# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_philpv32
_database_code_depnum_ccdc_archive 'CCDC 1438300'
_audit_update_record             
;
2015-11-23 deposited with the CCDC.
2016-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H10 Br2 Ge2 O4, C4 H8 O2'
_chemical_formula_sum            'C18 H18 Br2 Ge2 O6'
_chemical_formula_weight         635.32

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'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.1184(6)
_cell_length_b                   5.8156(4)
_cell_length_c                   18.7848(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.848(5)
_cell_angle_gamma                90.00
_cell_volume                     995.62(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    1142
_cell_measurement_theta_min      3.2486
_cell_measurement_theta_max      24.9940


_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    7.066
_exptl_absorpt_correction_T_min  0.39161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3242
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1738
_reflns_number_gt                1233
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0549P)²+0.0000P] 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         1738
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0692(7) 0.7608(9) 0.1261(3) 0.0235(13) Uani 1 1 d . . .
C2 C 0.1891(7) 0.8765(10) 0.1563(3) 0.0268(14) Uani 1 1 d . . .
H2 H 0.2166 1.0181 0.1380 0.032 Uiso 1 1 calc R . .
C3 C 0.2687(7) 0.7818(10) 0.2140(3) 0.0251(14) Uani 1 1 d . . .
H3 H 0.3478 0.8603 0.2349 0.030 Uiso 1 1 calc R . .
C4 C 0.2273(6) 0.5684(9) 0.2395(3) 0.0245(9) Uani 1 1 d . . .
C5 C 0.1124(6) 0.4487(10) 0.2095(3) 0.0245(9) Uani 1 1 d . . .
H5 H 0.0888 0.3040 0.2269 0.029 Uiso 1 1 calc R . .
C6 C 0.0303(6) 0.5431(10) 0.1531(3) 0.0242(13) Uani 1 1 d . . .
C7 C -0.0973(7) 0.4166(11) 0.1187(3) 0.0275(14) Uani 1 1 d . . .
H7A H -0.0995 0.2603 0.1367 0.033 Uiso 1 1 calc R . .
H7B H -0.1882 0.4914 0.1310 0.033 Uiso 1 1 calc R . .
C8 C -0.5153(7) 0.4859(10) 0.0740(3) 0.0315(15) Uani 1 1 d . . .
H8A H -0.6188 0.5184 0.0790 0.038 Uiso 1 1 calc R . .
H8B H -0.4726 0.4544 0.1209 0.038 Uiso 1 1 calc R . .
C9 C -0.5025(7) 0.7203(10) -0.0268(3) 0.0295(14) Uani 1 1 d . . .
H9A H -0.4525 0.8506 -0.0473 0.035 Uiso 1 1 calc R . .
H9B H -0.6058 0.7584 -0.0248 0.035 Uiso 1 1 calc R . .
O1 O -0.0102(4) 0.8616(6) 0.07238(19) 0.0242(9) Uani 1 1 d . . .
O2 O -0.0856(4) 0.4128(7) 0.04142(19) 0.0275(9) Uani 1 1 d . . .
O3 O -0.4446(5) 0.6810(7) 0.0439(2) 0.0317(10) Uani 1 1 d . . .
Ge1 Ge -0.10266(7) 0.71574(10) -0.00501(3) 0.0244(2) Uani 1 1 d . . .
Br1 Br 0.33718(7) 0.43745(10) 0.31806(3) 0.0293(2) Uani 1 1 d . . .


_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
C1 O1 1.357(7) . ?
C1 C2 1.389(8) . ?
C1 C6 1.413(8) . ?
C2 C3 1.398(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(8) . ?
C4 Br1 1.915(6) . ?
C5 C6 1.391(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.505(8) . ?
C7 O2 1.460(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O3 1.430(7) . ?
C8 C9 1.503(8) 3_465 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.432(7) . ?
C9 C8 1.503(8) 3_465 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O1 Ge1 1.862(4) . ?
O2 Ge1 1.970(4) . ?
O2 Ge1 2.012(4) 3_565 ?
Ge1 O2 2.012(4) 3_565 ?

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
O1 C1 C2 119.3(5) . . ?
O1 C1 C6 121.3(5) . . ?
C2 C1 C6 119.4(5) . . ?
C1 C2 C3 120.5(6) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 118.7(6) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 121.9(5) . . ?
C5 C4 Br1 119.4(4) . . ?
C3 C4 Br1 118.7(5) . . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 119.5(5) . . ?
C5 C6 C7 121.6(5) . . ?
C1 C6 C7 118.9(5) . . ?
O2 C7 C6 110.7(5) . . ?
O2 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
O3 C8 C9 110.0(5) . 3_465 ?
O3 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 3_465 . ?
O3 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 3_465 . ?
H8A C8 H8B 108.2 . . ?
O3 C9 C8 112.0(5) . 3_465 ?
O3 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 3_465 . ?
O3 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 3_465 . ?
H9A C9 H9B 107.9 . . ?
C1 O1 Ge1 127.0(3) . . ?
C7 O2 Ge1 114.8(3) . . ?
C7 O2 Ge1 115.7(3) . 3_565 ?
Ge1 O2 Ge1 103.76(17) . 3_565 ?
C8 O3 C9 109.6(4) . . ?
O1 Ge1 O2 91.98(16) . . ?
O1 Ge1 O2 93.73(16) . 3_565 ?
O2 Ge1 O2 76.24(17) . 3_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 176.9(5) . . . . ?
C6 C1 C2 C3 -1.6(8) . . . . ?
C1 C2 C3 C4 1.3(8) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C2 C3 C4 Br1 179.5(4) . . . . ?
C3 C4 C5 C6 -1.8(8) . . . . ?
Br1 C4 C5 C6 179.1(4) . . . . ?
C4 C5 C6 C1 1.5(8) . . . . ?
C4 C5 C6 C7 -179.9(5) . . . . ?
O1 C1 C6 C5 -178.2(5) . . . . ?
C2 C1 C6 C5 0.2(8) . . . . ?
O1 C1 C6 C7 3.2(8) . . . . ?
C2 C1 C6 C7 -178.4(5) . . . . ?
C5 C6 C7 O2 -130.0(6) . . . . ?
C1 C6 C7 O2 48.6(7) . . . . ?
C2 C1 O1 Ge1 145.8(4) . . . . ?
C6 C1 O1 Ge1 -35.8(7) . . . . ?
C6 C7 O2 Ge1 -65.9(5) . . . . ?
C6 C7 O2 Ge1 55.0(5) . . . 3_565 ?
C9 C8 O3 C9 56.4(7) 3_465 . . . ?
C8 C9 O3 C8 -57.6(7) 3_465 . . . ?
C1 O1 Ge1 O2 15.4(4) . . . . ?
C1 O1 Ge1 O2 -60.9(4) . . . 3_565 ?
C7 O2 Ge1 O1 33.9(4) . . . . ?
Ge1 O2 Ge1 O1 -93.35(19) 3_565 . . . ?
C7 O2 Ge1 O2 127.3(4) . . . 3_565 ?
Ge1 O2 Ge1 O2 0.0 3_565 . . 3_565 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.151
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pk11
_database_code_depnum_ccdc_archive 'CCDC 1438301'
_audit_update_record             
;
2015-11-23 deposited with the CCDC.
2016-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Ge3 O6'

_chemical_formula_sum            'C21 H18 Ge3 O6'
_chemical_formula_weight         584.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_Hall  '-P 2yn'


loop_
_symmetry_equiv_pos_as_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                   11.5755(3)
_cell_length_b                   16.1191(10)
_cell_length_c                   11.8463(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.168(4)
_cell_angle_gamma                90.00
_cell_volume                     2074.83(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    3781
_cell_measurement_theta_min      3.9723
_cell_measurement_theta_max      63.8460

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_absorpt_coefficient_mu    5.455
_exptl_absorpt_correction_T_min  0.69033
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
_diffrn_standards_decay_%        0

_diffrn_reflns_number            6394
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.83
_diffrn_reflns_theta_max         63.94
_reflns_number_total             3365
_reflns_number_gt                3124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0679P)²+0.2165P] 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         3365
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6002(3) -0.00731(19) 0.8915(2) 0.0209(6) Uani 1 1 d . . .
C2 C 0.5689(3) -0.0831(2) 0.9302(3) 0.0241(6) Uani 1 1 d . . .
H2 H 0.5118 -0.1177 0.8763 0.029 Uiso 1 1 calc R . .
C3 C 0.6237(3) -0.1064(2) 1.0497(3) 0.0265(6) Uani 1 1 d . . .
H3 H 0.6019 -0.1564 1.0760 0.032 Uiso 1 1 calc R . .
C4 C 0.7103(3) -0.05617(19) 1.1299(3) 0.0271(7) Uani 1 1 d . . .
H4 H 0.7455 -0.0720 1.2100 0.032 Uiso 1 1 calc R . .
C5 C 0.7449(3) 0.0179(2) 1.0909(3) 0.0264(7) Uani 1 1 d . . .
H5 H 0.8052 0.0509 1.1443 0.032 Uiso 1 1 calc R . .
C6 C 0.6891(3) 0.04301(18) 0.9715(3) 0.0220(6) Uani 1 1 d . . .
C7 C 0.7186(3) 0.12296(19) 0.9239(3) 0.0275(7) Uani 1 1 d . . .
H7A H 0.6464 0.1584 0.8994 0.033 Uiso 1 1 calc R . .
H7B H 0.7835 0.1513 0.9867 0.033 Uiso 1 1 calc R . .
C8 C 0.8799(3) -0.15735(18) 0.6346(3) 0.0245(6) Uani 1 1 d . . .
C9 C 0.9473(3) -0.18451(19) 0.5629(3) 0.0275(7) Uani 1 1 d . . .
H9 H 1.0328 -0.1865 0.5946 0.033 Uiso 1 1 calc R . .
C10 C 0.8858(3) -0.2083(2) 0.4445(3) 0.0310(7) Uani 1 1 d . . .
H10 H 0.9307 -0.2269 0.3979 0.037 Uiso 1 1 calc R . .
C11 C 0.7598(3) -0.20473(19) 0.3955(3) 0.0303(7) Uani 1 1 d . . .
H11 H 0.7196 -0.2210 0.3162 0.036 Uiso 1 1 calc R . .
C12 C 0.6926(3) -0.17644(19) 0.4658(3) 0.0259(6) Uani 1 1 d . . .
H12 H 0.6073 -0.1728 0.4325 0.031 Uiso 1 1 calc R . .
C13 C 0.7523(3) -0.15359(18) 0.5854(3) 0.0236(6) Uani 1 1 d . . .
C14 C 0.6825(3) -0.12337(19) 0.6629(3) 0.0257(6) Uani 1 1 d . . .
H14A H 0.5970 -0.1144 0.6141 0.031 Uiso 1 1 calc R . .
H14B H 0.6857 -0.1647 0.7234 0.031 Uiso 1 1 calc R . .
C15 C 0.8301(2) 0.16460(19) 0.5933(2) 0.0212(6) Uani 1 1 d . . .
C16 C 0.7350(3) 0.20779(19) 0.5080(3) 0.0246(6) Uani 1 1 d . . .
H16 H 0.7143 0.2612 0.5236 0.030 Uiso 1 1 calc R . .
C17 C 0.6717(3) 0.1690(2) 0.3987(2) 0.0270(7) Uani 1 1 d . . .
H17 H 0.6090 0.1975 0.3408 0.032 Uiso 1 1 calc R . .
C18 C 0.7003(3) 0.0894(2) 0.3751(3) 0.0268(7) Uani 1 1 d . . .
H18 H 0.6562 0.0640 0.3025 0.032 Uiso 1 1 calc R . .
C19 C 0.7956(3) 0.04714(19) 0.4606(3) 0.0237(6) Uani 1 1 d . . .
H19 H 0.8149 -0.0067 0.4452 0.028 Uiso 1 1 calc R . .
C20 C 0.8619(3) 0.08511(18) 0.5689(2) 0.0203(6) Uani 1 1 d . . .
C21 C 0.9698(3) 0.04412(19) 0.6607(3) 0.0228(6) Uani 1 1 d . . .
H21A H 0.9787 -0.0118 0.6347 0.027 Uiso 1 1 calc R . .
H21B H 1.0442 0.0746 0.6679 0.027 Uiso 1 1 calc R . .
O1 O 0.54283(18) 0.01915(14) 0.77650(18) 0.0247(4) Uani 1 1 d . . .
O2 O 0.75846(19) 0.10784(13) 0.82069(17) 0.0247(4) Uani 1 1 d . . .
O3 O 0.94218(18) -0.13704(13) 0.75111(18) 0.0260(5) Uani 1 1 d . . .
O4 O 0.73687(19) -0.04599(12) 0.72081(19) 0.0240(5) Uani 1 1 d . . .
O5 O 0.89462(18) 0.20145(13) 0.70070(17) 0.0232(4) Uani 1 1 d . . .
O6 O 0.95365(18) 0.04106(13) 0.77805(18) 0.0224(4) Uani 1 1 d . . .
Ge1 Ge 0.63136(3) 0.05373(2) 0.68247(3) 0.02230(13) Uani 1 1 d . . .
Ge2 Ge 0.89806(3) -0.05900(2) 0.84308(3) 0.02268(13) Uani 1 1 d . . .
Ge3 Ge 0.92830(3) 0.14708(2) 0.84554(3) 0.02197(13) Uani 1 1 d . . .


_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
C1 O1 1.362(4) . ?
C1 C6 1.394(4) . ?
C1 C2 1.396(4) . ?
C2 C3 1.389(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.492(4) . ?
C7 O2 1.468(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O3 1.358(4) . ?
C8 C13 1.389(4) . ?
C8 C9 1.408(4) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.395(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.497(4) . ?
C14 O4 1.458(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O5 1.369(3) . ?
C15 C20 1.391(4) . ?
C15 C16 1.396(4) . ?
C16 C17 1.396(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.378(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.391(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.390(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.497(4) . ?
C21 O6 1.465(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O1 Ge1 1.8408(19) . ?
O2 Ge1 1.986(2) . ?
O2 Ge3 1.988(2) . ?
O3 Ge2 1.848(2) . ?
O4 Ge2 1.939(2) . ?
O4 Ge1 1.975(2) . ?
O5 Ge3 1.8447(19) . ?
O6 Ge3 1.951(2) . ?
O6 Ge2 1.988(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
O1 C1 C6 119.2(3) . . ?
O1 C1 C2 120.7(3) . . ?
C6 C1 C2 120.1(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 119.6(3) . . ?
C1 C6 C7 117.2(3) . . ?
C5 C6 C7 123.1(3) . . ?
O2 C7 C6 110.5(2) . . ?
O2 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
O2 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
O3 C8 C13 122.1(3) . . ?
O3 C8 C9 118.5(3) . . ?
C13 C8 C9 119.4(3) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.3(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C8 C13 C12 119.8(3) . . ?
C8 C13 C14 118.5(3) . . ?
C12 C13 C14 121.7(3) . . ?
O4 C14 C13 109.3(2) . . ?
O4 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
O4 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
O5 C15 C20 119.6(3) . . ?
O5 C15 C16 119.9(3) . . ?
C20 C15 C16 120.5(3) . . ?
C17 C16 C15 118.6(3) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 120.3(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C15 119.7(3) . . ?
C19 C20 C21 122.2(3) . . ?
C15 C20 C21 118.1(3) . . ?
O6 C21 C20 110.9(2) . . ?
O6 C21 H21A 109.5 . . ?
C20 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.0 . . ?
C1 O1 Ge1 121.27(17) . . ?
C7 O2 Ge1 113.79(17) . . ?
C7 O2 Ge3 113.72(17) . . ?
Ge1 O2 Ge3 132.48(10) . . ?
C8 O3 Ge2 127.24(18) . . ?
C14 O4 Ge2 114.02(17) . . ?
C14 O4 Ge1 117.13(17) . . ?
Ge2 O4 Ge1 128.28(11) . . ?
C15 O5 Ge3 122.07(18) . . ?
C21 O6 Ge3 116.45(17) . . ?
C21 O6 Ge2 123.98(17) . . ?
Ge3 O6 Ge2 115.94(10) . . ?
O1 Ge1 O4 92.50(9) . . ?
O1 Ge1 O2 92.45(9) . . ?
O4 Ge1 O2 86.80(9) . . ?
O3 Ge2 O4 91.35(9) . . ?
O3 Ge2 O6 97.57(9) . . ?
O4 Ge2 O6 88.82(8) . . ?
O5 Ge3 O6 92.77(9) . . ?
O5 Ge3 O2 97.60(8) . . ?
O6 Ge3 O2 86.64(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -176.3(2) . . . . ?
C6 C1 C2 C3 2.4(4) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C2 C3 C4 C5 -1.0(4) . . . . ?
C3 C4 C5 C6 2.1(4) . . . . ?
O1 C1 C6 C5 177.4(2) . . . . ?
C2 C1 C6 C5 -1.3(4) . . . . ?
O1 C1 C6 C7 -1.7(4) . . . . ?
C2 C1 C6 C7 179.6(3) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C4 C5 C6 C7 178.1(3) . . . . ?
C1 C6 C7 O2 -57.2(3) . . . . ?
C5 C6 C7 O2 123.8(3) . . . . ?
O3 C8 C9 C10 177.9(3) . . . . ?
C13 C8 C9 C10 -0.9(4) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C9 C10 C11 C12 0.2(5) . . . . ?
C10 C11 C12 C13 -1.3(5) . . . . ?
O3 C8 C13 C12 -178.9(3) . . . . ?
C9 C8 C13 C12 -0.2(4) . . . . ?
O3 C8 C13 C14 2.1(4) . . . . ?
C9 C8 C13 C14 -179.1(3) . . . . ?
C11 C12 C13 C8 1.3(4) . . . . ?
C11 C12 C13 C14 -179.8(3) . . . . ?
C8 C13 C14 O4 49.3(4) . . . . ?
C12 C13 C14 O4 -129.7(3) . . . . ?
O5 C15 C16 C17 179.3(2) . . . . ?
C20 C15 C16 C17 0.9(4) . . . . ?
C15 C16 C17 C18 0.9(4) . . . . ?
C16 C17 C18 C19 -1.2(4) . . . . ?
C17 C18 C19 C20 -0.3(4) . . . . ?
C18 C19 C20 C15 2.1(4) . . . . ?
C18 C19 C20 C21 -176.4(3) . . . . ?
O5 C15 C20 C19 179.2(2) . . . . ?
C16 C15 C20 C19 -2.4(4) . . . . ?
O5 C15 C20 C21 -2.2(4) . . . . ?
C16 C15 C20 C21 176.2(3) . . . . ?
C19 C20 C21 O6 -125.6(3) . . . . ?
C15 C20 C21 O6 55.8(3) . . . . ?
C6 C1 O1 Ge1 52.5(3) . . . . ?
C2 C1 O1 Ge1 -128.8(2) . . . . ?
C6 C7 O2 Ge1 61.5(3) . . . . ?
C6 C7 O2 Ge3 -119.4(2) . . . . ?
C13 C8 O3 Ge2 -31.8(4) . . . . ?
C9 C8 O3 Ge2 149.5(2) . . . . ?
C13 C14 O4 Ge2 -70.0(3) . . . . ?
C13 C14 O4 Ge1 118.0(2) . . . . ?
C20 C15 O5 Ge3 -48.0(3) . . . . ?
C16 C15 O5 Ge3 133.6(2) . . . . ?
C20 C21 O6 Ge3 -57.2(3) . . . . ?
C20 C21 O6 Ge2 100.4(2) . . . . ?
C1 O1 Ge1 O4 49.3(2) . . . . ?
C1 O1 Ge1 O2 -37.6(2) . . . . ?
C14 O4 Ge1 O1 74.74(19) . . . . ?
Ge2 O4 Ge1 O1 -95.95(14) . . . . ?
C14 O4 Ge1 O2 167.06(19) . . . . ?
Ge2 O4 Ge1 O2 -3.63(13) . . . . ?
C7 O2 Ge1 O1 -17.67(19) . . . . ?
Ge3 O2 Ge1 O1 163.42(15) . . . . ?
C7 O2 Ge1 O4 -110.04(19) . . . . ?
Ge3 O2 Ge1 O4 71.06(15) . . . . ?
C8 O3 Ge2 O4 9.8(2) . . . . ?
C8 O3 Ge2 O6 -79.2(2) . . . . ?
C14 O4 Ge2 O3 39.21(18) . . . . ?
Ge1 O4 Ge2 O3 -149.87(14) . . . . ?
C14 O4 Ge2 O6 136.75(18) . . . . ?
Ge1 O4 Ge2 O6 -52.32(14) . . . . ?
C21 O6 Ge2 O3 22.1(2) . . . . ?
Ge3 O6 Ge2 O3 179.83(10) . . . . ?
C21 O6 Ge2 O4 -69.1(2) . . . . ?
Ge3 O6 Ge2 O4 88.63(11) . . . . ?
C15 O5 Ge3 O6 37.1(2) . . . . ?
C15 O5 Ge3 O2 -49.9(2) . . . . ?
C21 O6 Ge3 O5 14.83(19) . . . . ?
Ge2 O6 Ge3 O5 -144.58(11) . . . . ?
C21 O6 Ge3 O2 112.29(19) . . . . ?
Ge2 O6 Ge3 O2 -47.12(11) . . . . ?
C7 O2 Ge3 O5 -132.76(19) . . . . ?
Ge1 O2 Ge3 O5 46.15(16) . . . . ?
C7 O2 Ge3 O6 134.89(19) . . . . ?
Ge1 O2 Ge3 O6 -46.21(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        63.94
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.107
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1438302'
_audit_update_record             
;
2015-11-23 deposited with the CCDC.
2016-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 Ge2 O4'
_chemical_formula_sum            'C16 H16 Ge2 O4'
_chemical_formula_weight         417.47

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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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                   5.0400(8)
_cell_length_b                   5.7142(6)
_cell_length_c                   13.393(2)
_cell_angle_alpha                78.607(11)
_cell_angle_beta                 81.131(14)
_cell_angle_gamma                89.160(11)
_cell_volume                     373.54(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    110
_cell_measurement_reflns_used    1095
_cell_measurement_theta_min      4.0630
_cell_measurement_theta_max      27.7310
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.9991 -0.0238 -0.0014 0.0003 -0.9989 0.0002 0.7820 -0.0108 -0.9999
_exptl_crystal_size_max          0.4974
_exptl_crystal_size_mid          0.4881
_exptl_crystal_size_min          0.0897
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7 0 2 0.2143 -6.9919 0.0021 1.5118 -0.1001 -0.9530 0.3256
0 0 18 0.0512 0.0236 -0.0097 18.0014 0.9082 -0.3675 -0.0923
0 0 -18 0.0385 -0.0236 0.0097 -18.0014 -0.9082 0.3675 0.0923
0 -8 0 0.2738 -0.1875 -7.9969 -0.0901 -0.0314 -0.3788 -0.9385
7 0 -2 0.2401 6.9919 -0.0021 -1.5118 0.1001 0.9530 -0.3256
0 8 0 0.1907 0.1875 7.9969 0.0901 0.0314 0.3788 0.9385
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_min  0.50052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_crystal_description       plate
_exptl_crystal_colour            colorless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_F_000             208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1656
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.141
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_orient_matrix_UB_11      0.0252138000
_diffrn_orient_matrix_UB_12      0.0027629000
_diffrn_orient_matrix_UB_13      0.0504175000
_diffrn_orient_matrix_UB_21      0.1318722000
_diffrn_orient_matrix_UB_22      0.0445043000
_diffrn_orient_matrix_UB_23      -0.0205620000
_diffrn_orient_matrix_UB_31      -0.0476196000
_diffrn_orient_matrix_UB_32      0.1185313000
_diffrn_orient_matrix_UB_33      -0.0050018000
_diffrn_oxdiff_twin_integration_method simultaneous
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.4617 459 1705
2 0.5383 463 1705

_reflns_number_total             1656
_reflns_number_gt                1558
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1321P)²+2.0827P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1656
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1798
_refine_ls_wR_factor_gt          0.1783
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002

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
C1 C -0.005(2) 0.3169(16) 0.3142(8) 0.015(2) Uani 1 1 d . . . . .
C2 C -0.193(2) 0.2242(16) 0.2645(7) 0.016(2) Uani 1 1 d . . . . .
H2 H -0.2602 0.0698 0.2900 0.019 Uiso 1 1 calc R U . . .
C3 C -0.277(2) 0.3574(18) 0.1791(8) 0.019(2) Uani 1 1 d . . . . .
H3 H -0.3996 0.2895 0.1473 0.023 Uiso 1 1 calc R U . . .
C4 C -0.188(2) 0.5908(17) 0.1378(7) 0.017(2) Uani 1 1 d . . . . .
C5 C -0.0069(18) 0.6826(16) 0.1888(7) 0.016(2) Uani 1 1 d . . . . .
H5 H 0.0556 0.8386 0.1636 0.019 Uiso 1 1 calc R U . . .
C6 C 0.0861(19) 0.5538(17) 0.2756(7) 0.014(2) Uani 1 1 d . . . . .
C7 C 0.276(2) 0.6620(17) 0.3308(7) 0.015(2) Uani 1 1 d . . . . .
H7A H 0.4522 0.5934 0.3186 0.018 Uiso 1 1 calc R U . . .
H7B H 0.2922 0.8326 0.3042 0.018 Uiso 1 1 calc R U . . .
C8 C -0.283(2) 0.7378(18) 0.0441(8) 0.021(2) Uani 1 1 d . . . . .
H8A H -0.4066 0.6442 0.0195 0.032 Uiso 1 1 calc R U . . .
H8B H -0.1325 0.7858 -0.0090 0.032 Uiso 1 1 calc R U . . .
H8C H -0.3723 0.8769 0.0620 0.032 Uiso 1 1 calc R U . . .
O1 O 0.0866(14) 0.1783(11) 0.3956(5) 0.0159(14) Uani 1 1 d . . . . .
O2 O 0.1776(14) 0.6176(11) 0.4414(5) 0.0157(14) Uani 1 1 d . . . . .
Ge1 Ge 0.1836(2) 0.27632(18) 0.50974(8) 0.0143(4) Uani 1 1 d . . . . .


_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
C1 O1 1.354(12) . ?
C1 C2 1.401(14) . ?
C1 C6 1.406(14) . ?
C2 C3 1.367(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(14) . ?
C4 C8 1.508(14) . ?
C5 C6 1.391(14) . ?
C5 H5 0.9300 . ?
C6 C7 1.503(13) . ?
C7 O2 1.460(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O1 Ge1 1.862(7) . ?
O2 Ge1 1.966(7) 2_566 ?
O2 Ge1 1.986(6) . ?
Ge1 O2 1.966(7) 2_566 ?

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
O1 C1 C2 120.1(8) . . ?
O1 C1 C6 121.9(9) . . ?
C2 C1 C6 118.0(9) . . ?
C3 C2 C1 120.9(9) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 122.5(10) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C5 C4 C3 116.1(9) . . ?
C5 C4 C8 121.5(9) . . ?
C3 C4 C8 122.4(10) . . ?
C4 C5 C6 123.5(9) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C5 C6 C1 118.9(9) . . ?
C5 C6 C7 122.0(9) . . ?
C1 C6 C7 119.1(9) . . ?
O2 C7 C6 110.3(8) . . ?
O2 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
O2 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 O1 Ge1 127.1(6) . . ?
C7 O2 Ge1 119.1(6) . 2_566 ?
C7 O2 Ge1 113.8(5) . . ?
Ge1 O2 Ge1 104.6(3) 2_566 . ?
O1 Ge1 O2 94.9(3) . 2_566 ?
O1 Ge1 O2 91.6(3) . . ?
O2 Ge1 O2 75.4(3) 2_566 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -176.7(9) . . . . ?
C6 C1 C2 C3 2.1(15) . . . . ?
C1 C2 C3 C4 -1.1(16) . . . . ?
C2 C3 C4 C5 -0.3(15) . . . . ?
C2 C3 C4 C8 -179.5(9) . . . . ?
C3 C4 C5 C6 0.6(15) . . . . ?
C8 C4 C5 C6 179.8(9) . . . . ?
C4 C5 C6 C1 0.5(15) . . . . ?
C4 C5 C6 C7 -178.1(9) . . . . ?
O1 C1 C6 C5 177.0(8) . . . . ?
C2 C1 C6 C5 -1.8(14) . . . . ?
O1 C1 C6 C7 -4.4(14) . . . . ?
C2 C1 C6 C7 176.8(9) . . . . ?
C5 C6 C7 O2 130.6(9) . . . . ?
C1 C6 C7 O2 -47.9(12) . . . . ?
C2 C1 O1 Ge1 -146.7(8) . . . . ?
C6 C1 O1 Ge1 34.5(13) . . . . ?
C6 C7 O2 Ge1 -56.6(9) . . . 2_566 ?
C6 C7 O2 Ge1 67.5(9) . . . . ?
C1 O1 Ge1 O2 63.3(8) . . . 2_566 ?
C1 O1 Ge1 O2 -12.2(8) . . . . ?

_refine_diff_density_max         1.495
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.237

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1438303'
_audit_update_record             
;
2015-11-23 deposited with the CCDC.
2016-01-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C28 H24 Ge4 O8), C5 H12'
_chemical_formula_sum            'C61 H60 Ge8 O16'
_chemical_formula_weight         1629.81

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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

_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'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   14.4998(3)
_cell_length_b                   14.4998(3)
_cell_length_c                   14.6335(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3076.61(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    110
_cell_measurement_reflns_used    3207
_cell_measurement_theta_min      3.4100
_cell_measurement_theta_max      28.1490

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colourless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_F_000             1620
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    3.920
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.87230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5657
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.421
_diffrn_reflns_theta_max         24.977
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             2651
_reflns_number_gt                2550
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_max     0.962
_reflns_Friedel_fraction_full    0.962

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.038(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2651
_refine_ls_number_parameters     191
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0463
_refine_ls_wR_factor_gt          0.0458
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.055
_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
C1 C 0.8592(3) 0.3824(3) 0.3658(4) 0.0411(12) Uani 1 1 d . . . . .
H1A H 0.8002 0.3610 0.3429 0.049 Uiso 1 1 calc R U . . .
H1B H 0.8483 0.4170 0.4215 0.049 Uiso 1 1 calc R U . . .
C1O C 0.4980(16) 0.0330(9) 0.1635(9) 0.107(3) Uani 0.5 1 d D U P . .
H1O1 H 0.4426 0.0706 0.1635 0.128 Uiso 0.5 1 calc R U P . .
H1O2 H 0.5485 0.0769 0.1635 0.128 Uiso 0.5 1 calc R U P . .
C2 C 0.9198(3) 0.3012(3) 0.3862(3) 0.0350(11) Uani 1 1 d . . . . .
C2O C 0.5000 0.0000 0.0773(8) 0.107(3) Uani 1 2 d DS TU P . .
H2O1 H 0.4966 0.0504 0.0349 0.160 Uiso 0.5 1 calc R U P . .
H2O2 H 0.4484 -0.0405 0.0680 0.160 Uiso 0.5 1 calc R U P . .
H2O3 H 0.5563 -0.0334 0.0678 0.160 Uiso 0.5 1 calc R U P . .
C3 C 0.9503(4) 0.2792(4) 0.4738(4) 0.0542(16) Uani 1 1 d . . . . .
H3 H 0.9316 0.3150 0.5232 0.065 Uiso 1 1 calc R U . . .
C3O C 0.5000 0.0000 0.2500 0.107(3) Uani 1 4 d DS TU P . .
H3O1 H 0.5107 -0.0646 0.2365 0.128 Uiso 0.25 1 calc R U P . .
H3O2 H 0.4346 0.0029 0.2635 0.128 Uiso 0.25 1 calc R U P . .
C4 C 1.0078(4) 0.2049(5) 0.4879(5) 0.065(2) Uani 1 1 d . . . . .
H4 H 1.0276 0.1908 0.5468 0.079 Uiso 1 1 calc R U . . .
C5 C 1.0356(4) 0.1525(5) 0.4165(5) 0.0644(19) Uani 1 1 d . . . . .
H5 H 1.0752 0.1031 0.4266 0.077 Uiso 1 1 calc R U . . .
C6 C 1.0056(3) 0.1715(3) 0.3285(4) 0.0459(13) Uani 1 1 d . . . . .
H6 H 1.0242 0.1345 0.2800 0.055 Uiso 1 1 calc R U . . .
C7 C 0.9471(3) 0.2468(3) 0.3133(4) 0.0332(11) Uani 1 1 d . . . . .
C11 C 0.4258(3) 0.3301(3) 0.3837(4) 0.0473(14) Uani 1 1 d . . . . .
H11A H 0.3971 0.3559 0.3295 0.057 Uiso 1 1 calc R U . . .
H11B H 0.3854 0.2827 0.4078 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5164(4) 0.2890(3) 0.3591(4) 0.0408(13) Uani 1 1 d . . . . .
C13 C 0.5491(4) 0.2864(3) 0.2710(4) 0.0484(14) Uani 1 1 d . . . . .
H13 H 0.5134 0.3103 0.2238 0.058 Uiso 1 1 calc R U . . .
C14 C 0.6351(4) 0.2486(4) 0.2516(4) 0.0526(15) Uani 1 1 d . . . . .
H14 H 0.6572 0.2469 0.1920 0.063 Uiso 1 1 calc R U . . .
C15 C 0.6873(4) 0.2133(3) 0.3229(4) 0.0468(13) Uani 1 1 d . . . . .
H15 H 0.7446 0.1875 0.3105 0.056 Uiso 1 1 calc R U . . .
C16 C 0.6561(3) 0.2158(3) 0.4114(4) 0.0382(12) Uani 1 1 d . . . . .
H16 H 0.6922 0.1917 0.4582 0.046 Uiso 1 1 calc R U . . .
C17 C 0.5706(3) 0.2541(3) 0.4310(4) 0.0356(11) Uani 1 1 d . . . . .
O1 O 0.9023(2) 0.4422(2) 0.2980(2) 0.0323(8) Uani 1 1 d . . . . .
O2 O 0.9174(2) 0.2657(2) 0.2271(2) 0.0334(8) Uani 1 1 d . . . . .
O3 O 0.4385(2) 0.4027(2) 0.4521(3) 0.0380(8) Uani 1 1 d . . . . .
O4 O 0.5374(2) 0.2560(2) 0.5179(2) 0.0378(8) Uani 1 1 d . . . . .
Ge1 Ge 0.92170(3) 0.38491(3) 0.17613(3) 0.02987(13) Uani 1 1 d . . . . .
Ge2 Ge 0.48628(3) 0.36045(3) 0.57116(4) 0.03529(15) Uani 1 1 d . . . . .


_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
C1 O1 1.458(6) . ?
C1 C2 1.500(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1O C2O 1.350(13) . ?
C1O C3O 1.353(13) . ?
C1O H1O1 0.9700 . ?
C1O H1O2 0.9700 . ?
C2 C7 1.384(7) . ?
C2 C3 1.393(7) . ?
C2O H2O1 0.9600 . ?
C2O H2O2 0.9600 . ?
C2O H2O3 0.9600 . ?
C3 C4 1.378(9) . ?
C3 H3 0.9300 . ?
C3O C1O 1.353(13) 7 ?
C3O H3O1 0.9700 . ?
C3O H3O2 0.9700 . ?
C4 C5 1.354(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.401(6) . ?
C6 H6 0.9300 . ?
C7 O2 1.360(6) . ?
C11 O3 1.464(6) . ?
C11 C12 1.486(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.375(7) . ?
C12 C17 1.407(7) . ?
C13 C14 1.392(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.386(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(6) . ?
C16 H16 0.9300 . ?
C17 O4 1.359(6) . ?
O1 Ge1 1.987(3) . ?
O1 Ge1 2.025(3) 7_565 ?
O2 Ge1 1.884(3) . ?
O3 Ge2 1.973(4) . ?
O3 Ge2 1.997(3) 3_566 ?
O4 Ge2 1.857(3) . ?
Ge1 O1 2.025(3) 8_645 ?
Ge2 O3 1.997(3) 4_656 ?

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
O1 C1 C2 110.6(4) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C2O C1O C3O 138.4(11) . . ?
C2O C1O H1O1 102.5 . . ?
C3O C1O H1O1 102.5 . . ?
C2O C1O H1O2 102.5 . . ?
C3O C1O H1O2 102.5 . . ?
H1O1 C1O H1O2 104.9 . . ?
C7 C2 C3 119.2(5) . . ?
C7 C2 C1 117.5(4) . . ?
C3 C2 C1 123.3(5) . . ?
C1O C2O H2O1 109.5 . . ?
C1O C2O H2O2 109.5 . . ?
H2O1 C2O H2O2 109.5 . . ?
C1O C2O H2O3 109.5 . . ?
H2O1 C2O H2O3 109.5 . . ?
H2O2 C2O H2O3 109.5 . . ?
C4 C3 C2 120.6(6) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C1O C3O C1O 150.9(8) . 7 ?
C1O C3O H3O1 98.9 . . ?
C1O C3O H3O1 98.9 7 . ?
C1O C3O H3O2 98.9 . . ?
C1O C3O H3O2 98.9 7 . ?
H3O1 C3O H3O2 103.9 . . ?
C5 C4 C3 120.2(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.8(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C7 119.5(6) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
O2 C7 C2 120.6(4) . . ?
O2 C7 C6 119.7(5) . . ?
C2 C7 C6 119.7(5) . . ?
O3 C11 C12 110.1(4) . . ?
O3 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
O3 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C17 119.9(5) . . ?
C13 C12 C11 122.9(5) . . ?
C17 C12 C11 117.2(5) . . ?
C12 C13 C14 120.7(6) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C16 C15 C14 121.4(5) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.9(5) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
O4 C17 C16 121.1(5) . . ?
O4 C17 C12 119.6(4) . . ?
C16 C17 C12 119.2(5) . . ?
C1 O1 Ge1 115.0(3) . . ?
C1 O1 Ge1 113.5(3) . 7_565 ?
Ge1 O1 Ge1 126.37(16) . 7_565 ?
C7 O2 Ge1 122.8(3) . . ?
C11 O3 Ge2 115.2(3) . . ?
C11 O3 Ge2 113.1(3) . 3_566 ?
Ge2 O3 Ge2 126.87(18) . 3_566 ?
C17 O4 Ge2 123.4(3) . . ?
O2 Ge1 O1 91.36(13) . . ?
O2 Ge1 O1 94.14(12) . 8_645 ?
O1 Ge1 O1 85.29(14) . 8_645 ?
O4 Ge2 O3 91.30(14) . . ?
O4 Ge2 O3 93.91(14) . 4_656 ?
O3 Ge2 O3 87.53(15) . 4_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C7 -55.5(6) . . . . ?
O1 C1 C2 C3 123.6(5) . . . . ?
C7 C2 C3 C4 0.8(8) . . . . ?
C1 C2 C3 C4 -178.4(5) . . . . ?
C2O C1O C3O C1O 133.08(10) . . . 7 ?
C2 C3 C4 C5 0.1(9) . . . . ?
C3 C4 C5 C6 -1.1(9) . . . . ?
C4 C5 C6 C7 1.0(8) . . . . ?
C3 C2 C7 O2 179.0(4) . . . . ?
C1 C2 C7 O2 -1.8(6) . . . . ?
C3 C2 C7 C6 -0.8(7) . . . . ?
C1 C2 C7 C6 178.4(4) . . . . ?
C5 C6 C7 O2 -179.9(4) . . . . ?
C5 C6 C7 C2 -0.1(7) . . . . ?
O3 C11 C12 C13 -123.1(5) . . . . ?
O3 C11 C12 C17 54.9(6) . . . . ?
C17 C12 C13 C14 0.9(8) . . . . ?
C11 C12 C13 C14 178.9(5) . . . . ?
C12 C13 C14 C15 0.0(8) . . . . ?
C13 C14 C15 C16 -0.4(8) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C15 C16 C17 O4 178.9(4) . . . . ?
C15 C16 C17 C12 0.9(6) . . . . ?
C13 C12 C17 O4 -179.4(4) . . . . ?
C11 C12 C17 O4 2.5(6) . . . . ?
C13 C12 C17 C16 -1.3(7) . . . . ?
C11 C12 C17 C16 -179.4(4) . . . . ?
C2 C1 O1 Ge1 63.3(5) . . . . ?
C2 C1 O1 Ge1 -140.3(3) . . . 7_565 ?
C2 C7 O2 Ge1 48.0(5) . . . . ?
C6 C7 O2 Ge1 -132.2(4) . . . . ?
C12 C11 O3 Ge2 -64.4(5) . . . . ?
C12 C11 O3 Ge2 138.6(4) . . . 3_566 ?
C16 C17 O4 Ge2 132.7(4) . . . . ?
C12 C17 O4 Ge2 -49.2(5) . . . . ?
C7 O2 Ge1 O1 -31.6(3) . . . . ?
C7 O2 Ge1 O1 53.8(3) . . . 8_645 ?
C17 O4 Ge2 O3 32.0(3) . . . . ?
C17 O4 Ge2 O3 -55.6(4) . . . 4_656 ?

_refine_diff_density_max         0.301
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.044

_shelxl_version_number           2013-4

