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

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

data_Ta_calix
_database_code_depnum_ccdc_archive 'CCDC 1043647'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;


_vrf_CHEMW03_Ta_calix            
;
RESPONSE: SQUEEZE was employed to model disordered solvent. Formula quoted 
includes this solvent.
;

_vrf_PLAT041_Ta_calix            
;
RESPONSE: SQUEEZE was employed to model disordered solvent. Formula quoted 
includes this solvent.
;

_vrf_PLAT068_Ta_calix            
;
RESPONSE: SQUEEZE was employed to model disordered solvent. Formula quoted 
includes this solvent. F000 is thus different from that calculated from the 
atom list. 
;


_vrf_PLAT242_Ta_calix            
;
RESPONSE: This is a false alert for a tertiary butyl group. The central atom 
has a much smaller displacement parameter than the attached methyl groups. 

Note that The tantalum is much heavier than the attached to it and thus has a
smaller diaplacement parameter.  Similarly, the central carbon atoms of 
tBu groups have much smaller displacements than those of the methyl groups.    
;


_vrf_PLAT342_Ta_calix            
;
RESPONSE: The crystal examined was twinned. The bond precision is less than 
would be ideal, but there is no serious problem with this structure. Note 
that the presence of peripheral tertiary butyl groups leads to moderate
C-C bond precision.      
;



_vrf_PLAT220_Ta_calix            
;
RESPONSE: The tetraphenolate core is well determined and the atoms there have 
small displacement parameters. Peripheral tertiary butyl groups have much larger
displacement parameters. This explains the range of values for displacement 
parameters for carbon and also for hydrogen atoms. 

;

_vrf_PLAT222_Ta_calix            
;
RESPONSE: The tetraphenolate core is well determined and the atoms there have 
small displacement parameters. Peripheral tertiary butyl groups have much larger
displacement parameters. This explains the range of values for displacement 
parameters for carbon and also for hydrogen atoms. 
;

_vrf_PLAT234_Ta_calix            
;
RESPONSE: The nitrogen is bound to one of the tantalum ions and has a small
displacement parameter. The carbon chain attached is much freer to move. This
gives rise to this alert. 

;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C72 H102 Cl4 N2 O6 Ta2, 5(C2 H3 N)
;

_chemical_formula_sum            'C82 H117 Cl4 N7 O6 Ta2'
_chemical_formula_weight         1800.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

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

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

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

_cell_length_a                   12.6367(8)
_cell_length_b                   16.8848(11)
_cell_length_c                   21.6085(14)
_cell_angle_alpha                87.781(5)
_cell_angle_beta                 87.412(5)
_cell_angle_gamma                73.944(5)
_cell_volume                     4424.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    23092
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      27.85

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             1840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.643
_shelx_estimated_absorpt_T_min   0.458
_shelx_estimated_absorpt_T_max   0.620
_exptl_absorpt_correction_type   Analytical
_exptl_absorpt_correction_T_min  0.4120
_exptl_absorpt_correction_T_max  0.6243
_exptl_absorpt_process_details   
;
TwinAbs (Stoe X-AREA suite)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            93502
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.550
_diffrn_reflns_theta_max         25.512
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             40462
_reflns_number_gt                26933
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Stoe X-AREA'
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_solution    'Sir92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Twin, SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1501P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         40462
_refine_ls_number_parameters     862
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2258
_refine_ls_wR_factor_gt          0.2159
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_restrained_S_all      0.940
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.19863(4) 1.15733(3) 0.03210(2) 0.03917(16) Uani 1 1 d . . . . .
O1 O 0.3043(6) 1.1426(5) 0.0933(4) 0.040(2) Uani 1 1 d . . . . .
O2 O 0.0816(7) 1.1859(5) 0.0902(4) 0.0383(19) Uani 1 1 d . . . . .
O5 O 0.2022(7) 1.2614(5) 0.0050(4) 0.051(2) Uani 1 1 d . . . . .
C65 C 0.1998(15) 1.3160(9) -0.0492(7) 0.069(5) Uani 1 1 d . . . . .
H65A H 0.1299 1.3236 -0.0706 0.082 Uiso 1 1 calc R U . . .
H65B H 0.2614 1.2908 -0.0785 0.082 Uiso 1 1 calc R U . . .
C66 C 0.2097(18) 1.3967(10) -0.0304(9) 0.093(6) Uani 1 1 d . . . . .
H66A H 0.2081 1.4328 -0.0672 0.139 Uiso 1 1 calc R U . . .
H66B H 0.1482 1.4218 -0.0019 0.139 Uiso 1 1 calc R U . . .
H66C H 0.2795 1.3890 -0.0098 0.139 Uiso 1 1 calc R U . . .
N1 N 0.3441(9) 1.1183(7) -0.0366(5) 0.049(3) Uani 1 1 d . . . . .
C67 C 0.214(2) 0.3638(11) 0.2128(10) 0.097(7) Uani 1 1 d . . . . .
H67A H 0.1798 0.3560 0.1740 0.117 Uiso 1 1 calc R U . . .
H67B H 0.2941 0.3374 0.2077 0.117 Uiso 1 1 calc R U . . .
C68 C 0.1722(17) 0.3215(10) 0.2612(11) 0.102(7) Uani 1 1 d . . . . .
H68A H 0.1881 0.2631 0.2513 0.154 Uiso 1 1 calc R U . . .
H68B H 0.2071 0.3267 0.2998 0.154 Uiso 1 1 calc R U . . .
H68C H 0.0923 0.3453 0.2660 0.154 Uiso 1 1 calc R U . . .
Ta2 Ta 0.20574(5) 0.55120(4) 0.19142(3) 0.0565(2) Uani 1 1 d . . . . .
O3 O 0.2999(8) 0.5696(5) 0.2535(5) 0.056(3) Uani 1 1 d . . . . .
O4 O 0.0804(7) 0.6165(5) 0.2348(4) 0.046(2) Uani 1 1 d . . . . .
O6 O 0.1981(9) 0.4489(6) 0.2195(6) 0.077(4) Uani 1 1 d . . . . .
C69 C 0.4162(12) 1.0955(9) -0.0684(7) 0.053(3) Uani 1 1 d . . . . .
C70 C 0.5116(14) 1.0645(10) -0.1108(8) 0.073(5) Uani 1 1 d . . . . .
H70A H 0.4930 1.0301 -0.1418 0.109 Uiso 1 1 calc R U . . .
H70B H 0.5741 1.0317 -0.0873 0.109 Uiso 1 1 calc R U . . .
H70C H 0.5316 1.1112 -0.1318 0.109 Uiso 1 1 calc R U . . .
N2 N 0.2183(12) 0.6686(8) 0.1361(6) 0.067(4) Uani 1 1 d . . . . .
C71 C 0.2144(15) 0.7296(12) 0.1110(8) 0.070(5) Uani 1 1 d . . . . .
C72 C 0.2095(15) 0.8096(12) 0.0803(8) 0.079(5) Uani 1 1 d . . . . .
H72A H 0.2108 0.8498 0.1116 0.118 Uiso 1 1 calc R U . . .
H72B H 0.1414 0.8286 0.0575 0.118 Uiso 1 1 calc R U . . .
H72C H 0.2731 0.8037 0.0515 0.118 Uiso 1 1 calc R U . . .
C1 C 0.3404(10) 1.1350(7) 0.1533(6) 0.037(3) Uani 1 1 d . . . . .
C2 C 0.2841(9) 1.0983(7) 0.1989(5) 0.035(3) Uani 1 1 d . . . . .
C3 C 0.3192(10) 1.0901(7) 0.2594(6) 0.039(3) Uani 1 1 d . . . . .
H3 H 0.2800 1.0668 0.2903 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4087(10) 1.1146(8) 0.2761(6) 0.042(3) Uani 1 1 d . . . . .
C5 C 0.4638(10) 1.1503(8) 0.2294(7) 0.046(3) Uani 1 1 d . . . . .
H5 H 0.5256 1.1677 0.2405 0.055 Uiso 1 1 calc R U . . .
C6 C 0.4325(10) 1.1615(7) 0.1678(6) 0.040(3) Uani 1 1 d . . . . .
C7 C 0.4506(12) 1.1025(9) 0.3427(7) 0.055(4) Uani 1 1 d . . . . .
C8 C 0.382(2) 1.0638(17) 0.3857(9) 0.115(9) Uani 1 1 d . . . . .
H8A H 0.3795 1.0112 0.3693 0.172 Uiso 1 1 calc R U . . .
H8B H 0.4147 1.0543 0.4266 0.172 Uiso 1 1 calc R U . . .
H8C H 0.3073 1.1007 0.3895 0.172 Uiso 1 1 calc R U . . .
C9 C 0.5655(18) 1.0414(15) 0.3405(10) 0.108(7) Uani 1 1 d . . . . .
H9A H 0.5610 0.9889 0.3245 0.162 Uiso 1 1 calc R U . . .
H9B H 0.6149 1.0639 0.3133 0.162 Uiso 1 1 calc R U . . .
H9C H 0.5942 1.0323 0.3824 0.162 Uiso 1 1 calc R U . . .
C10 C 0.456(2) 1.1821(15) 0.3667(10) 0.122(9) Uani 1 1 d . . . . .
H10A H 0.5008 1.2067 0.3381 0.183 Uiso 1 1 calc R U . . .
H10B H 0.3810 1.2193 0.3704 0.183 Uiso 1 1 calc R U . . .
H10C H 0.4885 1.1729 0.4075 0.183 Uiso 1 1 calc R U . . .
C11 C 0.4986(11) 1.1986(9) 0.1182(7) 0.054(4) Uani 1 1 d . . . . .
C12 C 0.5589(12) 1.1331(11) 0.0742(7) 0.063(4) Uani 1 1 d . . . . .
H12A H 0.5059 1.1099 0.0547 0.095 Uiso 1 1 calc R U . . .
H12B H 0.5987 1.1573 0.0421 0.095 Uiso 1 1 calc R U . . .
H12C H 0.6115 1.0893 0.0970 0.095 Uiso 1 1 calc R U . . .
C13 C 0.5842(13) 1.2332(11) 0.1476(8) 0.068(5) Uani 1 1 d . . . . .
H13A H 0.5469 1.2761 0.1766 0.101 Uiso 1 1 calc R U . . .
H13B H 0.6366 1.1887 0.1699 0.101 Uiso 1 1 calc R U . . .
H13C H 0.6238 1.2568 0.1150 0.101 Uiso 1 1 calc R U . . .
C14 C 0.4225(14) 1.2729(10) 0.0831(8) 0.075(5) Uani 1 1 d . . . . .
H14A H 0.3843 1.3147 0.1127 0.113 Uiso 1 1 calc R U . . .
H14B H 0.4669 1.2967 0.0534 0.113 Uiso 1 1 calc R U . . .
H14C H 0.3683 1.2543 0.0609 0.113 Uiso 1 1 calc R U . . .
C15 C 0.1836(9) 1.0702(7) 0.1833(5) 0.034(2) Uani 1 1 d . . . . .
H15 H 0.1890 1.0625 0.1375 0.040 Uiso 1 1 calc R U . . .
C16 C 0.0319(9) 1.1952(7) 0.1490(5) 0.033(2) Uani 1 1 d . . . . .
C17 C -0.0612(9) 1.2605(7) 0.1604(5) 0.036(3) Uani 1 1 d . . . . .
C18 C -0.1093(10) 1.2653(7) 0.2207(6) 0.040(3) Uani 1 1 d . . . . .
H18 H -0.1744 1.3081 0.2293 0.048 Uiso 1 1 calc R U . . .
C19 C -0.0646(10) 1.2092(8) 0.2681(6) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.0298(9) 1.1477(7) 0.2550(5) 0.038(3) Uani 1 1 d . . . . .
H20 H 0.0622 1.1102 0.2872 0.046 Uiso 1 1 calc R U . . .
C21 C 0.0795(9) 1.1386(7) 0.1955(6) 0.038(3) Uani 1 1 d . . . . .
C22 C -0.1146(10) 1.3259(8) 0.1101(6) 0.044(3) Uani 1 1 d . . . . .
C23 C -0.1445(11) 1.2859(9) 0.0546(7) 0.055(3) Uani 1 1 d . . . . .
H23A H -0.0792 1.2448 0.0386 0.082 Uiso 1 1 calc R U . . .
H23B H -0.2020 1.2591 0.0670 0.082 Uiso 1 1 calc R U . . .
H23C H -0.1718 1.3281 0.0223 0.082 Uiso 1 1 calc R U . . .
C24 C -0.2171(11) 1.3899(8) 0.1345(7) 0.051(3) Uani 1 1 d . . . . .
H24A H -0.1985 1.4162 0.1706 0.077 Uiso 1 1 calc R U . . .
H24B H -0.2443 1.4318 0.1020 0.077 Uiso 1 1 calc R U . . .
H24C H -0.2745 1.3628 0.1467 0.077 Uiso 1 1 calc R U . . .
C25 C -0.0294(11) 1.3731(8) 0.0887(7) 0.058(4) Uani 1 1 d . . . . .
H25A H -0.0093 1.3993 0.1243 0.087 Uiso 1 1 calc R U . . .
H25B H 0.0366 1.3344 0.0708 0.087 Uiso 1 1 calc R U . . .
H25C H -0.0617 1.4154 0.0574 0.087 Uiso 1 1 calc R U . . .
C26 C -0.1237(11) 1.2170(9) 0.3328(6) 0.048(3) Uani 1 1 d . . . . .
C27 C -0.0666(15) 1.1491(13) 0.3769(7) 0.089(6) Uani 1 1 d . . . . .
H27A H -0.0620 1.0956 0.3593 0.133 Uiso 1 1 calc R U . . .
H27B H 0.0078 1.1534 0.3836 0.133 Uiso 1 1 calc R U . . .
H27C H -0.1085 1.1542 0.4165 0.133 Uiso 1 1 calc R U . . .
C28 C -0.2419(13) 1.2088(11) 0.3250(7) 0.066(4) Uani 1 1 d . . . . .
H28A H -0.2814 1.2523 0.2964 0.099 Uiso 1 1 calc R U . . .
H28B H -0.2374 1.1548 0.3084 0.099 Uiso 1 1 calc R U . . .
H28C H -0.2814 1.2142 0.3654 0.099 Uiso 1 1 calc R U . . .
C29 C -0.1317(15) 1.2998(11) 0.3589(8) 0.075(5) Uani 1 1 d . . . . .
H29A H -0.1689 1.3435 0.3297 0.112 Uiso 1 1 calc R U . . .
H29B H -0.1738 1.3055 0.3985 0.112 Uiso 1 1 calc R U . . .
H29C H -0.0575 1.3046 0.3655 0.112 Uiso 1 1 calc R U . . .
C30 C 0.1838(9) 0.9856(7) 0.2131(5) 0.033(2) Uani 1 1 d . . . . .
C31 C 0.2800(9) 0.9253(7) 0.2244(5) 0.034(3) Uani 1 1 d . . . . .
H31 H 0.3483 0.9381 0.2173 0.041 Uiso 1 1 calc R U . . .
C32 C 0.2809(9) 0.8469(7) 0.2456(5) 0.036(3) Uani 1 1 d . . . . .
H32 H 0.3490 0.8071 0.2532 0.043 Uiso 1 1 calc R U . . .
C33 C 0.1810(9) 0.8254(7) 0.2562(5) 0.035(3) Uani 1 1 d . . . . .
C34 C 0.0845(10) 0.8853(7) 0.2436(6) 0.040(3) Uani 1 1 d . . . . .
H34 H 0.0162 0.8724 0.2497 0.048 Uiso 1 1 calc R U . . .
C35 C 0.0847(10) 0.9638(7) 0.2223(6) 0.039(3) Uani 1 1 d . . . . .
H35 H 0.0169 1.0034 0.2138 0.047 Uiso 1 1 calc R U . . .
C36 C 0.1833(9) 0.7356(7) 0.2738(6) 0.038(3) Uani 1 1 d . . . . .
H36 H 0.1942 0.7059 0.2338 0.045 Uiso 1 1 calc R U . . .
C37 C 0.3329(10) 0.6073(7) 0.3007(6) 0.043(3) Uani 1 1 d . . . . .
C38 C 0.4199(11) 0.5636(8) 0.3389(7) 0.053(4) Uani 1 1 d . . . . .
C39 C 0.4523(11) 0.6070(9) 0.3831(7) 0.052(4) Uani 1 1 d . . . . .
H39 H 0.5137 0.5789 0.4068 0.062 Uiso 1 1 calc R U . . .
C40 C 0.4024(11) 0.6886(9) 0.3958(6) 0.047(3) Uani 1 1 d . . . . .
C41 C 0.3120(10) 0.7287(8) 0.3592(6) 0.044(3) Uani 1 1 d . . . . .
H41 H 0.2736 0.7844 0.3672 0.053 Uiso 1 1 calc R U . . .
C42 C 0.2784(9) 0.6903(7) 0.3131(6) 0.038(3) Uani 1 1 d . . . . .
C43 C 0.4776(13) 0.4710(9) 0.3305(9) 0.068(5) Uani 1 1 d . . . . .
C44 C 0.5350(14) 0.4552(10) 0.2662(10) 0.081(6) Uani 1 1 d . . . . .
H44A H 0.4811 0.4766 0.2342 0.122 Uiso 1 1 calc R U . . .
H44B H 0.5935 0.4832 0.2621 0.122 Uiso 1 1 calc R U . . .
H44C H 0.5671 0.3958 0.2614 0.122 Uiso 1 1 calc R U . . .
C45 C 0.5643(15) 0.4368(10) 0.3792(10) 0.090(6) Uani 1 1 d . . . . .
H45A H 0.5296 0.4461 0.4207 0.136 Uiso 1 1 calc R U . . .
H45B H 0.5962 0.3775 0.3736 0.136 Uiso 1 1 calc R U . . .
H45C H 0.6225 0.4649 0.3743 0.136 Uiso 1 1 calc R U . . .
C46 C 0.3892(16) 0.4220(10) 0.3398(11) 0.097(7) Uani 1 1 d . . . . .
H46A H 0.3318 0.4419 0.3094 0.146 Uiso 1 1 calc R U . . .
H46B H 0.4244 0.3631 0.3340 0.146 Uiso 1 1 calc R U . . .
H46C H 0.3560 0.4301 0.3817 0.146 Uiso 1 1 calc R U . . .
C47 C 0.4389(12) 0.7367(10) 0.4455(7) 0.058(4) Uani 1 1 d . . . . .
C48 C 0.3490(15) 0.7587(15) 0.4963(8) 0.093(6) Uani 1 1 d . . . . .
H48A H 0.3721 0.7895 0.5282 0.139 Uiso 1 1 calc R U . . .
H48B H 0.2808 0.7928 0.4785 0.139 Uiso 1 1 calc R U . . .
H48C H 0.3363 0.7082 0.5149 0.139 Uiso 1 1 calc R U . . .
C49 C 0.5466(14) 0.6871(14) 0.4752(9) 0.086(6) Uani 1 1 d . . . . .
H49A H 0.6054 0.6724 0.4431 0.129 Uiso 1 1 calc R U . . .
H49B H 0.5672 0.7206 0.5061 0.129 Uiso 1 1 calc R U . . .
H49C H 0.5358 0.6368 0.4954 0.129 Uiso 1 1 calc R U . . .
C50 C 0.4626(16) 0.8149(12) 0.4162(9) 0.085(6) Uani 1 1 d . . . . .
H50A H 0.5205 0.7994 0.3837 0.127 Uiso 1 1 calc R U . . .
H50B H 0.3953 0.8502 0.3982 0.127 Uiso 1 1 calc R U . . .
H50C H 0.4868 0.8450 0.4482 0.127 Uiso 1 1 calc R U . . .
C51 C 0.0273(10) 0.6667(7) 0.2811(6) 0.039(3) Uani 1 1 d . . . . .
C52 C -0.0748(10) 0.6577(8) 0.3080(6) 0.044(3) Uani 1 1 d . . . . .
C53 C -0.1202(11) 0.7085(9) 0.3569(7) 0.051(3) Uani 1 1 d . . . . .
H53 H -0.1877 0.7037 0.3755 0.061 Uiso 1 1 calc R U . . .
C54 C -0.0740(11) 0.7656(9) 0.3804(6) 0.049(3) Uani 1 1 d . . . . .
C55 C 0.0239(11) 0.7733(8) 0.3514(6) 0.046(3) Uani 1 1 d . . . . .
H55 H 0.0569 0.8128 0.3660 0.055 Uiso 1 1 calc R U . . .
C56 C 0.0737(10) 0.7263(7) 0.3030(6) 0.037(3) Uani 1 1 d . . . . .
C57 C -0.1322(12) 0.5961(9) 0.2823(7) 0.054(4) Uani 1 1 d . . . . .
C58 C -0.0590(13) 0.5077(10) 0.2931(9) 0.073(5) Uani 1 1 d . . . . .
H58A H 0.0129 0.5015 0.2718 0.109 Uiso 1 1 calc R U . . .
H58B H -0.0488 0.4968 0.3376 0.109 Uiso 1 1 calc R U . . .
H58C H -0.0944 0.4684 0.2767 0.109 Uiso 1 1 calc R U . . .
C59 C -0.2425(13) 0.6027(11) 0.3160(8) 0.070(5) Uani 1 1 d . . . . .
H59A H -0.2311 0.5921 0.3605 0.104 Uiso 1 1 calc R U . . .
H59B H -0.2916 0.6583 0.3093 0.104 Uiso 1 1 calc R U . . .
H59C H -0.2759 0.5621 0.3001 0.104 Uiso 1 1 calc R U . . .
C60 C -0.1516(13) 0.6128(11) 0.2128(8) 0.068(4) Uani 1 1 d . . . . .
H60A H -0.0810 0.6087 0.1906 0.102 Uiso 1 1 calc R U . . .
H60B H -0.1852 0.5721 0.1971 0.102 Uiso 1 1 calc R U . . .
H60C H -0.2009 0.6683 0.2064 0.102 Uiso 1 1 calc R U . . .
C61 C -0.1301(13) 0.8192(13) 0.4344(8) 0.071(5) Uani 1 1 d . . . . .
C62 C -0.2473(18) 0.856(2) 0.4268(13) 0.168(15) Uani 1 1 d . . . . .
H62A H -0.2800 0.8148 0.4110 0.252 Uiso 1 1 calc R U . . .
H62B H -0.2827 0.8748 0.4669 0.252 Uiso 1 1 calc R U . . .
H62C H -0.2582 0.9028 0.3974 0.252 Uiso 1 1 calc R U . . .
C63 C -0.132(3) 0.758(2) 0.4929(13) 0.187(16) Uani 1 1 d . . . . .
H63A H -0.0561 0.7285 0.5032 0.280 Uiso 1 1 calc R U . . .
H63B H -0.1690 0.7897 0.5285 0.280 Uiso 1 1 calc R U . . .
H63C H -0.1715 0.7180 0.4827 0.280 Uiso 1 1 calc R U . . .
C64 C -0.064(2) 0.869(2) 0.4576(14) 0.161(14) Uani 1 1 d . . . . .
H64A H 0.0128 0.8361 0.4602 0.241 Uiso 1 1 calc R U . . .
H64B H -0.0678 0.9168 0.4294 0.241 Uiso 1 1 calc R U . . .
H64C H -0.0924 0.8887 0.4989 0.241 Uiso 1 1 calc R U . . .
C73 C 0.5037(16) 0.7018(12) 0.1302(11) 0.084(6) Uani 1 1 d . . . . .
C74 C 0.5271(16) 0.6433(13) 0.1817(10) 0.093(6) Uani 1 1 d . . . . .
H74A H 0.5222 0.6730 0.2203 0.139 Uiso 1 1 calc R U . . .
H74B H 0.6015 0.6063 0.1760 0.139 Uiso 1 1 calc R U . . .
H74C H 0.4734 0.6110 0.1838 0.139 Uiso 1 1 calc R U . . .
C75 C 0.6740(19) 0.8348(13) 0.2337(9) 0.087(6) Uani 1 1 d . . . . .
C76 C 0.7798(15) 0.8534(14) 0.2252(10) 0.093(6) Uani 1 1 d . . . . .
H76A H 0.7723 0.9096 0.2384 0.140 Uiso 1 1 calc R U . . .
H76B H 0.8036 0.8487 0.1814 0.140 Uiso 1 1 calc R U . . .
H76C H 0.8347 0.8143 0.2502 0.140 Uiso 1 1 calc R U . . .
C77 C -0.153(2) 1.0477(13) 0.1413(14) 0.094(7) Uani 1 1 d . . . . .
C78 C -0.0808(19) 1.0506(13) 0.0867(10) 0.097(7) Uani 1 1 d . . . . .
H78A H -0.0062 1.0159 0.0946 0.145 Uiso 1 1 calc R U . . .
H78B H -0.0786 1.1076 0.0782 0.145 Uiso 1 1 calc R U . . .
H78C H -0.1091 1.0303 0.0508 0.145 Uiso 1 1 calc R U . . .
N3 N 0.4837(19) 0.7485(13) 0.0907(10) 0.127(8) Uani 1 1 d . . . . .
N4 N 0.5904(16) 0.8240(13) 0.2411(10) 0.115(7) Uani 1 1 d . . . . .
N5 N -0.2047(16) 1.0435(14) 0.1841(13) 0.123(8) Uani 1 1 d . . . . .
Cl1 Cl 0.0815(3) 1.1604(2) -0.05466(16) 0.0560(8) Uani 1 1 d . . . . .
Cl2 Cl 0.2232(3) 1.00905(19) 0.03121(15) 0.0489(8) Uani 1 1 d . . . . .
Cl3 Cl 0.0929(4) 0.5484(3) 0.1050(2) 0.0785(13) Uani 1 1 d . . . . .
Cl4 Cl 0.3652(5) 0.4922(4) 0.1294(3) 0.114(2) 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
Ta1 O5 1.842(8) . ?
Ta1 O2 1.866(8) . ?
Ta1 O1 1.883(9) . ?
Ta1 N1 2.275(11) . ?
Ta1 Cl1 2.431(3) . ?
Ta1 Cl2 2.437(3) . ?
O1 C1 1.383(14) . ?
O2 C16 1.387(13) . ?
O5 C65 1.459(15) . ?
C65 C66 1.48(2) . ?
N1 C69 1.105(17) . ?
C67 C68 1.41(3) . ?
C67 O6 1.408(18) . ?
Ta2 O6 1.834(10) . ?
Ta2 O4 1.893(9) . ?
Ta2 O3 1.921(10) . ?
Ta2 N2 2.314(12) . ?
Ta2 Cl4 2.366(5) . ?
Ta2 Cl3 2.409(4) . ?
O3 C37 1.363(16) . ?
O4 C51 1.363(15) . ?
C69 C70 1.47(2) . ?
N2 C71 1.14(2) . ?
C71 C72 1.47(2) . ?
C1 C6 1.410(16) . ?
C1 C2 1.412(15) . ?
C2 C3 1.390(16) . ?
C2 C15 1.528(15) . ?
C3 C4 1.375(16) . ?
C4 C5 1.409(17) . ?
C4 C7 1.543(19) . ?
C5 C6 1.397(18) . ?
C6 C11 1.548(16) . ?
C7 C10 1.48(2) . ?
C7 C8 1.49(2) . ?
C7 C9 1.53(3) . ?
C11 C12 1.50(2) . ?
C11 C13 1.533(19) . ?
C11 C14 1.55(2) . ?
C15 C21 1.513(16) . ?
C15 C30 1.544(14) . ?
C16 C17 1.393(16) . ?
C16 C21 1.394(16) . ?
C17 C18 1.406(17) . ?
C17 C22 1.555(16) . ?
C18 C19 1.396(17) . ?
C19 C20 1.375(17) . ?
C19 C26 1.546(17) . ?
C20 C21 1.399(16) . ?
C22 C23 1.509(19) . ?
C22 C24 1.528(18) . ?
C22 C25 1.552(15) . ?
C26 C27 1.50(2) . ?
C26 C29 1.50(2) . ?
C26 C28 1.56(2) . ?
C30 C31 1.377(16) . ?
C30 C35 1.403(15) . ?
C31 C32 1.382(15) . ?
C32 C33 1.412(15) . ?
C33 C34 1.383(17) . ?
C33 C36 1.542(15) . ?
C34 C35 1.387(16) . ?
C36 C42 1.512(17) . ?
C36 C56 1.541(15) . ?
C37 C42 1.410(17) . ?
C37 C38 1.422(19) . ?
C38 C39 1.37(2) . ?
C38 C43 1.55(2) . ?
C39 C40 1.38(2) . ?
C40 C41 1.416(18) . ?
C40 C47 1.53(2) . ?
C41 C42 1.353(18) . ?
C43 C45 1.53(2) . ?
C43 C44 1.54(2) . ?
C43 C46 1.56(2) . ?
C47 C48 1.52(2) . ?
C47 C49 1.54(2) . ?
C47 C50 1.54(2) . ?
C51 C56 1.404(16) . ?
C51 C52 1.436(16) . ?
C52 C53 1.39(2) . ?
C52 C57 1.555(17) . ?
C53 C54 1.380(18) . ?
C54 C55 1.398(17) . ?
C54 C61 1.53(2) . ?
C55 C56 1.359(18) . ?
C57 C59 1.52(2) . ?
C57 C60 1.53(2) . ?
C57 C58 1.54(2) . ?
C61 C62 1.45(3) . ?
C61 C64 1.46(3) . ?
C61 C63 1.61(3) . ?
C73 N3 1.13(3) . ?
C73 C74 1.44(3) . ?
C75 N4 1.12(2) . ?
C75 C76 1.46(3) . ?
C77 N5 1.12(3) . ?
C77 C78 1.47(3) . ?

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
O5 Ta1 O2 99.2(4) . . ?
O5 Ta1 O1 97.3(4) . . ?
O2 Ta1 O1 92.5(3) . . ?
O5 Ta1 N1 82.6(4) . . ?
O2 Ta1 N1 177.9(4) . . ?
O1 Ta1 N1 86.2(4) . . ?
O5 Ta1 Cl1 86.0(3) . . ?
O2 Ta1 Cl1 94.4(3) . . ?
O1 Ta1 Cl1 171.7(3) . . ?
N1 Ta1 Cl1 86.8(3) . . ?
O5 Ta1 Cl2 159.6(3) . . ?
O2 Ta1 Cl2 99.2(2) . . ?
O1 Ta1 Cl2 90.6(2) . . ?
N1 Ta1 Cl2 79.2(3) . . ?
Cl1 Ta1 Cl2 83.86(12) . . ?
C1 O1 Ta1 155.2(7) . . ?
C16 O2 Ta1 155.9(8) . . ?
C65 O5 Ta1 144.9(10) . . ?
O5 C65 C66 110.2(14) . . ?
C69 N1 Ta1 176.3(11) . . ?
C68 C67 O6 116.9(17) . . ?
O6 Ta2 O4 99.0(4) . . ?
O6 Ta2 O3 97.6(5) . . ?
O4 Ta2 O3 90.5(4) . . ?
O6 Ta2 N2 168.2(5) . . ?
O4 Ta2 N2 88.6(4) . . ?
O3 Ta2 N2 91.3(4) . . ?
O6 Ta2 Cl4 91.3(4) . . ?
O4 Ta2 Cl4 169.8(3) . . ?
O3 Ta2 Cl4 88.5(3) . . ?
N2 Ta2 Cl4 81.2(4) . . ?
O6 Ta2 Cl3 91.8(4) . . ?
O4 Ta2 Cl3 89.6(3) . . ?
O3 Ta2 Cl3 170.4(3) . . ?
N2 Ta2 Cl3 79.1(3) . . ?
Cl4 Ta2 Cl3 89.6(2) . . ?
C37 O3 Ta2 158.4(9) . . ?
C51 O4 Ta2 154.6(8) . . ?
C67 O6 Ta2 152.9(12) . . ?
N1 C69 C70 179.5(19) . . ?
C71 N2 Ta2 173.4(14) . . ?
N2 C71 C72 178.2(17) . . ?
O1 C1 C6 120.5(10) . . ?
O1 C1 C2 118.2(10) . . ?
C6 C1 C2 121.3(11) . . ?
C3 C2 C1 119.0(10) . . ?
C3 C2 C15 119.7(9) . . ?
C1 C2 C15 121.3(11) . . ?
C4 C3 C2 122.1(11) . . ?
C3 C4 C5 117.5(12) . . ?
C3 C4 C7 122.2(11) . . ?
C5 C4 C7 120.2(11) . . ?
C6 C5 C4 123.6(11) . . ?
C5 C6 C1 116.4(10) . . ?
C5 C6 C11 121.2(11) . . ?
C1 C6 C11 122.3(12) . . ?
C10 C7 C8 110.3(19) . . ?
C10 C7 C9 110.3(17) . . ?
C8 C7 C9 105.6(17) . . ?
C10 C7 C4 110.1(13) . . ?
C8 C7 C4 112.7(12) . . ?
C9 C7 C4 107.6(14) . . ?
C12 C11 C13 107.8(12) . . ?
C12 C11 C14 111.1(14) . . ?
C13 C11 C14 105.2(12) . . ?
C12 C11 C6 109.8(11) . . ?
C13 C11 C6 111.6(12) . . ?
C14 C11 C6 111.2(11) . . ?
C21 C15 C2 109.9(9) . . ?
C21 C15 C30 115.0(9) . . ?
C2 C15 C30 113.2(9) . . ?
O2 C16 C17 119.9(10) . . ?
O2 C16 C21 117.9(10) . . ?
C17 C16 C21 122.1(10) . . ?
C16 C17 C18 117.1(10) . . ?
C16 C17 C22 123.4(10) . . ?
C18 C17 C22 119.5(11) . . ?
C19 C18 C17 122.3(12) . . ?
C20 C19 C18 118.2(11) . . ?
C20 C19 C26 122.4(11) . . ?
C18 C19 C26 119.4(12) . . ?
C19 C20 C21 122.0(11) . . ?
C16 C21 C20 118.2(11) . . ?
C16 C21 C15 121.7(10) . . ?
C20 C21 C15 120.1(11) . . ?
C23 C22 C24 108.9(11) . . ?
C23 C22 C25 108.7(11) . . ?
C24 C22 C25 107.0(10) . . ?
C23 C22 C17 111.4(10) . . ?
C24 C22 C17 112.7(11) . . ?
C25 C22 C17 108.0(10) . . ?
C27 C26 C29 110.3(14) . . ?
C27 C26 C19 111.8(12) . . ?
C29 C26 C19 110.4(11) . . ?
C27 C26 C28 107.4(13) . . ?
C29 C26 C28 109.0(13) . . ?
C19 C26 C28 108.0(11) . . ?
C31 C30 C35 117.3(10) . . ?
C31 C30 C15 122.1(9) . . ?
C35 C30 C15 120.1(10) . . ?
C30 C31 C32 122.4(10) . . ?
C31 C32 C33 120.4(11) . . ?
C34 C33 C32 117.3(10) . . ?
C34 C33 C36 122.4(9) . . ?
C32 C33 C36 119.9(10) . . ?
C33 C34 C35 121.8(10) . . ?
C34 C35 C30 120.8(11) . . ?
C42 C36 C56 110.3(9) . . ?
C42 C36 C33 114.5(9) . . ?
C56 C36 C33 113.7(10) . . ?
O3 C37 C42 119.8(12) . . ?
O3 C37 C38 121.0(12) . . ?
C42 C37 C38 119.2(13) . . ?
C39 C38 C37 117.4(13) . . ?
C39 C38 C43 120.9(14) . . ?
C37 C38 C43 121.7(14) . . ?
C38 C39 C40 124.9(13) . . ?
C39 C40 C41 115.9(13) . . ?
C39 C40 C47 124.6(13) . . ?
C41 C40 C47 119.5(13) . . ?
C42 C41 C40 122.2(13) . . ?
C41 C42 C37 120.2(12) . . ?
C41 C42 C36 120.8(11) . . ?
C37 C42 C36 119.0(11) . . ?
C45 C43 C44 107.9(15) . . ?
C45 C43 C38 111.9(15) . . ?
C44 C43 C38 111.3(13) . . ?
C45 C43 C46 106.7(13) . . ?
C44 C43 C46 110.3(15) . . ?
C38 C43 C46 108.6(13) . . ?
C48 C47 C40 109.2(12) . . ?
C48 C47 C49 108.5(14) . . ?
C40 C47 C49 112.5(14) . . ?
C48 C47 C50 110.8(16) . . ?
C40 C47 C50 109.9(12) . . ?
C49 C47 C50 106.0(13) . . ?
O4 C51 C56 119.8(10) . . ?
O4 C51 C52 120.1(11) . . ?
C56 C51 C52 120.1(12) . . ?
C53 C52 C51 116.2(11) . . ?
C53 C52 C57 122.3(11) . . ?
C51 C52 C57 121.5(13) . . ?
C54 C53 C52 124.6(11) . . ?
C53 C54 C55 116.8(13) . . ?
C53 C54 C61 121.0(12) . . ?
C55 C54 C61 122.2(12) . . ?
C56 C55 C54 122.5(12) . . ?
C55 C56 C51 119.8(10) . . ?
C55 C56 C36 120.5(11) . . ?
C51 C56 C36 119.7(11) . . ?
C59 C57 C60 108.8(12) . . ?
C59 C57 C58 107.6(12) . . ?
C60 C57 C58 109.8(14) . . ?
C59 C57 C52 111.0(13) . . ?
C60 C57 C52 110.7(11) . . ?
C58 C57 C52 108.9(12) . . ?
C62 C61 C64 119(2) . . ?
C62 C61 C54 113.2(14) . . ?
C64 C61 C54 113.4(14) . . ?
C62 C61 C63 101(2) . . ?
C64 C61 C63 101(2) . . ?
C54 C61 C63 106.7(18) . . ?
N3 C73 C74 179(3) . . ?
N4 C75 C76 177(3) . . ?
N5 C77 C78 177(3) . . ?

_refine_diff_density_max         2.476
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.172



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_nb
_database_code_depnum_ccdc_archive 'CCDC 1043648'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_vrf_THETM01_Nb_calix2           
;
RESPONSE: The crystal was very weakly scattering. Data were truncated
at 40 degrees 2theta (Mo radiation). There were no useful data beyond 
this point. 
;

_vrf_PLAT026_Nb_calix2           
;
RESPONSE: The crystal was very weakly scattering. Data were truncated
at 40 degrees 2theta (Mo radiation). A large number of weak data were 
still included in the refinement. 
;

_vrf_PLAT242_Nb_calix2           
;
RESPONSE: The central atom of a tertiary butyl group. It has a smaller
displacement parameter than the surrounding atoms.  
;

_vrf_PLAT342_Nb_calix2           
;
RESPONSE: The crystal was very weakly scattering. Data were truncated
at 40 degrees 2theta (Mo radiation). This give rise to moderately good
C-C precision. 
;

_vrf_PLAT420_Nb_calix2           
;
RESPONSE: These are phenol groups from the calixarenes that do not 
bind to the metal and do not form hydrogen bonds. This is a reflection 
of the geometry of the calixarenes and the small number of 
hydrogen-bond acceptors present.  
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C130 H179 Cl N Nb O8, 5(C2 H3 N)'
_chemical_formula_sum            'C140 H194 Cl N6 Nb O8'
_chemical_formula_weight         2217.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 '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'

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

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

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

_cell_length_a                   17.5553(17)
_cell_length_b                   19.1574(15)
_cell_length_c                   22.552(3)
_cell_angle_alpha                74.926(8)
_cell_angle_beta                 81.846(9)
_cell_angle_gamma                73.063(7)
_cell_volume                     6988.0(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9671
_cell_measurement_theta_min      1.3
_cell_measurement_theta_max      20.3

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_F_000             2396
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            25016
_diffrn_reflns_av_unetI/netI     0.2609
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.429
_diffrn_reflns_theta_max         19.782
_diffrn_reflns_theta_full        19.782
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             12529
_reflns_number_gt                3851
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Stoe X-AREA'
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_solution    SHELXS-86
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0965P)²] 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         12529
_refine_ls_number_parameters     1396
_refine_ls_number_restraints     1316
_refine_ls_R_factor_all          0.2149
_refine_ls_R_factor_gt           0.0822
_refine_ls_wR_factor_ref         0.2375
_refine_ls_wR_factor_gt          0.1846
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_restrained_S_all      0.791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.17988(8) 0.39983(6) 0.14232(7) 0.0855(5) Uani 1 1 d . U . . .
Cl1 Cl 0.1392(2) 0.44576(16) 0.03797(16) 0.0940(11) Uani 1 1 d . U . . .
C1 C 0.1188(8) 0.2542(7) 0.1646(7) 0.089(4) Uani 1 1 d . U . . .
C2 C 0.0653(8) 0.2529(6) 0.2170(7) 0.086(3) Uani 1 1 d . U . . .
C3 C 0.0161(8) 0.2056(6) 0.2302(7) 0.109(4) Uani 1 1 d . U . . .
H3 H -0.0205 0.2067 0.2655 0.131 Uiso 1 1 calc R U . . .
C4 C 0.0175(9) 0.1564(7) 0.1941(8) 0.114(4) Uani 1 1 d . U . . .
C5 C 0.0764(9) 0.1533(7) 0.1458(7) 0.111(4) Uani 1 1 d . U . . .
H5 H 0.0824 0.1169 0.1226 0.133 Uiso 1 1 calc R U . . .
C6 C 0.1274(8) 0.2008(6) 0.1294(7) 0.090(3) Uani 1 1 d . U . . .
C7 C -0.0359(12) 0.1052(10) 0.2092(11) 0.163(6) Uani 1 1 d . U . . .
C8 C -0.1161(11) 0.1471(9) 0.2084(12) 0.220(8) Uani 1 1 d . U . . .
H8A H -0.1506 0.1130 0.2184 0.331 Uiso 1 1 calc R U . . .
H8B H -0.1276 0.1777 0.2390 0.331 Uiso 1 1 calc R U . . .
H8C H -0.1261 0.1799 0.1674 0.331 Uiso 1 1 calc R U . . .
C9 C -0.0199(11) 0.0540(10) 0.2758(10) 0.196(7) Uani 1 1 d . U . . .
H9A H 0.0360 0.0245 0.2766 0.294 Uiso 1 1 calc R U . . .
H9B H -0.0313 0.0855 0.3056 0.294 Uiso 1 1 calc R U . . .
H9C H -0.0546 0.0200 0.2865 0.294 Uiso 1 1 calc R U . . .
C10 C -0.0090(10) 0.0444(9) 0.1730(10) 0.202(7) Uani 1 1 d . U . . .
H10A H 0.0479 0.0198 0.1775 0.303 Uiso 1 1 calc R U . . .
H10B H -0.0398 0.0074 0.1888 0.303 Uiso 1 1 calc R U . . .
H10C H -0.0178 0.0670 0.1294 0.303 Uiso 1 1 calc R U . . .
C11 C 0.1917(8) 0.1937(6) 0.0751(7) 0.094(3) Uani 1 1 d . U . . .
C12 C 0.1671(8) 0.2581(6) 0.0200(6) 0.108(4) Uani 1 1 d . U . . .
H12A H 0.2083 0.2529 -0.0139 0.162 Uiso 1 1 calc R U . . .
H12B H 0.1163 0.2574 0.0072 0.162 Uiso 1 1 calc R U . . .
H12C H 0.1608 0.3057 0.0313 0.162 Uiso 1 1 calc R U . . .
C13 C 0.2049(8) 0.1174(6) 0.0547(6) 0.114(5) Uani 1 1 d . U . . .
H13A H 0.2208 0.0750 0.0898 0.170 Uiso 1 1 calc R U . . .
H13B H 0.1551 0.1162 0.0406 0.170 Uiso 1 1 calc R U . . .
H13C H 0.2469 0.1140 0.0211 0.170 Uiso 1 1 calc R U . . .
C14 C 0.2754(7) 0.1899(7) 0.0954(6) 0.103(4) Uani 1 1 d . U . . .
H14A H 0.2897 0.1478 0.1310 0.154 Uiso 1 1 calc R U . . .
H14B H 0.3160 0.1827 0.0613 0.154 Uiso 1 1 calc R U . . .
H14C H 0.2727 0.2368 0.1065 0.154 Uiso 1 1 calc R U . . .
C15 C 0.0565(7) 0.3086(6) 0.2583(6) 0.085(3) Uani 1 1 d . U . . .
H15 H 0.1050 0.3280 0.2486 0.102 Uiso 1 1 calc R U . . .
C16 C -0.0030(8) 0.4430(7) 0.1991(6) 0.081(3) Uani 1 1 d . U . . .
C17 C -0.0668(8) 0.5085(6) 0.1852(6) 0.085(3) Uani 1 1 d . U . . .
C18 C -0.1432(8) 0.4993(7) 0.2083(6) 0.084(3) Uani 1 1 d . U . . .
H18 H -0.1879 0.5417 0.1995 0.101 Uiso 1 1 calc R U . . .
C19 C -0.1575(8) 0.4305(7) 0.2438(7) 0.095(4) Uani 1 1 d . U . . .
C20 C -0.0911(8) 0.3717(6) 0.2586(6) 0.087(4) Uani 1 1 d . U . . .
H20 H -0.0984 0.3258 0.2842 0.105 Uiso 1 1 calc R U . . .
C21 C -0.0158(7) 0.3760(6) 0.2384(6) 0.075(3) Uani 1 1 d . U . . .
C22 C -0.0561(8) 0.5856(6) 0.1491(6) 0.089(3) Uani 1 1 d . U . . .
C23 C 0.0026(8) 0.6075(6) 0.1787(6) 0.099(4) Uani 1 1 d . U . . .
H23A H 0.0089 0.6566 0.1554 0.149 Uiso 1 1 calc R U . . .
H23B H -0.0174 0.6102 0.2212 0.149 Uiso 1 1 calc R U . . .
H23C H 0.0543 0.5700 0.1789 0.149 Uiso 1 1 calc R U . . .
C24 C -0.0264(7) 0.5822(6) 0.0820(6) 0.094(4) Uani 1 1 d . U . . .
H24A H -0.0649 0.5679 0.0633 0.141 Uiso 1 1 calc R U . . .
H24B H -0.0208 0.6315 0.0588 0.141 Uiso 1 1 calc R U . . .
H24C H 0.0255 0.5450 0.0814 0.141 Uiso 1 1 calc R U . . .
C25 C -0.1365(7) 0.6474(6) 0.1477(6) 0.103(4) Uani 1 1 d . U . . .
H25A H -0.1755 0.6343 0.1286 0.154 Uiso 1 1 calc R U . . .
H25B H -0.1564 0.6515 0.1899 0.154 Uiso 1 1 calc R U . . .
H25C H -0.1281 0.6956 0.1238 0.154 Uiso 1 1 calc R U . . .
C26 C -0.2433(9) 0.4271(8) 0.2655(8) 0.108(4) Uani 1 1 d . U . . .
C27 C -0.2985(8) 0.4590(8) 0.2133(7) 0.134(5) Uani 1 1 d . U . . .
H27A H -0.2967 0.5107 0.1941 0.201 Uiso 1 1 calc R U . . .
H27B H -0.2812 0.4286 0.1826 0.201 Uiso 1 1 calc R U . . .
H27C H -0.3532 0.4585 0.2295 0.201 Uiso 1 1 calc R U . . .
C28 C -0.2734(9) 0.4720(8) 0.3150(7) 0.139(5) Uani 1 1 d . U . . .
H28A H -0.2726 0.5243 0.2976 0.208 Uiso 1 1 calc R U . . .
H28B H -0.3282 0.4699 0.3298 0.208 Uiso 1 1 calc R U . . .
H28C H -0.2389 0.4505 0.3494 0.208 Uiso 1 1 calc R U . . .
C29 C -0.2461(9) 0.3476(8) 0.2950(8) 0.157(6) Uani 1 1 d . U . . .
H29A H -0.2104 0.3270 0.3287 0.235 Uiso 1 1 calc R U . . .
H29B H -0.3008 0.3471 0.3112 0.235 Uiso 1 1 calc R U . . .
H29C H -0.2287 0.3172 0.2643 0.235 Uiso 1 1 calc R U . . .
C30 C 0.0529(8) 0.2724(7) 0.3279(7) 0.087(3) Uani 1 1 d . U . . .
C31 C 0.1034(8) 0.2020(7) 0.3477(7) 0.102(4) Uani 1 1 d . U . . .
H31 H 0.1367 0.1762 0.3188 0.123 Uiso 1 1 calc R U . . .
C32 C 0.1051(9) 0.1691(8) 0.4108(7) 0.119(5) Uani 1 1 d . U . . .
H32 H 0.1401 0.1208 0.4247 0.143 Uiso 1 1 calc R U . . .
C33 C 0.0559(8) 0.2066(8) 0.4537(7) 0.111(5) Uani 1 1 d . U . . .
H33 H 0.0571 0.1837 0.4964 0.134 Uiso 1 1 calc R U . . .
C34 C 0.0047(8) 0.2781(7) 0.4333(7) 0.093(4) Uani 1 1 d . U . . .
C35 C 0.0055(8) 0.3100(7) 0.3705(7) 0.094(4) Uani 1 1 d . U . . .
H35 H -0.0274 0.3591 0.3563 0.113 Uiso 1 1 calc R U . . .
C36 C -0.0553(8) 0.3197(7) 0.4774(7) 0.096(3) Uani 1 1 d . U . . .
H36 H -0.0667 0.3743 0.4571 0.115 Uiso 1 1 calc R U . . .
C37 C 0.0364(9) 0.3434(7) 0.5422(8) 0.101(4) Uani 1 1 d . U . . .
C38 C 0.0667(9) 0.3388(7) 0.5979(8) 0.101(4) Uani 1 1 d . U . . .
C39 C 0.0269(9) 0.3038(7) 0.6502(8) 0.111(4) Uani 1 1 d . U . . .
H39 H 0.0417 0.3030 0.6893 0.133 Uiso 1 1 calc R U . . .
C40 C -0.0325(9) 0.2704(7) 0.6489(8) 0.103(4) Uani 1 1 d . U . . .
C41 C -0.0557(9) 0.2727(8) 0.5927(7) 0.111(4) Uani 1 1 d . U . . .
H41 H -0.0952 0.2483 0.5911 0.133 Uiso 1 1 calc R U . . .
C42 C -0.0226(9) 0.3102(7) 0.5374(8) 0.100(4) Uani 1 1 d . U . . .
C43 C 0.1307(9) 0.3770(8) 0.6006(7) 0.104(4) Uani 1 1 d . U . . .
C44 C 0.1038(8) 0.4610(7) 0.5741(7) 0.118(5) Uani 1 1 d . U . . .
H44A H 0.0904 0.4704 0.5315 0.177 Uiso 1 1 calc DR U . . .
H44B H 0.0567 0.4832 0.5986 0.177 Uiso 1 1 calc R U . . .
H44C H 0.1469 0.4835 0.5750 0.177 Uiso 1 1 calc R U . . .
C45 C 0.2083(8) 0.3421(8) 0.5657(7) 0.127(5) Uani 1 1 d . U . . .
H45A H 0.1986 0.3492 0.5226 0.190 Uiso 1 1 calc DR U . . .
H45B H 0.2494 0.3665 0.5680 0.190 Uiso 1 1 calc R U . . .
H45C H 0.2264 0.2884 0.5845 0.190 Uiso 1 1 calc R U . . .
C46 C 0.1511(9) 0.3635(8) 0.6664(7) 0.130(5) Uani 1 1 d . U . . .
H46A H 0.1685 0.3095 0.6840 0.194 Uiso 1 1 calc R U . . .
H46B H 0.1941 0.3864 0.6670 0.194 Uiso 1 1 calc R U . . .
H46C H 0.1038 0.3860 0.6907 0.194 Uiso 1 1 calc R U . . .
C47 C -0.0740(10) 0.2302(7) 0.7083(8) 0.117(4) Uani 1 1 d . U . . .
C48 C -0.0502(10) 0.1448(7) 0.7080(7) 0.147(6) Uani 1 1 d . U . . .
H48A H -0.0621 0.1390 0.6687 0.220 Uiso 1 1 calc R U . . .
H48B H 0.0071 0.1237 0.7134 0.220 Uiso 1 1 calc R U . . .
H48C H -0.0805 0.1185 0.7418 0.220 Uiso 1 1 calc R U . . .
C49 C -0.0568(10) 0.2412(7) 0.7673(7) 0.137(5) Uani 1 1 d . U . . .
H49A H -0.0856 0.2138 0.8016 0.205 Uiso 1 1 calc R U . . .
H49B H 0.0007 0.2223 0.7723 0.205 Uiso 1 1 calc R U . . .
H49C H -0.0741 0.2947 0.7671 0.205 Uiso 1 1 calc R U . . .
C50 C -0.1683(9) 0.2591(8) 0.7064(7) 0.133(5) Uani 1 1 d . U . . .
H50A H -0.1840 0.2534 0.6683 0.200 Uiso 1 1 calc R U . . .
H50B H -0.1934 0.2297 0.7419 0.200 Uiso 1 1 calc R U . . .
H50C H -0.1858 0.3121 0.7080 0.200 Uiso 1 1 calc R U . . .
C51 C -0.2042(9) 0.3476(8) 0.5059(7) 0.110(5) Uani 1 1 d . U . . .
C52 C -0.2754(9) 0.3322(9) 0.5118(7) 0.122(5) Uani 1 1 d . U . . .
C53 C -0.2798(10) 0.2673(9) 0.4967(8) 0.143(6) Uani 1 1 d . U . . .
H53 H -0.3301 0.2570 0.4996 0.172 Uiso 1 1 calc R U . . .
C54 C -0.2089(10) 0.2156(9) 0.4767(9) 0.143(6) Uani 1 1 d . U . . .
C55 C -0.1398(9) 0.2361(8) 0.4693(7) 0.123(5) Uani 1 1 d . U . . .
H55 H -0.0931 0.2047 0.4534 0.148 Uiso 1 1 calc R U . . .
C56 C -0.1337(9) 0.2986(8) 0.4832(7) 0.104(4) Uani 1 1 d . U . . .
C57 C -0.3520(10) 0.3866(10) 0.5342(9) 0.140(5) Uani 1 1 d . U . . .
C58 C -0.3661(10) 0.4661(9) 0.4934(8) 0.163(6) Uani 1 1 d . U . . .
H58A H -0.3189 0.4843 0.4916 0.245 Uiso 1 1 calc R U . . .
H58B H -0.3758 0.4655 0.4519 0.245 Uiso 1 1 calc R U . . .
H58C H -0.4126 0.4993 0.5108 0.245 Uiso 1 1 calc R U . . .
C59 C -0.3447(9) 0.3892(9) 0.6012(8) 0.149(6) Uani 1 1 d . U . . .
H59A H -0.3356 0.3384 0.6275 0.224 Uiso 1 1 calc R U . . .
H59B H -0.2997 0.4093 0.6023 0.224 Uiso 1 1 calc R U . . .
H59C H -0.3941 0.4214 0.6161 0.224 Uiso 1 1 calc R U . . .
C60 C -0.4274(10) 0.3611(10) 0.5353(9) 0.183(7) Uani 1 1 d . U . . .
H60A H -0.4206 0.3102 0.5611 0.275 Uiso 1 1 calc R U . . .
H60B H -0.4734 0.3953 0.5522 0.275 Uiso 1 1 calc R U . . .
H60C H -0.4366 0.3615 0.4933 0.275 Uiso 1 1 calc R U . . .
C61 C -0.2191(15) 0.1438(12) 0.4614(14) 0.199(7) Uani 1 1 d . U . . .
C62 C -0.2845(13) 0.1156(11) 0.4945(11) 0.222(9) Uani 1 1 d . U . . .
H62A H -0.2869 0.1167 0.5379 0.333 Uiso 1 1 calc R U . . .
H62B H -0.3347 0.1471 0.4769 0.333 Uiso 1 1 calc R U . . .
H62C H -0.2765 0.0639 0.4911 0.333 Uiso 1 1 calc R U . . .
C63 C -0.2025(17) 0.1481(11) 0.3974(12) 0.268(10) Uani 1 1 d . U . . .
H63A H -0.1563 0.1685 0.3828 0.402 Uiso 1 1 calc R U . . .
H63B H -0.1909 0.0979 0.3896 0.402 Uiso 1 1 calc R U . . .
H63C H -0.2490 0.1810 0.3754 0.402 Uiso 1 1 calc R U . . .
C64 C -0.1478(16) 0.0772(13) 0.4933(14) 0.286(10) Uani 1 1 d . U . . .
H64A H -0.1555 0.0711 0.5381 0.429 Uiso 1 1 calc R U . . .
H64B H -0.1472 0.0305 0.4829 0.429 Uiso 1 1 calc R U . . .
H64C H -0.0968 0.0894 0.4785 0.429 Uiso 1 1 calc R U . . .
C65 C 0.3689(9) 0.3386(7) 0.1072(8) 0.094(4) Uani 1 1 d . U . . .
C66 C 0.4006(8) 0.2854(7) 0.1598(7) 0.094(3) Uani 1 1 d . U . . .
C67 C 0.4831(9) 0.2606(7) 0.1639(8) 0.111(4) Uani 1 1 d . U . . .
H67 H 0.5038 0.2272 0.2007 0.133 Uiso 1 1 calc R U . . .
C68 C 0.5343(10) 0.2824(8) 0.1171(9) 0.122(4) Uani 1 1 d . U . . .
C69 C 0.5007(9) 0.3310(8) 0.0638(8) 0.123(5) Uani 1 1 d . U . . .
H69 H 0.5360 0.3452 0.0297 0.148 Uiso 1 1 calc R U . . .
C70 C 0.4220(9) 0.3590(8) 0.0574(8) 0.109(4) Uani 1 1 d . U . . .
C71 C 0.6230(9) 0.2529(8) 0.1195(9) 0.169(6) Uani 1 1 d D U . . .
C72 C 0.6496(10) 0.1725(8) 0.1441(10) 0.258(9) Uani 1 1 d D U . . .
H72A H 0.6279 0.1466 0.1212 0.386 Uiso 1 1 calc R U . . .
H72B H 0.7081 0.1562 0.1401 0.386 Uiso 1 1 calc R U . . .
H72C H 0.6309 0.1605 0.1876 0.386 Uiso 1 1 calc R U . . .
C73 C 0.6556(10) 0.2923(10) 0.1539(10) 0.235(9) Uani 1 1 d D U . . .
H73A H 0.6375 0.3465 0.1372 0.352 Uiso 1 1 calc R U . . .
H73B H 0.6369 0.2804 0.1975 0.352 Uiso 1 1 calc R U . . .
H73C H 0.7141 0.2761 0.1499 0.352 Uiso 1 1 calc R U . . .
C74 C 0.6725(12) 0.2645(12) 0.0574(9) 0.271(9) Uani 1 1 d D U . . .
H74A H 0.6587 0.3178 0.0368 0.407 Uiso 1 1 calc R U . . .
H74B H 0.7294 0.2473 0.0646 0.407 Uiso 1 1 calc R U . . .
H74C H 0.6608 0.2356 0.0314 0.407 Uiso 1 1 calc R U . . .
C75 C 0.3906(9) 0.4106(7) -0.0060(8) 0.111(4) Uani 1 1 d . U . . .
C76 C 0.3375(8) 0.3719(7) -0.0280(7) 0.115(4) Uani 1 1 d . U . . .
H76A H 0.3691 0.3221 -0.0328 0.172 Uiso 1 1 calc R U . . .
H76B H 0.2926 0.3670 0.0025 0.172 Uiso 1 1 calc R U . . .
H76C H 0.3172 0.4022 -0.0675 0.172 Uiso 1 1 calc R U . . .
C77 C 0.3414(8) 0.4886(7) 0.0017(7) 0.115(5) Uani 1 1 d . U . . .
H77A H 0.3751 0.5130 0.0157 0.173 Uiso 1 1 calc R U . . .
H77B H 0.3211 0.5189 -0.0379 0.173 Uiso 1 1 calc R U . . .
H77C H 0.2964 0.4837 0.0322 0.173 Uiso 1 1 calc R U . . .
C78 C 0.4592(9) 0.4212(8) -0.0560(7) 0.142(5) Uani 1 1 d . U . . .
H78A H 0.4918 0.3720 -0.0619 0.213 Uiso 1 1 calc R U . . .
H78B H 0.4366 0.4514 -0.0948 0.213 Uiso 1 1 calc R U . . .
H78C H 0.4925 0.4467 -0.0429 0.213 Uiso 1 1 calc R U . . .
C79 C 0.3442(8) 0.2591(6) 0.2136(6) 0.092(3) Uani 1 1 d . U . . .
H79 H 0.2907 0.2728 0.1968 0.110 Uiso 1 1 calc R U . . .
C80 C 0.2696(8) 0.3662(6) 0.2655(7) 0.092(4) Uani 1 1 d . U . . .
C81 C 0.2605(8) 0.4043(6) 0.3134(6) 0.092(4) Uani 1 1 d . U . . .
C82 C 0.3222(10) 0.3798(7) 0.3535(7) 0.130(5) Uani 1 1 d . U . . .
H82 H 0.3184 0.4059 0.3848 0.156 Uiso 1 1 calc R U . . .
C83 C 0.3894(11) 0.3188(8) 0.3500(8) 0.152(6) Uani 1 1 d . U . . .
C84 C 0.3905(9) 0.2810(7) 0.3047(7) 0.120(5) Uani 1 1 d . U . . .
H84 H 0.4329 0.2374 0.3027 0.144 Uiso 1 1 calc R U . . .
C85 C 0.3341(8) 0.3033(7) 0.2630(7) 0.099(4) Uani 1 1 d . U . . .
C86 C 0.1891(8) 0.4697(7) 0.3217(6) 0.094(3) Uani 1 1 d . U . . .
C87 C 0.1099(8) 0.4512(7) 0.3212(6) 0.104(4) Uani 1 1 d . U . . .
H87A H 0.0654 0.4944 0.3267 0.155 Uiso 1 1 calc R U . . .
H87B H 0.1075 0.4396 0.2818 0.155 Uiso 1 1 calc R U . . .
H87C H 0.1063 0.4078 0.3548 0.155 Uiso 1 1 calc R U . . .
C88 C 0.1936(8) 0.5390(6) 0.2681(6) 0.100(4) Uani 1 1 d . U . . .
H88A H 0.1479 0.5814 0.2731 0.151 Uiso 1 1 calc R U . . .
H88B H 0.2432 0.5524 0.2688 0.151 Uiso 1 1 calc R U . . .
H88C H 0.1927 0.5268 0.2287 0.151 Uiso 1 1 calc R U . . .
C89 C 0.1857(9) 0.4948(7) 0.3823(6) 0.114(4) Uani 1 1 d . U . . .
H89A H 0.1384 0.5369 0.3845 0.171 Uiso 1 1 calc R U . . .
H89B H 0.1827 0.4529 0.4176 0.171 Uiso 1 1 calc R U . . .
H89C H 0.2338 0.5106 0.3831 0.171 Uiso 1 1 calc R U . . .
C90 C 0.4569(11) 0.2986(9) 0.3928(9) 0.194(7) Uani 1 1 d D U . . .
C91 C 0.5001(12) 0.3593(10) 0.3751(8) 0.233(8) Uani 1 1 d D U . . .
H91A H 0.4616 0.4080 0.3755 0.350 Uiso 1 1 calc R U . . .
H91B H 0.5401 0.3493 0.4045 0.350 Uiso 1 1 calc R U . . .
H91C H 0.5265 0.3602 0.3337 0.350 Uiso 1 1 calc R U . . .
C92 C 0.5175(13) 0.2297(10) 0.3910(10) 0.306(11) Uani 1 1 d D U . . .
H92A H 0.5392 0.2302 0.3484 0.458 Uiso 1 1 calc R U . . .
H92B H 0.5605 0.2248 0.4164 0.458 Uiso 1 1 calc R U . . .
H92C H 0.4941 0.1872 0.4069 0.458 Uiso 1 1 calc R U . . .
C93 C 0.4243(10) 0.2977(10) 0.4572(8) 0.219(8) Uani 1 1 d D U . . .
H93A H 0.3830 0.3446 0.4585 0.329 Uiso 1 1 calc R U . . .
H93B H 0.4010 0.2552 0.4731 0.329 Uiso 1 1 calc R U . . .
H93C H 0.4673 0.2928 0.4826 0.329 Uiso 1 1 calc R U . . .
C94 C 0.3650(8) 0.1725(7) 0.2418(7) 0.094(4) Uani 1 1 d . U . . .
C95 C 0.4168(7) 0.1228(6) 0.2070(7) 0.091(4) Uani 1 1 d . U . . .
H95 H 0.4409 0.1423 0.1682 0.109 Uiso 1 1 calc R U . . .
C96 C 0.4320(8) 0.0455(7) 0.2303(8) 0.100(4) Uani 1 1 d . U . . .
C97 C 0.3941(9) 0.0191(8) 0.2855(8) 0.126(5) Uani 1 1 d . U . . .
H97 H 0.4042 -0.0335 0.3012 0.151 Uiso 1 1 calc R U . . .
C98 C 0.3429(9) 0.0653(7) 0.3187(8) 0.128(5) Uani 1 1 d . U . . .
H98 H 0.3162 0.0449 0.3559 0.154 Uiso 1 1 calc R U . . .
C99 C 0.3292(9) 0.1444(8) 0.2975(8) 0.118(5) Uani 1 1 d . U . . .
H99 H 0.2958 0.1772 0.3215 0.142 Uiso 1 1 calc R U . . .
C100 C 0.4915(7) -0.0036(6) 0.1934(7) 0.099(4) Uani 1 1 d . U . . .
H100 H 0.4903 0.0251 0.1495 0.119 Uiso 1 1 calc DR U . . .
C101 C 0.4048(7) -0.0752(7) 0.1664(7) 0.103(4) Uani 1 1 d . U . . .
C102 C 0.3862(8) -0.1417(7) 0.1638(7) 0.110(4) Uani 1 1 d . U . . .
C103 C 0.4394(7) -0.2089(6) 0.1916(7) 0.101(4) Uani 1 1 d . U . . .
H103 H 0.4283 -0.2542 0.1906 0.121 Uiso 1 1 calc R U . . .
C104 C 0.5065(7) -0.2153(7) 0.2204(7) 0.103(4) Uani 1 1 d . U . . .
C105 C 0.5218(7) -0.1489(6) 0.2234(7) 0.106(5) Uani 1 1 d . U . . .
H105 H 0.5661 -0.1508 0.2441 0.127 Uiso 1 1 calc R U . . .
C106 C 0.4715(7) -0.0786(6) 0.1958(7) 0.098(4) Uani 1 1 d . U . . .
C107 C 0.3145(8) -0.1384(7) 0.1313(9) 0.115(4) Uani 1 1 d . U . . .
C108 C 0.3232(9) -0.0999(8) 0.0618(8) 0.135(5) Uani 1 1 d . U . . .
H10D H 0.2767 -0.0983 0.0416 0.203 Uiso 1 1 calc R U . . .
H10E H 0.3269 -0.0487 0.0575 0.203 Uiso 1 1 calc R U . . .
H10F H 0.3717 -0.1285 0.0425 0.203 Uiso 1 1 calc R U . . .
C109 C 0.2386(7) -0.0991(7) 0.1654(8) 0.136(5) Uani 1 1 d . U . . .
H10G H 0.1917 -0.0965 0.1451 0.204 Uiso 1 1 calc R U . . .
H10H H 0.2352 -0.1275 0.2082 0.204 Uiso 1 1 calc R U . . .
H10I H 0.2406 -0.0483 0.1646 0.204 Uiso 1 1 calc R U . . .
C110 C 0.3085(8) -0.2181(7) 0.1348(7) 0.134(5) Uani 1 1 d . U . . .
H11A H 0.2621 -0.2149 0.1137 0.201 Uiso 1 1 calc R U . . .
H11B H 0.3571 -0.2457 0.1149 0.201 Uiso 1 1 calc R U . . .
H11C H 0.3026 -0.2443 0.1780 0.201 Uiso 1 1 calc R U . . .
C111 C 0.5599(9) -0.2902(7) 0.2514(10) 0.136(5) Uani 1 1 d . U . . .
C112 C 0.5990(12) -0.2882(10) 0.3046(11) 0.211(7) Uani 1 1 d . U . . .
H11D H 0.6210 -0.2447 0.2941 0.316 Uiso 1 1 calc R U . . .
H11E H 0.5598 -0.2845 0.3400 0.316 Uiso 1 1 calc R U . . .
H11F H 0.6422 -0.3342 0.3151 0.316 Uiso 1 1 calc R U . . .
C113 C 0.6343(10) -0.3042(9) 0.2078(10) 0.201(7) Uani 1 1 d . U . . .
H11G H 0.6574 -0.2615 0.1990 0.301 Uiso 1 1 calc R U . . .
H11H H 0.6734 -0.3498 0.2270 0.301 Uiso 1 1 calc R U . . .
H11I H 0.6201 -0.3103 0.1694 0.301 Uiso 1 1 calc R U . . .
C114 C 0.5259(10) -0.3541(8) 0.2643(10) 0.205(8) Uani 1 1 d . U . . .
H11J H 0.5006 -0.3533 0.2280 0.307 Uiso 1 1 calc R U . . .
H11K H 0.5683 -0.4007 0.2744 0.307 Uiso 1 1 calc R U . . .
H11L H 0.4858 -0.3510 0.2993 0.307 Uiso 1 1 calc R U . . .
C115 C 0.6409(10) -0.0344(7) 0.1672(10) 0.118(4) Uani 1 1 d . U . . .
C116 C 0.7196(10) -0.0526(8) 0.1826(10) 0.138(4) Uani 1 1 d . U . . .
C117 C 0.7332(11) -0.0573(8) 0.2437(11) 0.154(5) Uani 1 1 d . U . . .
H117 H 0.7866 -0.0730 0.2555 0.184 Uiso 1 1 calc R U . . .
C118 C 0.6720(12) -0.0398(8) 0.2866(11) 0.149(5) Uani 1 1 d . U . . .
C119 C 0.5940(10) -0.0212(7) 0.2706(9) 0.134(5) Uani 1 1 d . U . . .
H119 H 0.5516 -0.0104 0.3008 0.161 Uiso 1 1 calc R U . . .
C120 C 0.5763(9) -0.0178(7) 0.2125(9) 0.115(4) Uani 1 1 d . U . . .
C121 C 0.7929(10) -0.0761(9) 0.1376(11) 0.158(5) Uani 1 1 d . U . . .
C122 C 0.7899(9) -0.1459(8) 0.1170(9) 0.167(6) Uani 1 1 d . U . . .
H12D H 0.7397 -0.1355 0.0981 0.251 Uiso 1 1 calc R U . . .
H12E H 0.8349 -0.1584 0.0871 0.251 Uiso 1 1 calc R U . . .
H12F H 0.7932 -0.1883 0.1529 0.251 Uiso 1 1 calc R U . . .
C123 C 0.7960(9) -0.0116(9) 0.0817(10) 0.184(6) Uani 1 1 d . U . . .
H12G H 0.7456 0.0049 0.0618 0.276 Uiso 1 1 calc R U . . .
H12H H 0.8044 0.0303 0.0949 0.276 Uiso 1 1 calc R U . . .
H12I H 0.8401 -0.0285 0.0524 0.276 Uiso 1 1 calc R U . . .
C124 C 0.8728(9) -0.0988(10) 0.1661(10) 0.206(7) Uani 1 1 d . U . . .
H12J H 0.8734 -0.1404 0.2023 0.308 Uiso 1 1 calc R U . . .
H12K H 0.9160 -0.1148 0.1359 0.308 Uiso 1 1 calc R U . . .
H12L H 0.8803 -0.0560 0.1784 0.308 Uiso 1 1 calc R U . . .
C125 C 0.6863(14) -0.0432(13) 0.3562(12) 0.195(6) Uani 1 1 d . U . . .
C126 C 0.6343(14) 0.0258(13) 0.3738(11) 0.243(9) Uani 1 1 d . U . . .
H12M H 0.5784 0.0295 0.3697 0.364 Uiso 1 1 calc R U . . .
H12N H 0.6415 0.0237 0.4166 0.364 Uiso 1 1 calc R U . . .
H12O H 0.6488 0.0698 0.3468 0.364 Uiso 1 1 calc R U . . .
C127 C 0.7721(13) -0.0535(13) 0.3610(11) 0.256(10) Uani 1 1 d . U . . .
H12P H 0.8031 -0.0998 0.3488 0.385 Uiso 1 1 calc R U . . .
H12Q H 0.7887 -0.0107 0.3338 0.385 Uiso 1 1 calc R U . . .
H12R H 0.7814 -0.0569 0.4036 0.385 Uiso 1 1 calc R U . . .
C128 C 0.6577(16) -0.1093(14) 0.3941(12) 0.268(10) Uani 1 1 d . U . . .
H12S H 0.6007 -0.1000 0.3895 0.403 Uiso 1 1 calc R U . . .
H12T H 0.6876 -0.1545 0.3799 0.403 Uiso 1 1 calc R U . . .
H12U H 0.6663 -0.1163 0.4375 0.403 Uiso 1 1 calc R U . . .
N1 N 0.1973(6) 0.5157(6) 0.1204(5) 0.086(3) Uani 1 1 d . U . . .
C129 C 0.2017(9) 0.5735(8) 0.1107(7) 0.104(5) Uani 1 1 d . U . . .
C130 C 0.2097(10) 0.6539(7) 0.0962(7) 0.142(6) Uani 1 1 d . U . . .
H13D H 0.2619 0.6556 0.0747 0.213 Uiso 1 1 calc R U . . .
H13E H 0.2049 0.6701 0.1347 0.213 Uiso 1 1 calc R U . . .
H13F H 0.1675 0.6873 0.0700 0.213 Uiso 1 1 calc R U . . .
O1 O 0.1614(4) 0.3063(4) 0.1501(4) 0.080(2) Uani 1 1 d . U . . .
O2 O 0.0730(5) 0.4438(3) 0.1723(4) 0.078(2) Uani 1 1 d . U . . .
O3 O 0.0724(5) 0.3777(5) 0.4875(5) 0.112(3) Uani 1 1 d . U . . .
H3A H 0.0485 0.4236 0.4781 0.168 Uiso 1 1 calc DR U . . .
O4 O -0.1981(5) 0.4103(4) 0.5212(4) 0.109(3) Uani 1 1 d . U . . .
H4 H -0.1503 0.4123 0.5152 0.163 Uiso 1 1 calc R U . . .
O5 O 0.2880(5) 0.3681(4) 0.1082(4) 0.083(2) Uani 1 1 d . U . . .
O6 O 0.2168(4) 0.3883(4) 0.2212(4) 0.080(2) Uani 1 1 d . U . . .
O7 O 0.3556(5) -0.0077(4) 0.1398(4) 0.114(3) Uani 1 1 d . U . . .
H7 H 0.3725 0.0272 0.1443 0.171 Uiso 1 1 calc R U . . .
O8 O 0.6282(6) -0.0320(5) 0.1073(6) 0.136(4) Uani 1 1 d . U . . .
H8 H 0.5899 0.0051 0.0950 0.203 Uiso 1 1 calc DR U . . .
N2 N 0.8711(15) 0.3079(13) 0.0323(10) 0.266(11) Uani 1 1 d D U . . .
C131 C 0.8989(10) 0.3396(9) 0.0554(7) 0.127(6) Uani 1 1 d D U . . .
C132 C 0.9377(8) 0.3776(7) 0.0844(6) 0.111(5) Uani 1 1 d D U . . .
H13G H 0.9719 0.3408 0.1153 0.167 Uiso 1 1 calc R U . . .
H13H H 0.8972 0.4133 0.1043 0.167 Uiso 1 1 calc R U . . .
H13I H 0.9704 0.4047 0.0532 0.167 Uiso 1 1 calc R U . . .
N3 N 0.3771(12) 0.5841(8) 0.1651(11) 0.264(11) Uani 1 1 d D U . . .
C133 C 0.4048(10) 0.5219(9) 0.1792(9) 0.153(7) Uani 1 1 d D U . . .
C134 C 0.4482(9) 0.4449(7) 0.1957(9) 0.163(7) Uani 1 1 d D U . . .
H13J H 0.4458 0.4199 0.1635 0.244 Uiso 1 1 calc R U . . .
H13K H 0.4245 0.4206 0.2348 0.244 Uiso 1 1 calc R U . . .
H13L H 0.5040 0.4413 0.2003 0.244 Uiso 1 1 calc R U . . .
N4 N 0.4999(12) -0.0717(13) -0.0423(9) 0.248(11) Uani 1 1 d D U . . .
C135 C 0.5301(10) -0.1086(11) 0.0009(9) 0.154(7) Uani 1 1 d D U . . .
C136 C 0.5691(9) -0.1525(8) 0.0564(7) 0.129(6) Uani 1 1 d D U . . .
H13M H 0.6231 -0.1809 0.0453 0.194 Uiso 1 1 calc R U . . .
H13N H 0.5383 -0.1873 0.0798 0.194 Uiso 1 1 calc R U . . .
H13O H 0.5721 -0.1189 0.0817 0.194 Uiso 1 1 calc R U . . .
N5 N 0.084(3) 0.910(3) 0.049(2) 0.34(3) Uiso 0.5 1 d D . P . .
C137 C 0.0740(17) 0.8648(17) 0.0257(13) 0.121(10) Uiso 0.5 1 d D . P . .
C138 C 0.018(3) 0.817(2) 0.032(2) 0.24(2) Uiso 0.5 1 d D . P . .
H13P H 0.0305 0.7909 -0.0019 0.367 Uiso 0.5 1 calc R U P . .
H13Q H -0.0372 0.8487 0.0300 0.367 Uiso 0.5 1 calc R U P . .
H13R H 0.0235 0.7800 0.0713 0.367 Uiso 0.5 1 calc R U P . .
N6 N -0.1974(19) 0.0239(16) 0.6736(16) 0.206(14) Uiso 0.5 1 d D . P . .
C139 C -0.246(2) 0.0852(18) 0.6697(19) 0.187(16) Uiso 0.5 1 d D . P . .
C140 C -0.3152(15) 0.1533(14) 0.6640(12) 0.111(9) Uiso 0.5 1 d D . P . .
H14D H -0.3520 0.1509 0.6362 0.166 Uiso 0.5 1 calc R U P . .
H14E H -0.2962 0.1984 0.6474 0.166 Uiso 0.5 1 calc R U P . .
H14F H -0.3429 0.1553 0.7046 0.166 Uiso 0.5 1 calc R U P . .
N7 N 0.320(2) 0.1010(17) 0.4634(17) 0.220(15) Uiso 0.5 1 d D . P . .
C141 C 0.283(2) 0.1620(18) 0.4451(18) 0.177(15) Uiso 0.5 1 d D . P . .
C142 C 0.2435(18) 0.2421(15) 0.4290(14) 0.137(11) Uiso 0.5 1 d D . P . .
H14G H 0.2065 0.2560 0.4635 0.206 Uiso 0.5 1 calc R U P . .
H14H H 0.2136 0.2532 0.3926 0.206 Uiso 0.5 1 calc R U P . .
H14I H 0.2834 0.2708 0.4201 0.206 Uiso 0.5 1 calc R U P . .


_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
Nb1 O1 1.873(7) . ?
Nb1 O6 1.916(8) . ?
Nb1 O2 1.925(8) . ?
Nb1 O5 1.928(8) . ?
Nb1 N1 2.246(10) . ?
Nb1 Cl1 2.420(4) . ?
C1 O1 1.363(13) . ?
C1 C2 1.401(16) . ?
C1 C6 1.414(16) . ?
C2 C3 1.379(15) . ?
C2 C15 1.552(16) . ?
C3 C4 1.387(17) . ?
C4 C5 1.393(18) . ?
C4 C7 1.49(2) . ?
C5 C6 1.405(16) . ?
C6 C11 1.547(17) . ?
C7 C8 1.40(2) . ?
C7 C10 1.52(2) . ?
C7 C9 1.58(2) . ?
C11 C12 1.516(16) . ?
C11 C14 1.578(15) . ?
C11 C13 1.587(15) . ?
C15 C30 1.544(16) . ?
C15 C21 1.544(15) . ?
C16 O2 1.387(13) . ?
C16 C21 1.414(15) . ?
C16 C17 1.416(15) . ?
C17 C18 1.412(15) . ?
C17 C22 1.539(16) . ?
C18 C19 1.423(16) . ?
C19 C20 1.374(15) . ?
C19 C26 1.533(18) . ?
C20 C21 1.356(15) . ?
C22 C23 1.510(16) . ?
C22 C24 1.540(15) . ?
C22 C25 1.554(15) . ?
C26 C29 1.506(17) . ?
C26 C27 1.517(18) . ?
C26 C28 1.528(18) . ?
C30 C31 1.381(15) . ?
C30 C35 1.383(16) . ?
C31 C32 1.400(17) . ?
C32 C33 1.400(17) . ?
C33 C34 1.403(17) . ?
C34 C35 1.390(16) . ?
C34 C36 1.535(17) . ?
C36 C42 1.491(17) . ?
C36 C56 1.525(17) . ?
C37 C42 1.394(18) . ?
C37 O3 1.398(16) . ?
C37 C38 1.404(18) . ?
C38 C39 1.399(17) . ?
C38 C43 1.524(18) . ?
C39 C40 1.380(18) . ?
C40 C41 1.372(18) . ?
C40 C47 1.559(19) . ?
C41 C42 1.409(17) . ?
C43 C46 1.514(17) . ?
C43 C44 1.518(16) . ?
C43 C45 1.537(18) . ?
C47 C49 1.486(18) . ?
C47 C48 1.566(17) . ?
C47 C50 1.588(19) . ?
C51 C52 1.346(17) . ?
C51 O4 1.369(14) . ?
C51 C56 1.439(18) . ?
C52 C53 1.397(17) . ?
C52 C57 1.55(2) . ?
C53 C54 1.445(19) . ?
C54 C55 1.356(18) . ?
C54 C61 1.57(2) . ?
C55 C56 1.349(16) . ?
C57 C58 1.53(2) . ?
C57 C60 1.53(2) . ?
C57 C59 1.55(2) . ?
C61 C63 1.42(3) . ?
C61 C62 1.44(2) . ?
C61 C64 1.60(3) . ?
C65 O5 1.368(14) . ?
C65 C70 1.403(18) . ?
C65 C66 1.407(17) . ?
C66 C67 1.395(17) . ?
C66 C79 1.530(17) . ?
C67 C68 1.347(19) . ?
C68 C69 1.40(2) . ?
C68 C71 1.50(2) . ?
C69 C70 1.342(17) . ?
C70 C75 1.58(2) . ?
C71 C72 1.451(13) . ?
C71 C73 1.478(14) . ?
C71 C74 1.539(14) . ?
C75 C77 1.534(16) . ?
C75 C76 1.545(17) . ?
C75 C78 1.549(18) . ?
C79 C85 1.528(16) . ?
C79 C94 1.567(17) . ?
C80 O6 1.361(13) . ?
C80 C85 1.400(16) . ?
C80 C81 1.419(16) . ?
C81 C82 1.405(16) . ?
C81 C86 1.523(16) . ?
C82 C83 1.407(19) . ?
C83 C84 1.393(18) . ?
C83 C90 1.53(2) . ?
C84 C85 1.363(16) . ?
C86 C87 1.534(16) . ?
C86 C89 1.551(16) . ?
C86 C88 1.559(15) . ?
C90 C92 1.440(14) . ?
C90 C93 1.482(14) . ?
C90 C91 1.508(14) . ?
C94 C99 1.372(17) . ?
C94 C95 1.425(16) . ?
C95 C96 1.395(16) . ?
C96 C97 1.372(17) . ?
C96 C100 1.501(17) . ?
C97 C98 1.357(18) . ?
C98 C99 1.423(17) . ?
C100 C120 1.536(17) . ?
C100 C106 1.563(15) . ?
C101 O7 1.367(13) . ?
C101 C106 1.403(16) . ?
C101 C102 1.422(16) . ?
C102 C103 1.404(16) . ?
C102 C107 1.522(18) . ?
C103 C104 1.383(16) . ?
C104 C105 1.396(15) . ?
C104 C111 1.519(18) . ?
C105 C106 1.417(15) . ?
C107 C109 1.535(17) . ?
C107 C110 1.541(16) . ?
C107 C108 1.557(19) . ?
C111 C114 1.459(19) . ?
C111 C112 1.48(2) . ?
C111 C113 1.52(2) . ?
C115 O8 1.386(18) . ?
C115 C116 1.393(19) . ?
C115 C120 1.44(2) . ?
C116 C117 1.41(2) . ?
C116 C121 1.56(2) . ?
C117 C118 1.37(2) . ?
C118 C119 1.38(2) . ?
C118 C125 1.61(3) . ?
C119 C120 1.37(2) . ?
C121 C124 1.52(2) . ?
C121 C123 1.53(2) . ?
C121 C122 1.541(19) . ?
C125 C127 1.48(3) . ?
C125 C126 1.49(3) . ?
C125 C128 1.51(3) . ?
N1 C129 1.095(13) . ?
C129 C130 1.533(17) . ?
N2 C131 1.135(13) . ?
C131 C132 1.444(13) . ?
N3 C133 1.126(13) . ?
C133 C134 1.425(13) . ?
N4 C135 1.140(14) . ?
C135 C136 1.450(14) . ?
N5 C137 1.174(19) . ?
C137 C138 1.501(18) . ?
N6 C139 1.222(16) . ?
C139 C140 1.496(17) . ?
N7 C141 1.158(17) . ?
C141 C142 1.461(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O6 101.7(3) . . ?
O1 Nb1 O2 93.8(3) . . ?
O6 Nb1 O2 89.7(3) . . ?
O1 Nb1 O5 92.9(3) . . ?
O6 Nb1 O5 91.1(3) . . ?
O2 Nb1 O5 173.0(3) . . ?
O1 Nb1 N1 172.5(4) . . ?
O6 Nb1 N1 85.8(3) . . ?
O2 Nb1 N1 86.5(3) . . ?
O5 Nb1 N1 86.7(3) . . ?
O1 Nb1 Cl1 93.1(2) . . ?
O6 Nb1 Cl1 165.3(2) . . ?
O2 Nb1 Cl1 89.6(2) . . ?
O5 Nb1 Cl1 87.8(3) . . ?
N1 Nb1 Cl1 79.5(3) . . ?
O1 C1 C2 118.5(12) . . ?
O1 C1 C6 122.6(14) . . ?
C2 C1 C6 118.8(13) . . ?
C3 C2 C1 120.2(13) . . ?
C3 C2 C15 119.2(13) . . ?
C1 C2 C15 120.5(12) . . ?
C2 C3 C4 123.0(15) . . ?
C3 C4 C5 115.9(14) . . ?
C3 C4 C7 122.3(16) . . ?
C5 C4 C7 121.6(15) . . ?
C4 C5 C6 123.7(14) . . ?
C5 C6 C1 117.8(14) . . ?
C5 C6 C11 120.7(12) . . ?
C1 C6 C11 121.4(12) . . ?
C8 C7 C4 110.1(14) . . ?
C8 C7 C10 118.0(19) . . ?
C4 C7 C10 111.8(16) . . ?
C8 C7 C9 109(2) . . ?
C4 C7 C9 108.4(17) . . ?
C10 C7 C9 98.6(15) . . ?
C12 C11 C6 110.3(10) . . ?
C12 C11 C14 111.4(11) . . ?
C6 C11 C14 110.4(11) . . ?
C12 C11 C13 108.2(11) . . ?
C6 C11 C13 111.6(11) . . ?
C14 C11 C13 104.8(10) . . ?
C30 C15 C21 113.7(11) . . ?
C30 C15 C2 113.8(10) . . ?
C21 C15 C2 107.8(10) . . ?
O2 C16 C21 119.4(11) . . ?
O2 C16 C17 119.4(12) . . ?
C21 C16 C17 121.2(13) . . ?
C18 C17 C16 115.0(12) . . ?
C18 C17 C22 120.9(11) . . ?
C16 C17 C22 124.1(12) . . ?
C17 C18 C19 124.1(12) . . ?
C20 C19 C18 116.4(13) . . ?
C20 C19 C26 124.2(13) . . ?
C18 C19 C26 119.4(12) . . ?
C21 C20 C19 123.0(12) . . ?
C20 C21 C16 119.9(12) . . ?
C20 C21 C15 120.5(12) . . ?
C16 C21 C15 119.5(11) . . ?
C23 C22 C17 110.2(11) . . ?
C23 C22 C24 110.2(11) . . ?
C17 C22 C24 109.4(10) . . ?
C23 C22 C25 108.1(10) . . ?
C17 C22 C25 111.3(11) . . ?
C24 C22 C25 107.6(10) . . ?
C29 C26 C27 109.5(13) . . ?
C29 C26 C28 106.9(14) . . ?
C27 C26 C28 109.2(12) . . ?
C29 C26 C19 110.8(12) . . ?
C27 C26 C19 112.1(13) . . ?
C28 C26 C19 108.3(12) . . ?
C31 C30 C35 119.9(14) . . ?
C31 C30 C15 117.6(13) . . ?
C35 C30 C15 122.3(12) . . ?
C30 C31 C32 119.3(14) . . ?
C33 C32 C31 120.7(14) . . ?
C32 C33 C34 119.8(15) . . ?
C35 C34 C33 118.2(14) . . ?
C35 C34 C36 119.3(13) . . ?
C33 C34 C36 122.3(14) . . ?
C30 C35 C34 122.1(13) . . ?
C42 C36 C56 114.3(13) . . ?
C42 C36 C34 113.1(12) . . ?
C56 C36 C34 109.2(11) . . ?
C42 C37 O3 117.4(15) . . ?
C42 C37 C38 124.3(17) . . ?
O3 C37 C38 118.1(15) . . ?
C39 C38 C37 114.0(16) . . ?
C39 C38 C43 123.5(15) . . ?
C37 C38 C43 122.1(16) . . ?
C40 C39 C38 124.6(16) . . ?
C41 C40 C39 118.2(17) . . ?
C41 C40 C47 118.8(15) . . ?
C39 C40 C47 123.0(16) . . ?
C40 C41 C42 121.7(16) . . ?
C37 C42 C41 116.9(16) . . ?
C37 C42 C36 122.1(15) . . ?
C41 C42 C36 120.8(14) . . ?
C46 C43 C44 108.8(12) . . ?
C46 C43 C38 110.6(13) . . ?
C44 C43 C38 111.5(12) . . ?
C46 C43 C45 105.8(12) . . ?
C44 C43 C45 110.2(13) . . ?
C38 C43 C45 109.8(12) . . ?
C49 C47 C40 115.9(14) . . ?
C49 C47 C48 111.0(13) . . ?
C40 C47 C48 106.9(12) . . ?
C49 C47 C50 105.2(14) . . ?
C40 C47 C50 110.5(12) . . ?
C48 C47 C50 107.0(12) . . ?
C52 C51 O4 120.5(14) . . ?
C52 C51 C56 120.4(14) . . ?
O4 C51 C56 119.1(13) . . ?
C51 C52 C53 119.2(15) . . ?
C51 C52 C57 120.4(14) . . ?
C53 C52 C57 120.3(14) . . ?
C52 C53 C54 120.9(15) . . ?
C55 C54 C53 116.7(14) . . ?
C55 C54 C61 125.7(17) . . ?
C53 C54 C61 117.5(15) . . ?
C56 C55 C54 123.6(16) . . ?
C55 C56 C51 119.0(14) . . ?
C55 C56 C36 123.5(14) . . ?
C51 C56 C36 117.6(12) . . ?
C58 C57 C60 107.2(16) . . ?
C58 C57 C59 109.1(14) . . ?
C60 C57 C59 106.3(16) . . ?
C58 C57 C52 112.1(15) . . ?
C60 C57 C52 112.6(14) . . ?
C59 C57 C52 109.4(15) . . ?
C63 C61 C62 121(2) . . ?
C63 C61 C54 109(2) . . ?
C62 C61 C54 116.3(19) . . ?
C63 C61 C64 105(2) . . ?
C62 C61 C64 98(2) . . ?
C54 C61 C64 104.4(19) . . ?
O5 C65 C70 123.9(15) . . ?
O5 C65 C66 117.8(15) . . ?
C70 C65 C66 118.4(15) . . ?
C67 C66 C65 119.7(16) . . ?
C67 C66 C79 120.5(14) . . ?
C65 C66 C79 119.7(13) . . ?
C68 C67 C66 121.9(17) . . ?
C67 C68 C69 116.7(16) . . ?
C67 C68 C71 122.5(17) . . ?
C69 C68 C71 120.7(17) . . ?
C70 C69 C68 124.5(18) . . ?
C69 C70 C65 118.5(17) . . ?
C69 C70 C75 120.2(16) . . ?
C65 C70 C75 121.2(15) . . ?
C72 C71 C73 109.7(12) . . ?
C72 C71 C68 113.8(14) . . ?
C73 C71 C68 111.9(13) . . ?
C72 C71 C74 103.0(11) . . ?
C73 C71 C74 101.2(11) . . ?
C68 C71 C74 116.2(16) . . ?
C77 C75 C76 109.6(11) . . ?
C77 C75 C78 107.7(12) . . ?
C76 C75 C78 108.8(13) . . ?
C77 C75 C70 111.0(12) . . ?
C76 C75 C70 107.1(12) . . ?
C78 C75 C70 112.7(13) . . ?
C85 C79 C66 110.5(10) . . ?
C85 C79 C94 111.7(11) . . ?
C66 C79 C94 115.7(11) . . ?
O6 C80 C85 117.6(12) . . ?
O6 C80 C81 122.2(11) . . ?
C85 C80 C81 120.2(13) . . ?
C82 C81 C80 116.9(13) . . ?
C82 C81 C86 119.9(12) . . ?
C80 C81 C86 123.2(12) . . ?
C81 C82 C83 123.7(14) . . ?
C84 C83 C82 115.7(14) . . ?
C84 C83 C90 123.6(14) . . ?
C82 C83 C90 120.7(14) . . ?
C85 C84 C83 123.5(14) . . ?
C84 C85 C80 119.8(13) . . ?
C84 C85 C79 118.5(12) . . ?
C80 C85 C79 121.7(12) . . ?
C81 C86 C87 111.7(10) . . ?
C81 C86 C89 114.1(11) . . ?
C87 C86 C89 106.9(11) . . ?
C81 C86 C88 108.9(11) . . ?
C87 C86 C88 108.7(11) . . ?
C89 C86 C88 106.4(10) . . ?
C92 C90 C93 109.4(13) . . ?
C92 C90 C91 105.6(13) . . ?
C93 C90 C91 105.6(11) . . ?
C92 C90 C83 116.1(15) . . ?
C93 C90 C83 110.7(16) . . ?
C91 C90 C83 108.8(15) . . ?
C99 C94 C95 120.2(13) . . ?
C99 C94 C79 120.4(13) . . ?
C95 C94 C79 119.3(14) . . ?
C96 C95 C94 119.7(14) . . ?
C97 C96 C95 118.7(15) . . ?
C97 C96 C100 124.3(14) . . ?
C95 C96 C100 117.0(14) . . ?
C98 C97 C96 122.6(15) . . ?
C97 C98 C99 119.8(16) . . ?
C94 C99 C98 118.9(15) . . ?
C96 C100 C120 110.5(12) . . ?
C96 C100 C106 113.8(11) . . ?
C120 C100 C106 111.5(10) . . ?
O7 C101 C106 120.9(11) . . ?
O7 C101 C102 118.1(12) . . ?
C106 C101 C102 120.9(12) . . ?
C103 C102 C101 115.2(13) . . ?
C103 C102 C107 123.5(12) . . ?
C101 C102 C107 121.3(12) . . ?
C104 C103 C102 126.1(12) . . ?
C103 C104 C105 117.1(12) . . ?
C103 C104 C111 123.1(13) . . ?
C105 C104 C111 119.6(13) . . ?
C104 C105 C106 120.3(13) . . ?
C101 C106 C105 120.3(11) . . ?
C101 C106 C100 118.3(11) . . ?
C105 C106 C100 121.3(11) . . ?
C102 C107 C109 108.2(13) . . ?
C102 C107 C110 110.6(12) . . ?
C109 C107 C110 107.1(12) . . ?
C102 C107 C108 110.5(13) . . ?
C109 C107 C108 113.5(13) . . ?
C110 C107 C108 106.8(13) . . ?
C114 C111 C112 112.1(18) . . ?
C114 C111 C104 115.7(14) . . ?
C112 C111 C104 114.7(14) . . ?
C114 C111 C113 109.2(15) . . ?
C112 C111 C113 97.6(14) . . ?
C104 C111 C113 105.5(14) . . ?
O8 C115 C116 117.8(19) . . ?
O8 C115 C120 122.3(15) . . ?
C116 C115 C120 120(2) . . ?
C115 C116 C117 118(2) . . ?
C115 C116 C121 123(2) . . ?
C117 C116 C121 118.2(16) . . ?
C118 C117 C116 121.9(19) . . ?
C117 C118 C119 119(2) . . ?
C117 C118 C125 122.7(19) . . ?
C119 C118 C125 118(2) . . ?
C120 C119 C118 122(2) . . ?
C119 C120 C115 118.6(15) . . ?
C119 C120 C100 124.3(17) . . ?
C115 C120 C100 116.9(16) . . ?
C124 C121 C123 106.7(15) . . ?
C124 C121 C122 104.7(13) . . ?
C123 C121 C122 110.3(18) . . ?
C124 C121 C116 113.8(18) . . ?
C123 C121 C116 110.5(13) . . ?
C122 C121 C116 110.6(14) . . ?
C127 C125 C126 113(2) . . ?
C127 C125 C128 112(2) . . ?
C126 C125 C128 108(2) . . ?
C127 C125 C118 109(2) . . ?
C126 C125 C118 108.7(18) . . ?
C128 C125 C118 104.4(18) . . ?
C129 N1 Nb1 176.3(12) . . ?
N1 C129 C130 178.7(18) . . ?
C1 O1 Nb1 156.6(8) . . ?
C16 O2 Nb1 155.1(7) . . ?
C65 O5 Nb1 158.2(9) . . ?
C80 O6 Nb1 157.3(8) . . ?
N2 C131 C132 177(2) . . ?
N3 C133 C134 174(2) . . ?
N4 C135 C136 177(3) . . ?
N5 C137 C138 140(3) . . ?
N6 C139 C140 170(4) . . ?
N7 C141 C142 171(5) . . ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.056



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr514
_database_code_depnum_ccdc_archive 'CCDC 1043851'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H92 Cl6 N2 Nb2 O4, 6(C2 H3 N)'
_chemical_formula_sum            'C80 H110 Cl6 N8 Nb2 O4'
_chemical_formula_weight         1646.27

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

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

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

_cell_length_a                   10.8601(8)
_cell_length_b                   12.1510(9)
_cell_length_c                   17.9452(13)
_cell_angle_alpha                72.153(13)
_cell_angle_beta                 79.492(15)
_cell_angle_gamma                77.185(14)
_cell_volume                     2181.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      25.0

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             862
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.495
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20034
_diffrn_reflns_av_unetI/netI     0.1240
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.403
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             7527
_reflns_number_gt                4629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1042P)²+2.4637P] 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         7527
_refine_ls_number_parameters     546
_refine_ls_number_restraints     465
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2070
_refine_ls_wR_factor_gt          0.1761
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.49707(7) 0.27876(6) 0.85054(3) 0.0251(2) Uani 1 1 d . . . . .
Cl1 Cl 0.59390(19) 0.08200(17) 0.90859(11) 0.0395(5) Uani 1 1 d . . . . .
Cl2 Cl 0.40869(19) 0.20704(17) 0.76603(10) 0.0364(5) Uani 1 1 d . . . . .
Cl3 Cl 0.5462(2) 0.33172(18) 0.95764(10) 0.0398(5) Uani 1 1 d . . . . .
O1 O 0.3964(4) 0.4276(4) 0.8163(2) 0.0247(11) Uani 1 1 d . . . . .
O2 O 0.6452(4) 0.3138(4) 0.7849(2) 0.0247(11) Uani 1 1 d . . . . .
C1 C 0.3620(6) 0.5417(6) 0.7733(3) 0.0208(15) Uani 1 1 d . . . . .
C2 C 0.2629(7) 0.6194(6) 0.8031(4) 0.0236(15) Uani 1 1 d . . . . .
C3 C 0.2459(7) 0.7363(6) 0.7588(4) 0.0256(16) Uani 1 1 d . . . . .
H3 H 0.1838 0.7914 0.7796 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3152(7) 0.7775(6) 0.6854(4) 0.0243(16) Uani 1 1 d . . . . .
C5 C 0.4068(7) 0.6966(6) 0.6557(4) 0.0263(16) Uani 1 1 d . . . . .
H5 H 0.4554 0.7227 0.6061 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4290(6) 0.5778(6) 0.6974(3) 0.0209(15) Uani 1 1 d . . . . .
C7 C 0.1725(6) 0.5776(6) 0.8790(4) 0.0287(17) Uani 1 1 d D . . . .
C8 C 0.2442(8) 0.5314(7) 0.9518(4) 0.038(2) Uani 1 1 d D . . . .
H8A H 0.3084 0.4624 0.9470 0.057 Uiso 1 1 calc R U . . .
H8B H 0.1839 0.5095 0.9993 0.057 Uiso 1 1 calc R U . . .
H8C H 0.2860 0.5928 0.9556 0.057 Uiso 1 1 calc R U . . .
C9 C 0.1103(7) 0.4821(6) 0.8699(4) 0.0312(17) Uani 1 1 d D . . . .
H9A H 0.1764 0.4186 0.8577 0.047 Uiso 1 1 calc R U . . .
H9B H 0.0568 0.5155 0.8271 0.047 Uiso 1 1 calc R U . . .
H9C H 0.0576 0.4508 0.9193 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0654(7) 0.6780(7) 0.8928(4) 0.042(2) Uani 1 1 d D . . . .
H10A H 0.0058 0.6476 0.9387 0.062 Uiso 1 1 calc R U . . .
H10B H 0.0203 0.7120 0.8461 0.062 Uiso 1 1 calc R U . . .
H10C H 0.1018 0.7388 0.9023 0.062 Uiso 1 1 calc R U . . .
C11 C 0.2935(7) 0.9075(6) 0.6389(4) 0.0391(18) Uani 1 1 d D U . . .
C12_a C 0.1956(15) 0.9836(13) 0.6811(8) 0.049(4) Uani 0.556(11) 1 d D U P A 1
H12A_a H 0.2175 0.9708 0.7341 0.073 Uiso 0.556(11) 1 calc R U P A 1
H12B_a H 0.1117 0.9633 0.6852 0.073 Uiso 0.556(11) 1 calc R U P A 1
H12C_a H 0.1937 1.0664 0.6516 0.073 Uiso 0.556(11) 1 calc R U P A 1
C13_a C 0.2692(19) 0.9187(13) 0.5573(7) 0.056(4) Uani 0.556(11) 1 d D U P A 1
H13A_a H 0.2554 1.0019 0.5274 0.084 Uiso 0.556(11) 1 calc R U P A 1
H13B_a H 0.1934 0.8857 0.5600 0.084 Uiso 0.556(11) 1 calc R U P A 1
H13C_a H 0.3428 0.8760 0.5309 0.084 Uiso 0.556(11) 1 calc R U P A 1
C14_a C 0.4256(12) 0.9477(13) 0.6312(10) 0.054(4) Uani 0.556(11) 1 d D U P A 1
H14A_a H 0.4443 0.9425 0.6837 0.080 Uiso 0.556(11) 1 calc R U P A 1
H14B_a H 0.4211 1.0290 0.5981 0.080 Uiso 0.556(11) 1 calc R U P A 1
H14C_a H 0.4931 0.8964 0.6071 0.080 Uiso 0.556(11) 1 calc R U P A 1
C12X_b C 0.1496(13) 0.9397(16) 0.6224(11) 0.048(4) Uani 0.444(11) 1 d D U P A 2
H12D_b H 0.0943 0.9190 0.6724 0.072 Uiso 0.444(11) 1 calc R U P A 2
H12E_b H 0.1373 0.8958 0.5875 0.072 Uiso 0.444(11) 1 calc R U P A 2
H12F_b H 0.1281 1.0241 0.5971 0.072 Uiso 0.444(11) 1 calc R U P A 2
C13X_b C 0.3666(19) 0.9429(16) 0.5567(8) 0.045(5) Uani 0.444(11) 1 d D U P A 2
H13D_b H 0.3435 1.0278 0.5337 0.067 Uiso 0.444(11) 1 calc R U P A 2
H13E_b H 0.3451 0.9013 0.5232 0.067 Uiso 0.444(11) 1 calc R U P A 2
H13F_b H 0.4582 0.9222 0.5605 0.067 Uiso 0.444(11) 1 calc R U P A 2
C14X_b C 0.300(2) 0.9903(14) 0.6861(9) 0.044(4) Uani 0.444(11) 1 d D U P A 2
H14D_b H 0.2532 0.9664 0.7387 0.066 Uiso 0.444(11) 1 calc R U P A 2
H14E_b H 0.2631 1.0707 0.6588 0.066 Uiso 0.444(11) 1 calc R U P A 2
H14F_b H 0.3896 0.9873 0.6911 0.066 Uiso 0.444(11) 1 calc R U P A 2
C15 C 0.5241(6) 0.4882(6) 0.6633(4) 0.0230(15) Uani 1 1 d . . . . .
H15 H 0.5020 0.4097 0.6939 0.028 Uiso 1 1 calc R U . . .
C16 C 0.5136(6) 0.5012(6) 0.5763(3) 0.0199(14) Uani 1 1 d . . . . .
C17 C 0.3975(6) 0.5406(7) 0.5474(4) 0.0286(17) Uani 1 1 d . . . . .
H17 H 0.3252 0.5673 0.5801 0.034 Uiso 1 1 calc R U . . .
C18 C 0.6158(7) 0.4579(7) 0.5287(4) 0.0296(17) Uani 1 1 d . . . . .
H18 H 0.6959 0.4268 0.5481 0.035 Uiso 1 1 calc R U . . .
C19 C 0.7202(6) 0.3890(6) 0.7330(4) 0.0212(15) Uani 1 1 d . . . . .
C20 C 0.8512(7) 0.3716(6) 0.7370(4) 0.0274(16) Uani 1 1 d . . . . .
C21 C 0.9149(7) 0.4622(6) 0.6893(4) 0.0279(16) Uani 1 1 d . . . . .
H21 H 1.0029 0.4548 0.6923 0.034 Uiso 1 1 calc R U . . .
C22 C 0.8542(7) 0.5637(7) 0.6370(4) 0.0300(17) Uani 1 1 d . . . . .
C23 C 0.7284(6) 0.5703(6) 0.6310(4) 0.0256(16) Uani 1 1 d . . . . .
H23 H 0.6870 0.6362 0.5943 0.031 Uiso 1 1 calc R U . . .
C24 C 0.6594(6) 0.4838(6) 0.6768(4) 0.0232(15) Uani 1 1 d . . . . .
C25 C 0.9241(6) 0.2583(6) 0.7895(4) 0.0320(17) Uani 1 1 d D . . . .
C26 C 0.8859(8) 0.2505(8) 0.8777(4) 0.041(2) Uani 1 1 d D . . . .
H26A H 0.9305 0.1766 0.9095 0.062 Uiso 1 1 calc R U . . .
H26B H 0.7938 0.2532 0.8907 0.062 Uiso 1 1 calc R U . . .
H26C H 0.9090 0.3167 0.8890 0.062 Uiso 1 1 calc R U . . .
C27 C 0.8973(8) 0.1497(7) 0.7726(5) 0.043(2) Uani 1 1 d D . . . .
H27A H 0.9231 0.1543 0.7166 0.064 Uiso 1 1 calc R U . . .
H27B H 0.8061 0.1472 0.7855 0.064 Uiso 1 1 calc R U . . .
H27C H 0.9455 0.0786 0.8048 0.064 Uiso 1 1 calc R U . . .
C28 C 1.0683(6) 0.2532(7) 0.7719(5) 0.040(2) Uani 1 1 d D . . . .
H28A H 1.0958 0.2554 0.7164 0.060 Uiso 1 1 calc R U . . .
H28B H 1.1112 0.1802 0.8057 0.060 Uiso 1 1 calc R U . . .
H28C H 1.0901 0.3206 0.7824 0.060 Uiso 1 1 calc R U . . .
C29 C 0.9264(7) 0.6623(7) 0.5874(4) 0.0400(18) Uani 1 1 d D U . . .
C30_a C 1.0658(8) 0.6351(10) 0.5941(7) 0.046(3) Uani 0.759(11) 1 d D U P B 1
H30A_a H 1.1032 0.5608 0.5815 0.068 Uiso 0.759(11) 1 calc R U P B 1
H30B_a H 1.0787 0.6283 0.6481 0.068 Uiso 0.759(11) 1 calc R U P B 1
H30C_a H 1.1068 0.6983 0.5572 0.068 Uiso 0.759(11) 1 calc R U P B 1
C31_a C 0.9126(11) 0.6815(11) 0.4975(5) 0.049(3) Uani 0.759(11) 1 d D U P B 1
H31A_a H 0.8222 0.6995 0.4904 0.074 Uiso 0.759(11) 1 calc R U P B 1
H31B_a H 0.9529 0.6098 0.4821 0.074 Uiso 0.759(11) 1 calc R U P B 1
H31C_a H 0.9542 0.7469 0.4644 0.074 Uiso 0.759(11) 1 calc R U P B 1
C32_a C 0.8629(10) 0.7748(9) 0.6068(7) 0.044(3) Uani 0.759(11) 1 d D U P B 1
H32A_a H 0.7719 0.7889 0.6021 0.066 Uiso 0.759(11) 1 calc R U P B 1
H32B_a H 0.9012 0.8400 0.5702 0.066 Uiso 0.759(11) 1 calc R U P B 1
H32C_a H 0.8742 0.7689 0.6610 0.066 Uiso 0.759(11) 1 calc R U P B 1
C30X_b C 0.995(3) 0.694(3) 0.6470(16) 0.050(7) Uani 0.241(11) 1 d D U P B 2
H30D_b H 1.0454 0.6220 0.6775 0.075 Uiso 0.241(11) 1 calc R U P B 2
H30E_b H 0.9316 0.7294 0.6830 0.075 Uiso 0.241(11) 1 calc R U P B 2
H30F_b H 1.0520 0.7493 0.6173 0.075 Uiso 0.241(11) 1 calc R U P B 2
C31X_b C 1.038(2) 0.620(3) 0.5318(16) 0.045(7) Uani 0.241(11) 1 d D U P B 2
H31D_b H 1.0851 0.5450 0.5603 0.067 Uiso 0.241(11) 1 calc R U P B 2
H31E_b H 1.0938 0.6784 0.5121 0.067 Uiso 0.241(11) 1 calc R U P B 2
H31F_b H 1.0053 0.6095 0.4874 0.067 Uiso 0.241(11) 1 calc R U P B 2
C32X_b C 0.850(2) 0.7800(18) 0.5488(18) 0.043(6) Uani 0.241(11) 1 d D U P B 2
H32D_b H 0.9085 0.8345 0.5201 0.064 Uiso 0.241(11) 1 calc R U P B 2
H32E_b H 0.7935 0.8114 0.5894 0.064 Uiso 0.241(11) 1 calc R U P B 2
H32F_b H 0.7998 0.7703 0.5120 0.064 Uiso 0.241(11) 1 calc R U P B 2
N1 N 0.3287(7) 0.2198(6) 0.9377(3) 0.0359(16) Uani 1 1 d . . . . .
C33 C 0.2487(8) 0.1757(7) 0.9785(4) 0.037(2) Uani 1 1 d . . . . .
C34 C 0.1468(7) 0.1184(7) 1.0316(5) 0.039(2) Uani 1 1 d . . . . .
H34A H 0.1589 0.0369 1.0296 0.059 Uiso 1 1 calc R U . . .
H34B H 0.0641 0.1607 1.0149 0.059 Uiso 1 1 calc R U . . .
H34C H 0.1495 0.1194 1.0857 0.059 Uiso 1 1 calc R U . . .
N2 N 0.1579(9) 0.9436(7) 0.9151(4) 0.056(2) Uani 1 1 d . . . . .
C35 C 0.2645(10) 0.9236(7) 0.8982(5) 0.042(2) Uani 1 1 d . . . . .
C36 C 0.3990(9) 0.8989(9) 0.8758(6) 0.056(3) Uani 1 1 d . . . . .
H36A H 0.4269 0.9692 0.8384 0.084 Uiso 1 1 calc R U . . .
H36B H 0.4192 0.8346 0.8509 0.084 Uiso 1 1 calc R U . . .
H36C H 0.4431 0.8761 0.9227 0.084 Uiso 1 1 calc R U . . .
N3 N 0.7417(10) 0.7885(10) 0.8352(7) 0.095(4) Uani 1 1 d . . . . .
C37 C 0.6963(11) 0.7114(11) 0.8374(6) 0.062(3) Uani 1 1 d . . . . .
C38 C 0.6424(12) 0.6144(10) 0.8407(6) 0.071(3) Uani 1 1 d . . . . .
H38A H 0.6017 0.5834 0.8943 0.106 Uiso 1 1 calc R U . . .
H38B H 0.7094 0.5530 0.8262 0.106 Uiso 1 1 calc R U . . .
H38C H 0.5788 0.6391 0.8037 0.106 Uiso 1 1 calc R U . . .
N4_a N 0.892(2) 0.085(3) 0.5756(13) 0.178(11) Uani 0.698(14) 1 d D U P C 1
C39_a C 0.791(2) 0.082(2) 0.6183(12) 0.106(7) Uani 0.698(14) 1 d D U P C 1
C40_a C 0.703(2) 0.034(2) 0.6821(15) 0.124(9) Uani 0.698(14) 1 d D U P C 1
H40A_a H 0.7393 0.0129 0.7316 0.187 Uiso 0.698(14) 1 calc R U P C 1
H40B_a H 0.6826 -0.0364 0.6745 0.187 Uiso 0.698(14) 1 calc R U P C 1
H40C_a H 0.6246 0.0923 0.6841 0.187 Uiso 0.698(14) 1 calc R U P C 1
N4X_b N 0.449(3) 0.217(3) 0.5509(18) 0.087(11) Uani 0.302(14) 1 d D U P C 2
C39X_b C 0.539(4) 0.185(5) 0.589(3) 0.113(15) Uani 0.302(14) 1 d D U P C 2
C40X_b C 0.647(3) 0.144(5) 0.631(2) 0.093(12) Uani 0.302(14) 1 d D U P C 2
H40D_b H 0.6332 0.1785 0.6751 0.139 Uiso 0.302(14) 1 calc R U P C 2
H40E_b H 0.7223 0.1683 0.5951 0.139 Uiso 0.302(14) 1 calc R U P C 2
H40F_b H 0.6607 0.0584 0.6507 0.139 Uiso 0.302(14) 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O2 1.860(5) . ?
Nb1 O1 1.879(5) . ?
Nb1 N1 2.270(6) . ?
Nb1 Cl1 2.380(2) . ?
Nb1 Cl3 2.3828(19) . ?
Nb1 Cl2 2.3860(19) . ?
O1 C1 1.371(8) . ?
O2 C19 1.378(8) . ?
C1 C2 1.408(9) . ?
C1 C6 1.411(8) . ?
C2 C3 1.389(10) . ?
C2 C7 1.546(9) . ?
C3 C4 1.397(9) . ?
C4 C5 1.390(10) . ?
C4 C11 1.532(10) . ?
C5 C6 1.397(10) . ?
C6 C15 1.519(9) . ?
C7 C9 1.528(9) . ?
C7 C10 1.534(9) . ?
C7 C8 1.535(8) . ?
C11 C13_a 1.496(11) . ?
C11 C12_a 1.503(11) . ?
C11 C14X_b 1.521(12) . ?
C11 C13X_b 1.525(12) . ?
C11 C12X_b 1.584(12) . ?
C11 C14_a 1.585(12) . ?
C15 C24 1.519(10) . ?
C15 C16 1.543(8) . ?
C16 C17 1.380(9) . ?
C16 C18 1.382(9) . ?
C17 C18 1.395(9) 2_666 ?
C18 C17 1.395(9) 2_666 ?
C19 C20 1.404(10) . ?
C19 C24 1.405(9) . ?
C20 C21 1.402(10) . ?
C20 C25 1.550(10) . ?
C21 C22 1.411(10) . ?
C22 C23 1.373(10) . ?
C22 C29 1.533(10) . ?
C23 C24 1.391(10) . ?
C25 C28 1.531(9) . ?
C25 C27 1.537(9) . ?
C25 C26 1.541(8) . ?
C29 C30_a 1.495(10) . ?
C29 C32_a 1.501(10) . ?
C29 C32X_b 1.511(14) . ?
C29 C31X_b 1.521(15) . ?
C29 C31_a 1.589(11) . ?
C29 C30X_b 1.589(14) . ?
N1 C33 1.146(10) . ?
C33 C34 1.474(11) . ?
N2 C35 1.134(11) . ?
C35 C36 1.432(14) . ?
N3 C37 1.139(13) . ?
C37 C38 1.409(15) . ?
N4_a C39_a 1.21(2) . ?
C39_a C40_a 1.42(3) . ?
N4X_b C39X_b 1.22(3) . ?
C39X_b C40X_b 1.43(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Nb1 O1 96.6(2) . . ?
O2 Nb1 N1 174.2(2) . . ?
O1 Nb1 N1 89.0(2) . . ?
O2 Nb1 Cl1 92.95(15) . . ?
O1 Nb1 Cl1 170.45(14) . . ?
N1 Nb1 Cl1 81.49(18) . . ?
O2 Nb1 Cl3 94.97(14) . . ?
O1 Nb1 Cl3 90.52(14) . . ?
N1 Nb1 Cl3 83.40(17) . . ?
Cl1 Nb1 Cl3 88.39(7) . . ?
O2 Nb1 Cl2 98.44(14) . . ?
O1 Nb1 Cl2 90.46(15) . . ?
N1 Nb1 Cl2 83.00(17) . . ?
Cl1 Nb1 Cl2 88.39(7) . . ?
Cl3 Nb1 Cl2 166.35(7) . . ?
C1 O1 Nb1 159.5(4) . . ?
C19 O2 Nb1 153.8(4) . . ?
O1 C1 C2 121.5(5) . . ?
O1 C1 C6 117.1(6) . . ?
C2 C1 C6 121.3(6) . . ?
C3 C2 C1 116.7(6) . . ?
C3 C2 C7 120.8(6) . . ?
C1 C2 C7 122.5(6) . . ?
C2 C3 C4 123.6(6) . . ?
C5 C4 C3 117.9(6) . . ?
C5 C4 C11 120.4(6) . . ?
C3 C4 C11 121.7(6) . . ?
C4 C5 C6 121.4(6) . . ?
C5 C6 C1 118.6(6) . . ?
C5 C6 C15 121.5(6) . . ?
C1 C6 C15 119.9(6) . . ?
C9 C7 C10 107.4(6) . . ?
C9 C7 C8 110.6(6) . . ?
C10 C7 C8 107.5(6) . . ?
C9 C7 C2 108.8(5) . . ?
C10 C7 C2 111.3(6) . . ?
C8 C7 C2 111.2(6) . . ?
C13_a C11 C12_a 114.3(10) . . ?
C14X_b C11 C13X_b 110.5(10) . . ?
C13_a C11 C4 109.3(8) . . ?
C12_a C11 C4 113.5(8) . . ?
C14X_b C11 C4 113.9(8) . . ?
C13X_b C11 C4 118.0(9) . . ?
C14X_b C11 C12X_b 103.3(10) . . ?
C13X_b C11 C12X_b 103.3(10) . . ?
C4 C11 C12X_b 106.1(8) . . ?
C13_a C11 C14_a 107.1(10) . . ?
C12_a C11 C14_a 107.1(9) . . ?
C4 C11 C14_a 104.8(8) . . ?
C6 C15 C24 112.1(5) . . ?
C6 C15 C16 113.6(5) . . ?
C24 C15 C16 112.3(5) . . ?
C17 C16 C18 118.0(6) . . ?
C17 C16 C15 120.7(6) . . ?
C18 C16 C15 120.6(6) . . ?
C16 C17 C18 121.4(6) . 2_666 ?
C16 C18 C17 120.5(6) . 2_666 ?
O2 C19 C20 121.1(6) . . ?
O2 C19 C24 117.1(6) . . ?
C20 C19 C24 121.8(6) . . ?
C21 C20 C19 116.3(6) . . ?
C21 C20 C25 121.0(6) . . ?
C19 C20 C25 122.7(6) . . ?
C20 C21 C22 123.0(7) . . ?
C23 C22 C21 117.6(7) . . ?
C23 C22 C29 121.0(7) . . ?
C21 C22 C29 121.4(6) . . ?
C22 C23 C24 122.3(7) . . ?
C23 C24 C19 118.4(6) . . ?
C23 C24 C15 120.9(6) . . ?
C19 C24 C15 120.7(6) . . ?
C28 C25 C27 106.5(6) . . ?
C28 C25 C26 107.6(6) . . ?
C27 C25 C26 109.7(6) . . ?
C28 C25 C20 111.7(6) . . ?
C27 C25 C20 109.9(6) . . ?
C26 C25 C20 111.2(6) . . ?
C30_a C29 C32_a 112.2(8) . . ?
C32X_b C29 C31X_b 112.9(15) . . ?
C30_a C29 C22 114.0(7) . . ?
C32_a C29 C22 109.2(7) . . ?
C32X_b C29 C22 118.4(13) . . ?
C31X_b C29 C22 112.4(14) . . ?
C30_a C29 C31_a 106.8(7) . . ?
C32_a C29 C31_a 106.6(8) . . ?
C22 C29 C31_a 107.6(7) . . ?
C32X_b C29 C30X_b 102.3(15) . . ?
C31X_b C29 C30X_b 102.6(14) . . ?
C22 C29 C30X_b 106.1(13) . . ?
C33 N1 Nb1 170.3(6) . . ?
N1 C33 C34 179.4(9) . . ?
N2 C35 C36 179.2(10) . . ?
N3 C37 C38 178.8(13) . . ?
N4_a C39_a C40_a 157(3) . . ?
N4X_b C39X_b C40X_b 177(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
O2 Nb1 O1 C1 4.6(12) . . . . ?
N1 Nb1 O1 C1 -176.9(12) . . . . ?
Cl3 Nb1 O1 C1 99.7(12) . . . . ?
Cl2 Nb1 O1 C1 -93.9(12) . . . . ?
O1 Nb1 O2 C19 11.5(9) . . . . ?
Cl1 Nb1 O2 C19 -168.3(9) . . . . ?
Cl3 Nb1 O2 C19 -79.6(9) . . . . ?
Cl2 Nb1 O2 C19 102.9(9) . . . . ?
Nb1 O1 C1 C2 -157.9(9) . . . . ?
Nb1 O1 C1 C6 23.0(15) . . . . ?
O1 C1 C2 C3 172.5(6) . . . . ?
C6 C1 C2 C3 -8.3(10) . . . . ?
O1 C1 C2 C7 -10.2(10) . . . . ?
C6 C1 C2 C7 169.0(6) . . . . ?
C1 C2 C3 C4 4.6(10) . . . . ?
C7 C2 C3 C4 -172.8(6) . . . . ?
C2 C3 C4 C5 -0.7(10) . . . . ?
C2 C3 C4 C11 -179.7(7) . . . . ?
C3 C4 C5 C6 0.3(10) . . . . ?
C11 C4 C5 C6 179.4(6) . . . . ?
C4 C5 C6 C1 -4.1(10) . . . . ?
C4 C5 C6 C15 176.7(6) . . . . ?
O1 C1 C6 C5 -172.6(6) . . . . ?
C2 C1 C6 C5 8.2(10) . . . . ?
O1 C1 C6 C15 6.6(9) . . . . ?
C2 C1 C6 C15 -172.5(6) . . . . ?
C3 C2 C7 C9 121.3(7) . . . . ?
C1 C2 C7 C9 -55.9(8) . . . . ?
C3 C2 C7 C10 3.2(9) . . . . ?
C1 C2 C7 C10 -174.0(6) . . . . ?
C3 C2 C7 C8 -116.7(7) . . . . ?
C1 C2 C7 C8 66.1(8) . . . . ?
C5 C4 C11 C13_a 53.9(11) . . . . ?
C3 C4 C11 C13_a -127.1(10) . . . . ?
C5 C4 C11 C12_a -177.2(9) . . . . ?
C3 C4 C11 C12_a 1.8(12) . . . . ?
C5 C4 C11 C14X_b -126.7(11) . . . . ?
C3 C4 C11 C14X_b 52.3(12) . . . . ?
C5 C4 C11 C13X_b 5.3(13) . . . . ?
C3 C4 C11 C13X_b -175.7(10) . . . . ?
C5 C4 C11 C12X_b 120.4(9) . . . . ?
C3 C4 C11 C12X_b -60.6(10) . . . . ?
C5 C4 C11 C14_a -60.7(9) . . . . ?
C3 C4 C11 C14_a 118.4(9) . . . . ?
C5 C6 C15 C24 83.6(7) . . . . ?
C1 C6 C15 C24 -95.7(7) . . . . ?
C5 C6 C15 C16 -45.1(9) . . . . ?
C1 C6 C15 C16 135.7(6) . . . . ?
C6 C15 C16 C17 -32.4(9) . . . . ?
C24 C15 C16 C17 -160.9(7) . . . . ?
C6 C15 C16 C18 157.1(7) . . . . ?
C24 C15 C16 C18 28.6(9) . . . . ?
C18 C16 C17 C18 -2.9(13) . . . 2_666 ?
C15 C16 C17 C18 -173.7(7) . . . 2_666 ?
C17 C16 C18 C17 2.9(12) . . . 2_666 ?
C15 C16 C18 C17 173.7(7) . . . 2_666 ?
Nb1 O2 C19 C20 140.7(7) . . . . ?
Nb1 O2 C19 C24 -38.6(12) . . . . ?
O2 C19 C20 C21 -171.0(6) . . . . ?
C24 C19 C20 C21 8.3(9) . . . . ?
O2 C19 C20 C25 10.3(10) . . . . ?
C24 C19 C20 C25 -170.4(6) . . . . ?
C19 C20 C21 C22 -2.7(10) . . . . ?
C25 C20 C21 C22 176.1(6) . . . . ?
C20 C21 C22 C23 -2.8(10) . . . . ?
C20 C21 C22 C29 178.4(7) . . . . ?
C21 C22 C23 C24 3.0(10) . . . . ?
C29 C22 C23 C24 -178.2(6) . . . . ?
C22 C23 C24 C19 2.3(10) . . . . ?
C22 C23 C24 C15 -174.3(6) . . . . ?
O2 C19 C24 C23 171.0(6) . . . . ?
C20 C19 C24 C23 -8.3(9) . . . . ?
O2 C19 C24 C15 -12.4(9) . . . . ?
C20 C19 C24 C15 168.4(6) . . . . ?
C6 C15 C24 C23 -77.0(7) . . . . ?
C16 C15 C24 C23 52.4(8) . . . . ?
C6 C15 C24 C19 106.5(7) . . . . ?
C16 C15 C24 C19 -124.2(6) . . . . ?
C21 C20 C25 C28 -8.6(9) . . . . ?
C19 C20 C25 C28 170.0(6) . . . . ?
C21 C20 C25 C27 -126.7(7) . . . . ?
C19 C20 C25 C27 52.0(8) . . . . ?
C21 C20 C25 C26 111.7(7) . . . . ?
C19 C20 C25 C26 -69.7(8) . . . . ?
C23 C22 C29 C30_a -173.3(7) . . . . ?
C21 C22 C29 C30_a 5.5(10) . . . . ?
C23 C22 C29 C32_a 60.4(9) . . . . ?
C21 C22 C29 C32_a -120.9(8) . . . . ?
C23 C22 C29 C32X_b 16.4(17) . . . . ?
C21 C22 C29 C32X_b -164.9(16) . . . . ?
C23 C22 C29 C31X_b -118.1(14) . . . . ?
C21 C22 C29 C31X_b 60.6(15) . . . . ?
C23 C22 C29 C31_a -55.0(9) . . . . ?
C21 C22 C29 C31_a 123.7(8) . . . . ?
C23 C22 C29 C30X_b 130.6(14) . . . . ?
C21 C22 C29 C30X_b -50.7(14) . . . . ?

_refine_diff_density_max         1.358
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.123

_shelxl_version_number           2014-1


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr522
_database_code_depnum_ccdc_archive 'CCDC 1043852'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C72 H102 Cl4 N2 Nb2 O6, 3.5(C2 H3 N), 0.614(C7 H8)'
_chemical_formula_sum            'C83.30 H117.41 Cl4 N5.50 Nb2 O6'
_chemical_formula_weight         1619.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.6086(9)
_cell_length_b                   16.8197(12)
_cell_length_c                   21.7135(15)
_cell_angle_alpha                89.714(2)
_cell_angle_beta                 86.846(2)
_cell_angle_gamma                73.006(2)
_cell_volume                     4396.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    73257
_cell_measurement_theta_min      1.6
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             1707
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.432
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            77150
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.691
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             20127
_reflns_number_gt                17091
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_structure_solution    'SHELXT, (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0941P)²+4.4734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         20127
_refine_ls_number_parameters     1054
_refine_ls_number_restraints     322
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.70212(2) 0.06064(2) 0.69625(2) 0.04697(9) Uani 1 1 d . . . . .
Cl1 Cl 0.59623(9) 0.05148(7) 0.60877(5) 0.0660(3) Uani 1 1 d . . . . .
Cl2 Cl 0.87078(10) -0.00802(8) 0.63791(6) 0.0815(4) Uani 1 1 d . . . . .
Nb2 Nb 0.69139(2) 0.65909(2) 0.52970(2) 0.03347(8) Uani 1 1 d . . . . .
Cl3 Cl 0.72120(6) 0.50889(4) 0.53056(3) 0.04150(16) Uani 1 1 d . . . . .
Cl4 Cl 0.57372(6) 0.65529(5) 0.44490(3) 0.04549(17) Uani 1 1 d . . . . .
O1 O 0.57275(17) 0.13122(13) 0.73775(10) 0.0434(5) Uani 1 1 d . . . . .
O2 O 0.79026(17) 0.08341(13) 0.75912(10) 0.0436(5) Uani 1 1 d . . . . .
O3 O 0.57326(15) 0.69146(11) 0.58876(9) 0.0337(4) Uani 1 1 d . . . . .
O4 O 0.79679(15) 0.65062(12) 0.59007(9) 0.0349(4) Uani 1 1 d . . . . .
C1 C 0.5170(2) 0.18668(19) 0.78269(14) 0.0415(6) Uani 1 1 d . . . . .
C2 C 0.4129(3) 0.1822(2) 0.80846(16) 0.0483(7) Uani 1 1 d . . . . .
C3 C 0.3615(3) 0.2405(3) 0.85464(17) 0.0565(9) Uani 1 1 d . . . . .
H3 H 0.2912 0.2392 0.8720 0.068 Uiso 1 1 calc R U . . .
C4 C 0.4068(3) 0.3007(3) 0.87688(16) 0.0547(8) Uani 1 1 d . . . . .
C5 C 0.5092(3) 0.3021(2) 0.85031(14) 0.0440(7) Uani 1 1 d . . . . .
H5 H 0.5428 0.3416 0.8649 0.053 Uiso 1 1 calc R U . . .
C6 C 0.5639(2) 0.24744(18) 0.80294(13) 0.0373(6) Uani 1 1 d . . . . .
C7 C 0.3592(3) 0.1167(2) 0.7867(2) 0.0600(9) Uani 1 1 d . . . . .
C8 C 0.4334(4) 0.0294(3) 0.8016(3) 0.0793(14) Uani 1 1 d . . . . .
H8A H 0.3978 -0.0122 0.7895 0.119 Uiso 1 1 calc R U . . .
H8B H 0.4443 0.0257 0.8460 0.119 Uiso 1 1 calc R U . . .
H8C H 0.5056 0.0191 0.7789 0.119 Uiso 1 1 calc R U . . .
C9 C 0.2451(3) 0.1265(3) 0.8202(2) 0.0736(12) Uani 1 1 d . . . . .
H9A H 0.1958 0.1824 0.8132 0.110 Uiso 1 1 calc R U . . .
H9B H 0.2543 0.1183 0.8645 0.110 Uiso 1 1 calc R U . . .
H9C H 0.2126 0.0850 0.8042 0.110 Uiso 1 1 calc R U . . .
C10 C 0.3415(3) 0.1247(3) 0.7167(2) 0.0661(11) Uani 1 1 d . . . . .
H10A H 0.2917 0.1799 0.7082 0.099 Uiso 1 1 calc R U . . .
H10B H 0.3084 0.0821 0.7035 0.099 Uiso 1 1 calc R U . . .
H10C H 0.4132 0.1172 0.6940 0.099 Uiso 1 1 calc R U . . .
C11 C 0.3473(3) 0.3648(3) 0.92713(19) 0.0755(12) Uani 1 1 d D U . . .
C12 C 0.2274(4) 0.3693(4) 0.9392(3) 0.0569(15) Uani 0.665(8) 1 d D U P A 1
H12A H 0.1912 0.3741 0.9000 0.085 Uiso 0.665(8) 1 calc R U P A 1
H12B H 0.2221 0.3189 0.9603 0.085 Uiso 0.665(8) 1 calc R U P A 1
H12C H 0.1905 0.4180 0.9653 0.085 Uiso 0.665(8) 1 calc R U P A 1
C13 C 0.3381(6) 0.4575(4) 0.8993(3) 0.076(2) Uani 0.665(8) 1 d D U P A 1
H13A H 0.2946 0.4662 0.8625 0.114 Uiso 0.665(8) 1 calc R U P A 1
H13B H 0.3014 0.5000 0.9305 0.114 Uiso 0.665(8) 1 calc R U P A 1
H13C H 0.4127 0.4616 0.8883 0.114 Uiso 0.665(8) 1 calc R U P A 1
C14 C 0.4118(6) 0.3576(6) 0.9805(3) 0.077(2) Uani 0.665(8) 1 d D U P A 1
H14A H 0.4884 0.3551 0.9676 0.116 Uiso 0.665(8) 1 calc R U P A 1
H14B H 0.3797 0.4060 1.0077 0.116 Uiso 0.665(8) 1 calc R U P A 1
H14C H 0.4113 0.3069 1.0027 0.116 Uiso 0.665(8) 1 calc R U P A 1
C12X C 0.2384(11) 0.4091(12) 0.9117(9) 0.107(6) Uani 0.335(8) 1 d D U P A 2
H12D H 0.2032 0.3708 0.8933 0.160 Uiso 0.335(8) 1 calc R U P A 2
H12E H 0.1948 0.4346 0.9490 0.160 Uiso 0.335(8) 1 calc R U P A 2
H12F H 0.2418 0.4526 0.8821 0.160 Uiso 0.335(8) 1 calc R U P A 2
C13X C 0.4244(11) 0.4062(11) 0.9566(7) 0.079(4) Uani 0.335(8) 1 d D U P A 2
H13D H 0.4953 0.3645 0.9634 0.118 Uiso 0.335(8) 1 calc R U P A 2
H13E H 0.4372 0.4494 0.9292 0.118 Uiso 0.335(8) 1 calc R U P A 2
H13F H 0.3903 0.4314 0.9962 0.118 Uiso 0.335(8) 1 calc R U P A 2
C14X C 0.3367(15) 0.3019(10) 0.9834(6) 0.111(5) Uani 0.335(8) 1 d D U P A 2
H14D H 0.4111 0.2703 0.9951 0.166 Uiso 0.335(8) 1 calc R U P A 2
H14E H 0.2955 0.3344 1.0190 0.166 Uiso 0.335(8) 1 calc R U P A 2
H14F H 0.2972 0.2634 0.9698 0.166 Uiso 0.335(8) 1 calc R U P A 2
C15 C 0.6745(2) 0.25293(17) 0.77484(13) 0.0353(5) Uani 1 1 d . . . . .
H15 H 0.6878 0.2195 0.7357 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8212(2) 0.12361(18) 0.80619(14) 0.0396(6) Uani 1 1 d . . . . .
C17 C 0.9051(3) 0.08068(19) 0.84511(16) 0.0461(7) Uani 1 1 d . . . . .
C18 C 0.9350(3) 0.1279(2) 0.89012(15) 0.0475(7) Uani 1 1 d . . . . .
H18 H 0.9926 0.1004 0.9160 0.057 Uiso 1 1 calc R U . . .
C19 C 0.8856(3) 0.2126(2) 0.89941(13) 0.0421(6) Uani 1 1 d . . . . .
C20 C 0.7999(2) 0.25101(18) 0.86201(13) 0.0371(6) Uani 1 1 d . . . . .
H20 H 0.7618 0.3083 0.8688 0.045 Uiso 1 1 calc R U . . .
C21 C 0.7680(2) 0.20881(17) 0.81516(13) 0.0360(5) Uani 1 1 d . . . . .
C22 C 0.9608(3) -0.0138(2) 0.83950(19) 0.0585(9) Uani 1 1 d . . . . .
C23 C 0.8708(4) -0.0605(2) 0.8452(2) 0.0746(12) Uani 1 1 d . . . . .
H23A H 0.8193 -0.0428 0.8121 0.112 Uiso 1 1 calc R U . . .
H23B H 0.8297 -0.0475 0.8853 0.112 Uiso 1 1 calc R U . . .
H23C H 0.9067 -0.1205 0.8416 0.112 Uiso 1 1 calc R U . . .
C24 C 1.0412(4) -0.0451(3) 0.8915(2) 0.0746(12) Uani 1 1 d . . . . .
H24A H 1.0678 -0.1060 0.8902 0.112 Uiso 1 1 calc R U . . .
H24B H 1.0023 -0.0265 0.9315 0.112 Uiso 1 1 calc R U . . .
H24C H 1.1045 -0.0226 0.8858 0.112 Uiso 1 1 calc R U . . .
C25 C 1.0265(3) -0.0361(2) 0.7777(2) 0.0661(10) Uani 1 1 d . . . . .
H25A H 0.9763 -0.0187 0.7440 0.099 Uiso 1 1 calc R U . . .
H25B H 1.0613 -0.0964 0.7750 0.099 Uiso 1 1 calc R U . . .
H25C H 1.0842 -0.0076 0.7742 0.099 Uiso 1 1 calc R U . . .
C26 C 0.9207(3) 0.2634(2) 0.94830(15) 0.0503(7) Uani 1 1 d . . . . .
C27 C 1.0258(4) 0.2129(3) 0.9792(2) 0.0846(14) Uani 1 1 d . . . . .
H27A H 1.0481 0.2487 1.0081 0.127 Uiso 1 1 calc R U . . .
H27B H 1.0859 0.1915 0.9475 0.127 Uiso 1 1 calc R U . . .
H27C H 1.0105 0.1663 1.0015 0.127 Uiso 1 1 calc R U . . .
C28 C 0.9493(4) 0.3366(3) 0.9172(2) 0.0754(12) Uani 1 1 d . . . . .
H28A H 0.8835 0.3723 0.8983 0.113 Uiso 1 1 calc R U . . .
H28B H 1.0090 0.3158 0.8853 0.113 Uiso 1 1 calc R U . . .
H28C H 0.9738 0.3688 0.9480 0.113 Uiso 1 1 calc R U . . .
C29 C 0.8257(4) 0.2954(4) 0.9958(2) 0.0904(16) Uani 1 1 d . . . . .
H29A H 0.7605 0.3295 0.9756 0.136 Uiso 1 1 calc R U . . .
H29B H 0.8472 0.3291 1.0268 0.136 Uiso 1 1 calc R U . . .
H29C H 0.8077 0.2483 1.0160 0.136 Uiso 1 1 calc R U . . .
C30 C 0.6753(2) 0.34014(17) 0.75571(12) 0.0334(5) Uani 1 1 d . . . . .
C31 C 0.5783(2) 0.40096(18) 0.74179(13) 0.0384(6) Uani 1 1 d . . . . .
H31 H 0.5092 0.3891 0.7470 0.046 Uiso 1 1 calc R U . . .
C32 C 0.5802(2) 0.47835(18) 0.72052(13) 0.0377(6) Uani 1 1 d . . . . .
H32 H 0.5122 0.5186 0.7122 0.045 Uiso 1 1 calc R U . . .
C33 C 0.6795(2) 0.49850(16) 0.71109(12) 0.0315(5) Uani 1 1 d . . . . .
C34 C 0.7764(2) 0.43736(17) 0.72434(12) 0.0335(5) Uani 1 1 d . . . . .
H34 H 0.8457 0.4488 0.7183 0.040 Uiso 1 1 calc R U . . .
C35 C 0.7745(2) 0.36009(17) 0.74608(12) 0.0343(5) Uani 1 1 d . . . . .
H35 H 0.8424 0.3199 0.7546 0.041 Uiso 1 1 calc R U . . .
C36 C 0.5258(2) 0.70568(16) 0.64791(12) 0.0323(5) Uani 1 1 d . . . . .
C37 C 0.4292(2) 0.77322(16) 0.65989(13) 0.0344(5) Uani 1 1 d . . . . .
C38 C 0.3846(2) 0.78198(17) 0.72034(14) 0.0384(6) Uani 1 1 d . . . . .
H38 H 0.3192 0.8263 0.7297 0.046 Uiso 1 1 calc R U . . .
C39 C 0.4308(2) 0.72911(19) 0.76821(13) 0.0400(6) Uani 1 1 d . . . . .
C40 C 0.5275(2) 0.66490(18) 0.75412(13) 0.0369(6) Uani 1 1 d . . . . .
H40 H 0.5619 0.6295 0.7861 0.044 Uiso 1 1 calc R U . . .
C41 C 0.5749(2) 0.65149(16) 0.69419(12) 0.0323(5) Uani 1 1 d . . . . .
C42 C 0.3775(2) 0.83509(17) 0.61008(14) 0.0371(6) Uani 1 1 d . . . . .
C43 C 0.4609(3) 0.88182(19) 0.58762(17) 0.0476(7) Uani 1 1 d . . . . .
H43A H 0.4760 0.9137 0.6220 0.071 Uiso 1 1 calc R U . . .
H43B H 0.4294 0.9198 0.5545 0.071 Uiso 1 1 calc R U . . .
H43C H 0.5303 0.8416 0.5721 0.071 Uiso 1 1 calc R U . . .
C44 C 0.3455(2) 0.7917(2) 0.55538(14) 0.0441(7) Uani 1 1 d . . . . .
H44A H 0.4124 0.7535 0.5353 0.066 Uiso 1 1 calc R U . . .
H44B H 0.3087 0.8334 0.5257 0.066 Uiso 1 1 calc R U . . .
H44C H 0.2947 0.7604 0.5700 0.066 Uiso 1 1 calc R U . . .
C45 C 0.2714(2) 0.90081(18) 0.63490(15) 0.0429(6) Uani 1 1 d . . . . .
H45A H 0.2162 0.8733 0.6494 0.064 Uiso 1 1 calc R U . . .
H45B H 0.2413 0.9394 0.6019 0.064 Uiso 1 1 calc R U . . .
H45C H 0.2891 0.9316 0.6692 0.064 Uiso 1 1 calc R U . . .
C46 C 0.3744(3) 0.7401(2) 0.83301(15) 0.0529(8) Uani 1 1 d D U . . .
C47 C 0.3531(4) 0.8291(3) 0.8550(2) 0.0600(13) Uani 0.758(6) 1 d D U P B 1
H47A H 0.3140 0.8671 0.8237 0.090 Uiso 0.758(6) 1 calc R U P B 1
H47B H 0.3074 0.8379 0.8937 0.090 Uiso 0.758(6) 1 calc R U P B 1
H47C H 0.4240 0.8397 0.8616 0.090 Uiso 0.758(6) 1 calc R U P B 1
C48 C 0.2561(4) 0.7251(3) 0.8260(2) 0.0529(11) Uani 0.758(6) 1 d D U P B 1
H48A H 0.2141 0.7649 0.7967 0.079 Uiso 0.758(6) 1 calc R U P B 1
H48B H 0.2668 0.6684 0.8109 0.079 Uiso 0.758(6) 1 calc R U P B 1
H48C H 0.2149 0.7329 0.8662 0.079 Uiso 0.758(6) 1 calc R U P B 1
C49 C 0.4335(5) 0.6783(4) 0.8778(2) 0.0693(17) Uani 0.758(6) 1 d D U P B 1
H49A H 0.4450 0.6221 0.8613 0.104 Uiso 0.758(6) 1 calc R U P B 1
H49B H 0.5055 0.6868 0.8848 0.104 Uiso 0.758(6) 1 calc R U P B 1
H49C H 0.3889 0.6851 0.9169 0.104 Uiso 0.758(6) 1 calc R U P B 1
C47X C 0.4637(11) 0.7641(12) 0.8755(7) 0.073(4) Uani 0.242(6) 1 d D U P B 2
H47D H 0.5354 0.7210 0.8707 0.110 Uiso 0.242(6) 1 calc R U P B 2
H47E H 0.4729 0.8177 0.8624 0.110 Uiso 0.242(6) 1 calc R U P B 2
H47F H 0.4365 0.7681 0.9189 0.110 Uiso 0.242(6) 1 calc R U P B 2
C48X C 0.2711(11) 0.8093(9) 0.8443(6) 0.058(4) Uani 0.242(6) 1 d D U P B 2
H48D H 0.2443 0.8089 0.8875 0.087 Uiso 0.242(6) 1 calc R U P B 2
H48E H 0.2862 0.8623 0.8355 0.087 Uiso 0.242(6) 1 calc R U P B 2
H48F H 0.2144 0.8025 0.8173 0.087 Uiso 0.242(6) 1 calc R U P B 2
C49X C 0.3738(16) 0.6562(8) 0.8606(8) 0.066(4) Uani 0.242(6) 1 d D U P B 2
H49D H 0.4455 0.6149 0.8506 0.099 Uiso 0.242(6) 1 calc R U P B 2
H49E H 0.3611 0.6620 0.9055 0.099 Uiso 0.242(6) 1 calc R U P B 2
H49F H 0.3144 0.6380 0.8434 0.099 Uiso 0.242(6) 1 calc R U P B 2
C50 C 0.6811(2) 0.58050(16) 0.68103(12) 0.0312(5) Uani 1 1 d . . . . .
H50 H 0.6864 0.5701 0.6355 0.037 Uiso 1 1 calc R U . . .
C51 C 0.8345(2) 0.64474(16) 0.64826(13) 0.0342(5) Uani 1 1 d . . . . .
C52 C 0.9252(2) 0.67384(18) 0.66047(14) 0.0382(6) Uani 1 1 d . . . . .
C53 C 0.9593(2) 0.6652(2) 0.72109(16) 0.0452(7) Uani 1 1 d . . . . .
H53 H 1.0209 0.6837 0.7304 0.054 Uiso 1 1 calc R U . . .
C54 C 0.9083(2) 0.63108(19) 0.76846(14) 0.0430(6) Uani 1 1 d . . . . .
C55 C 0.8175(2) 0.60520(17) 0.75413(13) 0.0369(6) Uani 1 1 d . . . . .
H55 H 0.7795 0.5835 0.7859 0.044 Uiso 1 1 calc R U . . .
C56 C 0.7806(2) 0.61003(16) 0.69471(12) 0.0329(5) Uani 1 1 d . . . . .
C57 C 0.9883(2) 0.7101(2) 0.61001(16) 0.0463(7) Uani 1 1 d . . . . .
C58 C 0.9105(3) 0.7783(2) 0.57326(18) 0.0546(8) Uani 1 1 d . . . . .
H58A H 0.8690 0.8236 0.6013 0.082 Uiso 1 1 calc R U . . .
H58B H 0.8585 0.7553 0.5527 0.082 Uiso 1 1 calc R U . . .
H58C H 0.9542 0.7997 0.5422 0.082 Uiso 1 1 calc R U . . .
C59 C 1.0723(3) 0.7480(3) 0.63733(19) 0.0589(9) Uani 1 1 d . . . . .
H59A H 1.0338 0.7912 0.6677 0.088 Uiso 1 1 calc R U . . .
H59B H 1.1081 0.7727 0.6043 0.088 Uiso 1 1 calc R U . . .
H59C H 1.1288 0.7045 0.6574 0.088 Uiso 1 1 calc R U . . .
C60 C 1.0523(3) 0.6385(2) 0.56609(18) 0.0568(9) Uani 1 1 d . . . . .
H60A H 1.0939 0.6598 0.5339 0.085 Uiso 1 1 calc R U . . .
H60B H 0.9997 0.6146 0.5470 0.085 Uiso 1 1 calc R U . . .
H60C H 1.1040 0.5956 0.5894 0.085 Uiso 1 1 calc R U . . .
C61 C 0.9493(3) 0.6222(2) 0.83356(17) 0.0572(8) Uani 1 1 d D U . . .
C62 C 1.0493(6) 0.6536(6) 0.8417(4) 0.080(2) Uani 0.595(6) 1 d D U P C 1
H62A H 1.0334 0.7108 0.8269 0.120 Uiso 0.595(6) 1 calc R U P C 1
H62B H 1.0649 0.6522 0.8855 0.120 Uiso 0.595(6) 1 calc R U P C 1
H62C H 1.1141 0.6180 0.8181 0.120 Uiso 0.595(6) 1 calc R U P C 1
C63 C 0.9668(10) 0.5350(5) 0.8551(4) 0.100(3) Uani 0.595(6) 1 d D U P C 1
H63A H 0.9001 0.5180 0.8488 0.151 Uiso 0.595(6) 1 calc R U P C 1
H63B H 1.0304 0.4978 0.8316 0.151 Uiso 0.595(6) 1 calc R U P C 1
H63C H 0.9813 0.5320 0.8991 0.151 Uiso 0.595(6) 1 calc R U P C 1
C64 C 0.8512(6) 0.6817(5) 0.8778(3) 0.0685(19) Uani 0.595(6) 1 d D U P C 1
H64A H 0.8376 0.7396 0.8649 0.103 Uiso 0.595(6) 1 calc R U P C 1
H64B H 0.7832 0.6653 0.8748 0.103 Uiso 0.595(6) 1 calc R U P C 1
H64C H 0.8732 0.6764 0.9206 0.103 Uiso 0.595(6) 1 calc R U P C 1
C62X C 1.0734(7) 0.5587(6) 0.8269(4) 0.059(2) Uani 0.405(6) 1 d D U P C 2
H62D H 1.0701 0.5042 0.8129 0.089 Uiso 0.405(6) 1 calc R U P C 2
H62E H 1.1186 0.5802 0.7968 0.089 Uiso 0.405(6) 1 calc R U P C 2
H62F H 1.1069 0.5530 0.8670 0.089 Uiso 0.405(6) 1 calc R U P C 2
C63X C 0.8856(9) 0.5817(7) 0.8776(4) 0.064(3) Uani 0.405(6) 1 d D U P C 2
H63D H 0.8841 0.5284 0.8601 0.097 Uiso 0.405(6) 1 calc R U P C 2
H63E H 0.9217 0.5721 0.9169 0.097 Uiso 0.405(6) 1 calc R U P C 2
H63F H 0.8095 0.6181 0.8845 0.097 Uiso 0.405(6) 1 calc R U P C 2
C64X C 0.9577(8) 0.7042(5) 0.8549(4) 0.061(2) Uani 0.405(6) 1 d D U P C 2
H64D H 1.0004 0.7262 0.8237 0.091 Uiso 0.405(6) 1 calc R U P C 2
H64E H 0.8831 0.7431 0.8614 0.091 Uiso 0.405(6) 1 calc R U P C 2
H64F H 0.9953 0.6971 0.8938 0.091 Uiso 0.405(6) 1 calc R U P C 2
N1 N 0.7220(3) 0.1721(2) 0.63986(13) 0.0573(8) Uani 1 1 d . . . . .
C65 C 0.7176(4) 0.2331(3) 0.61272(17) 0.0658(10) Uani 1 1 d . . . . .
C66 C 0.7194(4) 0.3075(3) 0.58176(18) 0.0661(10) Uani 1 1 d . . . . .
H66A H 0.7215 0.3499 0.6121 0.099 Uiso 1 1 calc R U . . .
H66B H 0.6526 0.3276 0.5584 0.099 Uiso 1 1 calc R U . . .
H66C H 0.7855 0.2963 0.5534 0.099 Uiso 1 1 calc R U . . .
N2 N 0.8396(2) 0.61509(16) 0.46052(11) 0.0432(6) Uani 1 1 d . . . . .
C67 C 0.9163(3) 0.5899(2) 0.42927(15) 0.0469(7) Uani 1 1 d . . . . .
C68 C 1.0158(3) 0.5580(2) 0.38899(18) 0.0615(10) Uani 1 1 d . . . . .
H68A H 1.0073 0.5129 0.3631 0.092 Uiso 1 1 calc R U . . .
H68B H 1.0802 0.5367 0.4140 0.092 Uiso 1 1 calc R U . . .
H68C H 1.0269 0.6027 0.3627 0.092 Uiso 1 1 calc R U . . .
O5 O 0.6923(2) -0.03954(15) 0.72448(13) 0.0593(6) Uani 1 1 d . . . . .
C69 C 0.7129(4) -0.1269(2) 0.7141(2) 0.0773(13) Uani 1 1 d . . . . .
H69A H 0.6857 -0.1356 0.6736 0.093 Uiso 1 1 calc R U . . .
H69B H 0.7941 -0.1541 0.7126 0.093 Uiso 1 1 calc R U . . .
C70 C 0.6609(4) -0.1653(3) 0.7605(3) 0.0795(13) Uani 1 1 d . . . . .
H70A H 0.6818 -0.1523 0.8012 0.119 Uiso 1 1 calc R U . . .
H70B H 0.6850 -0.2256 0.7539 0.119 Uiso 1 1 calc R U . . .
H70C H 0.5800 -0.1443 0.7583 0.119 Uiso 1 1 calc R U . . .
O6 O 0.69237(16) 0.76114(12) 0.49939(9) 0.0400(4) Uani 1 1 d . . . . .
C71 C 0.6898(3) 0.8107(2) 0.44529(16) 0.0533(8) Uani 1 1 d . . . . .
H71A H 0.6193 0.8174 0.4251 0.064 Uiso 1 1 calc R U . . .
H71B H 0.7518 0.7822 0.4158 0.064 Uiso 1 1 calc R U . . .
C72 C 0.6997(4) 0.8943(2) 0.4619(2) 0.0662(10) Uani 1 1 d . . . . .
H72A H 0.6384 0.9223 0.4912 0.099 Uiso 1 1 calc R U . . .
H72B H 0.6966 0.9278 0.4246 0.099 Uiso 1 1 calc R U . . .
H72C H 0.7706 0.8876 0.4807 0.099 Uiso 1 1 calc R U . . .
N3 N 0.0862(3) 0.3354(3) 0.7423(2) 0.0914(13) Uani 1 1 d D . . . .
C73 C 0.1680(4) 0.3498(3) 0.7323(2) 0.0714(11) Uani 1 1 d D . . . .
C74 C 0.2728(4) 0.3679(3) 0.7189(2) 0.0762(12) Uani 1 1 d D . . . .
H74A H 0.3035 0.3457 0.6779 0.114 Uiso 1 1 calc R U . . .
H74B H 0.3252 0.3419 0.7500 0.114 Uiso 1 1 calc R U . . .
H74C H 0.2604 0.4281 0.7198 0.114 Uiso 1 1 calc R U . . .
N4 N 0.2853(3) 0.5623(3) 0.6844(3) 0.0997(15) Uani 1 1 d D . . . .
C75 C 0.3416(4) 0.5609(3) 0.6411(3) 0.0747(13) Uani 1 1 d D . . . .
C76 C 0.4139(5) 0.5572(3) 0.5873(2) 0.0803(14) Uani 1 1 d D . . . .
H76A H 0.3968 0.6122 0.5682 0.120 Uiso 1 1 calc R U . . .
H76B H 0.4030 0.5167 0.5578 0.120 Uiso 1 1 calc R U . . .
H76C H 0.4912 0.5403 0.5990 0.120 Uiso 1 1 calc R U . . .
N5 N 1.0028(5) 0.7534(3) 0.4029(2) 0.1148(19) Uani 1 1 d D . . . .
C77 C 0.9892(3) 0.7985(3) 0.3630(2) 0.0652(10) Uani 1 1 d D . . . .
C78 C 0.9755(4) 0.8549(3) 0.3133(2) 0.0720(11) Uani 1 1 d D . . . .
H78A H 1.0359 0.8807 0.3116 0.108 Uiso 1 1 calc R U . . .
H78B H 0.9041 0.8980 0.3195 0.108 Uiso 1 1 calc R U . . .
H78C H 0.9769 0.8249 0.2746 0.108 Uiso 1 1 calc R U . . .
C79 C 0.6609(7) -0.0436(6) 0.9828(4) 0.127(3) Uani 0.614 1 d D U P . .
C80 C 0.7304(7) -0.0085(5) 1.0110(3) 0.104(2) Uani 0.614 1 d D U P . .
H80 H 0.7783 -0.0371 1.0414 0.125 Uiso 0.614 1 calc R U P . .
C81 C 0.7279(7) 0.0654(5) 0.9943(3) 0.102(2) Uani 0.614 1 d D U P . .
H81 H 0.7778 0.0896 1.0128 0.122 Uiso 0.614 1 calc R U P . .
C82 C 0.6601(7) 0.1125(5) 0.9525(3) 0.087(2) Uani 0.614 1 d D U P . .
H82 H 0.6581 0.1685 0.9445 0.104 Uiso 0.614 1 calc R U P . .
C83 C 0.6025(8) 0.0785(6) 0.9260(4) 0.112(3) Uani 0.614 1 d D U P . .
H83 H 0.5596 0.1078 0.8939 0.134 Uiso 0.614 1 calc R U P . .
C84 C 0.5957(9) -0.0002(7) 0.9395(5) 0.141(4) Uani 0.614 1 d D U P . .
H84 H 0.5466 -0.0231 0.9190 0.169 Uiso 0.614 1 calc R U P . .
C85 C 0.6595(10) -0.1346(8) 0.9947(6) 0.138(4) Uani 0.614 1 d D U P . .
H85A H 0.6210 -0.1526 0.9620 0.207 Uiso 0.614 1 calc R U P . .
H85B H 0.6207 -0.1373 1.0347 0.207 Uiso 0.614 1 calc R U P . .
H85C H 0.7360 -0.1710 0.9950 0.207 Uiso 0.614 1 calc R U P . .
N6 N 1.0886(10) 0.8847(7) 0.4809(6) 0.123(4) Uani 0.5 1 d D U P D -1
C86 C 1.0392(12) 0.9513(8) 0.4942(8) 0.084(3) Uani 0.5 1 d D U P D -1
C87 C 0.961(3) 1.0323(13) 0.5001(17) 0.231(13) Uani 0.5 1 d D U P D -1
H87A H 0.9359 1.0519 0.4594 0.347 Uiso 0.5 1 calc R U P D -1
H87B H 0.9964 1.0707 0.5181 0.347 Uiso 0.5 1 calc R U P D -1
H87C H 0.8971 1.0296 0.5270 0.347 Uiso 0.5 1 calc R U P D -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O5 1.826(2) . ?
Nb1 O1 1.897(2) . ?
Nb1 O2 1.915(2) . ?
Nb1 N1 2.300(3) . ?
Nb1 Cl2 2.3964(10) . ?
Nb1 Cl1 2.4116(10) . ?
Nb2 O6 1.838(2) . ?
Nb2 O3 1.8662(18) . ?
Nb2 O4 1.8931(19) . ?
Nb2 N2 2.278(2) . ?
Nb2 Cl4 2.4399(8) . ?
Nb2 Cl3 2.4432(8) . ?
O1 C1 1.366(4) . ?
O2 C16 1.363(4) . ?
O3 C36 1.378(3) . ?
O4 C51 1.368(3) . ?
C1 C6 1.405(4) . ?
C1 C2 1.420(4) . ?
C2 C3 1.398(5) . ?
C2 C7 1.541(5) . ?
C3 C4 1.398(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(4) . ?
C4 C11 1.537(5) . ?
C5 C6 1.393(4) . ?
C5 H5 0.9500 . ?
C6 C15 1.519(4) . ?
C7 C8 1.537(6) . ?
C7 C9 1.541(5) . ?
C7 C10 1.548(6) . ?
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 C12X 1.415(12) . ?
C11 C14 1.438(7) . ?
C11 C12 1.500(6) . ?
C11 C13X 1.520(12) . ?
C11 C14X 1.638(13) . ?
C11 C13 1.644(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12X H12D 0.9800 . ?
C12X H12E 0.9800 . ?
C12X H12F 0.9800 . ?
C13X H13D 0.9800 . ?
C13X H13E 0.9800 . ?
C13X H13F 0.9800 . ?
C14X H14D 0.9800 . ?
C14X H14E 0.9800 . ?
C14X H14F 0.9800 . ?
C15 C21 1.517(4) . ?
C15 C30 1.525(4) . ?
C15 H15 1.0000 . ?
C16 C21 1.403(4) . ?
C16 C17 1.415(4) . ?
C17 C18 1.397(5) . ?
C17 C22 1.541(4) . ?
C18 C19 1.388(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(4) . ?
C19 C26 1.527(5) . ?
C20 C21 1.386(4) . ?
C20 H20 0.9500 . ?
C22 C25 1.527(6) . ?
C22 C24 1.545(6) . ?
C22 C23 1.557(6) . ?
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 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C29 1.511(5) . ?
C26 C28 1.526(6) . ?
C26 C27 1.536(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C35 1.391(4) . ?
C30 C31 1.393(4) . ?
C31 C32 1.385(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.394(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(4) . ?
C33 C50 1.528(4) . ?
C34 C35 1.387(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C41 1.398(4) . ?
C36 C37 1.415(4) . ?
C37 C38 1.390(4) . ?
C37 C42 1.532(4) . ?
C38 C39 1.402(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.393(4) . ?
C39 C46 1.528(4) . ?
C40 C41 1.393(4) . ?
C40 H40 0.9500 . ?
C41 C50 1.525(3) . ?
C42 C44 1.530(4) . ?
C42 C45 1.537(4) . ?
C42 C43 1.544(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48X 1.481(11) . ?
C46 C49 1.483(6) . ?
C46 C47 1.515(6) . ?
C46 C49X 1.533(12) . ?
C46 C48 1.599(6) . ?
C46 C47X 1.633(12) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C47X H47D 0.9800 . ?
C47X H47E 0.9800 . ?
C47X H47F 0.9800 . ?
C48X H48D 0.9800 . ?
C48X H48E 0.9800 . ?
C48X H48F 0.9800 . ?
C49X H49D 0.9800 . ?
C49X H49E 0.9800 . ?
C49X H49F 0.9800 . ?
C50 C56 1.523(4) . ?
C50 H50 1.0000 . ?
C51 C56 1.404(4) . ?
C51 C52 1.407(4) . ?
C52 C53 1.401(4) . ?
C52 C57 1.545(4) . ?
C53 C54 1.392(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.388(4) . ?
C54 C61 1.523(4) . ?
C55 C56 1.389(4) . ?
C55 H55 0.9500 . ?
C57 C58 1.527(5) . ?
C57 C59 1.533(5) . ?
C57 C60 1.539(5) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C64X 1.492(8) . ?
C61 C63 1.495(8) . ?
C61 C63X 1.501(10) . ?
C61 C62 1.522(7) . ?
C61 C64 1.616(7) . ?
C61 C62X 1.616(8) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C62X H62D 0.9800 . ?
C62X H62E 0.9800 . ?
C62X H62F 0.9800 . ?
C63X H63D 0.9800 . ?
C63X H63E 0.9800 . ?
C63X H63F 0.9800 . ?
C64X H64D 0.9800 . ?
C64X H64E 0.9800 . ?
C64X H64F 0.9800 . ?
N1 C65 1.170(5) . ?
C65 C66 1.424(6) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
N2 C67 1.125(4) . ?
C67 C68 1.455(4) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
O5 C69 1.432(4) . ?
C69 C70 1.425(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
O6 C71 1.433(4) . ?
C71 C72 1.495(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N3 C73 1.136(5) . ?
C73 C74 1.454(6) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
N4 C75 1.141(6) . ?
C75 C76 1.432(7) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N5 C77 1.137(6) . ?
C77 C78 1.416(6) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C84 1.349(11) . ?
C79 C80 1.363(11) . ?
C79 C85 1.555(14) . ?
C80 C81 1.285(11) . ?
C80 H80 0.9500 . ?
C81 C82 1.366(9) . ?
C81 H81 0.9500 . ?
C82 C83 1.216(10) . ?
C82 H82 0.9500 . ?
C83 C84 1.380(12) . ?
C83 H83 0.9500 . ?
C84 H84 0.9500 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
N6 C86 1.142(12) . ?
C86 C87 1.430(11) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 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
O5 Nb1 O1 99.16(10) . . ?
O5 Nb1 O2 98.03(11) . . ?
O1 Nb1 O2 89.72(9) . . ?
O5 Nb1 N1 167.33(11) . . ?
O1 Nb1 N1 89.61(10) . . ?
O2 Nb1 N1 91.10(10) . . ?
O5 Nb1 Cl2 90.15(8) . . ?
O1 Nb1 Cl2 170.68(7) . . ?
O2 Nb1 Cl2 88.42(7) . . ?
N1 Nb1 Cl2 81.30(9) . . ?
O5 Nb1 Cl1 91.22(10) . . ?
O1 Nb1 Cl1 90.18(7) . . ?
O2 Nb1 Cl1 170.64(7) . . ?
N1 Nb1 Cl1 79.54(8) . . ?
Cl2 Nb1 Cl1 90.18(4) . . ?
O6 Nb2 O3 100.23(8) . . ?
O6 Nb2 O4 97.60(9) . . ?
O3 Nb2 O4 91.84(8) . . ?
O6 Nb2 N2 81.80(9) . . ?
O3 Nb2 N2 177.44(9) . . ?
O4 Nb2 N2 86.33(9) . . ?
O6 Nb2 Cl4 85.19(7) . . ?
O3 Nb2 Cl4 94.45(6) . . ?
O4 Nb2 Cl4 172.56(6) . . ?
N2 Nb2 Cl4 87.25(7) . . ?
O6 Nb2 Cl3 158.18(7) . . ?
O3 Nb2 Cl3 99.38(6) . . ?
O4 Nb2 Cl3 91.25(6) . . ?
N2 Nb2 Cl3 78.89(7) . . ?
Cl4 Nb2 Cl3 83.82(3) . . ?
C1 O1 Nb1 154.1(2) . . ?
C16 O2 Nb1 159.75(19) . . ?
C36 O3 Nb2 154.77(17) . . ?
C51 O4 Nb2 156.25(17) . . ?
O1 C1 C6 119.3(3) . . ?
O1 C1 C2 119.8(3) . . ?
C6 C1 C2 120.8(3) . . ?
C3 C2 C1 116.5(3) . . ?
C3 C2 C7 121.6(3) . . ?
C1 C2 C7 121.9(3) . . ?
C4 C3 C2 124.2(3) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
C5 C4 C3 117.0(3) . . ?
C5 C4 C11 120.1(3) . . ?
C3 C4 C11 123.0(3) . . ?
C4 C5 C6 122.0(3) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C15 119.7(3) . . ?
C1 C6 C15 120.8(3) . . ?
C8 C7 C9 106.8(3) . . ?
C8 C7 C2 109.3(3) . . ?
C9 C7 C2 111.9(3) . . ?
C8 C7 C10 110.6(4) . . ?
C9 C7 C10 107.6(3) . . ?
C2 C7 C10 110.6(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C12 116.1(5) . . ?
C12X C11 C13X 122.7(11) . . ?
C12X C11 C4 111.7(7) . . ?
C14 C11 C4 111.6(4) . . ?
C12 C11 C4 113.3(4) . . ?
C13X C11 C4 113.0(5) . . ?
C12X C11 C14X 107.7(12) . . ?
C13X C11 C14X 98.1(9) . . ?
C4 C11 C14X 99.7(7) . . ?
C14 C11 C13 105.5(5) . . ?
C12 C11 C13 101.8(4) . . ?
C4 C11 C13 107.3(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C12X H12D 109.5 . . ?
C11 C12X H12E 109.5 . . ?
H12D C12X H12E 109.5 . . ?
C11 C12X H12F 109.5 . . ?
H12D C12X H12F 109.5 . . ?
H12E C12X H12F 109.5 . . ?
C11 C13X H13D 109.5 . . ?
C11 C13X H13E 109.5 . . ?
H13D C13X H13E 109.5 . . ?
C11 C13X H13F 109.5 . . ?
H13D C13X H13F 109.5 . . ?
H13E C13X H13F 109.5 . . ?
C11 C14X H14D 109.5 . . ?
C11 C14X H14E 109.5 . . ?
H14D C14X H14E 109.5 . . ?
C11 C14X H14F 109.5 . . ?
H14D C14X H14F 109.5 . . ?
H14E C14X H14F 109.5 . . ?
C21 C15 C6 110.3(2) . . ?
C21 C15 C30 114.4(2) . . ?
C6 C15 C30 114.6(2) . . ?
C21 C15 H15 105.5 . . ?
C6 C15 H15 105.5 . . ?
C30 C15 H15 105.5 . . ?
O2 C16 C21 118.5(3) . . ?
O2 C16 C17 121.0(3) . . ?
C21 C16 C17 120.6(3) . . ?
C18 C17 C16 116.8(3) . . ?
C18 C17 C22 120.8(3) . . ?
C16 C17 C22 122.4(3) . . ?
C19 C18 C17 124.0(3) . . ?
C19 C18 H18 118.0 . . ?
C17 C18 H18 118.0 . . ?
C18 C19 C20 116.9(3) . . ?
C18 C19 C26 123.2(3) . . ?
C20 C19 C26 119.9(3) . . ?
C21 C20 C19 122.3(3) . . ?
C21 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
C20 C21 C16 119.2(3) . . ?
C20 C21 C15 120.9(2) . . ?
C16 C21 C15 119.8(3) . . ?
C25 C22 C17 110.8(3) . . ?
C25 C22 C24 108.2(3) . . ?
C17 C22 C24 111.1(3) . . ?
C25 C22 C23 109.2(4) . . ?
C17 C22 C23 109.9(3) . . ?
C24 C22 C23 107.6(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 C26 C28 109.6(4) . . ?
C29 C26 C19 109.2(3) . . ?
C28 C26 C19 108.8(3) . . ?
C29 C26 C27 110.7(4) . . ?
C28 C26 C27 106.4(4) . . ?
C19 C26 C27 112.2(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 116.9(2) . . ?
C35 C30 C15 121.2(2) . . ?
C31 C30 C15 121.7(2) . . ?
C32 C31 C30 121.6(3) . . ?
C32 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C31 C32 C33 121.5(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 H32 119.2 . . ?
C34 C33 C32 116.8(2) . . ?
C34 C33 C50 122.2(2) . . ?
C32 C33 C50 120.6(2) . . ?
C35 C34 C33 121.6(2) . . ?
C35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C34 C35 C30 121.5(2) . . ?
C34 C35 H35 119.2 . . ?
C30 C35 H35 119.2 . . ?
O3 C36 C41 118.2(2) . . ?
O3 C36 C37 119.6(2) . . ?
C41 C36 C37 122.1(2) . . ?
C38 C37 C36 116.1(3) . . ?
C38 C37 C42 121.3(2) . . ?
C36 C37 C42 122.6(2) . . ?
C37 C38 C39 123.7(3) . . ?
C37 C38 H38 118.1 . . ?
C39 C38 H38 118.1 . . ?
C40 C39 C38 117.7(3) . . ?
C40 C39 C46 121.4(3) . . ?
C38 C39 C46 120.9(3) . . ?
C41 C40 C39 121.4(3) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C40 C41 C36 118.8(2) . . ?
C40 C41 C50 119.5(2) . . ?
C36 C41 C50 121.6(2) . . ?
C44 C42 C37 111.8(2) . . ?
C44 C42 C45 106.9(2) . . ?
C37 C42 C45 111.9(2) . . ?
C44 C42 C43 109.7(3) . . ?
C37 C42 C43 109.2(2) . . ?
C45 C42 C43 107.2(2) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C49 C46 C47 112.9(4) . . ?
C48X C46 C39 118.3(6) . . ?
C49 C46 C39 113.8(3) . . ?
C47 C46 C39 109.8(3) . . ?
C48X C46 C49X 115.9(9) . . ?
C39 C46 C49X 111.2(6) . . ?
C49 C46 C48 106.8(4) . . ?
C47 C46 C48 107.3(3) . . ?
C39 C46 C48 105.7(3) . . ?
C48X C46 C47X 104.0(9) . . ?
C39 C46 C47X 104.0(6) . . ?
C49X C46 C47X 100.6(10) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C46 C47X H47D 109.5 . . ?
C46 C47X H47E 109.5 . . ?
H47D C47X H47E 109.5 . . ?
C46 C47X H47F 109.5 . . ?
H47D C47X H47F 109.5 . . ?
H47E C47X H47F 109.5 . . ?
C46 C48X H48D 109.5 . . ?
C46 C48X H48E 109.5 . . ?
H48D C48X H48E 109.5 . . ?
C46 C48X H48F 109.5 . . ?
H48D C48X H48F 109.5 . . ?
H48E C48X H48F 109.5 . . ?
C46 C49X H49D 109.5 . . ?
C46 C49X H49E 109.5 . . ?
H49D C49X H49E 109.5 . . ?
C46 C49X H49F 109.5 . . ?
H49D C49X H49F 109.5 . . ?
H49E C49X H49F 109.5 . . ?
C56 C50 C41 109.1(2) . . ?
C56 C50 C33 114.9(2) . . ?
C41 C50 C33 114.0(2) . . ?
C56 C50 H50 106.0 . . ?
C41 C50 H50 106.0 . . ?
C33 C50 H50 106.0 . . ?
O4 C51 C56 118.7(2) . . ?
O4 C51 C52 119.8(2) . . ?
C56 C51 C52 121.5(3) . . ?
C53 C52 C51 116.3(3) . . ?
C53 C52 C57 120.9(3) . . ?
C51 C52 C57 122.8(3) . . ?
C54 C53 C52 124.0(3) . . ?
C54 C53 H53 118.0 . . ?
C52 C53 H53 118.0 . . ?
C55 C54 C53 117.2(3) . . ?
C55 C54 C61 120.8(3) . . ?
C53 C54 C61 122.0(3) . . ?
C54 C55 C56 122.0(3) . . ?
C54 C55 H55 119.0 . . ?
C56 C55 H55 119.0 . . ?
C55 C56 C51 118.9(3) . . ?
C55 C56 C50 120.2(2) . . ?
C51 C56 C50 120.8(2) . . ?
C58 C57 C59 107.0(3) . . ?
C58 C57 C60 109.4(3) . . ?
C59 C57 C60 108.2(3) . . ?
C58 C57 C52 112.5(2) . . ?
C59 C57 C52 111.8(3) . . ?
C60 C57 C52 107.9(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C64X C61 C63X 114.7(6) . . ?
C63 C61 C62 112.9(6) . . ?
C64X C61 C54 109.0(5) . . ?
C63 C61 C54 110.1(4) . . ?
C63X C61 C54 114.0(4) . . ?
C62 C61 C54 114.4(4) . . ?
C63 C61 C64 107.4(6) . . ?
C62 C61 C64 104.7(5) . . ?
C54 C61 C64 106.8(3) . . ?
C64X C61 C62X 107.9(6) . . ?
C63X C61 C62X 105.4(6) . . ?
C54 C61 C62X 105.2(4) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C61 C62X H62D 109.5 . . ?
C61 C62X H62E 109.5 . . ?
H62D C62X H62E 109.5 . . ?
C61 C62X H62F 109.5 . . ?
H62D C62X H62F 109.5 . . ?
H62E C62X H62F 109.5 . . ?
C61 C63X H63D 109.5 . . ?
C61 C63X H63E 109.5 . . ?
H63D C63X H63E 109.5 . . ?
C61 C63X H63F 109.5 . . ?
H63D C63X H63F 109.5 . . ?
H63E C63X H63F 109.5 . . ?
C61 C64X H64D 109.5 . . ?
C61 C64X H64E 109.5 . . ?
H64D C64X H64E 109.5 . . ?
C61 C64X H64F 109.5 . . ?
H64D C64X H64F 109.5 . . ?
H64E C64X H64F 109.5 . . ?
C65 N1 Nb1 171.3(3) . . ?
N1 C65 C66 175.8(4) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C67 N2 Nb2 175.4(3) . . ?
N2 C67 C68 179.6(4) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C69 O5 Nb1 148.9(3) . . ?
C70 C69 O5 113.1(4) . . ?
C70 C69 H69A 109.0 . . ?
O5 C69 H69A 109.0 . . ?
C70 C69 H69B 109.0 . . ?
O5 C69 H69B 109.0 . . ?
H69A C69 H69B 107.8 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C71 O6 Nb2 145.7(2) . . ?
O6 C71 C72 110.4(3) . . ?
O6 C71 H71A 109.6 . . ?
C72 C71 H71A 109.6 . . ?
O6 C71 H71B 109.6 . . ?
C72 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N3 C73 C74 179.5(6) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N4 C75 C76 178.6(5) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N5 C77 C78 178.3(6) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C84 C79 C80 119.1(7) . . ?
C84 C79 C85 117.9(8) . . ?
C80 C79 C85 122.8(8) . . ?
C81 C80 C79 116.5(6) . . ?
C81 C80 H80 121.8 . . ?
C79 C80 H80 121.8 . . ?
C80 C81 C82 126.2(7) . . ?
C80 C81 H81 116.9 . . ?
C82 C81 H81 116.9 . . ?
C83 C82 C81 116.0(7) . . ?
C83 C82 H82 122.0 . . ?
C81 C82 H82 122.0 . . ?
C82 C83 C84 124.0(7) . . ?
C82 C83 H83 118.0 . . ?
C84 C83 H83 118.0 . . ?
C79 C84 C83 118.0(7) . . ?
C79 C84 H84 121.0 . . ?
C83 C84 H84 121.0 . . ?
C79 C85 H85A 109.5 . . ?
C79 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C79 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N6 C86 C87 166.7(15) . . ?
C86 C87 H87A 109.5 . . ?
C86 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C86 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 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
O5 Nb1 O1 C1 103.6(5) . . . . ?
O2 Nb1 O1 C1 5.5(5) . . . . ?
N1 Nb1 O1 C1 -85.6(5) . . . . ?
Cl1 Nb1 O1 C1 -165.1(5) . . . . ?
O6 Nb2 O3 C36 -106.5(4) . . . . ?
O4 Nb2 O3 C36 -8.4(4) . . . . ?
Cl4 Nb2 O3 C36 167.6(4) . . . . ?
Cl3 Nb2 O3 C36 83.1(4) . . . . ?
O6 Nb2 O4 C51 117.1(4) . . . . ?
O3 Nb2 O4 C51 16.6(4) . . . . ?
N2 Nb2 O4 C51 -161.6(4) . . . . ?
Cl3 Nb2 O4 C51 -82.9(4) . . . . ?
Nb1 O1 C1 C6 36.6(6) . . . . ?
Nb1 O1 C1 C2 -143.2(4) . . . . ?
O1 C1 C2 C3 179.4(3) . . . . ?
C6 C1 C2 C3 -0.4(5) . . . . ?
O1 C1 C2 C7 -0.8(5) . . . . ?
C6 C1 C2 C7 179.4(3) . . . . ?
C1 C2 C3 C4 -1.0(6) . . . . ?
C7 C2 C3 C4 179.1(4) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
C2 C3 C4 C11 179.1(4) . . . . ?
C3 C4 C5 C6 1.1(6) . . . . ?
C11 C4 C5 C6 -177.4(4) . . . . ?
C4 C5 C6 C1 -2.5(5) . . . . ?
C4 C5 C6 C15 178.8(3) . . . . ?
O1 C1 C6 C5 -177.7(3) . . . . ?
C2 C1 C6 C5 2.1(5) . . . . ?
O1 C1 C6 C15 0.9(4) . . . . ?
C2 C1 C6 C15 -179.2(3) . . . . ?
C3 C2 C7 C8 -116.4(4) . . . . ?
C1 C2 C7 C8 63.7(5) . . . . ?
C3 C2 C7 C9 1.6(6) . . . . ?
C1 C2 C7 C9 -178.2(4) . . . . ?
C3 C2 C7 C10 121.6(4) . . . . ?
C1 C2 C7 C10 -58.3(5) . . . . ?
C5 C4 C11 C12X 124.9(12) . . . . ?
C3 C4 C11 C12X -53.5(12) . . . . ?
C5 C4 C11 C14 -61.6(7) . . . . ?
C3 C4 C11 C14 120.0(6) . . . . ?
C5 C4 C11 C12 165.2(4) . . . . ?
C3 C4 C11 C12 -13.2(7) . . . . ?
C5 C4 C11 C13X -18.3(10) . . . . ?
C3 C4 C11 C13X 163.3(9) . . . . ?
C5 C4 C11 C14X -121.5(7) . . . . ?
C3 C4 C11 C14X 60.1(8) . . . . ?
C5 C4 C11 C13 53.6(5) . . . . ?
C3 C4 C11 C13 -124.8(5) . . . . ?
C5 C6 C15 C21 81.0(3) . . . . ?
C1 C6 C15 C21 -97.6(3) . . . . ?
C5 C6 C15 C30 -49.8(4) . . . . ?
C1 C6 C15 C30 131.6(3) . . . . ?
Nb1 O2 C16 C21 -19.6(7) . . . . ?
Nb1 O2 C16 C17 160.6(4) . . . . ?
O2 C16 C17 C18 176.9(3) . . . . ?
C21 C16 C17 C18 -2.9(4) . . . . ?
O2 C16 C17 C22 -4.0(5) . . . . ?
C21 C16 C17 C22 176.2(3) . . . . ?
C16 C17 C18 C19 1.7(5) . . . . ?
C22 C17 C18 C19 -177.5(3) . . . . ?
C17 C18 C19 C20 1.4(5) . . . . ?
C17 C18 C19 C26 -179.1(3) . . . . ?
C18 C19 C20 C21 -3.4(4) . . . . ?
C26 C19 C20 C21 177.1(3) . . . . ?
C19 C20 C21 C16 2.2(4) . . . . ?
C19 C20 C21 C15 -179.5(2) . . . . ?
O2 C16 C21 C20 -178.7(2) . . . . ?
C17 C16 C21 C20 1.1(4) . . . . ?
O2 C16 C21 C15 2.9(4) . . . . ?
C17 C16 C21 C15 -177.2(3) . . . . ?
C6 C15 C21 C20 -89.8(3) . . . . ?
C30 C15 C21 C20 41.1(3) . . . . ?
C6 C15 C21 C16 88.5(3) . . . . ?
C30 C15 C21 C16 -140.5(3) . . . . ?
C18 C17 C22 C25 -116.0(4) . . . . ?
C16 C17 C22 C25 64.9(4) . . . . ?
C18 C17 C22 C24 4.4(5) . . . . ?
C16 C17 C22 C24 -174.7(3) . . . . ?
C18 C17 C22 C23 123.3(4) . . . . ?
C16 C17 C22 C23 -55.8(5) . . . . ?
C18 C19 C26 C29 -115.2(4) . . . . ?
C20 C19 C26 C29 64.3(4) . . . . ?
C18 C19 C26 C28 125.3(4) . . . . ?
C20 C19 C26 C28 -55.3(4) . . . . ?
C18 C19 C26 C27 7.9(5) . . . . ?
C20 C19 C26 C27 -172.7(3) . . . . ?
C21 C15 C30 C35 32.6(3) . . . . ?
C6 C15 C30 C35 161.4(2) . . . . ?
C21 C15 C30 C31 -153.2(3) . . . . ?
C6 C15 C30 C31 -24.4(4) . . . . ?
C35 C30 C31 C32 -1.3(4) . . . . ?
C15 C30 C31 C32 -175.7(3) . . . . ?
C30 C31 C32 C33 1.1(4) . . . . ?
C31 C32 C33 C34 -0.3(4) . . . . ?
C31 C32 C33 C50 173.3(3) . . . . ?
C32 C33 C34 C35 -0.2(4) . . . . ?
C50 C33 C34 C35 -173.7(2) . . . . ?
C33 C34 C35 C30 -0.1(4) . . . . ?
C31 C30 C35 C34 0.8(4) . . . . ?
C15 C30 C35 C34 175.2(2) . . . . ?
Nb2 O3 C36 C41 -36.0(5) . . . . ?
Nb2 O3 C36 C37 144.7(3) . . . . ?
O3 C36 C37 C38 178.2(2) . . . . ?
C41 C36 C37 C38 -1.0(4) . . . . ?
O3 C36 C37 C42 -3.4(4) . . . . ?
C41 C36 C37 C42 177.4(2) . . . . ?
C36 C37 C38 C39 0.8(4) . . . . ?
C42 C37 C38 C39 -177.6(3) . . . . ?
C37 C38 C39 C40 0.8(5) . . . . ?
C37 C38 C39 C46 -177.2(3) . . . . ?
C38 C39 C40 C41 -2.3(4) . . . . ?
C46 C39 C40 C41 175.7(3) . . . . ?
C39 C40 C41 C36 2.2(4) . . . . ?
C39 C40 C41 C50 179.8(3) . . . . ?
O3 C36 C41 C40 -179.7(2) . . . . ?
C37 C36 C41 C40 -0.5(4) . . . . ?
O3 C36 C41 C50 2.7(4) . . . . ?
C37 C36 C41 C50 -178.1(2) . . . . ?
C38 C37 C42 C44 -123.3(3) . . . . ?
C36 C37 C42 C44 58.5(3) . . . . ?
C38 C37 C42 C45 -3.4(4) . . . . ?
C36 C37 C42 C45 178.4(2) . . . . ?
C38 C37 C42 C43 115.2(3) . . . . ?
C36 C37 C42 C43 -63.1(3) . . . . ?
C40 C39 C46 C48X -179.4(8) . . . . ?
C38 C39 C46 C48X -1.4(9) . . . . ?
C40 C39 C46 C49 1.3(6) . . . . ?
C38 C39 C46 C49 179.3(4) . . . . ?
C40 C39 C46 C47 129.0(4) . . . . ?
C38 C39 C46 C47 -53.0(5) . . . . ?
C40 C39 C46 C49X -41.5(10) . . . . ?
C38 C39 C46 C49X 136.4(9) . . . . ?
C40 C39 C46 C48 -115.6(3) . . . . ?
C38 C39 C46 C48 62.4(4) . . . . ?
C40 C39 C46 C47X 65.9(8) . . . . ?
C38 C39 C46 C47X -116.1(8) . . . . ?
C40 C41 C50 C56 -84.4(3) . . . . ?
C36 C41 C50 C56 93.2(3) . . . . ?
C40 C41 C50 C33 45.5(3) . . . . ?
C36 C41 C50 C33 -136.9(3) . . . . ?
C34 C33 C50 C56 -28.8(3) . . . . ?
C32 C33 C50 C56 158.0(2) . . . . ?
C34 C33 C50 C41 -155.7(2) . . . . ?
C32 C33 C50 C41 31.1(3) . . . . ?
Nb2 O4 C51 C56 25.9(6) . . . . ?
Nb2 O4 C51 C52 -153.7(3) . . . . ?
O4 C51 C52 C53 -179.6(2) . . . . ?
C56 C51 C52 C53 0.8(4) . . . . ?
O4 C51 C52 C57 -2.2(4) . . . . ?
C56 C51 C52 C57 178.3(3) . . . . ?
C51 C52 C53 C54 -0.8(4) . . . . ?
C57 C52 C53 C54 -178.3(3) . . . . ?
C52 C53 C54 C55 -0.7(5) . . . . ?
C52 C53 C54 C61 179.3(3) . . . . ?
C53 C54 C55 C56 2.2(4) . . . . ?
C61 C54 C55 C56 -177.8(3) . . . . ?
C54 C55 C56 C51 -2.2(4) . . . . ?
C54 C55 C56 C50 179.7(2) . . . . ?
O4 C51 C56 C55 -178.9(2) . . . . ?
C52 C51 C56 C55 0.6(4) . . . . ?
O4 C51 C56 C50 -0.8(4) . . . . ?
C52 C51 C56 C50 178.7(2) . . . . ?
C41 C50 C56 C55 86.3(3) . . . . ?
C33 C50 C56 C55 -43.1(3) . . . . ?
C41 C50 C56 C51 -91.8(3) . . . . ?
C33 C50 C56 C51 138.8(2) . . . . ?
C53 C52 C57 C58 -131.1(3) . . . . ?
C51 C52 C57 C58 51.6(4) . . . . ?
C53 C52 C57 C59 -10.6(4) . . . . ?
C51 C52 C57 C59 172.0(3) . . . . ?
C53 C52 C57 C60 108.2(3) . . . . ?
C51 C52 C57 C60 -69.1(4) . . . . ?
C55 C54 C61 C64X -127.8(5) . . . . ?
C53 C54 C61 C64X 52.2(6) . . . . ?
C55 C54 C61 C63 51.7(7) . . . . ?
C53 C54 C61 C63 -128.3(6) . . . . ?
C55 C54 C61 C63X 1.8(7) . . . . ?
C53 C54 C61 C63X -178.3(6) . . . . ?
C55 C54 C61 C62 -179.9(4) . . . . ?
C53 C54 C61 C62 0.0(6) . . . . ?
C55 C54 C61 C64 -64.6(5) . . . . ?
C53 C54 C61 C64 115.4(4) . . . . ?
C55 C54 C61 C62X 116.7(5) . . . . ?
C53 C54 C61 C62X -63.3(5) . . . . ?
O1 Nb1 O5 C69 148.8(6) . . . . ?
O2 Nb1 O5 C69 -120.2(6) . . . . ?
N1 Nb1 O5 C69 15.5(9) . . . . ?
Cl2 Nb1 O5 C69 -31.8(6) . . . . ?
Cl1 Nb1 O5 C69 58.4(6) . . . . ?
Nb1 O5 C69 C70 -170.6(4) . . . . ?
O3 Nb2 O6 C71 -126.6(4) . . . . ?
O4 Nb2 O6 C71 140.1(4) . . . . ?
N2 Nb2 O6 C71 54.9(4) . . . . ?
Cl4 Nb2 O6 C71 -33.0(4) . . . . ?
Cl3 Nb2 O6 C71 27.0(5) . . . . ?
Nb2 O6 C71 C72 -177.1(3) . . . . ?
C84 C79 C80 C81 0.7(7) . . . . ?
C85 C79 C80 C81 175.9(7) . . . . ?
C79 C80 C81 C82 2.0(7) . . . . ?
C80 C81 C82 C83 -5.1(12) . . . . ?
C81 C82 C83 C84 5.6(15) . . . . ?
C80 C79 C84 C83 -0.2(13) . . . . ?
C85 C79 C84 C83 -175.6(9) . . . . ?
C82 C83 C84 C79 -3.3(17) . . . . ?

_refine_diff_density_max         1.216
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.082


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr515
_database_code_depnum_ccdc_archive 'CCDC 1043853'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C130 H179 Cl N Nb O8, 3.5(C2 H3 N)'
_chemical_formula_sum            'C137 H189.50 Cl N4.50 Nb O8'
_chemical_formula_weight         2155.78

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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   30.358(2)
_cell_length_b                   17.6674(12)
_cell_length_c                   24.5131(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.6385(17)
_cell_angle_gamma                90
_cell_volume                     13121.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      25.0

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_F_000             4660
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.166
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            69292
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.323
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             22952
_reflns_number_gt                13966
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHEXTL'
_computing_publication_material  'Bruker SHEXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0567P)²+25.6859P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22952
_refine_ls_number_parameters     1529
_refine_ls_number_restraints     308
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1833
_refine_ls_wR_factor_gt          0.1493
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.74710(2) 0.81130(2) 0.63746(2) 0.02798(11) Uani 1 1 d . . . . .
Cl1 Cl 0.71719(4) 0.85474(7) 0.72048(5) 0.0435(3) Uani 1 1 d . . . . .
O1 O 0.70417(9) 0.85934(15) 0.59046(12) 0.0271(7) Uani 1 1 d . . . . .
O2 O 0.78559(9) 0.89857(16) 0.63971(13) 0.0313(7) Uani 1 1 d . . . . .
O3 O 0.94974(9) 1.11714(17) 0.42291(14) 0.0367(8) Uani 1 1 d . . . . .
H3 H 0.9452 1.0855 0.4475 0.055 Uiso 1 1 calc R U . . .
O4 O 0.92977(11) 0.85849(18) 0.42417(14) 0.0442(9) Uani 1 1 d . . . . .
H4 H 0.9082 0.8783 0.4386 0.066 Uiso 1 1 calc R U . . .
O5 O 0.71260(9) 0.72048(16) 0.64093(12) 0.0299(7) Uani 1 1 d . . . . .
O6 O 0.78497(9) 0.76560(16) 0.58543(12) 0.0291(7) Uani 1 1 d . . . . .
O7 O 0.50645(11) 0.5238(2) 0.42457(18) 0.0554(11) Uani 1 1 d . . . . .
H7 H 0.5061 0.5707 0.4188 0.083 Uiso 1 1 calc R U . . .
O8 O 0.55154(12) 0.77297(19) 0.43351(16) 0.0514(10) Uani 1 1 d . . . . .
H8 H 0.5776 0.7577 0.4391 0.077 Uiso 1 1 calc R U . . .
C1 C 0.68678(14) 0.9131(2) 0.55400(19) 0.0289(10) Uani 1 1 d . . . . .
C2 C 0.64088(14) 0.9253(2) 0.54830(19) 0.0299(10) Uani 1 1 d . . . . .
C3 C 0.62633(15) 0.9822(3) 0.5118(2) 0.0369(12) Uani 1 1 d . . . . .
H3A H 0.5955 0.9919 0.5073 0.044 Uiso 1 1 calc R U . . .
C4 C 0.65434(15) 1.0253(3) 0.4816(2) 0.0383(12) Uani 1 1 d . . . . .
C5 C 0.69894(14) 1.0088(3) 0.4875(2) 0.0357(11) Uani 1 1 d . . . . .
H5 H 0.7187 1.0369 0.4668 0.043 Uiso 1 1 calc R U . . .
C6 C 0.71578(14) 0.9528(2) 0.52243(19) 0.0300(10) Uani 1 1 d . . . . .
C7 C 0.60769(14) 0.8795(3) 0.5798(2) 0.0342(11) Uani 1 1 d . . . . .
C8 C 0.61444(15) 0.7939(2) 0.5697(2) 0.0399(12) Uani 1 1 d . . . . .
H8A H 0.6432 0.7782 0.5863 0.060 Uiso 1 1 calc R U . . .
H8B H 0.6134 0.7842 0.5302 0.060 Uiso 1 1 calc R U . . .
H8C H 0.5910 0.7652 0.5860 0.060 Uiso 1 1 calc R U . . .
C9 C 0.55982(14) 0.8975(3) 0.5608(2) 0.0442(13) Uani 1 1 d . . . . .
H9A H 0.5399 0.8659 0.5809 0.066 Uiso 1 1 calc R U . . .
H9B H 0.5552 0.8872 0.5216 0.066 Uiso 1 1 calc R U . . .
H9C H 0.5537 0.9510 0.5678 0.066 Uiso 1 1 calc R U . . .
C10 C 0.61452(15) 0.8971(3) 0.6408(2) 0.0414(12) Uani 1 1 d . . . . .
H10A H 0.6066 0.9500 0.6473 0.062 Uiso 1 1 calc R U . . .
H10B H 0.6455 0.8888 0.6529 0.062 Uiso 1 1 calc R U . . .
H10C H 0.5958 0.8638 0.6614 0.062 Uiso 1 1 calc R U . . .
C11 C 0.63811(17) 1.0878(3) 0.4413(3) 0.0583(16) Uani 1 1 d . U . . .
C12 C 0.58802(18) 1.0966(4) 0.4380(3) 0.0688(19) Uani 1 1 d . U . . .
H12A H 0.5794 1.1364 0.4116 0.103 Uiso 1 1 calc R U . . .
H12B H 0.5783 1.1104 0.4740 0.103 Uiso 1 1 calc R U . . .
H12C H 0.5742 1.0487 0.4262 0.103 Uiso 1 1 calc R U . . .
C13 C 0.6514(2) 1.0669(5) 0.3841(3) 0.096(2) Uani 1 1 d . U . . .
H13A H 0.6367 1.0197 0.3724 0.144 Uiso 1 1 calc R U . . .
H13B H 0.6835 1.0602 0.3848 0.144 Uiso 1 1 calc R U . . .
H13C H 0.6425 1.1075 0.3585 0.144 Uiso 1 1 calc R U . . .
C14 C 0.6590(2) 1.1626(4) 0.4597(4) 0.098(2) Uani 1 1 d . U . . .
H14A H 0.6912 1.1580 0.4611 0.146 Uiso 1 1 calc R U . . .
H14B H 0.6496 1.1754 0.4962 0.146 Uiso 1 1 calc R U . . .
H14C H 0.6495 1.2025 0.4338 0.146 Uiso 1 1 calc R U . . .
C15 C 0.76511(13) 0.9369(2) 0.52841(18) 0.0279(10) Uani 1 1 d . . . . .
H15 H 0.7686 0.8852 0.5447 0.033 Uiso 1 1 calc R U . . .
C16 C 0.79879(13) 0.9692(2) 0.6232(2) 0.0299(10) Uani 1 1 d . . . . .
C17 C 0.82226(14) 1.0187(2) 0.6602(2) 0.0316(11) Uani 1 1 d . . . . .
C18 C 0.82986(14) 1.0924(3) 0.6409(2) 0.0367(12) Uani 1 1 d . . . . .
H18 H 0.8453 1.1268 0.6649 0.044 Uiso 1 1 calc R U . . .
C19 C 0.81621(15) 1.1177(3) 0.5891(2) 0.0374(12) Uani 1 1 d . . . . .
C20 C 0.79539(14) 1.0663(2) 0.5540(2) 0.0329(11) Uani 1 1 d . . . . .
H20 H 0.7860 1.0822 0.5182 0.040 Uiso 1 1 calc R U . . .
C21 C 0.78753(13) 0.9917(2) 0.56931(19) 0.0289(10) Uani 1 1 d . . . . .
C22 C 0.83806(15) 0.9970(3) 0.7193(2) 0.0375(12) Uani 1 1 d . . . . .
C23 C 0.79860(18) 0.9956(3) 0.7541(2) 0.0567(16) Uani 1 1 d . . . . .
H23A H 0.7842 1.0453 0.7529 0.085 Uiso 1 1 calc R U . . .
H23B H 0.8084 0.9835 0.7920 0.085 Uiso 1 1 calc R U . . .
H23C H 0.7776 0.9571 0.7400 0.085 Uiso 1 1 calc R U . . .
C24 C 0.86217(18) 0.9203(3) 0.7210(2) 0.0558(16) Uani 1 1 d . . . . .
H24A H 0.8416 0.8804 0.7083 0.084 Uiso 1 1 calc R U . . .
H24B H 0.8733 0.9094 0.7586 0.084 Uiso 1 1 calc R U . . .
H24C H 0.8870 0.9223 0.6973 0.084 Uiso 1 1 calc R U . . .
C25 C 0.87164(16) 1.0544(3) 0.7453(2) 0.0495(14) Uani 1 1 d . . . . .
H25A H 0.8964 1.0598 0.7219 0.074 Uiso 1 1 calc R U . . .
H25B H 0.8826 1.0361 0.7814 0.074 Uiso 1 1 calc R U . . .
H25C H 0.8572 1.1035 0.7491 0.074 Uiso 1 1 calc R U . . .
C26 C 0.82360(16) 1.1997(3) 0.5696(2) 0.0436(13) Uani 1 1 d . . . . .
C27 C 0.7795(2) 1.2356(3) 0.5531(3) 0.076(2) Uani 1 1 d . . . . .
H27A H 0.7655 1.2080 0.5220 0.114 Uiso 1 1 calc R U . . .
H27B H 0.7841 1.2885 0.5427 0.114 Uiso 1 1 calc R U . . .
H27C H 0.7605 1.2337 0.5839 0.114 Uiso 1 1 calc R U . . .
C28 C 0.85241(19) 1.1980(3) 0.5208(3) 0.0604(17) Uani 1 1 d . . . . .
H28A H 0.8799 1.1710 0.5309 0.091 Uiso 1 1 calc R U . . .
H28B H 0.8592 1.2499 0.5100 0.091 Uiso 1 1 calc R U . . .
H28C H 0.8366 1.1719 0.4902 0.091 Uiso 1 1 calc R U . . .
C29 C 0.8471(2) 1.2479(3) 0.6145(3) 0.072(2) Uani 1 1 d . . . . .
H29A H 0.8291 1.2500 0.6462 0.109 Uiso 1 1 calc R U . . .
H29B H 0.8514 1.2993 0.6006 0.109 Uiso 1 1 calc R U . . .
H29C H 0.8759 1.2254 0.6252 0.109 Uiso 1 1 calc R U . . .
C30 C 0.78486(14) 0.9338(2) 0.47250(18) 0.0278(10) Uani 1 1 d . . . . .
C31 C 0.82528(13) 0.9655(2) 0.46126(19) 0.0284(10) Uani 1 1 d . . . . .
H31 H 0.8411 0.9936 0.4891 0.034 Uiso 1 1 calc R U . . .
C32 C 0.84327(14) 0.9576(2) 0.41092(19) 0.0299(10) Uani 1 1 d . . . . .
C33 C 0.82066(15) 0.9164(3) 0.3703(2) 0.0385(12) Uani 1 1 d . . . . .
H33 H 0.8323 0.9112 0.3354 0.046 Uiso 1 1 calc R U . . .
C34 C 0.78077(16) 0.8826(3) 0.3808(2) 0.0429(13) Uani 1 1 d . . . . .
H34 H 0.7656 0.8529 0.3533 0.052 Uiso 1 1 calc R U . . .
C35 C 0.76310(15) 0.8917(3) 0.4307(2) 0.0357(11) Uani 1 1 d . . . . .
H35 H 0.7355 0.8689 0.4368 0.043 Uiso 1 1 calc R U . . .
C36 C 0.88603(14) 0.9992(2) 0.40154(19) 0.0304(10) Uani 1 1 d . . . . .
H36 H 0.9039 0.9996 0.4373 0.036 Uiso 1 1 calc R U . . .
C37 C 0.90992(14) 1.1363(3) 0.3955(2) 0.0324(11) Uani 1 1 d . . . . .
C38 C 0.90464(14) 1.2104(2) 0.37549(19) 0.0326(11) Uani 1 1 d . . . . .
C39 C 0.86495(15) 1.2276(3) 0.3462(2) 0.0406(12) Uani 1 1 d . . . . .
H39 H 0.8610 1.2774 0.3320 0.049 Uiso 1 1 calc R U . . .
C40 C 0.83101(15) 1.1758(3) 0.3369(2) 0.0434(13) Uani 1 1 d . . . . .
C41 C 0.83794(15) 1.1029(3) 0.3572(2) 0.0395(12) Uani 1 1 d . . . . .
H41 H 0.8153 1.0662 0.3510 0.047 Uiso 1 1 calc R U . . .
C42 C 0.87688(14) 1.0821(2) 0.38606(18) 0.0290(10) Uani 1 1 d . . . . .
C43 C 0.94218(15) 1.2693(3) 0.3829(2) 0.0362(11) Uani 1 1 d . . . . .
C44 C 0.95353(17) 1.2840(3) 0.4440(2) 0.0461(13) Uani 1 1 d . . . . .
H44A H 0.9763 1.3233 0.4481 0.069 Uiso 1 1 calc R U . . .
H44B H 0.9646 1.2372 0.4615 0.069 Uiso 1 1 calc R U . . .
H44C H 0.9270 1.3008 0.4613 0.069 Uiso 1 1 calc R U . . .
C45 C 0.92923(17) 1.3448(3) 0.3560(3) 0.0539(15) Uani 1 1 d . . . . .
H45A H 0.9231 1.3373 0.3167 0.081 Uiso 1 1 calc R U . . .
H45B H 0.9535 1.3810 0.3621 0.081 Uiso 1 1 calc R U . . .
H45C H 0.9028 1.3646 0.3720 0.081 Uiso 1 1 calc R U . . .
C46 C 0.98279(15) 1.2403(3) 0.3549(2) 0.0429(13) Uani 1 1 d . . . . .
H46A H 0.9748 1.2308 0.3162 0.064 Uiso 1 1 calc R U . . .
H46B H 0.9932 1.1933 0.3725 0.064 Uiso 1 1 calc R U . . .
H46C H 1.0063 1.2785 0.3582 0.064 Uiso 1 1 calc R U . . .
C47 C 0.78759(16) 1.1944(3) 0.3043(3) 0.0666(17) Uani 1 1 d D U . . .
C48 C 0.7478(3) 1.1762(8) 0.3373(7) 0.098(4) Uani 0.81(2) 1 d D U P A 1
H48A H 0.7205 1.1885 0.3156 0.147 Uiso 0.81(2) 1 calc R U P A 1
H48B H 0.7479 1.1222 0.3465 0.147 Uiso 0.81(2) 1 calc R U P A 1
H48C H 0.7494 1.2062 0.3710 0.147 Uiso 0.81(2) 1 calc R U P A 1
C49 C 0.7839(4) 1.1450(5) 0.2523(5) 0.084(3) Uani 0.81(2) 1 d D U P A 1
H49A H 0.8090 1.1554 0.2302 0.126 Uiso 0.81(2) 1 calc R U P A 1
H49B H 0.7840 1.0915 0.2627 0.126 Uiso 0.81(2) 1 calc R U P A 1
H49C H 0.7564 1.1569 0.2311 0.126 Uiso 0.81(2) 1 calc R U P A 1
C50 C 0.7856(5) 1.2786(4) 0.2878(5) 0.060(3) Uani 0.81(2) 1 d D U P A 1
H50A H 0.8110 1.2909 0.2666 0.091 Uiso 0.81(2) 1 calc R U P A 1
H50B H 0.7582 1.2884 0.2655 0.091 Uiso 0.81(2) 1 calc R U P A 1
H50C H 0.7864 1.3101 0.3207 0.091 Uiso 0.81(2) 1 calc R U P A 1
C48X C 0.7594(10) 1.204(3) 0.3567(10) 0.067(7) Uani 0.19(2) 1 d D U P A 2
H48D H 0.7727 1.2439 0.3804 0.100 Uiso 0.19(2) 1 calc R U P A 2
H48E H 0.7291 1.2187 0.3450 0.100 Uiso 0.19(2) 1 calc R U P A 2
H48F H 0.7591 1.1564 0.3769 0.100 Uiso 0.19(2) 1 calc R U P A 2
C49X C 0.7631(17) 1.132(2) 0.272(2) 0.099(11) Uani 0.19(2) 1 d D U P A 2
H49D H 0.7362 1.1532 0.2540 0.148 Uiso 0.19(2) 1 calc R U P A 2
H49E H 0.7821 1.1116 0.2452 0.148 Uiso 0.19(2) 1 calc R U P A 2
H49F H 0.7553 1.0921 0.2976 0.148 Uiso 0.19(2) 1 calc R U P A 2
C50X C 0.782(2) 1.2708(18) 0.274(2) 0.080(12) Uani 0.19(2) 1 d D U P A 2
H50D H 0.7982 1.3104 0.2947 0.120 Uiso 0.19(2) 1 calc R U P A 2
H50E H 0.7941 1.2663 0.2376 0.120 Uiso 0.19(2) 1 calc R U P A 2
H50F H 0.7508 1.2840 0.2693 0.120 Uiso 0.19(2) 1 calc R U P A 2
C51 C 0.93506(15) 0.8921(3) 0.3739(2) 0.0341(11) Uani 1 1 d . . . . .
C52 C 0.96290(15) 0.8560(3) 0.3378(2) 0.0365(11) Uani 1 1 d . . . . .
C53 C 0.96730(15) 0.8905(3) 0.2877(2) 0.0375(12) Uani 1 1 d . . . . .
H53 H 0.9857 0.8670 0.2627 0.045 Uiso 1 1 calc R U . . .
C54 C 0.94608(14) 0.9580(3) 0.2718(2) 0.0340(11) Uani 1 1 d . . . . .
C55 C 0.91967(14) 0.9911(3) 0.30909(19) 0.0324(11) Uani 1 1 d . . . . .
H55 H 0.9047 1.0368 0.2992 0.039 Uiso 1 1 calc R U . . .
C56 C 0.91409(14) 0.9604(2) 0.36026(19) 0.0306(10) Uani 1 1 d . . . . .
C57 C 0.98768(17) 0.7819(3) 0.3546(2) 0.0461(13) Uani 1 1 d . . . . .
C58 C 1.0161(2) 0.7550(3) 0.3092(3) 0.0713(19) Uani 1 1 d . . . . .
H58A H 1.0382 0.7937 0.3023 0.107 Uiso 1 1 calc R U . . .
H58B H 0.9974 0.7461 0.2758 0.107 Uiso 1 1 calc R U . . .
H58C H 1.0311 0.7078 0.3205 0.107 Uiso 1 1 calc R U . . .
C59 C 1.01834(19) 0.7960(3) 0.4057(3) 0.0645(18) Uani 1 1 d . . . . .
H59A H 1.0402 0.8345 0.3977 0.097 Uiso 1 1 calc R U . . .
H59B H 1.0334 0.7488 0.4165 0.097 Uiso 1 1 calc R U . . .
H59C H 1.0009 0.8137 0.4355 0.097 Uiso 1 1 calc R U . . .
C60 C 0.9545(2) 0.7187(3) 0.3653(2) 0.0586(16) Uani 1 1 d . . . . .
H60A H 0.9706 0.6724 0.3762 0.088 Uiso 1 1 calc R U . . .
H60B H 0.9359 0.7090 0.3319 0.088 Uiso 1 1 calc R U . . .
H60C H 0.9360 0.7343 0.3946 0.088 Uiso 1 1 calc R U . . .
C61 C 0.95315(16) 0.9937(3) 0.2157(2) 0.0412(12) Uani 1 1 d . . . . .
C62 C 1.00159(17) 1.0176(3) 0.2136(2) 0.0574(16) Uani 1 1 d . . . . .
H62A H 1.0207 0.9733 0.2201 0.086 Uiso 1 1 calc R U . . .
H62B H 1.0087 1.0558 0.2418 0.086 Uiso 1 1 calc R U . . .
H62C H 1.0063 1.0389 0.1775 0.086 Uiso 1 1 calc R U . . .
C63 C 0.92393(18) 1.0640(3) 0.2049(2) 0.0502(14) Uani 1 1 d . . . . .
H63A H 0.9287 1.0842 0.1685 0.075 Uiso 1 1 calc R U . . .
H63B H 0.9316 1.1026 0.2326 0.075 Uiso 1 1 calc R U . . .
H63C H 0.8928 1.0499 0.2067 0.075 Uiso 1 1 calc R U . . .
C64 C 0.94112(19) 0.9368(3) 0.1700(2) 0.0537(15) Uani 1 1 d . . . . .
H64A H 0.9586 0.8906 0.1761 0.081 Uiso 1 1 calc R U . . .
H64B H 0.9475 0.9590 0.1347 0.081 Uiso 1 1 calc R U . . .
H64C H 0.9096 0.9245 0.1700 0.081 Uiso 1 1 calc R U . . .
C65 C 0.69449(13) 0.6508(2) 0.62728(19) 0.0295(10) Uani 1 1 d . . . . .
C66 C 0.69727(13) 0.6259(2) 0.57294(19) 0.0283(10) Uani 1 1 d . . . . .
C67 C 0.68247(14) 0.5535(2) 0.5588(2) 0.0311(11) Uani 1 1 d . . . . .
H67 H 0.6856 0.5357 0.5227 0.037 Uiso 1 1 calc R U . . .
C68 C 0.66330(15) 0.5065(3) 0.5959(2) 0.0371(12) Uani 1 1 d . . . . .
C69 C 0.65899(15) 0.5345(3) 0.6483(2) 0.0364(11) Uani 1 1 d . . . . .
H69 H 0.6455 0.5030 0.6739 0.044 Uiso 1 1 calc R U . . .
C70 C 0.67346(14) 0.6065(3) 0.6654(2) 0.0337(11) Uani 1 1 d . . . . .
C71 C 0.66563(16) 0.6342(3) 0.7235(2) 0.0404(12) Uani 1 1 d . . . . .
C72 C 0.64055(19) 0.5764(3) 0.7562(2) 0.0573(16) Uani 1 1 d . . . . .
H72A H 0.6117 0.5663 0.7374 0.086 Uiso 1 1 calc R U . . .
H72B H 0.6364 0.5965 0.7928 0.086 Uiso 1 1 calc R U . . .
H72C H 0.6575 0.5292 0.7594 0.086 Uiso 1 1 calc R U . . .
C73 C 0.70974(16) 0.6495(3) 0.7558(2) 0.0442(13) Uani 1 1 d . . . . .
H73A H 0.7285 0.6044 0.7547 0.066 Uiso 1 1 calc R U . . .
H73B H 0.7043 0.6614 0.7938 0.066 Uiso 1 1 calc R U . . .
H73C H 0.7246 0.6923 0.7394 0.066 Uiso 1 1 calc R U . . .
C74 C 0.63705(16) 0.7068(3) 0.7197(2) 0.0445(13) Uani 1 1 d . . . . .
H74A H 0.6523 0.7459 0.6998 0.067 Uiso 1 1 calc R U . . .
H74B H 0.6321 0.7249 0.7566 0.067 Uiso 1 1 calc R U . . .
H74C H 0.6086 0.6954 0.7003 0.067 Uiso 1 1 calc R U . . .
C75 C 0.64698(18) 0.4265(3) 0.5778(2) 0.0478(14) Uani 1 1 d . . . . .
C76 C 0.6860(2) 0.3802(3) 0.5617(3) 0.078(2) Uani 1 1 d . . . . .
H76A H 0.7010 0.4069 0.5332 0.117 Uiso 1 1 calc R U . . .
H76B H 0.6757 0.3309 0.5479 0.117 Uiso 1 1 calc R U . . .
H76C H 0.7066 0.3729 0.5937 0.117 Uiso 1 1 calc R U . . .
C77 C 0.6231(3) 0.3861(3) 0.6222(3) 0.083(2) Uani 1 1 d . . . . .
H77A H 0.6429 0.3811 0.6551 0.125 Uiso 1 1 calc R U . . .
H77B H 0.6139 0.3357 0.6092 0.125 Uiso 1 1 calc R U . . .
H77C H 0.5970 0.4154 0.6308 0.125 Uiso 1 1 calc R U . . .
C78 C 0.6136(2) 0.4347(3) 0.5284(3) 0.0702(19) Uani 1 1 d . . . . .
H78A H 0.5883 0.4646 0.5388 0.105 Uiso 1 1 calc R U . . .
H78B H 0.6036 0.3845 0.5161 0.105 Uiso 1 1 calc R U . . .
H78C H 0.6277 0.4604 0.4986 0.105 Uiso 1 1 calc R U . . .
C79 C 0.71689(13) 0.6767(2) 0.53026(18) 0.0268(10) Uani 1 1 d . . . . .
H79 H 0.7147 0.7297 0.5442 0.032 Uiso 1 1 calc R U . . .
C80 C 0.79792(14) 0.7053(2) 0.55520(19) 0.0305(10) Uani 1 1 d . . . . .
C81 C 0.84346(13) 0.6929(3) 0.54756(19) 0.0314(10) Uani 1 1 d . . . . .
C82 C 0.85413(15) 0.6274(3) 0.5204(2) 0.0416(13) Uani 1 1 d . . . . .
H82 H 0.8845 0.6161 0.5175 0.050 Uiso 1 1 calc R U . . .
C83 C 0.82300(16) 0.5769(3) 0.4971(2) 0.0448(13) Uani 1 1 d . . . . .
C84 C 0.77911(15) 0.5949(3) 0.5005(2) 0.0364(11) Uani 1 1 d . . . . .
H84 H 0.7572 0.5629 0.4835 0.044 Uiso 1 1 calc R U . . .
C85 C 0.76615(13) 0.6596(2) 0.52867(19) 0.0290(10) Uani 1 1 d . . . . .
C86 C 0.88006(14) 0.7507(3) 0.5647(2) 0.0395(12) Uani 1 1 d . . . . .
C87 C 0.86742(16) 0.8279(3) 0.5407(3) 0.0560(16) Uani 1 1 d . . . . .
H87A H 0.8610 0.8231 0.5012 0.084 Uiso 1 1 calc R U . . .
H87B H 0.8919 0.8634 0.5479 0.084 Uiso 1 1 calc R U . . .
H87C H 0.8412 0.8468 0.5576 0.084 Uiso 1 1 calc R U . . .
C88 C 0.88596(15) 0.7574(3) 0.6271(2) 0.0501(15) Uani 1 1 d . . . . .
H88A H 0.9098 0.7932 0.6370 0.075 Uiso 1 1 calc R U . . .
H88B H 0.8934 0.7077 0.6429 0.075 Uiso 1 1 calc R U . . .
H88C H 0.8584 0.7755 0.6414 0.075 Uiso 1 1 calc R U . . .
C89 C 0.92425(14) 0.7286(3) 0.5433(2) 0.0466(14) Uani 1 1 d . . . . .
H89A H 0.9211 0.7242 0.5034 0.070 Uiso 1 1 calc R U . . .
H89B H 0.9338 0.6799 0.5592 0.070 Uiso 1 1 calc R U . . .
H89C H 0.9463 0.7674 0.5536 0.070 Uiso 1 1 calc R U . . .
C90 C 0.83847(18) 0.5062(3) 0.4663(3) 0.0638(17) Uani 1 1 d . U . . .
C91 C 0.8006(2) 0.4565(4) 0.4454(4) 0.116(3) Uani 1 1 d . U . . .
H91A H 0.7844 0.4386 0.4762 0.174 Uiso 1 1 calc R U . . .
H91B H 0.8121 0.4130 0.4260 0.174 Uiso 1 1 calc R U . . .
H91C H 0.7807 0.4856 0.4203 0.174 Uiso 1 1 calc R U . . .
C92 C 0.8691(2) 0.4589(4) 0.5054(4) 0.101(3) Uani 1 1 d . U . . .
H92A H 0.8534 0.4449 0.5376 0.152 Uiso 1 1 calc R U . . .
H92B H 0.8953 0.4887 0.5168 0.152 Uiso 1 1 calc R U . . .
H92C H 0.8781 0.4129 0.4867 0.152 Uiso 1 1 calc R U . . .
C93 C 0.8650(3) 0.5330(4) 0.4172(3) 0.102(2) Uani 1 1 d . U . . .
H93A H 0.8739 0.4888 0.3963 0.152 Uiso 1 1 calc R U . . .
H93B H 0.8914 0.5607 0.4311 0.152 Uiso 1 1 calc R U . . .
H93C H 0.8464 0.5662 0.3935 0.152 Uiso 1 1 calc R U . . .
C94 C 0.69236(13) 0.6759(2) 0.47422(19) 0.0293(10) Uani 1 1 d . . . . .
C95 C 0.64798(13) 0.6553(2) 0.46715(19) 0.0268(10) Uani 1 1 d . . . . .
H95 H 0.6330 0.6396 0.4980 0.032 Uiso 1 1 calc R U . . .
C96 C 0.62505(14) 0.6571(2) 0.4160(2) 0.0309(11) Uani 1 1 d . . . . .
C97 C 0.64632(15) 0.6829(3) 0.3712(2) 0.0398(12) Uani 1 1 d . . . . .
H97 H 0.6307 0.6863 0.3365 0.048 Uiso 1 1 calc R U . . .
C98 C 0.69039(15) 0.7038(3) 0.3769(2) 0.0414(12) Uani 1 1 d . . . . .
H98 H 0.7050 0.7207 0.3460 0.050 Uiso 1 1 calc R U . . .
C99 C 0.71321(14) 0.7003(3) 0.4274(2) 0.0350(11) Uani 1 1 d . . . . .
H99 H 0.7434 0.7145 0.4307 0.042 Uiso 1 1 calc R U . . .
C100 C 0.57893(14) 0.6230(2) 0.4109(2) 0.0319(11) Uani 1 1 d . . . . .
H100 H 0.5673 0.6263 0.4481 0.038 Uiso 1 1 calc R U . . .
C101 C 0.54423(17) 0.4930(3) 0.4052(2) 0.0499(15) Uani 1 1 d . . . . .
C102 C 0.5444(2) 0.4152(3) 0.3945(3) 0.071(2) Uani 1 1 d . . . . .
C103 C 0.5821(2) 0.3864(3) 0.3735(3) 0.083(3) Uani 1 1 d . . . . .
H103 H 0.5833 0.3335 0.3667 0.100 Uiso 1 1 calc R U . . .
C104 C 0.61801(19) 0.4294(3) 0.3617(3) 0.0599(17) Uani 1 1 d . . . . .
C105 C 0.61687(16) 0.5061(3) 0.3751(2) 0.0440(13) Uani 1 1 d . . . . .
H105 H 0.6417 0.5368 0.3688 0.053 Uiso 1 1 calc R U . . .
C106 C 0.58072(15) 0.5385(3) 0.3971(2) 0.0398(12) Uani 1 1 d . . . . .
C107 C 0.4983(4) 0.3681(6) 0.3975(6) 0.050(3) Uani 0.584(14) 1 d D U P B 1
C108 C 0.4902(7) 0.3636(11) 0.4579(6) 0.071(5) Uani 0.584(14) 1 d D U P B 1
H10D H 0.4872 0.4149 0.4725 0.106 Uiso 0.584(14) 1 calc R U P B 1
H10E H 0.4630 0.3352 0.4626 0.106 Uiso 0.584(14) 1 calc R U P B 1
H10F H 0.5150 0.3380 0.4775 0.106 Uiso 0.584(14) 1 calc R U P B 1
C109 C 0.4568(4) 0.4032(8) 0.3660(6) 0.077(4) Uani 0.584(14) 1 d D U P B 1
H10G H 0.4522 0.4548 0.3792 0.116 Uiso 0.584(14) 1 calc R U P B 1
H10H H 0.4614 0.4044 0.3268 0.116 Uiso 0.584(14) 1 calc R U P B 1
H10I H 0.4308 0.3722 0.3723 0.116 Uiso 0.584(14) 1 calc R U P B 1
C110 C 0.5029(4) 0.2895(5) 0.3749(6) 0.059(4) Uani 0.584(14) 1 d D U P B 1
H11A H 0.5082 0.2925 0.3360 0.089 Uiso 0.584(14) 1 calc R U P B 1
H11B H 0.5278 0.2638 0.3945 0.089 Uiso 0.584(14) 1 calc R U P B 1
H11C H 0.4757 0.2610 0.3796 0.089 Uiso 0.584(14) 1 calc R U P B 1
C17X C 0.5145(6) 0.3592(8) 0.4164(8) 0.048(4) Uani 0.416(14) 1 d D U P B 2
C18X C 0.4974(8) 0.3743(12) 0.4723(7) 0.049(5) Uani 0.416(14) 1 d D U P B 2
H18A H 0.4779 0.3327 0.4820 0.073 Uiso 0.416(14) 1 calc R U P B 2
H18B H 0.5223 0.3778 0.4996 0.073 Uiso 0.416(14) 1 calc R U P B 2
H18C H 0.4808 0.4219 0.4714 0.073 Uiso 0.416(14) 1 calc R U P B 2
C19X C 0.4753(6) 0.3698(10) 0.3719(6) 0.053(4) Uani 0.416(14) 1 d D U P B 2
H19A H 0.4511 0.3357 0.3799 0.080 Uiso 0.416(14) 1 calc R U P B 2
H19B H 0.4649 0.4223 0.3725 0.080 Uiso 0.416(14) 1 calc R U P B 2
H19C H 0.4855 0.3581 0.3357 0.080 Uiso 0.416(14) 1 calc R U P B 2
C20X C 0.5272(4) 0.2756(6) 0.4152(6) 0.045(4) Uani 0.416(14) 1 d D U P B 2
H20A H 0.5043 0.2453 0.4311 0.068 Uiso 0.416(14) 1 calc R U P B 2
H20B H 0.5303 0.2598 0.3773 0.068 Uiso 0.416(14) 1 calc R U P B 2
H20C H 0.5554 0.2681 0.4365 0.068 Uiso 0.416(14) 1 calc R U P B 2
C111 C 0.6584(2) 0.3961(3) 0.3373(3) 0.0709(17) Uani 1 1 d D U . . .
C112 C 0.6459(5) 0.3155(6) 0.3146(5) 0.049(3) Uani 0.616(14) 1 d D U P C 1
H11D H 0.6201 0.3193 0.2887 0.074 Uiso 0.616(14) 1 calc R U P C 1
H11E H 0.6708 0.2946 0.2960 0.074 Uiso 0.616(14) 1 calc R U P C 1
H11F H 0.6391 0.2823 0.3449 0.074 Uiso 0.616(14) 1 calc R U P C 1
C113 C 0.6962(4) 0.3956(8) 0.3759(5) 0.073(4) Uani 0.616(14) 1 d D U P C 1
H11G H 0.7215 0.3737 0.3587 0.110 Uiso 0.616(14) 1 calc R U P C 1
H11H H 0.7032 0.4476 0.3875 0.110 Uiso 0.616(14) 1 calc R U P C 1
H11I H 0.6896 0.3652 0.4078 0.110 Uiso 0.616(14) 1 calc R U P C 1
C114 C 0.6670(4) 0.4420(5) 0.2830(4) 0.058(3) Uani 0.616(14) 1 d D U P C 1
H11J H 0.6404 0.4407 0.2581 0.087 Uiso 0.616(14) 1 calc R U P C 1
H11K H 0.6743 0.4947 0.2924 0.087 Uiso 0.616(14) 1 calc R U P C 1
H11L H 0.6917 0.4189 0.2651 0.087 Uiso 0.616(14) 1 calc R U P C 1
C12X C 0.6558(9) 0.3246(11) 0.3038(10) 0.069(7) Uani 0.384(14) 1 d D U P C 2
H12D H 0.6852 0.3123 0.2917 0.104 Uiso 0.384(14) 1 calc R U P C 2
H12E H 0.6454 0.2829 0.3260 0.104 Uiso 0.384(14) 1 calc R U P C 2
H12F H 0.6353 0.3320 0.2717 0.104 Uiso 0.384(14) 1 calc R U P C 2
C13X C 0.6885(5) 0.3703(12) 0.3913(7) 0.067(4) Uani 0.384(14) 1 d D U P C 2
H13S H 0.6924 0.4133 0.4164 0.100 Uiso 0.384(14) 1 calc R U P C 2
H13T H 0.6739 0.3288 0.4095 0.100 Uiso 0.384(14) 1 calc R U P C 2
H13U H 0.7174 0.3534 0.3805 0.100 Uiso 0.384(14) 1 calc R U P C 2
C14X C 0.6941(6) 0.4569(8) 0.3212(11) 0.093(7) Uani 0.384(14) 1 d D U P C 2
H14D H 0.6929 0.5009 0.3454 0.139 Uiso 0.384(14) 1 calc R U P C 2
H14E H 0.7236 0.4343 0.3250 0.139 Uiso 0.384(14) 1 calc R U P C 2
H14F H 0.6877 0.4730 0.2832 0.139 Uiso 0.384(14) 1 calc R U P C 2
C115 C 0.53272(15) 0.7393(3) 0.3870(2) 0.0384(12) Uani 1 1 d . . . . .
C116 C 0.49976(17) 0.7770(3) 0.3557(3) 0.0503(15) Uani 1 1 d . . . . .
C117 C 0.48080(17) 0.7397(4) 0.3103(3) 0.0575(16) Uani 1 1 d . . . . .
H117 H 0.4577 0.7643 0.2892 0.069 Uiso 1 1 calc R U . . .
C118 C 0.49372(16) 0.6683(4) 0.2939(2) 0.0518(15) Uani 1 1 d . . . . .
C119 C 0.52696(14) 0.6336(3) 0.3258(2) 0.0394(12) Uani 1 1 d . . . . .
H119 H 0.5371 0.5853 0.3149 0.047 Uiso 1 1 calc R U . . .
C120 C 0.54618(14) 0.6660(3) 0.3727(2) 0.0335(11) Uani 1 1 d . . . . .
C121 C 0.4844(2) 0.8572(3) 0.3722(4) 0.080(2) Uani 1 1 d . . . . .
C122 C 0.5235(2) 0.9127(3) 0.3739(4) 0.110(3) Uani 1 1 d . . . . .
H12G H 0.5471 0.8939 0.3995 0.165 Uiso 1 1 calc R U . . .
H12H H 0.5137 0.9625 0.3860 0.165 Uiso 1 1 calc R U . . .
H12I H 0.5345 0.9171 0.3373 0.165 Uiso 1 1 calc R U . . .
C123 C 0.4487(2) 0.8885(4) 0.3299(4) 0.124(4) Uani 1 1 d . . . . .
H12J H 0.4618 0.8963 0.2948 0.185 Uiso 1 1 calc R U . . .
H12K H 0.4375 0.9367 0.3430 0.185 Uiso 1 1 calc R U . . .
H12L H 0.4244 0.8521 0.3252 0.185 Uiso 1 1 calc R U . . .
C124 C 0.4639(2) 0.8523(4) 0.4275(4) 0.094(3) Uani 1 1 d . . . . .
H12M H 0.4382 0.8186 0.4245 0.140 Uiso 1 1 calc R U . . .
H12N H 0.4547 0.9029 0.4386 0.140 Uiso 1 1 calc R U . . .
H12O H 0.4858 0.8322 0.4549 0.140 Uiso 1 1 calc R U . . .
C125 C 0.47265(18) 0.6281(5) 0.2433(2) 0.087(2) Uani 1 1 d D U . . .
C126 C 0.4323(3) 0.6723(10) 0.2195(4) 0.117(3) Uani 0.92(3) 1 d D U P D 1
H12P H 0.4102 0.6756 0.2468 0.175 Uiso 0.92(3) 1 calc R U P D 1
H12Q H 0.4414 0.7234 0.2094 0.175 Uiso 0.92(3) 1 calc R U P D 1
H12R H 0.4196 0.6461 0.1869 0.175 Uiso 0.92(3) 1 calc R U P D 1
C127 C 0.4579(5) 0.5478(6) 0.2587(4) 0.102(3) Uani 0.92(3) 1 d D U P D 1
H12S H 0.4353 0.5513 0.2855 0.153 Uiso 0.92(3) 1 calc R U P D 1
H12T H 0.4456 0.5217 0.2260 0.153 Uiso 0.92(3) 1 calc R U P D 1
H12U H 0.4833 0.5194 0.2746 0.153 Uiso 0.92(3) 1 calc R U P D 1
C128 C 0.5077(3) 0.6219(7) 0.2016(4) 0.085(3) Uani 0.92(3) 1 d D U P D 1
H12V H 0.4952 0.5964 0.1687 0.127 Uiso 0.92(3) 1 calc R U P D 1
H12W H 0.5176 0.6727 0.1920 0.127 Uiso 0.92(3) 1 calc R U P D 1
H12X H 0.5329 0.5927 0.2173 0.127 Uiso 0.92(3) 1 calc R U P D 1
C26X C 0.4226(8) 0.637(7) 0.231(4) 0.092(8) Uani 0.08(3) 1 d D U P D 2
H26A H 0.4079 0.6371 0.2657 0.138 Uiso 0.08(3) 1 calc R U P D 2
H26B H 0.4166 0.6846 0.2118 0.138 Uiso 0.08(3) 1 calc R U P D 2
H26C H 0.4115 0.5945 0.2085 0.138 Uiso 0.08(3) 1 calc R U P D 2
C27X C 0.479(4) 0.546(3) 0.268(4) 0.091(9) Uani 0.08(3) 1 d D U P D 2
H27D H 0.4639 0.5432 0.3025 0.136 Uiso 0.08(3) 1 calc R U P D 2
H27E H 0.4659 0.5089 0.2423 0.136 Uiso 0.08(3) 1 calc R U P D 2
H27F H 0.5103 0.5356 0.2754 0.136 Uiso 0.08(3) 1 calc R U P D 2
C28X C 0.497(3) 0.627(6) 0.190(2) 0.089(9) Uani 0.08(3) 1 d D U P D 2
H28D H 0.4791 0.5996 0.1620 0.134 Uiso 0.08(3) 1 calc R U P D 2
H28E H 0.5012 0.6795 0.1780 0.134 Uiso 0.08(3) 1 calc R U P D 2
H28F H 0.5255 0.6026 0.1967 0.134 Uiso 0.08(3) 1 calc R U P D 2
N1 N 0.79511(12) 0.7572(2) 0.69991(17) 0.0378(10) Uani 1 1 d . . . . .
C129 C 0.8226(2) 0.7369(4) 0.7289(3) 0.079(2) Uani 1 1 d . . . . .
C130 C 0.8612(2) 0.7153(5) 0.7682(4) 0.113(3) Uani 1 1 d . . . . .
H13D H 0.8875 0.7435 0.7590 0.169 Uiso 1 1 calc R U . . .
H13E H 0.8668 0.6609 0.7653 0.169 Uiso 1 1 calc R U . . .
H13F H 0.8541 0.7276 0.8057 0.169 Uiso 1 1 calc R U . . .
N2 N 0.9476(2) 1.0270(4) 0.5216(2) 0.090(2) Uani 1 1 d . . . . .
C131 C 0.95497(19) 1.0060(3) 0.5650(3) 0.0577(16) Uani 1 1 d . . . . .
C132 C 0.96464(18) 0.9801(3) 0.6204(2) 0.0509(14) Uani 1 1 d . . . . .
H13G H 0.9705 1.0237 0.6444 0.076 Uiso 1 1 calc R U . . .
H13H H 0.9906 0.9470 0.6217 0.076 Uiso 1 1 calc R U . . .
H13I H 0.9393 0.9518 0.6327 0.076 Uiso 1 1 calc R U . . .
N3 N 0.6924(3) 1.2174(4) 0.6730(3) 0.121(3) Uani 1 1 d . . . . .
C133 C 0.6928(2) 1.1559(4) 0.6562(3) 0.0734(19) Uani 1 1 d . . . . .
C134 C 0.6956(2) 1.0811(4) 0.6369(3) 0.0714(19) Uani 1 1 d . . . . .
H13J H 0.7266 1.0681 0.6329 0.107 Uiso 1 1 calc R U . . .
H13K H 0.6791 1.0768 0.6014 0.107 Uiso 1 1 calc R U . . .
H13L H 0.6831 1.0465 0.6630 0.107 Uiso 1 1 calc R U . . .
N4 N 0.8206(2) 0.5656(5) 0.7163(4) 0.132(3) Uani 1 1 d . . . . .
C135 C 0.8035(2) 0.5378(5) 0.6785(4) 0.089(2) Uani 1 1 d . . . . .
C136 C 0.7830(3) 0.4959(5) 0.6354(3) 0.099(3) Uani 1 1 d . . . . .
H13M H 0.7937 0.4436 0.6372 0.149 Uiso 1 1 calc R U . . .
H13N H 0.7899 0.5185 0.6005 0.149 Uiso 1 1 calc R U . . .
H13O H 0.7509 0.4964 0.6386 0.149 Uiso 1 1 calc R U . . .
N5 N 0.8084(7) 0.7821(13) 0.8137(11) 0.080(7) Uiso 0.25 1 d . . P . .
C137 C 0.8211(8) 0.7754(15) 0.8568(12) 0.068(7) Uiso 0.25 1 d . . P . .
C138 C 0.8410(8) 0.7631(15) 0.9090(11) 0.069(7) Uiso 0.25 1 d . . P . .
H13P H 0.8688 0.7357 0.9060 0.103 Uiso 0.25 1 calc R U P . .
H13Q H 0.8212 0.7332 0.9305 0.103 Uiso 0.25 1 calc R U P . .
H13R H 0.8470 0.8119 0.9270 0.103 Uiso 0.25 1 calc R U P . .


_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
Nb1 O1 1.886(3) . ?
Nb1 O5 1.921(3) . ?
Nb1 O2 1.933(3) . ?
Nb1 O6 1.946(3) . ?
Nb1 N1 2.258(4) . ?
Nb1 Cl1 2.4063(13) . ?
O1 C1 1.386(5) . ?
O2 C16 1.379(5) . ?
O3 C37 1.386(5) . ?
O4 C51 1.386(5) . ?
O5 C65 1.380(5) . ?
O6 C80 1.369(5) . ?
O7 C101 1.380(6) . ?
O8 C115 1.379(6) . ?
C1 C6 1.398(6) . ?
C1 C2 1.408(6) . ?
C2 C3 1.398(6) . ?
C2 C7 1.539(6) . ?
C3 C4 1.389(6) . ?
C4 C5 1.383(6) . ?
C4 C11 1.542(7) . ?
C5 C6 1.385(6) . ?
C6 C15 1.521(6) . ?
C7 C10 1.528(7) . ?
C7 C9 1.531(6) . ?
C7 C8 1.549(6) . ?
C11 C14 1.522(9) . ?
C11 C12 1.526(7) . ?
C11 C13 1.528(9) . ?
C15 C21 1.522(6) . ?
C15 C30 1.532(6) . ?
C16 C21 1.401(6) . ?
C16 C17 1.418(6) . ?
C17 C18 1.409(6) . ?
C17 C22 1.545(7) . ?
C18 C19 1.385(7) . ?
C19 C20 1.376(6) . ?
C19 C26 1.547(6) . ?
C20 C21 1.395(6) . ?
C22 C23 1.514(7) . ?
C22 C24 1.540(7) . ?
C22 C25 1.546(6) . ?
C26 C27 1.512(7) . ?
C26 C28 1.525(7) . ?
C26 C29 1.532(8) . ?
C30 C31 1.392(6) . ?
C30 C35 1.398(6) . ?
C31 C32 1.388(6) . ?
C32 C33 1.381(6) . ?
C32 C36 1.522(6) . ?
C33 C34 1.389(6) . ?
C34 C35 1.375(7) . ?
C36 C56 1.526(6) . ?
C36 C42 1.534(6) . ?
C37 C42 1.395(6) . ?
C37 C38 1.405(6) . ?
C38 C39 1.396(6) . ?
C38 C43 1.545(6) . ?
C39 C40 1.386(7) . ?
C40 C41 1.392(6) . ?
C40 C47 1.532(7) . ?
C41 C42 1.388(6) . ?
C43 C45 1.528(6) . ?
C43 C46 1.536(6) . ?
C43 C44 1.538(7) . ?
C47 C49X 1.512(19) . ?
C47 C48 1.531(9) . ?
C47 C49 1.542(11) . ?
C47 C50 1.543(8) . ?
C47 C50X 1.549(16) . ?
C47 C48X 1.599(16) . ?
C51 C56 1.395(6) . ?
C51 C52 1.414(6) . ?
C52 C53 1.385(7) . ?
C52 C57 1.553(6) . ?
C53 C54 1.400(6) . ?
C54 C55 1.384(6) . ?
C54 C61 1.538(7) . ?
C55 C56 1.387(6) . ?
C57 C58 1.528(7) . ?
C57 C59 1.532(7) . ?
C57 C60 1.537(8) . ?
C61 C64 1.532(7) . ?
C61 C62 1.534(7) . ?
C61 C63 1.540(7) . ?
C65 C70 1.403(6) . ?
C65 C66 1.411(6) . ?
C66 C67 1.393(6) . ?
C66 C79 1.528(6) . ?
C67 C68 1.386(6) . ?
C68 C69 1.390(7) . ?
C68 C75 1.554(6) . ?
C69 C70 1.403(6) . ?
C70 C71 1.538(7) . ?
C71 C72 1.532(7) . ?
C71 C73 1.536(7) . ?
C71 C74 1.547(7) . ?
C75 C76 1.512(8) . ?
C75 C77 1.524(7) . ?
C75 C78 1.536(8) . ?
C79 C94 1.520(6) . ?
C79 C85 1.529(6) . ?
C80 C85 1.388(6) . ?
C80 C81 1.424(6) . ?
C81 C82 1.383(6) . ?
C81 C86 1.547(6) . ?
C82 C83 1.396(7) . ?
C83 C84 1.377(6) . ?
C83 C90 1.548(7) . ?
C84 C85 1.404(6) . ?
C86 C89 1.522(6) . ?
C86 C87 1.525(7) . ?
C86 C88 1.534(7) . ?
C90 C91 1.511(8) . ?
C90 C92 1.539(9) . ?
C90 C93 1.564(10) . ?
C94 C95 1.396(6) . ?
C94 C99 1.413(6) . ?
C95 C96 1.394(6) . ?
C96 C97 1.386(6) . ?
C96 C100 1.522(6) . ?
C97 C98 1.387(6) . ?
C98 C99 1.380(6) . ?
C100 C120 1.524(6) . ?
C100 C106 1.532(6) . ?
C101 C106 1.393(7) . ?
C101 C102 1.399(7) . ?
C102 C103 1.385(8) . ?
C102 C17X 1.465(17) . ?
C102 C107 1.632(12) . ?
C103 C104 1.373(8) . ?
C104 C105 1.395(7) . ?
C104 C111 1.516(8) . ?
C105 C106 1.379(6) . ?
C107 C110 1.505(11) . ?
C107 C108 1.517(13) . ?
C107 C109 1.565(15) . ?
C17X C18X 1.520(14) . ?
C17X C20X 1.528(13) . ?
C17X C19X 1.574(17) . ?
C111 C113 1.441(12) . ?
C111 C12X 1.506(13) . ?
C111 C112 1.565(10) . ?
C111 C14X 1.594(12) . ?
C111 C114 1.596(10) . ?
C111 C13X 1.626(15) . ?
C115 C116 1.391(7) . ?
C115 C120 1.408(6) . ?
C116 C117 1.388(8) . ?
C116 C121 1.553(8) . ?
C117 C118 1.387(8) . ?
C118 C119 1.379(7) . ?
C118 C125 1.534(8) . ?
C119 C120 1.382(6) . ?
C121 C124 1.529(10) . ?
C121 C122 1.537(9) . ?
C121 C123 1.553(10) . ?
C125 C128 1.526(8) . ?
C125 C28X 1.534(18) . ?
C125 C26X 1.537(17) . ?
C125 C126 1.537(9) . ?
C125 C127 1.542(11) . ?
C125 C27X 1.58(2) . ?
N1 C129 1.120(8) . ?
C129 C130 1.518(9) . ?
N2 C131 1.134(7) . ?
C131 C132 1.447(8) . ?
N3 C133 1.163(9) . ?
C133 C134 1.408(9) . ?
N4 C135 1.144(10) . ?
C135 C136 1.402(10) . ?
N5 C137 1.11(3) . ?
C137 C138 1.40(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O5 92.60(12) . . ?
O1 Nb1 O2 92.95(12) . . ?
O5 Nb1 O2 174.37(13) . . ?
O1 Nb1 O6 101.56(12) . . ?
O5 Nb1 O6 91.65(12) . . ?
O2 Nb1 O6 88.19(12) . . ?
O1 Nb1 N1 174.97(14) . . ?
O5 Nb1 N1 86.94(13) . . ?
O2 Nb1 N1 87.44(13) . . ?
O6 Nb1 N1 83.46(14) . . ?
O1 Nb1 Cl1 95.15(9) . . ?
O5 Nb1 Cl1 89.60(9) . . ?
O2 Nb1 Cl1 88.93(10) . . ?
O6 Nb1 Cl1 163.16(9) . . ?
N1 Nb1 Cl1 79.84(12) . . ?
C1 O1 Nb1 157.4(3) . . ?
C16 O2 Nb1 154.1(3) . . ?
C65 O5 Nb1 160.7(3) . . ?
C80 O6 Nb1 151.6(3) . . ?
O1 C1 C6 118.3(4) . . ?
O1 C1 C2 120.2(4) . . ?
C6 C1 C2 121.5(4) . . ?
C3 C2 C1 116.4(4) . . ?
C3 C2 C7 120.6(4) . . ?
C1 C2 C7 123.0(4) . . ?
C4 C3 C2 123.7(4) . . ?
C5 C4 C3 117.2(4) . . ?
C5 C4 C11 119.2(4) . . ?
C3 C4 C11 123.5(4) . . ?
C4 C5 C6 122.3(4) . . ?
C5 C6 C1 118.7(4) . . ?
C5 C6 C15 120.9(4) . . ?
C1 C6 C15 120.3(4) . . ?
C10 C7 C9 108.9(4) . . ?
C10 C7 C2 109.4(4) . . ?
C9 C7 C2 112.1(4) . . ?
C10 C7 C8 110.2(4) . . ?
C9 C7 C8 106.6(4) . . ?
C2 C7 C8 109.6(4) . . ?
C14 C11 C12 108.7(5) . . ?
C14 C11 C13 110.7(6) . . ?
C12 C11 C13 107.2(5) . . ?
C14 C11 C4 108.8(5) . . ?
C12 C11 C4 112.6(4) . . ?
C13 C11 C4 108.9(5) . . ?
C6 C15 C21 110.0(4) . . ?
C6 C15 C30 111.0(4) . . ?
C21 C15 C30 115.4(3) . . ?
O2 C16 C21 118.3(4) . . ?
O2 C16 C17 120.9(4) . . ?
C21 C16 C17 120.7(4) . . ?
C18 C17 C16 116.2(4) . . ?
C18 C17 C22 119.7(4) . . ?
C16 C17 C22 124.1(4) . . ?
C19 C18 C17 124.1(4) . . ?
C20 C19 C18 117.3(4) . . ?
C20 C19 C26 119.7(5) . . ?
C18 C19 C26 123.0(4) . . ?
C19 C20 C21 122.4(5) . . ?
C20 C21 C16 119.0(4) . . ?
C20 C21 C15 120.0(4) . . ?
C16 C21 C15 120.9(4) . . ?
C23 C22 C24 111.2(5) . . ?
C23 C22 C17 108.8(4) . . ?
C24 C22 C17 111.3(4) . . ?
C23 C22 C25 107.6(4) . . ?
C24 C22 C25 105.4(4) . . ?
C17 C22 C25 112.4(4) . . ?
C27 C26 C28 109.9(5) . . ?
C27 C26 C29 108.8(5) . . ?
C28 C26 C29 108.0(4) . . ?
C27 C26 C19 109.4(4) . . ?
C28 C26 C19 109.0(4) . . ?
C29 C26 C19 111.7(5) . . ?
C31 C30 C35 116.8(4) . . ?
C31 C30 C15 124.2(4) . . ?
C35 C30 C15 118.8(4) . . ?
C32 C31 C30 122.5(4) . . ?
C33 C32 C31 119.2(4) . . ?
C33 C32 C36 122.4(4) . . ?
C31 C32 C36 118.3(4) . . ?
C32 C33 C34 119.5(5) . . ?
C35 C34 C33 120.6(5) . . ?
C34 C35 C30 121.4(4) . . ?
C32 C36 C56 113.6(4) . . ?
C32 C36 C42 110.8(3) . . ?
C56 C36 C42 111.4(4) . . ?
O3 C37 C42 120.6(4) . . ?
O3 C37 C38 118.2(4) . . ?
C42 C37 C38 121.1(4) . . ?
C39 C38 C37 117.3(4) . . ?
C39 C38 C43 121.3(4) . . ?
C37 C38 C43 121.3(4) . . ?
C40 C39 C38 123.3(4) . . ?
C39 C40 C41 117.2(4) . . ?
C39 C40 C47 123.4(4) . . ?
C41 C40 C47 119.3(4) . . ?
C42 C41 C40 122.1(4) . . ?
C41 C42 C37 118.9(4) . . ?
C41 C42 C36 120.9(4) . . ?
C37 C42 C36 119.8(4) . . ?
C45 C43 C46 106.9(4) . . ?
C45 C43 C44 108.0(4) . . ?
C46 C43 C44 110.8(4) . . ?
C45 C43 C38 111.7(4) . . ?
C46 C43 C38 109.3(4) . . ?
C44 C43 C38 110.2(4) . . ?
C49X C47 C40 119.5(19) . . ?
C48 C47 C40 111.2(7) . . ?
C48 C47 C49 107.5(7) . . ?
C40 C47 C49 108.9(5) . . ?
C48 C47 C50 108.8(7) . . ?
C40 C47 C50 111.1(7) . . ?
C49 C47 C50 109.2(7) . . ?
C49X C47 C50X 110(2) . . ?
C40 C47 C50X 120(3) . . ?
C49X C47 C48X 102.9(17) . . ?
C40 C47 C48X 95.3(13) . . ?
C50X C47 C48X 104(2) . . ?
O4 C51 C56 120.5(4) . . ?
O4 C51 C52 118.1(4) . . ?
C56 C51 C52 121.4(4) . . ?
C53 C52 C51 116.9(4) . . ?
C53 C52 C57 122.3(4) . . ?
C51 C52 C57 120.8(4) . . ?
C52 C53 C54 123.6(4) . . ?
C55 C54 C53 116.9(4) . . ?
C55 C54 C61 122.5(4) . . ?
C53 C54 C61 120.7(4) . . ?
C54 C55 C56 122.8(4) . . ?
C55 C56 C51 118.4(4) . . ?
C55 C56 C36 122.0(4) . . ?
C51 C56 C36 119.6(4) . . ?
C58 C57 C59 107.7(5) . . ?
C58 C57 C60 107.7(5) . . ?
C59 C57 C60 110.4(5) . . ?
C58 C57 C52 110.9(4) . . ?
C59 C57 C52 109.8(4) . . ?
C60 C57 C52 110.3(4) . . ?
C64 C61 C62 109.9(4) . . ?
C64 C61 C54 110.2(4) . . ?
C62 C61 C54 109.4(4) . . ?
C64 C61 C63 107.1(4) . . ?
C62 C61 C63 108.4(4) . . ?
C54 C61 C63 111.9(4) . . ?
O5 C65 C70 121.8(4) . . ?
O5 C65 C66 117.4(4) . . ?
C70 C65 C66 120.8(4) . . ?
C67 C66 C65 119.0(4) . . ?
C67 C66 C79 120.2(4) . . ?
C65 C66 C79 120.8(4) . . ?
C68 C67 C66 121.9(5) . . ?
C67 C68 C69 117.6(4) . . ?
C67 C68 C75 119.8(4) . . ?
C69 C68 C75 122.7(4) . . ?
C68 C69 C70 123.5(4) . . ?
C69 C70 C65 117.0(4) . . ?
C69 C70 C71 120.1(4) . . ?
C65 C70 C71 122.9(4) . . ?
C72 C71 C73 107.0(4) . . ?
C72 C71 C70 112.6(4) . . ?
C73 C71 C70 110.6(4) . . ?
C72 C71 C74 106.8(4) . . ?
C73 C71 C74 110.7(4) . . ?
C70 C71 C74 109.1(4) . . ?
C76 C75 C77 110.5(5) . . ?
C76 C75 C78 109.5(5) . . ?
C77 C75 C78 106.7(5) . . ?
C76 C75 C68 109.0(4) . . ?
C77 C75 C68 112.4(4) . . ?
C78 C75 C68 108.7(4) . . ?
C94 C79 C66 115.0(3) . . ?
C94 C79 C85 113.5(4) . . ?
C66 C79 C85 109.0(3) . . ?
O6 C80 C85 119.4(4) . . ?
O6 C80 C81 120.4(4) . . ?
C85 C80 C81 120.0(4) . . ?
C82 C81 C80 116.8(4) . . ?
C82 C81 C86 119.8(4) . . ?
C80 C81 C86 123.3(4) . . ?
C81 C82 C83 124.0(4) . . ?
C84 C83 C82 117.4(4) . . ?
C84 C83 C90 122.7(4) . . ?
C82 C83 C90 119.8(4) . . ?
C83 C84 C85 121.3(4) . . ?
C80 C85 C84 119.7(4) . . ?
C80 C85 C79 121.6(4) . . ?
C84 C85 C79 118.6(4) . . ?
C89 C86 C87 107.6(4) . . ?
C89 C86 C88 108.3(4) . . ?
C87 C86 C88 109.0(4) . . ?
C89 C86 C81 111.8(4) . . ?
C87 C86 C81 109.1(4) . . ?
C88 C86 C81 111.0(4) . . ?
C91 C90 C92 108.2(6) . . ?
C91 C90 C83 112.8(4) . . ?
C92 C90 C83 109.0(5) . . ?
C91 C90 C93 109.4(6) . . ?
C92 C90 C93 108.9(6) . . ?
C83 C90 C93 108.5(5) . . ?
C95 C94 C99 117.2(4) . . ?
C95 C94 C79 121.9(4) . . ?
C99 C94 C79 120.8(4) . . ?
C96 C95 C94 121.9(4) . . ?
C97 C96 C95 119.2(4) . . ?
C97 C96 C100 122.5(4) . . ?
C95 C96 C100 118.0(4) . . ?
C96 C97 C98 120.2(5) . . ?
C99 C98 C97 120.3(5) . . ?
C98 C99 C94 121.1(4) . . ?
C96 C100 C120 114.5(4) . . ?
C96 C100 C106 111.0(4) . . ?
C120 C100 C106 112.4(4) . . ?
O7 C101 C106 120.4(4) . . ?
O7 C101 C102 117.6(4) . . ?
C106 C101 C102 121.9(5) . . ?
C103 C102 C101 116.3(5) . . ?
C103 C102 C17X 115.7(7) . . ?
C101 C102 C17X 125.8(7) . . ?
C103 C102 C107 124.1(6) . . ?
C101 C102 C107 118.7(6) . . ?
C104 C103 C102 124.1(5) . . ?
C103 C104 C105 117.2(5) . . ?
C103 C104 C111 122.6(5) . . ?
C105 C104 C111 120.2(5) . . ?
C106 C105 C104 121.9(5) . . ?
C105 C106 C101 118.4(4) . . ?
C105 C106 C100 122.1(4) . . ?
C101 C106 C100 119.4(4) . . ?
C110 C107 C108 109.6(11) . . ?
C110 C107 C109 105.9(10) . . ?
C108 C107 C109 109.0(10) . . ?
C110 C107 C102 110.8(7) . . ?
C108 C107 C102 105.3(11) . . ?
C109 C107 C102 116.2(9) . . ?
C102 C17X C18X 117.9(12) . . ?
C102 C17X C20X 118.8(12) . . ?
C18X C17X C20X 106.7(13) . . ?
C102 C17X C19X 97.1(12) . . ?
C18X C17X C19X 108.5(13) . . ?
C20X C17X C19X 106.4(12) . . ?
C113 C111 C104 111.9(8) . . ?
C12X C111 C104 121.8(11) . . ?
C113 C111 C112 113.1(9) . . ?
C104 C111 C112 108.1(7) . . ?
C12X C111 C14X 116.2(11) . . ?
C104 C111 C14X 114.5(7) . . ?
C113 C111 C114 112.6(7) . . ?
C104 C111 C114 108.2(6) . . ?
C112 C111 C114 102.4(7) . . ?
C12X C111 C13X 102.5(14) . . ?
C104 C111 C13X 102.4(9) . . ?
C14X C111 C13X 91.9(10) . . ?
O8 C115 C116 119.7(5) . . ?
O8 C115 C120 119.4(4) . . ?
C116 C115 C120 120.9(5) . . ?
C117 C116 C115 117.5(5) . . ?
C117 C116 C121 121.8(5) . . ?
C115 C116 C121 120.7(6) . . ?
C118 C117 C116 123.6(5) . . ?
C119 C118 C117 116.8(5) . . ?
C119 C118 C125 120.3(6) . . ?
C117 C118 C125 122.9(6) . . ?
C118 C119 C120 122.8(5) . . ?
C119 C120 C115 118.3(4) . . ?
C119 C120 C100 122.0(4) . . ?
C115 C120 C100 119.7(4) . . ?
C124 C121 C122 111.6(7) . . ?
C124 C121 C123 107.8(6) . . ?
C122 C121 C123 107.1(6) . . ?
C124 C121 C116 108.9(5) . . ?
C122 C121 C116 110.2(5) . . ?
C123 C121 C116 111.0(7) . . ?
C128 C125 C118 107.6(6) . . ?
C28X C125 C118 120(4) . . ?
C28X C125 C26X 111(3) . . ?
C118 C125 C26X 118(3) . . ?
C128 C125 C126 110.8(6) . . ?
C118 C125 C126 110.7(7) . . ?
C128 C125 C127 109.0(7) . . ?
C118 C125 C127 109.9(6) . . ?
C126 C125 C127 108.9(6) . . ?
C28X C125 C27X 106(2) . . ?
C118 C125 C27X 95(4) . . ?
C26X C125 C27X 105(2) . . ?
C129 N1 Nb1 171.3(5) . . ?
N1 C129 C130 175.8(7) . . ?
N2 C131 C132 179.3(7) . . ?
N3 C133 C134 177.0(9) . . ?
N4 C135 C136 173.5(11) . . ?
N5 C137 C138 174(3) . . ?

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
O5 Nb1 O1 C1 -165.8(7) . . . . ?
O2 Nb1 O1 C1 15.2(7) . . . . ?
O6 Nb1 O1 C1 -73.6(7) . . . . ?
Cl1 Nb1 O1 C1 104.4(7) . . . . ?
Nb1 O1 C1 C6 24.6(9) . . . . ?
Nb1 O1 C1 C2 -157.1(5) . . . . ?
O1 C1 C2 C3 178.2(4) . . . . ?
C6 C1 C2 C3 -3.5(6) . . . . ?
O1 C1 C2 C7 -1.9(6) . . . . ?
C6 C1 C2 C7 176.3(4) . . . . ?
C1 C2 C3 C4 0.5(7) . . . . ?
C7 C2 C3 C4 -179.4(5) . . . . ?
C2 C3 C4 C5 1.8(8) . . . . ?
C2 C3 C4 C11 179.9(5) . . . . ?
C3 C4 C5 C6 -1.1(7) . . . . ?
C11 C4 C5 C6 -179.3(5) . . . . ?
C4 C5 C6 C1 -1.8(7) . . . . ?
C4 C5 C6 C15 -179.2(4) . . . . ?
O1 C1 C6 C5 -177.4(4) . . . . ?
C2 C1 C6 C5 4.2(7) . . . . ?
O1 C1 C6 C15 -0.1(6) . . . . ?
C2 C1 C6 C15 -178.4(4) . . . . ?
C3 C2 C7 C10 -113.9(5) . . . . ?
C1 C2 C7 C10 66.2(5) . . . . ?
C3 C2 C7 C9 7.0(6) . . . . ?
C1 C2 C7 C9 -172.9(4) . . . . ?
C3 C2 C7 C8 125.2(5) . . . . ?
C1 C2 C7 C8 -54.7(6) . . . . ?
C5 C4 C11 C14 -61.7(7) . . . . ?
C3 C4 C11 C14 120.2(6) . . . . ?
C5 C4 C11 C12 177.7(5) . . . . ?
C3 C4 C11 C12 -0.4(8) . . . . ?
C5 C4 C11 C13 58.9(7) . . . . ?
C3 C4 C11 C13 -119.1(6) . . . . ?
C5 C6 C15 C21 83.6(5) . . . . ?
C1 C6 C15 C21 -93.7(5) . . . . ?
C5 C6 C15 C30 -45.4(6) . . . . ?
C1 C6 C15 C30 137.3(4) . . . . ?
Nb1 O2 C16 C21 -28.2(8) . . . . ?
Nb1 O2 C16 C17 150.4(5) . . . . ?
O2 C16 C17 C18 -173.2(4) . . . . ?
C21 C16 C17 C18 5.3(6) . . . . ?
O2 C16 C17 C22 4.8(6) . . . . ?
C21 C16 C17 C22 -176.7(4) . . . . ?
C16 C17 C18 C19 -0.5(7) . . . . ?
C22 C17 C18 C19 -178.6(4) . . . . ?
C17 C18 C19 C20 -2.4(7) . . . . ?
C17 C18 C19 C26 177.9(4) . . . . ?
C18 C19 C20 C21 0.7(6) . . . . ?
C26 C19 C20 C21 -179.6(4) . . . . ?
C19 C20 C21 C16 4.0(6) . . . . ?
C19 C20 C21 C15 -178.8(4) . . . . ?
O2 C16 C21 C20 171.5(4) . . . . ?
C17 C16 C21 C20 -7.0(6) . . . . ?
O2 C16 C21 C15 -5.6(6) . . . . ?
C17 C16 C21 C15 175.8(4) . . . . ?
C6 C15 C21 C20 -76.6(5) . . . . ?
C30 C15 C21 C20 49.9(5) . . . . ?
C6 C15 C21 C16 100.5(5) . . . . ?
C30 C15 C21 C16 -132.9(4) . . . . ?
C18 C17 C22 C23 103.8(5) . . . . ?
C16 C17 C22 C23 -74.1(6) . . . . ?
C18 C17 C22 C24 -133.3(4) . . . . ?
C16 C17 C22 C24 48.7(6) . . . . ?
C18 C17 C22 C25 -15.3(6) . . . . ?
C16 C17 C22 C25 166.7(4) . . . . ?
C20 C19 C26 C27 59.3(6) . . . . ?
C18 C19 C26 C27 -121.0(6) . . . . ?
C20 C19 C26 C28 -60.9(6) . . . . ?
C18 C19 C26 C28 118.8(5) . . . . ?
C20 C19 C26 C29 179.8(4) . . . . ?
C18 C19 C26 C29 -0.5(7) . . . . ?
C6 C15 C30 C31 138.6(4) . . . . ?
C21 C15 C30 C31 12.5(6) . . . . ?
C6 C15 C30 C35 -46.6(5) . . . . ?
C21 C15 C30 C35 -172.7(4) . . . . ?
C35 C30 C31 C32 1.2(6) . . . . ?
C15 C30 C31 C32 176.1(4) . . . . ?
C30 C31 C32 C33 -0.5(7) . . . . ?
C30 C31 C32 C36 175.7(4) . . . . ?
C31 C32 C33 C34 -1.0(7) . . . . ?
C36 C32 C33 C34 -177.1(4) . . . . ?
C32 C33 C34 C35 1.9(7) . . . . ?
C33 C34 C35 C30 -1.1(8) . . . . ?
C31 C30 C35 C34 -0.4(7) . . . . ?
C15 C30 C35 C34 -175.5(4) . . . . ?
C33 C32 C36 C56 -31.9(6) . . . . ?
C31 C32 C36 C56 152.0(4) . . . . ?
C33 C32 C36 C42 94.5(5) . . . . ?
C31 C32 C36 C42 -81.6(5) . . . . ?
O3 C37 C38 C39 177.6(4) . . . . ?
C42 C37 C38 C39 0.5(7) . . . . ?
O3 C37 C38 C43 0.7(7) . . . . ?
C42 C37 C38 C43 -176.3(4) . . . . ?
C37 C38 C39 C40 0.7(7) . . . . ?
C43 C38 C39 C40 177.6(5) . . . . ?
C38 C39 C40 C41 -1.2(8) . . . . ?
C38 C39 C40 C47 -179.4(5) . . . . ?
C39 C40 C41 C42 0.5(8) . . . . ?
C47 C40 C41 C42 178.7(5) . . . . ?
C40 C41 C42 C37 0.7(7) . . . . ?
C40 C41 C42 C36 -172.1(5) . . . . ?
O3 C37 C42 C41 -178.2(4) . . . . ?
C38 C37 C42 C41 -1.2(7) . . . . ?
O3 C37 C42 C36 -5.4(7) . . . . ?
C38 C37 C42 C36 171.6(4) . . . . ?
C32 C36 C42 C41 -31.4(6) . . . . ?
C56 C36 C42 C41 96.2(5) . . . . ?
C32 C36 C42 C37 155.9(4) . . . . ?
C56 C36 C42 C37 -76.5(5) . . . . ?
C39 C38 C43 C45 1.3(7) . . . . ?
C37 C38 C43 C45 178.0(5) . . . . ?
C39 C38 C43 C46 -116.7(5) . . . . ?
C37 C38 C43 C46 60.0(6) . . . . ?
C39 C38 C43 C44 121.3(5) . . . . ?
C37 C38 C43 C44 -61.9(6) . . . . ?
C39 C40 C47 C49X 150(3) . . . . ?
C41 C40 C47 C49X -28(3) . . . . ?
C39 C40 C47 C48 -125.8(9) . . . . ?
C41 C40 C47 C48 56.1(10) . . . . ?
C39 C40 C47 C49 115.9(8) . . . . ?
C41 C40 C47 C49 -62.2(8) . . . . ?
C39 C40 C47 C50 -4.4(10) . . . . ?
C41 C40 C47 C50 177.5(7) . . . . ?
C39 C40 C47 C50X 8(3) . . . . ?
C41 C40 C47 C50X -170(3) . . . . ?
C39 C40 C47 C48X -102.1(19) . . . . ?
C41 C40 C47 C48X 79.8(19) . . . . ?
O4 C51 C52 C53 179.5(4) . . . . ?
C56 C51 C52 C53 -1.9(7) . . . . ?
O4 C51 C52 C57 -1.4(7) . . . . ?
C56 C51 C52 C57 177.2(4) . . . . ?
C51 C52 C53 C54 0.4(7) . . . . ?
C57 C52 C53 C54 -178.7(4) . . . . ?
C52 C53 C54 C55 0.3(7) . . . . ?
C52 C53 C54 C61 179.0(4) . . . . ?
C53 C54 C55 C56 0.4(7) . . . . ?
C61 C54 C55 C56 -178.2(4) . . . . ?
C54 C55 C56 C51 -1.9(7) . . . . ?
C54 C55 C56 C36 177.9(4) . . . . ?
O4 C51 C56 C55 -178.8(4) . . . . ?
C52 C51 C56 C55 2.6(7) . . . . ?
O4 C51 C56 C36 1.4(7) . . . . ?
C52 C51 C56 C36 -177.2(4) . . . . ?
C32 C36 C56 C55 110.2(5) . . . . ?
C42 C36 C56 C55 -15.9(6) . . . . ?
C32 C36 C56 C51 -70.1(5) . . . . ?
C42 C36 C56 C51 163.9(4) . . . . ?
C53 C52 C57 C58 0.0(7) . . . . ?
C51 C52 C57 C58 -179.0(5) . . . . ?
C53 C52 C57 C59 118.9(5) . . . . ?
C51 C52 C57 C59 -60.1(6) . . . . ?
C53 C52 C57 C60 -119.2(5) . . . . ?
C51 C52 C57 C60 61.8(6) . . . . ?
C55 C54 C61 C64 -125.0(5) . . . . ?
C53 C54 C61 C64 56.4(6) . . . . ?
C55 C54 C61 C62 114.1(5) . . . . ?
C53 C54 C61 C62 -64.5(6) . . . . ?
C55 C54 C61 C63 -5.9(6) . . . . ?
C53 C54 C61 C63 175.5(4) . . . . ?
Nb1 O5 C65 C70 164.4(6) . . . . ?
Nb1 O5 C65 C66 -16.5(10) . . . . ?
O5 C65 C66 C67 175.0(4) . . . . ?
C70 C65 C66 C67 -5.9(6) . . . . ?
O5 C65 C66 C79 -4.0(6) . . . . ?
C70 C65 C66 C79 175.1(4) . . . . ?
C65 C66 C67 C68 2.9(6) . . . . ?
C79 C66 C67 C68 -178.1(4) . . . . ?
C66 C67 C68 C69 0.4(7) . . . . ?
C66 C67 C68 C75 179.5(4) . . . . ?
C67 C68 C69 C70 -0.9(7) . . . . ?
C75 C68 C69 C70 -180.0(5) . . . . ?
C68 C69 C70 C65 -2.0(7) . . . . ?
C68 C69 C70 C71 177.4(4) . . . . ?
O5 C65 C70 C69 -175.6(4) . . . . ?
C66 C65 C70 C69 5.3(6) . . . . ?
O5 C65 C70 C71 5.0(7) . . . . ?
C66 C65 C70 C71 -174.0(4) . . . . ?
C69 C70 C71 C72 -1.4(7) . . . . ?
C65 C70 C71 C72 177.9(4) . . . . ?
C69 C70 C71 C73 118.3(5) . . . . ?
C65 C70 C71 C73 -62.4(6) . . . . ?
C69 C70 C71 C74 -119.8(5) . . . . ?
C65 C70 C71 C74 59.6(6) . . . . ?
C67 C68 C75 C76 62.6(6) . . . . ?
C69 C68 C75 C76 -118.4(6) . . . . ?
C67 C68 C75 C77 -174.6(5) . . . . ?
C69 C68 C75 C77 4.4(8) . . . . ?
C67 C68 C75 C78 -56.7(6) . . . . ?
C69 C68 C75 C78 122.3(5) . . . . ?
C67 C66 C79 C94 42.4(5) . . . . ?
C65 C66 C79 C94 -138.6(4) . . . . ?
C67 C66 C79 C85 -86.4(5) . . . . ?
C65 C66 C79 C85 92.6(5) . . . . ?
Nb1 O6 C80 C85 42.6(8) . . . . ?
Nb1 O6 C80 C81 -142.2(4) . . . . ?
O6 C80 C81 C82 174.7(4) . . . . ?
C85 C80 C81 C82 -10.0(7) . . . . ?
O6 C80 C81 C86 -9.2(7) . . . . ?
C85 C80 C81 C86 166.1(4) . . . . ?
C80 C81 C82 C83 4.9(8) . . . . ?
C86 C81 C82 C83 -171.3(5) . . . . ?
C81 C82 C83 C84 1.5(8) . . . . ?
C81 C82 C83 C90 178.4(5) . . . . ?
C82 C83 C84 C85 -3.0(8) . . . . ?
C90 C83 C84 C85 -179.9(5) . . . . ?
O6 C80 C85 C84 -175.9(4) . . . . ?
C81 C80 C85 C84 8.8(7) . . . . ?
O6 C80 C85 C79 2.7(6) . . . . ?
C81 C80 C85 C79 -172.6(4) . . . . ?
C83 C84 C85 C80 -2.1(7) . . . . ?
C83 C84 C85 C79 179.2(5) . . . . ?
C94 C79 C85 C80 130.3(4) . . . . ?
C66 C79 C85 C80 -100.1(5) . . . . ?
C94 C79 C85 C84 -51.0(5) . . . . ?
C66 C79 C85 C84 78.6(5) . . . . ?
C82 C81 C86 C89 5.4(6) . . . . ?
C80 C81 C86 C89 -170.6(4) . . . . ?
C82 C81 C86 C87 124.2(5) . . . . ?
C80 C81 C86 C87 -51.8(6) . . . . ?
C82 C81 C86 C88 -115.6(5) . . . . ?
C80 C81 C86 C88 68.4(6) . . . . ?
C84 C83 C90 C91 -5.2(9) . . . . ?
C82 C83 C90 C91 178.0(7) . . . . ?
C84 C83 C90 C92 -125.3(6) . . . . ?
C82 C83 C90 C92 57.9(8) . . . . ?
C84 C83 C90 C93 116.2(6) . . . . ?
C82 C83 C90 C93 -60.5(7) . . . . ?
C66 C79 C94 C95 23.3(6) . . . . ?
C85 C79 C94 C95 149.7(4) . . . . ?
C66 C79 C94 C99 -160.3(4) . . . . ?
C85 C79 C94 C99 -33.9(5) . . . . ?
C99 C94 C95 C96 1.1(6) . . . . ?
C79 C94 C95 C96 177.7(4) . . . . ?
C94 C95 C96 C97 -2.6(6) . . . . ?
C94 C95 C96 C100 171.3(4) . . . . ?
C95 C96 C97 C98 2.5(7) . . . . ?
C100 C96 C97 C98 -171.1(4) . . . . ?
C96 C97 C98 C99 -1.0(7) . . . . ?
C97 C98 C99 C94 -0.4(7) . . . . ?
C95 C94 C99 C98 0.3(6) . . . . ?
C79 C94 C99 C98 -176.2(4) . . . . ?
C97 C96 C100 C120 -43.9(6) . . . . ?
C95 C96 C100 C120 142.5(4) . . . . ?
C97 C96 C100 C106 84.8(5) . . . . ?
C95 C96 C100 C106 -88.9(5) . . . . ?
O7 C101 C102 C103 177.9(6) . . . . ?
C106 C101 C102 C103 -2.4(11) . . . . ?
O7 C101 C102 C17X -19.4(14) . . . . ?
C106 C101 C102 C17X 160.2(11) . . . . ?
O7 C101 C102 C107 8.1(11) . . . . ?
C106 C101 C102 C107 -172.2(8) . . . . ?
C101 C102 C103 C104 -1.5(12) . . . . ?
C17X C102 C103 C104 -165.9(10) . . . . ?
C107 C102 C103 C104 167.7(9) . . . . ?
C102 C103 C104 C105 3.9(12) . . . . ?
C102 C103 C104 C111 -178.4(7) . . . . ?
C103 C104 C105 C106 -2.5(10) . . . . ?
C111 C104 C105 C106 179.7(6) . . . . ?
C104 C105 C106 C101 -1.1(9) . . . . ?
C104 C105 C106 C100 -178.8(5) . . . . ?
O7 C101 C106 C105 -176.7(5) . . . . ?
C102 C101 C106 C105 3.7(9) . . . . ?
O7 C101 C106 C100 1.1(8) . . . . ?
C102 C101 C106 C100 -178.5(6) . . . . ?
C96 C100 C106 C105 -19.7(7) . . . . ?
C120 C100 C106 C105 110.0(5) . . . . ?
C96 C100 C106 C101 162.6(5) . . . . ?
C120 C100 C106 C101 -67.6(6) . . . . ?
C103 C102 C107 C110 0.6(15) . . . . ?
C101 C102 C107 C110 169.5(9) . . . . ?
C17X C102 C107 C110 -76.4(19) . . . . ?
C103 C102 C107 C108 119.0(11) . . . . ?
C101 C102 C107 C108 -72.0(13) . . . . ?
C17X C102 C107 C108 42.1(19) . . . . ?
C103 C102 C107 C109 -120.3(10) . . . . ?
C101 C102 C107 C109 48.6(12) . . . . ?
C17X C102 C107 C109 163(2) . . . . ?
C103 C102 C17X C18X 132.4(13) . . . . ?
C101 C102 C17X C18X -30(2) . . . . ?
C107 C102 C17X C18X -111(2) . . . . ?
C103 C102 C17X C20X 0.9(18) . . . . ?
C101 C102 C17X C20X -161.8(11) . . . . ?
C107 C102 C17X C20X 117(3) . . . . ?
C103 C102 C17X C19X -112.3(11) . . . . ?
C101 C102 C17X C19X 85.0(13) . . . . ?
C107 C102 C17X C19X 4.1(15) . . . . ?
C103 C104 C111 C113 -110.0(10) . . . . ?
C105 C104 C111 C113 67.6(10) . . . . ?
C103 C104 C111 C12X 25.3(17) . . . . ?
C105 C104 C111 C12X -157.0(15) . . . . ?
C103 C104 C111 C112 15.2(11) . . . . ?
C105 C104 C111 C112 -167.2(8) . . . . ?
C103 C104 C111 C14X 174.0(13) . . . . ?
C105 C104 C111 C14X -8.3(15) . . . . ?
C103 C104 C111 C114 125.4(8) . . . . ?
C105 C104 C111 C114 -57.0(9) . . . . ?
C103 C104 C111 C13X -88.0(10) . . . . ?
C105 C104 C111 C13X 89.6(9) . . . . ?
O8 C115 C116 C117 -177.9(5) . . . . ?
C120 C115 C116 C117 0.0(8) . . . . ?
O8 C115 C116 C121 1.0(8) . . . . ?
C120 C115 C116 C121 178.8(5) . . . . ?
C115 C116 C117 C118 -1.6(8) . . . . ?
C121 C116 C117 C118 179.6(5) . . . . ?
C116 C117 C118 C119 0.7(8) . . . . ?
C116 C117 C118 C125 -179.5(5) . . . . ?
C117 C118 C119 C120 1.9(8) . . . . ?
C125 C118 C119 C120 -177.9(5) . . . . ?
C118 C119 C120 C115 -3.4(7) . . . . ?
C118 C119 C120 C100 172.7(4) . . . . ?
O8 C115 C120 C119 -179.7(4) . . . . ?
C116 C115 C120 C119 2.4(7) . . . . ?
O8 C115 C120 C100 4.1(7) . . . . ?
C116 C115 C120 C100 -173.7(4) . . . . ?
C96 C100 C120 C119 117.1(5) . . . . ?
C106 C100 C120 C119 -10.8(6) . . . . ?
C96 C100 C120 C115 -66.9(6) . . . . ?
C106 C100 C120 C115 165.2(4) . . . . ?
C117 C116 C121 C124 115.2(7) . . . . ?
C115 C116 C121 C124 -63.6(7) . . . . ?
C117 C116 C121 C122 -122.0(7) . . . . ?
C115 C116 C121 C122 59.2(8) . . . . ?
C117 C116 C121 C123 -3.4(8) . . . . ?
C115 C116 C121 C123 177.8(6) . . . . ?
C119 C118 C125 C128 -67.0(9) . . . . ?
C117 C118 C125 C128 113.3(8) . . . . ?
C119 C118 C125 C28X -79(4) . . . . ?
C117 C118 C125 C28X 101(4) . . . . ?
C119 C118 C125 C26X 141(5) . . . . ?
C117 C118 C125 C26X -38(5) . . . . ?
C119 C118 C125 C126 171.8(7) . . . . ?
C117 C118 C125 C126 -7.9(9) . . . . ?
C119 C118 C125 C127 51.5(8) . . . . ?
C117 C118 C125 C127 -128.2(8) . . . . ?
C119 C118 C125 C27X 32(4) . . . . ?
C117 C118 C125 C27X -148(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 N2 0.84 2.09 2.900(7) 163.0 .

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3


# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 129 10 ' '
2 0.500 0.000 0.500 13 1 ' '
3 0.388 0.079 0.238 9 0 ' '
4 0.240 0.095 0.150 9 1 ' '
5 0.356 0.141 0.586 27 1 ' '
6 0.455 0.167 0.742 7 0 ' '
7 0.888 0.243 0.228 14 1 ' '
8 0.888 0.257 0.728 14 1 ' '
9 0.356 0.359 0.086 27 1 ' '
10 0.455 0.333 0.242 7 0 ' '
11 0.000 0.500 0.500 129 10 ' '
12 0.240 0.405 0.650 9 1 ' '
13 0.388 0.420 0.738 9 0 ' '
14 0.500 0.500 1.000 13 1 ' '
15 0.612 0.579 0.262 9 0 ' '
16 0.760 0.595 0.350 9 1 ' '
17 0.644 0.641 0.914 27 1 ' '
18 0.545 0.667 0.758 7 0 ' '
19 0.112 0.743 0.271 14 1 ' '
20 0.112 0.757 0.771 14 1 ' '
21 0.644 0.859 0.414 27 1 ' '
22 0.545 0.833 0.258 7 0 ' '
23 0.760 0.905 0.850 9 1 ' '
24 0.612 0.920 0.762 9 0 ' '
_platon_squeeze_details          
; (replace by semicolon in column 1 when used as .sqf) 
TITL CR515 in P2(1)/c 
CELL   30.3580   17.6674   24.5131     90.00     93.64     90.00 
SPGR P21/c 
# Solvent Accessible Volume =     549.7 
# Electrons Found in S.A.V. =      34.9 
# Note: Atoms in Void as Cxxx and Qxxx all others 
Q101 0.765 0.819 0.664 !       1.39 eA-3 
C102 1.002 0.468 0.537 !       1.30 eA-3 
Q103 0.723 0.686 0.163 !       1.21 eA-3 
Q104 0.804 0.894 0.177 !       1.08 eA-3 
C105 1.000 1.000 0.000 !       1.06 eA-3 
Q106 0.277 0.187 0.381 !       0.90 eA-3 
Q107 0.304 0.655 0.591 !       0.69 eA-3 
Q108 0.232 0.175 0.384 !       0.67 eA-3 
Q109 0.400 0.580 0.415 !       0.63 eA-3 
Q110 0.461 0.405 0.437 !       0.60 eA-3 
Q111 0.985 0.922 0.174 !       0.60 eA-3 
Q112 0.202 0.754 0.390 !       0.60 eA-3 
Q113 0.788 0.654 0.555 !       0.59 eA-3 
C114 0.399 0.794 0.006 !       0.58 eA-3 
Q115 0.491 0.455 0.530 !       0.57 eA-3 
Q116 0.172 0.433 0.283 !       0.57 eA-3 
Q117 0.209 0.045 0.861 !       0.57 eA-3 
Q118 0.678 0.471-0.003 !       0.55 eA-3 
Q119 0.806 0.099 0.365 !       0.55 eA-3 
Q120 0.819 0.521 0.409 !       0.55 eA-3 
Q121 0.233 0.267 0.779 !       0.54 eA-3 
C122 0.642 0.846 0.368 !       0.54 eA-3 
Q123 0.025 0.418 0.736 !       0.54 eA-3 
Q124 0.771 0.719 0.106 !       0.53 eA-3 
Q125 0.220 0.271 0.817 !       0.53 eA-3 
Q126 0.861 0.074 0.350 !       0.52 eA-3 
Q127 0.743 0.830 0.125 !       0.52 eA-3 
Q128 0.905 0.250 0.694 !       0.51 eA-3 
Q129 0.196 0.833 0.070 !       0.51 eA-3 
Q130 0.196 0.277 0.750 !       0.50 eA-3 
Q131 0.186 0.313 0.409 !       0.50 eA-3 
Q132 0.750 0.671 0.196 !       0.50 eA-3 
;



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr511
_database_code_depnum_ccdc_archive 'CCDC 1043854'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H90 O4'
_chemical_formula_sum            'C64 H90 O4'
_chemical_formula_weight         923.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 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 0.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.778(11)
_cell_length_b                   15.190(15)
_cell_length_c                   18.55(2)
_cell_angle_alpha                68.19(3)
_cell_angle_beta                 83.42(5)
_cell_angle_gamma                69.19(4)
_cell_volume                     2880(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3614
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      24.2

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_F_000             1012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.061
_shelx_estimated_absorpt_T_min   0.994
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_exptl_absorpt_special_details   ?
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           synchrotron
_diffrn_source                   'DLS beamline I19'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            32266
_diffrn_reflns_av_unetI/netI     0.1483
_diffrn_reflns_av_R_equivalents  0.1786
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.178
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        22.499
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8221
_reflns_number_gt                4391
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1242P)²+2.8347P] 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         8221
_refine_ls_number_parameters     651
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1157
_refine_ls_wR_factor_ref         0.3131
_refine_ls_wR_factor_gt          0.2572
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5818(4) 0.6499(3) 0.0795(3) 0.0562(12) Uani 1 1 d . . . . .
H1 H 0.5877 0.6041 0.0628 0.084 Uiso 1 1 calc R U . . .
C1 C 0.4992(5) 0.6477(4) 0.1392(3) 0.0418(15) Uani 1 1 d . . . . .
C2 C 0.4356(5) 0.7379(4) 0.1529(3) 0.0398(14) Uani 1 1 d . . . . .
C3 C 0.3582(5) 0.7298(4) 0.2173(4) 0.0484(16) Uani 1 1 d . . . . .
H3 H 0.3161 0.7891 0.2288 0.058 Uiso 1 1 calc R U . . .
C4 C 0.3395(6) 0.6409(4) 0.2651(3) 0.0455(15) Uani 1 1 d . . . . .
C5 C 0.4004(6) 0.5537(4) 0.2454(3) 0.0463(15) Uani 1 1 d . . . . .
H5 H 0.3858 0.4927 0.2747 0.056 Uiso 1 1 calc R U . . .
C6 C 0.4808(5) 0.5559(4) 0.1843(3) 0.0430(15) Uani 1 1 d . . . . .
C7 C 0.4466(5) 0.8395(4) 0.0987(3) 0.0431(15) Uani 1 1 d . . . . .
C8 C 0.5788(6) 0.8376(5) 0.0941(4) 0.0619(19) Uani 1 1 d . . . . .
H8A H 0.6088 0.8214 0.1463 0.093 Uiso 1 1 calc R U . . .
H8B H 0.5821 0.9038 0.0603 0.093 Uiso 1 1 calc R U . . .
H8C H 0.6296 0.7863 0.0730 0.093 Uiso 1 1 calc R U . . .
C9 C 0.3684(6) 0.9272(4) 0.1266(4) 0.0537(17) Uani 1 1 d . . . . .
H9A H 0.2830 0.9321 0.1282 0.081 Uiso 1 1 calc R U . . .
H9B H 0.3769 0.9906 0.0905 0.081 Uiso 1 1 calc R U . . .
H9C H 0.3962 0.9139 0.1786 0.081 Uiso 1 1 calc R U . . .
C10 C 0.3983(6) 0.8644(4) 0.0175(4) 0.0543(17) Uani 1 1 d . . . . .
H10A H 0.4466 0.8116 -0.0028 0.081 Uiso 1 1 calc R U . . .
H10B H 0.4045 0.9293 -0.0173 0.081 Uiso 1 1 calc R U . . .
H10C H 0.3132 0.8683 0.0206 0.081 Uiso 1 1 calc R U . . .
C11 C 0.2624(6) 0.6322(5) 0.3386(4) 0.0554(18) Uani 1 1 d . . . . .
C12 C 0.3466(7) 0.5630(5) 0.4106(4) 0.074(2) Uani 1 1 d . . . . .
H12A H 0.3839 0.4952 0.4085 0.111 Uiso 1 1 calc R U . . .
H12B H 0.2990 0.5598 0.4578 0.111 Uiso 1 1 calc R U . . .
H12C H 0.4104 0.5903 0.4110 0.111 Uiso 1 1 calc R U . . .
C13 C 0.1999(8) 0.7371(5) 0.3471(4) 0.086(3) Uani 1 1 d . . . . .
H13A H 0.2617 0.7665 0.3470 0.130 Uiso 1 1 calc R U . . .
H13B H 0.1562 0.7289 0.3961 0.130 Uiso 1 1 calc R U . . .
H13C H 0.1425 0.7817 0.3037 0.130 Uiso 1 1 calc R U . . .
C14 C 0.1668(8) 0.5887(6) 0.3360(5) 0.090(3) Uani 1 1 d . . . . .
H14A H 0.1115 0.6342 0.2916 0.135 Uiso 1 1 calc R U . . .
H14B H 0.1208 0.5807 0.3841 0.135 Uiso 1 1 calc R U . . .
H14C H 0.2059 0.5228 0.3305 0.135 Uiso 1 1 calc R U . . .
C15 C 0.5533(5) 0.4622(4) 0.1631(3) 0.0417(14) Uani 1 1 d . . . . .
H15 H 0.6407 0.4556 0.1641 0.050 Uiso 1 1 calc R U . . .
C16 C 0.5244(5) 0.4798(4) 0.0791(3) 0.0354(13) Uani 1 1 d . . . . .
C17 C 0.6144(5) 0.4416(4) 0.0322(4) 0.0452(15) Uani 1 1 d . . . . .
H17 H 0.6938 0.4010 0.0533 0.054 Uiso 1 1 calc R U . . .
C18 C 0.4101(6) 0.5381(4) 0.0452(3) 0.0469(16) Uani 1 1 d . . . . .
H18 H 0.3466 0.5649 0.0757 0.056 Uiso 1 1 calc R U . . .
O2 O 0.6475(4) 0.3792(3) 0.3190(3) 0.0554(12) Uani 1 1 d . . . . .
H2 H 0.6122 0.4414 0.2969 0.083 Uiso 1 1 calc R U . . .
C19 C 0.5901(6) 0.3267(4) 0.2984(3) 0.0452(15) Uani 1 1 d . . . . .
C20 C 0.5830(5) 0.2362(4) 0.3552(3) 0.0431(15) Uani 1 1 d . . . . .
C21 C 0.5350(5) 0.1802(4) 0.3301(4) 0.0455(15) Uani 1 1 d . . . . .
H21 H 0.5331 0.1173 0.3666 0.055 Uiso 1 1 calc R U . . .
C22 C 0.4898(5) 0.2103(4) 0.2553(3) 0.0439(15) Uani 1 1 d . . . . .
C23 C 0.4922(5) 0.3036(4) 0.2024(3) 0.0446(15) Uani 1 1 d . . . . .
H23 H 0.4584 0.3278 0.1517 0.054 Uiso 1 1 calc R U . . .
C24 C 0.5432(6) 0.3622(4) 0.2222(3) 0.0432(15) Uani 1 1 d . . . . .
C25 C 0.6290(6) 0.1998(5) 0.4400(3) 0.0519(17) Uani 1 1 d . . . . .
C26 C 0.5600(6) 0.2813(5) 0.4756(4) 0.0650(19) Uani 1 1 d . . . . .
H26A H 0.5841 0.2564 0.5303 0.097 Uiso 1 1 calc R U . . .
H26B H 0.4723 0.2965 0.4715 0.097 Uiso 1 1 calc R U . . .
H26C H 0.5798 0.3426 0.4474 0.097 Uiso 1 1 calc R U . . .
C27 C 0.7659(6) 0.1749(5) 0.4436(4) 0.0623(19) Uani 1 1 d . . . . .
H27A H 0.8068 0.1239 0.4201 0.093 Uiso 1 1 calc R U . . .
H27B H 0.7929 0.1487 0.4980 0.093 Uiso 1 1 calc R U . . .
H27C H 0.7860 0.2360 0.4152 0.093 Uiso 1 1 calc R U . . .
C28 C 0.5992(7) 0.1035(5) 0.4917(4) 0.073(2) Uani 1 1 d . . . . .
H28A H 0.6399 0.0492 0.4715 0.109 Uiso 1 1 calc R U . . .
H28B H 0.5111 0.1183 0.4911 0.109 Uiso 1 1 calc R U . . .
H28C H 0.6276 0.0826 0.5451 0.109 Uiso 1 1 calc R U . . .
C29 C 0.4493(6) 0.1409(4) 0.2288(4) 0.0495(16) Uani 1 1 d . . . . .
C30 C 0.5598(7) 0.0815(6) 0.1918(5) 0.074(2) Uani 1 1 d . . . . .
H30A H 0.5363 0.0368 0.1743 0.111 Uiso 1 1 calc R U . . .
H30B H 0.6261 0.0412 0.2303 0.111 Uiso 1 1 calc R U . . .
H30C H 0.5867 0.1288 0.1473 0.111 Uiso 1 1 calc R U . . .
C31 C 0.4095(8) 0.0640(6) 0.2963(4) 0.081(2) Uani 1 1 d . . . . .
H31A H 0.3454 0.0991 0.3246 0.121 Uiso 1 1 calc R U . . .
H31B H 0.4791 0.0181 0.3314 0.121 Uiso 1 1 calc R U . . .
H31C H 0.3784 0.0254 0.2763 0.121 Uiso 1 1 calc R U . . .
C32 C 0.3467(8) 0.2010(6) 0.1692(5) 0.093(3) Uani 1 1 d . . . . .
H32A H 0.3238 0.1551 0.1529 0.140 Uiso 1 1 calc R U . . .
H32B H 0.3732 0.2478 0.1241 0.140 Uiso 1 1 calc R U . . .
H32C H 0.2766 0.2392 0.1921 0.140 Uiso 1 1 calc R U . . .
O3 O 0.8873(4) 0.3062(3) 0.1424(2) 0.0579(12) Uani 1 1 d . . . . .
H3A H 0.8972 0.3547 0.1047 0.087 Uiso 1 1 calc R U . . .
C33 C 0.9443(5) 0.2952(4) 0.2074(3) 0.0414(14) Uani 1 1 d . . . . .
C34 C 0.9869(5) 0.1974(4) 0.2649(3) 0.0430(15) Uani 1 1 d . . . . .
C35 C 1.0393(5) 0.1903(4) 0.3310(4) 0.0455(15) Uani 1 1 d . . . . .
H35 H 1.0683 0.1254 0.3703 0.055 Uiso 1 1 calc R U . . .
C36 C 1.0533(5) 0.2708(4) 0.3446(3) 0.0430(15) Uani 1 1 d . . . . .
C37 C 1.0123(5) 0.3660(4) 0.2841(3) 0.0444(15) Uani 1 1 d . . . . .
H37 H 1.0252 0.4216 0.2894 0.053 Uiso 1 1 calc R U . . .
C38 C 0.9535(5) 0.3813(4) 0.2170(3) 0.0406(14) Uani 1 1 d . . . . .
C39 C 0.9821(6) 0.1037(4) 0.2532(4) 0.0472(16) Uani 1 1 d . . . . .
C40 C 0.8509(6) 0.1145(5) 0.2400(4) 0.069(2) Uani 1 1 d . . . . .
H40A H 0.8020 0.1244 0.2846 0.103 Uiso 1 1 calc R U . . .
H40B H 0.8498 0.0533 0.2341 0.103 Uiso 1 1 calc R U . . .
H40C H 0.8169 0.1727 0.1928 0.103 Uiso 1 1 calc R U . . .
C41 C 1.0321(7) 0.0074(5) 0.3261(4) 0.073(2) Uani 1 1 d . . . . .
H41A H 0.9930 0.0200 0.3726 0.109 Uiso 1 1 calc R U . . .
H41B H 1.1201 -0.0100 0.3308 0.109 Uiso 1 1 calc R U . . .
H41C H 1.0148 -0.0485 0.3209 0.109 Uiso 1 1 calc R U . . .
C42 C 1.0621(7) 0.0868(5) 0.1853(4) 0.068(2) Uani 1 1 d . . . . .
H42A H 1.0576 0.0278 0.1772 0.103 Uiso 1 1 calc R U . . .
H42B H 1.1464 0.0752 0.1969 0.103 Uiso 1 1 calc R U . . .
H42C H 1.0335 0.1463 0.1381 0.103 Uiso 1 1 calc R U . . .
C43 C 1.1071(6) 0.2607(5) 0.4200(3) 0.0495(16) Uani 1 1 d . . . . .
C44 C 1.2251(7) 0.2820(7) 0.4026(4) 0.084(3) Uani 1 1 d . . . . .
H44A H 1.2829 0.2327 0.3821 0.127 Uiso 1 1 calc R U . . .
H44B H 1.2589 0.2771 0.4504 0.127 Uiso 1 1 calc R U . . .
H44C H 1.2102 0.3500 0.3641 0.127 Uiso 1 1 calc R U . . .
C45 C 1.0170(7) 0.3370(5) 0.4536(4) 0.069(2) Uani 1 1 d . . . . .
H45A H 1.0492 0.3281 0.5032 0.103 Uiso 1 1 calc R U . . .
H45B H 0.9388 0.3258 0.4619 0.103 Uiso 1 1 calc R U . . .
H45C H 1.0056 0.4056 0.4172 0.103 Uiso 1 1 calc R U . . .
C46 C 1.1324(9) 0.1546(6) 0.4817(4) 0.097(3) Uani 1 1 d . . . . .
H46A H 1.1919 0.1051 0.4620 0.146 Uiso 1 1 calc R U . . .
H46B H 1.0568 0.1393 0.4931 0.146 Uiso 1 1 calc R U . . .
H46C H 1.1648 0.1518 0.5292 0.146 Uiso 1 1 calc R U . . .
C47 C 0.8952(5) 0.4846(4) 0.1553(3) 0.0374(14) Uani 1 1 d . . . . .
H47 H 0.8091 0.4904 0.1497 0.045 Uiso 1 1 calc R U . . .
C48 C 0.9513(5) 0.4924(4) 0.0748(3) 0.0367(13) Uani 1 1 d . . . . .
C49 C 0.8774(5) 0.5479(4) 0.0079(3) 0.0417(14) Uani 1 1 d . . . . .
H49 H 0.7932 0.5813 0.0125 0.050 Uiso 1 1 calc R U . . .
C50 C 1.0736(6) 0.4450(4) 0.0661(3) 0.0448(15) Uani 1 1 d . . . . .
H50 H 1.1254 0.4072 0.1109 0.054 Uiso 1 1 calc R U . . .
O4 O 0.7570(4) 0.5267(3) 0.2838(2) 0.0538(12) Uani 1 1 d . . . . .
H4 H 0.7890 0.4707 0.2782 0.081 Uiso 1 1 calc R U . . .
C51 C 0.8188(5) 0.5901(4) 0.2412(3) 0.0401(14) Uani 1 1 d . . . . .
C52 C 0.8074(5) 0.6731(4) 0.2614(3) 0.0431(15) Uani 1 1 d . . . . .
C53 C 0.8630(6) 0.7418(4) 0.2142(3) 0.0474(16) Uani 1 1 d . . . . .
H53 H 0.8546 0.7987 0.2271 0.057 Uiso 1 1 calc R U . . .
C54 C 0.9304(5) 0.7309(4) 0.1485(3) 0.0443(15) Uani 1 1 d . . . . .
C55 C 0.9429(5) 0.6441(4) 0.1329(3) 0.0430(15) Uani 1 1 d . . . . .
H55 H 0.9910 0.6324 0.0905 0.052 Uiso 1 1 calc R U . . .
C56 C 0.8875(5) 0.5748(4) 0.1773(3) 0.0390(14) Uani 1 1 d . . . . .
C57 C 0.7348(6) 0.6901(5) 0.3342(3) 0.0474(16) Uani 1 1 d . . . . .
C58 C 0.6008(6) 0.7045(6) 0.3257(4) 0.072(2) Uani 1 1 d . . . . .
H58A H 0.5947 0.6450 0.3194 0.108 Uiso 1 1 calc R U . . .
H58B H 0.5647 0.7643 0.2800 0.108 Uiso 1 1 calc R U . . .
H58C H 0.5574 0.7133 0.3722 0.108 Uiso 1 1 calc R U . . .
C59 C 0.7934(7) 0.5997(5) 0.4077(3) 0.0589(18) Uani 1 1 d . . . . .
H59A H 0.7518 0.6120 0.4537 0.088 Uiso 1 1 calc R U . . .
H59B H 0.8794 0.5910 0.4110 0.088 Uiso 1 1 calc R U . . .
H59C H 0.7863 0.5386 0.4051 0.088 Uiso 1 1 calc R U . . .
C60 C 0.7387(7) 0.7849(5) 0.3459(4) 0.0618(19) Uani 1 1 d . . . . .
H60A H 0.7091 0.8439 0.2985 0.093 Uiso 1 1 calc R U . . .
H60B H 0.8224 0.7752 0.3574 0.093 Uiso 1 1 calc R U . . .
H60C H 0.6870 0.7957 0.3893 0.093 Uiso 1 1 calc R U . . .
C61 C 0.9801(5) 0.8116(4) 0.0930(4) 0.0509(16) Uani 1 1 d D U . . .
C62 C 0.8959(14) 0.8657(12) 0.0195(8) 0.064(4) Uani 0.56(3) 1 d D U P A 1
H62A H 0.8129 0.8976 0.0338 0.097 Uiso 0.56(3) 1 calc R U P A 1
H62B H 0.9253 0.9173 -0.0188 0.097 Uiso 0.56(3) 1 calc R U P A 1
H62C H 0.8964 0.8164 -0.0028 0.097 Uiso 0.56(3) 1 calc R U P A 1
C63 C 0.970(3) 0.8912(14) 0.1268(9) 0.084(6) Uani 0.56(3) 1 d D U P A 1
H63A H 0.8848 0.9205 0.1396 0.126 Uiso 0.56(3) 1 calc R U P A 1
H63B H 1.0206 0.8601 0.1740 0.126 Uiso 0.56(3) 1 calc R U P A 1
H63C H 0.9968 0.9443 0.0887 0.126 Uiso 0.56(3) 1 calc R U P A 1
C64 C 1.1091(11) 0.7618(10) 0.0713(12) 0.065(4) Uani 0.56(3) 1 d D U P A 1
H64A H 1.1102 0.7115 0.0499 0.097 Uiso 0.56(3) 1 calc R U P A 1
H64B H 1.1383 0.8130 0.0324 0.097 Uiso 0.56(3) 1 calc R U P A 1
H64C H 1.1620 0.7289 0.1177 0.097 Uiso 0.56(3) 1 calc R U P A 1
C62X C 0.8765(16) 0.8962(17) 0.0402(14) 0.086(8) Uiso 0.44(3) 1 d D . P A 2
H62D H 0.9072 0.9485 0.0043 0.128 Uiso 0.44(3) 1 calc R U P A 2
H62E H 0.8429 0.8692 0.0106 0.128 Uiso 0.44(3) 1 calc R U P A 2
H62F H 0.8128 0.9254 0.0719 0.128 Uiso 0.44(3) 1 calc R U P A 2
C63X C 1.037(2) 0.8533(17) 0.1375(11) 0.064(6) Uiso 0.44(3) 1 d D . P A 2
H63D H 1.1037 0.7982 0.1711 0.096 Uiso 0.44(3) 1 calc R U P A 2
H63E H 1.0691 0.9041 0.1005 0.096 Uiso 0.44(3) 1 calc R U P A 2
H63F H 0.9755 0.8841 0.1692 0.096 Uiso 0.44(3) 1 calc R U P A 2
C64X C 1.0790(18) 0.7732(15) 0.0385(12) 0.060(6) Uiso 0.44(3) 1 d D . P A 2
H64D H 1.1482 0.7183 0.0697 0.089 Uiso 0.44(3) 1 calc R U P A 2
H64E H 1.0452 0.7484 0.0072 0.089 Uiso 0.44(3) 1 calc R U P A 2
H64F H 1.1062 0.8285 0.0042 0.089 Uiso 0.44(3) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.387(6) . ?
O1 H1 0.8400 . ?
C1 C2 1.411(7) . ?
C1 C6 1.412(8) . ?
C2 C3 1.411(8) . ?
C2 C7 1.539(8) . ?
C3 C4 1.391(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.422(8) . ?
C4 C11 1.540(8) . ?
C5 C6 1.390(8) . ?
C5 H5 0.9500 . ?
C6 C15 1.545(7) . ?
C7 C10 1.534(8) . ?
C7 C8 1.540(9) . ?
C7 C9 1.556(7) . ?
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 C14 1.507(10) . ?
C11 C12 1.546(10) . ?
C11 C13 1.560(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.537(8) . ?
C15 C24 1.544(8) . ?
C15 H15 1.0000 . ?
C16 C18 1.387(8) . ?
C16 C17 1.395(8) . ?
C17 C18 1.394(8) 2_665 ?
C17 H17 0.9500 . ?
C18 C17 1.394(8) 2_665 ?
C18 H18 0.9500 . ?
O2 C19 1.381(7) . ?
O2 H2 0.8400 . ?
C19 C20 1.412(8) . ?
C19 C24 1.414(8) . ?
C20 C21 1.398(8) . ?
C20 C25 1.553(8) . ?
C21 C22 1.395(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.401(8) . ?
C22 C29 1.542(8) . ?
C23 C24 1.399(8) . ?
C23 H23 0.9500 . ?
C25 C27 1.522(9) . ?
C25 C26 1.549(8) . ?
C25 C28 1.558(9) . ?
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 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C32 1.512(10) . ?
C29 C31 1.522(9) . ?
C29 C30 1.549(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O3 C33 1.374(7) . ?
O3 H3A 0.8400 . ?
C33 C34 1.419(8) . ?
C33 C38 1.425(8) . ?
C34 C35 1.386(8) . ?
C34 C39 1.538(8) . ?
C35 C36 1.404(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.415(8) . ?
C36 C43 1.534(8) . ?
C37 C38 1.397(8) . ?
C37 H37 0.9500 . ?
C38 C47 1.524(8) . ?
C39 C42 1.529(8) . ?
C39 C40 1.534(9) . ?
C39 C41 1.555(9) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.510(9) . ?
C43 C46 1.537(9) . ?
C43 C45 1.539(8) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C56 1.538(7) . ?
C47 C48 1.543(7) . ?
C47 H47 1.0000 . ?
C48 C50 1.384(8) . ?
C48 C49 1.398(8) . ?
C49 C50 1.408(8) 2_765 ?
C49 H49 0.9500 . ?
C50 C49 1.408(8) 2_765 ?
C50 H50 0.9500 . ?
O4 C51 1.372(6) . ?
O4 H4 0.8400 . ?
C51 C56 1.402(7) . ?
C51 C52 1.404(8) . ?
C52 C53 1.399(8) . ?
C52 C57 1.567(8) . ?
C53 C54 1.405(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.409(8) . ?
C54 C61 1.530(8) . ?
C55 C56 1.390(8) . ?
C55 H55 0.9500 . ?
C57 C58 1.533(9) . ?
C57 C59 1.539(9) . ?
C57 C60 1.552(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C64 1.520(11) . ?
C61 C63 1.521(11) . ?
C61 C62X 1.524(13) . ?
C61 C63X 1.534(14) . ?
C61 C64X 1.550(12) . ?
C61 C62 1.554(11) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C62X H62D 0.9800 . ?
C62X H62E 0.9800 . ?
C62X H62F 0.9800 . ?
C63X H63D 0.9800 . ?
C63X H63E 0.9800 . ?
C63X H63F 0.9800 . ?
C64X H64D 0.9800 . ?
C64X H64E 0.9800 . ?
C64X H64F 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 O1 H1 109.5 . . ?
O1 C1 C2 118.6(5) . . ?
O1 C1 C6 119.4(4) . . ?
C2 C1 C6 122.0(5) . . ?
C1 C2 C3 116.0(5) . . ?
C1 C2 C7 121.6(5) . . ?
C3 C2 C7 122.3(5) . . ?
C4 C3 C2 124.4(5) . . ?
C4 C3 H3 117.8 . . ?
C2 C3 H3 117.8 . . ?
C3 C4 C5 116.9(5) . . ?
C3 C4 C11 123.4(5) . . ?
C5 C4 C11 119.6(5) . . ?
C6 C5 C4 121.4(5) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 119.1(5) . . ?
C5 C6 C15 123.3(5) . . ?
C1 C6 C15 117.6(5) . . ?
C10 C7 C2 109.1(5) . . ?
C10 C7 C8 110.1(5) . . ?
C2 C7 C8 111.6(5) . . ?
C10 C7 C9 106.9(5) . . ?
C2 C7 C9 111.7(5) . . ?
C8 C7 C9 107.4(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C4 110.3(5) . . ?
C14 C11 C12 109.8(6) . . ?
C4 C11 C12 108.9(5) . . ?
C14 C11 C13 109.4(6) . . ?
C4 C11 C13 111.0(5) . . ?
C12 C11 C13 107.4(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C24 113.2(4) . . ?
C16 C15 C6 110.8(5) . . ?
C24 C15 C6 114.4(4) . . ?
C16 C15 H15 105.9 . . ?
C24 C15 H15 105.9 . . ?
C6 C15 H15 105.9 . . ?
C18 C16 C17 116.9(5) . . ?
C18 C16 C15 122.0(5) . . ?
C17 C16 C15 121.0(5) . . ?
C18 C17 C16 121.1(6) 2_665 . ?
C18 C17 H17 119.4 2_665 . ?
C16 C17 H17 119.4 . . ?
C16 C18 C17 121.9(5) . 2_665 ?
C16 C18 H18 119.0 . . ?
C17 C18 H18 119.0 2_665 . ?
C19 O2 H2 109.5 . . ?
O2 C19 C20 117.8(5) . . ?
O2 C19 C24 120.4(5) . . ?
C20 C19 C24 121.8(5) . . ?
C21 C20 C19 116.2(6) . . ?
C21 C20 C25 122.1(5) . . ?
C19 C20 C25 121.7(5) . . ?
C22 C21 C20 124.5(6) . . ?
C22 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
C21 C22 C23 117.1(5) . . ?
C21 C22 C29 122.1(5) . . ?
C23 C22 C29 120.6(5) . . ?
C24 C23 C22 121.8(6) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C19 118.5(5) . . ?
C23 C24 C15 122.4(5) . . ?
C19 C24 C15 119.1(5) . . ?
C27 C25 C26 111.5(6) . . ?
C27 C25 C20 111.3(5) . . ?
C26 C25 C20 109.3(5) . . ?
C27 C25 C28 108.1(6) . . ?
C26 C25 C28 105.8(5) . . ?
C20 C25 C28 110.8(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C29 C31 108.9(6) . . ?
C32 C29 C22 111.3(5) . . ?
C31 C29 C22 112.3(5) . . ?
C32 C29 C30 109.0(6) . . ?
C31 C29 C30 107.4(5) . . ?
C22 C29 C30 107.8(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C33 O3 H3A 109.5 . . ?
O3 C33 C34 117.7(5) . . ?
O3 C33 C38 119.9(5) . . ?
C34 C33 C38 122.2(5) . . ?
C35 C34 C33 115.9(5) . . ?
C35 C34 C39 121.7(5) . . ?
C33 C34 C39 122.3(5) . . ?
C34 C35 C36 125.4(6) . . ?
C34 C35 H35 117.3 . . ?
C36 C35 H35 117.3 . . ?
C35 C36 C37 116.0(5) . . ?
C35 C36 C43 123.9(5) . . ?
C37 C36 C43 120.1(5) . . ?
C38 C37 C36 122.6(5) . . ?
C38 C37 H37 118.7 . . ?
C36 C37 H37 118.7 . . ?
C37 C38 C33 117.6(5) . . ?
C37 C38 C47 123.9(5) . . ?
C33 C38 C47 118.4(5) . . ?
C42 C39 C40 111.2(6) . . ?
C42 C39 C34 109.6(5) . . ?
C40 C39 C34 110.9(5) . . ?
C42 C39 C41 107.1(5) . . ?
C40 C39 C41 106.7(5) . . ?
C34 C39 C41 111.2(5) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C36 109.2(5) . . ?
C44 C43 C46 108.5(7) . . ?
C36 C43 C46 112.0(5) . . ?
C44 C43 C45 109.5(6) . . ?
C36 C43 C45 109.4(5) . . ?
C46 C43 C45 108.2(6) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C38 C47 C56 115.1(5) . . ?
C38 C47 C48 112.2(4) . . ?
C56 C47 C48 111.9(4) . . ?
C38 C47 H47 105.5 . . ?
C56 C47 H47 105.5 . . ?
C48 C47 H47 105.5 . . ?
C50 C48 C49 118.2(5) . . ?
C50 C48 C47 122.0(5) . . ?
C49 C48 C47 119.8(5) . . ?
C48 C49 C50 120.7(5) . 2_765 ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 2_765 . ?
C48 C50 C49 121.0(5) . 2_765 ?
C48 C50 H50 119.5 . . ?
C49 C50 H50 119.5 2_765 . ?
C51 O4 H4 109.5 . . ?
O4 C51 C56 121.0(5) . . ?
O4 C51 C52 118.1(5) . . ?
C56 C51 C52 120.8(5) . . ?
C53 C52 C51 117.9(5) . . ?
C53 C52 C57 120.3(5) . . ?
C51 C52 C57 121.9(5) . . ?
C52 C53 C54 123.4(5) . . ?
C52 C53 H53 118.3 . . ?
C54 C53 H53 118.3 . . ?
C53 C54 C55 116.2(5) . . ?
C53 C54 C61 122.8(5) . . ?
C55 C54 C61 120.9(5) . . ?
C56 C55 C54 122.4(5) . . ?
C56 C55 H55 118.8 . . ?
C54 C55 H55 118.8 . . ?
C55 C56 C51 119.2(5) . . ?
C55 C56 C47 121.3(5) . . ?
C51 C56 C47 119.5(5) . . ?
C58 C57 C59 111.1(6) . . ?
C58 C57 C60 107.2(5) . . ?
C59 C57 C60 106.5(5) . . ?
C58 C57 C52 110.7(5) . . ?
C59 C57 C52 109.1(5) . . ?
C60 C57 C52 112.2(5) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C64 C61 C63 113.2(10) . . ?
C64 C61 C54 109.7(7) . . ?
C63 C61 C54 111.2(7) . . ?
C62X C61 C54 108.6(10) . . ?
C62X C61 C63X 110.2(11) . . ?
C54 C61 C63X 111.3(9) . . ?
C62X C61 C64X 106.2(11) . . ?
C54 C61 C64X 113.7(9) . . ?
C63X C61 C64X 106.7(10) . . ?
C64 C61 C62 109.9(9) . . ?
C63 C61 C62 106.6(9) . . ?
C54 C61 C62 106.1(6) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C61 C62X H62D 109.5 . . ?
C61 C62X H62E 109.5 . . ?
H62D C62X H62E 109.5 . . ?
C61 C62X H62F 109.5 . . ?
H62D C62X H62F 109.5 . . ?
H62E C62X H62F 109.5 . . ?
C61 C63X H63D 109.5 . . ?
C61 C63X H63E 109.5 . . ?
H63D C63X H63E 109.5 . . ?
C61 C63X H63F 109.5 . . ?
H63D C63X H63F 109.5 . . ?
H63E C63X H63F 109.5 . . ?
C61 C64X H64D 109.5 . . ?
C61 C64X H64E 109.5 . . ?
H64D C64X H64E 109.5 . . ?
C61 C64X H64F 109.5 . . ?
H64D C64X H64F 109.5 . . ?
H64E C64X H64F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -176.4(5) . . . . ?
C6 C1 C2 C3 3.7(9) . . . . ?
O1 C1 C2 C7 6.1(9) . . . . ?
C6 C1 C2 C7 -173.8(6) . . . . ?
C1 C2 C3 C4 -1.8(9) . . . . ?
C7 C2 C3 C4 175.8(6) . . . . ?
C2 C3 C4 C5 -2.0(9) . . . . ?
C2 C3 C4 C11 175.1(6) . . . . ?
C3 C4 C5 C6 4.0(9) . . . . ?
C11 C4 C5 C6 -173.2(6) . . . . ?
C4 C5 C6 C1 -2.1(9) . . . . ?
C4 C5 C6 C15 177.2(6) . . . . ?
O1 C1 C6 C5 178.2(5) . . . . ?
C2 C1 C6 C5 -1.9(9) . . . . ?
O1 C1 C6 C15 -1.2(8) . . . . ?
C2 C1 C6 C15 178.7(5) . . . . ?
C1 C2 C7 C10 62.4(7) . . . . ?
C3 C2 C7 C10 -115.0(6) . . . . ?
C1 C2 C7 C8 -59.5(7) . . . . ?
C3 C2 C7 C8 123.1(6) . . . . ?
C1 C2 C7 C9 -179.7(6) . . . . ?
C3 C2 C7 C9 3.0(8) . . . . ?
C3 C4 C11 C14 126.8(7) . . . . ?
C5 C4 C11 C14 -56.3(8) . . . . ?
C3 C4 C11 C12 -112.7(7) . . . . ?
C5 C4 C11 C12 64.2(7) . . . . ?
C3 C4 C11 C13 5.3(9) . . . . ?
C5 C4 C11 C13 -177.7(6) . . . . ?
C5 C6 C15 C16 121.2(6) . . . . ?
C1 C6 C15 C16 -59.4(7) . . . . ?
C5 C6 C15 C24 -8.2(8) . . . . ?
C1 C6 C15 C24 171.2(5) . . . . ?
C24 C15 C16 C18 96.3(6) . . . . ?
C6 C15 C16 C18 -33.7(7) . . . . ?
C24 C15 C16 C17 -86.9(6) . . . . ?
C6 C15 C16 C17 143.1(5) . . . . ?
C18 C16 C17 C18 0.4(9) . . . 2_665 ?
C15 C16 C17 C18 -176.6(5) . . . 2_665 ?
C17 C16 C18 C17 -0.4(9) . . . 2_665 ?
C15 C16 C18 C17 176.6(5) . . . 2_665 ?
O2 C19 C20 C21 -174.0(5) . . . . ?
C24 C19 C20 C21 4.5(8) . . . . ?
O2 C19 C20 C25 4.5(8) . . . . ?
C24 C19 C20 C25 -177.0(5) . . . . ?
C19 C20 C21 C22 -3.1(8) . . . . ?
C25 C20 C21 C22 178.4(5) . . . . ?
C20 C21 C22 C23 -0.6(8) . . . . ?
C20 C21 C22 C29 174.0(5) . . . . ?
C21 C22 C23 C24 3.1(8) . . . . ?
C29 C22 C23 C24 -171.6(5) . . . . ?
C22 C23 C24 C19 -1.8(8) . . . . ?
C22 C23 C24 C15 176.3(5) . . . . ?
O2 C19 C24 C23 176.2(5) . . . . ?
C20 C19 C24 C23 -2.2(8) . . . . ?
O2 C19 C24 C15 -1.9(8) . . . . ?
C20 C19 C24 C15 179.6(5) . . . . ?
C16 C15 C24 C23 -10.6(8) . . . . ?
C6 C15 C24 C23 117.6(6) . . . . ?
C16 C15 C24 C19 167.5(5) . . . . ?
C6 C15 C24 C19 -64.3(7) . . . . ?
C21 C20 C25 C27 113.4(6) . . . . ?
C19 C20 C25 C27 -65.0(7) . . . . ?
C21 C20 C25 C26 -123.1(6) . . . . ?
C19 C20 C25 C26 58.5(7) . . . . ?
C21 C20 C25 C28 -6.9(8) . . . . ?
C19 C20 C25 C28 174.7(5) . . . . ?
C21 C22 C29 C32 148.5(6) . . . . ?
C23 C22 C29 C32 -37.1(8) . . . . ?
C21 C22 C29 C31 26.1(8) . . . . ?
C23 C22 C29 C31 -159.5(6) . . . . ?
C21 C22 C29 C30 -92.0(7) . . . . ?
C23 C22 C29 C30 82.4(7) . . . . ?
O3 C33 C34 C35 -177.4(5) . . . . ?
C38 C33 C34 C35 -0.6(8) . . . . ?
O3 C33 C34 C39 5.9(8) . . . . ?
C38 C33 C34 C39 -177.3(5) . . . . ?
C33 C34 C35 C36 -0.2(9) . . . . ?
C39 C34 C35 C36 176.5(5) . . . . ?
C34 C35 C36 C37 -1.6(9) . . . . ?
C34 C35 C36 C43 177.3(5) . . . . ?
C35 C36 C37 C38 4.4(8) . . . . ?
C43 C36 C37 C38 -174.6(5) . . . . ?
C36 C37 C38 C33 -5.2(8) . . . . ?
C36 C37 C38 C47 172.5(5) . . . . ?
O3 C33 C38 C37 180.0(5) . . . . ?
C34 C33 C38 C37 3.2(8) . . . . ?
O3 C33 C38 C47 2.1(8) . . . . ?
C34 C33 C38 C47 -174.7(5) . . . . ?
C35 C34 C39 C42 -113.5(7) . . . . ?
C33 C34 C39 C42 63.0(8) . . . . ?
C35 C34 C39 C40 123.3(6) . . . . ?
C33 C34 C39 C40 -60.2(7) . . . . ?
C35 C34 C39 C41 4.8(8) . . . . ?
C33 C34 C39 C41 -178.8(5) . . . . ?
C35 C36 C43 C44 114.7(7) . . . . ?
C37 C36 C43 C44 -66.4(7) . . . . ?
C35 C36 C43 C46 -5.5(9) . . . . ?
C37 C36 C43 C46 173.4(6) . . . . ?
C35 C36 C43 C45 -125.5(6) . . . . ?
C37 C36 C43 C45 53.5(7) . . . . ?
C37 C38 C47 C56 -9.0(8) . . . . ?
C33 C38 C47 C56 168.7(5) . . . . ?
C37 C38 C47 C48 120.6(6) . . . . ?
C33 C38 C47 C48 -61.7(7) . . . . ?
C38 C47 C48 C50 -35.8(7) . . . . ?
C56 C47 C48 C50 95.4(6) . . . . ?
C38 C47 C48 C49 143.6(5) . . . . ?
C56 C47 C48 C49 -85.1(6) . . . . ?
C50 C48 C49 C50 0.3(9) . . . 2_765 ?
C47 C48 C49 C50 -179.2(5) . . . 2_765 ?
C49 C48 C50 C49 -0.3(9) . . . 2_765 ?
C47 C48 C50 C49 179.2(5) . . . 2_765 ?
O4 C51 C52 C53 -175.2(5) . . . . ?
C56 C51 C52 C53 2.3(9) . . . . ?
O4 C51 C52 C57 4.5(8) . . . . ?
C56 C51 C52 C57 -177.9(5) . . . . ?
C51 C52 C53 C54 -0.9(9) . . . . ?
C57 C52 C53 C54 179.4(6) . . . . ?
C52 C53 C54 C55 -1.6(9) . . . . ?
C52 C53 C54 C61 173.9(6) . . . . ?
C53 C54 C55 C56 2.9(9) . . . . ?
C61 C54 C55 C56 -172.8(6) . . . . ?
C54 C55 C56 C51 -1.6(9) . . . . ?
C54 C55 C56 C47 175.6(5) . . . . ?
O4 C51 C56 C55 176.3(5) . . . . ?
C52 C51 C56 C55 -1.2(9) . . . . ?
O4 C51 C56 C47 -0.9(8) . . . . ?
C52 C51 C56 C47 -178.3(5) . . . . ?
C38 C47 C56 C55 120.7(6) . . . . ?
C48 C47 C56 C55 -9.0(7) . . . . ?
C38 C47 C56 C51 -62.2(7) . . . . ?
C48 C47 C56 C51 168.1(5) . . . . ?
C53 C52 C57 C58 117.6(6) . . . . ?
C51 C52 C57 C58 -62.1(8) . . . . ?
C53 C52 C57 C59 -119.8(6) . . . . ?
C51 C52 C57 C59 60.4(7) . . . . ?
C53 C52 C57 C60 -2.1(8) . . . . ?
C51 C52 C57 C60 178.2(6) . . . . ?
C53 C54 C61 C64 137.5(11) . . . . ?
C55 C54 C61 C64 -47.2(12) . . . . ?
C53 C54 C61 C63 11.6(14) . . . . ?
C55 C54 C61 C63 -173.1(13) . . . . ?
C53 C54 C61 C62X -77.6(13) . . . . ?
C55 C54 C61 C62X 97.8(13) . . . . ?
C53 C54 C61 C63X 44.0(12) . . . . ?
C55 C54 C61 C63X -140.7(11) . . . . ?
C53 C54 C61 C64X 164.4(12) . . . . ?
C55 C54 C61 C64X -20.2(13) . . . . ?
C53 C54 C61 C62 -103.9(10) . . . . ?
C55 C54 C61 C62 71.5(10) . . . . ?

_refine_diff_density_max         0.337
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.071


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr521
_database_code_depnum_ccdc_archive 'CCDC 1043855'
_audit_update_record             
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H90 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H96 N2 O4'
_chemical_formula_weight         1005.46

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.6430(10)
_cell_length_b                   15.4125(11)
_cell_length_c                   16.1202(11)
_cell_angle_alpha                75.412(12)
_cell_angle_beta                 69.309(11)
_cell_angle_gamma                73.026(12)
_cell_volume                     3209.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21877
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.9

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.063
_shelx_estimated_absorpt_T_min   0.994
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            21642
_diffrn_reflns_av_unetI/netI     0.2223
_diffrn_reflns_av_R_equivalents  0.2157
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.291
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        22.500
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             8056
_reflns_number_gt                3030
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_structure_solution    'SHELXT, (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1940P)²+13.0654P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8056
_refine_ls_number_parameters     728
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.2856
_refine_ls_R_factor_gt           0.1460
_refine_ls_wR_factor_ref         0.4837
_refine_ls_wR_factor_gt          0.3418
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1003(7) 0.6981(5) 0.3501(7) 0.078(3) Uani 1 1 d D . . . .
H1 H 0.103(10) 0.641(2) 0.362(10) 0.117 Uiso 1 1 d D U . . .
O2 O 0.2565(6) 0.4283(5) 0.5145(6) 0.072(3) Uani 1 1 d D . . . .
H2 H 0.3057 0.4268 0.4675 0.108 Uiso 1 1 calc DR U . . .
O3 O 0.4657(12) 0.2410(8) 0.3517(11) 0.144(5) Uani 1 1 d D . . . .
H3 H 0.485(19) 0.186(6) 0.375(16) 0.215 Uiso 1 1 d D U . . .
O4 O 0.6787(7) 0.4438(5) 0.0669(7) 0.077(3) Uani 1 1 d . . . . .
H4 H 0.619(11) 0.473(10) 0.084(11) 0.115 Uiso 1 1 d . U . . .
C1 C 0.1837(10) 0.7367(7) 0.3181(8) 0.060(3) Uani 1 1 d . . . . .
C2 C 0.1705(9) 0.8304(7) 0.2754(8) 0.056(3) Uani 1 1 d . . . . .
C3 C 0.2562(11) 0.8685(8) 0.2491(9) 0.070(4) Uani 1 1 d . . . . .
H3A H 0.2489 0.9321 0.2243 0.084 Uiso 1 1 calc R U . . .
C4 C 0.3487(10) 0.8201(7) 0.2569(9) 0.064(4) Uani 1 1 d . . . . .
C5 C 0.3595(10) 0.7261(7) 0.2963(8) 0.063(3) Uani 1 1 d . . . . .
H5 H 0.4225 0.6911 0.3030 0.075 Uiso 1 1 calc R U . . .
C6 C 0.2764(10) 0.6839(7) 0.3260(8) 0.060(3) Uani 1 1 d . . . . .
C7 C 0.0695(12) 0.8883(8) 0.2636(10) 0.078(4) Uani 1 1 d . . . . .
C8 C 0.0406(11) 0.8430(8) 0.2038(10) 0.087(5) Uani 1 1 d . . . . .
H8A H -0.0213 0.8810 0.1917 0.130 Uiso 1 1 calc R U . . .
H8B H 0.0302 0.7816 0.2350 0.130 Uiso 1 1 calc R U . . .
H8C H 0.0945 0.8377 0.1469 0.130 Uiso 1 1 calc R U . . .
C9 C -0.0107(12) 0.8904(9) 0.3563(10) 0.089(4) Uani 1 1 d . . . . .
H9A H -0.0726 0.9338 0.3495 0.133 Uiso 1 1 calc R U . . .
H9B H 0.0134 0.9099 0.3966 0.133 Uiso 1 1 calc R U . . .
H9C H -0.0237 0.8288 0.3816 0.133 Uiso 1 1 calc R U . . .
C10 C 0.0742(11) 0.9865(7) 0.2171(10) 0.084(4) Uani 1 1 d . . . . .
H10A H 0.1285 0.9859 0.1601 0.126 Uiso 1 1 calc R U . . .
H10B H 0.0867 1.0187 0.2559 0.126 Uiso 1 1 calc R U . . .
H10C H 0.0104 1.0184 0.2054 0.126 Uiso 1 1 calc R U . . .
C11 C 0.4410(11) 0.8631(9) 0.2262(11) 0.081(4) Uani 1 1 d . . . . .
C12 C 0.4772(12) 0.8524(9) 0.3088(13) 0.112(6) Uani 1 1 d . . . . .
H12A H 0.5366 0.8782 0.2899 0.168 Uiso 1 1 calc R U . . .
H12B H 0.4941 0.7870 0.3340 0.168 Uiso 1 1 calc R U . . .
H12C H 0.4238 0.8852 0.3546 0.168 Uiso 1 1 calc R U . . .
C13 C 0.4154(12) 0.9648(9) 0.1896(13) 0.120(7) Uani 1 1 d . . . . .
H13A H 0.3980 0.9733 0.1342 0.180 Uiso 1 1 calc R U . . .
H13B H 0.4732 0.9912 0.1766 0.180 Uiso 1 1 calc R U . . .
H13C H 0.3583 0.9958 0.2343 0.180 Uiso 1 1 calc R U . . .
C14 C 0.5266(12) 0.8114(9) 0.1561(11) 0.100(5) Uani 1 1 d . . . . .
H14A H 0.5067 0.8196 0.1021 0.150 Uiso 1 1 calc R U . . .
H14B H 0.5414 0.7458 0.1811 0.150 Uiso 1 1 calc R U . . .
H14C H 0.5864 0.8358 0.1404 0.150 Uiso 1 1 calc R U . . .
C15 C 0.2869(9) 0.5877(7) 0.3821(8) 0.052(3) Uani 1 1 d . . . . .
H15 H 0.2393 0.5593 0.3718 0.063 Uiso 1 1 calc R U . . .
C16 C 0.2377(10) 0.5104(7) 0.5469(9) 0.063(3) Uani 1 1 d . . . . .
C17 C 0.2066(10) 0.5086(8) 0.6383(9) 0.064(4) Uani 1 1 d . . . . .
C18 C 0.1824(9) 0.5949(7) 0.6683(9) 0.064(3) Uani 1 1 d . . . . .
H18 H 0.1583 0.5967 0.7310 0.077 Uiso 1 1 calc R U . . .
C19 C 0.1935(10) 0.6774(7) 0.6067(9) 0.062(3) Uani 1 1 d . . . . .
C20 C 0.2276(10) 0.6741(7) 0.5164(10) 0.069(4) Uani 1 1 d . . . . .
H20 H 0.2365 0.7294 0.4752 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2503(9) 0.5912(7) 0.4812(8) 0.055(3) Uani 1 1 d . . . . .
C22 C 0.2014(10) 0.4191(7) 0.7054(9) 0.063(3) Uani 1 1 d . . . . .
C23 C 0.3022(10) 0.3512(8) 0.6867(9) 0.079(4) Uani 1 1 d . . . . .
H23A H 0.3221 0.3379 0.6256 0.118 Uiso 1 1 calc R U . . .
H23B H 0.2969 0.2941 0.7301 0.118 Uiso 1 1 calc R U . . .
H23C H 0.3525 0.3777 0.6923 0.118 Uiso 1 1 calc R U . . .
C24 C 0.1211(10) 0.3740(8) 0.7017(9) 0.077(4) Uani 1 1 d . . . . .
H24A H 0.0556 0.4169 0.7150 0.116 Uiso 1 1 calc R U . . .
H24B H 0.1183 0.3175 0.7464 0.116 Uiso 1 1 calc R U . . .
H24C H 0.1389 0.3590 0.6416 0.116 Uiso 1 1 calc R U . . .
C25 C 0.1726(10) 0.4358(8) 0.8034(8) 0.075(4) Uani 1 1 d . . . . .
H25A H 0.2240 0.4606 0.8094 0.112 Uiso 1 1 calc R U . . .
H25B H 0.1677 0.3775 0.8448 0.112 Uiso 1 1 calc R U . . .
H25C H 0.1079 0.4798 0.8177 0.112 Uiso 1 1 calc R U . . .
C26 C 0.1671(10) 0.7714(7) 0.6376(10) 0.070(4) Uani 1 1 d . . . . .
C27 C 0.2644(11) 0.8128(8) 0.5974(9) 0.082(4) Uani 1 1 d . . . . .
H27A H 0.2837 0.8233 0.5316 0.123 Uiso 1 1 calc R U . . .
H27B H 0.3192 0.7694 0.6176 0.123 Uiso 1 1 calc R U . . .
H27C H 0.2501 0.8712 0.6183 0.123 Uiso 1 1 calc R U . . .
C28 C 0.0855(11) 0.8356(8) 0.5993(10) 0.086(4) Uani 1 1 d . . . . .
H28A H 0.1087 0.8413 0.5337 0.129 Uiso 1 1 calc R U . . .
H28B H 0.0700 0.8963 0.6161 0.129 Uiso 1 1 calc R U . . .
H28C H 0.0252 0.8106 0.6236 0.129 Uiso 1 1 calc R U . . .
C29 C 0.1334(10) 0.7649(7) 0.7388(9) 0.072(4) Uani 1 1 d . . . . .
H29A H 0.1163 0.8265 0.7539 0.109 Uiso 1 1 calc R U . . .
H29B H 0.1876 0.7260 0.7627 0.109 Uiso 1 1 calc R U . . .
H29C H 0.0744 0.7379 0.7652 0.109 Uiso 1 1 calc R U . . .
C30 C 0.3880(10) 0.5254(7) 0.3521(9) 0.063(4) Uani 1 1 d D . . . .
C31 C 0.4102(10) 0.4753(7) 0.2829(8) 0.060(3) Uani 1 1 d . . . . .
H31 H 0.3596 0.4823 0.2562 0.072 Uiso 1 1 calc R U . . .
C32 C 0.5015(11) 0.4164(7) 0.2514(9) 0.062(3) Uani 1 1 d . . . . .
C33 C 0.5776(10) 0.4084(7) 0.2871(8) 0.064(3) Uani 1 1 d . . . . .
H33 H 0.6421 0.3709 0.2646 0.077 Uiso 1 1 calc R U . . .
C34 C 0.5575(10) 0.4565(8) 0.3570(8) 0.061(3) Uani 1 1 d . . . . .
H34 H 0.6081 0.4487 0.3840 0.073 Uiso 1 1 calc R U . . .
C35 C 0.4646(10) 0.5157(8) 0.3880(9) 0.064(3) Uani 1 1 d . . . . .
H35 H 0.4538 0.5494 0.4337 0.077 Uiso 1 1 calc R U . . .
C36 C 0.4100(11) 0.2515(8) 0.2974(10) 0.072(4) Uani 1 1 d . . . . .
C37 C 0.3374(11) 0.1983(7) 0.3321(10) 0.073(4) Uani 1 1 d . . . . .
C38 C 0.2829(11) 0.2054(8) 0.2753(12) 0.086(5) Uani 1 1 d . . . . .
H38 H 0.2317 0.1719 0.2957 0.103 Uiso 1 1 calc R U . . .
C39 C 0.2982(10) 0.2587(9) 0.1899(12) 0.085(4) Uani 1 1 d . U . . .
C40 C 0.3720(9) 0.3136(8) 0.1540(10) 0.078(4) Uani 1 1 d . U . . .
H40 H 0.3819 0.3519 0.0967 0.094 Uiso 1 1 calc R U . . .
C41 C 0.4312(9) 0.3051(7) 0.2144(9) 0.059(3) Uani 1 1 d . U . . .
C42 C 0.3208(13) 0.1372(9) 0.4245(10) 0.094(4) Uani 1 1 d . U . . .
C43 C 0.2793(14) 0.1956(9) 0.4977(11) 0.111(5) Uani 1 1 d . U . . .
H43A H 0.3316 0.2235 0.4977 0.167 Uiso 1 1 calc R U . . .
H43B H 0.2572 0.1571 0.5561 0.167 Uiso 1 1 calc R U . . .
H43C H 0.2224 0.2442 0.4868 0.167 Uiso 1 1 calc R U . . .
C44 C 0.2371(14) 0.0841(10) 0.4396(12) 0.122(5) Uani 1 1 d . U . . .
H44A H 0.1757 0.1286 0.4329 0.183 Uiso 1 1 calc R U . . .
H44B H 0.2232 0.0478 0.5003 0.183 Uiso 1 1 calc R U . . .
H44C H 0.2604 0.0431 0.3951 0.183 Uiso 1 1 calc R U . . .
C45 C 0.4078(13) 0.0630(9) 0.4326(12) 0.116(5) Uani 1 1 d . U . . .
H45A H 0.4364 0.0345 0.3783 0.174 Uiso 1 1 calc R U . . .
H45B H 0.3871 0.0166 0.4852 0.174 Uiso 1 1 calc R U . . .
H45C H 0.4583 0.0881 0.4399 0.174 Uiso 1 1 calc R U . . .
C46 C 0.2313(11) 0.2658(10) 0.1319(10) 0.098(4) Uani 1 1 d D U . . .
C47 C 0.1251(16) 0.3253(16) 0.1733(18) 0.097(7) Uani 0.612(17) 1 d D U P A 1
H47A H 0.1321 0.3822 0.1847 0.146 Uiso 0.612(17) 1 calc R U P A 1
H47B H 0.0861 0.3404 0.1311 0.146 Uiso 0.612(17) 1 calc R U P A 1
H47C H 0.0907 0.2906 0.2299 0.146 Uiso 0.612(17) 1 calc R U P A 1
C48 C 0.229(2) 0.1766(12) 0.1117(18) 0.099(8) Uani 0.612(17) 1 d D U P A 1
H48A H 0.1846 0.1887 0.0747 0.149 Uiso 0.612(17) 1 calc R U P A 1
H48B H 0.2968 0.1466 0.0791 0.149 Uiso 0.612(17) 1 calc R U P A 1
H48C H 0.2042 0.1362 0.1682 0.149 Uiso 0.612(17) 1 calc R U P A 1
C49 C 0.2661(18) 0.3274(14) 0.0348(14) 0.095(7) Uani 0.612(17) 1 d D U P A 1
H49A H 0.2694 0.3874 0.0423 0.142 Uiso 0.612(17) 1 calc R U P A 1
H49B H 0.3323 0.2962 0.0004 0.142 Uiso 0.612(17) 1 calc R U P A 1
H49C H 0.2177 0.3360 0.0026 0.142 Uiso 0.612(17) 1 calc R U P A 1
C47X C 0.159(3) 0.3566(17) 0.113(3) 0.116(12) Uani 0.388(17) 1 d D U P A 2
H47D H 0.1222 0.3493 0.0750 0.175 Uiso 0.388(17) 1 calc R U P A 2
H47E H 0.1111 0.3740 0.1693 0.175 Uiso 0.388(17) 1 calc R U P A 2
H47F H 0.1963 0.4046 0.0808 0.175 Uiso 0.388(17) 1 calc R U P A 2
C48X C 0.168(3) 0.1910(19) 0.184(3) 0.101(10) Uani 0.388(17) 1 d D U P A 2
H48D H 0.2134 0.1320 0.1975 0.151 Uiso 0.388(17) 1 calc R U P A 2
H48E H 0.1213 0.2100 0.2407 0.151 Uiso 0.388(17) 1 calc R U P A 2
H48F H 0.1309 0.1844 0.1473 0.151 Uiso 0.388(17) 1 calc R U P A 2
C49X C 0.304(2) 0.222(3) 0.048(2) 0.113(11) Uani 0.388(17) 1 d D U P A 2
H49D H 0.3470 0.1643 0.0680 0.170 Uiso 0.388(17) 1 calc R U P A 2
H49E H 0.2648 0.2093 0.0160 0.170 Uiso 0.388(17) 1 calc R U P A 2
H49F H 0.3454 0.2646 0.0083 0.170 Uiso 0.388(17) 1 calc R U P A 2
C50 C 0.5147(10) 0.3610(7) 0.1793(9) 0.063(4) Uani 1 1 d . . . . .
H50 H 0.5001 0.4074 0.1270 0.076 Uiso 1 1 calc R U . . .
C51 C 0.6982(11) 0.3487(7) 0.0881(9) 0.064(4) Uani 1 1 d . . . . .
C52 C 0.7938(10) 0.3008(7) 0.0500(9) 0.063(4) Uani 1 1 d . . . . .
C53 C 0.8114(10) 0.2023(8) 0.0664(9) 0.065(4) Uani 1 1 d . . . . .
H53 H 0.8767 0.1670 0.0423 0.078 Uiso 1 1 calc R U . . .
C54 C 0.7338(10) 0.1579(8) 0.1175(9) 0.062(3) Uani 1 1 d . . . . .
C55 C 0.6406(10) 0.2082(7) 0.1550(8) 0.060(3) Uani 1 1 d . . . . .
H55 H 0.5896 0.1761 0.1908 0.072 Uiso 1 1 calc R U . . .
C56 C 0.6158(10) 0.3049(7) 0.1435(9) 0.061(3) Uani 1 1 d . . . . .
C57 C 0.8810(10) 0.3478(8) -0.0100(9) 0.066(4) Uani 1 1 d . . . . .
C58 C 0.8922(11) 0.4176(8) 0.0384(9) 0.084(4) Uani 1 1 d . . . . .
H58A H 0.9508 0.4430 0.0017 0.126 Uiso 1 1 calc R U . . .
H58B H 0.9009 0.3863 0.0970 0.126 Uiso 1 1 calc R U . . .
H58C H 0.8320 0.4676 0.0471 0.126 Uiso 1 1 calc R U . . .
C59 C 0.8587(11) 0.3978(8) -0.0980(9) 0.077(4) Uani 1 1 d . . . . .
H59A H 0.9137 0.4272 -0.1369 0.116 Uiso 1 1 calc R U . . .
H59B H 0.7961 0.4447 -0.0849 0.116 Uiso 1 1 calc R U . . .
H59C H 0.8520 0.3535 -0.1285 0.116 Uiso 1 1 calc R U . . .
C60 C 0.9813(10) 0.2768(8) -0.0304(10) 0.078(4) Uani 1 1 d . . . . .
H60A H 0.9778 0.2326 -0.0628 0.116 Uiso 1 1 calc R U . . .
H60B H 0.9948 0.2443 0.0262 0.116 Uiso 1 1 calc R U . . .
H60C H 1.0351 0.3084 -0.0674 0.116 Uiso 1 1 calc R U . . .
C61 C 0.7534(10) 0.0506(8) 0.1292(10) 0.070(4) Uani 1 1 d . . . . .
C62 C 0.8584(12) 0.0059(8) 0.0806(11) 0.093(5) Uani 1 1 d . . . . .
H62A H 0.8647 -0.0605 0.0888 0.139 Uiso 1 1 calc R U . . .
H62B H 0.9055 0.0176 0.1049 0.139 Uiso 1 1 calc R U . . .
H62C H 0.8735 0.0316 0.0164 0.139 Uiso 1 1 calc R U . . .
C63 C 0.6807(12) 0.0295(9) 0.0882(14) 0.126(7) Uani 1 1 d . . . . .
H63A H 0.6947 0.0577 0.0246 0.189 Uiso 1 1 calc R U . . .
H63B H 0.6112 0.0550 0.1209 0.189 Uiso 1 1 calc R U . . .
H63C H 0.6911 -0.0372 0.0936 0.189 Uiso 1 1 calc R U . . .
C64 C 0.7294(13) 0.0113(9) 0.2301(11) 0.109(5) Uani 1 1 d . . . . .
H64A H 0.7444 -0.0560 0.2384 0.163 Uiso 1 1 calc R U . . .
H64B H 0.6583 0.0343 0.2602 0.163 Uiso 1 1 calc R U . . .
H64C H 0.7702 0.0305 0.2559 0.163 Uiso 1 1 calc R U . . .
N1 N 0.0965(12) 0.5095(8) 0.3784(13) 0.152(7) Uani 1 1 d D U . . .
C65 C 0.0693(12) 0.4423(9) 0.4008(12) 0.102(5) Uani 1 1 d . U . . .
C66 C 0.0347(12) 0.3567(8) 0.4269(11) 0.100(5) Uani 1 1 d . U . . .
H66A H 0.0883 0.3081 0.3987 0.150 Uiso 1 1 calc R U . . .
H66B H -0.0240 0.3657 0.4071 0.150 Uiso 1 1 calc R U . . .
H66C H 0.0165 0.3388 0.4925 0.150 Uiso 1 1 calc R U . . .
N2 N 0.4880(12) 0.5805(9) 0.0685(9) 0.109(5) Uani 1 1 d . . . . .
C67 C 0.4226(14) 0.6432(11) 0.0737(11) 0.095(5) Uani 1 1 d . . . . .
C68 C 0.3514(12) 0.7260(9) 0.0764(10) 0.093(5) Uani 1 1 d . . . . .
H68A H 0.3851 0.7772 0.0486 0.139 Uiso 1 1 calc R U . . .
H68B H 0.3129 0.7318 0.1391 0.139 Uiso 1 1 calc R U . . .
H68C H 0.3060 0.7272 0.0435 0.139 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.391(14) . ?
O1 H1 0.843(18) . ?
O2 C16 1.406(12) . ?
O2 H2 0.8400 . ?
O3 C36 1.348(17) . ?
O3 H3 0.85(2) . ?
O4 C51 1.384(13) . ?
O4 H4 0.84(15) . ?
C1 C6 1.395(15) . ?
C1 C2 1.424(14) . ?
C2 C3 1.424(16) . ?
C2 C7 1.537(17) . ?
C3 C4 1.376(16) . ?
C3 H3A 0.9500 . ?
C4 C5 1.414(14) . ?
C4 C11 1.548(17) . ?
C5 C6 1.424(16) . ?
C5 H5 0.9500 . ?
C6 C15 1.526(14) . ?
C7 C10 1.521(15) . ?
C7 C9 1.541(19) . ?
C7 C8 1.547(16) . ?
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 C13 1.515(17) . ?
C11 C14 1.53(2) . ?
C11 C12 1.56(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C30 1.499(16) . ?
C15 C21 1.504(15) . ?
C15 H15 1.0000 . ?
C16 C17 1.375(16) . ?
C16 C21 1.429(15) . ?
C17 C18 1.435(15) . ?
C17 C22 1.526(15) . ?
C18 C19 1.413(15) . ?
C18 H18 0.9500 . ?
C19 C20 1.373(16) . ?
C19 C26 1.547(15) . ?
C20 C21 1.430(14) . ?
C20 H20 0.9500 . ?
C22 C23 1.519(17) . ?
C22 C25 1.552(16) . ?
C22 C24 1.555(15) . ?
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 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C29 1.514(17) . ?
C26 C28 1.520(16) . ?
C26 C27 1.590(17) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C35 1.390(15) . ?
C30 C31 1.406(15) . ?
C31 C32 1.382(16) . ?
C31 H31 0.9500 . ?
C32 C33 1.388(16) . ?
C32 C50 1.537(15) . ?
C33 C34 1.403(15) . ?
C33 H33 0.9500 . ?
C34 C35 1.399(16) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C41 1.366(16) . ?
C36 C37 1.404(18) . ?
C37 C38 1.379(18) . ?
C37 C42 1.528(18) . ?
C38 C39 1.39(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.437(18) . ?
C39 C46 1.543(19) . ?
C40 C41 1.477(17) . ?
C40 H40 0.9500 . ?
C41 C50 1.561(15) . ?
C42 C45 1.46(2) . ?
C42 C43 1.51(2) . ?
C42 C44 1.58(2) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.503(19) . ?
C46 C47X 1.53(2) . ?
C46 C49X 1.56(2) . ?
C46 C47 1.563(18) . ?
C46 C48X 1.57(2) . ?
C46 C49 1.606(18) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C47X H47D 0.9800 . ?
C47X H47E 0.9800 . ?
C47X H47F 0.9800 . ?
C48X H48D 0.9800 . ?
C48X H48E 0.9800 . ?
C48X H48F 0.9800 . ?
C49X H49D 0.9800 . ?
C49X H49E 0.9800 . ?
C49X H49F 0.9800 . ?
C50 C56 1.473(16) . ?
C50 H50 1.0000 . ?
C51 C52 1.378(17) . ?
C51 C56 1.457(17) . ?
C52 C53 1.433(14) . ?
C52 C57 1.551(17) . ?
C53 C54 1.395(16) . ?
C53 H53 0.9500 . ?
C54 C55 1.365(16) . ?
C54 C61 1.568(15) . ?
C55 C56 1.407(14) . ?
C55 H55 0.9500 . ?
C57 C59 1.530(17) . ?
C57 C60 1.538(17) . ?
C57 C58 1.553(14) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.501(18) . ?
C61 C64 1.535(19) . ?
C61 C63 1.576(18) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N1 C65 1.144(15) . ?
C65 C66 1.462(17) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
N2 C67 1.141(17) . ?
C67 C68 1.392(19) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 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 O1 H1 124(10) . . ?
C16 O2 H2 109.5 . . ?
C36 O3 H3 115(10) . . ?
C51 O4 H4 118(10) . . ?
O1 C1 C6 120.6(10) . . ?
O1 C1 C2 117.2(11) . . ?
C6 C1 C2 122.2(11) . . ?
C1 C2 C3 115.1(11) . . ?
C1 C2 C7 122.7(11) . . ?
C3 C2 C7 122.1(10) . . ?
C4 C3 C2 124.8(11) . . ?
C4 C3 H3A 117.6 . . ?
C2 C3 H3A 117.6 . . ?
C3 C4 C5 118.1(11) . . ?
C3 C4 C11 123.6(10) . . ?
C5 C4 C11 118.3(12) . . ?
C4 C5 C6 120.2(11) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.4(10) . . ?
C1 C6 C15 121.5(11) . . ?
C5 C6 C15 118.0(11) . . ?
C10 C7 C2 112.7(11) . . ?
C10 C7 C9 108.9(11) . . ?
C2 C7 C9 109.5(11) . . ?
C10 C7 C8 107.7(11) . . ?
C2 C7 C8 107.8(10) . . ?
C9 C7 C8 110.2(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C14 111.0(13) . . ?
C13 C11 C4 111.5(11) . . ?
C14 C11 C4 109.9(10) . . ?
C13 C11 C12 107.8(11) . . ?
C14 C11 C12 107.9(13) . . ?
C4 C11 C12 108.7(12) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C30 C15 C21 113.8(10) . . ?
C30 C15 C6 114.2(10) . . ?
C21 C15 C6 111.7(9) . . ?
C30 C15 H15 105.4 . . ?
C21 C15 H15 105.4 . . ?
C6 C15 H15 105.4 . . ?
C17 C16 O2 118.8(11) . . ?
C17 C16 C21 124.4(10) . . ?
O2 C16 C21 116.7(11) . . ?
C16 C17 C18 116.8(11) . . ?
C16 C17 C22 122.2(10) . . ?
C18 C17 C22 120.9(12) . . ?
C19 C18 C17 121.5(12) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C18 118.7(10) . . ?
C20 C19 C26 118.9(11) . . ?
C18 C19 C26 122.4(12) . . ?
C19 C20 C21 123.1(11) . . ?
C19 C20 H20 118.5 . . ?
C21 C20 H20 118.5 . . ?
C16 C21 C20 115.4(11) . . ?
C16 C21 C15 121.5(9) . . ?
C20 C21 C15 123.1(10) . . ?
C23 C22 C17 110.9(11) . . ?
C23 C22 C25 107.2(10) . . ?
C17 C22 C25 111.5(9) . . ?
C23 C22 C24 108.9(10) . . ?
C17 C22 C24 111.2(10) . . ?
C25 C22 C24 107.0(10) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 C26 C28 109.9(11) . . ?
C29 C26 C19 113.5(10) . . ?
C28 C26 C19 108.5(10) . . ?
C29 C26 C27 108.0(10) . . ?
C28 C26 C27 108.8(11) . . ?
C19 C26 C27 108.1(10) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 116.7(12) . . ?
C35 C30 C15 123.0(11) . . ?
C31 C30 C15 120.3(11) . . ?
C32 C31 C30 123.9(11) . . ?
C32 C31 H31 118.1 . . ?
C30 C31 H31 118.1 . . ?
C31 C32 C33 118.7(11) . . ?
C31 C32 C50 119.0(11) . . ?
C33 C32 C50 122.3(12) . . ?
C32 C33 C34 118.8(12) . . ?
C32 C33 H33 120.6 . . ?
C34 C33 H33 120.6 . . ?
C35 C34 C33 121.5(11) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C30 C35 C34 120.3(11) . . ?
C30 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
O3 C36 C41 120.0(13) . . ?
O3 C36 C37 113.7(13) . . ?
C41 C36 C37 126.1(12) . . ?
C38 C37 C36 114.2(13) . . ?
C38 C37 C42 122.9(13) . . ?
C36 C37 C42 122.9(14) . . ?
C37 C38 C39 124.0(12) . . ?
C37 C38 H38 118.0 . . ?
C39 C38 H38 118.0 . . ?
C38 C39 C40 122.1(13) . . ?
C38 C39 C46 120.8(13) . . ?
C40 C39 C46 116.9(15) . . ?
C39 C40 C41 113.7(13) . . ?
C39 C40 H40 123.1 . . ?
C41 C40 H40 123.1 . . ?
C36 C41 C40 119.7(11) . . ?
C36 C41 C50 123.4(11) . . ?
C40 C41 C50 116.8(11) . . ?
C45 C42 C43 114.5(13) . . ?
C45 C42 C37 113.6(14) . . ?
C43 C42 C37 110.2(11) . . ?
C45 C42 C44 103.3(12) . . ?
C43 C42 C44 105.3(14) . . ?
C37 C42 C44 109.2(13) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C46 C39 116.0(14) . . ?
C47X C46 C39 119.9(19) . . ?
C47X C46 C49X 116(2) . . ?
C39 C46 C49X 104.7(17) . . ?
C48 C46 C47 113.7(15) . . ?
C39 C46 C47 108.7(14) . . ?
C47X C46 C48X 108.0(17) . . ?
C39 C46 C48X 104.2(18) . . ?
C49X C46 C48X 102.0(16) . . ?
C48 C46 C49 104.5(13) . . ?
C39 C46 C49 111.8(13) . . ?
C47 C46 C49 101.1(15) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C46 C47X H47D 109.5 . . ?
C46 C47X H47E 109.5 . . ?
H47D C47X H47E 109.5 . . ?
C46 C47X H47F 109.5 . . ?
H47D C47X H47F 109.5 . . ?
H47E C47X H47F 109.5 . . ?
C46 C48X H48D 109.5 . . ?
C46 C48X H48E 109.5 . . ?
H48D C48X H48E 109.5 . . ?
C46 C48X H48F 109.5 . . ?
H48D C48X H48F 109.5 . . ?
H48E C48X H48F 109.5 . . ?
C46 C49X H49D 109.5 . . ?
C46 C49X H49E 109.5 . . ?
H49D C49X H49E 109.5 . . ?
C46 C49X H49F 109.5 . . ?
H49D C49X H49F 109.5 . . ?
H49E C49X H49F 109.5 . . ?
C56 C50 C32 116.4(10) . . ?
C56 C50 C41 113.3(9) . . ?
C32 C50 C41 108.7(10) . . ?
C56 C50 H50 105.9 . . ?
C32 C50 H50 105.9 . . ?
C41 C50 H50 105.9 . . ?
C52 C51 O4 117.6(11) . . ?
C52 C51 C56 123.6(10) . . ?
O4 C51 C56 118.6(11) . . ?
C51 C52 C53 117.3(11) . . ?
C51 C52 C57 123.4(10) . . ?
C53 C52 C57 119.3(12) . . ?
C54 C53 C52 120.8(12) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C55 C54 C53 119.9(11) . . ?
C55 C54 C61 120.3(11) . . ?
C53 C54 C61 119.7(12) . . ?
C54 C55 C56 123.7(12) . . ?
C54 C55 H55 118.2 . . ?
C56 C55 H55 118.2 . . ?
C55 C56 C51 114.7(11) . . ?
C55 C56 C50 124.8(11) . . ?
C51 C56 C50 120.5(10) . . ?
C59 C57 C60 109.7(11) . . ?
C59 C57 C52 108.6(10) . . ?
C60 C57 C52 111.1(10) . . ?
C59 C57 C58 109.7(10) . . ?
C60 C57 C58 107.1(10) . . ?
C52 C57 C58 110.6(10) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 C64 109.8(12) . . ?
C62 C61 C54 113.8(11) . . ?
C64 C61 C54 108.5(11) . . ?
C62 C61 C63 107.5(12) . . ?
C64 C61 C63 110.4(13) . . ?
C54 C61 C63 106.8(10) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N1 C65 C66 178.4(19) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N2 C67 C68 173.2(18) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 176.1(10) . . . . ?
C6 C1 C2 C3 -5.7(16) . . . . ?
O1 C1 C2 C7 -0.3(16) . . . . ?
C6 C1 C2 C7 177.9(11) . . . . ?
C1 C2 C3 C4 4.4(18) . . . . ?
C7 C2 C3 C4 -179.1(12) . . . . ?
C2 C3 C4 C5 -2.0(19) . . . . ?
C2 C3 C4 C11 178.9(12) . . . . ?
C3 C4 C5 C6 0.5(17) . . . . ?
C11 C4 C5 C6 179.7(11) . . . . ?
O1 C1 C6 C5 -177.2(10) . . . . ?
C2 C1 C6 C5 4.6(17) . . . . ?
O1 C1 C6 C15 -9.7(16) . . . . ?
C2 C1 C6 C15 172.1(10) . . . . ?
C4 C5 C6 C1 -1.8(17) . . . . ?
C4 C5 C6 C15 -169.7(10) . . . . ?
C1 C2 C7 C10 179.2(11) . . . . ?
C3 C2 C7 C10 3.1(17) . . . . ?
C1 C2 C7 C9 57.8(14) . . . . ?
C3 C2 C7 C9 -118.3(12) . . . . ?
C1 C2 C7 C8 -62.1(15) . . . . ?
C3 C2 C7 C8 121.7(12) . . . . ?
C3 C4 C11 C13 1.8(19) . . . . ?
C5 C4 C11 C13 -177.4(13) . . . . ?
C3 C4 C11 C14 -121.7(14) . . . . ?
C5 C4 C11 C14 59.1(16) . . . . ?
C3 C4 C11 C12 120.4(14) . . . . ?
C5 C4 C11 C12 -58.7(15) . . . . ?
C1 C6 C15 C30 153.3(10) . . . . ?
C5 C6 C15 C30 -39.0(13) . . . . ?
C1 C6 C15 C21 -75.8(13) . . . . ?
C5 C6 C15 C21 91.9(13) . . . . ?
O2 C16 C17 C18 -176.3(10) . . . . ?
C21 C16 C17 C18 2.1(19) . . . . ?
O2 C16 C17 C22 6.0(18) . . . . ?
C21 C16 C17 C22 -175.6(11) . . . . ?
C16 C17 C18 C19 -2.2(18) . . . . ?
C22 C17 C18 C19 175.5(11) . . . . ?
C17 C18 C19 C20 0.5(18) . . . . ?
C17 C18 C19 C26 179.5(11) . . . . ?
C18 C19 C20 C21 1.5(19) . . . . ?
C26 C19 C20 C21 -177.6(11) . . . . ?
C17 C16 C21 C20 -0.3(18) . . . . ?
O2 C16 C21 C20 178.1(10) . . . . ?
C17 C16 C21 C15 178.7(12) . . . . ?
O2 C16 C21 C15 -2.9(16) . . . . ?
C19 C20 C21 C16 -1.6(17) . . . . ?
C19 C20 C21 C15 179.5(11) . . . . ?
C30 C15 C21 C16 -59.1(14) . . . . ?
C6 C15 C21 C16 169.8(11) . . . . ?
C30 C15 C21 C20 119.8(11) . . . . ?
C6 C15 C21 C20 -11.3(16) . . . . ?
C16 C17 C22 C23 55.8(15) . . . . ?
C18 C17 C22 C23 -121.8(12) . . . . ?
C16 C17 C22 C25 175.2(12) . . . . ?
C18 C17 C22 C25 -2.4(16) . . . . ?
C16 C17 C22 C24 -65.5(16) . . . . ?
C18 C17 C22 C24 116.9(12) . . . . ?
C20 C19 C26 C29 -178.3(11) . . . . ?
C18 C19 C26 C29 2.7(17) . . . . ?
C20 C19 C26 C28 59.3(16) . . . . ?
C18 C19 C26 C28 -119.7(13) . . . . ?
C20 C19 C26 C27 -58.5(15) . . . . ?
C18 C19 C26 C27 122.5(13) . . . . ?
C21 C15 C30 C35 -36.7(15) . . . . ?
C6 C15 C30 C35 93.2(13) . . . . ?
C21 C15 C30 C31 145.3(10) . . . . ?
C6 C15 C30 C31 -84.9(12) . . . . ?
C35 C30 C31 C32 1.8(17) . . . . ?
C15 C30 C31 C32 -180.0(11) . . . . ?
C30 C31 C32 C33 -2.7(18) . . . . ?
C30 C31 C32 C50 176.3(10) . . . . ?
C31 C32 C33 C34 3.3(17) . . . . ?
C50 C32 C33 C34 -175.6(10) . . . . ?
C32 C33 C34 C35 -3.4(17) . . . . ?
C31 C30 C35 C34 -1.8(16) . . . . ?
C15 C30 C35 C34 -179.9(11) . . . . ?
C33 C34 C35 C30 2.6(18) . . . . ?
O3 C36 C37 C38 -177.3(13) . . . . ?
C41 C36 C37 C38 -2(2) . . . . ?
O3 C36 C37 C42 2.2(19) . . . . ?
C41 C36 C37 C42 177.6(13) . . . . ?
C36 C37 C38 C39 1(2) . . . . ?
C42 C37 C38 C39 -178.3(13) . . . . ?
C37 C38 C39 C40 -2(2) . . . . ?
C37 C38 C39 C46 -177.7(13) . . . . ?
C38 C39 C40 C41 2.2(18) . . . . ?
C46 C39 C40 C41 178.4(11) . . . . ?
O3 C36 C41 C40 177.9(12) . . . . ?
C37 C36 C41 C40 3(2) . . . . ?
O3 C36 C41 C50 -3(2) . . . . ?
C37 C36 C41 C50 -178.7(11) . . . . ?
C39 C40 C41 C36 -2.6(16) . . . . ?
C39 C40 C41 C50 178.7(10) . . . . ?
C38 C37 C42 C45 116.8(16) . . . . ?
C36 C37 C42 C45 -62.6(17) . . . . ?
C38 C37 C42 C43 -113.2(15) . . . . ?
C36 C37 C42 C43 67.3(18) . . . . ?
C38 C37 C42 C44 2.0(19) . . . . ?
C36 C37 C42 C44 -177.4(12) . . . . ?
C38 C39 C46 C48 -58(2) . . . . ?
C40 C39 C46 C48 125.8(16) . . . . ?
C38 C39 C46 C47X 111(3) . . . . ?
C40 C39 C46 C47X -65(3) . . . . ?
C38 C39 C46 C49X -116(2) . . . . ?
C40 C39 C46 C49X 67(2) . . . . ?
C38 C39 C46 C47 71.7(19) . . . . ?
C40 C39 C46 C47 -104.6(16) . . . . ?
C38 C39 C46 C48X -10(2) . . . . ?
C40 C39 C46 C48X 174.2(16) . . . . ?
C38 C39 C46 C49 -177.5(14) . . . . ?
C40 C39 C46 C49 6.1(17) . . . . ?
C31 C32 C50 C56 175.5(11) . . . . ?
C33 C32 C50 C56 -5.5(16) . . . . ?
C31 C32 C50 C41 -55.2(14) . . . . ?
C33 C32 C50 C41 123.7(12) . . . . ?
C36 C41 C50 C56 81.3(15) . . . . ?
C40 C41 C50 C56 -100.1(12) . . . . ?
C36 C41 C50 C32 -49.7(16) . . . . ?
C40 C41 C50 C32 129.0(11) . . . . ?
O4 C51 C52 C53 -175.1(10) . . . . ?
C56 C51 C52 C53 0.3(18) . . . . ?
O4 C51 C52 C57 3.8(18) . . . . ?
C56 C51 C52 C57 179.2(11) . . . . ?
C51 C52 C53 C54 1.2(17) . . . . ?
C57 C52 C53 C54 -177.8(11) . . . . ?
C52 C53 C54 C55 -2.2(18) . . . . ?
C52 C53 C54 C61 176.0(11) . . . . ?
C53 C54 C55 C56 1.7(19) . . . . ?
C61 C54 C55 C56 -176.5(11) . . . . ?
C54 C55 C56 C51 -0.3(17) . . . . ?
C54 C55 C56 C50 176.7(12) . . . . ?
C52 C51 C56 C55 -0.7(17) . . . . ?
O4 C51 C56 C55 174.6(10) . . . . ?
C52 C51 C56 C50 -177.8(11) . . . . ?
O4 C51 C56 C50 -2.5(17) . . . . ?
C32 C50 C56 C55 114.7(12) . . . . ?
C41 C50 C56 C55 -12.3(17) . . . . ?
C32 C50 C56 C51 -68.5(15) . . . . ?
C41 C50 C56 C51 164.5(10) . . . . ?
C51 C52 C57 C59 -67.9(14) . . . . ?
C53 C52 C57 C59 111.0(12) . . . . ?
C51 C52 C57 C60 171.4(11) . . . . ?
C53 C52 C57 C60 -9.8(15) . . . . ?
C51 C52 C57 C58 52.6(17) . . . . ?
C53 C52 C57 C58 -128.5(12) . . . . ?
C55 C54 C61 C62 177.4(12) . . . . ?
C53 C54 C61 C62 -0.8(17) . . . . ?
C55 C54 C61 C64 -60.1(16) . . . . ?
C53 C54 C61 C64 121.7(14) . . . . ?
C55 C54 C61 C63 58.9(17) . . . . ?
C53 C54 C61 C63 -119.3(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 C30 0.84 2.30 2.990(15) 139.9 .
O4 H4 N2 0.84(15) 2.19(15) 2.963(18) 155(16) .
O1 H1 N1 0.843(18) 2.006(18) 2.842(13) 171(11) .

_refine_diff_density_max         1.166
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.080


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
