)
_cell_angle_gamma                107.259(2)
_cell_volume                     783.81(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    20255
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      32.81

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    3.832
_shelx_estimated_absorpt_T_min   0.322
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-RAY tube'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_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_detector_area_resol_mean 512
_diffrn_reflns_number            27425
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.227
_diffrn_reflns_theta_max         32.812
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5640
_reflns_number_gt                5242
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS Inc. 2013 Vers. 2013/4'
_computing_molecular_graphics    'BRUKER AXS Inc. 2008 Vers. 2008/4'
_computing_publication_material  'BRUKER AXS Inc. 2013 Vers. 2013/4'

_refine_special_details          
;
 Treatment of hydrogen atoms:    
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0171P)²+0.2084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5640
_refine_ls_number_parameters     144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0149
_refine_ls_wR_factor_ref         0.0376
_refine_ls_wR_factor_gt          0.0364
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.72850(2) 0.44514(2) 0.42792(2) 0.01151(2) Uani 1 1 d . . . . .
Ge1 Ge 0.35635(2) 0.46815(2) 0.37568(2) 0.00898(3) Uani 1 1 d . . . . .
Si1 Si 0.15848(5) 0.41695(3) 0.17869(2) 0.01141(5) Uani 1 1 d . . . . .
N1 N 0.15555(15) 0.31362(10) 0.25923(7) 0.01171(16) Uani 1 1 d . . . . .
N2 N 0.33789(15) 0.57032(10) 0.28659(8) 0.01258(16) Uani 1 1 d . . . . .
C1 C 0.07625(18) 0.15386(12) 0.23261(9) 0.01364(19) Uani 1 1 d . . . . .
C2 C 0.2461(2) 0.08509(14) 0.18894(11) 0.0217(2) Uani 1 1 d . . . . .
H2A H 0.2838 0.1064 0.1243 0.033 Uiso 1 1 calc R U . . .
H2B H 0.1866 -0.0219 0.1681 0.033 Uiso 1 1 calc R U . . .
H2C H 0.3764 0.1268 0.2465 0.033 Uiso 1 1 calc R U . . .
C3 C 0.0221(2) 0.12472(13) 0.33544(10) 0.0191(2) Uani 1 1 d . . . . .
H3A H 0.1518 0.1740 0.3939 0.029 Uiso 1 1 calc R U . . .
H3B H -0.0271 0.0183 0.3179 0.029 Uiso 1 1 calc R U . . .
H3C H -0.0931 0.1632 0.3605 0.029 Uiso 1 1 calc R U . . .
C4 C -0.1308(2) 0.08427(14) 0.14440(10) 0.0199(2) Uani 1 1 d . . . . .
H4A H -0.2395 0.1278 0.1726 0.030 Uiso 1 1 calc R U . . .
H4B H -0.1876 -0.0223 0.1260 0.030 Uiso 1 1 calc R U . . .
H4C H -0.0977 0.1028 0.0782 0.030 Uiso 1 1 calc R U . . .
C5 C 0.40309(19) 0.72947(12) 0.31138(9) 0.01487(19) Uani 1 1 d . . . . .
C6 C 0.4546(2) 0.75537(15) 0.20681(11) 0.0241(3) Uani 1 1 d . . . . .
H6A H 0.5714 0.7182 0.1827 0.036 Uiso 1 1 calc R U . . .
H6B H 0.5007 0.8612 0.2224 0.036 Uiso 1 1 calc R U . . .
H6C H 0.3247 0.7033 0.1485 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2213(2) 0.78771(15) 0.34970(12) 0.0234(2) Uani 1 1 d . . . . .
H7A H 0.0924 0.7380 0.2907 0.035 Uiso 1 1 calc R U . . .
H7B H 0.2692 0.8942 0.3676 0.035 Uiso 1 1 calc R U . . .
H7C H 0.1859 0.7682 0.4153 0.035 Uiso 1 1 calc R U . . .
C8 C 0.6058(2) 0.81134(14) 0.40190(11) 0.0220(2) Uani 1 1 d . . . . .
H8A H 0.5729 0.7968 0.4694 0.033 Uiso 1 1 calc R U . . .
H8B H 0.6530 0.9168 0.4161 0.033 Uiso 1 1 calc R U . . .
H8C H 0.7218 0.7730 0.3783 0.033 Uiso 1 1 calc R U . . .
C9 C 0.2714(2) 0.35663(14) 0.05100(10) 0.0182(2) Uani 1 1 d . . . . .
H9A H 0.3018 0.4335 0.0207 0.027 Uiso 1 1 calc R U . . .
H9B H 0.1656 0.2652 -0.0035 0.027 Uiso 1 1 calc R U . . .
H9C H 0.4059 0.3396 0.0688 0.027 Uiso 1 1 calc R U . . .
C10 C -0.10665(19) 0.43224(15) 0.13597(10) 0.0194(2) Uani 1 1 d . . . . .
H10A H -0.1749 0.4595 0.2003 0.029 Uiso 1 1 calc R U . . .
H10B H -0.2017 0.3373 0.0804 0.029 Uiso 1 1 calc R U . . .
H10C H -0.0828 0.5080 0.1047 0.029 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Te1 Ge1 2.5883(2) 2_666 ?
Te1 Ge1 2.59678(19) . ?
Ge1 N2 1.8460(9) . ?
Ge1 N1 1.8472(9) . ?
Ge1 Te1 2.5883(2) 2_666 ?
Ge1 Si1 2.6249(3) . ?
Si1 N2 1.7362(10) . ?
Si1 N1 1.7402(9) . ?
Si1 C10 1.8629(12) . ?
Si1 C9 1.8678(12) . ?
N1 C1 1.4708(14) . ?
N2 C5 1.4714(14) . ?
C1 C3 1.5286(16) . ?
C1 C4 1.5313(16) . ?
C1 C2 1.5343(17) . ?
C5 C8 1.5261(17) . ?
C5 C7 1.5301(18) . ?
C5 C6 1.5326(16) . ?

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
Ge1 Te1 Ge1 82.382(5) 2_666 . ?
N2 Ge1 N1 82.62(4) . . ?
N2 Ge1 Te1 120.55(3) . 2_666 ?
N1 Ge1 Te1 121.41(3) . 2_666 ?
N2 Ge1 Te1 118.25(3) . . ?
N1 Ge1 Te1 118.33(3) . . ?
Te1 Ge1 Te1 97.617(5) 2_666 . ?
N2 Ge1 Si1 41.27(3) . . ?
N1 Ge1 Si1 41.40(3) . . ?
Te1 Ge1 Si1 134.931(9) 2_666 . ?
Te1 Ge1 Si1 127.447(8) . . ?
N2 Si1 N1 89.07(4) . . ?
N2 Si1 C10 115.69(5) . . ?
N1 Si1 C10 115.95(5) . . ?
N2 Si1 C9 114.36(5) . . ?
N1 Si1 C9 114.68(5) . . ?
C10 Si1 C9 106.74(6) . . ?
N2 Si1 Ge1 44.54(3) . . ?
N1 Si1 Ge1 44.59(3) . . ?
C10 Si1 Ge1 129.53(4) . . ?
C9 Si1 Ge1 123.73(4) . . ?
C1 N1 Si1 132.32(7) . . ?
C1 N1 Ge1 131.40(7) . . ?
Si1 N1 Ge1 94.01(4) . . ?
C5 N2 Si1 132.53(7) . . ?
C5 N2 Ge1 131.35(7) . . ?
Si1 N2 Ge1 94.18(4) . . ?
N1 C1 C3 109.69(9) . . ?
N1 C1 C4 108.03(9) . . ?
C3 C1 C4 108.91(10) . . ?
N1 C1 C2 111.04(9) . . ?
C3 C1 C2 109.60(10) . . ?
C4 C1 C2 109.53(10) . . ?
N2 C5 C8 109.48(9) . . ?
N2 C5 C7 110.70(10) . . ?
C8 C5 C7 109.20(11) . . ?
N2 C5 C6 108.53(10) . . ?
C8 C5 C6 109.14(10) . . ?
C7 C5 C6 109.75(10) . . ?

_refine_diff_density_max         0.799
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

