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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_4043_0m0
_database_code_depnum_ccdc_archive 'CCDC 1553387'
_audit_update_record             
;
2017-05-31 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        DH-113
_chemical_formula_moiety         'C36 H76 Nb O2 P3 Si6'
_chemical_formula_sum            'C36 H76 Nb O2 P3 Si6'
_chemical_formula_weight         895.32
_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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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      monoclinic
_space_group_IT_number           14
_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                   13.548(5)
_cell_length_b                   18.581(9)
_cell_length_c                   20.379(7)
_cell_angle_alpha                90
_cell_angle_beta                 100.01(2)
_cell_angle_gamma                90
_cell_volume                     5052(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12043
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.999
_cell_measurement_theta_min      2.006
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.942
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.745830
_exptl_absorpt_correction_T_min  0.537366
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (2009/2), Bruker AXS 2009'
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.4568
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12043
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.006
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3808
_reflns_number_total             12043
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         1.087
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         12043
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2870
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      0.826
_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)+(0.0445P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1713
_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:
 C7(H7), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_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
Nb Nb 0.47533(5) 0.77040(4) 0.82577(3) 0.02607(19) Uani 1 1 d . . . . .
P1 P 0.53218(14) 0.64619(11) 0.78699(8) 0.0301(5) Uani 1 1 d . . . . .
P2 P 0.65622(14) 0.81196(12) 0.82196(8) 0.0317(5) Uani 1 1 d . . . . .
P3 P 0.43106(13) 0.80019(11) 0.69975(7) 0.0269(5) Uani 1 1 d . . . . .
Si1 Si 0.32262(15) 0.74974(11) 0.85999(8) 0.0288(5) Uani 1 1 d . . . . .
Si2 Si 0.30266(14) 0.93157(12) 1.00130(8) 0.0288(5) Uani 1 1 d . . . . .
Si3 Si 0.12569(14) 0.93298(11) 0.87062(8) 0.0288(5) Uani 1 1 d . . . . .
Si4 Si 0.27814(14) 0.53971(12) 0.95423(8) 0.0288(5) Uani 1 1 d . . . . .
Si5 Si 0.09532(15) 0.57943(12) 0.83270(8) 0.0305(5) Uani 1 1 d . . . . .
Si6 Si 0.63704(15) 0.73121(12) 0.68456(8) 0.0307(5) Uani 1 1 d . . . . .
O1 O 0.4423(4) 0.9387(3) 0.8580(2) 0.0409(14) Uani 1 1 d . . . . .
O2 O 0.5593(4) 0.7271(3) 0.9794(2) 0.0523(17) Uani 1 1 d . . . . .
C1 C 0.2264(5) 0.7454(4) 0.9168(3) 0.0204(17) Uani 1 1 d . . . . .
C2 C 0.1935(5) 0.8095(4) 0.9445(3) 0.0194(16) Uani 1 1 d . . . . .
C3 C 0.1218(5) 0.8025(4) 0.9862(3) 0.0247(17) Uani 1 1 d . . . . .
H3 H 0.0983 0.8450 1.0043 0.030 Uiso 1 1 calc R . . . .
C4 C 0.0834(5) 0.7371(4) 1.0023(3) 0.0279(18) Uani 1 1 d . . . . .
C5 C 0.1174(5) 0.6746(4) 0.9740(3) 0.0250(17) Uani 1 1 d . . . . .
H5 H 0.0926 0.6290 0.9846 0.030 Uiso 1 1 calc R . . . .
C6 C 0.1863(5) 0.6782(4) 0.9310(3) 0.0240(18) Uani 1 1 d . . . . .
C7 C 0.2275(5) 0.8828(4) 0.9276(3) 0.0238(17) Uani 1 1 d . . . . .
H7 H 0.2781 0.8724 0.8985 0.029 Uiso 1 1 calc R . . . .
C8 C 0.3295(6) 1.0258(4) 0.9799(3) 0.045(2) Uani 1 1 d . . . . .
H8A H 0.3633 1.0262 0.9411 0.068 Uiso 1 1 calc GR . . . .
H8B H 0.3728 1.0484 1.0178 0.068 Uiso 1 1 calc GR . . . .
H8C H 0.2664 1.0527 0.9694 0.068 Uiso 1 1 calc GR . . . .
C9 C 0.4232(5) 0.8817(4) 1.0254(3) 0.042(2) Uani 1 1 d . . . . .
H9A H 0.4092 0.8319 1.0365 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.4636 0.9050 1.0642 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.4602 0.8822 0.9881 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.2353(5) 0.9367(4) 1.0752(3) 0.0316(19) Uani 1 1 d . . . . .
H10A H 0.1682 0.9570 1.0609 0.047 Uiso 1 1 calc GR . . . .
H10B H 0.2733 0.9674 1.1097 0.047 Uiso 1 1 calc GR . . . .
H10C H 0.2294 0.8883 1.0932 0.047 Uiso 1 1 calc GR . . . .
C11 C 0.1829(6) 1.0014(4) 0.8216(3) 0.047(2) Uani 1 1 d . . . . .
H11A H 0.2066 1.0424 0.8503 0.070 Uiso 1 1 calc GR . . . .
H11B H 0.1326 1.0179 0.7841 0.070 Uiso 1 1 calc GR . . . .
H11C H 0.2395 0.9798 0.8046 0.070 Uiso 1 1 calc GR . . . .
C12 C 0.0527(5) 0.8682(4) 0.8125(3) 0.045(2) Uani 1 1 d . . . . .
H12A H 0.0963 0.8466 0.7842 0.067 Uiso 1 1 calc GR . . . .
H12B H -0.0029 0.8933 0.7846 0.067 Uiso 1 1 calc GR . . . .
H12C H 0.0262 0.8303 0.8380 0.067 Uiso 1 1 calc GR . . . .
C13 C 0.0382(6) 0.9802(4) 0.9179(3) 0.047(2) Uani 1 1 d . . . . .
H13A H -0.0004 0.9445 0.9382 0.070 Uiso 1 1 calc GR . . . .
H13B H -0.0077 1.0107 0.8873 0.070 Uiso 1 1 calc GR . . . .
H13C H 0.0769 1.0101 0.9528 0.070 Uiso 1 1 calc GR . . . .
C14 C 0.0089(5) 0.7304(4) 1.0508(3) 0.0321(18) Uani 1 1 d . . . . .
C15 C 0.0610(6) 0.6909(5) 1.1159(3) 0.068(3) Uani 1 1 d . . . . .
H15A H 0.0833 0.6431 1.1043 0.103 Uiso 1 1 calc GR . . . .
H15B H 0.0132 0.6859 1.1466 0.103 Uiso 1 1 calc GR . . . .
H15C H 0.1190 0.7190 1.1372 0.103 Uiso 1 1 calc GR . . . .
C16 C -0.0805(5) 0.6833(4) 1.0198(3) 0.042(2) Uani 1 1 d . . . . .
H16A H -0.1158 0.7063 0.9791 0.063 Uiso 1 1 calc GR . . . .
H16B H -0.1265 0.6778 1.0516 0.063 Uiso 1 1 calc GR . . . .
H16C H -0.0562 0.6359 1.0089 0.063 Uiso 1 1 calc GR . . . .
C17 C -0.0321(7) 0.8039(5) 1.0673(4) 0.079(3) Uani 1 1 d . . . . .
H17A H 0.0227 0.8332 1.0913 0.119 Uiso 1 1 calc GR . . . .
H17B H -0.0834 0.7971 1.0952 0.119 Uiso 1 1 calc GR . . . .
H17C H -0.0617 0.8283 1.0259 0.119 Uiso 1 1 calc GR . . . .
C18 C 0.2094(5) 0.6093(4) 0.8957(3) 0.0232(16) Uani 1 1 d . . . . .
H18 H 0.2593 0.6245 0.8676 0.028 Uiso 1 1 calc R . . . .
C19 C 0.4006(5) 0.5797(4) 0.9912(3) 0.0306(18) Uani 1 1 d . . . . .
H19A H 0.4404 0.5879 0.9561 0.046 Uiso 1 1 calc GR . . . .
H19B H 0.4365 0.5468 1.0246 0.046 Uiso 1 1 calc GR . . . .
H19C H 0.3895 0.6257 1.0124 0.046 Uiso 1 1 calc GR . . . .
C20 C 0.3024(5) 0.4546(4) 0.9081(3) 0.040(2) Uani 1 1 d . . . . .
H20A H 0.2387 0.4302 0.8919 0.060 Uiso 1 1 calc GR . . . .
H20B H 0.3463 0.4226 0.9384 0.060 Uiso 1 1 calc GR . . . .
H20C H 0.3349 0.4671 0.8703 0.060 Uiso 1 1 calc GR . . . .
C21 C 0.2091(5) 0.5128(4) 1.0226(3) 0.038(2) Uani 1 1 d . . . . .
H21A H 0.2116 0.5523 1.0547 0.058 Uiso 1 1 calc GR . . . .
H21B H 0.2406 0.4699 1.0452 0.058 Uiso 1 1 calc GR . . . .
H21C H 0.1391 0.5021 1.0036 0.058 Uiso 1 1 calc GR . . . .
C22 C 0.0239(5) 0.6596(4) 0.7981(3) 0.050(2) Uani 1 1 d . . . . .
H22A H -0.0107 0.6805 0.8320 0.075 Uiso 1 1 calc GR . . . .
H22B H -0.0254 0.6457 0.7592 0.075 Uiso 1 1 calc GR . . . .
H22C H 0.0701 0.6953 0.7849 0.075 Uiso 1 1 calc GR . . . .
C23 C 0.1415(5) 0.5314(5) 0.7625(3) 0.047(2) Uani 1 1 d . . . . .
H23A H 0.1836 0.5640 0.7415 0.070 Uiso 1 1 calc GR . . . .
H23B H 0.0841 0.5159 0.7294 0.070 Uiso 1 1 calc GR . . . .
H23C H 0.1809 0.4892 0.7800 0.070 Uiso 1 1 calc GR . . . .
C24 C 0.0098(5) 0.5179(5) 0.8707(3) 0.050(2) Uani 1 1 d . . . . .
H24A H 0.0428 0.4714 0.8811 0.074 Uiso 1 1 calc GR . . . .
H24B H -0.0527 0.5109 0.8391 0.074 Uiso 1 1 calc GR . . . .
H24C H -0.0051 0.5396 0.9117 0.074 Uiso 1 1 calc GR . . . .
C25 C 0.5811(5) 0.6444(4) 0.7078(3) 0.0297(19) Uani 1 1 d . . . . .
H25A H 0.5258 0.6308 0.6715 0.036 Uiso 1 1 calc R . . . .
H25B H 0.6329 0.6063 0.7109 0.036 Uiso 1 1 calc R . . . .
C26 C 0.4404(5) 0.5730(4) 0.7741(3) 0.048(2) Uani 1 1 d . . . . .
H26A H 0.4239 0.5583 0.8171 0.071 Uiso 1 1 calc GR . . . .
H26B H 0.4687 0.5320 0.7535 0.071 Uiso 1 1 calc GR . . . .
H26C H 0.3795 0.5895 0.7448 0.071 Uiso 1 1 calc GR . . . .
C27 C 0.6319(5) 0.6031(4) 0.8445(3) 0.044(2) Uani 1 1 d . . . . .
H27A H 0.6913 0.6341 0.8513 0.066 Uiso 1 1 calc GR . . . .
H27B H 0.6484 0.5568 0.8261 0.066 Uiso 1 1 calc GR . . . .
H27C H 0.6098 0.5951 0.8872 0.066 Uiso 1 1 calc GR . . . .
C28 C 0.7209(5) 0.7672(4) 0.7607(3) 0.0371(19) Uani 1 1 d . . . . .
H28A H 0.7609 0.7268 0.7832 0.045 Uiso 1 1 calc R . . . .
H28B H 0.7682 0.8019 0.7463 0.045 Uiso 1 1 calc R . . . .
C29 C 0.6684(6) 0.9054(4) 0.7996(3) 0.043(2) Uani 1 1 d . . . . .
H29A H 0.6322 0.9136 0.7542 0.064 Uiso 1 1 calc GR . . . .
H29B H 0.7394 0.9171 0.8017 0.064 Uiso 1 1 calc GR . . . .
H29C H 0.6401 0.9362 0.8307 0.064 Uiso 1 1 calc GR . . . .
C30 C 0.7470(5) 0.8055(5) 0.8995(3) 0.056(3) Uani 1 1 d . . . . .
H30A H 0.7225 0.8328 0.9345 0.084 Uiso 1 1 calc GR . . . .
H30B H 0.8114 0.8254 0.8926 0.084 Uiso 1 1 calc GR . . . .
H30C H 0.7558 0.7550 0.9128 0.084 Uiso 1 1 calc GR . . . .
C31 C 0.5359(5) 0.7989(4) 0.6534(3) 0.0299(18) Uani 1 1 d . . . . .
H31A H 0.5664 0.8474 0.6556 0.036 Uiso 1 1 calc R . . . .
H31B H 0.5091 0.7884 0.6060 0.036 Uiso 1 1 calc R . . . .
C32 C 0.3758(6) 0.8873(4) 0.6774(3) 0.045(2) Uani 1 1 d . . . . .
H32A H 0.3146 0.8927 0.6965 0.067 Uiso 1 1 calc GR . . . .
H32B H 0.3591 0.8912 0.6288 0.067 Uiso 1 1 calc GR . . . .
H32C H 0.4235 0.9252 0.6947 0.067 Uiso 1 1 calc GR . . . .
C33 C 0.3370(5) 0.7422(4) 0.6515(3) 0.043(2) Uani 1 1 d . . . . .
H33A H 0.3615 0.6925 0.6537 0.065 Uiso 1 1 calc GR . . . .
H33B H 0.3241 0.7583 0.6050 0.065 Uiso 1 1 calc GR . . . .
H33C H 0.2749 0.7447 0.6698 0.065 Uiso 1 1 calc GR . . . .
C34 C 0.7135(6) 0.7130(4) 0.6190(3) 0.050(2) Uani 1 1 d . . . . .
H34A H 0.7412 0.7583 0.6056 0.075 Uiso 1 1 calc GR . . . .
H34B H 0.6712 0.6909 0.5804 0.075 Uiso 1 1 calc GR . . . .
H34C H 0.7683 0.6801 0.6366 0.075 Uiso 1 1 calc GR . . . .
C35 C 0.4522(6) 0.8770(5) 0.8480(3) 0.036(2) Uani 1 1 d . . . . .
C36 C 0.5263(5) 0.7434(4) 0.9240(4) 0.0339(19) 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
Nb P1 2.599(2) . ?
Nb P2 2.584(2) . ?
Nb P3 2.5933(18) . ?
Nb Si1 2.327(2) . ?
Nb C35 2.068(9) . ?
Nb C36 2.063(7) . ?
P1 C25 1.848(6) . ?
P1 C26 1.830(7) . ?
P1 C27 1.814(6) . ?
P2 C28 1.843(7) . ?
P2 C29 1.810(8) . ?
P2 C30 1.829(6) . ?
P3 C31 1.837(7) . ?
P3 C32 1.809(7) . ?
P3 C33 1.821(7) . ?
Si1 C1 1.890(7) . ?
Si2 C7 1.893(6) . ?
Si2 C8 1.856(8) . ?
Si2 C9 1.868(7) . ?
Si2 C10 1.894(6) . ?
Si3 C7 1.888(6) . ?
Si3 C11 1.867(7) . ?
Si3 C12 1.850(7) . ?
Si3 C13 1.870(7) . ?
Si4 C18 1.891(6) . ?
Si4 C19 1.854(6) . ?
Si4 C20 1.897(7) . ?
Si4 C21 1.876(7) . ?
Si5 C18 1.911(6) . ?
Si5 C22 1.848(7) . ?
Si5 C23 1.884(7) . ?
Si5 C24 1.887(8) . ?
Si6 C25 1.878(7) . ?
Si6 C28 1.880(6) . ?
Si6 C31 1.887(7) . ?
Si6 C34 1.858(7) . ?
O1 C35 1.176(8) . ?
O2 C36 1.179(7) . ?
C1 C2 1.423(9) . ?
C1 C6 1.412(9) . ?
C2 C3 1.402(8) . ?
C2 C7 1.497(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(9) . ?
C4 C5 1.409(9) . ?
C4 C14 1.537(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(8) . ?
C6 C18 1.529(9) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
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 C15 1.571(9) . ?
C14 C16 1.538(10) . ?
C14 C17 1.533(11) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
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 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
P2 Nb P1 85.61(7) . . ?
P2 Nb P3 87.92(6) . . ?
P3 Nb P1 85.31(6) . . ?
Si1 Nb P1 105.70(7) . . ?
Si1 Nb P2 162.88(6) . . ?
Si1 Nb P3 105.52(6) . . ?
C35 Nb P1 168.9(2) . . ?
C35 Nb P2 84.3(2) . . ?
C35 Nb P3 89.70(17) . . ?
C35 Nb Si1 85.2(2) . . ?
C36 Nb P1 90.7(2) . . ?
C36 Nb P2 86.7(2) . . ?
C36 Nb P3 173.5(2) . . ?
C36 Nb Si1 80.5(2) . . ?
C36 Nb C35 93.3(3) . . ?
C25 P1 Nb 116.9(2) . . ?
C26 P1 Nb 118.3(3) . . ?
C26 P1 C25 101.5(3) . . ?
C27 P1 Nb 115.0(2) . . ?
C27 P1 C25 102.5(3) . . ?
C27 P1 C26 100.1(3) . . ?
C28 P2 Nb 116.8(2) . . ?
C29 P2 Nb 115.0(3) . . ?
C29 P2 C28 100.8(3) . . ?
C29 P2 C30 101.7(4) . . ?
C30 P2 Nb 117.0(3) . . ?
C30 P2 C28 103.2(3) . . ?
C31 P3 Nb 116.09(18) . . ?
C32 P3 Nb 117.1(2) . . ?
C32 P3 C31 101.9(3) . . ?
C32 P3 C33 100.0(3) . . ?
C33 P3 Nb 115.4(2) . . ?
C33 P3 C31 104.2(3) . . ?
C1 Si1 Nb 159.17(18) . . ?
C7 Si2 C10 112.8(3) . . ?
C8 Si2 C7 111.5(3) . . ?
C8 Si2 C9 109.4(4) . . ?
C8 Si2 C10 106.3(3) . . ?
C9 Si2 C7 107.2(3) . . ?
C9 Si2 C10 109.7(3) . . ?
C11 Si3 C7 109.8(3) . . ?
C11 Si3 C13 108.4(4) . . ?
C12 Si3 C7 108.9(3) . . ?
C12 Si3 C11 109.0(3) . . ?
C12 Si3 C13 108.6(3) . . ?
C13 Si3 C7 112.1(3) . . ?
C18 Si4 C20 111.5(3) . . ?
C19 Si4 C18 106.8(3) . . ?
C19 Si4 C20 108.4(3) . . ?
C19 Si4 C21 109.4(3) . . ?
C21 Si4 C18 113.4(3) . . ?
C21 Si4 C20 107.3(4) . . ?
C22 Si5 C18 109.3(3) . . ?
C22 Si5 C23 108.3(4) . . ?
C22 Si5 C24 109.1(4) . . ?
C23 Si5 C18 108.1(3) . . ?
C23 Si5 C24 109.5(4) . . ?
C24 Si5 C18 112.5(3) . . ?
C25 Si6 C28 108.0(3) . . ?
C25 Si6 C31 110.9(3) . . ?
C28 Si6 C31 109.9(3) . . ?
C34 Si6 C25 108.9(3) . . ?
C34 Si6 C28 109.0(3) . . ?
C34 Si6 C31 110.0(3) . . ?
C2 C1 Si1 120.4(5) . . ?
C6 C1 Si1 119.6(5) . . ?
C6 C1 C2 120.0(6) . . ?
C1 C2 C7 122.6(6) . . ?
C3 C2 C1 117.4(7) . . ?
C3 C2 C7 119.8(6) . . ?
C2 C3 H3 118.2 . . ?
C4 C3 C2 123.6(7) . . ?
C4 C3 H3 118.2 . . ?
C3 C4 C5 117.7(6) . . ?
C3 C4 C14 122.6(7) . . ?
C5 C4 C14 119.7(7) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(7) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C18 121.8(6) . . ?
C5 C6 C1 119.8(7) . . ?
C5 C6 C18 118.2(7) . . ?
Si2 C7 H7 103.5 . . ?
Si3 C7 Si2 119.1(4) . . ?
Si3 C7 H7 103.5 . . ?
C2 C7 Si2 113.4(4) . . ?
C2 C7 Si3 111.7(4) . . ?
C2 C7 H7 103.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C15 109.3(5) . . ?
C4 C14 C16 109.9(5) . . ?
C16 C14 C15 106.7(6) . . ?
C17 C14 C4 111.9(7) . . ?
C17 C14 C15 111.0(6) . . ?
C17 C14 C16 107.9(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C18 Si5 118.5(4) . . ?
Si4 C18 H18 104.3 . . ?
Si5 C18 H18 104.3 . . ?
C6 C18 Si4 113.2(4) . . ?
C6 C18 Si5 110.6(4) . . ?
C6 C18 H18 104.3 . . ?
Si4 C19 H19A 109.5 . . ?
Si4 C19 H19B 109.5 . . ?
Si4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si5 C22 H22A 109.5 . . ?
Si5 C22 H22B 109.5 . . ?
Si5 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si5 C23 H23A 109.5 . . ?
Si5 C23 H23B 109.5 . . ?
Si5 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si5 C24 H24A 109.5 . . ?
Si5 C24 H24B 109.5 . . ?
Si5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P1 C25 Si6 115.2(3) . . ?
P1 C25 H25A 108.5 . . ?
P1 C25 H25B 108.5 . . ?
Si6 C25 H25A 108.5 . . ?
Si6 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
P1 C26 H26A 109.5 . . ?
P1 C26 H26B 109.5 . . ?
P1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
P1 C27 H27A 109.5 . . ?
P1 C27 H27B 109.5 . . ?
P1 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
P2 C28 Si6 115.4(3) . . ?
P2 C28 H28A 108.4 . . ?
P2 C28 H28B 108.4 . . ?
Si6 C28 H28A 108.4 . . ?
Si6 C28 H28B 108.4 . . ?
H28A C28 H28B 107.5 . . ?
P2 C29 H29A 109.5 . . ?
P2 C29 H29B 109.5 . . ?
P2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P2 C30 H30A 109.5 . . ?
P2 C30 H30B 109.5 . . ?
P2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
P3 C31 Si6 114.6(3) . . ?
P3 C31 H31A 108.6 . . ?
P3 C31 H31B 108.6 . . ?
Si6 C31 H31A 108.6 . . ?
Si6 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si6 C34 H34A 109.5 . . ?
Si6 C34 H34B 109.5 . . ?
Si6 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O1 C35 Nb 176.2(6) . . ?
O2 C36 Nb 177.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nb P1 C25 Si6 26.0(4) . . . . ?
Nb P2 C28 Si6 27.5(5) . . . . ?
Nb P3 C31 Si6 32.5(4) . . . . ?
Nb Si1 C1 C2 63.9(8) . . . . ?
Nb Si1 C1 C6 -116.8(6) . . . . ?
Si1 C1 C2 C3 179.9(4) . . . . ?
Si1 C1 C2 C7 3.7(7) . . . . ?
Si1 C1 C6 C5 178.4(4) . . . . ?
Si1 C1 C6 C18 -7.1(7) . . . . ?
C1 C2 C3 C4 1.2(8) . . . . ?
C1 C2 C7 Si2 -116.0(5) . . . . ?
C1 C2 C7 Si3 106.0(6) . . . . ?
C1 C6 C18 Si4 117.6(5) . . . . ?
C1 C6 C18 Si5 -106.7(6) . . . . ?
C2 C1 C6 C5 -2.3(8) . . . . ?
C2 C1 C6 C18 172.2(5) . . . . ?
C2 C3 C4 C5 -1.2(9) . . . . ?
C2 C3 C4 C14 176.9(5) . . . . ?
C3 C2 C7 Si2 67.9(6) . . . . ?
C3 C2 C7 Si3 -70.1(6) . . . . ?
C3 C4 C5 C6 -0.5(9) . . . . ?
C3 C4 C14 C15 -112.2(7) . . . . ?
C3 C4 C14 C16 131.1(6) . . . . ?
C3 C4 C14 C17 11.2(8) . . . . ?
C4 C5 C6 C1 2.3(8) . . . . ?
C4 C5 C6 C18 -172.5(5) . . . . ?
C5 C4 C14 C15 65.9(8) . . . . ?
C5 C4 C14 C16 -50.9(8) . . . . ?
C5 C4 C14 C17 -170.7(6) . . . . ?
C5 C6 C18 Si4 -67.8(6) . . . . ?
C5 C6 C18 Si5 67.9(6) . . . . ?
C6 C1 C2 C3 0.6(8) . . . . ?
C6 C1 C2 C7 -175.6(5) . . . . ?
C7 C2 C3 C4 177.5(5) . . . . ?
C8 Si2 C7 Si3 -38.4(5) . . . . ?
C8 Si2 C7 C2 -173.1(5) . . . . ?
C9 Si2 C7 Si3 -158.1(4) . . . . ?
C9 Si2 C7 C2 67.2(6) . . . . ?
C10 Si2 C7 Si3 81.0(4) . . . . ?
C10 Si2 C7 C2 -53.6(6) . . . . ?
C11 Si3 C7 Si2 69.9(5) . . . . ?
C11 Si3 C7 C2 -154.7(5) . . . . ?
C12 Si3 C7 Si2 -170.8(4) . . . . ?
C12 Si3 C7 C2 -35.4(5) . . . . ?
C13 Si3 C7 Si2 -50.6(5) . . . . ?
C13 Si3 C7 C2 84.7(5) . . . . ?
C14 C4 C5 C6 -178.7(5) . . . . ?
C19 Si4 C18 Si5 165.1(4) . . . . ?
C19 Si4 C18 C6 -63.0(6) . . . . ?
C20 Si4 C18 Si5 46.8(5) . . . . ?
C20 Si4 C18 C6 178.8(5) . . . . ?
C21 Si4 C18 Si5 -74.4(4) . . . . ?
C21 Si4 C18 C6 57.6(6) . . . . ?
C25 Si6 C28 P2 -78.2(5) . . . . ?
C25 Si6 C31 P3 40.2(4) . . . . ?
C26 P1 C25 Si6 156.2(4) . . . . ?
C27 P1 C25 Si6 -100.6(4) . . . . ?
C28 Si6 C25 P1 45.6(4) . . . . ?
C28 Si6 C31 P3 -79.2(4) . . . . ?
C29 P2 C28 Si6 -97.9(4) . . . . ?
C30 P2 C28 Si6 157.3(4) . . . . ?
C31 Si6 C25 P1 -74.9(4) . . . . ?
C31 Si6 C28 P2 42.9(5) . . . . ?
C32 P3 C31 Si6 160.9(4) . . . . ?
C33 P3 C31 Si6 -95.5(4) . . . . ?
C34 Si6 C25 P1 163.9(3) . . . . ?
C34 Si6 C28 P2 163.6(4) . . . . ?
C34 Si6 C31 P3 160.8(4) . . . . ?

_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_3399f
_database_code_depnum_ccdc_archive 'CCDC 1555671'
_audit_update_record             
;
2017-06-12 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 Cl Ge Nb O3'
_chemical_formula_sum            'C32 H30 Cl Ge Nb O3'
_chemical_formula_weight         663.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   20.237(3)
_cell_length_b                   15.315(2)
_cell_length_c                   9.1804(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2845.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1732
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      25.10

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8576
_exptl_absorpt_correction_T_max  0.9690
_exptl_absorpt_process_details   'Bruker Sadabs 2009/2'

_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  'Bruker X8-KappaApexII'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11778
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         28.00
_reflns_number_total             3556
_reflns_number_gt                2725
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0000P)²+1.1214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3556
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.011
_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
C1 C 0.08674(19) 0.2500 0.3738(4) 0.0158(8) Uani 1 2 d S . .
C2 C 0.07506(14) 0.1700(2) 0.4437(3) 0.0183(6) Uani 1 1 d . . .
C3 C 0.05202(16) 0.1715(2) 0.5865(4) 0.0284(8) Uani 1 1 d . . .
H3A H 0.0442 0.1182 0.6364 0.034 Uiso 1 1 calc R . .
C4 C 0.0405(3) 0.2500 0.6568(5) 0.0338(12) Uani 1 2 d S . .
H4 H 0.0244 0.2500 0.7541 0.041 Uiso 1 2 calc SR . .
C5 C 0.08669(14) 0.08714(19) 0.3610(3) 0.0167(6) Uani 1 1 d . . .
C6 C 0.03560(14) 0.0496(2) 0.2791(3) 0.0192(6) Uani 1 1 d . . .
C7 C 0.04925(14) -0.0218(2) 0.1906(3) 0.0200(7) Uani 1 1 d . . .
H7A H 0.0148 -0.0464 0.1333 0.024 Uiso 1 1 calc R . .
C8 C 0.11216(15) -0.0582(2) 0.1839(4) 0.0222(7) Uani 1 1 d . . .
C9 C 0.16089(15) -0.0238(2) 0.2728(4) 0.0217(7) Uani 1 1 d . . .
H9A H 0.2035 -0.0497 0.2723 0.026 Uiso 1 1 calc R . .
C10 C 0.14929(15) 0.0474(2) 0.3624(3) 0.0203(7) Uani 1 1 d . . .
C11 C -0.03468(15) 0.0833(2) 0.2902(4) 0.0265(7) Uani 1 1 d . . .
H11A H -0.0352 0.1464 0.2718 0.032 Uiso 1 1 calc R . .
H11B H -0.0519 0.0717 0.3880 0.032 Uiso 1 1 calc R . .
H11C H -0.0624 0.0538 0.2179 0.032 Uiso 1 1 calc R . .
C12 C 0.12631(18) -0.1332(2) 0.0824(5) 0.0398(10) Uani 1 1 d . . .
H12A H 0.1399 -0.1104 -0.0127 0.048 Uiso 1 1 calc R . .
H12B H 0.0864 -0.1688 0.0709 0.048 Uiso 1 1 calc R . .
H12C H 0.1619 -0.1692 0.1230 0.048 Uiso 1 1 calc R . .
C13 C 0.20316(16) 0.0791(2) 0.4630(4) 0.0287(8) Uani 1 1 d . . .
H13C H 0.2444 0.0485 0.4406 0.034 Uiso 1 1 calc R . .
H13B H 0.1905 0.0675 0.5642 0.034 Uiso 1 1 calc R . .
H13A H 0.2095 0.1420 0.4494 0.034 Uiso 1 1 calc R . .
C14 C 0.2934(2) 0.2500 0.2496(5) 0.0268(11) Uani 1 2 d S . .
H14A H 0.2734 0.2500 0.3433 0.032 Uiso 1 2 calc SR . .
C15 C 0.31070(15) 0.1758(3) 0.1680(4) 0.0310(8) Uani 1 1 d . . .
H15A H 0.3045 0.1169 0.1971 0.037 Uiso 1 1 calc R . .
C16 C 0.33880(15) 0.2039(3) 0.0355(4) 0.0339(9) Uani 1 1 d . . .
H16A H 0.3549 0.1674 -0.0403 0.041 Uiso 1 1 calc R . .
C17 C 0.17386(15) 0.1400(2) -0.0387(3) 0.0199(7) Uani 1 1 d . . .
C18 C 0.22002(19) 0.2500 -0.1957(5) 0.0180(9) Uani 1 2 d S . .
O1 O 0.14798(12) 0.07868(16) -0.0838(3) 0.0320(6) Uani 1 1 d . . .
O2 O 0.21768(15) 0.2500 -0.3202(3) 0.0279(8) Uani 1 2 d S . .
Cl Cl 0.02530(5) 0.2500 0.05502(11) 0.0307(3) Uani 1 2 d S . .
Ge Ge 0.11948(2) 0.2500 0.17268(5) 0.01392(12) Uani 1 2 d S . .
Nb Nb 0.225330(17) 0.2500 0.02854(4) 0.01419(11) Uani 1 2 d S . .


_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
C1 C2 1.404(4) . ?
C1 C2 1.404(4) 8_565 ?
C1 Ge 1.962(4) . ?
C2 C3 1.392(4) . ?
C2 C5 1.497(4) . ?
C3 C4 1.384(4) . ?
C3 H3A 0.9500 . ?
C4 C3 1.384(4) 8_565 ?
C4 H4 0.9500 . ?
C5 C6 1.402(4) . ?
C5 C10 1.406(4) . ?
C6 C7 1.390(4) . ?
C6 C11 1.517(4) . ?
C7 C8 1.391(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.384(4) . ?
C8 C12 1.506(5) . ?
C9 C10 1.385(4) . ?
C9 H9A 0.9500 . ?
C10 C13 1.509(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13A 0.9800 . ?
C14 C15 1.405(4) . ?
C14 C15 1.405(4) 8_565 ?
C14 Nb 2.452(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.410(5) . ?
C15 Nb 2.432(3) . ?
C15 H15A 0.9500 . ?
C16 C16 1.411(8) 8_565 ?
C16 Nb 2.403(3) . ?
C16 H16A 0.9500 . ?
C17 O1 1.152(4) . ?
C17 Nb 2.074(3) . ?
C18 O2 1.145(5) . ?
C18 Nb 2.061(4) . ?
Cl Ge 2.1907(11) . ?
Ge Nb 2.5178(6) . ?
Nb C17 2.074(3) 8_565 ?
Nb C16 2.403(3) 8_565 ?
Nb C15 2.432(3) 8_565 ?

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
C2 C1 C2 121.7(4) . 8_565 ?
C2 C1 Ge 119.15(18) . . ?
C2 C1 Ge 119.14(18) 8_565 . ?
C3 C2 C1 118.1(3) . . ?
C3 C2 C5 123.0(3) . . ?
C1 C2 C5 118.8(3) . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C3 120.6(4) . 8_565 ?
C3 C4 H4 119.7 . . ?
C3 C4 H4 119.7 8_565 . ?
C6 C5 C10 119.5(3) . . ?
C6 C5 C2 120.2(3) . . ?
C10 C5 C2 120.3(3) . . ?
C7 C6 C5 119.3(3) . . ?
C7 C6 C11 119.6(3) . . ?
C5 C6 C11 121.0(3) . . ?
C6 C7 C8 121.5(3) . . ?
C6 C7 H7A 119.2 . . ?
C8 C7 H7A 119.2 . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 C12 121.3(3) . . ?
C7 C8 C12 120.4(3) . . ?
C8 C9 C10 121.9(3) . . ?
C8 C9 H9A 119.0 . . ?
C10 C9 H9A 119.0 . . ?
C9 C10 C5 119.2(3) . . ?
C9 C10 C13 119.6(3) . . ?
C5 C10 C13 121.1(3) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13C 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
C10 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
C15 C14 C15 107.9(4) . 8_565 ?
C15 C14 Nb 72.5(2) . . ?
C15 C14 Nb 72.5(2) 8_565 . ?
C15 C14 H14A 126.1 . . ?
C15 C14 H14A 126.1 8_565 . ?
Nb C14 H14A 120.7 . . ?
C14 C15 C16 108.3(3) . . ?
C14 C15 Nb 74.1(2) . . ?
C16 C15 Nb 71.93(18) . . ?
C14 C15 H15A 125.9 . . ?
C16 C15 H15A 125.9 . . ?
Nb C15 H15A 119.9 . . ?
C15 C16 C16 107.8(2) . 8_565 ?
C15 C16 Nb 74.16(18) . . ?
C16 C16 Nb 72.93(10) 8_565 . ?
C15 C16 H16A 126.1 . . ?
C16 C16 H16A 126.1 8_565 . ?
Nb C16 H16A 118.7 . . ?
O1 C17 Nb 175.5(3) . . ?
O2 C18 Nb 179.4(3) . . ?
C1 Ge Cl 99.81(12) . . ?
C1 Ge Nb 141.44(12) . . ?
Cl Ge Nb 118.75(4) . . ?
C18 Nb C17 71.14(10) . . ?
C18 Nb C17 71.13(10) . 8_565 ?
C17 Nb C17 108.58(17) . 8_565 ?
C18 Nb C16 94.37(13) . 8_565 ?
C17 Nb C16 136.56(13) . 8_565 ?
C17 Nb C16 104.44(13) 8_565 8_565 ?
C18 Nb C16 94.37(13) . . ?
C17 Nb C16 104.44(13) . . ?
C17 Nb C16 136.56(13) 8_565 . ?
C16 Nb C16 34.15(19) 8_565 . ?
C18 Nb C15 124.24(12) . . ?
C17 Nb C15 97.71(12) . . ?
C17 Nb C15 153.21(12) 8_565 . ?
C16 Nb C15 56.25(13) 8_565 . ?
C16 Nb C15 33.91(11) . . ?
C18 Nb C15 124.24(12) . 8_565 ?
C17 Nb C15 153.21(12) . 8_565 ?
C17 Nb C15 97.70(12) 8_565 8_565 ?
C16 Nb C15 33.91(11) 8_565 8_565 ?
C16 Nb C15 56.25(13) . 8_565 ?
C15 Nb C15 55.70(18) . 8_565 ?
C18 Nb C14 148.84(16) . . ?
C17 Nb C14 121.88(9) . . ?
C17 Nb C14 121.88(9) 8_565 . ?
C16 Nb C14 56.06(13) 8_565 . ?
C16 Nb C14 56.06(13) . . ?
C15 Nb C14 33.44(10) . . ?
C15 Nb C14 33.44(10) 8_565 . ?
C18 Nb Ge 118.72(11) . . ?
C17 Nb Ge 74.29(8) . . ?
C17 Nb Ge 74.29(8) 8_565 . ?
C16 Nb Ge 143.04(9) 8_565 . ?
C16 Nb Ge 143.04(9) . . ?
C15 Nb Ge 109.13(9) . . ?
C15 Nb Ge 109.13(9) 8_565 . ?
C14 Nb Ge 92.45(11) . . ?

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
C2 C1 C2 C3 -0.8(6) 8_565 . . . ?
Ge C1 C2 C3 179.8(2) . . . . ?
C2 C1 C2 C5 178.2(2) 8_565 . . . ?
Ge C1 C2 C5 -1.3(4) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C5 C2 C3 C4 -178.3(4) . . . . ?
C2 C3 C4 C3 -0.5(8) . . . 8_565 ?
C3 C2 C5 C6 89.3(4) . . . . ?
C1 C2 C5 C6 -89.6(4) . . . . ?
C3 C2 C5 C10 -92.0(4) . . . . ?
C1 C2 C5 C10 89.1(4) . . . . ?
C10 C5 C6 C7 -5.6(4) . . . . ?
C2 C5 C6 C7 173.0(3) . . . . ?
C10 C5 C6 C11 171.9(3) . . . . ?
C2 C5 C6 C11 -9.5(4) . . . . ?
C5 C6 C7 C8 1.5(5) . . . . ?
C11 C6 C7 C8 -176.1(3) . . . . ?
C6 C7 C8 C9 2.7(5) . . . . ?
C6 C7 C8 C12 -177.4(3) . . . . ?
C7 C8 C9 C10 -2.7(5) . . . . ?
C12 C8 C9 C10 177.4(3) . . . . ?
C8 C9 C10 C5 -1.4(5) . . . . ?
C8 C9 C10 C13 176.7(3) . . . . ?
C6 C5 C10 C9 5.6(4) . . . . ?
C2 C5 C10 C9 -173.1(3) . . . . ?
C6 C5 C10 C13 -172.5(3) . . . . ?
C2 C5 C10 C13 8.8(4) . . . . ?
C15 C14 C15 C16 0.0(5) 8_565 . . . ?
Nb C14 C15 C16 64.3(2) . . . . ?
C15 C14 C15 Nb -64.3(3) 8_565 . . . ?
C14 C15 C16 C16 0.0(3) . . . 8_565 ?
Nb C15 C16 C16 65.70(9) . . . 8_565 ?
C14 C15 C16 Nb -65.7(3) . . . . ?
C2 C1 Ge Cl 89.7(3) . . . . ?
C2 C1 Ge Cl -89.7(3) 8_565 . . . ?
C2 C1 Ge Nb -90.3(3) . . . . ?
C2 C1 Ge Nb 90.3(3) 8_565 . . . ?
O2 C18 Nb C17 -120.90(11) . . . . ?
O2 C18 Nb C17 120.90(10) . . . 8_565 ?
O2 C18 Nb C16 17.13(10) . . . 8_565 ?
O2 C18 Nb C16 -17.12(10) . . . . ?
O2 C18 Nb C15 -34.41(12) . . . . ?
O2 C18 Nb C15 34.41(13) . . . 8_565 ?
O2 C18 Nb C14 0.00(3) . . . . ?
O2 C18 Nb Ge 180.00(3) . . . . ?
O1 C17 Nb C18 36(3) . . . . ?
O1 C17 Nb C17 97(3) . . . 8_565 ?
O1 C17 Nb C16 -40(4) . . . 8_565 ?
O1 C17 Nb C16 -54(3) . . . . ?
O1 C17 Nb C15 -88(3) . . . . ?
O1 C17 Nb C15 -94(3) . . . 8_565 ?
O1 C17 Nb C14 -113(3) . . . . ?
O1 C17 Nb Ge 164(4) . . . . ?
C15 C16 Nb C18 -153.9(2) . . . . ?
C16 C16 Nb C18 91.35(4) 8_565 . . . ?
C15 C16 Nb C17 -82.3(2) . . . . ?
C16 C16 Nb C17 162.97(10) 8_565 . . . ?
C15 C16 Nb C17 139.1(2) . . . 8_565 ?
C16 C16 Nb C17 24.36(14) 8_565 . . 8_565 ?
C15 C16 Nb C16 114.8(2) . . . 8_565 ?
C16 C16 Nb C15 -114.8(2) 8_565 . . . ?
C15 C16 Nb C15 77.2(3) . . . 8_565 ?
C16 C16 Nb C15 -37.53(13) 8_565 . . 8_565 ?
C15 C16 Nb C14 36.70(19) . . . . ?
C16 C16 Nb C14 -78.07(9) 8_565 . . . ?
C15 C16 Nb Ge 0.7(3) . . . . ?
C16 C16 Nb Ge -114.09(13) 8_565 . . . ?
C14 C15 Nb C18 148.0(2) . . . . ?
C16 C15 Nb C18 32.1(3) . . . . ?
C14 C15 Nb C17 -139.7(2) . . . . ?
C16 C15 Nb C17 104.5(2) . . . . ?
C14 C15 Nb C17 29.2(4) . . . 8_565 ?
C16 C15 Nb C17 -86.6(3) . . . 8_565 ?
C14 C15 Nb C16 78.1(2) . . . 8_565 ?
C16 C15 Nb C16 -37.8(2) . . . 8_565 ?
C14 C15 Nb C16 115.9(3) . . . . ?
C14 C15 Nb C15 36.9(2) . . . 8_565 ?
C16 C15 Nb C15 -79.0(2) . . . 8_565 ?
C16 C15 Nb C14 -115.9(3) . . . . ?
C14 C15 Nb Ge -63.7(2) . . . . ?
C16 C15 Nb Ge -179.56(19) . . . . ?
C15 C14 Nb C18 -58.0(2) . . . . ?
C15 C14 Nb C18 58.0(2) 8_565 . . . ?
C15 C14 Nb C17 49.1(3) . . . . ?
C15 C14 Nb C17 165.0(2) 8_565 . . . ?
C15 C14 Nb C17 -165.0(2) . . . 8_565 ?
C15 C14 Nb C17 -49.1(3) 8_565 . . 8_565 ?
C15 C14 Nb C16 -78.7(3) . . . 8_565 ?
C15 C14 Nb C16 37.2(2) 8_565 . . 8_565 ?
C15 C14 Nb C16 -37.2(2) . . . . ?
C15 C14 Nb C16 78.7(3) 8_565 . . . ?
C15 C14 Nb C15 115.9(4) 8_565 . . . ?
C15 C14 Nb C15 -115.9(4) . . . 8_565 ?
C15 C14 Nb Ge 122.0(2) . . . . ?
C15 C14 Nb Ge -122.0(2) 8_565 . . . ?
C1 Ge Nb C18 180.0 . . . . ?
Cl Ge Nb C18 0.0 . . . . ?
C1 Ge Nb C17 122.49(9) . . . . ?
Cl Ge Nb C17 -57.51(9) . . . . ?
C1 Ge Nb C17 -122.49(9) . . . 8_565 ?
Cl Ge Nb C17 57.51(9) . . . 8_565 ?
C1 Ge Nb C16 -29.23(16) . . . 8_565 ?
Cl Ge Nb C16 150.77(16) . . . 8_565 ?
C1 Ge Nb C16 29.23(16) . . . . ?
Cl Ge Nb C16 -150.77(16) . . . . ?
C1 Ge Nb C15 29.63(10) . . . . ?
Cl Ge Nb C15 -150.37(10) . . . . ?
C1 Ge Nb C15 -29.63(10) . . . 8_565 ?
Cl Ge Nb C15 150.37(10) . . . 8_565 ?
C1 Ge Nb C14 0.0 . . . . ?
Cl Ge Nb C14 180.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_3697f
_database_code_depnum_ccdc_archive 'CCDC 1553389'
_audit_update_record             
;
2017-05-31 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_audit_creation_date             2014-09-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H52 Nb O2 P3 Si Sn, C7 H8'
_chemical_formula_sum            'C43 H60 Nb O2 P3 Si Sn'
_chemical_formula_weight         941.51
_chemical_absolute_configuration ?
_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'
Nb Nb -2.0727 0.6215 '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'
P P 0.1023 0.0942 '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'
Sn Sn -0.6537 1.4246 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5148(6)
_cell_length_b                   23.2579(16)
_cell_length_c                   12.0766(8)
_cell_angle_alpha                90
_cell_angle_beta                 108.779(2)
_cell_angle_gamma                90
_cell_volume                     2264.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   0.962
_shelx_estimated_absorpt_T_min   0.893
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5373
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.7202.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20515
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.725
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9665
_reflns_number_total             10697
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.403
_refine_diff_density_min         -2.852
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0703
_refine_ls_restrained_S_all      1.233
_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)+(0.0103P)²+27.6525P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1737
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_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. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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
Sn Sn 0.10520(11) 0.03511(4) 0.18745(7) 0.0190(2) Uani 1 1 d . . . . .
Nb Nb 0.04371(13) -0.03516(5) 0.01862(9) 0.0160(2) Uani 1 1 d . . . . .
P1 P 0.2635(4) -0.00733(16) -0.0803(3) 0.0202(7) Uani 1 1 d . . . . .
P2 P -0.0968(4) -0.09683(15) -0.1606(3) 0.0188(7) Uani 1 1 d . . . . .
P3 P 0.2323(4) -0.12253(16) 0.1028(3) 0.0172(7) Uani 1 1 d . . . . .
Si Si 0.2606(4) -0.13775(16) -0.1489(3) 0.0175(7) Uani 1 1 d . . . . .
O1 O -0.2308(14) -0.0922(6) 0.1163(9) 0.042(3) Uani 1 1 d . . . . .
O2 O -0.2246(17) 0.0590(5) -0.1209(10) 0.040(3) Uani 1 1 d . . . . .
C1 C 0.0714(16) 0.1004(6) 0.3029(11) 0.017(2) Uani 1 1 d . U . . .
C2 C 0.0612(15) 0.0837(6) 0.4157(11) 0.017(2) Uani 1 1 d . . . . .
C3 C 0.0569(18) 0.1267(6) 0.4938(11) 0.023(3) Uani 1 1 d . . . . .
H3 H 0.0516 0.1161 0.5686 0.028 Uiso 1 1 calc R . . . .
C4 C 0.060(2) 0.1835(7) 0.4677(12) 0.028(3) Uani 1 1 d . . . . .
H4 H 0.0556 0.2118 0.5234 0.033 Uiso 1 1 calc R . . . .
C5 C 0.0687(19) 0.2001(6) 0.3579(11) 0.024(3) Uani 1 1 d . . . . .
H5 H 0.0686 0.2397 0.3381 0.029 Uiso 1 1 calc R . . . .
C6 C 0.0778(15) 0.1578(6) 0.2786(11) 0.017(2) Uani 1 1 d . . . . .
C7 C 0.0502(16) 0.0213(5) 0.4379(10) 0.016(3) Uani 1 1 d . . . . .
C8 C -0.1070(16) -0.0058(6) 0.4044(12) 0.021(3) Uani 1 1 d . . . . .
C9 C -0.1121(19) -0.0652(7) 0.4143(11) 0.025(3) Uani 1 1 d . . . . .
H9 H -0.2173 -0.0836 0.3918 0.030 Uiso 1 1 calc R . . . .
C10 C 0.0286(19) -0.0987(6) 0.4553(12) 0.024(3) Uani 1 1 d . U . . .
C11 C 0.1806(17) -0.0711(7) 0.4894(11) 0.023(3) Uani 1 1 d . . . . .
H11 H 0.2785 -0.0936 0.5180 0.028 Uiso 1 1 calc R . . . .
C12 C 0.1960(16) -0.0117(6) 0.4834(10) 0.018(2) Uani 1 1 d . U . . .
C13 C -0.2631(17) 0.0286(8) 0.3574(16) 0.040(4) Uani 1 1 d . . . . .
H13A H -0.2650 0.0590 0.4131 0.060 Uiso 1 1 calc GR . . . .
H13B H -0.3593 0.0034 0.3455 0.060 Uiso 1 1 calc GR . . . .
H13C H -0.2670 0.0460 0.2826 0.060 Uiso 1 1 calc GR . . . .
C14 C 0.018(2) -0.1633(7) 0.4589(13) 0.036(4) Uani 1 1 d . . . . .
H14A H 0.0207 -0.1755 0.5372 0.054 Uiso 1 1 calc GR . . . .
H14B H 0.1128 -0.1802 0.4410 0.054 Uiso 1 1 calc GR . . . .
H14C H -0.0853 -0.1763 0.4011 0.054 Uiso 1 1 calc GR . . . .
C15 C 0.3643(17) 0.0163(6) 0.5177(13) 0.027(3) Uani 1 1 d . . . . .
H15A H 0.3742 0.0391 0.4520 0.041 Uiso 1 1 calc GR . . . .
H15B H 0.4505 -0.0134 0.5382 0.041 Uiso 1 1 calc GR . . . .
H15C H 0.3777 0.0415 0.5852 0.041 Uiso 1 1 calc GR . . . .
C16 C 0.0910(18) 0.1733(6) 0.1603(11) 0.020(3) Uani 1 1 d . . . . .
C17 C 0.2508(18) 0.1802(6) 0.1505(11) 0.021(3) Uani 1 1 d . . . . .
C18 C 0.261(2) 0.1922(6) 0.0393(14) 0.028(3) Uani 1 1 d . . . . .
H18 H 0.3674 0.1968 0.0312 0.034 Uiso 1 1 calc R . . . .
C19 C 0.124(2) 0.1975(6) -0.0584(13) 0.030(3) Uani 1 1 d . . . . .
C20 C -0.031(2) 0.1896(6) -0.0462(12) 0.028(3) Uani 1 1 d . . . . .
H20 H -0.1271 0.1927 -0.1131 0.034 Uiso 1 1 calc R . . . .
C21 C -0.0491(17) 0.1773(6) 0.0628(11) 0.019(3) Uani 1 1 d . . . . .
C22 C 0.4097(18) 0.1731(7) 0.2520(13) 0.031(3) Uani 1 1 d . . . . .
H22A H 0.3994 0.1932 0.3206 0.046 Uiso 1 1 calc GR . . . .
H22B H 0.5025 0.1894 0.2310 0.046 Uiso 1 1 calc GR . . . .
H22C H 0.4299 0.1322 0.2700 0.046 Uiso 1 1 calc GR . . . .
C23 C 0.140(3) 0.2099(8) -0.1771(14) 0.042(5) Uani 1 1 d . . . . .
H23A H 0.2055 0.2450 -0.1728 0.064 Uiso 1 1 calc GR . . . .
H23B H 0.0297 0.2151 -0.2345 0.064 Uiso 1 1 calc GR . . . .
H23C H 0.1959 0.1776 -0.2009 0.064 Uiso 1 1 calc GR . . . .
C24 C -0.2194(18) 0.1678(7) 0.0706(12) 0.025(3) Uani 1 1 d . . . . .
H24A H -0.2385 0.1265 0.0762 0.037 Uiso 1 1 calc GR . . . .
H24B H -0.3023 0.1834 0.0006 0.037 Uiso 1 1 calc GR . . . .
H24C H -0.2288 0.1873 0.1401 0.037 Uiso 1 1 calc GR . . . .
C25 C 0.3726(17) -0.0675(6) -0.1237(11) 0.022(3) Uani 1 1 d . . . . .
H25A H 0.4811 -0.0729 -0.0620 0.026 Uiso 1 1 calc R . . . .
H25B H 0.3951 -0.0565 -0.1964 0.026 Uiso 1 1 calc R . . . .
C26 C 0.4352(17) 0.0392(8) -0.0011(13) 0.033(3) Uani 1 1 d . . . . .
H26A H 0.3922 0.0771 0.0099 0.049 Uiso 1 1 calc GR . . . .
H26B H 0.5122 0.0433 -0.0459 0.049 Uiso 1 1 calc GR . . . .
H26C H 0.4936 0.0222 0.0754 0.049 Uiso 1 1 calc GR . . . .
C27 C 0.179(2) 0.0329(9) -0.2170(13) 0.037(3) Uani 1 1 d . . . . .
H27A H 0.0966 0.0094 -0.2742 0.056 Uiso 1 1 calc GR . . . .
H27B H 0.2695 0.0425 -0.2479 0.056 Uiso 1 1 calc GR . . . .
H27C H 0.1274 0.0684 -0.2021 0.056 Uiso 1 1 calc GR . . . .
C28 C 0.0383(15) -0.1248(6) -0.2393(10) 0.017(3) Uani 1 1 d . . . . .
H28A H 0.0365 -0.0974 -0.3024 0.021 Uiso 1 1 calc R . . . .
H28B H -0.0090 -0.1615 -0.2770 0.021 Uiso 1 1 calc R . . . .
C29 C -0.1917(17) -0.1630(7) -0.1328(13) 0.025(3) Uani 1 1 d . . . . .
H29A H -0.1048 -0.1908 -0.0943 0.037 Uiso 1 1 calc GR . . . .
H29B H -0.2628 -0.1790 -0.2071 0.037 Uiso 1 1 calc GR . . . .
H29C H -0.2587 -0.1548 -0.0822 0.037 Uiso 1 1 calc GR . . . .
C30 C -0.2664(18) -0.0645(7) -0.2787(11) 0.027(3) Uani 1 1 d . . . . .
H30A H -0.3567 -0.0537 -0.2489 0.041 Uiso 1 1 calc GR . . . .
H30B H -0.3075 -0.0923 -0.3425 0.041 Uiso 1 1 calc GR . . . .
H30C H -0.2258 -0.0301 -0.3078 0.041 Uiso 1 1 calc GR . . . .
C31 C 0.2735(16) -0.1721(6) -0.0045(12) 0.022(3) Uani 1 1 d . . . . .
H31A H 0.1928 -0.2041 -0.0195 0.026 Uiso 1 1 calc R . . . .
H31B H 0.3857 -0.1887 0.0304 0.026 Uiso 1 1 calc R . . . .
C32 C 0.1607(18) -0.1717(7) 0.1944(12) 0.027(3) Uani 1 1 d . . . . .
H32A H 0.1650 -0.1523 0.2674 0.040 Uiso 1 1 calc GR . . . .
H32B H 0.2325 -0.2057 0.2123 0.040 Uiso 1 1 calc GR . . . .
H32C H 0.0464 -0.1835 0.1527 0.040 Uiso 1 1 calc GR . . . .
C33 C 0.4429(18) -0.1072(7) 0.1986(12) 0.027(3) Uani 1 1 d . . . . .
H33A H 0.4982 -0.0816 0.1583 0.041 Uiso 1 1 calc GR . . . .
H33B H 0.5053 -0.1432 0.2188 0.041 Uiso 1 1 calc GR . . . .
H33C H 0.4380 -0.0885 0.2702 0.041 Uiso 1 1 calc GR . . . .
C34 C 0.3499(19) -0.1885(7) -0.2323(13) 0.028(3) Uani 1 1 d . . . . .
H34A H 0.3663 -0.1685 -0.2990 0.042 Uiso 1 1 calc GR . . . .
H34B H 0.2735 -0.2208 -0.2605 0.042 Uiso 1 1 calc GR . . . .
H34C H 0.4567 -0.2030 -0.1811 0.042 Uiso 1 1 calc GR . . . .
C35 C -0.1302(16) -0.0699(6) 0.0843(12) 0.022(3) Uani 1 1 d . U . . .
C36 C -0.1226(18) 0.0274(7) -0.0696(12) 0.027(3) Uani 1 1 d . . . . .
C37 C 0.508(2) 0.2522(8) 0.5625(13) 0.034(4) Uani 1 1 d . . . . .
C38 C 0.629(2) 0.2227(10) 0.5317(15) 0.043(4) Uani 1 1 d . . . . .
H38 H 0.6745 0.2391 0.4765 0.051 Uiso 1 1 calc R . . . .
C39 C 0.684(3) 0.1709(11) 0.579(2) 0.059(6) Uani 1 1 d . . . . .
H39 H 0.7601 0.1507 0.5513 0.070 Uiso 1 1 calc R . . . .
C40 C 0.637(3) 0.1469(11) 0.662(2) 0.070(8) Uani 1 1 d . . . . .
H40 H 0.6834 0.1113 0.6958 0.084 Uiso 1 1 calc R . . . .
C41 C 0.518(3) 0.1756(11) 0.6992(18) 0.063(7) Uani 1 1 d . . . . .
H41 H 0.4789 0.1590 0.7574 0.076 Uiso 1 1 calc R . . . .
C42 C 0.457(3) 0.2275(10) 0.6508(15) 0.050(5) Uani 1 1 d . . . . .
H42 H 0.3791 0.2473 0.6779 0.060 Uiso 1 1 calc R . . . .
C43 C 0.443(3) 0.3075(9) 0.5079(17) 0.051(5) Uani 1 1 d . . . . .
H43A H 0.5062 0.3390 0.5556 0.077 Uiso 1 1 calc GR . . . .
H43B H 0.3258 0.3110 0.5024 0.077 Uiso 1 1 calc GR . . . .
H43C H 0.4528 0.3093 0.4294 0.077 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
Sn Nb 2.5329(13) . ?
Sn C1 2.142(12) . ?
Nb P1 2.606(4) . ?
Nb P2 2.551(3) . ?
Nb P3 2.586(4) . ?
Nb C35 2.057(14) . ?
Nb C36 2.071(16) . ?
P1 C25 1.846(14) . ?
P1 C26 1.823(14) . ?
P1 C27 1.831(16) . ?
P2 C28 1.832(12) . ?
P2 C29 1.818(15) . ?
P2 C30 1.833(14) . ?
P3 C31 1.850(14) . ?
P3 C32 1.828(16) . ?
P3 C33 1.830(15) . ?
Si C25 1.867(14) . ?
Si C28 1.880(12) . ?
Si C31 1.888(14) . ?
Si C34 1.866(14) . ?
O1 C35 1.168(18) . ?
O2 C36 1.154(18) . ?
C1 C2 1.446(17) . ?
C1 C6 1.373(19) . ?
C2 C3 1.383(18) . ?
C2 C7 1.485(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.36(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.407(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(18) . ?
C6 C16 1.512(17) . ?
C7 C8 1.415(18) . ?
C7 C12 1.412(18) . ?
C8 C9 1.387(19) . ?
C8 C13 1.50(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.38(2) . ?
C10 C11 1.38(2) . ?
C10 C14 1.51(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.39(2) . ?
C12 C15 1.506(19) . ?
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 C17 1.41(2) . ?
C16 C21 1.383(19) . ?
C17 C18 1.400(19) . ?
C17 C22 1.513(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.37(2) . ?
C19 C20 1.38(2) . ?
C19 C23 1.511(19) . ?
C20 H20 0.9500 . ?
C20 C21 1.403(19) . ?
C21 C24 1.500(19) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C37 C38 1.39(3) . ?
C37 C42 1.40(2) . ?
C37 C43 1.47(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.35(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.31(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.41(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.37(3) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Sn Nb 160.9(3) . . ?
Sn Nb P1 102.47(9) . . ?
Sn Nb P2 164.77(9) . . ?
Sn Nb P3 104.44(8) . . ?
P2 Nb P1 87.74(11) . . ?
P2 Nb P3 87.36(11) . . ?
P3 Nb P1 85.91(12) . . ?
C35 Nb Sn 86.0(4) . . ?
C35 Nb P1 170.7(4) . . ?
C35 Nb P2 84.7(4) . . ?
C35 Nb P3 88.4(4) . . ?
C35 Nb C36 90.9(5) . . ?
C36 Nb Sn 83.7(4) . . ?
C36 Nb P1 93.6(4) . . ?
C36 Nb P2 84.4(4) . . ?
C36 Nb P3 171.7(4) . . ?
C25 P1 Nb 116.3(5) . . ?
C26 P1 Nb 118.7(5) . . ?
C26 P1 C25 101.9(7) . . ?
C26 P1 C27 100.6(9) . . ?
C27 P1 Nb 114.2(5) . . ?
C27 P1 C25 102.6(7) . . ?
C28 P2 Nb 116.0(4) . . ?
C28 P2 C30 102.2(6) . . ?
C29 P2 Nb 115.7(5) . . ?
C29 P2 C28 100.7(7) . . ?
C29 P2 C30 101.8(7) . . ?
C30 P2 Nb 117.8(5) . . ?
C31 P3 Nb 116.6(4) . . ?
C32 P3 Nb 116.4(5) . . ?
C32 P3 C31 102.1(7) . . ?
C32 P3 C33 100.9(7) . . ?
C33 P3 Nb 117.0(5) . . ?
C33 P3 C31 101.3(6) . . ?
C25 Si C28 108.7(6) . . ?
C25 Si C31 110.2(6) . . ?
C28 Si C31 110.6(6) . . ?
C34 Si C25 111.5(7) . . ?
C34 Si C28 107.3(6) . . ?
C34 Si C31 108.5(7) . . ?
C2 C1 Sn 119.0(9) . . ?
C6 C1 Sn 121.8(9) . . ?
C6 C1 C2 118.8(11) . . ?
C1 C2 C7 117.3(11) . . ?
C3 C2 C1 118.1(12) . . ?
C3 C2 C7 124.5(11) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.5(13) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(13) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 120.5 . . ?
C6 C5 C4 119.1(13) . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 121.7(12) . . ?
C1 C6 C16 117.0(11) . . ?
C5 C6 C16 121.3(12) . . ?
C8 C7 C2 119.5(12) . . ?
C12 C7 C2 120.2(11) . . ?
C12 C7 C8 120.1(12) . . ?
C7 C8 C13 120.8(13) . . ?
C9 C8 C7 118.1(14) . . ?
C9 C8 C13 121.0(14) . . ?
C8 C9 H9 118.5 . . ?
C10 C9 C8 123.0(15) . . ?
C10 C9 H9 118.5 . . ?
C9 C10 C11 117.7(14) . . ?
C9 C10 C14 121.5(15) . . ?
C11 C10 C14 120.8(14) . . ?
C10 C11 H11 118.7 . . ?
C10 C11 C12 122.7(14) . . ?
C12 C11 H11 118.7 . . ?
C7 C12 C15 120.8(12) . . ?
C11 C12 C7 118.3(13) . . ?
C11 C12 C15 120.8(12) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C6 118.2(12) . . ?
C21 C16 C6 120.9(12) . . ?
C21 C16 C17 120.7(11) . . ?
C16 C17 C22 123.6(12) . . ?
C18 C17 C16 117.4(13) . . ?
C18 C17 C22 119.0(13) . . ?
C17 C18 H18 118.5 . . ?
C19 C18 C17 123.1(14) . . ?
C19 C18 H18 118.5 . . ?
C18 C19 C20 118.1(13) . . ?
C18 C19 C23 121.3(16) . . ?
C20 C19 C23 120.5(15) . . ?
C19 C20 H20 119.2 . . ?
C19 C20 C21 121.5(14) . . ?
C21 C20 H20 119.2 . . ?
C16 C21 C20 119.1(13) . . ?
C16 C21 C24 121.5(12) . . ?
C20 C21 C24 119.3(12) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P1 C25 Si 115.6(7) . . ?
P1 C25 H25A 108.4 . . ?
P1 C25 H25B 108.4 . . ?
Si C25 H25A 108.4 . . ?
Si C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
P1 C26 H26A 109.5 . . ?
P1 C26 H26B 109.5 . . ?
P1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
P1 C27 H27A 109.5 . . ?
P1 C27 H27B 109.5 . . ?
P1 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
P2 C28 Si 116.0(6) . . ?
P2 C28 H28A 108.3 . . ?
P2 C28 H28B 108.3 . . ?
Si C28 H28A 108.3 . . ?
Si C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
P2 C29 H29A 109.5 . . ?
P2 C29 H29B 109.5 . . ?
P2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P2 C30 H30A 109.5 . . ?
P2 C30 H30B 109.5 . . ?
P2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
P3 C31 Si 114.6(8) . . ?
P3 C31 H31A 108.6 . . ?
P3 C31 H31B 108.6 . . ?
Si C31 H31A 108.6 . . ?
Si C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si C34 H34A 109.5 . . ?
Si C34 H34B 109.5 . . ?
Si C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O1 C35 Nb 175.8(12) . . ?
O2 C36 Nb 174.7(14) . . ?
C38 C37 C42 116.3(19) . . ?
C38 C37 C43 121.3(17) . . ?
C42 C37 C43 122.4(18) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.6(19) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 118.0 . . ?
C40 C39 C38 124(2) . . ?
C40 C39 H39 118.0 . . ?
C39 C40 H40 121.1 . . ?
C39 C40 C41 118(2) . . ?
C41 C40 H40 121.1 . . ?
C40 C41 H41 120.2 . . ?
C42 C41 C40 120(2) . . ?
C42 C41 H41 120.2 . . ?
C37 C42 H42 119.3 . . ?
C41 C42 C37 121(2) . . ?
C41 C42 H42 119.3 . . ?
C37 C43 H43A 109.5 . . ?
C37 C43 H43B 109.5 . . ?
C37 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 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
Sn C1 C2 C3 173.4(10) . . . . ?
Sn C1 C2 C7 -8.8(15) . . . . ?
Sn C1 C6 C5 -174.9(10) . . . . ?
Sn C1 C6 C16 6.6(16) . . . . ?
Nb P1 C25 Si 23.9(9) . . . . ?
Nb P2 C28 Si 29.2(9) . . . . ?
Nb P3 C31 Si 26.9(9) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C1 C2 C7 C8 -87.2(15) . . . . ?
C1 C2 C7 C12 87.8(14) . . . . ?
C1 C6 C16 C17 -91.5(15) . . . . ?
C1 C6 C16 C21 84.8(16) . . . . ?
C2 C1 C6 C5 -2.4(19) . . . . ?
C2 C1 C6 C16 179.1(11) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C2 C7 C8 C9 173.0(12) . . . . ?
C2 C7 C8 C13 -6(2) . . . . ?
C2 C7 C12 C11 -172.3(11) . . . . ?
C2 C7 C12 C15 4.1(18) . . . . ?
C3 C2 C7 C8 90.5(16) . . . . ?
C3 C2 C7 C12 -94.5(16) . . . . ?
C3 C4 C5 C6 -1(2) . . . . ?
C4 C5 C6 C1 3(2) . . . . ?
C4 C5 C6 C16 -178.8(13) . . . . ?
C5 C6 C16 C17 90.0(16) . . . . ?
C5 C6 C16 C21 -93.7(16) . . . . ?
C6 C1 C2 C3 0.6(18) . . . . ?
C6 C1 C2 C7 178.5(11) . . . . ?
C6 C16 C17 C18 177.4(12) . . . . ?
C6 C16 C17 C22 0(2) . . . . ?
C6 C16 C21 C20 -177.6(12) . . . . ?
C6 C16 C21 C24 1(2) . . . . ?
C7 C2 C3 C4 -176.9(14) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C8 C7 C12 C11 2.7(18) . . . . ?
C8 C7 C12 C15 179.1(12) . . . . ?
C8 C9 C10 C11 1(2) . . . . ?
C8 C9 C10 C14 -176.8(13) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C10 C11 C12 C7 -2(2) . . . . ?
C10 C11 C12 C15 -178.0(12) . . . . ?
C12 C7 C8 C9 -2.1(19) . . . . ?
C12 C7 C8 C13 179.3(13) . . . . ?
C13 C8 C9 C10 178.9(14) . . . . ?
C14 C10 C11 C12 177.6(13) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
C17 C16 C21 C20 -1(2) . . . . ?
C17 C16 C21 C24 177.6(13) . . . . ?
C17 C18 C19 C20 -1(2) . . . . ?
C17 C18 C19 C23 -179.4(14) . . . . ?
C18 C19 C20 C21 1(2) . . . . ?
C19 C20 C21 C16 0(2) . . . . ?
C19 C20 C21 C24 -178.6(13) . . . . ?
C21 C16 C17 C18 1(2) . . . . ?
C21 C16 C17 C22 -176.4(13) . . . . ?
C22 C17 C18 C19 177.9(14) . . . . ?
C23 C19 C20 C21 179.0(14) . . . . ?
C25 Si C28 P2 -79.0(9) . . . . ?
C25 Si C31 P3 45.3(9) . . . . ?
C26 P1 C25 Si 154.6(8) . . . . ?
C27 P1 C25 Si -101.5(9) . . . . ?
C28 Si C25 P1 45.4(9) . . . . ?
C28 Si C31 P3 -74.9(9) . . . . ?
C29 P2 C28 Si -96.5(8) . . . . ?
C30 P2 C28 Si 158.7(8) . . . . ?
C31 Si C25 P1 -75.9(9) . . . . ?
C31 Si C28 P2 42.1(10) . . . . ?
C32 P3 C31 Si 154.9(7) . . . . ?
C33 P3 C31 Si -101.2(8) . . . . ?
C34 Si C25 P1 163.5(7) . . . . ?
C34 Si C28 P2 160.3(8) . . . . ?
C34 Si C31 P3 167.7(7) . . . . ?
C37 C38 C39 C40 -5(3) . . . . ?
C38 C37 C42 C41 -4(3) . . . . ?
C38 C39 C40 C41 3(4) . . . . ?
C39 C40 C41 C42 -2(3) . . . . ?
C40 C41 C42 C37 2(3) . . . . ?
C42 C37 C38 C39 5(3) . . . . ?
C43 C37 C38 C39 -177.5(18) . . . . ?
C43 C37 C42 C41 178.9(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

#END---------------------------------------------------------------------------
####################################################################### 
# 
# 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_3550
_database_code_depnum_ccdc_archive 'CCDC 1553388'
_audit_update_record             
;
2017-05-31 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        DH-34-2
_chemical_formula_moiety         'C36 H52 Ge Nb O2 P3 Si, C4 H8 O'
_chemical_formula_sum            'C40 H60 Ge Nb O3 P3 Si'
_chemical_formula_weight         875.38
_chemical_absolute_configuration ad
_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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'
P P 0.1023 0.0942 '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'

_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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4180(3)
_cell_length_b                   22.9239(7)
_cell_length_c                   11.8653(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.5480(16)
_cell_angle_gamma                90
_cell_volume                     2183.14(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8273
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.662
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  0.8513
_exptl_absorpt_correction_T_min  0.7577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'R.H. Blessing, Acta Cryst. (1995), A51, 33-38'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8273
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.764
_diffrn_reflns_theta_full        25.247
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         2.530
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.549
_reflns_Friedel_fraction_full    0.557
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                5739
_reflns_number_total             6030
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 
;
 Flack x determined using 1950 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6030
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.026
_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)+(0.0326P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0675
_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 Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_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
Nb Nb -0.53773(5) -0.21708(2) -0.51004(3) 0.01486(10) Uani 1 1 d . . . . .
Ge Ge -0.59955(6) -0.28236(2) -0.67102(4) 0.01626(12) Uani 1 1 d . . . . .
P1 P -0.71032(15) -0.12540(5) -0.60015(10) 0.0166(3) Uani 1 1 d . . . . .
P2 P -0.39511(15) -0.15205(5) -0.33059(10) 0.0183(3) Uani 1 1 d . . . . .
P3 P -0.77040(16) -0.23808(5) -0.41141(11) 0.0189(3) Uani 1 1 d . . . . .
Si Si -0.75291(16) -0.10428(5) -0.34835(11) 0.0173(3) Uani 1 1 d . . . . .
O1 O -0.2998(5) -0.31650(15) -0.3534(3) 0.0363(10) Uani 1 1 d . . . . .
O2 O -0.2476(5) -0.16995(17) -0.6118(3) 0.0363(9) Uani 1 1 d . . . . .
C1 C -0.5833(6) -0.33959(17) -0.7901(4) 0.0157(9) Uani 1 1 d . . . . .
C2 C -0.6056(6) -0.39939(18) -0.7688(4) 0.0186(10) Uani 1 1 d . . . . .
C3 C -0.6054(6) -0.44002(19) -0.8553(4) 0.0255(11) Uani 1 1 d . . . . .
H3 H -0.6201 -0.4802 -0.8413 0.031 Uiso 1 1 calc R . . . .
C4 C -0.5843(8) -0.4231(2) -0.9615(5) 0.0318(13) Uani 1 1 d . . . . .
H4 H -0.5849 -0.4514 -1.0200 0.038 Uiso 1 1 calc R . . . .
C5 C -0.5623(7) -0.36447(19) -0.9826(4) 0.0252(11) Uani 1 1 d . . . . .
H5 H -0.5472 -0.3529 -1.0556 0.030 Uiso 1 1 calc R . . . .
C6 C -0.5621(6) -0.32293(18) -0.8983(4) 0.0177(10) Uani 1 1 d . . . . .
C7 C -0.6304(6) -0.41673(18) -0.6530(4) 0.0165(10) Uani 1 1 d . . . . .
C8 C -0.4898(6) -0.42417(18) -0.5529(4) 0.0192(10) Uani 1 1 d . . . . .
C9 C -0.5161(7) -0.43861(19) -0.4461(5) 0.0246(11) Uani 1 1 d . . . . .
H9 H -0.4223 -0.4439 -0.3784 0.030 Uiso 1 1 calc R . . . .
C10 C -0.6747(7) -0.4457(2) -0.4347(5) 0.0265(11) Uani 1 1 d . . . . .
C11 C -0.8106(7) -0.43761(18) -0.5347(4) 0.0237(11) Uani 1 1 d . . . . .
H11 H -0.9199 -0.4421 -0.5286 0.028 Uiso 1 1 calc R . . . .
C12 C -0.7906(6) -0.42310(18) -0.6443(4) 0.0209(10) Uani 1 1 d . . . . .
C13 C -0.3171(6) -0.4150(2) -0.5599(5) 0.0253(11) Uani 1 1 d . . . . .
H13A H -0.3038 -0.4360 -0.6284 0.038 Uiso 1 1 calc GR . . . .
H13B H -0.2363 -0.4298 -0.4877 0.038 Uiso 1 1 calc GR . . . .
H13C H -0.2981 -0.3733 -0.5682 0.038 Uiso 1 1 calc GR . . . .
C14 C -0.7008(8) -0.4603(2) -0.3181(5) 0.0399(15) Uani 1 1 d . . . . .
H14A H -0.5926 -0.4662 -0.2585 0.060 Uiso 1 1 calc GR . . . .
H14B H -0.7671 -0.4961 -0.3263 0.060 Uiso 1 1 calc GR . . . .
H14C H -0.7599 -0.4282 -0.2936 0.060 Uiso 1 1 calc GR . . . .
C15 C -0.9409(7) -0.4114(2) -0.7488(5) 0.0302(12) Uani 1 1 d . . . . .
H15A H -0.9366 -0.3712 -0.7760 0.045 Uiso 1 1 calc GR . . . .
H15B H -1.0423 -0.4168 -0.7256 0.045 Uiso 1 1 calc GR . . . .
H15C H -0.9418 -0.4385 -0.8128 0.045 Uiso 1 1 calc GR . . . .
C16 C -0.5358(6) -0.25951(18) -0.9185(4) 0.0170(10) Uani 1 1 d . . . . .
C17 C -0.3745(7) -0.23752(19) -0.8923(4) 0.0230(11) Uani 1 1 d . . . . .
C18 C -0.3521(7) -0.1778(2) -0.9071(4) 0.0286(13) Uani 1 1 d . . . . .
H18 H -0.2422 -0.1628 -0.8896 0.034 Uiso 1 1 calc R . . . .
C19 C -0.4857(8) -0.14015(19) -0.9463(4) 0.0284(12) Uani 1 1 d . . . . .
C20 C -0.6443(7) -0.1630(2) -0.9734(4) 0.0262(12) Uani 1 1 d . . . . .
H20 H -0.7369 -0.1375 -1.0018 0.031 Uiso 1 1 calc R . . . .
C21 C -0.6735(6) -0.2223(2) -0.9606(4) 0.0205(9) Uani 1 1 d . . . . .
C22 C -0.2260(7) -0.2767(2) -0.8447(5) 0.0347(12) Uani 1 1 d . . . . .
H22A H -0.2359 -0.2973 -0.7748 0.052 Uiso 1 1 calc GR . . . .
H22B H -0.1241 -0.2532 -0.8229 0.052 Uiso 1 1 calc GR . . . .
H22C H -0.2213 -0.3051 -0.9054 0.052 Uiso 1 1 calc GR . . . .
C23 C -0.4561(9) -0.0752(2) -0.9544(5) 0.0419(16) Uani 1 1 d . . . . .
H23A H -0.4367 -0.0574 -0.8763 0.063 Uiso 1 1 calc GR . . . .
H23B H -0.5540 -0.0573 -1.0105 0.063 Uiso 1 1 calc GR . . . .
H23C H -0.3584 -0.0690 -0.9816 0.063 Uiso 1 1 calc GR . . . .
C24 C -0.8488(6) -0.2449(2) -0.9889(5) 0.0294(12) Uani 1 1 d . . . . .
H24A H -0.8708 -0.2720 -1.0557 0.044 Uiso 1 1 calc GR . . . .
H24B H -0.9272 -0.2122 -1.0097 0.044 Uiso 1 1 calc GR . . . .
H24C H -0.8627 -0.2652 -0.9199 0.044 Uiso 1 1 calc GR . . . .
C25 C -0.7541(6) -0.07310(19) -0.4950(4) 0.0214(11) Uani 1 1 d . . . . .
H25A H -0.8647 -0.0553 -0.5325 0.026 Uiso 1 1 calc R . . . .
H25B H -0.6704 -0.0414 -0.4807 0.026 Uiso 1 1 calc R . . . .
C26 C -0.9176(6) -0.1368(2) -0.7050(4) 0.0255(11) Uani 1 1 d . . . . .
H26A H -0.9084 -0.1614 -0.7704 0.038 Uiso 1 1 calc GR . . . .
H26B H -0.9662 -0.0991 -0.7361 0.038 Uiso 1 1 calc GR . . . .
H26C H -0.9892 -0.1561 -0.6648 0.038 Uiso 1 1 calc GR . . . .
C27 C -0.6191(7) -0.0785(2) -0.6889(4) 0.0265(12) Uani 1 1 d . . . . .
H27A H -0.5120 -0.0633 -0.6393 0.040 Uiso 1 1 calc GR . . . .
H27B H -0.6947 -0.0460 -0.7208 0.040 Uiso 1 1 calc GR . . . .
H27C H -0.6017 -0.1012 -0.7542 0.040 Uiso 1 1 calc GR . . . .
C28 C -0.5339(6) -0.1193(2) -0.2538(4) 0.0207(10) Uani 1 1 d . . . . .
H28A H -0.4838 -0.0822 -0.2174 0.025 Uiso 1 1 calc R . . . .
H28B H -0.5386 -0.1458 -0.1889 0.025 Uiso 1 1 calc R . . . .
C29 C -0.2340(6) -0.1842(2) -0.2088(5) 0.0319(12) Uani 1 1 d . . . . .
H29A H -0.2830 -0.2144 -0.1713 0.048 Uiso 1 1 calc GR . . . .
H29B H -0.1838 -0.1539 -0.1507 0.048 Uiso 1 1 calc GR . . . .
H29C H -0.1481 -0.2015 -0.2386 0.048 Uiso 1 1 calc GR . . . .
C30 C -0.2882(6) -0.0876(2) -0.3614(5) 0.0280(12) Uani 1 1 d . . . . .
H30A H -0.2056 -0.0994 -0.4001 0.042 Uiso 1 1 calc GR . . . .
H30B H -0.2320 -0.0675 -0.2871 0.042 Uiso 1 1 calc GR . . . .
H30C H -0.3695 -0.0612 -0.4134 0.042 Uiso 1 1 calc GR . . . .
C31 C -0.8757(6) -0.17373(19) -0.3715(4) 0.0217(10) Uani 1 1 d . . . . .
H31A H -0.9036 -0.1828 -0.2981 0.026 Uiso 1 1 calc R . . . .
H31B H -0.9818 -0.1673 -0.4349 0.026 Uiso 1 1 calc R . . . .
C32 C -0.7021(7) -0.2777(2) -0.2716(5) 0.0348(13) Uani 1 1 d . . . . .
H32A H -0.6494 -0.3145 -0.2831 0.052 Uiso 1 1 calc GR . . . .
H32B H -0.7986 -0.2861 -0.2442 0.052 Uiso 1 1 calc GR . . . .
H32C H -0.6218 -0.2540 -0.2125 0.052 Uiso 1 1 calc GR . . . .
C33 C -0.9471(6) -0.2829(2) -0.4934(5) 0.0314(12) Uani 1 1 d . . . . .
H33A H -1.0089 -0.2626 -0.5661 0.047 Uiso 1 1 calc GR . . . .
H33B H -1.0208 -0.2896 -0.4446 0.047 Uiso 1 1 calc GR . . . .
H33C H -0.9065 -0.3204 -0.5133 0.047 Uiso 1 1 calc GR . . . .
C34 C -0.8426(6) -0.0497(2) -0.2667(4) 0.0235(11) Uani 1 1 d . . . . .
H34A H -0.7628 -0.0178 -0.2384 0.035 Uiso 1 1 calc GR . . . .
H34B H -0.8652 -0.0687 -0.1992 0.035 Uiso 1 1 calc GR . . . .
H34C H -0.9465 -0.0339 -0.3198 0.035 Uiso 1 1 calc GR . . . .
C35 C -0.3889(6) -0.2820(2) -0.4127(4) 0.0255(11) Uani 1 1 d . . . . .
C36 C -0.3518(6) -0.1882(2) -0.5768(4) 0.0219(10) Uani 1 1 d . . . . .
O3 O -0.0123(7) -0.4787(2) -0.1598(5) 0.0772(16) Uani 1 1 d . . . . .
C37 C -0.0350(10) -0.4156(3) -0.1708(8) 0.066(2) Uani 1 1 d . . . . .
H37A H -0.0906 -0.4048 -0.2542 0.079 Uiso 1 1 calc R . . . .
H37B H 0.0740 -0.3955 -0.1438 0.079 Uiso 1 1 calc R . . . .
C38 C -0.1406(13) -0.3990(3) -0.0952(7) 0.079(3) Uani 1 1 d . . . . .
H38A H -0.0751 -0.3767 -0.0251 0.094 Uiso 1 1 calc R . . . .
H38B H -0.2366 -0.3750 -0.1402 0.094 Uiso 1 1 calc R . . . .
C39 C -0.1979(9) -0.4555(4) -0.0593(6) 0.065(2) Uani 1 1 d . . . . .
H39A H -0.2086 -0.4530 0.0214 0.078 Uiso 1 1 calc R . . . .
H39B H -0.3068 -0.4671 -0.1149 0.078 Uiso 1 1 calc R . . . .
C40 C -0.0675(10) -0.4971(3) -0.0632(6) 0.0573(19) Uani 1 1 d . . . . .
H40A H 0.0254 -0.4962 0.0115 0.069 Uiso 1 1 calc R . . . .
H40B H -0.1126 -0.5373 -0.0763 0.069 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
Nb Ge 2.3579(6) . ?
Nb P1 2.5952(12) . ?
Nb P2 2.5798(12) . ?
Nb P3 2.6115(13) . ?
Nb C35 2.060(5) . ?
Nb C36 2.065(5) . ?
Ge C1 1.963(4) . ?
P1 C25 1.846(4) . ?
P1 C26 1.831(5) . ?
P1 C27 1.828(5) . ?
P2 C28 1.844(5) . ?
P2 C29 1.813(5) . ?
P2 C30 1.824(5) . ?
P3 C31 1.854(4) . ?
P3 C32 1.826(5) . ?
P3 C33 1.828(5) . ?
Si C25 1.878(5) . ?
Si C28 1.879(5) . ?
Si C31 1.873(5) . ?
Si C34 1.876(5) . ?
O1 C35 1.168(6) . ?
O2 C36 1.155(6) . ?
C1 C2 1.417(6) . ?
C1 C6 1.401(6) . ?
C2 C3 1.387(6) . ?
C2 C7 1.504(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(7) . ?
C6 C16 1.501(6) . ?
C7 C8 1.412(7) . ?
C7 C12 1.391(6) . ?
C8 C9 1.390(6) . ?
C8 C13 1.495(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(7) . ?
C10 C11 1.390(7) . ?
C10 C14 1.503(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(7) . ?
C12 C15 1.505(7) . ?
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 C17 1.393(7) . ?
C16 C21 1.405(6) . ?
C17 C18 1.399(6) . ?
C17 C22 1.504(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.383(8) . ?
C19 C20 1.378(8) . ?
C19 C23 1.517(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.398(7) . ?
C21 C24 1.504(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O3 C37 1.458(8) . ?
O3 C40 1.425(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.491(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.490(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.466(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 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
Ge Nb P1 102.76(3) . . ?
Ge Nb P2 165.81(3) . . ?
Ge Nb P3 103.52(3) . . ?
P1 Nb P3 86.08(4) . . ?
P2 Nb P1 86.30(4) . . ?
P2 Nb P3 87.82(4) . . ?
C35 Nb Ge 86.81(13) . . ?
C35 Nb P1 170.43(13) . . ?
C35 Nb P2 84.34(13) . . ?
C35 Nb P3 91.56(13) . . ?
C35 Nb C36 92.49(19) . . ?
C36 Nb Ge 84.28(13) . . ?
C36 Nb P1 88.70(13) . . ?
C36 Nb P2 85.03(13) . . ?
C36 Nb P3 171.40(13) . . ?
C1 Ge Nb 163.97(14) . . ?
C25 P1 Nb 116.65(15) . . ?
C26 P1 Nb 117.68(16) . . ?
C26 P1 C25 102.0(2) . . ?
C27 P1 Nb 115.67(17) . . ?
C27 P1 C25 102.2(2) . . ?
C27 P1 C26 99.9(2) . . ?
C28 P2 Nb 115.87(16) . . ?
C29 P2 Nb 118.26(17) . . ?
C29 P2 C28 101.8(2) . . ?
C29 P2 C30 101.1(3) . . ?
C30 P2 Nb 115.97(17) . . ?
C30 P2 C28 101.2(2) . . ?
C31 P3 Nb 116.65(15) . . ?
C32 P3 Nb 115.20(18) . . ?
C32 P3 C31 102.0(2) . . ?
C32 P3 C33 100.7(3) . . ?
C33 P3 Nb 117.73(16) . . ?
C33 P3 C31 102.0(2) . . ?
C25 Si C28 110.7(2) . . ?
C31 Si C25 109.8(2) . . ?
C31 Si C28 109.3(2) . . ?
C31 Si C34 110.7(2) . . ?
C34 Si C25 109.5(2) . . ?
C34 Si C28 106.8(2) . . ?
C2 C1 Ge 118.5(3) . . ?
C6 C1 Ge 122.2(3) . . ?
C6 C1 C2 119.2(4) . . ?
C1 C2 C7 118.8(4) . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 C7 122.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(4) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.5(4) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C16 118.5(4) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 C16 121.3(4) . . ?
C8 C7 C2 119.2(4) . . ?
C12 C7 C2 120.0(4) . . ?
C12 C7 C8 120.7(4) . . ?
C7 C8 C13 121.2(4) . . ?
C9 C8 C7 118.1(4) . . ?
C9 C8 C13 120.6(5) . . ?
C8 C9 H9 118.7 . . ?
C8 C9 C10 122.5(5) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C14 121.8(5) . . ?
C11 C10 C9 117.9(5) . . ?
C11 C10 C14 120.3(5) . . ?
C10 C11 H11 119.2 . . ?
C10 C11 C12 121.7(5) . . ?
C12 C11 H11 119.2 . . ?
C7 C12 C11 119.0(5) . . ?
C7 C12 C15 120.9(4) . . ?
C11 C12 C15 120.0(4) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C6 119.7(4) . . ?
C17 C16 C21 120.3(4) . . ?
C21 C16 C6 120.0(4) . . ?
C16 C17 C18 119.0(5) . . ?
C16 C17 C22 120.8(4) . . ?
C18 C17 C22 120.2(5) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.8(5) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C23 120.1(5) . . ?
C20 C19 C18 118.3(4) . . ?
C20 C19 C23 121.6(5) . . ?
C19 C20 H20 118.9 . . ?
C19 C20 C21 122.2(5) . . ?
C21 C20 H20 118.9 . . ?
C16 C21 C24 121.3(4) . . ?
C20 C21 C16 118.4(5) . . ?
C20 C21 C24 120.3(4) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P1 C25 Si 115.6(2) . . ?
P1 C25 H25A 108.4 . . ?
P1 C25 H25B 108.4 . . ?
Si C25 H25A 108.4 . . ?
Si C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
P1 C26 H26A 109.5 . . ?
P1 C26 H26B 109.5 . . ?
P1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
P1 C27 H27A 109.5 . . ?
P1 C27 H27B 109.5 . . ?
P1 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
P2 C28 Si 115.7(2) . . ?
P2 C28 H28A 108.4 . . ?
P2 C28 H28B 108.4 . . ?
Si C28 H28A 108.4 . . ?
Si C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
P2 C29 H29A 109.5 . . ?
P2 C29 H29B 109.5 . . ?
P2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P2 C30 H30A 109.5 . . ?
P2 C30 H30B 109.5 . . ?
P2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
P3 C31 Si 115.4(2) . . ?
P3 C31 H31A 108.4 . . ?
P3 C31 H31B 108.4 . . ?
Si C31 H31A 108.4 . . ?
Si C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si C34 H34A 109.5 . . ?
Si C34 H34B 109.5 . . ?
Si C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O1 C35 Nb 176.4(4) . . ?
O2 C36 Nb 177.2(4) . . ?
C40 O3 C37 107.5(5) . . ?
O3 C37 H37A 110.4 . . ?
O3 C37 H37B 110.4 . . ?
O3 C37 C38 106.6(6) . . ?
H37A C37 H37B 108.6 . . ?
C38 C37 H37A 110.4 . . ?
C38 C37 H37B 110.4 . . ?
C37 C38 H38A 110.8 . . ?
C37 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?
C39 C38 C37 104.6(6) . . ?
C39 C38 H38A 110.8 . . ?
C39 C38 H38B 110.8 . . ?
C38 C39 H39A 110.9 . . ?
C38 C39 H39B 110.9 . . ?
H39A C39 H39B 108.9 . . ?
C40 C39 C38 104.3(6) . . ?
C40 C39 H39A 110.9 . . ?
C40 C39 H39B 110.9 . . ?
O3 C40 C39 105.2(6) . . ?
O3 C40 H40A 110.7 . . ?
O3 C40 H40B 110.7 . . ?
C39 C40 H40A 110.7 . . ?
C39 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?

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
Nb P1 C25 Si -25.0(3) . . . . ?
Nb P2 C28 Si -29.7(3) . . . . ?
Nb P3 C31 Si -23.9(3) . . . . ?
Ge C1 C2 C3 175.8(4) . . . . ?
Ge C1 C2 C7 -3.6(6) . . . . ?
Ge C1 C6 C5 -175.7(4) . . . . ?
Ge C1 C6 C16 5.5(6) . . . . ?
C1 C2 C3 C4 -0.1(8) . . . . ?
C1 C2 C7 C8 -83.3(5) . . . . ?
C1 C2 C7 C12 94.3(5) . . . . ?
C1 C6 C16 C17 93.2(6) . . . . ?
C1 C6 C16 C21 -85.0(6) . . . . ?
C2 C1 C6 C5 -0.2(7) . . . . ?
C2 C1 C6 C16 -179.0(4) . . . . ?
C2 C3 C4 C5 0.2(9) . . . . ?
C2 C7 C8 C9 178.2(4) . . . . ?
C2 C7 C8 C13 0.1(6) . . . . ?
C2 C7 C12 C11 -178.2(4) . . . . ?
C2 C7 C12 C15 -1.6(6) . . . . ?
C3 C2 C7 C8 97.4(6) . . . . ?
C3 C2 C7 C12 -85.0(6) . . . . ?
C3 C4 C5 C6 -0.3(9) . . . . ?
C4 C5 C6 C1 0.3(8) . . . . ?
C4 C5 C6 C16 179.0(5) . . . . ?
C5 C6 C16 C17 -85.5(6) . . . . ?
C5 C6 C16 C21 96.3(6) . . . . ?
C6 C1 C2 C3 0.1(7) . . . . ?
C6 C1 C2 C7 -179.3(4) . . . . ?
C6 C16 C17 C18 -177.4(4) . . . . ?
C6 C16 C17 C22 0.5(7) . . . . ?
C6 C16 C21 C20 177.2(4) . . . . ?
C6 C16 C21 C24 -1.5(7) . . . . ?
C7 C2 C3 C4 179.2(5) . . . . ?
C7 C8 C9 C10 -0.2(6) . . . . ?
C8 C7 C12 C11 -0.6(6) . . . . ?
C8 C7 C12 C15 176.0(4) . . . . ?
C8 C9 C10 C11 -0.2(7) . . . . ?
C8 C9 C10 C14 -179.0(4) . . . . ?
C9 C10 C11 C12 0.3(7) . . . . ?
C10 C11 C12 C7 0.1(6) . . . . ?
C10 C11 C12 C15 -176.5(4) . . . . ?
C12 C7 C8 C9 0.7(6) . . . . ?
C12 C7 C8 C13 -177.4(4) . . . . ?
C13 C8 C9 C10 177.9(4) . . . . ?
C14 C10 C11 C12 179.1(4) . . . . ?
C16 C17 C18 C19 0.3(7) . . . . ?
C17 C16 C21 C20 -1.0(7) . . . . ?
C17 C16 C21 C24 -179.7(4) . . . . ?
C17 C18 C19 C20 -1.3(7) . . . . ?
C17 C18 C19 C23 176.5(5) . . . . ?
C18 C19 C20 C21 1.1(7) . . . . ?
C19 C20 C21 C16 0.0(7) . . . . ?
C19 C20 C21 C24 178.7(4) . . . . ?
C21 C16 C17 C18 0.9(7) . . . . ?
C21 C16 C17 C22 178.7(4) . . . . ?
C22 C17 C18 C19 -177.5(4) . . . . ?
C23 C19 C20 C21 -176.7(4) . . . . ?
C25 Si C28 P2 -41.7(3) . . . . ?
C25 Si C31 P3 75.7(3) . . . . ?
C26 P1 C25 Si 104.6(3) . . . . ?
C27 P1 C25 Si -152.3(3) . . . . ?
C28 Si C25 P1 74.3(3) . . . . ?
C28 Si C31 P3 -45.9(3) . . . . ?
C29 P2 C28 Si -159.4(3) . . . . ?
C30 P2 C28 Si 96.6(3) . . . . ?
C31 Si C25 P1 -46.5(3) . . . . ?
C31 Si C28 P2 79.3(3) . . . . ?
C32 P3 C31 Si 102.6(3) . . . . ?
C33 P3 C31 Si -153.6(3) . . . . ?
C34 Si C25 P1 -168.2(3) . . . . ?
C34 Si C28 P2 -160.9(3) . . . . ?
C34 Si C31 P3 -163.3(3) . . . . ?
O3 C37 C38 C39 -9.3(9) . . . . ?
C37 O3 C40 C39 29.7(8) . . . . ?
C37 C38 C39 C40 26.8(8) . . . . ?
C38 C39 C40 O3 -35.1(8) . . . . ?
C40 O3 C37 C38 -12.5(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
