# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1860359'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;

_audit_creation_method           'APEX3 v2016.5-0'
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H79 B2 Ge2 N7'
_chemical_formula_sum            'C54 H79 B2 Ge2 N7'
_chemical_formula_weight         993.04

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'
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                   11.2403(6)
_cell_length_b                   18.4973(9)
_cell_length_c                   25.9605(14)
_cell_angle_alpha                90
_cell_angle_beta                 95.945(2)
_cell_angle_gamma                90
_cell_volume                     5368.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    126118
_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    1.229
_exptl_crystal_F_000             2104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6813
_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 0.914
;
_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            124153
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.203
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12364
_reflns_number_gt                10194
_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)+(0.0426P)²+6.8183P] 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         12364
_refine_ls_number_parameters     602
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.61875(2) 0.27690(2) 0.39393(2) 0.01542(7) Uani 1 1 d . . . . .
N1 N 0.59293(18) 0.36104(11) 0.35494(8) 0.0166(4) Uani 1 1 d . . . . .
B1 B 0.4758(2) 0.33290(15) 0.33325(11) 0.0185(5) Uani 1 1 d . . . . .
C1 C 0.6366(2) 0.43067(13) 0.36973(9) 0.0179(5) Uani 1 1 d . . . . .
Ge2 Ge 0.73071(2) 0.24577(2) 0.47341(2) 0.01550(7) Uani 1 1 d . . . . .
N2 N 0.47943(18) 0.25787(11) 0.35186(8) 0.0178(4) Uani 1 1 d . . . . .
B2 B 0.8127(2) 0.23168(15) 0.56075(10) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.5843(2) 0.47164(14) 0.40722(10) 0.0234(5) Uani 1 1 d . . . . .
C3 C 0.6313(3) 0.53930(15) 0.42087(11) 0.0319(6) Uani 1 1 d . . . . .
H3 H 0.5959 0.5674 0.4458 0.038 Uiso 1 1 calc R U . . .
N3 N 0.3773(2) 0.36770(12) 0.30510(9) 0.0276(5) Uani 1 1 d . . . . .
N4 N 0.85873(17) 0.27473(11) 0.51988(7) 0.0165(4) Uani 1 1 d . . . . .
C4 C 0.7288(3) 0.56629(15) 0.39872(12) 0.0349(7) Uani 1 1 d . . . . .
H4 H 0.7595 0.6128 0.4081 0.042 Uiso 1 1 calc R U . . .
N5 N 0.71094(18) 0.19302(11) 0.53294(8) 0.0174(4) Uani 1 1 d . . . . .
C5 C 0.7814(3) 0.52526(15) 0.36285(11) 0.0286(6) Uani 1 1 d . . . . .
H5 H 0.8486 0.5440 0.3478 0.034 Uiso 1 1 calc R U . . .
N6 N 0.85040(18) 0.22894(11) 0.61460(8) 0.0188(4) Uani 1 1 d . . . . .
C6 C 0.7380(2) 0.45701(14) 0.34832(10) 0.0210(5) Uani 1 1 d . . . . .
C7 C 0.4796(3) 0.44293(16) 0.43262(11) 0.0314(6) Uani 1 1 d . . . . .
H7A H 0.4171 0.4269 0.4059 0.047 Uiso 1 1 calc R U . . .
H7B H 0.4479 0.4812 0.4535 0.047 Uiso 1 1 calc R U . . .
H7C H 0.5056 0.4020 0.4550 0.047 Uiso 1 1 calc R U . . .
N7 N 0.74853(18) 0.21563(11) 0.40600(8) 0.0185(4) Uani 1 1 d . . . . .
C8 C 0.8012(2) 0.41107(16) 0.31177(11) 0.0292(6) Uani 1 1 d . . . . .
H8A H 0.7428 0.3922 0.2844 0.044 Uiso 1 1 calc R U . . .
H8B H 0.8412 0.3707 0.3309 0.044 Uiso 1 1 calc R U . . .
H8C H 0.8607 0.4404 0.2963 0.044 Uiso 1 1 calc R U . . .
C9 C 0.4298(2) 0.19163(13) 0.33290(9) 0.0177(5) Uani 1 1 d . . . . .
C11 C 0.3308(2) 0.07932(15) 0.34897(12) 0.0278(6) Uani 1 1 d . . . . .
H11 H 0.2992 0.0467 0.3724 0.033 Uiso 1 1 calc R U . . .
C10 C 0.3807(2) 0.14462(14) 0.36749(10) 0.0211(5) Uani 1 1 d . . . . .
C12 C 0.3268(3) 0.06140(16) 0.29733(13) 0.0336(7) Uani 1 1 d . . . . .
H12 H 0.2898 0.0177 0.2850 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4313(2) 0.17190(15) 0.28053(10) 0.0245(5) Uani 1 1 d . . . . .
C13 C 0.3767(3) 0.10738(16) 0.26358(12) 0.0318(6) Uani 1 1 d . . . . .
H13 H 0.3737 0.0947 0.2280 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3802(3) 0.16436(16) 0.42372(11) 0.0337(7) Uani 1 1 d . . . . .
H15A H 0.3564 0.2151 0.4266 0.051 Uiso 1 1 calc R U . . .
H15B H 0.4606 0.1575 0.4416 0.051 Uiso 1 1 calc R U . . .
H15C H 0.3234 0.1334 0.4396 0.051 Uiso 1 1 calc R U . . .
C18 C 0.3815(3) 0.50401(17) 0.30130(14) 0.0417(8) Uani 1 1 d . . . . .
H18A H 0.3737 0.5431 0.2757 0.063 Uiso 1 1 calc R U . . .
H18B H 0.4565 0.5099 0.3238 0.063 Uiso 1 1 calc R U . . .
H18C H 0.3139 0.5056 0.3223 0.063 Uiso 1 1 calc R U . . .
C17 C 0.3822(4) 0.43319(18) 0.27412(13) 0.0488(9) Uani 1 1 d . . . . .
H17 H 0.3027 0.4329 0.2529 0.059 Uiso 1 1 calc R U . . .
C16 C 0.4925(3) 0.21742(17) 0.24289(11) 0.0318(6) Uani 1 1 d . . . . .
H16A H 0.5191 0.1864 0.2157 0.048 Uiso 1 1 calc R U . . .
H16B H 0.5618 0.2418 0.2613 0.048 Uiso 1 1 calc R U . . .
H16C H 0.4363 0.2537 0.2272 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4648(4) 0.4280(2) 0.23528(18) 0.0659(13) Uani 1 1 d . . . . .
H19A H 0.4532 0.3818 0.2170 0.099 Uiso 1 1 calc R U . . .
H19B H 0.5469 0.4310 0.2519 0.099 Uiso 1 1 calc R U . . .
H19C H 0.4502 0.4678 0.2105 0.099 Uiso 1 1 calc R U . . .
C20 C 0.2543(3) 0.3365(2) 0.30682(17) 0.0544(10) Uani 1 1 d . . . . .
H20 H 0.2679 0.2946 0.3310 0.065 Uiso 1 1 calc R U . . .
C21 C 0.1691(4) 0.3825(3) 0.33166(19) 0.0767(14) Uani 1 1 d . . . . .
H21A H 0.1489 0.4250 0.3100 0.115 Uiso 1 1 calc R U . . .
H21B H 0.2056 0.3981 0.3658 0.115 Uiso 1 1 calc R U . . .
H21C H 0.0962 0.3549 0.3357 0.115 Uiso 1 1 calc R U . . .
C22 C 0.2065(3) 0.3017(2) 0.25597(16) 0.0548(10) Uani 1 1 d . . . . .
H22A H 0.1971 0.3386 0.2288 0.082 Uiso 1 1 calc R U . . .
H22B H 0.1288 0.2793 0.2597 0.082 Uiso 1 1 calc R U . . .
H22C H 0.2627 0.2646 0.2466 0.082 Uiso 1 1 calc R U . . .
C23 C 0.9736(2) 0.29578(14) 0.50787(9) 0.0187(5) Uani 1 1 d . . . . .
C24 C 0.9893(2) 0.36472(15) 0.48738(10) 0.0247(6) Uani 1 1 d . . . . .
C25 C 1.1012(3) 0.38417(18) 0.47348(11) 0.0349(7) Uani 1 1 d . . . . .
H25 H 1.1121 0.4308 0.4593 0.042 Uiso 1 1 calc R U . . .
C26 C 1.1965(3) 0.3370(2) 0.47991(12) 0.0395(8) Uani 1 1 d . . . . .
H26 H 1.2726 0.3514 0.4707 0.047 Uiso 1 1 calc R U . . .
C27 C 1.1810(3) 0.26916(18) 0.49973(11) 0.0322(7) Uani 1 1 d . . . . .
H27 H 1.2473 0.2371 0.5043 0.039 Uiso 1 1 calc R U . . .
C28 C 1.0699(2) 0.24637(15) 0.51323(10) 0.0230(5) Uani 1 1 d . . . . .
C29 C 0.8857(3) 0.41672(16) 0.47970(12) 0.0347(7) Uani 1 1 d . . . . .
H29A H 0.9147 0.4642 0.4699 0.052 Uiso 1 1 calc R U . . .
H29B H 0.8481 0.4210 0.5120 0.052 Uiso 1 1 calc R U . . .
H29C H 0.8269 0.3987 0.4522 0.052 Uiso 1 1 calc R U . . .
C30 C 1.0551(3) 0.17040(16) 0.53125(11) 0.0302(6) Uani 1 1 d . . . . .
H30A H 0.9846 0.1487 0.5118 0.045 Uiso 1 1 calc R U . . .
H30B H 1.0446 0.1705 0.5683 0.045 Uiso 1 1 calc R U . . .
H30C H 1.1264 0.1422 0.5255 0.045 Uiso 1 1 calc R U . . .
C31 C 0.6074(2) 0.15992(14) 0.54941(9) 0.0199(5) Uani 1 1 d . . . . .
C32 C 0.5148(2) 0.20108(16) 0.56639(11) 0.0266(6) Uani 1 1 d . . . . .
C33 C 0.4161(3) 0.16523(19) 0.58302(12) 0.0355(7) Uani 1 1 d . . . . .
H33 H 0.3528 0.1926 0.5949 0.043 Uiso 1 1 calc R U . . .
C34 C 0.4093(3) 0.09075(19) 0.58242(13) 0.0390(8) Uani 1 1 d . . . . .
H34 H 0.3421 0.0672 0.5942 0.047 Uiso 1 1 calc R U . . .
C35 C 0.5000(3) 0.05028(17) 0.56471(12) 0.0336(7) Uani 1 1 d . . . . .
H35 H 0.4941 -0.0010 0.5638 0.040 Uiso 1 1 calc R U . . .
C36 C 0.6002(2) 0.08408(15) 0.54813(10) 0.0242(5) Uani 1 1 d . . . . .
C37 C 0.5190(3) 0.28232(17) 0.56668(13) 0.0360(7) Uani 1 1 d . . . . .
H37A H 0.5106 0.3002 0.5310 0.054 Uiso 1 1 calc R U . . .
H37B H 0.5956 0.2985 0.5844 0.054 Uiso 1 1 calc R U . . .
H37C H 0.4535 0.3012 0.5849 0.054 Uiso 1 1 calc R U . . .
C38 C 0.6997(3) 0.04035(15) 0.52960(12) 0.0305(6) Uani 1 1 d . . . . .
H38A H 0.6774 -0.0109 0.5286 0.046 Uiso 1 1 calc R U . . .
H38B H 0.7726 0.0470 0.5533 0.046 Uiso 1 1 calc R U . . .
H38C H 0.7142 0.0563 0.4948 0.046 Uiso 1 1 calc R U . . .
C39 C 0.9170(3) 0.28690(15) 0.64461(10) 0.0262(6) Uani 1 1 d . . . . .
H39 H 0.9057 0.2777 0.6818 0.031 Uiso 1 1 calc R U . . .
C40 C 1.0516(3) 0.28573(18) 0.64129(11) 0.0362(7) Uani 1 1 d . . . . .
H40A H 1.0684 0.3021 0.6069 0.054 Uiso 1 1 calc R U . . .
H40B H 1.0817 0.2364 0.6471 0.054 Uiso 1 1 calc R U . . .
H40C H 1.0912 0.3180 0.6677 0.054 Uiso 1 1 calc R U . . .
C41 C 0.8655(4) 0.36119(17) 0.63210(13) 0.0462(9) Uani 1 1 d . . . . .
H41A H 0.8791 0.3743 0.5966 0.069 Uiso 1 1 calc R U . . .
H41B H 0.9047 0.3966 0.6563 0.069 Uiso 1 1 calc R U . . .
H41C H 0.7794 0.3608 0.6353 0.069 Uiso 1 1 calc R U . . .
C42 C 0.8075(2) 0.16918(14) 0.64565(9) 0.0212(5) Uani 1 1 d . . . . .
H42 H 0.7658 0.1341 0.6206 0.025 Uiso 1 1 calc R U . . .
C43 C 0.9107(2) 0.12802(15) 0.67581(11) 0.0276(6) Uani 1 1 d . . . . .
H43A H 0.9688 0.1135 0.6521 0.041 Uiso 1 1 calc R U . . .
H43B H 0.8794 0.0849 0.6917 0.041 Uiso 1 1 calc R U . . .
H43C H 0.9499 0.1593 0.7029 0.041 Uiso 1 1 calc R U . . .
C44 C 0.7164(3) 0.19315(19) 0.68148(11) 0.0359(7) Uani 1 1 d . . . . .
H44A H 0.6515 0.2196 0.6615 0.054 Uiso 1 1 calc R U . . .
H44B H 0.7552 0.2247 0.7085 0.054 Uiso 1 1 calc R U . . .
H44C H 0.6836 0.1506 0.6976 0.054 Uiso 1 1 calc R U . . .
C45 C 0.8235(2) 0.16950(13) 0.37705(9) 0.0182(5) Uani 1 1 d . . . . .
C46 C 0.9516(2) 0.19976(15) 0.37960(11) 0.0249(5) Uani 1 1 d . . . . .
H46A H 0.9498 0.2491 0.3648 0.030 Uiso 1 1 calc R U . . .
H46B H 0.9864 0.2027 0.4162 0.030 Uiso 1 1 calc R U . . .
C47 C 1.0294(2) 0.15046(17) 0.34912(12) 0.0315(6) Uani 1 1 d . . . . .
H47 H 1.1126 0.1703 0.3510 0.038 Uiso 1 1 calc R U . . .
C48 C 1.0323(3) 0.07470(17) 0.37256(13) 0.0361(7) Uani 1 1 d . . . . .
H48A H 1.0670 0.0768 0.4092 0.043 Uiso 1 1 calc R U . . .
H48B H 1.0833 0.0428 0.3535 0.043 Uiso 1 1 calc R U . . .
C49 C 0.9055(3) 0.04388(16) 0.36951(13) 0.0339(7) Uani 1 1 d . . . . .
H49 H 0.9078 -0.0059 0.3846 0.041 Uiso 1 1 calc R U . . .
C50 C 0.8519(3) 0.04112(18) 0.31297(13) 0.0411(8) Uani 1 1 d . . . . .
H50A H 0.9006 0.0089 0.2931 0.049 Uiso 1 1 calc R U . . .
H50B H 0.7697 0.0213 0.3109 0.049 Uiso 1 1 calc R U . . .
C51 C 0.8488(3) 0.11680(19) 0.28966(12) 0.0375(7) Uani 1 1 d . . . . .
H51 H 0.8138 0.1146 0.2527 0.045 Uiso 1 1 calc R U . . .
C52 C 0.7713(2) 0.16560(16) 0.32037(10) 0.0269(6) Uani 1 1 d . . . . .
H52A H 0.7676 0.2148 0.3052 0.032 Uiso 1 1 calc R U . . .
H52B H 0.6888 0.1462 0.3182 0.032 Uiso 1 1 calc R U . . .
C53 C 0.8278(2) 0.09295(14) 0.39975(11) 0.0254(6) Uani 1 1 d . . . . .
H53A H 0.8610 0.0947 0.4366 0.031 Uiso 1 1 calc R U . . .
H53B H 0.7457 0.0730 0.3981 0.031 Uiso 1 1 calc R U . . .
C54 C 0.9757(3) 0.1471(2) 0.29251(12) 0.0399(8) Uani 1 1 d . . . . .
H54A H 0.9740 0.1962 0.2772 0.048 Uiso 1 1 calc R U . . .
H54B H 1.0257 0.1159 0.2725 0.048 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(2) . ?
Ge1 N7 1.848(2) . ?
Ge1 N1 1.863(2) . ?
Ge1 B1 2.369(3) . ?
Ge1 Ge2 2.3739(3) . ?
N1 C1 1.417(3) . ?
N1 B1 1.472(3) . ?
B1 N3 1.416(3) . ?
B1 N2 1.469(3) . ?
C1 C6 1.406(3) . ?
C1 C2 1.409(4) . ?
Ge2 N4 1.8583(19) . ?
Ge2 N5 1.860(2) . ?
Ge2 N7 1.867(2) . ?
Ge2 B2 2.372(3) . ?
N2 C9 1.414(3) . ?
B2 N6 1.419(3) . ?
B2 N4 1.463(3) . ?
B2 N5 1.473(3) . ?
C2 C3 1.390(4) . ?
C2 C7 1.504(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
N3 C17 1.458(4) . ?
N3 C20 1.503(4) . ?
N4 C23 1.414(3) . ?
C4 C5 1.381(4) . ?
C4 H4 0.9500 . ?
N5 C31 1.420(3) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
N6 C42 1.478(3) . ?
N6 C39 1.482(3) . ?
C6 C8 1.506(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N7 C45 1.461(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.403(3) . ?
C9 C14 1.409(4) . ?
C11 C12 1.377(4) . ?
C11 C10 1.396(4) . ?
C11 H11 0.9500 . ?
C10 C15 1.506(4) . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C14 C13 1.392(4) . ?
C14 C16 1.509(4) . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C18 C17 1.488(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 C19 1.442(5) . ?
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 C21 1.479(6) . ?
C20 C22 1.516(5) . ?
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 C24 1.400(4) . ?
C23 C28 1.413(4) . ?
C24 C25 1.391(4) . ?
C24 C29 1.508(4) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(4) . ?
C27 H27 0.9500 . ?
C28 C30 1.496(4) . ?
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 1.397(4) . ?
C31 C36 1.405(4) . ?
C32 C33 1.399(4) . ?
C32 C37 1.503(4) . ?
C33 C34 1.380(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(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 1.513(4) . ?
C39 C40 1.525(4) . ?
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 1.519(4) . ?
C42 C43 1.533(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 C52 1.528(3) . ?
C45 C53 1.533(4) . ?
C45 C46 1.540(3) . ?
C46 C47 1.538(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.527(4) . ?
C47 C54 1.531(4) . ?
C47 H47 1.0000 . ?
C48 C49 1.529(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.529(4) . ?
C49 C53 1.532(4) . ?
C49 H49 1.0000 . ?
C50 C51 1.524(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C54 1.527(4) . ?
C51 C52 1.534(4) . ?
C51 H51 1.0000 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 N7 126.09(9) . . ?
N2 Ge1 N1 76.30(9) . . ?
N7 Ge1 N1 132.86(9) . . ?
N2 Ge1 B1 38.31(9) . . ?
N7 Ge1 B1 148.21(9) . . ?
N1 Ge1 B1 38.43(9) . . ?
N2 Ge1 Ge2 143.91(7) . . ?
N7 Ge1 Ge2 50.64(6) . . ?
N1 Ge1 Ge2 135.54(6) . . ?
B1 Ge1 Ge2 161.10(7) . . ?
C1 N1 B1 134.1(2) . . ?
C1 N1 Ge1 125.60(15) . . ?
B1 N1 Ge1 89.73(15) . . ?
N3 B1 N2 126.4(2) . . ?
N3 B1 N1 131.1(2) . . ?
N2 B1 N1 102.4(2) . . ?
N3 B1 Ge1 169.1(2) . . ?
N2 B1 Ge1 51.26(11) . . ?
N1 B1 Ge1 51.84(11) . . ?
C6 C1 C2 120.0(2) . . ?
C6 C1 N1 118.7(2) . . ?
C2 C1 N1 121.2(2) . . ?
N4 Ge2 N5 76.29(9) . . ?
N4 Ge2 N7 122.92(9) . . ?
N5 Ge2 N7 130.97(9) . . ?
N4 Ge2 B2 38.10(9) . . ?
N5 Ge2 B2 38.39(9) . . ?
N7 Ge2 B2 142.61(9) . . ?
N4 Ge2 Ge1 143.08(6) . . ?
N5 Ge2 Ge1 138.69(6) . . ?
N7 Ge2 Ge1 49.94(6) . . ?
B2 Ge2 Ge1 167.45(7) . . ?
C9 N2 B1 135.1(2) . . ?
C9 N2 Ge1 130.61(16) . . ?
B1 N2 Ge1 90.42(15) . . ?
N6 B2 N4 129.9(2) . . ?
N6 B2 N5 127.1(2) . . ?
N4 B2 N5 102.9(2) . . ?
N6 B2 Ge2 173.0(2) . . ?
N4 B2 Ge2 51.59(11) . . ?
N5 B2 Ge2 51.67(11) . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 C7 120.0(3) . . ?
C1 C2 C7 121.0(2) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
B1 N3 C17 126.2(3) . . ?
B1 N3 C20 118.8(2) . . ?
C17 N3 C20 115.0(3) . . ?
C23 N4 B2 135.2(2) . . ?
C23 N4 Ge2 126.84(16) . . ?
B2 N4 Ge2 90.31(14) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C31 N5 B2 132.9(2) . . ?
C31 N5 Ge2 130.43(16) . . ?
B2 N5 Ge2 89.94(15) . . ?
C4 C5 C6 121.2(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
B2 N6 C42 118.9(2) . . ?
B2 N6 C39 125.1(2) . . ?
C42 N6 C39 115.47(19) . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C8 120.5(2) . . ?
C1 C6 C8 120.6(2) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C45 N7 Ge1 139.30(16) . . ?
C45 N7 Ge2 141.28(16) . . ?
Ge1 N7 Ge2 79.42(8) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 120.1(2) . . ?
C10 C9 N2 118.8(2) . . ?
C14 C9 N2 121.1(2) . . ?
C12 C11 C10 121.0(3) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 C15 120.1(2) . . ?
C9 C10 C15 120.8(2) . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C13 C14 C9 118.6(3) . . ?
C13 C14 C16 119.3(3) . . ?
C9 C14 C16 122.1(2) . . ?
C12 C13 C14 121.5(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
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 . . ?
C19 C17 N3 113.2(3) . . ?
C19 C17 C18 115.2(3) . . ?
N3 C17 C18 117.9(3) . . ?
C19 C17 H17 102.6 . . ?
N3 C17 H17 102.6 . . ?
C18 C17 H17 102.6 . . ?
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 . . ?
C21 C20 N3 115.6(3) . . ?
C21 C20 C22 115.9(3) . . ?
N3 C20 C22 112.4(3) . . ?
C21 C20 H20 103.6 . . ?
N3 C20 H20 103.6 . . ?
C22 C20 H20 103.6 . . ?
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 . . ?
C24 C23 C28 120.1(2) . . ?
C24 C23 N4 119.3(2) . . ?
C28 C23 N4 120.5(2) . . ?
C25 C24 C23 119.2(3) . . ?
C25 C24 C29 120.5(3) . . ?
C23 C24 C29 120.3(2) . . ?
C26 C25 C24 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C27 C26 C25 119.8(3) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 C28 121.4(3) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C27 C28 C23 118.4(3) . . ?
C27 C28 C30 119.6(3) . . ?
C23 C28 C30 122.0(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 120.6(2) . . ?
C32 C31 N5 121.4(2) . . ?
C36 C31 N5 118.1(2) . . ?
C31 C32 C33 118.7(3) . . ?
C31 C32 C37 121.5(2) . . ?
C33 C32 C37 119.9(3) . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 120.2(3) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 120.5(3) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 119.1(3) . . ?
C35 C36 C38 120.7(3) . . ?
C31 C36 C38 120.2(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 . . ?
N6 C39 C41 112.5(2) . . ?
N6 C39 C40 114.2(2) . . ?
C41 C39 C40 111.1(3) . . ?
N6 C39 H39 106.1 . . ?
C41 C39 H39 106.1 . . ?
C40 C39 H39 106.1 . . ?
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 . . ?
N6 C42 C44 113.2(2) . . ?
N6 C42 C43 112.2(2) . . ?
C44 C42 C43 110.8(2) . . ?
N6 C42 H42 106.7 . . ?
C44 C42 H42 106.7 . . ?
C43 C42 H42 106.7 . . ?
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 . . ?
N7 C45 C52 109.8(2) . . ?
N7 C45 C53 109.8(2) . . ?
C52 C45 C53 108.7(2) . . ?
N7 C45 C46 110.6(2) . . ?
C52 C45 C46 108.8(2) . . ?
C53 C45 C46 109.1(2) . . ?
C47 C46 C45 110.0(2) . . ?
C47 C46 H46A 109.7 . . ?
C45 C46 H46A 109.7 . . ?
C47 C46 H46B 109.7 . . ?
C45 C46 H46B 109.7 . . ?
H46A C46 H46B 108.2 . . ?
C48 C47 C54 109.6(3) . . ?
C48 C47 C46 109.2(2) . . ?
C54 C47 C46 109.2(2) . . ?
C48 C47 H47 109.6 . . ?
C54 C47 H47 109.6 . . ?
C46 C47 H47 109.6 . . ?
C47 C48 C49 109.9(2) . . ?
C47 C48 H48A 109.7 . . ?
C49 C48 H48A 109.7 . . ?
C47 C48 H48B 109.7 . . ?
C49 C48 H48B 109.7 . . ?
H48A C48 H48B 108.2 . . ?
C50 C49 C48 109.6(3) . . ?
C50 C49 C53 108.8(2) . . ?
C48 C49 C53 109.3(2) . . ?
C50 C49 H49 109.7 . . ?
C48 C49 H49 109.7 . . ?
C53 C49 H49 109.7 . . ?
C51 C50 C49 109.9(2) . . ?
C51 C50 H50A 109.7 . . ?
C49 C50 H50A 109.7 . . ?
C51 C50 H50B 109.7 . . ?
C49 C50 H50B 109.7 . . ?
H50A C50 H50B 108.2 . . ?
C50 C51 C54 109.6(3) . . ?
C50 C51 C52 108.9(3) . . ?
C54 C51 C52 109.7(3) . . ?
C50 C51 H51 109.5 . . ?
C54 C51 H51 109.5 . . ?
C52 C51 H51 109.5 . . ?
C45 C52 C51 110.2(2) . . ?
C45 C52 H52A 109.6 . . ?
C51 C52 H52A 109.6 . . ?
C45 C52 H52B 109.6 . . ?
C51 C52 H52B 109.6 . . ?
H52A C52 H52B 108.1 . . ?
C49 C53 C45 110.3(2) . . ?
C49 C53 H53A 109.6 . . ?
C45 C53 H53A 109.6 . . ?
C49 C53 H53B 109.6 . . ?
C45 C53 H53B 109.6 . . ?
H53A C53 H53B 108.1 . . ?
C51 C54 C47 109.6(2) . . ?
C51 C54 H54A 109.8 . . ?
C47 C54 H54A 109.8 . . ?
C51 C54 H54B 109.8 . . ?
C47 C54 H54B 109.8 . . ?
H54A C54 H54B 108.2 . . ?

_refine_diff_density_max         1.305
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1860360'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;

_audit_creation_method           'APEX3 v2016.5-0'
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H47 B Ge N4 O'
_chemical_formula_sum            'C33 H47 B Ge N4 O'
_chemical_formula_weight         599.14

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   8.3231(19)
_cell_length_b                   18.979(4)
_cell_length_c                   19.558(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3089.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    29344
_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    1.288
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4719
_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 0.633
;
_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            29267
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.146
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7047
_reflns_number_gt                5914
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.999

_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          
;
 Refined as a 2-component perfect inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0496P)²+47.1776P] 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_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_number_reflns         7047
_refine_ls_number_parameters     369
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1063
_refine_ls_wR_factor_ref         0.2857
_refine_ls_wR_factor_gt          0.2785
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.217
_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 0.31701(19) 0.28699(8) 0.68836(7) 0.0217(4) Uani 1 1 d . . . . .
O1 O 0.4137(13) 0.4915(5) 0.6752(5) 0.023(2) Uani 1 1 d . . . . .
N1 N 0.2503(13) 0.3062(6) 0.7748(5) 0.015(2) Uani 1 1 d . U . . .
B1 B 0.2833(15) 0.3707(7) 0.8156(8) 0.014(3) Uani 1 1 d . . . . .
C1 C 0.3935(17) 0.4349(7) 0.7040(7) 0.017(3) Uani 1 1 d . . . . .
N2 N 0.3377(13) 0.4319(5) 0.7713(5) 0.011(2) Uani 1 1 d . U . . .
C2 C 0.1966(18) 0.2400(6) 0.8058(7) 0.022(3) Uani 1 1 d . . . . .
N3 N 0.2725(12) 0.3781(6) 0.8869(5) 0.013(2) Uani 1 1 d . . . . .
C3 C 0.3091(18) 0.1928(6) 0.8317(7) 0.021(3) Uani 1 1 d . . . . .
C4 C 0.255(2) 0.1292(10) 0.8582(8) 0.038(4) Uani 1 1 d . . . . .
H4 H 0.3301 0.0962 0.8758 0.045 Uiso 1 1 calc R U . . .
N4 N 0.4347(13) 0.3693(5) 0.6737(5) 0.014(2) Uani 1 1 d . U . . .
C5 C 0.094(2) 0.1133(9) 0.8593(8) 0.033(4) Uani 1 1 d . . . . .
H5 H 0.0588 0.0709 0.8804 0.039 Uiso 1 1 calc R U . . .
C6 C -0.015(2) 0.1568(8) 0.8309(7) 0.026(3) Uani 1 1 d . . . . .
H6 H -0.1245 0.1429 0.8288 0.032 Uiso 1 1 calc R U . . .
C7 C 0.0314(16) 0.2226(6) 0.8044(7) 0.018(3) Uani 1 1 d . . . . .
C8 C 0.4884(18) 0.2076(10) 0.8295(8) 0.033(4) Uani 1 1 d . . . . .
H8A H 0.5374 0.1804 0.7923 0.049 Uiso 1 1 calc R U . . .
H8B H 0.5372 0.1939 0.8731 0.049 Uiso 1 1 calc R U . . .
H8C H 0.5062 0.2580 0.8216 0.049 Uiso 1 1 calc R U . . .
C9 C -0.0931(18) 0.2729(9) 0.7747(9) 0.033(4) Uani 1 1 d . . . . .
H9A H -0.0563 0.2898 0.7300 0.050 Uiso 1 1 calc R U . . .
H9B H -0.1073 0.3131 0.8056 0.050 Uiso 1 1 calc R U . . .
H9C H -0.1957 0.2482 0.7693 0.050 Uiso 1 1 calc R U . . .
C10 C 0.2935(16) 0.5022(6) 0.7950(5) 0.012(2) Uani 1 1 d . . . . .
C12 C 0.3627(18) 0.6142(7) 0.8428(7) 0.021(3) Uani 1 1 d . . . . .
H12 H 0.4416 0.6463 0.8589 0.026 Uiso 1 1 calc R U . . .
C11 C 0.4110(16) 0.5504(6) 0.8157(7) 0.018(3) Uani 1 1 d . . . . .
C13 C 0.200(2) 0.6326(7) 0.8469(7) 0.025(3) Uani 1 1 d . . . . .
H13 H 0.1686 0.6764 0.8662 0.030 Uiso 1 1 calc R U . . .
C14 C 0.0863(18) 0.5871(7) 0.8229(7) 0.023(3) Uani 1 1 d . . . . .
H14 H -0.0238 0.6002 0.8243 0.028 Uiso 1 1 calc R U . . .
C15 C 0.1296(16) 0.5212(6) 0.7964(6) 0.014(3) Uani 1 1 d . . . . .
C16 C 0.5899(16) 0.5345(7) 0.8077(9) 0.022(3) Uani 1 1 d . . . . .
H16A H 0.6339 0.5627 0.7702 0.033 Uiso 1 1 calc R U . . .
H16B H 0.6045 0.4843 0.7976 0.033 Uiso 1 1 calc R U . . .
H16C H 0.6461 0.5463 0.8502 0.033 Uiso 1 1 calc R U . . .
C17 C 0.0058(19) 0.4711(8) 0.7656(8) 0.024(3) Uani 1 1 d . . . . .
H17A H -0.0931 0.4971 0.7555 0.036 Uiso 1 1 calc R U . . .
H17B H -0.0176 0.4333 0.7983 0.036 Uiso 1 1 calc R U . . .
H17C H 0.0487 0.4507 0.7233 0.036 Uiso 1 1 calc R U . . .
C18 C 0.1433(17) 0.3428(7) 0.9250(7) 0.021(3) Uani 1 1 d . . . . .
H18 H 0.0916 0.3103 0.8913 0.026 Uiso 1 1 calc R U . . .
C19 C 0.0074(19) 0.3923(9) 0.9493(9) 0.031(4) Uani 1 1 d . . . . .
H19A H -0.0156 0.4270 0.9136 0.047 Uiso 1 1 calc R U . . .
H19B H 0.0411 0.4166 0.9911 0.047 Uiso 1 1 calc R U . . .
H19C H -0.0894 0.3645 0.9586 0.047 Uiso 1 1 calc R U . . .
C20 C 0.196(2) 0.2962(9) 0.9833(8) 0.040(4) Uani 1 1 d . . . . .
H20A H 0.2927 0.2700 0.9697 0.060 Uiso 1 1 calc R U . . .
H20B H 0.1102 0.2630 0.9946 0.060 Uiso 1 1 calc R U . . .
H20C H 0.2207 0.3253 1.0233 0.060 Uiso 1 1 calc R U . . .
C21 C 0.3945(16) 0.4203(7) 0.9228(6) 0.012(2) Uani 1 1 d . . . . .
H21 H 0.4474 0.4497 0.8868 0.015 Uiso 1 1 calc R U . . .
C22 C 0.329(2) 0.4727(8) 0.9758(7) 0.027(3) Uani 1 1 d . . . . .
H22A H 0.4177 0.5000 0.9952 0.040 Uiso 1 1 calc R U . . .
H22B H 0.2742 0.4468 1.0124 0.040 Uiso 1 1 calc R U . . .
H22C H 0.2523 0.5046 0.9537 0.040 Uiso 1 1 calc R U . . .
C23 C 0.5267(19) 0.3768(9) 0.9543(9) 0.031(4) Uani 1 1 d . . . . .
H23A H 0.5633 0.3414 0.9212 0.047 Uiso 1 1 calc R U . . .
H23B H 0.4860 0.3531 0.9953 0.047 Uiso 1 1 calc R U . . .
H23C H 0.6167 0.4075 0.9667 0.047 Uiso 1 1 calc R U . . .
C24 C 0.5465(16) 0.3730(7) 0.6139(6) 0.014(3) Uani 1 1 d . . . . .
C25 C 0.5939(18) 0.2965(7) 0.5931(7) 0.023(3) Uani 1 1 d . . . . .
H25A H 0.6416 0.2718 0.6328 0.027 Uiso 1 1 calc R U . . .
H25B H 0.4968 0.2702 0.5788 0.027 Uiso 1 1 calc R U . . .
C26 C 0.7158(16) 0.2979(7) 0.5339(7) 0.021(3) Uani 1 1 d . . . . .
H26 H 0.7440 0.2484 0.5213 0.025 Uiso 1 1 calc R U . . .
C27 C 0.6410(19) 0.3341(8) 0.4720(7) 0.025(3) Uani 1 1 d . . . . .
H27A H 0.7182 0.3341 0.4334 0.030 Uiso 1 1 calc R U . . .
H27B H 0.5435 0.3082 0.4574 0.030 Uiso 1 1 calc R U . . .
C28 C 0.5972(18) 0.4094(8) 0.4908(8) 0.022(3) Uani 1 1 d . . . . .
H28 H 0.5499 0.4338 0.4502 0.026 Uiso 1 1 calc R U . . .
C29 C 0.7498(18) 0.4488(8) 0.5142(7) 0.024(3) Uani 1 1 d . . . . .
H29A H 0.8289 0.4500 0.4764 0.028 Uiso 1 1 calc R U . . .
H29B H 0.7222 0.4980 0.5263 0.028 Uiso 1 1 calc R U . . .
C30 C 0.8224(19) 0.4120(7) 0.5757(7) 0.023(3) Uani 1 1 d . . . . .
H30 H 0.9217 0.4377 0.5901 0.028 Uiso 1 1 calc R U . . .
C31 C 0.7056(16) 0.4099(7) 0.6349(6) 0.018(3) Uani 1 1 d . . . . .
H31A H 0.6822 0.4586 0.6502 0.022 Uiso 1 1 calc R U . . .
H31B H 0.7548 0.3842 0.6737 0.022 Uiso 1 1 calc R U . . .
C32 C 0.4728(18) 0.4084(8) 0.5501(6) 0.020(3) Uani 1 1 d . . . . .
H32A H 0.4403 0.4572 0.5614 0.024 Uiso 1 1 calc R U . . .
H32B H 0.3758 0.3822 0.5356 0.024 Uiso 1 1 calc R U . . .
C33 C 0.8671(18) 0.3359(8) 0.5560(8) 0.026(3) Uani 1 1 d . . . . .
H33A H 0.9462 0.3361 0.5182 0.031 Uiso 1 1 calc R U . . .
H33B H 0.9158 0.3115 0.5957 0.031 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 N1 1.817(11) . ?
Ge1 N4 1.865(11) . ?
O1 C1 1.223(16) . ?
N1 C2 1.464(16) . ?
N1 B1 1.485(17) . ?
B1 N3 1.404(18) . ?
B1 N2 1.519(18) . ?
C1 N2 1.398(16) . ?
C1 N4 1.422(16) . ?
N2 C10 1.459(15) . ?
C2 C3 1.39(2) . ?
C2 C7 1.41(2) . ?
N3 C18 1.470(16) . ?
N3 C21 1.472(16) . ?
C3 C4 1.39(2) . ?
C3 C8 1.52(2) . ?
C4 C5 1.37(3) . ?
C4 H4 0.9500 . ?
N4 C24 1.495(16) . ?
C5 C6 1.35(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.406(19) . ?
C6 H6 0.9500 . ?
C7 C9 1.52(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.399(18) . ?
C10 C15 1.411(19) . ?
C12 C11 1.381(18) . ?
C12 C13 1.40(2) . ?
C12 H12 0.9500 . ?
C11 C16 1.527(18) . ?
C13 C14 1.36(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.401(18) . ?
C14 H14 0.9500 . ?
C15 C17 1.526(19) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.51(2) . ?
C18 C19 1.54(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.51(2) . ?
C21 C22 1.537(18) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C32 1.544(18) . ?
C24 C31 1.554(18) . ?
C24 C25 1.559(18) . ?
C25 C26 1.539(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C33 1.514(19) . ?
C26 C27 1.52(2) . ?
C26 H26 1.0000 . ?
C27 C28 1.52(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.54(2) . ?
C28 C32 1.56(2) . ?
C28 H28 1.0000 . ?
C29 C30 1.52(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.513(18) . ?
C30 C33 1.54(2) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 N4 97.8(5) . . ?
C2 N1 B1 122.8(10) . . ?
C2 N1 Ge1 107.8(8) . . ?
B1 N1 Ge1 127.5(9) . . ?
N3 B1 N1 127.1(12) . . ?
N3 B1 N2 120.5(11) . . ?
N1 B1 N2 112.3(11) . . ?
O1 C1 N2 121.0(12) . . ?
O1 C1 N4 123.0(12) . . ?
N2 C1 N4 115.9(11) . . ?
C1 N2 C10 110.2(9) . . ?
C1 N2 B1 131.8(10) . . ?
C10 N2 B1 116.4(9) . . ?
C3 C2 C7 120.7(12) . . ?
C3 C2 N1 119.9(13) . . ?
C7 C2 N1 119.3(12) . . ?
B1 N3 C18 120.4(10) . . ?
B1 N3 C21 119.0(10) . . ?
C18 N3 C21 120.7(10) . . ?
C4 C3 C2 118.5(15) . . ?
C4 C3 C8 119.4(15) . . ?
C2 C3 C8 122.1(13) . . ?
C5 C4 C3 120.9(18) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C1 N4 C24 115.8(10) . . ?
C1 N4 Ge1 122.9(9) . . ?
C24 N4 Ge1 119.1(8) . . ?
C6 C5 C4 121.0(16) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 120.8(15) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 117.8(13) . . ?
C6 C7 C9 120.7(13) . . ?
C2 C7 C9 121.5(12) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 120.2(11) . . ?
C11 C10 N2 120.9(11) . . ?
C15 C10 N2 118.9(11) . . ?
C11 C12 C13 121.4(13) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C11 C10 118.7(12) . . ?
C12 C11 C16 119.7(12) . . ?
C10 C11 C16 121.5(11) . . ?
C14 C13 C12 119.5(12) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 121.0(13) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C10 118.9(12) . . ?
C14 C15 C17 121.9(12) . . ?
C10 C15 C17 119.1(11) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C20 115.9(13) . . ?
N3 C18 C19 114.6(12) . . ?
C20 C18 C19 109.8(13) . . ?
N3 C18 H18 105.2 . . ?
C20 C18 H18 105.2 . . ?
C19 C18 H18 105.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 C23 113.6(11) . . ?
N3 C21 C22 115.4(11) . . ?
C23 C21 C22 109.8(12) . . ?
N3 C21 H21 105.7 . . ?
C23 C21 H21 105.7 . . ?
C22 C21 H21 105.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C32 113.9(11) . . ?
N4 C24 C31 110.1(9) . . ?
C32 C24 C31 110.8(11) . . ?
N4 C24 C25 108.5(10) . . ?
C32 C24 C25 107.2(10) . . ?
C31 C24 C25 105.9(11) . . ?
C26 C25 C24 110.3(11) . . ?
C26 C25 H25A 109.6 . . ?
C24 C25 H25A 109.6 . . ?
C26 C25 H25B 109.6 . . ?
C24 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
C33 C26 C27 110.7(12) . . ?
C33 C26 C25 110.0(11) . . ?
C27 C26 C25 109.7(12) . . ?
C33 C26 H26 108.8 . . ?
C27 C26 H26 108.8 . . ?
C25 C26 H26 108.8 . . ?
C28 C27 C26 109.2(11) . . ?
C28 C27 H27A 109.8 . . ?
C26 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 C29 109.3(12) . . ?
C27 C28 C32 109.2(12) . . ?
C29 C28 C32 109.4(12) . . ?
C27 C28 H28 109.7 . . ?
C29 C28 H28 109.7 . . ?
C32 C28 H28 109.7 . . ?
C30 C29 C28 109.9(12) . . ?
C30 C29 H29A 109.7 . . ?
C28 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
C28 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C31 C30 C29 111.3(13) . . ?
C31 C30 C33 108.7(11) . . ?
C29 C30 C33 109.3(12) . . ?
C31 C30 H30 109.2 . . ?
C29 C30 H30 109.2 . . ?
C33 C30 H30 109.2 . . ?
C30 C31 C24 110.9(10) . . ?
C30 C31 H31A 109.5 . . ?
C24 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C24 C31 H31B 109.5 . . ?
H31A C31 H31B 108.0 . . ?
C24 C32 C28 110.1(12) . . ?
C24 C32 H32A 109.6 . . ?
C28 C32 H32A 109.6 . . ?
C24 C32 H32B 109.6 . . ?
C28 C32 H32B 109.6 . . ?
H32A C32 H32B 108.2 . . ?
C26 C33 C30 108.5(12) . . ?
C26 C33 H33A 110.0 . . ?
C30 C33 H33A 110.0 . . ?
C26 C33 H33B 110.0 . . ?
C30 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?

_refine_diff_density_max         1.882
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.180

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1860362'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;

_audit_creation_method           'APEX3 v2016.5-0'
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H41 B Ge N4 O'
_chemical_formula_sum            'C27 H41 B Ge N4 O'
_chemical_formula_weight         521.04

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'
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'
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                   12.1642(6)
_cell_length_b                   15.7945(9)
_cell_length_c                   16.2275(8)
_cell_angle_alpha                64.044(2)
_cell_angle_beta                 81.299(3)
_cell_angle_gamma                86.724(3)
_cell_volume                     2770.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    61386
_cell_measurement_theta_min      1
_cell_measurement_theta_max      28

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5618
_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 0.753
;
_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            61386
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.129
_diffrn_reflns_theta_max         27.976
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             12665
_reflns_number_gt                7745
_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)+(0.0529P)²+7.7467P] 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         12665
_refine_ls_number_parameters     635
_refine_ls_number_restraints     564
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0738
_refine_ls_wR_factor_ref         0.1741
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.056
_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 0.45420(4) 0.38015(3) 0.70139(4) 0.03428(15) Uani 1 1 d . U . . .
C1 C 0.4446(3) 0.1830(3) 0.8251(3) 0.0202(8) Uani 1 1 d . U . . .
O1 O 0.4980(2) 0.1123(2) 0.8636(2) 0.0293(7) Uani 1 1 d . U . . .
N1 N 0.3166(3) 0.3440(2) 0.6920(2) 0.0222(7) Uani 1 1 d . U . . .
B1 B 0.2673(4) 0.2512(3) 0.7460(3) 0.0206(9) Uani 1 1 d . U . . .
Ge2 Ge 0.57135(5) 0.86892(4) 0.62613(4) 0.03841(16) Uani 1 1 d D U . . .
C2 C 0.2562(3) 0.4296(3) 0.6475(3) 0.0227(9) Uani 1 1 d . U . . .
O2 O 0.5436(3) 0.5940(3) 0.7944(3) 0.0557(11) Uani 1 1 d D U . . .
N2 N 0.3425(3) 0.1760(2) 0.7977(2) 0.0191(7) Uani 1 1 d . U . . .
B2 B 0.7399(4) 0.7772(3) 0.7508(3) 0.0188(9) Uani 1 1 d . U . . .
N3 N 0.1544(3) 0.2289(2) 0.7472(2) 0.0221(7) Uani 1 1 d . U . . .
C3 C 0.1973(4) 0.4714(3) 0.6998(3) 0.0255(9) Uani 1 1 d . U . . .
N4 N 0.4804(3) 0.2720(2) 0.8058(2) 0.0204(7) Uani 1 1 d . U . . .
C4 C 0.1436(4) 0.5563(3) 0.6545(3) 0.0339(11) Uani 1 1 d . U . . .
H4 H 0.1016 0.5850 0.6896 0.041 Uiso 1 1 calc R U . . .
N7 N 0.8381(3) 0.7809(2) 0.7876(2) 0.0204(7) Uani 1 1 d . U . . .
C7 C 0.2671(4) 0.4746(3) 0.5501(3) 0.0302(10) Uani 1 1 d . U . . .
N6 N 0.6798(3) 0.6886(2) 0.7810(3) 0.0245(8) Uani 1 1 d D U . . .
C6 C 0.2117(4) 0.5592(3) 0.5079(3) 0.0384(12) Uani 1 1 d . U . . .
H6 H 0.2162 0.5895 0.4423 0.046 Uiso 1 1 calc R U . . .
N5 N 0.6964(3) 0.8595(2) 0.6797(2) 0.0253(8) Uani 1 1 d . U . . .
C5 C 0.1507(4) 0.5990(3) 0.5597(4) 0.0404(12) Uani 1 1 d . U . . .
H5 H 0.1131 0.6565 0.5300 0.048 Uiso 1 1 calc R U . . .
N8 N 0.5243(3) 0.7446(2) 0.6936(2) 0.0220(7) Uani 1 1 d D U . . .
C8 C 0.1945(4) 0.4310(3) 0.8029(3) 0.0347(11) Uani 1 1 d . U . . .
H8A H 0.2653 0.4444 0.8168 0.052 Uiso 1 1 calc R U . . .
H8B H 0.1826 0.3627 0.8302 0.052 Uiso 1 1 calc R U . . .
H8C H 0.1337 0.4595 0.8288 0.052 Uiso 1 1 calc R U . . .
C9 C 0.3359(4) 0.4324(4) 0.4929(3) 0.0407(12) Uani 1 1 d . U . . .
H9A H 0.3289 0.4704 0.4274 0.061 Uiso 1 1 calc R U . . .
H9B H 0.3098 0.3681 0.5122 0.061 Uiso 1 1 calc R U . . .
H9C H 0.4141 0.4312 0.5017 0.061 Uiso 1 1 calc R U . . .
C18 C 0.0888(3) 0.1632(3) 0.8346(3) 0.0279(10) Uani 1 1 d . U . . .
H18 H 0.1436 0.1341 0.8792 0.033 Uiso 1 1 calc R U . . .
C14 C 0.2608(4) -0.0776(3) 0.9005(4) 0.0406(12) Uani 1 1 d . U . . .
H14 H 0.2360 -0.1279 0.9590 0.049 Uiso 1 1 calc R U . . .
C10 C 0.3217(3) 0.0820(3) 0.8088(3) 0.0239(9) Uani 1 1 d . U . . .
C11 C 0.3375(4) 0.0671(3) 0.7288(4) 0.0343(10) Uani 1 1 d . U . . .
C13 C 0.2692(5) -0.0915(4) 0.8215(5) 0.0482(13) Uani 1 1 d . U . . .
H13 H 0.2474 -0.1502 0.8257 0.058 Uiso 1 1 calc R U . . .
C15 C 0.2882(4) 0.0095(3) 0.8959(3) 0.0297(10) Uani 1 1 d . U . . .
C16 C 0.3902(5) 0.1405(4) 0.6374(4) 0.0454(13) Uani 1 1 d . U . . .
H16A H 0.3953 0.1165 0.5906 0.068 Uiso 1 1 calc R U . . .
H16B H 0.4649 0.1556 0.6430 0.068 Uiso 1 1 calc R U . . .
H16C H 0.3448 0.1975 0.6189 0.068 Uiso 1 1 calc R U . . .
C17 C 0.2821(4) 0.0206(3) 0.9838(3) 0.0365(11) Uani 1 1 d . U . . .
H17A H 0.2798 0.0877 0.9694 0.055 Uiso 1 1 calc R U . . .
H17B H 0.3478 -0.0078 1.0138 0.055 Uiso 1 1 calc R U . . .
H17C H 0.2148 -0.0109 1.0256 0.055 Uiso 1 1 calc R U . . .
C01C C 0.6261(4) 0.5696(4) 0.9838(4) 0.0464(14) Uani 1 1 d . U . . .
H01A H 0.5800 0.6205 0.9458 0.070 Uiso 1 1 calc R U . . .
H01B H 0.6623 0.5903 1.0220 0.070 Uiso 1 1 calc R U . . .
H01C H 0.5793 0.5142 1.0238 0.070 Uiso 1 1 calc R U . . .
C19 C 0.0029(4) 0.2114(4) 0.8794(4) 0.0404(12) Uani 1 1 d . U . . .
H19A H 0.0370 0.2668 0.8781 0.061 Uiso 1 1 calc R U . . .
H19B H -0.0223 0.1671 0.9437 0.061 Uiso 1 1 calc R U . . .
H19C H -0.0608 0.2309 0.8450 0.061 Uiso 1 1 calc R U . . .
C22 C -0.0006(4) 0.3279(4) 0.6623(4) 0.0463(14) Uani 1 1 d . U . . .
H22A H -0.0146 0.3683 0.5989 0.070 Uiso 1 1 calc R U . . .
H22B H 0.0076 0.3670 0.6942 0.070 Uiso 1 1 calc R U . . .
H22C H -0.0633 0.2840 0.6955 0.070 Uiso 1 1 calc R U . . .
C21 C 0.1055(4) 0.2726(3) 0.6600(3) 0.0295(10) Uani 1 1 d . U . . .
H21 H 0.1619 0.3202 0.6144 0.035 Uiso 1 1 calc R U . . .
C20 C 0.0335(4) 0.0815(4) 0.8312(4) 0.0407(12) Uani 1 1 d . U . . .
H20A H -0.0306 0.1043 0.7975 0.061 Uiso 1 1 calc R U . . .
H20B H 0.0084 0.0345 0.8944 0.061 Uiso 1 1 calc R U . . .
H20C H 0.0868 0.0527 0.7996 0.061 Uiso 1 1 calc R U . . .
C12 C 0.3088(4) -0.0212(4) 0.7376(4) 0.0460(13) Uani 1 1 d . U . . .
H12 H 0.3171 -0.0325 0.6841 0.055 Uiso 1 1 calc R U . . .
C23 C 0.0907(5) 0.2048(4) 0.6178(4) 0.0428(13) Uani 1 1 d . U . . .
H23A H 0.0801 0.2409 0.5528 0.064 Uiso 1 1 calc R U . . .
H23B H 0.0255 0.1643 0.6521 0.064 Uiso 1 1 calc R U . . .
H23C H 0.1570 0.1657 0.6216 0.064 Uiso 1 1 calc R U . . .
C26 C 0.5798(4) 0.3817(3) 0.8394(4) 0.0392(12) Uani 1 1 d . U . . .
H26A H 0.6139 0.4178 0.7751 0.059 Uiso 1 1 calc R U . . .
H26B H 0.6266 0.3865 0.8812 0.059 Uiso 1 1 calc R U . . .
H26C H 0.5060 0.4070 0.8490 0.059 Uiso 1 1 calc R U . . .
C25 C 0.5280(4) 0.2232(4) 0.9625(3) 0.0368(11) Uani 1 1 d . U . . .
H25A H 0.4547 0.2460 0.9778 0.055 Uiso 1 1 calc R U . . .
H25B H 0.5808 0.2321 0.9982 0.055 Uiso 1 1 calc R U . . .
H25C H 0.5226 0.1561 0.9779 0.055 Uiso 1 1 calc R U . . .
C24 C 0.5683(3) 0.2783(3) 0.8592(3) 0.0266(9) Uani 1 1 d . U . . .
C29 C 0.7266(4) 0.9536(3) 0.6626(3) 0.0257(9) Uani 1 1 d . U . . .
C28 C 0.5740(4) 0.6687(3) 0.7627(3) 0.0303(10) Uani 1 1 d D U . . .
C27 C 0.6808(4) 0.2451(4) 0.8301(4) 0.0377(12) Uani 1 1 d . U . . .
H27A H 0.7008 0.2791 0.7629 0.056 Uiso 1 1 calc R U . . .
H27B H 0.6770 0.1774 0.8480 0.056 Uiso 1 1 calc R U . . .
H27C H 0.7373 0.2574 0.8608 0.056 Uiso 1 1 calc R U . . .
C30 C 0.7948(4) 1.0117(3) 0.5804(3) 0.0327(10) Uani 1 1 d . U . . .
C31 C 0.8213(5) 1.1011(3) 0.5682(4) 0.0408(12) Uani 1 1 d . U . . .
H31 H 0.8700 1.1404 0.5148 0.049 Uiso 1 1 calc R U . . .
C32 C 0.7786(5) 1.1336(4) 0.6319(4) 0.0445(12) Uani 1 1 d . U . . .
H32 H 0.7982 1.1950 0.6223 0.053 Uiso 1 1 calc R U . . .
C33 C 0.7078(4) 1.0787(3) 0.7094(4) 0.0392(12) Uani 1 1 d . U . . .
H33 H 0.6775 1.1027 0.7523 0.047 Uiso 1 1 calc R U . . .
C34 C 0.6799(4) 0.9877(3) 0.7255(3) 0.0278(9) Uani 1 1 d . U . . .
C35 C 0.5963(4) 0.9307(4) 0.8084(4) 0.0391(12) Uani 1 1 d . U . . .
H35A H 0.5270 0.9246 0.7874 0.059 Uiso 1 1 calc R U . . .
H35B H 0.5813 0.9626 0.8489 0.059 Uiso 1 1 calc R U . . .
H35C H 0.6262 0.8680 0.8426 0.059 Uiso 1 1 calc R U . . .
C36 C 0.8367(5) 0.9788(4) 0.5070(3) 0.0463(13) Uani 1 1 d . U . . .
H36A H 0.7796 0.9894 0.4670 0.069 Uiso 1 1 calc R U . . .
H36B H 0.8534 0.9115 0.5366 0.069 Uiso 1 1 calc R U . . .
H36C H 0.9043 1.0141 0.4698 0.069 Uiso 1 1 calc R U . . .
C37 C 0.7380(3) 0.6002(3) 0.8266(3) 0.0248(9) Uani 1 1 d . U . . .
C38 C 0.7135(4) 0.5449(3) 0.9218(3) 0.0308(10) Uani 1 1 d . U . . .
C39 C 0.7731(4) 0.4616(3) 0.9607(4) 0.0402(12) Uani 1 1 d . U . . .
H39 H 0.7598 0.4234 1.0256 0.048 Uiso 1 1 calc R U . . .
C40 C 0.8503(4) 0.4342(4) 0.9066(4) 0.0427(12) Uani 1 1 d . U . . .
H40 H 0.8903 0.3776 0.9343 0.051 Uiso 1 1 calc R U . . .
C41 C 0.8703(4) 0.4879(4) 0.8130(4) 0.0381(11) Uani 1 1 d . U . . .
H41 H 0.9238 0.4681 0.7761 0.046 Uiso 1 1 calc R U . . .
C42 C 0.8129(4) 0.5714(3) 0.7711(3) 0.0298(10) Uani 1 1 d . U . . .
C43 C 0.8291(5) 0.6274(4) 0.6676(3) 0.0431(13) Uani 1 1 d . U . . .
H43A H 0.8816 0.5948 0.6394 0.065 Uiso 1 1 calc R U . . .
H43B H 0.8588 0.6900 0.6512 0.065 Uiso 1 1 calc R U . . .
H43C H 0.7576 0.6338 0.6447 0.065 Uiso 1 1 calc R U . . .
C44 C 0.8290(5) 0.8005(4) 0.9353(4) 0.0469(14) Uani 1 1 d . U . . .
H44A H 0.9024 0.8271 0.9290 0.070 Uiso 1 1 calc R U . . .
H44B H 0.8004 0.7653 1.0010 0.070 Uiso 1 1 calc R U . . .
H44C H 0.7779 0.8515 0.9058 0.070 Uiso 1 1 calc R U . . .
C45 C 0.8392(4) 0.7345(3) 0.8884(3) 0.0305(10) Uani 1 1 d . U . . .
H45 H 0.7698 0.6950 0.9143 0.037 Uiso 1 1 calc R U . . .
C46 C 0.9337(5) 0.6651(4) 0.9217(4) 0.0448(13) Uani 1 1 d . U . . .
H46A H 0.9439 0.6265 0.8876 0.067 Uiso 1 1 calc R U . . .
H46B H 0.9152 0.6244 0.9880 0.067 Uiso 1 1 calc R U . . .
H46C H 1.0026 0.7001 0.9108 0.067 Uiso 1 1 calc R U . . .
C48 C 1.0328(4) 0.7749(4) 0.7121(4) 0.0453(13) Uani 1 1 d . U . . .
H48A H 1.0036 0.7197 0.7095 0.068 Uiso 1 1 calc R U . . .
H48B H 1.0752 0.7543 0.7643 0.068 Uiso 1 1 calc R U . . .
H48C H 1.0816 0.8113 0.6544 0.068 Uiso 1 1 calc R U . . .
C49 C 0.9771(4) 0.9128(4) 0.7466(4) 0.0422(13) Uani 1 1 d . U . . .
H49A H 1.0273 0.9559 0.6931 0.063 Uiso 1 1 calc R U . . .
H49B H 1.0170 0.8836 0.8004 0.063 Uiso 1 1 calc R U . . .
H49C H 0.9136 0.9480 0.7603 0.063 Uiso 1 1 calc R U . . .
C50 C 0.4191(3) 0.7173(3) 0.6720(3) 0.0307(10) Uani 1 1 d . U . . .
C51 C 0.3621(4) 0.8040(4) 0.6080(4) 0.0465(14) Uani 1 1 d . U . . .
H51A H 0.4120 0.8366 0.5499 0.070 Uiso 1 1 calc R U . . .
H51B H 0.3438 0.8464 0.6377 0.070 Uiso 1 1 calc R U . . .
H51C H 0.2937 0.7852 0.5952 0.070 Uiso 1 1 calc R U . . .
C52 C 0.4439(4) 0.6514(4) 0.6265(4) 0.0489(14) Uani 1 1 d . U . . .
H52A H 0.3743 0.6335 0.6145 0.073 Uiso 1 1 calc R U . . .
H52B H 0.4801 0.5948 0.6677 0.073 Uiso 1 1 calc R U . . .
H52C H 0.4933 0.6831 0.5680 0.073 Uiso 1 1 calc R U . . .
C53 C 0.3353(4) 0.6715(4) 0.7610(4) 0.0475(14) Uani 1 1 d . U . . .
H53A H 0.2641 0.6615 0.7452 0.071 Uiso 1 1 calc R U . . .
H53B H 0.3246 0.7129 0.7922 0.071 Uiso 1 1 calc R U . . .
H53C H 0.3640 0.6108 0.8024 0.071 Uiso 1 1 calc R U . . .
C47 C 0.9356(4) 0.8368(3) 0.7250(3) 0.0271(9) Uani 1 1 d . U . . .
H47 H 0.9105 0.8709 0.6629 0.033 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 N1 1.848(3) . ?
Ge1 N4 1.860(3) . ?
C1 O1 1.219(5) . ?
C1 N4 1.380(5) . ?
C1 N2 1.407(5) . ?
N1 C2 1.443(5) . ?
N1 B1 1.447(6) . ?
B1 N3 1.431(6) . ?
B1 N2 1.479(6) . ?
Ge2 N5 1.831(3) . ?
Ge2 N8 1.855(3) . ?
C2 C3 1.386(6) . ?
C2 C7 1.409(6) . ?
O2 C28 1.119(5) . ?
N2 C10 1.447(5) . ?
B2 N7 1.428(5) . ?
B2 N5 1.448(6) . ?
B2 N6 1.463(6) . ?
N3 C18 1.479(5) . ?
N3 C21 1.479(5) . ?
C3 C4 1.396(6) . ?
C3 C8 1.501(6) . ?
N4 C24 1.509(5) . ?
C4 C5 1.373(7) . ?
C4 H4 0.9500 . ?
N7 C45 1.474(5) . ?
N7 C47 1.479(5) . ?
C7 C6 1.395(6) . ?
C7 C9 1.500(7) . ?
N6 C28 1.445(5) . ?
N6 C37 1.464(5) . ?
C6 C5 1.369(8) . ?
C6 H6 0.9500 . ?
N5 C29 1.446(5) . ?
C5 H5 0.9500 . ?
N8 C28 1.416(4) . ?
N8 C50 1.509(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C18 C20 1.515(6) . ?
C18 C19 1.537(7) . ?
C18 H18 1.0000 . ?
C14 C13 1.381(8) . ?
C14 C15 1.401(6) . ?
C14 H14 0.9500 . ?
C10 C15 1.392(6) . ?
C10 C11 1.402(6) . ?
C11 C12 1.398(7) . ?
C11 C16 1.499(7) . ?
C13 C12 1.364(8) . ?
C13 H13 0.9500 . ?
C15 C17 1.502(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C01C C38 1.505(7) . ?
C01C H01A 0.9800 . ?
C01C H01B 0.9800 . ?
C01C H01C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 C21 1.522(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 C23 1.533(7) . ?
C21 H21 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C12 H12 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C26 C24 1.530(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 C24 1.527(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C24 C27 1.520(6) . ?
C29 C34 1.388(6) . ?
C29 C30 1.410(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C30 C31 1.388(7) . ?
C30 C36 1.508(7) . ?
C31 C32 1.369(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.370(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.396(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.512(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C42 1.381(6) . ?
C37 C38 1.396(6) . ?
C38 C39 1.400(7) . ?
C39 C40 1.370(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.368(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.504(7) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.527(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.529(7) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C48 C47 1.540(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C47 1.521(6) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C52 1.514(7) . ?
C50 C51 1.516(7) . ?
C50 C53 1.540(7) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C47 H47 1.0000 . ?

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
N1 Ge1 N4 96.82(14) . . ?
O1 C1 N4 122.7(4) . . ?
O1 C1 N2 120.1(4) . . ?
N4 C1 N2 117.2(3) . . ?
C2 N1 B1 125.4(3) . . ?
C2 N1 Ge1 106.3(3) . . ?
B1 N1 Ge1 125.1(3) . . ?
N3 B1 N1 123.8(4) . . ?
N3 B1 N2 120.0(4) . . ?
N1 B1 N2 116.1(4) . . ?
N5 Ge2 N8 97.37(15) . . ?
C3 C2 C7 120.7(4) . . ?
C3 C2 N1 120.0(4) . . ?
C7 C2 N1 119.0(4) . . ?
C1 N2 C10 112.2(3) . . ?
C1 N2 B1 129.7(3) . . ?
C10 N2 B1 117.1(3) . . ?
N7 B2 N5 122.3(4) . . ?
N7 B2 N6 121.5(4) . . ?
N5 B2 N6 116.2(4) . . ?
B1 N3 C18 120.1(3) . . ?
B1 N3 C21 118.8(4) . . ?
C18 N3 C21 121.1(3) . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 C8 122.2(4) . . ?
C4 C3 C8 119.0(4) . . ?
C1 N4 C24 117.1(3) . . ?
C1 N4 Ge1 124.1(3) . . ?
C24 N4 Ge1 117.1(3) . . ?
C5 C4 C3 120.9(5) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
B2 N7 C45 119.8(3) . . ?
B2 N7 C47 119.9(3) . . ?
C45 N7 C47 120.1(3) . . ?
C6 C7 C2 118.5(5) . . ?
C6 C7 C9 120.6(4) . . ?
C2 C7 C9 121.0(4) . . ?
C28 N6 B2 131.6(3) . . ?
C28 N6 C37 109.2(3) . . ?
B2 N6 C37 118.4(3) . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C29 N5 B2 121.4(3) . . ?
C29 N5 Ge2 107.4(3) . . ?
B2 N5 Ge2 128.5(3) . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C28 N8 C50 113.6(3) . . ?
C28 N8 Ge2 129.5(3) . . ?
C50 N8 Ge2 116.9(3) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C18 C20 116.1(4) . . ?
N3 C18 C19 114.2(4) . . ?
C20 C18 C19 109.1(4) . . ?
N3 C18 H18 105.5 . . ?
C20 C18 H18 105.5 . . ?
C19 C18 H18 105.5 . . ?
C13 C14 C15 121.1(5) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C15 C10 C11 121.6(4) . . ?
C15 C10 N2 120.9(4) . . ?
C11 C10 N2 117.4(4) . . ?
C12 C11 C10 117.9(5) . . ?
C12 C11 C16 120.3(5) . . ?
C10 C11 C16 121.7(4) . . ?
C12 C13 C14 120.2(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C10 C15 C14 117.7(5) . . ?
C10 C15 C17 122.9(4) . . ?
C14 C15 C17 119.4(4) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C38 C01C H01A 109.5 . . ?
C38 C01C H01B 109.5 . . ?
H01A C01C H01B 109.5 . . ?
C38 C01C H01C 109.5 . . ?
H01A C01C H01C 109.5 . . ?
H01B C01C H01C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C21 C22 115.8(4) . . ?
N3 C21 C23 114.0(4) . . ?
C22 C21 C23 110.2(4) . . ?
N3 C21 H21 105.2 . . ?
C22 C21 H21 105.2 . . ?
C23 C21 H21 105.2 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
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 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C24 C27 112.0(4) . . ?
N4 C24 C25 108.6(3) . . ?
C27 C24 C25 112.3(4) . . ?
N4 C24 C26 107.8(3) . . ?
C27 C24 C26 108.3(4) . . ?
C25 C24 C26 107.5(4) . . ?
C34 C29 C30 120.9(4) . . ?
C34 C29 N5 118.3(4) . . ?
C30 C29 N5 120.7(4) . . ?
O2 C28 N8 124.0(4) . . ?
O2 C28 N6 119.1(4) . . ?
N8 C28 N6 116.1(3) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C31 C30 C29 117.9(5) . . ?
C31 C30 C36 120.7(5) . . ?
C29 C30 C36 121.4(4) . . ?
C32 C31 C30 121.1(5) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 120.7(5) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C32 C33 C34 120.4(5) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C29 C34 C33 118.8(4) . . ?
C29 C34 C35 121.8(4) . . ?
C33 C34 C35 119.4(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 121.8(4) . . ?
C42 C37 N6 117.5(4) . . ?
C38 C37 N6 120.7(4) . . ?
C37 C38 C39 117.6(5) . . ?
C37 C38 C01C 123.6(4) . . ?
C39 C38 C01C 118.8(5) . . ?
C40 C39 C38 121.0(5) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C41 C40 C39 120.4(5) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C42 120.7(5) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C37 C42 C41 118.5(4) . . ?
C37 C42 C43 120.7(4) . . ?
C41 C42 C43 120.8(5) . . ?
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 . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C45 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N7 C45 C44 115.2(4) . . ?
N7 C45 C46 115.8(4) . . ?
C44 C45 C46 109.9(4) . . ?
N7 C45 H45 104.9 . . ?
C44 C45 H45 104.9 . . ?
C46 C45 H45 104.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
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 . . ?
N8 C50 C52 110.9(4) . . ?
N8 C50 C51 110.5(4) . . ?
C52 C50 C51 108.9(4) . . ?
N8 C50 C53 110.2(4) . . ?
C52 C50 C53 110.5(4) . . ?
C51 C50 C53 105.7(4) . . ?
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 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N7 C47 C49 116.3(4) . . ?
N7 C47 C48 112.8(4) . . ?
C49 C47 C48 110.3(4) . . ?
N7 C47 H47 105.5 . . ?
C49 C47 H47 105.5 . . ?
C48 C47 H47 105.5 . . ?

_refine_diff_density_max         2.594
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.099

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1860361'
_audit_update_record             
;
2018-08-06 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;

_audit_creation_method           'APEX3 v2016.5-0'
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H96 B3 Ge3 N9 S, 0.5(C6 H14)'
_chemical_formula_sum            'C69 H103 B3 Ge3 N9 S'
_chemical_formula_weight         1340.86

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'
S S 0.1246 0.1234 '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                   17.3594(8)
_cell_length_b                   11.7876(5)
_cell_length_c                   36.4890(17)
_cell_angle_alpha                90
_cell_angle_beta                 91.6490(10)
_cell_angle_gamma                90
_cell_volume                     7463.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17247
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             2828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5913
_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 0.793
;

_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            151341
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.089
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17247
_reflns_number_gt                14361
_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-2013 (Sheldrick, 2013)'
_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)+(0.0373P)²+4.2067P] 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         17247
_refine_ls_number_parameters     763
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ge2 Ge 0.14634(2) 0.65324(2) 0.36055(2) 0.01952(5) Uani 1 1 d . . . . .
B2 B 0.03296(12) 0.59438(18) 0.32773(6) 0.0230(4) Uani 1 1 d . . . . .
C2 C 0.40721(12) 0.4979(2) 0.30763(6) 0.0400(5) Uani 1 1 d . . . . .
N2 N 0.42298(8) 0.76195(14) 0.38248(4) 0.0251(3) Uani 1 1 d . . . . .
Ge3 Ge 0.21923(2) 0.66268(2) 0.42084(2) 0.01799(5) Uani 1 1 d . . . . .
B3 B 0.20395(11) 0.69950(17) 0.48428(6) 0.0199(4) Uani 1 1 d . . . . .
C3 C 0.39985(15) 0.4051(3) 0.28411(7) 0.0570(8) Uani 1 1 d . . . . .
H3 H 0.4129 0.4133 0.2591 0.068 Uiso 1 1 calc R U . . .
N3 N 0.54420(9) 0.63686(16) 0.37463(5) 0.0341(4) Uani 1 1 d . . . . .
N5 N 0.04969(8) 0.70449(13) 0.34525(4) 0.0220(3) Uani 1 1 d . . . . .
C5 C 0.35323(14) 0.2897(2) 0.33218(8) 0.0510(6) Uani 1 1 d . . . . .
H5 H 0.3340 0.2189 0.3403 0.061 Uiso 1 1 calc R U . . .
N4 N 0.10307(9) 0.53010(13) 0.33612(4) 0.0238(3) Uani 1 1 d . . . . .
C4 C 0.37407(17) 0.3022(3) 0.29632(8) 0.0639(8) Uani 1 1 d . . . . .
H4 H 0.3706 0.2395 0.2800 0.077 Uiso 1 1 calc R U . . .
N6 N -0.03257(9) 0.55792(15) 0.30703(5) 0.0314(4) Uani 1 1 d . . . . .
C6 C 0.36005(12) 0.37967(19) 0.35660(6) 0.0366(5) Uani 1 1 d . . . . .
N8 N 0.21193(8) 0.58926(12) 0.46578(4) 0.0211(3) Uani 1 1 d . . . . .
C8 C 0.33391(15) 0.3645(2) 0.39533(7) 0.0470(6) Uani 1 1 d . . . . .
H8A H 0.2919 0.4176 0.4000 0.070 Uiso 1 1 calc R U . . .
H8B H 0.3771 0.3793 0.4125 0.070 Uiso 1 1 calc R U . . .
H8C H 0.3157 0.2865 0.3986 0.070 Uiso 1 1 calc R U . . .
N7 N 0.20169(8) 0.77995(12) 0.45348(4) 0.0198(3) Uani 1 1 d . . . . .
C7 C 0.43286(15) 0.6105(2) 0.29312(6) 0.0503(6) Uani 1 1 d . . . . .
H7A H 0.4340 0.6073 0.2663 0.075 Uiso 1 1 calc R U . . .
H7B H 0.4845 0.6280 0.3031 0.075 Uiso 1 1 calc R U . . .
H7C H 0.3968 0.6696 0.3005 0.075 Uiso 1 1 calc R U . . .
N9 N 0.20327(8) 0.72149(13) 0.52220(4) 0.0220(3) Uani 1 1 d . . . . .
C9 C 0.44622(10) 0.87074(17) 0.39534(5) 0.0271(4) Uani 1 1 d . . . . .
C10 C 0.47001(11) 0.88677(19) 0.43192(6) 0.0317(4) Uani 1 1 d . . . . .
C12 C 0.49128(15) 1.0846(2) 0.41951(8) 0.0524(7) Uani 1 1 d . . . . .
H12 H 0.5068 1.1578 0.4278 0.063 Uiso 1 1 calc R U . . .
C11 C 0.49261(13) 0.9948(2) 0.44336(7) 0.0442(6) Uani 1 1 d . . . . .
H11 H 0.5092 1.0064 0.4681 0.053 Uiso 1 1 calc R U . . .
C14 C 0.44536(12) 0.96215(19) 0.37081(6) 0.0362(5) Uani 1 1 d . . . . .
C13 C 0.46748(14) 1.0687(2) 0.38364(7) 0.0474(6) Uani 1 1 d . . . . .
H13 H 0.4661 1.1316 0.3673 0.057 Uiso 1 1 calc R U . . .
C15 C 0.46800(14) 0.7901(2) 0.45870(6) 0.0409(5) Uani 1 1 d . . . . .
H15A H 0.4145 0.7664 0.4619 0.061 Uiso 1 1 calc R U . . .
H15B H 0.4904 0.8146 0.4824 0.061 Uiso 1 1 calc R U . . .
H15C H 0.4978 0.7262 0.4493 0.061 Uiso 1 1 calc R U . . .
C18 C 0.64704(14) 0.7600(3) 0.40380(8) 0.0582(7) Uani 1 1 d . . . . .
H18A H 0.6830 0.6973 0.4086 0.087 Uiso 1 1 calc R U . . .
H18B H 0.6140 0.7698 0.4249 0.087 Uiso 1 1 calc R U . . .
H18C H 0.6761 0.8300 0.3998 0.087 Uiso 1 1 calc R U . . .
C17 C 0.59710(12) 0.7334(2) 0.36968(6) 0.0431(6) Uani 1 1 d . . . . .
H17 H 0.5642 0.8016 0.3648 0.052 Uiso 1 1 calc R U . . .
C16 C 0.42089(16) 0.9457(2) 0.33144(6) 0.0532(7) Uani 1 1 d . . . . .
H16A H 0.4270 1.0171 0.3181 0.080 Uiso 1 1 calc R U . . .
H16B H 0.3667 0.9222 0.3300 0.080 Uiso 1 1 calc R U . . .
H16C H 0.4529 0.8870 0.3205 0.080 Uiso 1 1 calc R U . . .
C19 C 0.64729(16) 0.7180(3) 0.33627(8) 0.0672(8) Uani 1 1 d . . . . .
H19A H 0.6144 0.7023 0.3146 0.101 Uiso 1 1 calc R U . . .
H19B H 0.6827 0.6543 0.3405 0.101 Uiso 1 1 calc R U . . .
H19C H 0.6769 0.7874 0.3323 0.101 Uiso 1 1 calc R U . . .
Ge1 Ge 0.32940(2) 0.68588(2) 0.37956(2) 0.02020(5) Uani 1 1 d . . . . .
B1 B 0.46364(12) 0.6554(2) 0.37511(6) 0.0274(5) Uani 1 1 d . . . . .
C1 C 0.38981(11) 0.48261(18) 0.34473(5) 0.0301(4) Uani 1 1 d . . . . .
N1 N 0.40076(9) 0.57298(14) 0.37000(4) 0.0258(3) Uani 1 1 d . . . . .
S1 S 0.24812(3) 0.72995(4) 0.33293(2) 0.02678(10) Uani 1 1 d . . . . .
C20 C 0.58213(13) 0.5258(2) 0.38135(7) 0.0446(6) Uani 1 1 d . . . . .
H20 H 0.6372 0.5428 0.3881 0.054 Uiso 1 1 calc R U . . .
C21 C 0.54884(15) 0.4664(2) 0.41427(8) 0.0584(7) Uani 1 1 d . . . . .
H21A H 0.4942 0.4501 0.4093 0.088 Uiso 1 1 calc R U . . .
H21B H 0.5542 0.5155 0.4359 0.088 Uiso 1 1 calc R U . . .
H21C H 0.5767 0.3952 0.4189 0.088 Uiso 1 1 calc R U . . .
C23 C 0.13246(11) 0.42601(16) 0.32295(5) 0.0262(4) Uani 1 1 d . . . . .
C22 C 0.58349(17) 0.4474(3) 0.34816(9) 0.0697(9) Uani 1 1 d . . . . .
H22A H 0.6001 0.4901 0.3267 0.105 Uiso 1 1 calc R U . . .
H22B H 0.5317 0.4167 0.3433 0.105 Uiso 1 1 calc R U . . .
H22C H 0.6195 0.3849 0.3531 0.105 Uiso 1 1 calc R U . . .
C26 C 0.17654(15) 0.2153(2) 0.29720(7) 0.0486(6) Uani 1 1 d . . . . .
H26 H 0.1906 0.1429 0.2881 0.058 Uiso 1 1 calc R U . . .
C25 C 0.18377(14) 0.3101(2) 0.27552(7) 0.0441(6) Uani 1 1 d . . . . .
H25 H 0.2034 0.3023 0.2516 0.053 Uiso 1 1 calc R U . . .
C24 C 0.16284(12) 0.41748(19) 0.28793(6) 0.0334(5) Uani 1 1 d . . . . .
C27 C 0.14900(14) 0.22505(19) 0.33194(7) 0.0439(6) Uani 1 1 d . . . . .
H27 H 0.1451 0.1595 0.3469 0.053 Uiso 1 1 calc R U . . .
C28 C 0.12677(12) 0.33018(17) 0.34538(6) 0.0326(5) Uani 1 1 d . . . . .
C29 C 0.17190(15) 0.5198(2) 0.26405(6) 0.0451(6) Uani 1 1 d . . . . .
H29A H 0.1865 0.4958 0.2395 0.068 Uiso 1 1 calc R U . . .
H29B H 0.2121 0.5692 0.2747 0.068 Uiso 1 1 calc R U . . .
H29C H 0.1230 0.5614 0.2624 0.068 Uiso 1 1 calc R U . . .
C30 C 0.09469(16) 0.3401(2) 0.38313(6) 0.0460(6) Uani 1 1 d . . . . .
H30A H 0.0505 0.3918 0.3824 0.069 Uiso 1 1 calc R U . . .
H30B H 0.1345 0.3697 0.4001 0.069 Uiso 1 1 calc R U . . .
H30C H 0.0781 0.2651 0.3915 0.069 Uiso 1 1 calc R U . . .
C31 C 0.00230(11) 0.79227(16) 0.35863(5) 0.0248(4) Uani 1 1 d . . . . .
C32 C 0.01544(12) 0.90392(17) 0.34726(5) 0.0314(4) Uani 1 1 d . . . . .
C33 C -0.03424(15) 0.9888(2) 0.35847(6) 0.0462(6) Uani 1 1 d . . . . .
H33 H -0.0264 1.0646 0.3506 0.055 Uiso 1 1 calc R U . . .
C34 C -0.09435(16) 0.9648(2) 0.38070(7) 0.0534(7) Uani 1 1 d . . . . .
H34 H -0.1286 1.0235 0.3876 0.064 Uiso 1 1 calc R U . . .
C35 C -0.10527(14) 0.8559(2) 0.39311(7) 0.0492(6) Uani 1 1 d . . . . .
H35 H -0.1465 0.8404 0.4090 0.059 Uiso 1 1 calc R U . . .
C36 C -0.05674(12) 0.76778(19) 0.38277(6) 0.0344(5) Uani 1 1 d . . . . .
C37 C 0.08195(14) 0.93155(19) 0.32346(6) 0.0415(5) Uani 1 1 d . . . . .
H37A H 0.0886 0.8706 0.3056 0.062 Uiso 1 1 calc R U . . .
H37B H 0.1290 0.9391 0.3387 0.062 Uiso 1 1 calc R U . . .
H37C H 0.0717 1.0031 0.3105 0.062 Uiso 1 1 calc R U . . .
C38 C -0.06923(15) 0.6493(2) 0.39677(7) 0.0464(6) Uani 1 1 d . . . . .
H38A H -0.0939 0.6033 0.3774 0.070 Uiso 1 1 calc R U . . .
H38B H -0.1024 0.6519 0.4180 0.070 Uiso 1 1 calc R U . . .
H38C H -0.0195 0.6156 0.4040 0.070 Uiso 1 1 calc R U . . .
C39 C -0.04790(14) 0.4334(2) 0.30329(7) 0.0473(6) Uani 1 1 d . . . . .
H39 H -0.0095 0.3946 0.3199 0.057 Uiso 1 1 calc R U . . .
C40 C -0.12637(17) 0.4000(3) 0.31656(9) 0.0665(8) Uani 1 1 d . . . . .
H40A H -0.1664 0.4325 0.3002 0.100 Uiso 1 1 calc R U . . .
H40B H -0.1327 0.4288 0.3415 0.100 Uiso 1 1 calc R U . . .
H40C H -0.1310 0.3172 0.3165 0.100 Uiso 1 1 calc R U . . .
C41 C -0.03367(16) 0.3889(2) 0.26489(8) 0.0609(8) Uani 1 1 d . . . . .
H41A H -0.0727 0.4198 0.2477 0.091 Uiso 1 1 calc R U . . .
H41B H -0.0369 0.3059 0.2649 0.091 Uiso 1 1 calc R U . . .
H41C H 0.0177 0.4123 0.2574 0.091 Uiso 1 1 calc R U . . .
C42 C -0.08359(12) 0.6305(2) 0.28443(6) 0.0409(5) Uani 1 1 d . . . . .
H42 H -0.1099 0.5780 0.2666 0.049 Uiso 1 1 calc R U . . .
C43 C -0.14787(14) 0.6890(3) 0.30413(8) 0.0546(7) Uani 1 1 d . . . . .
H43A H -0.1855 0.7191 0.2861 0.082 Uiso 1 1 calc R U . . .
H43B H -0.1266 0.7513 0.3190 0.082 Uiso 1 1 calc R U . . .
H43C H -0.1732 0.6344 0.3201 0.082 Uiso 1 1 calc R U . . .
C44 C -0.03876(16) 0.7108(2) 0.26152(8) 0.0581(7) Uani 1 1 d . . . . .
H44A H 0.0002 0.6686 0.2482 0.087 Uiso 1 1 calc R U . . .
H44B H -0.0134 0.7674 0.2774 0.087 Uiso 1 1 calc R U . . .
H44C H -0.0738 0.7490 0.2440 0.087 Uiso 1 1 calc R U . . .
C45 C 0.15821(10) 0.88044(15) 0.44775(5) 0.0206(4) Uani 1 1 d . . . . .
C46 C 0.08017(11) 0.88409(17) 0.45708(5) 0.0251(4) Uani 1 1 d . . . . .
C47 C 0.04083(12) 0.98634(18) 0.45379(6) 0.0338(5) Uani 1 1 d . . . . .
H47 H -0.0115 0.9902 0.4606 0.041 Uiso 1 1 calc R U . . .
C48 C 0.07628(13) 1.08203(18) 0.44089(6) 0.0391(5) Uani 1 1 d . . . . .
H48 H 0.0488 1.1516 0.4392 0.047 Uiso 1 1 calc R U . . .
C49 C 0.15194(13) 1.07669(17) 0.43033(6) 0.0351(5) Uani 1 1 d . . . . .
H49 H 0.1758 1.1426 0.4209 0.042 Uiso 1 1 calc R U . . .
C50 C 0.19362(11) 0.97662(16) 0.43328(5) 0.0254(4) Uani 1 1 d . . . . .
C51 C 0.03896(11) 0.78184(19) 0.47106(6) 0.0341(5) Uani 1 1 d . . . . .
H51A H -0.0168 0.7939 0.4687 0.051 Uiso 1 1 calc R U . . .
H51B H 0.0535 0.7697 0.4969 0.051 Uiso 1 1 calc R U . . .
H51C H 0.0533 0.7151 0.4567 0.051 Uiso 1 1 calc R U . . .
C52 C 0.27552(12) 0.97253(19) 0.42116(7) 0.0403(5) Uani 1 1 d . . . . .
H52A H 0.2775 0.9338 0.3974 0.060 Uiso 1 1 calc R U . . .
H52B H 0.3072 0.9311 0.4394 0.060 Uiso 1 1 calc R U . . .
H52C H 0.2953 1.0500 0.4188 0.060 Uiso 1 1 calc R U . . .
C53 C 0.23129(11) 0.47834(15) 0.47826(5) 0.0223(4) Uani 1 1 d . . . . .
C54 C 0.17219(12) 0.39962(16) 0.48356(5) 0.0282(4) Uani 1 1 d . . . . .
C55 C 0.19184(15) 0.29089(19) 0.49575(6) 0.0418(5) Uani 1 1 d . . . . .
H55 H 0.1522 0.2371 0.4998 0.050 Uiso 1 1 calc R U . . .
C56 C 0.26753(16) 0.2602(2) 0.50204(7) 0.0486(6) Uani 1 1 d . . . . .
H56 H 0.2800 0.1855 0.5099 0.058 Uiso 1 1 calc R U . . .
C57 C 0.32511(14) 0.33848(19) 0.49684(6) 0.0419(5) Uani 1 1 d . . . . .
H57 H 0.3773 0.3169 0.5013 0.050 Uiso 1 1 calc R U . . .
C58 C 0.30847(11) 0.44838(17) 0.48521(5) 0.0280(4) Uani 1 1 d . . . . .
C59 C 0.08908(12) 0.4311(2) 0.47717(6) 0.0382(5) Uani 1 1 d . . . . .
H59A H 0.0835 0.4751 0.4545 0.057 Uiso 1 1 calc R U . . .
H59B H 0.0716 0.4767 0.4978 0.057 Uiso 1 1 calc R U . . .
H59C H 0.0579 0.3620 0.4751 0.057 Uiso 1 1 calc R U . . .
C60 C 0.37207(12) 0.53319(19) 0.48030(6) 0.0365(5) Uani 1 1 d . . . . .
H60A H 0.3733 0.5560 0.4545 0.055 Uiso 1 1 calc R U . . .
H60B H 0.4215 0.4989 0.4877 0.055 Uiso 1 1 calc R U . . .
H60C H 0.3628 0.6000 0.4955 0.055 Uiso 1 1 calc R U . . .
C61 C 0.23469(11) 0.82513(17) 0.53993(5) 0.0288(4) Uani 1 1 d . . . . .
H61 H 0.2402 0.8079 0.5667 0.035 Uiso 1 1 calc R U . . .
C62 C 0.18319(14) 0.92906(19) 0.53654(6) 0.0419(5) Uani 1 1 d . . . . .
H62A H 0.1830 0.9570 0.5112 0.063 Uiso 1 1 calc R U . . .
H62B H 0.2028 0.9885 0.5531 0.063 Uiso 1 1 calc R U . . .
H62C H 0.1306 0.9088 0.5431 0.063 Uiso 1 1 calc R U . . .
C63 C 0.31515(13) 0.8523(2) 0.52706(7) 0.0472(6) Uani 1 1 d . . . . .
H63A H 0.3486 0.7863 0.5310 0.071 Uiso 1 1 calc R U . . .
H63B H 0.3360 0.9170 0.5410 0.071 Uiso 1 1 calc R U . . .
H63C H 0.3126 0.8713 0.5009 0.071 Uiso 1 1 calc R U . . .
C64 C 0.17823(11) 0.63195(17) 0.54771(5) 0.0269(4) Uani 1 1 d . . . . .
H64 H 0.1560 0.5693 0.5323 0.032 Uiso 1 1 calc R U . . .
C65 C 0.11418(13) 0.6726(2) 0.57236(6) 0.0377(5) Uani 1 1 d . . . . .
H65A H 0.0723 0.7053 0.5572 0.056 Uiso 1 1 calc R U . . .
H65B H 0.1347 0.7302 0.5894 0.056 Uiso 1 1 calc R U . . .
H65C H 0.0945 0.6082 0.5863 0.056 Uiso 1 1 calc R U . . .
C66 C 0.24428(13) 0.5806(2) 0.57060(6) 0.0392(5) Uani 1 1 d . . . . .
H66A H 0.2839 0.5522 0.5543 0.059 Uiso 1 1 calc R U . . .
H66B H 0.2248 0.5179 0.5853 0.059 Uiso 1 1 calc R U . . .
H66C H 0.2667 0.6388 0.5869 0.059 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
Ge2 N4 1.8513(15) . ?
Ge2 N5 1.8542(14) . ?
Ge2 S1 2.2488(5) . ?
Ge2 B2 2.378(2) . ?
Ge2 Ge3 2.5085(3) . ?
B2 N6 1.414(3) . ?
B2 N4 1.459(3) . ?
B2 N5 1.472(3) . ?
C2 C3 1.394(3) . ?
C2 C1 1.407(3) . ?
C2 C7 1.501(4) . ?
N2 C9 1.420(3) . ?
N2 B1 1.470(3) . ?
N2 Ge1 1.8559(15) . ?
Ge3 N7 1.8553(14) . ?
Ge3 N8 1.8617(14) . ?
Ge3 B3 2.377(2) . ?
Ge3 Ge1 2.4835(3) . ?
B3 N9 1.408(2) . ?
B3 N7 1.470(2) . ?
B3 N8 1.473(2) . ?
C3 C4 1.372(4) . ?
C3 H3 0.9500 . ?
N3 B1 1.416(3) . ?
N3 C17 1.476(3) . ?
N3 C20 1.482(3) . ?
N5 C31 1.417(2) . ?
C5 C4 1.376(4) . ?
C5 C6 1.388(3) . ?
C5 H5 0.9500 . ?
N4 C23 1.418(2) . ?
C4 H4 0.9500 . ?
N6 C42 1.468(3) . ?
N6 C39 1.497(3) . ?
C6 C1 1.393(3) . ?
C6 C8 1.507(3) . ?
N8 C53 1.421(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N7 C45 1.417(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N9 C61 1.479(2) . ?
N9 C64 1.481(2) . ?
C9 C14 1.400(3) . ?
C9 C10 1.399(3) . ?
C10 C11 1.393(3) . ?
C10 C15 1.502(3) . ?
C12 C11 1.370(4) . ?
C12 C13 1.374(4) . ?
C12 H12 0.9500 . ?
C11 H11 0.9500 . ?
C14 C13 1.391(3) . ?
C14 C16 1.499(3) . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C18 C17 1.529(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 C19 1.530(3) . ?
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 . ?
Ge1 N1 1.8579(15) . ?
Ge1 S1 2.2398(5) . ?
Ge1 B1 2.368(2) . ?
B1 N1 1.469(3) . ?
C1 N1 1.418(2) . ?
C20 C21 1.519(3) . ?
C20 C22 1.524(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 C28 1.400(3) . ?
C23 C24 1.400(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C26 C27 1.373(3) . ?
C26 C25 1.377(4) . ?
C26 H26 0.9500 . ?
C25 C24 1.396(3) . ?
C25 H25 0.9500 . ?
C24 C29 1.499(3) . ?
C27 C28 1.391(3) . ?
C27 H27 0.9500 . ?
C28 C30 1.505(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 C36 1.401(3) . ?
C31 C32 1.400(3) . ?
C32 C33 1.390(3) . ?
C32 C37 1.500(3) . ?
C33 C34 1.369(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.396(3) . ?
C35 H35 0.9500 . ?
C36 C38 1.505(3) . ?
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 C40 1.511(4) . ?
C39 C41 1.523(4) . ?
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 1.496(3) . ?
C42 C43 1.511(3) . ?
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 1.400(3) . ?
C45 C46 1.407(3) . ?
C46 C47 1.389(3) . ?
C46 C51 1.499(3) . ?
C47 C48 1.374(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.381(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.386(3) . ?
C49 H49 0.9500 . ?
C50 C52 1.502(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.401(3) . ?
C53 C58 1.402(3) . ?
C54 C55 1.396(3) . ?
C54 C59 1.501(3) . ?
C55 C56 1.376(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.377(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.391(3) . ?
C57 H57 0.9500 . ?
C58 C60 1.504(3) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.520(3) . ?
C61 C63 1.521(3) . ?
C61 H61 1.0000 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C66 1.524(3) . ?
C64 C65 1.527(3) . ?
C64 H64 1.0000 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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
N4 Ge2 N5 76.07(7) . . ?
N4 Ge2 S1 114.37(5) . . ?
N5 Ge2 S1 116.73(5) . . ?
N4 Ge2 B2 37.83(7) . . ?
N5 Ge2 B2 38.25(7) . . ?
S1 Ge2 B2 122.77(5) . . ?
N4 Ge2 Ge3 130.13(5) . . ?
N5 Ge2 Ge3 132.75(5) . . ?
S1 Ge2 Ge3 89.555(14) . . ?
B2 Ge2 Ge3 147.56(5) . . ?
N6 B2 N4 127.43(18) . . ?
N6 B2 N5 130.21(18) . . ?
N4 B2 N5 102.34(15) . . ?
N6 B2 Ge2 177.67(16) . . ?
N4 B2 Ge2 51.11(9) . . ?
N5 B2 Ge2 51.24(8) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C7 120.0(2) . . ?
C1 C2 C7 121.8(2) . . ?
C9 N2 B1 134.35(16) . . ?
C9 N2 Ge1 134.04(12) . . ?
B1 N2 Ge1 90.04(12) . . ?
N7 Ge3 N8 76.38(6) . . ?
N7 Ge3 B3 38.20(6) . . ?
N8 Ge3 B3 38.27(7) . . ?
N7 Ge3 Ge1 116.79(5) . . ?
N8 Ge3 Ge1 131.19(5) . . ?
B3 Ge3 Ge1 132.84(5) . . ?
N7 Ge3 Ge2 120.53(4) . . ?
N8 Ge3 Ge2 134.95(5) . . ?
B3 Ge3 Ge2 142.60(5) . . ?
Ge1 Ge3 Ge2 81.415(9) . . ?
N9 B3 N7 129.18(17) . . ?
N9 B3 N8 128.05(17) . . ?
N7 B3 N8 102.68(15) . . ?
N9 B3 Ge3 174.08(14) . . ?
N7 B3 Ge3 51.29(8) . . ?
N8 B3 Ge3 51.54(8) . . ?
C4 C3 C2 121.3(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
B1 N3 C17 120.06(18) . . ?
B1 N3 C20 124.62(19) . . ?
C17 N3 C20 115.19(17) . . ?
C31 N5 B2 133.16(15) . . ?
C31 N5 Ge2 131.55(12) . . ?
B2 N5 Ge2 90.52(11) . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C23 N4 B2 133.19(16) . . ?
C23 N4 Ge2 134.16(12) . . ?
B2 N4 Ge2 91.05(11) . . ?
C3 C4 C5 120.0(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
B2 N6 C42 125.88(18) . . ?
B2 N6 C39 119.00(18) . . ?
C42 N6 C39 114.67(17) . . ?
C5 C6 C1 119.4(2) . . ?
C5 C6 C8 119.2(2) . . ?
C1 C6 C8 121.31(19) . . ?
C53 N8 B3 133.58(15) . . ?
C53 N8 Ge3 133.48(12) . . ?
B3 N8 Ge3 90.18(11) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C45 N7 B3 130.87(15) . . ?
C45 N7 Ge3 128.66(11) . . ?
B3 N7 Ge3 90.51(11) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
B3 N9 C61 124.63(16) . . ?
B3 N9 C64 119.83(16) . . ?
C61 N9 C64 115.15(14) . . ?
C14 C9 C10 120.22(19) . . ?
C14 C9 N2 119.08(17) . . ?
C10 C9 N2 120.70(18) . . ?
C11 C10 C9 118.8(2) . . ?
C11 C10 C15 120.7(2) . . ?
C9 C10 C15 120.44(19) . . ?
C11 C12 C13 119.9(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C11 C10 121.1(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C13 C14 C9 118.8(2) . . ?
C13 C14 C16 120.5(2) . . ?
C9 C14 C16 120.7(2) . . ?
C12 C13 C14 121.1(2) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
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 . . ?
N3 C17 C18 113.5(2) . . ?
N3 C17 C19 112.1(2) . . ?
C18 C17 C19 110.5(2) . . ?
N3 C17 H17 106.7 . . ?
C18 C17 H17 106.7 . . ?
C19 C17 H17 106.7 . . ?
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 Ge1 N1 76.68(7) . . ?
N2 Ge1 S1 117.57(5) . . ?
N1 Ge1 S1 115.62(5) . . ?
N2 Ge1 B1 38.36(8) . . ?
N1 Ge1 B1 38.34(8) . . ?
S1 Ge1 B1 125.65(5) . . ?
N2 Ge1 Ge3 134.94(5) . . ?
N1 Ge1 Ge3 124.35(5) . . ?
S1 Ge1 Ge3 90.400(15) . . ?
B1 Ge1 Ge3 143.26(5) . . ?
N3 B1 N1 128.8(2) . . ?
N3 B1 N2 127.9(2) . . ?
N1 B1 N2 103.26(16) . . ?
N3 B1 Ge1 176.79(15) . . ?
N1 B1 Ge1 51.68(9) . . ?
N2 B1 Ge1 51.60(9) . . ?
C6 C1 C2 120.2(2) . . ?
C6 C1 N1 119.74(18) . . ?
C2 C1 N1 120.1(2) . . ?
C1 N1 B1 131.64(16) . . ?
C1 N1 Ge1 125.63(12) . . ?
B1 N1 Ge1 89.98(12) . . ?
Ge1 S1 Ge2 92.994(18) . . ?
N3 C20 C21 111.17(19) . . ?
N3 C20 C22 114.9(2) . . ?
C21 C20 C22 111.3(3) . . ?
N3 C20 H20 106.3 . . ?
C21 C20 H20 106.3 . . ?
C22 C20 H20 106.3 . . ?
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 . . ?
C28 C23 C24 120.69(18) . . ?
C28 C23 N4 117.91(17) . . ?
C24 C23 N4 121.33(18) . . ?
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 . . ?
C27 C26 C25 120.2(2) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C25 C24 121.4(2) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C24 C23 118.0(2) . . ?
C25 C24 C29 120.5(2) . . ?
C23 C24 C29 121.43(19) . . ?
C26 C27 C28 120.5(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C23 119.2(2) . . ?
C27 C28 C30 120.3(2) . . ?
C23 C28 C30 120.44(18) . . ?
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 . . ?
C36 C31 C32 120.55(19) . . ?
C36 C31 N5 120.57(18) . . ?
C32 C31 N5 118.88(17) . . ?
C33 C32 C31 118.8(2) . . ?
C33 C32 C37 120.6(2) . . ?
C31 C32 C37 120.67(18) . . ?
C34 C33 C32 121.1(2) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 120.1(2) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 121.0(2) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 118.3(2) . . ?
C35 C36 C38 120.3(2) . . ?
C31 C36 C38 121.32(19) . . ?
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 . . ?
N6 C39 C40 112.7(2) . . ?
N6 C39 C41 112.9(2) . . ?
C40 C39 C41 112.1(2) . . ?
N6 C39 H39 106.2 . . ?
C40 C39 H39 106.2 . . ?
C41 C39 H39 106.2 . . ?
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 . . ?
N6 C42 C44 111.57(19) . . ?
N6 C42 C43 116.13(19) . . ?
C44 C42 C43 112.4(2) . . ?
N6 C42 H42 105.2 . . ?
C44 C42 H42 105.2 . . ?
C43 C42 H42 105.2 . . ?
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 120.19(17) . . ?
C50 C45 N7 119.65(16) . . ?
C46 C45 N7 120.16(16) . . ?
C47 C46 C45 118.69(18) . . ?
C47 C46 C51 119.28(18) . . ?
C45 C46 C51 122.02(17) . . ?
C48 C47 C46 121.19(19) . . ?
C48 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
C47 C48 C49 119.81(19) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C48 C49 C50 121.03(19) . . ?
C48 C49 H49 119.5 . . ?
C50 C49 H49 119.5 . . ?
C49 C50 C45 118.97(18) . . ?
C49 C50 C52 120.05(18) . . ?
C45 C50 C52 120.98(17) . . ?
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 . . ?
C54 C53 C58 120.53(17) . . ?
C54 C53 N8 119.09(16) . . ?
C58 C53 N8 120.38(17) . . ?
C55 C54 C53 118.62(19) . . ?
C55 C54 C59 120.09(19) . . ?
C53 C54 C59 121.27(18) . . ?
C56 C55 C54 121.2(2) . . ?
C56 C55 H55 119.4 . . ?
C54 C55 H55 119.4 . . ?
C55 C56 C57 119.6(2) . . ?
C55 C56 H56 120.2 . . ?
C57 C56 H56 120.2 . . ?
C56 C57 C58 121.4(2) . . ?
C56 C57 H57 119.3 . . ?
C58 C57 H57 119.3 . . ?
C57 C58 C53 118.62(19) . . ?
C57 C58 C60 120.57(19) . . ?
C53 C58 C60 120.81(17) . . ?
C54 C59 H59A 109.5 . . ?
C54 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C54 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N9 C61 C62 114.94(16) . . ?
N9 C61 C63 111.69(16) . . ?
C62 C61 C63 110.38(19) . . ?
N9 C61 H61 106.4 . . ?
C62 C61 H61 106.4 . . ?
C63 C61 H61 106.4 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N9 C64 C66 113.43(16) . . ?
N9 C64 C65 112.25(16) . . ?
C66 C64 C65 110.54(16) . . ?
N9 C64 H64 106.7 . . ?
C66 C64 H64 106.7 . . ?
C65 C64 H64 106.7 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.750 -0.112 0.250 467 74 ' '
2 0.250 -0.066 0.750 467 74 ' '
_platon_squeeze_details          ?


_refine_diff_density_max         0.480
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.056

_shelxl_version_number           2013-4



