# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_rei134
_database_code_depnum_ccdc_archive 'CCDC 1429594'
_audit_update_record             
;
2015-10-06 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H48 F3 Ge N3 O3 S'
_chemical_formula_iupac          ?
_chemical_formula_weight         720.41

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   11.7454(9)
_cell_length_b                   24.4796(19)
_cell_length_c                   13.3037(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.166(2)
_cell_angle_gamma                90
_cell_volume                     3462.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4716
_cell_measurement_theta_min      2.5377
_cell_measurement_theta_max      24.0630
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512

_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/3 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            40551
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_full        28.44
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             8645
_reflns_number_gt                6433
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1184
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.008
_refine_ls_number_reflns         8645
_refine_ls_number_parameters     504
_refine_ls_number_restraints     531
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+1.9303P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.664
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables 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'
S S 0.1246 0.1234 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.7890(2) 0.15126(11) 0.4121(2) 0.0187(5) Uani d . . . 1.0 . .
H H1A 0.8529 0.1415 0.4861 0.028 Uiso calc U . R 1.0 . .
H H1B 0.7923 0.1906 0.4005 0.028 Uiso calc U . R 1.0 . .
H H1C 0.8053 0.1314 0.3556 0.028 Uiso calc U . R 1.0 . .
C C2 0.5739(2) 0.06700(10) 0.2947(2) 0.0140(5) Uani d . . . 1.0 . .
C C3 0.5075(2) -0.01376(10) 0.1951(2) 0.0194(5) Uani d . . . 1.0 . .
H H3A 0.4406 -0.0347 0.2046 0.023 Uiso calc U . R 1.0 . .
H H3B 0.5557 -0.0387 0.1691 0.023 Uiso calc U . R 1.0 . .
C C4 0.4523(2) 0.03378(10) 0.1146(2) 0.0156(5) Uani d . . . 1.0 . .
H H4A 0.4922 0.037 0.0626 0.019 Uiso calc U . R 1.0 . .
H H4B 0.3602 0.0299 0.0716 0.019 Uiso calc U . R 1.0 . .
C C5 0.6724(2) -0.01890(10) 0.3982(2) 0.0141(5) Uani d U . D 1.0 . .
C C6 0.5921(4) -0.06644(16) 0.4101(3) 0.0219(8) Uani d U P D 0.713(3) A 1
H H6A 0.5197 -0.0517 0.4212 0.026 Uiso calc U P R 0.713(3) A 1
H H6B 0.5591 -0.0889 0.3417 0.026 Uiso calc U P R 0.713(3) A 1
C C7 0.7810(3) -0.04034(17) 0.3791(3) 0.0215(8) Uani d U P D 0.713(3) A 1
H H7A 0.8311 -0.0096 0.3709 0.026 Uiso calc U P R 0.713(3) A 1
H H7B 0.7497 -0.0623 0.3101 0.026 Uiso calc U P R 0.713(3) A 1
C C8 0.7184(3) 0.01560(14) 0.5044(3) 0.0177(7) Uani d U P D 0.713(3) A 1
H H8A 0.6455 0.0297 0.5154 0.021 Uiso calc U P R 0.713(3) A 1
H H8B 0.7677 0.0471 0.498 0.021 Uiso calc U P R 0.713(3) A 1
C C9 0.7225(4) -0.06774(19) 0.6153(4) 0.0239(9) Uani d U P . 0.713(3) A 1
H H9A 0.775 -0.0908 0.6796 0.029 Uiso calc U P R 0.713(3) A 1
H H9B 0.6509 -0.0535 0.6281 0.029 Uiso calc U P R 0.713(3) A 1
C C10 0.6742(5) -0.10148(19) 0.5095(4) 0.0263(9) Uani d U P . 0.713(3) A 1
H H10 0.6233 -0.1327 0.5168 0.032 Uiso calc U P R 0.713(3) A 1
C C11 0.7835(5) -0.12347(18) 0.4894(4) 0.0292(10) Uani d U P . 0.713(3) A 1
H H11A 0.7511 -0.1453 0.4202 0.035 Uiso calc U P R 0.713(3) A 1
H H11B 0.8359 -0.1476 0.5516 0.035 Uiso calc U P R 0.713(3) A 1
C C12 0.8639(4) -0.07624(18) 0.4795(4) 0.0246(8) Uani d U P . 0.713(3) A 1
H H12 0.9366 -0.0911 0.4676 0.03 Uiso calc U P R 0.713(3) A 1
C C13 0.9125(4) -0.0424(2) 0.5856(4) 0.0211(8) Uani d U P . 0.713(3) A 1
H H13A 0.9642 -0.0117 0.5796 0.025 Uiso calc U P R 0.713(3) A 1
H H13B 0.9659 -0.0653 0.6497 0.025 Uiso calc U P R 0.713(3) A 1
C C14 0.8008(4) -0.02014(18) 0.6034(4) 0.0185(9) Uani d U P . 0.713(3) A 1
H H14 0.8326 0.0024 0.6727 0.022 Uiso calc U P R 0.713(3) A 1
C C6A 0.6017(8) -0.0341(4) 0.4632(8) 0.0206(15) Uani d U P D 0.287(3) A 2
H H6A1 0.5264 -0.0554 0.4155 0.025 Uiso calc U P R 0.287(3) A 2
H H6A2 0.5729 -0.0005 0.4867 0.025 Uiso calc U P R 0.287(3) A 2
C C7A 0.7231(9) -0.0723(4) 0.3632(8) 0.0217(15) Uani d U P D 0.287(3) A 2
H H7A1 0.7717 -0.0619 0.3209 0.026 Uiso calc U P R 0.287(3) A 2
H H7A2 0.6512 -0.0952 0.3147 0.026 Uiso calc U P R 0.287(3) A 2
C C8A 0.7950(8) 0.0129(4) 0.4716(8) 0.0225(17) Uani d U P D 0.287(3) A 2
H H8A1 0.7724 0.0483 0.4943 0.027 Uiso calc U P R 0.287(3) A 2
H H8A2 0.8432 0.0206 0.4277 0.027 Uiso calc U P R 0.287(3) A 2
C C9A 0.9191(10) -0.0721(4) 0.5431(10) 0.0226(16) Uani d U P . 0.287(3) A 2
H H9A1 0.9724 -0.0935 0.6099 0.027 Uiso calc U P R 0.287(3) A 2
H H9A2 0.9706 -0.0631 0.5027 0.027 Uiso calc U P R 0.287(3) A 2
C C10A 0.8105(11) -0.1062(5) 0.4707(9) 0.0195(16) Uani d U P . 0.287(3) A 2
H H10A 0.8402 -0.1406 0.449 0.023 Uiso calc U P R 0.287(3) A 2
C C11A 0.6825(10) -0.0682(5) 0.5667(10) 0.0215(16) Uani d U P . 0.287(3) A 2
H H11C 0.6335 -0.0777 0.6101 0.026 Uiso calc U P R 0.287(3) A 2
C C12A 0.7260(11) -0.1193(4) 0.5294(9) 0.0209(17) Uani d U P . 0.287(3) A 2
H H12A 0.6517 -0.1401 0.4782 0.025 Uiso calc U P R 0.287(3) A 2
H H12B 0.773 -0.1426 0.5949 0.025 Uiso calc U P R 0.287(3) A 2
C C13A 0.8794(11) -0.0208(5) 0.5782(9) 0.0220(17) Uani d U P . 0.287(3) A 2
H H13C 0.9547 0.001 0.627 0.026 Uiso calc U P R 0.287(3) A 2
C C14A 0.7984(12) -0.0326(5) 0.6371(10) 0.0221(18) Uani d U P . 0.287(3) A 2
H H14A 0.7692 0.0024 0.6554 0.027 Uiso calc U P R 0.287(3) A 2
H H14B 0.8491 -0.0517 0.7077 0.027 Uiso calc U P R 0.287(3) A 2
C C15 0.4490(2) 0.13562(10) 0.1687(2) 0.0137(5) Uani d . . . 1.0 . .
C C16 0.3346(2) 0.14932(10) 0.0590(2) 0.0148(5) Uani d . . . 1.0 . .
C C17 0.3559(2) 0.12793(11) -0.0417(2) 0.0175(5) Uani d . . . 1.0 . .
H H17A 0.3033 0.1488 -0.1083 0.026 Uiso calc U . R 1.0 . .
H H17B 0.3332 0.0892 -0.0537 0.026 Uiso calc U . R 1.0 . .
H H17C 0.4446 0.1324 -0.0267 0.026 Uiso calc U . R 1.0 . .
C C18 0.2188(2) 0.12179(10) 0.0654(2) 0.0177(5) Uani d . . . 1.0 . .
H H18A 0.2073 0.1365 0.1289 0.026 Uiso calc U . R 1.0 . .
H H18B 0.2325 0.0823 0.0745 0.026 Uiso calc U . R 1.0 . .
H H18C 0.1435 0.1292 -0.0031 0.026 Uiso calc U . R 1.0 . .
C C19 0.3044(2) 0.21037(10) 0.0397(2) 0.0183(5) Uani d . . . 1.0 . .
H H19A 0.2291 0.2154 -0.0301 0.027 Uiso calc U . R 1.0 . .
H H19B 0.3755 0.2295 0.0355 0.027 Uiso calc U . R 1.0 . .
H H19C 0.2891 0.2252 0.1013 0.027 Uiso calc U . R 1.0 . .
C C20 0.5083(2) 0.22663(10) 0.2526(2) 0.0147(5) Uani d . . . 1.0 . .
C C21 0.5805(2) 0.25616(10) 0.2099(2) 0.0160(5) Uani d . . . 1.0 . .
C C22 0.6526(3) 0.22748(11) 0.1546(2) 0.0226(6) Uani d . . . 1.0 . .
H H22A 0.5936 0.2141 0.0814 0.034 Uiso calc U . R 1.0 . .
H H22B 0.699 0.1966 0.2005 0.034 Uiso calc U . R 1.0 . .
H H22C 0.7118 0.2531 0.1458 0.034 Uiso calc U . R 1.0 . .
C C23 0.5781(2) 0.31267(11) 0.2144(2) 0.0186(5) Uani d . . . 1.0 . .
H H23 0.6261 0.3332 0.1856 0.022 Uiso calc U . R 1.0 . .
C C24 0.5072(2) 0.34039(10) 0.2600(2) 0.0192(5) Uani d . . . 1.0 . .
C C25 0.5018(3) 0.40212(11) 0.2592(2) 0.0282(7) Uani d . . . 1.0 . .
H H25A 0.4557 0.4151 0.1827 0.042 Uiso calc U . R 1.0 . .
H H25B 0.5875 0.4169 0.2903 0.042 Uiso calc U . R 1.0 . .
H H25C 0.4588 0.4144 0.3041 0.042 Uiso calc U . R 1.0 . .
C C26 0.4395(2) 0.30974(10) 0.3040(2) 0.0184(5) Uani d . . . 1.0 . .
H H26 0.3923 0.3281 0.3367 0.022 Uiso calc U . R 1.0 . .
C C27 0.4390(2) 0.25292(10) 0.3016(2) 0.0159(5) Uani d . . . 1.0 . .
C C28 0.3582(2) 0.22137(11) 0.3441(2) 0.0202(6) Uani d . . . 1.0 . .
H H28A 0.2918 0.2022 0.2822 0.03 Uiso calc U . R 1.0 . .
H H28B 0.3199 0.2467 0.3779 0.03 Uiso calc U . R 1.0 . .
H H28C 0.4102 0.1948 0.3997 0.03 Uiso calc U . R 1.0 . .
C C29 0.6033(3) 0.17770(13) 0.7528(3) 0.0361(8) Uani d . . . 1.0 . .
H H29 0.6412 0.1429 0.7586 0.043 Uiso calc U . R 1.0 . .
C C30 0.5779(3) 0.19674(14) 0.8377(3) 0.0370(8) Uani d . . . 1.0 . .
H H30 0.5978 0.1752 0.9024 0.044 Uiso calc U . R 1.0 . .
C C31 0.5233(3) 0.24730(14) 0.8290(3) 0.0349(7) Uani d . . . 1.0 . .
H H31 0.506 0.2605 0.8882 0.042 Uiso calc U . R 1.0 . .
C C32 0.4933(3) 0.27897(13) 0.7360(3) 0.0302(7) Uani d . . . 1.0 . .
H H32 0.4553 0.3137 0.7307 0.036 Uiso calc U . R 1.0 . .
C C33 0.5191(3) 0.25978(14) 0.6501(3) 0.0333(7) Uani d . . . 1.0 . .
H H33 0.4992 0.2814 0.5855 0.04 Uiso calc U . R 1.0 . .
C C34 0.5740(3) 0.20897(15) 0.6586(3) 0.0385(8) Uani d . . . 1.0 . .
H H34 0.5916 0.1956 0.5996 0.046 Uiso calc U . R 1.0 . .
C C35 0.8779(3) 0.06258(12) 0.0397(3) 0.0285(7) Uani d . . . 1.0 . .
F F1 0.8376(2) 0.03159(9) -0.05117(18) 0.0546(6) Uani d . . . 1.0 . .
F F2 0.89577(19) 0.11265(8) 0.01042(18) 0.0467(5) Uani d . . . 1.0 . .
F F3 0.98956(18) 0.04382(10) 0.1108(2) 0.0601(6) Uani d . . . 1.0 . .
Ge Ge1 0.61893(2) 0.13133(2) 0.40015(2) 0.01504(8) Uani d . . . 1.0 . .
N N1 0.59093(19) 0.01393(8) 0.29956(17) 0.0153(4) Uani d . . . 1.0 . .
N N2 0.48387(19) 0.08098(8) 0.19120(17) 0.0139(4) Uani d . . . 1.0 . .
N N3 0.51358(18) 0.16780(8) 0.25140(17) 0.0136(4) Uani d . . . 1.0 . .
O O1 0.65230(18) 0.08226(8) 0.01110(17) 0.0301(5) Uani d . . . 1.0 . .
O O2 0.8214(2) 0.09867(9) 0.19377(17) 0.0331(5) Uani d . . . 1.0 . .
O O3 0.75945(19) 0.00591(8) 0.12786(16) 0.0269(4) Uani d . . . 1.0 . .
S S2 0.76536(6) 0.06245(3) 0.10101(5) 0.01677(14) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 Ge1 . 1.996(2) ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 N1 . 1.312(3) ?
C2 N2 . 1.375(3) ?
C2 Ge1 . 2.024(2) ?
C3 N1 . 1.481(3) ?
C3 C4 . 1.527(3) ?
C3 H3A . 0.99 ?
C3 H3B . 0.99 ?
C4 N2 . 1.480(3) ?
C4 H4A . 0.99 ?
C4 H4B . 0.99 ?
C5 C6A . 1.478(8) ?
C5 N1 . 1.489(3) ?
C5 C7 . 1.497(4) ?
C5 C8 . 1.533(4) ?
C5 C6 . 1.548(4) ?
C5 C8A . 1.561(8) ?
C5 C7A . 1.585(8) ?
C6 C10 . 1.527(6) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C7 C12 . 1.549(5) ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 C14 . 1.534(5) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C10 . 1.518(6) ?
C9 C14 . 1.533(6) ?
C9 H9A . 0.99 ?
C9 H9B . 0.99 ?
C10 C11 . 1.518(7) ?
C10 H10 . 1.0 ?
C11 C12 . 1.533(6) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 C13 . 1.524(6) ?
C12 H12 . 1.0 ?
C13 C14 . 1.529(6) ?
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
C14 H14 . 1.0 ?
C6A C11A . 1.544(14) ?
C6A H6A1 . 0.99 ?
C6A H6A2 . 0.99 ?
C7A C10A . 1.593(14) ?
C7A H7A1 . 0.99 ?
C7A H7A2 . 0.99 ?
C8A C13A . 1.576(14) ?
C8A H8A1 . 0.99 ?
C8A H8A2 . 0.99 ?
C9A C13A . 1.483(14) ?
C9A C10A . 1.485(16) ?
C9A H9A1 . 0.99 ?
C9A H9A2 . 0.99 ?
C10A C12A . 1.536(14) ?
C10A H10A . 1.0 ?
C11A C12A . 1.513(16) ?
C11A C14A . 1.551(16) ?
C11A H11C . 1.0 ?
C12A H12A . 0.99 ?
C12A H12B . 0.99 ?
C13A C14A . 1.495(16) ?
C13A H13C . 1.0 ?
C14A H14A . 0.99 ?
C14A H14B . 0.99 ?
C15 N3 . 1.302(3) ?
C15 N2 . 1.394(3) ?
C15 C16 . 1.543(3) ?
C16 C19 . 1.532(3) ?
C16 C18 . 1.553(3) ?
C16 C17 . 1.555(3) ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 H19A . 0.98 ?
C19 H19B . 0.98 ?
C19 H19C . 0.98 ?
C20 C27 . 1.398(3) ?
C20 C21 . 1.404(3) ?
C20 N3 . 1.442(3) ?
C21 C23 . 1.385(4) ?
C21 C22 . 1.511(4) ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 C24 . 1.397(4) ?
C23 H23 . 0.95 ?
C24 C26 . 1.390(4) ?
C24 C25 . 1.512(4) ?
C25 H25A . 0.98 ?
C25 H25B . 0.98 ?
C25 H25C . 0.98 ?
C26 C27 . 1.391(4) ?
C26 H26 . 0.95 ?
C27 C28 . 1.508(3) ?
C28 H28A . 0.98 ?
C28 H28B . 0.98 ?
C28 H28C . 0.98 ?
C29 C30 . 1.368(5) ?
C29 C34 . 1.381(5) ?
C29 H29 . 0.95 ?
C30 C31 . 1.376(4) ?
C30 H30 . 0.95 ?
C31 C32 . 1.373(4) ?
C31 H31 . 0.95 ?
C32 C33 . 1.382(4) ?
C32 H32 . 0.95 ?
C33 C34 . 1.384(5) ?
C33 H33 . 0.95 ?
C34 H34 . 0.95 ?
C35 F2 . 1.330(3) ?
C35 F3 . 1.330(4) ?
C35 F1 . 1.332(4) ?
C35 S2 . 1.825(3) ?
Ge1 N3 . 2.040(2) ?
O1 S2 . 1.442(2) ?
O2 S2 . 1.432(2) ?
O3 S2 . 1.438(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ge1 C1 H1A . . 109.5 ?
Ge1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
Ge1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 N2 . . 109.4(2) ?
N1 C2 Ge1 . . 138.29(19) ?
N2 C2 Ge1 . . 111.30(17) ?
N1 C3 C4 . . 102.93(19) ?
N1 C3 H3A . . 111.2 ?
C4 C3 H3A . . 111.2 ?
N1 C3 H3B . . 111.2 ?
C4 C3 H3B . . 111.2 ?
H3A C3 H3B . . 109.1 ?
N2 C4 C3 . . 101.81(19) ?
N2 C4 H4A . . 111.4 ?
C3 C4 H4A . . 111.4 ?
N2 C4 H4B . . 111.4 ?
C3 C4 H4B . . 111.4 ?
H4A C4 H4B . . 109.3 ?
C6A C5 N1 . . 109.9(4) ?
N1 C5 C7 . . 108.3(2) ?
N1 C5 C8 . . 110.9(2) ?
C7 C5 C8 . . 111.0(3) ?
N1 C5 C6 . . 107.7(2) ?
C7 C5 C6 . . 110.7(3) ?
C8 C5 C6 . . 108.2(3) ?
C6A C5 C8A . . 111.0(6) ?
N1 C5 C8A . . 111.0(4) ?
C6A C5 C7A . . 109.8(6) ?
N1 C5 C7A . . 111.5(4) ?
C8A C5 C7A . . 103.5(5) ?
C10 C6 C5 . . 108.8(3) ?
C10 C6 H6A . . 109.9 ?
C5 C6 H6A . . 109.9 ?
C10 C6 H6B . . 109.9 ?
C5 C6 H6B . . 109.9 ?
H6A C6 H6B . . 108.3 ?
C5 C7 C12 . . 108.7(3) ?
C5 C7 H7A . . 109.9 ?
C12 C7 H7A . . 109.9 ?
C5 C7 H7B . . 109.9 ?
C12 C7 H7B . . 109.9 ?
H7A C7 H7B . . 108.3 ?
C5 C8 C14 . . 108.9(3) ?
C5 C8 H8A . . 109.9 ?
C14 C8 H8A . . 109.9 ?
C5 C8 H8B . . 109.9 ?
C14 C8 H8B . . 109.9 ?
H8A C8 H8B . . 108.3 ?
C10 C9 C14 . . 108.8(4) ?
C10 C9 H9A . . 109.9 ?
C14 C9 H9A . . 109.9 ?
C10 C9 H9B . . 109.9 ?
C14 C9 H9B . . 109.9 ?
H9A C9 H9B . . 108.3 ?
C9 C10 C11 . . 110.2(4) ?
C9 C10 C6 . . 110.3(4) ?
C11 C10 C6 . . 108.4(4) ?
C9 C10 H10 . . 109.3 ?
C11 C10 H10 . . 109.3 ?
C6 C10 H10 . . 109.3 ?
C10 C11 C12 . . 110.2(4) ?
C10 C11 H11A . . 109.6 ?
C12 C11 H11A . . 109.6 ?
C10 C11 H11B . . 109.6 ?
C12 C11 H11B . . 109.6 ?
H11A C11 H11B . . 108.1 ?
C13 C12 C11 . . 109.4(4) ?
C13 C12 C7 . . 109.9(4) ?
C11 C12 C7 . . 108.5(4) ?
C13 C12 H12 . . 109.7 ?
C11 C12 H12 . . 109.7 ?
C7 C12 H12 . . 109.7 ?
C12 C13 C14 . . 109.2(3) ?
C12 C13 H13A . . 109.8 ?
C14 C13 H13A . . 109.8 ?
C12 C13 H13B . . 109.8 ?
C14 C13 H13B . . 109.8 ?
H13A C13 H13B . . 108.3 ?
C13 C14 C9 . . 109.7(4) ?
C13 C14 C8 . . 109.8(4) ?
C9 C14 C8 . . 109.6(4) ?
C13 C14 H14 . . 109.2 ?
C9 C14 H14 . . 109.2 ?
C8 C14 H14 . . 109.2 ?
C5 C6A C11A . . 111.9(7) ?
C5 C6A H6A1 . . 109.2 ?
C11A C6A H6A1 . . 109.2 ?
C5 C6A H6A2 . . 109.2 ?
C11A C6A H6A2 . . 109.2 ?
H6A1 C6A H6A2 . . 107.9 ?
C5 C7A C10A . . 110.2(7) ?
C5 C7A H7A1 . . 109.6 ?
C10A C7A H7A1 . . 109.6 ?
C5 C7A H7A2 . . 109.6 ?
C10A C7A H7A2 . . 109.6 ?
H7A1 C7A H7A2 . . 108.1 ?
C5 C8A C13A . . 111.2(7) ?
C5 C8A H8A1 . . 109.4 ?
C13A C8A H8A1 . . 109.4 ?
C5 C8A H8A2 . . 109.4 ?
C13A C8A H8A2 . . 109.4 ?
H8A1 C8A H8A2 . . 108.0 ?
C13A C9A C10A . . 112.4(9) ?
C13A C9A H9A1 . . 109.1 ?
C10A C9A H9A1 . . 109.1 ?
C13A C9A H9A2 . . 109.1 ?
C10A C9A H9A2 . . 109.1 ?
H9A1 C9A H9A2 . . 107.9 ?
C9A C10A C12A . . 110.5(9) ?
C9A C10A C7A . . 109.8(10) ?
C12A C10A C7A . . 104.9(9) ?
C9A C10A H10A . . 110.5 ?
C12A C10A H10A . . 110.5 ?
C7A C10A H10A . . 110.5 ?
C12A C11A C6A . . 108.6(10) ?
C12A C11A C14A . . 109.3(9) ?
C6A C11A C14A . . 106.5(9) ?
C12A C11A H11C . . 110.8 ?
C6A C11A H11C . . 110.8 ?
C14A C11A H11C . . 110.8 ?
C11A C12A C10A . . 112.1(9) ?
C11A C12A H12A . . 109.2 ?
C10A C12A H12A . . 109.2 ?
C11A C12A H12B . . 109.2 ?
C10A C12A H12B . . 109.2 ?
H12A C12A H12B . . 107.9 ?
C9A C13A C14A . . 111.0(10) ?
C9A C13A C8A . . 108.8(9) ?
C14A C13A C8A . . 106.0(9) ?
C9A C13A H13C . . 110.3 ?
C14A C13A H13C . . 110.3 ?
C8A C13A H13C . . 110.3 ?
C13A C14A C11A . . 112.5(10) ?
C13A C14A H14A . . 109.1 ?
C11A C14A H14A . . 109.1 ?
C13A C14A H14B . . 109.1 ?
C11A C14A H14B . . 109.1 ?
H14A C14A H14B . . 107.8 ?
N3 C15 N2 . . 112.8(2) ?
N3 C15 C16 . . 128.9(2) ?
N2 C15 C16 . . 118.0(2) ?
C19 C16 C15 . . 114.7(2) ?
C19 C16 C18 . . 106.6(2) ?
C15 C16 C18 . . 106.5(2) ?
C19 C16 C17 . . 107.1(2) ?
C15 C16 C17 . . 110.3(2) ?
C18 C16 C17 . . 111.5(2) ?
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 ?
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 ?
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 ?
C27 C20 C21 . . 121.5(2) ?
C27 C20 N3 . . 120.1(2) ?
C21 C20 N3 . . 118.3(2) ?
C23 C21 C20 . . 118.0(2) ?
C23 C21 C22 . . 120.8(2) ?
C20 C21 C22 . . 121.2(2) ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C21 C23 C24 . . 122.1(2) ?
C21 C23 H23 . . 119.0 ?
C24 C23 H23 . . 119.0 ?
C26 C24 C23 . . 118.3(2) ?
C26 C24 C25 . . 120.9(2) ?
C23 C24 C25 . . 120.9(2) ?
C24 C25 H25A . . 109.5 ?
C24 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C24 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C24 C26 C27 . . 121.8(2) ?
C24 C26 H26 . . 119.1 ?
C27 C26 H26 . . 119.1 ?
C26 C27 C20 . . 118.3(2) ?
C26 C27 C28 . . 120.0(2) ?
C20 C27 C28 . . 121.6(2) ?
C27 C28 H28A . . 109.5 ?
C27 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
C27 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
C30 C29 C34 . . 120.2(3) ?
C30 C29 H29 . . 119.9 ?
C34 C29 H29 . . 119.9 ?
C29 C30 C31 . . 119.6(3) ?
C29 C30 H30 . . 120.2 ?
C31 C30 H30 . . 120.2 ?
C32 C31 C30 . . 121.0(3) ?
C32 C31 H31 . . 119.5 ?
C30 C31 H31 . . 119.5 ?
C31 C32 C33 . . 119.4(3) ?
C31 C32 H32 . . 120.3 ?
C33 C32 H32 . . 120.3 ?
C32 C33 C34 . . 119.8(3) ?
C32 C33 H33 . . 120.1 ?
C34 C33 H33 . . 120.1 ?
C29 C34 C33 . . 120.0(3) ?
C29 C34 H34 . . 120.0 ?
C33 C34 H34 . . 120.0 ?
F2 C35 F3 . . 107.2(2) ?
F2 C35 F1 . . 107.4(3) ?
F3 C35 F1 . . 108.2(3) ?
F2 C35 S2 . . 111.5(2) ?
F3 C35 S2 . . 111.3(2) ?
F1 C35 S2 . . 111.0(2) ?
C1 Ge1 C2 . . 101.71(10) ?
C1 Ge1 N3 . . 98.28(9) ?
C2 Ge1 N3 . . 78.23(9) ?
C2 N1 C3 . . 112.4(2) ?
C2 N1 C5 . . 127.3(2) ?
C3 N1 C5 . . 120.09(19) ?
C2 N2 C15 . . 119.0(2) ?
C2 N2 C4 . . 110.84(19) ?
C15 N2 C4 . . 129.6(2) ?
C15 N3 C20 . . 127.0(2) ?
C15 N3 Ge1 . . 116.72(17) ?
C20 N3 Ge1 . . 115.96(15) ?
O2 S2 O3 . . 115.77(13) ?
O2 S2 O1 . . 115.48(13) ?
O3 S2 O1 . . 113.89(12) ?
O2 S2 C35 . . 103.25(14) ?
O3 S2 C35 . . 103.48(13) ?
O1 S2 C35 . . 102.45(13) ?

####################################################################### 
# 
# 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_rei157
_database_code_depnum_ccdc_archive 'CCDC 1429595'
_audit_update_record             
;
2015-10-06 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H47 Cr Ge N3 O6'
_chemical_formula_iupac          ?
_chemical_formula_weight         742.35

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.2157(3)
_cell_length_b                   22.5884(5)
_cell_length_c                   15.2996(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.6480(13)
_cell_angle_gamma                90
_cell_volume                     3499.07(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7769
_cell_measurement_theta_min      2.2485
_cell_measurement_theta_max      30.1253
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552

_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/3 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.81

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            46257
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_full        31.08
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
;

_reflns_number_total             11215
_reflns_number_gt                8124
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0997
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_number_reflns         11215
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+1.3667P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.138
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables 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'
Cr Cr 0.3209 0.6236 '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'

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge1 0.44965(2) 0.65953(2) 0.69765(2) 0.02195(6) Uani d . . . 1 . .
Cr Cr1 0.61198(3) 0.58818(2) 0.65030(2) 0.01377(7) Uani d . . . 1 . .
C C1 0.28962(17) 0.67498(7) 0.73842(11) 0.0109(3) Uani d . . . 1 . .
C C2 0.11418(17) 0.69294(7) 0.81636(12) 0.0128(3) Uani d . . . 1 . .
H H2A 0.1553 0.6993 0.878 0.015 Uiso calc U . R 1 . .
H H2B 0.02 0.6825 0.8159 0.015 Uiso calc U . R 1 . .
C C3 0.12980(17) 0.74651(8) 0.76021(12) 0.0143(3) Uani d . . . 1 . .
H H3A 0.0599 0.7483 0.7088 0.017 Uiso calc U . R 1 . .
H H3B 0.1289 0.7836 0.7947 0.017 Uiso calc U . R 1 . .
C C4 0.34317(17) 0.77295(7) 0.69681(11) 0.0113(3) Uani d . . . 1 . .
C C5 0.31799(18) 0.84015(7) 0.69657(12) 0.0143(3) Uani d . . . 1 . .
C C6 0.3322(2) 0.86230(8) 0.79264(13) 0.0209(4) Uani d . . . 1 . .
H H6A 0.2724 0.8399 0.8253 0.031 Uiso calc U . R 1 . .
H H6B 0.3099 0.9045 0.7933 0.031 Uiso calc U . R 1 . .
H H6C 0.4235 0.8566 0.8203 0.031 Uiso calc U . R 1 . .
C C7 0.17969(19) 0.85488(8) 0.64735(14) 0.0203(4) Uani d . . . 1 . .
H H7A 0.1674 0.8345 0.5903 0.03 Uiso calc U . R 1 . .
H H7B 0.1722 0.8977 0.6379 0.03 Uiso calc U . R 1 . .
H H7C 0.1119 0.8418 0.6827 0.03 Uiso calc U . R 1 . .
C C8 0.4162(2) 0.87669(8) 0.65087(14) 0.0197(4) Uani d . . . 1 . .
H H8A 0.5059 0.8705 0.6812 0.029 Uiso calc U . R 1 . .
H H8B 0.3935 0.9188 0.653 0.029 Uiso calc U . R 1 . .
H H8C 0.412 0.8641 0.5893 0.029 Uiso calc U . R 1 . .
C C9 0.54722(17) 0.76703(7) 0.62550(12) 0.0122(3) Uani d . . . 1 . .
C C10 0.66976(18) 0.78284(8) 0.67082(12) 0.0152(3) Uani d . . . 1 . .
C C11 0.6968(2) 0.78014(9) 0.76971(13) 0.0235(4) Uani d . . . 1 . .
H H11A 0.6582 0.8149 0.7949 0.035 Uiso calc U . R 1 . .
H H11B 0.7924 0.7797 0.7882 0.035 Uiso calc U . R 1 . .
H H11C 0.6574 0.7441 0.7906 0.035 Uiso calc U . R 1 . .
C C12 0.76692(18) 0.80254(8) 0.62171(13) 0.0171(4) Uani d . . . 1 . .
H H12 0.8512 0.813 0.6517 0.021 Uiso calc U . R 1 . .
C C13 0.74459(19) 0.80735(8) 0.53037(13) 0.0179(4) Uani d . . . 1 . .
C C14 0.8513(2) 0.82811(10) 0.47824(16) 0.0283(5) Uani d . . . 1 . .
H H14A 0.9153 0.8523 0.5161 0.042 Uiso calc U . R 1 . .
H H14B 0.8117 0.8518 0.4279 0.042 Uiso calc U . R 1 . .
H H14C 0.8962 0.7937 0.4569 0.042 Uiso calc U . R 1 . .
C C15 0.62051(19) 0.79133(8) 0.48777(13) 0.0178(4) Uani d . . . 1 . .
H H15 0.603 0.795 0.4255 0.021 Uiso calc U . R 1 . .
C C16 0.52195(18) 0.77027(8) 0.53352(12) 0.0147(3) Uani d . . . 1 . .
C C17 0.39068(19) 0.75226(9) 0.48480(13) 0.0204(4) Uani d . . . 1 . .
H H17A 0.3917 0.7574 0.4213 0.031 Uiso calc U . R 1 . .
H H17B 0.321 0.777 0.504 0.031 Uiso calc U . R 1 . .
H H17C 0.3736 0.7106 0.4973 0.031 Uiso calc U . R 1 . .
C C18 0.19759(17) 0.58824(7) 0.81448(11) 0.0117(3) Uani d . . . 1 . .
C C19 0.28462(19) 0.58857(8) 0.90431(12) 0.0161(3) Uani d . . . 1 . .
H H19A 0.2479 0.6166 0.9444 0.019 Uiso calc U . R 1 . .
H H19B 0.3748 0.6019 0.8969 0.019 Uiso calc U . R 1 . .
C C20 0.25614(19) 0.54456(8) 0.75347(12) 0.0168(4) Uani d . . . 1 . .
H H20A 0.3459 0.5577 0.7446 0.02 Uiso calc U . R 1 . .
H H20B 0.2007 0.5439 0.6953 0.02 Uiso calc U . R 1 . .
C C21 0.05842(18) 0.56666(8) 0.82653(13) 0.0164(4) Uani d . . . 1 . .
H H21A 0.0185 0.5943 0.8657 0.02 Uiso calc U . R 1 . .
H H21B 0.0019 0.5661 0.7687 0.02 Uiso calc U . R 1 . .
C C22 0.06491(19) 0.50433(8) 0.86664(13) 0.0193(4) Uani d . . . 1 . .
H H22 -0.0262 0.491 0.8745 0.023 Uiso calc U . R 1 . .
C C23 0.1509(2) 0.50581(8) 0.95629(13) 0.0222(4) Uani d . . . 1 . .
H H23A 0.1543 0.4659 0.9832 0.027 Uiso calc U . R 1 . .
H H23B 0.1122 0.5334 0.9961 0.027 Uiso calc U . R 1 . .
C C24 0.2907(2) 0.52601(8) 0.94477(13) 0.0199(4) Uani d . . . 1 . .
H H24 0.3471 0.5266 1.0034 0.024 Uiso calc U . R 1 . .
C C25 0.3490(2) 0.48294(8) 0.88323(14) 0.0225(4) Uani d . . . 1 . .
H H25A 0.3532 0.4427 0.9092 0.027 Uiso calc U . R 1 . .
H H25B 0.4399 0.4953 0.876 0.027 Uiso calc U . R 1 . .
C C26 0.2632(2) 0.48199(8) 0.79337(13) 0.0208(4) Uani d . . . 1 . .
H H26 0.3024 0.4542 0.7531 0.025 Uiso calc U . R 1 . .
C C27 0.1236(2) 0.46157(8) 0.80453(14) 0.0227(4) Uani d . . . 1 . .
H H27A 0.1266 0.421 0.8293 0.027 Uiso calc U . R 1 . .
H H27B 0.0677 0.4609 0.7465 0.027 Uiso calc U . R 1 . .
C C28 0.59304(19) 0.61976(9) 0.53418(14) 0.0208(4) Uani d . . . 1 . .
C C29 0.75397(19) 0.64109(8) 0.67858(13) 0.0187(4) Uani d . . . 1 . .
C C30 0.7319(2) 0.53284(9) 0.62103(16) 0.0261(5) Uani d . . . 1 . .
C C31 0.6411(2) 0.55986(9) 0.76756(15) 0.0255(4) Uani d . . . 1 . .
C C32 0.4744(2) 0.53311(10) 0.61311(15) 0.0283(5) Uani d . . . 1 . .
C C33 0.0530(3) 0.82227(14) 1.02241(17) 0.0476(7) Uani d . . . 1 . .
H H33A 0.1388 0.8058 1.0492 0.057 Uiso calc U . R 1 . .
H H33B -0.0188 0.8013 1.0472 0.057 Uiso calc U . R 1 . .
C C34 0.0468(3) 0.88777(13) 1.03962(17) 0.0459(7) Uani d . . . 1 . .
H H34A 0.0131 0.896 1.0961 0.055 Uiso calc U . R 1 . .
H H34B 0.1345 0.9065 1.0404 0.055 Uiso calc U . R 1 . .
C C35 -0.0481(2) 0.90855(10) 0.96253(18) 0.0361(6) Uani d . . . 1 . .
H H35A -0.1407 0.9012 0.9718 0.043 Uiso calc U . R 1 . .
H H35B -0.0364 0.9512 0.9509 0.043 Uiso calc U . R 1 . .
C C36 -0.0093(3) 0.87112(10) 0.88938(15) 0.0321(5) Uani d . . . 1 . .
H H36A -0.0863 0.8643 0.8439 0.039 Uiso calc U . R 1 . .
H H36B 0.061 0.8909 0.8613 0.039 Uiso calc U . R 1 . .
N N1 0.18457(14) 0.64714(6) 0.77253(10) 0.0116(3) Uani d . . . 1 . .
N N2 0.26107(14) 0.73559(6) 0.73265(10) 0.0116(3) Uani d . . . 1 . .
N N3 0.44617(14) 0.74332(6) 0.67268(10) 0.0127(3) Uani d . . . 1 . .
O O1 0.58877(17) 0.63784(8) 0.46407(10) 0.0335(4) Uani d . . . 1 . .
O O2 0.84575(14) 0.67012(7) 0.69327(11) 0.0298(4) Uani d . . . 1 . .
O O3 0.80737(18) 0.49795(7) 0.60465(14) 0.0458(5) Uani d . . . 1 . .
O O4 0.66623(18) 0.54270(9) 0.83809(12) 0.0468(5) Uani d . . . 1 . .
O O5 0.39683(19) 0.49899(9) 0.58733(13) 0.0522(6) Uani d . . . 1 . .
O O6 0.0376(2) 0.81630(7) 0.92839(11) 0.0454(5) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ge1 C1 . 1.8587(17) ?
Ge1 N3 . 1.9303(14) ?
Ge1 Cr1 . 2.4883(3) ?
Cr1 C30 . 1.847(2) ?
Cr1 C29 . 1.885(2) ?
Cr1 C31 . 1.891(2) ?
Cr1 C28 . 1.900(2) ?
Cr1 C32 . 1.906(2) ?
C1 N2 . 1.400(2) ?
C1 N1 . 1.403(2) ?
C2 N1 . 1.471(2) ?
C2 C3 . 1.505(2) ?
C3 N2 . 1.479(2) ?
C4 N3 . 1.340(2) ?
C4 N2 . 1.356(2) ?
C4 C5 . 1.539(2) ?
C5 C8 . 1.538(3) ?
C5 C6 . 1.541(3) ?
C5 C7 . 1.546(3) ?
C9 C10 . 1.394(2) ?
C9 C16 . 1.398(2) ?
C9 N3 . 1.439(2) ?
C10 C12 . 1.395(3) ?
C10 C11 . 1.503(3) ?
C12 C13 . 1.390(3) ?
C13 C15 . 1.394(3) ?
C13 C14 . 1.509(3) ?
C15 C16 . 1.385(3) ?
C16 C17 . 1.501(3) ?
C18 N1 . 1.475(2) ?
C18 C20 . 1.533(2) ?
C18 C19 . 1.534(2) ?
C18 C21 . 1.537(2) ?
C19 C24 . 1.541(2) ?
C20 C26 . 1.537(2) ?
C21 C22 . 1.534(2) ?
C22 C23 . 1.527(3) ?
C22 C27 . 1.532(3) ?
C23 C24 . 1.531(3) ?
C24 C25 . 1.529(3) ?
C25 C26 . 1.529(3) ?
C26 C27 . 1.530(3) ?
C28 O1 . 1.143(2) ?
C29 O2 . 1.142(2) ?
C30 O3 . 1.153(2) ?
C31 O4 . 1.143(3) ?
C32 O5 . 1.138(3) ?
C33 O6 . 1.432(3) ?
C33 C34 . 1.506(4) ?
C34 C35 . 1.499(4) ?
C35 C36 . 1.497(3) ?
C36 O6 . 1.429(3) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Ge1 N3 . . 83.60(7) ?
C1 Ge1 Cr1 . . 150.38(5) ?
N3 Ge1 Cr1 . . 124.95(4) ?
C30 Cr1 C29 . . 88.25(9) ?
C30 Cr1 C31 . . 88.58(10) ?
C29 Cr1 C31 . . 88.71(9) ?
C30 Cr1 C28 . . 90.89(9) ?
C29 Cr1 C28 . . 87.48(9) ?
C31 Cr1 C28 . . 176.17(9) ?
C30 Cr1 C32 . . 88.43(10) ?
C29 Cr1 C32 . . 175.29(9) ?
C31 Cr1 C32 . . 94.54(10) ?
C28 Cr1 C32 . . 89.23(10) ?
C30 Cr1 Ge1 . . 176.73(7) ?
C29 Cr1 Ge1 . . 92.58(6) ?
C31 Cr1 Ge1 . . 88.27(7) ?
C28 Cr1 Ge1 . . 92.31(6) ?
C32 Cr1 Ge1 . . 90.93(6) ?
N2 C1 N1 . . 107.37(14) ?
N2 C1 Ge1 . . 110.34(12) ?
N1 C1 Ge1 . . 142.29(12) ?
N1 C2 C3 . . 102.11(13) ?
N2 C3 C2 . . 101.41(13) ?
N3 C4 N2 . . 110.56(14) ?
N3 C4 C5 . . 128.98(15) ?
N2 C4 C5 . . 120.17(15) ?
C8 C5 C4 . . 114.29(15) ?
C8 C5 C6 . . 105.95(15) ?
C4 C5 C6 . . 108.86(15) ?
C8 C5 C7 . . 105.81(15) ?
C4 C5 C7 . . 110.80(15) ?
C6 C5 C7 . . 111.02(16) ?
C10 C9 C16 . . 121.35(16) ?
C10 C9 N3 . . 120.15(16) ?
C16 C9 N3 . . 118.39(16) ?
C9 C10 C12 . . 118.02(17) ?
C9 C10 C11 . . 121.52(16) ?
C12 C10 C11 . . 120.45(17) ?
C13 C12 C10 . . 122.22(18) ?
C12 C13 C15 . . 117.85(17) ?
C12 C13 C14 . . 121.49(19) ?
C15 C13 C14 . . 120.65(18) ?
C16 C15 C13 . . 122.01(18) ?
C15 C16 C9 . . 118.51(17) ?
C15 C16 C17 . . 120.24(17) ?
C9 C16 C17 . . 121.24(16) ?
N1 C18 C20 . . 109.59(14) ?
N1 C18 C19 . . 113.15(14) ?
C20 C18 C19 . . 108.78(15) ?
N1 C18 C21 . . 107.87(14) ?
C20 C18 C21 . . 108.11(14) ?
C19 C18 C21 . . 109.21(15) ?
C18 C19 C24 . . 110.05(15) ?
C18 C20 C26 . . 110.57(15) ?
C22 C21 C18 . . 110.35(15) ?
C23 C22 C27 . . 110.18(17) ?
C23 C22 C21 . . 109.16(16) ?
C27 C22 C21 . . 109.27(15) ?
C22 C23 C24 . . 109.68(16) ?
C25 C24 C23 . . 109.08(16) ?
C25 C24 C19 . . 109.53(16) ?
C23 C24 C19 . . 109.35(16) ?
C24 C25 C26 . . 109.84(16) ?
C25 C26 C27 . . 109.56(16) ?
C25 C26 C20 . . 109.59(16) ?
C27 C26 C20 . . 109.02(16) ?
C26 C27 C22 . . 109.08(16) ?
O1 C28 Cr1 . . 176.18(18) ?
O2 C29 Cr1 . . 174.96(18) ?
O3 C30 Cr1 . . 178.5(2) ?
O4 C31 Cr1 . . 176.13(19) ?
O5 C32 Cr1 . . 175.90(19) ?
O6 C33 C34 . . 105.5(2) ?
C35 C34 C33 . . 102.0(2) ?
C36 C35 C34 . . 101.8(2) ?
O6 C36 C35 . . 106.53(19) ?
C1 N1 C2 . . 107.38(13) ?
C1 N1 C18 . . 122.47(14) ?
C2 N1 C18 . . 117.20(13) ?
C4 N2 C1 . . 119.95(14) ?
C4 N2 C3 . . 130.13(14) ?
C1 N2 C3 . . 109.52(14) ?
C4 N3 C9 . . 126.47(14) ?
C4 N3 Ge1 . . 115.45(11) ?
C9 N3 Ge1 . . 117.94(11) ?
C36 O6 C33 . . 108.88(18) ?

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1429596'
_audit_update_record             
;
2015-10-06 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H47 Ge Mo N3 O6'
_chemical_formula_iupac          ?
_chemical_formula_weight         786.29

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3172(9)
_cell_length_b                   22.6231(18)
_cell_length_c                   15.3939(12)
_cell_angle_alpha                90
_cell_angle_beta                 97.423(3)
_cell_angle_gamma                90
_cell_volume                     3562.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    601
_cell_measurement_theta_min      2.6722
_cell_measurement_theta_max      21.2530
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624

_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            32532
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19

_refine_special_details          
;
;

_reflns_number_total             7754
_reflns_number_gt                5077
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1846
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_number_reflns         7754
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0946P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.298
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2014)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge1 0.55710(6) 0.66243(2) 0.80065(4) 0.02219(18) Uani d . . . 1 . .
Mo Mo1 0.38580(5) 0.58787(2) 0.84863(3) 0.01664(15) Uani d . . . 1 . .
C C1 0.7158(5) 0.6778(2) 0.7601(3) 0.0130(11) Uani d . . . 1 . .
C C2 0.8888(6) 0.6955(2) 0.6811(3) 0.0170(12) Uani d . . . 1 . .
H H2A 0.847 0.7016 0.6202 0.02 Uiso calc U . R 1 . .
H H2B 0.9819 0.6851 0.6807 0.02 Uiso calc U . R 1 . .
C C3 0.8738(5) 0.7493(2) 0.7375(4) 0.0187(12) Uani d . . . 1 . .
H H3A 0.9432 0.7511 0.7882 0.022 Uiso calc U . R 1 . .
H H3B 0.8748 0.7863 0.7032 0.022 Uiso calc U . R 1 . .
C C4 0.6625(5) 0.7758(2) 0.8020(3) 0.0157(11) Uani d . . . 1 . .
C C5 0.6869(6) 0.8431(2) 0.8037(3) 0.0175(12) Uani d . . . 1 . .
C C6 0.6742(6) 0.8662(2) 0.7088(4) 0.0247(14) Uani d . . . 1 . .
H H6A 0.7352 0.8448 0.6764 0.037 Uiso calc U . R 1 . .
H H6B 0.6947 0.9085 0.7091 0.037 Uiso calc U . R 1 . .
H H6C 0.5846 0.86 0.6804 0.037 Uiso calc U . R 1 . .
C C7 0.8249(6) 0.8573(2) 0.8524(4) 0.0257(14) Uani d . . . 1 . .
H H7A 0.8359 0.8376 0.9096 0.039 Uiso calc U . R 1 . .
H H7B 0.834 0.9001 0.8606 0.039 Uiso calc U . R 1 . .
H H7C 0.8916 0.843 0.8176 0.039 Uiso calc U . R 1 . .
C C8 0.5889(6) 0.8794(2) 0.8499(4) 0.0237(13) Uani d . . . 1 . .
H H8A 0.5006 0.8741 0.8189 0.036 Uiso calc U . R 1 . .
H H8B 0.6126 0.9214 0.8494 0.036 Uiso calc U . R 1 . .
H H8C 0.5915 0.8659 0.9105 0.036 Uiso calc U . R 1 . .
C C9 0.4594(6) 0.7695(2) 0.8737(4) 0.0169(12) Uani d . . . 1 . .
C C10 0.4828(6) 0.7712(2) 0.9648(3) 0.0174(12) Uani d . . . 1 . .
C C11 0.6120(6) 0.7527(3) 1.0134(4) 0.0243(13) Uani d . . . 1 . .
H H11A 0.6086 0.7555 1.0765 0.036 Uiso calc U . R 1 . .
H H11B 0.681 0.7787 0.9972 0.036 Uiso calc U . R 1 . .
H H11C 0.6307 0.7118 0.998 0.036 Uiso calc U . R 1 . .
C C12 0.3848(6) 0.7912(2) 1.0101(4) 0.0201(12) Uani d . . . 1 . .
H H12 0.4008 0.7935 1.0722 0.024 Uiso calc U . R 1 . .
C C13 0.2632(6) 0.8083(2) 0.9680(4) 0.0210(13) Uani d . . . 1 . .
C C14 0.1571(6) 0.8288(3) 1.0197(4) 0.0311(15) Uani d . . . 1 . .
H H14A 0.1177 0.7945 1.0451 0.047 Uiso calc U . R 1 . .
H H14B 0.09 0.85 0.9809 0.047 Uiso calc U . R 1 . .
H H14C 0.1947 0.8552 1.0668 0.047 Uiso calc U . R 1 . .
C C15 0.2435(6) 0.8048(2) 0.8772(4) 0.0223(13) Uani d . . . 1 . .
H H15 0.1611 0.8163 0.8472 0.027 Uiso calc U . R 1 . .
C C16 0.3391(6) 0.7853(2) 0.8289(4) 0.0187(12) Uani d . . . 1 . .
C C17 0.3123(6) 0.7839(3) 0.7295(4) 0.0292(15) Uani d . . . 1 . .
H H17A 0.3526 0.8184 0.7054 0.044 Uiso calc U . R 1 . .
H H17B 0.2177 0.7846 0.7113 0.044 Uiso calc U . R 1 . .
H H17C 0.3492 0.7477 0.7077 0.044 Uiso calc U . R 1 . .
C C18 0.8065(5) 0.5907(2) 0.6855(3) 0.0160(11) Uani d . . . 1 . .
C C19 0.9435(6) 0.5697(2) 0.6712(4) 0.0216(13) Uani d . . . 1 . .
H H19A 1.0018 0.5702 0.7276 0.026 Uiso calc U . R 1 . .
H H19B 0.9804 0.5969 0.6302 0.026 Uiso calc U . R 1 . .
C C20 0.9358(6) 0.5065(2) 0.6331(4) 0.0245(13) Uani d . . . 1 . .
H H20 1.0253 0.4931 0.6235 0.029 Uiso calc U . R 1 . .
C C21 0.8466(7) 0.5074(3) 0.5450(4) 0.0291(15) Uani d . . . 1 . .
H H21A 0.8824 0.535 0.5042 0.035 Uiso calc U . R 1 . .
H H21B 0.8428 0.4675 0.5185 0.035 Uiso calc U . R 1 . .
C C22 0.7100(6) 0.5270(2) 0.5593(4) 0.0248(14) Uani d . . . 1 . .
H H22 0.6519 0.5269 0.5021 0.03 Uiso calc U . R 1 . .
C C23 0.7174(6) 0.5897(2) 0.5971(4) 0.0217(12) Uani d . . . 1 . .
H H23A 0.6287 0.6032 0.6056 0.026 Uiso calc U . R 1 . .
H H23B 0.7523 0.6169 0.5556 0.026 Uiso calc U . R 1 . .
C C24 0.7519(6) 0.5472(2) 0.7479(4) 0.0221(13) Uani d . . . 1 . .
H H24A 0.6633 0.56 0.758 0.027 Uiso calc U . R 1 . .
H H24B 0.8084 0.5474 0.805 0.027 Uiso calc U . R 1 . .
C C25 0.7451(6) 0.4843(2) 0.7101(4) 0.0261(14) Uani d . . . 1 . .
H H25 0.7086 0.4568 0.7516 0.031 Uiso calc U . R 1 . .
C C26 0.8816(7) 0.4649(2) 0.6967(4) 0.0277(14) Uani d . . . 1 . .
H H26A 0.8789 0.4241 0.6733 0.033 Uiso calc U . R 1 . .
H H26B 0.9389 0.4652 0.7535 0.033 Uiso calc U . R 1 . .
C C27 0.6563(6) 0.4849(2) 0.6218(4) 0.0270(14) Uani d . . . 1 . .
H H27A 0.6511 0.4446 0.5965 0.032 Uiso calc U . R 1 . .
H H27B 0.567 0.4972 0.6309 0.032 Uiso calc U . R 1 . .
C C28 0.4053(6) 0.6212(3) 0.9732(4) 0.0242(13) Uani d . . . 1 . .
C C29 0.2373(6) 0.6455(2) 0.8211(4) 0.0221(13) Uani d . . . 1 . .
C C30 0.3525(6) 0.5576(3) 0.7221(4) 0.0290(14) Uani d . . . 1 . .
C C31 0.5313(7) 0.5274(3) 0.8858(4) 0.0327(16) Uani d . . . 1 . .
C C32 0.2579(7) 0.5290(3) 0.8806(4) 0.0334(16) Uani d . . . 1 . .
C C33 1.0196(8) 0.6292(3) 0.1084(5) 0.0433(19) Uani d . . . 1 . .
H H33A 0.9513 0.6097 0.1379 0.052 Uiso calc U . R 1 . .
H H33B 1.0982 0.6349 0.1517 0.052 Uiso calc U . R 1 . .
C C34 1.0512(8) 0.5929(3) 0.0344(6) 0.048(2) Uani d . . . 1 . .
H H34A 1.1423 0.5997 0.0231 0.058 Uiso calc U . R 1 . .
H H34B 1.0393 0.5503 0.0459 0.058 Uiso calc U . R 1 . .
C C35 0.9587(9) 0.6129(4) -0.0390(5) 0.067(3) Uani d . . . 1 . .
H H35A 0.8718 0.5944 -0.0387 0.081 Uiso calc U . R 1 . .
H H35B 0.9906 0.6049 -0.0958 0.081 Uiso calc U . R 1 . .
C C36 0.9551(9) 0.6794(4) -0.0198(5) 0.067(3) Uani d . . . 1 . .
H H36A 1.0255 0.7001 -0.0456 0.081 Uiso calc U . R 1 . .
H H36B 0.8699 0.6964 -0.0447 0.081 Uiso calc U . R 1 . .
N N1 0.5605(5) 0.74619(18) 0.8259(3) 0.0169(10) Uani d . . . 1 . .
N N2 0.7439(4) 0.73870(18) 0.7656(3) 0.0141(9) Uani d . . . 1 . .
N N3 0.8200(4) 0.65016(18) 0.7260(3) 0.0152(10) Uani d . . . 1 . .
O O1 0.4097(5) 0.6399(2) 1.0422(3) 0.0364(11) Uani d . . . 1 . .
O O2 0.1475(4) 0.67586(19) 0.8071(3) 0.0346(11) Uani d . . . 1 . .
O O3 0.3254(5) 0.5421(2) 0.6519(3) 0.0471(14) Uani d . . . 1 . .
O O4 0.6094(5) 0.4935(2) 0.9105(3) 0.0555(16) Uani d . . . 1 . .
O O5 0.1828(5) 0.4946(2) 0.8978(4) 0.0519(15) Uani d . . . 1 . .
O O6 0.9734(7) 0.6850(2) 0.0725(3) 0.0659(19) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ge1 C1 . 1.858(6) ?
Ge1 N1 . 1.934(4) ?
Ge1 Mo1 . 2.6176(8) ?
Mo1 C32 . 1.981(7) ?
Mo1 C29 . 2.014(6) ?
Mo1 C28 . 2.046(6) ?
Mo1 C30 . 2.051(6) ?
Mo1 C31 . 2.057(7) ?
C1 N3 . 1.403(7) ?
C1 N2 . 1.409(6) ?
C2 N3 . 1.469(7) ?
C2 C3 . 1.515(7) ?
C3 N2 . 1.480(7) ?
C4 N1 . 1.338(7) ?
C4 N2 . 1.358(7) ?
C4 C5 . 1.543(7) ?
C5 C6 . 1.542(7) ?
C5 C8 . 1.545(8) ?
C5 C7 . 1.554(8) ?
C9 C16 . 1.386(8) ?
C9 C10 . 1.392(7) ?
C9 N1 . 1.452(7) ?
C10 C12 . 1.378(8) ?
C10 C11 . 1.501(8) ?
C12 C13 . 1.390(8) ?
C13 C15 . 1.389(8) ?
C13 C14 . 1.507(8) ?
C15 C16 . 1.383(8) ?
C16 C17 . 1.519(8) ?
C18 N3 . 1.481(6) ?
C18 C24 . 1.532(7) ?
C18 C19 . 1.534(8) ?
C18 C23 . 1.541(7) ?
C19 C20 . 1.545(7) ?
C20 C26 . 1.516(8) ?
C20 C21 . 1.538(8) ?
C21 C22 . 1.520(8) ?
C22 C27 . 1.509(8) ?
C22 C23 . 1.531(7) ?
C24 C25 . 1.535(7) ?
C25 C26 . 1.514(8) ?
C25 C27 . 1.538(8) ?
C28 O1 . 1.139(7) ?
C29 O2 . 1.152(7) ?
C30 O3 . 1.135(7) ?
C31 O4 . 1.140(7) ?
C32 O5 . 1.152(7) ?
C33 O6 . 1.433(8) ?
C33 C34 . 1.475(9) ?
C34 C35 . 1.454(11) ?
C35 C36 . 1.534(12) ?
C36 O6 . 1.415(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Ge1 N1 . . 83.7(2) ?
C1 Ge1 Mo1 . . 150.61(15) ?
N1 Ge1 Mo1 . . 124.76(14) ?
C32 Mo1 C29 . . 88.5(2) ?
C32 Mo1 C28 . . 90.2(2) ?
C29 Mo1 C28 . . 86.5(2) ?
C32 Mo1 C30 . . 88.6(3) ?
C29 Mo1 C30 . . 89.2(2) ?
C28 Mo1 C30 . . 175.6(2) ?
C32 Mo1 C31 . . 88.2(3) ?
C29 Mo1 C31 . . 175.4(2) ?
C28 Mo1 C31 . . 90.3(3) ?
C30 Mo1 C31 . . 94.0(3) ?
C32 Mo1 Ge1 . . 177.36(17) ?
C29 Mo1 Ge1 . . 92.66(16) ?
C28 Mo1 Ge1 . . 92.21(17) ?
C30 Mo1 Ge1 . . 89.06(19) ?
C31 Mo1 Ge1 . . 90.72(18) ?
N3 C1 N2 . . 107.2(4) ?
N3 C1 Ge1 . . 142.5(4) ?
N2 C1 Ge1 . . 110.3(4) ?
N3 C2 C3 . . 101.6(4) ?
N2 C3 C2 . . 101.5(4) ?
N1 C4 N2 . . 110.8(4) ?
N1 C4 C5 . . 128.4(5) ?
N2 C4 C5 . . 120.5(5) ?
C6 C5 C4 . . 108.9(4) ?
C6 C5 C8 . . 106.0(5) ?
C4 C5 C8 . . 114.7(4) ?
C6 C5 C7 . . 110.4(5) ?
C4 C5 C7 . . 110.4(4) ?
C8 C5 C7 . . 106.3(4) ?
C16 C9 C10 . . 121.5(5) ?
C16 C9 N1 . . 119.8(5) ?
C10 C9 N1 . . 118.5(5) ?
C12 C10 C9 . . 118.4(5) ?
C12 C10 C11 . . 120.1(5) ?
C9 C10 C11 . . 121.5(5) ?
C10 C12 C13 . . 122.2(5) ?
C15 C13 C12 . . 117.4(5) ?
C15 C13 C14 . . 121.8(6) ?
C12 C13 C14 . . 120.8(5) ?
C16 C15 C13 . . 122.5(6) ?
C15 C16 C9 . . 118.0(5) ?
C15 C16 C17 . . 119.9(5) ?
C9 C16 C17 . . 122.1(5) ?
N3 C18 C24 . . 110.0(4) ?
N3 C18 C19 . . 107.6(4) ?
C24 C18 C19 . . 108.2(4) ?
N3 C18 C23 . . 113.5(4) ?
C24 C18 C23 . . 108.5(5) ?
C19 C18 C23 . . 108.9(5) ?
C18 C19 C20 . . 109.8(5) ?
C26 C20 C21 . . 110.5(5) ?
C26 C20 C19 . . 109.5(5) ?
C21 C20 C19 . . 108.5(5) ?
C22 C21 C20 . . 109.7(5) ?
C27 C22 C21 . . 109.4(5) ?
C27 C22 C23 . . 110.3(5) ?
C21 C22 C23 . . 108.9(5) ?
C22 C23 C18 . . 110.2(4) ?
C18 C24 C25 . . 111.1(4) ?
C26 C25 C24 . . 108.8(5) ?
C26 C25 C27 . . 109.9(5) ?
C24 C25 C27 . . 108.7(5) ?
C25 C26 C20 . . 109.6(5) ?
C22 C27 C25 . . 110.0(5) ?
O1 C28 Mo1 . . 176.7(6) ?
O2 C29 Mo1 . . 175.8(5) ?
O3 C30 Mo1 . . 175.3(6) ?
O4 C31 Mo1 . . 176.5(5) ?
O5 C32 Mo1 . . 178.9(6) ?
O6 C33 C34 . . 106.8(6) ?
C35 C34 C33 . . 103.7(6) ?
C34 C35 C36 . . 100.7(6) ?
O6 C36 C35 . . 106.1(6) ?
C4 N1 C9 . . 126.8(4) ?
C4 N1 Ge1 . . 115.4(4) ?
C9 N1 Ge1 . . 117.6(3) ?
C4 N2 C1 . . 119.7(5) ?
C4 N2 C3 . . 130.7(4) ?
C1 N2 C3 . . 109.2(4) ?
C1 N3 C2 . . 107.8(4) ?
C1 N3 C18 . . 121.8(4) ?
C2 N3 C18 . . 117.4(4) ?
C36 O6 C33 . . 107.6(6) ?


####################################################################### 
# 
# 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_rei145
_database_code_depnum_ccdc_archive 'CCDC 1429597'
_audit_update_record             
;
2015-10-06 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H47 Ge N3 O6 W'
_chemical_formula_iupac          ?
_chemical_formula_weight         874.20

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3691(5)
_cell_length_b                   22.6170(7)
_cell_length_c                   15.3476(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.055(3)
_cell_angle_gamma                90
_cell_volume                     3572.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6375
_cell_measurement_theta_min      2.2431
_cell_measurement_theta_max      24.6478
_cell_measurement_temperature    133.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752

_exptl_absorpt_coefficient_mu    4.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/3'
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.79

_exptl_special_details           
;
;

_diffrn_ambient_temperature      133.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            50991
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_full        29.22
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21

_refine_special_details          
;
;

_reflns_number_total             9666
_reflns_number_gt                7112
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0998
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.996
_refine_ls_number_reflns         9666
_refine_ls_number_parameters     476
_refine_ls_number_restraints     244
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.289
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables 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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W1 0.38714(2) 0.58939(2) 0.34761(2) 0.02073(6) Uani d . . . 1.0 . .
Ge Ge1 0.55823(5) 0.66366(2) 0.30060(4) 0.02752(12) Uani d . . . 1.0 . .
C C1 0.2402(5) 0.6470(2) 0.3189(3) 0.0292(11) Uani d . . . 1.0 . .
C C2 0.4067(5) 0.6217(2) 0.4732(3) 0.0305(11) Uani d . . . 1.0 . .
C C3 0.2585(5) 0.5307(2) 0.3786(4) 0.0401(14) Uani d . . . 1.0 . .
C C4 0.5283(5) 0.5287(2) 0.3854(4) 0.0380(13) Uani d . . . 1.0 . .
C C5 0.3577(5) 0.5602(2) 0.2217(4) 0.0363(12) Uani d . . . 1.0 . .
C C6 0.7164(4) 0.67854(16) 0.2612(3) 0.0173(8) Uani d . . . 1.0 . .
C C7 0.8882(4) 0.69613(17) 0.1813(3) 0.0204(9) Uani d . . . 1.0 . .
H H7A 0.8462 0.7024 0.1205 0.024 Uiso calc U . R 1.0 . .
H H7B 0.9806 0.6857 0.18 0.024 Uiso calc U . R 1.0 . .
C C8 0.8742(4) 0.74968(17) 0.2377(3) 0.0215(9) Uani d . . . 1.0 . .
H H8A 0.9438 0.7513 0.288 0.026 Uiso calc U . R 1.0 . .
H H8B 0.875 0.7867 0.2033 0.026 Uiso calc U . R 1.0 . .
C C9 0.6653(4) 0.77646(17) 0.3038(3) 0.0172(8) Uani d . . . 1.0 . .
C C10 0.6912(5) 0.84355(17) 0.3052(3) 0.0241(10) Uani d . . . 1.0 . .
C C11 0.6787(5) 0.86653(19) 0.2107(3) 0.0336(12) Uani d . . . 1.0 . .
H H11A 0.5892 0.8612 0.1831 0.05 Uiso calc U . R 1.0 . .
H H11B 0.7379 0.8445 0.1776 0.05 Uiso calc U . R 1.0 . .
H H11C 0.7012 0.9086 0.211 0.05 Uiso calc U . R 1.0 . .
C C12 0.8273(5) 0.8568(2) 0.3540(4) 0.0336(12) Uani d . . . 1.0 . .
H H12A 0.8938 0.8431 0.3186 0.05 Uiso calc U . R 1.0 . .
H H12B 0.8378 0.8363 0.4107 0.05 Uiso calc U . R 1.0 . .
H H12C 0.8367 0.8995 0.3637 0.05 Uiso calc U . R 1.0 . .
C C13 0.5955(5) 0.87930(18) 0.3531(3) 0.0309(11) Uani d . . . 1.0 . .
H H13A 0.62 0.9212 0.3541 0.046 Uiso calc U . R 1.0 . .
H H13B 0.5979 0.8648 0.4135 0.046 Uiso calc U . R 1.0 . .
H H13C 0.5074 0.8748 0.3224 0.046 Uiso calc U . R 1.0 . .
C C14 0.8068(4) 0.59099(17) 0.1874(3) 0.0201(9) Uani d . . . 1.0 . .
C C15 0.7163(5) 0.58943(18) 0.1007(3) 0.0311(11) Uani d . . . 1.0 . .
H H15A 0.749 0.6169 0.0582 0.037 Uiso calc U . R 1.0 . .
H H15B 0.6283 0.6026 0.1108 0.037 Uiso calc U . R 1.0 . .
C C16 0.7580(5) 0.54785(18) 0.2512(3) 0.0303(11) Uani d . . . 1.0 . .
H H16A 0.6709 0.5604 0.2643 0.036 Uiso calc U . R 1.0 . .
H H16B 0.8174 0.5482 0.3069 0.036 Uiso calc U . R 1.0 . .
C C17 0.9421(5) 0.57028(19) 0.1697(4) 0.0309(11) Uani d . . . 1.0 . .
H H17A 0.9765 0.5977 0.1278 0.037 Uiso calc U . R 1.0 . .
H H17B 1.0021 0.5709 0.2251 0.037 Uiso calc U . R 1.0 . .
C C18 0.9356(5) 0.50752(19) 0.1317(4) 0.0328(12) Uani d . . . 1.0 . .
H H18 1.0244 0.4949 0.1201 0.039 Uiso calc U . R 1.0 . .
C C19 0.8449(6) 0.5072(2) 0.0462(4) 0.0400(13) Uani d . . . 1.0 . .
H H19A 0.8411 0.4669 0.0207 0.048 Uiso calc U . R 1.0 . .
H H19B 0.8782 0.5344 0.0037 0.048 Uiso calc U . R 1.0 . .
C C20 0.7093(6) 0.5264(2) 0.0629(3) 0.0376(13) Uani d . . . 1.0 . .
H H20 0.6496 0.5258 0.0065 0.045 Uiso calc U . R 1.0 . .
C C21 0.6590(5) 0.4845(2) 0.1282(4) 0.0434(15) Uani d . . . 1.0 . .
H H21A 0.5709 0.4968 0.1393 0.052 Uiso calc U . R 1.0 . .
H H21B 0.6532 0.444 0.1036 0.052 Uiso calc U . R 1.0 . .
C C22 0.7497(6) 0.48486(19) 0.2136(4) 0.0390(14) Uani d . . . 1.0 . .
H H22 0.7157 0.4574 0.2566 0.047 Uiso calc U . R 1.0 . .
C C23 0.8862(5) 0.4655(2) 0.1977(4) 0.0364(13) Uani d . . . 1.0 . .
H H23A 0.9452 0.4664 0.2535 0.044 Uiso calc U . R 1.0 . .
H H23B 0.8838 0.4246 0.1746 0.044 Uiso calc U . R 1.0 . .
C C24 0.4625(4) 0.77040(17) 0.3751(3) 0.0188(9) Uani d . . . 1.0 . .
C C25 0.4850(4) 0.77124(17) 0.4662(3) 0.0215(9) Uani d . . . 1.0 . .
C C26 0.6127(5) 0.7517(2) 0.5144(3) 0.0301(11) Uani d . . . 1.0 . .
H H26A 0.6817 0.7783 0.5001 0.045 Uiso calc U . R 1.0 . .
H H26B 0.6318 0.7113 0.4966 0.045 Uiso calc U . R 1.0 . .
H H26C 0.6081 0.7527 0.5777 0.045 Uiso calc U . R 1.0 . .
C C27 0.3866(5) 0.79146(18) 0.5122(3) 0.0272(10) Uani d . . . 1.0 . .
H H27 0.4018 0.7935 0.5744 0.033 Uiso calc U . R 1.0 . .
C C28 0.2664(5) 0.80872(18) 0.4699(3) 0.0281(11) Uani d . . . 1.0 . .
C C29 0.1590(5) 0.8283(2) 0.5223(4) 0.0415(14) Uani d . . . 1.0 . .
H H29A 0.0874 0.8452 0.4825 0.062 Uiso calc U . R 1.0 . .
H H29B 0.1929 0.8581 0.5654 0.062 Uiso calc U . R 1.0 . .
H H29C 0.1275 0.7941 0.5528 0.062 Uiso calc U . R 1.0 . .
C C30 0.2471(5) 0.80617(18) 0.3791(3) 0.0269(10) Uani d . . . 1.0 . .
H H30 0.1652 0.8176 0.3493 0.032 Uiso calc U . R 1.0 . .
C C31 0.3436(5) 0.78747(18) 0.3300(3) 0.0231(9) Uani d . . . 1.0 . .
C C32 0.3199(5) 0.7872(2) 0.2315(3) 0.0399(13) Uani d . . . 1.0 . .
H H32A 0.2265 0.7909 0.2125 0.06 Uiso calc U . R 1.0 . .
H H32B 0.3519 0.75 0.2093 0.06 Uiso calc U . R 1.0 . .
H H32C 0.3659 0.8204 0.2085 0.06 Uiso calc U . R 1.0 . .
O O6 1.021(2) 0.8154(8) 0.0833(11) 0.061(4) Uani d U P D 0.305(11) A 1
C C33 0.959(3) 0.8047(8) -0.0012(16) 0.071(4) Uani d U P D 0.305(11) A 1
H H33A 0.8954 0.772 -0.0009 0.085 Uiso calc U P R 0.305(11) A 1
H H33B 1.0224 0.7946 -0.0419 0.085 Uiso calc U P R 0.305(11) A 1
C C34 0.890(2) 0.8630(9) -0.0273(16) 0.072(4) Uani d U P D 0.305(11) A 1
H H34A 0.817 0.871 0.0067 0.087 Uiso calc U P R 0.305(11) A 1
H H34B 0.8599 0.865 -0.091 0.087 Uiso calc U P R 0.305(11) A 1
C C35 1.007(3) 0.9033(9) -0.0005(17) 0.066(4) Uani d U P D 0.305(11) A 1
H H35A 1.074 0.8999 -0.0411 0.079 Uiso calc U P R 0.305(11) A 1
H H35B 0.9813 0.9452 0.0044 0.079 Uiso calc U P R 0.305(11) A 1
C C36 1.052(3) 0.8758(10) 0.0886(15) 0.066(4) Uani d U P D 0.305(11) A 1
H H36A 1.1464 0.8813 0.1039 0.08 Uiso calc U P R 0.305(11) A 1
H H36B 1.0067 0.8949 0.1345 0.08 Uiso calc U P R 0.305(11) A 1
O O6A 0.9512(10) 0.8173(3) 0.0671(5) 0.063(2) Uani d U P D 0.695(11) A 2
C C33A 0.9479(15) 0.8240(5) -0.0239(7) 0.077(3) Uani d U P D 0.695(11) A 2
H H33C 0.8643 0.8094 -0.0545 0.093 Uiso calc U P R 0.695(11) A 2
H H33D 1.0196 0.8016 -0.0454 0.093 Uiso calc U P R 0.695(11) A 2
C C34A 0.9628(11) 0.8895(5) -0.0401(6) 0.061(3) Uani d U P D 0.695(11) A 2
H H34C 0.8792 0.9107 -0.041 0.073 Uiso calc U P R 0.695(11) A 2
H H34D 0.9995 0.897 -0.0957 0.073 Uiso calc U P R 0.695(11) A 2
C C35A 1.0575(10) 0.9063(4) 0.0392(6) 0.045(2) Uani d U P D 0.695(11) A 2
H H35C 1.0511 0.9488 0.0533 0.054 Uiso calc U P R 0.695(11) A 2
H H35D 1.1482 0.8969 0.03 0.054 Uiso calc U P R 0.695(11) A 2
C C36A 1.0117(11) 0.8678(4) 0.1102(6) 0.052(2) Uani d U P D 0.695(11) A 2
H H36C 1.0863 0.8556 0.153 0.063 Uiso calc U P R 0.695(11) A 2
H H36D 0.949 0.8896 0.1418 0.063 Uiso calc U P R 0.695(11) A 2
N N1 0.8200(3) 0.65071(14) 0.2267(2) 0.0181(7) Uani d . . . 1.0 . .
N N2 0.7457(3) 0.73915(14) 0.2672(2) 0.0171(7) Uani d . . . 1.0 . .
N N3 0.5630(3) 0.74720(14) 0.3272(2) 0.0184(7) Uani d . . . 1.0 . .
O O1 0.1520(4) 0.67792(16) 0.3043(3) 0.0517(12) Uani d . . . 1.0 . .
O O2 0.4114(4) 0.63952(17) 0.5425(2) 0.0480(10) Uani d . . . 1.0 . .
O O3 0.1828(4) 0.49637(17) 0.3944(4) 0.0702(16) Uani d . . . 1.0 . .
O O4 0.6042(5) 0.4943(2) 0.4110(3) 0.0722(16) Uani d . . . 1.0 . .
O O5 0.3339(4) 0.54362(19) 0.1510(3) 0.0608(13) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 C3 . 1.981(5) ?
W1 C1 . 2.013(5) ?
W1 C5 . 2.029(6) ?
W1 C4 . 2.038(5) ?
W1 C2 . 2.048(5) ?
W1 Ge1 . 2.6085(5) ?
Ge1 C6 . 1.847(4) ?
Ge1 N3 . 1.932(3) ?
C1 O1 . 1.150(6) ?
C2 O2 . 1.132(6) ?
C3 O3 . 1.151(6) ?
C4 O4 . 1.142(6) ?
C5 O5 . 1.146(6) ?
C6 N1 . 1.404(5) ?
C6 N2 . 1.405(5) ?
C7 N1 . 1.470(5) ?
C7 C8 . 1.506(6) ?
C8 N2 . 1.479(5) ?
C9 N3 . 1.336(5) ?
C9 N2 . 1.356(5) ?
C9 C10 . 1.541(5) ?
C10 C11 . 1.531(6) ?
C10 C13 . 1.536(6) ?
C10 C12 . 1.543(7) ?
C14 N1 . 1.479(5) ?
C14 C16 . 1.513(6) ?
C14 C15 . 1.531(6) ?
C14 C17 . 1.536(6) ?
C15 C20 . 1.537(6) ?
C16 C22 . 1.536(6) ?
C17 C18 . 1.533(6) ?
C18 C19 . 1.518(8) ?
C18 C23 . 1.523(7) ?
C19 C20 . 1.523(7) ?
C20 C21 . 1.518(8) ?
C21 C22 . 1.517(8) ?
C22 C23 . 1.530(7) ?
C24 C25 . 1.390(6) ?
C24 C31 . 1.392(6) ?
C24 N3 . 1.445(5) ?
C25 C27 . 1.388(6) ?
C25 C26 . 1.502(6) ?
C27 C28 . 1.388(7) ?
C28 C30 . 1.385(7) ?
C28 C29 . 1.517(7) ?
C30 C31 . 1.391(6) ?
C31 C32 . 1.501(7) ?
O6 C33 . 1.396(15) ?
O6 C36 . 1.403(15) ?
C33 C34 . 1.528(15) ?
C34 C35 . 1.533(15) ?
C35 C36 . 1.521(15) ?
O6A C33A . 1.401(10) ?
O6A C36A . 1.425(9) ?
C33A C34A . 1.513(11) ?
C34A C35A . 1.516(10) ?
C35A C36A . 1.516(10) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 W1 C1 . . 88.4(2) ?
C3 W1 C5 . . 89.0(2) ?
C1 W1 C5 . . 88.9(2) ?
C3 W1 C4 . . 87.8(2) ?
C1 W1 C4 . . 175.1(2) ?
C5 W1 C4 . . 94.0(2) ?
C3 W1 C2 . . 90.3(2) ?
C1 W1 C2 . . 87.7(2) ?
C5 W1 C2 . . 176.6(2) ?
C4 W1 C2 . . 89.3(2) ?
C3 W1 Ge1 . . 177.34(15) ?
C1 W1 Ge1 . . 92.57(14) ?
C5 W1 Ge1 . . 88.51(16) ?
C4 W1 Ge1 . . 91.34(15) ?
C2 W1 Ge1 . . 92.23(13) ?
C6 Ge1 N3 . . 83.70(16) ?
C6 Ge1 W1 . . 150.36(12) ?
N3 Ge1 W1 . . 124.89(11) ?
O1 C1 W1 . . 176.5(5) ?
O2 C2 W1 . . 176.8(5) ?
O3 C3 W1 . . 178.3(6) ?
O4 C4 W1 . . 176.0(5) ?
O5 C5 W1 . . 176.2(5) ?
N1 C6 N2 . . 107.0(3) ?
N1 C6 Ge1 . . 142.5(3) ?
N2 C6 Ge1 . . 110.5(3) ?
N1 C7 C8 . . 101.8(3) ?
N2 C8 C7 . . 101.5(3) ?
N3 C9 N2 . . 110.6(3) ?
N3 C9 C10 . . 128.8(4) ?
N2 C9 C10 . . 120.2(4) ?
C11 C10 C13 . . 106.9(4) ?
C11 C10 C9 . . 109.1(4) ?
C13 C10 C9 . . 113.8(4) ?
C11 C10 C12 . . 111.1(4) ?
C13 C10 C12 . . 105.8(4) ?
C9 C10 C12 . . 110.2(4) ?
N1 C14 C16 . . 110.3(3) ?
N1 C14 C15 . . 113.1(3) ?
C16 C14 C15 . . 109.3(4) ?
N1 C14 C17 . . 108.0(3) ?
C16 C14 C17 . . 107.7(4) ?
C15 C14 C17 . . 108.4(4) ?
C14 C15 C20 . . 110.2(4) ?
C14 C16 C22 . . 111.3(4) ?
C18 C17 C14 . . 110.6(4) ?
C19 C18 C23 . . 110.4(4) ?
C19 C18 C17 . . 109.1(4) ?
C23 C18 C17 . . 109.1(4) ?
C18 C19 C20 . . 109.9(4) ?
C21 C20 C19 . . 109.3(4) ?
C21 C20 C15 . . 109.5(4) ?
C19 C20 C15 . . 109.1(4) ?
C22 C21 C20 . . 110.0(4) ?
C21 C22 C23 . . 110.3(4) ?
C21 C22 C16 . . 109.3(4) ?
C23 C22 C16 . . 108.4(4) ?
C18 C23 C22 . . 108.8(4) ?
C25 C24 C31 . . 121.7(4) ?
C25 C24 N3 . . 118.3(4) ?
C31 C24 N3 . . 119.8(4) ?
C27 C25 C24 . . 118.3(4) ?
C27 C25 C26 . . 120.4(4) ?
C24 C25 C26 . . 121.3(4) ?
C25 C27 C28 . . 121.9(4) ?
C30 C28 C27 . . 118.0(4) ?
C30 C28 C29 . . 121.4(5) ?
C27 C28 C29 . . 120.6(5) ?
C28 C30 C31 . . 122.3(5) ?
C30 C31 C24 . . 117.9(4) ?
C30 C31 C32 . . 120.5(4) ?
C24 C31 C32 . . 121.6(4) ?
C33 O6 C36 . . 107.4(14) ?
O6 C33 C34 . . 104.0(14) ?
C33 C34 C35 . . 96.6(14) ?
C36 C35 C34 . . 98.1(12) ?
O6 C36 C35 . . 107.7(13) ?
C33A O6A C36A . . 109.4(7) ?
O6A C33A C34A . . 106.2(7) ?
C33A C34A C35A . . 100.5(7) ?
C34A C35A C36A . . 101.8(7) ?
O6A C36A C35A . . 106.6(7) ?
C6 N1 C7 . . 107.5(3) ?
C6 N1 C14 . . 121.8(3) ?
C7 N1 C14 . . 118.1(3) ?
C9 N2 C6 . . 119.7(3) ?
C9 N2 C8 . . 130.5(3) ?
C6 N2 C8 . . 109.5(3) ?
C9 N3 C24 . . 127.0(3) ?
C9 N3 Ge1 . . 115.4(3) ?
C24 N3 Ge1 . . 117.5(3) ?

