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

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1032675'
_audit_update_record             
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C144 H132 K N2 Nb2 O4'
_chemical_formula_weight         2179.44

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I 23     '
_symmetry_Int_Tables_number      197

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

_cell_length_a                   46.870(2)
_cell_length_b                   46.878(2)
_cell_length_c                   46.878(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     102999(8)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(1)
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10

_exptl_crystal_density_diffrn    0.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             27432
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            186663
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_av_sigmaI/netI    0.1580
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.52
_reflns_number_total             39376
_reflns_number_gt                19758
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1183P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         39376
_refine_ls_number_parameters     1427
_refine_ls_number_restraints     297
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.0828
_refine_ls_wR_factor_ref         0.2154
_refine_ls_wR_factor_gt          0.1894
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_restrained_S_all      0.907
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.579005(11) 0.199775(12) 0.837627(12) 0.03783(14) Uani 1 1 d . . .
Nb2 Nb 0.608669(11) 0.207326(12) 0.786827(11) 0.03843(14) Uani 1 1 d . . .
K1 K 0.51338(3) 0.20358(3) 0.79441(3) 0.0466(3) Uani 1 1 d . . .
O1 O 0.53993(7) 0.21613(8) 0.84181(8) 0.0337(9) Uani 1 1 d . . .
O2 O 0.58483(7) 0.17341(7) 0.86922(7) 0.0298(8) Uani 1 1 d . . .
O3 O 0.59419(8) 0.22653(9) 0.75278(8) 0.0403(10) Uani 1 1 d . . .
O4 O 0.64539(7) 0.18849(8) 0.78217(8) 0.0331(9) Uani 1 1 d . . .
N1 N 0.57976(9) 0.18307(9) 0.80046(8) 0.0256(9) Uani 1 1 d . . .
N2 N 0.60652(9) 0.22543(9) 0.82278(9) 0.0297(10) Uani 1 1 d . . .
C1 C 0.53116(11) 0.23138(13) 0.86552(12) 0.0342(14) Uani 1 1 d . . .
C2 C 0.53488(11) 0.26080(13) 0.86690(12) 0.0349(14) Uani 1 1 d . . .
C3 C 0.52692(12) 0.27469(13) 0.89160(13) 0.0391(14) Uani 1 1 d . . .
H3 H 0.5302 0.2942 0.8929 0.052 Uiso 1 1 calc R . .
C4 C 0.51417(12) 0.26085(14) 0.91482(12) 0.0403(15) Uani 1 1 d . . .
C5 C 0.50970(12) 0.23158(13) 0.91188(12) 0.0368(14) Uani 1 1 d . . .
H5 H 0.5011 0.2219 0.9269 0.049 Uiso 1 1 calc R . .
C6 C 0.51725(10) 0.21598(12) 0.88787(11) 0.0302(13) Uani 1 1 d . . .
C7 C 0.54586(11) 0.27489(12) 0.84031(12) 0.0353(13) Uani 1 1 d . . .
H7 H 0.5641 0.2660 0.8354 0.047 Uiso 1 1 calc R . .
C8 C 0.52543(12) 0.27023(13) 0.81536(13) 0.0372(14) Uani 1 1 d . . .
C9 C 0.53502(12) 0.26853(14) 0.78791(14) 0.0428(15) Uani 1 1 d . . .
H9 H 0.5546 0.2695 0.7846 0.057 Uiso 1 1 calc R . .
C10 C 0.51673(16) 0.26536(15) 0.76460(14) 0.0537(19) Uani 1 1 d . . .
H10 H 0.5239 0.2647 0.7461 0.071 Uiso 1 1 calc R . .
C11 C 0.48697(14) 0.26319(15) 0.76961(16) 0.0566(19) Uani 1 1 d . . .
H11 H 0.4743 0.2613 0.7545 0.075 Uiso 1 1 calc R . .
C12 C 0.47710(13) 0.26391(15) 0.79729(15) 0.0514(17) Uani 1 1 d . . .
H12 H 0.4577 0.2618 0.8010 0.068 Uiso 1 1 calc R . .
C13 C 0.49611(12) 0.26771(13) 0.81957(14) 0.0398(15) Uani 1 1 d . . .
H13 H 0.4890 0.2686 0.8381 0.053 Uiso 1 1 calc R . .
C14 C 0.55088(13) 0.30689(13) 0.84392(13) 0.0417(15) Uani 1 1 d . . .
C15 C 0.57752(16) 0.31690(17) 0.8517(2) 0.085(3) Uani 1 1 d . . .
H15 H 0.5925 0.3040 0.8535 0.113 Uiso 1 1 calc R . .
C16 C 0.58273(18) 0.34515(19) 0.8570(3) 0.131(5) Uani 1 1 d . . .
H16 H 0.6006 0.3509 0.8633 0.174 Uiso 1 1 calc R . .
C17 C 0.56143(17) 0.36502(18) 0.8528(2) 0.096(3) Uani 1 1 d . . .
H17 H 0.5651 0.3844 0.8552 0.128 Uiso 1 1 calc R . .
C18 C 0.53510(18) 0.35598(15) 0.84521(19) 0.071(2) Uani 1 1 d . . .
H18 H 0.5204 0.3691 0.8429 0.094 Uiso 1 1 calc R . .
C19 C 0.52994(16) 0.32696(15) 0.84087(17) 0.061(2) Uani 1 1 d . . .
H19 H 0.5117 0.3211 0.8357 0.081 Uiso 1 1 calc R . .
C20 C 0.50633(14) 0.27775(15) 0.94102(12) 0.0470(17) Uani 1 1 d . . .
C21 C 0.48748(19) 0.30374(19) 0.93325(15) 0.078(3) Uani 1 1 d . . .
H21A H 0.4982 0.3167 0.9216 0.117 Uiso 1 1 calc R . .
H21B H 0.4816 0.3133 0.9504 0.117 Uiso 1 1 calc R . .
H21C H 0.4709 0.2973 0.9230 0.117 Uiso 1 1 calc R . .
C22 C 0.53347(15) 0.28749(17) 0.95491(14) 0.060(2) Uani 1 1 d . . .
H22a H 0.5439 0.2712 0.9616 0.090 Uiso 1 1 calc R . .
H22b H 0.5290 0.2997 0.9707 0.090 Uiso 1 1 calc R . .
H22c H 0.5448 0.2977 0.9413 0.090 Uiso 1 1 calc R . .
C23 C 0.48870(14) 0.25988(16) 0.96283(13) 0.0531(18) Uani 1 1 d . . .
H23a H 0.4720 0.2524 0.9536 0.080 Uiso 1 1 calc R . .
H23b H 0.4831 0.2718 0.9785 0.080 Uiso 1 1 calc R . .
H23c H 0.5002 0.2444 0.9698 0.080 Uiso 1 1 calc R . .
C24 C 0.51006(11) 0.18474(12) 0.88273(12) 0.0335(13) Uani 1 1 d . . .
H24 H 0.5276 0.1759 0.8755 0.045 Uiso 1 1 calc R . .
C25 C 0.50139(13) 0.16762(14) 0.90853(13) 0.0435(16) Uani 1 1 d . . .
C26 C 0.51975(16) 0.14826(15) 0.92007(16) 0.0587(19) Uani 1 1 d . . .
H26 H 0.5375 0.1457 0.9115 0.078 Uiso 1 1 calc R . .
C27 C 0.5132(2) 0.13220(18) 0.94404(18) 0.074(2) Uani 1 1 d . . .
H27 H 0.5262 0.1193 0.9517 0.098 Uiso 1 1 calc R . .
C28 C 0.4871(2) 0.1359(2) 0.95588(17) 0.081(3) Uani 1 1 d . . .
H28 H 0.4822 0.1254 0.9719 0.107 Uiso 1 1 calc R . .
C29 C 0.4679(2) 0.15470(18) 0.94494(18) 0.076(3) Uani 1 1 d . . .
H29 H 0.4502 0.1569 0.9537 0.101 Uiso 1 1 calc R . .
C30 C 0.47432(17) 0.17035(16) 0.92120(15) 0.061(2) Uani 1 1 d . . .
H30 H 0.4609 0.1827 0.9135 0.082 Uiso 1 1 calc R . .
C31 C 0.48800(12) 0.18190(13) 0.85896(12) 0.0378(14) Uani 1 1 d . . .
C32 C 0.48743(14) 0.15811(14) 0.84125(14) 0.0503(17) Uani 1 1 d . . .
H32 H 0.5013 0.1441 0.8436 0.067 Uiso 1 1 calc R . .
C33 C 0.46761(16) 0.15465(16) 0.82079(15) 0.0580(19) Uani 1 1 d . . .
H33 H 0.4675 0.1382 0.8097 0.077 Uiso 1 1 calc R . .
C34 C 0.44700(15) 0.17611(18) 0.81629(15) 0.063(2) Uani 1 1 d . . .
H34 H 0.4340 0.1745 0.8013 0.084 Uiso 1 1 calc R . .
C35 C 0.44615(12) 0.19935(15) 0.83408(13) 0.0447(15) Uani 1 1 d . . .
H35 H 0.4316 0.2127 0.8320 0.060 Uiso 1 1 calc R . .
C36 C 0.46642(12) 0.20316(14) 0.85489(12) 0.0412(15) Uani 1 1 d . . .
H36 H 0.4661 0.2194 0.8663 0.055 Uiso 1 1 calc R . .
C37 C 0.59258(12) 0.15484(12) 0.88934(12) 0.0343(13) Uani 1 1 d . . .
C38 C 0.59444(11) 0.16402(13) 0.91813(11) 0.0324(13) Uani 1 1 d . . .
C39 C 0.60232(13) 0.14440(15) 0.93841(13) 0.0462(16) Uani 1 1 d . . .
H39 H 0.6035 0.1504 0.9573 0.061 Uiso 1 1 calc R . .
C40 C 0.60853(17) 0.11642(16) 0.93240(15) 0.0595(19) Uani 1 1 d . A .
C41 C 0.60606(15) 0.10807(15) 0.90461(15) 0.0555(18) Uani 1 1 d . . .
H41 H 0.6100 0.0892 0.8999 0.074 Uiso 1 1 calc R . .
C42 C 0.59769(12) 0.12708(14) 0.88259(13) 0.0413(15) Uani 1 1 d . C .
C43 C 0.58761(12) 0.19514(13) 0.92506(11) 0.0356(14) Uani 1 1 d . . .
H43 H 0.5702 0.1995 0.9144 0.047 Uiso 1 1 calc R . .
C44 C 0.60986(13) 0.21636(13) 0.91445(11) 0.0367(14) Uani 1 1 d . . .
C45 C 0.63786(13) 0.20846(14) 0.91094(12) 0.0415(15) Uani 1 1 d . . .
H45 H 0.6431 0.1896 0.9143 0.055 Uiso 1 1 calc R . .
C46 C 0.65864(15) 0.22802(15) 0.90240(13) 0.0496(17) Uani 1 1 d . . .
H46 H 0.6775 0.2224 0.9001 0.066 Uiso 1 1 calc R . .
C47 C 0.65022(16) 0.25650(16) 0.89729(13) 0.0533(19) Uani 1 1 d . . .
H47 H 0.6633 0.2700 0.8909 0.071 Uiso 1 1 calc R . .
C48 C 0.62293(18) 0.26373(14) 0.90176(15) 0.0571(19) Uani 1 1 d . . .
H48 H 0.6176 0.2826 0.8990 0.076 Uiso 1 1 calc R . .
C49 C 0.60234(15) 0.24436(15) 0.91031(13) 0.0482(17) Uani 1 1 d . . .
H49 H 0.5836 0.2503 0.9132 0.064 Uiso 1 1 calc R . .
C50 C 0.58018(12) 0.19989(13) 0.95589(11) 0.0382(14) Uani 1 1 d . . .
C51 C 0.55295(13) 0.19651(17) 0.96604(13) 0.0557(19) Uani 1 1 d . . .
H51 H 0.5387 0.1910 0.9534 0.074 Uiso 1 1 calc R . .
C52 C 0.54602(12) 0.20083(18) 0.99345(14) 0.059(2) Uani 1 1 d . . .
H52 H 0.5269 0.2006 0.9989 0.079 Uiso 1 1 calc R . .
C53 C 0.56646(15) 0.20559(17) 1.01329(14) 0.0585(19) Uani 1 1 d . . .
H53 H 0.5616 0.2068 1.0325 0.078 Uiso 1 1 calc R . .
C54 C 0.59357(15) 0.20859(18) 1.00508(13) 0.063(2) Uani 1 1 d . . .
H54 H 0.6075 0.2128 1.0186 0.084 Uiso 1 1 calc R . .
C55 C 0.60123(14) 0.20542(18) 0.97655(13) 0.061(2) Uani 1 1 d . . .
H55 H 0.6203 0.2070 0.9712 0.081 Uiso 1 1 calc R . .
C56 C 0.6161(2) 0.09580(17) 0.95533(15) 0.101(3) Uani 1 1 d GDU . .
C57 C 0.5901(3) 0.0953(4) 0.9754(3) 0.151(7) Uani 0.55 1 d PGU A 1
H57a H 0.5932 0.0817 0.9903 0.226 Uiso 0.55 1 calc PR A 1
H57b H 0.5734 0.0900 0.9648 0.226 Uiso 0.55 1 calc PR A 1
H57c H 0.5874 0.1139 0.9835 0.226 Uiso 0.55 1 calc PR A 1
C58 C 0.6420(3) 0.1080(3) 0.9714(4) 0.112(5) Uani 0.55 1 d PGU A 1
H58a H 0.6477 0.0949 0.9861 0.168 Uiso 0.55 1 calc PR A 1
H58b H 0.6370 0.1259 0.9798 0.168 Uiso 0.55 1 calc PR A 1
H58c H 0.6575 0.1106 0.9582 0.168 Uiso 0.55 1 calc PR A 1
C59 C 0.6227(5) 0.0653(2) 0.9452(3) 0.146(8) Uani 0.55 1 d PGU A 1
H59a H 0.6270 0.0535 0.9614 0.219 Uiso 0.55 1 calc PR A 1
H59b H 0.6389 0.0657 0.9326 0.219 Uiso 0.55 1 calc PR A 1
H59c H 0.6065 0.0577 0.9353 0.219 Uiso 0.55 1 calc PR A 1
C57' C 0.5949(5) 0.0709(4) 0.9506(5) 0.129(8) Uani 0.45 1 d PGDU A 2
H57a' H 0.5983 0.0563 0.9646 0.194 Uiso 0.45 1 calc PR A 2
H57b' H 0.5975 0.0631 0.9319 0.194 Uiso 0.45 1 calc PR A 2
H57c' H 0.5757 0.0778 0.9525 0.194 Uiso 0.45 1 calc PR A 2
C58' C 0.6464(3) 0.0855(5) 0.9493(4) 0.125(7) Uani 0.45 1 d PGDU A 2
H58a' H 0.6520 0.0718 0.9635 0.187 Uiso 0.45 1 calc PR A 2
H58b' H 0.6593 0.1014 0.9498 0.187 Uiso 0.45 1 calc PR A 2
H58c' H 0.6471 0.0768 0.9308 0.187 Uiso 0.45 1 calc PR A 2
C59' C 0.6133(5) 0.1072(4) 0.9855(3) 0.124(8) Uani 0.45 1 d PGDU A 2
H59a' H 0.6187 0.0926 0.9988 0.186 Uiso 0.45 1 calc PR A 2
H59b' H 0.5940 0.1129 0.9889 0.186 Uiso 0.45 1 calc PR A 2
H59c' H 0.6257 0.1234 0.9878 0.186 Uiso 0.45 1 calc PR A 2
C60 C 0.59458(13) 0.11703(14) 0.85202(12) 0.0429(15) Uani 1 1 d . . .
H60 H 0.5982 0.1337 0.8399 0.057 Uiso 0.50 1 calc PR B 1
H60' H 0.5992 0.1337 0.8403 0.057 Uiso 0.50 1 calc PR B 2
C61 C 0.5623(4) 0.1067(5) 0.8452(5) 0.066(5) Uani 0.50 1 d PGU C 1
C62 C 0.5443(5) 0.0998(6) 0.8679(4) 0.067(4) Uani 0.50 1 d PGU C 1
H62 H 0.5503 0.1029 0.8866 0.089 Uiso 0.50 1 calc PR C 1
C63 C 0.5174(5) 0.0884(5) 0.8627(3) 0.076(5) Uani 0.50 1 d PGU C 1
H63 H 0.5054 0.0838 0.8778 0.101 Uiso 0.50 1 calc PR C 1
C64 C 0.5084(3) 0.0838(4) 0.8347(3) 0.074(5) Uani 0.50 1 d PGU C 1
H64 H 0.4904 0.0761 0.8312 0.098 Uiso 0.50 1 calc PR C 1
C65 C 0.5263(3) 0.0906(3) 0.8120(3) 0.065(4) Uani 0.50 1 d PGU C 1
H65 H 0.5203 0.0876 0.7933 0.086 Uiso 0.50 1 calc PR C 1
C66 C 0.5533(3) 0.1021(4) 0.8172(5) 0.055(4) Uani 0.50 1 d PGU C 1
H66 H 0.5652 0.1066 0.8021 0.073 Uiso 0.50 1 calc PR C 1
C61' C 0.5663(4) 0.1080(5) 0.8425(5) 0.054(4) Uani 0.50 1 d PGU C 2
C62' C 0.5459(5) 0.0962(5) 0.8608(3) 0.063(4) Uani 0.50 1 d PGU C 2
H62' H 0.5495 0.0954 0.8803 0.083 Uiso 0.50 1 calc PR C 2
C63' C 0.5203(4) 0.0857(4) 0.8499(3) 0.070(4) Uani 0.50 1 d PGU C 2
H63' H 0.5068 0.0779 0.8621 0.093 Uiso 0.50 1 calc PR C 2
C64' C 0.5150(3) 0.0870(4) 0.8206(3) 0.074(5) Uani 0.50 1 d PGU C 2
H64' H 0.4980 0.0800 0.8133 0.099 Uiso 0.50 1 calc PR C 2
C65' C 0.5353(3) 0.0987(3) 0.8023(3) 0.068(4) Uani 0.50 1 d PGU C 2
H65' H 0.5318 0.0995 0.7828 0.091 Uiso 0.50 1 calc PR C 2
C66' C 0.5610(3) 0.1092(4) 0.8132(5) 0.060(4) Uani 0.50 1 d PGU C 2
H66' H 0.5745 0.1170 0.8010 0.079 Uiso 0.50 1 calc PR C 2
C67 C 0.61641(14) 0.09433(14) 0.84324(13) 0.0458(16) Uani 1 1 d . C .
C68 C 0.61053(15) 0.06514(15) 0.84651(16) 0.0590(19) Uani 1 1 d . . .
H68 H 0.5927 0.0592 0.8529 0.078 Uiso 1 1 calc R C .
C69 C 0.63169(17) 0.04514(15) 0.84013(17) 0.064(2) Uani 1 1 d . C .
H69 H 0.6282 0.0258 0.8430 0.085 Uiso 1 1 calc R . .
C70 C 0.65703(18) 0.05366(17) 0.8298(2) 0.078(3) Uani 1 1 d . . .
H70 H 0.6715 0.0405 0.8265 0.104 Uiso 1 1 calc R C .
C71 C 0.66137(18) 0.08285(17) 0.82410(17) 0.070(2) Uani 1 1 d . C .
H71 H 0.6779 0.0890 0.8150 0.093 Uiso 1 1 calc R . .
C72 C 0.64099(18) 0.10191(16) 0.83213(17) 0.066(2) Uani 1 1 d . . .
H72 H 0.6446 0.1213 0.8296 0.088 Uiso 1 1 calc R C .
C73 C 0.58109(12) 0.24269(14) 0.73275(12) 0.0403(15) Uani 1 1 d . . .
C74 C 0.56407(14) 0.22923(14) 0.71229(13) 0.0456(15) Uani 1 1 d . . .
C75 C 0.55093(14) 0.24689(16) 0.69113(15) 0.0565(19) Uani 1 1 d . . .
H75 H 0.5397 0.2385 0.6770 0.075 Uiso 1 1 calc R . .
C76 C 0.55456(16) 0.27643(18) 0.69122(17) 0.068(2) Uani 1 1 d . . .
C77 C 0.57165(14) 0.28851(15) 0.71145(14) 0.0517(17) Uani 1 1 d . . .
H77 H 0.5739 0.3082 0.7116 0.069 Uiso 1 1 calc R . .
C78 C 0.58566(12) 0.27229(14) 0.73165(14) 0.0437(15) Uani 1 1 d . . .
C79 C 0.55992(12) 0.19802(13) 0.71227(13) 0.0418(15) Uani 1 1 d . . .
H79 H 0.5750 0.1902 0.7245 0.056 Uiso 1 1 calc R . .
C80 C 0.53177(13) 0.18804(14) 0.72528(13) 0.0420(16) Uani 1 1 d . . .
C81 C 0.53212(15) 0.16296(15) 0.74223(14) 0.0509(17) Uani 1 1 d . . .
H81 H 0.5492 0.1536 0.7459 0.068 Uiso 1 1 calc R . .
C82 C 0.50627(18) 0.15245(16) 0.75335(17) 0.064(2) Uani 1 1 d . . .
H82 H 0.5063 0.1368 0.7655 0.085 Uiso 1 1 calc R . .
C83 C 0.48106(15) 0.1655(2) 0.74617(17) 0.063(2) Uani 1 1 d . . .
H83 H 0.4639 0.1573 0.7519 0.083 Uiso 1 1 calc R . .
C84 C 0.48054(15) 0.18955(19) 0.73126(17) 0.062(2) Uani 1 1 d . . .
H84 H 0.4633 0.1989 0.7280 0.083 Uiso 1 1 calc R . .
C85 C 0.50624(13) 0.20098(16) 0.72033(14) 0.0509(17) Uani 1 1 d . . .
H85 H 0.5057 0.2176 0.7096 0.068 Uiso 1 1 calc R . .
C86 C 0.56445(14) 0.18453(16) 0.68233(14) 0.0527(18) Uani 1 1 d . . .
C87 C 0.58973(13) 0.19081(15) 0.66875(15) 0.0535(18) Uani 1 1 d . . .
H87 H 0.6030 0.2029 0.6772 0.071 Uiso 1 1 calc R . .
C88 C 0.59494(18) 0.1790(2) 0.64260(19) 0.077(2) Uani 1 1 d . . .
H88 H 0.6116 0.1840 0.6330 0.103 Uiso 1 1 calc R . .
C89 C 0.57724(19) 0.1607(3) 0.6305(2) 0.121(5) Uani 1 1 d . . .
H89 H 0.5813 0.1531 0.6126 0.161 Uiso 1 1 calc R . .
C90 C 0.5525(2) 0.1531(3) 0.6448(2) 0.139(5) Uani 1 1 d . . .
H90 H 0.5402 0.1396 0.6370 0.185 Uiso 1 1 calc R . .
C91 C 0.54612(17) 0.1656(2) 0.67061(17) 0.087(3) Uani 1 1 d . . .
H91 H 0.5292 0.1610 0.6800 0.116 Uiso 1 1 calc R . .
C92 C 0.53857(19) 0.29319(16) 0.66804(15) 0.113(3) Uani 1 1 d GU . .
C93 C 0.5063(2) 0.2875(3) 0.6708(3) 0.253(8) Uani 1 1 d GU . .
H93a H 0.5027 0.2674 0.6687 0.380 Uiso 1 1 calc R . .
H93b H 0.4963 0.2978 0.6562 0.380 Uiso 1 1 calc R . .
H93c H 0.4999 0.2937 0.6892 0.380 Uiso 1 1 calc R . .
C94 C 0.5490(3) 0.2832(2) 0.63852(18) 0.182(6) Uani 1 1 d GU . .
H94a H 0.5691 0.2867 0.6368 0.274 Uiso 1 1 calc R . .
H94b H 0.5389 0.2935 0.6239 0.274 Uiso 1 1 calc R . .
H94c H 0.5454 0.2631 0.6365 0.274 Uiso 1 1 calc R . .
C95 C 0.5443(3) 0.32536(17) 0.6714(3) 0.273(10) Uani 1 1 d GU . .
H95a H 0.5644 0.3289 0.6696 0.409 Uiso 1 1 calc R . .
H95b H 0.5379 0.3316 0.6898 0.409 Uiso 1 1 calc R . .
H95c H 0.5343 0.3356 0.6568 0.409 Uiso 1 1 calc R . .
C96 C 0.60774(14) 0.28482(13) 0.75184(13) 0.0448(15) Uani 1 1 d . . .
H96 H 0.6035 0.2772 0.7708 0.060 Uiso 1 1 calc R . .
C97 C 0.63667(12) 0.27321(12) 0.74343(12) 0.0330(13) Uani 1 1 d . . .
C98 C 0.65449(13) 0.26121(12) 0.76391(13) 0.0390(15) Uani 1 1 d . . .
H98 H 0.6485 0.2613 0.7828 0.052 Uiso 1 1 calc R . .
C99 C 0.68060(13) 0.24920(12) 0.75747(14) 0.0402(15) Uani 1 1 d . . .
H99 H 0.6919 0.2411 0.7716 0.053 Uiso 1 1 calc R . .
C100 C 0.68927(13) 0.24960(13) 0.72952(14) 0.0428(16) Uani 1 1 d . . .
H100 H 0.7068 0.2416 0.7247 0.057 Uiso 1 1 calc R . .
C101 C 0.67262(15) 0.26152(14) 0.70854(14) 0.0504(17) Uani 1 1 d . . .
H101 H 0.6789 0.2622 0.6897 0.067 Uiso 1 1 calc R . .
C102 C 0.64584(13) 0.27272(13) 0.71634(13) 0.0417(15) Uani 1 1 d . . .
H102 H 0.6341 0.2801 0.7022 0.055 Uiso 1 1 calc R . .
C103 C 0.60699(16) 0.31745(15) 0.75449(15) 0.0530(17) Uani 1 1 d . . .
C104 C 0.62470(16) 0.33523(17) 0.73878(18) 0.066(2) Uani 1 1 d . . .
H104 H 0.6376 0.3274 0.7259 0.087 Uiso 1 1 calc R . .
C105 C 0.6232(2) 0.36405(19) 0.7421(2) 0.084(3) Uani 1 1 d . . .
H105 H 0.6356 0.3754 0.7315 0.112 Uiso 1 1 calc R . .
C106 C 0.6054(2) 0.37641(19) 0.7594(2) 0.095(3) Uani 1 1 d . . .
H106 H 0.6047 0.3962 0.7610 0.126 Uiso 1 1 calc R . .
C107 C 0.5876(3) 0.35915(18) 0.7753(3) 0.128(5) Uani 1 1 d . . .
H107 H 0.5749 0.3672 0.7883 0.170 Uiso 1 1 calc R . .
C108 C 0.5886(2) 0.3301(2) 0.7720(2) 0.100(3) Uani 1 1 d . . .
H108 H 0.5761 0.3189 0.7825 0.133 Uiso 1 1 calc R . .
C109 C 0.66548(11) 0.16891(11) 0.77986(11) 0.0301(13) Uani 1 1 d . . .
C110 C 0.66694(13) 0.15121(12) 0.75524(13) 0.0375(14) Uani 1 1 d . . .
C111 C 0.69016(12) 0.13259(11) 0.75264(12) 0.0303(13) Uani 1 1 d . . .
H111 H 0.6917 0.1218 0.7361 0.040 Uiso 1 1 calc R . .
C112 C 0.71080(13) 0.12943(12) 0.77330(13) 0.0383(14) Uani 1 1 d . . .
C113 C 0.70807(11) 0.14574(11) 0.79752(13) 0.0327(13) Uani 1 1 d . . .
H113 H 0.7215 0.1435 0.8119 0.043 Uiso 1 1 calc R . .
C114 C 0.68615(11) 0.16553(11) 0.80159(13) 0.0347(14) Uani 1 1 d . . .
C115 C 0.64395(12) 0.15203(12) 0.73298(12) 0.0343(13) Uani 1 1 d . . .
H115 H 0.6319 0.1684 0.7380 0.046 Uiso 1 1 calc R . .
C116 C 0.65583(11) 0.15873(13) 0.70394(13) 0.0374(14) Uani 1 1 d . . .
C117 C 0.65999(12) 0.18705(13) 0.69666(14) 0.0420(15) Uani 1 1 d . . .
H117 H 0.6550 0.2014 0.7094 0.056 Uiso 1 1 calc R . .
C118 C 0.67159(14) 0.19416(15) 0.67032(17) 0.0572(19) Uani 1 1 d . . .
H118 H 0.6748 0.2132 0.6658 0.076 Uiso 1 1 calc R . .
C119 C 0.67850(13) 0.17307(16) 0.65057(15) 0.0529(19) Uani 1 1 d . . .
H119 H 0.6860 0.1778 0.6328 0.070 Uiso 1 1 calc R . .
C120 C 0.67400(13) 0.14527(15) 0.65788(13) 0.0473(16) Uani 1 1 d . . .
H120 H 0.6789 0.1311 0.6449 0.063 Uiso 1 1 calc R . .
C121 C 0.66259(13) 0.13754(14) 0.68354(13) 0.0447(15) Uani 1 1 d . . .
H121 H 0.6593 0.1184 0.6876 0.059 Uiso 1 1 calc R . .
C122 C 0.62391(12) 0.12588(11) 0.73341(13) 0.0356(14) Uani 1 1 d . . .
C123 C 0.60349(11) 0.12170(13) 0.71364(13) 0.0376(14) Uani 1 1 d . . .
H123 H 0.6014 0.1351 0.6991 0.050 Uiso 1 1 calc R . .
C124 C 0.58569(13) 0.09861(14) 0.71401(15) 0.0477(16) Uani 1 1 d . . .
H124 H 0.5720 0.0964 0.6998 0.063 Uiso 1 1 calc R . .
C125 C 0.58808(13) 0.07888(15) 0.73522(15) 0.0491(17) Uani 1 1 d . . .
H125 H 0.5759 0.0632 0.7355 0.065 Uiso 1 1 calc R . .
C126 C 0.60851(14) 0.08194(14) 0.75629(14) 0.0486(16) Uani 1 1 d . . .
H126 H 0.6101 0.0685 0.7708 0.065 Uiso 1 1 calc R . .
C127 C 0.62680(14) 0.10560(15) 0.75554(15) 0.0521(18) Uani 1 1 d . . .
H127 H 0.6407 0.1079 0.7695 0.069 Uiso 1 1 calc R . .
C128 C 0.73698(12) 0.10936(12) 0.76983(13) 0.0386(14) Uani 1 1 d . . .
C129 C 0.76408(14) 0.12677(14) 0.7714(2) 0.067(2) Uani 1 1 d . . .
H129a H 0.7645 0.1371 0.7891 0.101 Uiso 1 1 calc R . .
H129b H 0.7646 0.1400 0.7558 0.101 Uiso 1 1 calc R . .
H129c H 0.7803 0.1143 0.7704 0.101 Uiso 1 1 calc R . .
C130 C 0.73701(14) 0.09401(14) 0.74121(15) 0.0535(18) Uani 1 1 d . . .
H130a H 0.7520 0.0801 0.7410 0.080 Uiso 1 1 calc R . .
H130b H 0.7401 0.1076 0.7262 0.080 Uiso 1 1 calc R . .
H130c H 0.7190 0.0847 0.7384 0.080 Uiso 1 1 calc R . .
C131 C 0.73713(15) 0.08706(14) 0.79337(14) 0.0510(17) Uani 1 1 d . . .
H131a H 0.7200 0.0759 0.7923 0.077 Uiso 1 1 calc R . .
H131b H 0.7381 0.0964 0.8116 0.077 Uiso 1 1 calc R . .
H131c H 0.7534 0.0748 0.7911 0.077 Uiso 1 1 calc R . .
C132 C 0.68461(12) 0.18437(11) 0.82725(12) 0.0315(13) Uani 1 1 d . . .
H132 H 0.6645 0.1895 0.8295 0.042 Uiso 1 1 calc R . .
C133 C 0.70073(12) 0.21251(12) 0.82255(11) 0.0341(13) Uani 1 1 d . . .
C134 C 0.72630(11) 0.21379(12) 0.80877(11) 0.0309(12) Uani 1 1 d . . .
H134 H 0.7343 0.1970 0.8018 0.041 Uiso 1 1 calc R . .
C135 C 0.74062(13) 0.23906(13) 0.80487(12) 0.0410(15) Uani 1 1 d . . .
H135 H 0.7581 0.2393 0.7954 0.055 Uiso 1 1 calc R . .
C136 C 0.72889(14) 0.26430(12) 0.81517(12) 0.0370(14) Uani 1 1 d . . .
H136 H 0.7384 0.2815 0.8124 0.049 Uiso 1 1 calc R . .
C137 C 0.70376(14) 0.26374(12) 0.82910(12) 0.0394(14) Uani 1 1 d . . .
H137 H 0.6963 0.2805 0.8366 0.052 Uiso 1 1 calc R . .
C138 C 0.68876(13) 0.23838(12) 0.83243(11) 0.0348(13) Uani 1 1 d . . .
H138 H 0.6709 0.2384 0.8411 0.046 Uiso 1 1 calc R . .
C139 C 0.69341(13) 0.17020(12) 0.85501(12) 0.0377(14) Uani 1 1 d . . .
C140 C 0.72142(17) 0.16937(19) 0.86424(15) 0.072(2) Uani 1 1 d . . .
H140 H 0.7355 0.1779 0.8532 0.095 Uiso 1 1 calc R . .
C141 C 0.7292(2) 0.1555(3) 0.8906(2) 0.117(4) Uani 1 1 d . . .
H141 H 0.7478 0.1560 0.8976 0.155 Uiso 1 1 calc R . .
C142 C 0.7072(3) 0.1411(3) 0.9049(2) 0.126(5) Uani 1 1 d . . .
H142 H 0.7115 0.1312 0.9215 0.167 Uiso 1 1 calc R . .
C143 C 0.6804(2) 0.14120(19) 0.89588(19) 0.082(3) Uani 1 1 d . . .
H143 H 0.6666 0.1311 0.9059 0.109 Uiso 1 1 calc R . .
C144 C 0.67292(16) 0.15604(15) 0.87192(15) 0.0552(18) Uani 1 1 d . . .
H144 H 0.6538 0.1568 0.8666 0.073 Uiso 1 1 calc R . .


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 N2 1.896(4) . ?
Nb1 N1 1.910(4) . ?
Nb1 O2 1.948(3) . ?
Nb1 O1 1.995(4) . ?
Nb1 Nb2 2.7802(8) . ?
Nb1 K1 3.6874(14) . ?
Nb2 N1 1.880(4) . ?
Nb2 N2 1.890(4) . ?
Nb2 O4 1.947(4) . ?
Nb2 O3 1.954(4) . ?
K1 O1 2.614(4) . ?
K1 C82 3.092(7) . ?
K1 C81 3.222(7) . ?
K1 C10 3.220(7) . ?
K1 C9 3.224(7) . ?
K1 C83 3.255(7) . ?
K1 N1 3.269(4) . ?
K1 C11 3.270(7) . ?
K1 C32 3.293(6) . ?
K1 C12 3.303(7) . ?
K1 C8 3.324(6) . ?
K1 C13 3.330(6) . ?
O1 C1 1.384(6) . ?
O2 C37 1.334(6) . ?
O3 C73 1.354(7) . ?
O4 C109 1.319(6) . ?
C1 C2 1.392(8) . ?
C1 C6 1.430(8) . ?
C2 C3 1.380(8) . ?
C2 C7 1.502(8) . ?
C3 C4 1.401(8) . ?
C4 C5 1.395(8) . ?
C4 C20 1.507(8) . ?
C5 C6 1.388(8) . ?
C6 C24 1.522(8) . ?
C7 C8 1.527(8) . ?
C7 C14 1.528(8) . ?
C8 C9 1.365(8) . ?
C8 C13 1.394(8) . ?
C9 C10 1.397(9) . ?
C10 C11 1.418(9) . ?
C11 C12 1.378(10) . ?
C12 C13 1.385(9) . ?
C14 C19 1.367(9) . ?
C14 C15 1.383(9) . ?
C15 C16 1.369(11) . ?
C16 C17 1.379(12) . ?
C17 C18 1.353(11) . ?
C18 C19 1.397(10) . ?
C20 C22 1.500(9) . ?
C20 C21 1.548(10) . ?
C20 C23 1.559(9) . ?
C24 C25 1.508(8) . ?
C24 C31 1.526(8) . ?
C25 C26 1.363(9) . ?
C25 C30 1.407(9) . ?
C26 C27 1.387(10) . ?
C27 C28 1.353(12) . ?
C28 C29 1.359(12) . ?
C29 C30 1.366(10) . ?
C31 C32 1.390(9) . ?
C31 C36 1.433(8) . ?
C32 C33 1.345(9) . ?
C33 C34 1.411(11) . ?
C34 C35 1.372(9) . ?
C35 C36 1.373(8) . ?
C37 C42 1.361(8) . ?
C37 C38 1.419(8) . ?
C38 C39 1.373(8) . ?
C38 C43 1.528(8) . ?
C39 C40 1.373(9) . ?
C40 C41 1.365(9) . ?
C40 C56 1.489(9) . ?
C41 C42 1.419(9) . ?
C42 C60 1.516(8) . ?
C43 C50 1.503(7) . ?
C43 C44 1.525(8) . ?
C44 C45 1.373(8) . ?
C44 C49 1.373(9) . ?
C45 C46 1.396(9) . ?
C46 C47 1.413(10) . ?
C47 C48 1.339(10) . ?
C48 C49 1.385(9) . ?
C50 C51 1.371(8) . ?
C50 C55 1.406(8) . ?
C51 C52 1.341(9) . ?
C52 C53 1.354(9) . ?
C53 C54 1.335(9) . ?
C54 C55 1.393(8) . ?
C56 C59' 1.516(8) . ?
C56 C58' 1.530(8) . ?
C56 C59 1.5387 . ?
C56 C57 1.5393 . ?
C56 C58 1.5399 . ?
C56 C57' 1.549(8) . ?
C60 C61' 1.464(14) . ?
C60 C67 1.532(9) . ?
C60 C61 1.622(15) . ?
C61 C66 1.3949 . ?
C61 C62 1.3952 . ?
C62 C63 1.3948 . ?
C63 C64 1.3954 . ?
C64 C65 1.3950 . ?
C65 C66 1.3948 . ?
C61' C66' 1.3949 . ?
C61' C62' 1.3951 . ?
C62' C63' 1.3945 . ?
C63' C64' 1.3952 . ?
C64' C65' 1.3951 . ?
C65' C66' 1.3949 . ?
C67 C72 1.314(10) . ?
C67 C68 1.404(9) . ?
C68 C69 1.397(10) . ?
C69 C70 1.343(11) . ?
C70 C71 1.409(11) . ?
C71 C72 1.361(11) . ?
C73 C74 1.398(8) . ?
C73 C78 1.405(9) . ?
C74 C75 1.431(9) . ?
C74 C79 1.476(9) . ?
C75 C76 1.396(10) . ?
C76 C77 1.364(10) . ?
C76 C92 1.536(9) . ?
C77 C78 1.381(9) . ?
C78 C96 1.520(8) . ?
C79 C80 1.527(8) . ?
C79 C86 1.554(9) . ?
C80 C85 1.361(9) . ?
C80 C81 1.419(9) . ?
C81 C82 1.408(10) . ?
C82 C83 1.372(11) . ?
C83 C84 1.327(11) . ?
C84 C85 1.415(10) . ?
C86 C91 1.352(10) . ?
C86 C87 1.377(9) . ?
C87 C88 1.367(10) . ?
C88 C89 1.321(12) . ?
C89 C90 1.388(13) . ?
C90 C91 1.377(12) . ?
C92 C93 1.5399 . ?
C92 C94 1.5400 . ?
C92 C95 1.5400 . ?
C96 C97 1.514(9) . ?
C96 C103 1.535(9) . ?
C97 C102 1.341(8) . ?
C97 C98 1.391(8) . ?
C98 C99 1.380(8) . ?
C99 C100 1.372(8) . ?
C100 C101 1.374(9) . ?
C101 C102 1.409(9) . ?
C103 C108 1.330(10) . ?
C103 C104 1.388(10) . ?
C104 C105 1.361(11) . ?
C105 C106 1.302(13) . ?
C106 C107 1.382(14) . ?
C107 C108 1.370(12) . ?
C109 C114 1.415(8) . ?
C109 C110 1.423(8) . ?
C110 C111 1.401(8) . ?
C110 C115 1.500(8) . ?
C111 C112 1.377(8) . ?
C112 C113 1.375(8) . ?
C112 C128 1.555(8) . ?
C113 C114 1.397(8) . ?
C114 C132 1.494(8) . ?
C115 C116 1.504(8) . ?
C115 C122 1.545(7) . ?
C116 C117 1.384(8) . ?
C116 C121 1.415(8) . ?
C117 C118 1.390(9) . ?
C118 C119 1.393(10) . ?
C119 C120 1.364(9) . ?
C120 C121 1.365(9) . ?
C122 C123 1.346(8) . ?
C122 C127 1.414(9) . ?
C123 C124 1.367(8) . ?
C124 C125 1.362(9) . ?
C125 C126 1.383(9) . ?
C126 C127 1.402(9) . ?
C128 C129 1.511(8) . ?
C128 C131 1.520(9) . ?
C128 C130 1.522(9) . ?
C132 C139 1.518(8) . ?
C132 C133 1.536(8) . ?
C133 C134 1.363(8) . ?
C133 C138 1.414(8) . ?
C134 C135 1.374(8) . ?
C135 C136 1.391(8) . ?
C136 C137 1.347(8) . ?
C137 C138 1.390(8) . ?
C139 C140 1.383(9) . ?
C139 C144 1.411(9) . ?
C140 C141 1.442(12) . ?
C141 C142 1.406(14) . ?
C142 C143 1.322(13) . ?
C143 C144 1.368(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Nb1 N1 84.97(17) . . ?
N2 Nb1 O2 125.90(17) . . ?
N1 Nb1 O2 115.52(17) . . ?
N2 Nb1 O1 114.62(17) . . ?
N1 Nb1 O1 105.32(17) . . ?
O2 Nb1 O1 107.31(15) . . ?
N2 Nb1 Nb2 42.65(12) . . ?
N1 Nb1 Nb2 42.41(12) . . ?
O2 Nb1 Nb2 131.45(11) . . ?
O1 Nb1 Nb2 119.63(11) . . ?
N2 Nb1 K1 109.57(14) . . ?
N1 Nb1 K1 62.24(13) . . ?
O2 Nb1 K1 124.42(11) . . ?
O1 Nb1 K1 43.09(11) . . ?
Nb2 Nb1 K1 86.58(3) . . ?
N1 Nb2 N2 85.99(18) . . ?
N1 Nb2 O4 113.63(17) . . ?
N2 Nb2 O4 110.54(18) . . ?
N1 Nb2 O3 107.81(17) . . ?
N2 Nb2 O3 120.20(19) . . ?
O4 Nb2 O3 115.12(16) . . ?
N1 Nb2 Nb1 43.25(12) . . ?
N2 Nb2 Nb1 42.83(13) . . ?
O4 Nb2 Nb1 118.71(11) . . ?
O3 Nb2 Nb1 125.77(12) . . ?
O1 K1 C82 139.03(19) . . ?
O1 K1 C81 130.45(16) . . ?
C82 K1 C81 25.66(18) . . ?
O1 K1 C10 98.23(15) . . ?
C82 K1 C10 115.6(2) . . ?
C81 K1 C10 100.89(18) . . ?
O1 K1 C9 73.61(14) . . ?
C82 K1 C9 135.02(19) . . ?
C81 K1 C9 113.63(17) . . ?
C10 K1 C9 25.05(16) . . ?
O1 K1 C83 159.3(2) . . ?
C82 K1 C83 24.8(2) . . ?
C81 K1 C83 43.56(18) . . ?
C10 K1 C83 102.4(2) . . ?
C9 K1 C83 126.8(2) . . ?
O1 K1 N1 62.57(11) . . ?
C82 K1 N1 85.91(18) . . ?
C81 K1 N1 68.45(15) . . ?
C10 K1 N1 104.82(16) . . ?
C9 K1 N1 89.22(13) . . ?
C83 K1 N1 110.00(16) . . ?
O1 K1 C11 106.85(15) . . ?
C82 K1 C11 113.6(2) . . ?
C81 K1 C11 109.78(19) . . ?
C10 K1 C11 25.23(17) . . ?
C9 K1 C11 43.81(16) . . ?
C83 K1 C11 92.6(2) . . ?
N1 K1 C11 129.97(15) . . ?
O1 K1 C32 75.80(15) . . ?
C82 K1 C32 82.74(19) . . ?
C81 K1 C32 102.97(17) . . ?
C10 K1 C32 152.83(18) . . ?
C9 K1 C32 142.23(17) . . ?
C83 K1 C32 86.3(2) . . ?
N1 K1 C32 95.94(15) . . ?
C11 K1 C32 130.57(19) . . ?
O1 K1 C12 91.00(15) . . ?
C82 K1 C12 129.3(2) . . ?
C81 K1 C12 132.65(19) . . ?
C10 K1 C12 43.33(18) . . ?
C9 K1 C12 49.99(16) . . ?
C83 K1 C12 105.0(2) . . ?
N1 K1 C12 137.59(14) . . ?
C11 K1 C12 24.20(17) . . ?
C32 K1 C12 109.68(18) . . ?
O1 K1 C8 57.05(13) . . ?
C82 K1 C8 158.60(19) . . ?
C81 K1 C8 137.20(16) . . ?
C10 K1 C8 43.47(16) . . ?
C9 K1 C8 24.01(15) . . ?
C83 K1 C8 143.1(2) . . ?
N1 K1 C8 95.10(12) . . ?
C11 K1 C8 50.65(16) . . ?
C32 K1 C8 118.30(16) . . ?
C12 K1 C8 43.15(15) . . ?
O1 K1 C13 67.12(13) . . ?
C82 K1 C13 153.4(2) . . ?
C81 K1 C13 150.33(17) . . ?
C10 K1 C13 49.71(16) . . ?
C9 K1 C13 42.02(15) . . ?
C83 K1 C13 128.9(2) . . ?
N1 K1 C13 117.78(13) . . ?
C11 K1 C13 42.46(17) . . ?
C32 K1 C13 104.97(16) . . ?
C12 K1 C13 24.09(15) . . ?
C8 K1 C13 24.18(14) . . ?
C1 O1 Nb1 123.4(3) . . ?
C1 O1 K1 131.1(3) . . ?
Nb1 O1 K1 105.47(16) . . ?
C37 O2 Nb1 171.8(4) . . ?
C73 O3 Nb2 169.1(4) . . ?
C109 O4 Nb2 162.9(3) . . ?
Nb2 N1 Nb1 94.34(17) . . ?
Nb2 N1 K1 118.59(18) . . ?
Nb1 N1 K1 86.62(14) . . ?
Nb2 N2 Nb1 94.52(19) . . ?
O1 C1 C2 120.8(5) . . ?
O1 C1 C6 117.6(5) . . ?
C2 C1 C6 121.6(5) . . ?
C3 C2 C1 118.2(6) . . ?
C3 C2 C7 125.6(5) . . ?
C1 C2 C7 116.1(5) . . ?
C2 C3 C4 123.3(6) . . ?
C5 C4 C3 116.3(5) . . ?
C5 C4 C20 124.1(5) . . ?
C3 C4 C20 119.6(6) . . ?
C6 C5 C4 124.1(5) . . ?
C5 C6 C1 116.4(5) . . ?
C5 C6 C24 125.4(5) . . ?
C1 C6 C24 118.1(5) . . ?
C2 C7 C8 111.0(5) . . ?
C2 C7 C14 113.1(5) . . ?
C8 C7 C14 108.8(5) . . ?
C9 C8 C13 116.9(6) . . ?
C9 C8 C7 121.6(5) . . ?
C13 C8 C7 121.5(5) . . ?
C9 C8 K1 73.9(4) . . ?
C13 C8 K1 78.1(4) . . ?
C7 C8 K1 117.9(4) . . ?
C8 C9 C10 122.8(6) . . ?
C8 C9 K1 82.1(4) . . ?
C10 C9 K1 77.3(4) . . ?
C9 C10 C11 118.8(6) . . ?
C9 C10 K1 77.7(4) . . ?
C11 C10 K1 79.4(4) . . ?
C12 C11 C10 119.0(6) . . ?
C12 C11 K1 79.2(4) . . ?
C10 C11 K1 75.4(4) . . ?
C13 C12 C11 119.8(6) . . ?
C13 C12 K1 79.0(4) . . ?
C11 C12 K1 76.6(4) . . ?
C12 C13 C8 122.6(6) . . ?
C12 C13 K1 76.9(4) . . ?
C8 C13 K1 77.7(4) . . ?
C19 C14 C15 116.3(6) . . ?
C19 C14 C7 123.6(6) . . ?
C15 C14 C7 120.1(6) . . ?
C16 C15 C14 122.5(7) . . ?
C15 C16 C17 119.9(8) . . ?
C18 C17 C16 119.1(8) . . ?
C17 C18 C19 120.1(7) . . ?
C14 C19 C18 122.0(7) . . ?
C22 C20 C4 107.9(5) . . ?
C22 C20 C21 110.3(6) . . ?
C4 C20 C21 111.2(5) . . ?
C22 C20 C23 109.2(5) . . ?
C4 C20 C23 112.4(5) . . ?
C21 C20 C23 105.9(6) . . ?
C25 C24 C6 116.4(5) . . ?
C25 C24 C31 110.9(5) . . ?
C6 C24 C31 110.5(5) . . ?
C26 C25 C30 117.6(7) . . ?
C26 C25 C24 120.2(6) . . ?
C30 C25 C24 122.2(6) . . ?
C25 C26 C27 122.8(8) . . ?
C28 C27 C26 117.6(8) . . ?
C27 C28 C29 121.7(8) . . ?
C28 C29 C30 120.6(8) . . ?
C29 C30 C25 119.6(8) . . ?
C32 C31 C36 117.7(5) . . ?
C32 C31 C24 121.3(6) . . ?
C36 C31 C24 121.0(5) . . ?
C32 C31 K1 73.5(4) . . ?
C36 C31 K1 85.5(4) . . ?
C24 C31 K1 112.7(3) . . ?
C33 C32 C31 122.4(7) . . ?
C33 C32 K1 81.8(4) . . ?
C31 C32 K1 82.7(4) . . ?
C32 C33 C34 119.6(7) . . ?
C32 C33 K1 74.9(4) . . ?
C34 C33 K1 84.0(4) . . ?
C35 C34 C33 119.7(6) . . ?
C35 C34 K1 85.0(4) . . ?
C33 C34 K1 72.5(4) . . ?
C34 C35 C36 121.0(6) . . ?
C35 C36 C31 119.5(6) . . ?
O2 C37 C42 120.5(5) . . ?
O2 C37 C38 119.4(5) . . ?
C42 C37 C38 120.0(5) . . ?
C39 C38 C37 118.2(6) . . ?
C39 C38 C43 123.3(5) . . ?
C37 C38 C43 118.6(5) . . ?
C38 C39 C40 123.7(6) . . ?
C41 C40 C39 116.9(6) . . ?
C41 C40 C56 121.5(7) . . ?
C39 C40 C56 121.5(7) . . ?
C40 C41 C42 122.5(7) . . ?
C37 C42 C41 118.7(6) . . ?
C37 C42 C60 120.0(6) . . ?
C41 C42 C60 121.3(6) . . ?
C50 C43 C44 112.0(5) . . ?
C50 C43 C38 113.2(5) . . ?
C44 C43 C38 114.2(5) . . ?
C45 C44 C49 119.1(6) . . ?
C45 C44 C43 121.1(6) . . ?
C49 C44 C43 119.6(6) . . ?
C44 C45 C46 121.6(6) . . ?
C45 C46 C47 118.3(7) . . ?
C48 C47 C46 118.6(6) . . ?
C47 C48 C49 123.0(7) . . ?
C44 C49 C48 119.3(7) . . ?
C51 C50 C55 115.8(5) . . ?
C51 C50 C43 122.1(5) . . ?
C55 C50 C43 121.8(5) . . ?
C52 C51 C50 122.7(6) . . ?
C51 C52 C53 120.8(6) . . ?
C54 C53 C52 119.5(6) . . ?
C53 C54 C55 120.7(6) . . ?
C54 C55 C50 120.0(6) . . ?
C40 C56 C59' 115.1(9) . . ?
C40 C56 C58' 107.0(9) . . ?
C59' C56 C58' 111.2(6) . . ?
C40 C56 C59 115.4(7) . . ?
C59' C56 C59 129.2(10) . . ?
C58' C56 C59 57.4(8) . . ?
C40 C56 C57 105.3(7) . . ?
C59' C56 C57 51.0(8) . . ?
C58' C56 C57 147.7(9) . . ?
C59 C56 C57 109.5 . . ?
C40 C56 C58 107.5(7) . . ?
C59' C56 C58 58.7(7) . . ?
C58' C56 C58 58.1(7) . . ?
C59 C56 C58 109.5 . . ?
C57 C56 C58 109.5 . . ?
C40 C56 C57' 103.6(10) . . ?
C59' C56 C57' 110.2(6) . . ?
C58' C56 C57' 109.4(6) . . ?
C59 C56 C57' 52.1(8) . . ?
C57 C56 C57' 64.3(8) . . ?
C58 C56 C57' 148.8(10) . . ?
C61' C60 C42 117.8(11) . . ?
C61' C60 C67 108.8(10) . . ?
C42 C60 C67 113.9(5) . . ?
C61' C60 C61 6.5(19) . . ?
C42 C60 C61 111.7(10) . . ?
C67 C60 C61 111.2(10) . . ?
C66 C61 C62 120.0 . . ?
C66 C61 C60 121.0(14) . . ?
C62 C61 C60 118.8(15) . . ?
C63 C62 C61 120.0 . . ?
C62 C63 C64 120.0 . . ?
C65 C64 C63 120.0 . . ?
C66 C65 C64 120.0 . . ?
C65 C66 C61 120.0 . . ?
C66' C61' C62' 120.0 . . ?
C66' C61' C60 116.8(15) . . ?
C62' C61' C60 123.0(15) . . ?
C63' C62' C61' 120.0 . . ?
C62' C63' C64' 120.0 . . ?
C65' C64' C63' 120.0 . . ?
C66' C65' C64' 120.0 . . ?
C65' C66' C61' 120.0 . . ?
C72 C67 C68 118.6(7) . . ?
C72 C67 C60 120.3(6) . . ?
C68 C67 C60 121.1(6) . . ?
C69 C68 C67 119.4(7) . . ?
C70 C69 C68 120.3(7) . . ?
C69 C70 C71 119.0(7) . . ?
C72 C71 C70 118.9(7) . . ?
C67 C72 C71 123.2(7) . . ?
O3 C73 C74 118.8(6) . . ?
O3 C73 C78 120.6(5) . . ?
C74 C73 C78 120.5(6) . . ?
C73 C74 C75 117.4(6) . . ?
C73 C74 C79 121.5(6) . . ?
C75 C74 C79 121.1(6) . . ?
C76 C75 C74 121.3(6) . . ?
C77 C76 C75 119.1(7) . . ?
C77 C76 C92 124.5(7) . . ?
C75 C76 C92 116.5(7) . . ?
C76 C77 C78 121.8(7) . . ?
C77 C78 C73 119.8(6) . . ?
C77 C78 C96 122.5(6) . . ?
C73 C78 C96 117.6(6) . . ?
C74 C79 C80 114.7(5) . . ?
C74 C79 C86 112.7(5) . . ?
C80 C79 C86 110.7(5) . . ?
C85 C80 C81 118.4(6) . . ?
C85 C80 C79 123.7(6) . . ?
C81 C80 C79 117.9(6) . . ?
C85 C80 K1 81.1(4) . . ?
C81 C80 K1 69.5(3) . . ?
C79 C80 K1 121.9(3) . . ?
C82 C81 C80 119.2(7) . . ?
C82 C81 K1 72.0(4) . . ?
C80 C81 K1 86.1(4) . . ?
C83 C82 C81 119.6(8) . . ?
C83 C82 K1 84.3(4) . . ?
C81 C82 K1 82.3(4) . . ?
C84 C83 C82 121.5(7) . . ?
C84 C83 K1 84.7(4) . . ?
C82 C83 K1 70.9(4) . . ?
C83 C84 C85 119.8(7) . . ?
C83 C84 K1 72.4(4) . . ?
C85 C84 K1 81.8(4) . . ?
C80 C85 C84 121.2(7) . . ?
C80 C85 K1 76.2(4) . . ?
C84 C85 K1 74.6(4) . . ?
C91 C86 C87 120.0(7) . . ?
C91 C86 C79 123.2(6) . . ?
C87 C86 C79 116.6(6) . . ?
C88 C87 C86 118.8(7) . . ?
C89 C88 C87 122.5(8) . . ?
C88 C89 C90 118.9(8) . . ?
C91 C90 C89 119.8(9) . . ?
C86 C91 C90 119.9(8) . . ?
C76 C92 C93 109.3(7) . . ?
C76 C92 C94 109.0(6) . . ?
C93 C92 C94 109.5 . . ?
C76 C92 C95 110.1(6) . . ?
C93 C92 C95 109.5 . . ?
C94 C92 C95 109.5 . . ?
C97 C96 C78 108.0(5) . . ?
C97 C96 C103 113.6(5) . . ?
C78 C96 C103 114.8(5) . . ?
C102 C97 C98 117.0(6) . . ?
C102 C97 C96 122.7(5) . . ?
C98 C97 C96 120.2(5) . . ?
C99 C98 C97 123.1(6) . . ?
C100 C99 C98 117.8(6) . . ?
C99 C100 C101 121.4(6) . . ?
C100 C101 C102 118.1(6) . . ?
C97 C102 C101 122.5(6) . . ?
C108 C103 C104 116.5(7) . . ?
C108 C103 C96 120.7(7) . . ?
C104 C103 C96 122.8(6) . . ?
C105 C104 C103 120.4(8) . . ?
C106 C105 C104 123.0(9) . . ?
C105 C106 C107 117.7(9) . . ?
C108 C107 C106 119.9(10) . . ?
C103 C108 C107 122.5(9) . . ?
O4 C109 C114 120.5(5) . . ?
O4 C109 C110 120.4(5) . . ?
C114 C109 C110 119.1(5) . . ?
C111 C110 C109 118.1(5) . . ?
C111 C110 C115 120.9(5) . . ?
C109 C110 C115 121.0(5) . . ?
C112 C111 C110 123.5(5) . . ?
C113 C112 C111 117.1(5) . . ?
C113 C112 C128 119.8(5) . . ?
C111 C112 C128 123.1(5) . . ?
C112 C113 C114 123.4(6) . . ?
C113 C114 C109 118.6(5) . . ?
C113 C114 C132 122.6(5) . . ?
C109 C114 C132 118.7(5) . . ?
C110 C115 C116 111.7(5) . . ?
C110 C115 C122 114.0(5) . . ?
C116 C115 C122 113.7(4) . . ?
C117 C116 C121 118.4(6) . . ?
C117 C116 C115 118.4(5) . . ?
C121 C116 C115 123.2(5) . . ?
C116 C117 C118 120.3(6) . . ?
C119 C118 C117 120.7(6) . . ?
C120 C119 C118 118.4(6) . . ?
C121 C120 C119 122.4(7) . . ?
C120 C121 C116 119.8(6) . . ?
C123 C122 C127 118.4(5) . . ?
C123 C122 C115 122.6(5) . . ?
C127 C122 C115 119.0(6) . . ?
C122 C123 C124 122.7(6) . . ?
C125 C124 C123 119.8(6) . . ?
C124 C125 C126 120.5(6) . . ?
C125 C126 C127 119.2(6) . . ?
C126 C127 C122 119.4(6) . . ?
C129 C128 C131 109.3(6) . . ?
C129 C128 C130 107.4(5) . . ?
C131 C128 C130 108.4(5) . . ?
C129 C128 C112 109.3(5) . . ?
C131 C128 C112 110.1(5) . . ?
C130 C128 C112 112.3(5) . . ?
C114 C132 C139 114.7(5) . . ?
C114 C132 C133 111.6(4) . . ?
C139 C132 C133 111.4(4) . . ?
C134 C133 C138 117.8(5) . . ?
C134 C133 C132 122.6(5) . . ?
C138 C133 C132 119.6(5) . . ?
C133 C134 C135 122.1(5) . . ?
C134 C135 C136 119.6(5) . . ?
C137 C136 C135 119.8(5) . . ?
C136 C137 C138 120.9(5) . . ?
C137 C138 C133 119.7(6) . . ?
C140 C139 C144 117.2(6) . . ?
C140 C139 C132 122.6(5) . . ?
C144 C139 C132 120.1(5) . . ?
C139 C140 C141 121.4(7) . . ?
C142 C141 C140 116.0(9) . . ?
C143 C142 C141 122.9(8) . . ?
C142 C143 C144 120.5(7) . . ?
C143 C144 C139 121.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.088

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 -0.002 0.000 20266 3248 ' '
2 0.501 -0.017 0.494 20266 3248 ' '
3 0.273 0.033 0.403 10 2 ' '
4 0.727 0.033 0.597 10 2 ' '
5 0.533 0.097 0.227 10 2 ' '
6 0.467 0.097 0.773 10 2 ' '
7 0.903 0.227 0.467 10 2 ' '
8 0.097 0.227 0.533 10 2 ' '
9 0.403 0.273 0.033 10 2 ' '
10 0.597 0.273 0.967 10 2 ' '
11 0.033 0.403 0.273 10 2 ' '
12 0.967 0.403 0.727 10 2 ' '
13 0.773 0.467 0.097 10 2 ' '
14 0.227 0.467 0.903 10 2 ' '
15 0.227 0.533 0.097 10 2 ' '
16 0.773 0.533 0.903 10 2 ' '
17 0.967 0.597 0.273 10 2 ' '
18 0.033 0.597 0.727 10 2 ' '
19 0.597 0.727 0.033 10 2 ' '
20 0.403 0.727 0.967 10 2 ' '
21 0.097 0.773 0.467 10 2 ' '
22 0.903 0.773 0.533 10 2 ' '
23 0.467 0.903 0.227 10 2 ' '
24 0.533 0.903 0.773 10 2 ' '
25 0.727 0.967 0.403 10 2 ' '
26 0.273 0.967 0.597 10 2 ' '
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1032676'
_audit_update_record             
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C149 H144 Cl5 K3 Nb2 O4'
_chemical_formula_weight         2479.01

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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1       '
_symmetry_Int_Tables_number      2

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

_cell_length_a                   16.7009(14)
_cell_length_b                   17.9962(15)
_cell_length_c                   24.535(2)
_cell_angle_alpha                92.288(4)
_cell_angle_beta                 100.453(4)
_cell_angle_gamma                114.629(4)
_cell_volume                     6536.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05

_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2588
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            161655
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.73
_reflns_number_total             30335
_reflns_number_gt                24323
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0652P)²+9.6351P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         30335
_refine_ls_number_parameters     1483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1301
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_special_details          
;
The data were corrected for the presence of disordered solvent using the
program SQUEEZE.
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.607266(14) 0.185441(13) 0.241935(9) 0.01373(5) Uani 1 1 d . . .
Nb2 Nb 0.702840(14) 0.346628(13) 0.276970(9) 0.01466(5) Uani 1 1 d . . .
K1 K 0.65913(5) 0.26659(4) 0.08407(3) 0.03092(14) Uani 1 1 d . . .
K2 K 0.83596(4) 0.56101(4) 0.33987(3) 0.02400(12) Uani 1 1 d . . .
K3 K 0.45879(4) 0.18728(4) 0.34779(2) 0.02526(13) Uani 1 1 d . . .
Cl1 Cl 0.52561(4) 0.15083(4) 0.14370(2) 0.01830(12) Uani 1 1 d . . .
Cl2 Cl 0.85693(4) 0.38868(4) 0.32798(3) 0.02090(12) Uani 1 1 d . . .
Cl3 Cl 0.74466(4) 0.27122(4) 0.20475(3) 0.02113(12) Uani 1 1 d . . .
Cl4 Cl 0.53418(4) 0.28711(4) 0.25120(2) 0.01729(11) Uani 1 1 d . . .
Cl5 Cl 0.65846(4) 0.23603(4) 0.34452(2) 0.01788(12) Uani 1 1 d . . .
O1 O 0.66527(12) 0.11050(11) 0.24492(7) 0.0179(3) Uani 1 1 d . . .
O2 O 0.48709(11) 0.10631(10) 0.26547(7) 0.0165(3) Uani 1 1 d . . .
O3 O 0.69672(12) 0.42805(11) 0.34014(7) 0.0183(4) Uani 1 1 d . . .
O4 O 0.72699(12) 0.43451(11) 0.22502(7) 0.0181(3) Uani 1 1 d . . .
C1 C 0.72827(17) 0.08598(15) 0.23486(10) 0.0173(5) Uani 1 1 d . . .
C2 C 0.80951(18) 0.10645(17) 0.27418(11) 0.0231(5) Uani 1 1 d . . .
C3 C 0.86624(19) 0.07090(19) 0.26392(12) 0.0266(6) Uani 1 1 d . . .
H3 H 0.9194 0.0841 0.2903 0.035 Uiso 1 1 calc R . .
C4 C 0.84736(19) 0.01676(18) 0.21639(12) 0.0256(6) Uani 1 1 d . . .
C5 C 0.76964(19) 0.00132(17) 0.17718(11) 0.0236(5) Uani 1 1 d . . .
H5 H 0.7558 -0.0336 0.1445 0.031 Uiso 1 1 calc R . .
C6 C 0.71130(17) 0.03605(16) 0.18480(11) 0.0188(5) Uani 1 1 d . . .
C7 C 0.83900(19) 0.1666(2) 0.32768(12) 0.0287(6) Uani 1 1 d . . .
H7 H 0.8071 0.2017 0.3216 0.038 Uiso 1 1 calc R . .
C8 C 0.8149(2) 0.1244(2) 0.37827(13) 0.0362(7) Uani 1 1 d . . .
C9 C 0.7876(2) 0.0404(3) 0.37915(14) 0.0436(9) Uani 1 1 d . . .
H9 H 0.7807 0.0078 0.3467 0.058 Uiso 1 1 calc R . .
C10 C 0.7703(3) 0.0035(3) 0.42732(16) 0.0563(11) Uani 1 1 d . . .
H10 H 0.7515 -0.0530 0.4269 0.075 Uiso 1 1 calc R . .
C11 C 0.7815(3) 0.0524(4) 0.47568(16) 0.0596(13) Uani 1 1 d . . .
H11 H 0.7707 0.0287 0.5082 0.079 Uiso 1 1 calc R . .
C12 C 0.8087(3) 0.1366(4) 0.47598(15) 0.0596(13) Uani 1 1 d . . .
H12 H 0.8165 0.1691 0.5087 0.079 Uiso 1 1 calc R . .
C13 C 0.8241(2) 0.1722(3) 0.42757(14) 0.0472(10) Uani 1 1 d . . .
H13 H 0.8408 0.2284 0.4278 0.063 Uiso 1 1 calc R . .
C14 C 0.9407(2) 0.2231(2) 0.33696(13) 0.0345(7) Uani 1 1 d . . .
C15 C 0.9705(2) 0.2802(2) 0.30071(15) 0.0388(8) Uani 1 1 d . . .
H15 H 0.9287 0.2854 0.2724 0.052 Uiso 1 1 calc R . .
C16 C 1.0617(2) 0.3300(2) 0.30574(18) 0.0489(9) Uani 1 1 d . . .
H16 H 1.0803 0.3680 0.2808 0.065 Uiso 1 1 calc R . .
C17 C 1.1247(2) 0.3235(3) 0.34731(19) 0.0564(11) Uani 1 1 d . . .
H17 H 1.1858 0.3574 0.3510 0.075 Uiso 1 1 calc R . .
C18 C 1.0963(2) 0.2663(3) 0.38332(17) 0.0604(12) Uani 1 1 d . . .
H18 H 1.1389 0.2610 0.4111 0.080 Uiso 1 1 calc R . .
C19 C 1.0046(2) 0.2156(3) 0.37915(15) 0.0476(9) Uani 1 1 d . . .
H19 H 0.9864 0.1775 0.4041 0.063 Uiso 1 1 calc R . .
C20 C 0.9095(2) -0.0237(2) 0.20776(14) 0.0356(7) Uani 1 1 d . . .
C21 C 0.8712(5) -0.1079(3) 0.2261(4) 0.113(3) Uani 1 1 d . . .
H21a H 0.9064 -0.1363 0.2187 0.170 Uiso 1 1 calc R . .
H21b H 0.8099 -0.1386 0.2060 0.170 Uiso 1 1 calc R . .
H21c H 0.8730 -0.1025 0.2655 0.170 Uiso 1 1 calc R . .
C22 C 1.0041(3) 0.0259(4) 0.2383(3) 0.113(3) Uani 1 1 d . . .
H22a H 1.0069 0.0293 0.2778 0.170 Uiso 1 1 calc R . .
H22b H 1.0257 0.0804 0.2275 0.170 Uiso 1 1 calc R . .
H22c H 1.0411 0.0003 0.2293 0.170 Uiso 1 1 calc R . .
C23 C 0.9096(5) -0.0373(5) 0.1467(2) 0.116(3) Uani 1 1 d . . .
H23a H 0.9235 0.0136 0.1312 0.174 Uiso 1 1 calc R . .
H23b H 0.8512 -0.0777 0.1271 0.174 Uiso 1 1 calc R . .
H23c H 0.9543 -0.0566 0.1429 0.174 Uiso 1 1 calc R . .
C24 C 0.63542(17) 0.02597(16) 0.13624(10) 0.0181(5) Uani 1 1 d . . .
H24 H 0.5964 0.0461 0.1511 0.024 Uiso 1 1 calc R . .
C25 C 0.57751(17) -0.06417(16) 0.11285(11) 0.0192(5) Uani 1 1 d . . .
C26 C 0.50968(19) -0.1113(2) 0.13929(12) 0.0290(6) Uani 1 1 d . . .
H26 H 0.4991 -0.0867 0.1695 0.039 Uiso 1 1 calc R . .
C27 C 0.4577(2) -0.1946(2) 0.12113(15) 0.0376(8) Uani 1 1 d . . .
H27 H 0.4129 -0.2254 0.1395 0.050 Uiso 1 1 calc R . .
C28 C 0.4718(2) -0.23215(19) 0.07626(16) 0.0390(8) Uani 1 1 d . . .
H28 H 0.4370 -0.2882 0.0645 0.052 Uiso 1 1 calc R . .
C29 C 0.5378(2) -0.18627(19) 0.04871(15) 0.0362(7) Uani 1 1 d . . .
H29 H 0.5471 -0.2111 0.0180 0.048 Uiso 1 1 calc R . .
C30 C 0.59036(19) -0.10283(17) 0.06720(12) 0.0256(6) Uani 1 1 d . . .
H30 H 0.6350 -0.0723 0.0487 0.034 Uiso 1 1 calc R . .
C31 C 0.67167(18) 0.08000(16) 0.09159(11) 0.0211(5) Uani 1 1 d . . .
C32 C 0.6106(2) 0.07428(17) 0.04206(11) 0.0260(6) Uani 1 1 d . . .
H32 H 0.5495 0.0399 0.0379 0.035 Uiso 1 1 calc R . .
C33 C 0.6404(2) 0.11931(18) -0.00077(12) 0.0309(6) Uani 1 1 d . . .
H33 H 0.5996 0.1135 -0.0338 0.041 Uiso 1 1 calc R . .
C34 C 0.7307(2) 0.17275(18) 0.00555(12) 0.0316(7) Uani 1 1 d . . .
H34 H 0.7508 0.2022 -0.0234 0.042 Uiso 1 1 calc R . .
C35 C 0.7907(2) 0.18215(18) 0.05512(13) 0.0301(6) Uani 1 1 d . . .
H35 H 0.8509 0.2195 0.0600 0.040 Uiso 1 1 calc R . .
C36 C 0.76131(19) 0.13568(17) 0.09796(11) 0.0247(6) Uani 1 1 d . . .
H36 H 0.8023 0.1422 0.1310 0.033 Uiso 1 1 calc R . .
C37 C 0.43199(16) 0.02703(15) 0.24585(10) 0.0156(5) Uani 1 1 d . . .
C38 C 0.44919(17) -0.03635(16) 0.26972(10) 0.0183(5) Uani 1 1 d . . .
C39 C 0.38863(18) -0.11848(16) 0.25120(11) 0.0205(5) Uani 1 1 d . . .
H39 H 0.4017 -0.1597 0.2664 0.027 Uiso 1 1 calc R . .
C40 C 0.30966(17) -0.14100(16) 0.21106(11) 0.0201(5) Uani 1 1 d . . .
C41 C 0.29281(17) -0.07731(16) 0.18885(11) 0.0197(5) Uani 1 1 d . . .
H41 H 0.2402 -0.0908 0.1620 0.026 Uiso 1 1 calc R . .
C42 C 0.35142(17) 0.00520(15) 0.20527(10) 0.0167(5) Uani 1 1 d . . .
C43 C 0.52194(18) -0.01406(16) 0.32256(10) 0.0197(5) Uani 1 1 d . . .
H43 H 0.5753 0.0339 0.3176 0.026 Uiso 1 1 calc R . .
C44 C 0.48866(19) 0.01076(16) 0.37129(11) 0.0220(5) Uani 1 1 d . . .
C45 C 0.5495(2) 0.06681(18) 0.41646(12) 0.0281(6) Uani 1 1 d . . .
H45 H 0.6110 0.0892 0.4172 0.037 Uiso 1 1 calc R . .
C46 C 0.5196(2) 0.08997(19) 0.46070(13) 0.0358(7) Uani 1 1 d . . .
H46 H 0.5611 0.1280 0.4905 0.048 Uiso 1 1 calc R . .
C47 C 0.4287(2) 0.0568(2) 0.46064(13) 0.0352(7) Uani 1 1 d . . .
H47 H 0.4090 0.0721 0.4904 0.047 Uiso 1 1 calc R . .
C48 C 0.3674(2) 0.0009(2) 0.41616(13) 0.0355(7) Uani 1 1 d . . .
H48 H 0.3061 -0.0214 0.4158 0.047 Uiso 1 1 calc R . .
C49 C 0.3970(2) -0.0222(2) 0.37185(12) 0.0298(6) Uani 1 1 d . . .
H49 H 0.3551 -0.0602 0.3421 0.040 Uiso 1 1 calc R . .
C50 C 0.54847(18) -0.08464(17) 0.33248(11) 0.0231(5) Uani 1 1 d . . .
C51 C 0.5206(2) -0.13710(19) 0.37212(13) 0.0314(6) Uani 1 1 d . . .
H51 H 0.4881 -0.1272 0.3962 0.042 Uiso 1 1 calc R . .
C52 C 0.5410(2) -0.2044(2) 0.37597(16) 0.0423(8) Uani 1 1 d . . .
H52 H 0.5213 -0.2396 0.4024 0.056 Uiso 1 1 calc R . .
C53 C 0.5900(3) -0.2196(2) 0.34121(17) 0.0457(9) Uani 1 1 d . . .
H53 H 0.6040 -0.2643 0.3443 0.061 Uiso 1 1 calc R . .
C54 C 0.6183(2) -0.1675(2) 0.30163(15) 0.0381(7) Uani 1 1 d . . .
H54 H 0.6512 -0.1775 0.2778 0.051 Uiso 1 1 calc R . .
C55 C 0.5979(2) -0.10046(18) 0.29744(13) 0.0279(6) Uani 1 1 d . . .
H55 H 0.6174 -0.0656 0.2708 0.037 Uiso 1 1 calc R . .
C56 C 0.23718(18) -0.23023(16) 0.19771(11) 0.0235(5) Uani 1 1 d . . .
C57 C 0.1605(2) -0.23549(19) 0.22544(14) 0.0352(7) Uani 1 1 d . . .
H57a H 0.1141 -0.2910 0.2184 0.053 Uiso 1 1 calc R . .
H57b H 0.1361 -0.1990 0.2104 0.053 Uiso 1 1 calc R . .
H57c H 0.1833 -0.2197 0.2650 0.053 Uiso 1 1 calc R . .
C58 C 0.2721(2) -0.29124(17) 0.22084(13) 0.0307(6) Uani 1 1 d . . .
H58a H 0.2244 -0.3461 0.2120 0.046 Uiso 1 1 calc R . .
H58b H 0.2927 -0.2779 0.2607 0.046 Uiso 1 1 calc R . .
H58c H 0.3213 -0.2881 0.2044 0.046 Uiso 1 1 calc R . .
C59 C 0.2011(2) -0.25464(18) 0.13473(12) 0.0288(6) Uani 1 1 d . . .
H59a H 0.2488 -0.2528 0.1174 0.043 Uiso 1 1 calc R . .
H59b H 0.1784 -0.2169 0.1197 0.043 Uiso 1 1 calc R . .
H59c H 0.1532 -0.3095 0.1275 0.043 Uiso 1 1 calc R . .
C60 C 0.32441(17) 0.07295(15) 0.18761(10) 0.0178(5) Uani 1 1 d . . .
H60 H 0.3794 0.1194 0.1830 0.024 Uiso 1 1 calc R . .
C61 C 0.25782(17) 0.04785(16) 0.13122(11) 0.0196(5) Uani 1 1 d . . .
C62 C 0.28416(19) 0.02690(17) 0.08411(11) 0.0243(5) Uani 1 1 d . . .
H62 H 0.3410 0.0277 0.0881 0.032 Uiso 1 1 calc R . .
C63 C 0.2273(2) 0.00500(18) 0.03179(12) 0.0282(6) Uani 1 1 d . . .
H63 H 0.2463 -0.0085 0.0010 0.037 Uiso 1 1 calc R . .
C64 C 0.1423(2) 0.0030(2) 0.02495(13) 0.0352(7) Uani 1 1 d . . .
H64 H 0.1044 -0.0108 -0.0103 0.047 Uiso 1 1 calc R . .
C65 C 0.1144(2) 0.0218(2) 0.07126(14) 0.0407(8) Uani 1 1 d . . .
H65 H 0.0570 0.0196 0.0673 0.054 Uiso 1 1 calc R . .
C66 C 0.1721(2) 0.0439(2) 0.12381(12) 0.0308(6) Uani 1 1 d . . .
H66 H 0.1525 0.0563 0.1546 0.041 Uiso 1 1 calc R . .
C67 C 0.29141(17) 0.10341(17) 0.23409(11) 0.0211(5) Uani 1 1 d . . .
C68 C 0.25559(19) 0.05448(18) 0.27364(12) 0.0259(6) Uani 1 1 d . . .
H68 H 0.2508 0.0010 0.2721 0.034 Uiso 1 1 calc R . .
C69 C 0.2266(2) 0.0844(2) 0.31580(13) 0.0320(7) Uani 1 1 d . . .
H69 H 0.2026 0.0509 0.3421 0.043 Uiso 1 1 calc R . .
C70 C 0.2334(2) 0.1637(2) 0.31850(13) 0.0346(7) Uani 1 1 d . . .
H70 H 0.2142 0.1837 0.3466 0.046 Uiso 1 1 calc R . .
C71 C 0.2689(2) 0.21294(19) 0.27943(14) 0.0330(7) Uani 1 1 d . . .
H71 H 0.2735 0.2663 0.2811 0.044 Uiso 1 1 calc R . .
C72 C 0.29805(19) 0.18346(18) 0.23751(12) 0.0267(6) Uani 1 1 d . . .
H72 H 0.3222 0.2174 0.2114 0.036 Uiso 1 1 calc R . .
C73 C 0.63806(17) 0.41441(15) 0.37336(10) 0.0169(5) Uani 1 1 d . . .
C74 C 0.56185(17) 0.42998(15) 0.35713(10) 0.0171(5) Uani 1 1 d . . .
C75 C 0.49544(17) 0.40677(16) 0.38861(10) 0.0188(5) Uani 1 1 d . . .
H75 H 0.4438 0.4146 0.3764 0.025 Uiso 1 1 calc R . .
C76 C 0.50466(18) 0.37221(16) 0.43784(10) 0.0205(5) Uani 1 1 d . . .
C77 C 0.58675(18) 0.36816(17) 0.45679(10) 0.0213(5) Uani 1 1 d . . .
H77 H 0.5961 0.3491 0.4910 0.028 Uiso 1 1 calc R . .
C78 C 0.65497(17) 0.39109(16) 0.42716(10) 0.0200(5) Uani 1 1 d . . .
C79 C 0.56110(17) 0.48028(16) 0.30872(10) 0.0183(5) Uani 1 1 d . . .
H79 H 0.5722 0.4533 0.2773 0.024 Uiso 1 1 calc R . .
C80 C 0.47126(18) 0.48343(17) 0.28892(11) 0.0226(5) Uani 1 1 d . . .
C81 C 0.4043(2) 0.42210(19) 0.24902(14) 0.0359(7) Uani 1 1 d . . .
H81 H 0.4153 0.3801 0.2337 0.048 Uiso 1 1 calc R . .
C82 C 0.3201(2) 0.4228(2) 0.23165(17) 0.0464(9) Uani 1 1 d . . .
H82 H 0.2755 0.3813 0.2049 0.062 Uiso 1 1 calc R . .
C83 C 0.3030(2) 0.4846(2) 0.25388(17) 0.0470(9) Uani 1 1 d . . .
H83 H 0.2469 0.4848 0.2424 0.063 Uiso 1 1 calc R . .
C84 C 0.3693(2) 0.5459(2) 0.29322(15) 0.0419(8) Uani 1 1 d . . .
H84 H 0.3580 0.5880 0.3082 0.056 Uiso 1 1 calc R . .
C85 C 0.4524(2) 0.5456(2) 0.31072(13) 0.0321(7) Uani 1 1 d . . .
H85 H 0.4965 0.5875 0.3375 0.043 Uiso 1 1 calc R . .
C86 C 0.63915(17) 0.56698(16) 0.32450(11) 0.0208(5) Uani 1 1 d . . .
C87 C 0.67806(19) 0.61024(18) 0.28323(12) 0.0267(6) Uani 1 1 d . . .
H87 H 0.6576 0.5855 0.2463 0.036 Uiso 1 1 calc R . .
C88 C 0.7468(2) 0.68954(19) 0.29620(13) 0.0315(6) Uani 1 1 d . . .
H88 H 0.7719 0.7173 0.2679 0.042 Uiso 1 1 calc R . .
C89 C 0.7782(2) 0.72770(19) 0.35065(14) 0.0344(7) Uani 1 1 d . . .
H89 H 0.8242 0.7810 0.3593 0.046 Uiso 1 1 calc R . .
C90 C 0.7404(2) 0.68577(19) 0.39215(13) 0.0331(7) Uani 1 1 d . . .
H90 H 0.7607 0.7111 0.4290 0.044 Uiso 1 1 calc R . .
C91 C 0.67172(19) 0.60552(17) 0.37923(11) 0.0251(6) Uani 1 1 d . . .
H91 H 0.6475 0.5776 0.4077 0.033 Uiso 1 1 calc R . .
C92 C 0.43216(18) 0.34149(17) 0.47224(11) 0.0216(5) Uani 1 1 d . . .
C93 C 0.35237(19) 0.3607(2) 0.44991(12) 0.0289(6) Uani 1 1 d . . .
H93a H 0.3733 0.4192 0.4502 0.043 Uiso 1 1 calc R . .
H93b H 0.3092 0.3413 0.4731 0.043 Uiso 1 1 calc R . .
H93c H 0.3245 0.3338 0.4124 0.043 Uiso 1 1 calc R . .
C94 C 0.4720(2) 0.38134(18) 0.53320(11) 0.0264(6) Uani 1 1 d . . .
H94a H 0.4903 0.4397 0.5351 0.040 Uiso 1 1 calc R . .
H94b H 0.5235 0.3712 0.5477 0.040 Uiso 1 1 calc R . .
H94c H 0.4273 0.3581 0.5550 0.040 Uiso 1 1 calc R . .
C95 C 0.3968(2) 0.24735(18) 0.47076(13) 0.0303(6) Uani 1 1 d . . .
H95a H 0.3553 0.2283 0.4951 0.045 Uiso 1 1 calc R . .
H95b H 0.4465 0.2339 0.4830 0.045 Uiso 1 1 calc R . .
H95c H 0.3665 0.2212 0.4333 0.045 Uiso 1 1 calc R . .
C96 C 0.74873(18) 0.39723(18) 0.45248(11) 0.0227(5) Uani 1 1 d . . .
H96 H 0.7618 0.3627 0.4269 0.030 Uiso 1 1 calc R . .
C97 C 0.75030(19) 0.3630(2) 0.50885(11) 0.0299(7) Uani 1 1 d . . .
C98 C 0.7699(2) 0.4131(3) 0.55893(13) 0.0451(9) Uani 1 1 d . . .
H98 H 0.7883 0.4695 0.5592 0.060 Uiso 1 1 calc R . .
C99 C 0.7616(3) 0.3782(4) 0.60838(14) 0.0613(13) Uani 1 1 d . . .
H99 H 0.7741 0.4116 0.6416 0.082 Uiso 1 1 calc R . .
C100 C 0.7352(3) 0.2948(4) 0.60870(15) 0.0628(14) Uani 1 1 d . . .
H100 H 0.7286 0.2720 0.6419 0.084 Uiso 1 1 calc R . .
C101 C 0.7186(2) 0.2457(3) 0.55999(16) 0.0516(10) Uani 1 1 d . . .
H101 H 0.7024 0.1896 0.5602 0.069 Uiso 1 1 calc R . .
C102 C 0.7263(2) 0.2802(2) 0.50988(13) 0.0364(7) Uani 1 1 d . . .
H102 H 0.7150 0.2466 0.4769 0.048 Uiso 1 1 calc R . .
C103 C 0.8225(2) 0.48455(18) 0.45847(11) 0.0271(6) Uani 1 1 d . . .
C104 C 0.8104(2) 0.5539(2) 0.47315(15) 0.0417(8) Uani 1 1 d . . .
H104 H 0.7543 0.5479 0.4783 0.055 Uiso 1 1 calc R . .
C105 C 0.8815(3) 0.6324(2) 0.48020(18) 0.0568(11) Uani 1 1 d . . .
H105 H 0.8724 0.6782 0.4904 0.076 Uiso 1 1 calc R . .
C106 C 0.9646(3) 0.6431(2) 0.47227(17) 0.0536(11) Uani 1 1 d . . .
H106 H 1.0112 0.6959 0.4766 0.071 Uiso 1 1 calc R . .
C107 C 0.9786(2) 0.5759(2) 0.45799(14) 0.0417(8) Uani 1 1 d . . .
H107 H 1.0350 0.5828 0.4528 0.055 Uiso 1 1 calc R . .
C108 C 0.9080(2) 0.4970(2) 0.45125(12) 0.0294(6) Uani 1 1 d . . .
H108 H 0.9182 0.4517 0.4417 0.039 Uiso 1 1 calc R . .
C109 C 0.73790(18) 0.44177(15) 0.17186(10) 0.0186(5) Uani 1 1 d . . .
C110 C 0.82259(18) 0.45552(16) 0.15936(11) 0.0204(5) Uani 1 1 d . . .
C111 C 0.83340(19) 0.46279(16) 0.10489(11) 0.0229(5) Uani 1 1 d . . .
H111 H 0.8885 0.4699 0.0973 0.030 Uiso 1 1 calc R . .
C112 C 0.76592(19) 0.46000(16) 0.06090(11) 0.0230(5) Uani 1 1 d . . .
C113 C 0.68515(19) 0.44987(16) 0.07416(11) 0.0225(5) Uani 1 1 d . . .
H113 H 0.6391 0.4485 0.0458 0.030 Uiso 1 1 calc R . .
C114 C 0.66962(18) 0.44161(16) 0.12856(11) 0.0209(5) Uani 1 1 d . . .
C115 C 0.90252(18) 0.46874(16) 0.20620(11) 0.0213(5) Uani 1 1 d . . .
H115 H 0.8791 0.4281 0.2315 0.028 Uiso 1 1 calc R . .
C116 C 0.97356(18) 0.45063(17) 0.18482(11) 0.0228(5) Uani 1 1 d . . .
C117 C 1.05055(19) 0.51183(18) 0.17353(12) 0.0265(6) Uani 1 1 d . . .
H117 H 1.0612 0.5668 0.1800 0.035 Uiso 1 1 calc R . .
C118 C 1.1119(2) 0.49204(19) 0.15260(12) 0.0288(6) Uani 1 1 d . . .
H118 H 1.1635 0.5339 0.1454 0.038 Uiso 1 1 calc R . .
C119 C 1.0975(2) 0.41115(19) 0.14241(12) 0.0295(6) Uani 1 1 d . . .
H119 H 1.1390 0.3982 0.1284 0.039 Uiso 1 1 calc R . .
C120 C 1.0208(2) 0.34941(19) 0.15319(14) 0.0356(7) Uani 1 1 d . . .
H120 H 1.0105 0.2946 0.1468 0.047 Uiso 1 1 calc R . .
C121 C 0.9591(2) 0.36922(18) 0.17357(14) 0.0326(7) Uani 1 1 d . . .
H121 H 0.9069 0.3271 0.1798 0.043 Uiso 1 1 calc R . .
C122 C 0.94130(18) 0.55353(17) 0.24068(11) 0.0235(5) Uani 1 1 d . . .
C123 C 1.00396(19) 0.56937(19) 0.29082(12) 0.0280(6) Uani 1 1 d . . .
H123 H 1.0234 0.5296 0.3016 0.037 Uiso 1 1 calc R . .
C124 C 1.0375(2) 0.6441(2) 0.32478(13) 0.0347(7) Uani 1 1 d . . .
H124 H 1.0791 0.6540 0.3582 0.046 Uiso 1 1 calc R . .
C125 C 1.0093(2) 0.7039(2) 0.30913(15) 0.0373(8) Uani 1 1 d . . .
H125 H 1.0314 0.7536 0.3321 0.050 Uiso 1 1 calc R . .
C126 C 0.9483(2) 0.68934(19) 0.25935(15) 0.0351(7) Uani 1 1 d . . .
H126 H 0.9294 0.7295 0.2486 0.047 Uiso 1 1 calc R . .
C127 C 0.91495(19) 0.61476(17) 0.22528(13) 0.0276(6) Uani 1 1 d . . .
H127 H 0.8743 0.6057 0.1916 0.037 Uiso 1 1 calc R . .
C128 C 0.7852(2) 0.47078(17) 0.00226(11) 0.0273(6) Uani 1 1 d . . .
C129 C 0.8755(3) 0.5465(2) 0.00613(14) 0.0433(9) Uani 1 1 d . . .
H129a H 0.8875 0.5539 -0.0306 0.065 Uiso 1 1 calc R . .
H129b H 0.9231 0.5382 0.0294 0.065 Uiso 1 1 calc R . .
H129c H 0.8723 0.5946 0.0219 0.065 Uiso 1 1 calc R . .
C130 C 0.7931(3) 0.3943(2) -0.02079(13) 0.0385(8) Uani 1 1 d . . .
H130a H 0.7359 0.3472 -0.0259 0.058 Uiso 1 1 calc R . .
H130b H 0.8377 0.3853 0.0051 0.058 Uiso 1 1 calc R . .
H130c H 0.8108 0.4026 -0.0560 0.058 Uiso 1 1 calc R . .
C131 C 0.7120(2) 0.4833(2) -0.03790(12) 0.0356(7) Uani 1 1 d . . .
H131a H 0.6555 0.4357 -0.0419 0.053 Uiso 1 1 calc R . .
H131b H 0.7277 0.4911 -0.0737 0.053 Uiso 1 1 calc R . .
H131c H 0.7068 0.5310 -0.0234 0.053 Uiso 1 1 calc R . .
C132 C 0.58443(18) 0.44462(17) 0.13964(11) 0.0223(5) Uani 1 1 d . . .
H132 H 0.5775 0.4263 0.1763 0.030 Uiso 1 1 calc R . .
C133 C 0.49971(19) 0.38690(18) 0.09732(11) 0.0236(5) Uani 1 1 d . . .
C134 C 0.4524(2) 0.30574(18) 0.10591(12) 0.0280(6) Uani 1 1 d . . .
H134 H 0.4726 0.2871 0.1380 0.037 Uiso 1 1 calc R . .
C135 C 0.3755(2) 0.2518(2) 0.06766(14) 0.0353(7) Uani 1 1 d . . .
H135 H 0.3444 0.1978 0.0745 0.047 Uiso 1 1 calc R . .
C136 C 0.3448(2) 0.2782(2) 0.01920(13) 0.0348(7) Uani 1 1 d . . .
H136 H 0.2934 0.2421 -0.0066 0.046 Uiso 1 1 calc R . .
C137 C 0.3914(2) 0.3588(2) 0.00966(13) 0.0335(7) Uani 1 1 d . . .
H137 H 0.3716 0.3768 -0.0229 0.045 Uiso 1 1 calc R . .
C138 C 0.4673(2) 0.4126(2) 0.04848(12) 0.0309(6) Uani 1 1 d . . .
H138 H 0.4973 0.4669 0.0420 0.041 Uiso 1 1 calc R . .
C139 C 0.5943(2) 0.53379(19) 0.14342(11) 0.0269(6) Uani 1 1 d . . .
C140 C 0.5226(2) 0.5489(2) 0.15388(13) 0.0353(7) Uani 1 1 d . . .
H140 H 0.4689 0.5050 0.1564 0.047 Uiso 1 1 calc R . .
C141 C 0.5308(3) 0.6291(2) 0.16057(15) 0.0448(9) Uani 1 1 d . . .
H141 H 0.4830 0.6386 0.1680 0.060 Uiso 1 1 calc R . .
C142 C 0.6094(3) 0.6945(2) 0.15621(14) 0.0450(9) Uani 1 1 d . . .
H142 H 0.6146 0.7480 0.1608 0.060 Uiso 1 1 calc R . .
C143 C 0.6800(3) 0.6808(2) 0.14512(13) 0.0381(7) Uani 1 1 d . . .
H143 H 0.7329 0.7249 0.1418 0.051 Uiso 1 1 calc R . .
C144 C 0.6726(2) 0.60058(18) 0.13882(12) 0.0301(6) Uani 1 1 d . . .
H144 H 0.7209 0.5918 0.1314 0.040 Uiso 1 1 calc R . .
C145 C 0.0523(5) 0.2410(5) -0.1102(3) 0.105(2) Uani 1 1 d . . .
H145a H 0.1000 0.2957 -0.1051 0.158 Uiso 1 1 calc R . .
H145b H 0.0034 0.2366 -0.1397 0.158 Uiso 1 1 calc R . .
H145c H 0.0744 0.2019 -0.1200 0.158 Uiso 1 1 calc R . .
C146 C 0.0190(4) 0.2230(3) -0.0564(2) 0.0717(14) Uani 1 1 d . . .
H146a H -0.0032 0.2626 -0.0467 0.095 Uiso 1 1 calc R . .
H146b H -0.0309 0.1685 -0.0623 0.095 Uiso 1 1 calc R . .
C147 C 0.0918(4) 0.2269(3) -0.0084(2) 0.0661(13) Uani 1 1 d . . .
H147a H 0.1453 0.2778 -0.0068 0.088 Uiso 1 1 calc R . .
H147b H 0.1070 0.1816 -0.0159 0.088 Uiso 1 1 calc R . .
C148 C 0.0669(4) 0.2230(3) 0.0478(2) 0.0660(12) Uani 1 1 d . . .
H148a H 0.0186 0.1692 0.0480 0.088 Uiso 1 1 calc R . .
H148b H 0.0446 0.2640 0.0535 0.088 Uiso 1 1 calc R . .
C149 C 0.1470(4) 0.2383(3) 0.0964(2) 0.0750(14) Uani 1 1 d . . .
H149a H 0.1706 0.1990 0.0904 0.112 Uiso 1 1 calc R . .
H149b H 0.1269 0.2322 0.1309 0.112 Uiso 1 1 calc R . .
H149c H 0.1934 0.2930 0.0982 0.112 Uiso 1 1 calc R . .


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 1.9580(17) . ?
Nb1 O2 2.1199(17) . ?
Nb1 Cl1 2.4569(6) . ?
Nb1 Cl5 2.5065(6) . ?
Nb1 Cl3 2.5298(7) . ?
Nb1 Cl4 2.6110(6) . ?
Nb2 O4 2.0259(17) . ?
Nb2 O3 2.1356(17) . ?
Nb2 Cl2 2.4278(7) . ?
Nb2 Cl4 2.5032(7) . ?
Nb2 Cl3 2.5527(6) . ?
Nb2 Cl5 2.5956(6) . ?
Nb2 K2 3.6523(7) . ?
K1 Cl1 3.0013(9) . ?
K1 Cl3 3.0267(9) . ?
K1 C31 3.460(3) . ?
K1 C110 3.515(3) . ?
K2 O3 2.5498(19) . ?
K2 O4 3.2572(18) . ?
K2 Cl2 3.2705(9) . ?
K2 C107 3.324(3) . ?
K2 C127 3.329(3) . ?
K2 C88 3.348(3) . ?
K2 C104 3.374(4) . ?
K2 C106 3.434(4) . ?
K2 C91 3.439(3) . ?
K2 C105 3.459(4) . ?
K2 C73 3.528(3) . ?
K2 C89 3.527(3) . ?
K3 O2 2.6664(18) . ?
K3 Cl5 3.0918(9) . ?
K3 Cl4 3.1570(9) . ?
O1 C1 1.355(3) . ?
O2 C37 1.343(3) . ?
O3 C73 1.338(3) . ?
O4 C109 1.353(3) . ?
C1 C6 1.403(3) . ?
C1 C2 1.410(4) . ?
C2 C3 1.396(4) . ?
C2 C7 1.532(4) . ?
C3 C4 1.389(4) . ?
C4 C5 1.383(4) . ?
C4 C20 1.533(4) . ?
C5 C6 1.392(4) . ?
C6 C24 1.517(3) . ?
C7 C8 1.511(5) . ?
C7 C14 1.540(4) . ?
C8 C9 1.386(5) . ?
C8 C13 1.403(5) . ?
C9 C10 1.396(5) . ?
C10 C11 1.385(6) . ?
C11 C12 1.387(7) . ?
C12 C13 1.387(6) . ?
C14 C15 1.379(5) . ?
C14 C19 1.400(5) . ?
C15 C16 1.387(5) . ?
C16 C17 1.372(6) . ?
C17 C18 1.373(7) . ?
C18 C19 1.400(5) . ?
C20 C22 1.482(6) . ?
C20 C21 1.502(6) . ?
C20 C23 1.510(6) . ?
C24 C25 1.521(4) . ?
C24 C31 1.532(4) . ?
C25 C26 1.391(4) . ?
C25 C30 1.391(4) . ?
C26 C27 1.386(5) . ?
C27 C28 1.375(5) . ?
C28 C29 1.383(5) . ?
C29 C30 1.391(4) . ?
C31 C36 1.386(4) . ?
C31 C32 1.407(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.384(5) . ?
C34 C35 1.383(4) . ?
C35 C36 1.400(4) . ?
C37 C38 1.411(3) . ?
C37 C42 1.414(3) . ?
C38 C39 1.396(4) . ?
C38 C43 1.516(3) . ?
C39 C40 1.387(4) . ?
C40 C41 1.397(4) . ?
C40 C56 1.531(4) . ?
C41 C42 1.387(4) . ?
C42 C60 1.519(3) . ?
C43 C50 1.524(4) . ?
C43 C44 1.531(4) . ?
C44 C45 1.388(4) . ?
C44 C49 1.395(4) . ?
C45 C46 1.391(4) . ?
C46 C47 1.380(5) . ?
C47 C48 1.378(5) . ?
C48 C49 1.389(4) . ?
C50 C51 1.387(4) . ?
C50 C55 1.391(4) . ?
C51 C52 1.391(4) . ?
C52 C53 1.375(5) . ?
C53 C54 1.383(5) . ?
C54 C55 1.388(4) . ?
C56 C58 1.527(4) . ?
C56 C57 1.527(4) . ?
C56 C59 1.527(4) . ?
C60 C61 1.526(3) . ?
C60 C67 1.528(4) . ?
C61 C66 1.381(4) . ?
C61 C62 1.400(4) . ?
C62 C63 1.382(4) . ?
C63 C64 1.384(4) . ?
C64 C65 1.384(5) . ?
C65 C66 1.392(4) . ?
C67 C68 1.384(4) . ?
C67 C72 1.396(4) . ?
C68 C69 1.396(4) . ?
C69 C70 1.381(5) . ?
C70 C71 1.375(5) . ?
C71 C72 1.389(4) . ?
C73 C74 1.407(3) . ?
C73 C78 1.416(3) . ?
C74 C75 1.397(4) . ?
C74 C79 1.523(3) . ?
C75 C76 1.394(4) . ?
C76 C77 1.398(4) . ?
C76 C92 1.528(4) . ?
C77 C78 1.389(4) . ?
C78 C96 1.532(4) . ?
C79 C80 1.516(4) . ?
C79 C86 1.535(4) . ?
C80 C81 1.384(4) . ?
C80 C85 1.394(4) . ?
C81 C82 1.398(5) . ?
C82 C83 1.374(6) . ?
C83 C84 1.373(5) . ?
C84 C85 1.379(4) . ?
C86 C91 1.388(4) . ?
C86 C87 1.391(4) . ?
C87 C88 1.386(4) . ?
C88 C89 1.380(5) . ?
C89 C90 1.379(5) . ?
C90 C91 1.397(4) . ?
C92 C93 1.527(4) . ?
C92 C94 1.533(4) . ?
C92 C95 1.541(4) . ?
C96 C103 1.520(4) . ?
C96 C97 1.536(4) . ?
C97 C102 1.376(5) . ?
C97 C98 1.396(4) . ?
C98 C99 1.390(5) . ?
C99 C100 1.377(7) . ?
C100 C101 1.370(7) . ?
C101 C102 1.401(4) . ?
C103 C104 1.389(4) . ?
C103 C108 1.396(4) . ?
C104 C105 1.394(5) . ?
C105 C106 1.371(6) . ?
C106 C107 1.368(6) . ?
C107 C108 1.396(5) . ?
C109 C114 1.409(4) . ?
C109 C110 1.424(4) . ?
C110 C111 1.385(4) . ?
C110 C115 1.522(4) . ?
C111 C112 1.394(4) . ?
C112 C113 1.385(4) . ?
C112 C128 1.533(4) . ?
C113 C114 1.407(4) . ?
C114 C132 1.518(4) . ?
C115 C116 1.524(4) . ?
C115 C122 1.529(4) . ?
C116 C117 1.384(4) . ?
C116 C121 1.389(4) . ?
C117 C118 1.387(4) . ?
C118 C119 1.377(4) . ?
C119 C120 1.381(4) . ?
C120 C121 1.384(4) . ?
C122 C127 1.388(4) . ?
C122 C123 1.395(4) . ?
C123 C124 1.389(4) . ?
C124 C125 1.384(5) . ?
C125 C126 1.378(5) . ?
C126 C127 1.389(4) . ?
C128 C131 1.525(4) . ?
C128 C130 1.531(4) . ?
C128 C129 1.538(4) . ?
C132 C133 1.521(4) . ?
C132 C139 1.540(4) . ?
C133 C134 1.388(4) . ?
C133 C138 1.400(4) . ?
C134 C135 1.387(4) . ?
C135 C136 1.389(4) . ?
C136 C137 1.383(5) . ?
C137 C138 1.385(4) . ?
C139 C144 1.386(4) . ?
C139 C140 1.397(4) . ?
C140 C141 1.393(5) . ?
C141 C142 1.375(6) . ?
C142 C143 1.371(5) . ?
C143 C144 1.396(4) . ?
C145 C146 1.520(8) . ?
C146 C147 1.506(7) . ?
C147 C148 1.507(7) . ?
C148 C149 1.542(7) . ?

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 O2 97.95(7) . . ?
O1 Nb1 Cl1 100.29(5) . . ?
O2 Nb1 Cl1 89.51(5) . . ?
O1 Nb1 Cl5 94.95(5) . . ?
O2 Nb1 Cl5 82.87(5) . . ?
Cl1 Nb1 Cl5 163.79(2) . . ?
O1 Nb1 Cl3 80.51(5) . . ?
O2 Nb1 Cl3 174.44(5) . . ?
Cl1 Nb1 Cl3 85.53(2) . . ?
Cl5 Nb1 Cl3 102.55(2) . . ?
O1 Nb1 Cl4 173.03(5) . . ?
O2 Nb1 Cl4 79.98(5) . . ?
Cl1 Nb1 Cl4 86.39(2) . . ?
Cl5 Nb1 Cl4 78.22(2) . . ?
Cl3 Nb1 Cl4 102.17(2) . . ?
O4 Nb2 O3 90.51(7) . . ?
O4 Nb2 Cl2 98.43(5) . . ?
O3 Nb2 Cl2 85.29(5) . . ?
O4 Nb2 Cl4 96.88(5) . . ?
O3 Nb2 Cl4 86.82(5) . . ?
Cl2 Nb2 Cl4 162.82(2) . . ?
O4 Nb2 Cl3 84.50(5) . . ?
O3 Nb2 Cl3 167.99(5) . . ?
Cl2 Nb2 Cl3 84.65(2) . . ?
Cl4 Nb2 Cl3 104.59(2) . . ?
O4 Nb2 Cl5 174.55(5) . . ?
O3 Nb2 Cl5 86.26(5) . . ?
Cl2 Nb2 Cl5 85.70(2) . . ?
Cl4 Nb2 Cl5 78.57(2) . . ?
Cl3 Nb2 Cl5 99.49(2) . . ?
O4 Nb2 K2 62.49(5) . . ?
O3 Nb2 K2 43.06(5) . . ?
Cl2 Nb2 K2 61.222(19) . . ?
Cl4 Nb2 K2 120.516(18) . . ?
Cl3 Nb2 K2 125.452(18) . . ?
Cl5 Nb2 K2 117.153(18) . . ?
Cl1 K1 Cl3 68.35(2) . . ?
Cl1 K1 C31 66.81(5) . . ?
Cl3 K1 C31 74.53(5) . . ?
Cl1 K1 C110 118.04(5) . . ?
Cl3 K1 C110 60.87(5) . . ?
C31 K1 C110 124.67(7) . . ?
O3 K2 O4 59.75(5) . . ?
O3 K2 Cl2 62.91(4) . . ?
O4 K2 Cl2 62.42(3) . . ?
O3 K2 C107 103.87(8) . . ?
O4 K2 C107 139.09(8) . . ?
Cl2 K2 C107 76.70(7) . . ?
O3 K2 C127 122.85(7) . . ?
O4 K2 C127 63.10(6) . . ?
Cl2 K2 C127 91.27(5) . . ?
C107 K2 C127 119.29(9) . . ?
O3 K2 C88 102.69(7) . . ?
O4 K2 C88 90.77(7) . . ?
Cl2 K2 C88 153.07(6) . . ?
C107 K2 C88 130.14(9) . . ?
C127 K2 C88 77.50(7) . . ?
O3 K2 C104 73.36(7) . . ?
O4 K2 C104 133.06(7) . . ?
Cl2 K2 C104 95.55(6) . . ?
C107 K2 C104 48.78(9) . . ?
C127 K2 C104 163.68(8) . . ?
C88 K2 C104 101.94(8) . . ?
O3 K2 C106 111.84(8) . . ?
O4 K2 C106 162.00(8) . . ?
Cl2 K2 C106 99.70(7) . . ?
C107 K2 C106 23.30(9) . . ?
C127 K2 C106 122.79(9) . . ?
C88 K2 C106 106.98(9) . . ?
C104 K2 C106 41.37(10) . . ?
O3 K2 C91 69.91(6) . . ?
O4 K2 C91 102.65(6) . . ?
Cl2 K2 C91 131.59(5) . . ?
C107 K2 C91 105.68(9) . . ?
C127 K2 C91 124.42(7) . . ?
C88 K2 C91 47.91(7) . . ?
C104 K2 C91 59.87(7) . . ?
C106 K2 C91 87.66(9) . . ?
O3 K2 C105 96.75(9) . . ?
O4 K2 C105 156.49(8) . . ?
Cl2 K2 C105 108.91(7) . . ?
C107 K2 C105 40.84(10) . . ?
C127 K2 C105 140.40(9) . . ?
C88 K2 C105 94.79(9) . . ?
C104 K2 C105 23.50(9) . . ?
C106 K2 C105 22.94(10) . . ?
C91 K2 C105 65.65(9) . . ?
O3 K2 C73 17.49(5) . . ?
O4 K2 C73 75.24(5) . . ?
Cl2 K2 C73 76.25(4) . . ?
C107 K2 C73 97.52(8) . . ?
C127 K2 C73 137.43(7) . . ?
C88 K2 C73 95.44(7) . . ?
C104 K2 C73 58.82(7) . . ?
C106 K2 C73 99.55(9) . . ?
C91 K2 C73 55.37(6) . . ?
C105 K2 C73 81.50(9) . . ?
O3 K2 C89 108.48(7) . . ?
O4 K2 C89 113.08(6) . . ?
Cl2 K2 C89 171.32(6) . . ?
C107 K2 C89 107.65(9) . . ?
C127 K2 C89 92.95(8) . . ?
C88 K2 C89 22.96(8) . . ?
C104 K2 C89 82.38(8) . . ?
C106 K2 C89 84.36(9) . . ?
C91 K2 C89 40.44(7) . . ?
C105 K2 C89 72.15(9) . . ?
C73 K2 C89 95.56(7) . . ?
O2 K3 Cl5 64.07(4) . . ?
O2 K3 Cl4 62.82(4) . . ?
Cl5 K3 Cl4 62.225(19) . . ?
Nb1 Cl1 K1 103.55(3) . . ?
Nb2 Cl2 K2 78.19(2) . . ?
Nb1 Cl3 Nb2 63.459(16) . . ?
Nb1 Cl3 K1 101.07(3) . . ?
Nb2 Cl3 K1 115.52(3) . . ?
Nb2 Cl4 Nb1 62.981(16) . . ?
Nb2 Cl4 K3 107.86(2) . . ?
Nb1 Cl4 K3 84.81(2) . . ?
Nb1 Cl5 Nb2 63.160(16) . . ?
Nb1 Cl5 K3 87.97(2) . . ?
Nb2 Cl5 K3 107.34(2) . . ?
C1 O1 Nb1 153.95(16) . . ?
C37 O2 Nb1 128.88(14) . . ?
C37 O2 K3 122.04(14) . . ?
Nb1 O2 K3 109.04(7) . . ?
C73 O3 Nb2 130.34(15) . . ?
C73 O3 K2 127.55(15) . . ?
Nb2 O3 K2 102.07(7) . . ?
C109 O4 Nb2 137.68(15) . . ?
C109 O4 K2 130.74(14) . . ?
Nb2 O4 K2 84.02(6) . . ?
O1 C1 C6 119.5(2) . . ?
O1 C1 C2 122.0(2) . . ?
C6 C1 C2 118.5(2) . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 C7 118.2(2) . . ?
C1 C2 C7 123.0(2) . . ?
C4 C3 C2 123.3(3) . . ?
C5 C4 C3 116.5(2) . . ?
C5 C4 C20 121.7(3) . . ?
C3 C4 C20 121.8(3) . . ?
C4 C5 C6 122.6(3) . . ?
C5 C6 C1 120.0(2) . . ?
C5 C6 C24 118.8(2) . . ?
C1 C6 C24 120.9(2) . . ?
C8 C7 C2 113.3(3) . . ?
C8 C7 C14 112.0(2) . . ?
C2 C7 C14 109.1(2) . . ?
C9 C8 C13 118.0(3) . . ?
C9 C8 C7 123.0(3) . . ?
C13 C8 C7 118.9(3) . . ?
C8 C9 C10 122.0(4) . . ?
C11 C10 C9 118.8(5) . . ?
C10 C11 C12 120.4(4) . . ?
C13 C12 C11 120.1(4) . . ?
C12 C13 C8 120.6(4) . . ?
C15 C14 C19 118.6(3) . . ?
C15 C14 C7 119.0(3) . . ?
C19 C14 C7 122.3(3) . . ?
C14 C15 C16 121.3(3) . . ?
C17 C16 C15 120.4(4) . . ?
C18 C17 C16 119.2(4) . . ?
C17 C18 C19 121.4(4) . . ?
C14 C19 C18 119.1(4) . . ?
C22 C20 C21 111.2(5) . . ?
C22 C20 C23 107.8(5) . . ?
C21 C20 C23 106.1(5) . . ?
C22 C20 C4 112.6(3) . . ?
C21 C20 C4 107.6(3) . . ?
C23 C20 C4 111.3(3) . . ?
C6 C24 C25 111.7(2) . . ?
C6 C24 C31 111.1(2) . . ?
C25 C24 C31 113.0(2) . . ?
C26 C25 C30 118.0(3) . . ?
C26 C25 C24 118.5(2) . . ?
C30 C25 C24 123.5(2) . . ?
C27 C26 C25 120.8(3) . . ?
C28 C27 C26 120.6(3) . . ?
C27 C28 C29 119.7(3) . . ?
C28 C29 C30 119.7(3) . . ?
C25 C30 C29 121.3(3) . . ?
C36 C31 C32 118.2(3) . . ?
C36 C31 C24 123.4(2) . . ?
C32 C31 C24 118.4(2) . . ?
C36 C31 K1 77.26(15) . . ?
C32 C31 K1 70.91(15) . . ?
C24 C31 K1 120.75(15) . . ?
C33 C32 C31 120.8(3) . . ?
C34 C33 C32 120.2(3) . . ?
C35 C34 C33 119.6(3) . . ?
C34 C35 C36 120.4(3) . . ?
C31 C36 C35 120.7(3) . . ?
O2 C37 C38 120.0(2) . . ?
O2 C37 C42 121.1(2) . . ?
C38 C37 C42 118.6(2) . . ?
C39 C38 C37 119.5(2) . . ?
C39 C38 C43 120.4(2) . . ?
C37 C38 C43 118.9(2) . . ?
C40 C39 C38 122.6(2) . . ?
C39 C40 C41 117.0(2) . . ?
C39 C40 C56 121.8(2) . . ?
C41 C40 C56 120.6(2) . . ?
C42 C41 C40 122.6(2) . . ?
C41 C42 C37 119.6(2) . . ?
C41 C42 C60 121.2(2) . . ?
C37 C42 C60 118.5(2) . . ?
C38 C43 C50 110.7(2) . . ?
C38 C43 C44 108.7(2) . . ?
C50 C43 C44 113.1(2) . . ?
C45 C44 C49 118.1(3) . . ?
C45 C44 C43 120.5(2) . . ?
C49 C44 C43 121.3(2) . . ?
C44 C45 C46 120.8(3) . . ?
C47 C46 C45 120.4(3) . . ?
C48 C47 C46 119.5(3) . . ?
C47 C48 C49 120.2(3) . . ?
C48 C49 C44 120.9(3) . . ?
C51 C50 C55 118.5(3) . . ?
C51 C50 C43 123.2(3) . . ?
C55 C50 C43 118.1(2) . . ?
C50 C51 C52 120.4(3) . . ?
C53 C52 C51 120.8(3) . . ?
C52 C53 C54 119.4(3) . . ?
C53 C54 C55 120.1(3) . . ?
C54 C55 C50 120.9(3) . . ?
C58 C56 C57 108.2(2) . . ?
C58 C56 C59 108.7(2) . . ?
C57 C56 C59 109.4(2) . . ?
C58 C56 C40 112.3(2) . . ?
C57 C56 C40 107.2(2) . . ?
C59 C56 C40 111.0(2) . . ?
C42 C60 C61 112.6(2) . . ?
C42 C60 C67 110.4(2) . . ?
C61 C60 C67 113.2(2) . . ?
C66 C61 C62 117.6(2) . . ?
C66 C61 C60 123.7(2) . . ?
C62 C61 C60 118.6(2) . . ?
C63 C62 C61 121.2(3) . . ?
C62 C63 C64 120.3(3) . . ?
C63 C64 C65 119.2(3) . . ?
C64 C65 C66 120.1(3) . . ?
C61 C66 C65 121.5(3) . . ?
C68 C67 C72 118.3(3) . . ?
C68 C67 C60 122.2(2) . . ?
C72 C67 C60 119.4(2) . . ?
C67 C68 C69 120.8(3) . . ?
C70 C69 C68 120.1(3) . . ?
C71 C70 C69 119.6(3) . . ?
C70 C71 C72 120.4(3) . . ?
C71 C72 C67 120.7(3) . . ?
O3 C73 C74 120.0(2) . . ?
O3 C73 C78 121.1(2) . . ?
C74 C73 C78 118.6(2) . . ?
O3 C73 K2 34.95(11) . . ?
C74 C73 K2 114.09(16) . . ?
C78 C73 K2 112.26(16) . . ?
C75 C74 C73 119.8(2) . . ?
C75 C74 C79 122.7(2) . . ?
C73 C74 C79 117.1(2) . . ?
C76 C75 C74 121.7(2) . . ?
C75 C76 C77 116.8(2) . . ?
C75 C76 C92 123.9(2) . . ?
C77 C76 C92 119.2(2) . . ?
C78 C77 C76 123.3(2) . . ?
C77 C78 C73 118.2(2) . . ?
C77 C78 C96 122.0(2) . . ?
C73 C78 C96 119.7(2) . . ?
C80 C79 C74 113.2(2) . . ?
C80 C79 C86 111.7(2) . . ?
C74 C79 C86 109.9(2) . . ?
C81 C80 C85 118.1(3) . . ?
C81 C80 C79 119.8(3) . . ?
C85 C80 C79 122.0(2) . . ?
C80 C81 C82 120.4(3) . . ?
C83 C82 C81 120.4(3) . . ?
C84 C83 C82 119.5(3) . . ?
C83 C84 C85 120.5(3) . . ?
C84 C85 C80 121.0(3) . . ?
C91 C86 C87 117.9(3) . . ?
C91 C86 C79 122.0(2) . . ?
C87 C86 C79 120.1(2) . . ?
C88 C87 C86 121.1(3) . . ?
C89 C88 C87 120.6(3) . . ?
C89 C88 K2 85.84(19) . . ?
C87 C88 K2 72.81(17) . . ?
C90 C89 C88 119.1(3) . . ?
C90 C89 K2 80.47(19) . . ?
C88 C89 K2 71.20(18) . . ?
C89 C90 C91 120.4(3) . . ?
C86 C91 C90 120.9(3) . . ?
C86 C91 K2 72.01(15) . . ?
C90 C91 K2 83.74(18) . . ?
C93 C92 C76 112.4(2) . . ?
C93 C92 C94 108.3(2) . . ?
C76 C92 C94 110.2(2) . . ?
C93 C92 C95 108.3(2) . . ?
C76 C92 C95 109.1(2) . . ?
C94 C92 C95 108.5(2) . . ?
C103 C96 C78 112.5(2) . . ?
C103 C96 C97 110.7(2) . . ?
C78 C96 C97 111.1(2) . . ?
C102 C97 C98 118.9(3) . . ?
C102 C97 C96 119.5(3) . . ?
C98 C97 C96 121.5(3) . . ?
C99 C98 C97 119.8(4) . . ?
C100 C99 C98 120.8(4) . . ?
C101 C100 C99 119.8(3) . . ?
C100 C101 C102 119.9(4) . . ?
C97 C102 C101 120.8(4) . . ?
C104 C103 C108 117.3(3) . . ?
C104 C103 C96 123.0(3) . . ?
C108 C103 C96 119.6(3) . . ?
C103 C104 C105 120.6(3) . . ?
C103 C104 K2 73.86(19) . . ?
C105 C104 K2 81.7(3) . . ?
C106 C105 C104 120.9(4) . . ?
C106 C105 K2 77.5(2) . . ?
C104 C105 K2 74.8(2) . . ?
C107 C106 C105 119.8(4) . . ?
C107 C106 K2 73.8(2) . . ?
C105 C106 K2 79.6(2) . . ?
C106 C107 C108 119.7(4) . . ?
C106 C107 K2 82.9(2) . . ?
C108 C107 K2 74.09(17) . . ?
C107 C108 C103 121.7(3) . . ?
O4 C109 C114 122.0(2) . . ?
O4 C109 C110 119.7(2) . . ?
C114 C109 C110 118.2(2) . . ?
C111 C110 C109 119.5(2) . . ?
C111 C110 C115 120.3(2) . . ?
C109 C110 C115 120.1(2) . . ?
C111 C110 K1 76.18(15) . . ?
C109 C110 K1 71.94(14) . . ?
C115 C110 K1 127.05(16) . . ?
C110 C111 C112 123.4(3) . . ?
C113 C112 C111 116.4(2) . . ?
C113 C112 C128 124.1(3) . . ?
C111 C112 C128 119.5(3) . . ?
C112 C113 C114 123.0(3) . . ?
C113 C114 C109 119.4(2) . . ?
C113 C114 C132 117.8(2) . . ?
C109 C114 C132 122.3(2) . . ?
C110 C115 C116 111.9(2) . . ?
C110 C115 C122 111.9(2) . . ?
C116 C115 C122 113.2(2) . . ?
C117 C116 C121 118.0(3) . . ?
C117 C116 C115 122.8(2) . . ?
C121 C116 C115 119.1(2) . . ?
C116 C117 C118 120.6(3) . . ?
C119 C118 C117 120.8(3) . . ?
C118 C119 C120 119.3(3) . . ?
C119 C120 C121 119.9(3) . . ?
C120 C121 C116 121.4(3) . . ?
C127 C122 C123 118.3(3) . . ?
C127 C122 C115 123.0(3) . . ?
C123 C122 C115 118.6(3) . . ?
C124 C123 C122 120.5(3) . . ?
C125 C124 C123 120.3(3) . . ?
C126 C125 C124 119.7(3) . . ?
C125 C126 C127 120.0(3) . . ?
C122 C127 C126 121.1(3) . . ?
C122 C127 K2 75.94(16) . . ?
C126 C127 K2 76.52(18) . . ?
C131 C128 C130 109.4(3) . . ?
C131 C128 C112 112.5(2) . . ?
C130 C128 C112 108.8(2) . . ?
C131 C128 C129 108.3(3) . . ?
C130 C128 C129 108.6(3) . . ?
C112 C128 C129 109.2(2) . . ?
C114 C132 C133 113.1(2) . . ?
C114 C132 C139 110.6(2) . . ?
C133 C132 C139 111.4(2) . . ?
C134 C133 C138 117.7(3) . . ?
C134 C133 C132 120.3(2) . . ?
C138 C133 C132 122.0(3) . . ?
C135 C134 C133 121.4(3) . . ?
C134 C135 C136 120.1(3) . . ?
C137 C136 C135 119.4(3) . . ?
C136 C137 C138 120.1(3) . . ?
C137 C138 C133 121.3(3) . . ?
C144 C139 C140 118.1(3) . . ?
C144 C139 C132 123.0(3) . . ?
C140 C139 C132 118.9(3) . . ?
C141 C140 C139 120.5(3) . . ?
C142 C141 C140 120.4(3) . . ?
C143 C142 C141 119.9(3) . . ?
C142 C143 C144 120.1(3) . . ?
C139 C144 C143 121.0(3) . . ?
C147 C146 C145 112.5(5) . . ?
C146 C147 C148 114.6(4) . . ?
C147 C148 C149 112.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.73
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.538
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.101

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 0.500 378 57 ' '
2 0.036 0.425 0.404 16 0 ' '
3 0.036 0.845 0.833 7 0 ' '
4 0.084 0.906 0.180 6 0 ' '
5 0.916 0.094 0.820 7 0 ' '
6 0.963 0.575 0.596 16 0 ' '
7 0.964 0.155 0.167 7 0 ' '
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1032677'
_audit_update_record             
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C151 H140 N2 Nb2 O4'
_chemical_formula_weight         2232.47

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_Int_Tables_number      61

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

_cell_length_a                   24.6450(6)
_cell_length_b                   25.8062(5)
_cell_length_c                   37.2338(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     23680.5(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10

_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9392
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.7456
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            407228
_diffrn_reflns_av_R_equivalents  0.3233
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.62
_reflns_number_total             27382
_reflns_number_gt                12036
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1338P)²+146.2397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         27382
_refine_ls_number_parameters     1430
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.2176
_refine_ls_R_factor_gt           0.0920
_refine_ls_wR_factor_ref         0.3249
_refine_ls_wR_factor_gt          0.2415
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.040
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.95664(3) 0.77166(2) 0.121920(17) 0.02013(17) Uani 1 1 d . . .
Nb2 Nb 1.04646(3) 0.83648(2) 0.123620(17) 0.02080(17) Uani 1 1 d . . .
O1 O 0.8876(2) 0.80533(19) 0.12714(12) 0.0218(11) Uani 1 1 d . . .
O2 O 0.95753(19) 0.69759(19) 0.12233(13) 0.0212(10) Uani 1 1 d . . .
O3 O 1.0475(2) 0.91076(19) 0.12827(13) 0.0233(11) Uani 1 1 d . . .
O4 O 1.1138(2) 0.80371(19) 0.13077(13) 0.0234(11) Uani 1 1 d . . .
N1 N 1.0004(2) 0.8026(2) 0.15713(15) 0.0211(13) Uani 1 1 d . . .
N2 N 1.0023(3) 0.8047(2) 0.08848(15) 0.0222(13) Uani 1 1 d . . .
C1 C 0.8660(3) 0.8447(3) 0.14754(19) 0.0212(15) Uani 1 1 d . . .
C2 C 0.8557(3) 0.8364(3) 0.1840(2) 0.0235(16) Uani 1 1 d . . .
C3 C 0.8339(3) 0.8767(3) 0.20363(19) 0.0263(17) Uani 1 1 d . . .
H3 H 0.8260 0.8712 0.2278 0.035 Uiso 1 1 calc R . .
C4 C 0.8231(3) 0.9252(3) 0.1888(2) 0.0262(17) Uani 1 1 d . . .
C5 C 0.8332(3) 0.9314(3) 0.1522(2) 0.0259(17) Uani 1 1 d . . .
H5 H 0.8260 0.9632 0.1414 0.034 Uiso 1 1 calc R . .
C6 C 0.8539(3) 0.8910(3) 0.13125(19) 0.0249(17) Uani 1 1 d . . .
C7 C 0.8665(3) 0.7825(3) 0.20077(19) 0.0249(17) Uani 1 1 d . . .
H7 H 0.9018 0.7708 0.1917 0.033 Uiso 1 1 calc R . .
C8 C 0.8249(3) 0.7426(3) 0.18901(18) 0.0210(16) Uani 1 1 d . . .
C9 C 0.7695(3) 0.7542(3) 0.1880(2) 0.0270(17) Uani 1 1 d . . .
H9 H 0.7581 0.7882 0.1915 0.036 Uiso 1 1 calc R . .
C10 C 0.7311(4) 0.7157(3) 0.1818(2) 0.035(2) Uani 1 1 d . . .
H10 H 0.6942 0.7235 0.1820 0.046 Uiso 1 1 calc R . .
C11 C 0.7485(3) 0.6653(4) 0.1755(2) 0.034(2) Uani 1 1 d . . .
H11 H 0.7233 0.6391 0.1715 0.045 Uiso 1 1 calc R . .
C12 C 0.8036(4) 0.6539(3) 0.1750(2) 0.034(2) Uani 1 1 d . . .
H12 H 0.8152 0.6204 0.1700 0.045 Uiso 1 1 calc R . .
C13 C 0.8410(3) 0.6924(3) 0.18190(19) 0.0266(18) Uani 1 1 d . . .
H13 H 0.8777 0.6843 0.1818 0.035 Uiso 1 1 calc R . .
C14 C 0.8711(3) 0.7851(3) 0.2417(2) 0.0271(17) Uani 1 1 d . . .
C15 C 0.9168(4) 0.8103(4) 0.2565(2) 0.037(2) Uani 1 1 d . . .
H15 H 0.9425 0.8252 0.2414 0.050 Uiso 1 1 calc R . .
C16 C 0.9238(4) 0.8129(4) 0.2934(2) 0.047(3) Uani 1 1 d . . .
H16 H 0.9535 0.8303 0.3030 0.063 Uiso 1 1 calc R . .
C17 C 0.8861(4) 0.7896(4) 0.3161(2) 0.047(2) Uani 1 1 d . . .
H17 H 0.8911 0.7906 0.3408 0.062 Uiso 1 1 calc R . .
C18 C 0.8426(4) 0.7657(3) 0.3021(2) 0.035(2) Uani 1 1 d . . .
H18 H 0.8172 0.7507 0.3174 0.047 Uiso 1 1 calc R . .
C19 C 0.8346(4) 0.7629(3) 0.2648(2) 0.0336(19) Uani 1 1 d . . .
H19 H 0.8042 0.7459 0.2557 0.045 Uiso 1 1 calc R . .
C20 C 0.8021(3) 0.9688(3) 0.2126(2) 0.0278(18) Uani 1 1 d . . .
C21 C 0.7466(3) 0.9540(3) 0.2273(2) 0.035(2) Uani 1 1 d . . .
H21a H 0.7228 0.9454 0.2078 0.052 Uiso 1 1 calc R . .
H21b H 0.7317 0.9826 0.2405 0.052 Uiso 1 1 calc R . .
H21c H 0.7502 0.9246 0.2429 0.052 Uiso 1 1 calc R . .
C22 C 0.8415(4) 0.9761(3) 0.2443(2) 0.039(2) Uani 1 1 d . . .
H22a H 0.8445 0.9441 0.2574 0.059 Uiso 1 1 calc R . .
H22b H 0.8279 1.0027 0.2600 0.059 Uiso 1 1 calc R . .
H22c H 0.8765 0.9859 0.2354 0.059 Uiso 1 1 calc R . .
C23 C 0.7963(4) 1.0200(3) 0.1932(2) 0.040(2) Uani 1 1 d . . .
H23a H 0.8308 1.0300 0.1834 0.060 Uiso 1 1 calc R . .
H23b H 0.7840 1.0459 0.2097 0.060 Uiso 1 1 calc R . .
H23c H 0.7705 1.0164 0.1740 0.060 Uiso 1 1 calc R . .
C24 C 0.8560(3) 0.8956(3) 0.0899(2) 0.0263(17) Uani 1 1 d . . .
H24 H 0.8842 0.8717 0.0818 0.035 Uiso 1 1 calc R . .
C25 C 0.8030(4) 0.8771(3) 0.0731(2) 0.0302(18) Uani 1 1 d . . .
C26 C 0.7608(3) 0.8559(3) 0.0922(2) 0.0327(19) Uani 1 1 d . . .
H26 H 0.7641 0.8515 0.1169 0.044 Uiso 1 1 calc R . .
C27 C 0.7134(4) 0.8412(4) 0.0753(3) 0.044(2) Uani 1 1 d . . .
H27 H 0.6848 0.8277 0.0887 0.059 Uiso 1 1 calc R . .
C28 C 0.7082(4) 0.8463(4) 0.0384(3) 0.045(2) Uani 1 1 d . . .
H28 H 0.6761 0.8365 0.0271 0.060 Uiso 1 1 calc R . .
C29 C 0.7507(4) 0.8659(4) 0.0185(3) 0.048(2) Uani 1 1 d . . .
H29 H 0.7477 0.8686 -0.0064 0.063 Uiso 1 1 calc R . .
C30 C 0.7977(4) 0.8817(4) 0.0354(2) 0.041(2) Uani 1 1 d . . .
H30 H 0.8261 0.8953 0.0219 0.054 Uiso 1 1 calc R . .
C31 C 0.8718(3) 0.9489(3) 0.0763(2) 0.0282(18) Uani 1 1 d . . .
C32 C 0.9241(4) 0.9584(3) 0.0652(2) 0.038(2) Uani 1 1 d . . .
H32 H 0.9499 0.9323 0.0670 0.051 Uiso 1 1 calc R . .
C33 C 0.9394(4) 1.0075(4) 0.0511(2) 0.044(2) Uani 1 1 d . . .
H33 H 0.9749 1.0134 0.0437 0.059 Uiso 1 1 calc R . .
C34 C 0.9016(5) 1.0455(4) 0.0484(2) 0.050(3) Uani 1 1 d . . .
H34 H 0.9114 1.0778 0.0395 0.067 Uiso 1 1 calc R . .
C35 C 0.8479(4) 1.0363(4) 0.0589(2) 0.042(2) Uani 1 1 d . . .
H35 H 0.8223 1.0625 0.0568 0.057 Uiso 1 1 calc R . .
C36 C 0.8326(4) 0.9881(3) 0.0723(2) 0.037(2) Uani 1 1 d . . .
H36 H 0.7967 0.9819 0.0786 0.049 Uiso 1 1 calc R . .
C37 C 0.9355(3) 0.6487(3) 0.1159(2) 0.0274(17) Uani 1 1 d . . .
C38 C 0.8876(3) 0.6439(3) 0.09580(19) 0.0210(15) Uani 1 1 d . . .
C39 C 0.8663(3) 0.5944(3) 0.0916(2) 0.0268(17) Uani 1 1 d . . .
H39 H 0.8342 0.5908 0.0786 0.036 Uiso 1 1 calc R . .
C40 C 0.8901(3) 0.5504(3) 0.1056(2) 0.0285(18) Uani 1 1 d . . .
C41 C 0.9408(3) 0.5569(2) 0.12485(18) 0.0186(14) Uani 1 1 d U . .
H41 H 0.9595 0.5280 0.1331 0.025 Uiso 1 1 calc R . .
C42 C 0.9614(3) 0.6054(3) 0.13097(18) 0.0219(15) Uani 1 1 d . . .
C43 C 0.8613(3) 0.6919(3) 0.0805(2) 0.0254(17) Uani 1 1 d . . .
H43 H 0.8608 0.7177 0.0998 0.034 Uiso 1 1 calc R . .
C44 C 0.8940(3) 0.7157(3) 0.0496(2) 0.0278(18) Uani 1 1 d . . .
C45 C 0.8817(4) 0.7661(4) 0.0388(2) 0.038(2) Uani 1 1 d . . .
H45 H 0.8574 0.7859 0.0520 0.050 Uiso 1 1 calc R . .
C46 C 0.9058(4) 0.7866(4) 0.0084(3) 0.048(3) Uani 1 1 d . . .
H46 H 0.8984 0.8205 0.0014 0.064 Uiso 1 1 calc R . .
C47 C 0.9415(4) 0.7560(5) -0.0117(3) 0.064(4) Uani 1 1 d . . .
H47 H 0.9565 0.7688 -0.0328 0.086 Uiso 1 1 calc R . .
C48 C 0.9540(4) 0.7086(6) -0.0007(3) 0.068(4) Uani 1 1 d . . .
H48 H 0.9787 0.6890 -0.0137 0.090 Uiso 1 1 calc R . .
C49 C 0.9307(4) 0.6876(4) 0.0301(3) 0.054(3) Uani 1 1 d . . .
H49 H 0.9402 0.6543 0.0375 0.072 Uiso 1 1 calc R . .
C50 C 0.8023(3) 0.6843(3) 0.0688(2) 0.0263(17) Uani 1 1 d . . .
C51 C 0.7614(3) 0.7045(3) 0.0894(2) 0.0336(19) Uani 1 1 d . . .
H51 H 0.7701 0.7227 0.1102 0.045 Uiso 1 1 calc R . .
C52 C 0.7082(4) 0.6987(4) 0.0802(2) 0.039(2) Uani 1 1 d . . .
H52 H 0.6810 0.7117 0.0950 0.052 Uiso 1 1 calc R . .
C53 C 0.6949(4) 0.6731(3) 0.0487(2) 0.040(2) Uani 1 1 d . . .
H53 H 0.6587 0.6693 0.0421 0.053 Uiso 1 1 calc R . .
C54 C 0.7345(4) 0.6538(3) 0.0275(2) 0.038(2) Uani 1 1 d . . .
H54 H 0.7253 0.6365 0.0064 0.051 Uiso 1 1 calc R . .
C55 C 0.7886(4) 0.6595(3) 0.0368(2) 0.033(2) Uani 1 1 d . . .
H55 H 0.8156 0.6469 0.0217 0.044 Uiso 1 1 calc R . .
C56 C 0.8616(4) 0.4972(3) 0.1016(2) 0.038(2) Uani 1 1 d . . .
C57 C 0.8966(5) 0.4531(4) 0.1128(4) 0.074(4) Uani 1 1 d . . .
H57a H 0.8766 0.4213 0.1107 0.112 Uiso 1 1 calc R . .
H57b H 0.9078 0.4578 0.1372 0.112 Uiso 1 1 calc R . .
H57c H 0.9281 0.4516 0.0976 0.112 Uiso 1 1 calc R . .
C58 C 0.8400(5) 0.4887(4) 0.0640(3) 0.058(3) Uani 1 1 d . . .
H58a H 0.8695 0.4899 0.0471 0.087 Uiso 1 1 calc R . .
H58b H 0.8142 0.5154 0.0583 0.087 Uiso 1 1 calc R . .
H58c H 0.8226 0.4555 0.0627 0.087 Uiso 1 1 calc R . .
C59 C 0.8113(4) 0.4988(4) 0.1273(3) 0.059(3) Uani 1 1 d . . .
H59a H 0.8234 0.4998 0.1518 0.089 Uiso 1 1 calc R . .
H59b H 0.7895 0.4685 0.1235 0.089 Uiso 1 1 calc R . .
H59c H 0.7901 0.5292 0.1223 0.089 Uiso 1 1 calc R . .
C60 C 1.0084(3) 0.6121(3) 0.15729(19) 0.0244(16) Uani 1 1 d . . .
H60 H 1.0308 0.6409 0.1487 0.032 Uiso 1 1 calc R . .
C61 C 1.0427(3) 0.5644(3) 0.1574(2) 0.0257(16) Uani 1 1 d . . .
C62 C 1.0771(3) 0.5555(3) 0.1276(2) 0.036(2) Uani 1 1 d . . .
H62 H 1.0794 0.5803 0.1095 0.048 Uiso 1 1 calc R . .
C63 C 1.1069(4) 0.5110(4) 0.1248(3) 0.044(2) Uani 1 1 d . . .
H63 H 1.1286 0.5060 0.1047 0.059 Uiso 1 1 calc R . .
C64 C 1.1057(4) 0.4737(4) 0.1506(3) 0.050(3) Uani 1 1 d . . .
H64 H 1.1261 0.4435 0.1484 0.066 Uiso 1 1 calc R . .
C65 C 1.0728(4) 0.4822(4) 0.1808(3) 0.045(2) Uani 1 1 d . . .
H65 H 1.0712 0.4570 0.1986 0.060 Uiso 1 1 calc R . .
C66 C 1.0423(3) 0.5274(3) 0.1847(2) 0.0343(19) Uani 1 1 d . . .
H66 H 1.0218 0.5328 0.2053 0.046 Uiso 1 1 calc R . .
C67 C 0.9840(3) 0.6280(3) 0.1930(2) 0.0245(16) Uani 1 1 d . . .
C68 C 1.0021(4) 0.6735(3) 0.2103(2) 0.035(2) Uani 1 1 d . . .
H68 H 1.0304 0.6927 0.2006 0.046 Uiso 1 1 calc R . .
C69 C 0.9771(4) 0.6894(4) 0.2423(2) 0.042(2) Uani 1 1 d . . .
H69 H 0.9889 0.7195 0.2536 0.056 Uiso 1 1 calc R . .
C70 C 0.9357(4) 0.6614(4) 0.2569(2) 0.042(2) Uani 1 1 d . . .
H70 H 0.9194 0.6727 0.2780 0.055 Uiso 1 1 calc R . .
C71 C 0.9178(4) 0.6167(3) 0.2409(2) 0.034(2) Uani 1 1 d . . .
H71 H 0.8900 0.5974 0.2511 0.046 Uiso 1 1 calc R . .
C72 C 0.9420(3) 0.6007(3) 0.2089(2) 0.0322(19) Uani 1 1 d . . .
H72 H 0.9295 0.5706 0.1979 0.043 Uiso 1 1 calc R . .
C73 C 1.0656(3) 0.9595(3) 0.12251(19) 0.0207(15) Uani 1 1 d . . .
C74 C 1.1112(3) 0.9672(3) 0.1009(2) 0.0248(17) Uani 1 1 d . . .
C75 C 1.1305(3) 1.0174(3) 0.0957(2) 0.0262(17) Uani 1 1 d . . .
H75 H 1.1614 1.0222 0.0818 0.035 Uiso 1 1 calc R . .
C76 C 1.1053(3) 1.0602(3) 0.1105(2) 0.0263(17) Uani 1 1 d . . .
C77 C 1.0605(3) 1.0513(3) 0.1317(2) 0.0290(18) Uani 1 1 d . . .
H77 H 1.0431 1.0796 0.1420 0.039 Uiso 1 1 calc R . .
C78 C 1.0397(3) 1.0018(3) 0.13835(19) 0.0248(16) Uani 1 1 d . . .
C79 C 1.1407(3) 0.9203(3) 0.0843(2) 0.0242(16) Uani 1 1 d . . .
H79 H 1.1494 0.8967 0.1041 0.032 Uiso 1 1 calc R . .
C80 C 1.1062(3) 0.8903(3) 0.0582(2) 0.0261(17) Uani 1 1 d . . .
C81 C 1.0597(3) 0.9107(3) 0.0424(2) 0.0326(19) Uani 1 1 d . . .
H81 H 1.0478 0.9438 0.0484 0.043 Uiso 1 1 calc R . .
C82 C 1.0311(4) 0.8809(4) 0.0174(2) 0.044(2) Uani 1 1 d . . .
H82 H 0.9990 0.8936 0.0075 0.058 Uiso 1 1 calc R . .
C83 C 1.0501(4) 0.8334(4) 0.0074(2) 0.040(2) Uani 1 1 d . . .
H83 H 1.0310 0.8141 -0.0095 0.053 Uiso 1 1 calc R . .
C84 C 1.0967(4) 0.8135(3) 0.0218(2) 0.043(2) Uani 1 1 d . . .
H84 H 1.1096 0.7814 0.0144 0.057 Uiso 1 1 calc R . .
C85 C 1.1246(4) 0.8413(3) 0.0474(2) 0.0308(19) Uani 1 1 d . . .
H85 H 1.1558 0.8275 0.0576 0.041 Uiso 1 1 calc R . .
C86 C 1.1945(3) 0.9337(3) 0.0657(2) 0.0269(17) Uani 1 1 d . . .
C87 C 1.2434(3) 0.9155(3) 0.0798(2) 0.0330(19) Uani 1 1 d . . .
H87 H 1.2437 0.8964 0.1010 0.044 Uiso 1 1 calc R . .
C88 C 1.2920(4) 0.9263(4) 0.0617(3) 0.039(2) Uani 1 1 d . . .
H88 H 1.3246 0.9143 0.0711 0.053 Uiso 1 1 calc R . .
C89 C 1.2922(4) 0.9542(3) 0.0306(2) 0.036(2) Uani 1 1 d . . .
H89 H 1.3246 0.9609 0.0186 0.048 Uiso 1 1 calc R . .
C90 C 1.2441(4) 0.9724(3) 0.0171(2) 0.034(2) Uani 1 1 d . . .
H90 H 1.2440 0.9922 -0.0038 0.046 Uiso 1 1 calc R . .
C91 C 1.1958(3) 0.9614(3) 0.0343(2) 0.0324(19) Uani 1 1 d . . .
H91 H 1.1634 0.9731 0.0243 0.043 Uiso 1 1 calc R . .
C92 C 1.1242(4) 1.1158(3) 0.1035(2) 0.041(2) Uani 1 1 d U . .
C93 C 1.1237(7) 1.1483(5) 0.1360(4) 0.106(6) Uani 1 1 d U . .
H93a H 1.1522 1.1373 0.1519 0.159 Uiso 1 1 calc R . .
H93b H 1.0893 1.1448 0.1479 0.159 Uiso 1 1 calc R . .
H93c H 1.1293 1.1838 0.1294 0.159 Uiso 1 1 calc R . .
C94 C 1.0846(7) 1.1402(5) 0.0783(5) 0.114(5) Uani 1 1 d U . .
H94a H 1.0967 1.1745 0.0724 0.170 Uiso 1 1 calc R . .
H94b H 1.0496 1.1420 0.0896 0.170 Uiso 1 1 calc R . .
H94c H 1.0821 1.1198 0.0568 0.170 Uiso 1 1 calc R . .
C95 C 1.1737(6) 1.1188(5) 0.0825(5) 0.135(7) Uani 1 1 d U . .
H95a H 1.1792 1.1538 0.0747 0.203 Uiso 1 1 calc R . .
H95b H 1.1709 1.0964 0.0620 0.203 Uiso 1 1 calc R . .
H95c H 1.2039 1.1081 0.0971 0.203 Uiso 1 1 calc R . .
C96 C 0.9935(3) 0.9933(3) 0.16526(19) 0.0235(16) Uani 1 1 d . . .
H96 H 0.9703 0.9657 0.1556 0.031 Uiso 1 1 calc R . .
C97 C 0.9588(3) 1.0416(3) 0.1687(2) 0.0271(17) Uani 1 1 d . . .
C98 C 0.9634(3) 1.0763(3) 0.1965(2) 0.0317(19) Uani 1 1 d . . .
H98 H 0.9855 1.0689 0.2160 0.042 Uiso 1 1 calc R . .
C99 C 0.9342(4) 1.1231(3) 0.1951(3) 0.041(2) Uani 1 1 d . . .
H99 H 0.9380 1.1468 0.2138 0.055 Uiso 1 1 calc R . .
C100 C 0.9007(4) 1.1348(3) 0.1672(3) 0.038(2) Uani 1 1 d . . .
H100 H 0.8818 1.1660 0.1669 0.050 Uiso 1 1 calc R . .
C101 C 0.8950(3) 1.1001(4) 0.1395(3) 0.038(2) Uani 1 1 d . . .
H101 H 0.8726 1.1079 0.1202 0.050 Uiso 1 1 calc R . .
C102 C 0.9226(3) 1.0536(3) 0.1403(2) 0.036(2) Uani 1 1 d . . .
H102 H 0.9175 1.0297 0.1218 0.048 Uiso 1 1 calc R . .
C103 C 1.0166(3) 0.9741(3) 0.2002(2) 0.0233(16) Uani 1 1 d . . .
C104 C 0.9955(4) 0.9316(3) 0.2183(2) 0.038(2) Uani 1 1 d . . .
H104 H 0.9660 0.9144 0.2082 0.050 Uiso 1 1 calc R . .
C105 C 1.0155(5) 0.9140(4) 0.2498(3) 0.052(3) Uani 1 1 d . . .
H105 H 0.9996 0.8855 0.2609 0.069 Uiso 1 1 calc R . .
C106 C 1.0598(4) 0.9385(4) 0.2656(2) 0.041(2) Uani 1 1 d . . .
H106 H 1.0736 0.9270 0.2875 0.054 Uiso 1 1 calc R . .
C107 C 1.0822(4) 0.9793(4) 0.2486(2) 0.042(2) Uani 1 1 d . . .
H107 H 1.1124 0.9955 0.2584 0.056 Uiso 1 1 calc R . .
C108 C 1.0607(3) 0.9976(3) 0.2163(2) 0.0325(19) Uani 1 1 d . . .
H108 H 1.0765 1.0263 0.2054 0.043 Uiso 1 1 calc R . .
C109 C 1.1352(3) 0.7617(3) 0.14958(19) 0.0235(16) Uani 1 1 d . . .
C110 C 1.1437(3) 0.7664(3) 0.18657(19) 0.0238(16) Uani 1 1 d . . .
C111 C 1.1647(3) 0.7240(3) 0.2042(2) 0.0284(18) Uani 1 1 d . . .
H111 H 1.1706 0.7265 0.2288 0.038 Uiso 1 1 calc R . .
C112 C 1.1775(3) 0.6775(3) 0.1871(2) 0.0266(17) Uani 1 1 d . . .
C113 C 1.1704(3) 0.6757(3) 0.1499(2) 0.0305(18) Uani 1 1 d . . .
H113 H 1.1795 0.6455 0.1377 0.041 Uiso 1 1 calc R . .
C114 C 1.1503(3) 0.7175(3) 0.1305(2) 0.0249(17) Uani 1 1 d . . .
C115 C 1.1321(3) 0.8182(3) 0.2049(2) 0.0254(17) Uani 1 1 d . . .
H115 H 1.0969 0.8302 0.1960 0.034 Uiso 1 1 calc R . .
C116 C 1.1269(3) 0.8131(3) 0.2458(2) 0.0299(18) Uani 1 1 d . . .
C117 C 1.0834(4) 0.7858(4) 0.2596(2) 0.044(2) Uani 1 1 d . . .
H117 H 1.0595 0.7697 0.2438 0.058 Uiso 1 1 calc R . .
C118 C 1.0744(4) 0.7816(4) 0.2966(3) 0.047(2) Uani 1 1 d . . .
H118 H 1.0452 0.7623 0.3051 0.062 Uiso 1 1 calc R . .
C119 C 1.1075(4) 0.8052(4) 0.3197(2) 0.046(2) Uani 1 1 d . . .
H119 H 1.1011 0.8029 0.3442 0.061 Uiso 1 1 calc R . .
C120 C 1.1510(4) 0.8330(4) 0.3072(3) 0.046(2) Uani 1 1 d . . .
H120 H 1.1740 0.8496 0.3233 0.061 Uiso 1 1 calc R . .
C121 C 1.1610(4) 0.8364(3) 0.2704(2) 0.036(2) Uani 1 1 d . . .
H121 H 1.1912 0.8546 0.2623 0.048 Uiso 1 1 calc R . .
C122 C 1.1737(3) 0.8585(3) 0.19369(19) 0.0241(16) Uani 1 1 d . . .
C123 C 1.1571(3) 0.9086(3) 0.1861(2) 0.0296(18) Uani 1 1 d . . .
H123 H 1.1204 0.9167 0.1874 0.039 Uiso 1 1 calc R . .
C124 C 1.1930(3) 0.9465(3) 0.1770(2) 0.0307(19) Uani 1 1 d . . .
H124 H 1.1806 0.9798 0.1722 0.041 Uiso 1 1 calc R . .
C125 C 1.2481(4) 0.9353(3) 0.1747(2) 0.035(2) Uani 1 1 d . . .
H125 H 1.2728 0.9609 0.1682 0.047 Uiso 1 1 calc R . .
C126 C 1.2658(3) 0.8853(3) 0.1824(2) 0.033(2) Uani 1 1 d . . .
H126 H 1.3026 0.8775 0.1811 0.044 Uiso 1 1 calc R . .
C127 C 1.2289(3) 0.8470(3) 0.1920(2) 0.0300(18) Uani 1 1 d . . .
H127 H 1.2410 0.8137 0.1972 0.040 Uiso 1 1 calc R . .
C128 C 1.1982(3) 0.6315(3) 0.2084(2) 0.0322(19) Uani 1 1 d . . .
C129 C 1.2515(3) 0.6441(4) 0.2270(2) 0.036(2) Uani 1 1 d . . .
H129a H 1.2787 0.6517 0.2093 0.053 Uiso 1 1 calc R . .
H129b H 1.2629 0.6149 0.2412 0.053 Uiso 1 1 calc R . .
H129c H 1.2466 0.6737 0.2424 0.053 Uiso 1 1 calc R . .
C130 C 1.2071(4) 0.5829(3) 0.1853(3) 0.045(2) Uani 1 1 d . . .
H130a H 1.1742 0.5747 0.1727 0.068 Uiso 1 1 calc R . .
H130b H 1.2170 0.5543 0.2004 0.068 Uiso 1 1 calc R . .
H130c H 1.2355 0.5893 0.1682 0.068 Uiso 1 1 calc R . .
C131 C 1.1545(4) 0.6185(4) 0.2367(3) 0.044(2) Uani 1 1 d . . .
H131a H 1.1498 0.6475 0.2525 0.066 Uiso 1 1 calc R . .
H131b H 1.1658 0.5888 0.2504 0.066 Uiso 1 1 calc R . .
H131c H 1.1208 0.6110 0.2249 0.066 Uiso 1 1 calc R . .
C132 C 1.1538(3) 0.7204(3) 0.0900(2) 0.0291(18) Uani 1 1 d . . .
H132 H 1.1281 0.7474 0.0827 0.039 Uiso 1 1 calc R . .
C133 C 1.1367(3) 0.6715(3) 0.0705(2) 0.0305(18) Uani 1 1 d . . .
C134 C 1.1719(4) 0.6296(3) 0.0667(2) 0.036(2) Uani 1 1 d . . .
H134 H 1.2060 0.6309 0.0774 0.047 Uiso 1 1 calc R . .
C135 C 1.1572(4) 0.5867(4) 0.0475(3) 0.047(2) Uani 1 1 d . . .
H135 H 1.1810 0.5589 0.0454 0.062 Uiso 1 1 calc R . .
C136 C 1.1062(5) 0.5847(4) 0.0310(3) 0.056(3) Uani 1 1 d . . .
H136 H 1.0961 0.5561 0.0173 0.075 Uiso 1 1 calc R . .
C137 C 1.0720(4) 0.6252(4) 0.0353(3) 0.048(3) Uani 1 1 d . . .
H137 H 1.0377 0.6236 0.0249 0.064 Uiso 1 1 calc R . .
C138 C 1.0862(4) 0.6687(4) 0.0545(2) 0.044(2) Uani 1 1 d . . .
H138 H 1.0620 0.6961 0.0567 0.058 Uiso 1 1 calc R . .
C139 C 1.2097(3) 0.7393(3) 0.0784(2) 0.0309(19) Uani 1 1 d . . .
C140 C 1.2470(3) 0.7623(3) 0.1025(2) 0.0331(19) Uani 1 1 d . . .
H140 H 1.2379 0.7652 0.1266 0.044 Uiso 1 1 calc R . .
C141 C 1.2964(4) 0.7804(4) 0.0909(3) 0.046(2) Uani 1 1 d . . .
H141 H 1.3199 0.7958 0.1073 0.062 Uiso 1 1 calc R . .
C142 C 1.3117(5) 0.7763(4) 0.0559(3) 0.054(3) Uani 1 1 d . . .
H142 H 1.3455 0.7882 0.0484 0.072 Uiso 1 1 calc R . .
C143 C 1.2759(4) 0.7538(3) 0.0317(3) 0.044(3) Uani 1 1 d . . .
H143 H 1.2856 0.7508 0.0076 0.059 Uiso 1 1 calc R . .
C144 C 1.2260(4) 0.7360(3) 0.0429(2) 0.036(2) Uani 1 1 d . . .
H144 H 1.2025 0.7214 0.0262 0.048 Uiso 1 1 calc R . .
C145 C 0.9924(3) 0.3158(3) 0.10123(18) 0.077(3) Uani 1 1 d GU . .
C146 C 0.9514(3) 0.3175(3) 0.07546(18) 0.085(3) Uani 1 1 d GU . .
H146 H 0.9434 0.3485 0.0639 0.114 Uiso 1 1 calc R . .
C147 C 0.9223(3) 0.2728(4) 0.06707(19) 0.079(4) Uani 1 1 d GU . .
H147 H 0.8949 0.2739 0.0499 0.105 Uiso 1 1 calc R . .
C148 C 0.9343(3) 0.2263(3) 0.0844(2) 0.098(4) Uani 1 1 d GU . .
H148 H 0.9150 0.1964 0.0788 0.130 Uiso 1 1 calc R . .
C149 C 0.9753(4) 0.2245(3) 0.1102(2) 0.085(3) Uani 1 1 d GU . .
H149 H 0.9833 0.1936 0.1218 0.113 Uiso 1 1 calc R . .
C150 C 1.0044(3) 0.2693(3) 0.11860(19) 0.082(3) Uani 1 1 d GU . .
H150 H 1.0317 0.2682 0.1358 0.109 Uiso 1 1 calc R . .
C151 C 1.0245(4) 0.3653(3) 0.1105(3) 0.145(8) Uani 1 1 d GU . .
H151a H 1.0113 0.3936 0.0963 0.217 Uiso 1 1 calc R . .
H151b H 1.0623 0.3598 0.1055 0.217 Uiso 1 1 calc R . .
H151c H 1.0199 0.3732 0.1355 0.217 Uiso 1 1 calc R . .


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 N1 1.876(6) . ?
Nb1 N2 1.882(6) . ?
Nb1 O2 1.912(5) . ?
Nb1 O1 1.920(5) . ?
Nb1 Nb2 2.7753(9) . ?
Nb2 O4 1.881(5) . ?
Nb2 N2 1.889(6) . ?
Nb2 N1 1.900(6) . ?
Nb2 O3 1.925(5) . ?
O1 C1 1.375(8) . ?
O2 C37 1.395(9) . ?
O3 C73 1.353(8) . ?
O4 C109 1.394(9) . ?
C1 C6 1.374(10) . ?
C1 C2 1.398(10) . ?
C2 C3 1.379(10) . ?
C2 C7 1.549(10) . ?
C3 C4 1.393(10) . ?
C4 C5 1.396(10) . ?
C4 C20 1.523(10) . ?
C5 C6 1.397(10) . ?
C6 C24 1.543(10) . ?
C7 C8 1.515(11) . ?
C7 C14 1.528(10) . ?
C8 C13 1.382(10) . ?
C8 C9 1.400(11) . ?
C9 C10 1.391(11) . ?
C10 C11 1.390(12) . ?
C11 C12 1.388(12) . ?
C12 C13 1.379(11) . ?
C14 C19 1.371(11) . ?
C14 C15 1.413(12) . ?
C15 C16 1.386(12) . ?
C16 C17 1.392(13) . ?
C17 C18 1.342(13) . ?
C18 C19 1.406(11) . ?
C20 C23 1.511(11) . ?
C20 C21 1.522(11) . ?
C20 C22 1.542(11) . ?
C24 C31 1.518(11) . ?
C24 C25 1.526(11) . ?
C25 C26 1.372(12) . ?
C25 C30 1.416(11) . ?
C26 C27 1.381(12) . ?
C27 C28 1.385(13) . ?
C28 C29 1.380(14) . ?
C29 C30 1.380(13) . ?
C31 C32 1.374(12) . ?
C31 C36 1.406(12) . ?
C32 C33 1.422(12) . ?
C33 C34 1.356(14) . ?
C34 C35 1.401(14) . ?
C35 C36 1.392(12) . ?
C37 C38 1.402(11) . ?
C37 C42 1.405(10) . ?
C38 C39 1.389(10) . ?
C38 C43 1.511(10) . ?
C39 C40 1.382(11) . ?
C40 C41 1.450(11) . ?
C40 C56 1.547(11) . ?
C41 C42 1.368(10) . ?
C42 C60 1.527(10) . ?
C43 C50 1.530(11) . ?
C43 C44 1.533(10) . ?
C44 C49 1.369(12) . ?
C44 C45 1.394(11) . ?
C45 C46 1.384(13) . ?
C46 C47 1.400(16) . ?
C47 C48 1.327(17) . ?
C48 C49 1.390(13) . ?
C50 C51 1.370(11) . ?
C50 C55 1.396(11) . ?
C51 C52 1.364(12) . ?
C52 C53 1.386(13) . ?
C53 C54 1.351(13) . ?
C54 C55 1.385(13) . ?
C56 C57 1.488(13) . ?
C56 C58 1.516(12) . ?
C56 C59 1.567(14) . ?
C60 C61 1.494(10) . ?
C60 C67 1.516(10) . ?
C61 C66 1.396(11) . ?
C61 C62 1.415(12) . ?
C62 C63 1.367(12) . ?
C63 C64 1.361(14) . ?
C64 C65 1.402(14) . ?
C65 C66 1.396(12) . ?
C67 C72 1.386(11) . ?
C67 C68 1.412(11) . ?
C68 C69 1.401(12) . ?
C69 C70 1.365(13) . ?
C70 C71 1.371(13) . ?
C71 C72 1.392(11) . ?
C73 C78 1.395(10) . ?
C73 C74 1.395(10) . ?
C74 C75 1.393(10) . ?
C74 C79 1.541(10) . ?
C75 C76 1.382(11) . ?
C76 C77 1.377(11) . ?
C76 C92 1.530(11) . ?
C77 C78 1.400(11) . ?
C78 C96 1.532(10) . ?
C79 C80 1.506(11) . ?
C79 C86 1.535(10) . ?
C80 C81 1.391(11) . ?
C80 C85 1.402(11) . ?
C81 C82 1.400(12) . ?
C82 C83 1.365(13) . ?
C83 C84 1.369(14) . ?
C84 C85 1.375(12) . ?
C86 C91 1.371(11) . ?
C86 C87 1.394(11) . ?
C87 C88 1.403(12) . ?
C88 C89 1.365(13) . ?
C89 C90 1.370(12) . ?
C90 C91 1.382(11) . ?
C92 C95 1.450(14) . ?
C92 C93 1.474(14) . ?
C92 C94 1.491(17) . ?
C96 C103 1.504(10) . ?
C96 C97 1.518(11) . ?
C97 C98 1.371(11) . ?
C97 C102 1.419(12) . ?
C98 C99 1.407(12) . ?
C99 C100 1.361(13) . ?
C100 C101 1.375(13) . ?
C101 C102 1.379(12) . ?
C103 C108 1.382(11) . ?
C103 C104 1.387(11) . ?
C104 C105 1.351(12) . ?
C105 C106 1.393(14) . ?
C106 C107 1.347(13) . ?
C107 C108 1.394(12) . ?
C109 C114 1.397(10) . ?
C109 C110 1.399(10) . ?
C110 C111 1.377(11) . ?
C110 C115 1.527(10) . ?
C111 C112 1.394(11) . ?
C112 C113 1.399(11) . ?
C112 C128 1.516(11) . ?
C113 C114 1.389(11) . ?
C114 C132 1.509(11) . ?
C115 C122 1.520(11) . ?
C115 C116 1.534(11) . ?
C116 C121 1.379(11) . ?
C116 C117 1.382(12) . ?
C117 C118 1.401(13) . ?
C118 C119 1.334(13) . ?
C119 C120 1.370(14) . ?
C120 C121 1.395(12) . ?
C122 C123 1.386(11) . ?
C122 C127 1.392(11) . ?
C123 C124 1.361(11) . ?
C124 C125 1.392(12) . ?
C125 C126 1.391(12) . ?
C126 C127 1.390(11) . ?
C128 C129 1.522(11) . ?
C128 C130 1.537(12) . ?
C128 C131 1.543(12) . ?
C132 C133 1.516(11) . ?
C132 C139 1.525(12) . ?
C133 C138 1.381(12) . ?
C133 C134 1.394(12) . ?
C134 C135 1.367(12) . ?
C135 C136 1.399(15) . ?
C136 C137 1.353(14) . ?
C137 C138 1.377(13) . ?
C139 C144 1.382(11) . ?
C139 C140 1.416(12) . ?
C140 C141 1.373(12) . ?
C141 C142 1.359(14) . ?
C142 C143 1.390(15) . ?
C143 C144 1.378(13) . ?
C145 C150 1.3940 . ?
C145 C146 1.3948 . ?
C145 C151 1.5409 . ?
C146 C147 1.3948 . ?
C147 C148 1.3946 . ?
C148 C149 1.3950 . ?
C149 C150 1.3948 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Nb1 N2 85.8(3) . . ?
N1 Nb1 O2 114.4(2) . . ?
N2 Nb1 O2 116.8(2) . . ?
N1 Nb1 O1 104.2(2) . . ?
N2 Nb1 O1 113.0(2) . . ?
O2 Nb1 O1 117.5(2) . . ?
N1 Nb1 Nb2 43.03(18) . . ?
N2 Nb1 Nb2 42.72(18) . . ?
O2 Nb1 Nb2 126.40(15) . . ?
O1 Nb1 Nb2 115.57(15) . . ?
O4 Nb2 N2 114.3(2) . . ?
O4 Nb2 N1 103.1(2) . . ?
N2 Nb2 N1 84.9(2) . . ?
O4 Nb2 O3 115.0(2) . . ?
N2 Nb2 O3 120.1(2) . . ?
N1 Nb2 O3 114.0(2) . . ?
O4 Nb2 Nb1 115.84(15) . . ?
N2 Nb2 Nb1 42.52(18) . . ?
N1 Nb2 Nb1 42.36(17) . . ?
O3 Nb2 Nb1 127.79(15) . . ?
C1 O1 Nb1 137.2(5) . . ?
C37 O2 Nb1 154.0(5) . . ?
C73 O3 Nb2 156.4(4) . . ?
C109 O4 Nb2 138.9(5) . . ?
Nb1 N1 Nb2 94.6(3) . . ?
Nb1 N2 Nb2 94.8(3) . . ?
C6 C1 O1 118.9(6) . . ?
C6 C1 C2 121.4(7) . . ?
O1 C1 C2 119.7(6) . . ?
C3 C2 C1 118.1(7) . . ?
C3 C2 C7 122.1(7) . . ?
C1 C2 C7 119.8(7) . . ?
C2 C3 C4 122.8(7) . . ?
C3 C4 C5 117.2(7) . . ?
C3 C4 C20 119.9(7) . . ?
C5 C4 C20 122.9(7) . . ?
C4 C5 C6 121.6(7) . . ?
C1 C6 C5 118.9(7) . . ?
C1 C6 C24 120.0(7) . . ?
C5 C6 C24 120.7(7) . . ?
C8 C7 C14 111.6(6) . . ?
C8 C7 C2 112.2(6) . . ?
C14 C7 C2 112.0(6) . . ?
C13 C8 C9 118.3(7) . . ?
C13 C8 C7 119.9(7) . . ?
C9 C8 C7 121.6(7) . . ?
C10 C9 C8 121.1(8) . . ?
C11 C10 C9 119.1(8) . . ?
C12 C11 C10 120.2(8) . . ?
C13 C12 C11 119.9(8) . . ?
C12 C13 C8 121.4(8) . . ?
C19 C14 C15 118.1(7) . . ?
C19 C14 C7 123.9(8) . . ?
C15 C14 C7 118.0(7) . . ?
C16 C15 C14 120.6(8) . . ?
C15 C16 C17 119.8(9) . . ?
C18 C17 C16 119.8(9) . . ?
C17 C18 C19 121.2(8) . . ?
C14 C19 C18 120.5(8) . . ?
C23 C20 C21 107.9(7) . . ?
C23 C20 C4 113.6(7) . . ?
C21 C20 C4 109.2(7) . . ?
C23 C20 C22 108.7(7) . . ?
C21 C20 C22 108.6(7) . . ?
C4 C20 C22 108.8(7) . . ?
C31 C24 C25 111.6(6) . . ?
C31 C24 C6 114.3(6) . . ?
C25 C24 C6 110.9(6) . . ?
C26 C25 C30 118.6(8) . . ?
C26 C25 C24 124.1(7) . . ?
C30 C25 C24 117.3(8) . . ?
C25 C26 C27 120.8(8) . . ?
C26 C27 C28 120.4(9) . . ?
C29 C28 C27 119.8(9) . . ?
C30 C29 C28 120.0(9) . . ?
C29 C30 C25 120.3(9) . . ?
C32 C31 C36 118.9(8) . . ?
C32 C31 C24 120.3(7) . . ?
C36 C31 C24 120.6(7) . . ?
C31 C32 C33 121.3(9) . . ?
C34 C33 C32 119.2(9) . . ?
C33 C34 C35 120.4(9) . . ?
C36 C35 C34 120.5(9) . . ?
C35 C36 C31 119.6(9) . . ?
O2 C37 C38 120.0(7) . . ?
O2 C37 C42 118.3(7) . . ?
C38 C37 C42 121.7(7) . . ?
C39 C38 C37 117.4(7) . . ?
C39 C38 C43 123.3(7) . . ?
C37 C38 C43 119.3(7) . . ?
C40 C39 C38 123.5(7) . . ?
C39 C40 C41 117.2(7) . . ?
C39 C40 C56 120.0(7) . . ?
C41 C40 C56 122.8(7) . . ?
C42 C41 C40 120.5(7) . . ?
C41 C42 C37 119.5(7) . . ?
C41 C42 C60 119.5(7) . . ?
C37 C42 C60 120.7(7) . . ?
C38 C43 C50 114.2(6) . . ?
C38 C43 C44 112.7(6) . . ?
C50 C43 C44 109.7(6) . . ?
C49 C44 C45 119.0(8) . . ?
C49 C44 C43 122.3(8) . . ?
C45 C44 C43 118.4(8) . . ?
C46 C45 C44 120.0(9) . . ?
C45 C46 C47 119.4(10) . . ?
C48 C47 C46 120.0(10) . . ?
C47 C48 C49 121.3(11) . . ?
C44 C49 C48 120.2(10) . . ?
C51 C50 C55 118.4(8) . . ?
C51 C50 C43 119.4(7) . . ?
C55 C50 C43 122.2(8) . . ?
C52 C51 C50 121.6(8) . . ?
C51 C52 C53 119.5(9) . . ?
C54 C53 C52 120.0(9) . . ?
C53 C54 C55 120.7(8) . . ?
C54 C55 C50 119.7(9) . . ?
C57 C56 C58 110.5(9) . . ?
C57 C56 C40 112.9(8) . . ?
C58 C56 C40 112.2(7) . . ?
C57 C56 C59 108.0(9) . . ?
C58 C56 C59 106.8(8) . . ?
C40 C56 C59 106.1(7) . . ?
C61 C60 C67 116.4(6) . . ?
C61 C60 C42 109.7(6) . . ?
C67 C60 C42 107.1(6) . . ?
C66 C61 C62 117.7(7) . . ?
C66 C61 C60 124.2(7) . . ?
C62 C61 C60 118.1(7) . . ?
C63 C62 C61 121.1(9) . . ?
C64 C63 C62 122.0(10) . . ?
C63 C64 C65 117.8(9) . . ?
C66 C65 C64 121.7(9) . . ?
C61 C66 C65 119.5(9) . . ?
C72 C67 C68 117.6(7) . . ?
C72 C67 C60 122.3(7) . . ?
C68 C67 C60 120.0(7) . . ?
C69 C68 C67 119.5(8) . . ?
C70 C69 C68 120.8(9) . . ?
C69 C70 C71 120.9(8) . . ?
C70 C71 C72 118.9(9) . . ?
C67 C72 C71 122.2(8) . . ?
O3 C73 C78 120.5(6) . . ?
O3 C73 C74 119.3(6) . . ?
C78 C73 C74 120.2(7) . . ?
C75 C74 C73 119.1(7) . . ?
C75 C74 C79 120.8(7) . . ?
C73 C74 C79 120.0(7) . . ?
C76 C75 C74 122.3(7) . . ?
C77 C76 C75 117.1(7) . . ?
C77 C76 C92 119.9(7) . . ?
C75 C76 C92 123.0(7) . . ?
C76 C77 C78 123.2(8) . . ?
C73 C78 C77 118.1(7) . . ?
C73 C78 C96 120.4(7) . . ?
C77 C78 C96 121.2(7) . . ?
C80 C79 C86 108.2(6) . . ?
C80 C79 C74 113.4(6) . . ?
C86 C79 C74 114.3(6) . . ?
C81 C80 C85 119.1(8) . . ?
C81 C80 C79 122.9(7) . . ?
C85 C80 C79 117.8(7) . . ?
C80 C81 C82 119.3(8) . . ?
C83 C82 C81 120.1(9) . . ?
C82 C83 C84 121.3(8) . . ?
C83 C84 C85 119.7(8) . . ?
C84 C85 C80 120.6(9) . . ?
C91 C86 C87 118.5(8) . . ?
C91 C86 C79 121.4(7) . . ?
C87 C86 C79 120.0(7) . . ?
C86 C87 C88 119.3(8) . . ?
C89 C88 C87 121.0(9) . . ?
C88 C89 C90 119.3(8) . . ?
C89 C90 C91 120.3(8) . . ?
C86 C91 C90 121.4(8) . . ?
C95 C92 C93 114.7(11) . . ?
C95 C92 C94 101.0(12) . . ?
C93 C92 C94 105.7(12) . . ?
C95 C92 C76 113.5(8) . . ?
C93 C92 C76 112.9(8) . . ?
C94 C92 C76 107.8(9) . . ?
C103 C96 C97 114.2(6) . . ?
C103 C96 C78 109.4(6) . . ?
C97 C96 C78 110.9(6) . . ?
C98 C97 C102 118.2(8) . . ?
C98 C97 C96 123.7(7) . . ?
C102 C97 C96 118.0(7) . . ?
C97 C98 C99 119.4(8) . . ?
C100 C99 C98 121.8(8) . . ?
C99 C100 C101 119.4(8) . . ?
C100 C101 C102 120.1(9) . . ?
C101 C102 C97 121.0(8) . . ?
C108 C103 C104 115.6(8) . . ?
C108 C103 C96 121.9(7) . . ?
C104 C103 C96 122.5(7) . . ?
C105 C104 C103 123.3(9) . . ?
C104 C105 C106 120.1(9) . . ?
C107 C106 C105 118.4(9) . . ?
C106 C107 C108 121.1(9) . . ?
C103 C108 C107 121.6(8) . . ?
O4 C109 C114 118.7(6) . . ?
O4 C109 C110 118.9(7) . . ?
C114 C109 C110 122.2(7) . . ?
C111 C110 C109 117.1(7) . . ?
C111 C110 C115 123.5(7) . . ?
C109 C110 C115 119.3(7) . . ?
C110 C111 C112 123.5(7) . . ?
C111 C112 C113 116.9(7) . . ?
C111 C112 C128 120.8(7) . . ?
C113 C112 C128 122.3(7) . . ?
C114 C113 C112 122.3(7) . . ?
C113 C114 C109 117.7(7) . . ?
C113 C114 C132 122.6(7) . . ?
C109 C114 C132 118.8(7) . . ?
C122 C115 C110 110.5(6) . . ?
C122 C115 C116 112.9(6) . . ?
C110 C115 C116 112.7(6) . . ?
C121 C116 C117 116.7(8) . . ?
C121 C116 C115 124.8(8) . . ?
C117 C116 C115 118.4(7) . . ?
C116 C117 C118 121.8(9) . . ?
C119 C118 C117 120.1(9) . . ?
C118 C119 C120 120.0(9) . . ?
C119 C120 C121 120.2(9) . . ?
C116 C121 C120 121.1(9) . . ?
C123 C122 C127 118.6(8) . . ?
C123 C122 C115 119.7(7) . . ?
C127 C122 C115 121.6(7) . . ?
C124 C123 C122 121.9(8) . . ?
C123 C124 C125 120.0(8) . . ?
C126 C125 C124 119.1(8) . . ?
C127 C126 C125 120.4(8) . . ?
C126 C127 C122 119.9(8) . . ?
C112 C128 C129 111.1(7) . . ?
C112 C128 C130 113.2(7) . . ?
C129 C128 C130 107.9(7) . . ?
C112 C128 C131 107.0(7) . . ?
C129 C128 C131 109.7(7) . . ?
C130 C128 C131 107.8(7) . . ?
C114 C132 C133 114.9(7) . . ?
C114 C132 C139 110.6(7) . . ?
C133 C132 C139 112.3(7) . . ?
C138 C133 C134 118.4(8) . . ?
C138 C133 C132 120.0(8) . . ?
C134 C133 C132 121.5(8) . . ?
C135 C134 C133 121.1(9) . . ?
C134 C135 C136 120.0(9) . . ?
C137 C136 C135 118.5(9) . . ?
C136 C137 C138 122.3(10) . . ?
C137 C138 C133 119.7(9) . . ?
C144 C139 C140 116.3(8) . . ?
C144 C139 C132 120.9(8) . . ?
C140 C139 C132 122.7(7) . . ?
C141 C140 C139 121.2(9) . . ?
C142 C141 C140 121.4(10) . . ?
C141 C142 C143 118.5(10) . . ?
C144 C143 C142 120.6(9) . . ?
C143 C144 C139 121.9(9) . . ?
C150 C145 C146 120.0 . . ?
C150 C145 C151 120.0 . . ?
C146 C145 C151 120.0 . . ?
C145 C146 C147 120.0 . . ?
C148 C147 C146 120.0 . . ?
C147 C148 C149 120.0 . . ?
C150 C149 C148 120.0 . . ?
C145 C150 C149 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.504
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.146
####################################################################### 
# 
# 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_12039
_database_code_depnum_ccdc_archive 'CCDC 1032678'
_audit_update_record             
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C144 H132 Cl6 Nb2 O4, 3(C7 H8)'
_chemical_formula_sum            'C165 H156 Cl6 Nb2 O4'
_chemical_formula_weight         2601.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   18.1297(8)
_cell_length_b                   15.6334(8)
_cell_length_c                   26.0900(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.396(3)
_cell_angle_gamma                90.00
_cell_volume                     7381.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3483
_cell_measurement_theta_min      4.88
_cell_measurement_theta_max      52.92

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2724
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_details      
'0.50 degree frames measured for 60 seconds each'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_detector_area_resol_mean 83.33
_diffrn_reflns_number            44783
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         61.31
_reflns_number_total             11303
_reflns_number_gt                8070
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1235P)²+8.2346P] 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         11303
_refine_ls_number_parameters     811
_refine_ls_number_restraints     262
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.2116
_refine_ls_wR_factor_gt          0.1900
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.056
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.60389(2) 0.31621(3) 0.278536(15) 0.03986(17) Uani 1 1 d . . .
Cl1 Cl 0.58528(9) 0.16659(9) 0.27530(6) 0.0614(4) Uani 1 1 d . . .
Cl2 Cl 0.47251(7) 0.31523(8) 0.30704(4) 0.0426(3) Uani 1 1 d . . .
Cl3 Cl 0.58678(6) 0.46432(8) 0.28315(4) 0.0404(3) Uani 1 1 d . . .
O1 O 0.68309(19) 0.3211(2) 0.23736(13) 0.0440(9) Uani 1 1 d . . .
C1 C 0.7258(3) 0.3193(4) 0.1946(2) 0.0472(14) Uani 1 1 d . . .
C2 C 0.7334(3) 0.3915(4) 0.1646(2) 0.0463(13) Uani 1 1 d . . .
C3 C 0.7769(3) 0.3848(4) 0.1224(2) 0.0507(14) Uani 1 1 d . . .
H3 H 0.7841 0.4343 0.1022 0.061 Uiso 1 1 calc R . .
C4 C 0.8102(3) 0.3086(5) 0.1086(2) 0.0586(17) Uani 1 1 d . . .
C5 C 0.8002(4) 0.2368(5) 0.1408(2) 0.068(2) Uani 1 1 d . . .
H5 H 0.8220 0.1839 0.1319 0.081 Uiso 1 1 calc R . .
C6 C 0.7607(3) 0.2400(4) 0.1839(2) 0.0586(17) Uani 1 1 d . A .
C7 C 0.6982(3) 0.4768(3) 0.17660(19) 0.0414(12) Uani 1 1 d . . .
H7 H 0.6669 0.4656 0.2062 0.050 Uiso 1 1 calc R . .
C8 C 0.7546(3) 0.5437(4) 0.1955(2) 0.0509(14) Uani 1 1 d . . .
C9 C 0.7328(4) 0.6279(5) 0.1984(3) 0.076(2) Uani 1 1 d . . .
H9 H 0.6838 0.6436 0.1872 0.091 Uiso 1 1 calc R . .
C10 C 0.7825(6) 0.6910(5) 0.2179(3) 0.098(3) Uani 1 1 d . . .
H10 H 0.7672 0.7490 0.2190 0.117 Uiso 1 1 calc R . .
C11 C 0.8529(5) 0.6689(7) 0.2353(4) 0.100(3) Uani 1 1 d . . .
H11 H 0.8871 0.7113 0.2473 0.120 Uiso 1 1 calc R . .
C12 C 0.8725(4) 0.5845(8) 0.2348(4) 0.113(4) Uani 1 1 d . . .
H12 H 0.9202 0.5680 0.2485 0.136 Uiso 1 1 calc R . .
C13 C 0.8246(4) 0.5231(5) 0.2150(3) 0.083(2) Uani 1 1 d . . .
H13 H 0.8402 0.4651 0.2146 0.099 Uiso 1 1 calc R . .
C14 C 0.6453(3) 0.5098(4) 0.1334(2) 0.0466(13) Uani 1 1 d . . .
C15 C 0.5704(3) 0.5082(4) 0.1397(3) 0.0664(19) Uani 1 1 d . . .
H15 H 0.5531 0.4861 0.1707 0.080 Uiso 1 1 calc R . .
C16 C 0.5204(4) 0.5377(5) 0.1025(4) 0.087(3) Uani 1 1 d . . .
H16 H 0.4692 0.5368 0.1084 0.105 Uiso 1 1 calc R . .
C17 C 0.5428(4) 0.5682(5) 0.0572(3) 0.086(2) Uani 1 1 d . . .
H17 H 0.5079 0.5864 0.0309 0.103 Uiso 1 1 calc R . .
C18 C 0.6186(5) 0.5722(6) 0.0502(3) 0.093(3) Uani 1 1 d . . .
H18 H 0.6356 0.5946 0.0192 0.111 Uiso 1 1 calc R . .
C19 C 0.6690(4) 0.5436(5) 0.0885(2) 0.075(2) Uani 1 1 d . . .
H19 H 0.7205 0.5473 0.0837 0.090 Uiso 1 1 calc R . .
C20 C 0.8533(3) 0.2983(5) 0.0603(3) 0.0643(18) Uani 1 1 d . . .
C21 C 0.8653(4) 0.3849(6) 0.0340(3) 0.096(3) Uani 1 1 d . . .
H21A H 0.8174 0.4120 0.0256 0.144 Uiso 1 1 calc R . .
H21B H 0.8909 0.3757 0.0024 0.144 Uiso 1 1 calc R . .
H21C H 0.8953 0.4220 0.0572 0.144 Uiso 1 1 calc R . .
C22 C 0.8095(4) 0.2410(6) 0.0225(3) 0.091(3) Uani 1 1 d . . .
H22A H 0.7977 0.1872 0.0395 0.136 Uiso 1 1 calc R . .
H22B H 0.8389 0.2291 -0.0070 0.136 Uiso 1 1 calc R . .
H22C H 0.7636 0.2698 0.0108 0.136 Uiso 1 1 calc R . .
C23 C 0.9286(4) 0.2573(7) 0.0738(3) 0.102(3) Uani 1 1 d . . .
H23A H 0.9564 0.2928 0.0992 0.152 Uiso 1 1 calc R . .
H23B H 0.9563 0.2527 0.0427 0.152 Uiso 1 1 calc R . .
H23C H 0.9215 0.2001 0.0880 0.152 Uiso 1 1 calc R . .
C24 C 0.7549(4) 0.1647(4) 0.2203(2) 0.068(2) Uani 1 1 d D . .
H24 H 0.7062 0.1756 0.2351 0.082 Uiso 0.643(5) 1 calc PR A 1
H24D H 0.7046 0.1516 0.2319 0.082 Uiso 0.357(5) 1 calc PR A 2
C25 C 0.7432(4) 0.0710(3) 0.1966(3) 0.058(2) Uani 0.643(5) 1 d PGDU A 1
C26 C 0.8046(3) 0.0240(5) 0.1839(3) 0.078(3) Uani 0.643(5) 1 d PGU A 1
H26 H 0.8528 0.0473 0.1898 0.094 Uiso 0.643(5) 1 calc PR A 1
C27 C 0.7956(5) -0.0571(5) 0.1627(3) 0.094(3) Uani 0.643(5) 1 d PGU A 1
H27 H 0.8375 -0.0893 0.1540 0.112 Uiso 0.643(5) 1 calc PR A 1
C28 C 0.7251(5) -0.0912(4) 0.1540(4) 0.106(4) Uani 0.643(5) 1 d PGU A 1
H28 H 0.7189 -0.1467 0.1395 0.127 Uiso 0.643(5) 1 calc PR A 1
C29 C 0.6637(4) -0.0442(5) 0.1666(4) 0.118(5) Uani 0.643(5) 1 d PGU A 1
H29 H 0.6155 -0.0675 0.1607 0.142 Uiso 0.643(5) 1 calc PR A 1
C30 C 0.6727(3) 0.0369(5) 0.1879(3) 0.085(3) Uani 0.643(5) 1 d PGU A 1
H30 H 0.6308 0.0691 0.1965 0.102 Uiso 0.643(5) 1 calc PR A 1
C31 C 0.8081(4) 0.1655(7) 0.2686(3) 0.053(3) Uani 0.643(5) 1 d PGDU A 1
C32 C 0.8827(4) 0.1757(6) 0.2602(3) 0.070(3) Uani 0.643(5) 1 d PGU A 1
H32 H 0.8978 0.1850 0.2264 0.084 Uiso 0.643(5) 1 calc PR A 1
C33 C 0.9350(3) 0.1722(7) 0.3013(3) 0.084(4) Uani 0.643(5) 1 d PGU A 1
H33 H 0.9859 0.1791 0.2956 0.100 Uiso 0.643(5) 1 calc PR A 1
C34 C 0.9128(5) 0.1585(7) 0.3507(3) 0.077(5) Uani 0.643(5) 1 d PGU A 1
H34 H 0.9486 0.1562 0.3788 0.092 Uiso 0.643(5) 1 calc PR A 1
C35 C 0.8383(6) 0.1484(9) 0.3591(3) 0.0600(17) Uani 0.643(5) 1 d PGU A 1
H35 H 0.8232 0.1391 0.3929 0.072 Uiso 0.643(5) 1 calc PR A 1
C36 C 0.7860(4) 0.1519(9) 0.3180(4) 0.042(2) Uani 0.643(5) 1 d PGU A 1
H36 H 0.7351 0.1450 0.3237 0.050 Uiso 0.643(5) 1 calc PR A 1
C25D C 0.7935(7) 0.0922(7) 0.1896(5) 0.058(2) Uani 0.357(5) 1 d PGDU A 2
C26D C 0.8672(6) 0.0681(8) 0.1892(5) 0.078(3) Uani 0.357(5) 1 d PGU A 2
H26D H 0.9044 0.1022 0.2064 0.094 Uiso 0.357(5) 1 calc PR A 2
C27D C 0.8866(7) -0.0057(9) 0.1636(6) 0.094(3) Uani 0.357(5) 1 d PGU A 2
H27D H 0.9370 -0.0222 0.1633 0.112 Uiso 0.357(5) 1 calc PR A 2
C28D C 0.8323(10) -0.0555(8) 0.1384(6) 0.106(4) Uani 0.357(5) 1 d PGU A 2
H28D H 0.8455 -0.1060 0.1209 0.127 Uiso 0.357(5) 1 calc PR A 2
C29D C 0.7585(9) -0.0314(9) 0.1388(7) 0.118(5) Uani 0.357(5) 1 d PGU A 2
H29D H 0.7214 -0.0654 0.1215 0.142 Uiso 0.357(5) 1 calc PR A 2
C30D C 0.7391(6) 0.0425(9) 0.1644(6) 0.085(3) Uani 0.357(5) 1 d PGU A 2
H30D H 0.6887 0.0589 0.1647 0.102 Uiso 0.357(5) 1 calc PR A 2
C31D C 0.8175(8) 0.1854(14) 0.2639(6) 0.053(3) Uani 0.357(5) 1 d PGDU A 2
C32D C 0.8826(8) 0.2325(11) 0.2668(5) 0.070(3) Uani 0.357(5) 1 d PGU A 2
H32D H 0.8979 0.2620 0.2374 0.084 Uiso 0.357(5) 1 calc PR A 2
C33D C 0.9254(7) 0.2367(11) 0.3128(6) 0.084(4) Uani 0.357(5) 1 d PGU A 2
H33D H 0.9699 0.2690 0.3147 0.100 Uiso 0.357(5) 1 calc PR A 2
C34D C 0.9030(11) 0.1937(14) 0.3558(5) 0.077(5) Uani 0.357(5) 1 d PGU A 2
H34D H 0.9323 0.1965 0.3872 0.092 Uiso 0.357(5) 1 calc PR A 2
C35D C 0.8379(12) 0.1465(16) 0.3529(6) 0.0600(17) Uani 0.357(5) 1 d PGU A 2
H35D H 0.8227 0.1171 0.3823 0.072 Uiso 0.357(5) 1 calc PR A 2
C36D C 0.7952(9) 0.1423(17) 0.3070(8) 0.042(2) Uani 0.357(5) 1 d PGU A 2
H36D H 0.7507 0.1101 0.3050 0.050 Uiso 0.357(5) 1 calc PR A 2
O2 O 0.65083(18) 0.3099(2) 0.34270(13) 0.0421(8) Uani 1 1 d . . .
C37 C 0.6950(3) 0.3046(3) 0.38772(18) 0.0386(12) Uani 1 1 d . . .
C38 C 0.7501(3) 0.3653(4) 0.39752(19) 0.0411(12) Uani 1 1 d . B .
C39 C 0.7956(3) 0.3548(4) 0.4424(2) 0.0450(13) Uani 1 1 d . . .
H39 H 0.8345 0.3946 0.4495 0.054 Uiso 1 1 calc R . .
C40 C 0.7863(3) 0.2893(4) 0.4765(2) 0.0446(13) Uani 1 1 d . C .
C41 C 0.7287(3) 0.2319(4) 0.4660(2) 0.0463(13) Uani 1 1 d . . .
H41 H 0.7208 0.1874 0.4898 0.056 Uiso 1 1 calc R . .
C42 C 0.6825(3) 0.2377(4) 0.4219(2) 0.0449(13) Uani 1 1 d . D .
C43 C 0.7616(3) 0.4425(4) 0.3630(2) 0.0464(13) Uani 1 1 d D . .
H43 H 0.7425 0.4279 0.3273 0.056 Uiso 0.334(11) 1 calc PR B 1
H43D H 0.7383 0.4273 0.3285 0.056 Uiso 0.666(11) 1 calc PR B 2
C44 C 0.8427(7) 0.4732(16) 0.3610(9) 0.052(3) Uani 0.334(11) 1 d PGD B 1
C45 C 0.8820(8) 0.4413(14) 0.3210(7) 0.076(4) Uani 0.334(11) 1 d PG B 1
H45 H 0.8580 0.4057 0.2956 0.091 Uiso 0.334(11) 1 calc PR B 1
C46 C 0.9563(8) 0.4615(16) 0.3181(8) 0.097(5) Uani 0.334(11) 1 d PG B 1
H46 H 0.9831 0.4397 0.2908 0.116 Uiso 0.334(11) 1 calc PR B 1
C47 C 0.9913(7) 0.5135(14) 0.3552(10) 0.105(6) Uani 0.334(11) 1 d PG B 1
H47 H 1.0421 0.5273 0.3533 0.126 Uiso 0.334(11) 1 calc PR B 1
C48 C 0.9521(12) 0.5454(16) 0.3952(10) 0.102(6) Uani 0.334(11) 1 d PG B 1
H48 H 0.9761 0.5810 0.4206 0.122 Uiso 0.334(11) 1 calc PR B 1
C49 C 0.8778(12) 0.5253(19) 0.3981(10) 0.071(3) Uani 0.334(11) 1 d PG B 1
H49 H 0.8510 0.5471 0.4255 0.085 Uiso 0.334(11) 1 calc PR B 1
C44D C 0.8437(3) 0.4509(7) 0.3559(4) 0.052(3) Uani 0.666(11) 1 d PGD B 2
C45D C 0.8795(4) 0.3910(7) 0.3268(3) 0.076(4) Uani 0.666(11) 1 d PG B 2
H45D H 0.8521 0.3463 0.3100 0.091 Uiso 0.666(11) 1 calc PR B 2
C46D C 0.9553(4) 0.3966(7) 0.3223(4) 0.097(5) Uani 0.666(11) 1 d PG B 2
H46D H 0.9798 0.3556 0.3024 0.116 Uiso 0.666(11) 1 calc PR B 2
C47D C 0.9954(3) 0.4620(8) 0.3469(4) 0.105(6) Uani 0.666(11) 1 d PG B 2
H47D H 1.0473 0.4658 0.3439 0.126 Uiso 0.666(11) 1 calc PR B 2
C48D C 0.9597(5) 0.5219(7) 0.3760(5) 0.102(6) Uani 0.666(11) 1 d PG B 2
H48D H 0.9871 0.5666 0.3929 0.122 Uiso 0.666(11) 1 calc PR B 2
C49D C 0.8838(5) 0.5164(8) 0.3805(5) 0.071(3) Uani 0.666(11) 1 d PG B 2
H49D H 0.8594 0.5573 0.4004 0.085 Uiso 0.666(11) 1 calc PR B 2
C50 C 0.7220(3) 0.5215(4) 0.3800(2) 0.0477(14) Uani 1 1 d . B .
C51 C 0.7126(4) 0.5889(4) 0.3458(3) 0.0695(19) Uani 1 1 d . . .
H51 H 0.7299 0.5824 0.3123 0.083 Uiso 1 1 calc R B .
C52 C 0.6806(5) 0.6622(6) 0.3575(4) 0.092(3) Uani 1 1 d . B .
H52 H 0.6750 0.7069 0.3329 0.111 Uiso 1 1 calc R . .
C53 C 0.6550(4) 0.6723(5) 0.4075(6) 0.107(4) Uani 1 1 d . . .
H53 H 0.6314 0.7241 0.4163 0.128 Uiso 1 1 calc R B .
C54 C 0.6639(4) 0.6069(6) 0.4442(4) 0.086(2) Uani 1 1 d . B .
H54 H 0.6480 0.6139 0.4780 0.103 Uiso 1 1 calc R . .
C55 C 0.6974(3) 0.5305(4) 0.4289(3) 0.0598(16) Uani 1 1 d . . .
H55 H 0.7032 0.4844 0.4525 0.072 Uiso 1 1 calc R B .
C56 C 0.8395(3) 0.2768(4) 0.5242(2) 0.0531(14) Uani 1 1 d DU . .
C57 C 0.8607(15) 0.3671(10) 0.5423(15) 0.083(5) Uani 0.407(19) 1 d PDU C 1
H57A H 0.8932 0.3635 0.5736 0.124 Uiso 0.407(19) 1 calc PR C 1
H57B H 0.8160 0.3990 0.5495 0.124 Uiso 0.407(19) 1 calc PR C 1
H57C H 0.8866 0.3964 0.5154 0.124 Uiso 0.407(19) 1 calc PR C 1
C58 C 0.9064(12) 0.2301(17) 0.5057(9) 0.078(4) Uani 0.407(19) 1 d PDU C 1
H58A H 0.9338 0.2683 0.4840 0.118 Uiso 0.407(19) 1 calc PR C 1
H58B H 0.8901 0.1796 0.4859 0.118 Uiso 0.407(19) 1 calc PR C 1
H58C H 0.9384 0.2123 0.5354 0.118 Uiso 0.407(19) 1 calc PR C 1
C59 C 0.8051(19) 0.2252(18) 0.5663(12) 0.074(5) Uani 0.407(19) 1 d PDU C 1
H59A H 0.8368 0.2287 0.5980 0.111 Uiso 0.407(19) 1 calc PR C 1
H59B H 0.8003 0.1652 0.5555 0.111 Uiso 0.407(19) 1 calc PR C 1
H59C H 0.7562 0.2483 0.5723 0.111 Uiso 0.407(19) 1 calc PR C 1
C57D C 0.8901(9) 0.3517(10) 0.5359(9) 0.083(5) Uani 0.593(19) 1 d PD C 2
H57D H 0.9240 0.3583 0.5084 0.124 Uiso 0.593(19) 1 calc PR C 2
H57E H 0.9185 0.3416 0.5685 0.124 Uiso 0.593(19) 1 calc PR C 2
H57F H 0.8606 0.4039 0.5386 0.124 Uiso 0.593(19) 1 calc PR C 2
C58D C 0.8828(9) 0.1946(10) 0.5168(6) 0.078(4) Uani 0.593(19) 1 d PD C 2
H58D H 0.9003 0.1931 0.4819 0.118 Uiso 0.593(19) 1 calc PR C 2
H58E H 0.8508 0.1451 0.5218 0.118 Uiso 0.593(19) 1 calc PR C 2
H58F H 0.9253 0.1925 0.5418 0.118 Uiso 0.593(19) 1 calc PR C 2
C59D C 0.7936(12) 0.2622(13) 0.5716(7) 0.074(5) Uani 0.593(19) 1 d PD C 2
H59D H 0.8270 0.2538 0.6021 0.111 Uiso 0.593(19) 1 calc PR C 2
H59E H 0.7625 0.2113 0.5661 0.111 Uiso 0.593(19) 1 calc PR C 2
H59F H 0.7622 0.3122 0.5767 0.111 Uiso 0.593(19) 1 calc PR C 2
C60 C 0.6207(3) 0.1726(3) 0.4097(2) 0.0509(14) Uani 1 1 d D . .
H60 H 0.6234 0.1572 0.3727 0.061 Uiso 0.689(11) 1 calc PR D 1
H60D H 0.6231 0.1592 0.3724 0.061 Uiso 0.311(11) 1 calc PR D 2
C61 C 0.6365(3) 0.0894(3) 0.4407(2) 0.0560(19) Uani 0.689(11) 1 d PRD D 1
C62 C 0.6026(3) 0.0754(3) 0.4864(2) 0.072(2) Uani 0.689(11) 1 d PRD D 1
H62 H 0.5705 0.1173 0.4992 0.087 Uiso 0.689(11) 1 calc PR D 1
C63 C 0.616(2) -0.0004(17) 0.5132(11) 0.090(3) Uani 0.689(11) 1 d PD D 1
H63 H 0.5928 -0.0096 0.5445 0.109 Uiso 0.689(11) 1 calc PR D 1
C64 C 0.662(2) -0.0624(15) 0.4952(11) 0.109(5) Uani 0.689(11) 1 d PD D 1
H64 H 0.6685 -0.1150 0.5131 0.131 Uiso 0.689(11) 1 calc PR D 1
C65 C 0.6979(12) -0.0472(9) 0.4505(8) 0.095(7) Uani 0.689(11) 1 d PD D 1
H65 H 0.7320 -0.0882 0.4390 0.115 Uiso 0.689(11) 1 calc PR D 1
C66 C 0.6844(7) 0.0283(7) 0.4222(5) 0.073(4) Uani 0.689(11) 1 d PD D 1
H66 H 0.7076 0.0377 0.3910 0.088 Uiso 0.689(11) 1 calc PR D 1
C61D C 0.6252(13) 0.0853(10) 0.4376(8) 0.0560(19) Uani 0.311(11) 1 d PD D 2
C62D C 0.5980(14) 0.0721(15) 0.4857(8) 0.072(2) Uani 0.311(11) 1 d PD D 2
H62D H 0.5688 0.1148 0.5007 0.087 Uiso 0.311(11) 1 calc PR D 2
C63D C 0.614(5) -0.004(4) 0.512(2) 0.090(3) Uani 0.311(11) 1 d PD D 2
H63D H 0.5954 -0.0126 0.5446 0.109 Uiso 0.311(11) 1 calc PR D 2
C64D C 0.656(5) -0.067(3) 0.491(2) 0.109(5) Uani 0.311(11) 1 d PD D 2
H64D H 0.6685 -0.1170 0.5096 0.131 Uiso 0.311(11) 1 calc PR D 2
C65D C 0.680(3) -0.056(2) 0.4412(18) 0.095(7) Uani 0.311(11) 1 d PD D 2
H65D H 0.7060 -0.1002 0.4256 0.115 Uiso 0.311(11) 1 calc PR D 2
C66D C 0.665(2) 0.0210(16) 0.4144(12) 0.073(4) Uani 0.311(11) 1 d PD D 2
H66D H 0.6817 0.0289 0.3809 0.088 Uiso 0.311(11) 1 calc PR D 2
C67 C 0.5429(3) 0.2076(4) 0.4157(2) 0.0505(14) Uani 1 1 d . D .
C68 C 0.4822(4) 0.1574(4) 0.3990(3) 0.0663(18) Uani 1 1 d . . .
H68 H 0.4906 0.1026 0.3846 0.080 Uiso 1 1 calc R D .
C69 C 0.4116(4) 0.1850(5) 0.4029(3) 0.071(2) Uani 1 1 d . D .
H69 H 0.3714 0.1495 0.3914 0.085 Uiso 1 1 calc R . .
C70 C 0.3984(3) 0.2640(5) 0.4232(2) 0.0623(18) Uani 1 1 d . . .
H70 H 0.3491 0.2831 0.4260 0.075 Uiso 1 1 calc R D .
C71 C 0.4566(3) 0.3154(5) 0.4396(2) 0.0633(17) Uani 1 1 d . D .
H71 H 0.4475 0.3705 0.4533 0.076 Uiso 1 1 calc R . .
C72 C 0.5293(3) 0.2865(4) 0.4360(2) 0.0542(15) Uani 1 1 d . . .
H72 H 0.5694 0.3219 0.4477 0.065 Uiso 1 1 calc R D .
C1S C 0.2288(8) 0.8990(12) 0.1890(8) 0.070(4) Uani 0.345(6) 1 d PDU D 1
H1S1 H 0.2316 0.9598 0.1801 0.105 Uiso 0.345(6) 1 calc PR D 1
H1S2 H 0.2655 0.8670 0.1706 0.105 Uiso 0.345(6) 1 calc PR D 1
H1S3 H 0.2388 0.8920 0.2261 0.105 Uiso 0.345(6) 1 calc PR D 1
C2S C 0.1535(6) 0.8660(8) 0.1740(5) 0.059(3) Uani 0.345(6) 1 d PGDU D 1
C3S C 0.0906(7) 0.8858(7) 0.1996(4) 0.065(4) Uani 0.345(6) 1 d PGU D 1
H3S H 0.0921 0.9305 0.2244 0.078 Uiso 0.345(6) 1 calc PR D 1
C4S C 0.0257(6) 0.8403(9) 0.1891(4) 0.068(4) Uani 0.345(6) 1 d PGU D 1
H4S H -0.0173 0.8538 0.2066 0.081 Uiso 0.345(6) 1 calc PR D 1
C5S C 0.0235(6) 0.7749(9) 0.1530(4) 0.061(4) Uani 0.345(6) 1 d PGU D 1
H5S H -0.0209 0.7438 0.1458 0.074 Uiso 0.345(6) 1 calc PR D 1
C6S C 0.0864(8) 0.7551(7) 0.1273(4) 0.070(4) Uani 0.345(6) 1 d PGU D 1
H6S H 0.0849 0.7104 0.1026 0.084 Uiso 0.345(6) 1 calc PR D 1
C7S C 0.1513(6) 0.8006(8) 0.1378(5) 0.051(4) Uani 0.345(6) 1 d PGU D 1
H7S H 0.1943 0.7871 0.1203 0.061 Uiso 0.345(6) 1 calc PR D 1
C1E C 0.024(3) 0.9901(16) 0.1982(16) 0.070(4) Uani 0.155(6) 1 d PDU D 2
H1E1 H -0.0069 1.0135 0.1693 0.105 Uiso 0.155(6) 1 calc PR D 2
H1E2 H 0.0661 1.0276 0.2058 0.105 Uiso 0.155(6) 1 calc PR D 2
H1E3 H -0.0059 0.9863 0.2285 0.105 Uiso 0.155(6) 1 calc PR D 2
C2E C 0.1727(12) 0.851(2) 0.1715(13) 0.059(3) Uani 0.155(6) 1 d PGU D 2
H2E H 0.2248 0.8576 0.1757 0.071 Uiso 0.155(6) 1 calc PR D 2
C3E C 0.1264(17) 0.9125(16) 0.1907(12) 0.065(4) Uani 0.155(6) 1 d PGU D 2
H3E H 0.1469 0.9613 0.2080 0.078 Uiso 0.155(6) 1 calc PR D 2
C4E C 0.0502(16) 0.9027(17) 0.1847(11) 0.068(4) Uani 0.155(6) 1 d PGDU D 2
C5E C 0.0202(12) 0.8313(19) 0.1595(12) 0.061(4) Uani 0.155(6) 1 d PGU D 2
H5E H -0.0319 0.8246 0.1554 0.074 Uiso 0.155(6) 1 calc PR D 2
C6E C 0.0665(17) 0.7697(16) 0.1403(13) 0.070(4) Uani 0.155(6) 1 d PGU D 2
H6E H 0.0460 0.7209 0.1231 0.084 Uiso 0.155(6) 1 calc PR D 2
C7E C 0.1427(16) 0.7795(18) 0.1463(14) 0.051(4) Uani 0.155(6) 1 d PGU D 2
H7E H 0.1743 0.7374 0.1332 0.061 Uiso 0.155(6) 1 calc PR D 2
C8S C 0.4856(17) 0.6898(12) 0.2705(8) 0.149(9) Uiso 0.50 1 d PDU . .
H8A H 0.5127 0.7114 0.2427 0.224 Uiso 0.50 1 d PR . .
H8B H 0.5068 0.6364 0.2822 0.224 Uiso 0.50 1 d PR . .
H8C H 0.4350 0.6810 0.2588 0.224 Uiso 0.50 1 d PR . .
C9S C 0.4895(7) 0.7550(8) 0.3132(4) 0.112(6) Uiso 0.50 1 d PGDU . .
C10S C 0.5348(7) 0.8253(9) 0.3064(4) 0.137(8) Uiso 0.50 1 d PGU . .
H10S H 0.5575 0.8330 0.2748 0.164 Uiso 0.50 1 calc PR . .
C11S C 0.5470(6) 0.8844(7) 0.3458(5) 0.101(5) Uiso 0.50 1 d PGU . .
H11S H 0.5780 0.9324 0.3411 0.122 Uiso 0.50 1 calc PR . .
C12S C 0.5139(6) 0.8732(6) 0.3920(4) 0.092(5) Uiso 0.50 1 d PGU . .
H12S H 0.5222 0.9135 0.4190 0.110 Uiso 0.50 1 calc PR . .
C13S C 0.4686(6) 0.8029(7) 0.3988(4) 0.088(5) Uiso 0.50 1 d PGU . .
H13S H 0.4459 0.7952 0.4304 0.106 Uiso 0.50 1 calc PR . .
C14S C 0.4564(6) 0.7438(6) 0.3594(5) 0.091(5) Uiso 0.50 1 d PGU . .
H14S H 0.4254 0.6957 0.3641 0.109 Uiso 0.50 1 calc PR . .
C15S C -0.1028(10) -0.037(2) 0.4572(10) 0.149(6) Uiso 0.50 1 d PDU E -1
H15A H -0.1097 -0.0092 0.4236 0.223 Uiso 0.50 1 calc PR E -1
H15B H -0.1413 -0.0178 0.4793 0.223 Uiso 0.50 1 calc PR E -1
H15C H -0.1060 -0.0992 0.4528 0.223 Uiso 0.50 1 calc PR E -1
C16S C -0.0301(6) -0.0146(11) 0.4808(5) 0.092(5) Uiso 0.50 1 d PGDU E -1
C17S C 0.0264(9) -0.0010(10) 0.4479(5) 0.122(4) Uiso 0.50 1 d PGU E -1
H17S H 0.0169 -0.0063 0.4119 0.146 Uiso 0.50 1 calc PR E -1
C18S C 0.0967(7) 0.0205(11) 0.4679(7) 0.160(7) Uiso 0.50 1 d PGU E -1
H18S H 0.1353 0.0298 0.4454 0.192 Uiso 0.50 1 calc PR E -1
C19S C 0.1106(7) 0.0283(12) 0.5206(8) 0.149(6) Uiso 0.50 1 d PGU E -1
H19S H 0.1587 0.0430 0.5342 0.179 Uiso 0.50 1 calc PR E -1
C20S C 0.0541(9) 0.0147(12) 0.5534(5) 0.160(7) Uiso 0.50 1 d PGU E -1
H20S H 0.0636 0.0200 0.5895 0.192 Uiso 0.50 1 calc PR E -1
C21S C -0.0163(8) -0.0068(11) 0.5335(5) 0.122(4) Uiso 0.50 1 d PGU E -1
H21S H -0.0549 -0.0161 0.5560 0.146 Uiso 0.50 1 calc PR E -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 O2 1.835(3) . ?
Nb1 O1 1.845(4) . ?
Nb1 Cl3 2.3402(13) . ?
Nb1 Cl1 2.3641(15) . ?
Nb1 Cl2 2.5370(14) . ?
Nb1 Cl2 2.5567(12) 2_655 ?
Cl2 Nb1 2.5567(12) 2_655 ?
O1 C1 1.395(6) . ?
C1 C2 1.384(8) . ?
C1 C6 1.427(8) . ?
C2 C3 1.396(8) . ?
C2 C7 1.518(8) . ?
C3 C4 1.392(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.419(10) . ?
C4 C20 1.531(9) . ?
C5 C6 1.371(9) . ?
C5 H5 0.9500 . ?
C6 C24 1.519(10) . ?
C7 C8 1.524(8) . ?
C7 C14 1.526(7) . ?
C7 H7 1.0000 . ?
C8 C13 1.377(9) . ?
C8 C9 1.378(9) . ?
C9 C10 1.410(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(11) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.376(8) . ?
C14 C15 1.378(8) . ?
C15 C16 1.370(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.359(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.397(11) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(10) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C22 1.520(9) . ?
C20 C23 1.531(9) . ?
C20 C21 1.538(12) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C31 1.542(8) . ?
C24 C25D 1.575(9) . ?
C24 C31D 1.593(11) . ?
C24 C25 1.599(7) . ?
C24 H24 1.0000 . ?
C24 H24D 1.0000 . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9500 . ?
C27 C28 1.3900 . ?
C27 H27 0.9500 . ?
C28 C29 1.3900 . ?
C28 H28 0.9500 . ?
C29 C30 1.3900 . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C25D C26D 1.3900 . ?
C25D C30D 1.3900 . ?
C26D C27D 1.3900 . ?
C26D H26D 0.9500 . ?
C27D C28D 1.3900 . ?
C27D H27D 0.9500 . ?
C28D C29D 1.3900 . ?
C28D H28D 0.9500 . ?
C29D C30D 1.3900 . ?
C29D H29D 0.9500 . ?
C30D H30D 0.9500 . ?
C31D C32D 1.3900 . ?
C31D C36D 1.3900 . ?
C32D C33D 1.3900 . ?
C32D H32D 0.9500 . ?
C33D C34D 1.3900 . ?
C33D H33D 0.9500 . ?
C34D C35D 1.3900 . ?
C34D H34D 0.9500 . ?
C35D C36D 1.3900 . ?
C35D H35D 0.9500 . ?
C36D H36D 0.9500 . ?
O2 C37 1.385(6) . ?
C37 C38 1.390(7) . ?
C37 C42 1.402(7) . ?
C38 C39 1.401(7) . ?
C38 C43 1.529(7) . ?
C39 C40 1.372(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.392(8) . ?
C40 C56 1.541(7) . ?
C41 C42 1.384(7) . ?
C41 H41 0.9500 . ?
C42 C60 1.532(7) . ?
C43 C50 1.509(8) . ?
C43 C44D 1.516(7) . ?
C43 C44 1.550(13) . ?
C43 H43 1.0000 . ?
C43 H43D 1.0000 . ?
C44 C45 1.3900 . ?
C44 C49 1.3900 . ?
C45 C46 1.3900 . ?
C45 H45 0.9500 . ?
C46 C47 1.3900 . ?
C46 H46 0.9500 . ?
C47 C48 1.3900 . ?
C47 H47 0.9500 . ?
C48 C49 1.3900 . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C44D C45D 1.3900 . ?
C44D C49D 1.3900 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D C47D 1.3900 . ?
C46D H46D 0.9500 . ?
C47D C48D 1.3900 . ?
C47D H47D 0.9500 . ?
C48D C49D 1.3900 . ?
C48D H48D 0.9500 . ?
C49D H49D 0.9500 . ?
C50 C55 1.381(9) . ?
C50 C51 1.386(8) . ?
C51 C52 1.327(11) . ?
C51 H51 0.9500 . ?
C52 C53 1.420(14) . ?
C52 H52 0.9500 . ?
C53 C54 1.402(13) . ?
C53 H53 0.9500 . ?
C54 C55 1.409(10) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57D 1.508(11) . ?
C56 C58 1.517(12) . ?
C56 C58D 1.525(11) . ?
C56 C59 1.525(13) . ?
C56 C57 1.531(13) . ?
C56 C59D 1.549(11) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C57D H57D 0.9800 . ?
C57D H57E 0.9800 . ?
C57D H57F 0.9800 . ?
C58D H58D 0.9800 . ?
C58D H58E 0.9800 . ?
C58D H58F 0.9800 . ?
C59D H59D 0.9800 . ?
C59D H59E 0.9800 . ?
C59D H59F 0.9800 . ?
C60 C67 1.529(8) . ?
C60 C61D 1.547(14) . ?
C60 C61 1.5508 . ?
C60 H60 1.0000 . ?
C60 H60D 1.0000 . ?
C61 C62 1.3900 . ?
C61 C66 1.396(9) . ?
C62 C63 1.389(9) . ?
C62 H62 0.9500 . ?
C63 C64 1.377(12) . ?
C63 H63 0.9500 . ?
C64 C65 1.394(14) . ?
C64 H64 0.9500 . ?
C65 C66 1.406(11) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C61D C62D 1.3901(10) . ?
C61D C66D 1.396(9) . ?
C62D C63D 1.389(9) . ?
C62D H62D 0.9500 . ?
C63D C64D 1.377(12) . ?
C63D H63D 0.9500 . ?
C64D C65D 1.394(14) . ?
C64D H64D 0.9500 . ?
C65D C66D 1.406(11) . ?
C65D H65D 0.9500 . ?
C66D H66D 0.9500 . ?
C67 C72 1.371(9) . ?
C67 C68 1.400(8) . ?
C68 C69 1.361(10) . ?
C68 H68 0.9500 . ?
C69 C70 1.371(10) . ?
C69 H69 0.9500 . ?
C70 C71 1.374(9) . ?
C70 H70 0.9500 . ?
C71 C72 1.402(8) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C1S C2S 1.490(9) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S C3S 1.3900 . ?
C2S C7S 1.3900 . ?
C3S C4S 1.3900 . ?
C3S H3S 0.9500 . ?
C4S C5S 1.3900 . ?
C4S H4S 0.9500 . ?
C5S C6S 1.3900 . ?
C5S H5S 0.9500 . ?
C6S C7S 1.3900 . ?
C6S H6S 0.9500 . ?
C7S H7S 0.9500 . ?
C1E C4E 1.497(10) . ?
C1E H1E1 0.9800 . ?
C1E H1E2 0.9800 . ?
C1E H1E3 0.9800 . ?
C2E C3E 1.3900 . ?
C2E C7E 1.3900 . ?
C2E H2E 0.9500 . ?
C3E C4E 1.3900 . ?
C3E H3E 0.9500 . ?
C4E C5E 1.3900 . ?
C5E C6E 1.3900 . ?
C5E H5E 0.9500 . ?
C6E C7E 1.3900 . ?
C6E H6E 0.9500 . ?
C7E H7E 0.9500 . ?
C8S C8S 1.22(4) 2_655 ?
C8S C9S 1.510(10) . ?
C8S H8A 0.9600 . ?
C8S H8B 0.9600 . ?
C8S H8C 0.9600 . ?
C9S C10S 1.3900 . ?
C9S C14S 1.3900 . ?
C10S C11S 1.3900 . ?
C10S H10S 0.9500 . ?
C11S C12S 1.3900 . ?
C11S H11S 0.9500 . ?
C12S C13S 1.3900 . ?
C12S H12S 0.9500 . ?
C13S C14S 1.3900 . ?
C13S H13S 0.9500 . ?
C14S H14S 0.9500 . ?
C15S C16S 1.463(10) . ?
C15S H15A 0.9800 . ?
C15S H15B 0.9800 . ?
C15S H15C 0.9800 . ?
C16S C17S 1.3900 . ?
C16S C21S 1.3900 . ?
C17S C18S 1.3900 . ?
C17S H17S 0.9500 . ?
C18S C19S 1.3900 . ?
C18S H18S 0.9500 . ?
C19S C20S 1.3900 . ?
C19S H19S 0.9500 . ?
C20S C21S 1.3900 . ?
C20S H20S 0.9500 . ?
C21S H21S 0.9500 . ?

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 101.45(15) . . ?
O2 Nb1 Cl3 93.57(11) . . ?
O1 Nb1 Cl3 95.69(11) . . ?
O2 Nb1 Cl1 92.09(11) . . ?
O1 Nb1 Cl1 97.73(12) . . ?
Cl3 Nb1 Cl1 164.10(5) . . ?
O2 Nb1 Cl2 97.18(11) . . ?
O1 Nb1 Cl2 161.34(11) . . ?
Cl3 Nb1 Cl2 82.03(4) . . ?
Cl1 Nb1 Cl2 82.53(5) . . ?
O2 Nb1 Cl2 173.83(11) . 2_655 ?
O1 Nb1 Cl2 83.79(11) . 2_655 ?
Cl3 Nb1 Cl2 89.10(4) . 2_655 ?
Cl1 Nb1 Cl2 83.92(5) . 2_655 ?
Cl2 Nb1 Cl2 77.67(4) . 2_655 ?
Nb1 Cl2 Nb1 102.33(4) . 2_655 ?
C1 O1 Nb1 162.3(3) . . ?
C2 C1 O1 121.0(5) . . ?
C2 C1 C6 122.5(5) . . ?
O1 C1 C6 116.5(5) . . ?
C1 C2 C3 117.7(5) . . ?
C1 C2 C7 122.8(5) . . ?
C3 C2 C7 119.5(5) . . ?
C4 C3 C2 122.8(6) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 116.8(6) . . ?
C3 C4 C20 123.6(6) . . ?
C5 C4 C20 119.5(6) . . ?
C6 C5 C4 123.2(6) . . ?
C6 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C5 C6 C1 116.8(6) . . ?
C5 C6 C24 122.9(6) . . ?
C1 C6 C24 120.3(5) . . ?
C2 C7 C8 112.8(4) . . ?
C2 C7 C14 113.4(4) . . ?
C8 C7 C14 112.8(5) . . ?
C2 C7 H7 105.7 . . ?
C8 C7 H7 105.7 . . ?
C14 C7 H7 105.7 . . ?
C13 C8 C9 117.7(6) . . ?
C13 C8 C7 123.0(6) . . ?
C9 C8 C7 119.0(5) . . ?
C8 C9 C10 120.5(7) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 120.3(8) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 118.6(8) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C13 121.2(9) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 121.6(8) . . ?
C12 C13 H13 119.2 . . ?
C8 C13 H13 119.2 . . ?
C19 C14 C15 118.0(6) . . ?
C19 C14 C7 123.0(5) . . ?
C15 C14 C7 119.0(5) . . ?
C16 C15 C14 121.7(7) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 121.0(7) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 118.5(7) . . ?
C16 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
C19 C18 C17 120.2(7) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C14 C19 C18 120.7(7) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C22 C20 C4 108.8(5) . . ?
C22 C20 C23 109.1(6) . . ?
C4 C20 C23 110.3(6) . . ?
C22 C20 C21 108.2(7) . . ?
C4 C20 C21 111.5(6) . . ?
C23 C20 C21 108.9(7) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C6 C24 C31 116.1(6) . . ?
C6 C24 C25D 101.0(7) . . ?
C31 C24 C25D 98.4(7) . . ?
C6 C24 C31D 102.5(9) . . ?
C31 C24 C31D 13.7(11) . . ?
C25D C24 C31D 100.9(10) . . ?
C6 C24 C25 118.8(5) . . ?
C31 C24 C25 112.7(6) . . ?
C25D C24 C25 36.6(5) . . ?
C31D C24 C25 122.3(9) . . ?
C6 C24 H24 101.9 . . ?
C31 C24 H24 101.9 . . ?
C25D C24 H24 138.5 . . ?
C31D C24 H24 107.2 . . ?
C25 C24 H24 101.9 . . ?
C6 C24 H24D 116.6 . . ?
C31 C24 H24D 106.9 . . ?
C25D C24 H24D 116.6 . . ?
C31D C24 H24D 116.6 . . ?
C25 C24 H24D 80.1 . . ?
H24 C24 H24D 22.2 . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.1(5) . . ?
C30 C25 C24 120.9(5) . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.0 . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 C24 116.1(6) . . ?
C36 C31 C24 123.8(6) . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C26D C25D C30D 120.0 . . ?
C26D C25D C24 131.0(8) . . ?
C30D C25D C24 108.6(8) . . ?
C25D C26D C27D 120.0 . . ?
C25D C26D H26D 120.0 . . ?
C27D C26D H26D 120.0 . . ?
C26D C27D C28D 120.0 . . ?
C26D C27D H27D 120.0 . . ?
C28D C27D H27D 120.0 . . ?
C27D C28D C29D 120.0 . . ?
C27D C28D H28D 120.0 . . ?
C29D C28D H28D 120.0 . . ?
C30D C29D C28D 120.0 . . ?
C30D C29D H29D 120.0 . . ?
C28D C29D H29D 120.0 . . ?
C29D C30D C25D 120.0 . . ?
C29D C30D H30D 120.0 . . ?
C25D C30D H30D 120.0 . . ?
C32D C31D C36D 120.0 . . ?
C32D C31D C24 135.5(13) . . ?
C36D C31D C24 104.5(13) . . ?
C33D C32D C31D 120.0 . . ?
C33D C32D H32D 120.0 . . ?
C31D C32D H32D 120.0 . . ?
C34D C33D C32D 120.0 . . ?
C34D C33D H33D 120.0 . . ?
C32D C33D H33D 120.0 . . ?
C33D C34D C35D 120.0 . . ?
C33D C34D H34D 120.0 . . ?
C35D C34D H34D 120.0 . . ?
C36D C35D C34D 120.0 . . ?
C36D C35D H35D 120.0 . . ?
C34D C35D H35D 120.0 . . ?
C35D C36D C31D 120.0 . . ?
C35D C36D H36D 120.0 . . ?
C31D C36D H36D 120.0 . . ?
C37 O2 Nb1 172.3(3) . . ?
O2 C37 C38 119.3(4) . . ?
O2 C37 C42 118.5(4) . . ?
C38 C37 C42 122.3(4) . . ?
C37 C38 C39 117.1(5) . . ?
C37 C38 C43 123.5(4) . . ?
C39 C38 C43 119.4(5) . . ?
C40 C39 C38 122.6(5) . . ?
C40 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C39 C40 C41 118.3(5) . . ?
C39 C40 C56 121.5(5) . . ?
C41 C40 C56 120.2(5) . . ?
C42 C41 C40 122.1(5) . . ?
C42 C41 H41 118.9 . . ?
C40 C41 H41 118.9 . . ?
C41 C42 C37 117.6(5) . . ?
C41 C42 C60 121.9(5) . . ?
C37 C42 C60 120.5(4) . . ?
C50 C43 C44D 117.0(6) . . ?
C50 C43 C38 112.8(4) . . ?
C44D C43 C38 108.0(6) . . ?
C50 C43 C44 103.1(10) . . ?
C44D C43 C44 13.9(12) . . ?
C38 C43 C44 115.3(10) . . ?
C50 C43 H43 108.4 . . ?
C44D C43 H43 101.2 . . ?
C38 C43 H43 108.4 . . ?
C44 C43 H43 108.4 . . ?
C50 C43 H43D 106.1 . . ?
C44D C43 H43D 106.1 . . ?
C38 C43 H43D 106.1 . . ?
C44 C43 H43D 113.3 . . ?
H43 C43 H43D 4.9 . . ?
C45 C44 C49 120.0 . . ?
C45 C44 C43 116.3(14) . . ?
C49 C44 C43 123.6(14) . . ?
C44 C45 C46 120.0 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C47 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C49 C48 C47 120.0 . . ?
C49 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C48 C49 C44 120.0 . . ?
C48 C49 H49 120.0 . . ?
C44 C49 H49 120.0 . . ?
C45D C44D C49D 120.0 . . ?
C45D C44D C43 120.1(7) . . ?
C49D C44D C43 119.9(7) . . ?
C46D C45D C44D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C45D C46D C47D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C47D C46D H46D 120.0 . . ?
C46D C47D C48D 120.0 . . ?
C46D C47D H47D 120.0 . . ?
C48D C47D H47D 120.0 . . ?
C49D C48D C47D 120.0 . . ?
C49D C48D H48D 120.0 . . ?
C47D C48D H48D 120.0 . . ?
C48D C49D C44D 120.0 . . ?
C48D C49D H49D 120.0 . . ?
C44D C49D H49D 120.0 . . ?
C55 C50 C51 118.9(6) . . ?
C55 C50 C43 122.7(5) . . ?
C51 C50 C43 118.3(6) . . ?
C52 C51 C50 123.1(8) . . ?
C52 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
C51 C52 C53 118.6(8) . . ?
C51 C52 H52 120.7 . . ?
C53 C52 H52 120.7 . . ?
C54 C53 C52 121.0(8) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C53 C54 C55 117.3(9) . . ?
C53 C54 H54 121.4 . . ?
C55 C54 H54 121.4 . . ?
C50 C55 C54 121.1(7) . . ?
C50 C55 H55 119.5 . . ?
C54 C55 H55 119.5 . . ?
C57D C56 C58 87.2(12) . . ?
C57D C56 C58D 111.7(8) . . ?
C58 C56 C58D 29.2(9) . . ?
C57D C56 C59 122(2) . . ?
C58 C56 C59 110.0(12) . . ?
C58D C56 C59 83.2(11) . . ?
C57D C56 C57 23.3(13) . . ?
C58 C56 C57 110.5(12) . . ?
C58D C56 C57 134.0(12) . . ?
C59 C56 C57 111.8(15) . . ?
C57D C56 C40 114.2(9) . . ?
C58 C56 C40 106.2(10) . . ?
C58D C56 C40 107.9(7) . . ?
C59 C56 C40 112.7(16) . . ?
C57 C56 C40 105.4(12) . . ?
C57D C56 C59D 107.5(11) . . ?
C58 C56 C59D 131.3(11) . . ?
C58D C56 C59D 106.4(8) . . ?
C59 C56 C59D 23.8(13) . . ?
C57 C56 C59D 91.5(18) . . ?
C40 C56 C59D 108.9(10) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
C56 C57D H57D 109.5 . . ?
C56 C57D H57E 109.5 . . ?
H57D C57D H57E 109.5 . . ?
C56 C57D H57F 109.5 . . ?
H57D C57D H57F 109.5 . . ?
H57E C57D H57F 109.5 . . ?
C56 C58D H58D 109.5 . . ?
C56 C58D H58E 109.5 . . ?
H58D C58D H58E 109.5 . . ?
C56 C58D H58F 109.5 . . ?
H58D C58D H58F 109.5 . . ?
H58E C58D H58F 109.5 . . ?
C56 C59D H59D 109.5 . . ?
C56 C59D H59E 109.5 . . ?
H59D C59D H59E 109.5 . . ?
C56 C59D H59F 109.5 . . ?
H59D C59D H59F 109.5 . . ?
H59E C59D H59F 109.5 . . ?
C67 C60 C42 114.2(5) . . ?
C67 C60 C61D 106.8(10) . . ?
C42 C60 C61D 118.0(12) . . ?
C67 C60 C61 112.9(3) . . ?
C42 C60 C61 109.8(3) . . ?
C61D C60 C61 8.3(11) . . ?
C67 C60 H60 106.5 . . ?
C42 C60 H60 106.5 . . ?
C61D C60 H60 103.8 . . ?
C61 C60 H60 106.5 . . ?
C67 C60 H60D 105.6 . . ?
C42 C60 H60D 105.6 . . ?
C61D C60 H60D 105.6 . . ?
C61 C60 H60D 108.3 . . ?
H60 C60 H60D 1.8 . . ?
C62 C61 C66 120.4(5) . . ?
C62 C61 C60 120.1 . . ?
C66 C61 C60 119.5(5) . . ?
C63 C62 C61 119.6(6) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C64 C63 C62 121.3(8) . . ?
C64 C63 H63 119.4 . . ?
C62 C63 H63 119.4 . . ?
C63 C64 C65 119.3(8) . . ?
C63 C64 H64 120.4 . . ?
C65 C64 H64 120.4 . . ?
C64 C65 C66 120.4(8) . . ?
C64 C65 H65 119.8 . . ?
C66 C65 H65 119.8 . . ?
C61 C66 C65 119.0(8) . . ?
C61 C66 H66 120.5 . . ?
C65 C66 H66 120.5 . . ?
C62D C61D C66D 120.3(5) . . ?
C62D C61D C60 123.0(14) . . ?
C66D C61D C60 116.4(12) . . ?
C63D C62D C61D 119.5(6) . . ?
C63D C62D H62D 120.2 . . ?
C61D C62D H62D 120.2 . . ?
C64D C63D C62D 121.3(8) . . ?
C64D C63D H63D 119.4 . . ?
C62D C63D H63D 119.4 . . ?
C63D C64D C65D 119.3(8) . . ?
C63D C64D H64D 120.4 . . ?
C65D C64D H64D 120.4 . . ?
C64D C65D C66D 120.4(9) . . ?
C64D C65D H65D 119.8 . . ?
C66D C65D H65D 119.8 . . ?
C61D C66D C65D 119.0(8) . . ?
C61D C66D H66D 120.5 . . ?
C65D C66D H66D 120.5 . . ?
C72 C67 C68 117.9(6) . . ?
C72 C67 C60 123.3(5) . . ?
C68 C67 C60 118.7(6) . . ?
C69 C68 C67 121.7(7) . . ?
C69 C68 H68 119.2 . . ?
C67 C68 H68 119.2 . . ?
C68 C69 C70 120.0(6) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C69 C70 C71 120.0(6) . . ?
C69 C70 H70 120.0 . . ?
C71 C70 H70 120.0 . . ?
C70 C71 C72 119.8(7) . . ?
C70 C71 H71 120.1 . . ?
C72 C71 H71 120.1 . . ?
C67 C72 C71 120.5(6) . . ?
C67 C72 H72 119.7 . . ?
C71 C72 H72 119.7 . . ?
C3S C2S C7S 120.0 . . ?
C3S C2S C1S 124.2(12) . . ?
C7S C2S C1S 114.9(12) . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3S 120.0 . . ?
C2S C3S H3S 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C3S C4S H4S 120.0 . . ?
C5S C4S H4S 120.0 . . ?
C6S C5S C4S 120.0 . . ?
C6S C5S H5S 120.0 . . ?
C4S C5S H5S 120.0 . . ?
C5S C6S C7S 120.0 . . ?
C5S C6S H6S 120.0 . . ?
C7S C6S H6S 120.0 . . ?
C6S C7S C2S 120.0 . . ?
C6S C7S H7S 120.0 . . ?
C2S C7S H7S 120.0 . . ?
C4E C1E H1E1 109.5 . . ?
C4E C1E H1E2 109.5 . . ?
H1E1 C1E H1E2 109.5 . . ?
C4E C1E H1E3 109.5 . . ?
H1E1 C1E H1E3 109.5 . . ?
H1E2 C1E H1E3 109.5 . . ?
C3E C2E C7E 120.0 . . ?
C3E C2E H2E 120.0 . . ?
C7E C2E H2E 120.0 . . ?
C4E C3E C2E 120.0 . . ?
C4E C3E H3E 120.0 . . ?
C2E C3E H3E 120.0 . . ?
C3E C4E C5E 120.0 . . ?
C3E C4E C1E 102(3) . . ?
C5E C4E C1E 136(3) . . ?
C4E C5E C6E 120.0 . . ?
C4E C5E H5E 120.0 . . ?
C6E C5E H5E 120.0 . . ?
C7E C6E C5E 120.0 . . ?
C7E C6E H6E 120.0 . . ?
C5E C6E H6E 120.0 . . ?
C6E C7E C2E 120.0 . . ?
C6E C7E H7E 120.0 . . ?
C2E C7E H7E 120.0 . . ?
C8S C8S C9S 130.2(19) 2_655 . ?
C8S C8S H8A 22.0 2_655 . ?
C9S C8S H8A 108.4 . . ?
C8S C8S H8B 95.5 2_655 . ?
C9S C8S H8B 110.6 . . ?
H8A C8S H8B 109.5 . . ?
C8S C8S H8C 99.9 2_655 . ?
C9S C8S H8C 109.4 . . ?
H8A C8S H8C 109.5 . . ?
H8B C8S H8C 109.5 . . ?
C10S C9S C14S 120.0 . . ?
C10S C9S C8S 116.2(13) . . ?
C14S C9S C8S 123.5(12) . . ?
C9S C10S C11S 120.0 . . ?
C9S C10S H10S 120.0 . . ?
C11S C10S H10S 120.0 . . ?
C12S C11S C10S 120.0 . . ?
C12S C11S H11S 120.0 . . ?
C10S C11S H11S 120.0 . . ?
C11S C12S C13S 120.0 . . ?
C11S C12S H12S 120.0 . . ?
C13S C12S H12S 120.0 . . ?
C14S C13S C12S 120.0 . . ?
C14S C13S H13S 120.0 . . ?
C12S C13S H13S 120.0 . . ?
C13S C14S C9S 120.0 . . ?
C13S C14S H14S 120.0 . . ?
C9S C14S H14S 120.0 . . ?
C17S C16S C21S 120.0 . . ?
C17S C16S C15S 117.1(14) . . ?
C21S C16S C15S 122.9(14) . . ?
C18S C17S C16S 120.0 . . ?
C18S C17S H17S 120.0 . . ?
C16S C17S H17S 120.0 . . ?
C17S C18S C19S 120.0 . . ?
C17S C18S H18S 120.0 . . ?
C19S C18S H18S 120.0 . . ?
C20S C19S C18S 120.0 . . ?
C20S C19S H19S 120.0 . . ?
C18S C19S H19S 120.0 . . ?
C21S C20S C19S 120.0 . . ?
C21S C20S H20S 120.0 . . ?
C19S C20S H20S 120.0 . . ?
C20S C21S C16S 120.0 . . ?
C20S C21S H21S 120.0 . . ?
C16S C21S H21S 120.0 . . ?

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 Cl2 Nb1 -177.26(11) . . . 2_655 ?
O1 Nb1 Cl2 Nb1 6.0(4) . . . 2_655 ?
Cl3 Nb1 Cl2 Nb1 90.12(5) . . . 2_655 ?
Cl1 Nb1 Cl2 Nb1 -86.08(5) . . . 2_655 ?
Cl2 Nb1 Cl2 Nb1 -0.71(6) 2_655 . . 2_655 ?
O2 Nb1 O1 C1 166.2(11) . . . . ?
Cl3 Nb1 O1 C1 -99.0(11) . . . . ?
Cl1 Nb1 O1 C1 72.4(11) . . . . ?
Cl2 Nb1 O1 C1 -17.1(14) . . . . ?
Cl2 Nb1 O1 C1 -10.5(11) 2_655 . . . ?
Nb1 O1 C1 C2 85.5(13) . . . . ?
Nb1 O1 C1 C6 -94.6(11) . . . . ?
O1 C1 C2 C3 -179.9(5) . . . . ?
C6 C1 C2 C3 0.2(8) . . . . ?
O1 C1 C2 C7 1.7(8) . . . . ?
C6 C1 C2 C7 -178.3(5) . . . . ?
C1 C2 C3 C4 2.3(8) . . . . ?
C7 C2 C3 C4 -179.1(5) . . . . ?
C2 C3 C4 C5 -2.2(8) . . . . ?
C2 C3 C4 C20 175.3(5) . . . . ?
C3 C4 C5 C6 -0.6(9) . . . . ?
C20 C4 C5 C6 -178.2(6) . . . . ?
C4 C5 C6 C1 2.9(9) . . . . ?
C4 C5 C6 C24 -175.5(6) . . . . ?
C2 C1 C6 C5 -2.7(9) . . . . ?
O1 C1 C6 C5 177.3(5) . . . . ?
C2 C1 C6 C24 175.7(5) . . . . ?
O1 C1 C6 C24 -4.2(8) . . . . ?
C1 C2 C7 C8 109.1(6) . . . . ?
C3 C2 C7 C8 -69.4(6) . . . . ?
C1 C2 C7 C14 -121.1(6) . . . . ?
C3 C2 C7 C14 60.4(7) . . . . ?
C2 C7 C8 C13 -19.2(8) . . . . ?
C14 C7 C8 C13 -149.3(6) . . . . ?
C2 C7 C8 C9 167.6(6) . . . . ?
C14 C7 C8 C9 37.5(7) . . . . ?
C13 C8 C9 C10 3.6(11) . . . . ?
C7 C8 C9 C10 177.2(7) . . . . ?
C8 C9 C10 C11 -1.4(13) . . . . ?
C9 C10 C11 C12 -2.2(15) . . . . ?
C10 C11 C12 C13 3.4(16) . . . . ?
C11 C12 C13 C8 -1.1(15) . . . . ?
C9 C8 C13 C12 -2.4(12) . . . . ?
C7 C8 C13 C12 -175.7(8) . . . . ?
C2 C7 C14 C19 -74.1(8) . . . . ?
C8 C7 C14 C19 55.7(8) . . . . ?
C2 C7 C14 C15 107.8(6) . . . . ?
C8 C7 C14 C15 -122.4(6) . . . . ?
C19 C14 C15 C16 1.2(11) . . . . ?
C7 C14 C15 C16 179.3(7) . . . . ?
C14 C15 C16 C17 1.3(13) . . . . ?
C15 C16 C17 C18 -2.7(13) . . . . ?
C16 C17 C18 C19 1.5(13) . . . . ?
C15 C14 C19 C18 -2.3(11) . . . . ?
C7 C14 C19 C18 179.6(7) . . . . ?
C17 C18 C19 C14 1.0(13) . . . . ?
C3 C4 C20 C22 -110.5(7) . . . . ?
C5 C4 C20 C22 67.0(8) . . . . ?
C3 C4 C20 C23 129.9(7) . . . . ?
C5 C4 C20 C23 -52.6(8) . . . . ?
C3 C4 C20 C21 8.8(8) . . . . ?
C5 C4 C20 C21 -173.7(6) . . . . ?
C5 C6 C24 C31 97.6(8) . . . . ?
C1 C6 C24 C31 -80.7(8) . . . . ?
C5 C6 C24 C25D -7.5(9) . . . . ?
C1 C6 C24 C25D 174.2(7) . . . . ?
C5 C6 C24 C31D 96.5(10) . . . . ?
C1 C6 C24 C31D -81.9(10) . . . . ?
C5 C6 C24 C25 -41.8(9) . . . . ?
C1 C6 C24 C25 139.9(6) . . . . ?
C6 C24 C25 C26 85.6(7) . . . . ?
C31 C24 C25 C26 -55.1(8) . . . . ?
C25D C24 C25 C26 17.6(9) . . . . ?
C31D C24 C25 C26 -44.1(12) . . . . ?
C6 C24 C25 C30 -93.5(7) . . . . ?
C31 C24 C25 C30 125.8(6) . . . . ?
C25D C24 C25 C30 -161.6(11) . . . . ?
C31D C24 C25 C30 136.8(10) . . . . ?
C30 C25 C26 C27 0.0 . . . . ?
C24 C25 C26 C27 -179.2(6) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
C24 C25 C30 C29 179.1(7) . . . . ?
C6 C24 C31 C32 -53.1(9) . . . . ?
C25D C24 C31 C32 53.6(9) . . . . ?
C31D C24 C31 C32 -48(4) . . . . ?
C25 C24 C31 C32 88.7(8) . . . . ?
C6 C24 C31 C36 130.8(6) . . . . ?
C25D C24 C31 C36 -122.5(8) . . . . ?
C31D C24 C31 C36 136(5) . . . . ?
C25 C24 C31 C36 -87.4(8) . . . . ?
C36 C31 C32 C33 0.0 . . . . ?
C24 C31 C32 C33 -176.3(8) . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C31 0.0 . . . . ?
C32 C31 C36 C35 0.0 . . . . ?
C24 C31 C36 C35 176.0(9) . . . . ?
C6 C24 C25D C26D 88.3(11) . . . . ?
C31 C24 C25D C26D -30.5(12) . . . . ?
C31D C24 C25D C26D -16.9(14) . . . . ?
C25 C24 C25D C26D -147.7(16) . . . . ?
C6 C24 C25D C30D -99.4(8) . . . . ?
C31 C24 C25D C30D 141.8(8) . . . . ?
C31D C24 C25D C30D 155.5(11) . . . . ?
C25 C24 C25D C30D 24.7(8) . . . . ?
C30D C25D C26D C27D 0.0 . . . . ?
C24 C25D C26D C27D 171.6(13) . . . . ?
C25D C26D C27D C28D 0.0 . . . . ?
C26D C27D C28D C29D 0.0 . . . . ?
C27D C28D C29D C30D 0.0 . . . . ?
C28D C29D C30D C25D 0.0 . . . . ?
C26D C25D C30D C29D 0.0 . . . . ?
C24 C25D C30D C29D -173.4(10) . . . . ?
C6 C24 C31D C32D -24.7(19) . . . . ?
C31 C24 C31D C32D 160(6) . . . . ?
C25D C24 C31D C32D 79.3(18) . . . . ?
C25 C24 C31D C32D 111.6(17) . . . . ?
C6 C24 C31D C36D 155.4(8) . . . . ?
C31 C24 C31D C36D -20(4) . . . . ?
C25D C24 C31D C36D -100.6(10) . . . . ?
C25 C24 C31D C36D -68.3(11) . . . . ?
C36D C31D C32D C33D 0.0 . . . . ?
C24 C31D C32D C33D -179.9(19) . . . . ?
C31D C32D C33D C34D 0.0 . . . . ?
C32D C33D C34D C35D 0.0 . . . . ?
C33D C34D C35D C36D 0.0 . . . . ?
C34D C35D C36D C31D 0.0 . . . . ?
C32D C31D C36D C35D 0.0 . . . . ?
C24 C31D C36D C35D 179.9(14) . . . . ?
O1 Nb1 O2 C37 -4(3) . . . . ?
Cl3 Nb1 O2 C37 -101(2) . . . . ?
Cl1 Nb1 O2 C37 94(2) . . . . ?
Cl2 Nb1 O2 C37 177(2) . . . . ?
Cl2 Nb1 O2 C37 144(2) 2_655 . . . ?
Nb1 O2 C37 C38 57(3) . . . . ?
Nb1 O2 C37 C42 -123(2) . . . . ?
O2 C37 C38 C39 -177.0(5) . . . . ?
C42 C37 C38 C39 2.9(8) . . . . ?
O2 C37 C38 C43 4.6(8) . . . . ?
C42 C37 C38 C43 -175.5(5) . . . . ?
C37 C38 C39 C40 -1.6(8) . . . . ?
C43 C38 C39 C40 176.8(5) . . . . ?
C38 C39 C40 C41 -0.7(9) . . . . ?
C38 C39 C40 C56 177.0(5) . . . . ?
C39 C40 C41 C42 1.9(9) . . . . ?
C56 C40 C41 C42 -175.8(5) . . . . ?
C40 C41 C42 C37 -0.6(8) . . . . ?
C40 C41 C42 C60 178.0(5) . . . . ?
O2 C37 C42 C41 178.1(5) . . . . ?
C38 C37 C42 C41 -1.8(8) . . . . ?
O2 C37 C42 C60 -0.6(7) . . . . ?
C38 C37 C42 C60 179.5(5) . . . . ?
C37 C38 C43 C50 93.6(6) . . . . ?
C39 C38 C43 C50 -84.7(6) . . . . ?
C37 C38 C43 C44D -135.5(7) . . . . ?
C39 C38 C43 C44D 46.2(8) . . . . ?
C37 C38 C43 C44 -148.3(11) . . . . ?
C39 C38 C43 C44 33.4(12) . . . . ?
C50 C43 C44 C45 -142.1(14) . . . . ?
C44D C43 C44 C45 33(4) . . . . ?
C38 C43 C44 C45 94.5(15) . . . . ?
C50 C43 C44 C49 41.9(12) . . . . ?
C44D C43 C44 C49 -143(5) . . . . ?
C38 C43 C44 C49 -81.5(13) . . . . ?
C49 C44 C45 C46 0.0 . . . . ?
C43 C44 C45 C46 -176.1(17) . . . . ?
C44 C45 C46 C47 0.0 . . . . ?
C45 C46 C47 C48 0.0 . . . . ?
C46 C47 C48 C49 0.0 . . . . ?
C47 C48 C49 C44 0.0 . . . . ?
C45 C44 C49 C48 0.0 . . . . ?
C43 C44 C49 C48 175.8(18) . . . . ?
C50 C43 C44D C45D -161.4(6) . . . . ?
C38 C43 C44D C45D 70.0(8) . . . . ?
C44 C43 C44D C45D -166(6) . . . . ?
C50 C43 C44D C49D 21.6(7) . . . . ?
C38 C43 C44D C49D -107.0(6) . . . . ?
C44 C43 C44D C49D 17(5) . . . . ?
C49D C44D C45D C46D 0.0 . . . . ?
C43 C44D C45D C46D -177.0(8) . . . . ?
C44D C45D C46D C47D 0.0 . . . . ?
C45D C46D C47D C48D 0.0 . . . . ?
C46D C47D C48D C49D 0.0 . . . . ?
C47D C48D C49D C44D 0.0 . . . . ?
C45D C44D C49D C48D 0.0 . . . . ?
C43 C44D C49D C48D 177.0(8) . . . . ?
C44D C43 C50 C55 -107.9(7) . . . . ?
C38 C43 C50 C55 18.3(7) . . . . ?
C44 C43 C50 C55 -106.7(10) . . . . ?
C44D C43 C50 C51 69.4(8) . . . . ?
C38 C43 C50 C51 -164.3(5) . . . . ?
C44 C43 C50 C51 70.7(10) . . . . ?
C55 C50 C51 C52 -0.3(10) . . . . ?
C43 C50 C51 C52 -177.8(6) . . . . ?
C50 C51 C52 C53 0.2(12) . . . . ?
C51 C52 C53 C54 0.8(12) . . . . ?
C52 C53 C54 C55 -1.6(11) . . . . ?
C51 C50 C55 C54 -0.6(9) . . . . ?
C43 C50 C55 C54 176.8(5) . . . . ?
C53 C54 C55 C50 1.5(9) . . . . ?
C39 C40 C56 C57D 13.0(12) . . . . ?
C41 C40 C56 C57D -169.4(11) . . . . ?
C39 C40 C56 C58 -81.3(13) . . . . ?
C41 C40 C56 C58 96.3(13) . . . . ?
C39 C40 C56 C58D -111.8(10) . . . . ?
C41 C40 C56 C58D 65.8(10) . . . . ?
C39 C40 C56 C59 158.2(14) . . . . ?
C41 C40 C56 C59 -24.2(15) . . . . ?
C39 C40 C56 C57 36.0(15) . . . . ?
C41 C40 C56 C57 -146.4(15) . . . . ?
C39 C40 C56 C59D 133.1(10) . . . . ?
C41 C40 C56 C59D -49.3(11) . . . . ?
C41 C42 C60 C67 107.8(6) . . . . ?
C37 C42 C60 C67 -73.5(7) . . . . ?
C41 C42 C60 C61D -18.9(13) . . . . ?
C37 C42 C60 C61D 159.7(11) . . . . ?
C41 C42 C60 C61 -20.0(6) . . . . ?
C37 C42 C60 C61 158.6(4) . . . . ?
C67 C60 C61 C62 -30.7(3) . . . . ?
C42 C60 C61 C62 97.9(3) . . . . ?
C61D C60 C61 C62 -75(6) . . . . ?
C67 C60 C61 C66 148.7(9) . . . . ?
C42 C60 C61 C66 -82.7(8) . . . . ?
C61D C60 C61 C66 104(6) . . . . ?
C66 C61 C62 C63 -1(3) . . . . ?
C60 C61 C62 C63 178(3) . . . . ?
C61 C62 C63 C64 0(5) . . . . ?
C62 C63 C64 C65 3(6) . . . . ?
C63 C64 C65 C66 -4(5) . . . . ?
C62 C61 C66 C65 -0.2(18) . . . . ?
C60 C61 C66 C65 -179.5(13) . . . . ?
C64 C65 C66 C61 3(3) . . . . ?
C67 C60 C61D C62D -44(2) . . . . ?
C42 C60 C61D C62D 86(2) . . . . ?
C61 C60 C61D C62D 94(7) . . . . ?
C67 C60 C61D C66D 142(2) . . . . ?
C42 C60 C61D C66D -88(3) . . . . ?
C61 C60 C61D C66D -80(7) . . . . ?
C66D C61D C62D C63D 3(6) . . . . ?
C60 C61D C62D C63D -170(6) . . . . ?
C61D C62D C63D C64D 0(11) . . . . ?
C62D C63D C64D C65D -3(12) . . . . ?
C63D C64D C65D C66D 4(10) . . . . ?
C62D C61D C66D C65D -3(6) . . . . ?
C60 C61D C66D C65D 171(4) . . . . ?
C64D C65D C66D C61D -1(9) . . . . ?
C42 C60 C67 C72 -7.3(8) . . . . ?
C61D C60 C67 C72 125.1(12) . . . . ?
C61 C60 C67 C72 119.0(5) . . . . ?
C42 C60 C67 C68 171.5(5) . . . . ?
C61D C60 C67 C68 -56.1(13) . . . . ?
C61 C60 C67 C68 -62.2(5) . . . . ?
C72 C67 C68 C69 -0.5(9) . . . . ?
C60 C67 C68 C69 -179.4(6) . . . . ?
C67 C68 C69 C70 0.4(10) . . . . ?
C68 C69 C70 C71 0.2(10) . . . . ?
C69 C70 C71 C72 -0.8(9) . . . . ?
C68 C67 C72 C71 -0.1(9) . . . . ?
C60 C67 C72 C71 178.8(5) . . . . ?
C70 C71 C72 C67 0.7(9) . . . . ?
C7S C2S C3S C4S 0.0 . . . . ?
C1S C2S C3S C4S -168.1(14) . . . . ?
C2S C3S C4S C5S 0.0 . . . . ?
C3S C4S C5S C6S 0.0 . . . . ?
C4S C5S C6S C7S 0.0 . . . . ?
C5S C6S C7S C2S 0.0 . . . . ?
C3S C2S C7S C6S 0.0 . . . . ?
C1S C2S C7S C6S 169.2(13) . . . . ?
C7E C2E C3E C4E 0.0 . . . . ?
C2E C3E C4E C5E 0.0 . . . . ?
C2E C3E C4E C1E -167(3) . . . . ?
C3E C4E C5E C6E 0.0 . . . . ?
C1E C4E C5E C6E 161(4) . . . . ?
C4E C5E C6E C7E 0.0 . . . . ?
C5E C6E C7E C2E 0.0 . . . . ?
C3E C2E C7E C6E 0.0 . . . . ?
C8S C8S C9S C10S -3(5) 2_655 . . . ?
C8S C8S C9S C14S -176(3) 2_655 . . . ?
C14S C9S C10S C11S 0.0 . . . . ?
C8S C9S C10S C11S -174.0(17) . . . . ?
C9S C10S C11S C12S 0.0 . . . . ?
C10S C11S C12S C13S 0.0 . . . . ?
C11S C12S C13S C14S 0.0 . . . . ?
C12S C13S C14S C9S 0.0 . . . . ?
C10S C9S C14S C13S 0.0 . . . . ?
C8S C9S C14S C13S 173.6(19) . . . . ?
C21S C16S C17S C18S 0.0 . . . . ?
C15S C16S C17S C18S -180(2) . . . . ?
C16S C17S C18S C19S 0.0 . . . . ?
C17S C18S C19S C20S 0.0 . . . . ?
C18S C19S C20S C21S 0.0 . . . . ?
C19S C20S C21S C16S 0.0 . . . . ?
C17S C16S C21S C20S 0.0 . . . . ?
C15S C16S C21S C20S 180(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        61.31
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.110


# start Validation Reply Form
_vrf_THETM01_12039               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: No data in high resolution region. 
;

# end Validation Reply Form
####################################################################### 
# 
# 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_12108
_database_code_depnum_ccdc_archive 'CCDC 1032679'
_audit_update_record             
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_audit_creation_date             12-09-19
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '12108 in P2(1)/n'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_cell_length_a                   15.8132(5)
_cell_length_b                   14.3842(4)
_cell_length_c                   17.9838(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.412(2)
_cell_angle_gamma                90
_cell_volume                     3808.3(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C108 H99 Cl2 Nb1 O3 
# Dc =      1.40 Fooo =   1506.00 Mu =      2.88 M =    804.39
# Found Formula = C92 H94 Cl2 Nb1 O4 
# Dc =      1.24 FOOO =   1506.00 Mu =      2.80 M =    713.78

_chemical_formula_sum            'C92 H94 Cl2 Nb1 O4'
_chemical_formula_moiety         'C92 H94 Cl2 Nb1 O4'
_chemical_compound_source        ?
_chemical_formula_weight         1427.57


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_min          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_max          ?

_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1506
_exptl_absorpt_coefficient_mu    0.280

# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type   none
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            44469
_reflns_number_total             11194
_diffrn_reflns_av_R_equivalents  0.030
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11194 
# Theoretical number of reflections is about 22392 


_diffrn_reflns_theta_min         1.471
_diffrn_reflns_theta_max         30.087
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.087
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -22
_reflns_limit_h_max              20
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.36
_refine_diff_density_max         0.59


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         11154
_refine_ls_number_restraints     12
_refine_ls_number_parameters     467
_oxford_refine_ls_R_factor_ref   0.0409
_refine_ls_wR_factor_ref         0.0877
_refine_ls_goodness_of_fit_ref   1.0538
_refine_ls_shift/su_max          0.0014214
_refine_ls_shift/su_mean         0.0000517


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11164
_refine_ls_R_factor_all          0.0409
_refine_ls_wR_factor_all         0.0880

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9638
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_gt          0.0755

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.01P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Nb1 Nb 0.5000 0.5000 1.0000 0.0144 1.0000 Uani S . . . . .
Cl2 Cl 0.53245(2) 0.44075(2) 0.884973(17) 0.0218 1.0000 Uani . . . . . .
O1 O 0.37405(6) 0.51011(6) 0.93486(5) 0.0155 1.0000 Uani . . . . . .
O2 O 0.51339(6) 0.64530(7) 0.97419(6) 0.0219 1.0000 Uani . . . . . .
C1 C 0.28607(8) 0.53039(9) 0.88863(7) 0.0145 1.0000 Uani . . . . . .
C2 C 0.26323(8) 0.55091(9) 0.80682(7) 0.0157 1.0000 Uani . . . . . .
C3 C 0.17361(9) 0.57302(9) 0.76120(7) 0.0183 1.0000 Uani . . . . . .
C4 C 0.10493(8) 0.57672(9) 0.79276(7) 0.0180 1.0000 Uani . . . . . .
C5 C 0.12953(9) 0.55455(9) 0.87324(7) 0.0188 1.0000 Uani . . . . . .
C6 C 0.21839(8) 0.53082(9) 0.92211(7) 0.0158 1.0000 Uani . . . . . .
C7 C 0.33528(8) 0.54867(9) 0.76923(7) 0.0167 1.0000 Uani . . . . . .
C8 C 0.37436(9) 0.64349(10) 0.76141(7) 0.0197 1.0000 Uani . . . . . .
C9 C 0.46291(10) 0.64608(11) 0.76161(9) 0.0280 1.0000 Uani . . . . . .
C10 C 0.50123(12) 0.72992(13) 0.75177(10) 0.0354 1.0000 Uani . . . . . .
C11 C 0.45204(12) 0.81162(12) 0.74076(9) 0.0341 1.0000 Uani . . . . . .
C12 C 0.36540(12) 0.80992(11) 0.74116(10) 0.0330 1.0000 Uani . . . . . .
C13 C 0.32652(10) 0.72616(10) 0.75163(9) 0.0262 1.0000 Uani . . . . . .
C14 C 0.30264(9) 0.49574(9) 0.69005(7) 0.0183 1.0000 Uani . . . . . .
C15 C 0.26875(12) 0.53991(11) 0.61613(8) 0.0293 1.0000 Uani . . . . . .
C16 C 0.24053(14) 0.48853(13) 0.54581(9) 0.0398 1.0000 Uani . . . . . .
C17 C 0.24602(13) 0.39276(13) 0.54849(9) 0.0368 1.0000 Uani . . . . . .
C18 C 0.28021(12) 0.34783(11) 0.62132(10) 0.0324 1.0000 Uani . . . . . .
C19 C 0.30822(10) 0.39951(10) 0.69161(8) 0.0251 1.0000 Uani . . . . . .
C20 C 0.00909(9) 0.60890(10) 0.74079(8) 0.0228 1.0000 Uani . . . . . .
C21 C 0.01398(11) 0.71177(12) 0.71966(11) 0.0375 1.0000 Uani . . . . . .
C22 C -0.02717(11) 0.55301(13) 0.66279(10) 0.0354 1.0000 Uani . . . . . .
C23 C -0.05787(10) 0.59938(15) 0.78348(10) 0.0394 1.0000 Uani . . . . . .
C24 C 0.23917(8) 0.50759(9) 1.00987(7) 0.0171 1.0000 Uani . . . . . .
C25 C 0.19757(9) 0.58086(10) 1.04754(7) 0.0199 1.0000 Uani . . . . . .
C26 C 0.11522(10) 0.56716(11) 1.05762(9) 0.0285 1.0000 Uani . . . . . .
C27 C 0.07786(12) 0.63715(13) 1.08929(11) 0.0391 1.0000 Uani . . . . . .
C28 C 0.12231(15) 0.72069(13) 1.11187(12) 0.0441 1.0000 Uani . . . . . .
C29 C 0.20519(14) 0.73448(12) 1.10387(11) 0.0388 1.0000 Uani . . . . . .
C30 C 0.24212(11) 0.66521(11) 1.07142(9) 0.0279 1.0000 Uani . . . . . .
C31 C 0.21312(9) 0.40924(10) 1.02466(8) 0.0210 1.0000 Uani . . . . . .
C32 C 0.16987(10) 0.34710(11) 0.96390(9) 0.0265 1.0000 Uani . . . . . .
C33 C 0.14906(12) 0.25704(12) 0.98039(11) 0.0368 1.0000 Uani . . . . . .
C34 C 0.17139(14) 0.22849(12) 1.05846(12) 0.0422 1.0000 Uani . . . . . .
C35 C 0.21547(14) 0.28930(13) 1.12000(11) 0.0408 1.0000 Uani . . . . . .
C36 C 0.23658(11) 0.37874(11) 1.10380(9) 0.0302 1.0000 Uani . . . . . .
C37 C 0.44978(11) 0.71918(11) 0.97508(10) 0.0325 1.0000 Uani . . . . . .
C38 C 0.4865(2) 0.8066(2) 0.9578(2) 0.0325 0.682(8) Uani . U P . 2 .
C39 C 0.5880(3) 0.7891(3) 0.9932(3) 0.0453 0.682(8) Uani . U P . 2 .
C40 C 0.59772(11) 0.68570(13) 0.97462(12) 0.0400 1.0000 Uani . . . . . .
C41 C 0.61773(19) 0.53175(15) 0.60000(13) 0.0558 1.0000 Uani . . . . . .
C42 C 0.70045(16) 0.50341(15) 0.65400(14) 0.0517 1.0000 Uani . . . . . .
C43 C 0.70386(15) 0.44726(15) 0.71719(12) 0.0485 1.0000 Uani . . . . . .
C44 C 0.62553(17) 0.41909(16) 0.72541(12) 0.0508 1.0000 Uani . . . . . .
C45 C 0.54344(16) 0.44738(17) 0.67190(14) 0.0551 1.0000 Uani . . . . . .
C46 C 0.53933(17) 0.50366(16) 0.60904(14) 0.0553 1.0000 Uani . . . . . .
C381 C 0.5154(7) 0.8046(5) 0.9943(6) 0.0450 0.318(8) Uani . U P . 1 .
C391 C 0.5873(7) 0.7855(6) 0.9591(6) 0.0361 0.318(8) Uani . U P . 1 .
H31 H 0.1584 0.5860 0.7060 0.0211 1.0000 Uiso . . . . . .
H51 H 0.0839 0.5559 0.8963 0.0222 1.0000 Uiso . . . . . .
H71 H 0.3845 0.5132 0.8050 0.0197 1.0000 Uiso . . . . . .
H91 H 0.4973 0.5891 0.7679 0.0331 1.0000 Uiso . . . . . .
H101 H 0.5627 0.7320 0.7531 0.0429 1.0000 Uiso . . . . . .
H111 H 0.4788 0.8690 0.7325 0.0398 1.0000 Uiso . . . . . .
H121 H 0.3317 0.8669 0.7348 0.0406 1.0000 Uiso . . . . . .
H131 H 0.2659 0.7247 0.7516 0.0317 1.0000 Uiso . . . . . .
H151 H 0.2651 0.6057 0.6137 0.0344 1.0000 Uiso . . . . . .
H161 H 0.2193 0.5193 0.4955 0.0481 1.0000 Uiso . . . . . .
H171 H 0.2231 0.3576 0.5002 0.0429 1.0000 Uiso . . . . . .
H181 H 0.2856 0.2813 0.6242 0.0373 1.0000 Uiso . . . . . .
H191 H 0.3312 0.3684 0.7417 0.0305 1.0000 Uiso . . . . . .
H211 H -0.0448 0.7334 0.6871 0.0455 1.0000 Uiso . . . . . .
H212 H 0.0367 0.7482 0.7666 0.0455 1.0000 Uiso . . . . . .
H213 H 0.0537 0.7181 0.6904 0.0455 1.0000 Uiso . . . . . .
H221 H -0.0867 0.5731 0.6301 0.0438 1.0000 Uiso . . . . . .
H222 H -0.0294 0.4882 0.6737 0.0438 1.0000 Uiso . . . . . .
H223 H 0.0120 0.5608 0.6329 0.0438 1.0000 Uiso . . . . . .
H231 H -0.1162 0.6206 0.7496 0.0496 1.0000 Uiso . . . . . .
H232 H -0.0377 0.6359 0.8311 0.0496 1.0000 Uiso . . . . . .
H233 H -0.0615 0.5362 0.7970 0.0496 1.0000 Uiso . . . . . .
H241 H 0.3034 0.5121 1.0363 0.0204 1.0000 Uiso . . . . . .
H261 H 0.0851 0.5091 1.0430 0.0335 1.0000 Uiso . . . . . .
H271 H 0.0204 0.6268 1.0942 0.0472 1.0000 Uiso . . . . . .
H281 H 0.0979 0.7702 1.1343 0.0521 1.0000 Uiso . . . . . .
H291 H 0.2365 0.7919 1.1197 0.0450 1.0000 Uiso . . . . . .
H301 H 0.2994 0.6755 1.0659 0.0322 1.0000 Uiso . . . . . .
H321 H 0.1543 0.3663 0.9095 0.0308 1.0000 Uiso . . . . . .
H331 H 0.1189 0.2153 0.9375 0.0428 1.0000 Uiso . . . . . .
H341 H 0.1556 0.1665 1.0697 0.0492 1.0000 Uiso . . . . . .
H351 H 0.2323 0.2695 1.1741 0.0491 1.0000 Uiso . . . . . .
H361 H 0.2661 0.4205 1.1468 0.0354 1.0000 Uiso . . . . . .
H381 H 0.4706 0.8578 0.9845 0.0420 0.682(8) Uiso . . P . 2 .
H382 H 0.4662 0.8184 0.9029 0.0420 0.682(8) Uiso . . P . 2 .
H391 H 0.6098 0.8012 1.0482 0.0581 0.682(8) Uiso . . P . 2 .
H392 H 0.6163 0.8298 0.9672 0.0581 0.682(8) Uiso . . P . 2 .
H411 H 0.6164 0.5703 0.5568 0.0666 1.0000 Uiso . . . . . .
H421 H 0.7546 0.5228 0.6470 0.0585 1.0000 Uiso . . . . . .
H431 H 0.7614 0.4283 0.7550 0.0557 1.0000 Uiso . . . . . .
H441 H 0.6275 0.3802 0.7685 0.0621 1.0000 Uiso . . . . . .
H451 H 0.4887 0.4257 0.6769 0.0659 1.0000 Uiso . . . . . .
H461 H 0.4815 0.5238 0.5733 0.0663 1.0000 Uiso . . . . . .
H3811 H 0.5447 0.8147 1.0514 0.0517 0.318(8) Uiso . . P . 1 .
H3812 H 0.4852 0.8610 0.9714 0.0517 0.318(8) Uiso . . P . 1 .
H3911 H 0.6476 0.8178 0.9900 0.0463 0.318(8) Uiso . . P . 1 .
H3912 H 0.5736 0.8032 0.9059 0.0463 0.318(8) Uiso . . P . 1 .
H371 H 0.4443 0.7219 1.0260 0.0396 0.682(8) Uiso . . P . 2 .
H372 H 0.3915 0.7074 0.9353 0.0396 0.682(8) Uiso . . P . 2 .
H401 H 0.6489 0.6583 1.0147 0.0494 0.682(8) Uiso . . P . 2 .
H402 H 0.6036 0.6783 0.9239 0.0494 0.682(8) Uiso . . P . 2 .
H403 H 0.6444 0.6749 1.0250 0.0494 0.318(8) Uiso . . P . 1 .
H404 H 0.6140 0.6566 0.9339 0.0494 0.318(8) Uiso . . P . 1 .
H373 H 0.4249 0.7089 1.0153 0.0396 0.318(8) Uiso . . P . 1 .
H374 H 0.4016 0.7255 0.9247 0.0396 0.318(8) Uiso . . P . 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.087104(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nb1 . O2 2_667 2.1679(10) yes
Nb1 . Cl2 2_667 2.4585(3) yes
Nb1 . O1 2_667 1.9122(9) yes
Nb1 . Cl2 . 2.4585(3) yes
Nb1 . O1 . 1.9122(9) yes
Nb1 . O2 . 2.1679(10) yes
O1 . C1 . 1.3665(14) yes
O2 . C37 . 1.4673(17) yes
O2 . C40 . 1.4522(19) yes
C1 . C2 . 1.4122(16) yes
C1 . C6 . 1.4066(17) yes
C2 . C3 . 1.3906(17) yes
C2 . C7 . 1.5226(17) yes
C3 . C4 . 1.3980(18) yes
C3 . H31 . 0.951 no
C4 . C5 . 1.3916(17) yes
C4 . C20 . 1.5331(17) yes
C5 . C6 . 1.4005(17) yes
C5 . H51 . 0.955 no
C6 . C24 . 1.5270(17) yes
C7 . C8 . 1.5251(18) yes
C7 . C14 . 1.5288(17) yes
C7 . H71 . 0.956 no
C8 . C9 . 1.399(2) yes
C8 . C13 . 1.386(2) yes
C9 . C10 . 1.390(2) yes
C9 . H91 . 0.967 no
C10 . C11 . 1.383(3) yes
C10 . H101 . 0.965 no
C11 . C12 . 1.373(3) yes
C11 . H111 . 0.963 no
C12 . C13 . 1.396(2) yes
C12 . H121 . 0.962 no
C13 . H131 . 0.958 no
C14 . C15 . 1.3922(18) yes
C14 . C19 . 1.387(2) yes
C15 . C16 . 1.390(2) yes
C15 . H151 . 0.949 no
C16 . C17 . 1.380(3) yes
C16 . H161 . 0.951 no
C17 . C18 . 1.381(2) yes
C17 . H171 . 0.955 no
C18 . C19 . 1.392(2) yes
C18 . H181 . 0.960 no
C19 . H191 . 0.951 no
C20 . C21 . 1.537(2) yes
C20 . C22 . 1.535(2) yes
C20 . C23 . 1.524(2) yes
C21 . H211 . 0.952 no
C21 . H212 . 0.946 no
C21 . H213 . 0.959 no
C22 . H221 . 0.954 no
C22 . H222 . 0.956 no
C22 . H223 . 0.963 no
C23 . H231 . 0.951 no
C23 . H232 . 0.954 no
C23 . H233 . 0.948 no
C24 . C25 . 1.5257(18) yes
C24 . C31 . 1.5237(19) yes
C24 . H241 . 0.954 no
C25 . C26 . 1.3928(19) yes
C25 . C30 . 1.390(2) yes
C26 . C27 . 1.390(2) yes
C26 . H261 . 0.950 no
C27 . C28 . 1.376(3) yes
C27 . H271 . 0.957 no
C28 . C29 . 1.384(3) yes
C28 . H281 . 0.966 no
C29 . C30 . 1.387(2) yes
C29 . H291 . 0.952 no
C30 . H301 . 0.958 no
C31 . C32 . 1.384(2) yes
C31 . C36 . 1.4037(19) yes
C32 . C33 . 1.395(2) yes
C32 . H321 . 0.958 no
C33 . C34 . 1.379(3) yes
C33 . H331 . 0.956 no
C34 . C35 . 1.383(3) yes
C34 . H341 . 0.968 no
C35 . C36 . 1.386(2) yes
C35 . H351 . 0.954 no
C36 . H361 . 0.956 no
C37 . C381 . 1.563(8) yes
C37 . H373 . 0.953 no
C37 . H374 . 0.951 no
C38 . C39 . 1.516(6) yes
C38 . H381 . 0.961 no
C38 . H382 . 0.937 no
C39 . C40 . 1.545(5) yes
C39 . H391 . 0.937 no
C39 . H392 . 0.955 no
C40 . C391 . 1.460(9) yes
C40 . H403 . 0.949 no
C40 . H404 . 0.956 no
C41 . C42 . 1.376(3) yes
C41 . C46 . 1.369(4) yes
C41 . H411 . 0.949 no
C42 . C43 . 1.379(3) yes
C42 . H421 . 0.951 no
C43 . C44 . 1.362(3) yes
C43 . H431 . 0.955 no
C44 . C45 . 1.365(3) yes
C44 . H441 . 0.947 no
C45 . C46 . 1.373(3) yes
C45 . H451 . 0.955 no
C46 . H461 . 0.951 no
C381 . C391 . 1.516(13) yes
C381 . H3811 . 0.970 no
C381 . H3812 . 0.955 no
C391 . H3911 . 1.023 no
C391 . H3912 . 0.934 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 2_667 Nb1 . Cl2 2_667 95.01(3) yes
O2 2_667 Nb1 . O1 2_667 87.52(4) yes
Cl2 2_667 Nb1 . O1 2_667 90.09(3) yes
O2 2_667 Nb1 . Cl2 . 84.99(3) yes
Cl2 2_667 Nb1 . Cl2 . 179.995 yes
O1 2_667 Nb1 . Cl2 . 89.91(3) yes
O2 2_667 Nb1 . O1 . 92.48(4) yes
Cl2 2_667 Nb1 . O1 . 89.91(3) yes
O1 2_667 Nb1 . O1 . 179.994 yes
Cl2 . Nb1 . O1 . 90.09(3) yes
O2 2_667 Nb1 . O2 . 179.995 yes
Cl2 2_667 Nb1 . O2 . 84.99(3) yes
O1 2_667 Nb1 . O2 . 92.48(4) yes
Cl2 . Nb1 . O2 . 95.01(3) yes
O1 . Nb1 . O2 . 87.52(4) yes
Nb1 . O1 . C1 . 172.02(8) yes
Nb1 . O2 . C37 . 125.10(9) yes
Nb1 . O2 . C40 . 123.09(9) yes
C37 . O2 . C40 . 109.99(12) yes
O1 . C1 . C2 . 119.66(11) yes
O1 . C1 . C6 . 120.35(10) yes
C2 . C1 . C6 . 119.99(11) yes
C1 . C2 . C3 . 118.72(11) yes
C1 . C2 . C7 . 120.65(11) yes
C3 . C2 . C7 . 120.63(10) yes
C2 . C3 . C4 . 123.00(11) yes
C2 . C3 . H31 . 118.4 no
C4 . C3 . H31 . 118.6 no
C3 . C4 . C5 . 116.73(11) yes
C3 . C4 . C20 . 120.37(11) yes
C5 . C4 . C20 . 122.82(12) yes
C4 . C5 . C6 . 122.96(12) yes
C4 . C5 . H51 . 118.6 no
C6 . C5 . H51 . 118.4 no
C1 . C6 . C5 . 118.57(11) yes
C1 . C6 . C24 . 122.08(11) yes
C5 . C6 . C24 . 119.34(11) yes
C2 . C7 . C8 . 114.59(11) yes
C2 . C7 . C14 . 111.79(10) yes
C8 . C7 . C14 . 111.70(10) yes
C2 . C7 . H71 . 105.6 no
C8 . C7 . H71 . 106.4 no
C14 . C7 . H71 . 106.1 no
C7 . C8 . C9 . 117.54(12) yes
C7 . C8 . C13 . 123.94(12) yes
C9 . C8 . C13 . 118.48(13) yes
C8 . C9 . C10 . 120.34(15) yes
C8 . C9 . H91 . 119.8 no
C10 . C9 . H91 . 119.9 no
C9 . C10 . C11 . 120.47(15) yes
C9 . C10 . H101 . 120.4 no
C11 . C10 . H101 . 119.2 no
C10 . C11 . C12 . 119.62(15) yes
C10 . C11 . H111 . 119.6 no
C12 . C11 . H111 . 120.8 no
C11 . C12 . C13 . 120.36(15) yes
C11 . C12 . H121 . 119.7 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C8 . 120.71(14) yes
C12 . C13 . H131 . 120.5 no
C8 . C13 . H131 . 118.7 no
C7 . C14 . C15 . 122.93(12) yes
C7 . C14 . C19 . 118.74(11) yes
C15 . C14 . C19 . 118.32(13) yes
C14 . C15 . C16 . 120.65(14) yes
C14 . C15 . H151 . 119.7 no
C16 . C15 . H151 . 119.6 no
C15 . C16 . C17 . 120.25(15) yes
C15 . C16 . H161 . 120.1 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . C18 . 119.86(14) yes
C16 . C17 . H171 . 119.9 no
C18 . C17 . H171 . 120.1 no
C17 . C18 . C19 . 119.73(15) yes
C17 . C18 . H181 . 120.9 no
C19 . C18 . H181 . 119.4 no
C18 . C19 . C14 . 121.19(13) yes
C18 . C19 . H191 . 119.6 no
C14 . C19 . H191 . 119.2 no
C4 . C20 . C21 . 108.28(12) yes
C4 . C20 . C22 . 110.82(12) yes
C21 . C20 . C22 . 108.30(13) yes
C4 . C20 . C23 . 112.32(11) yes
C21 . C20 . C23 . 108.55(14) yes
C22 . C20 . C23 . 108.48(13) yes
C20 . C21 . H211 . 110.0 no
C20 . C21 . H212 . 110.5 no
H211 . C21 . H212 . 109.6 no
C20 . C21 . H213 . 109.2 no
H211 . C21 . H213 . 108.5 no
H212 . C21 . H213 . 109.0 no
C20 . C22 . H221 . 111.2 no
C20 . C22 . H222 . 110.6 no
H221 . C22 . H222 . 108.7 no
C20 . C22 . H223 . 110.3 no
H221 . C22 . H223 . 108.0 no
H222 . C22 . H223 . 107.9 no
C20 . C23 . H231 . 109.7 no
C20 . C23 . H232 . 109.6 no
H231 . C23 . H232 . 109.0 no
C20 . C23 . H233 . 109.5 no
H231 . C23 . H233 . 109.6 no
H232 . C23 . H233 . 109.3 no
C6 . C24 . C25 . 110.04(10) yes
C6 . C24 . C31 . 114.44(11) yes
C25 . C24 . C31 . 112.09(10) yes
C6 . C24 . H241 . 106.8 no
C25 . C24 . H241 . 106.6 no
C31 . C24 . H241 . 106.4 no
C24 . C25 . C26 . 122.35(13) yes
C24 . C25 . C30 . 119.22(12) yes
C26 . C25 . C30 . 118.41(13) yes
C25 . C26 . C27 . 120.54(15) yes
C25 . C26 . H261 . 119.1 no
C27 . C26 . H261 . 120.3 no
C26 . C27 . C28 . 120.36(16) yes
C26 . C27 . H271 . 119.1 no
C28 . C27 . H271 . 120.6 no
C27 . C28 . C29 . 119.70(15) yes
C27 . C28 . H281 . 121.9 no
C29 . C28 . H281 . 118.4 no
C28 . C29 . C30 . 120.06(17) yes
C28 . C29 . H291 . 120.1 no
C30 . C29 . H291 . 119.8 no
C25 . C30 . C29 . 120.90(15) yes
C25 . C30 . H301 . 119.6 no
C29 . C30 . H301 . 119.5 no
C24 . C31 . C32 . 123.30(12) yes
C24 . C31 . C36 . 118.62(13) yes
C32 . C31 . C36 . 118.04(14) yes
C31 . C32 . C33 . 121.27(14) yes
C31 . C32 . H321 . 119.3 no
C33 . C32 . H321 . 119.5 no
C32 . C33 . C34 . 120.02(16) yes
C32 . C33 . H331 . 119.9 no
C34 . C33 . H331 . 120.1 no
C33 . C34 . C35 . 119.55(16) yes
C33 . C34 . H341 . 119.8 no
C35 . C34 . H341 . 120.6 no
C34 . C35 . C36 . 120.56(15) yes
C34 . C35 . H351 . 120.0 no
C36 . C35 . H351 . 119.5 no
C31 . C36 . C35 . 120.55(15) yes
C31 . C36 . H361 . 119.6 no
C35 . C36 . H361 . 119.8 no
O2 . C37 . C381 . 99.8(3) yes
O2 . C37 . H373 . 111.8 no
C381 . C37 . H373 . 112.2 no
O2 . C37 . H374 . 111.9 no
C381 . C37 . H374 . 111.8 no
H373 . C37 . H374 . 109.1 no
C37 . C38 . C39 . 102.1(3) yes
C37 . C38 . H381 . 110.9 no
C39 . C38 . H381 . 110.3 no
C37 . C38 . H382 . 111.7 no
C39 . C38 . H382 . 111.9 no
H381 . C38 . H382 . 109.7 no
C38 . C39 . C40 . 104.0(3) yes
C38 . C39 . H391 . 109.7 no
C40 . C39 . H391 . 112.3 no
C38 . C39 . H392 . 107.9 no
C40 . C39 . H392 . 112.5 no
H391 . C39 . H392 . 110.1 no
O2 . C40 . C391 . 110.7(4) yes
O2 . C40 . H403 . 109.4 no
C391 . C40 . H403 . 109.7 no
O2 . C40 . H404 . 108.9 no
C391 . C40 . H404 . 109.1 no
H403 . C40 . H404 . 109.0 no
C42 . C41 . C46 . 119.8(2) yes
C42 . C41 . H411 . 118.9 no
C46 . C41 . H411 . 121.3 no
C41 . C42 . C43 . 119.7(2) yes
C41 . C42 . H421 . 119.3 no
C43 . C42 . H421 . 120.9 no
C42 . C43 . C44 . 120.0(2) yes
C42 . C43 . H431 . 119.6 no
C44 . C43 . H431 . 120.4 no
C43 . C44 . C45 . 120.2(2) yes
C43 . C44 . H441 . 120.3 no
C45 . C44 . H441 . 119.4 no
C44 . C45 . C46 . 120.2(2) yes
C44 . C45 . H451 . 119.8 no
C46 . C45 . H451 . 119.9 no
C45 . C46 . C41 . 120.0(2) yes
C45 . C46 . H461 . 118.7 no
C41 . C46 . H461 . 121.3 no
C37 . C381 . C391 . 107.7(6) yes
C37 . C381 . H3811 . 112.0 no
C391 . C381 . H3811 . 109.1 no
C37 . C381 . H3812 . 112.7 no
C391 . C381 . H3812 . 107.9 no
H3811 . C381 . H3812 . 107.4 no
C381 . C391 . C40 . 98.4(6) yes
C381 . C391 . H3911 . 112.5 no
C40 . C391 . H3911 . 109.0 no
C381 . C391 . H3912 . 116.7 no
C40 . C391 . H3912 . 115.5 no
H3911 . C391 . H3912 . 104.7 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/09/12 at 17:35:14
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX PART(0001,OCC) AND PART(0002,OCC) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/09/12 at 17:35:14
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.005000 = C(38) TO C(381) 
U(IJ)'S  0.0, 0.005000 = C(39) TO C(391) 
END                                                                             
;
