# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_Compound_6__sharma2m
_database_code_depnum_ccdc_archive 'CCDC 1564828'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 Cl2 Ge2 N4 O2'
_chemical_formula_sum            'C30 H46 Cl2 Ge2 N4 O2'
_chemical_formula_weight         710.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2234(14)
_cell_length_b                   10.4654(17)
_cell_length_c                   11.0901(19)
_cell_angle_alpha                105.331(3)
_cell_angle_beta                 105.474(3)
_cell_angle_gamma                104.265(3)
_cell_volume                     833.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2003
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.413
_exptl_crystal_size_min          0.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             368.0
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4407
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2943
_reflns_number_gt                2617
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0412P)²+0.0205P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2892
_refine_ls_number_parameters     185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0798
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.60976(3) -0.02719(3) 0.59693(3) 0.03456(11) Uani 1 1 d . . .
Cl1 Cl 0.45602(10) -0.20966(8) 0.63120(8) 0.0578(2) Uani 1 1 d . . .
O1 O 0.4445(3) 0.0614(2) 0.57854(18) 0.0522(5) Uani 1 1 d . . .
N1 N 0.7559(3) 0.1025(2) 0.7735(2) 0.0365(5) Uani 1 1 d . . .
N2 N 0.8306(3) -0.0695(2) 0.6104(2) 0.0386(5) Uani 1 1 d . . .
C7 C 0.9617(3) -0.0069(3) 0.7296(3) 0.0370(6) Uani 1 1 d . . .
C1 C 0.9162(3) 0.0913(3) 0.8273(3) 0.0362(6) Uani 1 1 d . . .
C8 C 0.6851(3) 0.1936(3) 0.8544(3) 0.0406(6) Uani 1 1 d . . .
H8A H 0.6969 0.1740 0.9364 0.049 Uiso 1 1 calc R . .
H8B H 0.5581 0.1687 0.8059 0.049 Uiso 1 1 calc R . .
C2 C 1.0220(4) 0.1635(3) 0.9613(3) 0.0446(6) Uani 1 1 d . . .
H2 H 0.9696 0.2165 1.0097 0.054 Uiso 1 1 calc R . .
C9 C 0.8477(4) -0.1648(3) 0.4942(3) 0.0471(7) Uani 1 1 d . . .
H9A H 0.9741 -0.1428 0.5067 0.056 Uiso 1 1 calc R . .
H9B H 0.7904 -0.1463 0.4152 0.056 Uiso 1 1 calc R . .
C6 C 1.1266(4) -0.0295(3) 0.7570(3) 0.0483(7) Uani 1 1 d . . .
H6 H 1.1381 -0.0895 0.6837 0.058 Uiso 1 1 calc R . .
C10 C 0.7757(4) 0.3518(3) 0.8908(3) 0.0481(7) Uani 1 1 d . . .
H10 H 0.9036 0.3771 0.9412 0.058 Uiso 1 1 calc R . .
C3 C 1.1915(4) 0.1715(3) 1.0368(3) 0.0512(7) Uani 1 1 d . . .
H3 H 1.2329 0.2273 1.1267 0.061 Uiso 1 1 calc R . .
C4 C 1.3060(4) 0.1091(3) 0.9979(3) 0.0567(8) Uani 1 1 d . . .
H4 H 1.4161 0.1289 1.0631 0.068 Uiso 1 1 calc R . .
C5 C 1.2744(4) 0.0204(3) 0.8721(3) 0.0543(8) Uani 1 1 d . . .
H5 H 1.3683 -0.0112 0.8633 0.065 Uiso 1 1 calc R . .
C11 C 0.7676(5) -0.3200(3) 0.4689(3) 0.0653(9) Uani 1 1 d . . .
H11 H 0.6400 -0.3404 0.4561 0.078 Uiso 1 1 calc R . .
C12 C 0.7578(6) 0.3928(4) 0.7686(4) 0.0780(11) Uani 1 1 d . . .
H12A H 0.6330 0.3652 0.7160 0.117 Uiso 1 1 calc R . .
H12B H 0.8164 0.3464 0.7162 0.117 Uiso 1 1 calc R . .
H12C H 0.8126 0.4931 0.7957 0.117 Uiso 1 1 calc R . .
C13 C 0.6946(6) 0.4280(4) 0.9807(4) 0.0909(13) Uani 1 1 d . . .
H13A H 0.7504 0.5278 1.0060 0.136 Uiso 1 1 calc R . .
H13B H 0.7136 0.4030 1.0594 0.136 Uiso 1 1 calc R . .
H13C H 0.5681 0.4016 0.9340 0.136 Uiso 1 1 calc R . .
C15 C 0.7792(7) -0.4049(4) 0.3390(4) 0.0983(14) Uani 1 1 d . . .
H15A H 0.7277 -0.3734 0.2689 0.147 Uiso 1 1 calc R . .
H15B H 0.7145 -0.5030 0.3160 0.147 Uiso 1 1 calc R . .
H15C H 0.9027 -0.3919 0.3501 0.147 Uiso 1 1 calc R . .
C14 C 0.8481(7) -0.3659(4) 0.5795(4) 0.0998(15) Uani 1 1 d . . .
H14A H 0.9704 -0.3562 0.5886 0.150 Uiso 1 1 calc R . .
H14B H 0.7813 -0.4627 0.5599 0.150 Uiso 1 1 calc R . .
H14C H 0.8448 -0.3085 0.6615 0.150 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.7899(19) 2_656 ?
Ge1 O1 1.8218(18) . ?
Ge1 N1 1.912(2) . ?
Ge1 N2 1.950(2) . ?
Ge1 Cl1 2.2000(8) . ?
Ge1 Ge1 2.6995(6) 2_656 ?
O1 Ge1 1.7899(19) 2_656 ?
N1 C1 1.342(3) . ?
N1 C8 1.467(3) . ?
N2 C7 1.331(3) . ?
N2 C9 1.470(3) . ?
C7 C6 1.402(4) . ?
C7 C1 1.479(4) . ?
C1 C2 1.389(4) . ?
C8 C10 1.529(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 C3 1.390(4) . ?
C2 H2 0.9300 . ?
C9 C11 1.512(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C6 C5 1.373(4) . ?
C6 H6 0.9300 . ?
C10 C13 1.506(4) . ?
C10 C12 1.509(4) . ?
C10 H10 0.9800 . ?
C3 C4 1.367(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C11 C14 1.487(5) . ?
C11 C15 1.520(5) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

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
O1 Ge1 O1 83.27(8) 2_656 . ?
O1 Ge1 N1 145.99(10) 2_656 . ?
O1 Ge1 N1 93.71(8) . . ?
O1 Ge1 N2 91.39(8) 2_656 . ?
O1 Ge1 N2 162.00(10) . . ?
N1 Ge1 N2 81.12(9) . . ?
O1 Ge1 Cl1 110.38(8) 2_656 . ?
O1 Ge1 Cl1 98.72(7) . . ?
N1 Ge1 Cl1 103.58(7) . . ?
N2 Ge1 Cl1 99.26(7) . . ?
O1 Ge1 Ge1 42.08(6) 2_656 2_656 ?
O1 Ge1 Ge1 41.18(6) . 2_656 ?
N1 Ge1 Ge1 126.39(6) . 2_656 ?
N2 Ge1 Ge1 131.14(7) . 2_656 ?
Cl1 Ge1 Ge1 109.46(3) . 2_656 ?
Ge1 O1 Ge1 96.73(8) 2_656 . ?
C1 N1 C8 121.1(2) . . ?
C1 N1 Ge1 116.70(17) . . ?
C8 N1 Ge1 121.48(16) . . ?
C7 N2 C9 123.2(2) . . ?
C7 N2 Ge1 115.90(17) . . ?
C9 N2 Ge1 120.94(17) . . ?
N2 C7 C6 123.0(2) . . ?
N2 C7 C1 112.8(2) . . ?
C6 C7 C1 124.1(2) . . ?
N1 C1 C2 122.1(2) . . ?
N1 C1 C7 112.6(2) . . ?
C2 C1 C7 125.3(2) . . ?
N1 C8 C10 115.4(2) . . ?
N1 C8 H8A 108.4 . . ?
C10 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C10 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C1 C2 C3 132.1(3) . . ?
C1 C2 H2 113.9 . . ?
C3 C2 H2 113.9 . . ?
N2 C9 C11 115.0(2) . . ?
N2 C9 H9A 108.5 . . ?
C11 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C11 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C5 C6 C7 131.9(3) . . ?
C5 C6 H6 114.0 . . ?
C7 C6 H6 114.0 . . ?
C13 C10 C12 111.7(3) . . ?
C13 C10 C8 107.8(3) . . ?
C12 C10 C8 112.1(3) . . ?
C13 C10 H10 108.4 . . ?
C12 C10 H10 108.4 . . ?
C8 C10 H10 108.4 . . ?
C4 C3 C2 129.3(3) . . ?
C4 C3 H3 115.3 . . ?
C2 C3 H3 115.3 . . ?
C3 C4 C5 126.4(3) . . ?
C3 C4 H4 116.8 . . ?
C5 C4 H4 116.8 . . ?
C4 C5 C6 130.5(3) . . ?
C4 C5 H5 114.7 . . ?
C6 C5 H5 114.7 . . ?
C14 C11 C9 114.8(3) . . ?
C14 C11 C15 110.5(3) . . ?
C9 C11 C15 109.0(3) . . ?
C14 C11 H11 107.4 . . ?
C9 C11 H11 107.4 . . ?
C15 C11 H11 107.4 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ge1 O1 Ge1 0.0 2_656 . . 2_656 ?
N1 Ge1 O1 Ge1 145.97(10) . . . 2_656 ?
N2 Ge1 O1 Ge1 73.5(3) . . . 2_656 ?
Cl1 Ge1 O1 Ge1 -109.67(8) . . . 2_656 ?
O1 Ge1 N1 C1 -88.0(2) 2_656 . . . ?
O1 Ge1 N1 C1 -171.45(19) . . . . ?
N2 Ge1 N1 C1 -8.81(18) . . . . ?
Cl1 Ge1 N1 C1 88.65(18) . . . . ?
Ge1 Ge1 N1 C1 -144.21(15) 2_656 . . . ?
O1 Ge1 N1 C8 101.8(2) 2_656 . . . ?
O1 Ge1 N1 C8 18.4(2) . . . . ?
N2 Ge1 N1 C8 -179.0(2) . . . . ?
Cl1 Ge1 N1 C8 -81.53(19) . . . . ?
Ge1 Ge1 N1 C8 45.6(2) 2_656 . . . ?
O1 Ge1 N2 C7 153.41(19) 2_656 . . . ?
O1 Ge1 N2 C7 81.2(3) . . . . ?
N1 Ge1 N2 C7 6.75(18) . . . . ?
Cl1 Ge1 N2 C7 -95.68(18) . . . . ?
Ge1 Ge1 N2 C7 138.12(16) 2_656 . . . ?
O1 Ge1 N2 C9 -26.3(2) 2_656 . . . ?
O1 Ge1 N2 C9 -98.6(3) . . . . ?
N1 Ge1 N2 C9 -173.0(2) . . . . ?
Cl1 Ge1 N2 C9 84.57(19) . . . . ?
Ge1 Ge1 N2 C9 -41.6(2) 2_656 . . . ?
C9 N2 C7 C6 -2.3(4) . . . . ?
Ge1 N2 C7 C6 178.0(2) . . . . ?
C9 N2 C7 C1 176.0(2) . . . . ?
Ge1 N2 C7 C1 -3.7(3) . . . . ?
C8 N1 C1 C2 0.6(4) . . . . ?
Ge1 N1 C1 C2 -169.6(2) . . . . ?
C8 N1 C1 C7 179.3(2) . . . . ?
Ge1 N1 C1 C7 9.1(3) . . . . ?
N2 C7 C1 N1 -3.3(3) . . . . ?
C6 C7 C1 N1 175.0(2) . . . . ?
N2 C7 C1 C2 175.4(2) . . . . ?
C6 C7 C1 C2 -6.3(4) . . . . ?
C1 N1 C8 C10 73.3(3) . . . . ?
Ge1 N1 C8 C10 -116.9(2) . . . . ?
N1 C1 C2 C3 -177.8(3) . . . . ?
C7 C1 C2 C3 3.7(5) . . . . ?
C7 N2 C9 C11 98.1(3) . . . . ?
Ge1 N2 C9 C11 -82.2(3) . . . . ?
N2 C7 C6 C5 -177.7(3) . . . . ?
C1 C7 C6 C5 4.2(5) . . . . ?
N1 C8 C10 C13 -176.3(3) . . . . ?
N1 C8 C10 C12 60.3(3) . . . . ?
C1 C2 C3 C4 0.9(5) . . . . ?
C2 C3 C4 C5 -1.4(5) . . . . ?
C3 C4 C5 C6 -0.9(6) . . . . ?
C7 C6 C5 C4 0.2(6) . . . . ?
N2 C9 C11 C14 -60.8(4) . . . . ?
N2 C9 C11 C15 174.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_Compound_8__sharma2m
_database_code_depnum_ccdc_archive 'CCDC 1564829'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H58 Ge2 N6 O2'
_chemical_formula_sum            'C42 H58 Ge2 N6 O2'
_chemical_formula_weight         824.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.571(4)
_cell_length_b                   13.665(7)
_cell_length_c                   15.943(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.027(14)
_cell_angle_gamma                90.00
_cell_volume                     2084.7(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1297
_cell_measurement_theta_min      2.5975
_cell_measurement_theta_max      21.561

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.157
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864.0
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4960
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3667
_reflns_number_gt                2226
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1225P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2853
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1912
_refine_ls_wR_factor_gt          0.1524
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.57364(6) 0.43861(4) 0.55076(4) 0.0444(3) Uani 1 1 d . . .
O1 O 0.4805(5) 0.5531(2) 0.5592(3) 0.0568(12) Uani 1 1 d . . .
N2 N 0.6588(5) 0.4588(3) 0.6637(3) 0.0486(14) Uani 1 1 d . . .
N1 N 0.7658(5) 0.4108(3) 0.5276(3) 0.0419(12) Uani 1 1 d . . .
C7 C 0.7926(7) 0.4370(3) 0.6728(4) 0.0459(18) Uani 1 1 d . . .
C9 C 0.5692(6) 0.4873(5) 0.7334(4) 0.0558(16) Uani 1 1 d . . .
H9A H 0.6028 0.4546 0.7839 0.067 Uiso 1 1 calc R . .
H9B H 0.4753 0.4637 0.7216 0.067 Uiso 1 1 calc R . .
C11 C 0.5616(9) 0.5967(6) 0.7511(5) 0.081(2) Uani 1 1 d . . .
H11 H 0.5235 0.6275 0.7001 0.097 Uiso 1 1 calc R . .
C16 C 0.4053(7) 0.2543(4) 0.5460(4) 0.0538(19) Uani 1 1 d . . .
C13 C 0.8845(10) 0.2683(7) 0.3350(5) 0.107(3) Uani 1 1 d . . .
H13A H 0.9073 0.2014 0.3231 0.161 Uiso 1 1 calc R . .
H13B H 0.9647 0.3088 0.3258 0.161 Uiso 1 1 calc R . .
H13C H 0.8088 0.2891 0.2989 0.161 Uiso 1 1 calc R . .
C2 C 0.9976(7) 0.3921(4) 0.5826(5) 0.0588(19) Uani 1 1 d . . .
H2 H 1.0220 0.3778 0.5278 0.071 Uiso 1 1 calc R . .
C17 C 0.4083(7) 0.1601(5) 0.5781(5) 0.074(2) Uani 1 1 d . . .
H17 H 0.4634 0.1479 0.6256 0.089 Uiso 1 1 calc R . .
C3 C 1.1100(9) 0.3897(5) 0.6389(6) 0.074(2) Uani 1 1 d . . .
H3 H 1.1964 0.3780 0.6151 0.089 Uiso 1 1 calc R . .
C8 C 0.8112(6) 0.3844(4) 0.4433(4) 0.0544(16) Uani 1 1 d . . .
H8A H 0.8954 0.4211 0.4316 0.065 Uiso 1 1 calc R . .
H8B H 0.7398 0.4057 0.4034 0.065 Uiso 1 1 calc R . .
C5 C 0.9982(10) 0.4213(5) 0.7728(6) 0.079(2) Uani 1 1 d . . .
H5 H 1.0162 0.4233 0.8303 0.094 Uiso 1 1 calc R . .
C4 C 1.1130(8) 0.4019(6) 0.7242(6) 0.079(2) Uani 1 1 d . . .
H4 H 1.1993 0.3966 0.7516 0.095 Uiso 1 1 calc R . .
C1 C 0.8574(7) 0.4113(3) 0.5915(5) 0.0494(18) Uani 1 1 d . . .
C12 C 0.7274(11) 0.2102(6) 0.4476(7) 0.127(4) Uani 1 1 d . . .
H12A H 0.7109 0.2124 0.5067 0.190 Uiso 1 1 calc R . .
H12B H 0.7531 0.1449 0.4318 0.190 Uiso 1 1 calc R . .
H12C H 0.6440 0.2291 0.4174 0.190 Uiso 1 1 calc R . .
C15 C 0.6945(10) 0.6458(6) 0.7705(6) 0.107(3) Uani 1 1 d . . .
H15A H 0.7244 0.6296 0.8266 0.160 Uiso 1 1 calc R . .
H15B H 0.6822 0.7153 0.7659 0.160 Uiso 1 1 calc R . .
H15C H 0.7638 0.6247 0.7316 0.160 Uiso 1 1 calc R . .
C6 C 0.8635(8) 0.4380(4) 0.7496(5) 0.062(2) Uani 1 1 d . . .
H6 H 0.8066 0.4533 0.7944 0.075 Uiso 1 1 calc R . .
C10 C 0.8405(8) 0.2774(5) 0.4274(5) 0.078(2) Uani 1 1 d . . .
H10 H 0.9215 0.2592 0.4624 0.094 Uiso 1 1 calc R . .
C14 C 0.4528(10) 0.6100(8) 0.8187(6) 0.125(4) Uani 1 1 d . . .
H14A H 0.4849 0.5792 0.8697 0.188 Uiso 1 1 calc R . .
H14B H 0.3663 0.5806 0.8006 0.188 Uiso 1 1 calc R . .
H14C H 0.4386 0.6786 0.8286 0.188 Uiso 1 1 calc R . .
C20 C 0.2469(8) 0.1966(6) 0.4418(5) 0.076(2) Uani 1 1 d . . .
H20 H 0.1901 0.2076 0.3948 0.091 Uiso 1 1 calc R . .
C18 C 0.3226(7) 0.2726(5) 0.4758(5) 0.0628(19) Uani 1 1 d . . .
H18 H 0.3183 0.3348 0.4523 0.075 Uiso 1 1 calc R . .
C21 C 0.2540(11) 0.1054(6) 0.4758(6) 0.103(3) Uani 1 1 d . . .
H21 H 0.2013 0.0553 0.4515 0.124 Uiso 1 1 calc R . .
C19 C 0.3356(11) 0.0852(6) 0.5440(7) 0.102(3) Uani 1 1 d . . .
H19 H 0.3411 0.0224 0.5663 0.123 Uiso 1 1 calc R . .
N3 N 0.4836(5) 0.3264(3) 0.5885(3) 0.0519(13) Uani 1 1 d . . .
H3A H 0.4914 0.3171 0.6418 0.062 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.807(3) . ?
Ge1 O1 1.823(5) 3_666 ?
Ge1 N3 1.864(4) . ?
Ge1 N1 1.920(5) . ?
Ge1 N2 1.983(5) . ?
Ge1 Ge1 2.7091(14) 3_666 ?
O1 Ge1 1.823(5) 3_666 ?
N2 C7 1.320(8) . ?
N2 C9 1.468(7) . ?
N1 C1 1.332(8) . ?
N1 C8 1.466(7) . ?
C7 C6 1.389(10) . ?
C7 C1 1.489(9) . ?
C9 C11 1.522(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C15 1.466(11) . ?
C11 C14 1.523(10) . ?
C11 H11 0.9800 . ?
C16 C18 1.382(9) . ?
C16 C17 1.386(9) . ?
C16 N3 1.405(8) . ?
C13 C10 1.543(10) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C2 C1 1.377(8) . ?
C2 C3 1.389(10) . ?
C2 H2 0.9300 . ?
C17 C19 1.346(10) . ?
C17 H17 0.9300 . ?
C3 C4 1.370(11) . ?
C3 H3 0.9300 . ?
C8 C10 1.511(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C5 C6 1.354(10) . ?
C5 C4 1.382(11) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C12 C10 1.460(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C6 H6 0.9300 . ?
C10 H10 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C20 C21 1.361(11) . ?
C20 C18 1.372(9) . ?
C20 H20 0.9300 . ?
C18 H18 0.9300 . ?
C21 C19 1.356(12) . ?
C21 H21 0.9300 . ?
C19 H19 0.9300 . ?
N3 H3A 0.8600 . ?

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
O1 Ge1 O1 83.4(2) . 3_666 ?
O1 Ge1 N3 117.1(2) . . ?
O1 Ge1 N3 103.7(2) 3_666 . ?
O1 Ge1 N1 131.40(19) . . ?
O1 Ge1 N1 94.8(2) 3_666 . ?
N3 Ge1 N1 110.45(19) . . ?
O1 Ge1 N2 90.4(2) . . ?
O1 Ge1 N2 165.93(18) 3_666 . ?
N3 Ge1 N2 90.3(2) . . ?
N1 Ge1 N2 79.8(2) . . ?
O1 Ge1 Ge1 41.95(16) . 3_666 ?
O1 Ge1 Ge1 41.49(11) 3_666 3_666 ?
N3 Ge1 Ge1 117.63(16) . 3_666 ?
N1 Ge1 Ge1 119.85(15) . 3_666 ?
N2 Ge1 Ge1 131.09(13) . 3_666 ?
Ge1 O1 Ge1 96.56(19) . 3_666 ?
C7 N2 C9 123.8(6) . . ?
C7 N2 Ge1 116.7(4) . . ?
C9 N2 Ge1 119.2(4) . . ?
C1 N1 C8 120.0(5) . . ?
C1 N1 Ge1 118.2(4) . . ?
C8 N1 Ge1 121.7(4) . . ?
N2 C7 C6 123.5(6) . . ?
N2 C7 C1 112.1(6) . . ?
C6 C7 C1 124.4(6) . . ?
N2 C9 C11 115.5(5) . . ?
N2 C9 H9A 108.4 . . ?
C11 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C11 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C15 C11 C9 116.4(6) . . ?
C15 C11 C14 113.4(8) . . ?
C9 C11 C14 106.5(7) . . ?
C15 C11 H11 106.6 . . ?
C9 C11 H11 106.6 . . ?
C14 C11 H11 106.6 . . ?
C18 C16 C17 118.3(6) . . ?
C18 C16 N3 123.9(6) . . ?
C17 C16 N3 117.8(7) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 C2 C3 133.1(7) . . ?
C1 C2 H2 113.5 . . ?
C3 C2 H2 113.5 . . ?
C19 C17 C16 123.4(8) . . ?
C19 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C4 C3 C2 129.8(8) . . ?
C4 C3 H3 115.1 . . ?
C2 C3 H3 115.1 . . ?
N1 C8 C10 116.8(5) . . ?
N1 C8 H8A 108.1 . . ?
C10 C8 H8A 108.1 . . ?
N1 C8 H8B 108.1 . . ?
C10 C8 H8B 108.1 . . ?
H8A C8 H8B 107.3 . . ?
C6 C5 C4 129.9(9) . . ?
C6 C5 H5 115.1 . . ?
C4 C5 H5 115.1 . . ?
C3 C4 C5 125.3(8) . . ?
C3 C4 H4 117.3 . . ?
C5 C4 H4 117.3 . . ?
N1 C1 C2 123.4(6) . . ?
N1 C1 C7 112.8(6) . . ?
C2 C1 C7 123.8(7) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 C6 C7 133.4(8) . . ?
C5 C6 H6 113.3 . . ?
C7 C6 H6 113.3 . . ?
C12 C10 C8 115.6(6) . . ?
C12 C10 C13 112.1(7) . . ?
C8 C10 C13 107.0(6) . . ?
C12 C10 H10 107.3 . . ?
C8 C10 H10 107.3 . . ?
C13 C10 H10 107.3 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C21 C20 C18 120.9(8) . . ?
C21 C20 H20 119.6 . . ?
C18 C20 H20 119.6 . . ?
C20 C18 C16 118.3(7) . . ?
C20 C18 H18 120.8 . . ?
C16 C18 H18 120.8 . . ?
C19 C21 C20 122.0(8) . . ?
C19 C21 H21 119.0 . . ?
C20 C21 H21 119.0 . . ?
C17 C19 C21 117.1(8) . . ?
C17 C19 H19 121.5 . . ?
C21 C19 H19 121.5 . . ?
C16 N3 Ge1 131.8(4) . . ?
C16 N3 H3A 114.1 . . ?
Ge1 N3 H3A 114.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ge1 O1 Ge1 0.0 3_666 . . 3_666 ?
N3 Ge1 O1 Ge1 -102.1(2) . . . 3_666 ?
N1 Ge1 O1 Ge1 90.7(3) . . . 3_666 ?
N2 Ge1 O1 Ge1 167.3(2) . . . 3_666 ?
O1 Ge1 N2 C7 -138.0(4) . . . . ?
O1 Ge1 N2 C7 -74.3(8) 3_666 . . . ?
N3 Ge1 N2 C7 104.9(4) . . . . ?
N1 Ge1 N2 C7 -5.9(4) . . . . ?
Ge1 Ge1 N2 C7 -126.8(3) 3_666 . . . ?
O1 Ge1 N2 C9 47.9(4) . . . . ?
O1 Ge1 N2 C9 111.6(7) 3_666 . . . ?
N3 Ge1 N2 C9 -69.3(4) . . . . ?
N1 Ge1 N2 C9 180.0(4) . . . . ?
Ge1 Ge1 N2 C9 59.1(4) 3_666 . . . ?
O1 Ge1 N1 C1 85.3(4) . . . . ?
O1 Ge1 N1 C1 170.8(4) 3_666 . . . ?
N3 Ge1 N1 C1 -82.6(4) . . . . ?
N2 Ge1 N1 C1 3.9(4) . . . . ?
Ge1 Ge1 N1 C1 135.7(3) 3_666 . . . ?
O1 Ge1 N1 C8 -98.0(5) . . . . ?
O1 Ge1 N1 C8 -12.5(4) 3_666 . . . ?
N3 Ge1 N1 C8 94.1(4) . . . . ?
N2 Ge1 N1 C8 -179.4(4) . . . . ?
Ge1 Ge1 N1 C8 -47.6(4) 3_666 . . . ?
C9 N2 C7 C6 0.4(8) . . . . ?
Ge1 N2 C7 C6 -173.5(4) . . . . ?
C9 N2 C7 C1 -179.7(4) . . . . ?
Ge1 N2 C7 C1 6.5(5) . . . . ?
C7 N2 C9 C11 90.9(7) . . . . ?
Ge1 N2 C9 C11 -95.4(6) . . . . ?
N2 C9 C11 C15 -58.1(9) . . . . ?
N2 C9 C11 C14 174.3(7) . . . . ?
C18 C16 C17 C19 0.5(11) . . . . ?
N3 C16 C17 C19 178.6(8) . . . . ?
C1 C2 C3 C4 3.6(13) . . . . ?
C1 N1 C8 C10 73.9(7) . . . . ?
Ge1 N1 C8 C10 -102.7(6) . . . . ?
C2 C3 C4 C5 -1.0(13) . . . . ?
C6 C5 C4 C3 -4.2(13) . . . . ?
C8 N1 C1 C2 3.0(7) . . . . ?
Ge1 N1 C1 C2 179.7(4) . . . . ?
C8 N1 C1 C7 -178.3(4) . . . . ?
Ge1 N1 C1 C7 -1.6(5) . . . . ?
C3 C2 C1 N1 179.1(6) . . . . ?
C3 C2 C1 C7 0.6(10) . . . . ?
N2 C7 C1 N1 -3.2(6) . . . . ?
C6 C7 C1 N1 176.7(5) . . . . ?
N2 C7 C1 C2 175.4(5) . . . . ?
C6 C7 C1 C2 -4.6(8) . . . . ?
C4 C5 C6 C7 3.6(13) . . . . ?
N2 C7 C6 C5 -177.8(6) . . . . ?
C1 C7 C6 C5 2.3(10) . . . . ?
N1 C8 C10 C12 53.8(10) . . . . ?
N1 C8 C10 C13 179.4(6) . . . . ?
C21 C20 C18 C16 -0.5(10) . . . . ?
C17 C16 C18 C20 0.4(9) . . . . ?
N3 C16 C18 C20 -177.6(5) . . . . ?
C18 C20 C21 C19 -0.3(13) . . . . ?
C16 C17 C19 C21 -1.2(14) . . . . ?
C20 C21 C19 C17 1.1(14) . . . . ?
C18 C16 N3 Ge1 -32.8(8) . . . . ?
C17 C16 N3 Ge1 149.1(5) . . . . ?
O1 Ge1 N3 C16 96.9(5) . . . . ?
O1 Ge1 N3 C16 7.3(6) 3_666 . . . ?
N1 Ge1 N3 C16 -93.3(6) . . . . ?
N2 Ge1 N3 C16 -172.5(5) . . . . ?
Ge1 Ge1 N3 C16 49.3(6) 3_666 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.250
####################################################################### 
# 
# 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_Compound_23__msh1_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1564836'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H28 B F15 Ge N2 O S'
_chemical_formula_sum            'C39 H28 B F15 Ge N2 O S'
_chemical_formula_weight         941.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   15.032(14)
_cell_length_b                   11.229(12)
_cell_length_c                   23.30(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.94(4)
_cell_angle_gamma                90.00
_cell_volume                     3800(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      24.91

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3032
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_T_max  0.486
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39248
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6692
_reflns_number_gt                4916
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0633P)²+6.2014P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6692
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.71605(3) 0.60151(4) 0.440837(19) 0.01400(14) Uani 1 1 d . . .
O1 O 0.75564(18) 0.6471(3) 0.51236(12) 0.0168(7) Uani 1 1 d . . .
S1 S 0.56732(7) 0.56698(10) 0.41023(5) 0.0182(3) Uani 1 1 d . . .
N1 N 0.7870(2) 0.4732(3) 0.42787(15) 0.0147(8) Uani 1 1 d . . .
N2 N 0.7619(3) 0.6812(3) 0.38427(16) 0.0231(9) Uani 1 1 d . . .
B1 B 0.7269(3) 0.6928(5) 0.5654(2) 0.0155(11) Uani 1 1 d . . .
F1 F 0.85113(17) 0.6715(2) 0.69455(10) 0.0235(6) Uani 1 1 d . . .
F2 F 0.86176(17) 0.4818(2) 0.76382(10) 0.0256(6) Uani 1 1 d . . .
F3 F 0.75543(17) 0.2859(2) 0.72686(11) 0.0256(6) Uani 1 1 d . . .
F4 F 0.64336(17) 0.2792(2) 0.61377(11) 0.0235(6) Uani 1 1 d . . .
F5 F 0.63287(16) 0.4669(2) 0.54127(10) 0.0211(6) Uani 1 1 d . . .
F6 F 0.57602(16) 0.6635(2) 0.63232(10) 0.0200(6) Uani 1 1 d . . .
F7 F 0.40539(16) 0.7494(2) 0.59752(11) 0.0230(6) Uani 1 1 d . . .
F8 F 0.34911(16) 0.8767(2) 0.49506(11) 0.0262(6) Uani 1 1 d . . .
F9 F 0.47210(17) 0.9211(2) 0.42797(11) 0.0236(6) Uani 1 1 d . . .
F10 F 0.64431(16) 0.8439(2) 0.46404(11) 0.0223(6) Uani 1 1 d . . .
F11 F 0.92582(16) 0.7071(2) 0.57126(12) 0.0278(6) Uani 1 1 d . . .
F12 F 1.04026(16) 0.8870(2) 0.60832(12) 0.0296(7) Uani 1 1 d . . .
F13 F 0.98093(17) 1.0893(2) 0.65306(11) 0.0257(6) Uani 1 1 d . . .
F14 F 0.80168(18) 1.1037(2) 0.65887(13) 0.0349(7) Uani 1 1 d . . .
F15 F 0.68645(17) 0.9238(2) 0.62380(13) 0.0339(7) Uani 1 1 d . . .
C1 C 0.8271(3) 0.4899(4) 0.38252(18) 0.0151(9) Uani 1 1 d . . .
C2 C 0.8700(3) 0.3958(4) 0.36015(18) 0.0192(10) Uani 1 1 d . . .
H2 H 0.8632 0.3202 0.3768 0.023 Uiso 1 1 calc R . .
C3 C 0.9204(3) 0.3942(4) 0.31814(19) 0.0229(10) Uani 1 1 d . . .
H3 H 0.9424 0.3181 0.3105 0.028 Uiso 1 1 calc R . .
C4 C 0.9437(3) 0.4870(4) 0.2855(2) 0.0267(11) Uani 1 1 d . . .
H4 H 0.9846 0.4689 0.2617 0.032 Uiso 1 1 calc R . .
C5 C 0.9133(3) 0.6028(5) 0.2842(2) 0.0297(12) Uani 1 1 d . . .
H5 H 0.9352 0.6543 0.2585 0.036 Uiso 1 1 calc R . .
C6 C 0.8551(3) 0.6564(5) 0.3148(2) 0.0277(11) Uani 1 1 d . . .
H6 H 0.8395 0.7367 0.3037 0.033 Uiso 1 1 calc R . .
C7 C 0.8158(3) 0.6122(4) 0.35907(18) 0.0202(10) Uani 1 1 d . . .
C8 C 0.7916(3) 0.3587(4) 0.45960(19) 0.0157(9) Uani 1 1 d . . .
H8A H 0.7729 0.2942 0.4300 0.019 Uiso 1 1 calc R . .
H8B H 0.7466 0.3605 0.4840 0.019 Uiso 1 1 calc R . .
C9 C 0.7260(4) 0.8005(5) 0.3592(3) 0.0395(14) Uani 1 1 d . . .
H9A H 0.7102 0.7964 0.3153 0.047 Uiso 1 1 calc R . .
H9B H 0.6690 0.8190 0.3712 0.047 Uiso 1 1 calc R . .
C10 C 0.8872(3) 0.3285(4) 0.50011(19) 0.0188(10) Uani 1 1 d . . .
H10 H 0.9321 0.3274 0.4750 0.023 Uiso 1 1 calc R . .
C11 C 0.7936(4) 0.8976(5) 0.3795(2) 0.0416(14) Uani 1 1 d . . .
H11 H 0.8405 0.8931 0.3560 0.050 Uiso 1 1 calc R . .
C12 C 0.9198(4) 0.4206(5) 0.5487(2) 0.0400(14) Uani 1 1 d . . .
H12A H 0.8800 0.4183 0.5761 0.060 Uiso 1 1 calc R . .
H12B H 0.9172 0.5000 0.5310 0.060 Uiso 1 1 calc R . .
H12C H 0.9833 0.4028 0.5706 0.060 Uiso 1 1 calc R . .
C13 C 0.8837(4) 0.2045(5) 0.5251(3) 0.0425(15) Uani 1 1 d . . .
H13A H 0.9457 0.1803 0.5472 0.064 Uiso 1 1 calc R . .
H13B H 0.8602 0.1485 0.4925 0.064 Uiso 1 1 calc R . .
H13C H 0.8429 0.2046 0.5518 0.064 Uiso 1 1 calc R . .
C14 C 0.8440(4) 0.8944(5) 0.4447(3) 0.0457(15) Uani 1 1 d . . .
H14A H 0.8005 0.9106 0.4687 0.069 Uiso 1 1 calc R . .
H14B H 0.8926 0.9550 0.4529 0.069 Uiso 1 1 calc R . .
H14C H 0.8715 0.8155 0.4548 0.069 Uiso 1 1 calc R . .
C15 C 0.7360(4) 1.0176(5) 0.3615(3) 0.0446(15) Uani 1 1 d . . .
H15A H 0.6972 1.0105 0.3208 0.067 Uiso 1 1 calc R . .
H15B H 0.7784 1.0848 0.3639 0.067 Uiso 1 1 calc R . .
H15C H 0.6970 1.0310 0.3887 0.067 Uiso 1 1 calc R . .
C16 C 0.5587(3) 0.5635(4) 0.33154(18) 0.0164(9) Uani 1 1 d . . .
C17 C 0.5994(3) 0.4728(4) 0.30616(19) 0.0207(10) Uani 1 1 d . . .
H17 H 0.6320 0.4105 0.3302 0.025 Uiso 1 1 calc R . .
C18 C 0.5919(3) 0.4742(4) 0.2452(2) 0.0245(11) Uani 1 1 d . . .
H18 H 0.6208 0.4137 0.2279 0.029 Uiso 1 1 calc R . .
C19 C 0.5427(4) 0.5632(5) 0.2100(2) 0.0349(13) Uani 1 1 d . . .
H19 H 0.5367 0.5634 0.1684 0.042 Uiso 1 1 calc R . .
C20 C 0.5022(4) 0.6516(5) 0.2356(2) 0.0411(15) Uani 1 1 d . . .
H20 H 0.4681 0.7125 0.2112 0.049 Uiso 1 1 calc R . .
C21 C 0.5104(3) 0.6535(4) 0.2967(2) 0.0267(11) Uani 1 1 d . . .
H21 H 0.4832 0.7157 0.3140 0.032 Uiso 1 1 calc R . .
C22 C 0.7400(3) 0.5806(4) 0.61309(18) 0.0145(9) Uani 1 1 d . . .
C23 C 0.7978(3) 0.5756(4) 0.67081(19) 0.0166(10) Uani 1 1 d . . .
C24 C 0.8043(3) 0.4790(4) 0.70848(18) 0.0174(10) Uani 1 1 d . . .
C25 C 0.7516(3) 0.3795(4) 0.68985(19) 0.0185(10) Uani 1 1 d . . .
C26 C 0.6943(3) 0.3771(4) 0.63280(19) 0.0169(10) Uani 1 1 d . . .
C27 C 0.6909(3) 0.4750(4) 0.59692(18) 0.0147(9) Uani 1 1 d . . .
C28 C 0.6189(3) 0.7410(4) 0.54753(18) 0.0139(9) Uani 1 1 d . . .
C29 C 0.5533(3) 0.7234(4) 0.57974(18) 0.0135(9) Uani 1 1 d . . .
C30 C 0.4648(3) 0.7676(4) 0.56310(19) 0.0183(10) Uani 1 1 d . . .
C31 C 0.4363(3) 0.8335(4) 0.51163(19) 0.0167(10) Uani 1 1 d . . .
C32 C 0.4974(3) 0.8563(4) 0.47857(18) 0.0174(10) Uani 1 1 d . . .
C33 C 0.5856(3) 0.8116(4) 0.49771(18) 0.0161(9) Uani 1 1 d . . .
C34 C 0.7973(3) 0.8062(4) 0.59194(17) 0.0144(9) Uani 1 1 d . . .
C35 C 0.8892(3) 0.8046(4) 0.59076(19) 0.0167(9) Uani 1 1 d . . .
C36 C 0.9501(3) 0.8966(4) 0.61053(19) 0.0185(10) Uani 1 1 d . . .
C37 C 0.9218(3) 0.9983(4) 0.63343(19) 0.0194(10) Uani 1 1 d . . .
C38 C 0.8311(3) 1.0048(4) 0.63631(19) 0.0200(10) Uani 1 1 d . . .
C39 C 0.7728(3) 0.9102(4) 0.61683(19) 0.0186(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.698(3) . ?
Ge1 N1 1.864(4) . ?
Ge1 N2 1.866(4) . ?
Ge1 S1 2.199(2) . ?
O1 B1 1.501(5) . ?
S1 C16 1.805(5) . ?
N1 C1 1.358(5) . ?
N1 C8 1.476(5) . ?
N2 C7 1.359(5) . ?
N2 C9 1.504(6) . ?
B1 C22 1.658(7) . ?
B1 C28 1.659(6) . ?
B1 C34 1.670(6) . ?
F1 C23 1.372(5) . ?
F2 C24 1.355(5) . ?
F3 C25 1.351(5) . ?
F4 C26 1.348(5) . ?
F5 C27 1.367(5) . ?
F6 C29 1.362(5) . ?
F7 C30 1.360(5) . ?
F8 C31 1.357(5) . ?
F9 C32 1.354(5) . ?
F10 C33 1.372(5) . ?
F11 C35 1.356(5) . ?
F12 C36 1.373(5) . ?
F13 C37 1.354(5) . ?
F14 C38 1.351(5) . ?
F15 C39 1.358(5) . ?
C1 C2 1.406(6) . ?
C1 C7 1.472(6) . ?
C2 C3 1.384(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.405(6) . ?
C6 H6 0.9500 . ?
C8 C10 1.540(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.483(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C13 1.516(7) . ?
C10 C12 1.519(7) . ?
C10 H10 1.0000 . ?
C11 C14 1.512(8) . ?
C11 C15 1.598(8) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.380(6) . ?
C16 C17 1.396(6) . ?
C17 C18 1.396(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(7) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C27 1.396(6) . ?
C22 C23 1.401(6) . ?
C23 C24 1.383(6) . ?
C24 C25 1.374(6) . ?
C25 C26 1.385(6) . ?
C26 C27 1.375(6) . ?
C28 C33 1.389(6) . ?
C28 C29 1.399(6) . ?
C29 C30 1.378(6) . ?
C30 C31 1.380(6) . ?
C31 C32 1.367(6) . ?
C32 C33 1.379(6) . ?
C34 C35 1.388(6) . ?
C34 C39 1.395(6) . ?
C35 C36 1.378(6) . ?
C36 C37 1.373(6) . ?
C37 C38 1.384(6) . ?
C38 C39 1.378(6) . ?

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
O1 Ge1 N1 108.78(15) . . ?
O1 Ge1 N2 116.67(17) . . ?
N1 Ge1 N2 85.72(16) . . ?
O1 Ge1 S1 116.19(10) . . ?
N1 Ge1 S1 112.82(12) . . ?
N2 Ge1 S1 112.65(13) . . ?
B1 O1 Ge1 144.0(3) . . ?
C16 S1 Ge1 97.70(14) . . ?
C1 N1 C8 122.5(3) . . ?
C1 N1 Ge1 114.0(3) . . ?
C8 N1 Ge1 123.2(3) . . ?
C7 N2 C9 122.2(4) . . ?
C7 N2 Ge1 113.7(3) . . ?
C9 N2 Ge1 122.8(3) . . ?
O1 B1 C22 106.4(3) . . ?
O1 B1 C28 112.0(3) . . ?
C22 B1 C28 110.9(3) . . ?
O1 B1 C34 106.0(3) . . ?
C22 B1 C34 112.2(3) . . ?
C28 B1 C34 109.3(3) . . ?
N1 C1 C2 121.5(4) . . ?
N1 C1 C7 112.7(4) . . ?
C2 C1 C7 125.7(4) . . ?
C3 C2 C1 131.2(4) . . ?
C3 C2 H2 114.4 . . ?
C1 C2 H2 114.4 . . ?
C2 C3 C4 129.8(4) . . ?
C2 C3 H3 115.1 . . ?
C4 C3 H3 115.1 . . ?
C5 C4 C3 126.4(4) . . ?
C5 C4 H4 116.8 . . ?
C3 C4 H4 116.8 . . ?
C4 C5 C6 130.0(5) . . ?
C4 C5 H5 115.0 . . ?
C6 C5 H5 115.0 . . ?
C5 C6 C7 131.2(5) . . ?
C5 C6 H6 114.4 . . ?
C7 C6 H6 114.4 . . ?
N2 C7 C6 121.8(4) . . ?
N2 C7 C1 113.4(4) . . ?
C6 C7 C1 124.9(4) . . ?
N1 C8 C10 114.4(3) . . ?
N1 C8 H8A 108.7 . . ?
C10 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C10 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C11 C9 N2 112.5(5) . . ?
C11 C9 H9A 109.1 . . ?
N2 C9 H9A 109.1 . . ?
C11 C9 H9B 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C13 C10 C12 112.0(4) . . ?
C13 C10 C8 108.5(4) . . ?
C12 C10 C8 112.3(4) . . ?
C13 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C8 C10 H10 108.0 . . ?
C9 C11 C14 115.3(5) . . ?
C9 C11 C15 104.8(4) . . ?
C14 C11 C15 112.5(5) . . ?
C9 C11 H11 108.0 . . ?
C14 C11 H11 108.0 . . ?
C15 C11 H11 108.0 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 120.5(4) . . ?
C21 C16 S1 118.1(3) . . ?
C17 C16 S1 121.5(3) . . ?
C16 C17 C18 119.6(4) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 120.2(4) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 119.6(5) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 121.2(5) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C20 118.9(5) . . ?
C16 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C27 C22 C23 112.3(4) . . ?
C27 C22 B1 120.1(4) . . ?
C23 C22 B1 127.7(4) . . ?
F1 C23 C24 114.9(4) . . ?
F1 C23 C22 120.6(4) . . ?
C24 C23 C22 124.4(4) . . ?
F2 C24 C25 119.6(4) . . ?
F2 C24 C23 120.6(4) . . ?
C25 C24 C23 119.8(4) . . ?
F3 C25 C24 120.3(4) . . ?
F3 C25 C26 120.7(4) . . ?
C24 C25 C26 119.0(4) . . ?
F4 C26 C27 121.6(4) . . ?
F4 C26 C25 119.5(4) . . ?
C27 C26 C25 119.0(4) . . ?
F5 C27 C26 116.0(4) . . ?
F5 C27 C22 118.5(4) . . ?
C26 C27 C22 125.5(4) . . ?
C33 C28 C29 112.1(4) . . ?
C33 C28 B1 121.0(4) . . ?
C29 C28 B1 126.8(4) . . ?
F6 C29 C30 115.6(3) . . ?
F6 C29 C28 120.3(3) . . ?
C30 C29 C28 124.1(4) . . ?
F7 C30 C31 119.3(4) . . ?
F7 C30 C29 120.8(4) . . ?
C31 C30 C29 119.9(4) . . ?
F8 C31 C32 120.8(4) . . ?
F8 C31 C30 120.0(4) . . ?
C32 C31 C30 119.2(4) . . ?
F9 C32 C31 120.8(4) . . ?
F9 C32 C33 120.5(4) . . ?
C31 C32 C33 118.6(4) . . ?
F10 C33 C32 115.2(4) . . ?
F10 C33 C28 118.8(4) . . ?
C32 C33 C28 126.0(4) . . ?
C35 C34 C39 113.0(4) . . ?
C35 C34 B1 121.5(4) . . ?
C39 C34 B1 125.6(4) . . ?
F11 C35 C36 115.2(4) . . ?
F11 C35 C34 120.6(4) . . ?
C36 C35 C34 124.2(4) . . ?
C37 C36 F12 119.1(4) . . ?
C37 C36 C35 120.5(4) . . ?
F12 C36 C35 120.4(4) . . ?
F13 C37 C36 121.1(4) . . ?
F13 C37 C38 120.8(4) . . ?
C36 C37 C38 118.1(4) . . ?
F14 C38 C39 121.1(4) . . ?
F14 C38 C37 119.2(4) . . ?
C39 C38 C37 119.6(4) . . ?
F15 C39 C38 114.9(4) . . ?
F15 C39 C34 120.5(4) . . ?
C38 C39 C34 124.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ge1 O1 B1 -141.5(5) . . . . ?
N2 Ge1 O1 B1 123.8(5) . . . . ?
S1 Ge1 O1 B1 -12.9(5) . . . . ?
O1 Ge1 S1 C16 165.21(18) . . . . ?
N1 Ge1 S1 C16 -68.19(19) . . . . ?
N2 Ge1 S1 C16 26.9(2) . . . . ?
O1 Ge1 N1 C1 -123.5(3) . . . . ?
N2 Ge1 N1 C1 -6.8(3) . . . . ?
S1 Ge1 N1 C1 106.0(3) . . . . ?
O1 Ge1 N1 C8 62.6(3) . . . . ?
N2 Ge1 N1 C8 179.4(3) . . . . ?
S1 Ge1 N1 C8 -67.8(3) . . . . ?
O1 Ge1 N2 C7 112.9(3) . . . . ?
N1 Ge1 N2 C7 4.0(3) . . . . ?
S1 Ge1 N2 C7 -108.9(3) . . . . ?
O1 Ge1 N2 C9 -80.0(4) . . . . ?
N1 Ge1 N2 C9 171.1(4) . . . . ?
S1 Ge1 N2 C9 58.1(4) . . . . ?
Ge1 O1 B1 C22 105.5(5) . . . . ?
Ge1 O1 B1 C28 -15.8(7) . . . . ?
Ge1 O1 B1 C34 -134.9(4) . . . . ?
C8 N1 C1 C2 4.7(6) . . . . ?
Ge1 N1 C1 C2 -169.2(3) . . . . ?
C8 N1 C1 C7 -178.2(4) . . . . ?
Ge1 N1 C1 C7 7.9(4) . . . . ?
N1 C1 C2 C3 -174.4(4) . . . . ?
C7 C1 C2 C3 9.0(7) . . . . ?
C1 C2 C3 C4 0.1(8) . . . . ?
C2 C3 C4 C5 -6.5(8) . . . . ?
C3 C4 C5 C6 1.4(9) . . . . ?
C4 C5 C6 C7 5.5(10) . . . . ?
C9 N2 C7 C6 11.7(7) . . . . ?
Ge1 N2 C7 C6 178.9(4) . . . . ?
C9 N2 C7 C1 -167.8(4) . . . . ?
Ge1 N2 C7 C1 -0.7(5) . . . . ?
C5 C6 C7 N2 178.5(5) . . . . ?
C5 C6 C7 C1 -2.0(9) . . . . ?
N1 C1 C7 N2 -4.7(5) . . . . ?
C2 C1 C7 N2 172.2(4) . . . . ?
N1 C1 C7 C6 175.8(4) . . . . ?
C2 C1 C7 C6 -7.3(7) . . . . ?
C1 N1 C8 C10 71.3(5) . . . . ?
Ge1 N1 C8 C10 -115.4(4) . . . . ?
C7 N2 C9 C11 -83.9(6) . . . . ?
Ge1 N2 C9 C11 110.1(4) . . . . ?
N1 C8 C10 C13 -174.9(4) . . . . ?
N1 C8 C10 C12 60.8(5) . . . . ?
N2 C9 C11 C14 -42.8(6) . . . . ?
N2 C9 C11 C15 -167.1(4) . . . . ?
Ge1 S1 C16 C21 -112.6(3) . . . . ?
Ge1 S1 C16 C17 67.5(4) . . . . ?
C21 C16 C17 C18 0.7(6) . . . . ?
S1 C16 C17 C18 -179.3(3) . . . . ?
C16 C17 C18 C19 -1.5(7) . . . . ?
C17 C18 C19 C20 1.0(8) . . . . ?
C18 C19 C20 C21 0.3(9) . . . . ?
C17 C16 C21 C20 0.6(7) . . . . ?
S1 C16 C21 C20 -179.4(4) . . . . ?
C19 C20 C21 C16 -1.1(8) . . . . ?
O1 B1 C22 C27 -60.5(5) . . . . ?
C28 B1 C22 C27 61.6(5) . . . . ?
C34 B1 C22 C27 -175.9(3) . . . . ?
O1 B1 C22 C23 118.8(4) . . . . ?
C28 B1 C22 C23 -119.2(4) . . . . ?
C34 B1 C22 C23 3.3(6) . . . . ?
C27 C22 C23 F1 -179.6(4) . . . . ?
B1 C22 C23 F1 1.0(6) . . . . ?
C27 C22 C23 C24 -1.5(6) . . . . ?
B1 C22 C23 C24 179.1(4) . . . . ?
F1 C23 C24 F2 -1.6(6) . . . . ?
C22 C23 C24 F2 -179.8(4) . . . . ?
F1 C23 C24 C25 178.0(4) . . . . ?
C22 C23 C24 C25 -0.2(7) . . . . ?
F2 C24 C25 F3 1.4(6) . . . . ?
C23 C24 C25 F3 -178.1(4) . . . . ?
F2 C24 C25 C26 -178.8(4) . . . . ?
C23 C24 C25 C26 1.6(6) . . . . ?
F3 C25 C26 F4 -1.3(6) . . . . ?
C24 C25 C26 F4 179.0(4) . . . . ?
F3 C25 C26 C27 178.7(4) . . . . ?
C24 C25 C26 C27 -1.1(6) . . . . ?
F4 C26 C27 F5 0.1(6) . . . . ?
C25 C26 C27 F5 -179.8(4) . . . . ?
F4 C26 C27 C22 179.0(4) . . . . ?
C25 C26 C27 C22 -0.9(7) . . . . ?
C23 C22 C27 F5 -179.0(3) . . . . ?
B1 C22 C27 F5 0.4(5) . . . . ?
C23 C22 C27 C26 2.1(6) . . . . ?
B1 C22 C27 C26 -178.5(4) . . . . ?
O1 B1 C28 C33 -44.3(5) . . . . ?
C22 B1 C28 C33 -163.0(4) . . . . ?
C34 B1 C28 C33 72.8(5) . . . . ?
O1 B1 C28 C29 139.1(4) . . . . ?
C22 B1 C28 C29 20.4(6) . . . . ?
C34 B1 C28 C29 -103.7(5) . . . . ?
C33 C28 C29 F6 -175.2(4) . . . . ?
B1 C28 C29 F6 1.6(6) . . . . ?
C33 C28 C29 C30 2.0(6) . . . . ?
B1 C28 C29 C30 178.8(4) . . . . ?
F6 C29 C30 F7 -1.0(6) . . . . ?
C28 C29 C30 F7 -178.3(4) . . . . ?
F6 C29 C30 C31 177.6(4) . . . . ?
C28 C29 C30 C31 0.2(7) . . . . ?
F7 C30 C31 F8 -1.7(6) . . . . ?
C29 C30 C31 F8 179.8(4) . . . . ?
F7 C30 C31 C32 177.0(4) . . . . ?
C29 C30 C31 C32 -1.6(6) . . . . ?
F8 C31 C32 F9 -1.0(6) . . . . ?
C30 C31 C32 F9 -179.7(4) . . . . ?
F8 C31 C32 C33 179.2(4) . . . . ?
C30 C31 C32 C33 0.5(6) . . . . ?
F9 C32 C33 F10 3.7(6) . . . . ?
C31 C32 C33 F10 -176.5(4) . . . . ?
F9 C32 C33 C28 -177.8(4) . . . . ?
C31 C32 C33 C28 2.1(7) . . . . ?
C29 C28 C33 F10 175.3(3) . . . . ?
B1 C28 C33 F10 -1.7(6) . . . . ?
C29 C28 C33 C32 -3.2(6) . . . . ?
B1 C28 C33 C32 179.8(4) . . . . ?
O1 B1 C34 C35 -36.0(5) . . . . ?
C22 B1 C34 C35 79.7(5) . . . . ?
C28 B1 C34 C35 -156.9(4) . . . . ?
O1 B1 C34 C39 143.8(4) . . . . ?
C22 B1 C34 C39 -100.4(5) . . . . ?
C28 B1 C34 C39 22.9(6) . . . . ?
C39 C34 C35 F11 176.0(4) . . . . ?
B1 C34 C35 F11 -4.1(6) . . . . ?
C39 C34 C35 C36 -1.6(6) . . . . ?
B1 C34 C35 C36 178.3(4) . . . . ?
F11 C35 C36 C37 -177.5(4) . . . . ?
C34 C35 C36 C37 0.2(7) . . . . ?
F11 C35 C36 F12 1.6(6) . . . . ?
C34 C35 C36 F12 179.3(4) . . . . ?
F12 C36 C37 F13 0.8(6) . . . . ?
C35 C36 C37 F13 180.0(4) . . . . ?
F12 C36 C37 C38 -178.7(4) . . . . ?
C35 C36 C37 C38 0.4(6) . . . . ?
F13 C37 C38 F14 0.2(6) . . . . ?
C36 C37 C38 F14 179.7(4) . . . . ?
F13 C37 C38 C39 -179.0(4) . . . . ?
C36 C37 C38 C39 0.5(6) . . . . ?
F14 C38 C39 F15 -1.7(6) . . . . ?
C37 C38 C39 F15 177.5(4) . . . . ?
F14 C38 C39 C34 178.6(4) . . . . ?
C37 C38 C39 C34 -2.1(7) . . . . ?
C35 C34 C39 F15 -177.0(4) . . . . ?
B1 C34 C39 F15 3.1(6) . . . . ?
C35 C34 C39 C38 2.5(6) . . . . ?
B1 C34 C39 C38 -177.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_Compound_10__msha44m
_database_code_depnum_ccdc_archive 'CCDC 1564831'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H54 Ge2 N6 O2, 2(C7 H8)'
_chemical_formula_sum            'C52 H70 Ge2 N6 O2'
_chemical_formula_weight         956.36

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   10.595(4)
_cell_length_b                   15.635(5)
_cell_length_c                   14.875(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.261(6)
_cell_angle_gamma                90.00
_cell_volume                     2462.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2003
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      24.94

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008.0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10217
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4312
_reflns_number_gt                3106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0442P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4312
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0923
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.11635(3) 0.96351(2) 0.00186(2) 0.01861(13) Uani 1 1 d . . .
N1 N 0.2645(2) 1.02106(16) 0.04948(18) 0.0193(7) Uani 1 1 d . . .
N3 N 0.1542(2) 0.91654(16) -0.11118(19) 0.0204(7) Uani 1 1 d . . .
N2 N 0.1929(2) 0.86928(16) 0.07242(18) 0.0197(6) Uani 1 1 d . . .
C3 C 0.5679(3) 0.9689(2) 0.1761(2) 0.0271(8) Uani 1 1 d . . .
H3 H 0.6335 1.0061 0.1920 0.033 Uiso 1 1 calc R . .
C7 C 0.3098(3) 0.8831(2) 0.1063(2) 0.0194(8) Uani 1 1 d . . .
C8 C 0.2969(3) 1.10837(19) 0.0206(2) 0.0217(8) Uani 1 1 d . . .
H8A H 0.2405 1.1237 -0.0298 0.026 Uiso 1 1 calc R . .
H8B H 0.3819 1.1071 -0.0015 0.026 Uiso 1 1 calc R . .
C1 C 0.3513(3) 0.9728(2) 0.0950(2) 0.0204(8) Uani 1 1 d . . .
C10 C 0.2910(3) 1.1793(2) 0.0913(3) 0.0274(9) Uani 1 1 d . . .
H10 H 0.3451 1.1625 0.1433 0.033 Uiso 1 1 calc R . .
C18 C 0.2328(3) 0.8335(2) -0.2186(2) 0.0274(9) Uani 1 1 d . . .
H18 H 0.2762 0.7903 -0.2473 0.033 Uiso 1 1 calc R . .
C2 C 0.4684(3) 1.0059(2) 0.1264(2) 0.0227(8) Uani 1 1 d . . .
H2 H 0.4816 1.0628 0.1111 0.027 Uiso 1 1 calc R . .
C6 C 0.3858(3) 0.8166(2) 0.1443(2) 0.0252(8) Uani 1 1 d . . .
H6 H 0.3499 0.7625 0.1390 0.030 Uiso 1 1 calc R . .
C19 C 0.1577(3) 0.8983(2) -0.2607(2) 0.0285(9) Uani 1 1 d . . .
H19 H 0.1426 0.9056 -0.3222 0.034 Uiso 1 1 calc R . .
C5 C 0.5035(3) 0.8176(2) 0.1878(2) 0.0276(9) Uani 1 1 d . . .
H5 H 0.5326 0.7646 0.2083 0.033 Uiso 1 1 calc R . .
C14 C 0.0128(4) 0.8171(2) 0.2144(3) 0.0373(10) Uani 1 1 d . . .
H14A H -0.0617 0.8307 0.1784 0.056 Uiso 1 1 calc R . .
H14B H 0.0617 0.8681 0.2248 0.056 Uiso 1 1 calc R . .
H14C H -0.0111 0.7939 0.2710 0.056 Uiso 1 1 calc R . .
C17 C 0.1117(3) 0.9480(2) -0.1941(2) 0.0272(9) Uani 1 1 d . . .
H17 H 0.0599 0.9955 -0.2030 0.033 Uiso 1 1 calc R . .
C4 C 0.5851(3) 0.8860(2) 0.2056(3) 0.0316(9) Uani 1 1 d . . .
H4 H 0.6578 0.8746 0.2406 0.038 Uiso 1 1 calc R . .
C9 C 0.1322(3) 0.7843(2) 0.0739(2) 0.0232(8) Uani 1 1 d . . .
H9A H 0.1905 0.7429 0.0503 0.028 Uiso 1 1 calc R . .
H9B H 0.0585 0.7857 0.0332 0.028 Uiso 1 1 calc R . .
C11 C 0.0908(3) 0.7521(2) 0.1657(2) 0.0252(8) Uani 1 1 d . . .
H11 H 0.1665 0.7391 0.2031 0.030 Uiso 1 1 calc R . .
C16 C 0.2292(3) 0.8466(2) -0.1283(3) 0.0256(8) Uani 1 1 d . . .
H16 H 0.2711 0.8135 -0.0846 0.031 Uiso 1 1 calc R . .
C12 C 0.1589(3) 1.1947(3) 0.1237(3) 0.0401(10) Uani 1 1 d . . .
H12A H 0.1614 1.2393 0.1681 0.060 Uiso 1 1 calc R . .
H12B H 0.1274 1.1431 0.1497 0.060 Uiso 1 1 calc R . .
H12C H 0.1042 1.2115 0.0737 0.060 Uiso 1 1 calc R . .
C13 C 0.3460(4) 1.2603(2) 0.0512(3) 0.0539(13) Uani 1 1 d . . .
H13A H 0.4312 1.2496 0.0347 0.081 Uiso 1 1 calc R . .
H13B H 0.3453 1.3055 0.0949 0.081 Uiso 1 1 calc R . .
H13C H 0.2960 1.2768 -0.0012 0.081 Uiso 1 1 calc R . .
C15 C 0.0172(3) 0.6690(2) 0.1491(3) 0.0365(10) Uani 1 1 d . . .
H15A H -0.0044 0.6447 0.2057 0.055 Uiso 1 1 calc R . .
H15B H 0.0684 0.6294 0.1174 0.055 Uiso 1 1 calc R . .
H15C H -0.0586 0.6810 0.1138 0.055 Uiso 1 1 calc R . .
C22 C 0.1525(4) 0.0604(3) 0.4095(4) 0.0589(14) Uani 1 1 d . . .
H22 H 0.0842 0.0967 0.3983 0.071 Uiso 1 1 calc R . .
C25 C 0.3543(4) -0.0470(3) 0.4397(3) 0.0514(12) Uani 1 1 d . . .
H25 H 0.4225 -0.0834 0.4510 0.062 Uiso 1 1 calc R . .
C21 C 0.2013(4) 0.0497(3) 0.4966(3) 0.0466(12) Uani 1 1 d . . .
C26 C 0.3066(5) -0.0363(3) 0.3526(3) 0.0581(13) Uani 1 1 d . . .
H26 H 0.3422 -0.0645 0.3048 0.070 Uiso 1 1 calc R . .
C23 C 0.3022(4) -0.0044(3) 0.5089(3) 0.0411(11) Uani 1 1 d . . .
H23 H 0.3364 -0.0125 0.5669 0.049 Uiso 1 1 calc R . .
C20 C 0.1468(5) 0.0953(3) 0.5742(4) 0.0776(17) Uani 1 1 d . . .
H20A H 0.1986 0.1437 0.5902 0.116 Uiso 1 1 calc R . .
H20B H 0.1436 0.0571 0.6246 0.116 Uiso 1 1 calc R . .
H20C H 0.0629 0.1144 0.5577 0.116 Uiso 1 1 calc R . .
C24 C 0.2055(6) 0.0169(4) 0.3391(4) 0.0738(18) Uani 1 1 d . . .
H24 H 0.1714 0.0243 0.2811 0.089 Uiso 1 1 calc R . .
O1 O -0.03807(19) 0.93810(13) 0.04067(15) 0.0223(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.801(2) . ?
Ge1 O1 1.848(2) 3_575 ?
Ge1 N3 1.892(3) . ?
Ge1 N1 1.920(3) . ?
Ge1 N2 1.966(3) . ?
Ge1 Ge1 2.7152(10) 3_575 ?
N1 C1 1.350(4) . ?
N1 C8 1.476(4) . ?
N3 C16 1.381(4) . ?
N3 C17 1.386(4) . ?
N2 C7 1.335(4) . ?
N2 C9 1.476(4) . ?
C3 C4 1.378(5) . ?
C3 C2 1.390(4) . ?
C3 H3 0.9300 . ?
C7 C6 1.420(4) . ?
C7 C1 1.482(4) . ?
C8 C10 1.531(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C1 C2 1.407(4) . ?
C10 C12 1.518(5) . ?
C10 C13 1.525(5) . ?
C10 H10 0.9800 . ?
C18 C16 1.361(5) . ?
C18 C19 1.419(5) . ?
C18 H18 0.9300 . ?
C2 H2 0.9300 . ?
C6 C5 1.381(4) . ?
C6 H6 0.9300 . ?
C19 C17 1.363(5) . ?
C19 H19 0.9300 . ?
C5 C4 1.394(5) . ?
C5 H5 0.9300 . ?
C14 C11 1.514(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 H17 0.9300 . ?
C4 H4 0.9300 . ?
C9 C11 1.535(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C15 1.530(5) . ?
C11 H11 0.9800 . ?
C16 H16 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C22 C24 1.386(7) . ?
C22 C21 1.386(6) . ?
C22 H22 0.9300 . ?
C25 C23 1.362(6) . ?
C25 C26 1.381(6) . ?
C25 H25 0.9300 . ?
C21 C23 1.370(5) . ?
C21 C20 1.492(6) . ?
C26 C24 1.365(7) . ?
C26 H26 0.9300 . ?
C23 H23 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24 0.9300 . ?
O1 Ge1 1.848(2) 3_575 ?

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
O1 Ge1 O1 83.81(10) . 3_575 ?
O1 Ge1 N3 115.24(11) . . ?
O1 Ge1 N3 97.29(11) 3_575 . ?
O1 Ge1 N1 136.46(11) . . ?
O1 Ge1 N1 94.90(10) 3_575 . ?
N3 Ge1 N1 108.11(11) . . ?
O1 Ge1 N2 91.41(10) . . ?
O1 Ge1 N2 167.76(11) 3_575 . ?
N3 Ge1 N2 94.94(11) . . ?
N1 Ge1 N2 80.80(11) . . ?
O1 Ge1 Ge1 42.57(7) . 3_575 ?
O1 Ge1 Ge1 41.25(7) 3_575 3_575 ?
N3 Ge1 Ge1 111.66(8) . 3_575 ?
N1 Ge1 Ge1 122.60(8) . 3_575 ?
N2 Ge1 Ge1 132.94(8) . 3_575 ?
C1 N1 C8 120.0(3) . . ?
C1 N1 Ge1 117.0(2) . . ?
C8 N1 Ge1 121.5(2) . . ?
C16 N3 C17 106.6(3) . . ?
C16 N3 Ge1 127.9(2) . . ?
C17 N3 Ge1 125.5(2) . . ?
C7 N2 C9 122.5(3) . . ?
C7 N2 Ge1 115.9(2) . . ?
C9 N2 Ge1 120.8(2) . . ?
C4 C3 C2 130.5(3) . . ?
C4 C3 H3 114.8 . . ?
C2 C3 H3 114.8 . . ?
N2 C7 C6 122.3(3) . . ?
N2 C7 C1 112.7(3) . . ?
C6 C7 C1 124.9(3) . . ?
N1 C8 C10 116.9(3) . . ?
N1 C8 H8A 108.1 . . ?
C10 C8 H8A 108.1 . . ?
N1 C8 H8B 108.1 . . ?
C10 C8 H8B 108.1 . . ?
H8A C8 H8B 107.3 . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 C7 112.7(3) . . ?
C2 C1 C7 124.9(3) . . ?
C12 C10 C13 111.3(3) . . ?
C12 C10 C8 113.4(3) . . ?
C13 C10 C8 107.8(3) . . ?
C12 C10 H10 108.1 . . ?
C13 C10 H10 108.1 . . ?
C8 C10 H10 108.1 . . ?
C16 C18 C19 106.9(3) . . ?
C16 C18 H18 126.5 . . ?
C19 C18 H18 126.5 . . ?
C3 C2 C1 131.6(3) . . ?
C3 C2 H2 114.2 . . ?
C1 C2 H2 114.2 . . ?
C5 C6 C7 131.8(3) . . ?
C5 C6 H6 114.1 . . ?
C7 C6 H6 114.1 . . ?
C17 C19 C18 107.2(3) . . ?
C17 C19 H19 126.4 . . ?
C18 C19 H19 126.4 . . ?
C6 C5 C4 129.7(3) . . ?
C6 C5 H5 115.2 . . ?
C4 C5 H5 115.2 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C19 C17 N3 109.4(3) . . ?
C19 C17 H17 125.3 . . ?
N3 C17 H17 125.3 . . ?
C3 C4 C5 126.0(3) . . ?
C3 C4 H4 117.0 . . ?
C5 C4 H4 117.0 . . ?
N2 C9 C11 116.7(3) . . ?
N2 C9 H9A 108.1 . . ?
C11 C9 H9A 108.1 . . ?
N2 C9 H9B 108.1 . . ?
C11 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C14 C11 C15 111.3(3) . . ?
C14 C11 C9 112.7(3) . . ?
C15 C11 C9 107.3(3) . . ?
C14 C11 H11 108.5 . . ?
C15 C11 H11 108.5 . . ?
C9 C11 H11 108.5 . . ?
C18 C16 N3 109.9(3) . . ?
C18 C16 H16 125.1 . . ?
N3 C16 H16 125.1 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C24 C22 C21 120.0(4) . . ?
C24 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C25 C26 120.4(4) . . ?
C23 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C23 C21 C22 117.4(5) . . ?
C23 C21 C20 121.0(5) . . ?
C22 C21 C20 121.6(4) . . ?
C24 C26 C25 117.9(5) . . ?
C24 C26 H26 121.1 . . ?
C25 C26 H26 121.1 . . ?
C25 C23 C21 122.6(5) . . ?
C25 C23 H23 118.7 . . ?
C21 C23 H23 118.7 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C24 C22 121.8(5) . . ?
C26 C24 H24 119.1 . . ?
C22 C24 H24 119.1 . . ?
Ge1 O1 Ge1 96.19(10) . 3_575 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ge1 N1 C1 89.7(3) . . . . ?
O1 Ge1 N1 C1 175.9(2) 3_575 . . . ?
N3 Ge1 N1 C1 -84.8(3) . . . . ?
N2 Ge1 N1 C1 7.4(2) . . . . ?
Ge1 Ge1 N1 C1 143.1(2) 3_575 . . . ?
O1 Ge1 N1 C8 -104.2(3) . . . . ?
O1 Ge1 N1 C8 -18.0(2) 3_575 . . . ?
N3 Ge1 N1 C8 81.3(2) . . . . ?
N2 Ge1 N1 C8 173.5(3) . . . . ?
Ge1 Ge1 N1 C8 -50.8(3) 3_575 . . . ?
O1 Ge1 N3 C16 -102.9(3) . . . . ?
O1 Ge1 N3 C16 170.5(3) 3_575 . . . ?
N1 Ge1 N3 C16 72.9(3) . . . . ?
N2 Ge1 N3 C16 -9.0(3) . . . . ?
Ge1 Ge1 N3 C16 -149.3(2) 3_575 . . . ?
O1 Ge1 N3 C17 78.1(3) . . . . ?
O1 Ge1 N3 C17 -8.4(3) 3_575 . . . ?
N1 Ge1 N3 C17 -106.0(3) . . . . ?
N2 Ge1 N3 C17 172.0(3) . . . . ?
Ge1 Ge1 N3 C17 31.7(3) 3_575 . . . ?
O1 Ge1 N2 C7 -145.9(2) . . . . ?
O1 Ge1 N2 C7 -79.2(5) 3_575 . . . ?
N3 Ge1 N2 C7 98.6(2) . . . . ?
N1 Ge1 N2 C7 -9.0(2) . . . . ?
Ge1 Ge1 N2 C7 -135.5(2) 3_575 . . . ?
O1 Ge1 N2 C9 44.0(2) . . . . ?
O1 Ge1 N2 C9 110.7(5) 3_575 . . . ?
N3 Ge1 N2 C9 -71.5(2) . . . . ?
N1 Ge1 N2 C9 -179.1(3) . . . . ?
Ge1 Ge1 N2 C9 54.4(3) 3_575 . . . ?
C9 N2 C7 C6 1.6(5) . . . . ?
Ge1 N2 C7 C6 -168.3(2) . . . . ?
C9 N2 C7 C1 178.6(3) . . . . ?
Ge1 N2 C7 C1 8.7(4) . . . . ?
C1 N1 C8 C10 -81.0(4) . . . . ?
Ge1 N1 C8 C10 113.3(3) . . . . ?
C8 N1 C1 C2 8.1(5) . . . . ?
Ge1 N1 C1 C2 174.4(3) . . . . ?
C8 N1 C1 C7 -171.1(3) . . . . ?
Ge1 N1 C1 C7 -4.8(4) . . . . ?
N2 C7 C1 N1 -2.6(4) . . . . ?
C6 C7 C1 N1 174.3(3) . . . . ?
N2 C7 C1 C2 178.2(3) . . . . ?
C6 C7 C1 C2 -4.9(5) . . . . ?
N1 C8 C10 C12 -64.4(4) . . . . ?
N1 C8 C10 C13 171.9(3) . . . . ?
C4 C3 C2 C1 4.3(7) . . . . ?
N1 C1 C2 C3 177.7(4) . . . . ?
C7 C1 C2 C3 -3.2(6) . . . . ?
N2 C7 C6 C5 -175.0(4) . . . . ?
C1 C7 C6 C5 8.4(6) . . . . ?
C16 C18 C19 C17 0.0(4) . . . . ?
C7 C6 C5 C4 -1.7(7) . . . . ?
C18 C19 C17 N3 -0.5(4) . . . . ?
C16 N3 C17 C19 0.8(4) . . . . ?
Ge1 N3 C17 C19 179.9(2) . . . . ?
C2 C3 C4 C5 2.7(7) . . . . ?
C6 C5 C4 C3 -5.5(7) . . . . ?
C7 N2 C9 C11 72.2(4) . . . . ?
Ge1 N2 C9 C11 -118.4(3) . . . . ?
N2 C9 C11 C14 50.5(4) . . . . ?
N2 C9 C11 C15 173.4(3) . . . . ?
C19 C18 C16 N3 0.5(4) . . . . ?
C17 N3 C16 C18 -0.8(4) . . . . ?
Ge1 N3 C16 C18 -179.9(2) . . . . ?
C24 C22 C21 C23 0.2(6) . . . . ?
C24 C22 C21 C20 -179.9(4) . . . . ?
C23 C25 C26 C24 -0.8(6) . . . . ?
C26 C25 C23 C21 0.4(6) . . . . ?
C22 C21 C23 C25 0.0(6) . . . . ?
C20 C21 C23 C25 -179.9(4) . . . . ?
C25 C26 C24 C22 0.9(7) . . . . ?
C21 C22 C24 C26 -0.6(7) . . . . ?
O1 Ge1 O1 Ge1 0.0 3_575 . . 3_575 ?
N3 Ge1 O1 Ge1 -95.16(12) . . . 3_575 ?
N1 Ge1 O1 Ge1 90.61(15) . . . 3_575 ?
N2 Ge1 O1 Ge1 168.70(11) . . . 3_575 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_Compound_18__msh32_1_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1851012'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H28 B F15 Ge N2 O, C H2 Cl2'
_chemical_formula_sum            'C40 H30 B Cl2 F15 Ge N2 O'
_chemical_formula_weight         993.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.501(3)
_cell_length_b                   12.739(3)
_cell_length_c                   15.229(4)
_cell_angle_alpha                97.161(8)
_cell_angle_beta                 106.180(8)
_cell_angle_gamma                115.904(7)
_cell_volume                     2008.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9799
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      26.74

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             996.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    1.002
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60329
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_av_R_equivalents  0.1897
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.915
_diffrn_reflns_theta_max         26.776
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8483
_reflns_number_gt                7594
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0572P)²+5.3225P] 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         8483
_refine_ls_number_parameters     563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1187
_refine_ls_wR_factor_gt          0.1120
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_restrained_S_all      0.824
_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 0.57132(2) 0.42624(2) 0.72605(2) 0.01272(8) Uani 1 1 d . . . . .
Cl2 Cl 0.80930(9) 0.93737(9) 0.91923(7) 0.0445(2) Uani 1 1 d . . . . .
Cl1 Cl 0.85664(14) 1.00327(10) 0.75292(8) 0.0671(3) Uani 1 1 d . . . . .
F1 F 0.88381(14) 0.35937(13) 0.89307(10) 0.0168(3) Uani 1 1 d . . . . .
F11 F 0.99225(14) 0.35394(14) 0.74919(10) 0.0192(3) Uani 1 1 d . . . . .
F5 F 0.52364(14) 0.13229(14) 0.60302(10) 0.0203(3) Uani 1 1 d . . . . .
F15 F 0.83583(14) 0.63232(13) 0.76660(11) 0.0196(3) Uani 1 1 d . . . . .
F6 F 0.76267(16) 0.13171(14) 0.60905(11) 0.0216(3) Uani 1 1 d . . . . .
F14 F 1.07232(15) 0.81419(13) 0.83916(12) 0.0234(3) Uani 1 1 d . . . . .
F2 F 0.78411(15) 0.18354(15) 0.96982(10) 0.0221(3) Uani 1 1 d . . . . .
F4 F 0.42365(15) -0.04053(14) 0.68450(12) 0.0236(3) Uani 1 1 d . . . . .
F3 F 0.55252(16) -0.01904(14) 0.86801(12) 0.0252(3) Uani 1 1 d . . . . .
F10 F 0.79604(16) 0.50182(14) 0.55274(11) 0.0235(3) Uani 1 1 d . . . . .
F7 F 0.81972(16) 0.08947(15) 0.45829(12) 0.0264(4) Uani 1 1 d . . . . .
F9 F 0.85237(17) 0.45517(16) 0.40128(12) 0.0303(4) Uani 1 1 d . . . . .
F13 F 1.27459(15) 0.77460(15) 0.86310(12) 0.0266(4) Uani 1 1 d . . . . .
F12 F 1.23200(15) 0.54173(16) 0.82118(11) 0.0246(3) Uani 1 1 d . . . . .
F8 F 0.86347(17) 0.24753(18) 0.35133(11) 0.0311(4) Uani 1 1 d . . . . .
O1 O 0.65640(16) 0.40012(15) 0.66309(12) 0.0142(3) Uani 1 1 d . . . . .
N1 N 0.6147(2) 0.41882(19) 0.85181(14) 0.0148(4) Uani 1 1 d . . . . .
N2 N 0.4168(2) 0.28614(19) 0.70047(15) 0.0148(4) Uani 1 1 d . . . . .
C26 C 0.5390(2) 0.0577(2) 0.73454(18) 0.0162(5) Uani 1 1 d . . . . .
C1 C 0.5272(2) 0.3156(2) 0.86263(18) 0.0149(5) Uani 1 1 d . . . . .
C25 C 0.6042(2) 0.0683(2) 0.82748(19) 0.0176(5) Uani 1 1 d . . . . .
C27 C 0.5926(2) 0.1499(2) 0.69455(17) 0.0156(5) Uani 1 1 d . . . . .
C34 C 0.9000(2) 0.4812(2) 0.75118(16) 0.0144(5) Uani 1 1 d . . . . .
C16 C 0.5448(2) 0.5582(2) 0.70071(17) 0.0144(5) Uani 1 1 d . . . . .
C24 C 0.7206(2) 0.1704(2) 0.87821(17) 0.0161(5) Uani 1 1 d . . . . .
C8 C 0.7431(2) 0.5058(2) 0.92400(17) 0.0156(5) Uani 1 1 d . . . . .
H8A H 0.8078 0.5171 0.8952 0.019 Uiso 1 1 calc R U . . .
H8B H 0.7603 0.4709 0.9773 0.019 Uiso 1 1 calc R U . . .
C23 C 0.7709(2) 0.2612(2) 0.83584(17) 0.0141(5) Uani 1 1 d . . . . .
C39 C 0.9293(2) 0.6018(2) 0.77760(17) 0.0152(5) Uani 1 1 d . . . . .
C31 C 0.8352(3) 0.2714(3) 0.42786(18) 0.0214(5) Uani 1 1 d . . . . .
C9 C 0.7584(2) 0.6300(2) 0.96360(18) 0.0177(5) Uani 1 1 d . . . . .
H9 H 0.7320 0.6604 0.9086 0.021 Uiso 1 1 calc R U . . .
C12 C 0.3205(2) 0.2264(2) 0.60284(18) 0.0195(5) Uani 1 1 d . . . . .
H12A H 0.2698 0.1383 0.5952 0.023 Uiso 1 1 calc R U . . .
H12B H 0.3652 0.2356 0.5575 0.023 Uiso 1 1 calc R U . . .
C3 C 0.4749(3) 0.1870(3) 0.97608(19) 0.0218(5) Uani 1 1 d . . . . .
H3 H 0.5105 0.1902 1.0409 0.026 Uiso 1 1 calc R U . . .
C32 C 0.8282(3) 0.3748(3) 0.45295(18) 0.0211(5) Uani 1 1 d . . . . .
C22 C 0.7102(2) 0.2554(2) 0.74222(17) 0.0135(4) Uani 1 1 d . . . . .
C38 C 1.0524(2) 0.6994(2) 0.81597(18) 0.0177(5) Uani 1 1 d . . . . .
C33 C 0.7974(2) 0.3964(2) 0.53149(18) 0.0174(5) Uani 1 1 d . . . . .
C28 C 0.7720(2) 0.3178(2) 0.58859(17) 0.0144(5) Uani 1 1 d . . . . .
C2 C 0.5468(3) 0.2890(2) 0.95030(18) 0.0186(5) Uani 1 1 d . . . . .
H2 H 0.6222 0.3511 1.0012 0.022 Uiso 1 1 calc R U . . .
C35 C 1.0080(2) 0.4674(2) 0.76995(17) 0.0157(5) Uani 1 1 d . . . . .
C30 C 0.8120(2) 0.1905(2) 0.48197(18) 0.0187(5) Uani 1 1 d . . . . .
C37 C 1.1547(2) 0.6800(2) 0.83016(18) 0.0190(5) Uani 1 1 d . . . . .
C7 C 0.4133(2) 0.2389(2) 0.77484(17) 0.0153(5) Uani 1 1 d . . . . .
C29 C 0.7814(2) 0.2155(2) 0.55988(17) 0.0166(5) Uani 1 1 d . . . . .
C36 C 1.1318(2) 0.5622(2) 0.80720(17) 0.0179(5) Uani 1 1 d . . . . .
C17 C 0.4883(3) 0.6030(3) 0.7502(2) 0.0229(6) Uani 1 1 d . . . . .
H17 H 0.4669 0.5711 0.7998 0.027 Uiso 1 1 calc R U . . .
C4 C 0.3607(3) 0.0827(3) 0.9224(2) 0.0261(6) Uani 1 1 d . . . . .
H4 H 0.3291 0.0217 0.9531 0.031 Uiso 1 1 calc R U . . .
C10 C 0.6747(3) 0.6224(3) 1.0207(2) 0.0294(6) Uani 1 1 d . . . . .
H10A H 0.7012 0.5955 1.0764 0.044 Uiso 1 1 calc R U . . .
H10B H 0.5849 0.5640 0.9807 0.044 Uiso 1 1 calc R U . . .
H10C H 0.6839 0.7028 1.0420 0.044 Uiso 1 1 calc R U . . .
C18 C 0.4630(3) 0.6944(3) 0.7275(2) 0.0235(6) Uani 1 1 d . . . . .
H18 H 0.4256 0.7257 0.7620 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2878(3) 0.0587(3) 0.8281(2) 0.0310(7) Uani 1 1 d . . . . .
H5 H 0.2104 -0.0172 0.8024 0.037 Uiso 1 1 calc R U . . .
C21 C 0.5748(3) 0.6041(3) 0.6275(2) 0.0303(7) Uani 1 1 d . . . . .
H21 H 0.6141 0.5747 0.5936 0.036 Uiso 1 1 calc R U . . .
C11 C 0.8990(3) 0.7192(3) 1.0242(2) 0.0256(6) Uani 1 1 d . . . . .
H11A H 0.9094 0.7994 1.0485 0.038 Uiso 1 1 calc R U . . .
H11B H 0.9508 0.7256 0.9851 0.038 Uiso 1 1 calc R U . . .
H11C H 0.9273 0.6901 1.0779 0.038 Uiso 1 1 calc R U . . .
C6 C 0.3094(3) 0.1273(3) 0.7651(2) 0.0259(6) Uani 1 1 d . . . . .
H6 H 0.2417 0.0926 0.7043 0.031 Uiso 1 1 calc R U . . .
C19 C 0.4926(3) 0.7389(3) 0.6548(2) 0.0282(6) Uani 1 1 d . . . . .
H19 H 0.4756 0.8014 0.6390 0.034 Uiso 1 1 calc R U . . .
C13 C 0.2280(3) 0.2776(3) 0.5767(2) 0.0335(7) Uani 1 1 d . . . . .
H13 H 0.2802 0.3663 0.5838 0.040 Uiso 1 1 calc R U . . .
B1 B 0.7556(3) 0.3633(2) 0.68842(19) 0.0128(5) Uani 1 1 d . . . . .
C15 C 0.1404(3) 0.2140(4) 0.4719(2) 0.0433(8) Uani 1 1 d . . . . .
H15A H 0.0906 0.1263 0.4628 0.065 Uiso 1 1 calc R U . . .
H15B H 0.1924 0.2285 0.4324 0.065 Uiso 1 1 calc R U . . .
H15C H 0.0819 0.2463 0.4533 0.065 Uiso 1 1 calc R U . . .
C20 C 0.5467(4) 0.6933(4) 0.6046(3) 0.0464(10) Uani 1 1 d . . . . .
H20 H 0.5650 0.7236 0.5536 0.056 Uiso 1 1 calc R U . . .
C40 C 0.8524(5) 0.9039(4) 0.8246(3) 0.0601(12) Uani 1 1 d . . . . .
H40A H 0.7901 0.8190 0.7851 0.072 Uiso 1 1 calc R U . . .
H40B H 0.9379 0.9107 0.8500 0.072 Uiso 1 1 calc R U . . .
C14 C 0.1523(4) 0.2648(4) 0.6391(3) 0.0524(11) Uani 1 1 d . . . . .
H14A H 0.0983 0.3018 0.6208 0.079 Uiso 1 1 calc R U . . .
H14B H 0.2109 0.3058 0.7058 0.079 Uiso 1 1 calc R U . . .
H14C H 0.0979 0.1783 0.6315 0.079 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 O1 1.7201(17) . ?
Ge1 N2 1.861(2) . ?
Ge1 N1 1.866(2) . ?
Ge1 C16 1.914(2) . ?
Cl2 C40 1.740(4) . ?
Cl1 C40 1.765(4) . ?
F1 C23 1.348(3) . ?
F11 C35 1.353(3) . ?
F5 C27 1.349(3) . ?
F15 C39 1.360(3) . ?
F6 C29 1.354(3) . ?
F14 C38 1.352(3) . ?
F2 C24 1.347(3) . ?
F4 C26 1.341(3) . ?
F3 C25 1.342(3) . ?
F10 C33 1.351(3) . ?
F7 C30 1.345(3) . ?
F9 C32 1.350(3) . ?
F13 C37 1.342(3) . ?
F12 C36 1.353(3) . ?
F8 C31 1.345(3) . ?
O1 B1 1.481(3) . ?
N1 C1 1.361(3) . ?
N1 C8 1.474(3) . ?
N2 C7 1.349(3) . ?
N2 C12 1.469(3) . ?
C26 C25 1.378(4) . ?
C26 C27 1.385(3) . ?
C1 C2 1.400(3) . ?
C1 C7 1.472(4) . ?
C25 C24 1.369(4) . ?
C27 C22 1.389(4) . ?
C34 C39 1.388(3) . ?
C34 C35 1.393(3) . ?
C34 B1 1.656(4) . ?
C16 C21 1.389(3) . ?
C16 C17 1.391(4) . ?
C24 C23 1.388(3) . ?
C8 C9 1.528(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C23 C22 1.391(3) . ?
C39 C38 1.380(4) . ?
C31 C32 1.372(4) . ?
C31 C30 1.381(4) . ?
C9 C10 1.516(4) . ?
C9 C11 1.524(4) . ?
C9 H9 1.0000 . ?
C12 C13 1.545(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C3 C4 1.376(4) . ?
C3 C2 1.398(4) . ?
C3 H3 0.9500 . ?
C32 C33 1.386(4) . ?
C22 B1 1.656(3) . ?
C38 C37 1.370(4) . ?
C33 C28 1.397(3) . ?
C28 C29 1.387(4) . ?
C28 B1 1.658(3) . ?
C2 H2 0.9500 . ?
C35 C36 1.372(4) . ?
C30 C29 1.386(3) . ?
C37 C36 1.377(4) . ?
C7 C6 1.400(4) . ?
C17 C18 1.390(4) . ?
C17 H17 0.9500 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C18 C19 1.373(4) . ?
C18 H18 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C21 C20 1.383(4) . ?
C21 H21 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C6 H6 0.9500 . ?
C19 C20 1.379(4) . ?
C19 H19 0.9500 . ?
C13 C14 1.493(5) . ?
C13 C15 1.527(5) . ?
C13 H13 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C20 H20 0.9500 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
O1 Ge1 N2 111.42(9) . . ?
O1 Ge1 N1 117.05(8) . . ?
N2 Ge1 N1 86.21(9) . . ?
O1 Ge1 C16 110.66(9) . . ?
N2 Ge1 C16 111.34(10) . . ?
N1 Ge1 C16 117.70(10) . . ?
B1 O1 Ge1 131.26(14) . . ?
C1 N1 C8 125.4(2) . . ?
C1 N1 Ge1 112.91(17) . . ?
C8 N1 Ge1 120.62(15) . . ?
C7 N2 C12 125.4(2) . . ?
C7 N2 Ge1 113.51(17) . . ?
C12 N2 Ge1 120.37(16) . . ?
F4 C26 C25 119.7(2) . . ?
F4 C26 C27 120.8(2) . . ?
C25 C26 C27 119.4(2) . . ?
N1 C1 C2 121.6(2) . . ?
N1 C1 C7 113.4(2) . . ?
C2 C1 C7 125.0(2) . . ?
F3 C25 C24 120.8(2) . . ?
F3 C25 C26 120.2(2) . . ?
C24 C25 C26 119.0(2) . . ?
F5 C27 C26 115.9(2) . . ?
F5 C27 C22 119.8(2) . . ?
C26 C27 C22 124.3(2) . . ?
C39 C34 C35 113.3(2) . . ?
C39 C34 B1 125.8(2) . . ?
C35 C34 B1 120.3(2) . . ?
C21 C16 C17 119.7(2) . . ?
C21 C16 Ge1 119.22(19) . . ?
C17 C16 Ge1 120.93(18) . . ?
F2 C24 C25 119.7(2) . . ?
F2 C24 C23 120.3(2) . . ?
C25 C24 C23 120.0(2) . . ?
N1 C8 C9 113.4(2) . . ?
N1 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
N1 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
F1 C23 C24 115.0(2) . . ?
F1 C23 C22 121.2(2) . . ?
C24 C23 C22 123.8(2) . . ?
F15 C39 C38 114.5(2) . . ?
F15 C39 C34 121.5(2) . . ?
C38 C39 C34 124.0(2) . . ?
F8 C31 C32 121.0(2) . . ?
F8 C31 C30 119.8(3) . . ?
C32 C31 C30 119.2(2) . . ?
C10 C9 C11 110.8(2) . . ?
C10 C9 C8 112.0(2) . . ?
C11 C9 C8 109.3(2) . . ?
C10 C9 H9 108.2 . . ?
C11 C9 H9 108.2 . . ?
C8 C9 H9 108.2 . . ?
N2 C12 C13 113.8(2) . . ?
N2 C12 H12A 108.8 . . ?
C13 C12 H12A 108.8 . . ?
N2 C12 H12B 108.8 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
C4 C3 C2 130.2(3) . . ?
C4 C3 H3 114.9 . . ?
C2 C3 H3 114.9 . . ?
F9 C32 C31 119.6(2) . . ?
F9 C32 C33 120.5(2) . . ?
C31 C32 C33 119.8(2) . . ?
C27 C22 C23 113.6(2) . . ?
C27 C22 B1 118.7(2) . . ?
C23 C22 B1 127.4(2) . . ?
F14 C38 C37 120.0(2) . . ?
F14 C38 C39 120.1(2) . . ?
C37 C38 C39 119.9(2) . . ?
F10 C33 C32 116.0(2) . . ?
F10 C33 C28 120.3(2) . . ?
C32 C33 C28 123.7(2) . . ?
C29 C28 C33 113.7(2) . . ?
C29 C28 B1 127.1(2) . . ?
C33 C28 B1 118.7(2) . . ?
C3 C2 C1 131.3(3) . . ?
C3 C2 H2 114.4 . . ?
C1 C2 H2 114.4 . . ?
F11 C35 C36 116.6(2) . . ?
F11 C35 C34 119.1(2) . . ?
C36 C35 C34 124.4(2) . . ?
F7 C30 C31 119.5(2) . . ?
F7 C30 C29 121.3(2) . . ?
C31 C30 C29 119.2(2) . . ?
F13 C37 C38 120.4(2) . . ?
F13 C37 C36 120.8(2) . . ?
C38 C37 C36 118.8(2) . . ?
N2 C7 C6 121.0(2) . . ?
N2 C7 C1 113.4(2) . . ?
C6 C7 C1 125.6(2) . . ?
F6 C29 C30 114.5(2) . . ?
F6 C29 C28 121.1(2) . . ?
C30 C29 C28 124.4(2) . . ?
F12 C36 C35 121.0(2) . . ?
F12 C36 C37 119.4(2) . . ?
C35 C36 C37 119.6(2) . . ?
C18 C17 C16 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C3 C4 C5 125.9(2) . . ?
C3 C4 H4 117.1 . . ?
C5 C4 H4 117.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C4 C5 C6 130.4(3) . . ?
C4 C5 H5 114.8 . . ?
C6 C5 H5 114.8 . . ?
C20 C21 C16 119.2(3) . . ?
C20 C21 H21 120.4 . . ?
C16 C21 H21 120.4 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5 C6 C7 131.4(3) . . ?
C5 C6 H6 114.3 . . ?
C7 C6 H6 114.3 . . ?
C18 C19 C20 120.2(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C14 C13 C15 111.3(3) . . ?
C14 C13 C12 113.3(3) . . ?
C15 C13 C12 108.0(3) . . ?
C14 C13 H13 108.0 . . ?
C15 C13 H13 108.0 . . ?
C12 C13 H13 108.0 . . ?
O1 B1 C34 112.0(2) . . ?
O1 B1 C28 107.49(19) . . ?
C34 B1 C28 101.89(18) . . ?
O1 B1 C22 108.51(18) . . ?
C34 B1 C22 113.69(19) . . ?
C28 B1 C22 113.07(19) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C20 C21 121.0(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
Cl2 C40 Cl1 111.6(2) . . ?
Cl2 C40 H40A 109.3 . . ?
Cl1 C40 H40A 109.3 . . ?
Cl2 C40 H40B 109.3 . . ?
Cl1 C40 H40B 109.3 . . ?
H40A C40 H40B 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_refine_diff_density_max         1.558
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_Compound_17__msh73_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1851011'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;
_audit_creation_date             2017-10-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C41 H28 B F15 Ge N2 O, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C42 H30 B Cl F15 Ge N2 O'
_chemical_formula_weight         982.55
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7566(13)
_cell_length_b                   13.7449(15)
_cell_length_c                   13.7689(15)
_cell_angle_alpha                65.642(3)
_cell_angle_beta                 74.276(3)
_cell_angle_gamma                74.609(3)
_cell_volume                     1920.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             986.0
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   0.822
_exptl_transmission_factor_min   0.763
_diffrn_reflns_av_R_equivalents  0.1800
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.679
_diffrn_reflns_theta_min         1.828
_diffrn_ambient_temperature      104.33
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6794
_reflns_number_total             8074
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.889
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8074
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+3.1313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1307
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C8(H8A,H8B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C2(H2), C4(H4), C19(H19), C20(H20), C23(H23),
 C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,
 H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.37917(3) 0.70330(2) 0.71885(2) 0.01373(10) Uani 1 1 d . . . . .
F5 F -0.06674(16) 0.57226(14) 0.76526(15) 0.0216(4) Uani 1 1 d . . . . .
F15 F 0.09865(17) 0.88282(14) 0.56189(14) 0.0219(4) Uani 1 1 d . . . . .
F6 F -0.00151(16) 0.71340(15) 0.55058(14) 0.0216(4) Uani 1 1 d . . . . .
F1 F 0.34861(16) 0.44488(15) 0.67213(15) 0.0242(4) Uani 1 1 d . . . . .
F2 F 0.30423(18) 0.24452(15) 0.74654(16) 0.0278(4) Uani 1 1 d . . . . .
F11 F 0.05299(17) 0.59167(15) 0.90218(14) 0.0243(4) Uani 1 1 d . . . . .
F3 F 0.07621(18) 0.20504(15) 0.82936(15) 0.0259(4) Uani 1 1 d . . . . .
F10 F 0.42165(16) 0.65185(15) 0.51505(14) 0.0224(4) Uani 1 1 d . . . . .
F4 F -0.10794(17) 0.37292(16) 0.83248(16) 0.0269(4) Uani 1 1 d . . . . .
F7 F 0.02323(18) 0.77240(17) 0.33759(15) 0.0302(5) Uani 1 1 d . . . . .
F9 F 0.44239(18) 0.71502(18) 0.30239(15) 0.0316(5) Uani 1 1 d . . . . .
F12 F -0.09978(19) 0.72854(19) 0.98815(15) 0.0365(5) Uani 1 1 d . . . . .
O1 O 0.29091(18) 0.61861(16) 0.72693(16) 0.0150(4) Uani 1 1 d . . . . .
F8 F 0.2469(2) 0.77411(18) 0.20942(15) 0.0349(5) Uani 1 1 d . . . . .
Cl1 Cl 0.4152(2) 0.09160(15) 0.94563(18) 0.1164(8) Uani 1 1 d . . . . .
F14 F -0.0408(2) 1.01768(16) 0.65410(18) 0.0354(5) Uani 1 1 d . . . . .
F13 F -0.1447(2) 0.94420(19) 0.86713(18) 0.0394(6) Uani 1 1 d . . . . .
N2 N 0.5297(2) 0.6266(2) 0.74425(19) 0.0146(5) Uani 1 1 d . . . . .
C7 C 0.5528(3) 0.6190(2) 0.8391(2) 0.0138(6) Uani 1 1 d . . . . .
C25 C 0.2338(3) 0.4318(2) 0.7141(2) 0.0165(6) Uani 1 1 d . . . . .
N1 N 0.3597(2) 0.7272(2) 0.8464(2) 0.0165(5) Uani 1 1 d . . . . .
C12 C 0.6123(3) 0.5664(2) 0.6775(2) 0.0157(6) Uani 1 1 d . . . . .
H12A H 0.5663 0.5572 0.6322 0.019 Uiso 1 1 calc R . . . .
H12B H 0.6437 0.4932 0.7263 0.019 Uiso 1 1 calc R . . . .
C26 C 0.2127(3) 0.3267(3) 0.7502(2) 0.0201(6) Uani 1 1 d . . . . .
C29 C 0.0308(3) 0.4949(2) 0.7578(2) 0.0167(6) Uani 1 1 d . . . . .
C32 C 0.1214(3) 0.7441(3) 0.3820(3) 0.0211(7) Uani 1 1 d . . . . .
C36 C 0.0824(3) 0.7280(2) 0.7257(2) 0.0156(6) Uani 1 1 d . . . . .
C24 C 0.1449(3) 0.5199(2) 0.7196(2) 0.0156(6) Uani 1 1 d . . . . .
C1 C 0.4541(3) 0.6768(2) 0.8978(2) 0.0145(6) Uani 1 1 d . . . . .
C31 C 0.1113(3) 0.7130(2) 0.4922(2) 0.0165(6) Uani 1 1 d . . . . .
C14 C 0.8108(3) 0.5412(3) 0.5585(3) 0.0260(7) Uani 1 1 d . . . . .
H14A H 0.8402 0.4782 0.6187 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.8783 0.5763 0.5096 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.7731 0.5176 0.5186 0.039 Uiso 1 1 calc GR . . . .
C30 C 0.2077(3) 0.6818(2) 0.5452(2) 0.0144(6) Uani 1 1 d . . . . .
C16 C 0.3725(3) 0.8313(3) 0.5983(3) 0.0201(6) Uani 1 1 d . . . . .
C13 C 0.7188(3) 0.6216(3) 0.6031(2) 0.0191(6) Uani 1 1 d . . . . .
H13 H 0.7573 0.6411 0.6476 0.023 Uiso 1 1 calc R . . . .
C6 C 0.6604(3) 0.5610(3) 0.8731(2) 0.0185(6) Uani 1 1 d . . . . .
H6 H 0.7134 0.5275 0.8257 0.022 Uiso 1 1 calc R . . . .
C9 C 0.2551(3) 0.8963(3) 0.8868(3) 0.0236(7) Uani 1 1 d . . . . .
H9 H 0.3279 0.8900 0.9147 0.028 Uiso 1 1 calc R . . . .
C35 C 0.3182(3) 0.6830(2) 0.4762(2) 0.0179(6) Uani 1 1 d . . . . .
C41 C 0.0546(3) 0.8385(3) 0.6690(2) 0.0186(6) Uani 1 1 d . . . . .
C5 C 0.7042(3) 0.5433(3) 0.9645(2) 0.0206(6) Uani 1 1 d . . . . .
H5 H 0.7823 0.5009 0.9687 0.025 Uiso 1 1 calc R . . . .
C27 C 0.0981(3) 0.3064(2) 0.7903(2) 0.0196(6) Uani 1 1 d . . . . .
C3 C 0.5377(3) 0.6377(3) 1.0649(2) 0.0224(7) Uani 1 1 d . . . . .
H3 H 0.5147 0.6521 1.1300 0.027 Uiso 1 1 calc R . . . .
C2 C 0.4522(3) 0.6797(3) 0.9987(2) 0.0195(6) Uani 1 1 d . . . . .
H2 H 0.3793 0.7172 1.0270 0.023 Uiso 1 1 calc R . . . .
C34 C 0.3330(3) 0.7144(3) 0.3646(2) 0.0213(7) Uani 1 1 d . . . . .
C28 C 0.0052(3) 0.3914(3) 0.7928(2) 0.0191(6) Uani 1 1 d . . . . .
C37 C 0.0284(3) 0.6961(3) 0.8354(2) 0.0187(6) Uani 1 1 d . . . . .
C17 C 0.3602(3) 0.9064(3) 0.5151(3) 0.0209(6) Uani 1 1 d . . . . .
C33 C 0.2335(3) 0.7454(3) 0.3175(2) 0.0228(7) Uani 1 1 d . . . . .
C8 C 0.2490(3) 0.7846(3) 0.8925(3) 0.0198(6) Uani 1 1 d . . . . .
H8A H 0.2255 0.7388 0.9696 0.024 Uiso 1 1 calc R . . . .
H8B H 0.1848 0.7928 0.8544 0.024 Uiso 1 1 calc R . . . .
C4 C 0.6515(3) 0.5780(3) 1.0498(2) 0.0232(7) Uani 1 1 d . . . . .
H4 H 0.6980 0.5589 1.1037 0.028 Uiso 1 1 calc R . . . .
C38 C -0.0484(3) 0.7663(3) 0.8824(3) 0.0244(7) Uani 1 1 d . . . . .
C18 C 0.3471(3) 0.9938(3) 0.4132(3) 0.0228(7) Uani 1 1 d . . . . .
C40 C -0.0192(3) 0.9120(3) 0.7145(3) 0.0241(7) Uani 1 1 d . . . . .
B1 B 0.1836(3) 0.6400(3) 0.6787(3) 0.0144(6) Uani 1 1 d . . . . .
C39 C -0.0715(3) 0.8748(3) 0.8222(3) 0.0269(8) Uani 1 1 d . . . . .
C11 C 0.2649(3) 0.9786(3) 0.7713(3) 0.0309(8) Uani 1 1 d . . . . .
H11A H 0.3345 0.9518 0.7251 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.2745 1.0477 0.7701 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.1919 0.9892 0.7441 0.046 Uiso 1 1 calc GR . . . .
C10 C 0.1446(3) 0.9322(3) 0.9605(3) 0.0314(8) Uani 1 1 d . . . . .
H10A H 0.0722 0.9386 0.9344 0.047 Uiso 1 1 calc GR . . . .
H10B H 0.1489 1.0027 0.9600 0.047 Uiso 1 1 calc GR . . . .
H10C H 0.1415 0.8785 1.0346 0.047 Uiso 1 1 calc GR . . . .
C15 C 0.6793(3) 0.7247(3) 0.5118(3) 0.0255(7) Uani 1 1 d . . . . .
H15A H 0.6421 0.7071 0.4668 0.038 Uiso 1 1 calc GR . . . .
H15B H 0.7492 0.7584 0.4672 0.038 Uiso 1 1 calc GR . . . .
H15C H 0.6210 0.7752 0.5423 0.038 Uiso 1 1 calc GR . . . .
C19 C 0.2577(3) 1.0838(3) 0.4067(3) 0.0275(7) Uani 1 1 d . . . . .
H19 H 0.2037 1.0889 0.4704 0.033 Uiso 1 1 calc R . . . .
C20 C 0.2470(4) 1.1668(3) 0.3066(3) 0.0320(8) Uani 1 1 d . . . . .
H20 H 0.1860 1.2290 0.3020 0.038 Uiso 1 1 calc R . . . .
C23 C 0.4242(4) 0.9856(4) 0.3200(3) 0.0469(11) Uani 1 1 d . . . . .
H23 H 0.4848 0.9233 0.3238 0.056 Uiso 1 1 calc R . . . .
C21 C 0.3238(4) 1.1588(3) 0.2154(3) 0.0398(10) Uani 1 1 d . . . . .
H21 H 0.3161 1.2157 0.1474 0.048 Uiso 1 1 calc R . . . .
C22 C 0.4121(4) 1.0698(4) 0.2206(3) 0.0605(15) Uani 1 1 d . . . . .
H22 H 0.4652 1.0653 0.1563 0.073 Uiso 1 1 calc R . . . .
C42 C 0.5773(9) 0.0540(10) 0.9343(6) 0.162(5) Uani 1 1 d . . . . .
H42A H 0.6118 0.1047 0.9478 0.194 Uiso 1 1 calc R . . . .
H42B H 0.6175 0.0489 0.8630 0.194 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.708(2) . ?
Ge1 N2 1.845(2) . ?
Ge1 N1 1.860(2) . ?
Ge1 C16 1.856(3) . ?
F5 C29 1.355(3) . ?
F15 C41 1.352(3) . ?
F6 C31 1.352(3) . ?
F1 C25 1.345(3) . ?
F2 C26 1.345(4) . ?
F11 C37 1.350(4) . ?
F3 C27 1.340(3) . ?
F10 C35 1.355(4) . ?
F4 C28 1.343(4) . ?
F7 C32 1.343(4) . ?
F9 C34 1.338(4) . ?
F12 C38 1.349(4) . ?
O1 B1 1.489(4) . ?
F8 C33 1.347(3) . ?
Cl1 C42 2.000(11) 2_657 ?
Cl1 C42 1.818(10) . ?
F14 C40 1.338(4) . ?
F13 C39 1.341(4) . ?
N2 C7 1.362(3) . ?
N2 C12 1.479(3) . ?
C7 C1 1.471(4) . ?
C7 C6 1.390(4) . ?
C25 C26 1.387(4) . ?
C25 C24 1.387(4) . ?
N1 C1 1.351(4) . ?
N1 C8 1.462(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.537(4) . ?
C26 C27 1.366(4) . ?
C29 C24 1.380(4) . ?
C29 C28 1.390(4) . ?
C32 C31 1.376(4) . ?
C32 C33 1.375(5) . ?
C36 C41 1.385(4) . ?
C36 C37 1.400(4) . ?
C36 B1 1.662(4) . ?
C24 B1 1.656(4) . ?
C1 C2 1.401(4) . ?
C31 C30 1.391(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 C13 1.528(4) . ?
C30 C35 1.385(4) . ?
C30 B1 1.649(4) . ?
C16 C17 1.197(5) . ?
C13 H13 1.0000 . ?
C13 C15 1.517(5) . ?
C6 H6 0.9500 . ?
C6 C5 1.393(4) . ?
C9 H9 1.0000 . ?
C9 C8 1.525(4) . ?
C9 C11 1.519(5) . ?
C9 C10 1.524(4) . ?
C35 C34 1.388(4) . ?
C41 C40 1.389(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.378(4) . ?
C27 C28 1.376(4) . ?
C3 H3 0.9500 . ?
C3 C2 1.388(5) . ?
C3 C4 1.383(5) . ?
C2 H2 0.9500 . ?
C34 C33 1.374(5) . ?
C37 C38 1.379(4) . ?
C17 C18 1.438(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C4 H4 0.9500 . ?
C38 C39 1.368(5) . ?
C18 C19 1.382(5) . ?
C18 C23 1.384(5) . ?
C40 C39 1.373(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.392(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.360(6) . ?
C23 H23 0.9500 . ?
C23 C22 1.395(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.369(6) . ?
C22 H22 0.9500 . ?
C42 Cl1 2.000(11) 2_657 ?
C42 H42A 0.9900 . ?
C42 H42B 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
O1 Ge1 N2 110.17(10) . . ?
O1 Ge1 N1 114.10(10) . . ?
O1 Ge1 C16 113.63(12) . . ?
N2 Ge1 N1 86.91(10) . . ?
N2 Ge1 C16 116.98(12) . . ?
C16 Ge1 N1 112.42(12) . . ?
B1 O1 Ge1 131.46(19) . . ?
C42 Cl1 C42 81.3(4) . 2_657 ?
C7 N2 Ge1 113.23(18) . . ?
C7 N2 C12 121.9(2) . . ?
C12 N2 Ge1 124.37(18) . . ?
N2 C7 C1 113.2(3) . . ?
N2 C7 C6 121.2(2) . . ?
C6 C7 C1 125.6(3) . . ?
F1 C25 C26 115.7(3) . . ?
F1 C25 C24 120.4(3) . . ?
C26 C25 C24 123.9(3) . . ?
C1 N1 Ge1 112.92(18) . . ?
C1 N1 C8 123.1(2) . . ?
C8 N1 Ge1 123.7(2) . . ?
N2 C12 H12A 108.7 . . ?
N2 C12 H12B 108.7 . . ?
N2 C12 C13 114.2(2) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
F2 C26 C25 120.6(3) . . ?
F2 C26 C27 119.7(3) . . ?
C27 C26 C25 119.8(3) . . ?
F5 C29 C24 121.2(3) . . ?
F5 C29 C28 114.3(3) . . ?
C24 C29 C28 124.4(3) . . ?
F7 C32 C31 120.6(3) . . ?
F7 C32 C33 120.2(3) . . ?
C33 C32 C31 119.2(3) . . ?
C41 C36 C37 113.3(3) . . ?
C41 C36 B1 125.8(3) . . ?
C37 C36 B1 120.3(3) . . ?
C25 C24 B1 118.9(3) . . ?
C29 C24 C25 113.5(3) . . ?
C29 C24 B1 127.5(3) . . ?
N1 C1 C7 113.6(2) . . ?
N1 C1 C2 121.0(3) . . ?
C2 C1 C7 125.3(3) . . ?
F6 C31 C32 116.0(3) . . ?
F6 C31 C30 119.4(2) . . ?
C32 C31 C30 124.6(3) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C31 C30 B1 119.7(3) . . ?
C35 C30 C31 113.4(3) . . ?
C35 C30 B1 126.7(3) . . ?
C17 C16 Ge1 170.3(3) . . ?
C12 C13 H13 108.3 . . ?
C14 C13 C12 108.9(3) . . ?
C14 C13 H13 108.3 . . ?
C15 C13 C12 111.8(3) . . ?
C15 C13 C14 111.0(3) . . ?
C15 C13 H13 108.3 . . ?
C7 C6 H6 114.3 . . ?
C7 C6 C5 131.4(3) . . ?
C5 C6 H6 114.3 . . ?
C8 C9 H9 108.4 . . ?
C11 C9 H9 108.4 . . ?
C11 C9 C8 111.8(3) . . ?
C11 C9 C10 111.3(3) . . ?
C10 C9 H9 108.4 . . ?
C10 C9 C8 108.6(3) . . ?
F10 C35 C30 121.1(3) . . ?
F10 C35 C34 114.8(3) . . ?
C30 C35 C34 124.1(3) . . ?
F15 C41 C36 121.0(3) . . ?
F15 C41 C40 114.6(3) . . ?
C36 C41 C40 124.4(3) . . ?
C6 C5 H5 115.1 . . ?
C4 C5 C6 129.8(3) . . ?
C4 C5 H5 115.1 . . ?
F3 C27 C26 120.8(3) . . ?
F3 C27 C28 120.1(3) . . ?
C26 C27 C28 119.1(3) . . ?
C2 C3 H3 115.3 . . ?
C4 C3 H3 115.3 . . ?
C4 C3 C2 129.4(3) . . ?
C1 C2 H2 114.2 . . ?
C3 C2 C1 131.6(3) . . ?
C3 C2 H2 114.2 . . ?
F9 C34 C35 121.0(3) . . ?
F9 C34 C33 119.7(3) . . ?
C33 C34 C35 119.3(3) . . ?
F4 C28 C29 120.9(3) . . ?
F4 C28 C27 119.9(3) . . ?
C27 C28 C29 119.1(3) . . ?
F11 C37 C36 119.9(3) . . ?
F11 C37 C38 116.3(3) . . ?
C38 C37 C36 123.8(3) . . ?
C16 C17 C18 177.9(3) . . ?
F8 C33 C32 120.8(3) . . ?
F8 C33 C34 119.9(3) . . ?
C34 C33 C32 119.3(3) . . ?
N1 C8 C9 115.8(3) . . ?
N1 C8 H8A 108.3 . . ?
N1 C8 H8B 108.3 . . ?
C9 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C5 C4 C3 126.7(3) . . ?
C5 C4 H4 116.7 . . ?
C3 C4 H4 116.7 . . ?
F12 C38 C37 120.2(3) . . ?
F12 C38 C39 119.8(3) . . ?
C39 C38 C37 120.0(3) . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 C23 120.0(3) . . ?
C23 C18 C17 118.8(3) . . ?
F14 C40 C41 120.6(3) . . ?
F14 C40 C39 120.2(3) . . ?
C39 C40 C41 119.2(3) . . ?
O1 B1 C36 105.7(2) . . ?
O1 B1 C24 105.1(2) . . ?
O1 B1 C30 115.5(2) . . ?
C24 B1 C36 114.4(2) . . ?
C30 B1 C36 112.4(2) . . ?
C30 B1 C24 103.8(2) . . ?
F13 C39 C38 120.7(3) . . ?
F13 C39 C40 120.1(3) . . ?
C38 C39 C40 119.2(3) . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.8(3) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.0 . . ?
C18 C23 H23 120.4 . . ?
C18 C23 C22 119.3(4) . . ?
C22 C23 H23 120.4 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(4) . . ?
C22 C21 H21 119.6 . . ?
C23 C22 H22 119.9 . . ?
C21 C22 C23 120.1(4) . . ?
C21 C22 H22 119.9 . . ?
Cl1 C42 Cl1 98.7(4) . 2_657 ?
Cl1 C42 H42A 112.0 2_657 . ?
Cl1 C42 H42A 112.0 . . ?
Cl1 C42 H42B 112.0 . . ?
Cl1 C42 H42B 112.0 2_657 . ?
H42A C42 H42B 109.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound_22__msh22_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1851015'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;
_audit_creation_date             2017-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C39 H41 B F15 Ge N3 O Si2'
_chemical_formula_sum            'C39 H41 B F15 Ge N3 O Si2'
_chemical_formula_weight         992.35
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6826(7)
_cell_length_b                   12.4053(8)
_cell_length_c                   17.1901(11)
_cell_angle_alpha                83.572(2)
_cell_angle_beta                 87.402(2)
_cell_angle_gamma                73.342(2)
_cell_volume                     2371.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      32.28
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1647
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62263
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.561
_diffrn_reflns_theta_min         1.991
_diffrn_ambient_temperature      102.71
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13007
_reflns_number_total             15738
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         15738
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+1.6565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1253
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C6(H6), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.79151(2) 0.47965(2) 0.76033(2) 0.01178(5) Uani 1 1 d . . . . .
Si2 Si 0.99510(4) 0.57243(4) 0.79113(3) 0.01430(9) Uani 1 1 d . . . . .
Si1 Si 0.53118(5) 0.44567(5) 0.74755(3) 0.01971(11) Uani 1 1 d . . . . .
F10 F 0.69035(10) 0.67737(10) 0.61777(6) 0.0212(2) Uani 1 1 d . . . . .
F15 F 0.92367(10) 0.68773(9) 0.61988(6) 0.0195(2) Uani 1 1 d . . . . .
F1 F 0.66642(10) 0.61654(9) 0.89993(7) 0.0201(2) Uani 1 1 d . . . . .
F2 F 0.68228(12) 0.63850(11) 1.05087(7) 0.0288(3) Uani 1 1 d . . . . .
F11 F 0.65543(11) 0.96909(9) 0.75840(7) 0.0238(3) Uani 1 1 d . . . . .
F5 F 0.86331(11) 0.90053(10) 0.83501(7) 0.0244(2) Uani 1 1 d . . . . .
F6 F 0.51318(11) 0.82314(11) 0.85178(7) 0.0288(3) Uani 1 1 d . . . . .
F14 F 0.95126(13) 0.84554(10) 0.51282(7) 0.0298(3) Uani 1 1 d . . . . .
F4 F 0.87833(13) 0.91971(12) 0.98479(8) 0.0319(3) Uani 1 1 d . . . . .
F9 F 0.47563(12) 0.73484(12) 0.55410(7) 0.0312(3) Uani 1 1 d . . . . .
F12 F 0.68609(13) 1.12644(9) 0.64791(8) 0.0317(3) Uani 1 1 d . . . . .
F8 F 0.27634(12) 0.83301(15) 0.63901(9) 0.0421(4) Uani 1 1 d . . . . .
F3 F 0.78995(14) 0.78926(13) 1.09621(7) 0.0370(3) Uani 1 1 d . . . . .
F13 F 0.83483(14) 1.06744(10) 0.52303(8) 0.0344(3) Uani 1 1 d . . . . .
O3 O 0.63799(11) 0.50700(11) 0.75379(8) 0.0177(2) Uani 1 1 d . . . . .
F7 F 0.30319(12) 0.87399(15) 0.78889(8) 0.0435(4) Uani 1 1 d . . . . .
N0AA N 0.86275(13) 0.38621(12) 0.68304(8) 0.0137(3) Uani 1 1 d . . . . .
N2 N 0.84942(13) 0.35205(12) 0.83217(8) 0.0146(3) Uani 1 1 d . . . . .
N1 N 0.84268(13) 0.60077(12) 0.76579(8) 0.0133(3) Uani 1 1 d . . . . .
C1 C 0.91313(15) 0.27770(14) 0.71135(10) 0.0148(3) Uani 1 1 d . . . . .
C8 C 0.88324(16) 0.43458(15) 0.60299(9) 0.0151(3) Uani 1 1 d . . . . .
H8A H 0.9570 0.3845 0.5816 0.018 Uiso 1 1 calc R . . . .
H8B H 0.8975 0.5088 0.6062 0.018 Uiso 1 1 calc R . . . .
C7 C 0.90655(15) 0.25803(14) 0.79695(10) 0.0146(3) Uani 1 1 d . . . . .
C20 C 1.02170(17) 0.54373(17) 0.89916(11) 0.0205(3) Uani 1 1 d . . . . .
H20A H 0.9752 0.6092 0.9252 0.031 Uiso 1 1 calc GR . . . .
H20B H 1.1069 0.5302 0.9090 0.031 Uiso 1 1 calc GR . . . .
H20C H 0.9969 0.4769 0.9198 0.031 Uiso 1 1 calc GR . . . .
C24 C 0.72732(18) 0.70265(17) 0.99675(11) 0.0215(4) Uani 1 1 d . . . . .
C28 C 0.61727(16) 0.74560(14) 0.73887(10) 0.0162(3) Uani 1 1 d . . . . .
C27 C 0.81518(17) 0.83254(15) 0.88493(10) 0.0184(3) Uani 1 1 d . . . . .
C22 C 0.76279(15) 0.75730(15) 0.85774(10) 0.0159(3) Uani 1 1 d . . . . .
C33 C 0.59629(16) 0.72715(15) 0.66295(10) 0.0179(3) Uani 1 1 d . . . . .
C39 C 0.86436(16) 0.79487(14) 0.63325(10) 0.0163(3) Uani 1 1 d . . . . .
C3 C 1.02614(17) 0.08165(16) 0.67526(12) 0.0213(4) Uani 1 1 d . . . . .
H3 H 1.0538 0.0439 0.6299 0.026 Uiso 1 1 calc R . . . .
C34 C 0.79298(16) 0.81869(14) 0.69950(10) 0.0155(3) Uani 1 1 d . . . . .
C29 C 0.51210(17) 0.79666(17) 0.77818(11) 0.0212(4) Uani 1 1 d . . . . .
C23 C 0.71987(16) 0.69330(15) 0.91821(10) 0.0170(3) Uani 1 1 d . . . . .
C2 C 0.96790(17) 0.19569(15) 0.66113(11) 0.0193(3) Uani 1 1 d . . . . .
H2 H 0.9643 0.2237 0.6073 0.023 Uiso 1 1 calc R . . . .
C19 C 1.09052(16) 0.44416(16) 0.74769(11) 0.0200(3) Uani 1 1 d . . . . .
H19A H 1.0724 0.3765 0.7739 0.030 Uiso 1 1 calc GR . . . .
H19B H 1.1750 0.4381 0.7547 0.030 Uiso 1 1 calc GR . . . .
H19C H 1.0741 0.4507 0.6917 0.030 Uiso 1 1 calc GR . . . .
C9 C 0.78252(17) 0.45110(15) 0.54539(10) 0.0173(3) Uani 1 1 d . . . . .
H9 H 0.7064 0.4960 0.5690 0.021 Uiso 1 1 calc R . . . .
C13 C 0.75671(18) 0.29185(16) 0.96055(11) 0.0206(4) Uani 1 1 d . . . . .
H13 H 0.7466 0.2333 0.9280 0.025 Uiso 1 1 calc R . . . .
C6 C 0.95864(16) 0.15501(15) 0.84136(11) 0.0180(3) Uani 1 1 d . . . . .
H6 H 0.9498 0.1579 0.8964 0.022 Uiso 1 1 calc R . . . .
C4 C 1.05027(17) 0.01397(15) 0.74614(12) 0.0216(4) Uani 1 1 d . . . . .
H4 H 1.0907 -0.0639 0.7438 0.026 Uiso 1 1 calc R . . . .
C12 C 0.84520(16) 0.35049(15) 0.91792(10) 0.0164(3) Uani 1 1 d . . . . .
H12A H 0.8238 0.4295 0.9312 0.020 Uiso 1 1 calc R . . . .
H12B H 0.9263 0.3119 0.9382 0.020 Uiso 1 1 calc R . . . .
C10 C 0.7647(2) 0.34130(17) 0.52442(13) 0.0261(4) Uani 1 1 d . . . . .
H10A H 0.8355 0.2999 0.4961 0.039 Uiso 1 1 calc GR . . . .
H10B H 0.6945 0.3582 0.4912 0.039 Uiso 1 1 calc GR . . . .
H10C H 0.7527 0.2949 0.5724 0.039 Uiso 1 1 calc GR . . . .
C38 C 0.87997(18) 0.87608(16) 0.57511(11) 0.0211(4) Uani 1 1 d . . . . .
C11 C 0.8118(2) 0.52056(19) 0.47189(11) 0.0272(4) Uani 1 1 d . . . . .
H11A H 0.8184 0.5930 0.4858 0.041 Uiso 1 1 calc GR . . . .
H11B H 0.7480 0.5344 0.4338 0.041 Uiso 1 1 calc GR . . . .
H11C H 0.8876 0.4787 0.4490 0.041 Uiso 1 1 calc GR . . . .
C35 C 0.73399(17) 0.93399(15) 0.69983(11) 0.0184(3) Uani 1 1 d . . . . .
C21 C 1.06254(17) 0.68999(16) 0.75924(12) 0.0219(4) Uani 1 1 d . . . . .
H21A H 1.0784 0.6926 0.7027 0.033 Uiso 1 1 calc GR . . . .
H21B H 1.1376 0.6771 0.7869 0.033 Uiso 1 1 calc GR . . . .
H21C H 1.0070 0.7620 0.7714 0.033 Uiso 1 1 calc GR . . . .
C25 C 0.78115(19) 0.77874(18) 1.02008(11) 0.0246(4) Uani 1 1 d . . . . .
C31 C 0.38547(18) 0.8062(2) 0.67068(13) 0.0284(4) Uani 1 1 d . . . . .
C36 C 0.74670(19) 1.01751(15) 0.64317(12) 0.0225(4) Uani 1 1 d . . . . .
C15 C 0.63492(19) 0.37650(18) 0.97135(12) 0.0260(4) Uani 1 1 d . . . . .
H15A H 0.5787 0.3364 0.9949 0.039 Uiso 1 1 calc GR . . . .
H15B H 0.6053 0.4156 0.9203 0.039 Uiso 1 1 calc GR . . . .
H15C H 0.6425 0.4319 1.0057 0.039 Uiso 1 1 calc GR . . . .
C5 C 1.02098(17) 0.04945(16) 0.81917(12) 0.0214(4) Uani 1 1 d . . . . .
H5 H 1.0477 -0.0074 0.8614 0.026 Uiso 1 1 calc R . . . .
C37 C 0.8213(2) 0.98846(16) 0.57947(11) 0.0236(4) Uani 1 1 d . . . . .
C16 C 0.40203(18) 0.5278(2) 0.80393(15) 0.0311(5) Uani 1 1 d . . . . .
H16A H 0.4290 0.5375 0.8552 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.3412 0.4870 0.8112 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.3678 0.6022 0.7752 0.047 Uiso 1 1 calc GR . . . .
C26 C 0.82553(18) 0.84451(17) 0.96341(11) 0.0230(4) Uani 1 1 d . . . . .
C32 C 0.48612(18) 0.75588(17) 0.62786(11) 0.0234(4) Uani 1 1 d . . . . .
C30 C 0.39931(18) 0.8259(2) 0.74567(12) 0.0287(5) Uani 1 1 d . . . . .
C17 C 0.4875(2) 0.4539(2) 0.64403(14) 0.0352(5) Uani 1 1 d . . . . .
H17A H 0.4691 0.5326 0.6205 0.053 Uiso 1 1 calc GR . . . .
H17B H 0.4168 0.4269 0.6420 0.053 Uiso 1 1 calc GR . . . .
H17C H 0.5535 0.4067 0.6149 0.053 Uiso 1 1 calc GR . . . .
B1 B 0.75684(17) 0.72613(16) 0.76684(11) 0.0145(3) Uani 1 1 d . . . . .
C18 C 0.5772(2) 0.29339(18) 0.78563(14) 0.0289(4) Uani 1 1 d . . . . .
H18A H 0.6568 0.2570 0.7650 0.043 Uiso 1 1 calc GR . . . .
H18B H 0.5198 0.2566 0.7691 0.043 Uiso 1 1 calc GR . . . .
H18C H 0.5792 0.2863 0.8429 0.043 Uiso 1 1 calc GR . . . .
C14 C 0.8067(2) 0.2329(2) 1.04011(12) 0.0340(5) Uani 1 1 d . . . . .
H14A H 0.8214 0.2886 1.0716 0.051 Uiso 1 1 calc GR . . . .
H14B H 0.8818 0.1745 1.0321 0.051 Uiso 1 1 calc GR . . . .
H14C H 0.7488 0.1979 1.0675 0.051 Uiso 1 1 calc GR . . . .


_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 O3 1.7336(13) . ?
Ge1 N0AA 1.8689(14) . ?
Ge1 N2 1.8741(14) . ?
Ge1 N1 1.7820(15) . ?
Si2 N1 1.7780(16) . ?
Si2 C20 1.8743(19) . ?
Si2 C19 1.8723(19) . ?
Si2 C21 1.868(2) . ?
Si1 O3 1.6500(15) . ?
Si1 C16 1.861(2) . ?
Si1 C17 1.857(2) . ?
Si1 C18 1.860(2) . ?
F10 C33 1.3538(19) . ?
F15 C39 1.3511(19) . ?
F1 C23 1.349(2) . ?
F2 C24 1.344(2) . ?
F11 C35 1.3531(19) . ?
F5 C27 1.353(2) . ?
F6 C29 1.344(2) . ?
F14 C38 1.3464(19) . ?
F4 C26 1.346(2) . ?
F9 C32 1.341(2) . ?
F12 C36 1.343(2) . ?
F8 C31 1.346(2) . ?
F3 C25 1.341(2) . ?
F13 C37 1.337(2) . ?
F7 C30 1.345(2) . ?
N0AA C1 1.349(2) . ?
N0AA C8 1.476(2) . ?
N2 C7 1.359(2) . ?
N2 C12 1.471(2) . ?
N1 B1 1.592(2) . ?
C1 C7 1.467(2) . ?
C1 C2 1.401(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.526(3) . ?
C7 C6 1.401(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C24 C23 1.377(3) . ?
C24 C25 1.377(3) . ?
C28 C33 1.394(3) . ?
C28 C29 1.394(2) . ?
C28 B1 1.664(3) . ?
C27 C22 1.384(3) . ?
C27 C26 1.388(3) . ?
C22 C23 1.399(2) . ?
C22 B1 1.660(3) . ?
C33 C32 1.381(3) . ?
C39 C34 1.388(2) . ?
C39 C38 1.382(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.382(3) . ?
C3 C4 1.391(3) . ?
C34 C35 1.399(2) . ?
C34 B1 1.665(3) . ?
C29 C30 1.388(3) . ?
C2 H2 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C9 H9 1.0000 . ?
C9 C10 1.519(3) . ?
C9 C11 1.530(3) . ?
C13 H13 1.0000 . ?
C13 C12 1.542(3) . ?
C13 C15 1.525(3) . ?
C13 C14 1.533(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C38 C37 1.375(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C35 C36 1.376(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C25 C26 1.379(3) . ?
C31 C32 1.385(3) . ?
C31 C30 1.364(3) . ?
C36 C37 1.382(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C5 H5 0.9500 . ?
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 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
O3 Ge1 N0AA 107.82(7) . . ?
O3 Ge1 N2 108.80(6) . . ?
O3 Ge1 N1 115.16(6) . . ?
N0AA Ge1 N2 86.14(6) . . ?
N1 Ge1 N0AA 116.32(6) . . ?
N1 Ge1 N2 118.83(7) . . ?
N1 Si2 C20 113.71(8) . . ?
N1 Si2 C19 111.28(8) . . ?
N1 Si2 C21 114.56(8) . . ?
C19 Si2 C20 105.66(9) . . ?
C21 Si2 C20 104.20(9) . . ?
C21 Si2 C19 106.70(9) . . ?
O3 Si1 C16 105.60(10) . . ?
O3 Si1 C17 110.60(9) . . ?
O3 Si1 C18 112.66(9) . . ?
C17 Si1 C16 109.20(12) . . ?
C17 Si1 C18 107.10(12) . . ?
C18 Si1 C16 111.69(10) . . ?
Si1 O3 Ge1 142.94(8) . . ?
C1 N0AA Ge1 113.53(11) . . ?
C1 N0AA C8 124.19(14) . . ?
C8 N0AA Ge1 120.95(11) . . ?
C7 N2 Ge1 112.77(11) . . ?
C7 N2 C12 121.19(14) . . ?
C12 N2 Ge1 125.86(11) . . ?
Si2 N1 Ge1 115.67(8) . . ?
B1 N1 Ge1 124.06(12) . . ?
B1 N1 Si2 119.02(12) . . ?
N0AA C1 C7 113.54(14) . . ?
N0AA C1 C2 120.99(15) . . ?
C2 C1 C7 125.46(16) . . ?
N0AA C8 H8A 108.3 . . ?
N0AA C8 H8B 108.3 . . ?
N0AA C8 C9 115.80(14) . . ?
H8A C8 H8B 107.4 . . ?
C9 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
N2 C7 C1 113.90(15) . . ?
N2 C7 C6 120.96(15) . . ?
C6 C7 C1 125.05(15) . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
F2 C24 C23 120.67(19) . . ?
F2 C24 C25 119.66(17) . . ?
C23 C24 C25 119.66(18) . . ?
C33 C28 B1 119.46(14) . . ?
C29 C28 C33 112.21(17) . . ?
C29 C28 B1 127.50(17) . . ?
F5 C27 C22 121.25(16) . . ?
F5 C27 C26 114.16(17) . . ?
C22 C27 C26 124.58(17) . . ?
C27 C22 C23 112.79(16) . . ?
C27 C22 B1 129.08(15) . . ?
C23 C22 B1 117.84(16) . . ?
F10 C33 C28 118.84(16) . . ?
F10 C33 C32 115.34(17) . . ?
C32 C33 C28 125.82(16) . . ?
F15 C39 C34 121.80(15) . . ?
F15 C39 C38 114.11(14) . . ?
C38 C39 C34 124.08(16) . . ?
C2 C3 H3 115.3 . . ?
C2 C3 C4 129.49(18) . . ?
C4 C3 H3 115.3 . . ?
C39 C34 C35 112.72(15) . . ?
C39 C34 B1 127.15(15) . . ?
C35 C34 B1 119.38(14) . . ?
F6 C29 C28 121.51(18) . . ?
F6 C29 C30 114.47(16) . . ?
C30 C29 C28 124.02(18) . . ?
F1 C23 C24 116.22(16) . . ?
F1 C23 C22 119.03(16) . . ?
C24 C23 C22 124.75(18) . . ?
C1 C2 H2 114.0 . . ?
C3 C2 C1 132.04(17) . . ?
C3 C2 H2 114.0 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 C9 H9 108.5 . . ?
C8 C9 C11 107.01(15) . . ?
C10 C9 C8 113.94(15) . . ?
C10 C9 H9 108.5 . . ?
C10 C9 C11 110.38(16) . . ?
C11 C9 H9 108.5 . . ?
C12 C13 H13 108.5 . . ?
C15 C13 H13 108.5 . . ?
C15 C13 C12 111.02(16) . . ?
C15 C13 C14 110.23(17) . . ?
C14 C13 H13 108.5 . . ?
C14 C13 C12 110.04(17) . . ?
C7 C6 H6 114.3 . . ?
C5 C6 C7 131.40(17) . . ?
C5 C6 H6 114.3 . . ?
C3 C4 H4 117.0 . . ?
C5 C4 C3 125.92(17) . . ?
C5 C4 H4 117.0 . . ?
N2 C12 C13 115.29(15) . . ?
N2 C12 H12A 108.5 . . ?
N2 C12 H12B 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
F14 C38 C39 120.20(16) . . ?
F14 C38 C37 119.31(16) . . ?
C37 C38 C39 120.48(16) . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
F11 C35 C34 119.37(15) . . ?
F11 C35 C36 115.56(15) . . ?
C36 C35 C34 125.05(16) . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
F3 C25 C24 120.87(18) . . ?
F3 C25 C26 120.5(2) . . ?
C24 C25 C26 118.58(18) . . ?
F8 C31 C32 120.3(2) . . ?
F8 C31 C30 121.03(18) . . ?
C30 C31 C32 118.62(19) . . ?
F12 C36 C35 121.17(16) . . ?
F12 C36 C37 119.46(17) . . ?
C35 C36 C37 119.36(17) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C6 C5 H5 114.7 . . ?
C4 C5 C6 130.52(18) . . ?
C4 C5 H5 114.7 . . ?
F13 C37 C38 120.87(17) . . ?
F13 C37 C36 120.86(17) . . ?
C38 C37 C36 118.26(17) . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
F4 C26 C27 120.70(18) . . ?
F4 C26 C25 119.67(18) . . ?
C25 C26 C27 119.63(19) . . ?
F9 C32 C33 121.15(17) . . ?
F9 C32 C31 120.16(19) . . ?
C33 C32 C31 118.69(19) . . ?
F7 C30 C29 119.4(2) . . ?
F7 C30 C31 120.01(19) . . ?
C31 C30 C29 120.63(17) . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 B1 C28 115.57(15) . . ?
N1 B1 C22 104.94(13) . . ?
N1 B1 C34 113.40(13) . . ?
C28 B1 C34 97.86(13) . . ?
C22 B1 C28 112.18(13) . . ?
C22 B1 C34 113.19(15) . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 -0.524 401.5 143.8 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Compound_11__sharma3m
_database_code_depnum_ccdc_archive 'CCDC 1564832'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H23 B Cl F15 Ge N2 O, C H2 Cl2'
_chemical_formula_sum            'C34 H25 B Cl3 F15 Ge N2 O'
_chemical_formula_weight         952.33

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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7309(18)
_cell_length_b                   13.344(2)
_cell_length_c                   13.627(2)
_cell_angle_alpha                62.827(3)
_cell_angle_beta                 73.967(3)
_cell_angle_gamma                81.201(3)
_cell_volume                     1823.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3310
_cell_measurement_theta_min      2.183
_cell_measurement_theta_max      24.9465

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.393
_exptl_crystal_size_min          0.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948.0
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9590
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6318
_reflns_number_gt                5373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0828P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6318
_refine_ls_number_parameters     518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1384
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.91286(3) 0.71683(3) 0.70299(3) 0.01382(14) Uani 1 1 d . . .
Cl1 Cl 0.92652(8) 0.87388(8) 0.55741(8) 0.0227(2) Uani 1 1 d . . .
Cl2 Cl 0.78050(15) 0.13154(12) 0.29248(15) 0.0675(5) Uani 1 1 d . . .
Cl3 Cl 0.87177(13) 0.03002(15) 0.13663(13) 0.0657(5) Uani 1 1 d . . .
O1 O 0.8140(2) 0.6326(2) 0.7086(2) 0.0174(6) Uani 1 1 d . . .
N1 N 1.0529(3) 0.6405(3) 0.7303(3) 0.0142(7) Uani 1 1 d . . .
N2 N 0.8959(3) 0.7375(3) 0.8313(3) 0.0154(7) Uani 1 1 d . . .
B1 B 0.7084(4) 0.6529(4) 0.6602(4) 0.0170(9) Uani 1 1 d . . .
F1 F 0.84767(19) 0.45085(19) 0.6721(2) 0.0256(5) Uani 1 1 d . . .
F2 F 0.7749(2) 0.24105(19) 0.7689(2) 0.0301(6) Uani 1 1 d . . .
F3 F 0.5412(2) 0.19648(19) 0.8552(2) 0.0276(6) Uani 1 1 d . . .
F4 F 0.37929(19) 0.3696(2) 0.8435(2) 0.0288(6) Uani 1 1 d . . .
F5 F 0.44878(18) 0.57801(18) 0.7572(2) 0.0236(5) Uani 1 1 d . . .
F6 F 0.94989(18) 0.6724(2) 0.48963(19) 0.0259(5) Uani 1 1 d . . .
F7 F 0.9776(2) 0.7247(2) 0.2726(2) 0.0332(6) Uani 1 1 d . . .
F8 F 0.7882(2) 0.7673(2) 0.1806(2) 0.0342(6) Uani 1 1 d . . .
F9 F 0.5648(2) 0.7644(2) 0.3123(2) 0.0288(6) Uani 1 1 d . . .
F10 F 0.53380(18) 0.71706(19) 0.52979(18) 0.0226(5) Uani 1 1 d . . .
F11 F 0.5714(2) 0.6024(2) 0.89152(19) 0.0285(6) Uani 1 1 d . . .
F12 F 0.4349(2) 0.7429(3) 0.9656(2) 0.0428(7) Uani 1 1 d . . .
F13 F 0.4188(2) 0.9663(2) 0.8234(2) 0.0440(7) Uani 1 1 d . . .
F14 F 0.5330(2) 1.0418(2) 0.6007(2) 0.0378(6) Uani 1 1 d . . .
F15 F 0.6589(2) 0.90212(19) 0.52094(19) 0.0251(5) Uani 1 1 d . . .
C1 C 1.0740(3) 0.6293(3) 0.8280(3) 0.0149(8) Uani 1 1 d . . .
C2 C 1.1738(3) 0.5689(3) 0.8653(3) 0.0187(8) Uani 1 1 d . . .
H2 H 1.2208 0.5368 0.8191 0.022 Uiso 1 1 calc R . .
C3 C 1.2157(3) 0.5480(3) 0.9588(3) 0.0218(9) Uani 1 1 d . . .
H3 H 1.2877 0.5077 0.9634 0.026 Uiso 1 1 calc R . .
C4 C 1.1662(4) 0.5785(4) 1.0461(3) 0.0252(9) Uani 1 1 d . . .
H4 H 1.2086 0.5577 1.1013 0.030 Uiso 1 1 calc R . .
C5 C 1.0593(4) 0.6370(3) 1.0594(3) 0.0237(9) Uani 1 1 d . . .
H5 H 1.0382 0.6488 1.1243 0.028 Uiso 1 1 calc R . .
C6 C 0.9793(3) 0.6804(3) 0.9912(3) 0.0204(9) Uani 1 1 d . . .
H6 H 0.9110 0.7132 1.0201 0.025 Uiso 1 1 calc R . .
C7 C 0.9825(3) 0.6839(3) 0.8873(3) 0.0145(8) Uani 1 1 d . . .
C8 C 1.1285(3) 0.5817(3) 0.6641(3) 0.0166(8) Uani 1 1 d . . .
H8A H 1.0836 0.5762 0.6168 0.020 Uiso 1 1 calc R . .
H8B H 1.1463 0.5056 0.7167 0.020 Uiso 1 1 calc R . .
C9 C 0.7922(3) 0.7962(3) 0.8762(3) 0.0186(8) Uani 1 1 d . . .
H9A H 0.7587 0.7458 0.9546 0.022 Uiso 1 1 calc R . .
H9B H 0.7325 0.8105 0.8339 0.022 Uiso 1 1 calc R . .
C10 C 1.2461(3) 0.6388(3) 0.5880(3) 0.0194(8) Uani 1 1 d . . .
H10 H 1.2866 0.6529 0.6343 0.023 Uiso 1 1 calc R . .
C11 C 0.8172(4) 0.9073(3) 0.8714(3) 0.0230(9) Uani 1 1 d . . .
H11 H 0.8773 0.8926 0.9144 0.028 Uiso 1 1 calc R . .
C12 C 1.2277(4) 0.7512(4) 0.4888(4) 0.0293(10) Uani 1 1 d . . .
H12A H 1.3034 0.7819 0.4422 0.044 Uiso 1 1 calc R . .
H12B H 1.1832 0.8028 0.5174 0.044 Uiso 1 1 calc R . .
H12C H 1.1848 0.7396 0.4443 0.044 Uiso 1 1 calc R . .
C13 C 1.3239(4) 0.5573(4) 0.5453(4) 0.0267(9) Uani 1 1 d . . .
H13A H 1.2825 0.5372 0.5055 0.040 Uiso 1 1 calc R . .
H13B H 1.3419 0.4906 0.6086 0.040 Uiso 1 1 calc R . .
H13C H 1.3964 0.5928 0.4949 0.040 Uiso 1 1 calc R . .
C14 C 0.8638(4) 0.9946(4) 0.7518(4) 0.0351(11) Uani 1 1 d . . .
H14A H 0.8054 1.0116 0.7086 0.053 Uiso 1 1 calc R . .
H14B H 0.9353 0.9657 0.7172 0.053 Uiso 1 1 calc R . .
H14C H 0.8805 1.0619 0.7536 0.053 Uiso 1 1 calc R . .
C15 C 0.7035(4) 0.9501(4) 0.9298(4) 0.0343(11) Uani 1 1 d . . .
H15A H 0.7186 1.0187 0.9301 0.052 Uiso 1 1 calc R . .
H15B H 0.6774 0.8944 1.0064 0.052 Uiso 1 1 calc R . .
H15C H 0.6429 0.9643 0.8894 0.052 Uiso 1 1 calc R . .
C16 C 0.6528(3) 0.5266(3) 0.7140(3) 0.0163(8) Uani 1 1 d . . .
C17 C 0.7298(3) 0.4350(3) 0.7174(3) 0.0181(8) Uani 1 1 d . . .
C18 C 0.6948(3) 0.3257(3) 0.7637(3) 0.0196(8) Uani 1 1 d . . .
C19 C 0.5763(3) 0.3023(3) 0.8073(3) 0.0201(9) Uani 1 1 d . . .
C20 C 0.4964(3) 0.3906(3) 0.8011(3) 0.0193(8) Uani 1 1 d . . .
C21 C 0.5353(3) 0.4977(3) 0.7564(3) 0.0177(8) Uani 1 1 d . . .
C22 C 0.7390(3) 0.6939(3) 0.5221(3) 0.0169(8) Uani 1 1 d . . .
C23 C 0.8492(3) 0.6961(3) 0.4506(3) 0.0184(8) Uani 1 1 d . . .
C24 C 0.8671(3) 0.7222(4) 0.3373(3) 0.0233(9) Uani 1 1 d . . .
C25 C 0.7715(4) 0.7453(3) 0.2900(3) 0.0227(9) Uani 1 1 d . . .
C26 C 0.6594(3) 0.7440(3) 0.3568(3) 0.0200(9) Uani 1 1 d . . .
C27 C 0.6462(3) 0.7185(3) 0.4687(3) 0.0171(8) Uani 1 1 d . . .
C28 C 0.6187(3) 0.7426(3) 0.7015(3) 0.0177(8) Uani 1 1 d . . .
C29 C 0.5612(3) 0.7101(3) 0.8143(3) 0.0220(9) Uani 1 1 d . . .
C30 C 0.4912(3) 0.7822(4) 0.8559(3) 0.0256(10) Uani 1 1 d . . .
C31 C 0.4825(4) 0.8942(4) 0.7843(4) 0.0276(10) Uani 1 1 d . . .
C32 C 0.5407(4) 0.9323(4) 0.6722(4) 0.0260(10) Uani 1 1 d . . .
C33 C 0.6061(3) 0.8567(3) 0.6329(3) 0.0206(9) Uani 1 1 d . . .
C37 C 0.8083(5) 0.0067(4) 0.2785(4) 0.0452(13) Uani 1 1 d . . .
H37A H 0.7345 -0.0322 0.3052 0.054 Uiso 1 1 calc R . .
H37B H 0.8617 -0.0415 0.3257 0.054 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.698(2) . ?
Ge1 N1 1.831(3) . ?
Ge1 N2 1.846(3) . ?
Ge1 Cl1 2.1173(10) . ?
Cl2 C37 1.734(5) . ?
Cl3 C37 1.765(5) . ?
O1 B1 1.493(5) . ?
N1 C1 1.359(4) . ?
N1 C8 1.486(4) . ?
N2 C7 1.354(5) . ?
N2 C9 1.484(4) . ?
B1 C22 1.648(6) . ?
B1 C16 1.658(6) . ?
B1 C28 1.662(6) . ?
F1 C17 1.355(4) . ?
F2 C18 1.343(4) . ?
F3 C19 1.333(4) . ?
F4 C20 1.353(4) . ?
F5 C21 1.360(4) . ?
F6 C23 1.362(4) . ?
F7 C24 1.347(4) . ?
F8 C25 1.342(4) . ?
F9 C26 1.342(4) . ?
F10 C27 1.349(4) . ?
F11 C29 1.350(5) . ?
F12 C30 1.337(5) . ?
F13 C31 1.341(4) . ?
F14 C32 1.342(5) . ?
F15 C33 1.352(4) . ?
C1 C2 1.394(5) . ?
C1 C7 1.468(5) . ?
C2 C3 1.387(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(5) . ?
C6 H6 0.9300 . ?
C8 C10 1.539(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.524(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C12 1.528(6) . ?
C10 C13 1.529(5) . ?
C10 H10 0.9800 . ?
C11 C14 1.510(6) . ?
C11 C15 1.528(6) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C21 1.378(5) . ?
C16 C17 1.395(5) . ?
C17 C18 1.375(5) . ?
C18 C19 1.375(5) . ?
C19 C20 1.374(5) . ?
C20 C21 1.369(5) . ?
C22 C23 1.383(5) . ?
C22 C27 1.389(5) . ?
C23 C24 1.379(5) . ?
C24 C25 1.372(6) . ?
C25 C26 1.375(5) . ?
C26 C27 1.370(5) . ?
C28 C29 1.383(5) . ?
C28 C33 1.386(6) . ?
C29 C30 1.386(6) . ?
C30 C31 1.368(6) . ?
C31 C32 1.370(6) . ?
C32 C33 1.386(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ge1 N1 111.60(13) . . ?
O1 Ge1 N2 116.79(13) . . ?
N1 Ge1 N2 87.46(13) . . ?
O1 Ge1 Cl1 112.25(9) . . ?
N1 Ge1 Cl1 116.19(10) . . ?
N2 Ge1 Cl1 110.52(10) . . ?
B1 O1 Ge1 134.6(2) . . ?
C1 N1 C8 121.8(3) . . ?
C1 N1 Ge1 112.8(2) . . ?
C8 N1 Ge1 124.8(2) . . ?
C7 N2 C9 122.8(3) . . ?
C7 N2 Ge1 112.9(2) . . ?
C9 N2 Ge1 124.1(2) . . ?
O1 B1 C22 114.9(3) . . ?
O1 B1 C16 104.7(3) . . ?
C22 B1 C16 103.5(3) . . ?
O1 B1 C28 106.2(3) . . ?
C22 B1 C28 113.5(3) . . ?
C16 B1 C28 113.8(3) . . ?
N1 C1 C2 120.8(3) . . ?
N1 C1 C7 113.7(3) . . ?
C2 C1 C7 125.5(3) . . ?
C3 C2 C1 131.6(4) . . ?
C3 C2 H2 114.2 . . ?
C1 C2 H2 114.2 . . ?
C4 C3 C2 129.4(4) . . ?
C4 C3 H3 115.3 . . ?
C2 C3 H3 115.3 . . ?
C3 C4 C5 126.2(4) . . ?
C3 C4 H4 116.9 . . ?
C5 C4 H4 116.9 . . ?
C6 C5 C4 130.0(4) . . ?
C6 C5 H5 115.0 . . ?
C4 C5 H5 115.0 . . ?
C5 C6 C7 131.5(4) . . ?
C5 C6 H6 114.2 . . ?
C7 C6 H6 114.2 . . ?
N2 C7 C6 121.6(3) . . ?
N2 C7 C1 113.0(3) . . ?
C6 C7 C1 125.4(3) . . ?
N1 C8 C10 114.8(3) . . ?
N1 C8 H8A 108.6 . . ?
C10 C8 H8A 108.6 . . ?
N1 C8 H8B 108.6 . . ?
C10 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N2 C9 C11 115.9(3) . . ?
N2 C9 H9A 108.3 . . ?
C11 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C11 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C12 C10 C13 110.8(3) . . ?
C12 C10 C8 112.6(3) . . ?
C13 C10 C8 108.3(3) . . ?
C12 C10 H10 108.3 . . ?
C13 C10 H10 108.3 . . ?
C8 C10 H10 108.3 . . ?
C14 C11 C9 112.7(3) . . ?
C14 C11 C15 111.2(4) . . ?
C9 C11 C15 108.5(3) . . ?
C14 C11 H11 108.1 . . ?
C9 C11 H11 108.1 . . ?
C15 C11 H11 108.1 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 112.9(3) . . ?
C21 C16 B1 128.1(3) . . ?
C17 C16 B1 119.1(3) . . ?
F1 C17 C18 115.6(3) . . ?
F1 C17 C16 120.0(3) . . ?
C18 C17 C16 124.4(4) . . ?
F2 C18 C19 119.4(4) . . ?
F2 C18 C17 121.0(3) . . ?
C19 C18 C17 119.6(4) . . ?
F3 C19 C20 121.5(4) . . ?
F3 C19 C18 120.3(4) . . ?
C20 C19 C18 118.1(4) . . ?
F4 C20 C21 120.6(3) . . ?
F4 C20 C19 119.1(3) . . ?
C21 C20 C19 120.3(4) . . ?
F5 C21 C20 115.3(3) . . ?
F5 C21 C16 120.1(3) . . ?
C20 C21 C16 124.6(4) . . ?
C23 C22 C27 113.1(3) . . ?
C23 C22 B1 127.4(3) . . ?
C27 C22 B1 119.1(3) . . ?
F6 C23 C24 115.1(3) . . ?
F6 C23 C22 120.7(3) . . ?
C24 C23 C22 124.2(3) . . ?
F7 C24 C25 119.5(4) . . ?
F7 C24 C23 120.7(4) . . ?
C25 C24 C23 119.8(4) . . ?
F8 C25 C24 120.0(4) . . ?
F8 C25 C26 121.1(4) . . ?
C24 C25 C26 118.8(4) . . ?
F9 C26 C27 121.1(3) . . ?
F9 C26 C25 119.6(3) . . ?
C27 C26 C25 119.3(3) . . ?
F10 C27 C26 116.2(3) . . ?
F10 C27 C22 118.9(3) . . ?
C26 C27 C22 124.9(4) . . ?
C29 C28 C33 114.0(3) . . ?
C29 C28 B1 120.9(3) . . ?
C33 C28 B1 124.6(3) . . ?
F11 C29 C28 120.2(3) . . ?
F11 C29 C30 115.8(4) . . ?
C28 C29 C30 124.0(4) . . ?
F12 C30 C31 120.5(4) . . ?
F12 C30 C29 120.2(4) . . ?
C31 C30 C29 119.3(4) . . ?
F13 C31 C30 120.4(4) . . ?
F13 C31 C32 120.2(4) . . ?
C30 C31 C32 119.4(4) . . ?
F14 C32 C31 120.2(4) . . ?
F14 C32 C33 120.3(4) . . ?
C31 C32 C33 119.6(4) . . ?
F15 C33 C32 115.2(4) . . ?
F15 C33 C28 121.2(3) . . ?
C32 C33 C28 123.7(4) . . ?
Cl2 C37 Cl3 112.0(3) . . ?
Cl2 C37 H37A 109.2 . . ?
Cl3 C37 H37A 109.2 . . ?
Cl2 C37 H37B 109.2 . . ?
Cl3 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ge1 O1 B1 -156.7(3) . . . . ?
N2 Ge1 O1 B1 104.9(3) . . . . ?
Cl1 Ge1 O1 B1 -24.2(4) . . . . ?
O1 Ge1 N1 C1 -114.3(3) . . . . ?
N2 Ge1 N1 C1 3.6(3) . . . . ?
Cl1 Ge1 N1 C1 115.3(2) . . . . ?
O1 Ge1 N1 C8 57.1(3) . . . . ?
N2 Ge1 N1 C8 175.0(3) . . . . ?
Cl1 Ge1 N1 C8 -73.3(3) . . . . ?
O1 Ge1 N2 C7 108.5(3) . . . . ?
N1 Ge1 N2 C7 -4.5(3) . . . . ?
Cl1 Ge1 N2 C7 -121.6(2) . . . . ?
O1 Ge1 N2 C9 -65.4(3) . . . . ?
N1 Ge1 N2 C9 -178.4(3) . . . . ?
Cl1 Ge1 N2 C9 64.5(3) . . . . ?
Ge1 O1 B1 C22 71.8(4) . . . . ?
Ge1 O1 B1 C16 -175.4(2) . . . . ?
Ge1 O1 B1 C28 -54.6(4) . . . . ?
C8 N1 C1 C2 5.3(5) . . . . ?
Ge1 N1 C1 C2 177.0(3) . . . . ?
C8 N1 C1 C7 -173.7(3) . . . . ?
Ge1 N1 C1 C7 -2.0(4) . . . . ?
N1 C1 C2 C3 178.2(4) . . . . ?
C7 C1 C2 C3 -2.9(7) . . . . ?
C1 C2 C3 C4 3.0(7) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C3 C4 C5 C6 -1.5(7) . . . . ?
C4 C5 C6 C7 -3.3(8) . . . . ?
C9 N2 C7 C6 0.1(5) . . . . ?
Ge1 N2 C7 C6 -173.9(3) . . . . ?
C9 N2 C7 C1 178.3(3) . . . . ?
Ge1 N2 C7 C1 4.4(4) . . . . ?
C5 C6 C7 N2 -175.9(4) . . . . ?
C5 C6 C7 C1 6.1(7) . . . . ?
N1 C1 C7 N2 -1.6(4) . . . . ?
C2 C1 C7 N2 179.5(3) . . . . ?
N1 C1 C7 C6 176.6(3) . . . . ?
C2 C1 C7 C6 -2.3(6) . . . . ?
C1 N1 C8 C10 -80.1(4) . . . . ?
Ge1 N1 C8 C10 109.2(3) . . . . ?
C7 N2 C9 C11 73.1(5) . . . . ?
Ge1 N2 C9 C11 -113.6(3) . . . . ?
N1 C8 C10 C12 -68.5(4) . . . . ?
N1 C8 C10 C13 168.6(3) . . . . ?
N2 C9 C11 C14 61.2(5) . . . . ?
N2 C9 C11 C15 -175.3(3) . . . . ?
O1 B1 C16 C21 137.6(4) . . . . ?
C22 B1 C16 C21 -101.6(4) . . . . ?
C28 B1 C16 C21 22.0(5) . . . . ?
O1 B1 C16 C17 -43.7(4) . . . . ?
C22 B1 C16 C17 77.1(4) . . . . ?
C28 B1 C16 C17 -159.3(3) . . . . ?
C21 C16 C17 F1 175.8(3) . . . . ?
B1 C16 C17 F1 -3.1(5) . . . . ?
C21 C16 C17 C18 -3.7(5) . . . . ?
B1 C16 C17 C18 177.4(3) . . . . ?
F1 C17 C18 F2 3.8(5) . . . . ?
C16 C17 C18 F2 -176.6(3) . . . . ?
F1 C17 C18 C19 -177.3(3) . . . . ?
C16 C17 C18 C19 2.2(6) . . . . ?
F2 C18 C19 F3 0.6(5) . . . . ?
C17 C18 C19 F3 -178.3(3) . . . . ?
F2 C18 C19 C20 179.9(3) . . . . ?
C17 C18 C19 C20 1.0(6) . . . . ?
F3 C19 C20 F4 -0.8(5) . . . . ?
C18 C19 C20 F4 180.0(3) . . . . ?
F3 C19 C20 C21 176.9(3) . . . . ?
C18 C19 C20 C21 -2.4(6) . . . . ?
F4 C20 C21 F5 -0.7(5) . . . . ?
C19 C20 C21 F5 -178.3(3) . . . . ?
F4 C20 C21 C16 178.3(3) . . . . ?
C19 C20 C21 C16 0.7(6) . . . . ?
C17 C16 C21 F5 -178.8(3) . . . . ?
B1 C16 C21 F5 0.0(6) . . . . ?
C17 C16 C21 C20 2.2(6) . . . . ?
B1 C16 C21 C20 -179.0(4) . . . . ?
O1 B1 C22 C23 9.7(6) . . . . ?
C16 B1 C22 C23 -103.8(4) . . . . ?
C28 B1 C22 C23 132.3(4) . . . . ?
O1 B1 C22 C27 -177.8(3) . . . . ?
C16 B1 C22 C27 68.6(4) . . . . ?
C28 B1 C22 C27 -55.3(5) . . . . ?
C27 C22 C23 F6 -179.2(3) . . . . ?
B1 C22 C23 F6 -6.4(6) . . . . ?
C27 C22 C23 C24 1.3(6) . . . . ?
B1 C22 C23 C24 174.1(4) . . . . ?
F6 C23 C24 F7 -0.9(5) . . . . ?
C22 C23 C24 F7 178.7(4) . . . . ?
F6 C23 C24 C25 178.8(3) . . . . ?
C22 C23 C24 C25 -1.6(6) . . . . ?
F7 C24 C25 F8 1.8(6) . . . . ?
C23 C24 C25 F8 -177.9(4) . . . . ?
F7 C24 C25 C26 -179.0(4) . . . . ?
C23 C24 C25 C26 1.2(6) . . . . ?
F8 C25 C26 F9 0.3(6) . . . . ?
C24 C25 C26 F9 -178.8(4) . . . . ?
F8 C25 C26 C27 178.5(4) . . . . ?
C24 C25 C26 C27 -0.7(6) . . . . ?
F9 C26 C27 F10 -0.9(5) . . . . ?
C25 C26 C27 F10 -179.0(3) . . . . ?
F9 C26 C27 C22 178.5(3) . . . . ?
C25 C26 C27 C22 0.4(6) . . . . ?
C23 C22 C27 F10 178.8(3) . . . . ?
B1 C22 C27 F10 5.3(5) . . . . ?
C23 C22 C27 C26 -0.7(6) . . . . ?
B1 C22 C27 C26 -174.1(4) . . . . ?
O1 B1 C28 C29 -68.7(4) . . . . ?
C22 B1 C28 C29 164.1(3) . . . . ?
C16 B1 C28 C29 46.0(5) . . . . ?
O1 B1 C28 C33 102.8(4) . . . . ?
C22 B1 C28 C33 -24.5(5) . . . . ?
C16 B1 C28 C33 -142.6(4) . . . . ?
C33 C28 C29 F11 -176.5(3) . . . . ?
B1 C28 C29 F11 -4.2(5) . . . . ?
C33 C28 C29 C30 3.5(6) . . . . ?
B1 C28 C29 C30 175.8(4) . . . . ?
F11 C29 C30 F12 -2.5(5) . . . . ?
C28 C29 C30 F12 177.4(3) . . . . ?
F11 C29 C30 C31 176.0(3) . . . . ?
C28 C29 C30 C31 -4.1(6) . . . . ?
F12 C30 C31 F13 1.0(6) . . . . ?
C29 C30 C31 F13 -177.5(4) . . . . ?
F12 C30 C31 C32 -179.8(4) . . . . ?
C29 C30 C31 C32 1.7(6) . . . . ?
F13 C31 C32 F14 -0.9(6) . . . . ?
C30 C31 C32 F14 179.9(4) . . . . ?
F13 C31 C32 C33 -179.9(4) . . . . ?
C30 C31 C32 C33 0.9(6) . . . . ?
F14 C32 C33 F15 0.1(5) . . . . ?
C31 C32 C33 F15 179.1(3) . . . . ?
F14 C32 C33 C28 179.7(3) . . . . ?
C31 C32 C33 C28 -1.3(6) . . . . ?
C29 C28 C33 F15 178.7(3) . . . . ?
B1 C28 C33 F15 6.8(6) . . . . ?
C29 C28 C33 C32 -0.8(6) . . . . ?
B1 C28 C33 C32 -172.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.176
####################################################################### 
# 
# 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_Compound_19__msh30_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1851013'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H26 B F15 Ge N2 O, C H2 Cl2'
_chemical_formula_sum            'C35 H28 B Cl2 F15 Ge N2 O'
_chemical_formula_weight         931.91

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   12.1298(9)
_cell_length_b                   15.8356(12)
_cell_length_c                   19.4206(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3730.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9540
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.51

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             1864.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.073
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34274
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.361
_diffrn_reflns_theta_max         28.563
_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             9489
_reflns_number_gt                8648
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0289P)²+0.9827P] 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 
;
 Flack x determined using 3450 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9489
_refine_ls_number_parameters     519
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0932
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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 0.21807(3) 0.48099(2) 0.34320(2) 0.01193(8) Uani 1 1 d . . . . .
Cl1 Cl 0.68564(11) 0.52598(7) 0.14574(7) 0.0442(3) Uani 1 1 d . . . . .
Cl2 Cl 0.85398(11) 0.39818(9) 0.12029(8) 0.0510(3) Uani 1 1 d . . . . .
F5 F 0.37929(18) 0.72139(13) 0.38468(11) 0.0208(4) Uani 1 1 d . . . . .
F15 F 0.50912(18) 0.41456(13) 0.24633(11) 0.0190(4) Uani 1 1 d . . . . .
F11 F 0.64413(18) 0.54628(14) 0.44942(11) 0.0241(5) Uani 1 1 d . . . . .
F7 F 0.3502(2) 0.69089(13) 0.12605(11) 0.0243(5) Uani 1 1 d . . . . .
F6 F 0.30557(17) 0.57829(13) 0.22118(11) 0.0190(4) Uani 1 1 d . . . . .
F14 F 0.69207(19) 0.32413(13) 0.23942(11) 0.0244(5) Uani 1 1 d . . . . .
F1 F 0.44774(19) 0.45064(13) 0.47856(11) 0.0226(5) Uani 1 1 d . . . . .
F10 F 0.62884(17) 0.66076(13) 0.34166(12) 0.0243(5) Uani 1 1 d . . . . .
F4 F 0.33472(19) 0.77882(14) 0.50952(12) 0.0265(5) Uani 1 1 d . . . . .
F9 F 0.6785(2) 0.76508(14) 0.23912(14) 0.0323(6) Uani 1 1 d . . . . .
F8 F 0.5405(2) 0.78195(14) 0.12929(12) 0.0281(5) Uani 1 1 d . . . . .
F2 F 0.3974(2) 0.50912(15) 0.60282(11) 0.0294(5) Uani 1 1 d . . . . .
F12 F 0.82552(19) 0.45644(17) 0.44001(13) 0.0326(6) Uani 1 1 d . . . . .
F3 F 0.3449(2) 0.67451(15) 0.62112(11) 0.0305(6) Uani 1 1 d . . . . .
F13 F 0.8547(2) 0.34391(16) 0.33509(13) 0.0337(6) Uani 1 1 d . . . . .
O1 O 0.35810(19) 0.48093(15) 0.33076(12) 0.0148(5) Uani 1 1 d . . . . .
N1 N 0.1506(2) 0.58168(17) 0.36865(15) 0.0143(6) Uani 1 1 d . . . . .
N2 N 0.1880(2) 0.44596(17) 0.43304(15) 0.0142(6) Uani 1 1 d . . . . .
C33 C 0.6790(3) 0.3791(2) 0.29179(19) 0.0192(7) Uani 1 1 d . . . . .
C17 C 0.4202(3) 0.5827(2) 0.42447(18) 0.0155(7) Uani 1 1 d . . . . .
C18 C 0.4208(3) 0.5335(2) 0.48338(18) 0.0174(7) Uani 1 1 d . . . . .
C32 C 0.7609(3) 0.3888(2) 0.3398(2) 0.0223(7) Uani 1 1 d . . . . .
C24 C 0.3999(3) 0.6232(2) 0.23041(18) 0.0154(7) Uani 1 1 d . . . . .
C4 C 0.0836(3) 0.6379(2) 0.59365(19) 0.0231(8) Uani 1 1 d . . . . .
H4 H 0.0690 0.6656 0.6361 0.028 Uiso 1 1 calc R U . . .
C25 C 0.4221(3) 0.6807(2) 0.17816(18) 0.0173(7) Uani 1 1 d . . . . .
C23 C 0.4663(3) 0.6113(2) 0.28741(17) 0.0142(6) Uani 1 1 d . . . . .
C8 C 0.1176(3) 0.6470(2) 0.31927(18) 0.0161(7) Uani 1 1 d . . . . .
H8A H 0.1473 0.6321 0.2734 0.019 Uiso 1 1 calc R U . . .
H8B H 0.1513 0.7013 0.3332 0.019 Uiso 1 1 calc R U . . .
C1 C 0.1341(3) 0.5882(2) 0.43744(18) 0.0139(7) Uani 1 1 d . . . . .
C12 C 0.2211(3) 0.3606(2) 0.45629(18) 0.0188(7) Uani 1 1 d . . . . .
H12A H 0.2277 0.3608 0.5071 0.023 Uiso 1 1 calc R U . . .
H12B H 0.2946 0.3473 0.4370 0.023 Uiso 1 1 calc R U . . .
C16 C 0.1467(3) 0.4236(2) 0.26968(19) 0.0191(7) Uani 1 1 d . . . . .
H16A H 0.1452 0.4600 0.2289 0.029 Uiso 1 1 calc R U . . .
H16B H 0.0710 0.4095 0.2832 0.029 Uiso 1 1 calc R U . . .
H16C H 0.1870 0.3716 0.2590 0.029 Uiso 1 1 calc R U . . .
C14 C 0.0250(3) 0.3051(3) 0.4636(2) 0.0290(9) Uani 1 1 d . . . . .
H14A H 0.0261 0.2985 0.5138 0.044 Uiso 1 1 calc R U . . .
H14B H -0.0254 0.2635 0.4435 0.044 Uiso 1 1 calc R U . . .
H14C H -0.0002 0.3621 0.4519 0.044 Uiso 1 1 calc R U . . .
C34 C 0.5831(3) 0.4266(2) 0.29699(17) 0.0152(7) Uani 1 1 d . . . . .
C30 C 0.6496(3) 0.4916(2) 0.39603(18) 0.0179(7) Uani 1 1 d . . . . .
C35 C 0.7207(4) 0.4344(3) 0.0999(2) 0.0339(9) Uani 1 1 d . . . . .
H35A H 0.7167 0.4463 0.0499 0.041 Uiso 1 1 calc R U . . .
H35B H 0.6666 0.3895 0.1105 0.041 Uiso 1 1 calc R U . . .
C22 C 0.3892(3) 0.6662(2) 0.43714(18) 0.0163(7) Uani 1 1 d . . . . .
C31 C 0.7456(3) 0.4458(3) 0.39261(19) 0.0217(8) Uani 1 1 d . . . . .
C20 C 0.3686(3) 0.6456(3) 0.55804(19) 0.0221(8) Uani 1 1 d . . . . .
C29 C 0.5632(3) 0.4843(2) 0.34923(17) 0.0150(6) Uani 1 1 d . . . . .
C3 C 0.0920(3) 0.6875(2) 0.53570(19) 0.0195(7) Uani 1 1 d . . . . .
H3 H 0.0845 0.7464 0.5438 0.023 Uiso 1 1 calc R U . . .
C27 C 0.5861(3) 0.7188(2) 0.2353(2) 0.0212(8) Uani 1 1 d . . . . .
C28 C 0.5591(3) 0.6632(2) 0.28743(19) 0.0181(7) Uani 1 1 d . . . . .
C2 C 0.1095(3) 0.6657(2) 0.46744(19) 0.0173(7) Uani 1 1 d . . . . .
H2 H 0.1037 0.7113 0.4359 0.021 Uiso 1 1 calc R U . . .
C9 C -0.0061(3) 0.6589(2) 0.3134(2) 0.0229(8) Uani 1 1 d . . . . .
H9 H -0.0340 0.6823 0.3579 0.027 Uiso 1 1 calc R U . . .
C26 C 0.5172(3) 0.7280(2) 0.1800(2) 0.0210(7) Uani 1 1 d . . . . .
C21 C 0.3652(3) 0.6974(2) 0.50197(19) 0.0198(7) Uani 1 1 d . . . . .
C5 C 0.0948(3) 0.5499(3) 0.59518(19) 0.0235(8) Uani 1 1 d . . . . .
H5 H 0.0796 0.5245 0.6385 0.028 Uiso 1 1 calc R U . . .
C6 C 0.1243(3) 0.4944(2) 0.54380(18) 0.0198(7) Uani 1 1 d . . . . .
H6 H 0.1282 0.4371 0.5580 0.024 Uiso 1 1 calc R U . . .
C19 C 0.3951(3) 0.5611(2) 0.54878(18) 0.0211(7) Uani 1 1 d . . . . .
C13 C 0.1404(4) 0.2915(2) 0.4351(2) 0.0243(8) Uani 1 1 d . . . . .
H13 H 0.1356 0.2911 0.3837 0.029 Uiso 1 1 calc R U . . .
C7 C 0.1496(3) 0.5076(2) 0.47392(18) 0.0148(6) Uani 1 1 d . . . . .
C15 C 0.1873(4) 0.2064(2) 0.4584(3) 0.0389(11) Uani 1 1 d . . . . .
H15A H 0.2612 0.1989 0.4389 0.058 Uiso 1 1 calc R U . . .
H15B H 0.1391 0.1608 0.4424 0.058 Uiso 1 1 calc R U . . .
H15C H 0.1917 0.2052 0.5088 0.058 Uiso 1 1 calc R U . . .
C10 C -0.0668(4) 0.5774(3) 0.2985(3) 0.0374(11) Uani 1 1 d . . . . .
H10A H -0.0428 0.5550 0.2539 0.056 Uiso 1 1 calc R U . . .
H10B H -0.1463 0.5883 0.2972 0.056 Uiso 1 1 calc R U . . .
H10C H -0.0505 0.5361 0.3347 0.056 Uiso 1 1 calc R U . . .
C11 C -0.0284(4) 0.7230(3) 0.2570(2) 0.0359(11) Uani 1 1 d . . . . .
H11A H 0.0003 0.7017 0.2131 0.054 Uiso 1 1 calc R U . . .
H11B H 0.0081 0.7764 0.2684 0.054 Uiso 1 1 calc R U . . .
H11C H -0.1080 0.7323 0.2530 0.054 Uiso 1 1 calc R U . . .
B1 B 0.4472(3) 0.5404(2) 0.3488(2) 0.0146(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.716(2) . ?
Ge1 N1 1.859(3) . ?
Ge1 N2 1.867(3) . ?
Ge1 C16 1.901(3) . ?
Cl1 C35 1.754(5) . ?
Cl2 C35 1.760(5) . ?
F5 C22 1.347(4) . ?
F15 C34 1.345(4) . ?
F11 C30 1.352(4) . ?
F7 C25 1.345(4) . ?
F6 C24 1.359(4) . ?
F14 C33 1.348(4) . ?
F1 C18 1.355(4) . ?
F10 C28 1.351(4) . ?
F4 C21 1.349(4) . ?
F9 C27 1.341(4) . ?
F8 C26 1.335(4) . ?
F2 C19 1.334(4) . ?
F12 C31 1.347(4) . ?
F3 C20 1.339(4) . ?
F13 C32 1.345(4) . ?
O1 B1 1.475(4) . ?
N1 C1 1.355(4) . ?
N1 C8 1.466(4) . ?
N2 C7 1.342(4) . ?
N2 C12 1.481(4) . ?
C33 C32 1.371(5) . ?
C33 C34 1.388(5) . ?
C17 C18 1.385(5) . ?
C17 C22 1.396(5) . ?
C17 B1 1.648(5) . ?
C18 C19 1.379(5) . ?
C32 C31 1.378(5) . ?
C24 C23 1.382(5) . ?
C24 C25 1.389(5) . ?
C4 C3 1.376(5) . ?
C4 C5 1.400(5) . ?
C4 H4 0.9500 . ?
C25 C26 1.376(5) . ?
C23 C28 1.393(5) . ?
C23 B1 1.656(5) . ?
C8 C9 1.517(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C1 C2 1.391(5) . ?
C1 C7 1.471(5) . ?
C12 C13 1.525(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C14 C13 1.521(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C34 C29 1.388(5) . ?
C30 C31 1.374(5) . ?
C30 C29 1.392(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C22 C21 1.384(5) . ?
C20 C21 1.364(5) . ?
C20 C19 1.388(6) . ?
C29 B1 1.663(5) . ?
C3 C2 1.386(5) . ?
C3 H3 0.9500 . ?
C27 C26 1.368(6) . ?
C27 C28 1.381(5) . ?
C2 H2 0.9500 . ?
C9 C10 1.514(6) . ?
C9 C11 1.518(5) . ?
C9 H9 1.0000 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.407(5) . ?
C6 H6 0.9500 . ?
C13 C15 1.531(5) . ?
C13 H13 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O1 Ge1 N1 118.29(12) . . ?
O1 Ge1 N2 108.96(12) . . ?
N1 Ge1 N2 85.43(12) . . ?
O1 Ge1 C16 110.17(14) . . ?
N1 Ge1 C16 114.15(14) . . ?
N2 Ge1 C16 118.09(15) . . ?
B1 O1 Ge1 133.7(2) . . ?
C1 N1 C8 123.5(3) . . ?
C1 N1 Ge1 113.1(2) . . ?
C8 N1 Ge1 123.5(2) . . ?
C7 N2 C12 125.3(3) . . ?
C7 N2 Ge1 113.9(2) . . ?
C12 N2 Ge1 120.2(2) . . ?
F14 C33 C32 120.0(3) . . ?
F14 C33 C34 120.2(3) . . ?
C32 C33 C34 119.8(3) . . ?
C18 C17 C22 112.9(3) . . ?
C18 C17 B1 120.4(3) . . ?
C22 C17 B1 126.6(3) . . ?
F1 C18 C19 115.2(3) . . ?
F1 C18 C17 119.3(3) . . ?
C19 C18 C17 125.5(3) . . ?
F13 C32 C33 120.5(3) . . ?
F13 C32 C31 120.7(3) . . ?
C33 C32 C31 118.8(3) . . ?
F6 C24 C23 121.7(3) . . ?
F6 C24 C25 114.1(3) . . ?
C23 C24 C25 124.2(3) . . ?
C3 C4 C5 125.4(3) . . ?
C3 C4 H4 117.3 . . ?
C5 C4 H4 117.3 . . ?
F7 C25 C26 119.8(3) . . ?
F7 C25 C24 120.2(3) . . ?
C26 C25 C24 119.9(3) . . ?
C24 C23 C28 113.0(3) . . ?
C24 C23 B1 126.0(3) . . ?
C28 C23 B1 120.9(3) . . ?
N1 C8 C9 114.0(3) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N1 C1 C2 120.8(3) . . ?
N1 C1 C7 113.0(3) . . ?
C2 C1 C7 126.2(3) . . ?
N2 C12 C13 113.5(3) . . ?
N2 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
Ge1 C16 H16A 109.5 . . ?
Ge1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Ge1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
F15 C34 C29 120.8(3) . . ?
F15 C34 C33 115.4(3) . . ?
C29 C34 C33 123.8(3) . . ?
F11 C30 C31 114.6(3) . . ?
F11 C30 C29 121.1(3) . . ?
C31 C30 C29 124.3(3) . . ?
Cl1 C35 Cl2 112.2(3) . . ?
Cl1 C35 H35A 109.2 . . ?
Cl2 C35 H35A 109.2 . . ?
Cl1 C35 H35B 109.2 . . ?
Cl2 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
F5 C22 C21 116.0(3) . . ?
F5 C22 C17 120.3(3) . . ?
C21 C22 C17 123.7(3) . . ?
F12 C31 C30 120.7(3) . . ?
F12 C31 C32 119.6(3) . . ?
C30 C31 C32 119.7(3) . . ?
F3 C20 C21 121.2(4) . . ?
F3 C20 C19 119.9(4) . . ?
C21 C20 C19 118.9(3) . . ?
C34 C29 C30 113.6(3) . . ?
C34 C29 B1 119.7(3) . . ?
C30 C29 B1 126.6(3) . . ?
C4 C3 C2 130.6(3) . . ?
C4 C3 H3 114.7 . . ?
C2 C3 H3 114.7 . . ?
F9 C27 C26 119.7(3) . . ?
F9 C27 C28 120.4(4) . . ?
C26 C27 C28 119.9(3) . . ?
F10 C28 C27 116.1(3) . . ?
F10 C28 C23 119.3(3) . . ?
C27 C28 C23 124.6(3) . . ?
C3 C2 C1 130.8(3) . . ?
C3 C2 H2 114.6 . . ?
C1 C2 H2 114.6 . . ?
C10 C9 C8 113.0(3) . . ?
C10 C9 C11 110.2(4) . . ?
C8 C9 C11 108.3(3) . . ?
C10 C9 H9 108.4 . . ?
C8 C9 H9 108.4 . . ?
C11 C9 H9 108.4 . . ?
F8 C26 C27 121.2(3) . . ?
F8 C26 C25 120.4(4) . . ?
C27 C26 C25 118.4(3) . . ?
F4 C21 C20 119.7(3) . . ?
F4 C21 C22 119.9(3) . . ?
C20 C21 C22 120.4(3) . . ?
C6 C5 C4 130.1(4) . . ?
C6 C5 H5 114.9 . . ?
C4 C5 H5 114.9 . . ?
C5 C6 C7 131.3(3) . . ?
C5 C6 H6 114.3 . . ?
C7 C6 H6 114.3 . . ?
F2 C19 C18 121.6(3) . . ?
F2 C19 C20 119.9(3) . . ?
C18 C19 C20 118.5(3) . . ?
C14 C13 C12 113.0(3) . . ?
C14 C13 C15 111.1(3) . . ?
C12 C13 C15 108.2(3) . . ?
C14 C13 H13 108.1 . . ?
C12 C13 H13 108.1 . . ?
C15 C13 H13 108.1 . . ?
N2 C7 C6 122.6(3) . . ?
N2 C7 C1 113.0(3) . . ?
C6 C7 C1 124.5(3) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 B1 C17 109.1(3) . . ?
O1 B1 C23 111.4(3) . . ?
C17 B1 C23 113.2(3) . . ?
O1 B1 C29 106.3(3) . . ?
C17 B1 C29 112.4(3) . . ?
C23 B1 C29 104.3(3) . . ?

_refine_diff_density_max         0.521
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_Compound_9__sharma5m
_database_code_depnum_ccdc_archive 'CCDC 1564830'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H62 Ge2 N6 O2'
_chemical_formula_sum            'C44 H62 Ge2 N6 O2'
_chemical_formula_weight         852.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9207(10)
_cell_length_b                   12.9316(11)
_cell_length_c                   14.5928(12)
_cell_angle_alpha                69.9910(10)
_cell_angle_beta                 89.472(2)
_cell_angle_gamma                71.2250(10)
_cell_volume                     2155.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6685
_cell_measurement_theta_min      2.742
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11344
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7473
_reflns_number_gt                6499
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0557P)²+0.3026P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7473
_refine_ls_number_parameters     497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.524789(18) 0.575349(19) 0.419806(16) 0.03063(9) Uani 1 1 d . . .
Ge2 Ge 0.061182(18) 0.437105(19) 0.088696(16) 0.03101(9) Uani 1 1 d . . .
O1 O 0.43992(13) 0.58324(13) 0.51750(11) 0.0363(4) Uani 1 1 d . . .
O2 O -0.02038(14) 0.41360(13) 0.00363(11) 0.0373(4) Uani 1 1 d . . .
N1 N 0.45070(15) 0.74453(16) 0.34668(13) 0.0305(4) Uani 1 1 d . . .
N4 N 0.01780(15) 0.49086(16) 0.19514(13) 0.0336(4) Uani 1 1 d . . .
N2 N 0.49188(15) 0.57340(16) 0.29212(13) 0.0325(4) Uani 1 1 d . . .
N5 N 0.06373(15) 0.28868(16) 0.19179(14) 0.0349(4) Uani 1 1 d . . .
N6 N 0.21100(16) 0.38933(18) 0.07605(14) 0.0417(5) Uani 1 1 d . . .
N3 N 0.66179(16) 0.58836(17) 0.44272(14) 0.0377(4) Uani 1 1 d . . .
C7 C 0.44850(18) 0.67763(19) 0.21866(16) 0.0323(5) Uani 1 1 d . . .
C8 C 0.44130(19) 0.82564(19) 0.39815(17) 0.0349(5) Uani 1 1 d . . .
H8A H 0.4825 0.8764 0.3665 0.042 Uiso 1 1 calc R . .
H8B H 0.4766 0.7805 0.4647 0.042 Uiso 1 1 calc R . .
C1 C 0.42818(18) 0.7775(2) 0.25137(16) 0.0335(5) Uani 1 1 d . . .
C40 C 0.3773(2) 0.2049(2) 0.31598(18) 0.0431(6) Uani 1 1 d . . .
H40 H 0.3747 0.1985 0.3813 0.052 Uiso 1 1 calc R . .
C39 C 0.29409(19) 0.2902(2) 0.24582(17) 0.0382(5) Uani 1 1 d . . .
H39 H 0.2365 0.3410 0.2647 0.046 Uiso 1 1 calc R . .
C6 C 0.4257(2) 0.6868(2) 0.12199(17) 0.0403(6) Uani 1 1 d . . .
H6 H 0.4425 0.6153 0.1135 0.048 Uiso 1 1 calc R . .
C5 C 0.3822(2) 0.7840(3) 0.03624(19) 0.0532(7) Uani 1 1 d . . .
H5 H 0.3705 0.7670 -0.0190 0.064 Uiso 1 1 calc R . .
C43 C 0.3841(2) 0.2243(2) 0.12278(19) 0.0421(6) Uani 1 1 d . . .
H43 H 0.3878 0.2297 0.0577 0.051 Uiso 1 1 calc R . .
C9 C 0.5171(2) 0.4641(2) 0.27309(17) 0.0357(5) Uani 1 1 d . . .
H9A H 0.4553 0.4694 0.2323 0.043 Uiso 1 1 calc R . .
H9B H 0.5257 0.4003 0.3349 0.043 Uiso 1 1 calc R . .
C27 C 0.0257(3) 0.1770(3) 0.4556(2) 0.0585(8) Uani 1 1 d . . .
H27 H 0.0394 0.0999 0.4967 0.070 Uiso 1 1 calc R . .
C11 C 0.6214(2) 0.4358(2) 0.22229(18) 0.0392(5) Uani 1 1 d . . .
H11 H 0.6216 0.5086 0.1715 0.047 Uiso 1 1 calc R . .
C2 C 0.3939(2) 0.8967(2) 0.18888(18) 0.0445(6) Uani 1 1 d . . .
H2 H 0.3928 0.9483 0.2206 0.053 Uiso 1 1 calc R . .
C38 C 0.29461(18) 0.3018(2) 0.14723(17) 0.0350(5) Uani 1 1 d . . .
C29 C 0.04172(18) 0.2920(2) 0.27853(16) 0.0358(5) Uani 1 1 d . . .
C16 C 0.69301(18) 0.6817(2) 0.38369(17) 0.0367(5) Uani 1 1 d . . .
C30 C -0.00914(19) 0.6140(2) 0.18369(18) 0.0383(5) Uani 1 1 d . . .
H30A H -0.0753 0.6372 0.2144 0.046 Uiso 1 1 calc R . .
H30B H -0.0251 0.6612 0.1143 0.046 Uiso 1 1 calc R . .
C10 C 0.3255(2) 0.9027(2) 0.40362(18) 0.0422(6) Uani 1 1 d . . .
H10 H 0.3039 0.9729 0.3440 0.051 Uiso 1 1 calc R . .
C23 C 0.01176(17) 0.4112(2) 0.28120(16) 0.0353(5) Uani 1 1 d . . .
C17 C 0.68204(19) 0.7123(2) 0.28132(18) 0.0405(6) Uani 1 1 d . . .
H17 H 0.6585 0.6670 0.2543 0.049 Uiso 1 1 calc R . .
C31 C 0.0943(2) 0.1831(2) 0.16678(19) 0.0449(6) Uani 1 1 d . . .
H31A H 0.1351 0.1168 0.2242 0.054 Uiso 1 1 calc R . .
H31B H 0.1433 0.1907 0.1160 0.054 Uiso 1 1 calc R . .
C28 C 0.0511(2) 0.1908(2) 0.36146(18) 0.0486(6) Uani 1 1 d . . .
H28 H 0.0795 0.1210 0.3501 0.058 Uiso 1 1 calc R . .
C24 C -0.0224(2) 0.4424(3) 0.36247(19) 0.0474(6) Uani 1 1 d . . .
H24 H -0.0383 0.5213 0.3519 0.057 Uiso 1 1 calc R . .
C22 C 0.7069(2) 0.5370(3) 0.54662(19) 0.0527(7) Uani 1 1 d . . .
H22A H 0.7834 0.5286 0.5517 0.079 Uiso 1 1 calc R . .
H22B H 0.6989 0.4616 0.5758 0.079 Uiso 1 1 calc R . .
H22C H 0.6678 0.5873 0.5803 0.079 Uiso 1 1 calc R . .
C32 C 0.0815(2) 0.6401(2) 0.2278(2) 0.0466(6) Uani 1 1 d . . .
H32 H 0.1048 0.5840 0.2952 0.056 Uiso 1 1 calc R . .
C26 C -0.0163(3) 0.2583(3) 0.4987(2) 0.0658(9) Uani 1 1 d . . .
H26 H -0.0326 0.2309 0.5629 0.079 Uiso 1 1 calc R . .
C25 C -0.0364(2) 0.3752(3) 0.4566(2) 0.0610(8) Uani 1 1 d . . .
H25 H -0.0641 0.4175 0.4970 0.073 Uiso 1 1 calc R . .
C20 C 0.7576(2) 0.8440(3) 0.3575(2) 0.0591(8) Uani 1 1 d . . .
H20 H 0.7848 0.8877 0.3836 0.071 Uiso 1 1 calc R . .
C13 C 0.2407(2) 0.8433(3) 0.4103(2) 0.0552(7) Uani 1 1 d . . .
H13A H 0.2640 0.7703 0.4647 0.083 Uiso 1 1 calc R . .
H13B H 0.2330 0.8292 0.3507 0.083 Uiso 1 1 calc R . .
H13C H 0.1713 0.8928 0.4197 0.083 Uiso 1 1 calc R . .
C21 C 0.7344(2) 0.7493(2) 0.4202(2) 0.0483(6) Uani 1 1 d . . .
H21 H 0.7464 0.7298 0.4877 0.058 Uiso 1 1 calc R . .
C42 C 0.4668(2) 0.1400(2) 0.1937(2) 0.0475(6) Uani 1 1 d . . .
H42 H 0.5254 0.0896 0.1756 0.057 Uiso 1 1 calc R . .
C18 C 0.7053(2) 0.8076(2) 0.2203(2) 0.0513(7) Uani 1 1 d . . .
H18 H 0.6963 0.8264 0.1527 0.062 Uiso 1 1 calc R . .
C41 C 0.4644(2) 0.1291(2) 0.2901(2) 0.0466(6) Uani 1 1 d . . .
H41 H 0.5204 0.0716 0.3375 0.056 Uiso 1 1 calc R . .
C15 C 0.7251(2) 0.3882(3) 0.2932(2) 0.0544(7) Uani 1 1 d . . .
H15A H 0.7233 0.4421 0.3255 0.082 Uiso 1 1 calc R . .
H15B H 0.7883 0.3784 0.2577 0.082 Uiso 1 1 calc R . .
H15C H 0.7293 0.3140 0.3413 0.082 Uiso 1 1 calc R . .
C19 C 0.7417(2) 0.8757(3) 0.2576(2) 0.0577(8) Uani 1 1 d . . .
H19 H 0.7552 0.9416 0.2161 0.069 Uiso 1 1 calc R . .
C14 C 0.6198(3) 0.3510(3) 0.1722(3) 0.0665(9) Uani 1 1 d . . .
H14A H 0.6176 0.2794 0.2204 0.100 Uiso 1 1 calc R . .
H14B H 0.6849 0.3349 0.1398 0.100 Uiso 1 1 calc R . .
H14C H 0.5559 0.3849 0.1248 0.100 Uiso 1 1 calc R . .
C33 C -0.0009(3) 0.1571(2) 0.1316(2) 0.0615(8) Uani 1 1 d . . .
H33 H -0.0502 0.2302 0.0833 0.074 Uiso 1 1 calc R . .
C35 C 0.0369(3) 0.7618(3) 0.2315(3) 0.0755(10) Uani 1 1 d . . .
H35A H 0.0947 0.7787 0.2580 0.113 Uiso 1 1 calc R . .
H35B H -0.0217 0.7662 0.2725 0.113 Uiso 1 1 calc R . .
H35C H 0.0095 0.8177 0.1664 0.113 Uiso 1 1 calc R . .
C34 C 0.1803(3) 0.6275(3) 0.1716(3) 0.0667(9) Uani 1 1 d . . .
H34A H 0.2054 0.5512 0.1672 0.100 Uiso 1 1 calc R . .
H34B H 0.2380 0.6374 0.2051 0.100 Uiso 1 1 calc R . .
H34C H 0.1606 0.6859 0.1068 0.100 Uiso 1 1 calc R . .
C3 C 0.3619(3) 0.9495(2) 0.0896(2) 0.0619(8) Uani 1 1 d . . .
H3 H 0.3426 1.0305 0.0651 0.074 Uiso 1 1 calc R . .
C12 C 0.3294(3) 0.9404(3) 0.4912(2) 0.0583(7) Uani 1 1 d . . .
H12A H 0.2608 0.9996 0.4894 0.087 Uiso 1 1 calc R . .
H12B H 0.3882 0.9713 0.4886 0.087 Uiso 1 1 calc R . .
H12C H 0.3418 0.8742 0.5509 0.087 Uiso 1 1 calc R . .
C44 C 0.2385(2) 0.4221(3) -0.0248(2) 0.0711(10) Uani 1 1 d . . .
H44A H 0.3112 0.4267 -0.0256 0.107 Uiso 1 1 calc R . .
H44B H 0.1865 0.4968 -0.0639 0.107 Uiso 1 1 calc R . .
H44C H 0.2358 0.3643 -0.0511 0.107 Uiso 1 1 calc R . .
C4 C 0.3542(3) 0.9004(3) 0.0208(2) 0.0691(9) Uani 1 1 d . . .
H4 H 0.3271 0.9521 -0.0430 0.083 Uiso 1 1 calc R . .
C37 C -0.0681(3) 0.1121(3) 0.2110(3) 0.0781(10) Uani 1 1 d . . .
H37A H -0.1283 0.1008 0.1825 0.117 Uiso 1 1 calc R . .
H37B H -0.0962 0.1680 0.2426 0.117 Uiso 1 1 calc R . .
H37C H -0.0224 0.0390 0.2585 0.117 Uiso 1 1 calc R . .
C36 C 0.0427(4) 0.0711(3) 0.0791(3) 0.0954(13) Uani 1 1 d . . .
H36A H 0.0807 0.1033 0.0259 0.143 Uiso 1 1 calc R . .
H36B H -0.0176 0.0567 0.0539 0.143 Uiso 1 1 calc R . .
H36C H 0.0925 -0.0011 0.1244 0.143 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.8011(15) . ?
Ge1 O1 1.8365(15) 2_666 ?
Ge1 N3 1.8747(19) . ?
Ge1 N2 1.9253(18) . ?
Ge1 N1 1.9785(18) . ?
Ge1 Ge1 2.7093(5) 2_666 ?
Ge2 O2 1.7979(16) . ?
Ge2 O2 1.8435(15) 2_565 ?
Ge2 N6 1.8613(19) . ?
Ge2 N4 1.9189(18) . ?
Ge2 N5 1.9831(18) . ?
Ge2 Ge2 2.7176(5) 2_565 ?
O1 Ge1 1.8365(15) 2_666 ?
O2 Ge2 1.8435(15) 2_565 ?
N1 C1 1.312(3) . ?
N1 C8 1.461(3) . ?
N4 C23 1.345(3) . ?
N4 C30 1.465(3) . ?
N2 C7 1.348(3) . ?
N2 C9 1.467(3) . ?
N5 C29 1.307(3) . ?
N5 C31 1.464(3) . ?
N6 C38 1.399(3) . ?
N6 C44 1.460(3) . ?
N3 C16 1.399(3) . ?
N3 C22 1.469(3) . ?
C7 C6 1.401(3) . ?
C7 C1 1.472(3) . ?
C8 C10 1.527(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C1 C2 1.418(3) . ?
C40 C41 1.380(4) . ?
C40 C39 1.380(3) . ?
C40 H40 0.9300 . ?
C39 C38 1.395(3) . ?
C39 H39 0.9300 . ?
C6 C5 1.395(3) . ?
C6 H6 0.9300 . ?
C5 C4 1.366(4) . ?
C5 H5 0.9300 . ?
C43 C42 1.378(4) . ?
C43 C38 1.400(3) . ?
C43 H43 0.9300 . ?
C9 C11 1.533(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C27 C26 1.369(5) . ?
C27 C28 1.374(4) . ?
C27 H27 0.9300 . ?
C11 C14 1.516(3) . ?
C11 C15 1.518(4) . ?
C11 H11 0.9800 . ?
C2 C3 1.374(4) . ?
C2 H2 0.9300 . ?
C29 C28 1.417(3) . ?
C29 C23 1.477(3) . ?
C16 C21 1.399(4) . ?
C16 C17 1.404(3) . ?
C30 C32 1.522(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C10 C13 1.512(4) . ?
C10 C12 1.523(4) . ?
C10 H10 0.9800 . ?
C23 C24 1.403(3) . ?
C17 C18 1.373(4) . ?
C17 H17 0.9300 . ?
C31 C33 1.513(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C28 H28 0.9300 . ?
C24 C25 1.398(4) . ?
C24 H24 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C32 C34 1.505(4) . ?
C32 C35 1.512(4) . ?
C32 H32 0.9800 . ?
C26 C25 1.358(5) . ?
C26 H26 0.9300 . ?
C25 H25 0.9300 . ?
C20 C19 1.370(4) . ?
C20 C21 1.376(4) . ?
C20 H20 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C21 H21 0.9300 . ?
C42 C41 1.366(4) . ?
C42 H42 0.9300 . ?
C18 C19 1.376(4) . ?
C18 H18 0.9300 . ?
C41 H41 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C19 H19 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C33 C37 1.510(5) . ?
C33 C36 1.521(4) . ?
C33 H33 0.9800 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C3 C4 1.378(4) . ?
C3 H3 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C4 H4 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

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
O1 Ge1 O1 83.72(7) . 2_666 ?
O1 Ge1 N3 113.28(8) . . ?
O1 Ge1 N3 99.05(8) 2_666 . ?
O1 Ge1 N2 130.71(8) . . ?
O1 Ge1 N2 94.57(7) 2_666 . ?
N3 Ge1 N2 115.59(8) . . ?
O1 Ge1 N1 90.38(7) . . ?
O1 Ge1 N1 165.99(7) 2_666 . ?
N3 Ge1 N1 94.95(8) . . ?
N2 Ge1 N1 79.66(7) . . ?
O1 Ge1 Ge1 42.36(5) . 2_666 ?
O1 Ge1 Ge1 41.36(5) 2_666 2_666 ?
N3 Ge1 Ge1 111.67(6) . 2_666 ?
N2 Ge1 Ge1 119.18(6) . 2_666 ?
N1 Ge1 Ge1 131.46(5) . 2_666 ?
O2 Ge2 O2 83.46(7) . 2_565 ?
O2 Ge2 N6 113.64(9) . . ?
O2 Ge2 N6 98.67(8) 2_565 . ?
O2 Ge2 N4 129.51(8) . . ?
O2 Ge2 N4 93.51(7) 2_565 . ?
N6 Ge2 N4 116.62(9) . . ?
O2 Ge2 N5 90.43(7) . . ?
O2 Ge2 N5 165.10(8) 2_565 . ?
N6 Ge2 N5 96.23(8) . . ?
N4 Ge2 N5 79.89(8) . . ?
O2 Ge2 Ge2 42.37(5) . 2_565 ?
O2 Ge2 Ge2 41.09(5) 2_565 2_565 ?
N6 Ge2 Ge2 111.56(6) . 2_565 ?
N4 Ge2 Ge2 117.55(6) . 2_565 ?
N5 Ge2 Ge2 131.34(6) . 2_565 ?
Ge1 O1 Ge1 96.28(7) . 2_666 ?
Ge2 O2 Ge2 96.54(7) . 2_565 ?
C1 N1 C8 123.78(19) . . ?
C1 N1 Ge1 116.99(15) . . ?
C8 N1 Ge1 118.39(14) . . ?
C23 N4 C30 120.80(19) . . ?
C23 N4 Ge2 117.44(15) . . ?
C30 N4 Ge2 121.75(15) . . ?
C7 N2 C9 120.56(19) . . ?
C7 N2 Ge1 117.19(15) . . ?
C9 N2 Ge1 122.19(15) . . ?
C29 N5 C31 124.9(2) . . ?
C29 N5 Ge2 116.99(16) . . ?
C31 N5 Ge2 118.11(15) . . ?
C38 N6 C44 116.1(2) . . ?
C38 N6 Ge2 126.47(15) . . ?
C44 N6 Ge2 114.99(17) . . ?
C16 N3 C22 116.3(2) . . ?
C16 N3 Ge1 122.63(15) . . ?
C22 N3 Ge1 113.95(16) . . ?
N2 C7 C6 122.1(2) . . ?
N2 C7 C1 113.03(19) . . ?
C6 C7 C1 124.8(2) . . ?
N1 C8 C10 117.13(19) . . ?
N1 C8 H8A 108.0 . . ?
C10 C8 H8A 108.0 . . ?
N1 C8 H8B 108.0 . . ?
C10 C8 H8B 108.0 . . ?
H8A C8 H8B 107.3 . . ?
N1 C1 C2 122.2(2) . . ?
N1 C1 C7 112.39(19) . . ?
C2 C1 C7 125.3(2) . . ?
C41 C40 C39 120.7(2) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C39 C38 121.3(2) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C5 C6 C7 131.4(2) . . ?
C5 C6 H6 114.3 . . ?
C7 C6 H6 114.3 . . ?
C4 C5 C6 130.0(3) . . ?
C4 C5 H5 115.0 . . ?
C6 C5 H5 115.0 . . ?
C42 C43 C38 121.0(2) . . ?
C42 C43 H43 119.5 . . ?
C38 C43 H43 119.5 . . ?
N2 C9 C11 113.57(18) . . ?
N2 C9 H9A 108.9 . . ?
C11 C9 H9A 108.9 . . ?
N2 C9 H9B 108.9 . . ?
C11 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C26 C27 C28 130.5(3) . . ?
C26 C27 H27 114.7 . . ?
C28 C27 H27 114.7 . . ?
C14 C11 C15 110.9(2) . . ?
C14 C11 C9 110.2(2) . . ?
C15 C11 C9 111.9(2) . . ?
C14 C11 H11 107.9 . . ?
C15 C11 H11 107.9 . . ?
C9 C11 H11 107.9 . . ?
C3 C2 C1 131.3(3) . . ?
C3 C2 H2 114.4 . . ?
C1 C2 H2 114.4 . . ?
C39 C38 N6 121.2(2) . . ?
C39 C38 C43 116.9(2) . . ?
N6 C38 C43 121.8(2) . . ?
N5 C29 C28 123.1(2) . . ?
N5 C29 C23 112.6(2) . . ?
C28 C29 C23 124.2(2) . . ?
C21 C16 N3 123.9(2) . . ?
C21 C16 C17 116.7(2) . . ?
N3 C16 C17 119.4(2) . . ?
N4 C30 C32 114.13(19) . . ?
N4 C30 H30A 108.7 . . ?
C32 C30 H30A 108.7 . . ?
N4 C30 H30B 108.7 . . ?
C32 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
C13 C10 C12 110.9(2) . . ?
C13 C10 C8 113.2(2) . . ?
C12 C10 C8 108.2(2) . . ?
C13 C10 H10 108.1 . . ?
C12 C10 H10 108.1 . . ?
C8 C10 H10 108.1 . . ?
N4 C23 C24 121.7(2) . . ?
N4 C23 C29 112.96(19) . . ?
C24 C23 C29 125.3(2) . . ?
C18 C17 C16 121.3(2) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
N5 C31 C33 115.2(2) . . ?
N5 C31 H31A 108.5 . . ?
C33 C31 H31A 108.5 . . ?
N5 C31 H31B 108.5 . . ?
C33 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C27 C28 C29 131.7(3) . . ?
C27 C28 H28 114.1 . . ?
C29 C28 H28 114.1 . . ?
C25 C24 C23 131.0(3) . . ?
C25 C24 H24 114.5 . . ?
C23 C24 H24 114.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C34 C32 C35 110.5(2) . . ?
C34 C32 C30 112.1(2) . . ?
C35 C32 C30 109.6(2) . . ?
C34 C32 H32 108.2 . . ?
C35 C32 H32 108.2 . . ?
C30 C32 H32 108.2 . . ?
C25 C26 C27 126.2(3) . . ?
C25 C26 H26 116.9 . . ?
C27 C26 H26 116.9 . . ?
C26 C25 C24 130.6(3) . . ?
C26 C25 H25 114.7 . . ?
C24 C25 H25 114.7 . . ?
C19 C20 C21 121.7(3) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C20 C21 C16 120.8(3) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
C41 C42 C43 121.3(2) . . ?
C41 C42 H42 119.4 . . ?
C43 C42 H42 119.4 . . ?
C17 C18 C19 121.0(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C42 C41 C40 118.8(2) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C19 C18 118.4(3) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C37 C33 C31 114.6(3) . . ?
C37 C33 C36 110.4(3) . . ?
C31 C33 C36 108.9(3) . . ?
C37 C33 H33 107.6 . . ?
C31 C33 H33 107.6 . . ?
C36 C33 H33 107.6 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C2 C3 C4 129.8(3) . . ?
C2 C3 H3 115.1 . . ?
C4 C3 H3 115.1 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N6 C44 H44A 109.5 . . ?
N6 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N6 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C5 C4 C3 126.9(3) . . ?
C5 C4 H4 116.5 . . ?
C3 C4 H4 116.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ge1 O1 Ge1 0.0 2_666 . . 2_666 ?
N3 Ge1 O1 Ge1 -97.17(9) . . . 2_666 ?
N2 Ge1 O1 Ge1 90.63(10) . . . 2_666 ?
N1 Ge1 O1 Ge1 167.27(8) . . . 2_666 ?
O2 Ge2 O2 Ge2 0.0 2_565 . . 2_565 ?
N6 Ge2 O2 Ge2 -96.63(9) . . . 2_565 ?
N4 Ge2 O2 Ge2 89.16(10) . . . 2_565 ?
N5 Ge2 O2 Ge2 166.38(8) . . . 2_565 ?
O1 Ge1 N1 C1 -139.57(17) . . . . ?
O1 Ge1 N1 C1 -74.8(3) 2_666 . . . ?
N3 Ge1 N1 C1 107.01(17) . . . . ?
N2 Ge1 N1 C1 -8.13(16) . . . . ?
Ge1 Ge1 N1 C1 -128.15(14) 2_666 . . . ?
O1 Ge1 N1 C8 50.46(16) . . . . ?
O1 Ge1 N1 C8 115.3(3) 2_666 . . . ?
N3 Ge1 N1 C8 -62.96(17) . . . . ?
N2 Ge1 N1 C8 -178.10(17) . . . . ?
Ge1 Ge1 N1 C8 61.88(18) 2_666 . . . ?
O2 Ge2 N4 C23 83.09(18) . . . . ?
O2 Ge2 N4 C23 167.52(16) 2_565 . . . ?
N6 Ge2 N4 C23 -90.97(17) . . . . ?
N5 Ge2 N4 C23 0.98(16) . . . . ?
Ge2 Ge2 N4 C23 132.56(14) 2_565 . . . ?
O2 Ge2 N4 C30 -96.21(18) . . . . ?
O2 Ge2 N4 C30 -11.79(17) 2_565 . . . ?
N6 Ge2 N4 C30 89.73(18) . . . . ?
N5 Ge2 N4 C30 -178.33(17) . . . . ?
Ge2 Ge2 N4 C30 -46.74(18) 2_565 . . . ?
O1 Ge1 N2 C7 87.31(18) . . . . ?
O1 Ge1 N2 C7 172.95(16) 2_666 . . . ?
N3 Ge1 N2 C7 -84.74(17) . . . . ?
N1 Ge1 N2 C7 5.83(16) . . . . ?
Ge1 Ge1 N2 C7 137.82(14) 2_666 . . . ?
O1 Ge1 N2 C9 -95.49(17) . . . . ?
O1 Ge1 N2 C9 -9.85(17) 2_666 . . . ?
N3 Ge1 N2 C9 92.46(17) . . . . ?
N1 Ge1 N2 C9 -176.97(17) . . . . ?
Ge1 Ge1 N2 C9 -44.98(18) 2_666 . . . ?
O2 Ge2 N5 C29 -132.79(17) . . . . ?
O2 Ge2 N5 C29 -67.3(3) 2_565 . . . ?
N6 Ge2 N5 C29 113.38(18) . . . . ?
N4 Ge2 N5 C29 -2.62(17) . . . . ?
Ge2 Ge2 N5 C29 -120.58(15) 2_565 . . . ?
O2 Ge2 N5 C31 49.69(18) . . . . ?
O2 Ge2 N5 C31 115.2(3) 2_565 . . . ?
N6 Ge2 N5 C31 -64.14(18) . . . . ?
N4 Ge2 N5 C31 179.86(18) . . . . ?
Ge2 Ge2 N5 C31 61.90(19) 2_565 . . . ?
O2 Ge2 N6 C38 -117.5(2) . . . . ?
O2 Ge2 N6 C38 155.9(2) 2_565 . . . ?
N4 Ge2 N6 C38 57.5(2) . . . . ?
N5 Ge2 N6 C38 -24.3(2) . . . . ?
Ge2 Ge2 N6 C38 -163.55(18) 2_565 . . . ?
O2 Ge2 N6 C44 43.8(2) . . . . ?
O2 Ge2 N6 C44 -42.8(2) 2_565 . . . ?
N4 Ge2 N6 C44 -141.2(2) . . . . ?
N5 Ge2 N6 C44 137.0(2) . . . . ?
Ge2 Ge2 N6 C44 -2.3(2) 2_565 . . . ?
O1 Ge1 N3 C16 -115.85(17) . . . . ?
O1 Ge1 N3 C16 157.14(17) 2_666 . . . ?
N2 Ge1 N3 C16 57.6(2) . . . . ?
N1 Ge1 N3 C16 -23.29(19) . . . . ?
Ge1 Ge1 N3 C16 -161.85(16) 2_666 . . . ?
O1 Ge1 N3 C22 33.4(2) . . . . ?
O1 Ge1 N3 C22 -53.62(18) 2_666 . . . ?
N2 Ge1 N3 C22 -153.15(17) . . . . ?
N1 Ge1 N3 C22 125.95(18) . . . . ?
Ge1 Ge1 N3 C22 -12.60(19) 2_666 . . . ?
C9 N2 C7 C6 0.0(3) . . . . ?
Ge1 N2 C7 C6 177.23(17) . . . . ?
C9 N2 C7 C1 179.73(18) . . . . ?
Ge1 N2 C7 C1 -3.0(2) . . . . ?
C1 N1 C8 C10 69.7(3) . . . . ?
Ge1 N1 C8 C10 -121.10(18) . . . . ?
C8 N1 C1 C2 1.0(3) . . . . ?
Ge1 N1 C1 C2 -168.34(18) . . . . ?
C8 N1 C1 C7 177.95(19) . . . . ?
Ge1 N1 C1 C7 8.6(2) . . . . ?
N2 C7 C1 N1 -3.6(3) . . . . ?
C6 C7 C1 N1 176.1(2) . . . . ?
N2 C7 C1 C2 173.2(2) . . . . ?
C6 C7 C1 C2 -7.1(4) . . . . ?
C41 C40 C39 C38 0.7(4) . . . . ?
N2 C7 C6 C5 -179.6(3) . . . . ?
C1 C7 C6 C5 0.7(4) . . . . ?
C7 C6 C5 C4 3.9(5) . . . . ?
C7 N2 C9 C11 75.8(3) . . . . ?
Ge1 N2 C9 C11 -101.3(2) . . . . ?
N2 C9 C11 C14 -159.2(2) . . . . ?
N2 C9 C11 C15 76.9(3) . . . . ?
N1 C1 C2 C3 -176.6(3) . . . . ?
C7 C1 C2 C3 6.9(5) . . . . ?
C40 C39 C38 N6 -179.1(2) . . . . ?
C40 C39 C38 C43 -1.0(4) . . . . ?
C44 N6 C38 C39 157.8(3) . . . . ?
Ge2 N6 C38 C39 -41.1(3) . . . . ?
C44 N6 C38 C43 -20.2(4) . . . . ?
Ge2 N6 C38 C43 140.9(2) . . . . ?
C42 C43 C38 C39 0.6(4) . . . . ?
C42 C43 C38 N6 178.7(2) . . . . ?
C31 N5 C29 C28 3.7(4) . . . . ?
Ge2 N5 C29 C28 -173.59(18) . . . . ?
C31 N5 C29 C23 -179.1(2) . . . . ?
Ge2 N5 C29 C23 3.6(2) . . . . ?
C22 N3 C16 C21 -19.7(3) . . . . ?
Ge1 N3 C16 C21 128.9(2) . . . . ?
C22 N3 C16 C17 160.9(2) . . . . ?
Ge1 N3 C16 C17 -50.5(3) . . . . ?
C23 N4 C30 C32 78.1(3) . . . . ?
Ge2 N4 C30 C32 -102.6(2) . . . . ?
N1 C8 C10 C13 33.5(3) . . . . ?
N1 C8 C10 C12 156.9(2) . . . . ?
C30 N4 C23 C24 1.3(3) . . . . ?
Ge2 N4 C23 C24 -178.05(18) . . . . ?
C30 N4 C23 C29 179.89(19) . . . . ?
Ge2 N4 C23 C29 0.6(2) . . . . ?
N5 C29 C23 N4 -2.7(3) . . . . ?
C28 C29 C23 N4 174.4(2) . . . . ?
N5 C29 C23 C24 175.9(2) . . . . ?
C28 C29 C23 C24 -7.0(4) . . . . ?
C21 C16 C17 C18 -3.4(4) . . . . ?
N3 C16 C17 C18 176.0(2) . . . . ?
C29 N5 C31 C33 89.5(3) . . . . ?
Ge2 N5 C31 C33 -93.2(2) . . . . ?
C26 C27 C28 C29 -0.5(6) . . . . ?
N5 C29 C28 C27 -175.4(3) . . . . ?
C23 C29 C28 C27 7.8(4) . . . . ?
N4 C23 C24 C25 178.6(3) . . . . ?
C29 C23 C24 C25 0.1(4) . . . . ?
N4 C30 C32 C34 69.0(3) . . . . ?
N4 C30 C32 C35 -167.9(2) . . . . ?
C28 C27 C26 C25 -4.6(6) . . . . ?
C27 C26 C25 C24 1.0(6) . . . . ?
C23 C24 C25 C26 3.4(5) . . . . ?
C19 C20 C21 C16 -0.3(4) . . . . ?
N3 C16 C21 C20 -176.3(2) . . . . ?
C17 C16 C21 C20 3.1(4) . . . . ?
C38 C43 C42 C41 0.1(4) . . . . ?
C16 C17 C18 C19 0.9(4) . . . . ?
C43 C42 C41 C40 -0.4(4) . . . . ?
C39 C40 C41 C42 0.1(4) . . . . ?
C21 C20 C19 C18 -2.3(4) . . . . ?
C17 C18 C19 C20 2.0(4) . . . . ?
N5 C31 C33 C37 -73.4(3) . . . . ?
N5 C31 C33 C36 162.4(2) . . . . ?
C1 C2 C3 C4 -0.2(6) . . . . ?
C6 C5 C4 C3 -0.8(6) . . . . ?
C2 C3 C4 C5 -3.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_Compound_15__sharma8m
_database_code_depnum_ccdc_archive 'CCDC 1564834'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H27 B F15 Ge N3 O, C H2 Cl2'
_chemical_formula_sum            'C38 H29 B Cl2 F15 Ge N3 O'
_chemical_formula_weight         982.96

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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.436(2)
_cell_length_b                   12.462(2)
_cell_length_c                   15.186(3)
_cell_angle_alpha                106.723(4)
_cell_angle_beta                 96.368(3)
_cell_angle_gamma                115.028(3)
_cell_volume                     1967.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2030
_cell_measurement_theta_min      2.295
_cell_measurement_theta_max      23.497

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.443
_exptl_crystal_size_min          0.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984.0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9788
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6771
_reflns_number_gt                4527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0799P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6771
_refine_ls_number_parameters     554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1319
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.91984(5) 0.57684(5) 0.21869(4) 0.02080(17) Uani 1 1 d . . .
Cl2 Cl 0.43962(16) 0.81381(18) 0.42352(13) 0.0595(5) Uani 1 1 d . . .
Cl1 Cl 0.50231(18) 0.8608(2) 0.25627(14) 0.0788(6) Uani 1 1 d . . .
F1 F 0.8508(2) 0.8779(2) 0.38830(18) 0.0232(6) Uani 1 1 d . . .
F14 F 1.3150(2) 1.0746(3) 0.3455(2) 0.0298(7) Uani 1 1 d . . .
F11 F 0.8497(2) 0.9987(2) 0.24705(19) 0.0260(7) Uani 1 1 d . . .
F15 F 1.1334(2) 0.8402(2) 0.26523(19) 0.0262(7) Uani 1 1 d . . .
F5 F 0.6274(2) 0.5370(2) 0.08974(19) 0.0300(7) Uani 1 1 d . . .
F2 F 0.6714(3) 0.7708(3) 0.46218(19) 0.0293(7) Uani 1 1 d . . .
F3 F 0.4652(3) 0.5473(3) 0.3534(2) 0.0359(8) Uani 1 1 d . . .
F9 F 0.9626(3) 0.8546(3) -0.1053(2) 0.0347(8) Uani 1 1 d . . .
F6 F 0.6326(2) 0.7792(3) 0.10498(19) 0.0286(7) Uani 1 1 d . . .
F13 F 1.2721(3) 1.2777(2) 0.3734(2) 0.0333(7) Uani 1 1 d . . .
F12 F 1.0380(3) 1.2371(3) 0.3267(2) 0.0317(7) Uani 1 1 d . . .
F4 F 0.4449(3) 0.4347(3) 0.1657(2) 0.0386(8) Uani 1 1 d . . .
F10 F 1.0078(2) 0.8032(3) 0.04894(19) 0.0296(7) Uani 1 1 d . . .
F8 F 0.7543(3) 0.8701(3) -0.1551(2) 0.0401(8) Uani 1 1 d . . .
F7 F 0.5933(3) 0.8347(3) -0.0462(2) 0.0353(7) Uani 1 1 d . . .
O1 O 0.9033(3) 0.6649(3) 0.1568(2) 0.0209(8) Uani 1 1 d . . .
N2 N 0.9152(3) 0.6165(4) 0.3449(3) 0.0205(9) Uani 1 1 d . . .
N3 N 1.0494(3) 0.5510(4) 0.1964(3) 0.0226(9) Uani 1 1 d . . .
N1 N 0.7817(4) 0.4238(4) 0.1910(3) 0.0226(9) Uani 1 1 d . . .
B1 B 0.8622(5) 0.7638(5) 0.1829(4) 0.0214(13) Uani 1 1 d . . .
C22 C 0.6591(5) 0.7142(5) 0.3691(3) 0.0214(11) Uani 1 1 d . . .
C20 C 0.7490(4) 0.7133(4) 0.2340(3) 0.0190(11) Uani 1 1 d . . .
C23 C 0.5566(4) 0.6030(5) 0.3149(4) 0.0239(12) Uani 1 1 d . . .
C32 C 0.9798(4) 0.9059(4) 0.2495(3) 0.0194(11) Uani 1 1 d . . .
C1 C 0.7345(4) 0.4169(5) 0.2675(4) 0.0215(11) Uani 1 1 d . . .
C25 C 0.6427(4) 0.6012(5) 0.1832(4) 0.0235(11) Uani 1 1 d . . .
C37 C 1.1014(4) 0.9335(4) 0.2776(3) 0.0201(11) Uani 1 1 d . . .
C24 C 0.5466(5) 0.5453(5) 0.2206(4) 0.0279(12) Uani 1 1 d . . .
C21 C 0.7527(4) 0.7687(4) 0.3283(3) 0.0185(11) Uani 1 1 d . . .
C33 C 0.9645(4) 1.0138(5) 0.2703(3) 0.0218(11) Uani 1 1 d . . .
C28 C 0.6947(4) 0.8237(4) -0.0229(3) 0.0232(11) Uani 1 1 d . . .
C31 C 0.9015(4) 0.8055(4) 0.0266(3) 0.0222(11) Uani 1 1 d . . .
C36 C 1.1988(4) 1.0566(5) 0.3213(3) 0.0218(11) Uani 1 1 d . . .
C7 C 0.8099(4) 0.5255(4) 0.3549(4) 0.0214(11) Uani 1 1 d . . .
C8 C 0.7241(5) 0.3296(5) 0.0924(4) 0.0276(12) Uani 1 1 d . . .
H8A H 0.7356 0.3746 0.0488 0.033 Uiso 1 1 calc R . .
H8B H 0.6363 0.2813 0.0840 0.033 Uiso 1 1 calc R . .
C9 C 1.0020(4) 0.7421(4) 0.4186(3) 0.0227(11) Uani 1 1 d . . .
H9A H 0.9655 0.7578 0.4709 0.027 Uiso 1 1 calc R . .
H9B H 1.0140 0.8070 0.3919 0.027 Uiso 1 1 calc R . .
C27 C 0.7182(4) 0.7951(4) 0.0557(3) 0.0205(11) Uani 1 1 d . . .
C30 C 0.8810(5) 0.8340(5) -0.0529(3) 0.0233(11) Uani 1 1 d . . .
C17 C 1.1049(5) 0.5725(5) 0.1245(4) 0.0318(13) Uani 1 1 d . . .
H17 H 1.0894 0.6116 0.0847 0.038 Uiso 1 1 calc R . .
C35A C 1.1779(4) 1.1583(5) 0.3370(3) 0.0244(12) Uani 1 1 d . . .
C34 C 1.0599(5) 1.1372(5) 0.3118(3) 0.0239(12) Uani 1 1 d . . .
C4 C 0.5781(5) 0.3581(5) 0.4148(4) 0.0324(13) Uani 1 1 d . . .
H4 H 0.5176 0.3271 0.4454 0.039 Uiso 1 1 calc R . .
C26 C 0.8209(4) 0.7832(4) 0.0843(3) 0.0186(11) Uani 1 1 d . . .
C5 C 0.6817(5) 0.4686(5) 0.4684(4) 0.0283(13) Uani 1 1 d . . .
H5 H 0.6848 0.5002 0.5326 0.034 Uiso 1 1 calc R . .
C2 C 0.6227(5) 0.3133(5) 0.2566(4) 0.0320(13) Uani 1 1 d . . .
H2 H 0.5884 0.2502 0.1958 0.038 Uiso 1 1 calc R . .
C3 C 0.5535(5) 0.2879(5) 0.3208(4) 0.0361(14) Uani 1 1 d . . .
H3 H 0.4797 0.2118 0.2961 0.043 Uiso 1 1 calc R . .
C10 C 0.7760(5) 0.2364(5) 0.0659(4) 0.0356(14) Uani 1 1 d . . .
H10 H 0.8639 0.2860 0.0718 0.043 Uiso 1 1 calc R . .
C6 C 0.7840(5) 0.5425(5) 0.4431(4) 0.0256(12) Uani 1 1 d . . .
H6 H 0.8448 0.6148 0.4933 0.031 Uiso 1 1 calc R . .
C29 C 0.7773(5) 0.8432(5) -0.0776(3) 0.0272(12) Uani 1 1 d . . .
C14 C 1.1180(5) 0.6668(5) 0.5088(4) 0.0364(14) Uani 1 1 d . . .
H14A H 1.1977 0.6741 0.5286 0.055 Uiso 1 1 calc R . .
H14B H 1.0615 0.5808 0.4666 0.055 Uiso 1 1 calc R . .
H14C H 1.0889 0.6884 0.5639 0.055 Uiso 1 1 calc R . .
C11 C 1.1273(4) 0.7561(5) 0.4580(4) 0.0255(12) Uani 1 1 d . . .
H11 H 1.1605 0.7343 0.4039 0.031 Uiso 1 1 calc R . .
C38 C 0.3951(6) 0.8362(7) 0.3246(6) 0.064(2) Uani 1 1 d . . .
H38A H 0.3810 0.9094 0.3430 0.077 Uiso 1 1 calc R . .
H38B H 0.3175 0.7622 0.2852 0.077 Uiso 1 1 calc R . .
C15 C 1.2139(5) 0.8941(5) 0.5211(4) 0.0332(13) Uani 1 1 d . . .
H15A H 1.1804 0.9199 0.5723 0.050 Uiso 1 1 calc R . .
H15B H 1.2235 0.9468 0.4841 0.050 Uiso 1 1 calc R . .
H15C H 1.2926 0.9032 0.5470 0.050 Uiso 1 1 calc R . .
C18 C 1.1806(5) 0.4725(5) 0.1952(4) 0.0372(14) Uani 1 1 d . . .
H18 H 1.2260 0.4339 0.2100 0.045 Uiso 1 1 calc R . .
C16 C 1.0960(5) 0.4894(5) 0.2380(4) 0.0311(13) Uani 1 1 d . . .
H16 H 1.0729 0.4636 0.2877 0.037 Uiso 1 1 calc R . .
C19 C 1.1866(6) 0.5257(6) 0.1228(4) 0.0472(17) Uani 1 1 d . . .
H19 H 1.2371 0.5280 0.0818 0.057 Uiso 1 1 calc R . .
C13 C 0.7114(5) 0.1489(5) -0.0396(4) 0.0413(15) Uani 1 1 d . . .
H13A H 0.7457 0.0926 -0.0593 0.062 Uiso 1 1 calc R . .
H13B H 0.7235 0.1999 -0.0782 0.062 Uiso 1 1 calc R . .
H13C H 0.6249 0.0995 -0.0472 0.062 Uiso 1 1 calc R . .
C12 C 0.7630(6) 0.1608(6) 0.1290(4) 0.0449(16) Uani 1 1 d . . .
H12A H 0.8041 0.2180 0.1941 0.067 Uiso 1 1 calc R . .
H12B H 0.7995 0.1065 0.1101 0.067 Uiso 1 1 calc R . .
H12C H 0.6773 0.1096 0.1230 0.067 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.695(3) . ?
Ge1 N3 1.819(4) . ?
Ge1 N1 1.836(4) . ?
Ge1 N2 1.851(4) . ?
Cl2 C38 1.682(8) . ?
Cl1 C38 1.758(6) . ?
F1 C21 1.343(5) . ?
F14 C36 1.354(5) . ?
F11 C33 1.350(5) . ?
F15 C37 1.353(5) . ?
F5 C25 1.360(5) . ?
F2 C22 1.344(5) . ?
F3 C23 1.352(5) . ?
F9 C30 1.343(5) . ?
F6 C27 1.348(5) . ?
F13 C35A 1.341(5) . ?
F12 C34 1.347(5) . ?
F4 C24 1.350(6) . ?
F10 C31 1.343(5) . ?
F8 C29 1.345(5) . ?
F7 C28 1.345(5) . ?
O1 B1 1.494(6) . ?
N2 C7 1.381(6) . ?
N2 C9 1.471(6) . ?
N3 C16 1.378(6) . ?
N3 C17 1.385(6) . ?
N1 C1 1.366(6) . ?
N1 C8 1.473(6) . ?
B1 C26 1.646(7) . ?
B1 C32 1.658(7) . ?
B1 C20 1.660(7) . ?
C22 C23 1.356(7) . ?
C22 C21 1.390(6) . ?
C20 C25 1.374(7) . ?
C20 C21 1.385(6) . ?
C23 C24 1.370(7) . ?
C32 C37 1.385(6) . ?
C32 C33 1.389(6) . ?
C1 C2 1.391(7) . ?
C1 C7 1.445(7) . ?
C25 C24 1.381(7) . ?
C37 C36 1.387(7) . ?
C33 C34 1.379(7) . ?
C28 C27 1.376(6) . ?
C28 C29 1.378(7) . ?
C31 C30 1.379(7) . ?
C31 C26 1.396(6) . ?
C36 C35A 1.360(7) . ?
C7 C6 1.392(7) . ?
C8 C10 1.533(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.523(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C27 C26 1.384(6) . ?
C30 C29 1.364(7) . ?
C17 C19 1.368(7) . ?
C17 H17 0.9300 . ?
C35A C34 1.364(7) . ?
C4 C5 1.357(7) . ?
C4 C3 1.361(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(6) . ?
C5 H5 0.9300 . ?
C2 C3 1.388(7) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C10 C12 1.502(7) . ?
C10 C13 1.539(8) . ?
C10 H10 0.9800 . ?
C6 H6 0.9300 . ?
C14 C11 1.501(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11 C15 1.514(7) . ?
C11 H11 0.9800 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 C16 1.356(7) . ?
C18 C19 1.432(8) . ?
C18 H18 0.9300 . ?
C16 H16 0.9300 . ?
C19 H19 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
O1 Ge1 N3 108.17(16) . . ?
O1 Ge1 N1 114.37(17) . . ?
N3 Ge1 N1 110.33(17) . . ?
O1 Ge1 N2 120.92(16) . . ?
N3 Ge1 N2 113.92(18) . . ?
N1 Ge1 N2 87.67(17) . . ?
B1 O1 Ge1 129.0(3) . . ?
C7 N2 C9 126.0(4) . . ?
C7 N2 Ge1 111.4(3) . . ?
C9 N2 Ge1 121.5(3) . . ?
C16 N3 C17 108.5(4) . . ?
C16 N3 Ge1 125.6(3) . . ?
C17 N3 Ge1 125.2(4) . . ?
C1 N1 C8 126.1(4) . . ?
C1 N1 Ge1 112.7(3) . . ?
C8 N1 Ge1 120.8(3) . . ?
O1 B1 C26 107.2(4) . . ?
O1 B1 C32 111.0(4) . . ?
C26 B1 C32 102.9(4) . . ?
O1 B1 C20 107.7(4) . . ?
C26 B1 C20 113.7(4) . . ?
C32 B1 C20 114.1(4) . . ?
F2 C22 C23 120.4(4) . . ?
F2 C22 C21 119.9(4) . . ?
C23 C22 C21 119.7(4) . . ?
C25 C20 C21 114.0(4) . . ?
C25 C20 B1 119.5(4) . . ?
C21 C20 B1 126.3(4) . . ?
F3 C23 C22 120.7(4) . . ?
F3 C23 C24 119.6(4) . . ?
C22 C23 C24 119.6(4) . . ?
C37 C32 C33 113.4(4) . . ?
C37 C32 B1 126.0(4) . . ?
C33 C32 B1 120.0(4) . . ?
N1 C1 C2 120.3(5) . . ?
N1 C1 C7 113.6(4) . . ?
C2 C1 C7 126.1(4) . . ?
F5 C25 C20 119.9(4) . . ?
F5 C25 C24 115.6(4) . . ?
C20 C25 C24 124.5(5) . . ?
F15 C37 C32 121.6(4) . . ?
F15 C37 C36 114.8(4) . . ?
C32 C37 C36 123.6(4) . . ?
F4 C24 C23 120.2(4) . . ?
F4 C24 C25 120.8(4) . . ?
C23 C24 C25 118.9(5) . . ?
F1 C21 C20 121.7(4) . . ?
F1 C21 C22 115.0(4) . . ?
C20 C21 C22 123.3(4) . . ?
F11 C33 C34 117.0(4) . . ?
F11 C33 C32 118.7(4) . . ?
C34 C33 C32 124.2(5) . . ?
F7 C28 C27 121.0(4) . . ?
F7 C28 C29 119.7(4) . . ?
C27 C28 C29 119.4(5) . . ?
F10 C31 C30 116.2(4) . . ?
F10 C31 C26 119.8(4) . . ?
C30 C31 C26 123.9(5) . . ?
F14 C36 C35A 120.3(4) . . ?
F14 C36 C37 119.5(4) . . ?
C35A C36 C37 120.1(4) . . ?
N2 C7 C6 120.5(5) . . ?
N2 C7 C1 114.0(4) . . ?
C6 C7 C1 125.5(4) . . ?
N1 C8 C10 113.9(4) . . ?
N1 C8 H8A 108.8 . . ?
C10 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C10 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C11 114.3(4) . . ?
N2 C9 H9A 108.7 . . ?
C11 C9 H9A 108.7 . . ?
N2 C9 H9B 108.7 . . ?
C11 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
F6 C27 C28 114.7(4) . . ?
F6 C27 C26 121.1(4) . . ?
C28 C27 C26 124.1(4) . . ?
F9 C30 C29 119.6(4) . . ?
F9 C30 C31 120.9(5) . . ?
C29 C30 C31 119.5(4) . . ?
C19 C17 N3 107.6(5) . . ?
C19 C17 H17 126.2 . . ?
N3 C17 H17 126.2 . . ?
F13 C35A C36 120.7(4) . . ?
F13 C35A C34 120.3(5) . . ?
C36 C35A C34 119.0(4) . . ?
F12 C34 C35A 119.7(4) . . ?
F12 C34 C33 120.7(4) . . ?
C35A C34 C33 119.6(5) . . ?
C5 C4 C3 126.6(5) . . ?
C5 C4 H4 116.7 . . ?
C3 C4 H4 116.7 . . ?
C27 C26 C31 113.6(4) . . ?
C27 C26 B1 126.7(4) . . ?
C31 C26 B1 119.2(4) . . ?
C4 C5 C6 130.7(5) . . ?
C4 C5 H5 114.7 . . ?
C6 C5 H5 114.7 . . ?
C3 C2 C1 131.2(5) . . ?
C3 C2 H2 114.4 . . ?
C1 C2 H2 114.4 . . ?
C4 C3 C2 129.4(5) . . ?
C4 C3 H3 115.3 . . ?
C2 C3 H3 115.3 . . ?
C12 C10 C8 113.5(4) . . ?
C12 C10 C13 111.5(5) . . ?
C8 C10 C13 107.7(5) . . ?
C12 C10 H10 108.0 . . ?
C8 C10 H10 108.0 . . ?
C13 C10 H10 108.0 . . ?
C5 C6 C7 130.3(5) . . ?
C5 C6 H6 114.8 . . ?
C7 C6 H6 114.8 . . ?
F8 C29 C30 120.9(4) . . ?
F8 C29 C28 119.7(5) . . ?
C30 C29 C28 119.4(4) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C14 C11 C15 112.3(5) . . ?
C14 C11 C9 112.0(4) . . ?
C15 C11 C9 109.1(4) . . ?
C14 C11 H11 107.7 . . ?
C15 C11 H11 107.7 . . ?
C9 C11 H11 107.7 . . ?
Cl2 C38 Cl1 113.8(4) . . ?
Cl2 C38 H38A 108.8 . . ?
Cl1 C38 H38A 108.8 . . ?
Cl2 C38 H38B 108.8 . . ?
Cl1 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C18 C19 106.6(5) . . ?
C16 C18 H18 126.7 . . ?
C19 C18 H18 126.7 . . ?
C18 C16 N3 109.3(5) . . ?
C18 C16 H16 125.4 . . ?
N3 C16 H16 125.4 . . ?
C17 C19 C18 108.0(5) . . ?
C17 C19 H19 126.0 . . ?
C18 C19 H19 126.0 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ge1 O1 B1 -145.9(4) . . . . ?
N1 Ge1 O1 B1 90.7(4) . . . . ?
N2 Ge1 O1 B1 -12.0(4) . . . . ?
O1 Ge1 N2 C7 110.5(3) . . . . ?
N3 Ge1 N2 C7 -117.9(3) . . . . ?
N1 Ge1 N2 C7 -6.7(3) . . . . ?
O1 Ge1 N2 C9 -58.3(4) . . . . ?
N3 Ge1 N2 C9 73.3(4) . . . . ?
N1 Ge1 N2 C9 -175.5(4) . . . . ?
O1 Ge1 N3 C16 176.3(4) . . . . ?
N1 Ge1 N3 C16 -57.9(4) . . . . ?
N2 Ge1 N3 C16 38.8(5) . . . . ?
O1 Ge1 N3 C17 -14.1(4) . . . . ?
N1 Ge1 N3 C17 111.6(4) . . . . ?
N2 Ge1 N3 C17 -151.6(4) . . . . ?
O1 Ge1 N1 C1 -116.2(3) . . . . ?
N3 Ge1 N1 C1 121.6(3) . . . . ?
N2 Ge1 N1 C1 6.9(3) . . . . ?
O1 Ge1 N1 C8 56.8(4) . . . . ?
N3 Ge1 N1 C8 -65.4(4) . . . . ?
N2 Ge1 N1 C8 179.9(4) . . . . ?
Ge1 O1 B1 C26 -162.0(3) . . . . ?
Ge1 O1 B1 C32 86.4(4) . . . . ?
Ge1 O1 B1 C20 -39.3(5) . . . . ?
O1 B1 C20 C25 -61.0(6) . . . . ?
C26 B1 C20 C25 57.6(6) . . . . ?
C32 B1 C20 C25 175.2(4) . . . . ?
O1 B1 C20 C21 113.7(5) . . . . ?
C26 B1 C20 C21 -127.7(5) . . . . ?
C32 B1 C20 C21 -10.1(7) . . . . ?
F2 C22 C23 F3 0.1(7) . . . . ?
C21 C22 C23 F3 179.0(4) . . . . ?
F2 C22 C23 C24 -178.8(5) . . . . ?
C21 C22 C23 C24 0.1(7) . . . . ?
O1 B1 C32 C37 0.7(6) . . . . ?
C26 B1 C32 C37 -113.7(5) . . . . ?
C20 B1 C32 C37 122.7(5) . . . . ?
O1 B1 C32 C33 171.1(4) . . . . ?
C26 B1 C32 C33 56.7(5) . . . . ?
C20 B1 C32 C33 -66.9(6) . . . . ?
C8 N1 C1 C2 0.6(7) . . . . ?
Ge1 N1 C1 C2 173.2(4) . . . . ?
C8 N1 C1 C7 -178.2(4) . . . . ?
Ge1 N1 C1 C7 -5.6(5) . . . . ?
C21 C20 C25 F5 -179.9(4) . . . . ?
B1 C20 C25 F5 -4.6(7) . . . . ?
C21 C20 C25 C24 -0.4(7) . . . . ?
B1 C20 C25 C24 174.9(5) . . . . ?
C33 C32 C37 F15 178.3(4) . . . . ?
B1 C32 C37 F15 -10.7(7) . . . . ?
C33 C32 C37 C36 -0.8(6) . . . . ?
B1 C32 C37 C36 170.2(4) . . . . ?
F3 C23 C24 F4 1.3(8) . . . . ?
C22 C23 C24 F4 -179.8(4) . . . . ?
F3 C23 C24 C25 -177.7(4) . . . . ?
C22 C23 C24 C25 1.1(8) . . . . ?
F5 C25 C24 F4 -0.5(7) . . . . ?
C20 C25 C24 F4 180.0(4) . . . . ?
F5 C25 C24 C23 178.5(4) . . . . ?
C20 C25 C24 C23 -1.0(8) . . . . ?
C25 C20 C21 F1 179.2(4) . . . . ?
B1 C20 C21 F1 4.2(7) . . . . ?
C25 C20 C21 C22 1.7(7) . . . . ?
B1 C20 C21 C22 -173.2(5) . . . . ?
F2 C22 C21 F1 -0.4(6) . . . . ?
C23 C22 C21 F1 -179.3(4) . . . . ?
F2 C22 C21 C20 177.2(4) . . . . ?
C23 C22 C21 C20 -1.6(7) . . . . ?
C37 C32 C33 F11 -179.3(4) . . . . ?
B1 C32 C33 F11 9.1(6) . . . . ?
C37 C32 C33 C34 2.2(7) . . . . ?
B1 C32 C33 C34 -169.3(4) . . . . ?
F15 C37 C36 F14 1.6(6) . . . . ?
C32 C37 C36 F14 -179.2(4) . . . . ?
F15 C37 C36 C35A 179.6(4) . . . . ?
C32 C37 C36 C35A -1.3(7) . . . . ?
C9 N2 C7 C6 -6.7(7) . . . . ?
Ge1 N2 C7 C6 -175.0(4) . . . . ?
C9 N2 C7 C1 173.3(4) . . . . ?
Ge1 N2 C7 C1 5.1(5) . . . . ?
N1 C1 C7 N2 0.3(6) . . . . ?
C2 C1 C7 N2 -178.4(5) . . . . ?
N1 C1 C7 C6 -179.6(4) . . . . ?
C2 C1 C7 C6 1.7(8) . . . . ?
C1 N1 C8 C10 -99.0(5) . . . . ?
Ge1 N1 C8 C10 89.0(5) . . . . ?
C7 N2 C9 C11 110.6(5) . . . . ?
Ge1 N2 C9 C11 -82.3(5) . . . . ?
F7 C28 C27 F6 0.2(6) . . . . ?
C29 C28 C27 F6 179.2(4) . . . . ?
F7 C28 C27 C26 -179.5(4) . . . . ?
C29 C28 C27 C26 -0.5(7) . . . . ?
F10 C31 C30 F9 1.6(7) . . . . ?
C26 C31 C30 F9 179.9(4) . . . . ?
F10 C31 C30 C29 -177.3(4) . . . . ?
C26 C31 C30 C29 0.9(8) . . . . ?
C16 N3 C17 C19 -0.8(6) . . . . ?
Ge1 N3 C17 C19 -171.8(4) . . . . ?
F14 C36 C35A F13 2.4(7) . . . . ?
C37 C36 C35A F13 -175.5(4) . . . . ?
F14 C36 C35A C34 179.9(4) . . . . ?
C37 C36 C35A C34 1.9(7) . . . . ?
F13 C35A C34 F12 -2.4(7) . . . . ?
C36 C35A C34 F12 -179.8(4) . . . . ?
F13 C35A C34 C33 176.9(4) . . . . ?
C36 C35A C34 C33 -0.5(7) . . . . ?
F11 C33 C34 F12 -0.9(6) . . . . ?
C32 C33 C34 F12 177.6(4) . . . . ?
F11 C33 C34 C35A 179.8(4) . . . . ?
C32 C33 C34 C35A -1.7(7) . . . . ?
F6 C27 C26 C31 -178.6(4) . . . . ?
C28 C27 C26 C31 1.2(7) . . . . ?
F6 C27 C26 B1 -6.5(7) . . . . ?
C28 C27 C26 B1 173.3(4) . . . . ?
F10 C31 C26 C27 176.8(4) . . . . ?
C30 C31 C26 C27 -1.4(7) . . . . ?
F10 C31 C26 B1 4.0(6) . . . . ?
C30 C31 C26 B1 -174.1(4) . . . . ?
O1 B1 C26 C27 137.3(4) . . . . ?
C32 B1 C26 C27 -105.6(5) . . . . ?
C20 B1 C26 C27 18.4(7) . . . . ?
O1 B1 C26 C31 -51.0(5) . . . . ?
C32 B1 C26 C31 66.2(5) . . . . ?
C20 B1 C26 C31 -169.9(4) . . . . ?
C3 C4 C5 C6 4.3(10) . . . . ?
N1 C1 C2 C3 -176.1(5) . . . . ?
C7 C1 C2 C3 2.5(9) . . . . ?
C5 C4 C3 C2 -3.5(10) . . . . ?
C1 C2 C3 C4 -1.4(11) . . . . ?
N1 C8 C10 C12 58.6(6) . . . . ?
N1 C8 C10 C13 -177.5(4) . . . . ?
C4 C5 C6 C7 0.7(10) . . . . ?
N2 C7 C6 C5 175.7(5) . . . . ?
C1 C7 C6 C5 -4.4(9) . . . . ?
F9 C30 C29 F8 1.5(7) . . . . ?
C31 C30 C29 F8 -179.6(4) . . . . ?
F9 C30 C29 C28 -179.1(4) . . . . ?
C31 C30 C29 C28 -0.2(7) . . . . ?
F7 C28 C29 F8 -1.6(7) . . . . ?
C27 C28 C29 F8 179.4(4) . . . . ?
F7 C28 C29 C30 179.0(4) . . . . ?
C27 C28 C29 C30 -0.1(7) . . . . ?
N2 C9 C11 C14 -63.7(5) . . . . ?
N2 C9 C11 C15 171.3(4) . . . . ?
C19 C18 C16 N3 -0.3(6) . . . . ?
C17 N3 C16 C18 0.7(6) . . . . ?
Ge1 N3 C16 C18 171.7(4) . . . . ?
N3 C17 C19 C18 0.6(7) . . . . ?
C16 C18 C19 C17 -0.1(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_Compound_12__msh300m
_database_code_depnum_ccdc_archive 'CCDC 1564833'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H38 B F15 Ge N2 O2 Si'
_chemical_formula_sum            'C51 H38 B F15 Ge N2 O2 Si'
_chemical_formula_weight         1107.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6250(11)
_cell_length_b                   15.0956(14)
_cell_length_c                   15.2052(14)
_cell_angle_alpha                82.564(2)
_cell_angle_beta                 69.443(2)
_cell_angle_gamma                69.8390(10)
_cell_volume                     2345.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7391
_cell_measurement_theta_min      2.794
_cell_measurement_theta_max      25.05

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120.0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12248
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8104
_reflns_number_gt                7387
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0715P)²+0.4154P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8104
_refine_ls_number_parameters     662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.1169
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_restrained_S_all      1.189
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.29201(2) 0.259912(16) 0.220311(16) 0.01212(10) Uani 1 1 d . . .
Si1 Si 0.15815(6) 0.23097(4) 0.44171(5) 0.01435(15) Uani 1 1 d . . .
O1 O 0.18953(16) 0.27648(11) 0.33462(11) 0.0165(4) Uani 1 1 d . . .
O2 O 0.44929(15) 0.20967(11) 0.21485(11) 0.0157(4) Uani 1 1 d . . .
B1 B 0.5718(3) 0.21744(19) 0.14210(19) 0.0149(5) Uani 1 1 d . . .
N2 N 0.24238(18) 0.19674(13) 0.15100(14) 0.0140(4) Uani 1 1 d . . .
N1 N 0.24491(19) 0.36552(13) 0.14813(14) 0.0141(4) Uani 1 1 d . . .
F1 F 0.61729(13) 0.14293(10) 0.31469(10) 0.0190(3) Uani 1 1 d . . .
F11 F 0.81644(13) 0.25022(10) 0.04599(10) 0.0206(3) Uani 1 1 d . . .
F4 F 0.95616(13) -0.08190(10) 0.02062(10) 0.0209(3) Uani 1 1 d . . .
F5 F 0.78604(13) 0.07583(10) -0.01189(10) 0.0197(3) Uani 1 1 d . . .
F15 F 0.42714(13) 0.36235(10) 0.30105(10) 0.0234(3) Uani 1 1 d . . .
F6 F 0.53109(13) 0.08598(10) 0.04133(10) 0.0203(3) Uani 1 1 d . . .
F10 F 0.56673(14) 0.39289(10) 0.01515(10) 0.0228(3) Uani 1 1 d . . .
F13 F 0.78202(15) 0.45975(11) 0.26273(11) 0.0279(4) Uani 1 1 d . . .
F2 F 0.78844(15) -0.01734(10) 0.34389(10) 0.0251(3) Uani 1 1 d . . .
F9 F 0.52543(16) 0.41589(11) -0.14812(11) 0.0313(4) Uani 1 1 d . . .
F7 F 0.49529(15) 0.11044(11) -0.12489(11) 0.0276(4) Uani 1 1 d . . .
F3 F 0.96018(15) -0.13318(10) 0.19784(11) 0.0262(3) Uani 1 1 d . . .
F14 F 0.53274(15) 0.46494(11) 0.35687(11) 0.0276(4) Uani 1 1 d . . .
F12 F 0.91907(14) 0.35632(10) 0.10373(11) 0.0271(4) Uani 1 1 d . . .
F8 F 0.49030(15) 0.27610(12) -0.22155(10) 0.0318(4) Uani 1 1 d . . .
C22 C 0.2241(2) 0.28146(17) 0.51139(17) 0.0165(5) Uani 1 1 d . . .
C39 C 0.7782(2) 0.05568(17) 0.07892(17) 0.0151(5) Uani 1 1 d . . .
C47 C 0.7428(2) 0.30193(16) 0.12432(17) 0.0160(5) Uani 1 1 d . . .
C1 C 0.2167(2) 0.34507(16) 0.07509(17) 0.0146(5) Uani 1 1 d . . .
C46 C 0.6183(2) 0.29761(16) 0.17234(17) 0.0147(5) Uani 1 1 d . . .
C35 C 0.6949(2) 0.08746(16) 0.23903(17) 0.0155(5) Uani 1 1 d . . .
C45 C 0.5508(2) 0.31925(17) -0.01565(18) 0.0184(5) Uani 1 1 d . . .
C51 C 0.5517(2) 0.35565(17) 0.24945(17) 0.0170(5) Uani 1 1 d . . .
C37 C 0.8721(2) -0.05292(16) 0.18283(19) 0.0186(5) Uani 1 1 d . . .
C40 C 0.5543(2) 0.23659(17) 0.03707(17) 0.0158(5) Uani 1 1 d . . .
C5 C 0.1753(2) 0.24369(18) -0.07620(18) 0.0213(5) Uani 1 1 d . . .
H5 H 0.1699 0.2012 -0.1125 0.026 Uiso 1 1 calc R . .
C9 C 0.2494(2) 0.09678(16) 0.17108(18) 0.0172(5) Uani 1 1 d . . .
H9A H 0.3193 0.0655 0.1965 0.021 Uiso 1 1 calc R . .
H9B H 0.2701 0.0660 0.1127 0.021 Uiso 1 1 calc R . .
C2 C 0.1888(2) 0.41379(17) 0.00831(18) 0.0196(5) Uani 1 1 d . . .
H2 H 0.1875 0.4730 0.0204 0.024 Uiso 1 1 calc R . .
C42 C 0.5140(2) 0.17939(18) -0.08965(18) 0.0203(5) Uani 1 1 d . . .
C4 C 0.1594(2) 0.33392(18) -0.11333(18) 0.0208(5) Uani 1 1 d . . .
H4 H 0.1452 0.3447 -0.1709 0.025 Uiso 1 1 calc R . .
C16 C -0.0226(2) 0.26487(17) 0.49196(18) 0.0181(5) Uani 1 1 d . . .
C50 C 0.6027(2) 0.41063(17) 0.28050(17) 0.0190(5) Uani 1 1 d . . .
C29 C 0.1620(2) 0.03744(17) 0.47055(18) 0.0196(5) Uani 1 1 d . . .
H29 H 0.0718 0.0611 0.4912 0.023 Uiso 1 1 calc R . .
C6 C 0.1979(2) 0.20688(17) 0.00612(18) 0.0188(5) Uani 1 1 d . . .
H6 H 0.2009 0.1442 0.0176 0.023 Uiso 1 1 calc R . .
C28 C 0.2337(2) 0.10020(17) 0.43963(17) 0.0174(5) Uani 1 1 d . . .
C43 C 0.5123(2) 0.2628(2) -0.13903(18) 0.0236(6) Uani 1 1 d . . .
C8 C 0.2532(2) 0.45858(16) 0.15811(17) 0.0158(5) Uani 1 1 d . . .
H8A H 0.2995 0.4795 0.0971 0.019 Uiso 1 1 calc R . .
H8B H 0.3031 0.4524 0.1993 0.019 Uiso 1 1 calc R . .
C49 C 0.7282(2) 0.40928(17) 0.23236(19) 0.0203(5) Uani 1 1 d . . .
C38 C 0.8690(2) -0.02651(16) 0.09367(18) 0.0169(5) Uani 1 1 d . . .
C24 C 0.2880(3) 0.40697(19) 0.54505(19) 0.0258(6) Uani 1 1 d . . .
H24 H 0.2966 0.4667 0.5314 0.031 Uiso 1 1 calc R . .
C30 C 0.2234(3) -0.05929(18) 0.47088(19) 0.0242(6) Uani 1 1 d . . .
H30 H 0.1743 -0.0999 0.4912 0.029 Uiso 1 1 calc R . .
C44 C 0.5303(2) 0.33344(19) -0.10176(18) 0.0228(6) Uani 1 1 d . . .
C13 C 0.1358(3) 0.63146(18) 0.1779(2) 0.0252(6) Uani 1 1 d . . .
H13A H 0.0536 0.6784 0.2057 0.038 Uiso 1 1 calc R . .
H13B H 0.1655 0.6421 0.1112 0.038 Uiso 1 1 calc R . .
H13C H 0.1978 0.6354 0.2042 0.038 Uiso 1 1 calc R . .
C41 C 0.5337(2) 0.16875(17) -0.00440(18) 0.0181(5) Uani 1 1 d . . .
C7 C 0.2173(2) 0.24759(16) 0.07635(17) 0.0148(5) Uani 1 1 d . . .
C48 C 0.7974(2) 0.35591(17) 0.15257(18) 0.0190(5) Uani 1 1 d . . .
C17 C -0.1020(3) 0.2984(2) 0.4372(2) 0.0292(6) Uani 1 1 d . . .
H17 H -0.0650 0.3053 0.3728 0.035 Uiso 1 1 calc R . .
C10 C 0.1207(2) 0.53387(16) 0.19752(18) 0.0185(5) Uani 1 1 d . . .
H10 H 0.0638 0.5291 0.1649 0.022 Uiso 1 1 calc R . .
C26 C 0.3119(3) 0.26580(19) 0.6383(2) 0.0268(6) Uani 1 1 d . . .
H26 H 0.3354 0.2306 0.6879 0.032 Uiso 1 1 calc R . .
C36 C 0.7845(2) 0.00494(17) 0.25634(18) 0.0183(5) Uani 1 1 d . . .
C27 C 0.2623(3) 0.22978(18) 0.58523(19) 0.0232(6) Uani 1 1 d . . .
H27 H 0.2544 0.1699 0.5992 0.028 Uiso 1 1 calc R . .
C23 C 0.2371(2) 0.37137(18) 0.49295(18) 0.0211(5) Uani 1 1 d . . .
H23 H 0.2110 0.4079 0.4449 0.025 Uiso 1 1 calc R . .
C34 C 0.6849(2) 0.11631(16) 0.15087(17) 0.0148(5) Uani 1 1 d . . .
C33 C 0.3685(3) 0.06199(19) 0.4099(2) 0.0267(6) Uani 1 1 d . . .
H33 H 0.4184 0.1021 0.3895 0.032 Uiso 1 1 calc R . .
C20 C -0.2144(3) 0.2768(2) 0.6284(2) 0.0392(8) Uani 1 1 d . . .
H20 H -0.2517 0.2686 0.6926 0.047 Uiso 1 1 calc R . .
C3 C 0.1626(3) 0.40967(18) -0.07299(18) 0.0225(6) Uani 1 1 d . . .
H3 H 0.1444 0.4666 -0.1054 0.027 Uiso 1 1 calc R . .
C15 C 0.1439(3) -0.02147(19) 0.2545(2) 0.0309(7) Uani 1 1 d . . .
H15A H 0.0673 -0.0309 0.3001 0.046 Uiso 1 1 calc R . .
H15B H 0.2165 -0.0510 0.2764 0.046 Uiso 1 1 calc R . .
H15C H 0.1604 -0.0490 0.1960 0.046 Uiso 1 1 calc R . .
C31 C 0.3569(3) -0.09546(19) 0.4412(2) 0.0302(6) Uani 1 1 d . . .
H31 H 0.3979 -0.1603 0.4420 0.036 Uiso 1 1 calc R . .
C25 C 0.3261(2) 0.35374(19) 0.6174(2) 0.0261(6) Uani 1 1 d . . .
H25 H 0.3612 0.3774 0.6517 0.031 Uiso 1 1 calc R . .
C21 C -0.0809(3) 0.2535(2) 0.5885(2) 0.0327(7) Uani 1 1 d . . .
H21 H -0.0291 0.2300 0.6264 0.039 Uiso 1 1 calc R . .
C11 C 0.1238(3) 0.08484(19) 0.2402(2) 0.0268(6) Uani 1 1 d . . .
H11 H 0.1098 0.1103 0.3005 0.032 Uiso 1 1 calc R . .
C19 C -0.2923(3) 0.31250(19) 0.5723(2) 0.0334(7) Uani 1 1 d . . .
H19 H -0.3821 0.3299 0.5990 0.040 Uiso 1 1 calc R . .
C18 C -0.2361(3) 0.3222(2) 0.4767(2) 0.0386(8) Uani 1 1 d . . .
H18 H -0.2879 0.3446 0.4387 0.046 Uiso 1 1 calc R . .
C32 C 0.4296(3) -0.03470(19) 0.4102(2) 0.0348(7) Uani 1 1 d . . .
H32 H 0.5197 -0.0589 0.3895 0.042 Uiso 1 1 calc R . .
C14 C 0.0050(3) 0.1361(2) 0.2124(2) 0.0347(7) Uani 1 1 d . . .
H14A H -0.0011 0.2013 0.1999 0.052 Uiso 1 1 calc R . .
H14B H -0.0709 0.1316 0.2626 0.052 Uiso 1 1 calc R . .
H14C H 0.0115 0.1081 0.1569 0.052 Uiso 1 1 calc R . .
C12 C 0.0576(3) 0.5199(2) 0.3020(2) 0.0361(7) Uani 1 1 d . . .
H12A H 0.1110 0.5258 0.3354 0.054 Uiso 1 1 calc R . .
H12B H 0.0484 0.4583 0.3130 0.054 Uiso 1 1 calc R . .
H12C H -0.0264 0.5669 0.3235 0.054 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O2 1.6967(16) . ?
Ge1 O1 1.7193(16) . ?
Ge1 N1 1.8476(19) . ?
Ge1 N2 1.8492(19) . ?
Si1 O1 1.6499(17) . ?
Si1 C28 1.863(2) . ?
Si1 C22 1.864(2) . ?
Si1 C16 1.869(3) . ?
O2 B1 1.497(3) . ?
B1 C46 1.654(3) . ?
B1 C40 1.656(4) . ?
B1 C34 1.662(3) . ?
N2 C7 1.347(3) . ?
N2 C9 1.480(3) . ?
N1 C1 1.360(3) . ?
N1 C8 1.471(3) . ?
F1 C35 1.356(3) . ?
F11 C47 1.351(3) . ?
F4 C38 1.351(3) . ?
F5 C39 1.353(3) . ?
F15 C51 1.358(3) . ?
F6 C41 1.353(3) . ?
F10 C45 1.351(3) . ?
F13 C49 1.345(3) . ?
F2 C36 1.343(3) . ?
F9 C44 1.342(3) . ?
F7 C42 1.342(3) . ?
F3 C37 1.344(3) . ?
F14 C50 1.344(3) . ?
F12 C48 1.349(3) . ?
F8 C43 1.343(3) . ?
C22 C27 1.397(4) . ?
C22 C23 1.398(3) . ?
C39 C38 1.377(3) . ?
C39 C34 1.397(3) . ?
C47 C48 1.376(4) . ?
C47 C46 1.394(3) . ?
C1 C2 1.393(3) . ?
C1 C7 1.467(3) . ?
C46 C51 1.379(3) . ?
C35 C36 1.385(3) . ?
C35 C34 1.387(3) . ?
C45 C44 1.389(4) . ?
C45 C40 1.389(3) . ?
C51 C50 1.379(4) . ?
C37 C38 1.372(4) . ?
C37 C36 1.375(4) . ?
C40 C41 1.395(4) . ?
C5 C6 1.377(4) . ?
C5 C4 1.382(4) . ?
C5 H5 0.9300 . ?
C9 C11 1.524(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C2 C3 1.386(4) . ?
C2 H2 0.9300 . ?
C42 C41 1.374(4) . ?
C42 C43 1.377(4) . ?
C4 C3 1.383(4) . ?
C4 H4 0.9300 . ?
C16 C17 1.382(4) . ?
C16 C21 1.400(4) . ?
C50 C49 1.377(4) . ?
C29 C30 1.387(4) . ?
C29 C28 1.402(3) . ?
C29 H29 0.9300 . ?
C6 C7 1.416(3) . ?
C6 H6 0.9300 . ?
C28 C33 1.393(4) . ?
C43 C44 1.378(4) . ?
C8 C10 1.531(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C49 C48 1.374(4) . ?
C24 C25 1.385(4) . ?
C24 C23 1.388(4) . ?
C24 H24 0.9300 . ?
C30 C31 1.377(4) . ?
C30 H30 0.9300 . ?
C13 C10 1.522(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C17 C18 1.390(4) . ?
C17 H17 0.9300 . ?
C10 C12 1.518(4) . ?
C10 H10 0.9800 . ?
C26 C25 1.377(4) . ?
C26 C27 1.392(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C23 H23 0.9300 . ?
C33 C32 1.386(4) . ?
C33 H33 0.9300 . ?
C20 C21 1.385(4) . ?
C20 C19 1.387(5) . ?
C20 H20 0.9300 . ?
C3 H3 0.9300 . ?
C15 C11 1.538(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C31 C32 1.386(4) . ?
C31 H31 0.9300 . ?
C25 H25 0.9300 . ?
C21 H21 0.9300 . ?
C11 C14 1.507(4) . ?
C11 H11 0.9800 . ?
C19 C18 1.381(5) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C32 H32 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
O2 Ge1 O1 111.43(8) . . ?
O2 Ge1 N1 120.05(8) . . ?
O1 Ge1 N1 110.46(8) . . ?
O2 Ge1 N2 113.29(8) . . ?
O1 Ge1 N2 112.20(8) . . ?
N1 Ge1 N2 87.34(8) . . ?
O1 Si1 C28 111.32(10) . . ?
O1 Si1 C22 109.25(10) . . ?
C28 Si1 C22 108.66(11) . . ?
O1 Si1 C16 105.67(10) . . ?
C28 Si1 C16 110.75(11) . . ?
C22 Si1 C16 111.18(11) . . ?
Si1 O1 Ge1 145.51(11) . . ?
B1 O2 Ge1 130.94(15) . . ?
O2 B1 C46 110.63(19) . . ?
O2 B1 C40 110.25(19) . . ?
C46 B1 C40 113.5(2) . . ?
O2 B1 C34 104.58(19) . . ?
C46 B1 C34 103.56(18) . . ?
C40 B1 C34 113.77(19) . . ?
C7 N2 C9 125.8(2) . . ?
C7 N2 Ge1 112.37(15) . . ?
C9 N2 Ge1 121.25(15) . . ?
C1 N1 C8 122.18(19) . . ?
C1 N1 Ge1 111.94(15) . . ?
C8 N1 Ge1 125.37(16) . . ?
C27 C22 C23 117.4(2) . . ?
C27 C22 Si1 120.39(19) . . ?
C23 C22 Si1 122.22(19) . . ?
F5 C39 C38 115.2(2) . . ?
F5 C39 C34 121.1(2) . . ?
C38 C39 C34 123.7(2) . . ?
F11 C47 C48 116.9(2) . . ?
F11 C47 C46 119.5(2) . . ?
C48 C47 C46 123.6(2) . . ?
N1 C1 C2 120.7(2) . . ?
N1 C1 C7 113.7(2) . . ?
C2 C1 C7 125.6(2) . . ?
C51 C46 C47 113.9(2) . . ?
C51 C46 B1 126.4(2) . . ?
C47 C46 B1 119.2(2) . . ?
F1 C35 C36 115.6(2) . . ?
F1 C35 C34 120.1(2) . . ?
C36 C35 C34 124.2(2) . . ?
F10 C45 C44 115.1(2) . . ?
F10 C45 C40 121.1(2) . . ?
C44 C45 C40 123.8(2) . . ?
F15 C51 C50 114.8(2) . . ?
F15 C51 C46 120.8(2) . . ?
C50 C51 C46 124.4(2) . . ?
F3 C37 C38 120.6(2) . . ?
F3 C37 C36 120.7(2) . . ?
C38 C37 C36 118.7(2) . . ?
C45 C40 C41 113.4(2) . . ?
C45 C40 B1 125.9(2) . . ?
C41 C40 B1 120.6(2) . . ?
C6 C5 C4 130.1(2) . . ?
C6 C5 H5 114.9 . . ?
C4 C5 H5 114.9 . . ?
N2 C9 C11 113.2(2) . . ?
N2 C9 H9A 108.9 . . ?
C11 C9 H9A 108.9 . . ?
N2 C9 H9B 108.9 . . ?
C11 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C3 C2 C1 131.5(2) . . ?
C3 C2 H2 114.2 . . ?
C1 C2 H2 114.2 . . ?
F7 C42 C41 121.1(2) . . ?
F7 C42 C43 119.7(2) . . ?
C41 C42 C43 119.2(2) . . ?
C5 C4 C3 126.1(2) . . ?
C5 C4 H4 116.9 . . ?
C3 C4 H4 116.9 . . ?
C17 C16 C21 118.0(2) . . ?
C17 C16 Si1 122.7(2) . . ?
C21 C16 Si1 119.2(2) . . ?
F14 C50 C49 119.5(2) . . ?
F14 C50 C51 121.3(2) . . ?
C49 C50 C51 119.1(2) . . ?
C30 C29 C28 121.1(2) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C5 C6 C7 131.4(2) . . ?
C5 C6 H6 114.3 . . ?
C7 C6 H6 114.3 . . ?
C33 C28 C29 117.7(2) . . ?
C33 C28 Si1 118.79(19) . . ?
C29 C28 Si1 123.49(19) . . ?
F8 C43 C42 120.6(2) . . ?
F8 C43 C44 120.2(2) . . ?
C42 C43 C44 119.2(2) . . ?
N1 C8 C10 113.56(19) . . ?
N1 C8 H8A 108.9 . . ?
C10 C8 H8A 108.9 . . ?
N1 C8 H8B 108.9 . . ?
C10 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
F13 C49 C48 120.4(2) . . ?
F13 C49 C50 120.5(2) . . ?
C48 C49 C50 119.1(2) . . ?
F4 C38 C37 119.3(2) . . ?
F4 C38 C39 120.4(2) . . ?
C37 C38 C39 120.3(2) . . ?
C25 C24 C23 120.1(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C31 C30 C29 120.2(2) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
F9 C44 C43 119.7(2) . . ?
F9 C44 C45 120.7(2) . . ?
C43 C44 C45 119.6(2) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
F6 C41 C42 116.1(2) . . ?
F6 C41 C40 119.2(2) . . ?
C42 C41 C40 124.8(2) . . ?
N2 C7 C6 121.3(2) . . ?
N2 C7 C1 113.6(2) . . ?
C6 C7 C1 125.1(2) . . ?
F12 C48 C49 119.3(2) . . ?
F12 C48 C47 120.9(2) . . ?
C49 C48 C47 119.8(2) . . ?
C16 C17 C18 121.3(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C12 C10 C13 110.6(2) . . ?
C12 C10 C8 112.0(2) . . ?
C13 C10 C8 109.6(2) . . ?
C12 C10 H10 108.2 . . ?
C13 C10 H10 108.2 . . ?
C8 C10 H10 108.2 . . ?
C25 C26 C27 119.8(3) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
F2 C36 C37 120.0(2) . . ?
F2 C36 C35 120.4(2) . . ?
C37 C36 C35 119.6(2) . . ?
C26 C27 C22 121.6(2) . . ?
C26 C27 H27 119.2 . . ?
C22 C27 H27 119.2 . . ?
C24 C23 C22 121.2(2) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C35 C34 C39 113.5(2) . . ?
C35 C34 B1 118.2(2) . . ?
C39 C34 B1 128.2(2) . . ?
C32 C33 C28 121.2(2) . . ?
C32 C33 H33 119.4 . . ?
C28 C33 H33 119.4 . . ?
C21 C20 C19 119.8(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C4 C3 C2 130.0(2) . . ?
C4 C3 H3 115.0 . . ?
C2 C3 H3 115.0 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C30 C31 C32 119.6(2) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C26 C25 C24 119.9(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C20 C21 C16 121.1(3) . . ?
C20 C21 H21 119.5 . . ?
C16 C21 H21 119.5 . . ?
C14 C11 C9 114.5(2) . . ?
C14 C11 C15 111.8(2) . . ?
C9 C11 C15 107.9(2) . . ?
C14 C11 H11 107.4 . . ?
C9 C11 H11 107.4 . . ?
C15 C11 H11 107.4 . . ?
C18 C19 C20 119.8(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C33 C32 C31 120.2(3) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C28 Si1 O1 Ge1 -22.2(2) . . . . ?
C22 Si1 O1 Ge1 97.8(2) . . . . ?
C16 Si1 O1 Ge1 -142.52(18) . . . . ?
O2 Ge1 O1 Si1 -40.2(2) . . . . ?
N1 Ge1 O1 Si1 -176.26(18) . . . . ?
N2 Ge1 O1 Si1 88.1(2) . . . . ?
O1 Ge1 O2 B1 -150.59(19) . . . . ?
N1 Ge1 O2 B1 -19.2(2) . . . . ?
N2 Ge1 O2 B1 81.8(2) . . . . ?
Ge1 O2 B1 C46 96.5(2) . . . . ?
Ge1 O2 B1 C40 -29.9(3) . . . . ?
Ge1 O2 B1 C34 -152.56(15) . . . . ?
O2 Ge1 N2 C7 -112.20(16) . . . . ?
O1 Ge1 N2 C7 120.56(16) . . . . ?
N1 Ge1 N2 C7 9.52(16) . . . . ?
O2 Ge1 N2 C9 59.84(19) . . . . ?
O1 Ge1 N2 C9 -67.40(18) . . . . ?
N1 Ge1 N2 C9 -178.44(18) . . . . ?
O2 Ge1 N1 C1 106.99(16) . . . . ?
O1 Ge1 N1 C1 -121.23(15) . . . . ?
N2 Ge1 N1 C1 -8.50(16) . . . . ?
O2 Ge1 N1 C8 -64.9(2) . . . . ?
O1 Ge1 N1 C8 66.84(19) . . . . ?
N2 Ge1 N1 C8 179.57(19) . . . . ?
O1 Si1 C22 C27 -152.0(2) . . . . ?
C28 Si1 C22 C27 -30.3(2) . . . . ?
C16 Si1 C22 C27 91.8(2) . . . . ?
O1 Si1 C22 C23 28.3(2) . . . . ?
C28 Si1 C22 C23 149.9(2) . . . . ?
C16 Si1 C22 C23 -87.9(2) . . . . ?
C8 N1 C1 C2 -2.8(3) . . . . ?
Ge1 N1 C1 C2 -175.03(18) . . . . ?
C8 N1 C1 C7 178.06(19) . . . . ?
Ge1 N1 C1 C7 5.8(2) . . . . ?
F11 C47 C46 C51 -178.2(2) . . . . ?
C48 C47 C46 C51 2.5(3) . . . . ?
F11 C47 C46 B1 9.3(3) . . . . ?
C48 C47 C46 B1 -170.0(2) . . . . ?
O2 B1 C46 C51 -4.4(3) . . . . ?
C40 B1 C46 C51 120.1(2) . . . . ?
C34 B1 C46 C51 -116.0(2) . . . . ?
O2 B1 C46 C47 167.0(2) . . . . ?
C40 B1 C46 C47 -68.4(3) . . . . ?
C34 B1 C46 C47 55.5(3) . . . . ?
C47 C46 C51 F15 177.1(2) . . . . ?
B1 C46 C51 F15 -11.0(4) . . . . ?
C47 C46 C51 C50 -2.7(4) . . . . ?
B1 C46 C51 C50 169.1(2) . . . . ?
F10 C45 C40 C41 178.8(2) . . . . ?
C44 C45 C40 C41 -0.7(3) . . . . ?
F10 C45 C40 B1 2.4(4) . . . . ?
C44 C45 C40 B1 -177.1(2) . . . . ?
O2 B1 C40 C45 111.8(3) . . . . ?
C46 B1 C40 C45 -12.9(3) . . . . ?
C34 B1 C40 C45 -131.1(2) . . . . ?
O2 B1 C40 C41 -64.4(3) . . . . ?
C46 B1 C40 C41 170.9(2) . . . . ?
C34 B1 C40 C41 52.8(3) . . . . ?
C7 N2 C9 C11 -97.3(3) . . . . ?
Ge1 N2 C9 C11 91.8(2) . . . . ?
N1 C1 C2 C3 177.1(3) . . . . ?
C7 C1 C2 C3 -3.9(4) . . . . ?
C6 C5 C4 C3 -0.3(5) . . . . ?
O1 Si1 C16 C17 15.0(2) . . . . ?
C28 Si1 C16 C17 -105.7(2) . . . . ?
C22 Si1 C16 C17 133.4(2) . . . . ?
O1 Si1 C16 C21 -166.9(2) . . . . ?
C28 Si1 C16 C21 72.4(2) . . . . ?
C22 Si1 C16 C21 -48.5(2) . . . . ?
F15 C51 C50 F14 0.8(3) . . . . ?
C46 C51 C50 F14 -179.3(2) . . . . ?
F15 C51 C50 C49 -179.5(2) . . . . ?
C46 C51 C50 C49 0.3(4) . . . . ?
C4 C5 C6 C7 -3.0(5) . . . . ?
C30 C29 C28 C33 -0.4(4) . . . . ?
C30 C29 C28 Si1 -177.4(2) . . . . ?
O1 Si1 C28 C33 66.8(2) . . . . ?
C22 Si1 C28 C33 -53.6(2) . . . . ?
C16 Si1 C28 C33 -176.0(2) . . . . ?
O1 Si1 C28 C29 -116.2(2) . . . . ?
C22 Si1 C28 C29 123.4(2) . . . . ?
C16 Si1 C28 C29 1.0(2) . . . . ?
F7 C42 C43 F8 0.9(4) . . . . ?
C41 C42 C43 F8 -178.4(2) . . . . ?
F7 C42 C43 C44 179.4(2) . . . . ?
C41 C42 C43 C44 0.1(4) . . . . ?
C1 N1 C8 C10 78.9(3) . . . . ?
Ge1 N1 C8 C10 -110.0(2) . . . . ?
F14 C50 C49 F13 1.9(4) . . . . ?
C51 C50 C49 F13 -177.8(2) . . . . ?
F14 C50 C49 C48 -177.9(2) . . . . ?
C51 C50 C49 C48 2.5(4) . . . . ?
F3 C37 C38 F4 -0.4(3) . . . . ?
C36 C37 C38 F4 178.8(2) . . . . ?
F3 C37 C38 C39 179.8(2) . . . . ?
C36 C37 C38 C39 -1.0(4) . . . . ?
F5 C39 C38 F4 -1.3(3) . . . . ?
C34 C39 C38 F4 179.8(2) . . . . ?
F5 C39 C38 C37 178.5(2) . . . . ?
C34 C39 C38 C37 -0.3(4) . . . . ?
C28 C29 C30 C31 0.4(4) . . . . ?
F8 C43 C44 F9 0.2(4) . . . . ?
C42 C43 C44 F9 -178.3(2) . . . . ?
F8 C43 C44 C45 178.9(2) . . . . ?
C42 C43 C44 C45 0.4(4) . . . . ?
F10 C45 C44 F9 -0.9(3) . . . . ?
C40 C45 C44 F9 178.6(2) . . . . ?
F10 C45 C44 C43 -179.6(2) . . . . ?
C40 C45 C44 C43 -0.1(4) . . . . ?
F7 C42 C41 F6 -0.8(3) . . . . ?
C43 C42 C41 F6 178.4(2) . . . . ?
F7 C42 C41 C40 179.8(2) . . . . ?
C43 C42 C41 C40 -1.0(4) . . . . ?
C45 C40 C41 F6 -178.2(2) . . . . ?
B1 C40 C41 F6 -1.5(3) . . . . ?
C45 C40 C41 C42 1.2(3) . . . . ?
B1 C40 C41 C42 177.9(2) . . . . ?
C9 N2 C7 C6 -1.7(3) . . . . ?
Ge1 N2 C7 C6 169.91(17) . . . . ?
C9 N2 C7 C1 -180.0(2) . . . . ?
Ge1 N2 C7 C1 -8.4(2) . . . . ?
C5 C6 C7 N2 -177.8(3) . . . . ?
C5 C6 C7 C1 0.3(4) . . . . ?
N1 C1 C7 N2 1.7(3) . . . . ?
C2 C1 C7 N2 -177.4(2) . . . . ?
N1 C1 C7 C6 -176.5(2) . . . . ?
C2 C1 C7 C6 4.4(4) . . . . ?
F13 C49 C48 F12 -1.5(4) . . . . ?
C50 C49 C48 F12 178.2(2) . . . . ?
F13 C49 C48 C47 177.6(2) . . . . ?
C50 C49 C48 C47 -2.7(4) . . . . ?
F11 C47 C48 F12 -0.1(3) . . . . ?
C46 C47 C48 F12 179.2(2) . . . . ?
F11 C47 C48 C49 -179.2(2) . . . . ?
C46 C47 C48 C49 0.1(4) . . . . ?
C21 C16 C17 C18 1.3(4) . . . . ?
Si1 C16 C17 C18 179.4(2) . . . . ?
N1 C8 C10 C12 74.0(3) . . . . ?
N1 C8 C10 C13 -162.9(2) . . . . ?
F3 C37 C36 F2 1.7(4) . . . . ?
C38 C37 C36 F2 -177.5(2) . . . . ?
F3 C37 C36 C35 179.8(2) . . . . ?
C38 C37 C36 C35 0.6(4) . . . . ?
F1 C35 C36 F2 1.8(3) . . . . ?
C34 C35 C36 F2 179.4(2) . . . . ?
F1 C35 C36 C37 -176.3(2) . . . . ?
C34 C35 C36 C37 1.3(4) . . . . ?
C25 C26 C27 C22 -1.1(4) . . . . ?
C23 C22 C27 C26 -0.3(4) . . . . ?
Si1 C22 C27 C26 180.0(2) . . . . ?
C25 C24 C23 C22 -0.6(4) . . . . ?
C27 C22 C23 C24 1.1(4) . . . . ?
Si1 C22 C23 C24 -179.16(19) . . . . ?
F1 C35 C34 C39 175.0(2) . . . . ?
C36 C35 C34 C39 -2.5(3) . . . . ?
F1 C35 C34 B1 -2.6(3) . . . . ?
C36 C35 C34 B1 179.9(2) . . . . ?
F5 C39 C34 C35 -176.8(2) . . . . ?
C38 C39 C34 C35 2.0(3) . . . . ?
F5 C39 C34 B1 0.5(4) . . . . ?
C38 C39 C34 B1 179.3(2) . . . . ?
O2 B1 C34 C35 -50.9(3) . . . . ?
C46 B1 C34 C35 65.0(3) . . . . ?
C40 B1 C34 C35 -171.3(2) . . . . ?
O2 B1 C34 C39 131.9(2) . . . . ?
C46 B1 C34 C39 -112.2(3) . . . . ?
C40 B1 C34 C39 11.5(3) . . . . ?
C29 C28 C33 C32 0.5(4) . . . . ?
Si1 C28 C33 C32 177.7(2) . . . . ?
C5 C4 C3 C2 4.1(5) . . . . ?
C1 C2 C3 C4 -1.7(5) . . . . ?
C29 C30 C31 C32 -0.6(4) . . . . ?
C27 C26 C25 C24 1.6(4) . . . . ?
C23 C24 C25 C26 -0.8(4) . . . . ?
C19 C20 C21 C16 -0.3(5) . . . . ?
C17 C16 C21 C20 -1.2(4) . . . . ?
Si1 C16 C21 C20 -179.3(2) . . . . ?
N2 C9 C11 C14 54.6(3) . . . . ?
N2 C9 C11 C15 179.8(2) . . . . ?
C21 C20 C19 C18 1.7(5) . . . . ?
C20 C19 C18 C17 -1.6(5) . . . . ?
C16 C17 C18 C19 0.1(5) . . . . ?
C28 C33 C32 C31 -0.6(5) . . . . ?
C30 C31 C32 C33 0.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.154
####################################################################### 
# 
# 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_Compound_20__msh102_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1851014'
loop_
_audit_author_name
_audit_author_address
'Mahendra Kumar Sharma'
;IIT Delhi, India
India
;
_audit_update_record             
;
2018-06-22 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H32 B F15 Ge N2 O2'
_chemical_formula_sum            'C37 H32 B F15 Ge N2 O2'
_chemical_formula_weight         905.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.415(3)
_cell_length_b                   38.762(14)
_cell_length_c                   17.556(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.277(8)
_cell_angle_gamma                90
_cell_volume                     7722(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    918
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      16.28

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             3648.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.902
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            253267
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_av_R_equivalents  0.1875
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.961
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             19194
_reflns_number_gt                12820
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0384P)²+3.8265P] 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         19194
_refine_ls_number_parameters     1059
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Ge2 Ge 0.04250(2) 0.38421(2) 0.28686(2) 0.01711(7) Uani 1 1 d . . . . .
Ge1 Ge 0.80561(2) 0.13081(2) 0.32343(2) 0.01795(7) Uani 1 1 d . . . . .
F5 F 0.73371(14) 0.22855(5) 0.42149(10) 0.0276(4) Uani 1 1 d . . . . .
F20 F 0.47108(13) 0.45312(5) 0.29081(10) 0.0265(4) Uani 1 1 d . . . . .
F30 F 0.37017(15) 0.40072(5) 0.18837(9) 0.0285(4) Uani 1 1 d . . . . .
F15 F 0.58828(15) 0.17224(5) 0.12913(9) 0.0270(4) Uani 1 1 d . . . . .
F25 F 0.48334(14) 0.41788(5) 0.43745(10) 0.0269(4) Uani 1 1 d . . . . .
F16 F 0.05934(14) 0.46649(5) 0.22347(10) 0.0291(4) Uani 1 1 d . . . . .
F1 F 0.35523(14) 0.18754(5) 0.32167(10) 0.0292(4) Uani 1 1 d . . . . .
F26 F 0.28800(14) 0.37255(5) 0.44014(9) 0.0256(4) Uani 1 1 d . . . . .
F10 F 0.87769(14) 0.21149(5) 0.28720(11) 0.0337(5) Uani 1 1 d . . . . .
F11 F 0.49062(14) 0.12980(5) 0.36757(9) 0.0257(4) Uani 1 1 d . . . . .
F6 F 0.47122(14) 0.22521(5) 0.20511(10) 0.0285(4) Uani 1 1 d . . . . .
F12 F 0.34798(15) 0.08360(5) 0.29313(11) 0.0352(5) Uani 1 1 d . . . . .
F13 F 0.31886(14) 0.08231(5) 0.13673(11) 0.0357(5) Uani 1 1 d . . . . .
F14 F 0.43733(16) 0.12876(5) 0.05740(10) 0.0345(5) Uani 1 1 d . . . . .
F29 F 0.50155(16) 0.34435(5) 0.18632(10) 0.0361(5) Uani 1 1 d . . . . .
F2 F 0.26003(16) 0.22357(5) 0.42635(12) 0.0418(5) Uani 1 1 d . . . . .
F24 F 0.54082(15) 0.45429(5) 0.56220(10) 0.0362(5) Uani 1 1 d . . . . .
F28 F 0.52325(16) 0.30010(5) 0.30764(11) 0.0400(5) Uani 1 1 d . . . . .
F23 F 0.39565(18) 0.50471(6) 0.60601(11) 0.0469(6) Uani 1 1 d . . . . .
F7 F 0.52149(17) 0.27774(5) 0.11627(11) 0.0358(5) Uani 1 1 d . . . . .
F3 F 0.39511(19) 0.26222(5) 0.53120(11) 0.0432(5) Uani 1 1 d . . . . .
F9 F 0.92544(17) 0.26417(6) 0.19962(12) 0.0463(6) Uani 1 1 d . . . . .
F21 F 0.12586(15) 0.48140(5) 0.39327(11) 0.0343(5) Uani 1 1 d . . . . .
F17 F 0.10165(16) 0.51810(5) 0.13301(11) 0.0378(5) Uani 1 1 d . . . . .
F18 F 0.32626(19) 0.53988(6) 0.12056(12) 0.0473(6) Uani 1 1 d . . . . .
F27 F 0.41270(17) 0.31509(5) 0.43365(11) 0.0399(5) Uani 1 1 d . . . . .
F4 F 0.63247(18) 0.26655(5) 0.52187(10) 0.0386(5) Uani 1 1 d . . . . .
O3 O 0.12318(15) 0.41669(5) 0.33356(11) 0.0197(4) Uani 1 1 d . . . . .
O4 O -0.10801(16) 0.39101(6) 0.27539(12) 0.0250(5) Uani 1 1 d . . . . .
F19 F 0.51074(16) 0.50649(6) 0.20201(12) 0.0452(6) Uani 1 1 d . . . . .
F8 F 0.7500(2) 0.29816(6) 0.11254(12) 0.0482(6) Uani 1 1 d . . . . .
O1 O 0.72607(16) 0.16542(5) 0.34982(11) 0.0206(4) Uani 1 1 d . . . . .
O2 O 0.94043(17) 0.12624(6) 0.37713(12) 0.0292(5) Uani 1 1 d . . . . .
F22 F 0.18873(18) 0.51789(5) 0.51808(13) 0.0454(6) Uani 1 1 d . . . . .
N3 N 0.08565(19) 0.37084(7) 0.19286(13) 0.0191(5) Uani 1 1 d . . . . .
N2 N 0.8198(2) 0.12561(6) 0.22016(13) 0.0203(5) Uani 1 1 d . . . . .
N1 N 0.7263(2) 0.08909(6) 0.31745(14) 0.0200(5) Uani 1 1 d . . . . .
N4 N 0.0785(2) 0.33971(6) 0.31951(14) 0.0197(5) Uani 1 1 d . . . . .
C69 C 0.3257(2) 0.39080(7) 0.31606(16) 0.0171(6) Uani 1 1 d . . . . .
C32 C 0.5427(2) 0.15509(8) 0.25333(16) 0.0191(6) Uani 1 1 d . . . . .
C35 C 0.3895(2) 0.10600(8) 0.17391(18) 0.0248(7) Uani 1 1 d . . . . .
C33 C 0.4797(2) 0.13058(8) 0.28994(16) 0.0202(6) Uani 1 1 d . . . . .
C37 C 0.5268(2) 0.15234(8) 0.17403(16) 0.0198(6) Uani 1 1 d . . . . .
C49 C 0.0612(3) 0.32580(8) 0.39596(16) 0.0238(7) Uani 1 1 d . . . . .
H49A H 0.0375 0.3449 0.4283 0.029 Uiso 1 1 calc R U . . .
H49B H 0.1375 0.3168 0.4201 0.029 Uiso 1 1 calc R U . . .
C68 C 0.4039(2) 0.44179(8) 0.45453(16) 0.0203(6) Uani 1 1 d . . . . .
C36 C 0.4495(2) 0.12926(9) 0.13467(17) 0.0247(7) Uani 1 1 d . . . . .
C34 C 0.4045(2) 0.10655(8) 0.25338(19) 0.0237(7) Uani 1 1 d . . . . .
C26 C 0.6707(2) 0.21511(8) 0.25041(16) 0.0200(6) Uani 1 1 d . . . . .
C38 C 0.1346(2) 0.33899(8) 0.19414(16) 0.0198(6) Uani 1 1 d . . . . .
C74 C 0.3806(2) 0.38102(8) 0.25255(16) 0.0203(6) Uani 1 1 d . . . . .
C44 C 0.1315(2) 0.32119(8) 0.26726(17) 0.0206(6) Uani 1 1 d . . . . .
C57 C 0.2642(2) 0.45624(8) 0.26204(16) 0.0199(6) Uani 1 1 d . . . . .
C24 C 0.5655(3) 0.24523(8) 0.47458(17) 0.0272(7) Uani 1 1 d . . . . .
C1 C 0.6946(2) 0.07934(8) 0.24394(17) 0.0207(6) Uani 1 1 d . . . . .
C31 C 0.7842(3) 0.22677(8) 0.24586(17) 0.0246(7) Uani 1 1 d . . . . .
C30 C 0.8123(3) 0.25409(9) 0.20079(18) 0.0309(8) Uani 1 1 d . . . . .
C6 C 0.7216(2) 0.09896(9) 0.10796(17) 0.0249(7) Uani 1 1 d . . . . .
H6 H 0.7652 0.1146 0.0802 0.030 Uiso 1 1 calc R U . . .
C53 C -0.1835(3) 0.41276(8) 0.31798(18) 0.0252(7) Uani 1 1 d . . . . .
C25 C 0.6152(3) 0.22549(8) 0.42148(16) 0.0222(6) Uani 1 1 d . . . . .
C58 C 0.1744(2) 0.47464(8) 0.22021(17) 0.0217(6) Uani 1 1 d . . . . .
C70 C 0.3394(2) 0.36668(8) 0.37487(16) 0.0199(6) Uani 1 1 d . . . . .
C59 C 0.1936(3) 0.50212(8) 0.17328(18) 0.0281(7) Uani 1 1 d . . . . .
C20 C 0.5518(2) 0.20433(7) 0.36773(16) 0.0196(6) Uani 1 1 d . . . . .
C63 C 0.2980(2) 0.44666(7) 0.40849(16) 0.0185(6) Uani 1 1 d . . . . .
C7 C 0.7462(2) 0.10108(8) 0.18780(17) 0.0211(6) Uani 1 1 d . . . . .
C66 C 0.3657(3) 0.48615(9) 0.54226(18) 0.0304(8) Uani 1 1 d . . . . .
C22 C 0.3782(3) 0.22415(8) 0.42573(19) 0.0274(7) Uani 1 1 d . . . . .
C60 C 0.3067(3) 0.51317(9) 0.16640(19) 0.0316(8) Uani 1 1 d . . . . .
C71 C 0.4036(3) 0.33668(8) 0.37351(18) 0.0249(7) Uani 1 1 d . . . . .
C45 C 0.0661(2) 0.39358(8) 0.12561(16) 0.0229(6) Uani 1 1 d . . . . .
H45A H 0.1270 0.3888 0.0910 0.028 Uiso 1 1 calc R U . . .
H45B H 0.0754 0.4179 0.1427 0.028 Uiso 1 1 calc R U . . .
C5 C 0.6444(3) 0.07796(9) 0.06269(18) 0.0322(8) Uani 1 1 d . . . . .
H5 H 0.6388 0.0827 0.0093 0.039 Uiso 1 1 calc R U . . .
C50 C -0.0311(3) 0.29705(8) 0.39530(18) 0.0258(7) Uani 1 1 d . . . . .
H50 H -0.0112 0.2789 0.3583 0.031 Uiso 1 1 calc R U . . .
C46 C -0.0563(3) 0.38907(9) 0.08086(17) 0.0274(7) Uani 1 1 d . . . . .
H46 H -0.1165 0.3915 0.1178 0.033 Uiso 1 1 calc R U . . .
C27 C 0.5863(3) 0.23413(8) 0.20525(17) 0.0229(6) Uani 1 1 d . . . . .
C29 C 0.7249(3) 0.27136(9) 0.15699(18) 0.0310(8) Uani 1 1 d . . . . .
C43 C 0.1786(2) 0.28858(8) 0.28507(18) 0.0260(7) Uani 1 1 d . . . . .
H43 H 0.1744 0.2816 0.3366 0.031 Uiso 1 1 calc R U . . .
C62 C 0.3761(2) 0.46866(8) 0.25260(16) 0.0224(7) Uani 1 1 d . . . . .
C73 C 0.4472(2) 0.35130(8) 0.24917(17) 0.0240(7) Uani 1 1 d . . . . .
C21 C 0.4313(3) 0.20528(8) 0.37206(17) 0.0236(7) Uani 1 1 d . . . . .
C64 C 0.2307(2) 0.47335(8) 0.43294(18) 0.0237(7) Uani 1 1 d . . . . .
C39 C 0.1843(2) 0.32608(9) 0.13043(17) 0.0257(7) Uani 1 1 d . . . . .
H39 H 0.1820 0.3416 0.0885 0.031 Uiso 1 1 calc R U . . .
C12 C 0.8994(2) 0.14616(9) 0.17753(17) 0.0262(7) Uani 1 1 d . . . . .
H12A H 0.9356 0.1646 0.2114 0.031 Uiso 1 1 calc R U . . .
H12B H 0.8528 0.1574 0.1335 0.031 Uiso 1 1 calc R U . . .
C4 C 0.5743(3) 0.05113(9) 0.0831(2) 0.0338(8) Uani 1 1 d . . . . .
H4 H 0.5256 0.0402 0.0428 0.041 Uiso 1 1 calc R U . . .
C42 C 0.2304(3) 0.26447(9) 0.2407(2) 0.0323(8) Uani 1 1 d . . . . .
H42 H 0.2523 0.2434 0.2658 0.039 Uiso 1 1 calc R U . . .
C52 C -0.0231(3) 0.28092(10) 0.47474(19) 0.0416(10) Uani 1 1 d . . . . .
H52A H -0.0415 0.2984 0.5121 0.062 Uiso 1 1 calc R U . . .
H52B H 0.0568 0.2721 0.4888 0.062 Uiso 1 1 calc R U . . .
H52C H -0.0796 0.2619 0.4746 0.062 Uiso 1 1 calc R U . . .
C40 C 0.2360(3) 0.29464(9) 0.11805(19) 0.0311(8) Uani 1 1 d . . . . .
H40 H 0.2626 0.2920 0.0690 0.037 Uiso 1 1 calc R U . . .
C23 C 0.4452(3) 0.24399(8) 0.47798(18) 0.0293(7) Uani 1 1 d . . . . .
C28 C 0.6099(3) 0.26144(8) 0.15938(18) 0.0274(7) Uani 1 1 d . . . . .
C67 C 0.4369(3) 0.46078(8) 0.52016(16) 0.0237(7) Uani 1 1 d . . . . .
C72 C 0.4600(3) 0.32913(8) 0.31043(19) 0.0264(7) Uani 1 1 d . . . . .
C65 C 0.2612(3) 0.49276(8) 0.49792(19) 0.0288(7) Uani 1 1 d . . . . .
C16 C 0.9830(3) 0.14328(10) 0.44964(18) 0.0336(8) Uani 1 1 d . . . . .
C41 C 0.2547(3) 0.26666(10) 0.1657(2) 0.0358(9) Uani 1 1 d . . . . .
H41 H 0.2879 0.2468 0.1448 0.043 Uiso 1 1 calc R U . . .
C54 C -0.3053(3) 0.39735(10) 0.3003(2) 0.0371(9) Uani 1 1 d . . . . .
H54A H -0.3301 0.3992 0.2452 0.056 Uiso 1 1 calc R U . . .
H54B H -0.3611 0.4099 0.3288 0.056 Uiso 1 1 calc R U . . .
H54C H -0.3036 0.3730 0.3155 0.056 Uiso 1 1 calc R U . . .
C2 C 0.6215(3) 0.05086(8) 0.2259(2) 0.0298(7) Uani 1 1 d . . . . .
H2 H 0.6056 0.0375 0.2690 0.036 Uiso 1 1 calc R U . . .
C61 C 0.3996(3) 0.49614(9) 0.20732(18) 0.0295(7) Uani 1 1 d . . . . .
C47 C -0.0719(3) 0.35357(9) 0.04342(19) 0.0344(8) Uani 1 1 d . . . . .
H47A H -0.1513 0.3517 0.0163 0.052 Uiso 1 1 calc R U . . .
H47B H -0.0608 0.3357 0.0830 0.052 Uiso 1 1 calc R U . . .
H47C H -0.0135 0.3505 0.0070 0.052 Uiso 1 1 calc R U . . .
C48 C -0.0762(3) 0.41806(9) 0.0217(2) 0.0391(9) Uani 1 1 d . . . . .
H48A H -0.0158 0.4168 -0.0138 0.059 Uiso 1 1 calc R U . . .
H48B H -0.0711 0.4404 0.0479 0.059 Uiso 1 1 calc R U . . .
H48C H -0.1544 0.4155 -0.0069 0.059 Uiso 1 1 calc R U . . .
C8 C 0.6851(3) 0.07106(8) 0.38330(17) 0.0257(7) Uani 1 1 d . . . . .
H8A H 0.6003 0.0657 0.3712 0.031 Uiso 1 1 calc R U . . .
H8B H 0.6929 0.0868 0.4280 0.031 Uiso 1 1 calc R U . . .
C55 C -0.1424(3) 0.41022(10) 0.40313(19) 0.0367(9) Uani 1 1 d . . . . .
H55A H -0.1375 0.3859 0.4184 0.055 Uiso 1 1 calc R U . . .
H55B H -0.1987 0.4222 0.4323 0.055 Uiso 1 1 calc R U . . .
H55C H -0.0646 0.4209 0.4136 0.055 Uiso 1 1 calc R U . . .
C51 C -0.1549(3) 0.30994(9) 0.3699(2) 0.0361(8) Uani 1 1 d . . . . .
H51A H -0.2100 0.2905 0.3672 0.054 Uiso 1 1 calc R U . . .
H51B H -0.1568 0.3207 0.3194 0.054 Uiso 1 1 calc R U . . .
H51C H -0.1778 0.3269 0.4070 0.054 Uiso 1 1 calc R U . . .
C13 C 0.9977(3) 0.12451(10) 0.14794(19) 0.0342(8) Uani 1 1 d . . . . .
H13 H 0.9607 0.1078 0.1091 0.041 Uiso 1 1 calc R U . . .
B2 B 0.2496(3) 0.42616(9) 0.32791(18) 0.0176(7) Uani 1 1 d . . . . .
C56 C -0.1775(3) 0.44942(9) 0.2902(2) 0.0417(9) Uani 1 1 d . . . . .
H56A H -0.0982 0.4586 0.3046 0.063 Uiso 1 1 calc R U . . .
H56B H -0.2352 0.4635 0.3135 0.063 Uiso 1 1 calc R U . . .
H56C H -0.1951 0.4500 0.2343 0.063 Uiso 1 1 calc R U . . .
C18 C 1.0134(3) 0.18013(11) 0.4334(2) 0.0490(11) Uani 1 1 d . . . . .
H18A H 1.0698 0.1807 0.3952 0.073 Uiso 1 1 calc R U . . .
H18B H 1.0484 0.1911 0.4808 0.073 Uiso 1 1 calc R U . . .
H18C H 0.9417 0.1926 0.4137 0.073 Uiso 1 1 calc R U . . .
B1 B 0.6254(3) 0.18386(9) 0.30456(18) 0.0177(7) Uani 1 1 d . . . . .
C9 C 0.7518(3) 0.03744(9) 0.4057(2) 0.0361(9) Uani 1 1 d . . . . .
H9 H 0.7511 0.0227 0.3589 0.043 Uiso 1 1 calc R U . . .
C3 C 0.5681(3) 0.03873(9) 0.1563(2) 0.0336(8) Uani 1 1 d . . . . .
H3 H 0.5200 0.0189 0.1594 0.040 Uiso 1 1 calc R U . . .
C11 C 0.8786(3) 0.04352(10) 0.4376(2) 0.0448(10) Uani 1 1 d . . . . .
H11A H 0.8808 0.0560 0.4864 0.067 Uiso 1 1 calc R U . . .
H11B H 0.9182 0.0572 0.4012 0.067 Uiso 1 1 calc R U . . .
H11C H 0.9189 0.0213 0.4461 0.067 Uiso 1 1 calc R U . . .
C17 C 0.8895(3) 0.14120(11) 0.50429(19) 0.0454(10) Uani 1 1 d . . . . .
H17A H 0.8189 0.1537 0.4825 0.068 Uiso 1 1 calc R U . . .
H17B H 0.9195 0.1516 0.5534 0.068 Uiso 1 1 calc R U . . .
H17C H 0.8695 0.1170 0.5123 0.068 Uiso 1 1 calc R U . . .
C14 C 1.0661(3) 0.10405(12) 0.2129(2) 0.0558(12) Uani 1 1 d . . . . .
H14A H 1.1275 0.0903 0.1923 0.084 Uiso 1 1 calc R U . . .
H14B H 1.0120 0.0887 0.2363 0.084 Uiso 1 1 calc R U . . .
H14C H 1.1025 0.1201 0.2518 0.084 Uiso 1 1 calc R U . . .
C15 C 1.0773(3) 0.14829(13) 0.1088(2) 0.0616(13) Uani 1 1 d . . . . .
H15A H 1.0297 0.1624 0.0708 0.092 Uiso 1 1 calc R U . . .
H15B H 1.1335 0.1345 0.0832 0.092 Uiso 1 1 calc R U . . .
H15C H 1.1203 0.1633 0.1470 0.092 Uiso 1 1 calc R U . . .
C19 C 1.0916(3) 0.12236(11) 0.4786(2) 0.0564(13) Uani 1 1 d . . . . .
H19A H 1.0693 0.0982 0.4846 0.085 Uiso 1 1 calc R U . . .
H19B H 1.1256 0.1315 0.5283 0.085 Uiso 1 1 calc R U . . .
H19C H 1.1499 0.1239 0.4418 0.085 Uiso 1 1 calc R U . . .
C10 C 0.6860(4) 0.01838(12) 0.4641(3) 0.0712(16) Uani 1 1 d . . . . .
H10A H 0.7225 -0.0042 0.4750 0.107 Uiso 1 1 calc R U . . .
H10B H 0.6035 0.0152 0.4433 0.107 Uiso 1 1 calc R U . . .
H10C H 0.6897 0.0319 0.5115 0.107 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 O3 1.7149(19) . ?
Ge2 O4 1.7281(19) . ?
Ge2 N3 1.847(2) . ?
Ge2 N4 1.849(3) . ?
Ge1 O1 1.712(2) . ?
Ge1 O2 1.7237(18) . ?
Ge1 N2 1.849(2) . ?
Ge1 N1 1.851(3) . ?
F5 C25 1.357(3) . ?
F20 C62 1.352(3) . ?
F30 C74 1.356(3) . ?
F15 C37 1.353(3) . ?
F25 C68 1.353(3) . ?
F16 C58 1.359(3) . ?
F1 C21 1.357(3) . ?
F26 C70 1.362(3) . ?
F10 C31 1.359(3) . ?
F11 C33 1.355(3) . ?
F6 C27 1.358(3) . ?
F12 C34 1.339(3) . ?
F13 C35 1.343(3) . ?
F14 C36 1.348(3) . ?
F29 C73 1.351(3) . ?
F2 C22 1.350(3) . ?
F24 C67 1.351(3) . ?
F28 C72 1.341(3) . ?
F23 C66 1.343(3) . ?
F7 C28 1.351(3) . ?
F3 C23 1.348(3) . ?
F9 C30 1.351(3) . ?
F21 C64 1.353(3) . ?
F17 C59 1.350(3) . ?
F18 C60 1.345(4) . ?
F27 C71 1.342(3) . ?
F4 C24 1.348(3) . ?
O3 B2 1.502(3) . ?
O4 C53 1.467(3) . ?
F19 C61 1.344(3) . ?
F8 C29 1.349(4) . ?
O1 B1 1.505(3) . ?
O2 C16 1.469(3) . ?
F22 C65 1.350(4) . ?
N3 C38 1.354(4) . ?
N3 C45 1.471(3) . ?
N2 C7 1.352(3) . ?
N2 C12 1.473(4) . ?
N1 C1 1.355(3) . ?
N1 C8 1.471(4) . ?
N4 C44 1.359(4) . ?
N4 C49 1.480(4) . ?
C69 C70 1.389(4) . ?
C69 C74 1.390(4) . ?
C69 B2 1.648(4) . ?
C32 C37 1.388(4) . ?
C32 C33 1.391(4) . ?
C32 B1 1.661(4) . ?
C35 C36 1.364(4) . ?
C35 C34 1.387(4) . ?
C33 C34 1.377(4) . ?
C37 C36 1.386(4) . ?
C49 C50 1.533(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C68 C67 1.384(4) . ?
C68 C63 1.392(4) . ?
C26 C31 1.383(4) . ?
C26 C27 1.390(4) . ?
C26 B1 1.657(4) . ?
C38 C39 1.401(4) . ?
C38 C44 1.461(4) . ?
C74 C73 1.385(4) . ?
C44 C43 1.395(4) . ?
C57 C58 1.390(4) . ?
C57 C62 1.393(4) . ?
C57 B2 1.664(4) . ?
C24 C25 1.376(4) . ?
C24 C23 1.382(4) . ?
C1 C2 1.399(4) . ?
C1 C7 1.468(4) . ?
C31 C30 1.380(4) . ?
C30 C29 1.367(5) . ?
C6 C5 1.385(4) . ?
C6 C7 1.401(4) . ?
C6 H6 0.9500 . ?
C53 C56 1.507(5) . ?
C53 C54 1.515(4) . ?
C53 C55 1.520(4) . ?
C25 C20 1.392(4) . ?
C58 C59 1.379(4) . ?
C70 C71 1.376(4) . ?
C59 C60 1.378(4) . ?
C20 C21 1.387(4) . ?
C20 B1 1.664(4) . ?
C63 C64 1.385(4) . ?
C63 B2 1.663(4) . ?
C66 C67 1.359(4) . ?
C66 C65 1.376(4) . ?
C22 C23 1.366(4) . ?
C22 C21 1.384(4) . ?
C60 C61 1.382(4) . ?
C71 C72 1.372(4) . ?
C45 C46 1.536(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C5 C4 1.383(5) . ?
C5 H5 0.9500 . ?
C50 C51 1.519(4) . ?
C50 C52 1.522(4) . ?
C50 H50 1.0000 . ?
C46 C47 1.527(4) . ?
C46 C48 1.530(4) . ?
C46 H46 1.0000 . ?
C27 C28 1.374(4) . ?
C29 C28 1.373(4) . ?
C43 C42 1.390(4) . ?
C43 H43 0.9500 . ?
C62 C61 1.373(4) . ?
C73 C72 1.372(4) . ?
C64 C65 1.379(4) . ?
C39 C40 1.382(4) . ?
C39 H39 0.9500 . ?
C12 C13 1.536(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C4 C3 1.381(5) . ?
C4 H4 0.9500 . ?
C42 C41 1.378(5) . ?
C42 H42 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C40 C41 1.372(5) . ?
C40 H40 0.9500 . ?
C16 C18 1.504(5) . ?
C16 C17 1.514(5) . ?
C16 C19 1.522(4) . ?
C41 H41 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C8 C9 1.539(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C13 C15 1.511(5) . ?
C13 C14 1.531(5) . ?
C13 H13 1.0000 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C9 C11 1.512(5) . ?
C9 C10 1.527(5) . ?
C9 H9 1.0000 . ?
C3 H3 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
O3 Ge2 O4 114.76(9) . . ?
O3 Ge2 N3 116.83(10) . . ?
O4 Ge2 N3 107.31(10) . . ?
O3 Ge2 N4 116.55(10) . . ?
O4 Ge2 N4 111.27(10) . . ?
N3 Ge2 N4 86.75(11) . . ?
O1 Ge1 O2 113.62(9) . . ?
O1 Ge1 N2 117.18(10) . . ?
O2 Ge1 N2 110.87(10) . . ?
O1 Ge1 N1 115.42(10) . . ?
O2 Ge1 N1 110.08(11) . . ?
N2 Ge1 N1 86.79(11) . . ?
B2 O3 Ge2 128.11(18) . . ?
C53 O4 Ge2 131.29(17) . . ?
B1 O1 Ge1 128.80(17) . . ?
C16 O2 Ge1 128.24(18) . . ?
C38 N3 C45 125.9(2) . . ?
C38 N3 Ge2 113.01(19) . . ?
C45 N3 Ge2 121.1(2) . . ?
C7 N2 C12 123.8(2) . . ?
C7 N2 Ge1 111.8(2) . . ?
C12 N2 Ge1 124.37(19) . . ?
C1 N1 C8 122.7(3) . . ?
C1 N1 Ge1 112.1(2) . . ?
C8 N1 Ge1 124.53(19) . . ?
C44 N4 C49 122.2(3) . . ?
C44 N4 Ge2 112.6(2) . . ?
C49 N4 Ge2 125.0(2) . . ?
C70 C69 C74 112.9(3) . . ?
C70 C69 B2 118.9(3) . . ?
C74 C69 B2 128.2(3) . . ?
C37 C32 C33 113.2(3) . . ?
C37 C32 B1 126.8(3) . . ?
C33 C32 B1 120.0(3) . . ?
F13 C35 C36 121.0(3) . . ?
F13 C35 C34 120.0(3) . . ?
C36 C35 C34 119.0(3) . . ?
F11 C33 C34 116.0(3) . . ?
F11 C33 C32 119.0(3) . . ?
C34 C33 C32 125.1(3) . . ?
F15 C37 C36 114.8(3) . . ?
F15 C37 C32 121.4(3) . . ?
C36 C37 C32 123.8(3) . . ?
N4 C49 C50 114.7(2) . . ?
N4 C49 H49A 108.6 . . ?
C50 C49 H49A 108.6 . . ?
N4 C49 H49B 108.6 . . ?
C50 C49 H49B 108.6 . . ?
H49A C49 H49B 107.6 . . ?
F25 C68 C67 114.9(2) . . ?
F25 C68 C63 121.7(3) . . ?
C67 C68 C63 123.5(3) . . ?
F14 C36 C35 119.7(3) . . ?
F14 C36 C37 120.1(3) . . ?
C35 C36 C37 120.1(3) . . ?
F12 C34 C33 121.2(3) . . ?
F12 C34 C35 120.0(3) . . ?
C33 C34 C35 118.8(3) . . ?
C31 C26 C27 112.9(3) . . ?
C31 C26 B1 128.7(3) . . ?
C27 C26 B1 118.3(2) . . ?
N3 C38 C39 121.0(3) . . ?
N3 C38 C44 113.3(3) . . ?
C39 C38 C44 125.7(3) . . ?
F30 C74 C73 115.6(3) . . ?
F30 C74 C69 120.4(3) . . ?
C73 C74 C69 124.0(3) . . ?
N4 C44 C43 121.1(3) . . ?
N4 C44 C38 113.5(3) . . ?
C43 C44 C38 125.4(3) . . ?
C58 C57 C62 113.1(3) . . ?
C58 C57 B2 127.1(3) . . ?
C62 C57 B2 119.2(2) . . ?
F4 C24 C25 120.7(3) . . ?
F4 C24 C23 119.6(3) . . ?
C25 C24 C23 119.7(3) . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 C7 113.2(3) . . ?
C2 C1 C7 125.1(3) . . ?
F10 C31 C30 115.0(3) . . ?
F10 C31 C26 120.9(3) . . ?
C30 C31 C26 124.2(3) . . ?
F9 C30 C29 119.3(3) . . ?
F9 C30 C31 120.9(3) . . ?
C29 C30 C31 119.8(3) . . ?
C5 C6 C7 130.8(3) . . ?
C5 C6 H6 114.6 . . ?
C7 C6 H6 114.6 . . ?
O4 C53 C56 109.1(3) . . ?
O4 C53 C54 104.3(2) . . ?
C56 C53 C54 112.3(3) . . ?
O4 C53 C55 109.2(2) . . ?
C56 C53 C55 111.1(3) . . ?
C54 C53 C55 110.7(3) . . ?
F5 C25 C24 115.9(3) . . ?
F5 C25 C20 119.7(3) . . ?
C24 C25 C20 124.4(3) . . ?
F16 C58 C59 115.0(3) . . ?
F16 C58 C57 121.2(3) . . ?
C59 C58 C57 123.8(3) . . ?
F26 C70 C71 115.8(3) . . ?
F26 C70 C69 119.3(3) . . ?
C71 C70 C69 125.0(3) . . ?
F17 C59 C60 119.6(3) . . ?
F17 C59 C58 120.1(3) . . ?
C60 C59 C58 120.3(3) . . ?
C21 C20 C25 113.1(3) . . ?
C21 C20 B1 128.7(3) . . ?
C25 C20 B1 118.0(3) . . ?
C64 C63 C68 113.4(3) . . ?
C64 C63 B2 118.5(2) . . ?
C68 C63 B2 128.0(3) . . ?
N2 C7 C6 120.6(3) . . ?
N2 C7 C1 113.5(3) . . ?
C6 C7 C1 125.9(3) . . ?
F23 C66 C67 121.4(3) . . ?
F23 C66 C65 119.8(3) . . ?
C67 C66 C65 118.8(3) . . ?
F2 C22 C23 119.4(3) . . ?
F2 C22 C21 120.6(3) . . ?
C23 C22 C21 120.0(3) . . ?
F18 C60 C59 120.7(3) . . ?
F18 C60 C61 120.7(3) . . ?
C59 C60 C61 118.6(3) . . ?
F27 C71 C72 119.9(3) . . ?
F27 C71 C70 120.6(3) . . ?
C72 C71 C70 119.5(3) . . ?
N3 C45 C46 113.1(2) . . ?
N3 C45 H45A 109.0 . . ?
C46 C45 H45A 109.0 . . ?
N3 C45 H45B 109.0 . . ?
C46 C45 H45B 109.0 . . ?
H45A C45 H45B 107.8 . . ?
C4 C5 C6 130.1(3) . . ?
C4 C5 H5 115.0 . . ?
C6 C5 H5 115.0 . . ?
C51 C50 C52 111.3(3) . . ?
C51 C50 C49 112.3(3) . . ?
C52 C50 C49 108.6(2) . . ?
C51 C50 H50 108.1 . . ?
C52 C50 H50 108.1 . . ?
C49 C50 H50 108.1 . . ?
C47 C46 C48 111.6(3) . . ?
C47 C46 C45 112.3(3) . . ?
C48 C46 C45 108.8(3) . . ?
C47 C46 H46 108.0 . . ?
C48 C46 H46 108.0 . . ?
C45 C46 H46 108.0 . . ?
F6 C27 C28 116.5(3) . . ?
F6 C27 C26 118.4(3) . . ?
C28 C27 C26 125.1(3) . . ?
F8 C29 C30 121.0(3) . . ?
F8 C29 C28 119.8(3) . . ?
C30 C29 C28 119.2(3) . . ?
C42 C43 C44 131.3(3) . . ?
C42 C43 H43 114.3 . . ?
C44 C43 H43 114.3 . . ?
F20 C62 C61 115.9(3) . . ?
F20 C62 C57 118.9(3) . . ?
C61 C62 C57 125.2(3) . . ?
F29 C73 C72 119.8(3) . . ?
F29 C73 C74 120.3(3) . . ?
C72 C73 C74 120.0(3) . . ?
F1 C21 C22 114.5(3) . . ?
F1 C21 C20 121.2(3) . . ?
C22 C21 C20 124.3(3) . . ?
F21 C64 C65 115.4(3) . . ?
F21 C64 C63 120.1(3) . . ?
C65 C64 C63 124.4(3) . . ?
C40 C39 C38 131.1(3) . . ?
C40 C39 H39 114.4 . . ?
C38 C39 H39 114.4 . . ?
N2 C12 C13 113.0(3) . . ?
N2 C12 H12A 109.0 . . ?
C13 C12 H12A 109.0 . . ?
N2 C12 H12B 109.0 . . ?
C13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C3 C4 C5 126.3(3) . . ?
C3 C4 H4 116.8 . . ?
C5 C4 H4 116.8 . . ?
C41 C42 C43 129.6(3) . . ?
C41 C42 H42 115.2 . . ?
C43 C42 H42 115.2 . . ?
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 . . ?
C41 C40 C39 130.0(3) . . ?
C41 C40 H40 115.0 . . ?
C39 C40 H40 115.0 . . ?
F3 C23 C22 120.8(3) . . ?
F3 C23 C24 120.7(3) . . ?
C22 C23 C24 118.5(3) . . ?
F7 C28 C29 120.7(3) . . ?
F7 C28 C27 120.4(3) . . ?
C29 C28 C27 118.9(3) . . ?
F24 C67 C66 119.7(3) . . ?
F24 C67 C68 119.9(3) . . ?
C66 C67 C68 120.4(3) . . ?
F28 C72 C73 120.6(3) . . ?
F28 C72 C71 120.7(3) . . ?
C73 C72 C71 118.7(3) . . ?
F22 C65 C66 120.3(3) . . ?
F22 C65 C64 120.2(3) . . ?
C66 C65 C64 119.5(3) . . ?
O2 C16 C18 108.9(3) . . ?
O2 C16 C17 109.6(3) . . ?
C18 C16 C17 111.3(3) . . ?
O2 C16 C19 103.3(3) . . ?
C18 C16 C19 111.9(3) . . ?
C17 C16 C19 111.4(3) . . ?
C40 C41 C42 126.6(3) . . ?
C40 C41 H41 116.7 . . ?
C42 C41 H41 116.7 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C3 C2 C1 131.3(3) . . ?
C3 C2 H2 114.3 . . ?
C1 C2 H2 114.3 . . ?
F19 C61 C62 121.2(3) . . ?
F19 C61 C60 119.9(3) . . ?
C62 C61 C60 119.0(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N1 C8 C9 114.2(3) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
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 . . ?
C15 C13 C14 111.8(3) . . ?
C15 C13 C12 108.5(3) . . ?
C14 C13 C12 111.3(3) . . ?
C15 C13 H13 108.4 . . ?
C14 C13 H13 108.4 . . ?
C12 C13 H13 108.4 . . ?
O3 B2 C69 109.2(2) . . ?
O3 B2 C63 107.0(2) . . ?
C69 B2 C63 112.0(2) . . ?
O3 B2 C57 112.8(2) . . ?
C69 B2 C57 113.6(2) . . ?
C63 B2 C57 101.9(2) . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 B1 C26 112.5(2) . . ?
O1 B1 C32 108.8(2) . . ?
C26 B1 C32 112.0(2) . . ?
O1 B1 C20 106.7(2) . . ?
C26 B1 C20 104.2(2) . . ?
C32 B1 C20 112.5(2) . . ?
C11 C9 C10 110.3(3) . . ?
C11 C9 C8 112.9(3) . . ?
C10 C9 C8 108.4(3) . . ?
C11 C9 H9 108.4 . . ?
C10 C9 H9 108.4 . . ?
C8 C9 H9 108.4 . . ?
C4 C3 C2 129.8(3) . . ?
C4 C3 H3 115.1 . . ?
C2 C3 H3 115.1 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.077

