Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Power, Philip'
'Phillips, Andrew D.'
'Stender, Matthias'

_publ_contact_author_name     	'Prof Philip Power'  
_publ_contact_author_address 
;
Department of Chemistry
University of California
One Shields Avenue
Davis
CA
95616
UNITED STATES OF AMERICA
;

_publ_contact_author_email       'PPPOWER@UCDAVIS.EDU'

_publ_section_title		
;
Formation of [Ar*Ge{CH2C(Me)C(Me)CH2}CH2C(Me)=]2 (Ar* =
C6H3-2,6-Trip2; Trip = C6H2-2,4,6-i-Pr3) via reaction of Ar*GeGeAr* with
2,3-dimethyl-1,3-butadiene:  Evidence for the existence of a germanium
anlogue of an alkyne
;

data_mas82 

_database_code_CSD	185422


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             '[Bert*Ge(C6H10)(mu-C6H10)]2' 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C90 H128 Ge2' 
_chemical_formula_weight          1355.19 

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    'P2(1)/c' 

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

_cell_length_a                    12.8612(8) 
_cell_length_b                    19.4797(12) 
_cell_length_c                    16.8275(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.8280(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      4035.3(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     90(2) 
_cell_measurement_reflns_used     5061 
_cell_measurement_theta_min       2.44 
_cell_measurement_theta_max       28.90 

_exptl_crystal_description        cube 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.27 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.24 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.115 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     0.787 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.8156 
_exptl_absorpt_correction_T_max   0.8336 
_exptl_absorpt_process_details     
;
SADABS: an empirical absorption program by G. M. Sheldrick
using the method described by Blessing, R. H.; Acta Cryst.
A51, 1995, 33.
; 
_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       90(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type  'Bruker SMART 1000' 
_diffrn_measurement_method        /w 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          '50 frames remeasured' 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         '<0.01'
_diffrn_reflns_number             25194 
_diffrn_reflns_av_R_equivalents   0.0556 
_diffrn_reflns_av_sigmaI/netI     0.0609 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -23 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.96 
_diffrn_reflns_theta_max          25.25 
_reflns_number_total              7285 
_reflns_number_gt                 5196 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL v. 5.10' 
_computing_structure_solution     'XS, Bruker SHELXTL v. 5.10' 
_computing_structure_refinement   'XL, Bruker SHELXTL v. 5.10' 
_computing_molecular_graphics     'XP, Bruker SHELXTL v. 5.10' 
_computing_publication_material   'XCIF, Bruker SHELXTL v. 5.10' 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger.
The structure shows some dissorder. One of the flanking Aryl groups is 
dissordered over 2 positions. One of the i-Pr groups of the other flanking 
Aryl shows the same type of dissorder. This was fixed using the PART statement.
The occupancy of the carbon atoms within the PART statement has been refined. 
The
carbon atoms have been refined isotropically because otherwise the thermal 
ellipsoids would overlap. The geometry of the dissordered Aryl group has been 
restraint using the SAME command. The was no more residual electron density 
left. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+11.6563P] where P=(Fo^2^+2Fc^2^)/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          7285 
_refine_ls_number_parameters      399 
_refine_ls_number_restraints      36 
_refine_ls_R_factor_all           0.0991 
_refine_ls_R_factor_gt            0.0671 
_refine_ls_wR_factor_ref          0.1770 
_refine_ls_wR_factor_gt           0.1581 
_refine_ls_goodness_of_fit_ref    1.038 
_refine_ls_restrained_S_all       1.059 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Ge1 Ge 0.47196(4) 0.60812(2) 0.64077(3) 0.02564(16) Uani 1 1 d . A . 
C37 C 0.5750(3) 0.5550(2) 0.5972(3) 0.0303(10) Uani 1 1 d . . . 
H37A H 0.6098 0.5860 0.5659 0.036 Uiso 1 1 calc R . . 
H37B H 0.6327 0.5355 0.6442 0.036 Uiso 1 1 calc R . . 
C38 C 0.5182(4) 0.4976(3) 0.5411(3) 0.0332(11) Uani 1 1 d . . . 
C39 C 0.5037(5) 0.4328(3) 0.5862(3) 0.0448(13) Uani 1 1 d . . . 
H39A H 0.4658 0.3983 0.5458 0.067 Uiso 1 1 calc R . . 
H39B H 0.4609 0.4431 0.6244 0.067 Uiso 1 1 calc R . . 
H39C H 0.5750 0.4151 0.6177 0.067 Uiso 1 1 calc R . . 
C40 C 0.3335(4) 0.6127(3) 0.5517(4) 0.0556(17) Uani 1 1 d . A . 
H40A H 0.2980 0.6578 0.5516 0.067 Uiso 1 1 calc R . . 
H40B H 0.3451 0.6051 0.4968 0.067 Uiso 1 1 calc R . . 
C41 C 0.2679(5) 0.5575(5) 0.5714(6) 0.084(3) Uani 1 1 d . . . 
C42 C 0.2980(6) 0.5292(3) 0.6453(7) 0.078(3) Uani 1 1 d . A . 
C43 C 0.4061(5) 0.5510(3) 0.7086(4) 0.0591(18) Uani 1 1 d . . . 
H43A H 0.4521 0.5107 0.7312 0.071 Uiso 1 1 calc R A . 
H43B H 0.3932 0.5775 0.7551 0.071 Uiso 1 1 calc R . . 
C44A C 0.1683(14) 0.5146(9) 0.5368(12) 0.056(5) Uiso 0.366(13) 1 d P A 1 
H44A H 0.1325 0.5285 0.4794 0.084 Uiso 0.366(13) 1 calc PR A 1 
H44B H 0.1182 0.5212 0.5704 0.084 Uiso 0.366(13) 1 calc PR A 1 
H44C H 0.1889 0.4661 0.5380 0.084 Uiso 0.366(13) 1 calc PR A 1 
C45A C 0.2751(13) 0.4603(8) 0.7124(10) 0.043(4) Uiso 0.366(13) 1 d P A 1 
H45A H 0.3280 0.4642 0.7674 0.065 Uiso 0.366(13) 1 calc PR A 1 
H45B H 0.2836 0.4157 0.6880 0.065 Uiso 0.366(13) 1 calc PR A 1 
H45C H 0.2014 0.4641 0.7178 0.065 Uiso 0.366(13) 1 calc PR A 1 
C44B C 0.1642(8) 0.5478(5) 0.4942(7) 0.056(3) Uiso 0.634(13) 1 d P A 2 
H44D H 0.1696 0.5781 0.4490 0.084 Uiso 0.634(13) 1 calc PR A 2 
H44E H 0.0989 0.5593 0.5101 0.084 Uiso 0.634(13) 1 calc PR A 2 
H44F H 0.1600 0.4999 0.4755 0.084 Uiso 0.634(13) 1 calc PR A 2 
C45B C 0.2246(8) 0.4788(5) 0.6648(6) 0.047(3) Uiso 0.634(13) 1 d P A 2 
H45D H 0.2563 0.4616 0.7214 0.071 Uiso 0.634(13) 1 calc PR A 2 
H45E H 0.2139 0.4406 0.6255 0.071 Uiso 0.634(13) 1 calc PR A 2 
H45F H 0.1545 0.5006 0.6606 0.071 Uiso 0.634(13) 1 calc PR A 2 
C1 C 0.5357(3) 0.6917(2) 0.7038(3) 0.0247(9) Uani 1 1 d . . . 
C2 C 0.4732(4) 0.7508(2) 0.7045(3) 0.0315(11) Uani 1 1 d . A . 
C3 C 0.5139(4) 0.8034(3) 0.7611(4) 0.0499(16) Uani 1 1 d . . . 
H3A H 0.4705 0.8429 0.7610 0.060 Uiso 1 1 calc R A . 
C4 C 0.6148(5) 0.7992(3) 0.8165(5) 0.070(2) Uani 1 1 d . A . 
H4A H 0.6404 0.8344 0.8564 0.084 Uiso 1 1 calc R . . 
C5 C 0.6793(4) 0.7433(3) 0.8138(4) 0.0583(18) Uani 1 1 d . . . 
H5A H 0.7506 0.7412 0.8511 0.070 Uiso 1 1 calc R A . 
C6 C 0.6425(4) 0.6898(3) 0.7581(3) 0.0327(11) Uani 1 1 d . A . 
C7 C 0.7247(4) 0.6349(3) 0.7565(3) 0.0312(11) Uani 1 1 d . . . 
C8 C 0.7917(3) 0.6431(3) 0.7044(3) 0.0321(11) Uani 1 1 d . A . 
C9 C 0.8755(4) 0.5961(3) 0.7096(3) 0.0401(12) Uani 1 1 d . . . 
H9A H 0.9205 0.6023 0.6743 0.048 Uiso 1 1 calc R A . 
C10 C 0.8959(4) 0.5414(3) 0.7633(3) 0.0439(13) Uani 1 1 d . A . 
C31 C 0.9900(5) 0.4928(4) 0.7670(4) 0.0620(18) Uani 1 1 d . . . 
H31A H 1.0240 0.5086 0.7237 0.074 Uiso 1 1 calc R A . 
C32 C 1.0761(5) 0.4962(4) 0.8480(5) 0.0645(19) Uani 1 1 d . A . 
H32A H 1.1351 0.4647 0.8472 0.097 Uiso 1 1 calc R . . 
H32B H 1.0453 0.4831 0.8927 0.097 Uiso 1 1 calc R . . 
H32C H 1.1044 0.5431 0.8574 0.097 Uiso 1 1 calc R . . 
C33 C 0.9535(6) 0.4218(4) 0.7455(5) 0.083(2) Uani 1 1 d . A . 
H33A H 1.0164 0.3926 0.7482 0.125 Uiso 1 1 calc R . . 
H33B H 0.9035 0.4206 0.6891 0.125 Uiso 1 1 calc R . . 
H33C H 0.9161 0.4049 0.7848 0.125 Uiso 1 1 calc R . . 
C11 C 0.8276(5) 0.5335(3) 0.8128(3) 0.0477(14) Uani 1 1 d . . . 
H11A H 0.8387 0.4953 0.8494 0.057 Uiso 1 1 calc R A . 
C12 C 0.7426(4) 0.5790(3) 0.8115(3) 0.0438(13) Uani 1 1 d . A . 
C13A C 0.3739(8) 0.7674(5) 0.6466(6) 0.028(3) Uiso 0.588(6) 1 d PD A 1 
C14A C 0.3796(8) 0.7990(5) 0.5732(5) 0.036(2) Uiso 0.588(6) 1 d PD A 1 
C15A C 0.2825(7) 0.8174(4) 0.5139(5) 0.033(2) Uiso 0.588(6) 1 d PD A 1 
H15A H 0.2859 0.8400 0.4647 0.040 Uiso 0.588(6) 1 calc PR A 1 
C16A C 0.1803(7) 0.8034(5) 0.5248(5) 0.037(2) Uiso 0.588(6) 1 d PD A 1 
C17A C 0.1780(6) 0.7749(5) 0.5989(5) 0.0312(19) Uiso 0.588(6) 1 d PD A 1 
H17A H 0.1098 0.7663 0.6084 0.037 Uiso 0.588(6) 1 calc PR A 1 
C18A C 0.2723(6) 0.7583(5) 0.6600(5) 0.027(2) Uiso 0.588(6) 1 d PD A 1 
C19A C 0.2651(7) 0.7306(5) 0.7422(5) 0.030(3) Uiso 0.588(6) 1 d PD A 1 
H19A H 0.3380 0.7123 0.7736 0.036 Uiso 0.588(6) 1 calc PR A 1 
C20A C 0.1806(6) 0.6719(4) 0.7315(5) 0.0251(18) Uiso 0.588(6) 1 d PD A 1 
H20A H 0.1801 0.6550 0.7863 0.038 Uiso 0.588(6) 1 calc PR A 1 
H20B H 0.2000 0.6343 0.6999 0.038 Uiso 0.588(6) 1 calc PR A 1 
H20C H 0.1083 0.6893 0.7018 0.038 Uiso 0.588(6) 1 calc PR A 1 
C21A C 0.2356(9) 0.7894(5) 0.7931(6) 0.039(3) Uiso 0.588(6) 1 d PD A 1 
H21A H 0.2306 0.7714 0.8463 0.058 Uiso 0.588(6) 1 calc PR A 1 
H21B H 0.1655 0.8092 0.7621 0.058 Uiso 0.588(6) 1 calc PR A 1 
H21C H 0.2918 0.8249 0.8033 0.058 Uiso 0.588(6) 1 calc PR A 1 
C22A C 0.0775(8) 0.8216(5) 0.4599(7) 0.061(3) Uiso 0.588(6) 1 d PD A 1 
H22A H 0.0981 0.8454 0.4140 0.073 Uiso 0.588(6) 1 calc PR A 1 
C23A C 0.0184(11) 0.7562(7) 0.4241(9) 0.080(4) Uiso 0.588(6) 1 d PD A 1 
H23A H -0.0458 0.7676 0.3781 0.120 Uiso 0.588(6) 1 calc PR A 1 
H23B H -0.0042 0.7319 0.4674 0.120 Uiso 0.588(6) 1 calc PR A 1 
H23C H 0.0670 0.7268 0.4038 0.120 Uiso 0.588(6) 1 calc PR A 1 
C24A C 0.0071(11) 0.8698(7) 0.4909(9) 0.081(4) Uiso 0.588(6) 1 d PD A 1 
H24A H -0.0521 0.8864 0.4439 0.122 Uiso 0.588(6) 1 calc PR A 1 
H24B H 0.0508 0.9088 0.5187 0.122 Uiso 0.588(6) 1 calc PR A 1 
H24C H -0.0232 0.8457 0.5302 0.122 Uiso 0.588(6) 1 calc PR A 1 
C25A C 0.4868(8) 0.8124(4) 0.5555(6) 0.041(2) Uiso 0.588(6) 1 d PD A 1 
H25A H 0.5533 0.8260 0.6004 0.049 Uiso 0.588(6) 1 calc PR A 1 
C26A C 0.4889(9) 0.7524(6) 0.4925(7) 0.048(3) Uiso 0.588(6) 1 d PD A 1 
H26A H 0.5456 0.7616 0.4656 0.072 Uiso 0.588(6) 1 calc PR A 1 
H26B H 0.4182 0.7496 0.4503 0.072 Uiso 0.588(6) 1 calc PR A 1 
H26C H 0.5042 0.7088 0.5227 0.072 Uiso 0.588(6) 1 calc PR A 1 
C27A C 0.4185(10) 0.8731(6) 0.4682(8) 0.074(4) Uiso 0.588(6) 1 d PD A 1 
H27A H 0.4713 0.8884 0.4401 0.111 Uiso 0.588(6) 1 calc PR A 1 
H27B H 0.3904 0.9130 0.4910 0.111 Uiso 0.588(6) 1 calc PR A 1 
H27C H 0.3583 0.8495 0.4284 0.111 Uiso 0.588(6) 1 calc PR A 1 
C13B C 0.3533(11) 0.7567(8) 0.6389(7) 0.025(4) Uiso 0.412(6) 1 d PD A 2 
C14B C 0.3401(10) 0.7863(6) 0.5575(7) 0.028(3) Uiso 0.412(6) 1 d PD A 2 
C15B C 0.2333(8) 0.7875(6) 0.5054(7) 0.030(3) Uiso 0.412(6) 1 d PD A 2 
H15B H 0.2210 0.8036 0.4502 0.036 Uiso 0.412(6) 1 calc PR A 2 
C16B C 0.1428(8) 0.7661(6) 0.5306(6) 0.034(3) Uiso 0.412(6) 1 d PD A 2 
C17B C 0.1615(8) 0.7426(6) 0.6103(6) 0.027(3) Uiso 0.412(6) 1 d PD A 2 
H17B H 0.1007 0.7293 0.6281 0.033 Uiso 0.412(6) 1 calc PR A 2 
C18B C 0.2650(8) 0.7370(7) 0.6671(6) 0.019(3) Uiso 0.412(6) 1 d PD A 2 
C19B C 0.2751(9) 0.7126(6) 0.7541(6) 0.016(3) Uiso 0.412(6) 1 d PD A 2 
H19B H 0.3522 0.6977 0.7788 0.019 Uiso 0.412(6) 1 calc PR A 2 
C20B C 0.2030(9) 0.6517(6) 0.7617(8) 0.030(3) Uiso 0.412(6) 1 d PD A 2 
H20D H 0.2156 0.6402 0.8205 0.044 Uiso 0.412(6) 1 calc PR A 2 
H20E H 0.2207 0.6120 0.7324 0.044 Uiso 0.412(6) 1 calc PR A 2 
H20F H 0.1265 0.6640 0.7373 0.044 Uiso 0.412(6) 1 calc PR A 2 
C21B C 0.2552(10) 0.7732(6) 0.8069(7) 0.019(3) Uiso 0.412(6) 1 d PD A 2 
H21D H 0.2633 0.7575 0.8636 0.028 Uiso 0.412(6) 1 calc PR A 2 
H21E H 0.1815 0.7910 0.7826 0.028 Uiso 0.412(6) 1 calc PR A 2 
H21F H 0.3081 0.8096 0.8078 0.028 Uiso 0.412(6) 1 calc PR A 2 
C22B C 0.0274(11) 0.7650(7) 0.4733(9) 0.050(4) Uiso 0.412(6) 1 d PD A 2 
H22B H -0.0239 0.7756 0.5064 0.060 Uiso 0.412(6) 1 calc PR A 2 
C23B C 0.0014(11) 0.6944(6) 0.4350(8) 0.044(3) Uiso 0.412(6) 1 d PD A 2 
H23D H 0.0122 0.6600 0.4792 0.066 Uiso 0.412(6) 1 calc PR A 2 
H23E H 0.0496 0.6843 0.4008 0.066 Uiso 0.412(6) 1 calc PR A 2 
H23F H -0.0743 0.6932 0.4003 0.066 Uiso 0.412(6) 1 calc PR A 2 
C24B C 0.0084(11) 0.8125(7) 0.4049(8) 0.047(3) Uiso 0.412(6) 1 d PD A 2 
H24D H 0.0226 0.8594 0.4263 0.070 Uiso 0.412(6) 1 calc PR A 2 
H24E H -0.0673 0.8088 0.3705 0.070 Uiso 0.412(6) 1 calc PR A 2 
H24F H 0.0569 0.8016 0.3712 0.070 Uiso 0.412(6) 1 calc PR A 2 
C25B C 0.4329(9) 0.8100(5) 0.5280(7) 0.028(3) Uiso 0.412(6) 1 d PD A 2 
H25B H 0.3853 0.8326 0.4769 0.034 Uiso 0.412(6) 1 calc PR A 2 
C26B C 0.5051(11) 0.7787(7) 0.4847(9) 0.039(3) Uiso 0.412(6) 1 d PD A 2 
H26D H 0.4944 0.7289 0.4820 0.059 Uiso 0.412(6) 1 calc PR A 2 
H26E H 0.5808 0.7891 0.5149 0.059 Uiso 0.412(6) 1 calc PR A 2 
H26F H 0.4884 0.7973 0.4283 0.059 Uiso 0.412(6) 1 calc PR A 2 
C27B C 0.5156(12) 0.8866(7) 0.5632(10) 0.056(4) Uiso 0.412(6) 1 d PD A 2 
H27D H 0.5035 0.9034 0.6146 0.084 Uiso 0.412(6) 1 calc PR A 2 
H27E H 0.4951 0.9222 0.5204 0.084 Uiso 0.412(6) 1 calc PR A 2 
H27F H 0.5925 0.8750 0.5733 0.084 Uiso 0.412(6) 1 calc PR A 2 
C28 C 0.7762(4) 0.7024(3) 0.6433(3) 0.0357(12) Uani 1 1 d . . . 
H28A H 0.6987 0.7173 0.6304 0.043 Uiso 1 1 calc R A . 
C29 C 0.7962(4) 0.6830(3) 0.5607(4) 0.0485(14) Uani 1 1 d . A . 
H29A H 0.7507 0.6435 0.5366 0.073 Uiso 1 1 calc R . . 
H29B H 0.8728 0.6710 0.5704 0.073 Uiso 1 1 calc R . . 
H29C H 0.7777 0.7219 0.5224 0.073 Uiso 1 1 calc R . . 
C30 C 0.8465(4) 0.7642(3) 0.6811(4) 0.0467(14) Uani 1 1 d . A . 
H30A H 0.8333 0.7766 0.7338 0.070 Uiso 1 1 calc R . . 
H30B H 0.8280 0.8032 0.6428 0.070 Uiso 1 1 calc R . . 
H30C H 0.9234 0.7525 0.6911 0.070 Uiso 1 1 calc R . . 
C34 C 0.6745(7) 0.5685(5) 0.8704(4) 0.093(3) Uani 1 1 d . . . 
H34A H 0.5996 0.5873 0.8467 0.112 Uiso 1 1 calc R A 1 
C35A C 0.6725(12) 0.5115(7) 0.9040(9) 0.053(4) Uiso 0.434(11) 1 d P A 1 
H35A H 0.6242 0.5139 0.9395 0.079 Uiso 0.434(11) 1 calc PR A 1 
H35B H 0.7460 0.4994 0.9378 0.079 Uiso 0.434(11) 1 calc PR A 1 
H35C H 0.6458 0.4765 0.8611 0.079 Uiso 0.434(11) 1 calc PR A 1 
C36A C 0.7576(11) 0.6245(7) 0.9563(8) 0.048(4) Uiso 0.434(11) 1 d P A 1 
H36A H 0.7628 0.6708 0.9348 0.071 Uiso 0.434(11) 1 calc PR A 1 
H36B H 0.8306 0.6051 0.9781 0.071 Uiso 0.434(11) 1 calc PR A 1 
H36C H 0.7227 0.6270 1.0009 0.071 Uiso 0.434(11) 1 calc PR A 1 
C35B C 0.6278(8) 0.4803(5) 0.8533(7) 0.048(3) Uiso 0.566(11) 1 d P A 2 
H35D H 0.5948 0.4725 0.7938 0.072 Uiso 0.566(11) 1 calc PR A 2 
H35E H 0.5739 0.4716 0.8830 0.072 Uiso 0.566(11) 1 calc PR A 2 
H35F H 0.6896 0.4491 0.8740 0.072 Uiso 0.566(11) 1 calc PR A 2 
C36B C 0.7177(10) 0.5726(7) 0.9560(8) 0.068(4) Uiso 0.566(11) 1 d P A 2 
H36D H 0.6605 0.5638 0.9824 0.103 Uiso 0.566(11) 1 calc PR A 2 
H36E H 0.7478 0.6186 0.9712 0.103 Uiso 0.566(11) 1 calc PR A 2 
H36F H 0.7754 0.5383 0.9747 0.103 Uiso 0.566(11) 1 calc PR A 2 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Ge1 0.0181(2) 0.0338(3) 0.0259(3) -0.0151(2) 0.00783(18) -0.0074(2) 
C37 0.018(2) 0.042(3) 0.030(3) -0.016(2) 0.007(2) -0.0044(19) 
C38 0.022(2) 0.042(3) 0.036(3) -0.017(2) 0.009(2) 0.000(2) 
C39 0.067(4) 0.039(3) 0.037(3) 0.001(2) 0.030(3) 0.007(3) 
C40 0.025(3) 0.087(4) 0.049(4) -0.044(3) 0.002(2) 0.005(3) 
C41 0.030(3) 0.104(6) 0.129(7) -0.091(6) 0.041(4) -0.032(4) 
C42 0.067(5) 0.053(4) 0.146(8) -0.069(5) 0.084(6) -0.047(4) 
C43 0.093(5) 0.036(3) 0.076(4) -0.022(3) 0.069(4) -0.020(3) 
C1 0.019(2) 0.033(2) 0.023(2) -0.0131(18) 0.0082(18) -0.0084(18) 
C2 0.029(3) 0.034(2) 0.040(3) -0.010(2) 0.023(2) -0.008(2) 
C3 0.038(3) 0.043(3) 0.081(4) -0.037(3) 0.037(3) -0.020(2) 
C4 0.039(3) 0.082(5) 0.100(5) -0.077(4) 0.038(4) -0.035(3) 
C5 0.027(3) 0.088(5) 0.061(4) -0.052(4) 0.014(3) -0.022(3) 
C6 0.023(2) 0.048(3) 0.027(3) -0.019(2) 0.007(2) -0.010(2) 
C7 0.020(2) 0.048(3) 0.020(2) -0.015(2) -0.0015(19) -0.008(2) 
C8 0.017(2) 0.044(3) 0.031(3) -0.014(2) 0.0001(19) -0.007(2) 
C9 0.024(2) 0.057(3) 0.036(3) -0.014(3) 0.003(2) -0.002(2) 
C10 0.035(3) 0.061(4) 0.029(3) -0.015(3) -0.001(2) 0.004(3) 
C31 0.056(4) 0.078(5) 0.051(4) -0.007(3) 0.013(3) 0.021(3) 
C32 0.033(3) 0.069(4) 0.090(5) -0.001(4) 0.016(3) 0.014(3) 
C33 0.060(4) 0.079(5) 0.103(6) -0.038(5) 0.012(4) 0.002(4) 
C11 0.051(3) 0.056(3) 0.025(3) -0.005(2) -0.007(3) 0.005(3) 
C12 0.034(3) 0.073(4) 0.019(3) -0.009(2) -0.001(2) -0.001(3) 
C28 0.016(2) 0.054(3) 0.038(3) -0.008(2) 0.010(2) -0.003(2) 
C29 0.039(3) 0.064(4) 0.050(3) -0.005(3) 0.025(3) -0.008(3) 
C30 0.032(3) 0.048(3) 0.060(4) -0.005(3) 0.012(3) -0.007(2) 
C34 0.088(6) 0.162(8) 0.039(4) 0.048(5) 0.032(4) 0.050(6) 

_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 C43 1.954(5) . ? 
Ge1 C40 1.970(5) . ? 
Ge1 C37 1.982(4) . ? 
Ge1 C1 1.986(4) . ? 
C37 C38 1.507(6) . ? 
C38 C38 1.329(10) 3_666 ? 
C38 C39 1.512(7) . ? 
C40 C41 1.461(11) . ? 
C41 C42 1.313(12) . ? 
C41 C44A 1.500(17) . ? 
C41 C44B 1.582(13) . ? 
C42 C45B 1.461(10) . ? 
C42 C43 1.546(11) . ? 
C42 C45A 1.831(17) . ? 
C1 C2 1.406(6) . ? 
C1 C6 1.413(6) . ? 
C2 C3 1.394(7) . ? 
C2 C13A 1.401(11) . ? 
C2 C13B 1.619(14) . ? 
C3 C4 1.365(9) . ? 
C4 C5 1.377(9) . ? 
C5 C6 1.390(7) . ? 
C6 C7 1.508(7) . ? 
C7 C12 1.403(8) . ? 
C7 C8 1.406(7) . ? 
C8 C9 1.398(7) . ? 
C8 C28 1.520(7) . ? 
C9 C10 1.372(8) . ? 
C10 C11 1.383(8) . ? 
C10 C31 1.525(8) . ? 
C31 C33 1.471(10) . ? 
C31 C32 1.488(9) . ? 
C11 C12 1.403(8) . ? 
C12 C34 1.515(8) . ? 
C13A C18A 1.400(11) . ? 
C13A C14A 1.401(10) . ? 
C14A C15A 1.400(12) . ? 
C14A C25A 1.516(12) . ? 
C15A C16A 1.406(11) . ? 
C16A C17A 1.373(11) . ? 
C16A C22A 1.494(12) . ? 
C17A C18A 1.383(10) . ? 
C18A C19A 1.511(11) . ? 
C19A C21A 1.542(11) . ? 
C19A C20A 1.553(10) . ? 
C22A C24A 1.499(14) . ? 
C22A C23A 1.515(15) . ? 
C25A C26A 1.583(11) . ? 
C25A C27A 1.892(13) . ? 
C13B C18B 1.405(13) . ? 
C13B C14B 1.450(12) . ? 
C14B C15B 1.400(14) . ? 
C14B C25B 1.493(13) . ? 
C15B C16B 1.412(14) . ? 
C16B C17B 1.371(13) . ? 
C16B C22B 1.518(14) . ? 
C17B C18B 1.400(12) . ? 
C18B C19B 1.508(13) . ? 
C19B C20B 1.534(12) . ? 
C19B C21B 1.543(12) . ? 
C22B C24B 1.443(16) . ? 
C22B C23B 1.514(16) . ? 
C25B C26B 1.468(12) . ? 
C25B C27B 1.827(14) . ? 
C28 C30 1.529(7) . ? 
C28 C29 1.532(7) . ? 
C34 C35A 1.250(15) . ? 
C34 C36B 1.387(14) . ? 
C34 C35B 1.816(14) . ? 
C34 C36A 1.878(16) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C43 Ge1 C40 91.2(3) . . ? 
C43 Ge1 C37 111.6(2) . . ? 
C40 Ge1 C37 107.2(2) . . ? 
C43 Ge1 C1 109.7(2) . . ? 
C40 Ge1 C1 120.8(2) . . ? 
C37 Ge1 C1 114.15(17) . . ? 
C38 C37 Ge1 111.4(3) . . ? 
C38 C38 C37 124.1(6) 3_666 . ? 
C38 C38 C39 121.5(6) 3_666 . ? 
C37 C38 C39 114.3(4) . . ? 
C41 C40 Ge1 104.4(5) . . ? 
C42 C41 C40 119.6(6) . . ? 
C42 C41 C44A 96.7(10) . . ? 
C40 C41 C44A 143.7(12) . . ? 
C42 C41 C44B 132.5(8) . . ? 
C40 C41 C44B 107.8(9) . . ? 
C44A C41 C44B 36.0(7) . . ? 
C41 C42 C45B 117.6(8) . . ? 
C41 C42 C43 119.7(6) . . ? 
C45B C42 C43 122.7(9) . . ? 
C41 C42 C45A 146.8(8) . . ? 
C45B C42 C45A 30.8(6) . . ? 
C43 C42 C45A 92.9(8) . . ? 
C42 C43 Ge1 102.1(5) . . ? 
C2 C1 C6 117.9(4) . . ? 
C2 C1 Ge1 121.8(3) . . ? 
C6 C1 Ge1 119.8(3) . . ? 
C3 C2 C13A 113.0(6) . . ? 
C3 C2 C1 120.3(5) . . ? 
C13A C2 C1 126.3(6) . . ? 
C3 C2 C13B 120.5(7) . . ? 
C13A C2 C13B 9.5(7) . . ? 
C1 C2 C13B 119.2(6) . . ? 
C4 C3 C2 121.1(5) . . ? 
C3 C4 C5 119.2(5) . . ? 
C4 C5 C6 121.6(5) . . ? 
C5 C6 C1 119.6(5) . . ? 
C5 C6 C7 116.1(4) . . ? 
C1 C6 C7 124.2(4) . . ? 
C12 C7 C8 119.1(5) . . ? 
C12 C7 C6 121.4(4) . . ? 
C8 C7 C6 119.3(5) . . ? 
C9 C8 C7 119.1(5) . . ? 
C9 C8 C28 119.2(4) . . ? 
C7 C8 C28 121.6(4) . . ? 
C10 C9 C8 123.2(5) . . ? 
C9 C10 C11 116.7(5) . . ? 
C9 C10 C31 120.5(5) . . ? 
C11 C10 C31 122.8(6) . . ? 
C33 C31 C32 111.6(6) . . ? 
C33 C31 C10 112.4(6) . . ? 
C32 C31 C10 112.3(5) . . ? 
C10 C11 C12 123.2(5) . . ? 
C7 C12 C11 118.7(5) . . ? 
C7 C12 C34 121.3(5) . . ? 
C11 C12 C34 120.0(6) . . ? 
C18A C13A C2 124.3(7) . . ? 
C18A C13A C14A 119.1(9) . . ? 
C2 C13A C14A 116.4(8) . . ? 
C15A C14A C13A 118.6(9) . . ? 
C15A C14A C25A 119.3(7) . . ? 
C13A C14A C25A 122.1(9) . . ? 
C14A C15A C16A 122.1(8) . . ? 
C17A C16A C15A 117.7(7) . . ? 
C17A C16A C22A 120.8(8) . . ? 
C15A C16A C22A 121.4(8) . . ? 
C16A C17A C18A 121.6(8) . . ? 
C17A C18A C13A 120.6(8) . . ? 
C17A C18A C19A 119.4(7) . . ? 
C13A C18A C19A 120.0(7) . . ? 
C18A C19A C21A 109.5(8) . . ? 
C18A C19A C20A 112.6(7) . . ? 
C21A C19A C20A 109.5(7) . . ? 
C16A C22A C24A 112.9(9) . . ? 
C16A C22A C23A 109.1(9) . . ? 
C24A C22A C23A 112.4(10) . . ? 
C14A C25A C26A 101.4(8) . . ? 
C14A C25A C27A 90.9(7) . . ? 
C26A C25A C27A 92.1(7) . . ? 
C18B C13B C14B 122.9(11) . . ? 
C18B C13B C2 117.0(8) . . ? 
C14B C13B C2 120.0(9) . . ? 
C15B C14B C13B 115.0(10) . . ? 
C15B C14B C25B 121.3(9) . . ? 
C13B C14B C25B 123.5(11) . . ? 
C14B C15B C16B 123.5(10) . . ? 
C17B C16B C15B 117.7(10) . . ? 
C17B C16B C22B 118.6(10) . . ? 
C15B C16B C22B 123.6(10) . . ? 
C16B C17B C18B 123.9(10) . . ? 
C17B C18B C13B 116.7(10) . . ? 
C17B C18B C19B 119.0(9) . . ? 
C13B C18B C19B 124.2(9) . . ? 
C18B C19B C20B 116.2(9) . . ? 
C18B C19B C21B 109.6(10) . . ? 
C20B C19B C21B 109.7(8) . . ? 
C24B C22B C23B 106.1(11) . . ? 
C24B C22B C16B 114.0(11) . . ? 
C23B C22B C16B 109.7(11) . . ? 
C26B C25B C14B 135.9(10) . . ? 
C26B C25B C27B 96.1(9) . . ? 
C14B C25B C27B 126.2(9) . . ? 
C8 C28 C30 111.8(4) . . ? 
C8 C28 C29 113.7(4) . . ? 
C30 C28 C29 109.8(4) . . ? 
C35A C34 C36B 68.7(9) . . ? 
C35A C34 C12 120.5(10) . . ? 
C36B C34 C12 122.5(9) . . ? 
C35A C34 C35B 35.0(8) . . ? 
C36B C34 C35B 103.5(8) . . ? 
C12 C34 C35B 104.6(6) . . ? 
C35A C34 C36A 104.5(9) . . ? 
C36B C34 C36A 36.9(7) . . ? 
C12 C34 C36A 96.7(7) . . ? 
C35B C34 C36A 139.5(7) . . ? 

_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              25.25 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.027 
_refine_diff_density_min   -0.533 
_refine_diff_density_rms    0.089