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

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

data_Eind2Ge2Br2
_database_code_depnum_ccdc_archive 'CCDC 1542495'
_audit_update_record             
;
2017-04-06 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

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

_chemical_formula_sum            'C56 H90 Br2 Ge2'
_chemical_formula_moiety         'C56 H90 Br2 Ge2'
_chemical_formula_weight         1068.32
_chemical_melting_point          423-425

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.43530(14)
_cell_length_b                   10.52080(14)
_cell_length_c                   12.12440(14)
_cell_angle_alpha                97.1732(10)
_cell_angle_beta                 93.3651(10)
_cell_angle_gamma                97.2483(11)
_cell_volume                     1306.38(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    35324
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      32.79
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.058
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560.00
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.3b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.854

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

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            79445
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.037
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             7611
_reflns_number_gt                6867
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0616
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7611
_refine_ls_number_parameters     279
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0290P)²+1.1579P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.003
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Br Br -0.2901 2.4595
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ge Ge 0.1547 1.8001
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

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

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.25189(2) 1.06428(2) 1.12346(2) 0.01765(4) Uani 1 1 d . . . . .
Ge1 Ge 0.09733(2) 0.95181(2) 0.98341(2) 0.01022(4) Uani 1 1 d . . . . .
C1 C 0.18209(12) 0.93932(12) 0.84102(11) 0.0087(2) Uani 1 1 d . . . . .
C2 C 0.20618(13) 1.03636(12) 0.77064(11) 0.0086(2) Uani 1 1 d . . . . .
C3 C 0.16401(13) 1.17164(12) 0.77809(11) 0.0091(2) Uani 1 1 d . . . . .
C4 C 0.23637(13) 1.23206(13) 0.68438(11) 0.0109(2) Uani 1 1 d . . . . .
H4A H 0.1783 1.2804 0.6432 0.013 Uiso 1 1 calc R U . . .
H4B H 0.3131 1.2930 0.7174 0.013 Uiso 1 1 calc R U . . .
C5 C 0.27920(13) 1.12166(13) 0.60391(11) 0.0095(2) Uani 1 1 d . . . . .
C6 C 0.26940(13) 1.01070(12) 0.67322(11) 0.0091(2) Uani 1 1 d . . . . .
C7 C 0.31202(13) 0.89192(13) 0.64392(11) 0.0101(2) Uani 1 1 d . . . . .
H7 H 0.3563 0.8765 0.5783 0.012 Uiso 1 1 calc R U . . .
C8 C 0.28873(13) 0.79607(12) 0.71228(11) 0.0090(2) Uani 1 1 d . . . . .
C9 C 0.33722(13) 0.66550(12) 0.69745(11) 0.0093(2) Uani 1 1 d . . . . .
C10 C 0.26189(13) 0.59410(13) 0.78274(11) 0.0105(2) Uani 1 1 d . . . . .
H10A H 0.3195 0.5437 0.8220 0.013 Uiso 1 1 calc R U . . .
H10B H 0.1882 0.5335 0.7437 0.013 Uiso 1 1 calc R U . . .
C11 C 0.21088(13) 0.69579(12) 0.86854(11) 0.0089(2) Uani 1 1 d . . . . .
C12 C 0.22262(12) 0.81717(12) 0.80870(11) 0.0086(2) Uani 1 1 d . . . . .
C13 C 0.01539(13) 1.15398(13) 0.74948(12) 0.0120(2) Uani 1 1 d . . . . .
H13A H -0.0032 1.1059 0.6735 0.014 Uiso 1 1 calc R U . . .
H13B H -0.0264 1.0994 0.8017 0.014 Uiso 1 1 calc R U . . .
C14 C -0.04832(15) 1.27753(15) 0.75394(14) 0.0194(3) Uani 1 1 d . . . . .
H14A H -0.1405 1.2554 0.7293 0.023 Uiso 1 1 calc R U . . .
H14B H -0.0062 1.3344 0.7048 0.023 Uiso 1 1 calc R U . . .
H14C H -0.0391 1.3220 0.8306 0.023 Uiso 1 1 calc R U . . .
C15 C 0.20156(13) 1.25516(13) 0.89219(11) 0.0113(2) Uani 1 1 d . . . . .
H15A H 0.1769 1.3423 0.8880 0.014 Uiso 1 1 calc R U . . .
H15B H 0.1505 1.2165 0.9489 0.014 Uiso 1 1 calc R U . . .
C16 C 0.34547(14) 1.26955(14) 0.93130(12) 0.0153(3) Uani 1 1 d . . . . .
H16A H 0.3746 1.1841 0.9247 0.018 Uiso 1 1 calc R U . . .
H16B H 0.3582 1.3095 1.0093 0.018 Uiso 1 1 calc R U . . .
H16C H 0.3957 1.3242 0.8850 0.018 Uiso 1 1 calc R U . . .
C17 C 0.18455(14) 1.08095(14) 0.49859(12) 0.0137(3) Uani 1 1 d . . . . .
H17A H 0.2147 1.0068 0.4536 0.016 Uiso 1 1 calc R U . . .
H17B H 0.0984 1.0501 0.5227 0.016 Uiso 1 1 calc R U . . .
C18 C 0.16793(18) 1.18467(17) 0.42317(14) 0.0233(3) Uani 1 1 d . . . . .
H18A H 0.2518 1.2146 0.3964 0.028 Uiso 1 1 calc R U . . .
H18B H 0.1347 1.2576 0.4653 0.028 Uiso 1 1 calc R U . . .
H18C H 0.1066 1.1483 0.3594 0.028 Uiso 1 1 calc R U . . .
C19 C 0.41722(14) 1.15718(14) 0.56734(12) 0.0130(2) Uani 1 1 d . . . . .
H19A H 0.4333 1.0897 0.5071 0.016 Uiso 1 1 calc R U . . .
H19B H 0.4203 1.2396 0.5355 0.016 Uiso 1 1 calc R U . . .
C20 C 0.52712(15) 1.17161(16) 0.65878(13) 0.0192(3) Uani 1 1 d . . . . .
H20A H 0.5292 1.0891 0.6880 0.023 Uiso 1 1 calc R U . . .
H20B H 0.5129 1.2382 0.7192 0.023 Uiso 1 1 calc R U . . .
H20C H 0.6098 1.1968 0.6279 0.023 Uiso 1 1 calc R U . . .
C21 C 0.31213(14) 0.59486(14) 0.57702(12) 0.0139(3) Uani 1 1 d . . . . .
H21A H 0.3706 0.6408 0.5291 0.017 Uiso 1 1 calc R U . . .
H21B H 0.3361 0.5067 0.5764 0.017 Uiso 1 1 calc R U . . .
C22 C 0.17359(17) 0.58338(17) 0.52495(14) 0.0224(3) Uani 1 1 d . . . . .
H22A H 0.1469 0.6697 0.5276 0.027 Uiso 1 1 calc R U . . .
H22B H 0.1154 0.5300 0.5666 0.027 Uiso 1 1 calc R U . . .
H22C H 0.1696 0.5431 0.4472 0.027 Uiso 1 1 calc R U . . .
C23 C 0.48531(13) 0.68920(14) 0.72959(12) 0.0138(3) Uani 1 1 d . . . . .
H23A H 0.5261 0.7496 0.6814 0.017 Uiso 1 1 calc R U . . .
H23B H 0.4999 0.7327 0.8074 0.017 Uiso 1 1 calc R U . . .
C24 C 0.55485(16) 0.56917(17) 0.72042(16) 0.0229(3) Uani 1 1 d . . . . .
H24A H 0.5513 0.5312 0.6421 0.028 Uiso 1 1 calc R U . . .
H24B H 0.5123 0.5058 0.7639 0.028 Uiso 1 1 calc R U . . .
H24C H 0.6455 0.5936 0.7493 0.028 Uiso 1 1 calc R U . . .
C25 C 0.07086(13) 0.64479(13) 0.89328(12) 0.0125(2) Uani 1 1 d . . . . .
H25A H 0.0692 0.5547 0.9094 0.015 Uiso 1 1 calc R U . . .
H25B H 0.0489 0.6971 0.9615 0.015 Uiso 1 1 calc R U . . .
C26 C -0.03412(14) 0.64700(15) 0.80084(14) 0.0184(3) Uani 1 1 d . . . . .
H26A H -0.0088 0.6046 0.7303 0.022 Uiso 1 1 calc R U . . .
H26B H -0.0450 0.7368 0.7933 0.022 Uiso 1 1 calc R U . . .
H26C H -0.1160 0.6011 0.8194 0.022 Uiso 1 1 calc R U . . .
C27 C 0.29769(14) 0.72422(13) 0.97927(12) 0.0128(2) Uani 1 1 d . . . . .
H27A H 0.3867 0.7566 0.9623 0.015 Uiso 1 1 calc R U . . .
H27B H 0.2656 0.7946 1.0276 0.015 Uiso 1 1 calc R U . . .
C28 C 0.30454(16) 0.61012(15) 1.04504(13) 0.0181(3) Uani 1 1 d . . . . .
H28A H 0.3450 0.5432 1.0016 0.022 Uiso 1 1 calc R U . . .
H28B H 0.2168 0.5745 1.0599 0.022 Uiso 1 1 calc R U . . .
H28C H 0.3562 0.6395 1.1158 0.022 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_molecular_graphics    'CrystalStructure 4.2.1'

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

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ge1 2.3622(2) . ?
Ge1 C1 1.9830(13) . ?
Ge1 Ge1 2.4145(3) 2_577 ?
C1 C2 1.4183(17) . ?
C1 C12 1.4195(18) . ?
C2 C6 1.4001(18) . ?
C2 C3 1.5356(18) . ?
C3 C15 1.5444(19) . ?
C3 C13 1.5518(19) . ?
C3 C4 1.5572(18) . ?
C4 C5 1.5492(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5180(18) . ?
C5 C19 1.5463(19) . ?
C5 C17 1.549(2) . ?
C6 C7 1.3906(18) . ?
C7 C8 1.3905(18) . ?
C7 H7 0.9500 . ?
C8 C12 1.4002(18) . ?
C8 C9 1.5165(18) . ?
C9 C21 1.5453(19) . ?
C9 C10 1.5466(18) . ?
C9 C23 1.5524(19) . ?
C10 C11 1.5624(18) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.5408(18) . ?
C11 C27 1.5496(19) . ?
C11 C25 1.5513(19) . ?
C13 C14 1.530(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.531(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.528(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.527(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.527(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.529(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.525(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.528(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ge1 Br1 107.48(4) . . ?
C1 Ge1 Ge1 125.38(4) . 2_577 ?
Br1 Ge1 Ge1 104.276(9) . 2_577 ?
C2 C1 C12 118.00(11) . . ?
C2 C1 Ge1 127.90(10) . . ?
C12 C1 Ge1 114.10(9) . . ?
C6 C2 C1 120.04(12) . . ?
C6 C2 C3 110.01(11) . . ?
C1 C2 C3 129.79(12) . . ?
C2 C3 C15 113.86(11) . . ?
C2 C3 C13 107.53(11) . . ?
C15 C3 C13 111.17(11) . . ?
C2 C3 C4 102.83(10) . . ?
C15 C3 C4 110.77(11) . . ?
C13 C3 C4 110.34(11) . . ?
C5 C4 C3 108.57(10) . . ?
C5 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C5 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 C19 112.99(11) . . ?
C6 C5 C17 107.92(11) . . ?
C19 C5 C17 108.86(11) . . ?
C6 C5 C4 102.10(10) . . ?
C19 C5 C4 112.27(11) . . ?
C17 C5 C4 112.57(11) . . ?
C7 C6 C2 121.52(12) . . ?
C7 C6 C5 125.29(12) . . ?
C2 C6 C5 113.13(11) . . ?
C8 C7 C6 118.88(12) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C12 121.12(12) . . ?
C7 C8 C9 125.61(12) . . ?
C12 C8 C9 113.14(11) . . ?
C8 C9 C21 113.29(11) . . ?
C8 C9 C10 101.85(10) . . ?
C21 C9 C10 113.08(11) . . ?
C8 C9 C23 107.26(11) . . ?
C21 C9 C23 109.12(11) . . ?
C10 C9 C23 112.01(11) . . ?
C9 C10 C11 108.98(10) . . ?
C9 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 C27 109.31(11) . . ?
C12 C11 C25 114.71(11) . . ?
C27 C11 C25 109.11(11) . . ?
C12 C11 C10 102.39(10) . . ?
C27 C11 C10 111.84(11) . . ?
C25 C11 C10 109.40(11) . . ?
C8 C12 C1 120.38(12) . . ?
C8 C12 C11 110.22(11) . . ?
C1 C12 C11 129.34(11) . . ?
C14 C13 C3 116.49(12) . . ?
C14 C13 H13A 108.2 . . ?
C3 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
C3 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C3 114.82(11) . . ?
C16 C15 H15A 108.6 . . ?
C3 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C3 C15 H15B 108.6 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C5 116.54(12) . . ?
C18 C17 H17A 108.2 . . ?
C5 C17 H17A 108.2 . . ?
C18 C17 H17B 108.2 . . ?
C5 C17 H17B 108.2 . . ?
H17A C17 H17B 107.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C5 115.81(12) . . ?
C20 C19 H19A 108.3 . . ?
C5 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C5 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C9 116.04(12) . . ?
C22 C21 H21A 108.3 . . ?
C9 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
C9 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C9 116.11(12) . . ?
C24 C23 H23A 108.3 . . ?
C9 C23 H23A 108.3 . . ?
C24 C23 H23B 108.3 . . ?
C9 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C11 115.79(12) . . ?
C26 C25 H25A 108.3 . . ?
C11 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C11 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C11 115.89(12) . . ?
C28 C27 H27A 108.3 . . ?
C11 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
C11 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C1 C2 C6 -0.64(19) . . . . ?
Ge1 C1 C2 C6 179.07(10) . . . . ?
C12 C1 C2 C3 174.18(13) . . . . ?
Ge1 C1 C2 C3 -6.1(2) . . . . ?
C6 C2 C3 C15 -131.18(12) . . . . ?
C1 C2 C3 C15 53.59(18) . . . . ?
C6 C2 C3 C13 105.18(12) . . . . ?
C1 C2 C3 C13 -70.04(17) . . . . ?
C6 C2 C3 C4 -11.29(14) . . . . ?
C1 C2 C3 C4 173.49(13) . . . . ?
C2 C3 C4 C5 17.94(14) . . . . ?
C15 C3 C4 C5 139.95(11) . . . . ?
C13 C3 C4 C5 -96.51(13) . . . . ?
C3 C4 C5 C6 -17.58(13) . . . . ?
C3 C4 C5 C19 -138.86(11) . . . . ?
C3 C4 C5 C17 97.88(13) . . . . ?
C1 C2 C6 C7 -1.2(2) . . . . ?
C3 C2 C6 C7 -176.96(12) . . . . ?
C1 C2 C6 C5 176.11(12) . . . . ?
C3 C2 C6 C5 0.35(16) . . . . ?
C19 C5 C6 C7 -51.25(18) . . . . ?
C17 C5 C6 C7 69.16(17) . . . . ?
C4 C5 C6 C7 -172.03(13) . . . . ?
C19 C5 C6 C2 131.56(12) . . . . ?
C17 C5 C6 C2 -108.03(13) . . . . ?
C4 C5 C6 C2 10.78(15) . . . . ?
C2 C6 C7 C8 1.3(2) . . . . ?
C5 C6 C7 C8 -175.71(12) . . . . ?
C6 C7 C8 C12 0.5(2) . . . . ?
C6 C7 C8 C9 -175.08(13) . . . . ?
C7 C8 C9 C21 -48.52(18) . . . . ?
C12 C8 C9 C21 135.56(12) . . . . ?
C7 C8 C9 C10 -170.27(13) . . . . ?
C12 C8 C9 C10 13.81(15) . . . . ?
C7 C8 C9 C23 71.95(16) . . . . ?
C12 C8 C9 C23 -103.97(13) . . . . ?
C8 C9 C10 C11 -18.55(13) . . . . ?
C21 C9 C10 C11 -140.45(11) . . . . ?
C23 C9 C10 C11 95.76(13) . . . . ?
C9 C10 C11 C12 16.76(13) . . . . ?
C9 C10 C11 C27 -100.16(13) . . . . ?
C9 C10 C11 C25 138.83(11) . . . . ?
C7 C8 C12 C1 -2.4(2) . . . . ?
C9 C8 C12 C1 173.74(12) . . . . ?
C7 C8 C12 C11 -179.78(12) . . . . ?
C9 C8 C12 C11 -3.65(15) . . . . ?
C2 C1 C12 C8 2.40(19) . . . . ?
Ge1 C1 C12 C8 -177.35(10) . . . . ?
C2 C1 C12 C11 179.23(12) . . . . ?
Ge1 C1 C12 C11 -0.53(18) . . . . ?
C27 C11 C12 C8 110.57(12) . . . . ?
C25 C11 C12 C8 -126.54(12) . . . . ?
C10 C11 C12 C8 -8.15(14) . . . . ?
C27 C11 C12 C1 -66.52(17) . . . . ?
C25 C11 C12 C1 56.38(18) . . . . ?
C10 C11 C12 C1 174.76(13) . . . . ?
C2 C3 C13 C14 178.91(12) . . . . ?
C15 C3 C13 C14 53.65(16) . . . . ?
C4 C3 C13 C14 -69.66(15) . . . . ?
C2 C3 C15 C16 54.09(15) . . . . ?
C13 C3 C15 C16 175.73(11) . . . . ?
C4 C3 C15 C16 -61.22(15) . . . . ?
C6 C5 C17 C18 173.46(13) . . . . ?
C19 C5 C17 C18 -63.58(16) . . . . ?
C4 C5 C17 C18 61.57(16) . . . . ?
C6 C5 C19 C20 -47.50(16) . . . . ?
C17 C5 C19 C20 -167.37(12) . . . . ?
C4 C5 C19 C20 67.31(15) . . . . ?
C8 C9 C21 C22 -50.94(17) . . . . ?
C10 C9 C21 C22 64.29(16) . . . . ?
C23 C9 C21 C22 -170.35(12) . . . . ?
C8 C9 C23 C24 -179.89(13) . . . . ?
C21 C9 C23 C24 -56.81(16) . . . . ?
C10 C9 C23 C24 69.17(16) . . . . ?
C12 C11 C25 C26 40.84(16) . . . . ?
C27 C11 C25 C26 163.84(12) . . . . ?
C10 C11 C25 C26 -73.51(15) . . . . ?
C12 C11 C27 C28 -175.80(12) . . . . ?
C25 C11 C27 C28 58.04(16) . . . . ?
C10 C11 C27 C28 -63.14(16) . . . . ?

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

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

_shelxl_version_number           2013-4



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        dibromodigermene
_chemical_name_common            (Eind)BrGe=GeBe(Eind)
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_egebr2k
_database_code_depnum_ccdc_archive 'CCDC 1543096'
_audit_update_record             
;
2017-04-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        Eind-germylenoid
_chemical_name_common            '[K(crypt-222)][(Eind)GeBr2]'
_chemical_melting_point          404-405
_chemical_formula_moiety         'C28 H45 Br2 Ge, C18 H36 K N2 O6'
_chemical_formula_sum            'C46 H81 Br2 Ge K N2 O6'
_chemical_formula_weight         1029.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.2880(9)
_cell_length_b                   12.8136(7)
_cell_length_c                   18.9434(17)
_cell_angle_alpha                104.562(4)
_cell_angle_beta                 96.164(5)
_cell_angle_gamma                107.936(5)
_cell_volume                     2471.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    103
_cell_measurement_reflns_used    43225
_cell_measurement_theta_min      1.134
_cell_measurement_theta_max      25.999

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.366
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_process_details   
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Fin-focus rotating anode'
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            43225
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.134
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             9641
_reflns_number_gt                7691
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       CrystalClear
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+5.4193P] 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         9641
_refine_ls_number_parameters     566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
GE1 Ge 0.58922(4) 0.69849(4) 0.32134(3) 0.03686(13) Uani 1 1 d . . . . .
BR1 Br 0.46407(5) 0.49107(4) 0.29159(3) 0.05214(16) Uani 1 1 d . . . . .
BR2 Br 0.47435(4) 0.77024(4) 0.42183(2) 0.03796(12) Uani 1 1 d . . . . .
C1 C 0.5323(4) 0.7217(3) 0.2198(2) 0.0303(9) Uani 1 1 d . . . . .
C2 C 0.6289(4) 0.7276(3) 0.1767(2) 0.0296(8) Uani 1 1 d . . . . .
C3 C 0.6094(4) 0.7373(3) 0.1047(2) 0.0291(8) Uani 1 1 d . . . . .
C4 C 0.4979(4) 0.7464(4) 0.0742(2) 0.0331(9) Uani 1 1 d . . . . .
H1 H 0.485897 0.754039 0.025563 0.040 Uiso 1 1 calc R U . . .
C5 C 0.4042(4) 0.7444(4) 0.1152(2) 0.0330(9) Uani 1 1 d . . . . .
C6 C 0.4193(4) 0.7313(3) 0.1860(2) 0.0290(8) Uani 1 1 d . . . . .
C7 C 0.7631(4) 0.7208(4) 0.1952(2) 0.0319(9) Uani 1 1 d . . . . .
C8 C 0.8250(4) 0.7574(4) 0.1318(2) 0.0326(9) Uani 1 1 d . . . . .
H2 H 0.879459 0.839679 0.150166 0.039 Uiso 1 1 calc R U . . .
H3 H 0.878937 0.711638 0.115450 0.039 Uiso 1 1 calc R U . . .
C9 C 0.7203(4) 0.7378(3) 0.0664(2) 0.0301(9) Uani 1 1 d . . . . .
C10 C 0.2774(4) 0.7549(5) 0.0892(3) 0.0428(11) Uani 1 1 d . . . . .
C11 C 0.2103(4) 0.7406(4) 0.1535(2) 0.0368(10) Uani 1 1 d . . . . .
H4 H 0.136492 0.667812 0.136780 0.044 Uiso 1 1 calc R U . . .
H5 H 0.178489 0.804835 0.169882 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3030(4) 0.7391(4) 0.2194(2) 0.0302(9) Uani 1 1 d . . . . .
C13 C 0.7483(4) 0.5948(4) 0.1906(3) 0.0372(10) Uani 1 1 d . . . . .
H6 H 0.704793 0.574475 0.230465 0.045 Uiso 1 1 calc R U . . .
H7 H 0.692717 0.543779 0.142305 0.045 Uiso 1 1 calc R U . . .
C14 C 0.8727(5) 0.5704(5) 0.1977(3) 0.0548(14) Uani 1 1 d . . . . .
H8 H 0.915126 0.586841 0.157140 0.082 Uiso 1 1 calc R U . . .
H9 H 0.854554 0.489395 0.194768 0.082 Uiso 1 1 calc R U . . .
H10 H 0.928266 0.619364 0.245598 0.082 Uiso 1 1 calc R U . . .
C15 C 0.8500(4) 0.8028(4) 0.2693(2) 0.0402(10) Uani 1 1 d . . . . .
H11 H 0.830205 0.766641 0.309113 0.048 Uiso 1 1 calc R U . . .
H12 H 0.939177 0.811978 0.265574 0.048 Uiso 1 1 calc R U . . .
C16 C 0.8392(5) 0.9210(4) 0.2924(3) 0.0473(12) Uani 1 1 d . . . . .
H13 H 0.848049 0.954092 0.251097 0.071 Uiso 1 1 calc R U . . .
H14 H 0.906577 0.970764 0.335645 0.071 Uiso 1 1 calc R U . . .
H15 H 0.756122 0.914593 0.305449 0.071 Uiso 1 1 calc R U . . .
C17 C 0.6948(4) 0.6212(4) 0.0071(2) 0.0355(9) Uani 1 1 d . . . . .
H16 H 0.774730 0.622985 -0.010351 0.043 Uiso 1 1 calc R U . . .
H17 H 0.673421 0.560063 0.031687 0.043 Uiso 1 1 calc R U . . .
C18 C 0.5904(4) 0.5873(4) -0.0606(3) 0.0434(11) Uani 1 1 d . . . . .
H18 H 0.510854 0.587703 -0.044549 0.065 Uiso 1 1 calc R U . . .
H19 H 0.578816 0.509981 -0.092153 0.065 Uiso 1 1 calc R U . . .
H20 H 0.614166 0.642216 -0.088980 0.065 Uiso 1 1 calc R U . . .
C19 C 0.7544(4) 0.8378(4) 0.0325(2) 0.0355(9) Uani 1 1 d . . . . .
H21 H 0.681368 0.825494 -0.006534 0.043 Uiso 1 1 calc R U . . .
H22 H 0.767386 0.910076 0.071771 0.043 Uiso 1 1 calc R U . . .
C20 C 0.8719(5) 0.8523(4) -0.0015(3) 0.0461(11) Uani 1 1 d . . . . .
H23 H 0.944904 0.864202 0.036523 0.069 Uiso 1 1 calc R U . . .
H24 H 0.888581 0.919078 -0.020183 0.069 Uiso 1 1 calc R U . . .
H25 H 0.858178 0.783130 -0.042633 0.069 Uiso 1 1 calc R U . . .
C21 C 0.3074(9) 0.8941(10) 0.0993(6) 0.035(2) Uani 0.568(12) 1 d . . P A 1
H26 H 0.225243 0.906823 0.092698 0.041 Uiso 0.568(12) 1 calc R U P A 1
H27 H 0.353376 0.938374 0.150943 0.041 Uiso 0.568(12) 1 calc R U P A 1
C22 C 0.3852(9) 0.9436(8) 0.0459(6) 0.045(3) Uani 0.568(12) 1 d . . P A 1
H28 H 0.397295 1.025523 0.056537 0.068 Uiso 0.568(12) 1 calc R U P A 1
H29 H 0.468218 0.934253 0.052840 0.068 Uiso 0.568(12) 1 calc R U P A 1
H30 H 0.339698 0.902607 -0.005581 0.068 Uiso 0.568(12) 1 calc R U P A 1
C23 C 0.2215(9) 0.6863(11) 0.0155(5) 0.038(2) Uani 0.568(12) 1 d . . P A 1
H31 H 0.212961 0.605796 0.011825 0.045 Uiso 0.568(12) 1 calc R U P A 1
H32 H 0.279507 0.711783 -0.017299 0.045 Uiso 0.568(12) 1 calc R U P A 1
C24 C 0.0927(8) 0.6890(11) -0.0130(5) 0.047(3) Uani 0.568(12) 1 d . . P A 1
H33 H 0.060918 0.639054 -0.064556 0.071 Uiso 0.568(12) 1 calc R U P A 1
H34 H 0.033435 0.661738 0.018059 0.071 Uiso 0.568(12) 1 calc R U P A 1
H35 H 0.100119 0.767946 -0.011125 0.071 Uiso 0.568(12) 1 calc R U P A 1
C25 C 0.3460(4) 0.8549(4) 0.2814(2) 0.0326(9) Uani 1 1 d . . . . .
H36 H 0.422137 0.860774 0.315586 0.039 Uiso 1 1 calc R U . . .
H37 H 0.371961 0.917538 0.258312 0.039 Uiso 1 1 calc R U . . .
C26 C 0.2488(4) 0.8753(4) 0.3272(3) 0.0424(11) Uani 1 1 d . . . . .
H38 H 0.170572 0.865114 0.293953 0.064 Uiso 1 1 calc R U . . .
H39 H 0.282596 0.953763 0.361423 0.064 Uiso 1 1 calc R U . . .
H40 H 0.230196 0.820172 0.355698 0.064 Uiso 1 1 calc R U . . .
C27 C 0.2415(4) 0.6372(4) 0.2483(2) 0.0354(9) Uani 1 1 d . . . . .
H41 H 0.302721 0.639772 0.290789 0.042 Uiso 1 1 calc R U . . .
H42 H 0.166216 0.647375 0.267341 0.042 Uiso 1 1 calc R U . . .
C28 C 0.2003(5) 0.5193(4) 0.1917(3) 0.0522(13) Uani 1 1 d . . . . .
H43 H 0.131448 0.511669 0.152418 0.078 Uiso 1 1 calc R U . . .
H44 H 0.170344 0.460077 0.216297 0.078 Uiso 1 1 calc R U . . .
H45 H 0.272546 0.509758 0.169773 0.078 Uiso 1 1 calc R U . . .
K1 K 0.04037(8) 0.75791(8) 0.64044(5) 0.0325(2) Uani 1 1 d . . . . .
N1 N -0.2175(3) 0.7414(3) 0.57210(19) 0.0333(8) Uani 1 1 d . . . . .
N2 N 0.3014(3) 0.7783(3) 0.7106(2) 0.0415(9) Uani 1 1 d . . . . .
C29 C -0.1976(4) 0.8316(4) 0.5353(2) 0.0354(9) Uani 1 1 d . . . . .
H46 H -0.169939 0.907135 0.574021 0.042 Uiso 1 1 calc R U . . .
H47 H -0.279904 0.820957 0.504972 0.042 Uiso 1 1 calc R U . . .
C30 C -0.1022(4) 0.8338(4) 0.4864(2) 0.0353(9) Uani 1 1 d . . . . .
H48 H -0.124057 0.756619 0.450356 0.042 Uiso 1 1 calc R U . . .
H49 H -0.103424 0.888860 0.458098 0.042 Uiso 1 1 calc R U . . .
O1 O 0.0208(3) 0.8671(2) 0.53021(15) 0.0323(6) Uani 1 1 d . . . . .
C31 C 0.1147(4) 0.8698(4) 0.4853(2) 0.0358(10) Uani 1 1 d . . . . .
H50 H 0.106485 0.915436 0.451205 0.043 Uiso 1 1 calc R U . . .
H51 H 0.102060 0.790628 0.454903 0.043 Uiso 1 1 calc R U . . .
C32 C 0.2434(4) 0.9219(4) 0.5338(3) 0.0383(10) Uani 1 1 d . . . . .
H52 H 0.309108 0.927720 0.502871 0.046 Uiso 1 1 calc R U . . .
H53 H 0.255531 1.000208 0.565412 0.046 Uiso 1 1 calc R U . . .
O2 O 0.2545(3) 0.8510(3) 0.57899(17) 0.0390(7) Uani 1 1 d . . . . .
C33 C 0.3754(4) 0.8978(4) 0.6278(3) 0.0464(12) Uani 1 1 d . . . . .
H54 H 0.380880 0.968103 0.666664 0.056 Uiso 1 1 calc R U . . .
H55 H 0.443424 0.918796 0.599565 0.056 Uiso 1 1 calc R U . . .
C34 C 0.3921(4) 0.8104(5) 0.6628(3) 0.0481(12) Uani 1 1 d . . . . .
H56 H 0.384015 0.740303 0.622905 0.058 Uiso 1 1 calc R U . . .
H57 H 0.479325 0.840358 0.692970 0.058 Uiso 1 1 calc R U . . .
C35 C -0.2924(4) 0.7625(4) 0.6294(3) 0.0385(10) Uani 1 1 d . . . . .
H58 H -0.333737 0.689458 0.640097 0.046 Uiso 1 1 calc R U . . .
H59 H -0.360430 0.787394 0.609692 0.046 Uiso 1 1 calc R U . . .
C36 C -0.2151(4) 0.8518(4) 0.7008(3) 0.0406(10) Uani 1 1 d . . . . .
H60 H -0.171683 0.924806 0.690705 0.049 Uiso 1 1 calc R U . . .
H61 H -0.271628 0.866063 0.735696 0.049 Uiso 1 1 calc R U . . .
O3 O -0.1240(3) 0.8137(3) 0.73320(16) 0.0356(7) Uani 1 1 d . . . . .
C37 C -0.0701(4) 0.8812(4) 0.8082(2) 0.0413(10) Uani 1 1 d . . . . .
H62 H -0.136483 0.872176 0.838619 0.050 Uiso 1 1 calc R U . . .
H63 H -0.034140 0.963397 0.811110 0.050 Uiso 1 1 calc R U . . .
C38 C 0.0317(4) 0.8427(4) 0.8370(2) 0.0406(10) Uani 1 1 d . . . . .
H64 H 0.065479 0.884675 0.890548 0.049 Uiso 1 1 calc R U . . .
H65 H -0.003520 0.759451 0.831476 0.049 Uiso 1 1 calc R U . . .
O4 O 0.1311(3) 0.8642(3) 0.79660(16) 0.0377(7) Uani 1 1 d . . . . .
C39 C 0.2416(5) 0.8535(5) 0.8310(3) 0.0470(12) Uani 1 1 d . . . . .
H66 H 0.220559 0.777142 0.839288 0.056 Uiso 1 1 calc R U . . .
H67 H 0.276416 0.913107 0.879974 0.056 Uiso 1 1 calc R U . . .
C40 C 0.3396(5) 0.8667(5) 0.7827(3) 0.0481(12) Uani 1 1 d . . . . .
H68 H 0.358788 0.942902 0.774361 0.058 Uiso 1 1 calc R U . . .
H69 H 0.418861 0.865319 0.809835 0.058 Uiso 1 1 calc R U . . .
C41 C -0.2856(4) 0.6272(4) 0.5177(3) 0.0373(10) Uani 1 1 d . . . . .
H70 H -0.250181 0.622625 0.471887 0.045 Uiso 1 1 calc R U . . .
H71 H -0.376317 0.617737 0.504322 0.045 Uiso 1 1 calc R U . . .
C42 C -0.2758(4) 0.5316(4) 0.5470(3) 0.0418(11) Uani 1 1 d . . . . .
H72 H -0.307169 0.537687 0.594135 0.050 Uiso 1 1 calc R U . . .
H73 H -0.329029 0.456727 0.510626 0.050 Uiso 1 1 calc R U . . .
O5 O -0.1463(3) 0.5379(3) 0.55958(17) 0.0376(7) Uani 1 1 d . . . . .
C43 C -0.1319(5) 0.4559(4) 0.5949(3) 0.0451(11) Uani 1 1 d . . . . .
H74 H -0.192221 0.378455 0.565917 0.054 Uiso 1 1 calc R U . . .
H75 H -0.151021 0.475107 0.645374 0.054 Uiso 1 1 calc R U . . .
C44 C 0.0005(5) 0.4562(4) 0.6002(3) 0.0441(11) Uani 1 1 d . . . . .
H76 H 0.007611 0.391797 0.618137 0.053 Uiso 1 1 calc R U . . .
H77 H 0.022648 0.445417 0.550292 0.053 Uiso 1 1 calc R U . . .
O6 O 0.0860(3) 0.5621(3) 0.64997(17) 0.0406(7) Uani 1 1 d . . . . .
C45 C 0.2145(5) 0.5669(4) 0.6553(3) 0.0459(11) Uani 1 1 d . . . . .
H78 H 0.243329 0.575171 0.608832 0.055 Uiso 1 1 calc R U . . .
H79 H 0.221302 0.494814 0.662431 0.055 Uiso 1 1 calc R U . . .
C46 C 0.2962(5) 0.6672(4) 0.7199(3) 0.0478(12) Uani 1 1 d . . . . .
H80 H 0.263303 0.659825 0.765418 0.057 Uiso 1 1 calc R U . . .
H81 H 0.383530 0.665015 0.727000 0.057 Uiso 1 1 calc R U . . .
C47 C 0.2725(10) 0.8370(11) 0.0490(8) 0.038(3) Uani 0.432(12) 1 d . . P A 2
H82 H 0.184492 0.836438 0.038349 0.045 Uiso 0.432(12) 1 calc R U P A 2
H83 H 0.299697 0.815728 0.001033 0.045 Uiso 0.432(12) 1 calc R U P A 2
C48 C 0.3596(13) 0.9549(12) 0.0961(9) 0.045(4) Uani 0.432(12) 1 d . . P A 2
H84 H 0.357136 1.011024 0.069563 0.067 Uiso 0.432(12) 1 calc R U P A 2
H85 H 0.331768 0.975596 0.143251 0.067 Uiso 0.432(12) 1 calc R U P A 2
H86 H 0.446619 0.954949 0.106049 0.067 Uiso 0.432(12) 1 calc R U P A 2
C49 C 0.1950(11) 0.6271(12) 0.0222(6) 0.031(3) Uani 0.432(12) 1 d . . P A 2
H87 H 0.243365 0.619263 -0.018211 0.037 Uiso 0.432(12) 1 calc R U P A 2
H88 H 0.192387 0.564197 0.044203 0.037 Uiso 0.432(12) 1 calc R U P A 2
C50 C 0.0574(10) 0.6089(13) -0.0129(7) 0.045(3) Uani 0.432(12) 1 d . . P A 2
H89 H 0.020088 0.533061 -0.050273 0.068 Uiso 0.432(12) 1 calc R U P A 2
H90 H 0.006822 0.613373 0.025962 0.068 Uiso 0.432(12) 1 calc R U P A 2
H91 H 0.057987 0.668641 -0.036680 0.068 Uiso 0.432(12) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
GE1 C1 2.084(4) . ?
GE1 BR1 2.4780(7) . ?
GE1 BR2 2.5562(6) . ?
C1 C6 1.419(6) . ?
C1 C2 1.426(5) . ?
C2 C3 1.400(6) . ?
C2 C7 1.551(5) . ?
C3 C4 1.379(6) . ?
C3 C9 1.512(5) . ?
C4 C5 1.376(6) . ?
C4 H1 0.9500 . ?
C5 C6 1.391(6) . ?
C5 C10 1.519(6) . ?
C6 C12 1.536(5) . ?
C7 C15 1.538(6) . ?
C7 C13 1.550(6) . ?
C7 C8 1.554(5) . ?
C8 C9 1.531(6) . ?
C8 H2 0.9900 . ?
C8 H3 0.9900 . ?
C9 C19 1.538(6) . ?
C9 C17 1.549(6) . ?
C10 C23 1.404(11) . ?
C10 C47 1.456(11) . ?
C10 C11 1.522(6) . ?
C10 C21 1.667(11) . ?
C10 C49 1.709(13) . ?
C11 C12 1.550(6) . ?
C11 H4 0.9900 . ?
C11 H5 0.9900 . ?
C12 C27 1.539(6) . ?
C12 C25 1.541(6) . ?
C13 C14 1.529(6) . ?
C13 H6 0.9900 . ?
C13 H7 0.9900 . ?
C14 H8 0.9800 . ?
C14 H9 0.9800 . ?
C14 H10 0.9800 . ?
C15 C16 1.513(7) . ?
C15 H11 0.9900 . ?
C15 H12 0.9900 . ?
C16 H13 0.9800 . ?
C16 H14 0.9800 . ?
C16 H15 0.9800 . ?
C17 C18 1.517(6) . ?
C17 H16 0.9900 . ?
C17 H17 0.9900 . ?
C18 H18 0.9800 . ?
C18 H19 0.9800 . ?
C18 H20 0.9800 . ?
C19 C20 1.516(6) . ?
C19 H21 0.9900 . ?
C19 H22 0.9900 . ?
C20 H23 0.9800 . ?
C20 H24 0.9800 . ?
C20 H25 0.9800 . ?
C21a C22 1.537(13) . ?
C21a H26 0.9900 . ?
C21a H27 0.9900 . ?
C22a H28 0.9800 . ?
C22a H29 0.9800 . ?
C22a H30 0.9800 . ?
C23a C24 1.509(12) . ?
C23a H31 0.9900 . ?
C23a H32 0.9900 . ?
C24a H33 0.9800 . ?
C24a H34 0.9800 . ?
C24a H35 0.9800 . ?
C25 C26 1.513(6) . ?
C25 H36 0.9900 . ?
C25 H37 0.9900 . ?
C26 H38 0.9800 . ?
C26 H39 0.9800 . ?
C26 H40 0.9800 . ?
C27 C28 1.515(6) . ?
C27 H41 0.9900 . ?
C27 H42 0.9900 . ?
C28 H43 0.9800 . ?
C28 H44 0.9800 . ?
C28 H45 0.9800 . ?
K1 O6 2.756(3) . ?
K1 O1 2.815(3) . ?
K1 O3 2.815(3) . ?
K1 O4 2.849(3) . ?
K1 O2 2.854(3) . ?
K1 O5 2.866(3) . ?
K1 N1 2.978(4) . ?
K1 N2 3.005(4) . ?
N1 C29 1.466(5) . ?
N1 C35 1.470(5) . ?
N1 C41 1.473(5) . ?
N2 C40 1.460(6) . ?
N2 C46 1.463(6) . ?
N2 C34 1.470(6) . ?
C29 C30 1.493(6) . ?
C29 H46 0.9900 . ?
C29 H47 0.9900 . ?
C30 O1 1.417(5) . ?
C30 H48 0.9900 . ?
C30 H49 0.9900 . ?
O1 C31 1.426(5) . ?
C31 C32 1.485(6) . ?
C31 H50 0.9900 . ?
C31 H51 0.9900 . ?
C32 O2 1.419(5) . ?
C32 H52 0.9900 . ?
C32 H53 0.9900 . ?
O2 C33 1.423(5) . ?
C33 C34 1.485(7) . ?
C33 H54 0.9900 . ?
C33 H55 0.9900 . ?
C34 H56 0.9900 . ?
C34 H57 0.9900 . ?
C35 C36 1.500(6) . ?
C35 H58 0.9900 . ?
C35 H59 0.9900 . ?
C36 O3 1.413(5) . ?
C36 H60 0.9900 . ?
C36 H61 0.9900 . ?
O3 C37 1.417(5) . ?
C37 C38 1.488(6) . ?
C37 H62 0.9900 . ?
C37 H63 0.9900 . ?
C38 O4 1.421(5) . ?
C38 H64 0.9900 . ?
C38 H65 0.9900 . ?
O4 C39 1.406(5) . ?
C39 C40 1.506(7) . ?
C39 H66 0.9900 . ?
C39 H67 0.9900 . ?
C40 H68 0.9900 . ?
C40 H69 0.9900 . ?
C41 C42 1.494(6) . ?
C41 H70 0.9900 . ?
C41 H71 0.9900 . ?
C42 O5 1.429(5) . ?
C42 H72 0.9900 . ?
C42 H73 0.9900 . ?
O5 C43 1.418(5) . ?
C43 C44 1.486(7) . ?
C43 H74 0.9900 . ?
C43 H75 0.9900 . ?
C44 O6 1.420(6) . ?
C44 H76 0.9900 . ?
C44 H77 0.9900 . ?
O6 C45 1.425(5) . ?
C45 C46 1.495(7) . ?
C45 H78 0.9900 . ?
C45 H79 0.9900 . ?
C46 H80 0.9900 . ?
C46 H81 0.9900 . ?
C47b C48 1.505(19) . ?
C47b H82 0.9900 . ?
C47b H83 0.9900 . ?
C48b H84 0.9800 . ?
C48b H85 0.9800 . ?
C48b H86 0.9800 . ?
C49b C50 1.545(15) . ?
C49b H87 0.9900 . ?
C49b H88 0.9900 . ?
C50b H89 0.9800 . ?
C50b H90 0.9800 . ?
C50b H91 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 GE1 BR1 98.57(11) . . ?
C1 GE1 BR2 113.09(11) . . ?
BR1 GE1 BR2 96.65(2) . . ?
C6 C1 C2 115.5(4) . . ?
C6 C1 GE1 133.3(3) . . ?
C2 C1 GE1 111.2(3) . . ?
C3 C2 C1 121.3(4) . . ?
C3 C2 C7 108.8(3) . . ?
C1 C2 C7 129.9(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 C9 125.0(4) . . ?
C2 C3 C9 113.9(3) . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H1 120.5 . . ?
C3 C4 H1 120.5 . . ?
C4 C5 C6 121.2(4) . . ?
C4 C5 C10 124.8(4) . . ?
C6 C5 C10 114.0(4) . . ?
C5 C6 C1 121.9(4) . . ?
C5 C6 C12 109.3(3) . . ?
C1 C6 C12 128.7(4) . . ?
C15 C7 C13 110.0(4) . . ?
C15 C7 C2 117.3(3) . . ?
C13 C7 C2 108.6(3) . . ?
C15 C7 C8 107.1(3) . . ?
C13 C7 C8 111.7(3) . . ?
C2 C7 C8 101.9(3) . . ?
C9 C8 C7 109.2(3) . . ?
C9 C8 H2 109.8 . . ?
C7 C8 H2 109.8 . . ?
C9 C8 H3 109.8 . . ?
C7 C8 H3 109.8 . . ?
H2 C8 H3 108.3 . . ?
C3 C9 C8 101.2(3) . . ?
C3 C9 C19 110.5(3) . . ?
C8 C9 C19 111.0(3) . . ?
C3 C9 C17 112.0(3) . . ?
C8 C9 C17 110.4(3) . . ?
C19 C9 C17 111.3(3) . . ?
C23a C10 C5 112.1(5) . . ?
C47b C10 C5 119.8(5) . . ?
C23a C10 C11 121.8(6) . . ?
C47b C10 C11 124.3(6) . . ?
C5 C10 C11 102.3(3) . . ?
C23a C10 C21 112.0(6) . . ?
C5 C10 C21 105.9(5) . . ?
C11 C10 C21 100.9(5) . . ?
C47b C10 C49 101.4(7) . . ?
C5 C10 C49 104.5(5) . . ?
C11 C10 C49 101.4(5) . . ?
C10 C11 C12 110.2(3) . . ?
C10 C11 H4 109.6 . . ?
C12 C11 H4 109.6 . . ?
C10 C11 H5 109.6 . . ?
C12 C11 H5 109.6 . . ?
H4 C11 H5 108.1 . . ?
C6 C12 C27 113.4(3) . . ?
C6 C12 C25 107.4(3) . . ?
C27 C12 C25 111.8(3) . . ?
C6 C12 C11 103.3(3) . . ?
C27 C12 C11 110.7(3) . . ?
C25 C12 C11 109.9(3) . . ?
C14 C13 C7 115.1(4) . . ?
C14 C13 H6 108.5 . . ?
C7 C13 H6 108.5 . . ?
C14 C13 H7 108.5 . . ?
C7 C13 H7 108.5 . . ?
H6 C13 H7 107.5 . . ?
C13 C14 H8 109.5 . . ?
C13 C14 H9 109.5 . . ?
H8 C14 H9 109.5 . . ?
C13 C14 H10 109.5 . . ?
H8 C14 H10 109.5 . . ?
H9 C14 H10 109.5 . . ?
C16 C15 C7 115.2(4) . . ?
C16 C15 H11 108.5 . . ?
C7 C15 H11 108.5 . . ?
C16 C15 H12 108.5 . . ?
C7 C15 H12 108.5 . . ?
H11 C15 H12 107.5 . . ?
C15 C16 H13 109.5 . . ?
C15 C16 H14 109.5 . . ?
H13 C16 H14 109.5 . . ?
C15 C16 H15 109.5 . . ?
H13 C16 H15 109.5 . . ?
H14 C16 H15 109.5 . . ?
C18 C17 C9 116.9(4) . . ?
C18 C17 H16 108.1 . . ?
C9 C17 H16 108.1 . . ?
C18 C17 H17 108.1 . . ?
C9 C17 H17 108.1 . . ?
H16 C17 H17 107.3 . . ?
C17 C18 H18 109.5 . . ?
C17 C18 H19 109.5 . . ?
H18 C18 H19 109.5 . . ?
C17 C18 H20 109.5 . . ?
H18 C18 H20 109.5 . . ?
H19 C18 H20 109.5 . . ?
C20 C19 C9 114.6(4) . . ?
C20 C19 H21 108.6 . . ?
C9 C19 H21 108.6 . . ?
C20 C19 H22 108.6 . . ?
C9 C19 H22 108.6 . . ?
H21 C19 H22 107.6 . . ?
C19 C20 H23 109.5 . . ?
C19 C20 H24 109.5 . . ?
H23 C20 H24 109.5 . . ?
C19 C20 H25 109.5 . . ?
H23 C20 H25 109.5 . . ?
H24 C20 H25 109.5 . . ?
C22a C21a C10 116.1(7) . . ?
C22a C21a H26 108.3 . . ?
C10 C21a H26 108.3 . . ?
C22a C21a H27 108.3 . . ?
C10 C21a H27 108.3 . . ?
H26a C21a H27 107.4 . . ?
C21a C22a H28 109.5 . . ?
C21a C22a H29 109.5 . . ?
H28a C22a H29 109.5 . . ?
C21a C22a H30 109.5 . . ?
H28a C22a H30 109.5 . . ?
H29a C22a H30 109.5 . . ?
C10 C23a C24 115.0(8) . . ?
C10 C23a H31 108.5 . . ?
C24a C23a H31 108.5 . . ?
C10 C23a H32 108.5 . . ?
C24a C23a H32 108.5 . . ?
H31a C23a H32 107.5 . . ?
C23a C24a H33 109.5 . . ?
C23a C24a H34 109.5 . . ?
H33a C24a H34 109.5 . . ?
C23a C24a H35 109.5 . . ?
H33a C24a H35 109.5 . . ?
H34a C24a H35 109.5 . . ?
C26 C25 C12 116.2(4) . . ?
C26 C25 H36 108.2 . . ?
C12 C25 H36 108.2 . . ?
C26 C25 H37 108.2 . . ?
C12 C25 H37 108.2 . . ?
H36 C25 H37 107.4 . . ?
C25 C26 H38 109.5 . . ?
C25 C26 H39 109.5 . . ?
H38 C26 H39 109.5 . . ?
C25 C26 H40 109.5 . . ?
H38 C26 H40 109.5 . . ?
H39 C26 H40 109.5 . . ?
C28 C27 C12 115.5(4) . . ?
C28 C27 H41 108.4 . . ?
C12 C27 H41 108.4 . . ?
C28 C27 H42 108.4 . . ?
C12 C27 H42 108.4 . . ?
H41 C27 H42 107.5 . . ?
C27 C28 H43 109.5 . . ?
C27 C28 H44 109.5 . . ?
H43 C28 H44 109.5 . . ?
C27 C28 H45 109.5 . . ?
H43 C28 H45 109.5 . . ?
H44 C28 H45 109.5 . . ?
O6 K1 O1 136.77(9) . . ?
O6 K1 O3 112.46(9) . . ?
O1 K1 O3 104.82(9) . . ?
O6 K1 O4 91.17(9) . . ?
O1 K1 O4 127.39(9) . . ?
O3 K1 O4 59.37(8) . . ?
O6 K1 O2 97.67(9) . . ?
O1 K1 O2 58.87(8) . . ?
O3 K1 O2 144.40(9) . . ?
O4 K1 O2 103.24(9) . . ?
O6 K1 O5 61.09(9) . . ?
O1 K1 O5 97.22(9) . . ?
O3 K1 O5 92.35(9) . . ?
O4 K1 O5 130.44(9) . . ?
O2 K1 O5 119.54(9) . . ?
O6 K1 N1 119.94(10) . . ?
O1 K1 N1 61.88(9) . . ?
O3 K1 N1 60.63(9) . . ?
O4 K1 N1 119.23(9) . . ?
O2 K1 N1 120.05(9) . . ?
O5 K1 N1 59.91(9) . . ?
O6 K1 N2 60.86(10) . . ?
O1 K1 N2 117.83(10) . . ?
O3 K1 N2 118.92(10) . . ?
O4 K1 N2 60.21(9) . . ?
O2 K1 N2 59.80(10) . . ?
O5 K1 N2 120.93(10) . . ?
N1 K1 N2 179.15(11) . . ?
C29 N1 C35 109.2(3) . . ?
C29 N1 C41 110.6(3) . . ?
C35 N1 C41 109.3(3) . . ?
C29 N1 K1 106.1(2) . . ?
C35 N1 K1 110.8(2) . . ?
C41 N1 K1 110.8(2) . . ?
C40 N2 C46 110.5(4) . . ?
C40 N2 C34 110.0(4) . . ?
C46 N2 C34 109.5(4) . . ?
C40 N2 K1 108.0(3) . . ?
C46 N2 K1 108.6(3) . . ?
C34 N2 K1 110.2(3) . . ?
N1 C29 C30 114.6(3) . . ?
N1 C29 H46 108.6 . . ?
C30 C29 H46 108.6 . . ?
N1 C29 H47 108.6 . . ?
C30 C29 H47 108.6 . . ?
H46 C29 H47 107.6 . . ?
O1 C30 C29 109.9(3) . . ?
O1 C30 H48 109.7 . . ?
C29 C30 H48 109.7 . . ?
O1 C30 H49 109.7 . . ?
C29 C30 H49 109.7 . . ?
H48 C30 H49 108.2 . . ?
C30 O1 C31 111.6(3) . . ?
C30 O1 K1 116.0(2) . . ?
C31 O1 K1 114.6(2) . . ?
O1 C31 C32 109.6(3) . . ?
O1 C31 H50 109.7 . . ?
C32 C31 H50 109.7 . . ?
O1 C31 H51 109.7 . . ?
C32 C31 H51 109.7 . . ?
H50 C31 H51 108.2 . . ?
O2 C32 C31 108.3(3) . . ?
O2 C32 H52 110.0 . . ?
C31 C32 H52 110.0 . . ?
O2 C32 H53 110.0 . . ?
C31 C32 H53 110.0 . . ?
H52 C32 H53 108.4 . . ?
C32 O2 C33 110.9(3) . . ?
C32 O2 K1 117.6(2) . . ?
C33 O2 K1 116.6(3) . . ?
O2 C33 C34 108.7(4) . . ?
O2 C33 H54 109.9 . . ?
C34 C33 H54 109.9 . . ?
O2 C33 H55 109.9 . . ?
C34 C33 H55 109.9 . . ?
H54 C33 H55 108.3 . . ?
N2 C34 C33 114.9(4) . . ?
N2 C34 H56 108.6 . . ?
C33 C34 H56 108.6 . . ?
N2 C34 H57 108.6 . . ?
C33 C34 H57 108.6 . . ?
H56 C34 H57 107.5 . . ?
N1 C35 C36 113.5(4) . . ?
N1 C35 H58 108.9 . . ?
C36 C35 H58 108.9 . . ?
N1 C35 H59 108.9 . . ?
C36 C35 H59 108.9 . . ?
H58 C35 H59 107.7 . . ?
O3 C36 C35 109.9(4) . . ?
O3 C36 H60 109.7 . . ?
C35 C36 H60 109.7 . . ?
O3 C36 H61 109.7 . . ?
C35 C36 H61 109.7 . . ?
H60 C36 H61 108.2 . . ?
C36 O3 C37 111.6(3) . . ?
C36 O3 K1 114.5(2) . . ?
C37 O3 K1 118.1(2) . . ?
O3 C37 C38 108.8(4) . . ?
O3 C37 H62 109.9 . . ?
C38 C37 H62 109.9 . . ?
O3 C37 H63 109.9 . . ?
C38 C37 H63 109.9 . . ?
H62 C37 H63 108.3 . . ?
O4 C38 C37 109.4(4) . . ?
O4 C38 H64 109.8 . . ?
C37 C38 H64 109.8 . . ?
O4 C38 H65 109.8 . . ?
C37 C38 H65 109.8 . . ?
H64 C38 H65 108.2 . . ?
C39 O4 C38 112.3(3) . . ?
C39 O4 K1 119.1(3) . . ?
C38 O4 K1 111.9(2) . . ?
O4 C39 C40 110.1(4) . . ?
O4 C39 H66 109.6 . . ?
C40 C39 H66 109.6 . . ?
O4 C39 H67 109.6 . . ?
C40 C39 H67 109.6 . . ?
H66 C39 H67 108.1 . . ?
N2 C40 C39 114.4(4) . . ?
N2 C40 H68 108.7 . . ?
C39 C40 H68 108.7 . . ?
N2 C40 H69 108.7 . . ?
C39 C40 H69 108.7 . . ?
H68 C40 H69 107.6 . . ?
N1 C41 C42 112.4(4) . . ?
N1 C41 H70 109.1 . . ?
C42 C41 H70 109.1 . . ?
N1 C41 H71 109.1 . . ?
C42 C41 H71 109.1 . . ?
H70 C41 H71 107.8 . . ?
O5 C42 C41 109.6(3) . . ?
O5 C42 H72 109.7 . . ?
C41 C42 H72 109.7 . . ?
O5 C42 H73 109.7 . . ?
C41 C42 H73 109.7 . . ?
H72 C42 H73 108.2 . . ?
C43 O5 C42 110.9(3) . . ?
C43 O5 K1 108.7(3) . . ?
C42 O5 K1 116.9(2) . . ?
O5 C43 C44 109.6(4) . . ?
O5 C43 H74 109.8 . . ?
C44 C43 H74 109.8 . . ?
O5 C43 H75 109.8 . . ?
C44 C43 H75 109.8 . . ?
H74 C43 H75 108.2 . . ?
O6 C44 C43 109.9(4) . . ?
O6 C44 H76 109.7 . . ?
C43 C44 H76 109.7 . . ?
O6 C44 H77 109.7 . . ?
C43 C44 H77 109.7 . . ?
H76 C44 H77 108.2 . . ?
C44 O6 C45 111.7(3) . . ?
C44 O6 K1 116.5(2) . . ?
C45 O6 K1 116.5(3) . . ?
O6 C45 C46 109.1(4) . . ?
O6 C45 H78 109.9 . . ?
C46 C45 H78 109.9 . . ?
O6 C45 H79 109.9 . . ?
C46 C45 H79 109.9 . . ?
H78 C45 H79 108.3 . . ?
N2 C46 C45 113.5(4) . . ?
N2 C46 H80 108.9 . . ?
C45 C46 H80 108.9 . . ?
N2 C46 H81 108.9 . . ?
C45 C46 H81 108.9 . . ?
H80 C46 H81 107.7 . . ?
C10 C47b C48 108.7(11) . . ?
C10 C47b H82 109.9 . . ?
C48b C47b H82 109.9 . . ?
C10 C47b H83 109.9 . . ?
C48b C47b H83 109.9 . . ?
H82b C47b H83 108.3 . . ?
C47b C48b H84 109.5 . . ?
C47b C48b H85 109.5 . . ?
H84b C48b H85 109.5 . . ?
C47b C48b H86 109.5 . . ?
H84b C48b H86 109.5 . . ?
H85b C48b H86 109.5 . . ?
C50b C49b C10 116.9(8) . . ?
C50b C49b H87 108.1 . . ?
C10 C49b H87 108.1 . . ?
C50b C49b H88 108.1 . . ?
C10 C49b H88 108.1 . . ?
H87b C49b H88 107.3 . . ?
C49b C50b H89 109.5 . . ?
C49b C50b H90 109.5 . . ?
H89b C50b H90 109.5 . . ?
C49b C50b H91 109.5 . . ?
H89b C50b H91 109.5 . . ?
H90b C50b H91 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.6(6) . . . . ?
GE1 C1 C2 C3 176.8(3) . . . . ?
C6 C1 C2 C7 179.8(4) . . . . ?
GE1 C1 C2 C7 -0.8(5) . . . . ?
C1 C2 C3 C4 2.8(6) . . . . ?
C7 C2 C3 C4 -179.1(4) . . . . ?
C1 C2 C3 C9 -177.8(4) . . . . ?
C7 C2 C3 C9 0.2(5) . . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
C9 C3 C4 C5 179.8(4) . . . . ?
C3 C4 C5 C6 -1.1(6) . . . . ?
C3 C4 C5 C10 179.3(4) . . . . ?
C4 C5 C6 C1 1.2(6) . . . . ?
C10 C5 C6 C1 -179.2(4) . . . . ?
C4 C5 C6 C12 176.9(4) . . . . ?
C10 C5 C6 C12 -3.5(5) . . . . ?
C2 C1 C6 C5 0.6(6) . . . . ?
GE1 C1 C6 C5 -178.6(3) . . . . ?
C2 C1 C6 C12 -174.1(4) . . . . ?
GE1 C1 C6 C12 6.7(7) . . . . ?
C3 C2 C7 C15 129.6(4) . . . . ?
C1 C2 C7 C15 -52.6(6) . . . . ?
C3 C2 C7 C13 -104.9(4) . . . . ?
C1 C2 C7 C13 72.9(5) . . . . ?
C3 C2 C7 C8 13.1(4) . . . . ?
C1 C2 C7 C8 -169.1(4) . . . . ?
C15 C7 C8 C9 -145.6(4) . . . . ?
C13 C7 C8 C9 93.9(4) . . . . ?
C2 C7 C8 C9 -21.8(4) . . . . ?
C4 C3 C9 C8 165.7(4) . . . . ?
C2 C3 C9 C8 -13.6(4) . . . . ?
C4 C3 C9 C19 48.1(5) . . . . ?
C2 C3 C9 C19 -131.3(4) . . . . ?
C4 C3 C9 C17 -76.7(5) . . . . ?
C2 C3 C9 C17 104.0(4) . . . . ?
C7 C8 C9 C3 21.7(4) . . . . ?
C7 C8 C9 C19 139.0(3) . . . . ?
C7 C8 C9 C17 -97.1(4) . . . . ?
C4 C5 C10 C23a 44.8(8) . . . . ?
C6 C5 C10 C23a -134.8(7) . . . . ?
C4 C5 C10 C47b -41.0(9) . . . . ?
C6 C5 C10 C47b 139.4(8) . . . . ?
C4 C5 C10 C11 177.0(4) . . . . ?
C6 C5 C10 C11 -2.6(5) . . . . ?
C4 C5 C10 C21a -77.7(6) . . . . ?
C6 C5 C10 C21a 102.7(5) . . . . ?
C4 C5 C10 C49b 71.6(7) . . . . ?
C6 C5 C10 C49b -108.0(6) . . . . ?
C23a C10 C11 C12 133.8(6) . . . . ?
C47b C10 C11 C12 -132.0(7) . . . . ?
C5 C10 C11 C12 7.7(5) . . . . ?
C21a C10 C11 C12 -101.5(5) . . . . ?
C49b C10 C11 C12 115.5(5) . . . . ?
C5 C6 C12 C27 127.8(4) . . . . ?
C1 C6 C12 C27 -56.9(6) . . . . ?
C5 C6 C12 C25 -108.1(4) . . . . ?
C1 C6 C12 C25 67.1(5) . . . . ?
C5 C6 C12 C11 8.0(4) . . . . ?
C1 C6 C12 C11 -176.8(4) . . . . ?
C10 C11 C12 C6 -9.7(5) . . . . ?
C10 C11 C12 C27 -131.5(4) . . . . ?
C10 C11 C12 C25 104.6(4) . . . . ?
C15 C7 C13 C14 -57.8(5) . . . . ?
C2 C7 C13 C14 172.5(4) . . . . ?
C8 C7 C13 C14 61.0(5) . . . . ?
C13 C7 C15 C16 -161.1(4) . . . . ?
C2 C7 C15 C16 -36.3(5) . . . . ?
C8 C7 C15 C16 77.4(4) . . . . ?
C3 C9 C17 C18 66.3(5) . . . . ?
C8 C9 C17 C18 178.3(4) . . . . ?
C19 C9 C17 C18 -57.9(5) . . . . ?
C3 C9 C19 C20 174.9(4) . . . . ?
C8 C9 C19 C20 63.4(5) . . . . ?
C17 C9 C19 C20 -60.0(5) . . . . ?
C23a C10 C21a C22a -53.1(9) . . . . ?
C5 C10 C21a C22a 69.4(8) . . . . ?
C11 C10 C21a C22a 175.7(7) . . . . ?
C5 C10 C23a C24a 177.7(7) . . . . ?
C11 C10 C23a C24a 56.2(11) . . . . ?
C21a C10 C23a C24a -63.3(10) . . . . ?
C6 C12 C25 C26 -174.2(3) . . . . ?
C27 C12 C25 C26 -49.2(5) . . . . ?
C11 C12 C25 C26 74.1(4) . . . . ?
C6 C12 C27 C28 -56.4(5) . . . . ?
C25 C12 C27 C28 -178.0(4) . . . . ?
C11 C12 C27 C28 59.2(5) . . . . ?
C35 N1 C29 C30 168.6(4) . . . . ?
C41 N1 C29 C30 -71.1(4) . . . . ?
K1 N1 C29 C30 49.2(4) . . . . ?
N1 C29 C30 O1 -67.6(5) . . . . ?
C29 C30 O1 C31 179.7(3) . . . . ?
C29 C30 O1 K1 46.1(4) . . . . ?
C30 O1 C31 C32 171.3(3) . . . . ?
K1 O1 C31 C32 -54.3(4) . . . . ?
O1 C31 C32 O2 62.6(4) . . . . ?
C31 C32 O2 C33 -178.9(3) . . . . ?
C31 C32 O2 K1 -41.1(4) . . . . ?
C32 O2 C33 C34 -169.0(4) . . . . ?
K1 O2 C33 C34 52.7(4) . . . . ?
C40 N2 C34 C33 -78.4(5) . . . . ?
C46 N2 C34 C33 160.0(4) . . . . ?
K1 N2 C34 C33 40.6(5) . . . . ?
O2 C33 C34 N2 -63.6(5) . . . . ?
C29 N1 C35 C36 -80.4(4) . . . . ?
C41 N1 C35 C36 158.5(4) . . . . ?
K1 N1 C35 C36 36.0(4) . . . . ?
N1 C35 C36 O3 -63.4(5) . . . . ?
C35 C36 O3 C37 -165.9(4) . . . . ?
C35 C36 O3 K1 56.7(4) . . . . ?
C36 O3 C37 C38 -175.6(4) . . . . ?
K1 O3 C37 C38 -39.8(4) . . . . ?
O3 C37 C38 O4 64.0(5) . . . . ?
C37 C38 O4 C39 167.1(4) . . . . ?
C37 C38 O4 K1 -56.0(4) . . . . ?
C38 O4 C39 C40 175.0(4) . . . . ?
K1 O4 C39 C40 41.4(5) . . . . ?
C46 N2 C40 C39 -69.5(5) . . . . ?
C34 N2 C40 C39 169.6(4) . . . . ?
K1 N2 C40 C39 49.2(5) . . . . ?
O4 C39 C40 N2 -63.1(5) . . . . ?
C29 N1 C41 C42 163.6(3) . . . . ?
C35 N1 C41 C42 -76.1(4) . . . . ?
K1 N1 C41 C42 46.3(4) . . . . ?
N1 C41 C42 O5 -64.5(5) . . . . ?
C41 C42 O5 C43 173.7(4) . . . . ?
C41 C42 O5 K1 48.3(4) . . . . ?
C42 O5 C43 C44 174.2(4) . . . . ?
K1 O5 C43 C44 -56.0(4) . . . . ?
O5 C43 C44 O6 67.3(5) . . . . ?
C43 C44 O6 C45 -178.7(4) . . . . ?
C43 C44 O6 K1 -41.5(4) . . . . ?
C44 O6 C45 C46 -167.7(4) . . . . ?
K1 O6 C45 C46 55.1(4) . . . . ?
C40 N2 C46 C45 158.6(4) . . . . ?
C34 N2 C46 C45 -80.1(5) . . . . ?
K1 N2 C46 C45 40.3(4) . . . . ?
O6 C45 C46 N2 -65.1(5) . . . . ?
C5 C10 C47b C48b -56.6(12) . . . . ?
C11 C10 C47b C48b 76.8(10) . . . . ?
C49b C10 C47b C48b -170.8(9) . . . . ?
C47b C10 C49b C50b -57.8(11) . . . . ?
C5 C10 C49b C50b 177.1(9) . . . . ?
C11 C10 C49b C50b 71.1(10) . . . . ?

_refine_diff_density_max         1.303
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.087


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

data_Eind_Li_THF_LiBr2
_database_code_depnum_ccdc_archive 'CCDC 1543443'
_audit_update_record             
;
2017-04-11 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        '(Eind)Li LiBr complex'
_chemical_name_common            (Eind)Li(THF)(LiBr)]2
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H106 Br2 Li4 O2'
_chemical_formula_sum            'C64 H106 Br2 Li4 O2'
_chemical_formula_weight         1095.06

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.486(5)
_cell_length_b                   19.226(5)
_cell_length_c                   17.324(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6490(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    16172
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      32.57

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_F_000             2352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.521
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.289
_exptl_absorpt_coefficient_mu    1.287
_shelx_estimated_absorpt_T_min   0.554
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Fine-focus rotating anode'
_diffrn_measurement_device_type  'Rigaku AFC-10 with Saturn724'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            53484
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.351
_diffrn_reflns_theta_max         27.423
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7388
_reflns_number_gt                5422
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    SIR2002
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0559P)²+7.8206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7388
_refine_ls_number_parameters     337
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0762
_refine_ls_wR_factor_ref         0.1696
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
BR1 Br 0.59581(2) 0.20697(2) 0.21460(2) 0.04560(15) Uani 1 1 d . . . . .
C1 C 0.58923(17) 0.25005(17) 0.42911(19) 0.0301(7) Uani 1 1 d . . . . .
C2 C 0.60474(17) 0.31832(18) 0.45429(18) 0.0288(7) Uani 1 1 d . . . . .
C3 C 0.59531(18) 0.38494(17) 0.40593(18) 0.0308(7) Uani 1 1 d . . . . .
C4 C 0.60132(19) 0.44343(18) 0.46798(19) 0.0345(8) Uani 1 1 d . . . . .
H4A H 0.555049 0.459780 0.483065 0.041 Uiso 1 1 calc R U . . .
H4B H 0.627208 0.483407 0.446788 0.041 Uiso 1 1 calc R U . . .
C5 C 0.63960(18) 0.41300(18) 0.5399(2) 0.0337(8) Uani 1 1 d . . . . .
C6 C 0.62990(17) 0.33518(17) 0.52820(19) 0.0289(7) Uani 1 1 d . . . . .
C7 C 0.64050(17) 0.28258(18) 0.58260(19) 0.0309(7) Uani 1 1 d . . . . .
H7 H 0.657408 0.293398 0.632607 0.037 Uiso 1 1 calc R U . . .
C8 C 0.62585(17) 0.21391(17) 0.56230(19) 0.0301(7) Uani 1 1 d . . . . .
C9 C 0.63256(19) 0.15012(19) 0.6128(2) 0.0363(8) Uani 1 1 d . . . . .
C10 C 0.5939(2) 0.0939(2) 0.5653(2) 0.0425(9) Uani 1 1 d . . . . .
H10A H 0.548448 0.084684 0.588622 0.051 Uiso 1 1 calc R U . . .
H10B H 0.620417 0.050023 0.565033 0.051 Uiso 1 1 calc R U . . .
C11 C 0.58487(19) 0.12122(18) 0.4810(2) 0.0372(8) Uani 1 1 d . . . . .
C12 C 0.60036(17) 0.19963(17) 0.48801(19) 0.0295(7) Uani 1 1 d . . . . .
C13 C 0.5255(2) 0.38677(19) 0.3645(2) 0.0424(9) Uani 1 1 d . . . . .
H13A H 0.520090 0.432982 0.340033 0.051 Uiso 1 1 calc R U . . .
H13B H 0.526164 0.351710 0.322659 0.051 Uiso 1 1 calc R U . . .
C14 C 0.4627(2) 0.3732(2) 0.4149(3) 0.0506(10) Uani 1 1 d . . . . .
H14A H 0.457634 0.411050 0.452323 0.061 Uiso 1 1 calc R U . . .
H14B H 0.468536 0.329044 0.442316 0.061 Uiso 1 1 calc R U . . .
H14C H 0.421668 0.370835 0.382289 0.061 Uiso 1 1 calc R U . . .
C15 C 0.6530(2) 0.38902(19) 0.3445(2) 0.0409(9) Uani 1 1 d . . . . .
H15A H 0.697559 0.382878 0.371084 0.049 Uiso 1 1 calc R U . . .
H15B H 0.647333 0.349332 0.308663 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6567(3) 0.4559(2) 0.2964(3) 0.0662(14) Uani 1 1 d . . . . .
H16A H 0.664483 0.495704 0.330682 0.079 Uiso 1 1 calc R U . . .
H16B H 0.613470 0.462331 0.268479 0.079 Uiso 1 1 calc R U . . .
H16C H 0.694614 0.452402 0.259442 0.079 Uiso 1 1 calc R U . . .
C17 C 0.6082(2) 0.4385(2) 0.6165(2) 0.0425(9) Uani 1 1 d . . . . .
H17A H 0.636917 0.420874 0.659392 0.051 Uiso 1 1 calc R U . . .
H17B H 0.610896 0.489944 0.617560 0.051 Uiso 1 1 calc R U . . .
C18 C 0.5337(2) 0.4172(2) 0.6318(2) 0.0536(11) Uani 1 1 d . . . . .
H18A H 0.529350 0.366615 0.627357 0.064 Uiso 1 1 calc R U . . .
H18B H 0.503590 0.439716 0.594009 0.064 Uiso 1 1 calc R U . . .
H18C H 0.520451 0.431757 0.683984 0.064 Uiso 1 1 calc R U . . .
C19 C 0.7160(2) 0.4350(2) 0.5366(2) 0.0449(9) Uani 1 1 d . . . . .
H19A H 0.734458 0.421070 0.485666 0.054 Uiso 1 1 calc R U . . .
H19B H 0.717937 0.486430 0.539104 0.054 Uiso 1 1 calc R U . . .
C20 C 0.7638(2) 0.4064(3) 0.5984(3) 0.0616(13) Uani 1 1 d . . . . .
H20A H 0.810118 0.424844 0.590496 0.074 Uiso 1 1 calc R U . . .
H20B H 0.764874 0.355504 0.595143 0.074 Uiso 1 1 calc R U . . .
H20C H 0.747093 0.420339 0.649512 0.074 Uiso 1 1 calc R U . . .
C21 C 0.5989(2) 0.1621(2) 0.6921(2) 0.0519(11) Uani 1 1 d . . . . .
H21A H 0.621990 0.201984 0.717320 0.062 Uiso 1 1 calc R U . . .
H21B H 0.550358 0.175238 0.683868 0.062 Uiso 1 1 calc R U . . .
C22 C 0.6011(3) 0.0999(3) 0.7475(3) 0.0761(16) Uani 1 1 d . . . . .
H22A H 0.579724 0.059473 0.722783 0.091 Uiso 1 1 calc R U . . .
H22B H 0.576090 0.111399 0.794863 0.091 Uiso 1 1 calc R U . . .
H22C H 0.648934 0.088993 0.760198 0.091 Uiso 1 1 calc R U . . .
C23 C 0.7092(2) 0.1273(2) 0.6191(2) 0.0498(10) Uani 1 1 d . . . . .
H23A H 0.710641 0.081880 0.646068 0.060 Uiso 1 1 calc R U . . .
H23B H 0.726744 0.119539 0.566140 0.060 Uiso 1 1 calc R U . . .
C24 C 0.7574(3) 0.1752(3) 0.6592(3) 0.0655(13) Uani 1 1 d . . . . .
H24A H 0.741080 0.183802 0.711866 0.079 Uiso 1 1 calc R U . . .
H24B H 0.759798 0.219367 0.631045 0.079 Uiso 1 1 calc R U . . .
H24C H 0.803182 0.154118 0.661183 0.079 Uiso 1 1 calc R U . . .
C25 C 0.5101(2) 0.1078(2) 0.4529(2) 0.0474(10) Uani 1 1 d . . . . .
H25A H 0.507861 0.118118 0.397001 0.057 Uiso 1 1 calc R U . . .
H25B H 0.499814 0.057747 0.459577 0.057 Uiso 1 1 calc R U . . .
C26 C 0.4546(2) 0.1495(3) 0.4934(3) 0.0631(13) Uani 1 1 d . . . . .
H26A H 0.463645 0.199273 0.486888 0.076 Uiso 1 1 calc R U . . .
H26B H 0.454385 0.137985 0.548520 0.076 Uiso 1 1 calc R U . . .
H26C H 0.409794 0.138091 0.470947 0.076 Uiso 1 1 calc R U . . .
C27 C 0.6364(2) 0.08804(19) 0.4244(2) 0.0445(10) Uani 1 1 d . . . . .
H27A H 0.631365 0.111314 0.373719 0.053 Uiso 1 1 calc R U . . .
H27B H 0.683379 0.097945 0.443256 0.053 Uiso 1 1 calc R U . . .
C28 C 0.6300(3) 0.0092(2) 0.4118(3) 0.0642(13) Uani 1 1 d . . . . .
H28A H 0.585126 -0.001321 0.389022 0.077 Uiso 1 1 calc R U . . .
H28B H 0.634296 -0.014828 0.461477 0.077 Uiso 1 1 calc R U . . .
H28C H 0.666381 -0.006593 0.376936 0.077 Uiso 1 1 calc R U . . .
O1 O 0.7519(2) 0.2212(8) 0.3547(8) 0.0455(10) Uani 0.529(15) 1 d D . P A 1
C29 C 0.7982(6) 0.1707(7) 0.3212(8) 0.0558(12) Uani 0.529(15) 1 d D . P A 1
H29A H 0.811247 0.184428 0.268074 0.067 Uiso 0.529(15) 1 calc R U P A 1
H29B H 0.776602 0.124088 0.319390 0.067 Uiso 0.529(15) 1 calc R U P A 1
C30 C 0.8597(5) 0.1702(8) 0.3730(8) 0.091(3) Uani 0.529(15) 1 d D . P A 1
H30A H 0.877570 0.122254 0.379053 0.110 Uiso 0.529(15) 1 calc R U P A 1
H30B H 0.896614 0.199753 0.351364 0.110 Uiso 0.529(15) 1 calc R U P A 1
C31 C 0.8368(6) 0.1973(8) 0.4466(7) 0.091(3) Uani 0.529(15) 1 d D . P A 1
H31A H 0.874334 0.222649 0.472844 0.110 Uiso 0.529(15) 1 calc R U P A 1
H31B H 0.820908 0.159168 0.480580 0.110 Uiso 0.529(15) 1 calc R U P A 1
C32 C 0.7788(6) 0.2456(6) 0.4278(7) 0.0558(12) Uani 0.529(15) 1 d D . P A 1
H32A H 0.743025 0.243679 0.468321 0.067 Uiso 0.529(15) 1 calc R U P A 1
H32B H 0.795424 0.294054 0.423185 0.067 Uiso 0.529(15) 1 calc R U P A 1
O1B O 0.7529(2) 0.2205(9) 0.3468(9) 0.0455(10) Uani 0.471(15) 1 d D . P A 2
C29B C 0.7890(7) 0.1672(7) 0.3040(8) 0.0558(12) Uani 0.471(15) 1 d D . P A 2
H29C H 0.792346 0.179784 0.248750 0.067 Uiso 0.471(15) 1 calc R U P A 2
H29D H 0.765072 0.121927 0.308522 0.067 Uiso 0.471(15) 1 calc R U P A 2
C30B C 0.8588(6) 0.1635(9) 0.3400(9) 0.091(3) Uani 0.471(15) 1 d D . P A 2
H30C H 0.875008 0.114727 0.342325 0.110 Uiso 0.471(15) 1 calc R U P A 2
H30D H 0.892209 0.191095 0.309648 0.110 Uiso 0.471(15) 1 calc R U P A 2
C31B C 0.8515(6) 0.1920(8) 0.4171(8) 0.091(3) Uani 0.471(15) 1 d D . P A 2
H31C H 0.894593 0.214692 0.433860 0.110 Uiso 0.471(15) 1 calc R U P A 2
H31D H 0.839677 0.154930 0.454446 0.110 Uiso 0.471(15) 1 calc R U P A 2
C32B C 0.7945(6) 0.2441(7) 0.4110(8) 0.0558(12) Uani 0.471(15) 1 d D . P A 2
H32C H 0.767258 0.245272 0.459185 0.067 Uiso 0.471(15) 1 calc R U P A 2
H32D H 0.813007 0.291168 0.400910 0.067 Uiso 0.471(15) 1 calc R U P A 2
LI1 Li 0.6578(3) 0.2320(4) 0.3349(4) 0.0450(16) Uani 1 1 d D . . . .
LI2 Li 0.5220(3) 0.2242(4) 0.3352(4) 0.0434(16) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
BR1 LI1 2.456(6) . ?
BR1 LI2 2.475(6) 4_655 ?
BR1 LI2 2.558(6) . ?
C1 C2 1.416(5) . ?
C1 C12 1.424(5) . ?
C1 LI1 2.138(7) . ?
C1 LI2 2.147(7) . ?
C2 C6 1.409(4) . ?
C2 C3 1.542(5) . ?
C3 C13 1.539(5) . ?
C3 C15 1.550(5) . ?
C3 C4 1.560(5) . ?
C4 C5 1.565(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.522(5) . ?
C5 C17 1.541(5) . ?
C5 C19 1.549(5) . ?
C6 C7 1.398(5) . ?
C7 C8 1.396(5) . ?
C7 H7 0.9500 . ?
C8 C12 1.407(5) . ?
C8 C9 1.512(5) . ?
C9 C21 1.540(5) . ?
C9 C10 1.553(5) . ?
C9 C23 1.561(6) . ?
C10 C11 1.560(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.542(5) . ?
C11 C27 1.543(5) . ?
C11 C25 1.557(5) . ?
C13 C14 1.524(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.534(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.532(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.522(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.534(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.489(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.519(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.537(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O1 C29 1.448(4) . ?
O1 C32 1.448(4) . ?
O1 LI1 1.877(7) . ?
C29 C30 1.498(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.449(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.498(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O1B C29B 1.448(4) . ?
O1B C32B 1.449(4) . ?
O1B LI1 1.878(7) . ?
C29B C30B 1.498(5) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C30B C31B 1.450(10) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.499(5) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
LI1 LI2 2.650(9) . ?
LI2 BR1 2.475(6) 4_655 ?
LI2 LI2 3.075(12) 4_655 ?

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
LI1 BR1 LI2 136.5(2) . 4_655 ?
LI1 BR1 LI2 63.8(2) . . ?
LI2 BR1 LI2 75.3(2) 4_655 . ?
C2 C1 C12 112.2(3) . . ?
C2 C1 LI1 104.6(3) . . ?
C12 C1 LI1 110.0(3) . . ?
C2 C1 LI2 125.4(3) . . ?
C12 C1 LI2 118.5(3) . . ?
LI1 C1 LI2 76.4(3) . . ?
C6 C2 C1 124.6(3) . . ?
C6 C2 C3 110.1(3) . . ?
C1 C2 C3 125.3(3) . . ?
C13 C3 C2 112.2(3) . . ?
C13 C3 C15 108.7(3) . . ?
C2 C3 C15 109.2(3) . . ?
C13 C3 C4 111.8(3) . . ?
C2 C3 C4 102.4(3) . . ?
C15 C3 C4 112.5(3) . . ?
C3 C4 C5 108.4(3) . . ?
C3 C4 H4A 110.0 . . ?
C5 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
C5 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 C17 112.2(3) . . ?
C6 C5 C19 112.5(3) . . ?
C17 C5 C19 109.0(3) . . ?
C6 C5 C4 101.7(3) . . ?
C17 C5 C4 112.2(3) . . ?
C19 C5 C4 109.1(3) . . ?
C7 C6 C2 119.8(3) . . ?
C7 C6 C5 127.1(3) . . ?
C2 C6 C5 113.0(3) . . ?
C8 C7 C6 119.0(3) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C12 119.2(3) . . ?
C7 C8 C9 127.1(3) . . ?
C12 C8 C9 113.7(3) . . ?
C8 C9 C21 111.0(3) . . ?
C8 C9 C10 102.4(3) . . ?
C21 C9 C10 111.8(3) . . ?
C8 C9 C23 110.6(3) . . ?
C21 C9 C23 112.8(3) . . ?
C10 C9 C23 107.8(3) . . ?
C9 C10 C11 108.5(3) . . ?
C9 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C12 C11 C27 109.1(3) . . ?
C12 C11 C25 111.7(3) . . ?
C27 C11 C25 110.0(3) . . ?
C12 C11 C10 103.5(3) . . ?
C27 C11 C10 112.5(3) . . ?
C25 C11 C10 110.0(3) . . ?
C8 C12 C1 125.2(3) . . ?
C8 C12 C11 109.4(3) . . ?
C1 C12 C11 125.4(3) . . ?
C14 C13 C3 116.0(3) . . ?
C14 C13 H13A 108.3 . . ?
C3 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
C3 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C3 116.7(3) . . ?
C16 C15 H15A 108.1 . . ?
C3 C15 H15A 108.1 . . ?
C16 C15 H15B 108.1 . . ?
C3 C15 H15B 108.1 . . ?
H15A C15 H15B 107.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C5 116.1(3) . . ?
C18 C17 H17A 108.3 . . ?
C5 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
C5 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C5 117.6(3) . . ?
C20 C19 H19A 107.9 . . ?
C5 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
C5 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C9 115.4(4) . . ?
C22 C21 H21A 108.4 . . ?
C9 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C9 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C9 117.5(4) . . ?
C24 C23 H23A 107.9 . . ?
C9 C23 H23A 107.9 . . ?
C24 C23 H23B 107.9 . . ?
C9 C23 H23B 107.9 . . ?
H23A C23 H23B 107.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C11 115.8(3) . . ?
C26 C25 H25A 108.3 . . ?
C11 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C11 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C11 116.4(4) . . ?
C28 C27 H27A 108.2 . . ?
C11 C27 H27A 108.2 . . ?
C28 C27 H27B 108.2 . . ?
C11 C27 H27B 108.2 . . ?
H27A C27 H27B 107.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 O1 C32 110.0(3) . . ?
C29 O1 LI1 127.6(9) . . ?
C32 O1 LI1 118.5(9) . . ?
O1 C29 C30 105.2(3) . . ?
O1 C29 H29A 110.7 . . ?
C30 C29 H29A 110.7 . . ?
O1 C29 H29B 110.7 . . ?
C30 C29 H29B 110.7 . . ?
H29A C29 H29B 108.8 . . ?
C31 C30 C29 106.1(3) . . ?
C31 C30 H30A 110.5 . . ?
C29 C30 H30A 110.5 . . ?
C31 C30 H30B 110.5 . . ?
C29 C30 H30B 110.5 . . ?
H30A C30 H30B 108.7 . . ?
C30 C31 C32 105.4(3) . . ?
C30 C31 H31A 110.7 . . ?
C32 C31 H31A 110.7 . . ?
C30 C31 H31B 110.7 . . ?
C32 C31 H31B 110.7 . . ?
H31A C31 H31B 108.8 . . ?
O1 C32 C31 105.2(3) . . ?
O1 C32 H32A 110.7 . . ?
C31 C32 H32A 110.7 . . ?
O1 C32 H32B 110.7 . . ?
C31 C32 H32B 110.7 . . ?
H32A C32 H32B 108.8 . . ?
C29B O1B C32B 110.0(3) . . ?
C29B O1B LI1 120.4(10) . . ?
C32B O1B LI1 126.9(10) . . ?
O1B C29B C30B 105.2(3) . . ?
O1B C29B H29C 110.7 . . ?
C30B C29B H29C 110.7 . . ?
O1B C29B H29D 110.7 . . ?
C30B C29B H29D 110.7 . . ?
H29C C29B H29D 108.8 . . ?
C31B C30B C29B 106.0(3) . . ?
C31B C30B H30C 110.5 . . ?
C29B C30B H30C 110.5 . . ?
C31B C30B H30D 110.5 . . ?
C29B C30B H30D 110.5 . . ?
H30C C30B H30D 108.7 . . ?
C30B C31B C32B 105.1(3) . . ?
C30B C31B H31C 110.7 . . ?
C32B C31B H31C 110.7 . . ?
C30B C31B H31D 110.7 . . ?
C32B C31B H31D 110.7 . . ?
H31C C31B H31D 108.8 . . ?
O1B C32B C31B 105.1(3) . . ?
O1B C32B H32C 110.7 . . ?
C31B C32B H32C 110.7 . . ?
O1B C32B H32D 110.7 . . ?
C31B C32B H32D 110.7 . . ?
H32C C32B H32D 108.8 . . ?
O1 LI1 C1 119.3(5) . . ?
O1B LI1 C1 123.5(6) . . ?
O1 LI1 BR1 127.9(5) . . ?
O1B LI1 BR1 123.8(6) . . ?
C1 LI1 BR1 111.9(3) . . ?
O1 LI1 LI2 165.6(6) . . ?
O1B LI1 LI2 168.1(6) . . ?
C1 LI1 LI2 51.9(2) . . ?
BR1 LI1 LI2 59.99(19) . . ?
C1 LI2 BR1 149.5(3) . 4_655 ?
C1 LI2 BR1 107.8(3) . . ?
BR1 LI2 BR1 102.7(2) 4_655 . ?
C1 LI2 LI1 51.6(2) . . ?
BR1 LI2 LI1 158.9(3) 4_655 . ?
BR1 LI2 LI1 56.23(19) . . ?
C1 LI2 LI2 153.8(4) . 4_655 ?
BR1 LI2 LI2 53.59(18) 4_655 4_655 ?
BR1 LI2 LI2 51.12(19) . 4_655 ?
LI1 LI2 LI2 106.0(3) . 4_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C1 C2 C6 1.4(5) . . . . ?
LI1 C1 C2 C6 -117.7(4) . . . . ?
LI2 C1 C2 C6 158.7(3) . . . . ?
C12 C1 C2 C3 -177.2(3) . . . . ?
LI1 C1 C2 C3 63.6(4) . . . . ?
LI2 C1 C2 C3 -19.9(5) . . . . ?
C6 C2 C3 C13 -133.3(3) . . . . ?
C1 C2 C3 C13 45.5(4) . . . . ?
C6 C2 C3 C15 106.2(3) . . . . ?
C1 C2 C3 C15 -75.0(4) . . . . ?
C6 C2 C3 C4 -13.3(4) . . . . ?
C1 C2 C3 C4 165.6(3) . . . . ?
C13 C3 C4 C5 140.9(3) . . . . ?
C2 C3 C4 C5 20.6(4) . . . . ?
C15 C3 C4 C5 -96.5(3) . . . . ?
C3 C4 C5 C6 -20.0(4) . . . . ?
C3 C4 C5 C17 -140.1(3) . . . . ?
C3 C4 C5 C19 99.0(3) . . . . ?
C1 C2 C6 C7 -0.6(5) . . . . ?
C3 C2 C6 C7 178.2(3) . . . . ?
C1 C2 C6 C5 -178.0(3) . . . . ?
C3 C2 C6 C5 0.8(4) . . . . ?
C17 C5 C6 C7 -45.2(5) . . . . ?
C19 C5 C6 C7 78.2(4) . . . . ?
C4 C5 C6 C7 -165.3(3) . . . . ?
C17 C5 C6 C2 132.0(3) . . . . ?
C19 C5 C6 C2 -104.6(3) . . . . ?
C4 C5 C6 C2 11.9(4) . . . . ?
C2 C6 C7 C8 0.1(5) . . . . ?
C5 C6 C7 C8 177.1(3) . . . . ?
C6 C7 C8 C12 -0.5(5) . . . . ?
C6 C7 C8 C9 -178.9(3) . . . . ?
C7 C8 C9 C21 48.3(5) . . . . ?
C12 C8 C9 C21 -130.2(4) . . . . ?
C7 C8 C9 C10 167.7(3) . . . . ?
C12 C8 C9 C10 -10.7(4) . . . . ?
C7 C8 C9 C23 -77.7(5) . . . . ?
C12 C8 C9 C23 103.9(4) . . . . ?
C8 C9 C10 C11 15.7(4) . . . . ?
C21 C9 C10 C11 134.6(3) . . . . ?
C23 C9 C10 C11 -100.9(3) . . . . ?
C9 C10 C11 C12 -15.2(4) . . . . ?
C9 C10 C11 C27 102.4(4) . . . . ?
C9 C10 C11 C25 -134.6(3) . . . . ?
C7 C8 C12 C1 1.6(5) . . . . ?
C9 C8 C12 C1 -179.9(3) . . . . ?
C7 C8 C12 C11 -177.2(3) . . . . ?
C9 C8 C12 C11 1.4(4) . . . . ?
C2 C1 C12 C8 -1.9(5) . . . . ?
LI1 C1 C12 C8 114.0(4) . . . . ?
LI2 C1 C12 C8 -160.9(3) . . . . ?
C2 C1 C12 C11 176.6(3) . . . . ?
LI1 C1 C12 C11 -67.4(4) . . . . ?
LI2 C1 C12 C11 17.6(5) . . . . ?
C27 C11 C12 C8 -111.3(3) . . . . ?
C25 C11 C12 C8 126.9(3) . . . . ?
C10 C11 C12 C8 8.6(4) . . . . ?
C27 C11 C12 C1 69.9(4) . . . . ?
C25 C11 C12 C1 -51.8(5) . . . . ?
C10 C11 C12 C1 -170.1(3) . . . . ?
C2 C3 C13 C14 51.0(4) . . . . ?
C15 C3 C13 C14 171.9(3) . . . . ?
C4 C3 C13 C14 -63.4(4) . . . . ?
C13 C3 C15 C16 63.7(4) . . . . ?
C2 C3 C15 C16 -173.6(4) . . . . ?
C4 C3 C15 C16 -60.6(5) . . . . ?
C6 C5 C17 C18 -50.9(4) . . . . ?
C19 C5 C17 C18 -176.3(3) . . . . ?
C4 C5 C17 C18 62.8(4) . . . . ?
C6 C5 C19 C20 -63.6(5) . . . . ?
C17 C5 C19 C20 61.6(4) . . . . ?
C4 C5 C19 C20 -175.7(3) . . . . ?
C8 C9 C21 C22 178.5(4) . . . . ?
C10 C9 C21 C22 64.8(5) . . . . ?
C23 C9 C21 C22 -56.8(5) . . . . ?
C8 C9 C23 C24 65.8(5) . . . . ?
C21 C9 C23 C24 -59.1(5) . . . . ?
C10 C9 C23 C24 177.0(4) . . . . ?
C12 C11 C25 C26 -46.8(5) . . . . ?
C27 C11 C25 C26 -168.0(3) . . . . ?
C10 C11 C25 C26 67.6(4) . . . . ?
C12 C11 C27 C28 178.4(3) . . . . ?
C25 C11 C27 C28 -58.8(4) . . . . ?
C10 C11 C27 C28 64.2(4) . . . . ?
C32 O1 C29 C30 -5.9(9) . . . . ?
LI1 O1 C29 C30 -163.2(11) . . . . ?
O1 C29 C30 C31 21.8(9) . . . . ?
C29 C30 C31 C32 -28.8(10) . . . . ?
C29 O1 C32 C31 -11.5(9) . . . . ?
LI1 O1 C32 C31 148.2(11) . . . . ?
C30 C31 C32 O1 24.9(9) . . . . ?
C32B O1B C29B C30B -5.7(9) . . . . ?
LI1 O1B C29B C30B -168.4(12) . . . . ?
O1B C29B C30B C31B 22.2(10) . . . . ?
C29B C30B C31B C32B -29.8(10) . . . . ?
C29B O1B C32B C31B -12.4(9) . . . . ?
LI1 O1B C32B C31B 148.9(13) . . . . ?
C30B C31B C32B O1B 26.1(9) . . . . ?
C29 O1 LI1 C1 137.2(8) . . . . ?
C32 O1 LI1 C1 -18.5(11) . . . . ?
C29 O1 LI1 BR1 -30.3(12) . . . . ?
C32 O1 LI1 BR1 174.1(6) . . . . ?
C29 O1 LI1 LI2 88(2) . . . . ?
C32 O1 LI1 LI2 -67(3) . . . . ?
C29B O1B LI1 C1 137.5(8) . . . . ?
C32B O1B LI1 C1 -22.1(14) . . . . ?
C29B O1B LI1 BR1 -30.8(12) . . . . ?
C32B O1B LI1 BR1 169.6(8) . . . . ?
C29B O1B LI1 LI2 74(3) . . . . ?
C32B O1B LI1 LI2 -86(3) . . . . ?

_refine_diff_density_max         0.537
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.067


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

data_Eind2Ge2Cl2
_database_code_depnum_ccdc_archive 'CCDC 1542496'
_audit_update_record             
;
2017-04-06 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        dichlorodigermene
_chemical_name_common            (Eind)ClGe=GeCl(Eind)
_chemical_melting_point          403-407
_chemical_formula_moiety         'C56 H90 Cl2 Ge2'
_chemical_formula_sum            'C56 H90 Cl2 Ge2'
_chemical_formula_weight         979.35

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.4792(3)
_cell_length_b                   10.5003(2)
_cell_length_c                   12.0496(3)
_cell_angle_alpha                97.829(2)
_cell_angle_beta                 93.325(2)
_cell_angle_gamma                97.830(2)
_cell_volume                     1297.30(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    12419
_cell_measurement_theta_min      3.6940
_cell_measurement_theta_max      31.5060

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    1.296
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   Empirical
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            30745
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.657
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7495
_reflns_number_gt                6614
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    SIR2011
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+1.6289P] 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         7495
_refine_ls_number_parameters     292
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.09781(2) 0.95376(2) 0.98449(2) 0.01265(7) Uani 0.9390(6) 1 d . . P A 1
Cl1 Cl 0.24071(17) 1.06844(12) 1.11530(12) 0.0190(2) Uani 0.9390(6) 1 d . U P A
1
Ge1B Ge 0.1048(3) 1.0387(3) 0.9768(3) 0.01265(7) Uani 0.0610(6) 1 d . . P A 2
Cl1B Cl 0.234(3) 1.042(2) 1.131(2) 0.026(4) Uani 0.0610(6) 1 d . U P A 2
C1 C 0.18299(19) 0.94154(19) 0.84192(17) 0.0122(4) Uani 1 1 d . . . . .
C2 C 0.20652(19) 1.03733(18) 0.77065(17) 0.0124(4) Uani 1 1 d . . . . .
C3 C 0.16453(19) 1.17281(18) 0.77781(17) 0.0128(4) Uani 1 1 d . . . . .
C4 C 0.2369(2) 1.23280(19) 0.68386(17) 0.0146(4) Uani 1 1 d . . . . .
H4A H 0.1792 1.2800 0.6421 0.017 Uiso 1 1 calc R U . . .
H4B H 0.3133 1.2951 0.7175 0.017 Uiso 1 1 calc R U . . .
C5 C 0.28008(19) 1.12186(18) 0.60298(17) 0.0129(4) Uani 1 1 d . . . . .
C6 C 0.27013(19) 1.01168(18) 0.67280(17) 0.0127(4) Uani 1 1 d . . . . .
C7 C 0.31327(19) 0.89270(19) 0.64432(17) 0.0140(4) Uani 1 1 d . . . . .
H7 H 0.3579 0.8767 0.5786 0.017 Uiso 1 1 calc R U . . .
C8 C 0.29028(19) 0.79788(19) 0.71326(17) 0.0130(4) Uani 1 1 d . . . . .
C9 C 0.33933(19) 0.66759(19) 0.69927(17) 0.0134(4) Uani 1 1 d . . . . .
C10 C 0.2637(2) 0.59646(19) 0.78502(17) 0.0142(4) Uani 1 1 d . . . . .
H10A H 0.3213 0.5478 0.8254 0.017 Uiso 1 1 calc R U . . .
H10B H 0.1908 0.5338 0.7454 0.017 Uiso 1 1 calc R U . . .
C11 C 0.21164(19) 0.69896(19) 0.87028(17) 0.0129(4) Uani 1 1 d . . . . .
C12 C 0.22379(19) 0.81902(18) 0.80988(17) 0.0128(4) Uani 1 1 d . . . . .
C13 C 0.0166(2) 1.1537(2) 0.74820(18) 0.0153(4) Uani 1 1 d . . . . .
H13A H -0.0016 1.1039 0.6717 0.018 Uiso 1 1 calc R U . . .
H13B H -0.0254 1.0996 0.8008 0.018 Uiso 1 1 calc R U . . .
C14 C -0.0467(2) 1.2763(2) 0.7516(2) 0.0235(5) Uani 1 1 d . . . . .
H14A H -0.0039 1.3331 0.7025 0.028 Uiso 1 1 calc R U . . .
H14B H -0.0385 1.3220 0.8288 0.028 Uiso 1 1 calc R U . . .
H14C H -0.1383 1.2527 0.7258 0.028 Uiso 1 1 calc R U . . .
C15 C 0.2014(2) 1.25795(19) 0.89313(18) 0.0151(4) Uani 1 1 d . . . . .
H15A H 0.1782 1.3455 0.8886 0.018 Uiso 1 1 calc R U . . .
H15B H 0.1491 1.2200 0.9496 0.018 Uiso 1 1 calc R U . . .
C16 C 0.3442(2) 1.2725(2) 0.93423(19) 0.0180(4) Uani 1 1 d . . . . .
H16A H 0.3717 1.1865 0.9290 0.022 Uiso 1 1 calc R U . . .
H16B H 0.3564 1.3147 1.0126 0.022 Uiso 1 1 calc R U . . .
H16C H 0.3959 1.3257 0.8875 0.022 Uiso 1 1 calc R U . . .
C17 C 0.1856(2) 1.0787(2) 0.49623(18) 0.0165(4) Uani 1 1 d . . . . .
H17A H 0.2151 1.0035 0.4514 0.020 Uiso 1 1 calc R U . . .
H17B H 0.0994 1.0482 0.5203 0.020 Uiso 1 1 calc R U . . .
C18 C 0.1705(3) 1.1810(2) 0.4198(2) 0.0263(5) Uani 1 1 d . . . . .
H18A H 0.2549 1.2123 0.3948 0.032 Uiso 1 1 calc R U . . .
H18B H 0.1356 1.2538 0.4611 0.032 Uiso 1 1 calc R U . . .
H18C H 0.1112 1.1425 0.3542 0.032 Uiso 1 1 calc R U . . .
C19 C 0.4176(2) 1.1578(2) 0.56632(19) 0.0170(4) Uani 1 1 d . . . . .
H19A H 0.4336 1.0891 0.5060 0.020 Uiso 1 1 calc R U . . .
H19B H 0.4209 1.2397 0.5338 0.020 Uiso 1 1 calc R U . . .
C20 C 0.5269(2) 1.1749(2) 0.6593(2) 0.0230(5) Uani 1 1 d . . . . .
H20A H 0.6093 1.2027 0.6291 0.028 Uiso 1 1 calc R U . . .
H20B H 0.5302 1.0921 0.6876 0.028 Uiso 1 1 calc R U . . .
H20C H 0.5112 1.2408 0.7208 0.028 Uiso 1 1 calc R U . . .
C21 C 0.3148(2) 0.5944(2) 0.57782(18) 0.0176(4) Uani 1 1 d . . . . .
H21A H 0.3731 0.6403 0.5296 0.021 Uiso 1 1 calc R U . . .
H21B H 0.3390 0.5064 0.5776 0.021 Uiso 1 1 calc R U . . .
C22 C 0.1771(2) 0.5802(2) 0.5251(2) 0.0266(5) Uani 1 1 d . . . . .
H22A H 0.1724 0.5350 0.4479 0.032 Uiso 1 1 calc R U . . .
H22B H 0.1516 0.6665 0.5243 0.032 Uiso 1 1 calc R U . . .
H22C H 0.1186 0.5300 0.5691 0.032 Uiso 1 1 calc R U . . .
C23 C 0.4865(2) 0.6941(2) 0.73270(19) 0.0175(4) Uani 1 1 d . . . . .
H23A H 0.5273 0.7543 0.6842 0.021 Uiso 1 1 calc R U . . .
H23B H 0.5003 0.7392 0.8111 0.021 Uiso 1 1 calc R U . . .
C24 C 0.5565(2) 0.5752(2) 0.7245(2) 0.0265(5) Uani 1 1 d . . . . .
H24A H 0.5523 0.5348 0.6459 0.032 Uiso 1 1 calc R U . . .
H24B H 0.5150 0.5125 0.7694 0.032 Uiso 1 1 calc R U . . .
H24C H 0.6470 0.6018 0.7531 0.032 Uiso 1 1 calc R U . . .
C25 C 0.0720(2) 0.6460(2) 0.89358(19) 0.0169(4) Uani 1 1 d . . . . .
H25A H 0.0703 0.5555 0.9090 0.020 Uiso 1 1 calc R U . . .
H25B H 0.0495 0.6981 0.9626 0.020 Uiso 1 1 calc R U . . .
C26 C -0.0316(2) 0.6467(2) 0.8004(2) 0.0224(5) Uani 1 1 d . . . . .
H26A H -0.1137 0.6006 0.8186 0.027 Uiso 1 1 calc R U . . .
H26B H -0.0063 0.6035 0.7294 0.027 Uiso 1 1 calc R U . . .
H26C H -0.0417 0.7367 0.7929 0.027 Uiso 1 1 calc R U . . .
C27 C 0.2978(2) 0.7297(2) 0.98285(18) 0.0157(4) Uani 1 1 d . . . . .
H27A H 0.3868 0.7622 0.9665 0.019 Uiso 1 1 calc R U . . .
H27B H 0.2659 0.8008 1.0312 0.019 Uiso 1 1 calc R U . . .
C28 C 0.3030(2) 0.6163(2) 1.0491(2) 0.0219(5) Uani 1 1 d . . . . .
H28A H 0.3472 0.5507 1.0075 0.026 Uiso 1 1 calc R U . . .
H28B H 0.2150 0.5776 1.0601 0.026 Uiso 1 1 calc R U . . .
H28C H 0.3504 0.6478 1.1224 0.026 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C1 1.9783(19) . ?
Ge1 Cl1 2.2124(15) . ?
Ge1 Ge1 2.4119(5) 2_577 ?
Ge1B C1 2.070(4) . ?
Ge1B Cl1B 2.23(3) . ?
Ge1B Ge1B 2.363(7) 2_577 ?
C1 C2 1.415(3) . ?
C1 C12 1.421(3) . ?
C2 C6 1.400(3) . ?
C2 C3 1.538(3) . ?
C3 C15 1.544(3) . ?
C3 C13 1.549(3) . ?
C3 C4 1.555(3) . ?
C4 C5 1.548(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.516(3) . ?
C5 C19 1.544(3) . ?
C5 C17 1.553(3) . ?
C6 C7 1.392(3) . ?
C7 C8 1.387(3) . ?
C7 H7 0.9500 . ?
C8 C12 1.399(3) . ?
C8 C9 1.518(3) . ?
C9 C21 1.548(3) . ?
C9 C10 1.548(3) . ?
C9 C23 1.549(3) . ?
C10 C11 1.561(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.534(3) . ?
C11 C25 1.549(3) . ?
C11 C27 1.555(3) . ?
C13 C14 1.523(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.529(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.525(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.529(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.523(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.527(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.518(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.526(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ge1 Cl1 106.85(7) . . ?
C1 Ge1 Ge1 125.05(6) . 2_577 ?
Cl1 Ge1 Ge1 103.96(5) . 2_577 ?
C1 Ge1B Cl1B 108.5(7) . . ?
C1 Ge1B Ge1B 119.8(2) . 2_577 ?
Cl1B Ge1B Ge1B 105.5(7) . 2_577 ?
C2 C1 C12 117.97(17) . . ?
C2 C1 Ge1 128.38(14) . . ?
C12 C1 Ge1 113.66(14) . . ?
C2 C1 Ge1B 103.03(16) . . ?
C12 C1 Ge1B 138.80(18) . . ?
C6 C2 C1 120.44(17) . . ?
C6 C2 C3 109.68(17) . . ?
C1 C2 C3 129.76(17) . . ?
C2 C3 C15 113.69(17) . . ?
C2 C3 C13 107.68(16) . . ?
C15 C3 C13 111.07(16) . . ?
C2 C3 C4 102.91(15) . . ?
C15 C3 C4 110.98(16) . . ?
C13 C3 C4 110.18(17) . . ?
C5 C4 C3 108.67(15) . . ?
C5 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C5 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.3 . . ?
C6 C5 C19 112.91(17) . . ?
C6 C5 C4 101.98(16) . . ?
C19 C5 C4 112.67(16) . . ?
C6 C5 C17 108.01(16) . . ?
C19 C5 C17 108.69(16) . . ?
C4 C5 C17 112.44(17) . . ?
C7 C6 C2 120.98(18) . . ?
C7 C6 C5 125.57(18) . . ?
C2 C6 C5 113.40(17) . . ?
C8 C7 C6 119.09(18) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C12 121.37(18) . . ?
C7 C8 C9 125.70(18) . . ?
C12 C8 C9 112.81(17) . . ?
C8 C9 C21 113.16(18) . . ?
C8 C9 C10 101.84(15) . . ?
C21 C9 C10 113.00(16) . . ?
C8 C9 C23 107.24(16) . . ?
C21 C9 C23 109.33(17) . . ?
C10 C9 C23 112.00(18) . . ?
C9 C10 C11 108.93(15) . . ?
C9 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 C25 114.85(17) . . ?
C12 C11 C27 109.59(16) . . ?
C25 C11 C27 109.29(17) . . ?
C12 C11 C10 102.41(16) . . ?
C25 C11 C10 109.19(16) . . ?
C27 C11 C10 111.38(16) . . ?
C8 C12 C1 120.09(18) . . ?
C8 C12 C11 110.64(16) . . ?
C1 C12 C11 129.21(18) . . ?
C14 C13 C3 116.75(17) . . ?
C14 C13 H13A 108.1 . . ?
C3 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
C3 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C3 114.84(17) . . ?
C16 C15 H15A 108.6 . . ?
C3 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C3 C15 H15B 108.6 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C5 116.53(18) . . ?
C18 C17 H17A 108.2 . . ?
C5 C17 H17A 108.2 . . ?
C18 C17 H17B 108.2 . . ?
C5 C17 H17B 108.2 . . ?
H17A C17 H17B 107.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C5 115.54(18) . . ?
C20 C19 H19A 108.4 . . ?
C5 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
C5 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C9 115.92(18) . . ?
C22 C21 H21A 108.3 . . ?
C9 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
C9 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C9 116.16(18) . . ?
C24 C23 H23A 108.2 . . ?
C9 C23 H23A 108.2 . . ?
C24 C23 H23B 108.2 . . ?
C9 C23 H23B 108.2 . . ?
H23A C23 H23B 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C11 115.86(18) . . ?
C26 C25 H25A 108.3 . . ?
C11 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C11 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C11 115.78(17) . . ?
C28 C27 H27A 108.3 . . ?
C11 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
C11 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C1 C2 C6 -1.1(3) . . . . ?
Ge1 C1 C2 C6 179.21(15) . . . . ?
Ge1B C1 C2 C6 174.71(19) . . . . ?
C12 C1 C2 C3 174.51(19) . . . . ?
Ge1 C1 C2 C3 -5.2(3) . . . . ?
Ge1B C1 C2 C3 -9.7(3) . . . . ?
C6 C2 C3 C15 -131.23(18) . . . . ?
C1 C2 C3 C15 52.8(3) . . . . ?
C6 C2 C3 C13 105.27(19) . . . . ?
C1 C2 C3 C13 -70.7(3) . . . . ?
C6 C2 C3 C4 -11.1(2) . . . . ?
C1 C2 C3 C4 172.9(2) . . . . ?
C2 C3 C4 C5 17.9(2) . . . . ?
C15 C3 C4 C5 139.84(17) . . . . ?
C13 C3 C4 C5 -96.72(19) . . . . ?
C3 C4 C5 C6 -17.6(2) . . . . ?
C3 C4 C5 C19 -138.90(18) . . . . ?
C3 C4 C5 C17 97.85(19) . . . . ?
C1 C2 C6 C7 -1.0(3) . . . . ?
C3 C2 C6 C7 -177.38(18) . . . . ?
C1 C2 C6 C5 176.55(18) . . . . ?
C3 C2 C6 C5 0.2(2) . . . . ?
C19 C5 C6 C7 -50.6(3) . . . . ?
C4 C5 C6 C7 -171.71(19) . . . . ?
C17 C5 C6 C7 69.7(2) . . . . ?
C19 C5 C6 C2 132.04(18) . . . . ?
C4 C5 C6 C2 10.9(2) . . . . ?
C17 C5 C6 C2 -107.75(19) . . . . ?
C2 C6 C7 C8 1.2(3) . . . . ?
C5 C6 C7 C8 -175.97(19) . . . . ?
C6 C7 C8 C12 0.6(3) . . . . ?
C6 C7 C8 C9 -175.09(19) . . . . ?
C7 C8 C9 C21 -48.6(3) . . . . ?
C12 C8 C9 C21 135.42(19) . . . . ?
C7 C8 C9 C10 -170.2(2) . . . . ?
C12 C8 C9 C10 13.8(2) . . . . ?
C7 C8 C9 C23 72.1(3) . . . . ?
C12 C8 C9 C23 -103.9(2) . . . . ?
C8 C9 C10 C11 -18.4(2) . . . . ?
C21 C9 C10 C11 -140.10(18) . . . . ?
C23 C9 C10 C11 95.89(19) . . . . ?
C9 C10 C11 C12 16.5(2) . . . . ?
C9 C10 C11 C25 138.64(18) . . . . ?
C9 C10 C11 C27 -100.57(19) . . . . ?
C7 C8 C12 C1 -2.7(3) . . . . ?
C9 C8 C12 C1 173.52(18) . . . . ?
C7 C8 C12 C11 179.93(18) . . . . ?
C9 C8 C12 C11 -3.9(2) . . . . ?
C2 C1 C12 C8 2.9(3) . . . . ?
Ge1 C1 C12 C8 -177.38(15) . . . . ?
Ge1B C1 C12 C8 -170.9(2) . . . . ?
C2 C1 C12 C11 179.71(19) . . . . ?
Ge1 C1 C12 C11 -0.5(3) . . . . ?
Ge1B C1 C12 C11 6.0(4) . . . . ?
C25 C11 C12 C8 -126.09(19) . . . . ?
C27 C11 C12 C8 110.46(19) . . . . ?
C10 C11 C12 C8 -7.9(2) . . . . ?
C25 C11 C12 C1 56.8(3) . . . . ?
C27 C11 C12 C1 -66.6(3) . . . . ?
C10 C11 C12 C1 175.0(2) . . . . ?
C2 C3 C13 C14 179.17(18) . . . . ?
C15 C3 C13 C14 54.1(2) . . . . ?
C4 C3 C13 C14 -69.3(2) . . . . ?
C2 C3 C15 C16 53.3(2) . . . . ?
C13 C3 C15 C16 174.93(17) . . . . ?
C4 C3 C15 C16 -62.1(2) . . . . ?
C6 C5 C17 C18 174.07(19) . . . . ?
C19 C5 C17 C18 -63.1(2) . . . . ?
C4 C5 C17 C18 62.3(2) . . . . ?
C6 C5 C19 C20 -47.8(2) . . . . ?
C4 C5 C19 C20 67.1(2) . . . . ?
C17 C5 C19 C20 -167.64(18) . . . . ?
C8 C9 C21 C22 -50.9(2) . . . . ?
C10 C9 C21 C22 64.1(2) . . . . ?
C23 C9 C21 C22 -170.39(18) . . . . ?
C8 C9 C23 C24 -179.85(19) . . . . ?
C21 C9 C23 C24 -56.8(2) . . . . ?
C10 C9 C23 C24 69.2(2) . . . . ?
C12 C11 C25 C26 39.9(2) . . . . ?
C27 C11 C25 C26 163.49(18) . . . . ?
C10 C11 C25 C26 -74.4(2) . . . . ?
C12 C11 C27 C28 -176.02(17) . . . . ?
C25 C11 C27 C28 57.3(2) . . . . ?
C10 C11 C27 C28 -63.4(2) . . . . ?

_refine_diff_density_max         0.953
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.082


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

data_TbbBromogermylenoid
_database_code_depnum_ccdc_archive 'CCDC 1542499'
_audit_update_record             
;
2017-04-06 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Tbb-germylemoid
_chemical_name_common            '[K(crypt-222)][(Tbb)GeBr2]'
_chemical_melting_point          408-409
_chemical_formula_moiety         
'C24 H49 Br2 Ge Si4, C18 H36 K N2 O6, 0.5(C6 H6) '
_chemical_formula_sum            'C45 H88 Br2 Ge K N2 O6 Si4'
_chemical_formula_weight         1137.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.8021(2)
_cell_length_b                   12.4235(3)
_cell_length_c                   20.4661(4)
_cell_angle_alpha                79.3220(10)
_cell_angle_beta                 78.1190(10)
_cell_angle_gamma                85.9350(10)
_cell_volume                     2884.00(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    103
_cell_measurement_reflns_used    51886
_cell_measurement_theta_min      1.033
_cell_measurement_theta_max      25.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             1194
_exptl_transmission_factor_min   0.816
_exptl_transmission_factor_max   0.939
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.113
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Fine-focus rotating-anode'
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            51886
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.033
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             10639
_reflns_number_gt                9545
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       CrystalClear
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  
;Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+54.3273P] 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         10639
_refine_ls_number_parameters     565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2200
_refine_ls_wR_factor_gt          0.2161
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_restrained_S_all      1.200
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.39730(9) 0.22580(8) 0.70041(5) 0.0299(2) Uani 1 1 d . . . . .
Br1 Br 0.39766(8) 0.42392(8) 0.65348(5) 0.0328(2) Uani 1 1 d . . . . .
Br2 Br 0.60864(10) 0.19350(8) 0.66025(5) 0.0420(3) Uani 1 1 d . . . . .
C1 C 0.3809(7) 0.2212(6) 0.8023(4) 0.0189(16) Uani 1 1 d . . . . .
C2 C 0.4330(7) 0.2836(6) 0.8385(4) 0.0178(16) Uani 1 1 d . . . . .
C3 C 0.3975(7) 0.2733(7) 0.9095(4) 0.0202(17) Uani 1 1 d . . . . .
H1 H 0.4303 0.3193 0.9325 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3159(7) 0.1982(7) 0.9473(4) 0.0216(17) Uani 1 1 d . . . . .
C5 C 0.2700(7) 0.1339(7) 0.9114(4) 0.0226(17) Uani 1 1 d . . . . .
H2 H 0.2170 0.0796 0.9359 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2981(7) 0.1453(6) 0.8409(4) 0.0184(16) Uani 1 1 d . . . . .
C7 C 0.5229(7) 0.3681(6) 0.8062(4) 0.0186(16) Uani 1 1 d . . . . .
H3 H 0.5386 0.3653 0.7566 0.022 Uiso 1 1 calc R U . . .
Si1 Si 0.6658(2) 0.3278(2) 0.83437(12) 0.0249(5) Uani 1 1 d . . . . .
C8 C 0.7229(9) 0.1942(9) 0.8082(6) 0.045(3) Uani 1 1 d . . . . .
H4 H 0.7898 0.1679 0.8289 0.067 Uiso 1 1 calc R U . . .
H5 H 0.7465 0.2047 0.7587 0.067 Uiso 1 1 calc R U . . .
H6 H 0.6622 0.1401 0.8233 0.067 Uiso 1 1 calc R U . . .
C9 C 0.7743(8) 0.4352(8) 0.7951(5) 0.034(2) Uani 1 1 d . . . . .
H7 H 0.8495 0.4104 0.8067 0.051 Uiso 1 1 calc R U . . .
H8 H 0.7487 0.5033 0.8122 0.051 Uiso 1 1 calc R U . . .
H9 H 0.7817 0.4483 0.7457 0.051 Uiso 1 1 calc R U . . .
C10 C 0.6604(8) 0.3056(9) 0.9277(5) 0.038(2) Uani 1 1 d . . . . .
H10 H 0.6073 0.2469 0.9504 0.058 Uiso 1 1 calc R U . . .
H11 H 0.6330 0.3734 0.9449 0.058 Uiso 1 1 calc R U . . .
H12 H 0.7380 0.2849 0.9368 0.058 Uiso 1 1 calc R U . . .
Si2 Si 0.4641(2) 0.51160(19) 0.81371(12) 0.0241(5) Uani 1 1 d . . . . .
C11 C 0.5385(9) 0.6130(7) 0.7401(5) 0.034(2) Uani 1 1 d . . . . .
H13 H 0.5157 0.6020 0.6984 0.050 Uiso 1 1 calc R U . . .
H14 H 0.6226 0.6021 0.7355 0.050 Uiso 1 1 calc R U . . .
H15 H 0.5158 0.6876 0.7480 0.050 Uiso 1 1 calc R U . . .
C12 C 0.4834(10) 0.5556(8) 0.8935(5) 0.042(2) Uani 1 1 d . . . . .
H16 H 0.4449 0.6275 0.8966 0.062 Uiso 1 1 calc R U . . .
H17 H 0.5662 0.5604 0.8927 0.062 Uiso 1 1 calc R U . . .
H18 H 0.4493 0.5019 0.9328 0.062 Uiso 1 1 calc R U . . .
C13 C 0.3058(8) 0.5202(8) 0.8149(5) 0.034(2) Uani 1 1 d . . . . .
H19 H 0.2676 0.4619 0.8499 0.052 Uiso 1 1 calc R U . . .
H20 H 0.2922 0.5115 0.7706 0.052 Uiso 1 1 calc R U . . .
H21 H 0.2740 0.5917 0.8250 0.052 Uiso 1 1 calc R U . . .
C14 C 0.2784(8) 0.1852(8) 1.0245(4) 0.028(2) Uani 1 1 d . . . . .
C15 C 0.3359(10) 0.2684(9) 1.0535(5) 0.039(2) Uani 1 1 d . . . . .
H22 H 0.3077 0.2593 1.1026 0.059 Uiso 1 1 calc R U . . .
H23 H 0.3164 0.3430 1.0323 0.059 Uiso 1 1 calc R U . . .
H24 H 0.4202 0.2559 1.0439 0.059 Uiso 1 1 calc R U . . .
C16 C 0.1464(9) 0.2041(9) 1.0432(5) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.1227 0.1994 1.0924 0.058 Uiso 1 1 calc R U . . .
H26 H 0.1077 0.1480 1.0286 0.058 Uiso 1 1 calc R U . . .
H27 H 0.1247 0.2768 1.0203 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3121(10) 0.0701(9) 1.0553(5) 0.041(3) Uani 1 1 d . . . . .
H28 H 0.3961 0.0583 1.0424 0.062 Uiso 1 1 calc R U . . .
H29 H 0.2725 0.0171 1.0387 0.062 Uiso 1 1 calc R U . . .
H30 H 0.2896 0.0605 1.1049 0.062 Uiso 1 1 calc R U . . .
C18 C 0.2381(7) 0.0672(6) 0.8100(4) 0.0183(16) Uani 1 1 d . . . . .
H31 H 0.2695 0.0868 0.7602 0.022 Uiso 1 1 calc R U . . .
Si3 Si 0.2901(2) -0.07905(19) 0.83203(13) 0.0247(5) Uani 1 1 d . . . . .
C19 C 0.4437(8) -0.0791(9) 0.8413(6) 0.040(2) Uani 1 1 d . . . . .
H32 H 0.4856 -0.0249 0.8050 0.060 Uiso 1 1 calc R U . . .
H33 H 0.4798 -0.1520 0.8385 0.060 Uiso 1 1 calc R U . . .
H34 H 0.4465 -0.0603 0.8854 0.060 Uiso 1 1 calc R U . . .
C20 C 0.2023(10) -0.1577(9) 0.9108(6) 0.047(3) Uani 1 1 d . . . . .
H35 H 0.1978 -0.1181 0.9485 0.071 Uiso 1 1 calc R U . . .
H36 H 0.2392 -0.2303 0.9216 0.071 Uiso 1 1 calc R U . . .
H37 H 0.1241 -0.1660 0.9036 0.071 Uiso 1 1 calc R U . . .
C21 C 0.2848(9) -0.1467(8) 0.7585(6) 0.039(2) Uani 1 1 d . . . . .
H38 H 0.2046 -0.1641 0.7597 0.059 Uiso 1 1 calc R U . . .
H39 H 0.3329 -0.2144 0.7611 0.059 Uiso 1 1 calc R U . . .
H40 H 0.3141 -0.0971 0.7161 0.059 Uiso 1 1 calc R U . . .
Si4 Si 0.07972(19) 0.10342(19) 0.81788(11) 0.0202(5) Uani 1 1 d . . . . .
C22 C 0.0682(8) 0.2452(8) 0.7693(5) 0.035(2) Uani 1 1 d . . . . .
H41 H -0.0125 0.2630 0.7651 0.052 Uiso 1 1 calc R U . . .
H42 H 0.1170 0.2498 0.7239 0.052 Uiso 1 1 calc R U . . .
H43 H 0.0941 0.2974 0.7932 0.052 Uiso 1 1 calc R U . . .
C23 C -0.0026(7) 0.1016(8) 0.9058(4) 0.0279(19) Uani 1 1 d . . . . .
H44 H 0.0235 0.1603 0.9247 0.042 Uiso 1 1 calc R U . . .
H45 H 0.0108 0.0307 0.9338 0.042 Uiso 1 1 calc R U . . .
H46 H -0.0854 0.1129 0.9053 0.042 Uiso 1 1 calc R U . . .
C24 C 0.0094(7) 0.0065(8) 0.7798(5) 0.0275(19) Uani 1 1 d . . . . .
H47 H 0.0077 -0.0663 0.8082 0.041 Uiso 1 1 calc R U . . .
H48 H 0.0537 0.0021 0.7342 0.041 Uiso 1 1 calc R U . . .
H49 H -0.0699 0.0331 0.7769 0.041 Uiso 1 1 calc R U . . .
K1 K 0.87133(16) 0.72432(14) 0.57629(9) 0.0220(4) Uani 1 1 d . . . . .
N1 N 1.0819(6) 0.6409(6) 0.6364(4) 0.0263(16) Uani 1 1 d . . . . .
C25 C 1.1872(7) 0.6579(8) 0.5829(5) 0.030(2) Uani 1 1 d . . . . .
H50 H 1.1928 0.6009 0.5543 0.036 Uiso 1 1 calc R U . . .
H51 H 1.2557 0.6479 0.6047 0.036 Uiso 1 1 calc R U . . .
C26 C 1.1911(8) 0.7685(8) 0.5382(5) 0.0290(19) Uani 1 1 d . . . . .
H52 H 1.1856 0.8267 0.5660 0.035 Uiso 1 1 calc R U . . .
H53 H 1.2655 0.7753 0.5051 0.035 Uiso 1 1 calc R U . . .
O1 O 1.0961(5) 0.7811(5) 0.5030(3) 0.0246(13) Uani 1 1 d . . . . .
C27 C 1.1029(7) 0.8806(7) 0.4558(5) 0.0267(19) Uani 1 1 d . . . . .
H54 H 1.1808 0.8855 0.4262 0.032 Uiso 1 1 calc R U . . .
H55 H 1.0909 0.9434 0.4803 0.032 Uiso 1 1 calc R U . . .
C28 C 1.0130(8) 0.8855(8) 0.4136(4) 0.028(2) Uani 1 1 d . . . . .
H56 H 1.0215 0.9526 0.3786 0.034 Uiso 1 1 calc R U . . .
H57 H 1.0233 0.8213 0.3904 0.034 Uiso 1 1 calc R U . . .
O2 O 0.8995(5) 0.8860(5) 0.4560(3) 0.0248(13) Uani 1 1 d . . . . .
C29 C 0.8117(8) 0.8929(9) 0.4173(4) 0.032(2) Uani 1 1 d . . . . .
H58 H 0.8146 0.8257 0.3974 0.038 Uiso 1 1 calc R U . . .
H59 H 0.8245 0.9564 0.3797 0.038 Uiso 1 1 calc R U . . .
C30 C 0.6955(8) 0.9058(7) 0.4618(5) 0.029(2) Uani 1 1 d . . . . .
H60 H 0.6950 0.9709 0.4834 0.035 Uiso 1 1 calc R U . . .
H61 H 0.6356 0.9187 0.4335 0.035 Uiso 1 1 calc R U . . .
N2 N 0.6657(6) 0.8085(6) 0.5153(4) 0.0253(16) Uani 1 1 d . . . . .
C31 C 1.0881(8) 0.7011(8) 0.6909(5) 0.031(2) Uani 1 1 d . . . . .
H62 H 1.1212 0.7735 0.6703 0.037 Uiso 1 1 calc R U . . .
H63 H 1.1414 0.6604 0.7190 0.037 Uiso 1 1 calc R U . . .
C32 C 0.9738(9) 0.7181(8) 0.7356(5) 0.033(2) Uani 1 1 d . . . . .
H64 H 0.9356 0.6471 0.7527 0.040 Uiso 1 1 calc R U . . .
H65 H 0.9851 0.7489 0.7750 0.040 Uiso 1 1 calc R U . . .
O3 O 0.9025(5) 0.7920(5) 0.6976(3) 0.0244(13) Uani 1 1 d . . . . .
C33 C 0.7955(8) 0.8187(8) 0.7389(5) 0.030(2) Uani 1 1 d . . . . .
H66 H 0.8105 0.8531 0.7761 0.036 Uiso 1 1 calc R U . . .
H67 H 0.7527 0.7510 0.7594 0.036 Uiso 1 1 calc R U . . .
C34 C 0.7249(9) 0.8953(8) 0.6973(5) 0.033(2) Uani 1 1 d . . . . .
H68 H 0.6528 0.9178 0.7267 0.040 Uiso 1 1 calc R U . . .
H69 H 0.7688 0.9618 0.6755 0.040 Uiso 1 1 calc R U . . .
O4 O 0.6981(5) 0.8443(5) 0.6486(3) 0.0248(13) Uani 1 1 d . . . . .
C35 C 0.6109(8) 0.9045(8) 0.6144(5) 0.034(2) Uani 1 1 d . . . . .
H70 H 0.6431 0.9738 0.5869 0.040 Uiso 1 1 calc R U . . .
H71 H 0.5434 0.9232 0.6485 0.040 Uiso 1 1 calc R U . . .
C36 C 0.5727(8) 0.8380(8) 0.5695(5) 0.031(2) Uani 1 1 d . . . . .
H72 H 0.5390 0.7699 0.5977 0.038 Uiso 1 1 calc R U . . .
H73 H 0.5108 0.8799 0.5485 0.038 Uiso 1 1 calc R U . . .
C37 C 1.0717(8) 0.5238(7) 0.6642(5) 0.0276(19) Uani 1 1 d . . . . .
H74 H 1.0201 0.5150 0.7094 0.033 Uiso 1 1 calc R U . . .
H75 H 1.1490 0.4924 0.6703 0.033 Uiso 1 1 calc R U . . .
C38 C 1.0249(8) 0.4598(7) 0.6204(5) 0.0279(19) Uani 1 1 d . . . . .
H76 H 1.0753 0.4680 0.5748 0.033 Uiso 1 1 calc R U . . .
H77 H 1.0238 0.3810 0.6408 0.033 Uiso 1 1 calc R U . . .
O5 O 0.9102(5) 0.4999(5) 0.6149(3) 0.0252(13) Uani 1 1 d . . . . .
C39 C 0.8540(8) 0.4270(7) 0.5865(5) 0.0277(19) Uani 1 1 d . . . . .
H78 H 0.8516 0.3532 0.6150 0.033 Uiso 1 1 calc R U . . .
H79 H 0.8977 0.4207 0.5405 0.033 Uiso 1 1 calc R U . . .
C40 C 0.7339(7) 0.4698(7) 0.5828(4) 0.0244(18) Uani 1 1 d . . . . .
H80 H 0.6933 0.4180 0.5649 0.029 Uiso 1 1 calc R U . . .
H81 H 0.6905 0.4766 0.6288 0.029 Uiso 1 1 calc R U . . .
O6 O 0.7377(5) 0.5740(5) 0.5397(3) 0.0260(13) Uani 1 1 d . . . . .
C41 C 0.6239(8) 0.6106(7) 0.5287(5) 0.029(2) Uani 1 1 d . . . . .
H82 H 0.5715 0.6141 0.5728 0.035 Uiso 1 1 calc R U . . .
H83 H 0.5929 0.5578 0.5066 0.035 Uiso 1 1 calc R U . . .
C42 C 0.6286(8) 0.7216(8) 0.4846(5) 0.030(2) Uani 1 1 d . . . . .
H84 H 0.6828 0.7173 0.4412 0.037 Uiso 1 1 calc R U . . .
H85 H 0.5508 0.7423 0.4743 0.037 Uiso 1 1 calc R U . . .
C43 C 0.0353(11) 0.5124(13) 0.9310(7) 0.066(4) Uani 1 1 d . . . . .
H86 H 0.0601 0.5230 0.8831 0.079 Uiso 1 1 calc R U . . .
C44 C 0.1070(11) 0.5360(11) 0.9708(8) 0.066(4) Uani 1 1 d . . . . .
H87 H 0.1830 0.5595 0.9502 0.080 Uiso 1 1 calc R U . . .
C45 C 0.0719(12) 0.5265(13) 1.0396(7) 0.067(4) Uani 1 1 d . . . . .
H88 H 0.1212 0.5467 1.0663 0.080 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C1 2.044(8) . ?
Ge1 Br1 2.4708(14) . ?
Ge1 Br2 2.4888(15) . ?
C1 C2 1.414(11) . ?
C1 C6 1.416(11) . ?
C2 C3 1.410(11) . ?
C2 C7 1.508(11) . ?
C3 C4 1.397(11) . ?
C3 H1 0.9500 . ?
C4 C5 1.382(12) . ?
C4 C14 1.532(11) . ?
C5 C6 1.396(11) . ?
C5 H2 0.9500 . ?
C6 C18 1.534(11) . ?
C7 Si2 1.889(8) . ?
C7 Si1 1.897(8) . ?
C7 H3 1.0000 . ?
Si1 C10 1.867(10) . ?
Si1 C9 1.867(9) . ?
Si1 C8 1.876(11) . ?
C8 H4 0.9800 . ?
C8 H5 0.9800 . ?
C8 H6 0.9800 . ?
C9 H7 0.9800 . ?
C9 H8 0.9800 . ?
C9 H9 0.9800 . ?
C10 H10 0.9800 . ?
C10 H11 0.9800 . ?
C10 H12 0.9800 . ?
Si2 C13 1.860(10) . ?
Si2 C12 1.875(10) . ?
Si2 C11 1.881(9) . ?
C11 H13 0.9800 . ?
C11 H14 0.9800 . ?
C11 H15 0.9800 . ?
C12 H16 0.9800 . ?
C12 H17 0.9800 . ?
C12 H18 0.9800 . ?
C13 H19 0.9800 . ?
C13 H20 0.9800 . ?
C13 H21 0.9800 . ?
C14 C17 1.512(14) . ?
C14 C16 1.538(13) . ?
C14 C15 1.540(12) . ?
C15 H22 0.9800 . ?
C15 H23 0.9800 . ?
C15 H24 0.9800 . ?
C16 H25 0.9800 . ?
C16 H26 0.9800 . ?
C16 H27 0.9800 . ?
C17 H28 0.9800 . ?
C17 H29 0.9800 . ?
C17 H30 0.9800 . ?
C18 Si4 1.873(8) . ?
C18 Si3 1.880(8) . ?
C18 H31 1.0000 . ?
Si3 C19 1.861(10) . ?
Si3 C21 1.868(10) . ?
Si3 C20 1.871(11) . ?
C19 H32 0.9800 . ?
C19 H33 0.9800 . ?
C19 H34 0.9800 . ?
C20 H35 0.9800 . ?
C20 H36 0.9800 . ?
C20 H37 0.9800 . ?
C21 H38 0.9800 . ?
C21 H39 0.9800 . ?
C21 H40 0.9800 . ?
Si4 C23 1.858(8) . ?
Si4 C22 1.867(10) . ?
Si4 C24 1.871(9) . ?
C22 H41 0.9800 . ?
C22 H42 0.9800 . ?
C22 H43 0.9800 . ?
C23 H44 0.9800 . ?
C23 H45 0.9800 . ?
C23 H46 0.9800 . ?
C24 H47 0.9800 . ?
C24 H48 0.9800 . ?
C24 H49 0.9800 . ?
K1 O4 2.781(6) . ?
K1 O5 2.786(6) . ?
K1 O6 2.820(6) . ?
K1 O1 2.832(6) . ?
K1 O2 2.851(6) . ?
K1 O3 2.864(6) . ?
K1 N2 2.990(7) . ?
K1 N1 3.030(7) . ?
N1 C37 1.465(11) . ?
N1 C31 1.469(12) . ?
N1 C25 1.475(11) . ?
C25 C26 1.501(12) . ?
C25 H50 0.9900 . ?
C25 H51 0.9900 . ?
C26 O1 1.439(10) . ?
C26 H52 0.9900 . ?
C26 H53 0.9900 . ?
O1 C27 1.417(10) . ?
C27 C28 1.491(13) . ?
C27 H54 0.9900 . ?
C27 H55 0.9900 . ?
C28 O2 1.439(10) . ?
C28 H56 0.9900 . ?
C28 H57 0.9900 . ?
O2 C29 1.418(11) . ?
C29 C30 1.498(13) . ?
C29 H58 0.9900 . ?
C29 H59 0.9900 . ?
C30 N2 1.481(11) . ?
C30 H60 0.9900 . ?
C30 H61 0.9900 . ?
N2 C36 1.470(11) . ?
N2 C42 1.478(12) . ?
C31 C32 1.492(14) . ?
C31 H62 0.9900 . ?
C31 H63 0.9900 . ?
C32 O3 1.431(11) . ?
C32 H64 0.9900 . ?
C32 H65 0.9900 . ?
O3 C33 1.422(11) . ?
C33 C34 1.486(14) . ?
C33 H66 0.9900 . ?
C33 H67 0.9900 . ?
C34 O4 1.374(11) . ?
C34 H68 0.9900 . ?
C34 H69 0.9900 . ?
O4 C35 1.449(11) . ?
C35 C36 1.496(14) . ?
C35 H70 0.9900 . ?
C35 H71 0.9900 . ?
C36 H72 0.9900 . ?
C36 H73 0.9900 . ?
C37 C38 1.506(12) . ?
C37 H74 0.9900 . ?
C37 H75 0.9900 . ?
C38 O5 1.428(10) . ?
C38 H76 0.9900 . ?
C38 H77 0.9900 . ?
O5 C39 1.428(10) . ?
C39 C40 1.490(12) . ?
C39 H78 0.9900 . ?
C39 H79 0.9900 . ?
C40 O6 1.424(10) . ?
C40 H80 0.9900 . ?
C40 H81 0.9900 . ?
O6 C41 1.436(11) . ?
C41 C42 1.500(12) . ?
C41 H82 0.9900 . ?
C41 H83 0.9900 . ?
C42 H84 0.9900 . ?
C42 H85 0.9900 . ?
C43 C45 1.365(17) 2_567 ?
C43 C44 1.369(19) . ?
C43 H86 0.9500 . ?
C44 C45 1.368(19) . ?
C44 H87 0.9500 . ?
C45 C43 1.365(17) 2_567 ?
C45 H88 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ge1 Br1 103.5(2) . . ?
C1 Ge1 Br2 103.9(2) . . ?
Br1 Ge1 Br2 95.13(5) . . ?
C2 C1 C6 116.9(7) . . ?
C2 C1 Ge1 131.0(6) . . ?
C6 C1 Ge1 112.0(6) . . ?
C3 C2 C1 120.2(7) . . ?
C3 C2 C7 115.3(7) . . ?
C1 C2 C7 124.4(7) . . ?
C4 C3 C2 122.5(7) . . ?
C4 C3 H1 118.7 . . ?
C2 C3 H1 118.7 . . ?
C5 C4 C3 116.5(8) . . ?
C5 C4 C14 120.7(7) . . ?
C3 C4 C14 122.8(7) . . ?
C4 C5 C6 122.9(8) . . ?
C4 C5 H2 118.6 . . ?
C6 C5 H2 118.6 . . ?
C5 C6 C1 120.9(7) . . ?
C5 C6 C18 115.5(7) . . ?
C1 C6 C18 123.6(7) . . ?
C2 C7 Si2 111.7(5) . . ?
C2 C7 Si1 111.3(5) . . ?
Si2 C7 Si1 116.3(4) . . ?
C2 C7 H3 105.5 . . ?
Si2 C7 H3 105.5 . . ?
Si1 C7 H3 105.5 . . ?
C10 Si1 C9 106.5(5) . . ?
C10 Si1 C8 104.9(5) . . ?
C9 Si1 C8 109.1(5) . . ?
C10 Si1 C7 116.0(4) . . ?
C9 Si1 C7 110.4(4) . . ?
C8 Si1 C7 109.7(4) . . ?
Si1 C8 H4 109.5 . . ?
Si1 C8 H5 109.5 . . ?
H4 C8 H5 109.5 . . ?
Si1 C8 H6 109.5 . . ?
H4 C8 H6 109.5 . . ?
H5 C8 H6 109.5 . . ?
Si1 C9 H7 109.5 . . ?
Si1 C9 H8 109.5 . . ?
H7 C9 H8 109.5 . . ?
Si1 C9 H9 109.5 . . ?
H7 C9 H9 109.5 . . ?
H8 C9 H9 109.5 . . ?
Si1 C10 H10 109.5 . . ?
Si1 C10 H11 109.5 . . ?
H10 C10 H11 109.5 . . ?
Si1 C10 H12 109.5 . . ?
H10 C10 H12 109.5 . . ?
H11 C10 H12 109.5 . . ?
C13 Si2 C12 106.5(5) . . ?
C13 Si2 C11 109.1(5) . . ?
C12 Si2 C11 107.6(5) . . ?
C13 Si2 C7 109.9(4) . . ?
C12 Si2 C7 113.3(4) . . ?
C11 Si2 C7 110.3(4) . . ?
Si2 C11 H13 109.5 . . ?
Si2 C11 H14 109.5 . . ?
H13 C11 H14 109.5 . . ?
Si2 C11 H15 109.5 . . ?
H13 C11 H15 109.5 . . ?
H14 C11 H15 109.5 . . ?
Si2 C12 H16 109.5 . . ?
Si2 C12 H17 109.5 . . ?
H16 C12 H17 109.5 . . ?
Si2 C12 H18 109.5 . . ?
H16 C12 H18 109.5 . . ?
H17 C12 H18 109.5 . . ?
Si2 C13 H19 109.5 . . ?
Si2 C13 H20 109.5 . . ?
H19 C13 H20 109.5 . . ?
Si2 C13 H21 109.5 . . ?
H19 C13 H21 109.5 . . ?
H20 C13 H21 109.5 . . ?
C17 C14 C4 108.2(8) . . ?
C17 C14 C16 110.0(8) . . ?
C4 C14 C16 109.3(7) . . ?
C17 C14 C15 109.4(8) . . ?
C4 C14 C15 111.9(7) . . ?
C16 C14 C15 108.0(8) . . ?
C14 C15 H22 109.5 . . ?
C14 C15 H23 109.5 . . ?
H22 C15 H23 109.5 . . ?
C14 C15 H24 109.5 . . ?
H22 C15 H24 109.5 . . ?
H23 C15 H24 109.5 . . ?
C14 C16 H25 109.5 . . ?
C14 C16 H26 109.5 . . ?
H25 C16 H26 109.5 . . ?
C14 C16 H27 109.5 . . ?
H25 C16 H27 109.5 . . ?
H26 C16 H27 109.5 . . ?
C14 C17 H28 109.5 . . ?
C14 C17 H29 109.5 . . ?
H28 C17 H29 109.5 . . ?
C14 C17 H30 109.5 . . ?
H28 C17 H30 109.5 . . ?
H29 C17 H30 109.5 . . ?
C6 C18 Si4 111.0(5) . . ?
C6 C18 Si3 112.0(5) . . ?
Si4 C18 Si3 120.8(4) . . ?
C6 C18 H31 103.6 . . ?
Si4 C18 H31 103.6 . . ?
Si3 C18 H31 103.6 . . ?
C19 Si3 C21 108.4(5) . . ?
C19 Si3 C20 109.6(5) . . ?
C21 Si3 C20 109.3(5) . . ?
C19 Si3 C18 108.2(4) . . ?
C21 Si3 C18 106.9(4) . . ?
C20 Si3 C18 114.2(4) . . ?
Si3 C19 H32 109.5 . . ?
Si3 C19 H33 109.5 . . ?
H32 C19 H33 109.5 . . ?
Si3 C19 H34 109.5 . . ?
H32 C19 H34 109.5 . . ?
H33 C19 H34 109.5 . . ?
Si3 C20 H35 109.5 . . ?
Si3 C20 H36 109.5 . . ?
H35 C20 H36 109.5 . . ?
Si3 C20 H37 109.5 . . ?
H35 C20 H37 109.5 . . ?
H36 C20 H37 109.5 . . ?
Si3 C21 H38 109.5 . . ?
Si3 C21 H39 109.5 . . ?
H38 C21 H39 109.5 . . ?
Si3 C21 H40 109.5 . . ?
H38 C21 H40 109.5 . . ?
H39 C21 H40 109.5 . . ?
C23 Si4 C22 108.1(5) . . ?
C23 Si4 C24 107.4(4) . . ?
C22 Si4 C24 109.5(4) . . ?
C23 Si4 C18 115.4(4) . . ?
C22 Si4 C18 106.6(4) . . ?
C24 Si4 C18 109.8(4) . . ?
Si4 C22 H41 109.5 . . ?
Si4 C22 H42 109.5 . . ?
H41 C22 H42 109.5 . . ?
Si4 C22 H43 109.5 . . ?
H41 C22 H43 109.5 . . ?
H42 C22 H43 109.5 . . ?
Si4 C23 H44 109.5 . . ?
Si4 C23 H45 109.5 . . ?
H44 C23 H45 109.5 . . ?
Si4 C23 H46 109.5 . . ?
H44 C23 H46 109.5 . . ?
H45 C23 H46 109.5 . . ?
Si4 C24 H47 109.5 . . ?
Si4 C24 H48 109.5 . . ?
H47 C24 H48 109.5 . . ?
Si4 C24 H49 109.5 . . ?
H47 C24 H49 109.5 . . ?
H48 C24 H49 109.5 . . ?
O4 K1 O5 122.93(18) . . ?
O4 K1 O6 100.64(19) . . ?
O5 K1 O6 60.00(18) . . ?
O4 K1 O1 131.29(18) . . ?
O5 K1 O1 99.25(18) . . ?
O6 K1 O1 122.62(18) . . ?
O4 K1 O2 94.16(17) . . ?
O5 K1 O2 139.14(18) . . ?
O6 K1 O2 99.88(18) . . ?
O1 K1 O2 59.82(17) . . ?
O4 K1 O3 59.20(18) . . ?
O5 K1 O3 98.09(18) . . ?
O6 K1 O3 137.86(18) . . ?
O1 K1 O3 94.60(18) . . ?
O2 K1 O3 116.99(18) . . ?
O4 K1 N2 61.30(19) . . ?
O5 K1 N2 120.41(19) . . ?
O6 K1 N2 61.10(19) . . ?
O1 K1 N2 119.24(19) . . ?
O2 K1 N2 60.11(18) . . ?
O3 K1 N2 119.95(19) . . ?
O4 K1 N1 119.1(2) . . ?
O5 K1 N1 60.09(19) . . ?
O6 K1 N1 119.3(2) . . ?
O1 K1 N1 59.95(19) . . ?
O2 K1 N1 119.07(19) . . ?
O3 K1 N1 60.33(19) . . ?
N2 K1 N1 179.2(2) . . ?
C37 N1 C31 109.5(7) . . ?
C37 N1 C25 109.4(7) . . ?
C31 N1 C25 110.0(7) . . ?
C37 N1 K1 109.5(5) . . ?
C31 N1 K1 109.0(5) . . ?
C25 N1 K1 109.4(5) . . ?
N1 C25 C26 114.3(8) . . ?
N1 C25 H50 108.7 . . ?
C26 C25 H50 108.7 . . ?
N1 C25 H51 108.7 . . ?
C26 C25 H51 108.7 . . ?
H50 C25 H51 107.6 . . ?
O1 C26 C25 109.2(7) . . ?
O1 C26 H52 109.8 . . ?
C25 C26 H52 109.8 . . ?
O1 C26 H53 109.8 . . ?
C25 C26 H53 109.8 . . ?
H52 C26 H53 108.3 . . ?
C27 O1 C26 110.7(6) . . ?
C27 O1 K1 115.9(5) . . ?
C26 O1 K1 119.3(5) . . ?
O1 C27 C28 109.9(7) . . ?
O1 C27 H54 109.7 . . ?
C28 C27 H54 109.7 . . ?
O1 C27 H55 109.7 . . ?
C28 C27 H55 109.7 . . ?
H54 C27 H55 108.2 . . ?
O2 C28 C27 109.7(7) . . ?
O2 C28 H56 109.7 . . ?
C27 C28 H56 109.7 . . ?
O2 C28 H57 109.7 . . ?
C27 C28 H57 109.7 . . ?
H56 C28 H57 108.2 . . ?
C29 O2 C28 111.2(6) . . ?
C29 O2 K1 116.0(5) . . ?
C28 O2 K1 114.5(5) . . ?
O2 C29 C30 109.6(7) . . ?
O2 C29 H58 109.8 . . ?
C30 C29 H58 109.8 . . ?
O2 C29 H59 109.8 . . ?
C30 C29 H59 109.8 . . ?
H58 C29 H59 108.2 . . ?
N2 C30 C29 112.6(7) . . ?
N2 C30 H60 109.1 . . ?
C29 C30 H60 109.1 . . ?
N2 C30 H61 109.1 . . ?
C29 C30 H61 109.1 . . ?
H60 C30 H61 107.8 . . ?
C36 N2 C42 110.5(7) . . ?
C36 N2 C30 109.9(7) . . ?
C42 N2 C30 108.7(7) . . ?
C36 N2 K1 108.3(5) . . ?
C42 N2 K1 108.8(5) . . ?
C30 N2 K1 110.6(5) . . ?
N1 C31 C32 113.8(7) . . ?
N1 C31 H62 108.8 . . ?
C32 C31 H62 108.8 . . ?
N1 C31 H63 108.8 . . ?
C32 C31 H63 108.8 . . ?
H62 C31 H63 107.7 . . ?
O3 C32 C31 109.1(8) . . ?
O3 C32 H64 109.9 . . ?
C31 C32 H64 109.9 . . ?
O3 C32 H65 109.9 . . ?
C31 C32 H65 109.9 . . ?
H64 C32 H65 108.3 . . ?
C33 O3 C32 111.9(7) . . ?
C33 O3 K1 112.4(5) . . ?
C32 O3 K1 114.2(5) . . ?
O3 C33 C34 109.8(7) . . ?
O3 C33 H66 109.7 . . ?
C34 C33 H66 109.7 . . ?
O3 C33 H67 109.7 . . ?
C34 C33 H67 109.7 . . ?
H66 C33 H67 108.2 . . ?
O4 C34 C33 109.3(7) . . ?
O4 C34 H68 109.8 . . ?
C33 C34 H68 109.8 . . ?
O4 C34 H69 109.8 . . ?
C33 C34 H69 109.8 . . ?
H68 C34 H69 108.3 . . ?
C34 O4 C35 113.1(7) . . ?
C34 O4 K1 118.8(5) . . ?
C35 O4 K1 119.0(5) . . ?
O4 C35 C36 110.7(7) . . ?
O4 C35 H70 109.5 . . ?
C36 C35 H70 109.5 . . ?
O4 C35 H71 109.5 . . ?
C36 C35 H71 109.5 . . ?
H70 C35 H71 108.1 . . ?
N2 C36 C35 114.2(7) . . ?
N2 C36 H72 108.7 . . ?
C35 C36 H72 108.7 . . ?
N2 C36 H73 108.7 . . ?
C35 C36 H73 108.7 . . ?
H72 C36 H73 107.6 . . ?
N1 C37 C38 113.8(7) . . ?
N1 C37 H74 108.8 . . ?
C38 C37 H74 108.8 . . ?
N1 C37 H75 108.8 . . ?
C38 C37 H75 108.8 . . ?
H74 C37 H75 107.7 . . ?
O5 C38 C37 109.2(7) . . ?
O5 C38 H76 109.8 . . ?
C37 C38 H76 109.8 . . ?
O5 C38 H77 109.8 . . ?
C37 C38 H77 109.8 . . ?
H76 C38 H77 108.3 . . ?
C38 O5 C39 110.6(6) . . ?
C38 O5 K1 118.8(5) . . ?
C39 O5 K1 118.0(5) . . ?
O5 C39 C40 109.3(7) . . ?
O5 C39 H78 109.8 . . ?
C40 C39 H78 109.8 . . ?
O5 C39 H79 109.8 . . ?
C40 C39 H79 109.8 . . ?
H78 C39 H79 108.3 . . ?
O6 C40 C39 109.7(7) . . ?
O6 C40 H80 109.7 . . ?
C39 C40 H80 109.7 . . ?
O6 C40 H81 109.7 . . ?
C39 C40 H81 109.7 . . ?
H80 C40 H81 108.2 . . ?
C40 O6 C41 110.5(6) . . ?
C40 O6 K1 113.1(5) . . ?
C41 O6 K1 117.3(5) . . ?
O6 C41 C42 110.1(7) . . ?
O6 C41 H82 109.6 . . ?
C42 C41 H82 109.6 . . ?
O6 C41 H83 109.6 . . ?
C42 C41 H83 109.6 . . ?
H82 C41 H83 108.2 . . ?
N2 C42 C41 114.0(7) . . ?
N2 C42 H84 108.8 . . ?
C41 C42 H84 108.8 . . ?
N2 C42 H85 108.8 . . ?
C41 C42 H85 108.8 . . ?
H84 C42 H85 107.7 . . ?
C45 C43 C44 119.6(13) 2_567 . ?
C45 C43 H86 120.2 2_567 . ?
C44 C43 H86 120.2 . . ?
C45 C44 C43 121.6(12) . . ?
C45 C44 H87 119.2 . . ?
C43 C44 H87 119.2 . . ?
C43 C45 C44 118.7(13) 2_567 . ?
C43 C45 H88 120.6 2_567 . ?
C44 C45 H88 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.5(11) . . . . ?
Ge1 C1 C2 C3 172.8(6) . . . . ?
C6 C1 C2 C7 179.9(7) . . . . ?
Ge1 C1 C2 C7 -3.8(12) . . . . ?
C1 C2 C3 C4 3.8(12) . . . . ?
C7 C2 C3 C4 -179.3(7) . . . . ?
C2 C3 C4 C5 -0.6(12) . . . . ?
C2 C3 C4 C14 178.9(8) . . . . ?
C3 C4 C5 C6 -2.9(12) . . . . ?
C14 C4 C5 C6 177.6(8) . . . . ?
C4 C5 C6 C1 3.1(13) . . . . ?
C4 C5 C6 C18 -179.7(8) . . . . ?
C2 C1 C6 C5 0.2(11) . . . . ?
Ge1 C1 C6 C5 -176.8(6) . . . . ?
C2 C1 C6 C18 -176.7(7) . . . . ?
Ge1 C1 C6 C18 6.2(9) . . . . ?
C3 C2 C7 Si2 -65.8(8) . . . . ?
C1 C2 C7 Si2 110.9(8) . . . . ?
C3 C2 C7 Si1 66.0(8) . . . . ?
C1 C2 C7 Si1 -117.2(7) . . . . ?
C2 C7 Si1 C10 -57.6(7) . . . . ?
Si2 C7 Si1 C10 71.9(6) . . . . ?
C2 C7 Si1 C9 -178.7(6) . . . . ?
Si2 C7 Si1 C9 -49.3(6) . . . . ?
C2 C7 Si1 C8 61.0(7) . . . . ?
Si2 C7 Si1 C8 -169.5(5) . . . . ?
C2 C7 Si2 C13 -30.1(7) . . . . ?
Si1 C7 Si2 C13 -159.3(5) . . . . ?
C2 C7 Si2 C12 88.9(7) . . . . ?
Si1 C7 Si2 C12 -40.4(6) . . . . ?
C2 C7 Si2 C11 -150.4(6) . . . . ?
Si1 C7 Si2 C11 80.3(5) . . . . ?
C5 C4 C14 C17 62.1(11) . . . . ?
C3 C4 C14 C17 -117.4(9) . . . . ?
C5 C4 C14 C16 -57.7(11) . . . . ?
C3 C4 C14 C16 122.8(9) . . . . ?
C5 C4 C14 C15 -177.3(8) . . . . ?
C3 C4 C14 C15 3.2(13) . . . . ?
C5 C6 C18 Si4 70.1(8) . . . . ?
C1 C6 C18 Si4 -112.8(7) . . . . ?
C5 C6 C18 Si3 -68.1(8) . . . . ?
C1 C6 C18 Si3 109.0(7) . . . . ?
C6 C18 Si3 C19 -30.8(7) . . . . ?
Si4 C18 Si3 C19 -164.4(5) . . . . ?
C6 C18 Si3 C21 -147.4(6) . . . . ?
Si4 C18 Si3 C21 78.9(6) . . . . ?
C6 C18 Si3 C20 91.6(7) . . . . ?
Si4 C18 Si3 C20 -42.1(7) . . . . ?
C6 C18 Si4 C23 -58.5(7) . . . . ?
Si3 C18 Si4 C23 75.5(6) . . . . ?
C6 C18 Si4 C22 61.5(6) . . . . ?
Si3 C18 Si4 C22 -164.4(5) . . . . ?
C6 C18 Si4 C24 -180.0(5) . . . . ?
Si3 C18 Si4 C24 -45.9(6) . . . . ?
C37 N1 C25 C26 164.5(8) . . . . ?
C31 N1 C25 C26 -75.1(10) . . . . ?
K1 N1 C25 C26 44.6(9) . . . . ?
N1 C25 C26 O1 -62.1(10) . . . . ?
C25 C26 O1 C27 -174.9(7) . . . . ?
C25 C26 O1 K1 46.9(9) . . . . ?
C26 O1 C27 C28 172.7(7) . . . . ?
K1 O1 C27 C28 -47.4(8) . . . . ?
O1 C27 C28 O2 63.3(9) . . . . ?
C27 C28 O2 C29 178.8(7) . . . . ?
C27 C28 O2 K1 -47.3(8) . . . . ?
C28 O2 C29 C30 -173.8(7) . . . . ?
K1 O2 C29 C30 53.1(9) . . . . ?
O2 C29 C30 N2 -64.9(10) . . . . ?
C29 C30 N2 C36 161.6(8) . . . . ?
C29 C30 N2 C42 -77.4(9) . . . . ?
C29 C30 N2 K1 42.1(9) . . . . ?
C37 N1 C31 C32 -77.7(9) . . . . ?
C25 N1 C31 C32 162.0(8) . . . . ?
K1 N1 C31 C32 42.0(9) . . . . ?
N1 C31 C32 O3 -67.9(10) . . . . ?
C31 C32 O3 C33 -175.2(7) . . . . ?
C31 C32 O3 K1 55.7(8) . . . . ?
C32 O3 C33 C34 180.0(7) . . . . ?
K1 O3 C33 C34 -50.0(8) . . . . ?
O3 C33 C34 O4 63.3(9) . . . . ?
C33 C34 O4 C35 168.6(7) . . . . ?
C33 C34 O4 K1 -44.7(9) . . . . ?
C34 O4 C35 C36 -171.7(8) . . . . ?
K1 O4 C35 C36 41.6(9) . . . . ?
C42 N2 C36 C35 165.9(8) . . . . ?
C30 N2 C36 C35 -74.1(10) . . . . ?
K1 N2 C36 C35 46.8(9) . . . . ?
O4 C35 C36 N2 -61.0(10) . . . . ?
C31 N1 C37 C38 160.4(7) . . . . ?
C25 N1 C37 C38 -79.0(9) . . . . ?
K1 N1 C37 C38 40.9(9) . . . . ?
N1 C37 C38 O5 -62.3(10) . . . . ?
C37 C38 O5 C39 -167.5(7) . . . . ?
C37 C38 O5 K1 51.3(8) . . . . ?
C38 O5 C39 C40 178.8(7) . . . . ?
K1 O5 C39 C40 -39.7(8) . . . . ?
O5 C39 C40 O6 61.7(9) . . . . ?
C39 C40 O6 C41 172.8(7) . . . . ?
C39 C40 O6 K1 -53.3(8) . . . . ?
C40 O6 C41 C42 178.6(7) . . . . ?
K1 O6 C41 C42 46.9(9) . . . . ?
C36 N2 C42 C41 -73.5(10) . . . . ?
C30 N2 C42 C41 165.8(8) . . . . ?
K1 N2 C42 C41 45.2(9) . . . . ?
O6 C41 C42 N2 -63.6(10) . . . . ?
C45 C43 C44 C45 -3(3) 2_567 . . . ?
C43 C44 C45 C43 3(3) . . . 2_567 ?

_refine_diff_density_max         1.708
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.157


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

data_Eind2GeBr2
_database_code_depnum_ccdc_archive 'CCDC 1543095'
_audit_update_record             
;
2017-04-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        dibromogermane
_chemical_name_common            (Eind)2GeBr2
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H90 Br2 Ge'
_chemical_formula_sum            'C56 H90 Br2 Ge'
_chemical_formula_weight         995.68

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.6306(9)
_cell_length_b                   26.7797(16)
_cell_length_c                   18.0740(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.352(8)
_cell_angle_gamma                90
_cell_volume                     5044.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9517
_cell_measurement_theta_min      3.0260
_cell_measurement_theta_max      28.5770

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_F_000             2112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.047
_exptl_absorpt_coefficient_mu    2.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            44270
_diffrn_reflns_av_unetI/netI     0.1486
_diffrn_reflns_av_R_equivalents  0.1967
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.757
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             9587
_reflns_number_gt                7439
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     0.934
_reflns_Friedel_fraction_full    0.938

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

_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_structure_solution    SIR2011
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1808P)²+34.5014P] 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_abs_structure_details 
;
 Flack x determined using 2182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9587
_refine_ls_number_parameters     548
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1166
_refine_ls_wR_factor_ref         0.3219
_refine_ls_wR_factor_gt          0.2992
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.4717(3) 0.12594(5) 0.5113(2) 0.0360(4) Uani 1 1 d . . . . .
Br1 Br 0.2877(4) 0.12572(10) 0.4142(2) 0.0781(8) Uani 1 1 d . . . . .
Br2 Br 0.5821(4) 0.07402(8) 0.4397(2) 0.0752(8) Uani 1 1 d . . . . .
C8 C 0.5821(15) 0.0740(6) 0.7373(11) 0.044(4) Uani 1 1 d . . . . .
C39 C 0.663(2) 0.2113(8) 0.4190(10) 0.055(5) Uani 1 1 d . . . . .
C13 C 0.1636(17) 0.0590(8) 0.5460(11) 0.053(4) Uani 1 1 d . . . . .
H13A H 0.135193 0.065656 0.593999 0.064 Uiso 1 1 calc R U . . .
H13B H 0.195732 0.090866 0.529019 0.064 Uiso 1 1 calc R U . . .
C31 C 0.318(2) 0.2176(7) 0.6072(12) 0.052(5) Uani 1 1 d . . . . .
C7 C 0.4821(14) 0.0433(6) 0.7499(9) 0.038(3) Uani 1 1 d . . . . .
H7 H 0.476826 0.033131 0.799531 0.045 Uiso 1 1 calc R U . . .
C5 C 0.2941(17) -0.0107(7) 0.6918(11) 0.050(4) Uani 1 1 d . . . . .
C30 C 0.4357(19) 0.2283(7) 0.5685(11) 0.049(4) Uani 1 1 d . . . . .
C6 C 0.3913(15) 0.0280(5) 0.6886(10) 0.038(3) Uani 1 1 d . . . . .
C16 C 0.4268(18) -0.0290(8) 0.4966(13) 0.058(5) Uani 1 1 d . . . . .
H16A H 0.494480 -0.013932 0.534694 0.087 Uiso 1 1 calc R U . . .
H16B H 0.454838 -0.030338 0.448089 0.087 Uiso 1 1 calc R U . . .
H16C H 0.409466 -0.062964 0.512252 0.087 Uiso 1 1 calc R U . . .
C34 C 0.479(2) 0.2807(8) 0.5844(11) 0.060(5) Uani 1 1 d . . . . .
C32 C 0.303(2) 0.2678(7) 0.6485(13) 0.066(6) Uani 1 1 d . . . . .
H32A H 0.215311 0.281060 0.629541 0.080 Uiso 1 1 calc R U . . .
H32B H 0.311196 0.261178 0.703174 0.080 Uiso 1 1 calc R U . . .
C40 C 0.586(2) 0.2286(7) 0.4839(10) 0.051(4) Uani 1 1 d . . . . .
C9 C 0.6906(17) 0.0927(8) 0.7990(10) 0.052(4) Uani 1 1 d . . . . .
C11 C 0.7317(13) 0.1091(6) 0.6680(8) 0.033(3) Uani 1 1 d . . . . .
C38 C 0.714(2) 0.2624(8) 0.3968(13) 0.063(5) Uani 1 1 d . . . . .
H38A H 0.651928 0.277230 0.354309 0.075 Uiso 1 1 calc R U . . .
H38B H 0.796635 0.257689 0.380649 0.075 Uiso 1 1 calc R U . . .
C3 C 0.2747(18) 0.0221(7) 0.5615(10) 0.050(4) Uani 1 1 d . . . . .
C15 C 0.3059(18) 0.0021(7) 0.4884(10) 0.046(4) Uani 1 1 d . . . . .
H15A H 0.232650 -0.018491 0.462839 0.056 Uiso 1 1 calc R U . . .
H15B H 0.313679 0.030723 0.454976 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5887(14) 0.0896(5) 0.6641(9) 0.033(3) Uani 1 1 d . . . . .
C2 C 0.3913(15) 0.0468(5) 0.6162(8) 0.032(3) Uani 1 1 d . . . . .
C10 C 0.7972(15) 0.1000(9) 0.7525(11) 0.055(5) Uani 1 1 d . . . . .
H10A H 0.852385 0.069963 0.756545 0.066 Uiso 1 1 calc R U . . .
H10B H 0.851446 0.128988 0.772029 0.066 Uiso 1 1 calc R U . . .
C25 C 0.7408(19) 0.1636(7) 0.6465(10) 0.052(4) Uani 1 1 d . . . . .
H25A H 0.695967 0.184166 0.678820 0.063 Uiso 1 1 calc R U . . .
H25B H 0.695433 0.168119 0.593591 0.063 Uiso 1 1 calc R U . . .
C36 C 0.623(2) 0.2758(6) 0.5042(10) 0.052(4) Uani 1 1 d . . . . .
C17 C 0.1937(18) 0.0088(8) 0.7363(14) 0.061(5) Uani 1 1 d . . . . .
H17A H 0.239587 0.021348 0.785790 0.073 Uiso 1 1 calc R U . . .
H17B H 0.147924 0.037357 0.708482 0.073 Uiso 1 1 calc R U . . .
C35 C 0.565(2) 0.3018(8) 0.5572(11) 0.059(5) Uani 1 1 d . . . . .
H35 H 0.591461 0.334843 0.572039 0.071 Uiso 1 1 calc R U . . .
C14 C 0.048(2) 0.0427(10) 0.4876(14) 0.074(6) Uani 1 1 d . . . . .
H14A H 0.013019 0.011645 0.504078 0.111 Uiso 1 1 calc R U . . .
H14B H 0.073195 0.037312 0.439007 0.111 Uiso 1 1 calc R U . . .
H14C H -0.018363 0.068806 0.482023 0.111 Uiso 1 1 calc R U . . .
C53 C 0.561(2) 0.1918(9) 0.3524(12) 0.077(6) Uani 1 1 d D U . . .
H53A H 0.534059 0.158191 0.365868 0.092 Uiso 1 1 calc R U . . .
H53B H 0.603139 0.187748 0.308456 0.092 Uiso 1 1 calc R U . . .
C20 C 0.485(3) -0.0751(9) 0.7131(18) 0.081(7) Uani 1 1 d . . . . .
H20A H 0.470649 -0.091616 0.663767 0.122 Uiso 1 1 calc R U . . .
H20B H 0.526739 -0.098597 0.752033 0.122 Uiso 1 1 calc R U . . .
H20C H 0.541113 -0.046059 0.712328 0.122 Uiso 1 1 calc R U . . .
C21 C 0.657(2) 0.1431(9) 0.8302(11) 0.062(5) Uani 1 1 d . . . . .
H21A H 0.638955 0.167241 0.787949 0.074 Uiso 1 1 calc R U . . .
H21B H 0.732665 0.155359 0.866366 0.074 Uiso 1 1 calc R U . . .
C4 C 0.2390(19) -0.0211(7) 0.6081(13) 0.061(6) Uani 1 1 d . . . . .
H4A H 0.274479 -0.052721 0.592546 0.074 Uiso 1 1 calc R U . . .
H4B H 0.144480 -0.024374 0.599996 0.074 Uiso 1 1 calc R U . . .
C23 C 0.730(2) 0.0576(9) 0.8639(13) 0.077(6) Uani 1 1 d D U . . .
H23A H 0.654481 0.051658 0.887518 0.093 Uiso 1 1 calc R U . . .
H23B H 0.796421 0.074067 0.902012 0.093 Uiso 1 1 calc R U . . .
C44 C 0.238(3) 0.1640(8) 0.7068(14) 0.071(6) Uani 1 1 d . . . . .
H44A H 0.209328 0.194801 0.727677 0.107 Uiso 1 1 calc R U . . .
H44B H 0.268555 0.140409 0.747890 0.107 Uiso 1 1 calc R U . . .
H44C H 0.166114 0.149105 0.671345 0.107 Uiso 1 1 calc R U . . .
C41 C 0.197(2) 0.2071(8) 0.5459(14) 0.067(6) Uani 1 1 d . . . . .
H41A H 0.204645 0.173004 0.526190 0.081 Uiso 1 1 calc R U . . .
H41B H 0.121920 0.207005 0.570974 0.081 Uiso 1 1 calc R U . . .
C33 C 0.398(2) 0.3060(8) 0.6375(15) 0.070(6) Uani 1 1 d . . . . .
C27 C 0.7962(16) 0.0772(7) 0.6163(13) 0.054(5) Uani 1 1 d . . . . .
H27A H 0.762545 0.087404 0.563477 0.064 Uiso 1 1 calc R U . . .
H27B H 0.889310 0.084474 0.627539 0.064 Uiso 1 1 calc R U . . .
C54 C 0.440(2) 0.2239(10) 0.3278(14) 0.084(7) Uani 1 1 d D U . . .
H54A H 0.373675 0.212988 0.354759 0.126 Uiso 1 1 calc R U . . .
H54B H 0.408909 0.220188 0.273320 0.126 Uiso 1 1 calc R U . . .
H54C H 0.461069 0.259047 0.339526 0.126 Uiso 1 1 calc R U . . .
C37 C 0.732(2) 0.2988(7) 0.4694(13) 0.063(6) Uani 1 1 d . . . . .
C26 C 0.880(2) 0.1831(10) 0.6543(13) 0.069(6) Uani 1 1 d . . . . .
H26A H 0.905210 0.200887 0.702310 0.103 Uiso 1 1 calc R U . . .
H26B H 0.884808 0.205901 0.612505 0.103 Uiso 1 1 calc R U . . .
H26C H 0.938145 0.154858 0.652945 0.103 Uiso 1 1 calc R U . . .
C43 C 0.344(2) 0.1756(8) 0.6667(13) 0.065(6) Uani 1 1 d . . . . .
H43A H 0.364933 0.144760 0.641547 0.078 Uiso 1 1 calc R U . . .
H43B H 0.420561 0.184792 0.704910 0.078 Uiso 1 1 calc R U . . .
C49 C 0.705(2) 0.3539(9) 0.4398(15) 0.070(6) Uani 1 1 d . . . . .
H49A H 0.720225 0.376827 0.483696 0.084 Uiso 1 1 calc R U . . .
H49B H 0.767659 0.362556 0.407872 0.084 Uiso 1 1 calc R U . . .
C19 C 0.350(2) -0.0572(8) 0.7317(17) 0.074(7) Uani 1 1 d . . . . .
H19A H 0.287290 -0.084699 0.718440 0.088 Uiso 1 1 calc R U . . .
H19B H 0.361545 -0.051630 0.786752 0.088 Uiso 1 1 calc R U . . .
C24 C 0.781(2) 0.0068(9) 0.8436(16) 0.088(7) Uani 1 1 d D U . . .
H24A H 0.720610 -0.008156 0.801657 0.132 Uiso 1 1 calc R U . . .
H24B H 0.792484 -0.015345 0.887493 0.132 Uiso 1 1 calc R U . . .
H24C H 0.864375 0.011652 0.828576 0.132 Uiso 1 1 calc R U . . .
C22 C 0.541(3) 0.1430(11) 0.8700(13) 0.076(6) Uani 1 1 d . . . . .
H22A H 0.467911 0.126934 0.837373 0.114 Uiso 1 1 calc R U . . .
H22B H 0.518965 0.177429 0.880370 0.114 Uiso 1 1 calc R U . . .
H22C H 0.563695 0.124505 0.917571 0.114 Uiso 1 1 calc R U . . .
C1 C 0.4880(16) 0.0826(6) 0.6043(9) 0.039(3) Uani 1 1 d . . . . .
C42 C 0.168(3) 0.2407(11) 0.4820(14) 0.082(8) Uani 1 1 d . . . . .
H42A H 0.193524 0.274738 0.498556 0.124 Uiso 1 1 calc R U . . .
H42B H 0.076007 0.239871 0.460897 0.124 Uiso 1 1 calc R U . . .
H42C H 0.215874 0.230243 0.443459 0.124 Uiso 1 1 calc R U . . .
C28 C 0.778(2) 0.0220(8) 0.6223(17) 0.072(6) Uani 1 1 d . . . . .
H28A H 0.829017 0.009956 0.670231 0.108 Uiso 1 1 calc R U . . .
H28B H 0.806725 0.005215 0.580327 0.108 Uiso 1 1 calc R U . . .
H28C H 0.687356 0.014686 0.620401 0.108 Uiso 1 1 calc R U . . .
C55 C 0.765(2) 0.1755(7) 0.4436(14) 0.062(5) Uani 1 1 d . . . . .
H55A H 0.729276 0.147056 0.467653 0.074 Uiso 1 1 calc R U . . .
H55B H 0.830277 0.191640 0.483212 0.074 Uiso 1 1 calc R U . . .
C45 C 0.333(3) 0.3528(9) 0.5916(16) 0.083(7) Uani 1 1 d D U . . .
H45A H 0.399654 0.373998 0.576370 0.099 Uiso 1 1 calc R U . . .
H45B H 0.274057 0.341282 0.545325 0.099 Uiso 1 1 calc R U . . .
C46 C 0.257(3) 0.3834(11) 0.6404(19) 0.102(8) Uani 1 1 d D U . . .
H46A H 0.177184 0.366158 0.643039 0.153 Uiso 1 1 calc R U . . .
H46B H 0.238176 0.416483 0.617808 0.153 Uiso 1 1 calc R U . . .
H46C H 0.309090 0.387085 0.691365 0.153 Uiso 1 1 calc R U . . .
C51 C 0.862(2) 0.2967(9) 0.5172(11) 0.074(6) Uani 1 1 d D U . . .
H51A H 0.921826 0.313944 0.490051 0.089 Uiso 1 1 calc R U . . .
H51B H 0.888687 0.261287 0.522652 0.089 Uiso 1 1 calc R U . . .
C29 C 0.4979(18) 0.2006(6) 0.5212(9) 0.043(4) Uani 1 1 d . . . . .
C18 C 0.095(2) -0.0296(10) 0.7499(16) 0.073(6) Uani 1 1 d . . . . .
H18A H 0.038459 -0.038079 0.701769 0.109 Uiso 1 1 calc R U . . .
H18B H 0.043336 -0.015600 0.784326 0.109 Uiso 1 1 calc R U . . .
H18C H 0.138693 -0.059764 0.772251 0.109 Uiso 1 1 calc R U . . .
C50 C 0.580(3) 0.3625(11) 0.398(2) 0.091(8) Uani 1 1 d . . . . .
H50A H 0.559718 0.337615 0.357272 0.136 Uiso 1 1 calc R U . . .
H50B H 0.574961 0.396016 0.375621 0.136 Uiso 1 1 calc R U . . .
H50C H 0.517577 0.359687 0.431006 0.136 Uiso 1 1 calc R U . . .
C56 C 0.833(4) 0.1547(12) 0.386(2) 0.108(12) Uani 1 1 d . . . . .
H56A H 0.776806 0.131311 0.353138 0.162 Uiso 1 1 calc R U . . .
H56B H 0.911175 0.137263 0.410625 0.162 Uiso 1 1 calc R U . . .
H56C H 0.856805 0.182061 0.354821 0.162 Uiso 1 1 calc R U . . .
C52 C 0.879(3) 0.3196(11) 0.5968(13) 0.099(8) Uani 1 1 d D U . . .
H52A H 0.855158 0.354913 0.592837 0.148 Uiso 1 1 calc R U . . .
H52B H 0.969206 0.316463 0.622444 0.148 Uiso 1 1 calc R U . . .
H52C H 0.824509 0.301804 0.625834 0.148 Uiso 1 1 calc R U . . .
C47 C 0.484(3) 0.3236(10) 0.7088(15) 0.098(8) Uani 1 1 d D U . . .
H47A H 0.430588 0.338714 0.741731 0.118 Uiso 1 1 calc R U . . .
H47B H 0.541221 0.350066 0.695769 0.118 Uiso 1 1 calc R U . . .
C48 C 0.568(3) 0.2827(11) 0.7538(17) 0.106(9) Uani 1 1 d D U . . .
H48A H 0.514615 0.260557 0.777570 0.159 Uiso 1 1 calc R U . . .
H48B H 0.633687 0.298272 0.792903 0.159 Uiso 1 1 calc R U . . .
H48C H 0.610563 0.263305 0.719672 0.159 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 C1 2.021(15) . ?
Ge1 C29 2.022(16) . ?
Ge1 Br1 2.356(3) . ?
Ge1 Br2 2.363(3) . ?
C8 C7 1.40(2) . ?
C8 C12 1.40(2) . ?
C8 C9 1.52(3) . ?
C39 C55 1.46(3) . ?
C39 C53 1.54(3) . ?
C39 C38 1.55(3) . ?
C39 C40 1.62(3) . ?
C13 C14 1.52(3) . ?
C13 C3 1.52(3) . ?
C31 C43 1.54(3) . ?
C31 C41 1.55(4) . ?
C31 C32 1.56(3) . ?
C31 C30 1.57(3) . ?
C7 C6 1.38(2) . ?
C5 C6 1.47(2) . ?
C5 C19 1.50(3) . ?
C5 C4 1.54(3) . ?
C5 C17 1.55(2) . ?
C30 C29 1.39(2) . ?
C30 C34 1.49(3) . ?
C6 C2 1.40(2) . ?
C16 C15 1.51(3) . ?
C34 C35 1.26(3) . ?
C34 C33 1.56(3) . ?
C32 C33 1.48(3) . ?
C40 C36 1.35(3) . ?
C40 C29 1.46(3) . ?
C9 C23 1.50(3) . ?
C9 C21 1.53(3) . ?
C9 C10 1.55(2) . ?
C11 C25 1.52(2) . ?
C11 C27 1.53(3) . ?
C11 C10 1.57(2) . ?
C11 C12 1.596(18) . ?
C38 C37 1.62(3) . ?
C3 C4 1.52(3) . ?
C3 C15 1.52(2) . ?
C3 C2 1.57(2) . ?
C12 C1 1.38(2) . ?
C2 C1 1.45(2) . ?
C25 C26 1.55(3) . ?
C36 C35 1.42(3) . ?
C36 C37 1.55(3) . ?
C17 C18 1.52(3) . ?
C53 C54 1.540(3) . ?
C20 C19 1.61(3) . ?
C21 C22 1.54(3) . ?
C23 C24 1.540(3) . ?
C44 C43 1.49(3) . ?
C41 C42 1.45(4) . ?
C33 C47 1.50(4) . ?
C33 C45 1.59(4) . ?
C27 C28 1.50(3) . ?
C37 C51 1.48(4) . ?
C37 C49 1.58(3) . ?
C49 C50 1.42(4) . ?
C55 C56 1.49(3) . ?
C45 C46 1.540(3) . ?
C51 C52 1.540(3) . ?
C47 C48 1.540(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ge1 C29 120.4(6) . . ?
C1 Ge1 Br1 122.7(5) . . ?
C29 Ge1 Br1 98.5(4) . . ?
C1 Ge1 Br2 98.5(4) . . ?
C29 Ge1 Br2 123.8(5) . . ?
Br1 Ge1 Br2 91.15(11) . . ?
C7 C8 C12 120.6(16) . . ?
C7 C8 C9 124.4(15) . . ?
C12 C8 C9 115.0(13) . . ?
C55 C39 C53 112.5(18) . . ?
C55 C39 C38 112.2(18) . . ?
C53 C39 C38 108.8(17) . . ?
C55 C39 C40 114.9(16) . . ?
C53 C39 C40 106.8(17) . . ?
C38 C39 C40 100.7(15) . . ?
C14 C13 C3 115.9(18) . . ?
C43 C31 C41 111.8(19) . . ?
C43 C31 C32 108.3(17) . . ?
C41 C31 C32 110.0(16) . . ?
C43 C31 C30 113.5(15) . . ?
C41 C31 C30 109.7(16) . . ?
C32 C31 C30 103.1(16) . . ?
C6 C7 C8 118.6(14) . . ?
C6 C5 C19 112.8(16) . . ?
C6 C5 C4 103.0(14) . . ?
C19 C5 C4 111.1(17) . . ?
C6 C5 C17 110.1(15) . . ?
C19 C5 C17 106.1(16) . . ?
C4 C5 C17 113.8(17) . . ?
C29 C30 C34 117.2(17) . . ?
C29 C30 C31 133.7(17) . . ?
C34 C30 C31 109.0(15) . . ?
C7 C6 C2 120.9(13) . . ?
C7 C6 C5 124.3(15) . . ?
C2 C6 C5 114.7(16) . . ?
C35 C34 C30 124.6(17) . . ?
C35 C34 C33 125.2(19) . . ?
C30 C34 C33 110.2(19) . . ?
C33 C32 C31 112.8(17) . . ?
C36 C40 C29 122.3(16) . . ?
C36 C40 C39 107.5(17) . . ?
C29 C40 C39 130.0(15) . . ?
C23 C9 C8 115.0(16) . . ?
C23 C9 C21 108.2(17) . . ?
C8 C9 C21 111.0(15) . . ?
C23 C9 C10 112.7(16) . . ?
C8 C9 C10 100.0(14) . . ?
C21 C9 C10 109.7(17) . . ?
C25 C11 C27 108.8(13) . . ?
C25 C11 C10 111.1(14) . . ?
C27 C11 C10 110.1(14) . . ?
C25 C11 C12 114.3(13) . . ?
C27 C11 C12 109.2(12) . . ?
C10 C11 C12 103.2(11) . . ?
C39 C38 C37 108.3(15) . . ?
C4 C3 C15 109.5(15) . . ?
C4 C3 C13 109.0(16) . . ?
C15 C3 C13 111.2(16) . . ?
C4 C3 C2 102.9(15) . . ?
C15 C3 C2 114.5(14) . . ?
C13 C3 C2 109.2(14) . . ?
C16 C15 C3 115.7(16) . . ?
C1 C12 C8 121.7(13) . . ?
C1 C12 C11 131.7(12) . . ?
C8 C12 C11 106.3(13) . . ?
C6 C2 C1 120.4(14) . . ?
C6 C2 C3 106.9(13) . . ?
C1 C2 C3 132.7(14) . . ?
C9 C10 C11 108.4(12) . . ?
C11 C25 C26 114.1(17) . . ?
C40 C36 C35 119.9(19) . . ?
C40 C36 C37 117.6(17) . . ?
C35 C36 C37 122.5(17) . . ?
C18 C17 C5 115.2(17) . . ?
C34 C35 C36 119.4(19) . . ?
C39 C53 C54 117(2) . . ?
C9 C21 C22 115.9(19) . . ?
C3 C4 C5 108.6(14) . . ?
C9 C23 C24 115.1(19) . . ?
C42 C41 C31 118(2) . . ?
C32 C33 C47 115(2) . . ?
C32 C33 C34 104.9(16) . . ?
C47 C33 C34 110(2) . . ?
C32 C33 C45 112(2) . . ?
C47 C33 C45 109.3(18) . . ?
C34 C33 C45 105.0(19) . . ?
C28 C27 C11 115.4(16) . . ?
C51 C37 C36 115.8(18) . . ?
C51 C37 C49 108.6(19) . . ?
C36 C37 C49 114.1(16) . . ?
C51 C37 C38 113.7(17) . . ?
C36 C37 C38 96.2(16) . . ?
C49 C37 C38 107.7(18) . . ?
C44 C43 C31 116.6(16) . . ?
C50 C49 C37 115(2) . . ?
C5 C19 C20 115.5(18) . . ?
C12 C1 C2 115.8(13) . . ?
C12 C1 Ge1 120.2(11) . . ?
C2 C1 Ge1 123.7(12) . . ?
C39 C55 C56 118(2) . . ?
C46 C45 C33 110(2) . . ?
C37 C51 C52 117(2) . . ?
C30 C29 C40 115.7(15) . . ?
C30 C29 Ge1 120.4(14) . . ?
C40 C29 Ge1 123.8(12) . . ?
C33 C47 C48 115(2) . . ?

_refine_diff_density_max         1.728
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.176


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
