# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Extended-Ph-Ge4pericyclyne
_database_code_depnum_ccdc_archive 'CCDC 1516997'
_audit_update_record             
;
2016-11-12 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C66 H40 Cl4 Ge4'
_chemical_formula_moiety         'C66 H40 Cl4 Ge4'
_chemical_formula_weight         1265.21
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
_space_group_IT_number           87
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'
'-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                   13.7886(6)
_cell_length_b                   13.7886(6)
_cell_length_c                   15.0538(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     2862.13(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19219
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264.00
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_T_max  0.871

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            24146
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.419
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             1699
_reflns_number_gt                1503
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1108
_refine_ls_wR_factor_gt          0.1076
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         1699
_refine_ls_number_parameters     103
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0561P)²+6.1940P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Ge Ge 0.1547 1.8001
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.17377(3) 0.34657(3) 0.5000 0.03270(17) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.5000 0.9047(2) 0.1280(13) Uani 1 4 d S T P . .
Cl2 Cl 0.4001(4) 0.5325(4) 0.5000 0.1203(16) Uani 0.5 2 d S T P . .
C1 C 0.2328(3) 0.2223(3) 0.5000 0.0403(9) Uani 1 2 d S T P . .
C2 C 0.2636(3) 0.1403(3) 0.5000 0.0403(9) Uani 1 2 d S T P . .
C3 C 0.2949(3) 0.0461(3) 0.5000 0.0376(9) Uani 1 2 d S T P . .
C4 C 0.3199(3) -0.0375(3) 0.5000 0.0387(9) Uani 1 2 d S T P . .
C5 C 0.2045(2) 0.4141(2) 0.60800(19) 0.0372(6) Uani 1 1 d . . . . .
C6 C 0.2760(3) 0.3809(3) 0.6645(2) 0.0591(10) Uani 1 1 d . . . . .
H6 H 0.3106 0.3232 0.6507 0.071 Uiso 1 1 calc R U . . .
C7 C 0.2973(3) 0.4326(4) 0.7420(3) 0.0785(14) Uani 1 1 d . . . . .
H7 H 0.3469 0.4102 0.7807 0.094 Uiso 1 1 calc R U . . .
C8 C 0.2476(3) 0.5141(4) 0.7620(3) 0.0691(12) Uani 1 1 d . . . . .
H8 H 0.2624 0.5486 0.8149 0.083 Uiso 1 1 calc R U . . .
C9 C 0.1761(3) 0.5475(3) 0.7069(3) 0.0573(9) Uani 1 1 d . . . . .
H9 H 0.1415 0.6049 0.7216 0.069 Uiso 1 1 calc R U . . .
C10 C 0.1544(2) 0.4981(2) 0.6302(2) 0.0458(7) Uani 1 1 d . . . . .
H10 H 0.1047 0.5214 0.5921 0.055 Uiso 1 1 calc R U . . .
C11 C 0.485(5) 0.5476(17) 1.0000 0.065(7) Uani 0.25 2 d S T P . .
C12 C 0.5000 0.5000 0.5764(16) 0.133(10) Uani 0.5 4 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C1 1.896(4) . ?
Ge1 C4 1.915(4) 3 ?
Ge1 C5 1.921(3) . ?
Ge1 C5 1.921(3) 10_556 ?
Cl1 C11 1.592(9) 11_567 ?
Cl1 C11 1.592(9) 9_667 ?
Cl1 C11 1.592(9) 3_655 ?
Cl1 C11 1.592(9) . ?
Cl2 C12 1.850(16) . ?
Cl2 C12 1.850(16) 9_666 ?
Cl2 Cl2 2.048(8) 3_655 ?
Cl2 Cl2 2.048(8) 11_566 ?
C1 C2 1.209(6) . ?
C2 C3 1.369(6) . ?
C3 C4 1.203(6) . ?
C4 Ge1 1.915(4) 11_556 ?
C5 C6 1.380(4) . ?
C5 C10 1.390(4) . ?
C6 C7 1.399(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.351(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C11 0.97(3) 3_655 ?
C11 C11 0.97(3) 11_567 ?
C11 C11 1.38(4) 9_667 ?
C11 Cl1 1.592(9) 9_667 ?
C12 Cl2 1.850(16) 3_655 ?
C12 Cl2 1.850(16) 9_666 ?
C12 Cl2 1.850(16) 11_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
C1 Ge1 C4 104.32(18) . 3 ?
C1 Ge1 C5 110.06(11) . . ?
C4 Ge1 C5 108.05(10) 3 . ?
C1 Ge1 C5 110.06(11) . 10_556 ?
C4 Ge1 C5 108.04(10) 3 10_556 ?
C5 Ge1 C5 115.65(17) . 10_556 ?
C11 Cl1 C11 35.7(8) 11_567 9_667 ?
C11 Cl1 C11 51.3(13) 11_567 3_655 ?
C11 Cl1 C11 35.7(8) 9_667 3_655 ?
C11 Cl1 C11 35.7(8) 11_567 . ?
C11 Cl1 C11 51.3(13) 9_667 . ?
C11 Cl1 C11 35.7(8) 3_655 . ?
C12 Cl2 C12 76.9(12) . 9_666 ?
C12 Cl2 Cl2 56.4(3) . 3_655 ?
C12 Cl2 Cl2 56.4(3) 9_666 3_655 ?
C12 Cl2 Cl2 56.4(3) . 11_566 ?
C12 Cl2 Cl2 56.4(3) 9_666 11_566 ?
Cl2 Cl2 Cl2 90.000(1) 3_655 11_566 ?
C2 C1 Ge1 175.2(4) . . ?
C1 C2 C3 177.7(5) . . ?
C4 C3 C2 178.3(5) . . ?
C3 C4 Ge1 174.4(4) . 11_556 ?
C6 C5 C10 118.9(3) . . ?
C6 C5 Ge1 121.2(3) . . ?
C10 C5 Ge1 119.8(2) . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 120.6(4) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 120.0(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C5 120.5(3) . . ?
C9 C10 H10 119.8 . . ?
C5 C10 H10 119.8 . . ?
C11 C11 C11 90.000(6) 3_655 11_567 ?
C11 C11 C11 45.000(12) 3_655 9_667 ?
C11 C11 C11 45.000(13) 11_567 9_667 ?
C11 C11 Cl1 72.2(4) 3_655 9_667 ?
C11 C11 Cl1 72.2(4) 11_567 9_667 ?
C11 C11 Cl1 64.3(6) 9_667 9_667 ?
C11 C11 Cl1 72.2(4) 3_655 . ?
C11 C11 Cl1 72.2(4) 11_567 . ?
C11 C11 Cl1 64.3(6) 9_667 . ?
Cl1 C11 Cl1 128.7(13) 9_667 . ?
Cl2 C12 Cl2 67.2(7) 3_655 9_666 ?
Cl2 C12 Cl2 103.1(12) 3_655 11_566 ?
Cl2 C12 Cl2 67.2(7) 9_666 11_566 ?
Cl2 C12 Cl2 67.2(7) 3_655 . ?
Cl2 C12 Cl2 103.1(12) 9_666 . ?
Cl2 C12 Cl2 67.2(7) 11_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
C10 C5 C6 C7 -0.7(6) . . . . ?
Ge1 C5 C6 C7 179.2(3) . . . . ?
C5 C6 C7 C8 0.6(7) . . . . ?
C6 C7 C8 C9 -0.2(7) . . . . ?
C7 C8 C9 C10 -0.1(6) . . . . ?
C8 C9 C10 C5 0.0(5) . . . . ?
C6 C5 C10 C9 0.4(5) . . . . ?
Ge1 C5 C10 C9 -179.5(3) . . . . ?
C11 Cl1 C11 C11 -95.9(3) 11_567 . . 3_655 ?
C11 Cl1 C11 C11 -47.97(15) 9_667 . . 3_655 ?
C11 Cl1 C11 C11 47.97(15) 9_667 . . 11_567 ?
C11 Cl1 C11 C11 95.9(3) 3_655 . . 11_567 ?
C11 Cl1 C11 C11 -47.97(15) 11_567 . . 9_667 ?
C11 Cl1 C11 C11 47.97(14) 3_655 . . 9_667 ?
C11 Cl1 C11 Cl1 -47.97(15) 11_567 . . 9_667 ?
C11 Cl1 C11 Cl1 0.000(3) 9_667 . . 9_667 ?
C11 Cl1 C11 Cl1 47.97(15) 3_655 . . 9_667 ?
C12 Cl2 C12 Cl2 -58.1(3) 9_666 . . 3_655 ?
Cl2 Cl2 C12 Cl2 -116.2(7) 11_566 . . 3_655 ?
C12 Cl2 C12 Cl2 -0.001(0) 9_666 . . 9_666 ?
Cl2 Cl2 C12 Cl2 58.1(3) 3_655 . . 9_666 ?
Cl2 Cl2 C12 Cl2 -58.1(3) 11_566 . . 9_666 ?
C12 Cl2 C12 Cl2 58.1(3) 9_666 . . 11_566 ?
Cl2 Cl2 C12 Cl2 116.2(7) 3_655 . . 11_566 ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        'extended octaphenyl germa[4]pericyclyne'
_chemical_name_common            'Ext_PhGe4 with CH2Cl2'
####################################################################### 
# 
# 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_Extended-Diphenyl-Ge6pericyclytriclinic
_database_code_depnum_ccdc_archive 'CCDC 1516999'
_audit_update_record             
;
2016-11-12 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C96 H50 Ge6'
_chemical_formula_moiety         'C96 H50 Ge6'
_chemical_formula_weight         1638.99
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.8171(2)
_cell_length_b                   17.6246(5)
_cell_length_c                   17.7526(6)
_cell_angle_alpha                66.8920(5)
_cell_angle_beta                 87.6960(6)
_cell_angle_gamma                79.5920(6)
_cell_volume                     2494.2054(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    23926
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      25.36
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             818.00
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_T_max  0.964

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            34761
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.026
_diffrn_reflns_theta_full        25.242
_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_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             9140
_reflns_number_gt                6837
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1545
_refine_ls_wR_factor_gt          0.1439
_refine_ls_number_restraints     18
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9140
_refine_ls_number_parameters     515
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0836P)²+1.7553P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Ge Ge 0.1547 1.8001
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.38583(5) 0.14854(3) 0.83443(3) 0.04943(16) Uani 1 1 d . . . . .
Ge2 Ge 0.39341(5) 0.44608(3) 0.39047(3) 0.04448(15) Uani 1 1 d . . . . .
Ge3 Ge 0.05027(5) 0.23358(3) 0.15843(3) 0.05243(17) Uani 1 1 d . . . . .
C1 C 0.8055(5) -0.1382(3) 0.8386(3) 0.0568(12) Uani 1 1 d . . . . .
C2 C 0.7154(5) -0.0780(3) 0.8380(3) 0.0588(13) Uani 1 1 d . . . . .
C3 C 0.6121(5) -0.0085(3) 0.8370(3) 0.0570(12) Uani 1 1 d . . . . .
C4 C 0.5260(6) 0.0505(3) 0.8371(3) 0.0594(13) Uani 1 1 d . . . . .
C5 C 0.3816(5) 0.2249(3) 0.7233(3) 0.0579(12) Uani 1 1 d . . . . .
C6 C 0.3838(5) 0.2702(3) 0.6523(4) 0.0555(12) Uani 1 1 d . . . . .
C7 C 0.3834(6) 0.3240(3) 0.5713(3) 0.0544(12) Uani 1 1 d . . . . .
C8 C 0.3852(5) 0.3707(3) 0.5018(3) 0.0570(12) Uani 1 1 d . . . . .
C9 C 0.3201(5) 0.3903(3) 0.3304(3) 0.0513(11) Uani 1 1 d . . . . .
C10 C 0.2665(5) 0.3563(3) 0.2939(3) 0.0510(11) Uani 1 1 d . . . . .
C11 C 0.2020(5) 0.3177(3) 0.2517(3) 0.0543(12) Uani 1 1 d . . . . .
C12 C 0.1442(5) 0.2836(3) 0.2163(3) 0.0568(12) Uani 1 1 d . . . . .
C13 C 0.4647(6) 0.1933(3) 0.9037(4) 0.0690(15) Uani 1 1 d . . . . .
C14 C 0.4916(17) 0.2732(5) 0.8734(6) 0.201(7) Uani 1 1 d . . . . .
H14 H 0.4696 0.3091 0.8175 0.241 Uiso 1 1 calc R U . . .
C15 C 0.554(3) 0.3012(8) 0.9284(9) 0.305(12) Uani 1 1 d . . . . .
H15 H 0.5766 0.3562 0.9092 0.366 Uiso 1 1 calc R U . . .
C16 C 0.5817(17) 0.2477(7) 1.0105(7) 0.185(6) Uani 1 1 d . . . . .
H16 H 0.6147 0.2682 1.0480 0.222 Uiso 1 1 calc R U . . .
C17 C 0.5638(8) 0.1727(5) 1.0356(4) 0.100(2) Uani 1 1 d . . . . .
H17 H 0.5857 0.1363 1.0914 0.120 Uiso 1 1 calc R U . . .
C18 C 0.5131(6) 0.1446(4) 0.9827(4) 0.0762(16) Uani 1 1 d . . . . .
H18 H 0.5109 0.0863 1.0018 0.091 Uiso 1 1 calc R U . . .
C19 C 0.1834(5) 0.1206(3) 0.8634(3) 0.0513(11) Uani 1 1 d . . . . .
C20 C 0.1087(6) 0.1341(4) 0.9273(4) 0.0810(18) Uani 1 1 d . . . . .
H20 H 0.1580 0.1560 0.9590 0.097 Uiso 1 1 calc R U . . .
C21 C -0.0380(7) 0.1161(5) 0.9462(4) 0.100(2) Uani 1 1 d . . . . .
H21 H -0.0887 0.1261 0.9906 0.120 Uiso 1 1 calc R U . . .
C22 C -0.1095(6) 0.0849(4) 0.9028(4) 0.0811(18) Uani 1 1 d . . . . .
H22 H -0.2095 0.0719 0.9167 0.097 Uiso 1 1 calc R U . . .
C23 C -0.0377(7) 0.0721(4) 0.8390(5) 0.0846(19) Uani 1 1 d . . . . .
H23 H -0.0888 0.0509 0.8074 0.102 Uiso 1 1 calc R U . . .
C24 C 0.1101(6) 0.0895(3) 0.8189(4) 0.0695(15) Uani 1 1 d . . . . .
H24 H 0.1596 0.0797 0.7742 0.083 Uiso 1 1 calc R U . . .
C25 C 0.6041(5) 0.4567(3) 0.3641(3) 0.0491(11) Uani 1 1 d . . . . .
C26 C 0.6493(5) 0.5328(3) 0.3382(3) 0.0539(12) Uani 1 1 d . . . . .
H26 H 0.5755 0.5816 0.3314 0.065 Uiso 1 1 calc R U . . .
C27 C 0.8039(6) 0.5389(3) 0.3219(4) 0.0665(14) Uani 1 1 d . . . . .
H27 H 0.8347 0.5920 0.3041 0.080 Uiso 1 1 calc R U . . .
C28 C 0.9079(6) 0.4713(4) 0.3308(4) 0.0734(16) Uani 1 1 d . . . . .
H28 H 1.0120 0.4770 0.3179 0.088 Uiso 1 1 calc R U . . .
C29 C 0.8679(6) 0.3926(4) 0.3586(4) 0.0837(19) Uani 1 1 d . . . . .
H29 H 0.9435 0.3442 0.3660 0.100 Uiso 1 1 calc R U . . .
C30 C 0.7136(6) 0.3861(4) 0.3755(4) 0.0771(17) Uani 1 1 d . . . . .
H30 H 0.6838 0.3326 0.3951 0.092 Uiso 1 1 calc R U . . .
C31 C 0.2560(5) 0.5503(3) 0.3718(3) 0.0456(10) Uani 1 1 d . . . . .
C32 C 0.1743(6) 0.5640(3) 0.4354(3) 0.0632(13) Uani 1 1 d . . . . .
H32 H 0.1883 0.5220 0.4894 0.076 Uiso 1 1 calc R U . . .
C33 C 0.0734(7) 0.6381(4) 0.4204(4) 0.0806(17) Uani 1 1 d . . . . .
H33 H 0.0156 0.6461 0.4639 0.097 Uiso 1 1 calc R U . . .
C34 C 0.0554(6) 0.7003(3) 0.3435(4) 0.0720(16) Uani 1 1 d . . . . .
H34 H -0.0117 0.7521 0.3339 0.086 Uiso 1 1 calc R U . . .
C35 C 0.1346(7) 0.6874(3) 0.2809(4) 0.0732(16) Uani 1 1 d . . . . .
H35 H 0.1218 0.7304 0.2274 0.088 Uiso 1 1 calc R U . . .
C36 C 0.2335(6) 0.6124(3) 0.2942(3) 0.0646(14) Uani 1 1 d . . . . .
H36 H 0.2860 0.6038 0.2496 0.077 Uiso 1 1 calc R U . . .
C37A C 0.0231(18) 0.3056(12) 0.0432(13) 0.063(5) Uani 0.552(12) 1 d D . P A 1
C38A C 0.1424(14) 0.3239(7) -0.0075(8) 0.087(4) Uani 0.552(12) 1 d D . P A 1
C39A C 0.1189(17) 0.3771(8) -0.0889(8) 0.098(5) Uani 0.552(12) 1 d D . P A 1
C41A C -0.156(2) 0.393(2) -0.0695(11) 0.34(3) Uani 0.552(12) 1 d D . P A 1
C42A C -0.1230(15) 0.3409(17) 0.0134(9) 0.26(2) Uani 0.552(12) 1 d D . P A 1
C40A C -0.031(2) 0.4099(17) -0.1174(13) 0.146(12) Uani 0.552(12) 1 d D . P A 1
C41B C -0.038(3) 0.4638(13) -0.0405(14) 0.204(16) Uani 0.448(12) 1 d D . P A 2
C42B C -0.008(3) 0.4049(9) 0.0394(10) 0.124(8) Uani 0.448(12) 1 d D . P A 2
C38B C -0.007(3) 0.3037(9) -0.0136(9) 0.115(8) Uani 0.448(12) 1 d D . P A 2
C39B C -0.037(3) 0.3650(10) -0.0917(11) 0.139(14) Uani 0.448(12) 1 d D . P A 2
C37B C 0.008(3) 0.3217(13) 0.0534(16) 0.056(6) Uani 0.448(12) 1 d D . P A 2
C40B C -0.053(3) 0.4494(11) -0.111(2) 0.131(12) Uani 0.448(12) 1 d D . P A 2
C43 C -0.1323(5) 0.1958(3) 0.2138(3) 0.0569(12) Uani 1 1 d . . . . .
C44 C -0.2312(7) 0.2449(5) 0.2445(6) 0.116(3) Uani 1 1 d . . . . .
H44 H -0.2058 0.2959 0.2422 0.139 Uiso 1 1 calc R U . . .
C45 C -0.3676(8) 0.2216(6) 0.2787(7) 0.141(4) Uani 1 1 d . . . . .
H45 H -0.4361 0.2571 0.2987 0.170 Uiso 1 1 calc R U . . .
C46 C -0.4047(7) 0.1475(5) 0.2839(5) 0.099(2) Uani 1 1 d . . . . .
H46 H -0.4979 0.1309 0.3078 0.119 Uiso 1 1 calc R U . . .
C47 C -0.3059(7) 0.0985(4) 0.2544(4) 0.0835(18) Uani 1 1 d . . . . .
H47 H -0.3288 0.0463 0.2590 0.100 Uiso 1 1 calc R U . . .
C48 C -0.1734(6) 0.1230(4) 0.2180(4) 0.0705(15) Uani 1 1 d . . . . .
H48 H -0.1086 0.0889 0.1951 0.085 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C5 1.900(6) . ?
Ge1 C13 1.910(5) . ?
Ge1 C4 1.919(5) . ?
Ge1 C19 1.933(4) . ?
Ge2 C9 1.904(5) . ?
Ge2 C8 1.907(6) . ?
Ge2 C25 1.922(4) . ?
Ge2 C31 1.924(4) . ?
Ge3 C12 1.887(5) . ?
Ge3 C37B 1.90(3) . ?
Ge3 C1 1.900(5) 2_656 ?
Ge3 C37A 1.94(2) . ?
Ge3 C43 1.936(5) . ?
C1 C2 1.201(7) . ?
C1 Ge3 1.900(5) 2_656 ?
C2 C3 1.383(7) . ?
C3 C4 1.172(6) . ?
C5 C6 1.200(7) . ?
C6 C7 1.378(8) . ?
C7 C8 1.185(7) . ?
C9 C10 1.198(6) . ?
C10 C11 1.387(6) . ?
C11 C12 1.204(6) . ?
C13 C14 1.358(9) . ?
C13 C18 1.362(8) . ?
C14 C15 1.419(13) . ?
C15 C16 1.393(15) . ?
C16 C17 1.256(11) . ?
C17 C18 1.344(8) . ?
C19 C24 1.360(7) . ?
C19 C20 1.369(7) . ?
C20 C21 1.385(8) . ?
C21 C22 1.338(9) . ?
C22 C23 1.352(9) . ?
C23 C24 1.394(7) . ?
C25 C26 1.365(6) . ?
C25 C30 1.380(7) . ?
C26 C27 1.397(6) . ?
C27 C28 1.324(7) . ?
C28 C29 1.386(8) . ?
C29 C30 1.397(7) . ?
C31 C36 1.377(7) . ?
C31 C32 1.392(7) . ?
C32 C33 1.376(7) . ?
C33 C34 1.368(8) . ?
C34 C35 1.361(8) . ?
C35 C36 1.385(7) . ?
C37A C42A 1.354(17) . ?
C37A C38A 1.356(16) . ?
C38A C39A 1.378(13) . ?
C39A C40A 1.374(17) . ?
C41A C40A 1.367(17) . ?
C41A C42A 1.404(16) . ?
C41B C40B 1.391(19) . ?
C41B C42B 1.392(17) . ?
C42B C37B 1.369(18) . ?
C38B C37B 1.363(17) . ?
C38B C39B 1.383(16) . ?
C39B C40B 1.368(19) . ?
C43 C44 1.366(8) . ?
C43 C48 1.368(7) . ?
C44 C45 1.381(9) . ?
C45 C46 1.371(10) . ?
C46 C47 1.351(9) . ?
C47 C48 1.368(8) . ?

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
C5 Ge1 C13 110.1(2) . . ?
C5 Ge1 C4 104.1(2) . . ?
C13 Ge1 C4 109.8(2) . . ?
C5 Ge1 C19 109.8(2) . . ?
C13 Ge1 C19 113.4(2) . . ?
C4 Ge1 C19 109.20(19) . . ?
C9 Ge2 C8 103.4(2) . . ?
C9 Ge2 C25 109.15(19) . . ?
C8 Ge2 C25 109.4(2) . . ?
C9 Ge2 C31 109.91(18) . . ?
C8 Ge2 C31 109.7(2) . . ?
C25 Ge2 C31 114.64(19) . . ?
C12 Ge3 C37B 102.6(6) . . ?
C12 Ge3 C1 106.7(2) . 2_656 ?
C37B Ge3 C1 115.5(6) . 2_656 ?
C12 Ge3 C37A 110.9(5) . . ?
C1 Ge3 C37A 104.3(5) 2_656 . ?
C12 Ge3 C43 109.6(2) . . ?
C37B Ge3 C43 113.7(7) . . ?
C1 Ge3 C43 108.3(2) 2_656 . ?
C37A Ge3 C43 116.4(5) . . ?
C2 C1 Ge3 178.9(5) . 2_656 ?
C1 C2 C3 179.7(7) . . ?
C4 C3 C2 178.9(6) . . ?
C3 C4 Ge1 178.6(5) . . ?
C6 C5 Ge1 176.8(5) . . ?
C5 C6 C7 178.3(6) . . ?
C8 C7 C6 178.9(6) . . ?
C7 C8 Ge2 178.5(5) . . ?
C10 C9 Ge2 176.6(4) . . ?
C9 C10 C11 179.0(5) . . ?
C12 C11 C10 178.7(6) . . ?
C11 C12 Ge3 178.1(5) . . ?
C14 C13 C18 116.7(6) . . ?
C14 C13 Ge1 121.0(5) . . ?
C18 C13 Ge1 121.9(4) . . ?
C13 C14 C15 117.6(9) . . ?
C16 C15 C14 119.8(9) . . ?
C17 C16 C15 121.0(8) . . ?
C16 C17 C18 119.3(7) . . ?
C17 C18 C13 124.9(6) . . ?
C24 C19 C20 118.6(5) . . ?
C24 C19 Ge1 120.6(4) . . ?
C20 C19 Ge1 120.8(4) . . ?
C19 C20 C21 120.5(6) . . ?
C22 C21 C20 120.9(7) . . ?
C21 C22 C23 119.3(6) . . ?
C22 C23 C24 120.9(6) . . ?
C19 C24 C23 119.9(6) . . ?
C26 C25 C30 119.1(4) . . ?
C26 C25 Ge2 120.9(3) . . ?
C30 C25 Ge2 119.9(4) . . ?
C25 C26 C27 120.2(5) . . ?
C28 C27 C26 120.5(5) . . ?
C27 C28 C29 121.3(5) . . ?
C28 C29 C30 118.3(5) . . ?
C25 C30 C29 120.5(5) . . ?
C36 C31 C32 118.5(4) . . ?
C36 C31 Ge2 120.3(4) . . ?
C32 C31 Ge2 121.2(4) . . ?
C33 C32 C31 120.4(5) . . ?
C34 C33 C32 120.6(6) . . ?
C35 C34 C33 119.4(5) . . ?
C34 C35 C36 121.0(5) . . ?
C31 C36 C35 120.1(5) . . ?
C42A C37A C38A 119.3(18) . . ?
C42A C37A Ge3 117.4(13) . . ?
C38A C37A Ge3 123.3(13) . . ?
C37A C38A C39A 121.7(14) . . ?
C40A C39A C38A 117.3(13) . . ?
C40A C41A C42A 115.8(17) . . ?
C37A C42A C41A 122.1(15) . . ?
C41A C40A C39A 123.7(18) . . ?
C40B C41B C42B 128(2) . . ?
C37B C42B C41B 118(2) . . ?
C37B C38B C39B 122.8(18) . . ?
C40B C39B C38B 125(2) . . ?
C38B C37B C42B 116(2) . . ?
C38B C37B Ge3 120.0(14) . . ?
C42B C37B Ge3 123.7(16) . . ?
C39B C40B C41B 110(3) . . ?
C44 C43 C48 117.7(5) . . ?
C44 C43 Ge3 120.4(4) . . ?
C48 C43 Ge3 121.7(4) . . ?
C43 C44 C45 120.9(6) . . ?
C46 C45 C44 120.3(7) . . ?
C47 C46 C45 118.6(6) . . ?
C46 C47 C48 121.0(6) . . ?
C43 C48 C47 121.3(6) . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



# SQUEEZE RESULTS (Version =  70515)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.025 0.000 0.500 525 113 ' '
2 0.500 0.500 1.000 169 39 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        'extended dodecaphenyl germa[6]pericyclyne'
_chemical_name_common            Ext_PhGe[6]
####################################################################### 
# 
# 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_Extend_of_Ph-Ge8pericyclyne_2
_database_code_depnum_ccdc_archive 'CCDC 1517000'
_audit_update_record             
;
2016-11-12 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C130 H82 Cl2 Ge8'
_chemical_formula_moiety         'C128 H78 Ge8, C2 H4 Cl2'
_chemical_formula_weight         2295.70
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   8.5865(5)
_cell_length_b                   17.1492(10)
_cell_length_c                   23.1679(13)
_cell_angle_alpha                108.405(8)
_cell_angle_beta                 91.775(7)
_cell_angle_gamma                98.171(7)
_cell_volume                     3193.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    24449
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.40
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152.00
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_T_max  0.962

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            44255
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_full        25.242
_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_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             11684
_reflns_number_gt                7298
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0733
_refine_ls_wR_factor_ref         0.1744
_refine_ls_wR_factor_gt          0.1555
_refine_ls_number_restraints     12
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         11684
_refine_ls_number_parameters     668
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0643P)²+6.8043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Ge Ge 0.1547 1.8001
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 1.22656(8) 1.04422(5) 0.20626(3) 0.0485(2) Uani 1 1 d . . . . .
Ge2 Ge 0.66482(10) 0.65180(5) 0.02917(3) 0.0557(2) Uani 1 1 d . . . . .
Ge3 Ge 0.65187(9) 0.44736(4) 0.27503(3) 0.0500(2) Uani 1 1 d . . . . .
Ge4 Ge 1.19156(8) 0.80384(4) 0.50738(3) 0.0416(2) Uani 1 1 d . . . . .
Cl1 Cl 0.7085(3) 0.0419(2) 0.05944(11) 0.1303(14) Uani 1 1 d . . . . .
C1 C 1.0839(9) 0.9453(5) 0.1642(3) 0.060(2) Uani 1 1 d . . . . .
C2 C 0.9990(9) 0.8838(5) 0.1343(3) 0.063(2) Uani 1 1 d . . . . .
C3 C 0.8968(10) 0.8136(5) 0.1006(3) 0.065(2) Uani 1 1 d . . . . .
C4 C 0.8091(9) 0.7508(5) 0.0713(3) 0.061(2) Uani 1 1 d . . . . .
C5 C 0.6535(9) 0.5960(5) 0.0874(3) 0.063(2) Uani 1 1 d . . . . .
C6 C 0.6531(10) 0.5630(5) 0.1267(4) 0.062(2) Uani 1 1 d . . . . .
C7 C 0.6538(9) 0.5246(4) 0.1707(3) 0.058(2) Uani 1 1 d . . . . .
C8 C 0.6541(10) 0.4906(4) 0.2100(4) 0.061(2) Uani 1 1 d . . . . .
C9 C 0.7871(9) 0.5323(4) 0.3367(3) 0.0532(19) Uani 1 1 d . . . . .
C10 C 0.8734(8) 0.5900(4) 0.3718(3) 0.0449(16) Uani 1 1 d . . . . .
C11 C 0.9738(8) 0.6559(4) 0.4130(3) 0.0496(18) Uani 1 1 d . . . . .
C12 C 1.0584(8) 0.7128(4) 0.4495(3) 0.0453(16) Uani 1 1 d . . . . .
C13 C 1.0895(8) 0.8290(4) 0.5814(3) 0.0441(16) Uani 1 1 d . . . . .
C14 C 1.0241(8) 0.8503(4) 0.6273(3) 0.0434(16) Uani 1 1 d . . . . .
C15 C 0.9449(8) 0.8772(4) 0.6791(3) 0.0458(17) Uani 1 1 d . . . . .
C16 C 0.8778(8) 0.9029(4) 0.7244(3) 0.0468(17) Uani 1 1 d . . . . .
C17 C 1.2522(9) 1.1037(5) 0.1483(3) 0.0548(19) Uani 1 1 d . . . . .
C18 C 1.1358(8) 1.0895(5) 0.1010(3) 0.056(2) Uani 1 1 d . . . . .
H18 H 1.0400 1.0535 0.0997 0.068 Uiso 1 1 calc R U . . .
C19 C 1.1555(9) 1.1259(5) 0.0568(3) 0.059(2) Uani 1 1 d . . . . .
H19 H 1.0740 1.1154 0.0254 0.071 Uiso 1 1 calc R U . . .
C20 C 1.2945(9) 1.1780(5) 0.0577(4) 0.061(2) Uani 1 1 d . . . . .
H20 H 1.3096 1.2028 0.0265 0.073 Uiso 1 1 calc R U . . .
C21 C 1.4120(10) 1.1940(5) 0.1044(4) 0.062(2) Uani 1 1 d . . . . .
H21 H 1.5069 1.2307 0.1054 0.075 Uiso 1 1 calc R U . . .
C22 C 1.3922(8) 1.1574(4) 0.1492(3) 0.0494(18) Uani 1 1 d . . . . .
H22 H 1.4736 1.1685 0.1808 0.059 Uiso 1 1 calc R U . . .
C23 C 1.4210(8) 1.0169(4) 0.2343(4) 0.061(2) Uani 1 1 d . . . . .
C24 C 1.5289(11) 0.9889(6) 0.1918(5) 0.085(3) Uani 1 1 d . . . . .
H24 H 1.5097 0.9852 0.1503 0.102 Uiso 1 1 calc R U . . .
C25 C 1.6622(13) 0.9672(8) 0.2112(9) 0.125(5) Uani 1 1 d . . . . .
H25 H 1.7363 0.9472 0.1827 0.150 Uiso 1 1 calc R U . . .
C26 C 1.6917(12) 0.9736(6) 0.2714(8) 0.112(5) Uani 1 1 d . . . . .
H26 H 1.7849 0.9574 0.2839 0.135 Uiso 1 1 calc R U . . .
C27 C 1.5898(13) 1.0026(6) 0.3122(5) 0.107(4) Uani 1 1 d . . . . .
H27 H 1.6129 1.0090 0.3540 0.129 Uiso 1 1 calc R U . . .
C28 C 1.4503(11) 1.0232(5) 0.2938(4) 0.084(3) Uani 1 1 d . . . . .
H28 H 1.3759 1.0416 0.3225 0.100 Uiso 1 1 calc R U . . .
C29 C 0.4663(9) 0.6872(4) 0.0170(3) 0.0521(18) Uani 1 1 d . . . . .
C30 C 0.4307(12) 0.7579(7) 0.0573(6) 0.151(6) Uani 1 1 d . . . . .
H30 H 0.5031 0.7907 0.0909 0.181 Uiso 1 1 calc R U . . .
C31 C 0.2883(16) 0.7803(8) 0.0483(9) 0.193(9) Uani 1 1 d . . . . .
H31 H 0.2630 0.8295 0.0767 0.231 Uiso 1 1 calc R U . . .
C32 C 0.1813(13) 0.7367(8) 0.0015(6) 0.096(3) Uani 1 1 d . . . . .
H32 H 0.0842 0.7551 -0.0038 0.116 Uiso 1 1 calc R U . . .
C33 C 0.2166(11) 0.6667(8) -0.0374(4) 0.098(4) Uani 1 1 d . . . . .
H33 H 0.1423 0.6333 -0.0701 0.118 Uiso 1 1 calc R U . . .
C34 C 0.3602(11) 0.6426(6) -0.0302(4) 0.082(3) Uani 1 1 d . . . . .
H34 H 0.3852 0.5936 -0.0590 0.098 Uiso 1 1 calc R U . . .
C35 C 0.7473(9) 0.5832(5) -0.0431(3) 0.057(2) Uani 1 1 d . . . . .
C36 C 0.7417(10) 0.6005(5) -0.0982(3) 0.064(2) Uani 1 1 d . . . . .
H36 H 0.6952 0.6465 -0.1007 0.077 Uiso 1 1 calc R U . . .
C37 C 0.8022(11) 0.5520(6) -0.1484(4) 0.077(3) Uani 1 1 d . . . . .
H37 H 0.7997 0.5653 -0.1852 0.093 Uiso 1 1 calc R U . . .
C38 C 0.8669(12) 0.4839(7) -0.1461(4) 0.095(3) Uani 1 1 d . . . . .
H38 H 0.9076 0.4498 -0.1812 0.114 Uiso 1 1 calc R U . . .
C39 C 0.8720(16) 0.4659(9) -0.0928(6) 0.135(5) Uani 1 1 d . . . . .
H39 H 0.9154 0.4188 -0.0908 0.162 Uiso 1 1 calc R U . . .
C40 C 0.8147(14) 0.5157(8) -0.0425(5) 0.113(4) Uani 1 1 d . . . . .
H40 H 0.8219 0.5032 -0.0055 0.135 Uiso 1 1 calc R U . . .
C41 C 0.4411(9) 0.4370(5) 0.3010(3) 0.061(2) Uani 1 1 d . . . . .
C42 C 0.3411(10) 0.3634(5) 0.2835(4) 0.065(2) Uani 1 1 d . . . . .
H42 H 0.3764 0.3148 0.2582 0.078 Uiso 1 1 calc R U . . .
C43 C 0.1887(10) 0.3574(6) 0.3016(4) 0.074(2) Uani 1 1 d . . . . .
H43 H 0.1229 0.3047 0.2911 0.089 Uiso 1 1 calc R U . . .
C44 C 0.1361(12) 0.4248(8) 0.3334(6) 0.121(4) Uani 1 1 d . . . . .
H44 H 0.0301 0.4211 0.3442 0.145 Uiso 1 1 calc R U . . .
C45 C 0.2311(15) 0.4996(9) 0.3511(8) 0.199(9) Uani 1 1 d . . . . .
H45 H 0.1915 0.5477 0.3747 0.239 Uiso 1 1 calc R U . . .
C46 C 0.3859(13) 0.5071(7) 0.3351(7) 0.162(7) Uani 1 1 d . . . . .
H46 H 0.4521 0.5598 0.3476 0.195 Uiso 1 1 calc R U . . .
C47 C 0.7331(8) 0.3435(4) 0.2491(3) 0.0421(16) Uani 1 1 d . . . . .
C48 C 0.8064(9) 0.3198(5) 0.1961(3) 0.060(2) Uani 1 1 d . . . . .
H48 H 0.8219 0.3564 0.1726 0.073 Uiso 1 1 calc R U . . .
C49 C 0.8577(10) 0.2444(5) 0.1761(4) 0.068(2) Uani 1 1 d . . . . .
H49 H 0.9075 0.2292 0.1391 0.082 Uiso 1 1 calc R U . . .
C50 C 0.8375(9) 0.1909(5) 0.2094(3) 0.058(2) Uani 1 1 d . . . . .
H50 H 0.8750 0.1391 0.1958 0.070 Uiso 1 1 calc R U . . .
C51 C 0.7629(8) 0.2123(4) 0.2624(3) 0.0461(17) Uani 1 1 d . . . . .
H51 H 0.7456 0.1747 0.2850 0.055 Uiso 1 1 calc R U . . .
C52 C 0.7128(8) 0.2897(4) 0.2829(3) 0.0474(17) Uani 1 1 d . . . . .
H52 H 0.6644 0.3055 0.3202 0.057 Uiso 1 1 calc R U . . .
C53 C 1.3922(8) 0.7715(4) 0.5215(3) 0.0449(16) Uani 1 1 d . . . . .
C54 C 1.4808(10) 0.7437(5) 0.4719(4) 0.073(2) Uani 1 1 d . . . . .
H54 H 1.4421 0.7416 0.4324 0.088 Uiso 1 1 calc R U . . .
C55 C 1.6228(11) 0.7195(6) 0.4793(5) 0.085(3) Uani 1 1 d . . . . .
H55 H 1.6824 0.7012 0.4451 0.102 Uiso 1 1 calc R U . . .
C56 C 1.6797(10) 0.7215(5) 0.5354(5) 0.081(3) Uani 1 1 d . . . . .
H56 H 1.7763 0.7025 0.5403 0.097 Uiso 1 1 calc R U . . .
C57 C 1.5939(10) 0.7519(5) 0.5857(4) 0.073(2) Uani 1 1 d . . . . .
H57 H 1.6346 0.7560 0.6253 0.087 Uiso 1 1 calc R U . . .
C58 C 1.4492(8) 0.7760(4) 0.5779(3) 0.0516(18) Uani 1 1 d . . . . .
H58 H 1.3902 0.7958 0.6121 0.062 Uiso 1 1 calc R U . . .
C59 C 1.2055(8) 0.8985(4) 0.4786(3) 0.0454(16) Uani 1 1 d D . . . .
C60A C 1.0833(19) 0.9052(9) 0.4394(6) 0.060(5) Uani 0.507(10) 1 d D . P A 1
H60A H 0.9987 0.8601 0.4238 0.072 Uiso 0.507(10) 1 calc R U P A 1
C61A C 1.0843(18) 0.9771(9) 0.4231(8) 0.072(5) Uani 0.507(10) 1 d D . P A 1
H61A H 0.9954 0.9850 0.4013 0.087 Uiso 0.507(10) 1 calc R U P A 1
C63A C 1.335(2) 1.0356(10) 0.4827(8) 0.076(5) Uani 0.507(10) 1 d D . P A 1
H63A H 1.4134 1.0825 0.5022 0.091 Uiso 0.507(10) 1 calc R U P A 1
C64A C 1.3300(17) 0.9628(8) 0.4963(7) 0.060(5) Uani 0.507(10) 1 d D . P A 1
H64A H 1.4182 0.9567 0.5194 0.072 Uiso 0.507(10) 1 calc R U P A 1
C60B C 1.232(2) 0.8887(11) 0.4187(6) 0.076(6) Uani 0.493(10) 1 d D . P A 2
H60B H 1.2479 0.8366 0.3912 0.091 Uiso 0.493(10) 1 calc R U P A 2
C61B C 1.234(3) 0.9583(10) 0.4000(8) 0.095(7) Uani 0.493(10) 1 d D . P A 2
H61B H 1.2431 0.9517 0.3580 0.114 Uiso 0.493(10) 1 calc R U P A 2
C63B C 1.214(2) 1.0481(10) 0.5006(8) 0.080(6) Uani 0.493(10) 1 d D . P A 2
H63B H 1.2173 1.1019 0.5297 0.095 Uiso 0.493(10) 1 calc R U P A 2
C64B C 1.1987(19) 0.9775(8) 0.5185(6) 0.054(4) Uani 0.493(10) 1 d D . P A 2
H64B H 1.1830 0.9835 0.5600 0.065 Uiso 0.493(10) 1 calc R U P A 2
C62 C 1.2227(11) 1.0381(6) 0.4401(4) 0.076(2) Uani 1 1 d D . . . .
C65 C 0.5749(9) 0.0233(5) -0.0041(4) 0.070(2) Uani 1 1 d . . . . .
H65A H 0.5571 0.0768 -0.0087 0.084 Uiso 1 1 calc R U . . .
H65B H 0.6191 -0.0091 -0.0415 0.084 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C16 1.900(7) 2_776 ?
Ge1 C1 1.903(8) . ?
Ge1 C17 1.926(8) . ?
Ge1 C23 1.943(8) . ?
Ge2 C5 1.882(9) . ?
Ge2 C4 1.911(8) . ?
Ge2 C29 1.930(8) . ?
Ge2 C35 1.937(8) . ?
Ge3 C8 1.878(9) . ?
Ge3 C9 1.901(7) . ?
Ge3 C41 1.927(8) . ?
Ge3 C47 1.930(6) . ?
Ge4 C12 1.903(7) . ?
Ge4 C13 1.905(7) . ?
Ge4 C59 1.930(7) . ?
Ge4 C53 1.932(7) . ?
Cl1 C65 1.754(8) . ?
C1 C2 1.188(10) . ?
C2 C3 1.375(10) . ?
C3 C4 1.210(10) . ?
C5 C6 1.215(10) . ?
C6 C7 1.376(11) . ?
C7 C8 1.226(10) . ?
C9 C10 1.198(9) . ?
C10 C11 1.386(9) . ?
C11 C12 1.198(9) . ?
C13 C14 1.196(8) . ?
C14 C15 1.380(9) . ?
C15 C16 1.201(9) . ?
C16 Ge1 1.900(7) 2_776 ?
C17 C18 1.397(10) . ?
C17 C22 1.402(10) . ?
C18 C19 1.360(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.390(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.376(10) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.359(11) . ?
C23 C24 1.395(11) . ?
C24 C25 1.359(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.377(17) . ?
C25 H25 0.9500 . ?
C26 C27 1.336(16) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(12) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.350(10) . ?
C29 C30 1.358(11) . ?
C30 C31 1.363(18) . ?
C30 H30 0.9500 . ?
C31 C32 1.346(18) . ?
C31 H31 0.9500 . ?
C32 C33 1.334(14) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(12) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.369(12) . ?
C35 C36 1.400(10) . ?
C36 C37 1.365(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.378(12) . ?
C37 H37 0.9500 . ?
C38 C39 1.364(13) . ?
C38 H38 0.9500 . ?
C39 C40 1.363(13) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C42 1.357(10) . ?
C41 C46 1.371(12) . ?
C42 C43 1.387(11) . ?
C42 H42 0.9500 . ?
C43 C44 1.309(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.352(16) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(15) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.370(9) . ?
C47 C52 1.383(9) . ?
C48 C49 1.370(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.370(10) . ?
C49 H49 0.9500 . ?
C50 C51 1.372(10) . ?
C50 H50 0.9500 . ?
C51 C52 1.396(9) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C58 1.357(9) . ?
C53 C54 1.392(10) . ?
C54 C55 1.366(11) . ?
C54 H54 0.9500 . ?
C55 C56 1.363(13) . ?
C55 H55 0.9500 . ?
C56 C57 1.396(12) . ?
C56 H56 0.9500 . ?
C57 C58 1.388(10) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C64A 1.371(13) . ?
C59 C60B 1.375(13) . ?
C59 C64B 1.389(13) . ?
C59 C60A 1.407(13) . ?
C60A C61A 1.400(15) . ?
C60A H60A 0.9500 . ?
C61A C62 1.421(13) . ?
C61A H61A 0.9500 . ?
C63A C62 1.374(15) . ?
C63A C64A 1.377(14) . ?
C63A H63A 0.9500 . ?
C64A H64A 0.9500 . ?
C60B C61B 1.391(15) . ?
C60B H60B 0.9500 . ?
C61B C62 1.410(15) . ?
C61B H61B 0.9500 . ?
C63B C62 1.364(15) . ?
C63B C64B 1.391(15) . ?
C63B H63B 0.9500 . ?
C64B H64B 0.9500 . ?
C65 C65 1.465(15) 2_655 ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?

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
C16 Ge1 C1 104.3(3) 2_776 . ?
C16 Ge1 C17 114.4(3) 2_776 . ?
C1 Ge1 C17 104.4(3) . . ?
C16 Ge1 C23 108.4(3) 2_776 . ?
C1 Ge1 C23 110.3(3) . . ?
C17 Ge1 C23 114.5(3) . . ?
C5 Ge2 C4 101.5(3) . . ?
C5 Ge2 C29 110.9(3) . . ?
C4 Ge2 C29 106.1(3) . . ?
C5 Ge2 C35 108.6(3) . . ?
C4 Ge2 C35 112.4(3) . . ?
C29 Ge2 C35 116.3(3) . . ?
C8 Ge3 C9 102.4(3) . . ?
C8 Ge3 C41 109.2(3) . . ?
C9 Ge3 C41 109.7(3) . . ?
C8 Ge3 C47 108.4(3) . . ?
C9 Ge3 C47 112.8(3) . . ?
C41 Ge3 C47 113.6(3) . . ?
C12 Ge4 C13 106.8(3) . . ?
C12 Ge4 C59 108.2(3) . . ?
C13 Ge4 C59 108.5(3) . . ?
C12 Ge4 C53 109.7(3) . . ?
C13 Ge4 C53 108.9(3) . . ?
C59 Ge4 C53 114.5(3) . . ?
C2 C1 Ge1 175.5(7) . . ?
C1 C2 C3 178.2(9) . . ?
C4 C3 C2 178.6(10) . . ?
C3 C4 Ge2 176.7(7) . . ?
C6 C5 Ge2 176.5(7) . . ?
C5 C6 C7 179.1(9) . . ?
C8 C7 C6 179.7(9) . . ?
C7 C8 Ge3 175.0(6) . . ?
C10 C9 Ge3 173.9(7) . . ?
C9 C10 C11 179.1(8) . . ?
C12 C11 C10 178.6(8) . . ?
C11 C12 Ge4 179.5(7) . . ?
C14 C13 Ge4 175.2(6) . . ?
C13 C14 C15 177.2(7) . . ?
C16 C15 C14 178.1(8) . . ?
C15 C16 Ge1 173.1(7) . 2_776 ?
C18 C17 C22 117.8(7) . . ?
C18 C17 Ge1 120.6(6) . . ?
C22 C17 Ge1 121.4(5) . . ?
C19 C18 C17 122.0(7) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C18 C19 C20 119.9(7) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C21 119.6(8) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 120.6(7) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C17 120.2(7) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C28 C23 C24 120.5(8) . . ?
C28 C23 Ge1 121.0(6) . . ?
C24 C23 Ge1 118.4(7) . . ?
C25 C24 C23 118.3(11) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
C24 C25 C26 121.1(12) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C27 C26 C25 120.3(11) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.1(11) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C23 C28 C27 119.6(10) . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C34 C29 C30 119.0(9) . . ?
C34 C29 Ge2 121.6(6) . . ?
C30 C29 Ge2 119.4(7) . . ?
C29 C30 C31 118.1(11) . . ?
C29 C30 H30 121.0 . . ?
C31 C30 H30 121.0 . . ?
C32 C31 C30 123.7(12) . . ?
C32 C31 H31 118.1 . . ?
C30 C31 H31 118.1 . . ?
C33 C32 C31 117.6(10) . . ?
C33 C32 H32 121.2 . . ?
C31 C32 H32 121.2 . . ?
C32 C33 C34 120.4(10) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C29 C34 C33 121.2(9) . . ?
C29 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C40 C35 C36 116.8(8) . . ?
C40 C35 Ge2 121.5(6) . . ?
C36 C35 Ge2 121.7(6) . . ?
C37 C36 C35 120.9(8) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C36 C37 C38 120.4(9) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C39 C38 C37 119.4(9) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C40 C39 C38 119.8(10) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C39 C40 C35 122.7(9) . . ?
C39 C40 H40 118.7 . . ?
C35 C40 H40 118.7 . . ?
C42 C41 C46 118.4(8) . . ?
C42 C41 Ge3 122.3(6) . . ?
C46 C41 Ge3 119.1(7) . . ?
C41 C42 C43 121.5(8) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C44 C43 C42 119.6(9) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 120.6(10) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C44 C45 C46 121.0(10) . . ?
C44 C45 H45 119.5 . . ?
C46 C45 H45 119.5 . . ?
C41 C46 C45 118.7(10) . . ?
C41 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
C48 C47 C52 118.5(6) . . ?
C48 C47 Ge3 121.2(5) . . ?
C52 C47 Ge3 120.3(5) . . ?
C49 C48 C47 121.3(7) . . ?
C49 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C48 C49 C50 120.3(7) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 119.9(7) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C50 C51 C52 119.5(7) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
C47 C52 C51 120.5(7) . . ?
C47 C52 H52 119.8 . . ?
C51 C52 H52 119.8 . . ?
C58 C53 C54 119.6(7) . . ?
C58 C53 Ge4 122.1(5) . . ?
C54 C53 Ge4 118.3(6) . . ?
C55 C54 C53 120.6(8) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C56 C55 C54 120.6(9) . . ?
C56 C55 H55 119.7 . . ?
C54 C55 H55 119.7 . . ?
C55 C56 C57 119.1(8) . . ?
C55 C56 H56 120.5 . . ?
C57 C56 H56 120.5 . . ?
C58 C57 C56 120.2(8) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C53 C58 C57 119.9(7) . . ?
C53 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C60B C59 C64B 119.3(11) . . ?
C64A C59 C60A 117.0(10) . . ?
C64A C59 Ge4 122.5(7) . . ?
C60B C59 Ge4 119.8(8) . . ?
C64B C59 Ge4 120.8(7) . . ?
C60A C59 Ge4 120.5(7) . . ?
C61A C60A C59 121.0(13) . . ?
C61A C60A H60A 119.5 . . ?
C59 C60A H60A 119.5 . . ?
C60A C61A C62 117.8(13) . . ?
C60A C61A H61A 121.1 . . ?
C62 C61A H61A 121.1 . . ?
C62 C63A C64A 117.8(14) . . ?
C62 C63A H63A 121.1 . . ?
C64A C63A H63A 121.1 . . ?
C59 C64A C63A 124.0(13) . . ?
C59 C64A H64A 118.0 . . ?
C63A C64A H64A 118.0 . . ?
C59 C60B C61B 117.1(15) . . ?
C59 C60B H60B 121.4 . . ?
C61B C60B H60B 121.4 . . ?
C60B C61B C62 123.4(14) . . ?
C60B C61B H61B 118.3 . . ?
C62 C61B H61B 118.3 . . ?
C62 C63B C64B 118.1(15) . . ?
C62 C63B H63B 120.9 . . ?
C64B C63B H63B 120.9 . . ?
C59 C64B C63B 123.1(13) . . ?
C59 C64B H64B 118.5 . . ?
C63B C64B H64B 118.5 . . ?
C63B C62 C61B 118.3(12) . . ?
C63A C62 C61A 120.3(12) . . ?
C65 C65 Cl1 109.6(8) 2_655 . ?
C65 C65 H65A 109.8 2_655 . ?
Cl1 C65 H65A 109.8 . . ?
C65 C65 H65B 109.8 2_655 . ?
Cl1 C65 H65B 109.8 . . ?
H65A C65 H65B 108.2 . . ?

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
C22 C17 C18 C19 0.2(10) . . . . ?
Ge1 C17 C18 C19 -175.0(5) . . . . ?
C17 C18 C19 C20 0.5(11) . . . . ?
C18 C19 C20 C21 -1.1(12) . . . . ?
C19 C20 C21 C22 1.1(12) . . . . ?
C20 C21 C22 C17 -0.4(11) . . . . ?
C18 C17 C22 C21 -0.2(10) . . . . ?
Ge1 C17 C22 C21 175.0(5) . . . . ?
C28 C23 C24 C25 0.9(14) . . . . ?
Ge1 C23 C24 C25 -177.8(8) . . . . ?
C23 C24 C25 C26 -0.9(17) . . . . ?
C24 C25 C26 C27 -0.8(19) . . . . ?
C25 C26 C27 C28 2.6(18) . . . . ?
C24 C23 C28 C27 0.8(14) . . . . ?
Ge1 C23 C28 C27 179.5(7) . . . . ?
C26 C27 C28 C23 -2.6(16) . . . . ?
C34 C29 C30 C31 0.2(19) . . . . ?
Ge2 C29 C30 C31 -178.5(12) . . . . ?
C29 C30 C31 C32 0(3) . . . . ?
C30 C31 C32 C33 1(2) . . . . ?
C31 C32 C33 C34 -2.3(18) . . . . ?
C30 C29 C34 C33 -1.1(15) . . . . ?
Ge2 C29 C34 C33 177.6(8) . . . . ?
C32 C33 C34 C29 2.2(16) . . . . ?
C40 C35 C36 C37 -0.5(13) . . . . ?
Ge2 C35 C36 C37 179.2(6) . . . . ?
C35 C36 C37 C38 1.5(14) . . . . ?
C36 C37 C38 C39 -0.9(17) . . . . ?
C37 C38 C39 C40 -1(2) . . . . ?
C38 C39 C40 C35 2(2) . . . . ?
C36 C35 C40 C39 -1.1(17) . . . . ?
Ge2 C35 C40 C39 179.2(10) . . . . ?
C46 C41 C42 C43 -3.0(14) . . . . ?
Ge3 C41 C42 C43 -178.7(6) . . . . ?
C41 C42 C43 C44 4.0(15) . . . . ?
C42 C43 C44 C45 -3(2) . . . . ?
C43 C44 C45 C46 1(3) . . . . ?
C42 C41 C46 C45 1(2) . . . . ?
Ge3 C41 C46 C45 176.9(13) . . . . ?
C44 C45 C46 C41 0(3) . . . . ?
C52 C47 C48 C49 0.6(11) . . . . ?
Ge3 C47 C48 C49 -177.0(6) . . . . ?
C47 C48 C49 C50 -0.4(13) . . . . ?
C48 C49 C50 C51 1.2(13) . . . . ?
C49 C50 C51 C52 -2.0(11) . . . . ?
C48 C47 C52 C51 -1.4(10) . . . . ?
Ge3 C47 C52 C51 176.1(5) . . . . ?
C50 C51 C52 C47 2.2(10) . . . . ?
C58 C53 C54 C55 1.3(12) . . . . ?
Ge4 C53 C54 C55 -179.5(7) . . . . ?
C53 C54 C55 C56 0.5(14) . . . . ?
C54 C55 C56 C57 -2.6(14) . . . . ?
C55 C56 C57 C58 2.9(13) . . . . ?
C54 C53 C58 C57 -1.0(11) . . . . ?
Ge4 C53 C58 C57 179.8(5) . . . . ?
C56 C57 C58 C53 -1.1(11) . . . . ?
C64A C59 C60A C61A -4(2) . . . . ?
Ge4 C59 C60A C61A 173.6(12) . . . . ?
C59 C60A C61A C62 9(2) . . . . ?
C60A C59 C64A C63A 6(2) . . . . ?
Ge4 C59 C64A C63A -171.8(14) . . . . ?
C62 C63A C64A C59 -12(3) . . . . ?
C64B C59 C60B C61B -7(2) . . . . ?
Ge4 C59 C60B C61B 177.3(14) . . . . ?
C59 C60B C61B C62 5(3) . . . . ?
C60B C59 C64B C63B 2(2) . . . . ?
Ge4 C59 C64B C63B 177.7(12) . . . . ?
C62 C63B C64B C59 5(2) . . . . ?
C64B C63B C62 C61B -7(2) . . . . ?
C64A C63A C62 C61A 16(3) . . . . ?
C60B C61B C62 C63B 2(3) . . . . ?
C60A C61A C62 C63A -15(2) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



# SQUEEZE RESULTS (Version =  70515)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.004 0.250 0.737 238 81 ' '
2 -0.012 0.500 0.500 191 74 ' '
3 0.014 0.750 0.263 238 81 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        'extended hexadecaphenyl germa[8]pericyclyne'
_chemical_name_common            'Ext_PhGe[8] with CH2Cl2'
####################################################################### 
# 
# 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_Extended-Diphenyl-Ge5
_database_code_depnum_ccdc_archive 'CCDC 1516998'
_audit_update_record             
;
2016-11-12 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C86 H40 Ge5'
_chemical_formula_moiety         'C80 H40 Ge5, C6'
_chemical_formula_weight         1436.21
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   30.1774(6)
_cell_length_b                   27.4706(5)
_cell_length_c                   8.96993(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     7436.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    73340
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      25.36
_cell_measurement_temperature    123
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2864.00
_exptl_absorpt_coefficient_mu    2.038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.903

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            100653
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         3.030
_diffrn_reflns_theta_full        25.242
_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_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6951
_reflns_number_gt                5771
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1074
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         6951
_refine_ls_number_parameters     504
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0453P)²+20.4757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.15
_refine_diff_density_min         -1.14
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Ge Ge 0.1547 1.8001
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.79643(2) 0.7500 0.42905(5) 0.02518(13) Uani 1 2 d S T P A .
Ge2 Ge 0.65258(2) 0.57074(2) 0.84688(4) 0.03111(12) Uani 1 1 d . . . . .
Ge3 Ge 0.44164(2) 0.61167(2) 0.41292(5) 0.05855(18) Uani 1 1 d . . . . .
C1 C 0.76467(12) 0.69718(13) 0.5184(4) 0.0299(8) Uani 1 1 d . . . . .
C2 C 0.74083(12) 0.67097(12) 0.5884(4) 0.0282(7) Uani 1 1 d . . . . .
C3 C 0.71360(12) 0.64103(13) 0.6700(4) 0.0300(8) Uani 1 1 d . . . . .
C4 C 0.68930(12) 0.61544(14) 0.7416(4) 0.0351(8) Uani 1 1 d . . . . .
C5 C 0.59823(12) 0.57047(14) 0.7391(4) 0.0352(8) Uani 1 1 d . . . . .
C6 C 0.56423(12) 0.57519(15) 0.6704(4) 0.0356(9) Uani 1 1 d . . . . .
C7 C 0.52610(13) 0.58300(17) 0.5898(4) 0.0428(10) Uani 1 1 d . . . . .
C8 C 0.49314(14) 0.5914(2) 0.5194(4) 0.0547(13) Uani 1 1 d . . . . .
C9 C 0.44225(16) 0.6809(3) 0.4208(6) 0.0645(15) Uani 1 1 d . . . . .
C10 C 0.44256(15) 0.7241(3) 0.4215(5) 0.0673(17) Uani 1 1 d . . . . .
C11 C 0.78667(17) 0.7500 0.2165(5) 0.0319(11) Uani 1 2 d S T P . .
C12 C 0.8205(3) 0.7500 0.1170(8) 0.093(3) Uani 1 2 d S T P . .
H12 H 0.8502 0.7500 0.1516 0.112 Uiso 1 2 calc R U P . .
C13 C 0.8119(4) 0.7500 -0.0355(9) 0.116(4) Uani 1 2 d S T P . .
H13 H 0.8359 0.7500 -0.1041 0.139 Uiso 1 2 calc R U P . .
C14 C 0.7701(4) 0.7500 -0.0870(8) 0.074(2) Uani 1 2 d S T P . .
H14 H 0.7644 0.7500 -0.1911 0.089 Uiso 1 2 calc R U P . .
C15 C 0.7370(3) 0.7500 0.0097(9) 0.114(4) Uani 1 2 d S T P . .
H15 H 0.7074 0.7500 -0.0258 0.136 Uiso 1 2 calc R U P . .
C16 C 0.7450(3) 0.7500 0.1629(8) 0.095(3) Uani 1 2 d S T P . .
H16 H 0.7207 0.7500 0.2302 0.114 Uiso 1 2 calc R U P . .
C17 C 0.85644(17) 0.7500 0.4996(6) 0.0381(13) Uani 1 2 d S T P . .
C18 C 0.8698(3) 0.7844(4) 0.6054(11) 0.053(2) Uani 0.5 1 d . . P A -1
H18 H 0.8497 0.8089 0.6371 0.064 Uiso 0.5 1 calc R U P A -1
C19 C 0.9120(3) 0.7831(4) 0.6640(11) 0.063(3) Uani 0.5 1 d . . P A -1
H19 H 0.9205 0.8059 0.7383 0.075 Uiso 0.5 1 calc R U P A -1
C21 C 0.9290(5) 0.7183(7) 0.510(2) 0.159(9) Uani 0.5 1 d . . P A -1
H21 H 0.9500 0.6954 0.4739 0.190 Uiso 0.5 1 calc R U P A -1
C22 C 0.8865(4) 0.7189(6) 0.4513(19) 0.126(7) Uani 0.5 1 d . . P A -1
H22 H 0.8789 0.6965 0.3749 0.151 Uiso 0.5 1 calc R U P A -1
C20 C 0.9408(3) 0.7500 0.6168(12) 0.091(3) Uani 1 2 d S T P . .
H20 H 0.963(3) 0.7500 0.657(10) 0.09(3) Uiso 1 2 d S . P . .
C23 C 0.68256(12) 0.50899(15) 0.8372(4) 0.0358(9) Uani 1 1 d . . . . .
C24 C 0.70659(18) 0.49552(17) 0.7158(6) 0.0624(14) Uani 1 1 d . . . . .
H24 H 0.7084 0.5170 0.6331 0.075 Uiso 1 1 calc R U . . .
C25 C 0.7285(2) 0.45158(19) 0.7094(6) 0.0705(16) Uani 1 1 d . . . . .
H25 H 0.7451 0.4433 0.6231 0.085 Uiso 1 1 calc R U . . .
C26 C 0.72648(19) 0.4207(2) 0.8230(6) 0.0688(15) Uani 1 1 d . . . . .
H26 H 0.7388 0.3890 0.8154 0.083 Uiso 1 1 calc R U . . .
C27 C 0.7064(3) 0.4356(3) 0.9499(8) 0.126(4) Uani 1 1 d . . . . .
H27 H 0.7075 0.4154 1.0358 0.151 Uiso 1 1 calc R U . . .
C28 C 0.6844(3) 0.4797(2) 0.9569(7) 0.113(3) Uani 1 1 d . . . . .
H28 H 0.6705 0.4894 1.0471 0.135 Uiso 1 1 calc R U . . .
C29 C 0.64137(13) 0.59398(15) 1.0463(4) 0.0377(9) Uani 1 1 d . . . . .
C30 C 0.6049(2) 0.5777(3) 1.1225(7) 0.099(3) Uani 1 1 d . . . . .
H30 H 0.5846 0.5562 1.0754 0.119 Uiso 1 1 calc R U . . .
C31 C 0.5974(3) 0.5927(3) 1.2686(7) 0.123(3) Uani 1 1 d . . . . .
H31 H 0.5725 0.5804 1.3213 0.148 Uiso 1 1 calc R U . . .
C32 C 0.6249(2) 0.6241(2) 1.3361(5) 0.0694(15) Uani 1 1 d . . . . .
H32 H 0.6187 0.6355 1.4339 0.083 Uiso 1 1 calc R U . . .
C33 C 0.66123(17) 0.6392(2) 1.2638(5) 0.0630(14) Uani 1 1 d . . . . .
H33 H 0.6815 0.6604 1.3125 0.076 Uiso 1 1 calc R U . . .
C34 C 0.66962(14) 0.62433(19) 1.1185(5) 0.0509(11) Uani 1 1 d . . . . .
H34 H 0.6955 0.6356 1.0690 0.061 Uiso 1 1 calc R U . . .
C35A C 0.4456(6) 0.6019(5) 0.207(2) 0.039(3) Uani 0.526(8) 1 d . . P B 1
C36A C 0.4856(3) 0.6094(5) 0.1345(11) 0.075(4) Uani 0.526(8) 1 d . . P B 1
C37A C 0.4881(3) 0.6012(6) -0.0213(11) 0.087(4) Uani 0.526(8) 1 d . . P B 1
C38A C 0.4529(4) 0.5867(9) -0.0935(15) 0.088(6) Uani 0.526(8) 1 d . . P B 1
C39A C 0.4116(3) 0.5728(5) -0.0280(9) 0.063(3) Uani 0.526(8) 1 d . . P B 1
C40A C 0.4086(3) 0.5825(4) 0.1283(11) 0.045(3) Uani 0.526(8) 1 d . . P B 1
C35B C 0.4503(7) 0.5817(5) 0.207(2) 0.039(4) Uani 0.474(8) 1 d . . P B 2
C36B C 0.4763(3) 0.5436(4) 0.1743(12) 0.058(3) Uani 0.474(8) 1 d . . P B 2
C37B C 0.4820(4) 0.5271(5) 0.0244(14) 0.069(4) Uani 0.474(8) 1 d . . P B 2
C38B C 0.4595(5) 0.5512(5) -0.0855(12) 0.056(3) Uani 0.474(8) 1 d . . P B 2
C39B C 0.4330(8) 0.5906(9) -0.060(3) 0.107(8) Uiso 0.474(8) 1 d . . P B 2
C40B C 0.4295(9) 0.6089(8) 0.0933(14) 0.145(12) Uani 0.474(8) 1 d . . P B 2
C41 C 0.38948(14) 0.5888(3) 0.5150(5) 0.0671(17) Uani 1 1 d . . . . .
C42 C 0.35524(17) 0.6215(3) 0.5485(6) 0.088(2) Uani 1 1 d . . . . .
H42 H 0.3578 0.6548 0.5211 0.105 Uiso 1 1 calc R U . . .
C43 C 0.31761(19) 0.6050(4) 0.6222(7) 0.114(3) Uani 1 1 d . . . . .
H43 H 0.2948 0.6274 0.6473 0.136 Uiso 1 1 calc R U . . .
C44 C 0.3130(2) 0.5574(5) 0.6589(8) 0.126(4) Uani 1 1 d . . . . .
H44 H 0.2868 0.5465 0.7070 0.151 Uiso 1 1 calc R U . . .
C45 C 0.3464(2) 0.5246(4) 0.6263(8) 0.117(3) Uani 1 1 d . . . . .
H45 H 0.3432 0.4914 0.6534 0.140 Uiso 1 1 calc R U . . .
C46 C 0.38456(18) 0.5401(3) 0.5543(6) 0.088(2) Uani 1 1 d . . . . .
H46 H 0.4074 0.5174 0.5318 0.106 Uiso 1 1 calc R U . . .
C47 C 0.6345(5) 0.7500 0.5612(19) 0.135(5) Uani 1 2 d S T P . .
C48 C 0.6015(9) 0.7500 0.672(3) 0.289(15) Uani 1 2 d S T P . .
C49 C 0.6071(7) 0.7500 0.819(2) 0.178(8) Uani 1 2 d S T P . .
C50 C 0.5771(6) 0.7500 0.940(3) 0.214(10) Uani 1 2 d S T P . .
C51 C 0.5805(8) 0.7500 1.082(2) 0.244(12) Uani 1 2 d S T P . .
C52 C 0.5504(5) 0.7500 1.211(2) 0.203(8) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 C1 1.915(4) 7_575 ?
Ge1 C1 1.915(4) . ?
Ge1 C17 1.919(5) . ?
Ge1 C11 1.929(5) . ?
Ge2 C5 1.904(4) . ?
Ge2 C4 1.905(4) . ?
Ge2 C23 1.924(4) . ?
Ge2 C29 1.929(4) . ?
Ge3 C35A 1.871(18) . ?
Ge3 C9 1.903(8) . ?
Ge3 C8 1.907(4) . ?
Ge3 C41 1.926(5) . ?
Ge3 C35B 2.036(19) . ?
C1 C2 1.196(5) . ?
C2 C3 1.374(5) . ?
C3 C4 1.202(5) . ?
C5 C6 1.204(5) . ?
C6 C7 1.376(5) . ?
C7 C8 1.201(6) . ?
C9 C10 1.188(8) . ?
C10 C10 1.420(15) 7_575 ?
C11 C16 1.346(9) . ?
C11 C12 1.355(8) . ?
C12 C13 1.393(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.343(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.321(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.395(10) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.320(12) . ?
C17 C18 1.400(9) . ?
C18 C19 1.378(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.325(12) . ?
C19 H19 0.9500 . ?
C21 C20 1.343(15) . ?
C21 C22 1.385(16) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C20 H20 0.77(9) . ?
C23 C28 1.342(6) . ?
C23 C24 1.360(6) . ?
C24 C25 1.377(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.327(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.352(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(8) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.357(6) . ?
C29 C30 1.371(6) . ?
C30 C31 1.391(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.342(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.340(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35A C36A 1.39(2) . ?
C35A C40A 1.42(2) . ?
C36A C37A 1.418(13) . ?
C37A C38A 1.307(16) . ?
C38A C39A 1.429(17) . ?
C39A C40A 1.430(13) . ?
C35B C36B 1.343(18) . ?
C35B C40B 1.41(2) . ?
C36B C37B 1.429(15) . ?
C37B C38B 1.366(18) . ?
C37B C37B 1.90(2) 5_665 ?
C38B C39B 1.37(3) . ?
C39B C40B 1.47(3) . ?
C41 C46 1.390(9) . ?
C41 C42 1.403(8) . ?
C42 C43 1.391(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.355(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(12) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(8) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.41(2) . ?
C48 C49 1.33(3) . ?
C49 C50 1.42(2) . ?
C50 C51 1.28(2) . ?
C51 C52 1.47(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
C1 Ge1 C1 98.5(2) 7_575 . ?
C1 Ge1 C17 109.53(14) 7_575 . ?
C1 Ge1 C17 109.53(14) . . ?
C1 Ge1 C11 109.71(14) 7_575 . ?
C1 Ge1 C11 109.71(14) . . ?
C17 Ge1 C11 118.1(2) . . ?
C5 Ge2 C4 104.58(16) . . ?
C5 Ge2 C23 112.25(16) . . ?
C4 Ge2 C23 105.82(16) . . ?
C5 Ge2 C29 108.73(16) . . ?
C4 Ge2 C29 110.39(17) . . ?
C23 Ge2 C29 114.57(16) . . ?
C35A Ge3 C9 100.3(4) . . ?
C35A Ge3 C8 113.6(5) . . ?
C9 Ge3 C8 105.4(2) . . ?
C35A Ge3 C41 118.3(6) . . ?
C9 Ge3 C41 108.5(3) . . ?
C8 Ge3 C41 109.43(19) . . ?
C9 Ge3 C35B 115.8(5) . . ?
C8 Ge3 C35B 103.3(5) . . ?
C41 Ge3 C35B 113.8(6) . . ?
C2 C1 Ge1 167.7(3) . . ?
C1 C2 C3 179.5(4) . . ?
C4 C3 C2 178.9(4) . . ?
C3 C4 Ge2 175.6(3) . . ?
C6 C5 Ge2 173.6(4) . . ?
C5 C6 C7 177.0(5) . . ?
C8 C7 C6 177.9(5) . . ?
C7 C8 Ge3 174.0(5) . . ?
C10 C9 Ge3 178.2(5) . . ?
C9 C10 C10 179.5(4) . 7_575 ?
C16 C11 C12 117.9(6) . . ?
C16 C11 Ge1 119.7(4) . . ?
C12 C11 Ge1 122.4(5) . . ?
C11 C12 C13 120.4(8) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 120.9(8) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 118.9(7) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 121.1(8) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 120.9(7) . . ?
C11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C22 C17 C18 117.5(7) . . ?
C22 C17 Ge1 122.8(6) . . ?
C18 C17 Ge1 119.7(5) . . ?
C19 C18 C17 120.4(8) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 120.1(9) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C20 C21 C22 120.5(12) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 121.4(11) . . ?
C17 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C19 C20 C21 120.0(9) . . ?
C19 C20 H20 116(4) . . ?
C21 C20 H20 124(4) . . ?
C28 C23 C24 117.1(4) . . ?
C28 C23 Ge2 120.8(4) . . ?
C24 C23 Ge2 121.8(3) . . ?
C23 C24 C25 121.8(4) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C26 C25 C24 120.4(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 118.3(5) . . ?
C25 C26 H26 120.9 . . ?
C27 C26 H26 120.9 . . ?
C26 C27 C28 121.2(5) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C23 C28 C27 120.6(5) . . ?
C23 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C34 C29 C30 117.8(4) . . ?
C34 C29 Ge2 122.4(3) . . ?
C30 C29 Ge2 119.7(4) . . ?
C29 C30 C31 120.2(6) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C32 C31 C30 121.0(6) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 119.1(5) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 120.8(5) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C29 C34 C33 121.0(4) . . ?
C29 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C36A C35A C40A 120.4(14) . . ?
C36A C35A Ge3 119.8(12) . . ?
C40A C35A Ge3 119.6(11) . . ?
C35A C36A C37A 119.1(11) . . ?
C38A C37A C36A 119.5(10) . . ?
C37A C38A C39A 125.9(11) . . ?
C38A C39A C40A 114.1(10) . . ?
C35A C40A C39A 120.4(10) . . ?
C36B C35B C40B 120.8(16) . . ?
C36B C35B Ge3 126.2(12) . . ?
C40B C35B Ge3 112.7(11) . . ?
C35B C36B C37B 121.6(12) . . ?
C38B C37B C36B 117.9(11) . . ?
C38B C37B C37B 119.9(12) . 5_665 ?
C36B C37B C37B 122.2(13) . 5_665 ?
C37B C38B C39B 123.6(13) . . ?
C38B C39B C40B 117.9(18) . . ?
C35B C40B C39B 117.9(16) . . ?
C46 C41 C42 118.9(5) . . ?
C46 C41 Ge3 121.4(4) . . ?
C42 C41 Ge3 119.6(5) . . ?
C43 C42 C41 119.6(8) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 121.0(8) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 120.2(7) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 120.2(9) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 120.1(7) . . ?
C45 C46 H46 120.0 . . ?
C41 C46 H46 120.0 . . ?
C49 C48 C47 127(3) . . ?
C48 C49 C50 133(2) . . ?
C51 C50 C49 136(2) . . ?
C50 C51 C52 137(2) . . ?

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
C16 C11 C12 C13 0.000(1) . . . . ?
Ge1 C11 C12 C13 180.000(0) . . . . ?
C11 C12 C13 C14 0.000(1) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C12 C11 C16 C15 0.000(1) . . . . ?
Ge1 C11 C16 C15 180.000(0) . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
C22 C17 C18 C19 -4.8(17) . . . . ?
Ge1 C17 C18 C19 176.0(8) . . . . ?
C17 C18 C19 C20 2.2(16) . . . . ?
C18 C17 C22 C21 4(3) . . . . ?
Ge1 C17 C22 C21 -176.8(16) . . . . ?
C20 C21 C22 C17 -1(3) . . . . ?
C18 C19 C20 C21 1(2) . . . . ?
C22 C21 C20 C19 -2(3) . . . . ?
C28 C23 C24 C25 6.2(9) . . . . ?
Ge2 C23 C24 C25 179.3(4) . . . . ?
C23 C24 C25 C26 0.2(9) . . . . ?
C24 C25 C26 C27 -6.7(11) . . . . ?
C25 C26 C27 C28 6.7(13) . . . . ?
C24 C23 C28 C27 -6.1(11) . . . . ?
Ge2 C23 C28 C27 -179.3(7) . . . . ?
C26 C27 C28 C23 -0.2(15) . . . . ?
C34 C29 C30 C31 0.6(11) . . . . ?
Ge2 C29 C30 C31 177.3(7) . . . . ?
C29 C30 C31 C32 1.9(14) . . . . ?
C30 C31 C32 C33 -3.5(13) . . . . ?
C31 C32 C33 C34 2.7(10) . . . . ?
C30 C29 C34 C33 -1.4(8) . . . . ?
Ge2 C29 C34 C33 -178.0(4) . . . . ?
C32 C33 C34 C29 -0.2(8) . . . . ?
C9 Ge3 C35A C36A 74.4(11) . . . . ?
C8 Ge3 C35A C36A -37.6(12) . . . . ?
C41 Ge3 C35A C36A -168.0(10) . . . . ?
C9 Ge3 C35A C40A -111.3(10) . . . . ?
C8 Ge3 C35A C40A 136.7(10) . . . . ?
C41 Ge3 C35A C40A 6.3(13) . . . . ?
C40A C35A C36A C37A 5(2) . . . . ?
Ge3 C35A C36A C37A 179.1(11) . . . . ?
C35A C36A C37A C38A 0(2) . . . . ?
C36A C37A C38A C39A -7(3) . . . . ?
C37A C38A C39A C40A 9(3) . . . . ?
C36A C35A C40A C39A -3(2) . . . . ?
Ge3 C35A C40A C39A -177.3(9) . . . . ?
C38A C39A C40A C35A -3.3(19) . . . . ?
C40B C35B C36B C37B -4(3) . . . . ?
Ge3 C35B C36B C37B -176.4(11) . . . . ?
C35B C36B C37B C38B -0.8(19) . . . . ?
C35B C36B C37B C37B -179.2(14) . . . 5_665 ?
C36B C37B C38B C39B 2(2) . . . . ?
C37B C37B C38B C39B -179.9(17) 5_665 . . . ?
C37B C38B C39B C40B 2(3) . . . . ?
C36B C35B C40B C39B 7(4) . . . . ?
Ge3 C35B C40B C39B -179(2) . . . . ?
C38B C39B C40B C35B -6(4) . . . . ?
C46 C41 C42 C43 1.1(8) . . . . ?
Ge3 C41 C42 C43 -180.0(5) . . . . ?
C41 C42 C43 C44 -1.7(10) . . . . ?
C42 C43 C44 C45 1.5(12) . . . . ?
C43 C44 C45 C46 -0.8(12) . . . . ?
C44 C45 C46 C41 0.2(10) . . . . ?
C42 C41 C46 C45 -0.4(8) . . . . ?
Ge3 C41 C46 C45 -179.3(5) . . . . ?
C47 C48 C49 C50 180.000(6) . . . . ?
C48 C49 C50 C51 180.000(6) . . . . ?
C49 C50 C51 C52 180.000(6) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        'extended decaphenyl germa[5]pericyclyne'
_chemical_name_common            'Ext_PhGe[5] with hexane'
