# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ld140127Ge1
_database_code_depnum_ccdc_archive 'CCDC 1971050'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H41 B Ge N4'
_chemical_formula_sum            'C27 H41 B Ge N4'
_chemical_formula_weight         505.04

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   13.3959(8)
_cell_length_b                   10.9681(6)
_cell_length_c                   19.050(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.283(7)
_cell_angle_gamma                90
_cell_volume                     2754.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    24311
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.386
_exptl_absorpt_coefficient_mu    1.133
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.183
-1 0 -1 0.193
-1 1 -1 0.192
0 -1 0 0.200
0 1 1 0.199
1 0 -1 0.184
-1 0 1 0.178


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            24311
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.060
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             5924
_reflns_number_gt                5027
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0231P)²+3.0985P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5924
_refine_ls_number_parameters     298
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_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 0.63767(2) 0.25999(2) 0.16708(2) 0.01671(7) Uani 1 1 d . . . . .
N3 N 0.71897(12) 0.22027(15) 0.10182(8) 0.0177(3) Uani 1 1 d . . . . .
N2 N 0.73657(13) 0.37839(15) 0.18198(9) 0.0180(3) Uani 1 1 d . . . . .
C24 C 0.60490(16) 0.14732(18) 0.23945(11) 0.0211(4) Uani 1 1 d . . . . .
N1 N 0.86809(13) 0.37250(16) 0.09821(9) 0.0202(4) Uani 1 1 d . . . . .
C15 C 0.73711(16) 0.10395(18) 0.07395(10) 0.0198(4) Uani 1 1 d . . . . .
C26 C 0.56965(18) 0.2235(2) 0.29793(12) 0.0301(5) Uani 1 1 d . . . . .
H26A H 0.5115 0.2710 0.2775 0.036 Uiso 1 1 d R U . . .
H26B H 0.6234 0.2769 0.3192 0.036 Uiso 1 1 d R U . . .
H26C H 0.5520 0.1703 0.3338 0.036 Uiso 1 1 d R U . . .
C25 C 0.69893(18) 0.0735(2) 0.27020(12) 0.0285(5) Uani 1 1 d . . . . .
H25A H 0.6843 0.0219 0.3078 0.034 Uiso 1 1 d R U . . .
H25B H 0.7533 0.1280 0.2889 0.034 Uiso 1 1 d R U . . .
H25C H 0.7185 0.0242 0.2333 0.034 Uiso 1 1 d R U . . .
C12 C 0.78186(16) 0.5134(2) 0.28398(11) 0.0228(4) Uani 1 1 d . . . . .
C7 C 0.73698(15) 0.49700(18) 0.21224(11) 0.0195(4) Uani 1 1 d . . . . .
C16 C 0.82089(17) 0.0332(2) 0.10472(12) 0.0267(5) Uani 1 1 d . . . . .
C20 C 0.66819(17) 0.0597(2) 0.01517(12) 0.0264(5) Uani 1 1 d . . . . .
C23 C 0.50558(17) 0.3295(2) 0.12365(12) 0.0266(5) Uani 1 1 d . . . . .
C22 C 0.57692(18) 0.1339(2) -0.01697(13) 0.0345(5) Uani 1 1 d . . . . .
H22A H 0.5289 0.1341 0.0149 0.041 Uiso 1 1 d R U . . .
H22B H 0.5461 0.0988 -0.0618 0.041 Uiso 1 1 d R U . . .
H22C H 0.5974 0.2160 -0.0245 0.041 Uiso 1 1 d R U . . .
C14 C 0.83189(19) 0.4094(2) 0.32848(12) 0.0317(5) Uani 1 1 d . . . . .
H14A H 0.8645 0.4396 0.3741 0.038 Uiso 1 1 d R U . . .
H14B H 0.8815 0.3719 0.3047 0.038 Uiso 1 1 d R U . . .
H14C H 0.7815 0.3503 0.3350 0.038 Uiso 1 1 d R U . . .
N4 N 0.42635(16) 0.3659(2) 0.10230(13) 0.0438(6) Uani 1 1 d . . . . .
C17 C 0.8343(2) -0.0807(2) 0.07568(14) 0.0374(6) Uani 1 1 d . . . . .
H17 H 0.8895 -0.1284 0.0958 0.045 Uiso 1 1 d R U . . .
C8 C 0.69377(16) 0.5965(2) 0.17126(12) 0.0249(5) Uani 1 1 d . . . . .
C1 C 0.93915(16) 0.4556(2) 0.14364(12) 0.0252(5) Uani 1 1 d . . . . .
H1 H 0.9201 0.4550 0.1910 0.030 Uiso 1 1 d R U . . .
C11 C 0.78110(19) 0.6287(2) 0.31409(13) 0.0329(5) Uani 1 1 d . . . . .
H11 H 0.8099 0.6397 0.3618 0.039 Uiso 1 1 d R U . . .
C21 C 0.89818(19) 0.0773(2) 0.16671(13) 0.0348(6) Uani 1 1 d . . . . .
H21A H 0.9313 0.0087 0.1922 0.042 Uiso 1 1 d R U . . .
H21B H 0.8648 0.1246 0.1981 0.042 Uiso 1 1 d R U . . .
H21C H 0.9476 0.1270 0.1495 0.042 Uiso 1 1 d R U . . .
C3 C 0.9318(2) 0.5874(2) 0.11819(15) 0.0370(6) Uani 1 1 d . . . . .
H3A H 0.9488 0.5917 0.0714 0.044 Uiso 1 1 d R U . . .
H3B H 0.9781 0.6370 0.1504 0.044 Uiso 1 1 d R U . . .
H3C H 0.8638 0.6166 0.1165 0.044 Uiso 1 1 d R U . . .
C27 C 0.51939(19) 0.0630(2) 0.20467(13) 0.0335(5) Uani 1 1 d . . . . .
H27A H 0.5421 0.0156 0.1682 0.040 Uiso 1 1 d R U . . .
H27B H 0.4616 0.1109 0.1839 0.040 Uiso 1 1 d R U . . .
H27C H 0.5008 0.0096 0.2401 0.040 Uiso 1 1 d R U . . .
C9 C 0.69692(18) 0.7109(2) 0.20356(15) 0.0338(5) Uani 1 1 d . . . . .
H9 H 0.6709 0.7781 0.1766 0.041 Uiso 1 1 d R U . . .
B1 B 0.78356(17) 0.3269(2) 0.12423(11) 0.0181(4) Uani 1 1 d . U . . .
C13 C 0.64598(19) 0.5837(2) 0.09381(13) 0.0341(5) Uani 1 1 d . . . . .
H13A H 0.5826 0.5412 0.0900 0.041 Uiso 1 1 d R U . . .
H13B H 0.6907 0.5387 0.0693 0.041 Uiso 1 1 d R U . . .
H13C H 0.6343 0.6631 0.0727 0.041 Uiso 1 1 d R U . . .
C4 C 0.88945(17) 0.3540(2) 0.02508(11) 0.0266(5) Uani 1 1 d . . . . .
H4 H 0.9366 0.4188 0.0172 0.032 Uiso 1 1 d R U . . .
C5 C 0.9416(2) 0.2335(2) 0.01390(13) 0.0355(6) Uani 1 1 d . . . . .
H5A H 1.0003 0.2231 0.0505 0.043 Uiso 1 1 d R U . . .
H5B H 0.9619 0.2341 -0.0320 0.043 Uiso 1 1 d R U . . .
H5C H 0.8951 0.1675 0.0160 0.043 Uiso 1 1 d R U . . .
C6 C 0.7949(2) 0.3707(3) -0.03120(13) 0.0418(6) Uani 1 1 d . . . . .
H6A H 0.7466 0.3083 -0.0258 0.050 Uiso 1 1 d R U . . .
H6B H 0.8126 0.3649 -0.0778 0.050 Uiso 1 1 d R U . . .
H6C H 0.7658 0.4493 -0.0257 0.050 Uiso 1 1 d R U . . .
C18 C 0.7674(2) -0.1241(2) 0.01733(16) 0.0432(7) Uani 1 1 d . . . . .
H18 H 0.7777 -0.2005 -0.0014 0.052 Uiso 1 1 d R U . . .
C19 C 0.6861(2) -0.0547(2) -0.01240(14) 0.0380(6) Uani 1 1 d . . . . .
H19 H 0.6416 -0.0840 -0.0519 0.046 Uiso 1 1 d R U . . .
C10 C 0.73843(19) 0.7267(2) 0.27438(15) 0.0372(6) Uani 1 1 d . . . . .
H10 H 0.7375 0.8030 0.2955 0.045 Uiso 1 1 d R U . . .
C2 C 1.04812(17) 0.4097(3) 0.15307(14) 0.0386(6) Uani 1 1 d . . . . .
H2A H 1.0520 0.3292 0.1731 0.046 Uiso 1 1 d R U . . .
H2B H 1.0917 0.4634 0.1845 0.046 Uiso 1 1 d R U . . .
H2C H 1.0693 0.4075 0.1075 0.046 Uiso 1 1 d 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 N2 1.8406(16) . ?
Ge1 N3 1.8453(16) . ?
Ge1 C24 1.959(2) . ?
Ge1 C23 1.969(2) . ?
Ge1 B1 2.365(2) . ?
N3 C15 1.419(3) . ?
N3 B1 1.472(3) . ?
N2 C7 1.422(3) . ?
N2 B1 1.474(3) . ?
C24 C25 1.524(3) . ?
C24 C27 1.528(3) . ?
C24 C26 1.533(3) . ?
N1 B1 1.407(3) . ?
N1 C1 1.480(3) . ?
N1 C4 1.485(3) . ?
C15 C16 1.404(3) . ?
C15 C20 1.404(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9599 . ?
C26 H26C 0.9599 . ?
C25 H25A 0.9599 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C12 C11 1.390(3) . ?
C12 C7 1.403(3) . ?
C12 C14 1.505(3) . ?
C7 C8 1.405(3) . ?
C16 C17 1.391(3) . ?
C16 C21 1.505(3) . ?
C20 C19 1.397(3) . ?
C20 C22 1.504(3) . ?
C23 N4 1.139(3) . ?
C22 H22A 0.9599 . ?
C22 H22B 0.9601 . ?
C22 H22C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9602 . ?
C14 H14C 0.9599 . ?
C17 C18 1.382(4) . ?
C17 H17 0.9300 . ?
C8 C9 1.395(3) . ?
C8 C13 1.506(3) . ?
C1 C3 1.523(3) . ?
C1 C2 1.524(3) . ?
C1 H1 0.9800 . ?
C11 C10 1.378(4) . ?
C11 H11 0.9299 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9599 . ?
C3 H3A 0.9601 . ?
C3 H3B 0.9599 . ?
C3 H3C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9601 . ?
C9 C10 1.375(4) . ?
C9 H9 0.9299 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C4 C6 1.517(3) . ?
C4 C5 1.528(3) . ?
C4 H4 0.9799 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9601 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9600 . ?
C18 C19 1.367(4) . ?
C18 H18 0.9299 . ?
C19 H19 0.9299 . ?
C10 H10 0.9299 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9599 . ?
C2 H2C 0.9602 . ?

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
N2 Ge1 N3 77.02(7) . . ?
N2 Ge1 C24 125.61(8) . . ?
N3 Ge1 C24 123.97(8) . . ?
N2 Ge1 C23 111.08(8) . . ?
N3 Ge1 C23 113.74(8) . . ?
C24 Ge1 C23 104.05(9) . . ?
N2 Ge1 B1 38.55(7) . . ?
N3 Ge1 B1 38.49(7) . . ?
C24 Ge1 B1 137.86(8) . . ?
C23 Ge1 B1 118.09(8) . . ?
C15 N3 B1 133.76(17) . . ?
C15 N3 Ge1 128.70(13) . . ?
B1 N3 Ge1 90.23(12) . . ?
C7 N2 B1 132.96(17) . . ?
C7 N2 Ge1 131.18(13) . . ?
B1 N2 Ge1 90.35(12) . . ?
C25 C24 C27 110.46(19) . . ?
C25 C24 C26 110.54(18) . . ?
C27 C24 C26 109.91(19) . . ?
C25 C24 Ge1 109.39(14) . . ?
C27 C24 Ge1 108.75(14) . . ?
C26 C24 Ge1 107.73(14) . . ?
B1 N1 C1 119.15(17) . . ?
B1 N1 C4 125.74(17) . . ?
C1 N1 C4 114.88(16) . . ?
C16 C15 C20 120.3(2) . . ?
C16 C15 N3 121.22(19) . . ?
C20 C15 N3 118.46(19) . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.6 . . ?
C24 C25 H25B 109.4 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C11 C12 C7 119.0(2) . . ?
C11 C12 C14 119.5(2) . . ?
C7 C12 C14 121.45(19) . . ?
C12 C7 C8 120.26(19) . . ?
C12 C7 N2 118.81(18) . . ?
C8 C7 N2 120.92(18) . . ?
C17 C16 C15 118.8(2) . . ?
C17 C16 C21 118.8(2) . . ?
C15 C16 C21 122.4(2) . . ?
C19 C20 C15 118.5(2) . . ?
C19 C20 C22 120.9(2) . . ?
C15 C20 C22 120.6(2) . . ?
N4 C23 Ge1 175.1(2) . . ?
C20 C22 H22A 109.4 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.6 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.4 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C17 C16 121.2(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.3 . . ?
C9 C8 C7 118.5(2) . . ?
C9 C8 C13 119.3(2) . . ?
C7 C8 C13 122.2(2) . . ?
N1 C1 C3 113.60(19) . . ?
N1 C1 C2 111.58(18) . . ?
C3 C1 C2 110.9(2) . . ?
N1 C1 H1 106.7 . . ?
C3 C1 H1 106.6 . . ?
C2 C1 H1 106.9 . . ?
C10 C11 C12 121.1(2) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.3 . . ?
C16 C21 H21A 109.6 . . ?
C16 C21 H21B 109.3 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C1 C3 H3A 109.2 . . ?
C1 C3 H3B 109.7 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C24 C27 H27A 109.4 . . ?
C24 C27 H27B 109.6 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C9 C8 121.4(2) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
N1 B1 N3 130.45(18) . . ?
N1 B1 N2 127.21(19) . . ?
N3 B1 N2 102.33(17) . . ?
N1 B1 Ge1 177.13(16) . . ?
N3 B1 Ge1 51.28(9) . . ?
N2 B1 Ge1 51.10(10) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.3 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C4 C6 111.72(19) . . ?
N1 C4 C5 114.71(19) . . ?
C6 C4 C5 110.5(2) . . ?
N1 C4 H4 106.4 . . ?
C6 C4 H4 106.5 . . ?
C5 C4 H4 106.4 . . ?
C4 C5 H5A 109.7 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.3 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.6 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C19 C18 C17 119.7(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 121.5(2) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.2 . . ?
C9 C10 C11 119.7(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.4 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

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

data_ld150921Ge1
_database_code_depnum_ccdc_archive 'CCDC 1971053'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C55 H79 B2 Ge2 N7'
_chemical_formula_sum            'C55 H79 B2 Ge2 N7'
_chemical_formula_weight         1005.05

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   14.1030(17)
_cell_length_b                   22.561(2)
_cell_length_c                   18.1100(18)
_cell_angle_alpha                90
_cell_angle_beta                 112.285(6)
_cell_angle_gamma                90
_cell_volume                     5331.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    61097
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.170
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.133
0 0 -1 0.124
-1 0 1 0.075
1 0 -1 0.069
0 1 0 0.058
0 -1 0 0.094


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            61097
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.803
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             12060
_reflns_number_gt                7887
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0161P)²+30.7608P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12060
_refine_ls_number_parameters     595
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1214
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 -0.27992(4) 0.06716(2) 0.29017(3) 0.01415(11) Uani 1 1 d . U . . .
Ge2 Ge -0.13257(4) 0.00873(3) 0.37962(3) 0.02757(15) Uani 1 1 d . U . . .
N4 N -0.2478(3) 0.06024(16) 0.1993(2) 0.0151(8) Uani 1 1 d . . . . .
N2 N -0.3360(3) 0.14007(16) 0.3012(2) 0.0161(8) Uani 1 1 d . . . . .
N1 N -0.4149(3) 0.04954(17) 0.2810(2) 0.0167(8) Uani 1 1 d . . . . .
N3 N -0.5131(3) 0.13915(17) 0.3114(2) 0.0188(8) Uani 1 1 d . . . . .
N6 N -0.1339(3) 0.00689(17) 0.1404(2) 0.0174(8) Uani 1 1 d . . . . .
N5 N -0.1128(3) -0.00928(17) 0.2837(2) 0.0173(8) Uani 1 1 d . . . . .
C28 C -0.1976(4) 0.1507(2) 0.1489(3) 0.0212(10) Uani 1 1 d . . . . .
C1 C -0.4434(3) -0.0025(2) 0.3121(3) 0.0170(9) Uani 1 1 d . . . . .
C24 C -0.3643(3) 0.1082(2) 0.0750(3) 0.0204(10) Uani 1 1 d . . . . .
C23 C -0.2708(3) 0.1067(2) 0.1407(2) 0.0164(9) Uani 1 1 d . . . . .
C2 C -0.4233(3) -0.0077(2) 0.3942(3) 0.0223(10) Uani 1 1 d . . . . .
C25 C -0.3797(4) 0.1505(2) 0.0158(3) 0.0252(11) Uani 1 1 d . . . . .
H25 H -0.4411 0.1508 -0.0284 0.030 Uiso 1 1 d R U . . .
C20 C -0.4958(4) 0.1951(2) 0.3564(3) 0.0219(10) Uani 1 1 d . . . . .
H20 H -0.4219 0.2028 0.3760 0.026 Uiso 1 1 d R U . . .
C27 C -0.2160(4) 0.1923(2) 0.0884(3) 0.0278(11) Uani 1 1 d . . . . .
H27 H -0.1669 0.2211 0.0928 0.033 Uiso 1 1 d R U . . .
C17 C -0.6204(4) 0.1187(2) 0.2766(3) 0.0258(11) Uani 1 1 d . . . . .
H17 H -0.6622 0.1533 0.2770 0.031 Uiso 1 1 d R U . . .
C31 C -0.0662(4) -0.0663(2) 0.2876(3) 0.0213(10) Uani 1 1 d . . . . .
C6 C -0.4907(4) -0.0497(2) 0.2608(3) 0.0231(10) Uani 1 1 d . . . . .
C9 C -0.2961(3) 0.1986(2) 0.3119(3) 0.0227(11) Uani 1 1 d . . . . .
C8 C -0.5072(4) -0.0476(2) 0.1738(3) 0.0299(12) Uani 1 1 d . . . . .
H8A H -0.5397 -0.0836 0.1483 0.036 Uiso 1 1 d R U . . .
H8B H -0.4425 -0.0434 0.1682 0.036 Uiso 1 1 d R U . . .
H8C H -0.5503 -0.0145 0.1493 0.036 Uiso 1 1 d R U . . .
C30 C -0.1015(4) 0.1554(2) 0.2232(3) 0.0266(11) Uani 1 1 d . . . . .
H30A H -0.0531 0.1807 0.2130 0.032 Uiso 1 1 d R U . . .
H30B H -0.0724 0.1166 0.2378 0.032 Uiso 1 1 d R U . . .
H30C H -0.1179 0.1716 0.2659 0.032 Uiso 1 1 d R U . . .
C45 C -0.0380(4) 0.0816(3) 0.4095(3) 0.0360(13) Uani 1 1 d . . . . .
C14 C -0.2241(4) 0.2146(2) 0.3880(3) 0.0283(12) Uani 1 1 d . . . . .
C3 C -0.4585(4) -0.0577(2) 0.4212(3) 0.0287(12) Uani 1 1 d . . . . .
H3 H -0.4472 -0.0606 0.4751 0.034 Uiso 1 1 d R U . . .
C22 C -0.5475(4) 0.2487(2) 0.3069(3) 0.0359(13) Uani 1 1 d . . . . .
H22A H -0.5302 0.2509 0.2606 0.043 Uiso 1 1 d R U . . .
H22B H -0.5250 0.2841 0.3381 0.043 Uiso 1 1 d R U . . .
H22C H -0.6204 0.2448 0.2906 0.043 Uiso 1 1 d R U . . .
C26 C -0.3058(4) 0.1916(2) 0.0214(3) 0.0288(12) Uani 1 1 d . . . . .
H26 H -0.3164 0.2190 -0.0193 0.035 Uiso 1 1 d R U . . .
C39 C -0.2115(4) -0.0004(2) 0.0592(3) 0.0232(11) Uani 1 1 d . . . . .
H39 H -0.2766 0.0110 0.0629 0.028 Uiso 1 1 d R U . . .
C5 C -0.5230(4) -0.0987(2) 0.2909(3) 0.0321(12) Uani 1 1 d . . . . .
H5 H -0.5551 -0.1297 0.2566 0.039 Uiso 1 1 d R U . . .
B1 B -0.4296(4) 0.1120(2) 0.2985(3) 0.0175(11) Uani 1 1 d . . . . .
N7 N 0.0243(4) 0.1175(2) 0.4360(3) 0.0395(12) Uani 1 1 d . . . . .
C42 C -0.0235(4) 0.0023(2) 0.1559(3) 0.0263(11) Uani 1 1 d . . . . .
H42 H 0.0115 0.0030 0.2141 0.032 Uiso 1 1 d R U . . .
C21 C -0.5230(4) 0.1906(3) 0.4300(3) 0.0329(13) Uani 1 1 d . . . . .
H21A H -0.5956 0.1850 0.4135 0.039 Uiso 1 1 d R U . . .
H21B H -0.5032 0.2263 0.4610 0.039 Uiso 1 1 d R U . . .
H21C H -0.4877 0.1574 0.4618 0.039 Uiso 1 1 d R U . . .
C19 C -0.6504(4) 0.1015(3) 0.1897(3) 0.0353(13) Uani 1 1 d . . . . .
H19A H -0.6339 0.1332 0.1614 0.042 Uiso 1 1 d R U . . .
H19B H -0.7228 0.0939 0.1666 0.042 Uiso 1 1 d R U . . .
H19C H -0.6139 0.0664 0.1860 0.042 Uiso 1 1 d R U . . .
C29 C -0.4487(3) 0.0660(2) 0.0691(3) 0.0266(11) Uani 1 1 d . . . . .
H29A H -0.5087 0.0754 0.0230 0.032 Uiso 1 1 d R U . . .
H29B H -0.4641 0.0694 0.1162 0.032 Uiso 1 1 d R U . . .
H29C H -0.4275 0.0262 0.0645 0.032 Uiso 1 1 d R U . . .
C38 C 0.1074(4) -0.0230(3) 0.3703(3) 0.0420(16) Uani 1 1 d . . . . .
H38A H 0.1066 -0.0194 0.4229 0.050 Uiso 1 1 d R U . . .
H38B H 0.0823 0.0129 0.3411 0.050 Uiso 1 1 d R U . . .
H38C H 0.1762 -0.0302 0.3743 0.050 Uiso 1 1 d R U . . .
C36 C 0.0402(4) -0.0733(3) 0.3276(3) 0.0323(13) Uani 1 1 d . . . . .
B2 B -0.1643(4) 0.0193(2) 0.2064(3) 0.0160(10) Uani 1 1 d . . . . .
C10 C -0.3263(4) 0.2392(2) 0.2486(3) 0.0294(12) Uani 1 1 d . . . . .
C16 C -0.2012(4) 0.1745(3) 0.4581(3) 0.0362(14) Uani 1 1 d . . . . .
H16A H -0.1528 0.1935 0.5046 0.043 Uiso 1 1 d R U . . .
H16B H -0.1727 0.1380 0.4486 0.043 Uiso 1 1 d R U . . .
H16C H -0.2632 0.1664 0.4665 0.043 Uiso 1 1 d R U . . .
C15 C -0.4103(5) 0.2260(2) 0.1704(3) 0.0378(14) Uani 1 1 d . . . . .
H15A H -0.4639 0.2547 0.1608 0.045 Uiso 1 1 d R U . . .
H15B H -0.4371 0.1871 0.1717 0.045 Uiso 1 1 d R U . . .
H15C H -0.3843 0.2281 0.1286 0.045 Uiso 1 1 d R U . . .
C32 C -0.1284(5) -0.1154(2) 0.2527(3) 0.0299(12) Uani 1 1 d . . . . .
C11 C -0.2764(5) 0.2938(2) 0.2618(4) 0.0439(16) Uani 1 1 d . . . . .
H11 H -0.2931 0.3209 0.2201 0.053 Uiso 1 1 d R U . . .
C40 C -0.2006(4) 0.0395(3) -0.0053(3) 0.0357(13) Uani 1 1 d . . . . .
H40A H -0.1894 0.0796 0.0136 0.043 Uiso 1 1 d R U . . .
H40B H -0.2621 0.0375 -0.0524 0.043 Uiso 1 1 d R U . . .
H40C H -0.1435 0.0264 -0.0176 0.043 Uiso 1 1 d R U . . .
C4 C -0.5092(4) -0.1028(2) 0.3701(3) 0.0347(13) Uani 1 1 d . . . . .
H4 H -0.5335 -0.1354 0.3891 0.042 Uiso 1 1 d R U . . .
C54 C 0.0694(4) 0.2196(3) 0.4158(3) 0.0407(15) Uani 1 1 d . . . . .
H54A H 0.0709 0.2097 0.3641 0.049 Uiso 1 1 d R U . . .
H54B H 0.0005 0.2322 0.4080 0.049 Uiso 1 1 d R U . . .
C7 C -0.3661(4) 0.0388(2) 0.4539(3) 0.0261(11) Uani 1 1 d . . . . .
H7A H -0.3590 0.0264 0.5065 0.031 Uiso 1 1 d R U . . .
H7B H -0.4031 0.0755 0.4411 0.031 Uiso 1 1 d R U . . .
H7C H -0.2994 0.0442 0.4523 0.031 Uiso 1 1 d R U . . .
C47 C 0.2058(4) 0.1449(3) 0.4789(3) 0.0376(14) Uani 1 1 d . . . . .
H47A H 0.2249 0.1092 0.5111 0.045 Uiso 1 1 d R U . . .
H47B H 0.2063 0.1361 0.4266 0.045 Uiso 1 1 d R U . . .
C37 C -0.2426(5) -0.1099(3) 0.2190(3) 0.0409(15) Uani 1 1 d . . . . .
H37A H -0.2659 -0.0987 0.2604 0.049 Uiso 1 1 d R U . . .
H37B H -0.2722 -0.1473 0.1969 0.049 Uiso 1 1 d R U . . .
H37C H -0.2629 -0.0802 0.1779 0.049 Uiso 1 1 d R U . . .
C43 C 0.0198(4) 0.0554(3) 0.1259(3) 0.0371(14) Uani 1 1 d . . . . .
H43A H 0.0031 0.0512 0.0697 0.045 Uiso 1 1 d R U . . .
H43B H 0.0929 0.0569 0.1532 0.045 Uiso 1 1 d R U . . .
H43C H -0.0099 0.0913 0.1359 0.045 Uiso 1 1 d R U . . .
C13 C -0.1800(4) 0.2705(3) 0.3982(4) 0.0425(16) Uani 1 1 d . . . . .
H13 H -0.1343 0.2820 0.4485 0.051 Uiso 1 1 d R U . . .
C46 C 0.0989(4) 0.1648(3) 0.4713(3) 0.0378(14) Uani 1 1 d . . . . .
C52 C 0.1738(5) 0.2292(3) 0.5896(4) 0.0553(19) Uani 1 1 d . . . . .
H52 H 0.1727 0.2383 0.6422 0.066 Uiso 1 1 d R U . . .
C53 C 0.0955(4) 0.1797(3) 0.5504(3) 0.0349(13) Uani 1 1 d . . . . .
H53A H 0.1127 0.1448 0.5842 0.042 Uiso 1 1 d R U . . .
H53B H 0.0271 0.1924 0.5441 0.042 Uiso 1 1 d R U . . .
C18 C -0.6496(4) 0.0709(3) 0.3228(3) 0.0379(14) Uani 1 1 d . . . . .
H18A H -0.6177 0.0343 0.3183 0.045 Uiso 1 1 d R U . . .
H18B H -0.7227 0.0660 0.3018 0.045 Uiso 1 1 d R U . . .
H18C H -0.6265 0.0823 0.3779 0.045 Uiso 1 1 d R U . . .
C48 C 0.2811(5) 0.1934(3) 0.5174(4) 0.0506(17) Uani 1 1 d . . . . .
H48 H 0.3500 0.1807 0.5229 0.061 Uiso 1 1 d R U . . .
C33 C -0.0812(6) -0.1692(3) 0.2529(4) 0.0489(18) Uani 1 1 d . . . . .
H33 H -0.1213 -0.2018 0.2285 0.059 Uiso 1 1 d R U . . .
C49 C 0.2502(5) 0.2475(3) 0.4645(4) 0.0515(18) Uani 1 1 d . . . . .
H49A H 0.2526 0.2383 0.4129 0.062 Uiso 1 1 d R U . . .
H49B H 0.2983 0.2794 0.4882 0.062 Uiso 1 1 d R U . . .
C44 C 0.0108(4) -0.0552(3) 0.1288(3) 0.0378(14) Uani 1 1 d . . . . .
H44A H -0.0142 -0.0882 0.1495 0.045 Uiso 1 1 d R U . . .
H44B H 0.0843 -0.0567 0.1483 0.045 Uiso 1 1 d R U . . .
H44C H -0.0166 -0.0569 0.0715 0.045 Uiso 1 1 d R U . . .
C41 C -0.2265(5) -0.0644(3) 0.0295(3) 0.0390(14) Uani 1 1 d . . . . .
H41A H -0.1739 -0.0747 0.0103 0.047 Uiso 1 1 d R U . . .
H41B H -0.2924 -0.0684 -0.0130 0.047 Uiso 1 1 d R U . . .
H41C H -0.2226 -0.0904 0.0726 0.047 Uiso 1 1 d R U . . .
C12 C -0.2036(5) 0.3087(3) 0.3350(5) 0.055(2) Uani 1 1 d . . . . .
H12 H -0.1700 0.3449 0.3416 0.066 Uiso 1 1 d R U . . .
C34 C 0.0237(7) -0.1756(3) 0.2875(4) 0.057(2) Uani 1 1 d . . . . .
H34 H 0.0538 -0.2117 0.2848 0.068 Uiso 1 1 d R U . . .
C50 C 0.1427(5) 0.2676(3) 0.4532(4) 0.0433(15) Uani 1 1 d . . . . .
H50 H 0.1242 0.3028 0.4190 0.052 Uiso 1 1 d R U . . .
C55 C 0.2800(5) 0.2077(4) 0.6007(3) 0.058(2) Uani 1 1 d . . . . .
H55A H 0.3310 0.2377 0.6269 0.070 Uiso 1 1 d R U . . .
H55B H 0.2964 0.1722 0.6334 0.070 Uiso 1 1 d R U . . .
C35 C 0.0830(6) -0.1287(3) 0.3261(4) 0.0513(19) Uani 1 1 d . . . . .
H35 H 0.1534 -0.1338 0.3519 0.062 Uiso 1 1 d R U . . .
C51 C 0.1441(6) 0.2829(3) 0.5382(4) 0.0575(19) Uani 1 1 d . . . . .
H51A H 0.1927 0.3145 0.5618 0.069 Uiso 1 1 d R U . . .
H51B H 0.0767 0.2962 0.5337 0.069 Uiso 1 1 d 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 N2 1.869(4) . ?
Ge1 N4 1.872(3) . ?
Ge1 N1 1.890(4) . ?
Ge1 B1 2.396(5) . ?
Ge1 Ge2 2.4754(8) . ?
Ge2 N5 1.905(4) . ?
Ge2 C45 2.055(6) . ?
N4 C23 1.439(6) . ?
N4 B2 1.463(6) . ?
N2 C9 1.419(6) . ?
N2 B1 1.448(6) . ?
N1 C1 1.423(6) . ?
N1 B1 1.475(7) . ?
N3 B1 1.423(6) . ?
N3 C20 1.473(6) . ?
N3 C17 1.475(6) . ?
N6 B2 1.441(6) . ?
N6 C39 1.472(6) . ?
N6 C42 1.477(6) . ?
N5 C31 1.433(6) . ?
N5 B2 1.460(6) . ?
C28 C27 1.391(6) . ?
C28 C23 1.398(6) . ?
C28 C30 1.508(6) . ?
C1 C6 1.404(6) . ?
C1 C2 1.410(6) . ?
C24 C25 1.389(7) . ?
C24 C23 1.402(6) . ?
C24 C29 1.497(7) . ?
C2 C3 1.393(7) . ?
C2 C7 1.503(7) . ?
C25 C26 1.370(7) . ?
C25 H25 0.9300 . ?
C20 C22 1.516(7) . ?
C20 C21 1.525(7) . ?
C20 H20 0.9801 . ?
C27 C26 1.383(7) . ?
C27 H27 0.9300 . ?
C17 C18 1.514(7) . ?
C17 C19 1.518(7) . ?
C17 H17 0.9800 . ?
C31 C36 1.405(7) . ?
C31 C32 1.406(7) . ?
C6 C5 1.385(7) . ?
C6 C8 1.503(7) . ?
C9 C10 1.402(7) . ?
C9 C14 1.415(7) . ?
C8 H8A 0.9601 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C30 H30A 0.9599 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9601 . ?
C45 N7 1.157(7) . ?
C14 C13 1.386(8) . ?
C14 C16 1.491(8) . ?
C3 C4 1.379(8) . ?
C3 H3 0.9301 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9601 . ?
C22 H22C 0.9600 . ?
C26 H26 0.9299 . ?
C39 C41 1.527(7) . ?
C39 C40 1.528(7) . ?
C39 H39 0.9799 . ?
C5 C4 1.375(8) . ?
C5 H5 0.9300 . ?
N7 C46 1.464(7) . ?
C42 C44 1.529(7) . ?
C42 C43 1.535(7) . ?
C42 H42 0.9800 . ?
C21 H21A 0.9601 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9601 . ?
C19 H19C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9599 . ?
C38 C36 1.493(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9598 . ?
C38 H38C 0.9600 . ?
C36 C35 1.393(8) . ?
C10 C11 1.392(8) . ?
C10 C15 1.492(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9599 . ?
C16 H16C 0.9600 . ?
C15 H15A 0.9599 . ?
C15 H15B 0.9601 . ?
C15 H15C 0.9599 . ?
C32 C33 1.384(8) . ?
C32 C37 1.495(8) . ?
C11 C12 1.375(10) . ?
C11 H11 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9602 . ?
C4 H4 0.9300 . ?
C54 C50 1.473(9) . ?
C54 C46 1.548(8) . ?
C54 H54A 0.9699 . ?
C54 H54B 0.9702 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9599 . ?
C7 H7C 0.9601 . ?
C47 C48 1.501(9) . ?
C47 C46 1.528(8) . ?
C47 H47A 0.9699 . ?
C47 H47B 0.9702 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9599 . ?
C43 H43A 0.9599 . ?
C43 H43B 0.9601 . ?
C43 H43C 0.9600 . ?
C13 C12 1.370(10) . ?
C13 H13 0.9299 . ?
C46 C53 1.490(8) . ?
C52 C51 1.488(10) . ?
C52 C55 1.513(9) . ?
C52 C53 1.543(8) . ?
C52 H52 0.9800 . ?
C53 H53A 0.9699 . ?
C53 H53B 0.9700 . ?
C18 H18A 0.9601 . ?
C18 H18B 0.9599 . ?
C18 H18C 0.9600 . ?
C48 C49 1.511(9) . ?
C48 C55 1.548(9) . ?
C48 H48 0.9800 . ?
C33 C34 1.377(10) . ?
C33 H33 0.9300 . ?
C49 C50 1.520(8) . ?
C49 H49A 0.9701 . ?
C49 H49B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9599 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9599 . ?
C41 H41C 0.9601 . ?
C12 H12 0.9300 . ?
C34 C35 1.365(10) . ?
C34 H34 0.9299 . ?
C50 C51 1.571(9) . ?
C50 H50 0.9801 . ?
C55 H55A 0.9699 . ?
C55 H55B 0.9702 . ?
C35 H35 0.9300 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 N4 114.91(16) . . ?
N2 Ge1 N1 75.00(16) . . ?
N4 Ge1 N1 118.49(15) . . ?
N2 Ge1 B1 37.16(17) . . ?
N4 Ge1 B1 127.11(16) . . ?
N1 Ge1 B1 37.99(17) . . ?
N2 Ge1 Ge2 133.10(11) . . ?
N4 Ge1 Ge2 96.19(11) . . ?
N1 Ge1 Ge2 120.88(12) . . ?
B1 Ge1 Ge2 136.42(12) . . ?
N5 Ge2 C45 96.09(19) . . ?
N5 Ge2 Ge1 83.90(11) . . ?
C45 Ge2 Ge1 92.64(16) . . ?
C23 N4 B2 118.3(4) . . ?
C23 N4 Ge1 121.7(3) . . ?
B2 N4 Ge1 115.5(3) . . ?
C9 N2 B1 136.2(4) . . ?
C9 N2 Ge1 132.1(3) . . ?
B1 N2 Ge1 91.6(3) . . ?
C1 N1 B1 128.2(4) . . ?
C1 N1 Ge1 124.3(3) . . ?
B1 N1 Ge1 90.0(3) . . ?
B1 N3 C20 119.1(4) . . ?
B1 N3 C17 125.0(4) . . ?
C20 N3 C17 115.6(4) . . ?
B2 N6 C39 120.5(4) . . ?
B2 N6 C42 118.6(4) . . ?
C39 N6 C42 120.8(4) . . ?
C31 N5 B2 119.8(4) . . ?
C31 N5 Ge2 111.6(3) . . ?
B2 N5 Ge2 126.0(3) . . ?
C27 C28 C23 119.0(4) . . ?
C27 C28 C30 119.4(4) . . ?
C23 C28 C30 121.5(4) . . ?
C6 C1 C2 119.3(4) . . ?
C6 C1 N1 119.9(4) . . ?
C2 C1 N1 120.8(4) . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 C29 119.6(4) . . ?
C23 C24 C29 120.8(4) . . ?
C28 C23 C24 119.5(4) . . ?
C28 C23 N4 119.2(4) . . ?
C24 C23 N4 121.3(4) . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 C7 118.6(4) . . ?
C1 C2 C7 122.6(4) . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.5 . . ?
N3 C20 C22 114.5(4) . . ?
N3 C20 C21 112.5(4) . . ?
C22 C20 C21 110.3(4) . . ?
N3 C20 H20 106.5 . . ?
C22 C20 H20 106.2 . . ?
C21 C20 H20 106.2 . . ?
C26 C27 C28 121.3(5) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.5 . . ?
N3 C17 C18 115.9(4) . . ?
N3 C17 C19 111.1(4) . . ?
C18 C17 C19 111.2(5) . . ?
N3 C17 H17 105.8 . . ?
C18 C17 H17 105.9 . . ?
C19 C17 H17 106.2 . . ?
C36 C31 C32 120.3(5) . . ?
C36 C31 N5 120.4(5) . . ?
C32 C31 N5 119.3(4) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C8 119.6(5) . . ?
C1 C6 C8 121.1(4) . . ?
C10 C9 C14 120.8(5) . . ?
C10 C9 N2 121.0(4) . . ?
C14 C9 N2 118.2(5) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.8 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.1 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C28 C30 H30A 109.6 . . ?
C28 C30 H30B 109.2 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.6 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N7 C45 Ge2 169.7(5) . . ?
C13 C14 C9 118.9(5) . . ?
C13 C14 C16 119.8(5) . . ?
C9 C14 C16 121.2(5) . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 118.9 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.8 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.1 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C26 C27 119.4(5) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.5 . . ?
N6 C39 C41 114.1(4) . . ?
N6 C39 C40 116.5(4) . . ?
C41 C39 C40 109.2(4) . . ?
N6 C39 H39 105.2 . . ?
C41 C39 H39 105.4 . . ?
C40 C39 H39 105.4 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
N3 B1 N2 127.3(4) . . ?
N3 B1 N1 129.7(4) . . ?
N2 B1 N1 103.0(4) . . ?
N3 B1 Ge1 174.6(3) . . ?
N2 B1 Ge1 51.2(2) . . ?
N1 B1 Ge1 52.1(2) . . ?
C45 N7 C46 176.5(6) . . ?
N6 C42 C44 116.0(4) . . ?
N6 C42 C43 114.2(4) . . ?
C44 C42 C43 109.3(4) . . ?
N6 C42 H42 105.5 . . ?
C44 C42 H42 105.6 . . ?
C43 C42 H42 105.1 . . ?
C20 C21 H21A 109.2 . . ?
C20 C21 H21B 109.9 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.3 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.2 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.7 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C24 C29 H29A 109.6 . . ?
C24 C29 H29B 109.1 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.7 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C36 C38 H38A 109.6 . . ?
C36 C38 H38B 109.1 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.6 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C36 C31 118.5(6) . . ?
C35 C36 C38 119.8(5) . . ?
C31 C36 C38 121.7(5) . . ?
N6 B2 N5 120.8(4) . . ?
N6 B2 N4 122.1(4) . . ?
N5 B2 N4 117.0(4) . . ?
C11 C10 C9 117.4(5) . . ?
C11 C10 C15 120.5(5) . . ?
C9 C10 C15 122.0(5) . . ?
C14 C16 H16A 109.1 . . ?
C14 C16 H16B 109.8 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C10 C15 H15A 109.0 . . ?
C10 C15 H15B 109.8 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.6 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C33 C32 C31 118.2(6) . . ?
C33 C32 C37 121.1(6) . . ?
C31 C32 C37 120.6(5) . . ?
C12 C11 C10 121.7(6) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.4 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C5 C4 C3 118.8(5) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.3 . . ?
C50 C54 C46 108.7(5) . . ?
C50 C54 H54A 110.2 . . ?
C46 C54 H54A 110.0 . . ?
C50 C54 H54B 109.9 . . ?
C46 C54 H54B 109.7 . . ?
H54A C54 H54B 108.4 . . ?
C2 C7 H7A 109.6 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.3 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C48 C47 C46 109.2(5) . . ?
C48 C47 H47A 109.8 . . ?
C46 C47 H47A 109.7 . . ?
C48 C47 H47B 109.7 . . ?
C46 C47 H47B 110.1 . . ?
H47A C47 H47B 108.3 . . ?
C32 C37 H37A 109.8 . . ?
C32 C37 H37B 109.1 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C43 H43A 109.2 . . ?
C42 C43 H43B 109.9 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.4 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C12 C13 C14 120.4(6) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 119.6 . . ?
N7 C46 C53 107.7(5) . . ?
N7 C46 C47 110.3(5) . . ?
C53 C46 C47 111.7(5) . . ?
N7 C46 C54 109.0(5) . . ?
C53 C46 C54 110.2(5) . . ?
C47 C46 C54 107.9(5) . . ?
C51 C52 C55 112.0(6) . . ?
C51 C52 C53 108.6(6) . . ?
C55 C52 C53 109.2(6) . . ?
C51 C52 H52 109.5 . . ?
C55 C52 H52 108.6 . . ?
C53 C52 H52 109.0 . . ?
C46 C53 C52 109.1(5) . . ?
C46 C53 H53A 109.3 . . ?
C52 C53 H53A 109.5 . . ?
C46 C53 H53B 110.3 . . ?
C52 C53 H53B 110.3 . . ?
H53A C53 H53B 108.3 . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.0 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C47 C48 C49 108.1(5) . . ?
C47 C48 C55 109.7(5) . . ?
C49 C48 C55 110.0(6) . . ?
C47 C48 H48 109.5 . . ?
C49 C48 H48 109.7 . . ?
C55 C48 H48 109.8 . . ?
C34 C33 C32 121.6(6) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.1 . . ?
C48 C49 C50 111.1(5) . . ?
C48 C49 H49A 109.3 . . ?
C50 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
C42 C44 H44A 108.9 . . ?
C42 C44 H44B 109.9 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.6 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C39 C41 H41A 109.4 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.4 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C13 C12 C11 120.5(6) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.8 . . ?
C35 C34 C33 119.8(6) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.0 . . ?
C54 C50 C49 109.4(5) . . ?
C54 C50 C51 111.0(5) . . ?
C49 C50 C51 107.0(5) . . ?
C54 C50 H50 109.5 . . ?
C49 C50 H50 109.8 . . ?
C51 C50 H50 110.1 . . ?
C52 C55 C48 108.3(5) . . ?
C52 C55 H55A 110.7 . . ?
C48 C55 H55A 110.0 . . ?
C52 C55 H55B 109.9 . . ?
C48 C55 H55B 109.5 . . ?
H55A C55 H55B 108.4 . . ?
C34 C35 C36 121.2(6) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.2 . . ?
C52 C51 C50 109.3(5) . . ?
C52 C51 H51A 109.8 . . ?
C50 C51 H51A 109.7 . . ?
C52 C51 H51B 109.9 . . ?
C50 C51 H51B 109.8 . . ?
H51A C51 H51B 108.4 . . ?

_refine_diff_density_max         3.109
_refine_diff_density_min         -2.445
_refine_diff_density_rms         0.122

_shelxl_version_number           2013-4

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

data_ld150309Ge1
_database_code_depnum_ccdc_archive 'CCDC 1971052'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H74 B2 Ge2 N7'
_chemical_formula_weight         951.97

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'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.2361(11)
_cell_length_b                   14.0029(13)
_cell_length_c                   23.556(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.592(7)
_cell_angle_gamma                90
_cell_volume                     5132.5(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    54633
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             2012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.252
_exptl_absorpt_coefficient_mu    1.211
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.221
-1 0 0 0.129
0 0 -1 0.064
0 0 1 0.133
0 1 0 0.126
0 -1 0 0.088
-1 1 0 0.093
1 0 -1 0.177
0 1 1 0.110


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            54633
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.711
_diffrn_reflns_theta_max         26.999
_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             11084
_reflns_number_gt                8035
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0207P)²+11.1475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11084
_refine_ls_number_parameters     559
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.106
_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 0.74011(2) 0.20866(2) 0.55304(2) 0.01463(8) Uani 1 1 d . . . . .
Ge2 Ge 0.61139(2) 0.11435(2) 0.55229(2) 0.01878(9) Uani 1 1 d . . . . .
N1 N 0.78129(15) 0.27552(18) 0.49786(11) 0.0175(5) Uani 1 1 d . . . . .
C20 C 0.7880(2) 0.5363(3) 0.55520(18) 0.0356(9) Uani 1 1 d . U . . .
H20 H 0.7814 0.5002 0.5893 0.043 Uiso 1 1 d R U . . .
N4 N 0.81846(15) 0.12968(18) 0.60628(11) 0.0160(5) Uani 1 1 d . . . . .
C9 C 0.67446(19) 0.3788(2) 0.59729(14) 0.0176(6) Uani 1 1 d . . . . .
N2 N 0.73963(15) 0.33755(18) 0.57559(11) 0.0173(5) Uani 1 1 d . . . . .
N5 N 0.68777(15) 0.04346(19) 0.61498(11) 0.0174(5) Uani 1 1 d . . . . .
C31 C 0.64087(18) 0.0055(2) 0.65278(13) 0.0193(7) Uani 1 1 d . . . . .
N6 N 0.83297(15) 0.00131(19) 0.68439(11) 0.0195(6) Uani 1 1 d . . . . .
N7 N 0.61366(17) -0.0240(2) 0.44341(12) 0.0258(6) Uani 1 1 d . . . . .
N3 N 0.77977(17) 0.46240(19) 0.50844(12) 0.0239(6) Uani 1 1 d . . . . .
C45 C 0.6242(2) 0.0270(3) 0.48295(15) 0.0243(7) Uani 1 1 d . . . . .
C23 C 0.90570(18) 0.1177(2) 0.60458(13) 0.0170(6) Uani 1 1 d . . . . .
C32 C 0.59982(19) -0.0834(2) 0.64045(14) 0.0239(7) Uani 1 1 d . . . . .
C2 C 0.9007(2) 0.2515(2) 0.45432(14) 0.0214(7) Uani 1 1 d . . . . .
C28 C 0.92513(19) 0.0411(2) 0.57208(14) 0.0212(7) Uani 1 1 d . . . . .
C6 C 0.7549(2) 0.2128(2) 0.39774(14) 0.0212(7) Uani 1 1 d . . . . .
C1 C 0.8129(2) 0.2464(2) 0.45036(13) 0.0185(6) Uani 1 1 d . . . . .
C14 C 0.58969(19) 0.3894(2) 0.56033(14) 0.0222(7) Uani 1 1 d . . . . .
C10 C 0.6942(2) 0.4077(2) 0.65644(14) 0.0229(7) Uani 1 1 d . . . . .
C24 C 0.97091(19) 0.1793(2) 0.63560(14) 0.0220(7) Uani 1 1 d . . . . .
C8 C 0.6594(2) 0.2132(3) 0.38970(15) 0.0285(8) Uani 1 1 d . . . . .
H8A H 0.6465 0.1732 0.4191 0.034 Uiso 1 1 d R U . . .
H8B H 0.6300 0.1895 0.3510 0.034 Uiso 1 1 d R U . . .
H8C H 0.6410 0.2773 0.3938 0.034 Uiso 1 1 d R U . . .
C11 C 0.6299(2) 0.4474(3) 0.67797(16) 0.0330(8) Uani 1 1 d . . . . .
H11 H 0.6433 0.4671 0.7173 0.040 Uiso 1 1 d R U . . .
B2 B 0.7807(2) 0.0576(3) 0.63580(15) 0.0164(7) Uani 1 1 d . . . . .
C16 C 0.5646(2) 0.3616(3) 0.49629(15) 0.0274(8) Uani 1 1 d . . . . .
H16A H 0.5702 0.2938 0.4930 0.033 Uiso 1 1 d R U . . .
H16B H 0.6015 0.3934 0.4769 0.033 Uiso 1 1 d R U . . .
H16C H 0.5061 0.3800 0.4779 0.033 Uiso 1 1 d R U . . .
C5 C 0.7855(2) 0.1832(2) 0.35116(15) 0.0293(8) Uani 1 1 d . . . . .
H5 H 0.7470 0.1603 0.3166 0.035 Uiso 1 1 d R U . . .
C36 C 0.6324(2) 0.0600(3) 0.70118(14) 0.0251(7) Uani 1 1 d . . . . .
C4 C 0.8718(2) 0.1875(3) 0.35539(16) 0.0325(8) Uani 1 1 d . . . . .
H4 H 0.8917 0.1674 0.3241 0.039 Uiso 1 1 d R U . . .
C15 C 0.7839(2) 0.3975(3) 0.69762(15) 0.0306(8) Uani 1 1 d . . . . .
H15A H 0.7956 0.3313 0.7071 0.037 Uiso 1 1 d R U . . .
H15B H 0.7885 0.4329 0.7333 0.037 Uiso 1 1 d R U . . .
H15C H 0.8247 0.4218 0.6787 0.037 Uiso 1 1 d R U . . .
C38 C 0.6675(2) 0.1596(3) 0.71136(16) 0.0334(8) Uani 1 1 d . . . . .
H38A H 0.6372 0.1997 0.6791 0.040 Uiso 1 1 d R U . . .
H38B H 0.7275 0.1589 0.7137 0.040 Uiso 1 1 d R U . . .
H38C H 0.6603 0.1839 0.7477 0.040 Uiso 1 1 d R U . . .
C3 C 0.9283(2) 0.2216(3) 0.40659(16) 0.0281(8) Uani 1 1 d . . . . .
H3 H 0.9865 0.2249 0.4093 0.034 Uiso 1 1 d R U . . .
C22 C 0.7172(3) 0.6081(4) 0.5435(3) 0.0754(18) Uani 1 1 d . U . . .
H22A H 0.7179 0.6459 0.5096 0.090 Uiso 1 1 d R U . . .
H22B H 0.7249 0.6489 0.5774 0.090 Uiso 1 1 d R U . . .
H22C H 0.6632 0.5754 0.5359 0.090 Uiso 1 1 d R U . . .
C29 C 0.9519(2) 0.2675(3) 0.66525(16) 0.0305(8) Uani 1 1 d . . . . .
H29A H 0.8941 0.2879 0.6463 0.037 Uiso 1 1 d R U . . .
H29B H 0.9912 0.3172 0.6625 0.037 Uiso 1 1 d R U . . .
H29C H 0.9579 0.2537 0.7062 0.037 Uiso 1 1 d R U . . .
C41 C 0.9930(2) 0.0051(3) 0.73764(16) 0.0343(9) Uani 1 1 d . . . . .
H41A H 0.9970 -0.0550 0.7579 0.041 Uiso 1 1 d R U . . .
H41B H 1.0357 0.0481 0.7606 0.041 Uiso 1 1 d R U . . .
H41C H 1.0024 -0.0047 0.6996 0.041 Uiso 1 1 d R U . . .
C25 C 1.0559(2) 0.1569(3) 0.63810(16) 0.0307(8) Uani 1 1 d . . . . .
H25 H 1.1000 0.1961 0.6597 0.037 Uiso 1 1 d R U . . .
C30 C 0.8546(2) -0.0179(3) 0.53175(15) 0.0281(8) Uani 1 1 d . . . . .
H30A H 0.8218 0.0213 0.4998 0.034 Uiso 1 1 d R U . . .
H30B H 0.8176 -0.0420 0.5538 0.034 Uiso 1 1 d R U . . .
H30C H 0.8793 -0.0703 0.5161 0.034 Uiso 1 1 d R U . . .
C13 C 0.5276(2) 0.4288(3) 0.58372(17) 0.0322(8) Uani 1 1 d . . . . .
H13 H 0.4717 0.4356 0.5594 0.039 Uiso 1 1 d R U . . .
C27 C 1.0104(2) 0.0224(3) 0.57553(16) 0.0293(8) Uani 1 1 d . . . . .
H27 H 1.0236 -0.0287 0.5544 0.035 Uiso 1 1 d R U . . .
C26 C 1.0757(2) 0.0788(3) 0.60949(17) 0.0338(9) Uani 1 1 d . . . . .
H26 H 1.1327 0.0634 0.6131 0.041 Uiso 1 1 d R U . . .
C46 C 0.6037(2) -0.0892(3) 0.39420(16) 0.0286(8) Uani 1 1 d . . . . .
C37 C 0.6023(2) -0.1405(3) 0.58697(16) 0.0325(8) Uani 1 1 d . . . . .
H37A H 0.5965 -0.2072 0.5944 0.039 Uiso 1 1 d R U . . .
H37B H 0.6562 -0.1297 0.5788 0.039 Uiso 1 1 d R U . . .
H37C H 0.5561 -0.1208 0.5535 0.039 Uiso 1 1 d R U . . .
C7 C 0.9656(2) 0.2890(3) 0.50881(15) 0.0319(8) Uani 1 1 d . . . . .
H7A H 0.9901 0.2367 0.5344 0.038 Uiso 1 1 d R U . . .
H7B H 0.9380 0.3322 0.5293 0.038 Uiso 1 1 d R U . . .
H7C H 1.0102 0.3221 0.4974 0.038 Uiso 1 1 d R U . . .
C43 C 0.7993(2) -0.1373(3) 0.74374(18) 0.0423(10) Uani 1 1 d . . . . .
H43A H 0.8527 -0.1386 0.7747 0.051 Uiso 1 1 d R U . . .
H43B H 0.7756 -0.2006 0.7376 0.051 Uiso 1 1 d R U . . .
H43C H 0.7597 -0.0955 0.7549 0.051 Uiso 1 1 d R U . . .
C33 C 0.5554(2) -0.1191(3) 0.67860(17) 0.0338(9) Uani 1 1 d . . . . .
H33 H 0.5296 -0.1789 0.6713 0.041 Uiso 1 1 d R U . . .
C17 C 0.7863(2) 0.4956(4) 0.45132(18) 0.0532(13) Uani 1 1 d D . . . .
H17 H 0.7770 0.5637 0.4571 0.064 Uiso 1 1 d R U . . .
C39 C 0.9041(2) 0.0475(3) 0.72928(14) 0.0259(8) Uani 1 1 d . . . . .
H39 H 0.9071 0.1126 0.7148 0.031 Uiso 1 1 d R U . . .
C42 C 0.8153(2) -0.1013(2) 0.68671(15) 0.0263(8) Uani 1 1 d . . . . .
H42 H 0.7611 -0.1117 0.6557 0.032 Uiso 1 1 d R U . . .
C44 C 0.8812(2) -0.1658(3) 0.66981(18) 0.0383(9) Uani 1 1 d . . . . .
H44A H 0.8949 -0.1396 0.6360 0.046 Uiso 1 1 d R U . . .
H44B H 0.8574 -0.2286 0.6604 0.046 Uiso 1 1 d R U . . .
H44C H 0.9324 -0.1696 0.7025 0.046 Uiso 1 1 d R U . . .
C47 C 0.6675(3) -0.0636(3) 0.36078(18) 0.0405(10) Uani 1 1 d . . . . .
H47A H 0.7251 -0.0632 0.3878 0.049 Uiso 1 1 d R U . . .
H47B H 0.6549 0.0001 0.3444 0.049 Uiso 1 1 d R U . . .
C19 C 0.7125(3) 0.4816(4) 0.40143(18) 0.0602(14) Uani 1 1 d . . . . .
H19A H 0.7121 0.4167 0.3882 0.072 Uiso 1 1 d R U . . .
H19B H 0.7147 0.5240 0.3699 0.072 Uiso 1 1 d R U . . .
H19C H 0.6612 0.4937 0.4128 0.072 Uiso 1 1 d R U . . .
C35 C 0.5871(2) 0.0218(3) 0.73762(16) 0.0341(9) Uani 1 1 d . . . . .
H35 H 0.5818 0.0571 0.7698 0.041 Uiso 1 1 d R U . . .
C40 C 0.8878(3) 0.0589(3) 0.79001(16) 0.0445(10) Uani 1 1 d . . . . .
H40A H 0.8296 0.0791 0.7849 0.053 Uiso 1 1 d R U . . .
H40B H 0.9265 0.1059 0.8127 0.053 Uiso 1 1 d R U . . .
H40C H 0.8974 -0.0011 0.8105 0.053 Uiso 1 1 d R U . . .
C34 C 0.5492(2) -0.0672(3) 0.72677(17) 0.0386(10) Uani 1 1 d . . . . .
H34 H 0.5198 -0.0920 0.7520 0.046 Uiso 1 1 d R U . . .
B1 B 0.7683(2) 0.3667(3) 0.52401(15) 0.0181(7) Uani 1 1 d . . . . .
C12 C 0.5472(2) 0.4578(3) 0.64167(18) 0.0381(9) Uani 1 1 d . . . . .
H12 H 0.5050 0.4844 0.6565 0.046 Uiso 1 1 d R U . . .
C18 C 0.8714(3) 0.5042(4) 0.44217(19) 0.0609(14) Uani 1 1 d D . . . .
H18A H 0.9138 0.5143 0.4795 0.073 Uiso 1 1 d R U . . .
H18B H 0.8718 0.5572 0.4164 0.073 Uiso 1 1 d R U . . .
H18C H 0.8844 0.4465 0.4244 0.073 Uiso 1 1 d R U . . .
C49 C 0.6741(3) -0.2351(3) 0.3333(2) 0.0597(14) Uani 1 1 d . U . . .
H49A H 0.7321 -0.2442 0.3589 0.072 Uiso 1 1 d R U . . .
H49B H 0.6656 -0.2783 0.3000 0.072 Uiso 1 1 d R U . . .
C21 C 0.8759(3) 0.5788(4) 0.5772(2) 0.0611(14) Uani 1 1 d . U . . .
H21A H 0.8874 0.6170 0.5465 0.073 Uiso 1 1 d R U . . .
H21B H 0.9176 0.5284 0.5879 0.073 Uiso 1 1 d R U . . .
H21C H 0.8793 0.6180 0.6112 0.073 Uiso 1 1 d R U . . .
C50 C 0.6098(4) -0.2587(3) 0.3672(3) 0.0802(19) Uani 1 1 d . U . . .
H50A H 0.6203 -0.3231 0.3828 0.096 Uiso 1 1 d R U . . .
H50B H 0.5520 -0.2566 0.3404 0.096 Uiso 1 1 d R U . . .
C48 C 0.6633(3) -0.1337(3) 0.3112(2) 0.0514(12) Uani 1 1 d . . . . .
H48A H 0.6085 -0.1271 0.2811 0.062 Uiso 1 1 d R U . . .
H48B H 0.7083 -0.1189 0.2930 0.062 Uiso 1 1 d R U . . .
C51 C 0.6163(3) -0.1896(3) 0.4180(2) 0.0538(13) Uani 1 1 d . U . . .
H51A H 0.5726 -0.2047 0.4373 0.065 Uiso 1 1 d R U . . .
H51B H 0.6722 -0.1954 0.4469 0.065 Uiso 1 1 d 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 N4 1.872(2) . ?
Ge1 N1 1.874(2) . ?
Ge1 N2 1.882(3) . ?
Ge1 B1 2.399(4) . ?
Ge1 Ge2 2.4679(5) . ?
Ge2 N5 1.913(2) . ?
Ge2 C45 2.098(4) . ?
N1 C1 1.418(4) . ?
N1 B1 1.459(4) . ?
C20 N3 1.489(5) . ?
C20 C22 1.492(6) . ?
C20 C21 1.496(5) . ?
C20 H20 0.9801 . ?
N4 C23 1.438(4) . ?
N4 B2 1.457(4) . ?
C9 C10 1.398(4) . ?
C9 C14 1.411(4) . ?
C9 N2 1.422(4) . ?
N2 B1 1.477(4) . ?
N5 C31 1.429(4) . ?
N5 B2 1.461(4) . ?
C31 C32 1.403(5) . ?
C31 C36 1.411(5) . ?
N6 B2 1.448(4) . ?
N6 C42 1.470(4) . ?
N6 C39 1.474(4) . ?
N7 C45 1.147(4) . ?
N7 C46 1.448(4) . ?
N3 B1 1.415(4) . ?
N3 C17 1.456(5) . ?
C23 C24 1.398(4) . ?
C23 C28 1.406(4) . ?
C32 C33 1.395(5) . ?
C32 C37 1.502(5) . ?
C2 C3 1.388(5) . ?
C2 C1 1.403(4) . ?
C2 C7 1.503(5) . ?
C28 C27 1.389(4) . ?
C28 C30 1.508(4) . ?
C6 C5 1.391(5) . ?
C6 C1 1.406(4) . ?
C6 C8 1.506(4) . ?
C14 C13 1.393(5) . ?
C14 C16 1.497(5) . ?
C10 C11 1.400(5) . ?
C10 C15 1.509(5) . ?
C24 C25 1.400(4) . ?
C24 C29 1.494(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9300 . ?
C16 H16A 0.9599 . ?
C16 H16B 0.9601 . ?
C16 H16C 0.9600 . ?
C5 C4 1.377(5) . ?
C5 H5 0.9301 . ?
C36 C35 1.388(5) . ?
C36 C38 1.499(5) . ?
C4 C3 1.376(5) . ?
C4 H4 0.9301 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9601 . ?
C15 H15C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9599 . ?
C3 H3 0.9300 . ?
C22 H22A 0.9602 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9601 . ?
C41 C39 1.522(5) . ?
C41 H41A 0.9599 . ?
C41 H41B 0.9601 . ?
C41 H41C 0.9599 . ?
C25 C26 1.371(5) . ?
C25 H25 0.9301 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9599 . ?
C30 H30C 0.9600 . ?
C13 C12 1.372(5) . ?
C13 H13 0.9301 . ?
C27 C26 1.379(5) . ?
C27 H27 0.9300 . ?
C26 H26 0.9300 . ?
C46 C51 1.505(6) . ?
C46 C47 1.512(5) . ?
C37 H37A 0.9601 . ?
C37 H37B 0.9599 . ?
C37 H37C 0.9600 . ?
C7 H7A 0.9601 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9601 . ?
C43 C42 1.525(5) . ?
C43 H43A 0.9601 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C33 C34 1.375(6) . ?
C33 H33 0.9300 . ?
C17 C19 1.432(5) . ?
C17 C18 1.464(5) . ?
C17 H17 0.9800 . ?
C39 C40 1.535(5) . ?
C39 H39 0.9800 . ?
C42 C44 1.537(5) . ?
C42 H42 0.9799 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9601 . ?
C44 H44C 0.9599 . ?
C47 C48 1.512(6) . ?
C47 H47A 0.9701 . ?
C47 H47B 0.9699 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9598 . ?
C19 H19C 0.9600 . ?
C35 C34 1.381(6) . ?
C35 H35 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9601 . ?
C40 H40C 0.9600 . ?
C34 H34 0.9301 . ?
C12 H12 0.9300 . ?
C18 H18A 0.9599 . ?
C18 H18B 0.9602 . ?
C18 H18C 0.9599 . ?
C49 C48 1.506(6) . ?
C49 C50 1.521(6) . ?
C49 H49A 0.9701 . ?
C49 H49B 0.9699 . ?
C21 H21A 0.9599 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9601 . ?
C50 C51 1.518(6) . ?
C50 H50A 0.9699 . ?
C50 H50B 0.9699 . ?
C48 H48A 0.9701 . ?
C48 H48B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ge1 N1 116.82(11) . . ?
N4 Ge1 N2 115.75(11) . . ?
N1 Ge1 N2 75.38(11) . . ?
N4 Ge1 B1 126.00(11) . . ?
N1 Ge1 B1 37.46(11) . . ?
N2 Ge1 B1 38.01(11) . . ?
N4 Ge1 Ge2 95.79(8) . . ?
N1 Ge1 Ge2 137.03(8) . . ?
N2 Ge1 Ge2 116.32(7) . . ?
B1 Ge1 Ge2 136.19(8) . . ?
N5 Ge2 C45 96.42(12) . . ?
N5 Ge2 Ge1 84.90(7) . . ?
C45 Ge2 Ge1 92.59(9) . . ?
C1 N1 B1 135.5(3) . . ?
C1 N1 Ge1 133.2(2) . . ?
B1 N1 Ge1 91.22(19) . . ?
N3 C20 C22 115.5(3) . . ?
N3 C20 C21 114.1(3) . . ?
C22 C20 C21 113.8(4) . . ?
N3 C20 H20 103.9 . . ?
C22 C20 H20 103.9 . . ?
C21 C20 H20 103.8 . . ?
C23 N4 B2 119.0(2) . . ?
C23 N4 Ge1 122.44(19) . . ?
B2 N4 Ge1 115.56(19) . . ?
C10 C9 C14 119.4(3) . . ?
C10 C9 N2 119.6(3) . . ?
C14 C9 N2 121.0(3) . . ?
C9 N2 B1 128.7(3) . . ?
C9 N2 Ge1 123.6(2) . . ?
B1 N2 Ge1 90.32(19) . . ?
C31 N5 B2 121.6(2) . . ?
C31 N5 Ge2 109.30(18) . . ?
B2 N5 Ge2 124.7(2) . . ?
C32 C31 C36 119.8(3) . . ?
C32 C31 N5 120.5(3) . . ?
C36 C31 N5 119.6(3) . . ?
B2 N6 C42 119.0(3) . . ?
B2 N6 C39 119.4(3) . . ?
C42 N6 C39 121.6(3) . . ?
C45 N7 C46 177.9(3) . . ?
B1 N3 C17 126.3(3) . . ?
B1 N3 C20 117.2(3) . . ?
C17 N3 C20 116.5(3) . . ?
N7 C45 Ge2 165.9(3) . . ?
C24 C23 C28 120.1(3) . . ?
C24 C23 N4 121.2(3) . . ?
C28 C23 N4 118.7(3) . . ?
C33 C32 C31 119.1(3) . . ?
C33 C32 C37 119.5(3) . . ?
C31 C32 C37 121.4(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C7 119.1(3) . . ?
C1 C2 C7 121.7(3) . . ?
C27 C28 C23 119.2(3) . . ?
C27 C28 C30 119.9(3) . . ?
C23 C28 C30 120.8(3) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C8 119.2(3) . . ?
C1 C6 C8 121.1(3) . . ?
C2 C1 C6 119.2(3) . . ?
C2 C1 N1 121.5(3) . . ?
C6 C1 N1 119.3(3) . . ?
C13 C14 C9 119.1(3) . . ?
C13 C14 C16 118.8(3) . . ?
C9 C14 C16 122.1(3) . . ?
C9 C10 C11 119.6(3) . . ?
C9 C10 C15 121.2(3) . . ?
C11 C10 C15 119.2(3) . . ?
C23 C24 C25 118.3(3) . . ?
C23 C24 C29 121.8(3) . . ?
C25 C24 C29 119.9(3) . . ?
C6 C8 H8A 109.7 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.3 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C11 C10 120.8(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.4 . . ?
N6 B2 N4 121.6(3) . . ?
N6 B2 N5 120.5(3) . . ?
N4 B2 N5 117.9(3) . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.4 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.4 . . ?
C35 C36 C31 118.8(3) . . ?
C35 C36 C38 120.3(3) . . ?
C31 C36 C38 120.8(3) . . ?
C3 C4 C5 119.2(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.5 . . ?
C10 C15 H15A 109.4 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.6 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C36 C38 H38A 109.4 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.6 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C4 C3 C2 121.7(3) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.0 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.7 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.2 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.8 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.1 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C39 C41 H41A 109.4 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.4 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C26 C25 C24 121.6(3) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C28 C30 H30A 109.4 . . ?
C28 C30 H30B 109.4 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.6 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C12 C13 C14 121.5(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.2 . . ?
C26 C27 C28 120.9(3) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.5 . . ?
C25 C26 C27 119.6(3) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.0 . . ?
N7 C46 C51 108.6(3) . . ?
N7 C46 C47 109.3(3) . . ?
C51 C46 C47 111.9(3) . . ?
C32 C37 H37A 109.6 . . ?
C32 C37 H37B 109.3 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.6 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.3 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C42 C43 H43A 109.4 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C34 C33 C32 121.0(4) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C19 C17 C18 119.6(4) . . ?
C19 C17 N3 116.8(3) . . ?
C18 C17 N3 118.9(3) . . ?
C19 C17 H17 97.0 . . ?
C18 C17 H17 97.4 . . ?
N3 C17 H17 97.4 . . ?
N6 C39 C41 116.2(3) . . ?
N6 C39 C40 114.0(3) . . ?
C41 C39 C40 109.2(3) . . ?
N6 C39 H39 105.4 . . ?
C41 C39 H39 105.6 . . ?
C40 C39 H39 105.5 . . ?
N6 C42 C43 116.1(3) . . ?
N6 C42 C44 114.0(3) . . ?
C43 C42 C44 109.9(3) . . ?
N6 C42 H42 105.1 . . ?
C43 C42 H42 105.3 . . ?
C44 C42 H42 105.3 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.6 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.4 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C47 C48 111.2(3) . . ?
C46 C47 H47A 109.6 . . ?
C48 C47 H47A 109.5 . . ?
C46 C47 H47B 109.1 . . ?
C48 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C17 C19 H19A 108.8 . . ?
C17 C19 H19B 110.0 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.6 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C34 C35 C36 121.4(4) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.3 . . ?
C39 C40 H40A 109.8 . . ?
C39 C40 H40B 109.3 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.3 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C33 C34 C35 119.7(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.1 . . ?
N3 B1 N1 132.3(3) . . ?
N3 B1 N2 124.8(3) . . ?
N1 B1 N2 102.9(3) . . ?
N3 B1 Ge1 175.7(2) . . ?
N1 B1 Ge1 51.33(15) . . ?
N2 B1 Ge1 51.67(15) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.0 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.2 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C48 C49 C50 110.9(4) . . ?
C48 C49 H49A 109.7 . . ?
C50 C49 H49A 109.6 . . ?
C48 C49 H49B 109.4 . . ?
C50 C49 H49B 109.2 . . ?
H49A C49 H49B 108.0 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.2 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.8 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C51 C50 C49 111.7(4) . . ?
C51 C50 H50A 109.3 . . ?
C49 C50 H50A 109.1 . . ?
C51 C50 H50B 109.4 . . ?
C49 C50 H50B 109.4 . . ?
H50A C50 H50B 107.9 . . ?
C49 C48 C47 111.6(4) . . ?
C49 C48 H48A 109.5 . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48B 109.0 . . ?
C47 C48 H48B 109.3 . . ?
H48A C48 H48B 108.0 . . ?
C46 C51 C50 109.3(4) . . ?
C46 C51 H51A 109.7 . . ?
C50 C51 H51A 109.6 . . ?
C46 C51 H51B 110.0 . . ?
C50 C51 H51B 110.0 . . ?
H51A C51 H51B 108.2 . . ?

_refine_diff_density_max         0.795
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.101

_shelxl_version_number           2013-4



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

data_ld140304Ge1
_database_code_depnum_ccdc_archive 'CCDC 1971051'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H42 B Ge N5'
_chemical_formula_sum            'C29 H42 B Ge N5'
_chemical_formula_weight         544.07

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.9688(11)
_cell_length_b                   11.0690(6)
_cell_length_c                   15.7622(13)
_cell_angle_alpha                90
_cell_angle_beta                 102.325(6)
_cell_angle_gamma                90
_cell_volume                     2892.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    29521
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.133
_exptl_absorpt_coefficient_mu    1.085
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.066
0 0 -1 0.036
1 1 0 0.115
-1 -1 0 0.133
1 -1 0 0.061
-1 1 0 0.084
1 0 0 0.116


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            29521
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.212
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6529
_reflns_number_gt                5274
_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       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0196P)²+2.3361P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6529
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0740
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.84212(2) 0.06376(2) 0.34462(2) 0.01772(6) Uani 1 1 d . . . . .
N3 N 0.78117(9) 0.17576(14) 0.39785(10) 0.0175(3) Uani 1 1 d . . . . .
N4 N 0.87468(9) -0.04550(15) 0.45711(10) 0.0195(3) Uani 1 1 d . . . . .
N2 N 0.73153(9) 0.01187(15) 0.31443(10) 0.0185(3) Uani 1 1 d . . . . .
N5 N 0.94030(10) -0.27210(16) 0.67227(11) 0.0274(4) Uani 1 1 d . . . . .
C26 C 0.96561(11) -0.19050(18) 0.53793(12) 0.0204(4) Uani 1 1 d . . . . .
H26 H 1.0119 -0.2370 0.5420 0.025 Uiso 1 1 d R U . . .
C25 C 0.92032(11) -0.19694(18) 0.60339(12) 0.0212(4) Uani 1 1 d . . . . .
N1 N 0.62721(9) 0.15591(15) 0.36559(10) 0.0202(3) Uani 1 1 d . . . . .
C23 C 0.83210(11) -0.04995(19) 0.51981(13) 0.0237(4) Uani 1 1 d . . . . .
H23 H 0.7862 -0.0021 0.5134 0.028 Uiso 1 1 d R U . . .
B1 B 0.70469(13) 0.1162(2) 0.35608(13) 0.0178(4) Uani 1 1 d . . . . .
C8 C 0.68314(11) -0.19735(18) 0.29411(13) 0.0225(4) Uani 1 1 d . . . . .
C7 C 0.70226(11) -0.08640(17) 0.26019(12) 0.0185(4) Uani 1 1 d . . . . .
C12 C 0.69849(11) -0.0771(2) 0.16965(12) 0.0238(4) Uani 1 1 d . . . . .
C27 C 0.94094(11) -0.11547(18) 0.46863(12) 0.0196(4) Uani 1 1 d . . . . .
H27 H 0.9720 -0.1121 0.4267 0.024 Uiso 1 1 d R U . . .
C1 C 0.54831(11) 0.11509(19) 0.31444(13) 0.0233(4) Uani 1 1 d . . . . .
H1 H 0.5078 0.1691 0.3299 0.028 Uiso 1 1 d R U . . .
C24 C 0.85220(12) -0.12047(19) 0.59197(13) 0.0244(4) Uani 1 1 d . . . . .
H24 H 0.8210 -0.1182 0.6338 0.029 Uiso 1 1 d R U . . .
C15 C 0.80251(11) 0.29905(18) 0.41015(13) 0.0200(4) Uani 1 1 d . . . . .
C4 C 0.62169(12) 0.2444(2) 0.43441(13) 0.0248(4) Uani 1 1 d . . . . .
H4 H 0.6771 0.2625 0.4646 0.030 Uiso 1 1 d R U . . .
C17 C 0.81150(13) 0.5017(2) 0.35613(16) 0.0326(5) Uani 1 1 d . . . . .
H17 H 0.7987 0.5574 0.3111 0.039 Uiso 1 1 d R U . . .
C22 C 0.86319(13) 0.2510(2) 0.56723(14) 0.0309(5) Uani 1 1 d . . . . .
H22A H 0.8943 0.2914 0.6172 0.037 Uiso 1 1 d R U . . .
H22B H 0.8928 0.1827 0.5531 0.037 Uiso 1 1 d R U . . .
H22C H 0.8131 0.2241 0.5796 0.037 Uiso 1 1 d R U . . .
C21 C 0.74085(14) 0.3463(2) 0.25229(14) 0.0310(5) Uani 1 1 d . . . . .
H21A H 0.7333 0.4155 0.2147 0.037 Uiso 1 1 d R U . . .
H21B H 0.6893 0.3134 0.2556 0.037 Uiso 1 1 d R U . . .
H21C H 0.7717 0.2864 0.2296 0.037 Uiso 1 1 d R U . . .
C16 C 0.78509(12) 0.38323(19) 0.34179(13) 0.0239(4) Uani 1 1 d . . . . .
C29 C 1.01331(13) -0.3454(2) 0.68604(15) 0.0323(5) Uani 1 1 d . . . . .
H29A H 1.0170 -0.3841 0.6325 0.039 Uiso 1 1 d R U . . .
H29B H 1.0114 -0.4057 0.7293 0.039 Uiso 1 1 d R U . . .
H29C H 1.0596 -0.2947 0.7051 0.039 Uiso 1 1 d R U . . .
C20 C 0.84662(12) 0.33699(19) 0.49179(13) 0.0243(4) Uani 1 1 d . . . . .
C11 C 0.67488(13) -0.1767(2) 0.11677(14) 0.0329(5) Uani 1 1 d . . . . .
H11 H 0.6721 -0.1700 0.0574 0.040 Uiso 1 1 d R U . . .
C2 C 0.54169(12) 0.1305(2) 0.21758(13) 0.0290(5) Uani 1 1 d . . . . .
H2A H 0.5536 0.2126 0.2052 0.035 Uiso 1 1 d R U . . .
H2B H 0.4879 0.1108 0.1874 0.035 Uiso 1 1 d R U . . .
H2C H 0.5793 0.0775 0.1987 0.035 Uiso 1 1 d R U . . .
C10 C 0.65552(13) -0.2852(2) 0.15021(16) 0.0334(5) Uani 1 1 d . . . . .
H10 H 0.6399 -0.3511 0.1139 0.040 Uiso 1 1 d R U . . .
C6 C 0.57935(14) 0.1922(2) 0.50248(14) 0.0382(6) Uani 1 1 d . . . . .
H6A H 0.5247 0.1726 0.4754 0.046 Uiso 1 1 d R U . . .
H6B H 0.5796 0.2506 0.5476 0.046 Uiso 1 1 d R U . . .
H6C H 0.6069 0.1204 0.5270 0.046 Uiso 1 1 d R U . . .
C9 C 0.65972(12) -0.2947(2) 0.23848(15) 0.0293(5) Uani 1 1 d . . . . .
H9 H 0.6467 -0.3678 0.2612 0.035 Uiso 1 1 d R U . . .
C3 C 0.52483(13) -0.0125(2) 0.33598(15) 0.0306(5) Uani 1 1 d . . . . .
H3A H 0.5579 -0.0700 0.3142 0.037 Uiso 1 1 d R U . . .
H3B H 0.4692 -0.0267 0.3096 0.037 Uiso 1 1 d R U . . .
H3C H 0.5327 -0.0211 0.3978 0.037 Uiso 1 1 d R U . . .
C19 C 0.87300(13) 0.4563(2) 0.50290(16) 0.0349(5) Uani 1 1 d . . . . .
H19 H 0.9030 0.4807 0.5566 0.042 Uiso 1 1 d R U . . .
C13 C 0.68829(14) -0.2143(2) 0.38977(14) 0.0322(5) Uani 1 1 d . . . . .
H13A H 0.6501 -0.2745 0.3984 0.039 Uiso 1 1 d R U . . .
H13B H 0.6764 -0.1393 0.4150 0.039 Uiso 1 1 d R U . . .
H13C H 0.7417 -0.2400 0.4170 0.039 Uiso 1 1 d R U . . .
C5 C 0.58367(14) 0.3640(2) 0.39925(16) 0.0365(5) Uani 1 1 d . . . . .
H5A H 0.6114 0.3954 0.3569 0.044 Uiso 1 1 d R U . . .
H5B H 0.5875 0.4208 0.4460 0.044 Uiso 1 1 d R U . . .
H5C H 0.5279 0.3511 0.3726 0.044 Uiso 1 1 d R U . . .
C28 C 0.89704(15) -0.2673(2) 0.74237(15) 0.0403(6) Uani 1 1 d . . . . .
H28A H 0.9090 -0.1926 0.7734 0.048 Uiso 1 1 d R U . . .
H28B H 0.9134 -0.3338 0.7813 0.048 Uiso 1 1 d R U . . .
H28C H 0.8401 -0.2724 0.7187 0.048 Uiso 1 1 d R U . . .
C14 C 0.72251(14) 0.0376(2) 0.13128(14) 0.0333(5) Uani 1 1 d . . . . .
H14A H 0.7120 0.0304 0.0692 0.040 Uiso 1 1 d R U . . .
H14B H 0.7790 0.0519 0.1531 0.040 Uiso 1 1 d R U . . .
H14C H 0.6920 0.1039 0.1470 0.040 Uiso 1 1 d R U . . .
C18 C 0.85582(14) 0.5385(2) 0.43572(17) 0.0385(6) Uani 1 1 d . . . . .
H18 H 0.8739 0.6178 0.4439 0.046 Uiso 1 1 d 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 N3 1.9186(15) . ?
Ge1 N2 1.9226(15) . ?
Ge1 N4 2.1198(16) . ?
Ge1 B1 2.447(2) . ?
N3 C15 1.415(2) . ?
N3 B1 1.479(3) . ?
N4 C23 1.344(2) . ?
N4 C27 1.345(2) . ?
N2 C7 1.407(2) . ?
N2 B1 1.449(3) . ?
N5 C25 1.352(3) . ?
N5 C28 1.452(3) . ?
N5 C29 1.458(3) . ?
C26 C27 1.365(3) . ?
C26 C25 1.414(3) . ?
C26 H26 0.9301 . ?
C25 C24 1.413(3) . ?
N1 B1 1.424(3) . ?
N1 C1 1.478(2) . ?
N1 C4 1.479(3) . ?
C23 C24 1.362(3) . ?
C23 H23 0.9300 . ?
C8 C9 1.393(3) . ?
C8 C7 1.405(3) . ?
C8 C13 1.503(3) . ?
C7 C12 1.419(3) . ?
C12 C11 1.388(3) . ?
C12 C14 1.500(3) . ?
C27 H27 0.9299 . ?
C1 C2 1.516(3) . ?
C1 C3 1.525(3) . ?
C1 H1 0.9800 . ?
C24 H24 0.9300 . ?
C15 C16 1.407(3) . ?
C15 C20 1.408(3) . ?
C4 C5 1.525(3) . ?
C4 C6 1.526(3) . ?
C4 H4 0.9800 . ?
C17 C18 1.379(3) . ?
C17 C16 1.389(3) . ?
C17 H17 0.9300 . ?
C22 C20 1.502(3) . ?
C22 H22A 0.9599 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 C16 1.506(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9601 . ?
C29 H29A 0.9599 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C20 C19 1.393(3) . ?
C11 C10 1.380(3) . ?
C11 H11 0.9300 . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9599 . ?
C10 C9 1.382(3) . ?
C10 H10 0.9300 . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9601 . ?
C9 H9 0.9300 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9601 . ?
C3 H3C 0.9601 . ?
C19 C18 1.380(3) . ?
C19 H19 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9599 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9599 . ?
C5 H5C 0.9602 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9601 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9601 . ?
C14 H14C 0.9600 . ?
C18 H18 0.9300 . ?

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
N3 Ge1 N2 73.29(7) . . ?
N3 Ge1 N4 94.10(6) . . ?
N2 Ge1 N4 95.91(6) . . ?
N3 Ge1 B1 37.19(7) . . ?
N2 Ge1 B1 36.28(7) . . ?
N4 Ge1 B1 98.97(6) . . ?
C15 N3 B1 131.74(16) . . ?
C15 N3 Ge1 122.50(12) . . ?
B1 N3 Ge1 91.20(12) . . ?
C23 N4 C27 116.41(16) . . ?
C23 N4 Ge1 123.43(13) . . ?
C27 N4 Ge1 120.16(13) . . ?
C7 N2 B1 141.91(16) . . ?
C7 N2 Ge1 125.50(12) . . ?
B1 N2 Ge1 91.98(12) . . ?
C25 N5 C28 120.51(18) . . ?
C25 N5 C29 121.42(18) . . ?
C28 N5 C29 117.29(17) . . ?
C27 C26 C25 119.55(18) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.4 . . ?
N5 C25 C24 121.93(18) . . ?
N5 C25 C26 122.33(18) . . ?
C24 C25 C26 115.74(18) . . ?
B1 N1 C1 126.65(17) . . ?
B1 N1 C4 119.08(16) . . ?
C1 N1 C4 114.24(15) . . ?
N4 C23 C24 123.86(18) . . ?
N4 C23 H23 118.0 . . ?
C24 C23 H23 118.2 . . ?
N1 B1 N2 132.87(18) . . ?
N1 B1 N3 123.87(18) . . ?
N2 B1 N3 103.07(16) . . ?
N1 B1 Ge1 175.33(16) . . ?
N2 B1 Ge1 51.74(9) . . ?
N3 B1 Ge1 51.62(9) . . ?
C9 C8 C7 119.67(19) . . ?
C9 C8 C13 118.87(19) . . ?
C7 C8 C13 121.45(18) . . ?
C8 C7 N2 121.66(17) . . ?
C8 C7 C12 118.78(18) . . ?
N2 C7 C12 119.32(17) . . ?
C11 C12 C7 119.5(2) . . ?
C11 C12 C14 119.90(19) . . ?
C7 C12 C14 120.59(18) . . ?
N4 C27 C26 124.26(18) . . ?
N4 C27 H27 117.7 . . ?
C26 C27 H27 118.0 . . ?
N1 C1 C2 112.25(16) . . ?
N1 C1 C3 114.25(17) . . ?
C2 C1 C3 111.19(18) . . ?
N1 C1 H1 106.2 . . ?
C2 C1 H1 106.1 . . ?
C3 C1 H1 106.2 . . ?
C23 C24 C25 120.14(18) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 120.0 . . ?
C16 C15 C20 119.09(19) . . ?
C16 C15 N3 121.86(17) . . ?
C20 C15 N3 118.94(18) . . ?
N1 C4 C5 113.36(17) . . ?
N1 C4 C6 112.22(18) . . ?
C5 C4 C6 110.97(19) . . ?
N1 C4 H4 106.7 . . ?
C5 C4 H4 106.6 . . ?
C6 C4 H4 106.5 . . ?
C18 C17 C16 121.4(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.2 . . ?
C20 C22 H22A 109.4 . . ?
C20 C22 H22B 109.6 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C21 H21A 109.6 . . ?
C16 C21 H21B 109.3 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C16 C15 119.5(2) . . ?
C17 C16 C21 119.2(2) . . ?
C15 C16 C21 121.26(19) . . ?
N5 C29 H29A 109.3 . . ?
N5 C29 H29B 109.6 . . ?
H29A C29 H29B 109.5 . . ?
N5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C19 C20 C15 119.4(2) . . ?
C19 C20 C22 120.0(2) . . ?
C15 C20 C22 120.51(19) . . ?
C10 C11 C12 121.6(2) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.4 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.4 . . ?
C4 C6 H6A 109.2 . . ?
C4 C6 H6B 109.7 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C10 C9 C8 121.4(2) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.6 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.4 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C18 C19 C20 121.3(2) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.3 . . ?
C8 C13 H13A 109.4 . . ?
C8 C13 H13B 109.6 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.4 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.3 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C28 H28A 109.5 . . ?
N5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N5 C28 H28C 109.4 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.4 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.6 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.5 . . ?

_refine_diff_density_max         0.308
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.064

_shelxl_version_number           2013-4

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

data_ld180515Ge1
_database_code_depnum_ccdc_archive 'CCDC 1971054'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C67 H82 B2 F5 Ge2 N6 O'
_chemical_formula_weight         1249.18

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'

_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                   13.2217(10)
_cell_length_b                   13.5451(11)
_cell_length_c                   20.1024(15)
_cell_angle_alpha                78.791(2)
_cell_angle_beta                 74.532(2)
_cell_angle_gamma                66.824(2)
_cell_volume                     3173.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    120157
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1306
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.194
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5596
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.750
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            120157
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.417
_diffrn_reflns_theta_max         27.635
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14674
_reflns_number_gt                12670
_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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_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)+(0.0284P)²+5.9041P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14674
_refine_ls_number_parameters     763
_refine_ls_number_restraints     787
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.34180(2) 0.28404(2) 0.70163(2) 0.01819(6) Uani 1 1 d . U . . .
F1 F 0.44987(12) 0.32402(12) 0.64428(7) 0.0298(3) Uani 1 1 d . U . . .
O1 O 0.18705(14) 0.23593(14) 0.76646(9) 0.0267(4) Uani 1 1 d . U . . .
N1 N 0.41303(16) 0.20211(15) 0.77199(10) 0.0197(4) Uani 1 1 d . U . . .
B1 B 0.4309(2) 0.26220(19) 0.81823(13) 0.0180(4) Uani 1 1 d . U . . .
C1 C 0.3191(2) 0.20062(19) 0.64041(12) 0.0227(4) Uani 1 1 d . U . . .
F2 F 0.14781(17) 0.04070(16) 0.64798(11) 0.0576(5) Uani 1 1 d . U . . .
Ge2 Ge 0.24972(2) 0.43782(2) 0.76738(2) 0.01552(6) Uani 1 1 d . U . . .
N2 N 0.51793(16) 0.20770(15) 0.85757(10) 0.0224(4) Uani 1 1 d . U . . .
B2 B 0.0907(2) 0.6021(2) 0.77198(13) 0.0204(5) Uani 1 1 d . U . . .
C2 C 0.2375(2) 0.15227(19) 0.66648(13) 0.0261(5) Uani 1 1 d . U . . .
N3 N 0.36008(15) 0.37732(14) 0.82071(9) 0.0175(3) Uani 1 1 d . U . . .
F3 F 0.2725(2) 0.01246(18) 0.52030(12) 0.0665(6) Uani 1 1 d . U . . .
C3 C 0.2238(2) 0.0886(2) 0.62555(16) 0.0377(6) Uani 1 1 d . U . . .
N4 N 0.09529(15) 0.49328(15) 0.80472(10) 0.0198(4) Uani 1 1 d . U . . .
F4 F 0.43058(17) 0.10190(15) 0.47041(8) 0.0515(5) Uani 1 1 d . U . . .
C4 C 0.2877(3) 0.0727(2) 0.55945(16) 0.0423(7) Uani 1 1 d . U . . .
N5 N -0.00365(17) 0.69997(17) 0.76977(11) 0.0282(4) Uani 1 1 d . U . . .
F5 F 0.46220(15) 0.22345(15) 0.54452(8) 0.0439(4) Uani 1 1 d . U . . .
C5 C 0.3665(3) 0.1194(2) 0.53395(14) 0.0364(6) Uani 1 1 d . U . . .
N6 N 0.20917(15) 0.58438(14) 0.74029(10) 0.0200(4) Uani 1 1 d . U . . .
C6 C 0.3819(2) 0.1831(2) 0.57391(13) 0.0291(5) Uani 1 1 d . U . . .
C7 C 0.1710(2) 0.1727(2) 0.73831(14) 0.0292(5) Uani 1 1 d . U . . .
C8 C 0.0892(3) 0.1191(3) 0.7758(2) 0.0580(10) Uani 1 1 d . U . . .
H8A H 0.0266 0.1428 0.7520 0.087 Uiso 1 1 calc R U . . .
H8B H 0.0603 0.1389 0.8235 0.087 Uiso 1 1 calc R U . . .
H8C H 0.1271 0.0406 0.7765 0.087 Uiso 1 1 calc R U . . .
C9 C 0.4289(2) 0.09019(18) 0.78677(13) 0.0240(5) Uani 1 1 d . U . . .
C10 C 0.3660(2) 0.0537(2) 0.84789(14) 0.0326(6) Uani 1 1 d . U . . .
C11 C 0.3844(3) -0.0565(2) 0.86190(18) 0.0459(7) Uani 1 1 d . U . . .
H11 H 0.3421 -0.0815 0.9029 0.055 Uiso 1 1 calc R U . . .
C12 C 0.4624(3) -0.1292(2) 0.8175(2) 0.0542(9) Uani 1 1 d . U . . .
H12 H 0.4744 -0.2039 0.8282 0.065 Uiso 1 1 calc R U . . .
C13 C 0.5228(3) -0.0942(2) 0.75794(19) 0.0470(8) Uani 1 1 d . U . . .
H13 H 0.5760 -0.1452 0.7274 0.056 Uiso 1 1 calc R U . . .
C14 C 0.5083(2) 0.0152(2) 0.74082(15) 0.0319(6) Uani 1 1 d . U . . .
C15 C 0.2776(3) 0.1291(3) 0.89799(14) 0.0398(6) Uani 1 1 d . U . . .
H15A H 0.3021 0.1872 0.9011 0.060 Uiso 1 1 calc R U . . .
H15B H 0.2662 0.0892 0.9438 0.060 Uiso 1 1 calc R U . . .
H15C H 0.2068 0.1600 0.8817 0.060 Uiso 1 1 calc R U . . .
C18 C 0.6552(3) 0.0131(2) 0.8643(2) 0.0530(9) Uani 1 1 d . U . . .
H18A H 0.5888 -0.0077 0.8801 0.080 Uiso 1 1 calc R U . . .
H18B H 0.6834 0.0138 0.9046 0.080 Uiso 1 1 calc R U . . .
H18C H 0.7139 -0.0389 0.8338 0.080 Uiso 1 1 calc R U . . .
C17 C 0.6229(2) 0.1257(2) 0.82471(15) 0.0310(5) Uani 1 1 d . U . . .
H17 H 0.6081 0.1164 0.7805 0.037 Uiso 1 1 calc R U . . .
C16 C 0.5815(2) 0.0468(2) 0.67568(16) 0.0406(7) Uani 1 1 d . U . . .
H16A H 0.5720 0.0222 0.6358 0.061 Uiso 1 1 calc R U . . .
H16B H 0.6605 0.0133 0.6797 0.061 Uiso 1 1 calc R U . . .
H16C H 0.5597 0.1255 0.6691 0.061 Uiso 1 1 calc R U . . .
C19 C 0.7245(2) 0.1622(2) 0.80243(18) 0.0413(7) Uani 1 1 d . U . . .
H19A H 0.7826 0.1162 0.7682 0.062 Uiso 1 1 calc R U . . .
H19B H 0.7550 0.1563 0.8430 0.062 Uiso 1 1 calc R U . . .
H19C H 0.7006 0.2374 0.7819 0.062 Uiso 1 1 calc R U . . .
C20 C 0.5020(2) 0.2319(2) 0.92902(13) 0.0278(5) Uani 1 1 d . U . . .
H20 H 0.4307 0.2963 0.9365 0.033 Uiso 1 1 calc R U . . .
C21 C 0.4820(3) 0.1441(3) 0.98596(17) 0.0510(8) Uani 1 1 d . U . . .
H21A H 0.4295 0.1176 0.9754 0.077 Uiso 1 1 calc R U . . .
H21B H 0.4501 0.1743 1.0307 0.077 Uiso 1 1 calc R U . . .
H21C H 0.5536 0.0842 0.9882 0.077 Uiso 1 1 calc R U . . .
C22 C 0.5919(3) 0.2657(3) 0.94197(16) 0.0409(7) Uani 1 1 d . U . . .
H22A H 0.6621 0.2029 0.9414 0.061 Uiso 1 1 calc R U . . .
H22B H 0.5666 0.2940 0.9873 0.061 Uiso 1 1 calc R U . . .
H22C H 0.6048 0.3217 0.9056 0.061 Uiso 1 1 calc R U . . .
C23 C 0.39800(18) 0.44856(17) 0.84427(12) 0.0189(4) Uani 1 1 d . U . . .
C24 C 0.3475(2) 0.48656(18) 0.90989(12) 0.0235(5) Uani 1 1 d . U . . .
C25 C 0.3937(2) 0.5452(2) 0.93460(14) 0.0319(5) Uani 1 1 d . U . . .
H25 H 0.3618 0.5688 0.9796 0.038 Uiso 1 1 calc R U . . .
C26 C 0.4852(2) 0.5695(2) 0.89433(15) 0.0354(6) Uani 1 1 d . U . . .
H26 H 0.5168 0.6083 0.9120 0.042 Uiso 1 1 calc R U . . .
C27 C 0.5304(2) 0.5371(2) 0.82854(15) 0.0314(5) Uani 1 1 d . U . . .
H27 H 0.5915 0.5563 0.8005 0.038 Uiso 1 1 calc R U . . .
C28 C 0.4881(2) 0.47639(18) 0.80223(12) 0.0233(5) Uani 1 1 d . U . . .
C29 C 0.2450(2) 0.4653(2) 0.95335(14) 0.0349(6) Uani 1 1 d . U . . .
H29A H 0.1791 0.5114 0.9339 0.052 Uiso 1 1 calc R U . . .
H29B H 0.2329 0.4813 1.0009 0.052 Uiso 1 1 calc R U . . .
H29C H 0.2560 0.3893 0.9535 0.052 Uiso 1 1 calc R U . . .
C30 C 0.5390(2) 0.4432(2) 0.73019(13) 0.0311(5) Uani 1 1 d . U . . .
H30A H 0.4867 0.4855 0.6997 0.047 Uiso 1 1 calc R U . . .
H30B H 0.5537 0.3663 0.7308 0.047 Uiso 1 1 calc R U . . .
H30C H 0.6098 0.4562 0.7130 0.047 Uiso 1 1 calc R U . . .
C31 C 0.01312(18) 0.44690(18) 0.81002(12) 0.0217(4) Uani 1 1 d . U . . .
C32 C -0.0275(2) 0.3986(2) 0.87440(13) 0.0282(5) Uani 1 1 d . U . . .
C33 C -0.1155(2) 0.3626(2) 0.88017(17) 0.0426(7) Uani 1 1 d . U . . .
H33 H -0.1452 0.3321 0.9240 0.051 Uiso 1 1 calc R U . . .
C34 C -0.1597(3) 0.3703(3) 0.8246(2) 0.0505(8) Uani 1 1 d . U . . .
H34 H -0.2206 0.3469 0.8299 0.061 Uiso 1 1 calc R U . . .
C35 C -0.1152(3) 0.4123(3) 0.76029(19) 0.0455(7) Uani 1 1 d . U . . .
H35 H -0.1450 0.4159 0.7214 0.055 Uiso 1 1 calc R U . . .
C36 C -0.0275(2) 0.4494(2) 0.75151(14) 0.0301(5) Uani 1 1 d . U . . .
C37 C 0.0225(2) 0.3853(2) 0.93579(14) 0.0350(6) Uani 1 1 d . U . . .
H37A H 0.1040 0.3468 0.9237 0.053 Uiso 1 1 calc R U . . .
H37B H -0.0109 0.3440 0.9747 0.053 Uiso 1 1 calc R U . . .
H37C H 0.0071 0.4565 0.9491 0.053 Uiso 1 1 calc R U . . .
C38 C 0.0210(3) 0.4901(3) 0.68018(15) 0.0388(6) Uani 1 1 d . U . . .
H38A H 0.1002 0.4441 0.6665 0.058 Uiso 1 1 calc R U . . .
H38B H 0.0154 0.5644 0.6803 0.058 Uiso 1 1 calc R U . . .
H38C H -0.0210 0.4883 0.6472 0.058 Uiso 1 1 calc R U . . .
C39 C 0.0027(2) 0.7876(2) 0.71268(17) 0.0398(6) Uani 1 1 d . U . . .
H39 H 0.0776 0.7590 0.6806 0.048 Uiso 1 1 calc R U . . .
C40 C -0.0864(4) 0.8172(3) 0.6699(2) 0.0649(10) Uani 1 1 d . U . . .
H40A H -0.0747 0.8705 0.6310 0.097 Uiso 1 1 calc R U . . .
H40B H -0.1613 0.8479 0.6992 0.097 Uiso 1 1 calc R U . . .
H40C H -0.0805 0.7524 0.6520 0.097 Uiso 1 1 calc R U . . .
C41 C -0.0019(3) 0.8886(2) 0.7379(2) 0.0544(9) Uani 1 1 d . U . . .
H41A H 0.0048 0.9422 0.6982 0.082 Uiso 1 1 calc R U . . .
H41B H 0.0603 0.8700 0.7614 0.082 Uiso 1 1 calc R U . . .
H41C H -0.0737 0.9185 0.7703 0.082 Uiso 1 1 calc R U . . .
C42 C -0.1100(2) 0.7279(3) 0.82192(17) 0.0430(7) Uani 1 1 d . U . . .
H42 H -0.1456 0.8082 0.8141 0.052 Uiso 1 1 calc R U . . .
C43 C -0.1980(2) 0.6862(3) 0.8159(2) 0.0520(8) Uani 1 1 d . U . . .
H43A H -0.2002 0.6917 0.7669 0.078 Uiso 1 1 calc R U . . .
H43B H -0.2720 0.7294 0.8414 0.078 Uiso 1 1 calc R U . . .
H43C H -0.1787 0.6106 0.8354 0.078 Uiso 1 1 calc R U . . .
C44 C -0.0907(3) 0.7064(3) 0.89452(18) 0.0598(9) Uani 1 1 d . U . . .
H44A H -0.0591 0.6283 0.9069 0.090 Uiso 1 1 calc R U . . .
H44B H -0.1624 0.7375 0.9268 0.090 Uiso 1 1 calc R U . . .
H44C H -0.0380 0.7393 0.8972 0.090 Uiso 1 1 calc R U . . .
C45 C 0.2684(2) 0.65481(19) 0.70845(14) 0.0281(5) Uani 1 1 d . U . . .
C46 C 0.2746(2) 0.7275(2) 0.74719(18) 0.0394(7) Uani 1 1 d . U . . .
C47 C 0.3326(3) 0.7967(3) 0.7123(3) 0.0626(10) Uani 1 1 d . U . . .
H47 H 0.3374 0.8467 0.7374 0.075 Uiso 1 1 calc R U . . .
C48 C 0.3819(3) 0.7942(3) 0.6438(3) 0.0777(13) Uani 1 1 d . U . . .
H48 H 0.4214 0.8413 0.6219 0.093 Uiso 1 1 calc R U . . .
C49 C 0.3748(3) 0.7237(3) 0.6062(2) 0.0683(11) Uani 1 1 d . U . . .
H49 H 0.4099 0.7220 0.5584 0.082 Uiso 1 1 calc R U . . .
C50 C 0.3166(2) 0.6539(2) 0.63752(16) 0.0420(7) Uani 1 1 d . U . . .
C51 C 0.2244(3) 0.7324(2) 0.82231(19) 0.0502(8) Uani 1 1 d . U . . .
H51A H 0.2191 0.8000 0.8363 0.075 Uiso 1 1 calc R U . . .
H51B H 0.2718 0.6711 0.8487 0.075 Uiso 1 1 calc R U . . .
H51C H 0.1490 0.7294 0.8317 0.075 Uiso 1 1 calc R U . . .
C52 C 0.3047(3) 0.5815(3) 0.59449(16) 0.0555(9) Uani 1 1 d . U . . .
H52A H 0.3318 0.6009 0.5453 0.083 Uiso 1 1 calc R U . . .
H52B H 0.2253 0.5901 0.6026 0.083 Uiso 1 1 calc R U . . .
H52C H 0.3492 0.5062 0.6075 0.083 Uiso 1 1 calc R U . . .
C59 C 0.1321(4) 0.3877(4) 0.4995(2) 0.0750(12) Uani 1 1 d D U . . .
H59 H 0.0681 0.3987 0.5366 0.090 Uiso 1 1 calc R U . . .
C60 C 0.1539(3) 0.3172(4) 0.45206(19) 0.0707(11) Uani 1 1 d D U . . .
H60 H 0.1060 0.2783 0.4566 0.085 Uiso 1 1 calc R U . . .
C61 C 0.2466(3) 0.3037(4) 0.3976(2) 0.0749(12) Uani 1 1 d D U . . .
H61 H 0.2606 0.2565 0.3642 0.090 Uiso 1 1 calc R U . . .
C62 C 0.3188(4) 0.3572(4) 0.3911(2) 0.0786(12) Uani 1 1 d D U . . .
H62 H 0.3827 0.3463 0.3539 0.094 Uiso 1 1 calc R U . . .
C63 C 0.2972(5) 0.4265(5) 0.4391(3) 0.1027(18) Uani 1 1 d D U . . .
H63 H 0.3466 0.4636 0.4354 0.123 Uiso 1 1 calc R U . . .
C64 C 0.2034(5) 0.4423(5) 0.4928(3) 0.1033(18) Uani 1 1 d D U . . .
H64 H 0.1881 0.4913 0.5254 0.124 Uiso 1 1 calc R U . . .
C65 C -0.0793(7) 0.0775(7) 0.9664(5) 0.0714(10) Uani 0.601(6) 1 d D U P A 1
H65 H -0.1330 0.1318 0.9429 0.086 Uiso 0.601(6) 1 calc R U P A 1
C66 C -0.0329(9) -0.0266(7) 0.9485(5) 0.0714(10) Uani 0.601(6) 1 d D U P A 1
H66 H -0.0569 -0.0451 0.9136 0.086 Uiso 0.601(6) 1 calc R U P A 1
C67 C 0.0466(8) -0.1023(7) 0.9803(4) 0.0714(10) Uani 0.601(6) 1 d . U P A 1
H67 H 0.0807 -0.1732 0.9662 0.086 Uiso 0.601(6) 1 calc R U P A 1
C53 C 0.9278(3) 0.2246(4) 0.5858(3) 0.0803(13) Uani 1 1 d D U . . .
H53 H 0.9841 0.2365 0.6007 0.096 Uiso 1 1 calc R U . . .
C54 C 0.8161(3) 0.2763(4) 0.6126(2) 0.0768(13) Uani 1 1 d D U . . .
H54 H 0.7940 0.3294 0.6437 0.092 Uiso 1 1 calc R U . . .
C55 C 0.7356(3) 0.2520(4) 0.5950(2) 0.0799(14) Uani 1 1 d D U . . .
H55 H 0.6584 0.2872 0.6150 0.096 Uiso 1 1 calc R U . . .
C56 C 0.7648(3) 0.1786(3) 0.5494(2) 0.0641(10) Uani 1 1 d D U . . .
H56 H 0.7086 0.1604 0.5391 0.077 Uiso 1 1 calc R U . . .
C57 C 0.8759(4) 0.1305(5) 0.5182(3) 0.1013(19) Uani 1 1 d D U . . .
H57 H 0.8968 0.0814 0.4848 0.122 Uiso 1 1 calc R U . . .
C58 C 0.9567(4) 0.1548(5) 0.5363(3) 0.1078(18) Uani 1 1 d D U . . .
H58 H 1.0335 0.1228 0.5144 0.129 Uiso 1 1 calc R U . . .
C67A C 0.0133(12) -0.0657(11) 0.9525(7) 0.0714(10) Uani 0.399(6) 1 d . U P A 2
H67A H 0.0243 -0.1076 0.9166 0.086 Uiso 0.399(6) 1 calc R U P A 2
C66A C -0.0861(11) 0.0210(12) 0.9674(7) 0.0714(10) Uani 0.399(6) 1 d . U P A 2
H66A H -0.1476 0.0318 0.9473 0.086 Uiso 0.399(6) 1 calc R U P A 2
C65A C -0.0956(12) 0.0919(10) 1.0116(7) 0.0714(10) Uani 0.399(6) 1 d . U P A 2
H65A H -0.1584 0.1577 1.0168 0.086 Uiso 0.399(6) 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 F1 1.7752(14) . ?
Ge1 N1 1.8430(19) . ?
Ge1 C1 1.971(2) . ?
Ge1 O1 2.3679(17) . ?
Ge1 Ge2 2.4051(3) . ?
O1 C7 1.223(3) . ?
N1 C9 1.428(3) . ?
N1 B1 1.464(3) . ?
B1 N2 1.444(3) . ?
B1 N3 1.472(3) . ?
C1 C6 1.381(3) . ?
C1 C2 1.411(3) . ?
F2 C3 1.339(3) . ?
Ge2 N6 1.8500(18) . ?
Ge2 N4 1.8685(18) . ?
Ge2 N3 1.8712(18) . ?
Ge2 B2 2.382(3) . ?
N2 C17 1.476(3) . ?
N2 C20 1.477(3) . ?
B2 N5 1.422(3) . ?
B2 N6 1.466(3) . ?
B2 N4 1.477(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.490(4) . ?
N3 C23 1.446(3) . ?
F3 C4 1.338(3) . ?
C3 C4 1.377(4) . ?
N4 C31 1.427(3) . ?
F4 C5 1.337(3) . ?
C4 C5 1.362(5) . ?
N5 C42 1.473(3) . ?
N5 C39 1.494(4) . ?
F5 C6 1.331(3) . ?
C5 C6 1.388(4) . ?
N6 C45 1.420(3) . ?
C7 C8 1.494(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.410(4) . ?
C9 C14 1.412(4) . ?
C10 C11 1.398(4) . ?
C10 C15 1.502(4) . ?
C11 C12 1.371(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.365(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.402(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.506(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C18 C17 1.530(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 C19 1.538(4) . ?
C17 H17 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.526(4) . ?
C20 C21 1.534(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C28 1.403(3) . ?
C23 C24 1.405(3) . ?
C24 C25 1.395(3) . ?
C24 C29 1.504(4) . ?
C25 C26 1.384(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.399(3) . ?
C27 H27 0.9500 . ?
C28 C30 1.499(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.403(3) . ?
C31 C36 1.407(3) . ?
C32 C33 1.399(4) . ?
C32 C37 1.499(4) . ?
C33 C34 1.363(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(4) . ?
C35 H35 0.9500 . ?
C36 C38 1.500(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.522(4) . ?
C39 C40 1.524(5) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C44 1.501(5) . ?
C42 C43 1.519(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C50 1.398(4) . ?
C45 C46 1.407(4) . ?
C46 C47 1.408(4) . ?
C46 C51 1.482(5) . ?
C47 C48 1.358(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.371(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.402(4) . ?
C49 H49 0.9500 . ?
C50 C52 1.503(5) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C59 C60 1.376(4) . ?
C59 C64 1.377(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.385(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.376(4) . ?
C61 H61 0.9500 . ?
C62 C63 1.374(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.385(4) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.375(8) . ?
C65 C67 1.396(11) 2_557 ?
C65 H65 0.9500 . ?
C66 C67 1.350(10) . ?
C66 H66 0.9500 . ?
C67 C65 1.396(11) 2_557 ?
C67 H67 0.9500 . ?
C53 C54 1.368(4) . ?
C53 C58 1.381(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.375(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.357(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.374(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.383(4) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C67A C65A 1.359(17) 2_557 ?
C67A C66A 1.381(17) . ?
C67A H67A 0.9500 . ?
C66A C65A 1.380(17) . ?
C66A H66A 0.9500 . ?
C65A C67A 1.359(17) 2_557 ?
C65A H65A 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
F1 Ge1 N1 101.68(8) . . ?
F1 Ge1 C1 99.44(8) . . ?
N1 Ge1 C1 114.81(9) . . ?
F1 Ge1 O1 173.03(7) . . ?
N1 Ge1 O1 84.91(7) . . ?
C1 Ge1 O1 75.49(8) . . ?
F1 Ge1 Ge2 99.07(5) . . ?
N1 Ge1 Ge2 91.61(6) . . ?
C1 Ge1 Ge2 143.58(7) . . ?
O1 Ge1 Ge2 82.87(4) . . ?
C7 O1 Ge1 112.10(16) . . ?
C9 N1 B1 122.98(19) . . ?
C9 N1 Ge1 120.10(14) . . ?
B1 N1 Ge1 115.88(15) . . ?
N2 B1 N1 119.24(19) . . ?
N2 B1 N3 123.08(19) . . ?
N1 B1 N3 117.66(19) . . ?
C6 C1 C2 117.7(2) . . ?
C6 C1 Ge1 123.64(18) . . ?
C2 C1 Ge1 118.57(17) . . ?
N6 Ge2 N4 76.23(8) . . ?
N6 Ge2 N3 116.51(8) . . ?
N4 Ge2 N3 124.00(8) . . ?
N6 Ge2 B2 37.98(8) . . ?
N4 Ge2 B2 38.32(8) . . ?
N3 Ge2 B2 131.49(8) . . ?
N6 Ge2 Ge1 131.61(6) . . ?
N4 Ge2 Ge1 124.45(6) . . ?
N3 Ge2 Ge1 88.89(5) . . ?
B2 Ge2 Ge1 139.62(6) . . ?
B1 N2 C17 118.06(19) . . ?
B1 N2 C20 121.10(19) . . ?
C17 N2 C20 120.84(19) . . ?
N5 B2 N6 127.8(2) . . ?
N5 B2 N4 129.7(2) . . ?
N6 B2 N4 102.51(18) . . ?
N5 B2 Ge2 176.05(19) . . ?
N6 B2 Ge2 50.95(10) . . ?
N4 B2 Ge2 51.67(10) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C7 123.8(2) . . ?
C1 C2 C7 116.6(2) . . ?
C23 N3 B1 119.64(18) . . ?
C23 N3 Ge2 118.57(14) . . ?
B1 N3 Ge2 118.72(14) . . ?
F2 C3 C4 116.8(2) . . ?
F2 C3 C2 122.0(3) . . ?
C4 C3 C2 121.2(3) . . ?
C31 N4 B2 126.21(19) . . ?
C31 N4 Ge2 128.47(15) . . ?
B2 N4 Ge2 90.00(13) . . ?
F3 C4 C5 120.1(3) . . ?
F3 C4 C3 120.5(3) . . ?
C5 C4 C3 119.4(2) . . ?
B2 N5 C42 125.8(2) . . ?
B2 N5 C39 119.8(2) . . ?
C42 N5 C39 114.3(2) . . ?
F4 C5 C4 119.5(2) . . ?
F4 C5 C6 120.1(3) . . ?
C4 C5 C6 120.5(3) . . ?
C45 N6 B2 133.46(19) . . ?
C45 N6 Ge2 135.15(16) . . ?
B2 N6 Ge2 91.07(13) . . ?
F5 C6 C1 122.8(2) . . ?
F5 C6 C5 115.6(2) . . ?
C1 C6 C5 121.6(2) . . ?
O1 C7 C2 116.5(2) . . ?
O1 C7 C8 120.4(3) . . ?
C2 C7 C8 123.1(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 119.6(2) . . ?
C10 C9 N1 120.0(2) . . ?
C14 C9 N1 120.4(2) . . ?
C11 C10 C9 119.0(3) . . ?
C11 C10 C15 118.4(3) . . ?
C9 C10 C15 122.6(2) . . ?
C12 C11 C10 121.2(3) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 121.6(3) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C13 C14 C9 118.6(3) . . ?
C13 C14 C16 118.4(3) . . ?
C9 C14 C16 123.0(2) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
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 . . ?
N2 C17 C18 115.8(2) . . ?
N2 C17 C19 114.1(2) . . ?
C18 C17 C19 110.3(2) . . ?
N2 C17 H17 105.2 . . ?
C18 C17 H17 105.2 . . ?
C19 C17 H17 105.2 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C22 115.6(2) . . ?
N2 C20 C21 114.8(2) . . ?
C22 C20 C21 109.4(2) . . ?
N2 C20 H20 105.3 . . ?
C22 C20 H20 105.3 . . ?
C21 C20 H20 105.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C23 C24 120.2(2) . . ?
C28 C23 N3 119.57(19) . . ?
C24 C23 N3 120.2(2) . . ?
C25 C24 C23 119.0(2) . . ?
C25 C24 C29 119.9(2) . . ?
C23 C24 C29 121.1(2) . . ?
C26 C25 C24 120.9(2) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C27 C26 C25 119.8(2) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 C28 121.2(2) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C27 C28 C23 118.7(2) . . ?
C27 C28 C30 119.7(2) . . ?
C23 C28 C30 121.6(2) . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 119.9(2) . . ?
C32 C31 N4 119.4(2) . . ?
C36 C31 N4 120.7(2) . . ?
C33 C32 C31 118.6(3) . . ?
C33 C32 C37 120.5(2) . . ?
C31 C32 C37 120.8(2) . . ?
C34 C33 C32 121.7(3) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C33 C34 C35 119.6(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C36 121.2(3) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 C38 119.1(3) . . ?
C31 C36 C38 122.1(2) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N5 C39 C41 113.2(3) . . ?
N5 C39 C40 112.7(3) . . ?
C41 C39 C40 110.0(3) . . ?
N5 C39 H39 106.8 . . ?
C41 C39 H39 106.8 . . ?
C40 C39 H39 106.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N5 C42 C44 112.1(3) . . ?
N5 C42 C43 117.4(3) . . ?
C44 C42 C43 111.8(3) . . ?
N5 C42 H42 104.7 . . ?
C44 C42 H42 104.7 . . ?
C43 C42 H42 104.7 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C50 C45 C46 120.5(3) . . ?
C50 C45 N6 119.1(2) . . ?
C46 C45 N6 120.4(2) . . ?
C45 C46 C47 117.6(3) . . ?
C45 C46 C51 122.7(3) . . ?
C47 C46 C51 119.7(3) . . ?
C48 C47 C46 122.1(4) . . ?
C48 C47 H47 119.0 . . ?
C46 C47 H47 119.0 . . ?
C47 C48 C49 119.9(3) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 C50 120.9(4) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
C45 C50 C49 118.9(3) . . ?
C45 C50 C52 121.2(3) . . ?
C49 C50 C52 119.9(3) . . ?
C46 C51 H51A 109.5 . . ?
C46 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C46 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C60 C59 C64 119.7(4) . . ?
C60 C59 H59 120.1 . . ?
C64 C59 H59 120.1 . . ?
C59 C60 C61 119.3(4) . . ?
C59 C60 H60 120.4 . . ?
C61 C60 H60 120.4 . . ?
C62 C61 C60 121.3(4) . . ?
C62 C61 H61 119.3 . . ?
C60 C61 H61 119.3 . . ?
C63 C62 C61 119.0(4) . . ?
C63 C62 H62 120.5 . . ?
C61 C62 H62 120.5 . . ?
C62 C63 C64 120.1(5) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C59 C64 C63 120.6(5) . . ?
C59 C64 H64 119.7 . . ?
C63 C64 H64 119.7 . . ?
C66 C65 C67 119.2(7) . 2_557 ?
C66 C65 H65 120.4 . . ?
C67 C65 H65 120.4 2_557 . ?
C67 C66 C65 120.0(7) . . ?
C67 C66 H66 120.0 . . ?
C65 C66 H66 120.0 . . ?
C66 C67 C65 120.7(7) . 2_557 ?
C66 C67 H67 119.7 . . ?
C65 C67 H67 119.7 2_557 . ?
C54 C53 C58 118.3(4) . . ?
C54 C53 H53 120.8 . . ?
C58 C53 H53 120.8 . . ?
C53 C54 C55 120.4(4) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 H54 119.8 . . ?
C56 C55 C54 120.9(4) . . ?
C56 C55 H55 119.5 . . ?
C54 C55 H55 119.5 . . ?
C55 C56 C57 119.9(4) . . ?
C55 C56 H56 120.1 . . ?
C57 C56 H56 120.1 . . ?
C56 C57 C58 119.0(4) . . ?
C56 C57 H57 120.5 . . ?
C58 C57 H57 120.5 . . ?
C53 C58 C57 121.2(5) . . ?
C53 C58 H58 119.4 . . ?
C57 C58 H58 119.4 . . ?
C65A C67A C66A 121.0(12) 2_557 . ?
C65A C67A H67A 119.5 2_557 . ?
C66A C67A H67A 119.5 . . ?
C67A C66A C65A 119.6(11) . . ?
C67A C66A H66A 120.2 . . ?
C65A C66A H66A 120.2 . . ?
C67A C65A C66A 118.6(11) 2_557 . ?
C67A C65A H65A 120.7 2_557 . ?
C66A C65A H65A 120.7 . . ?

_refine_diff_density_max         0.837
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4

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

data_ld180521ge1
_database_code_depnum_ccdc_archive 'CCDC 1971055'
loop_
_audit_author_name
_audit_author_address
'Ales Ruzicka'
;University of Pardubice
Czech Republic
;
_audit_update_record             
;
2019-12-10 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H69 B2 F3 Ge2 N6 O, 0.5(C6 H6)'
_chemical_formula_sum            'C55 H72 B2 F3 Ge2 N6 O'
_chemical_formula_weight         1056.98

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   17.935(4)
_cell_length_b                   13.777(3)
_cell_length_c                   22.017(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.854(8)
_cell_angle_gamma                90
_cell_volume                     5412(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    89593
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_F_000             2212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.537
_exptl_crystal_size_min          0.414
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4836
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.649
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            89593
_diffrn_reflns_av_unetI/netI     0.1025
_diffrn_reflns_av_R_equivalents  0.1893
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.552
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             12206
_reflns_number_gt                8277
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12206
_refine_ls_number_parameters     611
_refine_ls_number_restraints     570
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2863
_refine_ls_wR_factor_gt          0.2252
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.014
_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 0.73455(3) 0.25654(4) 0.42585(2) 0.01316(18) Uani 1 1 d . U . . .
F1 F 0.6296(2) 0.3057(3) 0.29797(15) 0.0303(8) Uani 1 1 d . U . . .
O1 O 0.6204(2) 0.3722(3) 0.45281(18) 0.0194(8) Uani 1 1 d . U . . .
N1 N 0.7723(2) 0.1318(3) 0.4358(2) 0.0150(9) Uani 1 1 d . U . . .
B1 B 0.8276(3) 0.1526(4) 0.3903(3) 0.0137(10) Uani 1 1 d . U . . .
C1 C 0.6247(3) 0.3045(4) 0.4060(2) 0.0161(10) Uani 1 1 d . U . . .
Ge2 Ge 0.70632(3) 0.37354(4) 0.50677(2) 0.01396(18) Uani 1 1 d . U . . .
F2 F 0.6667(2) 0.4339(3) 0.34845(17) 0.0334(9) Uani 1 1 d . U . . .
N2 N 0.8054(3) 0.2524(3) 0.3706(2) 0.0168(9) Uani 1 1 d . U . . .
B2 B 0.7125(3) 0.4723(4) 0.5961(3) 0.0190(11) Uani 1 1 d . U . . .
C2 C 0.6170(3) 0.3610(4) 0.3468(3) 0.0227(11) Uani 1 1 d . U . . .
N3 N 0.8834(2) 0.0893(3) 0.3737(2) 0.0159(9) Uani 1 1 d . U . . .
F3 F 0.5487(2) 0.4001(3) 0.33358(17) 0.0356(9) Uani 1 1 d . U . . .
C3 C 0.5688(3) 0.2208(4) 0.4085(3) 0.0215(11) Uani 1 1 d . U . . .
N4 N 0.6836(3) 0.3718(3) 0.5871(2) 0.0175(9) Uani 1 1 d . U . . .
C4 C 0.5329(4) 0.2086(6) 0.4608(3) 0.0401(16) Uani 1 1 d . U . . .
H4 H 0.5427 0.2524 0.4940 0.048 Uiso 1 1 calc R U . . .
N5 N 0.7381(3) 0.4942(3) 0.5356(2) 0.0180(9) Uani 1 1 d . U . . .
C5 C 0.4830(5) 0.1336(8) 0.4652(5) 0.063(3) Uani 1 1 d . U . . .
H5 H 0.4596 0.1261 0.5018 0.075 Uiso 1 1 calc R U . . .
N6 N 0.7159(3) 0.5357(4) 0.6464(2) 0.0253(11) Uani 1 1 d . U . . .
C6 C 0.4663(4) 0.0698(6) 0.4185(4) 0.0489(19) Uani 1 1 d . U . . .
H6 H 0.4308 0.0194 0.4221 0.059 Uiso 1 1 calc R U . . .
C7 C 0.5021(4) 0.0793(6) 0.3654(4) 0.0428(17) Uani 1 1 d . U . . .
H7 H 0.4919 0.0347 0.3327 0.051 Uiso 1 1 calc R U . . .
C8 C 0.5534(4) 0.1556(5) 0.3609(3) 0.0365(15) Uani 1 1 d . U . . .
H8 H 0.5778 0.1626 0.3248 0.044 Uiso 1 1 calc R U . . .
C9 C 0.7836(3) 0.0732(4) 0.4893(2) 0.0167(10) Uani 1 1 d . U . . .
C10 C 0.8399(3) 0.0982(4) 0.5369(3) 0.0213(11) Uani 1 1 d . U . . .
C11 C 0.8524(4) 0.0359(5) 0.5875(3) 0.0318(14) Uani 1 1 d . U . . .
H11 H 0.8907 0.0510 0.6191 0.038 Uiso 1 1 calc R U . . .
C12 C 0.8100(4) -0.0466(5) 0.5919(3) 0.0359(15) Uani 1 1 d . U . . .
H12 H 0.8196 -0.0881 0.6263 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7531(4) -0.0698(5) 0.5462(3) 0.0335(14) Uani 1 1 d . U . . .
H13 H 0.7240 -0.1268 0.5495 0.040 Uiso 1 1 calc R U . . .
C15 C 0.8869(3) 0.1884(4) 0.5341(3) 0.0272(13) Uani 1 1 d . U . . .
H15A H 0.9163 0.1844 0.4990 0.041 Uiso 1 1 calc R U . . .
H15B H 0.9209 0.1940 0.5718 0.041 Uiso 1 1 calc R U . . .
H15C H 0.8542 0.2455 0.5298 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7389(3) -0.0091(4) 0.4957(3) 0.0228(11) Uani 1 1 d . U . . .
C16 C 0.6770(4) -0.0339(5) 0.4459(3) 0.0338(15) Uani 1 1 d . U . . .
H16A H 0.6965 -0.0296 0.4060 0.051 Uiso 1 1 calc R U . . .
H16B H 0.6355 0.0119 0.4474 0.051 Uiso 1 1 calc R U . . .
H16C H 0.6592 -0.1000 0.4521 0.051 Uiso 1 1 calc R U . . .
C19 C 0.8646(4) 0.4606(5) 0.2804(3) 0.0287(13) Uani 1 1 d . U . . .
H19 H 0.8875 0.5224 0.2871 0.034 Uiso 1 1 calc R U . . .
C18 C 0.8502(3) 0.4032(4) 0.3305(3) 0.0192(10) Uani 1 1 d . U . . .
C17 C 0.8180(3) 0.3113(4) 0.3194(2) 0.0162(10) Uani 1 1 d . U . . .
C20 C 0.8459(4) 0.4286(5) 0.2215(3) 0.0358(15) Uani 1 1 d . U . . .
H20 H 0.8563 0.4679 0.1879 0.043 Uiso 1 1 calc R U . . .
C21 C 0.8120(4) 0.3392(5) 0.2115(3) 0.0301(13) Uani 1 1 d . U . . .
H21 H 0.7990 0.3179 0.1707 0.036 Uiso 1 1 calc R U . . .
C22 C 0.7964(3) 0.2794(4) 0.2599(3) 0.0206(11) Uani 1 1 d . U . . .
C23 C 0.8684(4) 0.4407(5) 0.3943(3) 0.0314(14) Uani 1 1 d . U . . .
H23A H 0.8978 0.5004 0.3932 0.047 Uiso 1 1 calc R U . . .
H23B H 0.8974 0.3918 0.4189 0.047 Uiso 1 1 calc R U . . .
H23C H 0.8218 0.4543 0.4124 0.047 Uiso 1 1 calc R U . . .
C24 C 0.7579(4) 0.1820(5) 0.2471(3) 0.0294(13) Uani 1 1 d . U . . .
H24A H 0.7399 0.1776 0.2037 0.044 Uiso 1 1 calc R U . . .
H24B H 0.7154 0.1762 0.2715 0.044 Uiso 1 1 calc R U . . .
H24C H 0.7937 0.1295 0.2579 0.044 Uiso 1 1 calc R U . . .
C25 C 0.8759(3) -0.0157(4) 0.3856(3) 0.0201(11) Uani 1 1 d . U . . .
H25 H 0.8244 -0.0254 0.3982 0.024 Uiso 1 1 calc R U . . .
C26 C 0.9311(4) -0.0514(5) 0.4391(3) 0.0309(14) Uani 1 1 d . U . . .
H26A H 0.9821 -0.0512 0.4268 0.046 Uiso 1 1 calc R U . . .
H26B H 0.9176 -0.1176 0.4502 0.046 Uiso 1 1 calc R U . . .
H26C H 0.9286 -0.0084 0.4743 0.046 Uiso 1 1 calc R U . . .
C27 C 0.8807(4) -0.0773(5) 0.3292(3) 0.0342(15) Uani 1 1 d . U . . .
H27A H 0.8421 -0.0564 0.2971 0.051 Uiso 1 1 calc R U . . .
H27B H 0.8726 -0.1456 0.3391 0.051 Uiso 1 1 calc R U . . .
H27C H 0.9303 -0.0696 0.3149 0.051 Uiso 1 1 calc R U . . .
C28 C 0.9556(3) 0.1174(4) 0.3501(3) 0.0247(12) Uani 1 1 d . U . . .
H28 H 0.9903 0.0611 0.3586 0.030 Uiso 1 1 calc R U . . .
C29 C 0.9923(4) 0.2034(6) 0.3853(4) 0.0419(17) Uani 1 1 d . U . . .
H29A H 1.0437 0.2113 0.3748 0.063 Uiso 1 1 calc R U . . .
H29B H 0.9930 0.1915 0.4293 0.063 Uiso 1 1 calc R U . . .
H29C H 0.9636 0.2625 0.3745 0.063 Uiso 1 1 calc R U . . .
C30 C 0.9514(4) 0.1354(6) 0.2817(4) 0.0425(17) Uani 1 1 d . U . . .
H30A H 0.9271 0.0800 0.2599 0.064 Uiso 1 1 calc R U . . .
H30B H 1.0021 0.1436 0.2696 0.064 Uiso 1 1 calc R U . . .
H30C H 0.9221 0.1944 0.2715 0.064 Uiso 1 1 calc R U . . .
C31 C 0.6257(3) 0.3179(4) 0.6116(3) 0.0188(10) Uani 1 1 d . U . . .
C32 C 0.6428(3) 0.2258(4) 0.6380(3) 0.0235(11) Uani 1 1 d . U . . .
C33 C 0.5861(4) 0.1742(5) 0.6621(3) 0.0365(15) Uani 1 1 d . U . . .
H33 H 0.5974 0.1128 0.6804 0.044 Uiso 1 1 calc R U . . .
C34 C 0.5145(4) 0.2095(6) 0.6603(3) 0.0415(16) Uani 1 1 d . U . . .
H34 H 0.4769 0.1737 0.6781 0.050 Uiso 1 1 calc R U . . .
C35 C 0.4977(4) 0.2979(6) 0.6323(3) 0.0390(15) Uani 1 1 d . U . . .
H35 H 0.4477 0.3216 0.6303 0.047 Uiso 1 1 calc R U . . .
C36 C 0.5521(3) 0.3536(5) 0.6068(3) 0.0252(12) Uani 1 1 d . U . . .
C37 C 0.7200(4) 0.1834(5) 0.6392(3) 0.0354(15) Uani 1 1 d . U . . .
H37A H 0.7196 0.1166 0.6545 0.053 Uiso 1 1 calc R U . . .
H37B H 0.7552 0.2224 0.6660 0.053 Uiso 1 1 calc R U . . .
H37C H 0.7355 0.1835 0.5978 0.053 Uiso 1 1 calc R U . . .
C38 C 0.5320(4) 0.4480(6) 0.5758(3) 0.0381(16) Uani 1 1 d . U . . .
H38A H 0.5431 0.4446 0.5332 0.057 Uiso 1 1 calc R U . . .
H38B H 0.5612 0.5004 0.5967 0.057 Uiso 1 1 calc R U . . .
H38C H 0.4784 0.4607 0.5771 0.057 Uiso 1 1 calc R U . . .
C39 C 0.7938(3) 0.5569(4) 0.5165(2) 0.0176(10) Uani 1 1 d . U . . .
C40 C 0.8712(3) 0.5433(4) 0.5375(3) 0.0251(12) Uani 1 1 d . U . . .
C41 C 0.9229(3) 0.6042(5) 0.5161(3) 0.0316(14) Uani 1 1 d . U . . .
H41 H 0.9744 0.5949 0.5297 0.038 Uiso 1 1 calc R U . . .
C42 C 0.9031(4) 0.6786(5) 0.4754(4) 0.0366(16) Uani 1 1 d . U . . .
H42 H 0.9403 0.7199 0.4617 0.044 Uiso 1 1 calc R U . . .
C43 C 0.8288(4) 0.6919(5) 0.4553(3) 0.0299(13) Uani 1 1 d . U . . .
H43 H 0.8150 0.7424 0.4269 0.036 Uiso 1 1 calc R U . . .
C44 C 0.7729(3) 0.6329(4) 0.4756(3) 0.0230(12) Uani 1 1 d . U . . .
C45 C 0.8942(4) 0.4622(5) 0.5823(3) 0.0346(15) Uani 1 1 d . U . . .
H45A H 0.8615 0.4059 0.5733 0.052 Uiso 1 1 calc R U . . .
H45B H 0.8896 0.4846 0.6240 0.052 Uiso 1 1 calc R U . . .
H45C H 0.9463 0.4437 0.5785 0.052 Uiso 1 1 calc R U . . .
C46 C 0.6918(4) 0.6466(5) 0.4526(3) 0.0318(15) Uani 1 1 d . U . . .
H46A H 0.6870 0.7005 0.4234 0.048 Uiso 1 1 calc R U . . .
H46B H 0.6630 0.6611 0.4870 0.048 Uiso 1 1 calc R U . . .
H46C H 0.6725 0.5870 0.4323 0.048 Uiso 1 1 calc R U . . .
C47 C 0.7117(4) 0.5078(5) 0.7107(3) 0.0313(13) Uani 1 1 d . U . . .
H47 H 0.7295 0.5655 0.7356 0.038 Uiso 1 1 calc R U . . .
C48 C 0.6329(5) 0.4868(6) 0.7272(3) 0.0449(18) Uani 1 1 d . U . . .
H48A H 0.5994 0.5399 0.7126 0.067 Uiso 1 1 calc R U . . .
H48B H 0.6338 0.4812 0.7716 0.067 Uiso 1 1 calc R U . . .
H48C H 0.6149 0.4259 0.7080 0.067 Uiso 1 1 calc R U . . .
C49 C 0.7650(5) 0.4259(6) 0.7311(4) 0.049(2) Uani 1 1 d . U . . .
H49A H 0.7461 0.3649 0.7126 0.074 Uiso 1 1 calc R U . . .
H49B H 0.7687 0.4202 0.7757 0.074 Uiso 1 1 calc R U . . .
H49C H 0.8147 0.4398 0.7183 0.074 Uiso 1 1 calc R U . . .
C50 C 0.7274(4) 0.6419(5) 0.6368(3) 0.0338(14) Uani 1 1 d . U . . .
H50 H 0.7271 0.6511 0.5917 0.041 Uiso 1 1 calc R U . . .
C51 C 0.6622(5) 0.7032(6) 0.6562(4) 0.0467(18) Uani 1 1 d . U . . .
H51A H 0.6703 0.7716 0.6464 0.070 Uiso 1 1 calc R U . . .
H51B H 0.6597 0.6963 0.7002 0.070 Uiso 1 1 calc R U . . .
H51C H 0.6151 0.6809 0.6342 0.070 Uiso 1 1 calc R U . . .
C52 C 0.8036(5) 0.6774(6) 0.6649(4) 0.0467(19) Uani 1 1 d . U . . .
H52A H 0.8423 0.6307 0.6561 0.070 Uiso 1 1 calc R U . . .
H52B H 0.8031 0.6836 0.7092 0.070 Uiso 1 1 calc R U . . .
H52C H 0.8145 0.7407 0.6475 0.070 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 N2 1.848(5) . ?
Ge1 N1 1.852(4) . ?
Ge1 C1 2.082(5) . ?
Ge1 B1 2.391(6) . ?
Ge1 Ge2 2.4926(8) . ?
F1 C2 1.356(7) . ?
O1 C1 1.398(7) . ?
O1 Ge2 1.847(3) . ?
N1 C9 1.425(7) . ?
N1 B1 1.507(7) . ?
B1 N3 1.403(7) . ?
B1 N2 1.484(7) . ?
C1 C2 1.513(8) . ?
C1 C3 1.533(8) . ?
Ge2 N5 1.848(4) . ?
Ge2 N4 1.856(5) . ?
Ge2 B2 2.384(6) . ?
F2 C2 1.342(7) . ?
N2 C17 1.426(7) . ?
B2 N6 1.409(8) . ?
B2 N5 1.482(8) . ?
B2 N4 1.484(7) . ?
C2 F3 1.342(6) . ?
N3 C25 1.479(7) . ?
N3 C28 1.495(7) . ?
C3 C4 1.386(10) . ?
C3 C8 1.387(9) . ?
N4 C31 1.427(7) . ?
C4 C5 1.376(11) . ?
C4 H4 0.9500 . ?
N5 C39 1.417(7) . ?
C5 C6 1.363(13) . ?
C5 H5 0.9500 . ?
N6 C47 1.476(8) . ?
N6 C50 1.496(8) . ?
C6 C7 1.396(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.408(10) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.404(8) . ?
C9 C10 1.421(7) . ?
C10 C11 1.406(8) . ?
C10 C15 1.507(9) . ?
C11 C12 1.377(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(9) . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 C16 1.518(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C19 C20 1.378(10) . ?
C19 C18 1.403(8) . ?
C19 H19 0.9500 . ?
C18 C17 1.404(8) . ?
C18 C23 1.500(8) . ?
C17 C22 1.397(8) . ?
C20 C21 1.382(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(9) . ?
C21 H21 0.9500 . ?
C22 C24 1.521(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.514(8) . ?
C25 C26 1.540(8) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.520(10) . ?
C28 C29 1.528(9) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.402(8) . ?
C31 C32 1.416(8) . ?
C32 C33 1.389(9) . ?
C32 C37 1.500(9) . ?
C33 C34 1.371(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.403(10) . ?
C35 H35 0.9500 . ?
C36 C38 1.496(10) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C44 1.407(8) . ?
C39 C40 1.429(8) . ?
C40 C41 1.369(9) . ?
C40 C45 1.520(9) . ?
C41 C42 1.385(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(9) . ?
C42 H42 0.9500 . ?
C43 C44 1.399(9) . ?
C43 H43 0.9500 . ?
C44 C46 1.502(8) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C49 1.516(10) . ?
C47 C48 1.522(11) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C52 1.521(10) . ?
C50 C51 1.537(11) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 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
N2 Ge1 N1 77.4(2) . . ?
N2 Ge1 C1 124.8(2) . . ?
N1 Ge1 C1 130.2(2) . . ?
N2 Ge1 B1 38.37(19) . . ?
N1 Ge1 B1 39.1(2) . . ?
C1 Ge1 B1 143.01(19) . . ?
N2 Ge1 Ge2 133.98(14) . . ?
N1 Ge1 Ge2 127.87(14) . . ?
C1 Ge1 Ge2 71.80(15) . . ?
B1 Ge1 Ge2 145.20(13) . . ?
C1 O1 Ge2 112.1(3) . . ?
C9 N1 B1 127.5(4) . . ?
C9 N1 Ge1 130.0(4) . . ?
B1 N1 Ge1 90.1(3) . . ?
N3 B1 N2 132.6(5) . . ?
N3 B1 N1 126.2(5) . . ?
N2 B1 N1 101.3(4) . . ?
N3 B1 Ge1 175.9(4) . . ?
N2 B1 Ge1 50.6(3) . . ?
N1 B1 Ge1 50.8(2) . . ?
O1 C1 C2 106.5(4) . . ?
O1 C1 C3 113.0(5) . . ?
C2 C1 C3 114.5(4) . . ?
O1 C1 Ge1 100.3(3) . . ?
C2 C1 Ge1 110.2(4) . . ?
C3 C1 Ge1 111.3(4) . . ?
O1 Ge2 N5 115.95(18) . . ?
O1 Ge2 N4 111.30(19) . . ?
N5 Ge2 N4 76.9(2) . . ?
O1 Ge2 B2 120.09(19) . . ?
N5 Ge2 B2 38.4(2) . . ?
N4 Ge2 B2 38.5(2) . . ?
O1 Ge2 Ge1 75.58(12) . . ?
N5 Ge2 Ge1 138.52(16) . . ?
N4 Ge2 Ge1 138.89(14) . . ?
B2 Ge2 Ge1 164.31(15) . . ?
C17 N2 B1 134.4(5) . . ?
C17 N2 Ge1 132.7(3) . . ?
B1 N2 Ge1 91.0(3) . . ?
N6 B2 N5 126.0(5) . . ?
N6 B2 N4 132.1(6) . . ?
N5 B2 N4 102.0(5) . . ?
N6 B2 Ge2 176.4(5) . . ?
N5 B2 Ge2 50.8(3) . . ?
N4 B2 Ge2 51.1(3) . . ?
F3 C2 F2 107.1(5) . . ?
F3 C2 F1 106.0(4) . . ?
F2 C2 F1 106.1(5) . . ?
F3 C2 C1 113.3(5) . . ?
F2 C2 C1 111.1(4) . . ?
F1 C2 C1 112.7(5) . . ?
B1 N3 C25 118.7(4) . . ?
B1 N3 C28 126.6(5) . . ?
C25 N3 C28 114.4(4) . . ?
C4 C3 C8 118.4(6) . . ?
C4 C3 C1 118.9(5) . . ?
C8 C3 C1 122.7(6) . . ?
C31 N4 B2 133.9(5) . . ?
C31 N4 Ge2 127.3(3) . . ?
B2 N4 Ge2 90.4(4) . . ?
C5 C4 C3 120.7(7) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C39 N5 B2 133.2(4) . . ?
C39 N5 Ge2 130.4(4) . . ?
B2 N5 Ge2 90.7(3) . . ?
C6 C5 C4 121.7(9) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
B2 N6 C47 126.2(5) . . ?
B2 N6 C50 119.5(5) . . ?
C47 N6 C50 114.3(5) . . ?
C5 C6 C7 119.1(7) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C8 119.3(7) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C3 C8 C7 120.7(7) . . ?
C3 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C14 C9 C10 119.5(5) . . ?
C14 C9 N1 120.4(5) . . ?
C10 C9 N1 120.1(5) . . ?
C11 C10 C9 118.7(6) . . ?
C11 C10 C15 119.4(5) . . ?
C9 C10 C15 122.0(5) . . ?
C12 C11 C10 121.1(6) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.4(6) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 119.9(6) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 C9 120.4(5) . . ?
C13 C14 C16 120.1(6) . . ?
C9 C14 C16 119.5(5) . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C20 C19 C18 120.9(6) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C18 C17 118.5(5) . . ?
C19 C18 C23 120.2(5) . . ?
C17 C18 C23 121.4(5) . . ?
C22 C17 C18 121.2(5) . . ?
C22 C17 N2 120.6(5) . . ?
C18 C17 N2 118.1(5) . . ?
C19 C20 C21 119.8(6) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C21 C22 121.5(6) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C17 C22 C21 118.1(5) . . ?
C17 C22 C24 121.9(5) . . ?
C21 C22 C24 120.0(5) . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 C27 112.9(5) . . ?
N3 C25 C26 112.7(5) . . ?
C27 C25 C26 111.2(5) . . ?
N3 C25 H25 106.5 . . ?
C27 C25 H25 106.5 . . ?
C26 C25 H25 106.5 . . ?
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 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 C30 115.4(5) . . ?
N3 C28 C29 111.5(5) . . ?
C30 C28 C29 110.6(6) . . ?
N3 C28 H28 106.2 . . ?
C30 C28 H28 106.2 . . ?
C29 C28 H28 106.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 120.6(6) . . ?
C36 C31 N4 120.3(5) . . ?
C32 C31 N4 119.1(5) . . ?
C33 C32 C31 118.6(6) . . ?
C33 C32 C37 120.3(6) . . ?
C31 C32 C37 121.1(6) . . ?
C34 C33 C32 121.9(7) . . ?
C34 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C33 C34 C35 119.0(7) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C36 122.1(7) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 H35 119.0 . . ?
C31 C36 C35 117.8(6) . . ?
C31 C36 C38 121.4(6) . . ?
C35 C36 C38 120.8(6) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C44 C39 N5 119.7(5) . . ?
C44 C39 C40 119.4(5) . . ?
N5 C39 C40 121.0(5) . . ?
C41 C40 C39 118.6(6) . . ?
C41 C40 C45 121.6(6) . . ?
C39 C40 C45 119.8(6) . . ?
C40 C41 C42 122.5(6) . . ?
C40 C41 H41 118.7 . . ?
C42 C41 H41 118.7 . . ?
C43 C42 C41 119.0(6) . . ?
C43 C42 H42 120.5 . . ?
C41 C42 H42 120.5 . . ?
C42 C43 C44 121.5(6) . . ?
C42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
C43 C44 C39 119.0(5) . . ?
C43 C44 C46 121.3(5) . . ?
C39 C44 C46 119.6(5) . . ?
C40 C45 H45A 109.5 . . ?
C40 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C40 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N6 C47 C49 112.7(6) . . ?
N6 C47 C48 114.7(5) . . ?
C49 C47 C48 111.1(7) . . ?
N6 C47 H47 105.8 . . ?
C49 C47 H47 105.8 . . ?
C48 C47 H47 105.8 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N6 C50 C52 112.8(6) . . ?
N6 C50 C51 112.2(6) . . ?
C52 C50 C51 112.8(6) . . ?
N6 C50 H50 106.1 . . ?
C52 C50 H50 106.1 . . ?
C51 C50 H50 106.1 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         1.407
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.236

_shelxl_version_number           2013-4



