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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_GeC14Phcage


_audit_creation_method           SHELXL-97
_chemical_name_systematic        GeMolecularGyrotop
_chemical_name_common            GeMolecularGyrotop
_chemical_melting_point          '244-245 deg. C'
_chemical_formula_moiety         'C48 H88 Ge2'
_chemical_formula_sum            'C48 H88 Ge2'
_chemical_formula_weight         810.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   25.736(7)
_cell_length_b                   11.733(3)
_cell_length_c                   18.790(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.046(3)
_cell_angle_gamma                90.00
_cell_volume                     4911(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    2417
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      19.69

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_T_max  0.7879
_exptl_absorpt_process_details   'SADABS  Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            11694
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.10
_reflns_number_total             4954
_reflns_number_gt                2169
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'


_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)+(0.1252P)²+1.1909P] 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         4954
_refine_ls_number_parameters     264
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.2352
_refine_ls_wR_factor_gt          0.1884
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.045
_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
Ge01 Ge 0.34902(2) 0.02636(6) 0.13328(4) 0.1046(4) Uani 1 1 d . . .
C01 C 0.4366(2) 0.0203(4) 0.2009(3) 0.0864(13) Uani 1 1 d . C .
C02 C 0.4656(3) 0.0210(6) 0.2840(4) 0.128(2) Uani 1 1 d . . .
H02 H 0.4430 0.0218 0.3101 0.154 Uiso 1 1 calc R C .
C03 C 0.4724(3) 0.0204(6) 0.1680(4) 0.129(2) Uani 1 1 d . . .
H03 H 0.4550 0.0201 0.1111 0.154 Uiso 1 1 calc R C .
C04 C 0.3243(2) 0.1798(5) 0.0940(3) 0.1023(16) Uani 1 1 d . C .
H04A H 0.3321 0.1935 0.0492 0.123 Uiso 1 1 calc R . .
H04B H 0.2813 0.1855 0.0716 0.123 Uiso 1 1 calc R . .
C05 C 0.3545(3) 0.2734(6) 0.1574(4) 0.1119(18) Uani 1 1 d . . .
H05A H 0.3469 0.2599 0.2023 0.134 Uiso 1 1 calc R C .
H05B H 0.3975 0.2686 0.1795 0.134 Uiso 1 1 calc R . .
C06 C 0.3345(4) 0.3894(6) 0.1258(5) 0.149(3) Uani 1 1 d D B .
H06A H 0.2945 0.4041 0.1168 0.179 Uiso 1 1 calc R A 1
H06B H 0.3346 0.4015 0.0748 0.179 Uiso 1 1 calc R A 1
C07 C 0.3833(9) 0.4681(11) 0.1976(10) 0.160(10) Uani 0.56(2) 1 d PD B 1
H07A H 0.3812 0.4579 0.2473 0.192 Uiso 0.56(2) 1 calc PR B 1
H07B H 0.4233 0.4473 0.2094 0.192 Uiso 0.56(2) 1 calc PR B 1
C08 C 0.3702(7) 0.5927(12) 0.1694(10) 0.171(9) Uani 0.56(2) 1 d PD B 1
H08A H 0.3700 0.6035 0.1180 0.205 Uiso 0.56(2) 1 calc PR B 1
H08B H 0.3318 0.6169 0.1622 0.205 Uiso 0.56(2) 1 calc PR B 1
C107 C 0.3484(8) 0.4946(11) 0.1794(13) 0.112(7) Uani 0.44(2) 1 d PD B 2
H10A H 0.3496 0.4759 0.2305 0.134 Uiso 0.44(2) 1 calc PR B 2
H10B H 0.3182 0.5530 0.1512 0.134 Uiso 0.44(2) 1 calc PR B 2
C108 C 0.4098(10) 0.536(2) 0.196(2) 0.187(10) Uani 0.44(2) 1 d PDU B 2
H10C H 0.4106 0.5406 0.1451 0.225 Uiso 0.44(2) 1 calc PR B 2
H10D H 0.4409 0.4831 0.2325 0.225 Uiso 0.44(2) 1 calc PR B 2
C09 C 0.4203(5) 0.6564(9) 0.2372(6) 0.200(4) Uani 1 1 d DU . .
H09A H 0.4132 0.6462 0.2829 0.240 Uiso 1 1 calc R B 1
H09B H 0.4103 0.7354 0.2208 0.240 Uiso 1 1 calc R B 1
C10 C 0.4891(5) 0.6544(7) 0.2786(5) 0.166(3) Uani 1 1 d . . .
H10E H 0.5052 0.7205 0.3141 0.199 Uiso 1 1 calc R . .
H10F H 0.5041 0.5870 0.3129 0.199 Uiso 1 1 calc R . .
C11 C 0.3171(5) -0.0777(15) 0.0478(12) 0.110(6) Uani 0.54(2) 1 d PD C 3
H11A H 0.3015 -0.1407 0.0649 0.132 Uiso 0.54(2) 1 calc PR C 3
H11B H 0.2829 -0.0413 0.0019 0.132 Uiso 0.54(2) 1 calc PR C 3
C12 C 0.3532(8) -0.126(3) 0.0169(15) 0.230(19) Uani 0.54(2) 1 d PD C 3
H12A H 0.3900 -0.1546 0.0630 0.276 Uiso 0.54(2) 1 calc PR C 3
H12B H 0.3641 -0.0652 -0.0083 0.276 Uiso 0.54(2) 1 calc PR C 3
C111 C 0.3295(10) -0.0588(17) 0.0157(17) 0.136(8) Uani 0.46(2) 1 d PDU C 4
H11C H 0.2902 -0.0379 -0.0292 0.163 Uiso 0.46(2) 1 calc PR C 4
H11D H 0.3596 -0.0405 0.0009 0.163 Uiso 0.46(2) 1 calc PR C 4
C112 C 0.3318(11) -0.177(2) 0.0371(15) 0.158(9) Uani 0.46(2) 1 d PDU C 4
H11E H 0.2993 -0.1992 0.0465 0.190 Uiso 0.46(2) 1 calc PR C 4
H11F H 0.3701 -0.1990 0.0839 0.190 Uiso 0.46(2) 1 calc PR C 4
C13 C 0.3230(6) -0.2254(12) -0.0482(7) 0.246(7) Uani 1 1 d D . .
H13A H 0.3221 -0.2966 -0.0226 0.295 Uiso 1 1 calc R C 3
H13B H 0.2828 -0.2058 -0.0914 0.295 Uiso 1 1 calc R C 3
C14 C 0.3658(8) -0.2284(16) -0.0779(12) 0.303(8) Uani 1 1 d DU C .
H14A H 0.3432 -0.2429 -0.1366 0.363 Uiso 1 1 calc R . .
H14B H 0.3830 -0.1528 -0.0707 0.363 Uiso 1 1 calc R . .
C15 C 0.4157(9) -0.3102(18) -0.0415(12) 0.345(9) Uani 1 1 d DU . .
H15A H 0.4004 -0.3864 -0.0435 0.414 Uiso 1 1 calc R C .
H15B H 0.4429 -0.2908 0.0156 0.414 Uiso 1 1 calc R . .
C16 C 0.4502(8) -0.3068(15) -0.0908(9) 0.301(7) Uani 1 1 d DU C .
H16A H 0.4413 -0.3712 -0.1275 0.361 Uiso 1 1 calc R . .
H16B H 0.4452 -0.2356 -0.1198 0.361 Uiso 1 1 calc R . .
C17 C 0.5093(8) -0.3165(17) -0.0127(9) 0.296(7) Uani 1 1 d DU . .
H17A H 0.5163 -0.2452 0.0169 0.355 Uiso 1 1 calc R C .
H17B H 0.5053 -0.3753 0.0206 0.355 Uiso 1 1 calc R . .
C18 C 0.4396(8) -0.3410(13) 0.5175(10) 0.262(8) Uani 1 1 d . . .
H18A H 0.4377 -0.2860 0.5546 0.315 Uiso 1 1 calc R . .
H18B H 0.4455 -0.4152 0.5431 0.315 Uiso 1 1 calc R . .
C19 C 0.3772(8) -0.3422(16) 0.4378(14) 0.275(10) Uani 1 1 d . . .
H19A H 0.3774 -0.3964 0.3989 0.331 Uiso 1 1 calc R . .
H19B H 0.3466 -0.3651 0.4505 0.331 Uiso 1 1 calc R . .
C20 C 0.3640(6) -0.2262(15) 0.4014(8) 0.224(7) Uani 1 1 d D . .
H20A H 0.3927 -0.2070 0.3842 0.269 Uiso 1 1 calc R . .
H20B H 0.3685 -0.1715 0.4428 0.269 Uiso 1 1 calc R . .
C21 C 0.3020(7) -0.2179(18) 0.3293(10) 0.295(12) Uani 1 1 d D . .
H21A H 0.2974 -0.2756 0.2896 0.354 Uiso 1 1 calc R . .
H21B H 0.2737 -0.2354 0.3475 0.354 Uiso 1 1 calc R . .
C22 C 0.2869(6) -0.1126(14) 0.2898(9) 0.235(8) Uani 1 1 d . C .
H22A H 0.2980 -0.0517 0.3298 0.283 Uiso 1 1 calc R . .
H22B H 0.2439 -0.1085 0.2520 0.283 Uiso 1 1 calc R . .
C23 C 0.3210(5) -0.1010(12) 0.2431(7) 0.243(6) Uani 1 1 d D . .
H23A H 0.3637 -0.1073 0.2815 0.291 Uiso 1 1 calc R C .
H23B H 0.3096 -0.1629 0.2038 0.291 Uiso 1 1 calc R . .
C24 C 0.3100(4) -0.0017(9) 0.2032(8) 0.219(6) Uani 1 1 d D C .
H24A H 0.3225 0.0589 0.2436 0.263 Uiso 1 1 calc R . .
H24B H 0.2669 0.0051 0.1677 0.263 Uiso 1 1 calc R . .


_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
Ge01 C11 1.850(13) . ?
Ge01 C04 1.929(6) . ?
Ge01 C01 1.957(5) . ?
Ge01 C24 2.041(11) . ?
Ge01 C111 2.24(3) . ?
C01 C03 1.342(8) . ?
C01 C02 1.353(8) . ?
C02 C03 1.385(8) 2_655 ?
C02 H02 0.9300 . ?
C03 C02 1.385(8) 2_655 ?
C03 H03 0.9300 . ?
C04 C05 1.517(8) . ?
C04 H04A 0.9700 . ?
C04 H04B 0.9700 . ?
C05 C06 1.471(10) . ?
C05 H05A 0.9700 . ?
C05 H05B 0.9700 . ?
C06 C107 1.519(14) . ?
C06 C07 1.598(16) . ?
C06 H06A 0.9700 . ?
C06 H06B 0.9700 . ?
C07 C08 1.535(13) . ?
C07 H07A 0.9700 . ?
C07 H07B 0.9700 . ?
C08 C09 1.484(15) . ?
C08 H08A 0.9700 . ?
C08 H08B 0.9700 . ?
C107 C108 1.527(14) . ?
C107 H10A 0.9700 . ?
C107 H10B 0.9700 . ?
C108 C09 1.572(17) . ?
C108 H10C 0.9700 . ?
C108 H10D 0.9700 . ?
C09 C10 1.537(12) . ?
C09 H09A 0.9700 . ?
C09 H09B 0.9700 . ?
C10 C10 1.439(15) 2_655 ?
C10 H10E 0.9700 . ?
C10 H10F 0.9700 . ?
C11 C12 1.435(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.585(18) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C111 C112 1.443(18) . ?
C111 H11C 0.9700 . ?
C111 H11D 0.9700 . ?
C112 C13 1.60(3) . ?
C112 H11E 0.9700 . ?
C112 H11F 0.9700 . ?
C13 C14 1.464(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.470(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.570(16) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.499(18) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.393(16) 2_655 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C17 1.393(16) 2_655 ?
C18 C19 1.55(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.48(2) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.492(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.39(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.528(13) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.336(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Ge01 C04 111.5(7) . . ?
C11 Ge01 C01 113.9(4) . . ?
C04 Ge01 C01 109.5(2) . . ?
C11 Ge01 C24 107.7(7) . . ?
C04 Ge01 C24 102.9(3) . . ?
C01 Ge01 C24 110.8(3) . . ?
C11 Ge01 C111 21.1(6) . . ?
C04 Ge01 C111 99.8(6) . . ?
C01 Ge01 C111 103.9(6) . . ?
C24 Ge01 C111 128.5(7) . . ?
C03 C01 C02 114.9(5) . . ?
C03 C01 Ge01 122.3(4) . . ?
C02 C01 Ge01 122.7(4) . . ?
C01 C02 C03 122.9(6) . 2_655 ?
C01 C02 H02 118.5 . . ?
C03 C02 H02 118.5 2_655 . ?
C01 C03 C02 122.2(6) . 2_655 ?
C01 C03 H03 118.9 . . ?
C02 C03 H03 118.9 2_655 . ?
C05 C04 Ge01 115.7(4) . . ?
C05 C04 H04A 108.4 . . ?
Ge01 C04 H04A 108.4 . . ?
C05 C04 H04B 108.4 . . ?
Ge01 C04 H04B 108.4 . . ?
H04A C04 H04B 107.4 . . ?
C06 C05 C04 114.5(6) . . ?
C06 C05 H05A 108.6 . . ?
C04 C05 H05A 108.6 . . ?
C06 C05 H05B 108.6 . . ?
C04 C05 H05B 108.6 . . ?
H05A C05 H05B 107.6 . . ?
C05 C06 C107 124.5(10) . . ?
C05 C06 C07 103.1(8) . . ?
C107 C06 C07 31.3(7) . . ?
C05 C06 H06A 111.2 . . ?
C107 C06 H06A 81.3 . . ?
C07 C06 H06A 111.2 . . ?
C05 C06 H06B 111.2 . . ?
C107 C06 H06B 114.8 . . ?
C07 C06 H06B 111.2 . . ?
H06A C06 H06B 109.1 . . ?
C08 C07 C06 108.3(11) . . ?
C08 C07 H07A 110.0 . . ?
C06 C07 H07A 110.0 . . ?
C08 C07 H07B 110.0 . . ?
C06 C07 H07B 110.0 . . ?
H07A C07 H07B 108.4 . . ?
C09 C08 C07 103.7(11) . . ?
C09 C08 H08A 111.0 . . ?
C07 C08 H08A 111.0 . . ?
C09 C08 H08B 111.0 . . ?
C07 C08 H08B 111.0 . . ?
H08A C08 H08B 109.0 . . ?
C06 C107 C108 105.5(11) . . ?
C06 C107 H10A 110.6 . . ?
C108 C107 H10A 110.6 . . ?
C06 C107 H10B 110.6 . . ?
C108 C107 H10B 110.6 . . ?
H10A C107 H10B 108.8 . . ?
C107 C108 C09 106.9(14) . . ?
C107 C108 H10C 110.3 . . ?
C09 C108 H10C 110.3 . . ?
C107 C108 H10D 110.3 . . ?
C09 C108 H10D 110.3 . . ?
H10C C108 H10D 108.6 . . ?
C08 C09 C10 135.5(10) . . ?
C08 C09 C108 42.4(11) . . ?
C10 C09 C108 96.1(10) . . ?
C08 C09 H09A 103.3 . . ?
C10 C09 H09A 103.3 . . ?
C108 C09 H09A 105.2 . . ?
C08 C09 H09B 103.3 . . ?
C10 C09 H09B 103.3 . . ?
C108 C09 H09B 138.8 . . ?
H09A C09 H09B 105.2 . . ?
C10 C10 C09 113.7(10) 2_655 . ?
C10 C10 H10E 108.8 2_655 . ?
C09 C10 H10E 108.8 . . ?
C10 C10 H10F 108.8 2_655 . ?
C09 C10 H10F 108.8 . . ?
H10E C10 H10F 107.7 . . ?
C12 C11 Ge01 121.0(11) . . ?
C12 C11 H11A 107.1 . . ?
Ge01 C11 H11A 107.1 . . ?
C12 C11 H11B 107.1 . . ?
Ge01 C11 H11B 107.1 . . ?
H11A C11 H11B 106.8 . . ?
C11 C12 C13 115.9(15) . . ?
C11 C12 H12A 108.3 . . ?
C13 C12 H12A 108.3 . . ?
C11 C12 H12B 108.3 . . ?
C13 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C112 C111 Ge01 101(2) . . ?
C112 C111 H11C 111.5 . . ?
Ge01 C111 H11C 111.5 . . ?
C112 C111 H11D 111.5 . . ?
Ge01 C111 H11D 111.5 . . ?
H11C C111 H11D 109.3 . . ?
C111 C112 C13 95.4(18) . . ?
C111 C112 H11E 112.7 . . ?
C13 C112 H11E 112.7 . . ?
C111 C112 H11F 112.7 . . ?
C13 C112 H11F 112.7 . . ?
H11E C112 H11F 110.2 . . ?
C14 C13 C112 129.3(13) . . ?
C14 C13 C12 98.1(12) . . ?
C112 C13 C12 37.0(12) . . ?
C14 C13 H13A 112.1 . . ?
C112 C13 H13A 80.4 . . ?
C12 C13 H13A 112.1 . . ?
C14 C13 H13B 112.1 . . ?
C112 C13 H13B 108.2 . . ?
C12 C13 H13B 112.1 . . ?
H13A C13 H13B 109.8 . . ?
C15 C14 C13 119.2(19) . . ?
C15 C14 H14A 107.5 . . ?
C13 C14 H14A 107.5 . . ?
C15 C14 H14B 107.5 . . ?
C13 C14 H14B 107.5 . . ?
H14A C14 H14B 107.0 . . ?
C14 C15 C16 109.2(17) . . ?
C14 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
C17 C16 C15 90.9(11) . . ?
C17 C16 H16A 113.5 . . ?
C15 C16 H16A 113.5 . . ?
C17 C16 H16B 113.5 . . ?
C15 C16 H16B 113.5 . . ?
H16A C16 H16B 110.8 . . ?
C18 C17 C16 118.7(15) 2_655 . ?
C18 C17 H17A 107.6 2_655 . ?
C16 C17 H17A 107.6 . . ?
C18 C17 H17B 107.6 2_655 . ?
C16 C17 H17B 107.6 . . ?
H17A C17 H17B 107.1 . . ?
C17 C18 C19 119.6(15) 2_655 . ?
C17 C18 H18A 107.4 2_655 . ?
C19 C18 H18A 107.4 . . ?
C17 C18 H18B 107.4 2_655 . ?
C19 C18 H18B 107.4 . . ?
H18A C18 H18B 107.0 . . ?
C20 C19 C18 108.9(13) . . ?
C20 C19 H19A 109.9 . . ?
C18 C19 H19A 109.9 . . ?
C20 C19 H19B 109.9 . . ?
C18 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C19 C20 C21 111.9(14) . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C20 115.4(15) . . ?
C22 C21 H21A 108.4 . . ?
C20 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C20 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 C23 107.2(14) . . ?
C21 C22 H22A 110.3 . . ?
C23 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
C23 C22 H22B 110.3 . . ?
H22A C22 H22B 108.5 . . ?
C24 C23 C22 112.2(12) . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C22 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 Ge01 117.8(9) . . ?
C23 C24 H24A 107.8 . . ?
Ge01 C24 H24A 107.8 . . ?
C23 C24 H24B 107.8 . . ?
Ge01 C24 H24B 107.8 . . ?
H24A C24 H24B 107.2 . . ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.059
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_chemical_compound_source        no
_database_code_depnum_ccdc_archive 'CCDC 1026017'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_GeC14Phcage


_audit_creation_method           SHELXL-97
_chemical_name_systematic        GeMolecularGyrotop
_chemical_name_common            GeMolecularGyrotop
_chemical_melting_point          '244-245 deg. C'
_chemical_formula_moiety         'C48 H88 Ge2'
_chemical_formula_sum            'C48 H88 Ge2'
_chemical_formula_weight         810.36

# start Validation Reply Form
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low .... 29 %
RESPONSE: Because the collection temperature is high (300 K).
;
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact H13A .. H15B .. 1.60 Ang.
RESPONSE: Due to unresolved disorders.
;
# end Validation Reply Form


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C c  '

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

_cell_length_a                   26.056(10)
_cell_length_b                   11.558(4)
_cell_length_c                   19.190(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.979(4)
_cell_angle_gamma                90.00
_cell_volume                     5056(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    1428
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      16.30

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_T_max  0.7930
_exptl_absorpt_process_details   'SADABS  Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            10770
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6828
_reflns_number_gt                1984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.1254P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_number_reflns         6828
_refine_ls_number_parameters     450
_refine_ls_number_restraints     294
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.2648
_refine_ls_wR_factor_gt          0.1778
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.030

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
Ge01 Ge 0.34675(6) 0.01385(18) -0.03677(8) 0.1981(10) Uani 1 1 d U . .
Ge02 Ge 0.64117(6) 0.01447(17) 0.17579(9) 0.1994(10) Uani 1 1 d U B .
C01 C 0.4332(8) 0.0094(9) 0.0274(11) 0.146(5) Uani 1 1 d DU . .
C02 C 0.4593(9) -0.0023(13) 0.1080(12) 0.207(6) Uani 1 1 d DU . .
H02 H 0.4375 -0.0103 0.1343 0.248 Uiso 1 1 calc R . .
C03 C 0.5212(10) -0.0017(12) 0.1496(12) 0.203(6) Uani 1 1 d DU . .
H03 H 0.5388 -0.0132 0.2043 0.244 Uiso 1 1 calc R . .
C04 C 0.5595(9) 0.0143(12) 0.1180(12) 0.168(6) Uani 1 1 d DU . .
C05 C 0.5246(10) 0.0184(18) 0.0398(15) 0.255(8) Uani 1 1 d DU . .
H05 H 0.5441 0.0156 0.0101 0.305 Uiso 1 1 calc R . .
C06 C 0.4652(11) 0.0260(17) -0.0043(13) 0.247(8) Uani 1 1 d DU . .
H06 H 0.4481 0.0436 -0.0583 0.297 Uiso 1 1 calc R . .
C07 C 0.3235(7) 0.1718(17) -0.0871(11) 0.234(7) Uani 1 1 d DU . .
H07A H 0.3446 0.1902 -0.1157 0.281 Uiso 1 1 calc R . .
H07B H 0.2818 0.1744 -0.1242 0.281 Uiso 1 1 calc R . .
C08 C 0.3388(9) 0.2545(16) -0.0215(13) 0.254(9) Uani 1 1 d DU . .
H08A H 0.3806 0.2527 0.0155 0.305 Uiso 1 1 calc R . .
H08B H 0.3178 0.2363 0.0073 0.305 Uiso 1 1 calc R . .
C09 C 0.3197(14) 0.378(2) -0.0629(16) 0.394(16) Uani 1 1 d DU . .
H09A H 0.3288 0.3838 -0.1062 0.473 Uiso 1 1 calc R . .
H09B H 0.2778 0.3887 -0.0846 0.473 Uiso 1 1 calc R . .
C10 C 0.3524(16) 0.468(2) -0.002(2) 0.46(2) Uani 1 1 d DU . .
H10A H 0.3794 0.4330 0.0489 0.547 Uiso 1 1 calc R . .
H10B H 0.3255 0.5179 0.0061 0.547 Uiso 1 1 calc R . .
C11 C 0.385(2) 0.537(3) -0.035(2) 0.56(3) Uani 1 1 d DU . .
H11A H 0.3598 0.5802 -0.0830 0.673 Uiso 1 1 calc R . .
H11B H 0.4125 0.4897 -0.0445 0.673 Uiso 1 1 calc R . .
C12 C 0.4166(16) 0.613(3) 0.040(3) 0.54(3) Uani 1 1 d DU . .
H12A H 0.3950 0.6100 0.0695 0.653 Uiso 1 1 calc R . .
H12B H 0.4167 0.6932 0.0244 0.653 Uiso 1 1 calc R . .
C13 C 0.482(2) 0.572(3) 0.096(2) 0.52(2) Uani 1 1 d DU . .
H13A H 0.4975 0.5973 0.1505 0.624 Uiso 1 1 calc R . .
H13B H 0.4866 0.4889 0.0939 0.624 Uiso 1 1 calc R . .
C14 C 0.5081(12) 0.6380(14) 0.0520(16) 0.358(11) Uani 1 1 d DU . .
H14A H 0.4993 0.7201 0.0459 0.429 Uiso 1 1 calc R . .
H14B H 0.5011 0.6031 0.0022 0.429 Uiso 1 1 calc R . .
C15 C 0.5671(13) 0.606(3) 0.1240(19) 0.423(14) Uani 1 1 d DU . .
H15A H 0.5974 0.6581 0.1271 0.508 Uiso 1 1 calc R . .
H15B H 0.5646 0.6147 0.1726 0.508 Uiso 1 1 calc R . .
C16 C 0.5810(12) 0.494(2) 0.116(2) 0.358(12) Uani 1 1 d DU . .
H16A H 0.5578 0.4665 0.0620 0.430 Uiso 1 1 calc R . .
H16B H 0.5749 0.4424 0.1517 0.430 Uiso 1 1 calc R . .
C17 C 0.6460(12) 0.501(2) 0.140(2) 0.386(13) Uani 1 1 d DU . .
H17A H 0.6641 0.5720 0.1686 0.463 Uiso 1 1 calc R . .
H17B H 0.6527 0.4930 0.0946 0.463 Uiso 1 1 calc R . .
C18 C 0.6659(10) 0.392(2) 0.1956(18) 0.343(13) Uani 1 1 d DU . .
H18A H 0.7075 0.3826 0.2141 0.412 Uiso 1 1 calc R . .
H18B H 0.6623 0.4123 0.2420 0.412 Uiso 1 1 calc R . .
C19 C 0.6408(13) 0.278(2) 0.1725(19) 0.307(12) Uani 1 1 d DU . .
H19A H 0.6071 0.2757 0.1813 0.368 Uiso 1 1 calc R . .
H19B H 0.6255 0.2723 0.1154 0.368 Uiso 1 1 calc R . .
C20 C 0.6736(9) 0.1741(19) 0.2066(15) 0.276(8) Uani 1 1 d DU . .
H20A H 0.6885 0.1800 0.2636 0.331 Uiso 1 1 calc R . .
H20B H 0.7076 0.1776 0.1985 0.331 Uiso 1 1 calc R . .
C21 C 0.3142(8) -0.0294(15) 0.0275(13) 0.241(6) Uani 1 1 d DU . .
H21A H 0.3286 0.0257 0.0710 0.289 Uiso 1 1 calc R . .
H21B H 0.2723 -0.0167 -0.0040 0.289 Uiso 1 1 calc R . .
C22 C 0.3216(12) -0.1431(18) 0.0630(14) 0.330(13) Uani 1 1 d DU . .
H22A H 0.3620 -0.1575 0.1030 0.396 Uiso 1 1 calc R . .
H22B H 0.3082 -0.2041 0.0233 0.396 Uiso 1 1 calc R . .
C23 C 0.2800(13) -0.128(3) 0.1012(18) 0.421(17) Uani 1 1 d DU . .
H23A H 0.2818 -0.0520 0.1230 0.506 Uiso 1 1 calc R . .
H23B H 0.2397 -0.1511 0.0658 0.506 Uiso 1 1 calc R . .
C24 C 0.3145(15) -0.218(3) 0.1632(19) 0.443(19) Uani 1 1 d DU . .
H24A H 0.2845 -0.2389 0.1770 0.532 Uiso 1 1 calc R . .
H24B H 0.3397 -0.1654 0.2056 0.532 Uiso 1 1 calc R . .
C25 C 0.3522(16) -0.326(3) 0.194(3) 0.57(3) Uani 1 1 d DU . .
H25A H 0.3659 -0.3541 0.1585 0.688 Uiso 1 1 calc R . .
H25B H 0.3325 -0.3880 0.2063 0.688 Uiso 1 1 calc R . .
C26 C 0.4014(16) -0.271(3) 0.2698(18) 0.51(3) Uani 1 1 d DU . .
H26A H 0.3842 -0.2423 0.3014 0.612 Uiso 1 1 calc R . .
H26B H 0.4153 -0.2035 0.2535 0.612 Uiso 1 1 calc R . .
C27 C 0.4559(16) -0.345(2) 0.325(2) 0.500(19) Uani 1 1 d DU . .
H27A H 0.4703 -0.3899 0.2959 0.600 Uiso 1 1 calc R . .
H27B H 0.4485 -0.3948 0.3601 0.600 Uiso 1 1 calc R . .
C28 C 0.4973(15) -0.242(3) 0.371(3) 0.62(3) Uani 1 1 d DU . .
H28A H 0.4987 -0.1834 0.3359 0.742 Uiso 1 1 calc R . .
H28B H 0.4881 -0.2070 0.4097 0.742 Uiso 1 1 calc R . .
C29 C 0.5519(17) -0.316(4) 0.4093(19) 0.58(2) Uani 1 1 d DU . .
H29A H 0.5760 -0.2956 0.4649 0.694 Uiso 1 1 calc R . .
H29B H 0.5415 -0.3974 0.4062 0.694 Uiso 1 1 calc R . .
C30 C 0.5847(19) -0.294(4) 0.364(3) 0.54(3) Uani 1 1 d DU . .
H30A H 0.5572 -0.2869 0.3074 0.653 Uiso 1 1 calc R . .
H30B H 0.6110 -0.3579 0.3713 0.653 Uiso 1 1 calc R . .
C31 C 0.6197(18) -0.182(4) 0.395(2) 0.444(15) Uani 1 1 d DU . .
H31A H 0.6340 -0.1712 0.4516 0.533 Uiso 1 1 calc R . .
H31B H 0.5974 -0.1145 0.3660 0.533 Uiso 1 1 calc R . .
C32 C 0.6696(17) -0.210(3) 0.3766(19) 0.422(14) Uani 1 1 d DU . .
H32A H 0.6782 -0.2921 0.3834 0.507 Uiso 1 1 calc R . .
H32B H 0.7048 -0.1680 0.4127 0.507 Uiso 1 1 calc R . .
C33 C 0.6498(14) -0.174(2) 0.2896(15) 0.381(13) Uani 1 1 d DU . .
H33A H 0.6657 -0.2288 0.2668 0.457 Uiso 1 1 calc R . .
H33B H 0.6073 -0.1793 0.2592 0.457 Uiso 1 1 calc R . .
C34 C 0.6665(10) -0.063(2) 0.2808(14) 0.310(11) Uani 1 1 d DU . .
H34A H 0.7091 -0.0632 0.3083 0.373 Uiso 1 1 calc R . .
H34B H 0.6548 -0.0125 0.3108 0.373 Uiso 1 1 calc R . .
C35 C 0.3173(10) -0.108(2) -0.1212(13) 0.278(9) Uani 1 1 d DU . .
H35A H 0.3319 -0.1822 -0.0965 0.333 Uiso 1 1 calc R . .
H35B H 0.2748 -0.1098 -0.1465 0.333 Uiso 1 1 calc R . .
C36 C 0.3343(13) -0.089(2) -0.1820(16) 0.347(13) Uani 1 1 d DU B .
H36A H 0.3766 -0.0816 -0.1571 0.416 Uiso 1 1 calc R . .
H36B H 0.3169 -0.0180 -0.2106 0.416 Uiso 1 1 calc R . .
C37 C 0.3128(13) -0.197(3) -0.2442(18) 0.371(16) Uani 1 1 d DU . .
H37A H 0.3134 -0.2673 -0.2159 0.446 Uiso 1 1 calc R A 1
H37B H 0.2726 -0.1839 -0.2851 0.446 Uiso 1 1 calc R A 1
C38 C 0.351(3) -0.215(6) -0.284(4) 0.12(4) Uiso 0.12(3) 1 d PDU B 1
H38A H 0.3278 -0.2383 -0.3396 0.146 Uiso 0.12(3) 1 calc PR B 1
H38B H 0.3729 -0.1457 -0.2818 0.146 Uiso 0.12(3) 1 calc PR B 1
C39 C 0.393(2) -0.313(6) -0.235(5) 0.24(7) Uiso 0.12(3) 1 d PDU B 1
H39A H 0.3731 -0.3869 -0.2450 0.288 Uiso 0.12(3) 1 calc PR B 1
H39B H 0.4123 -0.2962 -0.1783 0.288 Uiso 0.12(3) 1 calc PR B 1
C138 C 0.3489(19) -0.269(3) -0.250(3) 0.39(2) Uiso 0.88(3) 1 d PDU B 2
H13C H 0.3275 -0.3054 -0.3025 0.464 Uiso 0.88(3) 1 calc PR B 2
H13D H 0.3572 -0.3298 -0.2114 0.464 Uiso 0.88(3) 1 calc PR B 2
C139 C 0.409(2) -0.230(5) -0.241(3) 0.48(3) Uiso 0.88(3) 1 d PDU B 2
H13E H 0.4028 -0.1579 -0.2695 0.578 Uiso 0.88(3) 1 calc PR B 2
H13F H 0.4350 -0.2154 -0.1854 0.578 Uiso 0.88(3) 1 calc PR B 2
C40 C 0.4366(14) -0.308(5) -0.269(2) 0.53(2) Uani 1 1 d DU . .
H40A H 0.4367 -0.3793 -0.2956 0.635 Uiso 1 1 calc R B 1
H40B H 0.4293 -0.2427 -0.3040 0.635 Uiso 1 1 calc R B 1
C41 C 0.4927(13) -0.294(4) -0.1887(18) 0.466(15) Uani 1 1 d DU B .
H41A H 0.4929 -0.2200 -0.1642 0.560 Uiso 1 1 calc R . .
H41B H 0.4971 -0.3557 -0.1523 0.560 Uiso 1 1 calc R . .
C42 C 0.5401(13) -0.298(3) -0.2117(16) 0.459(14) Uani 1 1 d DU . .
H42A H 0.5485 -0.2215 -0.2248 0.551 Uiso 1 1 calc R B .
H42B H 0.5298 -0.3494 -0.2564 0.551 Uiso 1 1 calc R . .
C43 C 0.5918(15) -0.345(3) -0.136(2) 0.478(15) Uani 1 1 d DU B .
H43A H 0.6218 -0.3787 -0.1454 0.574 Uiso 1 1 calc R . .
H43B H 0.5796 -0.3997 -0.1084 0.574 Uiso 1 1 calc R . .
C44 C 0.6111(15) -0.229(3) -0.092(2) 0.452(16) Uani 1 1 d DU . .
H44A H 0.5845 -0.2011 -0.0735 0.542 Uiso 1 1 calc R B .
H44B H 0.6171 -0.1695 -0.1228 0.542 Uiso 1 1 calc R . .
C45 C 0.6699(14) -0.276(3) -0.0225(19) 0.389(13) Uani 1 1 d DU B .
H45A H 0.6635 -0.3359 0.0080 0.467 Uiso 1 1 calc R . .
H45B H 0.6959 -0.3050 -0.0414 0.467 Uiso 1 1 calc R . .
C46 C 0.6916(13) -0.167(3) 0.0230(19) 0.372(11) Uani 1 1 d DU . .
H46A H 0.6885 -0.1079 -0.0145 0.447 Uiso 1 1 calc R B .
H46B H 0.7330 -0.1779 0.0597 0.447 Uiso 1 1 calc R . .
C47 C 0.6629(11) -0.116(2) 0.0732(18) 0.344(11) Uani 1 1 d DU B .
H47A H 0.6206 -0.1132 0.0404 0.413 Uiso 1 1 calc R . .
H47B H 0.6722 -0.1655 0.1187 0.413 Uiso 1 1 calc R . .
C48 C 0.6853(15) -0.003(2) 0.100(2) 0.331(11) Uani 1 1 d DU . .
H48A H 0.6713 0.0535 0.0568 0.398 Uiso 1 1 calc R B .
H48B H 0.7278 -0.0004 0.1305 0.398 Uiso 1 1 calc R . .


_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
Ge01 C21 1.871(18) . ?
Ge01 C01 1.977(18) . ?
Ge01 C35 1.995(19) . ?
Ge01 C07 2.016(18) . ?
Ge02 C04 1.86(2) . ?
Ge02 C34 2.00(2) . ?
Ge02 C20 1.996(19) . ?
Ge02 C48 2.26(3) . ?
C01 C06 1.26(3) . ?
C01 C02 1.36(2) . ?
C02 C03 1.41(3) . ?
C02 H02 0.9300 . ?
C03 C04 1.41(3) . ?
C03 H03 0.9300 . ?
C04 C05 1.33(3) . ?
C05 C06 1.36(3) . ?
C05 H05 0.9300 . ?
C06 H06 0.9300 . ?
C07 C08 1.474(16) . ?
C07 H07A 0.9700 . ?
C07 H07B 0.9700 . ?
C08 C09 1.592(17) . ?
C08 H08A 0.9700 . ?
C08 H08B 0.9700 . ?
C09 C10 1.492(19) . ?
C09 H09A 0.9700 . ?
C09 H09B 0.9700 . ?
C10 C11 1.53(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.551(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.59(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.517(19) . ?
C13 C15 2.05(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.533(18) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.38(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.528(19) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.576(17) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.44(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.436(17) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.449(15) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.583(18) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.501(19) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.525(19) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.535(19) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.555(19) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.56(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.51(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.51(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.53(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.54(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.547(19) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.387(18) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.451(17) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.628(17) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C138 1.31(4) . ?
C37 C38 1.55(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.53(5) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.56(2) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C138 C139 1.54(5) . ?
C138 H13C 0.9700 . ?
C138 H13D 0.9700 . ?
C139 C40 1.41(6) . ?
C139 H13E 0.9700 . ?
C139 H13F 0.9700 . ?
C40 C41 1.533(19) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.500(19) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.526(19) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.532(19) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.562(19) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.480(18) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.591(17) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.427(16) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?

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
C21 Ge01 C01 109.0(8) . . ?
C21 Ge01 C35 103.2(9) . . ?
C01 Ge01 C35 111.2(8) . . ?
C21 Ge01 C07 115.5(8) . . ?
C01 Ge01 C07 108.0(6) . . ?
C35 Ge01 C07 109.8(9) . . ?
C04 Ge02 C34 108.8(9) . . ?
C04 Ge02 C20 112.0(8) . . ?
C34 Ge02 C20 103.4(11) . . ?
C04 Ge02 C48 114.0(11) . . ?
C34 Ge02 C48 125.9(13) . . ?
C20 Ge02 C48 89.8(10) . . ?
C06 C01 C02 119(2) . . ?
C06 C01 Ge01 121.0(16) . . ?
C02 C01 Ge01 120.1(15) . . ?
C01 C02 C03 117(2) . . ?
C01 C02 H02 121.7 . . ?
C03 C02 H02 121.7 . . ?
C04 C03 C02 128(2) . . ?
C04 C03 H03 116.2 . . ?
C02 C03 H03 116.2 . . ?
C05 C04 C03 105(2) . . ?
C05 C04 Ge02 129.1(18) . . ?
C03 C04 Ge02 125.9(16) . . ?
C04 C05 C06 131(2) . . ?
C04 C05 H05 114.5 . . ?
C06 C05 H05 114.6 . . ?
C01 C06 C05 121(2) . . ?
C01 C06 H06 119.7 . . ?
C05 C06 H06 119.7 . . ?
C08 C07 Ge01 106.5(12) . . ?
C08 C07 H07A 110.4 . . ?
Ge01 C07 H07A 110.4 . . ?
C08 C07 H07B 110.5 . . ?
Ge01 C07 H07B 110.4 . . ?
H07A C07 H07B 108.6 . . ?
C07 C08 C09 105.4(19) . . ?
C07 C08 H08A 110.7 . . ?
C09 C08 H08A 110.9 . . ?
C07 C08 H08B 110.6 . . ?
C09 C08 H08B 110.5 . . ?
H08A C08 H08B 108.8 . . ?
C10 C09 C08 108(2) . . ?
C10 C09 H09A 109.9 . . ?
C08 C09 H09A 109.9 . . ?
C10 C09 H09B 110.2 . . ?
C08 C09 H09B 110.3 . . ?
H09A C09 H09B 108.4 . . ?
C09 C10 C11 105(2) . . ?
C09 C10 H10A 110.9 . . ?
C11 C10 H10A 110.9 . . ?
C09 C10 H10B 110.7 . . ?
C11 C10 H10B 110.8 . . ?
H10A C10 H10B 108.9 . . ?
C10 C11 C12 93(2) . . ?
C10 C11 H11A 113.2 . . ?
C12 C11 H11A 113.3 . . ?
C10 C11 H11B 113.1 . . ?
C12 C11 H11B 113.0 . . ?
H11A C11 H11B 110.5 . . ?
C11 C12 C13 111(4) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C12 96(2) . . ?
C14 C13 C15 48.1(12) . . ?
C12 C13 C15 142(2) . . ?
C14 C13 H13A 112.6 . . ?
C12 C13 H13A 112.7 . . ?
C15 C13 H13A 79.9 . . ?
C14 C13 H13B 112.6 . . ?
C12 C13 H13B 112.6 . . ?
C15 C13 H13B 93.9 . . ?
H13A C13 H13B 110.1 . . ?
C13 C14 C15 84(2) . . ?
C13 C14 H14A 114.6 . . ?
C15 C14 H14A 114.6 . . ?
C13 C14 H14B 114.6 . . ?
C15 C14 H14B 114.6 . . ?
H14A C14 H14B 111.7 . . ?
C16 C15 C14 109(2) . . ?
C16 C15 C13 95(2) . . ?
C14 C15 C13 47.5(11) . . ?
C16 C15 H15A 109.9 . . ?
C14 C15 H15A 109.8 . . ?
C13 C15 H15A 151.7 . . ?
C16 C15 H15B 109.8 . . ?
C14 C15 H15B 109.9 . . ?
C13 C15 H15B 73.0 . . ?
H15A C15 H15B 108.3 . . ?
C15 C16 C17 103(2) . . ?
C15 C16 H16A 111.2 . . ?
C17 C16 H16A 110.9 . . ?
C15 C16 H16B 111.2 . . ?
C17 C16 H16B 111.3 . . ?
H16A C16 H16B 109.1 . . ?
C16 C17 C18 96(2) . . ?
C16 C17 H17A 112.3 . . ?
C18 C17 H17A 112.3 . . ?
C16 C17 H17B 112.7 . . ?
C18 C17 H17B 112.7 . . ?
H17A C17 H17B 110.0 . . ?
C19 C18 C17 125(3) . . ?
C19 C18 H18A 105.9 . . ?
C17 C18 H18A 105.9 . . ?
C19 C18 H18B 106.2 . . ?
C17 C18 H18B 106.3 . . ?
H18A C18 H18B 106.3 . . ?
C20 C19 C18 123(2) . . ?
C20 C19 H19A 106.6 . . ?
C18 C19 H19A 106.5 . . ?
C20 C19 H19B 106.7 . . ?
C18 C19 H19B 106.7 . . ?
H19A C19 H19B 106.6 . . ?
C19 C20 Ge02 124.4(17) . . ?
C19 C20 H20A 106.3 . . ?
Ge02 C20 H20A 106.2 . . ?
C19 C20 H20B 106.2 . . ?
Ge02 C20 H20B 106.2 . . ?
H20A C20 H20B 106.4 . . ?
C22 C21 Ge01 123.6(14) . . ?
C22 C21 H21A 106.4 . . ?
Ge01 C21 H21A 106.4 . . ?
C22 C21 H21B 106.5 . . ?
Ge01 C21 H21B 106.4 . . ?
H21A C21 H21B 106.5 . . ?
C21 C22 C23 99(2) . . ?
C21 C22 H22A 112.0 . . ?
C23 C22 H22A 111.9 . . ?
C21 C22 H22B 112.0 . . ?
C23 C22 H22B 112.0 . . ?
H22A C22 H22B 109.7 . . ?
C24 C23 C22 90.8(17) . . ?
C24 C23 H23A 113.5 . . ?
C22 C23 H23A 113.5 . . ?
C24 C23 H23B 113.5 . . ?
C22 C23 H23B 113.5 . . ?
H23A C23 H23B 110.8 . . ?
C23 C24 C25 154(3) . . ?
C23 C24 H24A 97.9 . . ?
C25 C24 H24A 97.9 . . ?
C23 C24 H24B 97.9 . . ?
C25 C24 H24B 98.0 . . ?
H24A C24 H24B 103.7 . . ?
C24 C25 C26 96(2) . . ?
C24 C25 H25A 112.5 . . ?
C26 C25 H25A 112.5 . . ?
C24 C25 H25B 112.5 . . ?
C26 C25 H25B 112.5 . . ?
H25A C25 H25B 110.0 . . ?
C25 C26 C27 119(3) . . ?
C25 C26 H26A 107.6 . . ?
C27 C26 H26A 107.5 . . ?
C25 C26 H26B 107.6 . . ?
C27 C26 H26B 107.6 . . ?
H26A C26 H26B 107.1 . . ?
C26 C27 C28 96.8(19) . . ?
C26 C27 H27A 112.3 . . ?
C28 C27 H27A 112.3 . . ?
C26 C27 H27B 112.4 . . ?
C28 C27 H27B 112.5 . . ?
H27A C27 H27B 109.9 . . ?
C29 C28 C27 94(2) . . ?
C29 C28 H28A 113.0 . . ?
C27 C28 H28A 113.0 . . ?
C29 C28 H28B 112.7 . . ?
C27 C28 H28B 112.8 . . ?
H28A C28 H28B 110.3 . . ?
C30 C29 C28 107(2) . . ?
C30 C29 H29A 110.4 . . ?
C28 C29 H29A 110.6 . . ?
C30 C29 H29B 110.3 . . ?
C28 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
C29 C30 C31 108(4) . . ?
C29 C30 H30A 109.9 . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30B 110.2 . . ?
C31 C30 H30B 110.3 . . ?
H30A C30 H30B 108.4 . . ?
C30 C31 C32 98(3) . . ?
C30 C31 H31A 111.9 . . ?
C32 C31 H31A 112.0 . . ?
C30 C31 H31B 112.5 . . ?
C32 C31 H31B 112.3 . . ?
H31A C31 H31B 109.8 . . ?
C31 C32 C33 108(3) . . ?
C31 C32 H32A 110.1 . . ?
C33 C32 H32A 110.0 . . ?
C31 C32 H32B 110.1 . . ?
C33 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?
C34 C33 C32 115(2) . . ?
C34 C33 H33A 108.5 . . ?
C32 C33 H33A 108.6 . . ?
C34 C33 H33B 108.7 . . ?
C32 C33 H33B 108.5 . . ?
H33A C33 H33B 107.6 . . ?
C33 C34 Ge02 124(2) . . ?
C33 C34 H34A 106.3 . . ?
Ge02 C34 H34A 106.3 . . ?
C33 C34 H34B 106.1 . . ?
Ge02 C34 H34B 106.2 . . ?
H34A C34 H34B 106.4 . . ?
C36 C35 Ge01 113.8(16) . . ?
C36 C35 H35A 108.9 . . ?
Ge01 C35 H35A 108.9 . . ?
C36 C35 H35B 108.7 . . ?
Ge01 C35 H35B 108.7 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 C37 110(2) . . ?
C35 C36 H36A 109.5 . . ?
C37 C36 H36A 109.6 . . ?
C35 C36 H36B 109.7 . . ?
C37 C36 H36B 109.7 . . ?
H36A C36 H36B 108.1 . . ?
C138 C37 C38 37(3) . . ?
C138 C37 C36 123(3) . . ?
C38 C37 C36 113(4) . . ?
C138 C37 H37A 72.7 . . ?
C38 C37 H37A 109.0 . . ?
C36 C37 H37A 109.1 . . ?
C138 C37 H37B 124.8 . . ?
C38 C37 H37B 108.8 . . ?
C36 C37 H37B 108.9 . . ?
H37A C37 H37B 107.8 . . ?
C39 C38 C37 103(3) . . ?
C39 C38 H38A 111.3 . . ?
C37 C38 H38A 111.2 . . ?
C39 C38 H38B 111.0 . . ?
C37 C38 H38B 111.1 . . ?
H38A C38 H38B 109.1 . . ?
C38 C39 C40 99(3) . . ?
C38 C39 H39A 111.9 . . ?
C40 C39 H39A 111.9 . . ?
C38 C39 H39B 112.1 . . ?
C40 C39 H39B 112.0 . . ?
H39A C39 H39B 109.6 . . ?
C37 C138 C139 122(4) . . ?
C37 C138 H13C 106.9 . . ?
C139 C138 H13C 106.9 . . ?
C37 C138 H13D 106.6 . . ?
C139 C138 H13D 106.6 . . ?
H13C C138 H13D 106.6 . . ?
C40 C139 C138 117(5) . . ?
C40 C139 H13E 108.2 . . ?
C138 C139 H13E 108.0 . . ?
C40 C139 H13F 108.1 . . ?
C138 C139 H13F 108.3 . . ?
H13E C139 H13F 107.3 . . ?
C139 C40 C41 88(3) . . ?
C139 C40 C39 42(4) . . ?
C41 C40 C39 97(3) . . ?
C139 C40 H40A 150.6 . . ?
C41 C40 H40A 112.5 . . ?
C39 C40 H40A 112.4 . . ?
C139 C40 H40B 78.4 . . ?
C41 C40 H40B 112.1 . . ?
C39 C40 H40B 112.4 . . ?
H40A C40 H40B 109.9 . . ?
C42 C41 C40 103(2) . . ?
C42 C41 H41A 111.2 . . ?
C40 C41 H41A 111.4 . . ?
C42 C41 H41B 111.2 . . ?
C40 C41 H41B 110.9 . . ?
H41A C41 H41B 109.1 . . ?
C41 C42 C43 102(2) . . ?
C41 C42 H42A 111.4 . . ?
C43 C42 H42A 111.5 . . ?
C41 C42 H42B 111.5 . . ?
C43 C42 H42B 111.3 . . ?
H42A C42 H42B 109.3 . . ?
C42 C43 C44 97(2) . . ?
C42 C43 H43A 112.4 . . ?
C44 C43 H43A 112.3 . . ?
C42 C43 H43B 112.4 . . ?
C44 C43 H43B 112.4 . . ?
H43A C43 H43B 109.9 . . ?
C43 C44 C45 95(2) . . ?
C43 C44 H44A 112.7 . . ?
C45 C44 H44A 112.7 . . ?
C43 C44 H44B 112.8 . . ?
C45 C44 H44B 112.8 . . ?
H44A C44 H44B 110.2 . . ?
C46 C45 C44 98(3) . . ?
C46 C45 H45A 112.2 . . ?
C44 C45 H45A 112.2 . . ?
C46 C45 H45B 112.1 . . ?
C44 C45 H45B 112.1 . . ?
H45A C45 H45B 109.8 . . ?
C45 C46 C47 121(2) . . ?
C45 C46 H46A 107.0 . . ?
C47 C46 H46A 107.0 . . ?
C45 C46 H46B 107.1 . . ?
C47 C46 H46B 107.0 . . ?
H46A C46 H46B 106.8 . . ?
C48 C47 C46 109(2) . . ?
C48 C47 H47A 109.8 . . ?
C46 C47 H47A 109.9 . . ?
C48 C47 H47B 109.9 . . ?
C46 C47 H47B 109.9 . . ?
H47A C47 H47B 108.3 . . ?
C47 C48 Ge02 93.5(17) . . ?
C47 C48 H48A 113.1 . . ?
Ge02 C48 H48A 113.0 . . ?
C47 C48 H48B 113.0 . . ?
Ge02 C48 H48B 113.0 . . ?
H48A C48 H48B 110.4 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.056
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_chemical_compound_source        no
_database_code_depnum_ccdc_archive 'CCDC 1026018'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_shelx

# start Validation Reply Form
_vrf_SHFSU01_I                   
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Due to many restraints
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         22 %     
RESPONSE: The data collection temperature was too high.
;
_vrf_PLAT080_I                   
;
PROBLEM: Maximum Shift/Error ............................       0.74       
RESPONSE:Due to many restraints
;
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact  H09B   ..  H11A    ..       1.54 Ang.  
RESPONSE: Due to many restraints
;
# end Validation Reply Form



_audit_creation_method           SHELXL-97
_chemical_name_systematic        GeMolecularGyrotop

_chemical_name_common            GeMolecularGyrotop
_chemical_melting_point          '244-245 deg. C'
_chemical_formula_moiety         'C48 H88 Ge2'
_chemical_formula_sum            'C48 H88 Ge2'
_chemical_formula_weight         810.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C c  '
_symmetry_space_group_name_Hall  'C -2yc '

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

_cell_length_a                   26.170(17)
_cell_length_b                   11.561(8)
_cell_length_c                   19.398(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.837(7)
_cell_angle_gamma                90.00
_cell_volume                     5141(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    340(2)
_cell_measurement_reflns_used    1127
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      15.39

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_T_max  0.7960
_exptl_absorpt_process_details   'SADABS  Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      340(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            11576
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         26.70
_reflns_number_total             7471
_reflns_number_gt                1610
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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)+(0.0957P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         7471
_refine_ls_number_parameters     526
_refine_ls_number_restraints     473
_refine_ls_R_factor_all          0.2226
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.2312
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_restrained_S_all      0.874
_refine_ls_shift/su_max          0.735
_refine_ls_shift/su_mean         0.202

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
Ge01 Ge 0.16456(7) 0.48796(18) 0.47264(9) 0.2408(12) Uani 1 1 d DU A .
Ge02 Ge 0.45744(7) 0.48888(18) 0.68096(8) 0.2363(11) Uani 1 1 d D A .
C01 C 0.2444(10) 0.4908(13) 0.5319(13) 0.183(6) Uani 1 1 d DU . .
C04 C 0.3702(8) 0.4901(11) 0.6215(11) 0.165(5) Uani 1 1 d DU . .
C02 C 0.2738(17) 0.507(2) 0.614(2) 0.180(8) Uani 0.50(2) 1 d PDU A 1
H02 H 0.2514 0.5185 0.6387 0.216 Uiso 0.50(2) 1 calc PR A 1
C03 C 0.3353(16) 0.508(2) 0.661(2) 0.163(7) Uani 0.50(2) 1 d PDU A 1
H03 H 0.3528 0.5201 0.7153 0.196 Uiso 0.50(2) 1 calc PR A 1
C05 C 0.3393(17) 0.479(3) 0.539(2) 0.165(8) Uani 0.50(2) 1 d PDU A 1
H05 H 0.3590 0.4725 0.5106 0.198 Uiso 0.50(2) 1 calc PR A 1
C06 C 0.2811(17) 0.479(3) 0.503(2) 0.160(8) Uani 0.50(2) 1 d PDU A 1
H06 H 0.2633 0.4683 0.4491 0.192 Uiso 0.50(2) 1 calc PR A 1
C102 C 0.280(2) 0.441(3) 0.598(3) 0.177(10) Uani 0.317(19) 1 d PDU A 2
H102 H 0.2607 0.4018 0.6202 0.212 Uiso 0.317(19) 1 calc PR A 2
C103 C 0.342(2) 0.432(4) 0.643(3) 0.170(10) Uani 0.317(19) 1 d PDU A 2
H103 H 0.3592 0.3838 0.6870 0.204 Uiso 0.317(19) 1 calc PR A 2
C105 C 0.343(2) 0.547(4) 0.539(3) 0.174(10) Uani 0.317(19) 1 d PDU A 2
H105 H 0.3642 0.5817 0.5186 0.208 Uiso 0.317(19) 1 calc PR A 2
C106 C 0.284(2) 0.540(4) 0.500(3) 0.177(10) Uani 0.317(19) 1 d PDU A 2
H106 H 0.2658 0.5672 0.4490 0.213 Uiso 0.317(19) 1 calc PR A 2
C202 C 0.277(3) 0.564(5) 0.585(3) 0.164(11) Uani 0.190(14) 1 d PDU A 3
H202 H 0.2560 0.6245 0.5909 0.196 Uiso 0.190(14) 1 calc PR A 3
C203 C 0.338(3) 0.570(5) 0.636(4) 0.169(13) Uani 0.190(14) 1 d PDU A 3
H203 H 0.3547 0.6248 0.6756 0.203 Uiso 0.190(14) 1 calc PR A 3
C205 C 0.340(3) 0.391(5) 0.571(4) 0.188(13) Uani 0.190(14) 1 d PDU A 3
H205 H 0.3607 0.3283 0.5670 0.225 Uiso 0.190(14) 1 calc PR A 3
C206 C 0.282(3) 0.392(5) 0.532(4) 0.183(13) Uani 0.190(14) 1 d PDU A 3
H206 H 0.2633 0.3273 0.5030 0.219 Uiso 0.190(14) 1 calc PR A 3
C07 C 0.1235(12) 0.5272(17) 0.5467(15) 0.315(10) Uani 1 1 d DU . .
H07A H 0.0812 0.5290 0.5164 0.378 Uiso 1 1 calc R A .
H07B H 0.1356 0.4737 0.5904 0.378 Uiso 1 1 calc R . .
C08 C 0.1479(14) 0.640(2) 0.572(2) 0.49(2) Uani 1 1 d DU A .
H08A H 0.1348 0.6955 0.5292 0.592 Uiso 1 1 calc R . .
H08B H 0.1902 0.6397 0.6020 0.592 Uiso 1 1 calc R . .
C09 C 0.1182(13) 0.660(2) 0.6257(16) 0.437(14) Uani 1 1 d DU . .
H09A H 0.0765 0.6461 0.5967 0.524 Uiso 1 1 calc R A .
H09B H 0.1355 0.6106 0.6720 0.524 Uiso 1 1 calc R . .
C10 C 0.1323(13) 0.788(2) 0.6474(17) 0.503(19) Uani 1 1 d DU A .
H10A H 0.1017 0.8285 0.6524 0.603 Uiso 1 1 calc R . .
H10B H 0.1418 0.8297 0.6116 0.603 Uiso 1 1 calc R . .
C11 C 0.1865(12) 0.763(4) 0.7280(16) 0.60(4) Uani 1 1 d DU . .
H11A H 0.1767 0.6883 0.7415 0.724 Uiso 1 1 calc R A .
H11B H 0.2160 0.7457 0.7128 0.724 Uiso 1 1 calc R . .
C12 C 0.2225(13) 0.818(4) 0.808(2) 0.56(2) Uani 1 1 d DU A .
H12A H 0.2183 0.7779 0.8494 0.667 Uiso 1 1 calc R . .
H12B H 0.2139 0.8995 0.8087 0.667 Uiso 1 1 calc R . .
C13 C 0.2827(11) 0.797(4) 0.8139(17) 0.522(16) Uani 1 1 d DU . .
H13A H 0.2835 0.7237 0.7897 0.626 Uiso 1 1 calc R A .
H13B H 0.2928 0.8587 0.7890 0.626 Uiso 1 1 calc R . .
C14 C 0.3238(15) 0.794(4) 0.9028(17) 0.557(15) Uani 1 1 d DU A .
H14A H 0.3252 0.7170 0.9233 0.668 Uiso 1 1 calc R . .
H14B H 0.3103 0.8473 0.9292 0.668 Uiso 1 1 calc R . .
C15 C 0.3846(14) 0.830(3) 0.917(2) 0.547(17) Uani 1 1 d DU . .
H15A H 0.3844 0.9073 0.8971 0.656 Uiso 1 1 calc R A .
H15B H 0.4134 0.8265 0.9723 0.656 Uiso 1 1 calc R . .
C16 C 0.3953(12) 0.739(4) 0.870(2) 0.53(2) Uani 1 1 d DU A .
H16A H 0.3795 0.6645 0.8731 0.633 Uiso 1 1 calc R . .
H16B H 0.3787 0.7610 0.8147 0.633 Uiso 1 1 calc R . .
C17 C 0.4608(13) 0.736(4) 0.9092(19) 0.53(2) Uani 1 1 d DU . .
H17A H 0.4742 0.8146 0.9247 0.631 Uiso 1 1 calc R A .
H17B H 0.4738 0.6919 0.9574 0.631 Uiso 1 1 calc R . .
C18 C 0.4927(13) 0.690(3) 0.870(2) 0.49(2) Uani 1 1 d DU A .
H18A H 0.5331 0.6809 0.9098 0.590 Uiso 1 1 calc R . .
H18B H 0.4920 0.7497 0.8341 0.590 Uiso 1 1 calc R . .
C19 C 0.4745(14) 0.576(2) 0.8224(16) 0.414(15) Uani 1 1 d DU . .
H19A H 0.4990 0.5115 0.8513 0.496 Uiso 1 1 calc R A .
H19B H 0.4338 0.5575 0.8031 0.496 Uiso 1 1 calc R . .
C20 C 0.4867(9) 0.6191(15) 0.7590(13) 0.348(12) Uani 1 1 d DU A .
H20A H 0.5281 0.6319 0.7789 0.417 Uiso 1 1 calc R . .
H20B H 0.4657 0.6902 0.7359 0.417 Uiso 1 1 calc R . .
C21 C 0.1386(11) 0.545(2) 0.3603(13) 0.361(11) Uani 1 1 d DU . .
H21A H 0.1528 0.4915 0.3346 0.433 Uiso 1 1 calc R A .
H21B H 0.0963 0.5449 0.3306 0.433 Uiso 1 1 calc R . .
C22 C 0.1600(13) 0.658(2) 0.3600(14) 0.406(13) Uani 1 1 d DU A .
H22A H 0.2023 0.6599 0.3862 0.487 Uiso 1 1 calc R . .
H22B H 0.1463 0.7138 0.3849 0.487 Uiso 1 1 calc R . .
C23 C 0.1323(13) 0.683(3) 0.2672(15) 0.508(16) Uani 1 1 d DU . .
H23A H 0.1349 0.6166 0.2380 0.609 Uiso 1 1 calc R A .
H23B H 0.0926 0.7114 0.2433 0.609 Uiso 1 1 calc R . .
C24 C 0.1778(15) 0.778(2) 0.281(2) 0.52(2) Uani 1 1 d DU A .
H24A H 0.2021 0.7967 0.3360 0.620 Uiso 1 1 calc R . .
H24B H 0.1602 0.8478 0.2509 0.620 Uiso 1 1 calc R . .
C25 C 0.2110(15) 0.707(3) 0.247(2) 0.56(2) Uani 1 1 d DU . .
H25A H 0.1857 0.6802 0.1934 0.667 Uiso 1 1 calc R A .
H25B H 0.2328 0.6429 0.2800 0.667 Uiso 1 1 calc R . .
C26 C 0.2509(15) 0.809(3) 0.250(2) 0.58(2) Uani 1 1 d DU A .
H26A H 0.2432 0.8330 0.1977 0.702 Uiso 1 1 calc R . .
H26B H 0.2482 0.8746 0.2787 0.702 Uiso 1 1 calc R . .
C27 C 0.3090(15) 0.745(3) 0.2944(18) 0.58(3) Uani 1 1 d DU . .
H27A H 0.3092 0.6954 0.3347 0.690 Uiso 1 1 calc R A .
H27B H 0.3170 0.6990 0.2589 0.690 Uiso 1 1 calc R . .
C28 C 0.3532(16) 0.842(2) 0.331(2) 0.54(2) Uani 1 1 d DU A .
H28A H 0.3493 0.8855 0.3707 0.644 Uiso 1 1 calc R . .
H28B H 0.3549 0.8934 0.2923 0.644 Uiso 1 1 calc R . .
C29 C 0.4014(16) 0.752(3) 0.3635(19) 0.517(19) Uani 1 1 d DU . .
H29A H 0.4248 0.7535 0.3371 0.621 Uiso 1 1 calc R A .
H29B H 0.3863 0.6746 0.3610 0.621 Uiso 1 1 calc R . .
C30 C 0.4357(16) 0.798(3) 0.4495(18) 0.53(2) Uani 1 1 d DU A .
H30A H 0.4481 0.8776 0.4536 0.640 Uiso 1 1 calc R . .
H30B H 0.4165 0.7835 0.4807 0.640 Uiso 1 1 calc R . .
C31 C 0.4837(15) 0.709(4) 0.4629(18) 0.66(3) Uani 1 1 d DU . .
H31A H 0.4667 0.6398 0.4317 0.797 Uiso 1 1 calc R A .
H31B H 0.5113 0.7415 0.4484 0.797 Uiso 1 1 calc R . .
C32 C 0.5138(13) 0.680(3) 0.5508(19) 0.547(17) Uani 1 1 d DU A .
H32A H 0.5374 0.7466 0.5782 0.657 Uiso 1 1 calc R . .
H32B H 0.5407 0.6171 0.5588 0.657 Uiso 1 1 calc R . .
C33 C 0.4789(14) 0.645(3) 0.595(2) 0.466(17) Uani 1 1 d DU . .
H33A H 0.4932 0.6881 0.6439 0.559 Uiso 1 1 calc R A .
H33B H 0.4377 0.6620 0.5625 0.559 Uiso 1 1 calc R . .
C34 C 0.4877(17) 0.520(3) 0.611(2) 0.466(17) Uani 1 1 d DU A .
H34A H 0.5288 0.5010 0.6356 0.559 Uiso 1 1 calc R . .
H34B H 0.4669 0.4762 0.5630 0.559 Uiso 1 1 calc R . .
C35 C 0.1443(9) 0.3190(14) 0.4478(16) 0.372(13) Uani 1 1 d DU . .
H35A H 0.1027 0.3219 0.4118 0.447 Uiso 1 1 calc R A .
H35B H 0.1619 0.3008 0.4151 0.447 Uiso 1 1 calc R . .
C36 C 0.1501(10) 0.216(2) 0.4872(16) 0.368(11) Uani 1 1 d DU A .
H36A H 0.1270 0.2253 0.5137 0.442 Uiso 1 1 calc R . .
H36B H 0.1905 0.2136 0.5284 0.442 Uiso 1 1 calc R . .
C37 C 0.1366(9) 0.092(2) 0.4527(18) 0.435(14) Uani 1 1 d DU . .
H37A H 0.1081 0.0521 0.4624 0.522 Uiso 1 1 calc R A .
H37B H 0.1255 0.0893 0.3973 0.522 Uiso 1 1 calc R . .
C38 C 0.1990(11) 0.0511(18) 0.506(2) 0.505(19) Uani 1 1 d DU A .
H38A H 0.2219 0.0658 0.4799 0.606 Uiso 1 1 calc R . .
H38B H 0.2156 0.0965 0.5540 0.606 Uiso 1 1 calc R . .
C39 C 0.2038(13) -0.071(2) 0.527(2) 0.51(2) Uani 1 1 d DU . .
H39A H 0.1693 -0.1148 0.4914 0.609 Uiso 1 1 calc R A .
H39B H 0.2122 -0.0833 0.5808 0.609 Uiso 1 1 calc R . .
C40 C 0.2565(14) -0.101(3) 0.5148(19) 0.493(17) Uani 1 1 d DU A .
H40A H 0.2482 -0.1676 0.4810 0.592 Uiso 1 1 calc R . .
H40B H 0.2658 -0.0358 0.4910 0.592 Uiso 1 1 calc R . .
C41 C 0.3075(13) -0.126(3) 0.5973(17) 0.505(19) Uani 1 1 d DU . .
H41A H 0.3035 -0.2006 0.6169 0.607 Uiso 1 1 calc R A .
H41B H 0.3116 -0.0661 0.6348 0.607 Uiso 1 1 calc R . .
C42 C 0.3589(13) -0.124(2) 0.578(2) 0.518(17) Uani 1 1 d DU A .
H42A H 0.3892 -0.1799 0.6084 0.622 Uiso 1 1 calc R . .
H42B H 0.3464 -0.1313 0.5226 0.622 Uiso 1 1 calc R . .
C43 C 0.3752(14) -0.002(2) 0.608(2) 0.55(2) Uani 1 1 d DU . .
H43A H 0.3454 0.0350 0.6168 0.658 Uiso 1 1 calc R A .
H43B H 0.3839 0.0453 0.5740 0.658 Uiso 1 1 calc R . .
C44 C 0.4302(15) -0.031(3) 0.6862(18) 0.518(18) Uani 1 1 d DU A .
H44A H 0.4374 -0.1133 0.6953 0.622 Uiso 1 1 calc R . .
H44B H 0.4314 0.0066 0.7316 0.622 Uiso 1 1 calc R . .
C45 C 0.4694(14) 0.029(2) 0.656(2) 0.478(16) Uani 1 1 d DU . .
H45A H 0.5030 -0.0174 0.6659 0.573 Uiso 1 1 calc R A .
H45B H 0.4478 0.0503 0.6013 0.573 Uiso 1 1 calc R . .
C46 C 0.4855(11) 0.1337(19) 0.7114(15) 0.388(13) Uani 1 1 d DU A .
H46A H 0.5275 0.1431 0.7373 0.466 Uiso 1 1 calc R . .
H46B H 0.4750 0.1167 0.7519 0.466 Uiso 1 1 calc R . .
C47 C 0.4564(11) 0.2534(17) 0.6717(13) 0.354(13) Uani 1 1 d DU . .
H47A H 0.4589 0.2674 0.6241 0.425 Uiso 1 1 calc R A .
H47B H 0.4159 0.2572 0.6597 0.425 Uiso 1 1 calc R . .
C48 C 0.4921(10) 0.332(2) 0.7331(13) 0.379(14) Uani 1 1 d DU A .
H48A H 0.5328 0.3251 0.7466 0.454 Uiso 1 1 calc R . .
H48B H 0.4883 0.3195 0.7799 0.454 Uiso 1 1 calc R . .


_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
Ge01 C01 1.84(2) . ?
Ge01 C35 2.020(15) . ?
Ge01 C21 2.05(2) . ?
Ge01 C07 2.22(2) . ?
Ge02 C34 1.903(19) . ?
Ge02 C04 2.001(19) . ?
Ge02 C20 2.006(18) . ?
Ge02 C48 2.06(2) . ?
C01 C202 1.28(6) . ?
C01 C102 1.30(4) . ?
C01 C06 1.33(4) . ?
C01 C02 1.41(4) . ?
C01 C206 1.50(6) . ?
C01 C106 1.55(6) . ?
C04 C103 1.22(4) . ?
C04 C203 1.37(6) . ?
C04 C05 1.40(4) . ?
C04 C03 1.47(4) . ?
C04 C205 1.47(5) . ?
C04 C105 1.54(5) . ?
C02 C03 1.42(4) . ?
C02 H02 0.9300 . ?
C03 H03 0.9300 . ?
C05 C06 1.33(3) . ?
C05 H05 0.9300 . ?
C06 H06 0.9300 . ?
C102 C103 1.42(4) . ?
C102 H102 0.9300 . ?
C103 H103 0.9300 . ?
C105 C106 1.34(3) . ?
C105 H105 0.9300 . ?
C106 H106 0.9300 . ?
C202 C203 1.42(4) . ?
C202 H202 0.9300 . ?
C203 H203 0.9300 . ?
C205 C206 1.33(3) . ?
C205 H205 0.9300 . ?
C206 H206 0.9300 . ?
C07 C08 1.436(16) . ?
C07 H07A 0.9700 . ?
C07 H07B 0.9700 . ?
C08 C09 1.585(17) . ?
C08 H08A 0.9700 . ?
C08 H08B 0.9700 . ?
C09 C10 1.542(18) . ?
C09 H09A 0.9700 . ?
C09 H09B 0.9700 . ?
C10 C11 1.551(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.519(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.548(19) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.531(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.536(18) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.513(19) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.502(18) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.478(19) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.539(18) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.495(18) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.430(17) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.610(19) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.552(19) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.556(19) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.554(19) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.527(19) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.516(19) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.519(19) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.557(19) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.544(19) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.531(19) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.580(19) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.470(18) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.385(16) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.55(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.525(17) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.462(19) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.542(19) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.538(19) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.558(17) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.505(18) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.54(2) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.560(19) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.533(18) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.588(17) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.428(16) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?

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
C01 Ge01 C35 104.8(8) . . ?
C01 Ge01 C21 110.7(10) . . ?
C35 Ge01 C21 98.1(10) . . ?
C01 Ge01 C07 110.6(10) . . ?
C35 Ge01 C07 101.5(9) . . ?
C21 Ge01 C07 127.4(11) . . ?
C34 Ge02 C04 109.8(14) . . ?
C34 Ge02 C20 104.7(12) . . ?
C04 Ge02 C20 110.1(8) . . ?
C34 Ge02 C48 106.4(12) . . ?
C04 Ge02 C48 113.5(7) . . ?
C20 Ge02 C48 111.9(10) . . ?
C202 C01 C102 68(3) . . ?
C202 C01 C06 94(3) . . ?
C102 C01 C06 92(3) . . ?
C202 C01 C02 38.3(18) . . ?
C102 C01 C02 37.6(18) . . ?
C06 C01 C02 112(3) . . ?
C202 C01 C206 108(4) . . ?
C102 C01 C206 60(3) . . ?
C06 C01 C206 47(2) . . ?
C02 C01 C206 96(3) . . ?
C202 C01 C106 76(3) . . ?
C102 C01 C106 104(3) . . ?
C06 C01 C106 27(2) . . ?
C02 C01 C106 107(3) . . ?
C206 C01 C106 73(3) . . ?
C202 C01 Ge01 129(3) . . ?
C102 C01 Ge01 132(3) . . ?
C06 C01 Ge01 125(2) . . ?
C02 C01 Ge01 123(2) . . ?
C206 C01 Ge01 122(3) . . ?
C106 C01 Ge01 123(2) . . ?
C103 C04 C203 76(4) . . ?
C103 C04 C05 103(3) . . ?
C203 C04 C05 102(3) . . ?
C103 C04 C03 42(2) . . ?
C203 C04 C03 36(2) . . ?
C05 C04 C03 117(3) . . ?
C103 C04 C205 65(3) . . ?
C203 C04 C205 118(4) . . ?
C05 C04 C205 49(2) . . ?
C03 C04 C205 101(3) . . ?
C103 C04 C105 122(3) . . ?
C203 C04 C105 84(4) . . ?
C05 C04 C105 30(2) . . ?
C03 C04 C105 113(3) . . ?
C205 C04 C105 79(3) . . ?
C103 C04 Ge02 121(3) . . ?
C203 C04 Ge02 122(3) . . ?
C05 C04 Ge02 121.8(19) . . ?
C03 C04 Ge02 121.7(19) . . ?
C205 C04 Ge02 118(3) . . ?
C105 C04 Ge02 116(2) . . ?
C01 C02 C03 124(3) . . ?
C01 C02 H02 117.8 . . ?
C03 C02 H02 117.9 . . ?
C02 C03 C04 117(3) . . ?
C02 C03 H03 121.2 . . ?
C04 C03 H03 121.5 . . ?
C06 C05 C04 119(3) . . ?
C06 C05 H05 120.6 . . ?
C04 C05 H05 120.5 . . ?
C05 C06 C01 131(3) . . ?
C05 C06 H06 114.7 . . ?
C01 C06 H06 114.5 . . ?
C01 C102 C103 135(4) . . ?
C01 C102 H102 112.6 . . ?
C103 C102 H102 112.4 . . ?
C04 C103 C102 116(4) . . ?
C04 C103 H103 121.5 . . ?
C102 C103 H103 122.1 . . ?
C106 C105 C04 113(4) . . ?
C106 C105 H105 123.0 . . ?
C04 C105 H105 123.7 . . ?
C105 C106 C01 127(4) . . ?
C105 C106 H106 116.7 . . ?
C01 C106 H106 116.2 . . ?
C01 C202 C203 133(6) . . ?
C01 C202 H202 113.3 . . ?
C203 C202 H202 113.9 . . ?
C04 C203 C202 115(5) . . ?
C04 C203 H203 122.6 . . ?
C202 C203 H203 122.3 . . ?
C206 C205 C04 118(5) . . ?
C206 C205 H205 121.2 . . ?
C04 C205 H205 120.9 . . ?
C205 C206 C01 126(5) . . ?
C205 C206 H206 117.0 . . ?
C01 C206 H206 117.4 . . ?
C08 C07 Ge01 97.7(16) . . ?
C08 C07 H07A 111.9 . . ?
Ge01 C07 H07A 111.9 . . ?
C08 C07 H07B 112.5 . . ?
Ge01 C07 H07B 112.5 . . ?
H07A C07 H07B 109.8 . . ?
C07 C08 C09 94.3(16) . . ?
C07 C08 H08A 113.3 . . ?
C09 C08 H08A 113.3 . . ?
C07 C08 H08B 112.6 . . ?
C09 C08 H08B 112.3 . . ?
H08A C08 H08B 110.4 . . ?
C10 C09 C08 100.8(18) . . ?
C10 C09 H09A 111.4 . . ?
C08 C09 H09A 111.0 . . ?
C10 C09 H09B 111.9 . . ?
C08 C09 H09B 112.1 . . ?
H09A C09 H09B 109.5 . . ?
C09 C10 C11 94.2(18) . . ?
C09 C10 H10A 113.1 . . ?
C11 C10 H10A 112.8 . . ?
C09 C10 H10B 112.8 . . ?
C11 C10 H10B 113.0 . . ?
H10A C10 H10B 110.2 . . ?
C12 C11 C10 140(4) . . ?
C12 C11 H11A 102.4 . . ?
C10 C11 H11A 102.1 . . ?
C12 C11 H11B 101.8 . . ?
C10 C11 H11B 101.7 . . ?
H11A C11 H11B 104.7 . . ?
C11 C12 C13 96.3(19) . . ?
C11 C12 H12A 112.0 . . ?
C13 C12 H12A 112.2 . . ?
C11 C12 H12B 113.0 . . ?
C13 C12 H12B 112.8 . . ?
H12A C12 H12B 110.0 . . ?
C14 C13 C12 103(2) . . ?
C14 C13 H13A 112.2 . . ?
C12 C13 H13A 111.5 . . ?
C14 C13 H13B 110.3 . . ?
C12 C13 H13B 111.0 . . ?
H13A C13 H13B 109.2 . . ?
C13 C14 C15 108(2) . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14A 110.1 . . ?
C13 C14 H14B 110.8 . . ?
C15 C14 H14B 110.6 . . ?
H14A C14 H14B 108.5 . . ?
C16 C15 C14 100(2) . . ?
C16 C15 H15A 112.2 . . ?
C14 C15 H15A 111.5 . . ?
C16 C15 H15B 111.5 . . ?
C14 C15 H15B 111.5 . . ?
H15A C15 H15B 109.4 . . ?
C17 C16 C15 102(2) . . ?
C17 C16 H16A 110.5 . . ?
C15 C16 H16A 112.2 . . ?
C17 C16 H16B 111.7 . . ?
C15 C16 H16B 111.2 . . ?
H16A C16 H16B 109.4 . . ?
C18 C17 C16 122(3) . . ?
C18 C17 H17A 106.2 . . ?
C16 C17 H17A 105.6 . . ?
C18 C17 H17B 108.0 . . ?
C16 C17 H17B 107.3 . . ?
H17A C17 H17B 106.6 . . ?
C17 C18 C19 122(3) . . ?
C17 C18 H18A 106.1 . . ?
C19 C18 H18A 106.5 . . ?
C17 C18 H18B 108.1 . . ?
C19 C18 H18B 106.8 . . ?
H18A C18 H18B 106.7 . . ?
C20 C19 C18 94.7(18) . . ?
C20 C19 H19A 113.0 . . ?
C18 C19 H19A 113.2 . . ?
C20 C19 H19B 112.7 . . ?
C18 C19 H19B 112.2 . . ?
H19A C19 H19B 110.3 . . ?
C19 C20 Ge02 102.6(14) . . ?
C19 C20 H20A 111.0 . . ?
Ge02 C20 H20A 111.3 . . ?
C19 C20 H20B 111.3 . . ?
Ge02 C20 H20B 111.4 . . ?
H20A C20 H20B 109.1 . . ?
C22 C21 Ge01 111.5(17) . . ?
C22 C21 H21A 109.2 . . ?
Ge01 C21 H21A 109.2 . . ?
C22 C21 H21B 109.8 . . ?
Ge01 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 C23 101.4(19) . . ?
C21 C22 H22A 112.0 . . ?
C23 C22 H22A 111.8 . . ?
C21 C22 H22B 111.3 . . ?
C23 C22 H22B 111.0 . . ?
H22A C22 H22B 109.3 . . ?
C24 C23 C22 92.2(18) . . ?
C24 C23 H23A 112.9 . . ?
C22 C23 H23A 112.9 . . ?
C24 C23 H23B 113.5 . . ?
C22 C23 H23B 113.7 . . ?
H23A C23 H23B 110.6 . . ?
C23 C24 C25 95.3(19) . . ?
C23 C24 H24A 112.4 . . ?
C25 C24 H24A 112.1 . . ?
C23 C24 H24B 112.6 . . ?
C25 C24 H24B 113.5 . . ?
H24A C24 H24B 110.2 . . ?
C24 C25 C26 95.0(19) . . ?
C24 C25 H25A 112.2 . . ?
C26 C25 H25A 112.1 . . ?
C24 C25 H25B 113.6 . . ?
C26 C25 H25B 113.0 . . ?
H25A C25 H25B 110.2 . . ?
C27 C26 C25 97.2(17) . . ?
C27 C26 H26A 112.2 . . ?
C25 C26 H26A 113.0 . . ?
C27 C26 H26B 112.4 . . ?
C25 C26 H26B 111.8 . . ?
H26A C26 H26B 109.9 . . ?
C28 C27 C26 104(2) . . ?
C28 C27 H27A 110.9 . . ?
C26 C27 H27A 110.8 . . ?
C28 C27 H27B 111.5 . . ?
C26 C27 H27B 111.0 . . ?
H27A C27 H27B 108.9 . . ?
C27 C28 C29 89(2) . . ?
C27 C28 H28A 114.3 . . ?
C29 C28 H28A 113.9 . . ?
C27 C28 H28B 113.7 . . ?
C29 C28 H28B 113.6 . . ?
H28A C28 H28B 111.0 . . ?
C28 C29 C30 99(2) . . ?
C28 C29 H29A 112.1 . . ?
C30 C29 H29A 111.9 . . ?
C28 C29 H29B 112.1 . . ?
C30 C29 H29B 112.1 . . ?
H29A C29 H29B 109.7 . . ?
C31 C30 C29 87.6(18) . . ?
C31 C30 H30A 114.3 . . ?
C29 C30 H30A 114.1 . . ?
C31 C30 H30B 113.8 . . ?
C29 C30 H30B 113.9 . . ?
H30A C30 H30B 111.3 . . ?
C32 C31 C30 106(2) . . ?
C32 C31 H31A 111.4 . . ?
C30 C31 H31A 110.5 . . ?
C32 C31 H31B 110.3 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.6 . . ?
C31 C32 C33 123(3) . . ?
C31 C32 H32A 107.5 . . ?
C33 C32 H32A 107.2 . . ?
C31 C32 H32B 105.8 . . ?
C33 C32 H32B 106.3 . . ?
H32A C32 H32B 106.6 . . ?
C34 C33 C32 107(3) . . ?
C34 C33 H33A 110.5 . . ?
C32 C33 H33A 109.8 . . ?
C34 C33 H33B 110.6 . . ?
C32 C33 H33B 110.3 . . ?
H33A C33 H33B 108.6 . . ?
C33 C34 Ge02 105.2(19) . . ?
C33 C34 H34A 110.9 . . ?
Ge02 C34 H34A 110.8 . . ?
C33 C34 H34B 110.7 . . ?
Ge02 C34 H34B 110.4 . . ?
H34A C34 H34B 108.8 . . ?
C36 C35 Ge01 139(2) . . ?
C36 C35 H35A 102.0 . . ?
Ge01 C35 H35A 102.4 . . ?
C36 C35 H35B 102.4 . . ?
Ge01 C35 H35B 102.5 . . ?
H35A C35 H35B 104.9 . . ?
C35 C36 C37 128(3) . . ?
C35 C36 H36A 105.2 . . ?
C37 C36 H36A 105.7 . . ?
C35 C36 H36B 104.7 . . ?
C37 C36 H36B 105.4 . . ?
H36A C36 H36B 106.0 . . ?
C38 C37 C36 92.7(14) . . ?
C38 C37 H37A 112.9 . . ?
C36 C37 H37A 112.7 . . ?
C38 C37 H37B 113.3 . . ?
C36 C37 H37B 113.8 . . ?
H37A C37 H37B 110.5 . . ?
C39 C38 C37 114(2) . . ?
C39 C38 H38A 109.7 . . ?
C37 C38 H38A 108.6 . . ?
C39 C38 H38B 107.7 . . ?
C37 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C38 C39 C40 98(2) . . ?
C38 C39 H39A 111.6 . . ?
C40 C39 H39A 111.2 . . ?
C38 C39 H39B 113.3 . . ?
C40 C39 H39B 112.7 . . ?
H39A C39 H39B 109.8 . . ?
C41 C40 C39 106(2) . . ?
C41 C40 H40A 110.3 . . ?
C39 C40 H40A 111.5 . . ?
C41 C40 H40B 110.2 . . ?
C39 C40 H40B 110.1 . . ?
H40A C40 H40B 108.7 . . ?
C40 C41 C42 99.5(14) . . ?
C40 C41 H41A 111.7 . . ?
C42 C41 H41A 112.8 . . ?
C40 C41 H41B 111.6 . . ?
C42 C41 H41B 111.3 . . ?
H41A C41 H41B 109.6 . . ?
C43 C42 C41 92.1(19) . . ?
C43 C42 H42A 112.9 . . ?
C41 C42 H42A 112.5 . . ?
C43 C42 H42B 114.1 . . ?
C41 C42 H42B 113.5 . . ?
H42A C42 H42B 110.7 . . ?
C42 C43 C44 98(2) . . ?
C42 C43 H43A 112.5 . . ?
C44 C43 H43A 112.6 . . ?
C42 C43 H43B 111.6 . . ?
C44 C43 H43B 112.3 . . ?
H43A C43 H43B 109.9 . . ?
C43 C44 C45 90.7(19) . . ?
C43 C44 H44A 113.8 . . ?
C45 C44 H44A 113.7 . . ?
C43 C44 H44B 113.1 . . ?
C45 C44 H44B 113.5 . . ?
H44A C44 H44B 110.8 . . ?
C46 C45 C44 95.9(19) . . ?
C46 C45 H45A 111.9 . . ?
C44 C45 H45A 112.4 . . ?
C46 C45 H45B 113.2 . . ?
C44 C45 H45B 112.8 . . ?
H45A C45 H45B 110.1 . . ?
C45 C46 C47 116(2) . . ?
C45 C46 H46A 108.7 . . ?
C47 C46 H46A 108.3 . . ?
C45 C46 H46B 107.9 . . ?
C47 C46 H46B 108.0 . . ?
H46A C46 H46B 107.2 . . ?
C48 C47 C46 100.4(19) . . ?
C48 C47 H47A 111.5 . . ?
C46 C47 H47A 111.7 . . ?
C48 C47 H47B 111.7 . . ?
C46 C47 H47B 111.9 . . ?
H47A C47 H47B 109.4 . . ?
C47 C48 Ge02 101.2(13) . . ?
C47 C48 H48A 111.7 . . ?
Ge02 C48 H48A 111.6 . . ?
C47 C48 H48B 111.5 . . ?
Ge02 C48 H48B 111.4 . . ?
H48A C48 H48B 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.094
_refine_diff_density_rms         0.040
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/tetrahydrofuran'
_chemical_compound_source        no
_database_code_depnum_ccdc_archive 'CCDC 1026019'
