# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1_half_H2O
_database_code_depnum_ccdc_archive 'CCDC 1574239'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H4 O24 S4 V4 4-, 4(N C8 H20) 1+, 0.5(O H2)'
_chemical_formula_sum            'C32 H85 N4 O24.50 S4 V4'
_chemical_formula_weight         1250.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   21.424(6)
_cell_length_b                   11.429(3)
_cell_length_c                   21.431(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.541(5)
_cell_angle_gamma                90
_cell_volume                     5247(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    980
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      18.21

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             2628
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.932
_shelx_estimated_absorpt_T_min   0.807
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23195
_diffrn_reflns_av_unetI/netI     0.1452
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.901
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5418
_reflns_number_gt                2805
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'H atoms on water O not located, but could make H-bonds with O(1) and O(2).'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0773P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5418
_refine_ls_number_parameters     328
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2000
_refine_ls_wR_factor_gt          0.1619
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.02694(5) 0.86204(9) 0.31842(5) 0.0213(3) Uani 1 1 d . . . . .
O1 O 0.02997(19) 0.9993(4) 0.3263(2) 0.0295(11) Uani 1 1 d . . . . .
V2 V 0.06836(5) 0.63797(9) 0.22380(5) 0.0222(3) Uani 1 1 d . . . . .
O2 O 0.0769(2) 0.5002(4) 0.22095(19) 0.0300(11) Uani 1 1 d . . . . .
O3 O 0.05333(19) 0.8387(4) 0.22925(18) 0.0222(10) Uani 1 1 d D . . . .
H3 H 0.091(3) 0.871(8) 0.213(4) 0.10(4) Uiso 1 1 d D . . . .
O4 O 0.02121(19) 0.6616(3) 0.30384(18) 0.0210(9) Uani 1 1 d D . . . .
H4 H 0.033(3) 0.623(4) 0.3408(16) 0.023(17) Uiso 1 1 d D . . . .
O5 O 0.01429(19) 0.8092(4) 0.10281(18) 0.0255(10) Uani 1 1 d . . . . .
O6 O 0.0987(2) 0.6816(4) 0.13911(19) 0.0283(10) Uani 1 1 d . . . . .
S1 S 0.08395(8) 0.78444(16) 0.09705(7) 0.0291(4) Uani 1 1 d . . . . .
O7 O 0.1185(2) 0.8858(4) 0.1201(2) 0.0337(12) Uani 1 1 d . . . . .
O8 O 0.0969(2) 0.7530(4) 0.0338(2) 0.0414(13) Uani 1 1 d . . . . .
O9 O 0.11271(19) 0.8192(4) 0.34942(19) 0.0248(10) Uani 1 1 d . . . . .
O10 O 0.14751(18) 0.6895(4) 0.26681(19) 0.0277(10) Uani 1 1 d . . . . .
S2 S 0.15338(7) 0.71431(15) 0.33618(8) 0.0288(4) Uani 1 1 d . . . . .
O11 O 0.1291(2) 0.6151(4) 0.3708(2) 0.0340(12) Uani 1 1 d . . . . .
O12 O 0.2172(2) 0.7416(4) 0.3506(2) 0.0405(13) Uani 1 1 d . . . . .
N1 N 0.3140(2) 0.7394(4) 0.1563(2) 0.0234(12) Uani 1 1 d . . . . .
C1 C 0.2563(3) 0.7626(7) 0.1155(3) 0.0418(19) Uani 1 1 d . . . . .
H1A H 0.2218 0.7891 0.1425 0.050 Uiso 1 1 calc R U . . .
H1B H 0.2432 0.6884 0.0955 0.050 Uiso 1 1 calc R U . . .
C2 C 0.2673(4) 0.8551(7) 0.0646(4) 0.053(2) Uani 1 1 d . . . . .
H2A H 0.2813 0.9284 0.0840 0.079 Uiso 1 1 calc R U . . .
H2B H 0.2284 0.8688 0.0414 0.079 Uiso 1 1 calc R U . . .
H2C H 0.2994 0.8271 0.0359 0.079 Uiso 1 1 calc R U . . .
C3 C 0.3360(3) 0.8507(6) 0.1868(4) 0.046(2) Uani 1 1 d . . . . .
H3A H 0.3495 0.9057 0.1538 0.055 Uiso 1 1 calc R U . . .
H3B H 0.3729 0.8329 0.2132 0.055 Uiso 1 1 calc R U . . .
C4 C 0.2870(4) 0.9113(7) 0.2268(4) 0.050(2) Uani 1 1 d . . . . .
H4A H 0.2498 0.9278 0.2013 0.075 Uiso 1 1 calc R U . . .
H4B H 0.3041 0.9849 0.2432 0.075 Uiso 1 1 calc R U . . .
H4C H 0.2757 0.8602 0.2616 0.075 Uiso 1 1 calc R U . . .
C5 C 0.2940(3) 0.6506(6) 0.2053(3) 0.0426(19) Uani 1 1 d . . . . .
H5A H 0.2790 0.5790 0.1840 0.051 Uiso 1 1 calc R U . . .
H5B H 0.2587 0.6834 0.2292 0.051 Uiso 1 1 calc R U . . .
C6 C 0.3464(4) 0.6177(6) 0.2508(3) 0.043(2) Uani 1 1 d . . . . .
H6A H 0.3774 0.5697 0.2292 0.064 Uiso 1 1 calc R U . . .
H6B H 0.3291 0.5732 0.2857 0.064 Uiso 1 1 calc R U . . .
H6C H 0.3664 0.6889 0.2667 0.064 Uiso 1 1 calc R U . . .
C7 C 0.3661(3) 0.6926(6) 0.1170(3) 0.0385(18) Uani 1 1 d . . . . .
H7A H 0.4031 0.6796 0.1442 0.046 Uiso 1 1 calc R U . . .
H7B H 0.3774 0.7528 0.0859 0.046 Uiso 1 1 calc R U . . .
C8 C 0.3514(3) 0.5806(6) 0.0832(3) 0.0343(17) Uani 1 1 d . . . . .
H8A H 0.3479 0.5166 0.1134 0.051 Uiso 1 1 calc R U . . .
H8B H 0.3848 0.5631 0.0537 0.051 Uiso 1 1 calc R U . . .
H8C H 0.3117 0.5891 0.0604 0.051 Uiso 1 1 calc R U . . .
N2 N 0.1000(2) 0.7202(5) 0.5594(2) 0.0268(13) Uani 1 1 d . . . . .
C9 C 0.1387(4) 0.7616(7) 0.5044(4) 0.053(2) Uani 1 1 d . . . . .
H9A H 0.1104 0.7959 0.4725 0.064 Uiso 1 1 calc R U . . .
H9B H 0.1595 0.6931 0.4855 0.064 Uiso 1 1 calc R U . . .
C10 C 0.1890(4) 0.8538(7) 0.5226(4) 0.058(2) Uani 1 1 d . . . . .
H10A H 0.1691 0.9202 0.5434 0.088 Uiso 1 1 calc R U . . .
H10B H 0.2101 0.8811 0.4850 0.088 Uiso 1 1 calc R U . . .
H10C H 0.2197 0.8181 0.5510 0.088 Uiso 1 1 calc R U . . .
C11 C 0.1396(4) 0.6617(7) 0.6075(3) 0.047(2) Uani 1 1 d . . . . .
H11A H 0.1131 0.6417 0.6436 0.056 Uiso 1 1 calc R U . . .
H11B H 0.1716 0.7180 0.6223 0.056 Uiso 1 1 calc R U . . .
C12 C 0.1726(3) 0.5501(6) 0.5854(4) 0.043(2) Uani 1 1 d . . . . .
H12A H 0.1425 0.4857 0.5833 0.064 Uiso 1 1 calc R U . . .
H12B H 0.2063 0.5301 0.6147 0.064 Uiso 1 1 calc R U . . .
H12C H 0.1901 0.5634 0.5439 0.064 Uiso 1 1 calc R U . . .
C13 C 0.0512(4) 0.6398(7) 0.5317(4) 0.055(2) Uani 1 1 d . . . . .
H13A H 0.0721 0.5751 0.5094 0.066 Uiso 1 1 calc R U . . .
H13B H 0.0257 0.6838 0.5009 0.066 Uiso 1 1 calc R U . . .
C14 C 0.0075(4) 0.5875(7) 0.5823(4) 0.064(3) Uani 1 1 d . . . . .
H14A H 0.0284 0.5216 0.6029 0.096 Uiso 1 1 calc R U . . .
H14B H -0.0313 0.5602 0.5625 0.096 Uiso 1 1 calc R U . . .
H14C H -0.0022 0.6478 0.6133 0.096 Uiso 1 1 calc R U . . .
C15 C 0.0707(3) 0.8244(6) 0.5891(3) 0.0405(19) Uani 1 1 d . . . . .
H15A H 0.1042 0.8747 0.6066 0.049 Uiso 1 1 calc R U . . .
H15B H 0.0448 0.7975 0.6244 0.049 Uiso 1 1 calc R U . . .
C16 C 0.0299(3) 0.8982(6) 0.5456(3) 0.0397(19) Uani 1 1 d . . . . .
H16A H 0.0552 0.9273 0.5110 0.059 Uiso 1 1 calc R U . . .
H16B H 0.0128 0.9646 0.5688 0.059 Uiso 1 1 calc R U . . .
H16C H -0.0043 0.8502 0.5291 0.059 Uiso 1 1 calc R U . . .
O13 O 0.0000 0.258(2) 0.2500 0.168(13) Uani 0.5 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.580(4) . ?
V1 O5 2.006(4) 2 ?
V1 O9 2.009(4) . ?
V1 O3 2.010(4) 2 ?
V1 O3 2.016(4) . ?
V1 O4 2.315(4) . ?
V2 O2 1.587(4) . ?
V2 O6 1.997(4) . ?
V2 O10 2.011(4) . ?
V2 O4 2.017(4) . ?
V2 O4 2.021(4) 2 ?
V2 O3 2.320(4) . ?
O3 V1 2.010(4) 2 ?
O3 H3 0.95(2) . ?
O4 V2 2.021(4) 2 ?
O4 H4 0.94(2) . ?
O5 S1 1.525(4) . ?
O5 V1 2.006(4) 2 ?
O6 S1 1.513(4) . ?
S1 O8 1.432(5) . ?
S1 O7 1.459(5) . ?
O9 S2 1.510(4) . ?
O10 S2 1.518(4) . ?
S2 O12 1.433(4) . ?
S2 O11 1.454(5) . ?
N1 C7 1.503(8) . ?
N1 C3 1.503(8) . ?
N1 C5 1.525(8) . ?
N1 C1 1.530(8) . ?
C1 C2 1.540(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.528(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.528(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.503(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N2 C11 1.489(9) . ?
N2 C15 1.493(9) . ?
N2 C13 1.510(9) . ?
N2 C9 1.522(8) . ?
C9 C10 1.556(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.535(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.559(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.525(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 103.1(2) . 2 ?
O1 V1 O9 99.8(2) . . ?
O5 V1 O9 93.27(17) 2 . ?
O1 V1 O3 102.7(2) . 2 ?
O5 V1 O3 90.36(17) 2 2 ?
O9 V1 O3 155.71(17) . 2 ?
O1 V1 O3 102.8(2) . . ?
O5 V1 O3 152.60(18) 2 . ?
O9 V1 O3 91.00(17) . . ?
O3 V1 O3 75.33(19) 2 . ?
O1 V1 O4 178.2(2) . . ?
O5 V1 O4 78.02(16) 2 . ?
O9 V1 O4 81.40(15) . . ?
O3 V1 O4 75.88(16) 2 . ?
O3 V1 O4 75.89(16) . . ?
O2 V2 O6 100.03(19) . . ?
O2 V2 O10 102.2(2) . . ?
O6 V2 O10 93.62(18) . . ?
O2 V2 O4 102.98(19) . . ?
O6 V2 O4 155.42(17) . . ?
O10 V2 O4 89.88(17) . . ?
O2 V2 O4 103.4(2) . 2 ?
O6 V2 O4 90.94(17) . 2 ?
O10 V2 O4 152.81(18) . 2 ?
O4 V2 O4 75.50(18) . 2 ?
O2 V2 O3 178.48(19) . . ?
O6 V2 O3 81.10(16) . . ?
O10 V2 O3 78.70(16) . . ?
O4 V2 O3 75.75(15) . . ?
O4 V2 O3 75.56(16) 2 . ?
V1 O3 V1 102.60(19) 2 . ?
V1 O3 V2 102.95(17) 2 . ?
V1 O3 V2 102.64(17) . . ?
V1 O3 H3 119(6) 2 . ?
V1 O3 H3 123(6) . . ?
V2 O3 H3 104(6) . . ?
V2 O4 V2 102.39(18) . 2 ?
V2 O4 V1 102.76(17) . . ?
V2 O4 V1 102.76(17) 2 . ?
V2 O4 H4 121(4) . . ?
V2 O4 H4 116(4) 2 . ?
V1 O4 H4 110(4) . . ?
S1 O5 V1 124.3(2) . 2 ?
S1 O6 V2 131.9(3) . . ?
O8 S1 O7 114.7(3) . . ?
O8 S1 O6 109.2(3) . . ?
O7 S1 O6 108.2(3) . . ?
O8 S1 O5 108.7(3) . . ?
O7 S1 O5 108.6(3) . . ?
O6 S1 O5 107.2(2) . . ?
S2 O9 V1 131.2(2) . . ?
S2 O10 V2 124.4(2) . . ?
O12 S2 O11 113.9(3) . . ?
O12 S2 O9 109.7(3) . . ?
O11 S2 O9 108.2(3) . . ?
O12 S2 O10 108.8(3) . . ?
O11 S2 O10 109.1(3) . . ?
O9 S2 O10 106.8(2) . . ?
C7 N1 C3 108.2(5) . . ?
C7 N1 C5 111.4(5) . . ?
C3 N1 C5 110.7(5) . . ?
C7 N1 C1 109.9(5) . . ?
C3 N1 C1 110.5(5) . . ?
C5 N1 C1 106.1(5) . . ?
N1 C1 C2 113.3(6) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 114.4(6) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 113.1(6) . . ?
N1 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N1 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 C8 114.8(5) . . ?
N1 C7 H7A 108.6 . . ?
C8 C7 H7A 108.6 . . ?
N1 C7 H7B 108.6 . . ?
C8 C7 H7B 108.6 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 N2 C15 107.6(5) . . ?
C11 N2 C13 112.8(6) . . ?
C15 N2 C13 111.2(6) . . ?
C11 N2 C9 111.4(5) . . ?
C15 N2 C9 108.5(5) . . ?
C13 N2 C9 105.4(5) . . ?
N2 C9 C10 113.4(6) . . ?
N2 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N2 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 114.8(6) . . ?
N2 C11 H11A 108.6 . . ?
C12 C11 H11A 108.6 . . ?
N2 C11 H11B 108.6 . . ?
C12 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 112.2(6) . . ?
N2 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
N2 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 114.9(6) . . ?
N2 C15 H15A 108.5 . . ?
C16 C15 H15A 108.5 . . ?
N2 C15 H15B 108.5 . . ?
C16 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 O6 S1 O8 -156.8(4) . . . . ?
V2 O6 S1 O7 77.8(4) . . . . ?
V2 O6 S1 O5 -39.2(4) . . . . ?
V1 O5 S1 O8 -177.8(3) 2 . . . ?
V1 O5 S1 O7 -52.4(4) 2 . . . ?
V1 O5 S1 O6 64.3(4) 2 . . . ?
V1 O9 S2 O12 159.6(3) . . . . ?
V1 O9 S2 O11 -75.6(4) . . . . ?
V1 O9 S2 O10 41.8(4) . . . . ?
V2 O10 S2 O12 176.4(3) . . . . ?
V2 O10 S2 O11 51.6(4) . . . . ?
V2 O10 S2 O9 -65.2(4) . . . . ?
C7 N1 C1 C2 -61.8(8) . . . . ?
C3 N1 C1 C2 57.6(8) . . . . ?
C5 N1 C1 C2 177.7(6) . . . . ?
C7 N1 C3 C4 178.0(6) . . . . ?
C5 N1 C3 C4 -59.6(8) . . . . ?
C1 N1 C3 C4 57.6(8) . . . . ?
C7 N1 C5 C6 60.7(7) . . . . ?
C3 N1 C5 C6 -59.7(7) . . . . ?
C1 N1 C5 C6 -179.6(6) . . . . ?
C3 N1 C7 C8 180.0(6) . . . . ?
C5 N1 C7 C8 58.0(8) . . . . ?
C1 N1 C7 C8 -59.3(7) . . . . ?
C11 N2 C9 C10 -61.7(8) . . . . ?
C15 N2 C9 C10 56.5(8) . . . . ?
C13 N2 C9 C10 175.6(6) . . . . ?
C15 N2 C11 C12 178.7(6) . . . . ?
C13 N2 C11 C12 55.8(8) . . . . ?
C9 N2 C11 C12 -62.5(8) . . . . ?
C11 N2 C13 C14 57.5(8) . . . . ?
C15 N2 C13 C14 -63.4(8) . . . . ?
C9 N2 C13 C14 179.2(6) . . . . ?
C11 N2 C15 C16 177.9(6) . . . . ?
C13 N2 C15 C16 -58.2(8) . . . . ?
C9 N2 C15 C16 57.2(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O7 0.95(2) 2.09(8) 2.789(6) 129(8) .
O4 H4 O11 0.94(2) 2.15(5) 2.761(6) 122(4) .

_refine_diff_density_max         0.728
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.131

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_chemical_properties_physical    
'Crystals lost solvent and crmbled within 2 hours on the microscope slide under inert oil'
####################################################################### 
# 
# 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_3dotMeCN
_database_code_depnum_ccdc_archive 'CCDC 1574242'
_audit_update_record             
;
2018-10-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_3dotMeCN            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      21.21 Check
RESPONSE: H atoms not included on OH and cations.
;
_vrf_PLAT430_3dotMeCN            
;
PROBLEM: Short Inter D...A Contact  O4       ..N2       .       2.81 Ang.
RESPONSE: This is an H-bond & distance is good for this.
;
# Added during the CSD deposition process: Friday 12 October 2018 11:40 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H8 O27 S4 V6 1-, 2(C8 H20 N 1+), C2 H3 N'
_chemical_formula_sum            'C19 H31 N3 O28 S4 V6'
_chemical_formula_weight         1183.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0063 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0108 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2967 0.5131 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1217 0.1197 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

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

_cell_length_a                   11.3206(8)
_cell_length_b                   19.3232(13)
_cell_length_c                   11.4459(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.2257(8)
_cell_angle_gamma                90
_cell_volume                     2415.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9359
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      26.74

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.271
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   'TWINABS v2008/2, Sheldrick, G.M., (2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6939
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38192
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.800
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_full        24.604
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5670
_reflns_number_gt                4771
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1035P)²+2.9927P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5670
_refine_ls_number_parameters     411
_refine_ls_number_restraints     660
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1662
_refine_ls_wR_factor_gt          0.1569
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.21215(10) 0.66873(6) 0.67654(11) 0.0202(3) Uani 1 1 d . U . . .
V2 V 0.44152(16) 0.750000 0.60481(14) 0.0177(4) Uani 1 2 d S TU P A .
V3 V 0.52246(11) 0.59455(6) 0.75300(11) 0.0210(3) Uani 1 1 d . U . . .
V4 V 0.44639(16) 0.750000 0.86016(14) 0.0174(4) Uani 1 2 d S TU P A .
S1 S 0.35408(18) 0.60492(10) 0.49343(16) 0.0237(4) Uani 1 1 d . U . . .
S2 S 0.36306(19) 0.60547(10) 0.93191(16) 0.0240(4) Uani 1 1 d . U . . .
O1 O 0.4201(4) 0.6802(2) 0.7266(4) 0.0187(8) Uani 1 1 d . U . . .
O2 O 0.2265(7) 0.750000 0.5723(6) 0.0199(13) Uani 1 2 d S TU P . .
O3 O 0.2521(6) 0.6024(3) 0.5535(5) 0.0277(12) Uani 1 1 d . U . . .
O4 O 0.2344(7) 0.750000 0.7885(6) 0.0195(13) Uani 1 2 d S TU P . .
O5 O 0.2599(6) 0.6018(3) 0.8195(5) 0.0279(12) Uani 1 1 d . U . . .
O6 O 0.0683(5) 0.6548(3) 0.6445(6) 0.0333(12) Uani 1 1 d . U . . .
O7 O 0.3828(4) 0.6776(2) 0.4716(5) 0.0227(9) Uani 1 1 d . U . . .
O8 O 0.4635(6) 0.5729(3) 0.5779(5) 0.0318(13) Uani 1 1 d . U . . .
O9 O 0.3216(6) 0.5664(3) 0.3818(5) 0.0308(13) Uani 1 1 d . U . . .
O10 O 0.5834(7) 0.750000 0.6136(7) 0.0268(16) Uani 1 2 d S TU P . .
O11 O 0.5518(5) 0.4906(3) 0.7614(5) 0.0299(11) Uani 1 1 d D U . . .
H11A H 0.594(9) 0.467(5) 0.821(7) 0.045 Uiso 1 1 d D U . . .
H11B H 0.586(9) 0.471(6) 0.713(8) 0.045 Uiso 1 1 d D U . . .
O12 O 0.6579(5) 0.6227(3) 0.7839(5) 0.0290(11) Uani 1 1 d . U . . .
O13 O 0.5900(7) 0.750000 0.9187(7) 0.0271(16) Uani 1 2 d S TU P . .
O14 O 0.4731(6) 0.5743(3) 0.9033(5) 0.0300(12) Uani 1 1 d . U . . .
O15 O 0.3918(4) 0.6786(2) 0.9678(5) 0.0228(9) Uani 1 1 d . U . . .
O16 O 0.3324(6) 0.5671(3) 1.0280(5) 0.0310(13) Uani 1 1 d . U . . .
C1 C 0.138(2) 0.750000 0.452(2) 0.040(5) Uani 0.521(16) 2 d S TU P A 1
H1A H 0.150441 0.791128 0.406909 0.060 Uiso 0.261(8) 1 calc R U P A 1
H1B H 0.149154 0.708314 0.407648 0.060 Uiso 0.261(8) 1 calc R U P A 1
H1C H 0.054267 0.750558 0.462139 0.060 Uiso 0.521(16) 2 calc R U P A 1
N1 N 0.1198(19) 0.748(12) 0.3111(18) 0.026(7) Uani 0.239(8) 1 d D U P A -2
C2 C 0.188(2) 0.738(3) 0.256(2) 0.025(12) Uani 0.239(8) 1 d D U P A -2
C3 C 0.278(2) 0.7274(14) 0.191(2) 0.022(5) Uani 0.239(8) 1 d D U P A -2
H3A H 0.337735 0.692813 0.232913 0.033 Uiso 0.239(8) 1 calc R U P A -2
H3B H 0.320900 0.770989 0.185268 0.033 Uiso 0.239(8) 1 calc R U P A -2
H3C H 0.238627 0.710747 0.108751 0.033 Uiso 0.239(8) 1 calc R U P A -2
C4 C 0.153(3) 0.750000 0.868(3) 0.044(6) Uani 0.479(16) 2 d S TU P A 2
H4A H 0.169128 0.791104 0.920066 0.066 Uiso 0.239(8) 1 calc R U P A 2
H4B H 0.067849 0.750604 0.819382 0.066 Uiso 0.479(16) 2 calc R U P A 2
H4C H 0.167661 0.708292 0.918607 0.066 Uiso 0.239(8) 1 calc R U P A 2
N2 N 0.0597(15) 0.750000 0.9227(16) 0.033(5) Uani 0.521(16) 2 d DS TU P A 1
C5 C -0.0342(15) 0.750000 0.8555(19) 0.024(4) Uani 0.521(16) 2 d DS TU P A 1
C6 C -0.1536(19) 0.750000 0.775(3) 0.039(7) Uani 0.521(16) 2 d DS TU P A 1
H6A H -0.173405 0.703380 0.741492 0.059 Uiso 0.261(8) 1 calc R U P A 1
H6B H -0.156047 0.782512 0.708218 0.059 Uiso 0.261(8) 1 calc R U P A 1
H6C H -0.213404 0.764108 0.818169 0.059 Uiso 0.261(8) 1 calc R U P A 1
N3 N 0.7737(12) 0.6168(7) 0.3136(12) 0.040(3) Uani 0.5 1 d D U P . .
C7 C 0.9131(17) 0.6170(12) 0.342(2) 0.062(4) Uani 0.5 1 d D U P B .
C8 C 0.9730(12) 0.5427(8) 0.3485(11) 0.074(3) Uani 1 1 d D U . . .
C9 C 0.726(3) 0.5761(14) 0.406(2) 0.032(5) Uani 0.300(19) 1 d D U P B 1
C10 C 0.761(2) 0.6038(13) 0.5357(19) 0.022(5) Uani 0.300(19) 1 d D U P B 1
C9X C 0.776(5) 0.644(2) 0.438(3) 0.045(6) Uani 0.200(19) 1 d D U P B 2
C10X C 0.721(6) 0.593(3) 0.513(4) 0.044(8) Uani 0.200(19) 1 d D U P B 2
C11 C 0.729(2) 0.6901(10) 0.316(3) 0.072(5) Uani 0.5 1 d D U P B .
C12 C 0.586(3) 0.6952(19) 0.274(4) 0.115(12) Uani 0.5 1 d D U P . .
C13 C 0.726(2) 0.5847(16) 0.1896(18) 0.077(6) Uani 0.5 1 d D U P B .
C14 C 0.7703(18) 0.6368(11) 0.0953(13) 0.114(7) Uani 1 1 d D U . . .
N4 N 0.9593(12) 0.5574(7) 0.1251(13) 0.041(3) Uani 0.5 1 d D U P B 2
C15 C 0.8195(18) 0.5687(13) 0.095(2) 0.067(5) Uani 0.5 1 d D U P B 2
C16 C 1.018(2) 0.5823(13) 0.2541(17) 0.057(4) Uani 0.5 1 d D U P B 2
C17 C 1.024(3) 0.5952(14) 0.046(2) 0.068(6) Uani 0.5 1 d D U P B 2
C18 C 0.973(2) 0.5748(15) -0.093(2) 0.063(6) Uani 0.5 1 d D U P B 2
C19 C 0.968(2) 0.4791(9) 0.113(3) 0.056(5) Uani 0.5 1 d D U P B 2
C20 C 1.101(2) 0.4549(15) 0.146(3) 0.079(8) Uani 0.5 1 d D U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O6 1.595(5) . ?
V1 O4 2.000(4) . ?
V1 O2 2.004(4) . ?
V1 O3 2.041(6) . ?
V1 O5 2.044(6) . ?
V1 O1 2.283(5) . ?
V2 O10 1.583(8) . ?
V2 O1 1.999(5) . ?
V2 O1 1.999(5) 4_575 ?
V2 O7 2.047(5) 4_575 ?
V2 O7 2.047(5) . ?
V2 O2 2.364(8) . ?
V2 V4 2.909(2) . ?
V3 O12 1.577(5) . ?
V3 O14 1.983(6) . ?
V3 O8 1.984(6) . ?
V3 O1 1.997(4) . ?
V3 O11 2.035(5) . ?
V4 O13 1.587(8) . ?
V4 O1 2.002(5) 4_575 ?
V4 O1 2.002(5) . ?
V4 O15 2.050(5) . ?
V4 O15 2.050(5) 4_575 ?
V4 O4 2.324(8) . ?
S1 O9 1.440(5) . ?
S1 O7 1.477(5) . ?
S1 O8 1.491(6) . ?
S1 O3 1.492(6) . ?
S2 O16 1.442(6) . ?
S2 O15 1.483(5) . ?
S2 O5 1.494(6) . ?
S2 O14 1.495(6) . ?
O2 C1 1.48(2) . ?
O4 C4 1.46(3) . ?
O11 H11A 0.85(4) . ?
O11 H11B 0.85(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 C2 1.14(4) . ?
C2 C3 1.43(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N2 C5 1.14(2) . ?
C5 C6 1.42(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6A 0.98(10) 4_575 ?
C6 H6B 1.0(2) 4_575 ?
C6 H6C 0.98(13) 4_575 ?
N3 C9X 1.50(3) . ?
N3 C11 1.51(2) . ?
N3 C13 1.513(19) . ?
N3 C7 1.525(19) . ?
N3 C9 1.53(2) . ?
C7 C8 1.58(2) . ?
C7 C16 1.87(3) . ?
C8 C16 1.52(2) . ?
C9 C10 1.53(2) . ?
C9X C10X 1.53(3) . ?
C9X C11 1.62(5) . ?
C11 C12 1.57(3) . ?
C13 C14 1.64(2) . ?
C13 C15 1.73(3) . ?
C14 C15 1.43(2) . ?
N4 C17 1.49(2) . ?
N4 C19 1.526(18) . ?
N4 C16 1.528(19) . ?
N4 C15 1.543(19) . ?
C17 C18 1.59(2) . ?
C18 C20 1.07(4) 3_765 ?
C18 C19 1.29(3) 3_765 ?
C19 C20 1.53(2) . ?

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
O6 V1 O4 103.2(3) . . ?
O6 V1 O2 103.5(3) . . ?
O4 V1 O2 75.5(2) . . ?
O6 V1 O3 97.7(3) . . ?
O4 V1 O3 157.2(3) . . ?
O2 V1 O3 90.8(2) . . ?
O6 V1 O5 96.7(3) . . ?
O4 V1 O5 91.2(2) . . ?
O2 V1 O5 157.9(3) . . ?
O3 V1 O5 95.5(2) . . ?
O6 V1 O1 175.7(2) . . ?
O4 V1 O1 79.4(2) . . ?
O2 V1 O1 80.4(2) . . ?
O3 V1 O1 80.4(2) . . ?
O5 V1 O1 79.7(2) . . ?
O10 V2 O1 105.2(2) . . ?
O10 V2 O1 105.2(2) . 4_575 ?
O1 V2 O1 84.8(3) . 4_575 ?
O10 V2 O7 100.0(3) . 4_575 ?
O1 V2 O7 154.8(2) . 4_575 ?
O1 V2 O7 89.0(2) 4_575 4_575 ?
O10 V2 O7 100.0(3) . . ?
O1 V2 O7 89.0(2) . . ?
O1 V2 O7 154.8(2) 4_575 . ?
O7 V2 O7 86.2(3) 4_575 . ?
O10 V2 O2 174.8(3) . . ?
O1 V2 O2 78.55(18) . . ?
O1 V2 O2 78.55(18) 4_575 . ?
O7 V2 O2 76.30(19) 4_575 . ?
O7 V2 O2 76.30(19) . . ?
O10 V2 V4 100.7(3) . . ?
O1 V2 V4 43.39(13) . . ?
O1 V2 V4 43.39(13) 4_575 . ?
O7 V2 V4 131.68(15) 4_575 . ?
O7 V2 V4 131.68(15) . . ?
O2 V2 V4 84.55(17) . . ?
O12 V3 O14 110.6(3) . . ?
O12 V3 O8 110.4(3) . . ?
O14 V3 O8 137.6(3) . . ?
O12 V3 O1 103.8(2) . . ?
O14 V3 O1 90.6(2) . . ?
O8 V3 O1 89.7(2) . . ?
O12 V3 O11 101.1(3) . . ?
O14 V3 O11 81.0(2) . . ?
O8 V3 O11 81.2(2) . . ?
O1 V3 O11 155.0(2) . . ?
O13 V4 O1 104.6(2) . 4_575 ?
O13 V4 O1 104.6(2) . . ?
O1 V4 O1 84.7(3) 4_575 . ?
O13 V4 O15 100.6(3) . . ?
O1 V4 O15 154.8(2) 4_575 . ?
O1 V4 O15 89.9(2) . . ?
O13 V4 O15 100.6(3) . 4_575 ?
O1 V4 O15 89.88(19) 4_575 4_575 ?
O1 V4 O15 154.8(2) . 4_575 ?
O15 V4 O15 84.6(3) . 4_575 ?
O13 V4 O4 175.9(3) . . ?
O1 V4 O4 78.34(18) 4_575 . ?
O1 V4 O4 78.34(18) . . ?
O15 V4 O4 76.45(19) . . ?
O15 V4 O4 76.45(19) 4_575 . ?
O13 V4 V2 99.8(3) . . ?
O1 V4 V2 43.33(14) 4_575 . ?
O1 V4 V2 43.33(14) . . ?
O15 V4 V2 132.43(15) . . ?
O15 V4 V2 132.43(15) 4_575 . ?
O4 V4 V2 84.26(17) . . ?
O9 S1 O7 110.9(3) . . ?
O9 S1 O8 109.6(3) . . ?
O7 S1 O8 108.8(3) . . ?
O9 S1 O3 110.1(4) . . ?
O7 S1 O3 109.9(3) . . ?
O8 S1 O3 107.4(4) . . ?
O16 S2 O15 110.9(3) . . ?
O16 S2 O5 110.0(4) . . ?
O15 S2 O5 110.4(3) . . ?
O16 S2 O14 110.0(3) . . ?
O15 S2 O14 108.0(3) . . ?
O5 S2 O14 107.5(3) . . ?
V3 O1 V2 119.5(2) . . ?
V3 O1 V4 118.6(2) . . ?
V2 O1 V4 93.28(18) . . ?
V3 O1 V1 118.4(2) . . ?
V2 O1 V1 101.33(19) . . ?
V4 O1 V1 101.2(2) . . ?
C1 O2 V1 114.4(6) . . ?
C1 O2 V1 114.4(6) . 4_575 ?
V1 O2 V1 103.2(3) . 4_575 ?
C1 O2 V2 124.7(12) . . ?
V1 O2 V2 98.5(2) . . ?
V1 O2 V2 98.5(2) 4_575 . ?
S1 O3 V1 129.5(3) . . ?
C4 O4 V1 114.0(7) . . ?
V1 O4 V1 103.4(3) . 4_575 ?
C4 O4 V4 122.9(13) . . ?
V1 O4 V4 99.8(2) . . ?
V1 O4 V4 99.8(2) 4_575 . ?
S2 O5 V1 129.9(3) . . ?
S1 O7 V2 124.5(3) . . ?
S1 O8 V3 124.7(3) . . ?
V3 O11 H11A 127(8) . . ?
V3 O11 H11B 121(8) . . ?
H11A O11 H11B 91(9) . . ?
S2 O14 V3 123.5(3) . . ?
S2 O15 V4 123.6(3) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1A N1 H1B 73.9 4_575 4_575 ?
N1 C2 C3 177(6) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 N2 H4A 128.7(17) . 4_575 ?
C5 N2 H4C 127.9(17) . 4_575 ?
N2 C5 C6 178(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6 H6A 109(2) . 4_575 ?
H6A C6 H6A 133.6 . 4_575 ?
H6B C6 H6A 32.3 . 4_575 ?
H6C C6 H6A 79.7 . 4_575 ?
C5 C6 H6B 109(5) . 4_575 ?
H6A C6 H6B 32.3 . 4_575 ?
H6B C6 H6B 79.7 . 4_575 ?
H6C C6 H6B 133.6 . 4_575 ?
H6A C6 H6B 109.5 4_575 4_575 ?
C5 C6 H6C 109(3) . 4_575 ?
H6A C6 H6C 79.7 . 4_575 ?
H6B C6 H6C 133.6 . 4_575 ?
H6C C6 H6C 32.3 . 4_575 ?
H6A C6 H6C 109.5 4_575 4_575 ?
H6B C6 H6C 109.5 4_575 4_575 ?
C9X N3 C11 65(2) . . ?
C9X N3 C13 160(2) . . ?
C11 N3 C13 111.5(19) . . ?
C9X N3 C7 92(2) . . ?
C11 N3 C7 109.1(16) . . ?
C13 N3 C7 107.0(17) . . ?
C11 N3 C9 106.7(18) . . ?
C13 N3 C9 109.8(15) . . ?
C7 N3 C9 112.8(17) . . ?
N3 C7 C8 114.5(15) . . ?
N3 C7 C16 130.7(17) . . ?
C8 C7 C16 51.3(10) . . ?
C16 C8 C7 74.3(15) . . ?
C10 C9 N3 116.3(18) . . ?
N3 C9X C10X 113(3) . . ?
N3 C9X C11 57.5(15) . . ?
C10X C9X C11 138(4) . . ?
N3 C11 C12 112.3(19) . . ?
N3 C11 C9X 57.4(14) . . ?
C12 C11 C9X 113(3) . . ?
N3 C13 C14 105.7(17) . . ?
N3 C13 C15 122.6(18) . . ?
C14 C13 C15 50.1(10) . . ?
C15 C14 C13 67.9(16) . . ?
C17 N4 C19 112.0(18) . . ?
C17 N4 C16 105.7(16) . . ?
C19 N4 C16 112.3(17) . . ?
C17 N4 C15 115.6(18) . . ?
C19 N4 C15 101.9(14) . . ?
C16 N4 C15 109.4(16) . . ?
C14 C15 N4 120.5(19) . . ?
C14 C15 C13 62.0(13) . . ?
N4 C15 C13 130.0(18) . . ?
C8 C16 N4 112.8(16) . . ?
C8 C16 C7 54.4(11) . . ?
N4 C16 C7 117.1(16) . . ?
N4 C17 C18 112.1(18) . . ?
C20 C18 C17 137(3) 3_765 . ?
C19 C18 C17 108(2) 3_765 . ?
C18 C19 N4 150(2) 3_765 . ?
C18 C19 C20 43.5(17) 3_765 . ?
N4 C19 C20 111.3(17) . . ?
C18 C20 C19 56(2) 3_765 . ?

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
O9 S1 O3 V1 -156.9(4) . . . . ?
O7 S1 O3 V1 -34.4(5) . . . . ?
O8 S1 O3 V1 83.8(5) . . . . ?
O16 S2 O5 V1 154.5(4) . . . . ?
O15 S2 O5 V1 31.7(6) . . . . ?
O14 S2 O5 V1 -85.9(5) . . . . ?
O9 S1 O7 V2 -176.9(4) . . . . ?
O8 S1 O7 V2 -56.2(4) . . . . ?
O3 S1 O7 V2 61.1(4) . . . . ?
O9 S1 O8 V3 -166.8(4) . . . . ?
O7 S1 O8 V3 71.7(5) . . . . ?
O3 S1 O8 V3 -47.2(5) . . . . ?
O16 S2 O14 V3 164.1(4) . . . . ?
O15 S2 O14 V3 -74.7(5) . . . . ?
O5 S2 O14 V3 44.4(5) . . . . ?
O16 S2 O15 V4 177.6(4) . . . . ?
O5 S2 O15 V4 -60.2(4) . . . . ?
O14 S2 O15 V4 57.0(4) . . . . ?
C9X N3 C7 C8 113(2) . . . . ?
C11 N3 C7 C8 177(2) . . . . ?
C13 N3 C7 C8 -62(2) . . . . ?
C9 N3 C7 C8 59(2) . . . . ?
C9X N3 C7 C16 172(3) . . . . ?
C11 N3 C7 C16 -124(2) . . . . ?
C13 N3 C7 C16 -3(3) . . . . ?
N3 C7 C8 C16 124(2) . . . . ?
C11 N3 C9 C10 -56(3) . . . . ?
C13 N3 C9 C10 -177(2) . . . . ?
C7 N3 C9 C10 63(3) . . . . ?
C11 N3 C9X C10X 133(5) . . . . ?
C13 N3 C9X C10X 48(10) . . . . ?
C7 N3 C9X C10X -117(4) . . . . ?
C13 N3 C9X C11 -84(7) . . . . ?
C7 N3 C9X C11 110.2(18) . . . . ?
C9X N3 C11 C12 -103(4) . . . . ?
C13 N3 C11 C12 56(3) . . . . ?
C7 N3 C11 C12 174(3) . . . . ?
C9 N3 C11 C12 -64(3) . . . . ?
C13 N3 C11 C9X 159(2) . . . . ?
C7 N3 C11 C9X -83(3) . . . . ?
C10X C9X C11 N3 -90(4) . . . . ?
N3 C9X C11 C12 103(3) . . . . ?
C10X C9X C11 C12 13(5) . . . . ?
C9X N3 C13 C14 132(7) . . . . ?
C11 N3 C13 C14 56(2) . . . . ?
C7 N3 C13 C14 -63(2) . . . . ?
C9 N3 C13 C14 174.1(19) . . . . ?
C9X N3 C13 C15 -176(6) . . . . ?
C11 N3 C13 C15 108(2) . . . . ?
C7 N3 C13 C15 -11(3) . . . . ?
N3 C13 C14 C15 120(2) . . . . ?
C13 C14 C15 N4 -122(2) . . . . ?
C17 N4 C15 C14 -58(3) . . . . ?
C19 N4 C15 C14 -180(2) . . . . ?
C16 N4 C15 C14 61(3) . . . . ?
C17 N4 C15 C13 -135(2) . . . . ?
C19 N4 C15 C13 103(3) . . . . ?
C16 N4 C15 C13 -16(3) . . . . ?
N3 C13 C15 C14 -83(2) . . . . ?
N3 C13 C15 N4 24(4) . . . . ?
C14 C13 C15 N4 108(3) . . . . ?
C7 C8 C16 N4 -107.9(19) . . . . ?
C17 N4 C16 C8 -173(2) . . . . ?
C19 N4 C16 C8 -51(2) . . . . ?
C15 N4 C16 C8 62(2) . . . . ?
C17 N4 C16 C7 126.3(19) . . . . ?
C19 N4 C16 C7 -111.2(19) . . . . ?
C15 N4 C16 C7 1(2) . . . . ?
N3 C7 C16 C8 -91(2) . . . . ?
N3 C7 C16 N4 9(3) . . . . ?
C8 C7 C16 N4 99.7(19) . . . . ?
C19 N4 C17 C18 57(3) . . . . ?
C16 N4 C17 C18 180(2) . . . . ?
C15 N4 C17 C18 -59(3) . . . . ?
N4 C17 C18 C20 8(5) . . . 3_765 ?
N4 C17 C18 C19 -87(3) . . . 3_765 ?
C17 N4 C19 C18 31(6) . . . 3_765 ?
C16 N4 C19 C18 -88(5) . . . 3_765 ?
C15 N4 C19 C18 155(5) . . . 3_765 ?
C17 N4 C19 C20 59(3) . . . . ?
C16 N4 C19 C20 -60(3) . . . . ?
C15 N4 C19 C20 -177(2) . . . . ?
N4 C19 C20 C18 -160(3) . . . 3_765 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O11 H11A O16 0.85(4) 1.84(5) 2.667(8) 165(11) 3_667 yes
O11 H11B O9 0.85(4) 1.84(4) 2.681(8) 173(12) 3_666 yes

_refine_diff_density_max         1.178
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.131


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitril'
####################################################################### 
# 
# 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_2_4MeCN
_database_code_depnum_ccdc_archive 'CCDC 1574240'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O25 S4 V5 5-, 5(C6 H16 N 1+), 4(C2 H3 N)'
_chemical_formula_sum            'C38 H92 N9 O25 S4 V5'
_chemical_formula_weight         1458.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   13.4462(15)
_cell_length_b                   13.5404(16)
_cell_length_c                   35.104(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6391.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    21709
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      28.80

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             3048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.260
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.914
_shelx_estimated_absorpt_T_min   0.392
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69277
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.612
_diffrn_reflns_theta_max         29.177
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17270
_reflns_number_gt                15629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,In one HNEt3+ cation all three CH2 groups modelled as disordered over two sets of positions with major occupancy 64.8(5)%'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0368P)²+2.3698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.207(15)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         17270
_refine_ls_number_parameters     790
_refine_ls_number_restraints     139
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.41463(4) 0.31640(4) 0.89816(2) 0.01943(12) Uani 1 1 d . . . . .
O1 O 0.4294(2) 0.21911(18) 0.92303(9) 0.0323(6) Uani 1 1 d . . . . .
V2 V 0.18378(4) 0.45551(4) 0.90373(2) 0.01621(11) Uani 1 1 d . . . . .
O2 O 0.09422(18) 0.42690(19) 0.93130(7) 0.0261(5) Uani 1 1 d . . . . .
V3 V 0.32885(4) 0.68186(4) 0.91370(2) 0.01716(11) Uani 1 1 d . . . . .
O3 O 0.30626(19) 0.76476(18) 0.94472(8) 0.0280(5) Uani 1 1 d . . . . .
V4 V 0.56080(4) 0.53959(4) 0.91353(2) 0.01765(11) Uani 1 1 d . . . . .
O4 O 0.64422(18) 0.54807(19) 0.94562(8) 0.0267(5) Uani 1 1 d . . . . .
V5 V 0.36810(4) 0.48534(4) 0.94552(2) 0.01724(11) Uani 1 1 d . . . . .
O5 O 0.36366(19) 0.47062(19) 0.99063(7) 0.0253(5) Uani 1 1 d . . . . .
O6 O 0.30025(17) 0.38200(16) 0.92189(7) 0.0187(5) Uani 1 1 d . . . . .
O7 O 0.25920(17) 0.56052(16) 0.92887(7) 0.0182(5) Uani 1 1 d . . . . .
O8 O 0.43946(16) 0.60097(16) 0.93337(6) 0.0178(4) Uani 1 1 d . . . . .
O9 O 0.48128(16) 0.42225(16) 0.92640(7) 0.0176(5) Uani 1 1 d . . . . .
S1 S 0.22367(6) 0.27105(6) 0.84688(2) 0.01956(16) Uani 1 1 d . . . . .
O10 O 0.33405(18) 0.27544(18) 0.85358(7) 0.0256(5) Uani 1 1 d . . . . .
O11 O 0.17860(18) 0.36796(16) 0.85845(7) 0.0217(5) Uani 1 1 d . . . . .
O12 O 0.1814(2) 0.19337(18) 0.87065(8) 0.0313(6) Uani 1 1 d . . . . .
O13 O 0.2065(2) 0.2559(2) 0.80711(8) 0.0369(7) Uani 1 1 d . . . . .
S2 S 0.12344(6) 0.66490(5) 0.86968(2) 0.01821(15) Uani 1 1 d . . . . .
O14 O 0.12842(18) 0.55389(16) 0.86772(7) 0.0203(5) Uani 1 1 d . . . . .
O15 O 0.22889(17) 0.70124(16) 0.87288(7) 0.0221(5) Uani 1 1 d . . . . .
O16 O 0.0672(2) 0.6956(2) 0.90305(8) 0.0313(6) Uani 1 1 d . . . . .
O17 O 0.0825(2) 0.70102(18) 0.83443(7) 0.0277(6) Uani 1 1 d . . . . .
S3 S 0.53098(6) 0.75563(6) 0.87642(2) 0.02048(16) Uani 1 1 d . . . . .
O18 O 0.42003(17) 0.74021(17) 0.87536(7) 0.0214(5) Uani 1 1 d . . . . .
O19 O 0.57972(18) 0.65574(18) 0.87944(8) 0.0269(5) Uani 1 1 d . . . . .
O20 O 0.5578(2) 0.8177(2) 0.90778(9) 0.0382(7) Uani 1 1 d . . . . .
O21 O 0.5607(2) 0.7959(2) 0.83965(8) 0.0312(6) Uani 1 1 d . . . . .
S4 S 0.63231(6) 0.35334(6) 0.86700(2) 0.02002(16) Uani 1 1 d . . . . .
O22 O 0.62344(18) 0.46346(17) 0.87109(7) 0.0226(5) Uani 1 1 d . . . . .
O23 O 0.53011(18) 0.31190(19) 0.86200(8) 0.0260(5) Uani 1 1 d . . . . .
O24 O 0.67975(19) 0.31161(19) 0.90078(7) 0.0273(5) Uani 1 1 d . . . . .
O25 O 0.68942(18) 0.33267(19) 0.83287(7) 0.0272(5) Uani 1 1 d . . . . .
N1 N 0.2480(3) 0.0056(2) 0.85747(10) 0.0317(7) Uani 1 1 d D . . . .
H1 H 0.228(3) 0.064(3) 0.8632(13) 0.038 Uiso 1 1 d D U . . .
C1 C 0.1649(3) -0.0572(3) 0.87065(14) 0.0423(10) Uani 1 1 d . . . . .
H1A H 0.1509 -0.0422 0.8977 0.051 Uiso 1 1 calc R U . . .
H1B H 0.1851 -0.1273 0.8690 0.051 Uiso 1 1 calc R U . . .
C2 C 0.0722(4) -0.0424(4) 0.84796(18) 0.0581(14) Uani 1 1 d . . . . .
H2A H 0.0577 0.0284 0.8461 0.087 Uiso 1 1 calc R U . . .
H2B H 0.0167 -0.0760 0.8605 0.087 Uiso 1 1 calc R U . . .
H2C H 0.0814 -0.0698 0.8224 0.087 Uiso 1 1 calc R U . . .
C3 C 0.2706(3) -0.0015(3) 0.81622(13) 0.0387(10) Uani 1 1 d . . . . .
H3A H 0.3277 0.0420 0.8103 0.046 Uiso 1 1 calc R U . . .
H3B H 0.2126 0.0226 0.8015 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2951(4) -0.1061(4) 0.80353(15) 0.0530(13) Uani 1 1 d . . . . .
H4A H 0.3514 -0.1312 0.8184 0.079 Uiso 1 1 calc R U . . .
H4B H 0.3126 -0.1059 0.7764 0.079 Uiso 1 1 calc R U . . .
H4C H 0.2371 -0.1487 0.8076 0.079 Uiso 1 1 calc R U . . .
C5 C 0.3399(4) -0.0091(4) 0.88158(14) 0.0458(11) Uani 1 1 d . . . . .
H5A H 0.3646 -0.0773 0.8777 0.055 Uiso 1 1 calc R U . . .
H5B H 0.3922 0.0368 0.8726 0.055 Uiso 1 1 calc R U . . .
C6 C 0.3241(4) 0.0070(3) 0.92318(15) 0.0533(13) Uani 1 1 d . . . . .
H6A H 0.2919 0.0711 0.9272 0.080 Uiso 1 1 calc R U . . .
H6B H 0.3884 0.0062 0.9363 0.080 Uiso 1 1 calc R U . . .
H6C H 0.2817 -0.0456 0.9334 0.080 Uiso 1 1 calc R U . . .
N2 N 0.0448(3) 0.7145(3) 0.98109(11) 0.0376(8) Uani 1 1 d D U . . .
H2 H 0.063(4) 0.699(4) 0.9563(15) 0.045 Uiso 1 1 d . U . . .
C7 C -0.0149(6) 0.6303(5) 0.9959(2) 0.0465(19) Uani 0.648(6) 1 d D U P A 1
H7A H -0.0437 0.6487 1.0208 0.056 Uiso 0.648(6) 1 calc R U P A 1
H7B H 0.0294 0.5729 1.0000 0.056 Uiso 0.648(6) 1 calc R U P A 1
C8 C -0.0979(5) 0.6006(5) 0.96924(18) 0.0677(16) Uani 1 1 d D U . . .
H8A H -0.1348 0.5452 0.9803 0.102 Uiso 0.648(6) 1 calc R U P A 1
H8B H -0.1429 0.6567 0.9655 0.102 Uiso 0.648(6) 1 calc R U P A 1
H8C H -0.0697 0.5808 0.9446 0.102 Uiso 0.648(6) 1 calc R U P A 1
H8D H -0.1697 0.6033 0.9648 0.102 Uiso 0.352(6) 1 calc R U P A 2
H8E H -0.0651 0.5695 0.9474 0.102 Uiso 0.352(6) 1 calc R U P A 2
H8F H -0.0845 0.5620 0.9923 0.102 Uiso 0.352(6) 1 calc R U P A 2
C9 C -0.0225(5) 0.8061(5) 0.97734(19) 0.0374(15) Uani 0.648(6) 1 d D U P A 1
H9A H -0.0789 0.7902 0.9603 0.045 Uiso 0.648(6) 1 calc R U P A 1
H9B H -0.0500 0.8228 1.0027 0.045 Uiso 0.648(6) 1 calc R U P A 1
C10 C 0.0308(4) 0.8922(3) 0.96215(16) 0.0529(13) Uani 1 1 d D U . . .
H10A H -0.0149 0.9483 0.9603 0.079 Uiso 0.648(6) 1 calc R U P A 1
H10B H 0.0860 0.9092 0.9792 0.079 Uiso 0.648(6) 1 calc R U P A 1
H10C H 0.0570 0.8766 0.9368 0.079 Uiso 0.648(6) 1 calc R U P A 1
H10D H 0.0522 0.9581 0.9703 0.079 Uiso 0.352(6) 1 calc R U P A 2
H10E H 0.0565 0.8788 0.9365 0.079 Uiso 0.352(6) 1 calc R U P A 2
H10F H -0.0420 0.8892 0.9618 0.079 Uiso 0.352(6) 1 calc R U P A 2
C11 C 0.1296(5) 0.7423(5) 1.00736(17) 0.0339(14) Uani 0.648(6) 1 d D U P A 1
H11A H 0.1018 0.7702 1.0312 0.041 Uiso 0.648(6) 1 calc R U P A 1
H11B H 0.1701 0.7944 0.9950 0.041 Uiso 0.648(6) 1 calc R U P A 1
C12 C 0.1968(4) 0.6551(4) 1.01734(14) 0.0481(11) Uani 1 1 d D U . . .
H12A H 0.2501 0.6775 1.0343 0.072 Uiso 0.648(6) 1 calc R U P A 1
H12B H 0.1576 0.6039 1.0301 0.072 Uiso 0.648(6) 1 calc R U P A 1
H12C H 0.2259 0.6281 0.9940 0.072 Uiso 0.648(6) 1 calc R U P A 1
H12D H 0.2232 0.6000 1.0324 0.072 Uiso 0.352(6) 1 calc R U P A 2
H12E H 0.2387 0.6654 0.9948 0.072 Uiso 0.352(6) 1 calc R U P A 2
H12F H 0.1966 0.7152 1.0329 0.072 Uiso 0.352(6) 1 calc R U P A 2
C7X C -0.0611(9) 0.6966(9) 0.9739(4) 0.041(3) Uani 0.352(6) 1 d D U P A 2
H7C H -0.0983 0.7267 0.9953 0.049 Uiso 0.352(6) 1 calc R U P A 2
H7D H -0.0791 0.7341 0.9507 0.049 Uiso 0.352(6) 1 calc R U P A 2
C9X C 0.0709(11) 0.8152(9) 0.9898(4) 0.050(3) Uani 0.352(6) 1 d D U P A 2
H9C H 0.1444 0.8206 0.9905 0.060 Uiso 0.352(6) 1 calc R U P A 2
H9D H 0.0461 0.8310 1.0157 0.060 Uiso 0.352(6) 1 calc R U P A 2
C11X C 0.0949(9) 0.6322(10) 1.0052(4) 0.043(3) Uani 0.352(6) 1 d D U P A 2
H11C H 0.0538 0.6202 1.0282 0.051 Uiso 0.352(6) 1 calc R U P A 2
H11D H 0.0959 0.5704 0.9902 0.051 Uiso 0.352(6) 1 calc R U P A 2
N3 N 0.7549(2) 0.7290(3) 0.82414(9) 0.0291(7) Uani 1 1 d . . . . .
H3 H 0.687(3) 0.745(3) 0.8285(12) 0.035 Uiso 1 1 d . U . . .
C13 C 0.7866(3) 0.7916(3) 0.79073(11) 0.0314(8) Uani 1 1 d . . . . .
H13A H 0.7776 0.8620 0.7974 0.038 Uiso 1 1 calc R U . . .
H13B H 0.7427 0.7768 0.7688 0.038 Uiso 1 1 calc R U . . .
C14 C 0.8947(3) 0.7749(3) 0.77878(13) 0.0366(9) Uani 1 1 d . . . . .
H14A H 0.9389 0.7929 0.7998 0.055 Uiso 1 1 calc R U . . .
H14B H 0.9099 0.8159 0.7565 0.055 Uiso 1 1 calc R U . . .
H14C H 0.9044 0.7051 0.7723 0.055 Uiso 1 1 calc R U . . .
C15 C 0.8135(3) 0.7478(4) 0.85995(12) 0.0397(10) Uani 1 1 d . . . . .
H15A H 0.8843 0.7319 0.8552 0.048 Uiso 1 1 calc R U . . .
H15B H 0.7893 0.7031 0.8803 0.048 Uiso 1 1 calc R U . . .
C16 C 0.8055(4) 0.8542(4) 0.87367(16) 0.0525(13) Uani 1 1 d . . . . .
H16A H 0.8381 0.8981 0.8553 0.079 Uiso 1 1 calc R U . . .
H16B H 0.8379 0.8606 0.8985 0.079 Uiso 1 1 calc R U . . .
H16C H 0.7352 0.8725 0.8760 0.079 Uiso 1 1 calc R U . . .
C17 C 0.7556(3) 0.6205(3) 0.81532(13) 0.0379(10) Uani 1 1 d . . . . .
H17A H 0.8240 0.6006 0.8081 0.046 Uiso 1 1 calc R U . . .
H17B H 0.7371 0.5835 0.8386 0.046 Uiso 1 1 calc R U . . .
C18 C 0.6858(5) 0.5927(4) 0.78376(17) 0.0621(15) Uani 1 1 d . . . . .
H18A H 0.6190 0.6172 0.7896 0.093 Uiso 1 1 calc R U . . .
H18B H 0.6840 0.5206 0.7812 0.093 Uiso 1 1 calc R U . . .
H18C H 0.7089 0.6220 0.7598 0.093 Uiso 1 1 calc R U . . .
N4 N 0.6525(3) 0.2568(3) 0.97609(10) 0.0349(8) Uani 1 1 d . . . . .
H4 H 0.650(4) 0.273(4) 0.9524(14) 0.042 Uiso 1 1 d . U . . .
C19 C 0.7605(3) 0.2495(4) 0.98612(14) 0.0432(10) Uani 1 1 d . . . . .
H19A H 0.7923 0.1985 0.9700 0.052 Uiso 1 1 calc R U . . .
H19B H 0.7671 0.2285 1.0130 0.052 Uiso 1 1 calc R U . . .
C20 C 0.8141(4) 0.3468(4) 0.98061(15) 0.0550(13) Uani 1 1 d . . . . .
H20A H 0.7985 0.3734 0.9553 0.083 Uiso 1 1 calc R U . . .
H20B H 0.8860 0.3363 0.9827 0.083 Uiso 1 1 calc R U . . .
H20C H 0.7925 0.3937 1.0002 0.083 Uiso 1 1 calc R U . . .
C21 C 0.5950(4) 0.3324(4) 0.99877(13) 0.0463(12) Uani 1 1 d . . . . .
H21A H 0.6241 0.3984 0.9940 0.056 Uiso 1 1 calc R U . . .
H21B H 0.5255 0.3337 0.9895 0.056 Uiso 1 1 calc R U . . .
C22 C 0.5942(5) 0.3136(4) 1.04077(13) 0.0568(14) Uani 1 1 d . . . . .
H22A H 0.5623 0.2500 1.0459 0.085 Uiso 1 1 calc R U . . .
H22B H 0.5572 0.3663 1.0536 0.085 Uiso 1 1 calc R U . . .
H22C H 0.6627 0.3123 1.0503 0.085 Uiso 1 1 calc R U . . .
C23 C 0.6028(4) 0.1562(4) 0.97717(13) 0.0433(11) Uani 1 1 d . . . . .
H23A H 0.6193 0.1232 1.0015 0.052 Uiso 1 1 calc R U . . .
H23B H 0.5298 0.1649 0.9761 0.052 Uiso 1 1 calc R U . . .
C24 C 0.6353(4) 0.0916(4) 0.94452(15) 0.0524(12) Uani 1 1 d . . . . .
H24A H 0.6308 0.1289 0.9206 0.079 Uiso 1 1 calc R U . . .
H24B H 0.5921 0.0334 0.9431 0.079 Uiso 1 1 calc R U . . .
H24C H 0.7042 0.0705 0.9486 0.079 Uiso 1 1 calc R U . . .
N5 N 0.8938(2) 0.2927(2) 0.84217(10) 0.0277(7) Uani 1 1 d . . . . .
H5 H 0.825(3) 0.298(3) 0.8428(12) 0.033 Uiso 1 1 d . U . . .
C25 C 0.9304(3) 0.3978(3) 0.84173(12) 0.0317(8) Uani 1 1 d . . . . .
H25A H 1.0041 0.3971 0.8415 0.038 Uiso 1 1 calc R U . . .
H25B H 0.9080 0.4295 0.8178 0.038 Uiso 1 1 calc R U . . .
C26 C 0.8964(3) 0.4598(3) 0.87459(13) 0.0362(9) Uani 1 1 d . . . . .
H26A H 0.8238 0.4568 0.8765 0.054 Uiso 1 1 calc R U . . .
H26B H 0.9172 0.5284 0.8706 0.054 Uiso 1 1 calc R U . . .
H26C H 0.9261 0.4348 0.8982 0.054 Uiso 1 1 calc R U . . .
C27 C 0.9284(3) 0.2399(3) 0.87742(12) 0.0348(9) Uani 1 1 d . . . . .
H27A H 0.9202 0.2841 0.8997 0.042 Uiso 1 1 calc R U . . .
H27B H 1.0001 0.2245 0.8749 0.042 Uiso 1 1 calc R U . . .
C28 C 0.8716(3) 0.1452(3) 0.88447(14) 0.0416(10) Uani 1 1 d . . . . .
H28A H 0.8002 0.1594 0.8855 0.062 Uiso 1 1 calc R U . . .
H28B H 0.8930 0.1162 0.9087 0.062 Uiso 1 1 calc R U . . .
H28C H 0.8848 0.0985 0.8637 0.062 Uiso 1 1 calc R U . . .
C29 C 0.9253(3) 0.2394(3) 0.80677(12) 0.0348(9) Uani 1 1 d . . . . .
H29A H 0.9143 0.1677 0.8103 0.042 Uiso 1 1 calc R U . . .
H29B H 0.9974 0.2499 0.8028 0.042 Uiso 1 1 calc R U . . .
C30 C 0.8696(3) 0.2732(3) 0.77152(12) 0.0391(9) Uani 1 1 d . . . . .
H30A H 0.7978 0.2684 0.7761 0.059 Uiso 1 1 calc R U . . .
H30B H 0.8878 0.2311 0.7499 0.059 Uiso 1 1 calc R U . . .
H30C H 0.8872 0.3418 0.7658 0.059 Uiso 1 1 calc R U . . .
N6 N 0.3841(2) 0.4972(2) 0.85447(9) 0.0317(7) Uani 1 1 d . . . . .
C31 C 0.3765(3) 0.5532(3) 0.83011(11) 0.0302(8) Uani 1 1 d . . . . .
C32 C 0.3679(4) 0.6270(3) 0.80013(12) 0.0405(10) Uani 1 1 d . . . . .
H32A H 0.3012 0.6562 0.8008 0.061 Uiso 1 1 calc R U . . .
H32B H 0.3790 0.5958 0.7753 0.061 Uiso 1 1 calc R U . . .
H32C H 0.4177 0.6789 0.8042 0.061 Uiso 1 1 calc R U . . .
N7 N -0.0427(4) 0.5231(4) 0.74901(16) 0.0657(13) Uani 1 1 d . . . . .
C33 C 0.0363(5) 0.5171(3) 0.76111(14) 0.0462(12) Uani 1 1 d . . . . .
C34 C 0.1357(4) 0.5073(4) 0.77643(13) 0.0489(12) Uani 1 1 d . . . . .
H34A H 0.1446 0.4407 0.7868 0.073 Uiso 1 1 calc R U . . .
H34B H 0.1455 0.5560 0.7968 0.073 Uiso 1 1 calc R U . . .
H34C H 0.1844 0.5188 0.7562 0.073 Uiso 1 1 calc R U . . .
N8 N 0.5195(7) 0.9636(8) 0.7544(2) 0.122(3) Uani 1 1 d . . . . .
C35 C 0.5205(5) 0.8872(9) 0.7423(2) 0.088(3) Uani 1 1 d . . . . .
C36 C 0.5226(6) 0.7880(7) 0.72711(19) 0.085(2) Uani 1 1 d . . . . .
H36A H 0.4559 0.7697 0.7183 0.128 Uiso 1 1 calc R U . . .
H36B H 0.5438 0.7420 0.7471 0.128 Uiso 1 1 calc R U . . .
H36C H 0.5693 0.7849 0.7057 0.128 Uiso 1 1 calc R U . . .
N9 N 0.7446(4) 0.0603(4) 0.80524(16) 0.0687(14) Uani 1 1 d . . . . .
C37 C 0.6688(4) 0.0597(4) 0.81937(14) 0.0469(11) Uani 1 1 d . . . . .
C38 C 0.5733(4) 0.0568(4) 0.8377(2) 0.0680(17) Uani 1 1 d . . . . .
H38A H 0.5213 0.0477 0.8185 0.102 Uiso 1 1 calc R U . . .
H38B H 0.5621 0.1190 0.8513 0.102 Uiso 1 1 calc R U . . .
H38C H 0.5716 0.0018 0.8558 0.102 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.593(3) . ?
V1 O9 1.960(2) . ?
V1 O6 1.962(2) . ?
V1 O10 1.983(3) . ?
V1 O23 2.007(3) . ?
V1 V5 2.8962(8) . ?
V2 O2 1.593(2) . ?
V2 O7 1.957(2) . ?
V2 O6 1.962(2) . ?
V2 O14 1.981(2) . ?
V2 O11 1.984(2) . ?
V2 V5 2.9082(8) . ?
V3 O3 1.593(2) . ?
V3 O7 1.965(2) . ?
V3 O8 1.972(2) . ?
V3 O15 1.982(2) . ?
V3 O18 1.985(2) . ?
V3 V5 2.9338(8) . ?
V4 O4 1.594(3) . ?
V4 O8 1.959(2) . ?
V4 O9 1.968(2) . ?
V4 O19 1.992(2) . ?
V4 O22 1.998(2) . ?
V4 V5 2.9180(8) . ?
V5 O5 1.597(2) . ?
V5 O6 1.865(2) . ?
V5 O9 1.870(2) . ?
V5 O7 1.877(2) . ?
V5 O8 1.885(2) . ?
S1 O13 1.430(3) . ?
S1 O12 1.458(3) . ?
S1 O11 1.501(2) . ?
S1 O10 1.504(3) . ?
S2 O17 1.440(3) . ?
S2 O16 1.455(3) . ?
S2 O15 1.505(2) . ?
S2 O14 1.506(2) . ?
S3 O20 1.432(3) . ?
S3 O21 1.457(3) . ?
S3 O19 1.507(2) . ?
S3 O18 1.507(2) . ?
S4 O25 1.450(3) . ?
S4 O24 1.460(3) . ?
S4 O23 1.495(3) . ?
S4 O22 1.503(2) . ?
N1 C1 1.478(5) . ?
N1 C3 1.483(6) . ?
N1 C5 1.511(6) . ?
N1 H1 0.86(3) . ?
C1 C2 1.492(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.520(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.492(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N2 C9X 1.441(12) . ?
N2 C7X 1.466(12) . ?
N2 C7 1.489(7) . ?
N2 C11 1.513(7) . ?
N2 C9 1.541(7) . ?
N2 C11X 1.554(12) . ?
N2 H2 0.93(5) . ?
C7 C8 1.509(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C7X 1.400(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 H8D 0.9800 . ?
C8 H8E 0.9800 . ?
C8 H8F 0.9800 . ?
C9 C10 1.469(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C9X 1.524(14) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C11 C12 1.528(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C11X 1.468(13) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 0.9800 . ?
C12 H12F 0.9800 . ?
C7X H7C 0.9900 . ?
C7X H7D 0.9900 . ?
C9X H9C 0.9900 . ?
C9X H9D 0.9900 . ?
C11X H11C 0.9900 . ?
C11X H11D 0.9900 . ?
N3 C17 1.501(5) . ?
N3 C15 1.505(5) . ?
N3 C13 1.508(5) . ?
N3 H3 0.95(5) . ?
C13 C14 1.529(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.524(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.500(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N4 C19 1.498(5) . ?
N4 C21 1.511(6) . ?
N4 C23 1.517(6) . ?
N4 H4 0.86(5) . ?
C19 C20 1.514(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.496(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.507(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N5 C29 1.498(5) . ?
N5 C27 1.502(5) . ?
N5 C25 1.506(5) . ?
N5 H5 0.93(5) . ?
C25 C26 1.498(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.514(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.517(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N6 C31 1.148(5) . ?
C31 C32 1.456(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N7 C33 1.147(7) . ?
C33 C34 1.448(8) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N8 C35 1.119(13) . ?
C35 C36 1.445(13) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N9 C37 1.133(6) . ?
C37 C38 1.436(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O9 105.70(12) . . ?
O1 V1 O6 103.85(13) . . ?
O9 V1 O6 79.20(10) . . ?
O1 V1 O10 105.63(13) . . ?
O9 V1 O10 148.63(10) . . ?
O6 V1 O10 91.92(10) . . ?
O1 V1 O23 103.02(13) . . ?
O9 V1 O23 89.33(10) . . ?
O6 V1 O23 152.76(10) . . ?
O10 V1 O23 85.13(10) . . ?
O1 V1 V5 111.44(11) . . ?
O9 V1 V5 39.71(7) . . ?
O6 V1 V5 39.58(7) . . ?
O10 V1 V5 123.78(7) . . ?
O23 V1 V5 123.67(8) . . ?
O2 V2 O7 107.14(12) . . ?
O2 V2 O6 106.42(11) . . ?
O7 V2 O6 78.96(10) . . ?
O2 V2 O14 105.49(12) . . ?
O7 V2 O14 89.65(10) . . ?
O6 V2 O14 148.01(10) . . ?
O2 V2 O11 108.35(13) . . ?
O7 V2 O11 144.45(10) . . ?
O6 V2 O11 89.15(10) . . ?
O14 V2 O11 82.96(10) . . ?
O2 V2 V5 111.82(10) . . ?
O7 V2 V5 39.64(7) . . ?
O6 V2 V5 39.32(7) . . ?
O14 V2 V5 123.27(7) . . ?
O11 V2 V5 121.13(7) . . ?
O3 V3 O7 108.26(12) . . ?
O3 V3 O8 107.22(12) . . ?
O7 V3 O8 78.47(9) . . ?
O3 V3 O15 105.76(12) . . ?
O7 V3 O15 89.04(10) . . ?
O8 V3 O15 146.93(10) . . ?
O3 V3 O18 107.51(12) . . ?
O7 V3 O18 144.20(10) . . ?
O8 V3 O18 89.57(10) . . ?
O15 V3 O18 82.87(10) . . ?
O3 V3 V5 114.41(10) . . ?
O7 V3 V5 39.11(7) . . ?
O8 V3 V5 39.40(7) . . ?
O15 V3 V5 121.15(7) . . ?
O18 V3 V5 120.54(7) . . ?
O4 V4 O8 107.71(12) . . ?
O4 V4 O9 106.16(12) . . ?
O8 V4 O9 78.96(10) . . ?
O4 V4 O19 106.12(13) . . ?
O8 V4 O19 89.13(10) . . ?
O9 V4 O19 147.63(11) . . ?
O4 V4 O22 105.52(12) . . ?
O8 V4 O22 146.62(10) . . ?
O9 V4 O22 89.06(10) . . ?
O19 V4 O22 84.58(10) . . ?
O4 V4 V5 111.78(10) . . ?
O8 V4 V5 39.69(7) . . ?
O9 V4 V5 39.27(7) . . ?
O19 V4 V5 122.90(7) . . ?
O22 V4 V5 122.10(7) . . ?
O5 V5 O6 109.21(12) . . ?
O5 V5 O9 109.24(12) . . ?
O6 V5 O9 84.01(10) . . ?
O5 V5 O7 110.32(12) . . ?
O6 V5 O7 83.49(10) . . ?
O9 V5 O7 140.44(10) . . ?
O5 V5 O8 110.31(12) . . ?
O6 V5 O8 140.48(10) . . ?
O9 V5 O8 83.34(10) . . ?
O7 V5 O8 82.88(10) . . ?
O5 V5 V1 118.60(10) . . ?
O6 V5 V1 42.08(7) . . ?
O9 V5 V1 42.03(7) . . ?
O7 V5 V1 114.71(7) . . ?
O8 V5 V1 114.59(7) . . ?
O5 V5 V2 116.80(10) . . ?
O6 V5 V2 41.80(7) . . ?
O9 V5 V2 116.68(7) . . ?
O7 V5 V2 41.69(7) . . ?
O8 V5 V2 115.78(7) . . ?
V1 V5 V2 77.58(2) . . ?
O5 V5 V4 116.50(10) . . ?
O6 V5 V4 116.88(8) . . ?
O9 V5 V4 41.77(7) . . ?
O7 V5 V4 115.87(7) . . ?
O8 V5 V4 41.57(7) . . ?
V1 V5 V4 77.65(2) . . ?
V2 V5 V4 126.70(3) . . ?
O5 V5 V3 118.94(10) . . ?
O6 V5 V3 115.03(7) . . ?
O9 V5 V3 115.09(7) . . ?
O7 V5 V3 41.33(7) . . ?
O8 V5 V3 41.59(7) . . ?
V1 V5 V3 122.46(3) . . ?
V2 V5 V3 77.33(2) . . ?
V4 V5 V3 77.58(2) . . ?
V5 O6 V1 98.34(10) . . ?
V5 O6 V2 98.88(10) . . ?
V1 O6 V2 135.85(13) . . ?
V5 O7 V2 98.67(10) . . ?
V5 O7 V3 99.56(11) . . ?
V2 O7 V3 137.11(13) . . ?
V5 O8 V4 98.74(10) . . ?
V5 O8 V3 99.01(10) . . ?
V4 O8 V3 137.69(13) . . ?
V5 O9 V1 98.25(10) . . ?
V5 O9 V4 98.96(10) . . ?
V1 O9 V4 136.30(13) . . ?
O13 S1 O12 113.10(18) . . ?
O13 S1 O11 108.94(16) . . ?
O12 S1 O11 108.57(15) . . ?
O13 S1 O10 108.52(17) . . ?
O12 S1 O10 108.88(16) . . ?
O11 S1 O10 108.75(14) . . ?
S1 O10 V1 132.36(16) . . ?
S1 O11 V2 136.45(15) . . ?
O17 S2 O16 113.33(16) . . ?
O17 S2 O15 108.25(15) . . ?
O16 S2 O15 109.65(16) . . ?
O17 S2 O14 108.47(14) . . ?
O16 S2 O14 110.18(15) . . ?
O15 S2 O14 106.72(13) . . ?
S2 O14 V2 131.19(14) . . ?
S2 O15 V3 130.50(15) . . ?
O20 S3 O21 113.11(18) . . ?
O20 S3 O19 111.31(17) . . ?
O21 S3 O19 106.21(15) . . ?
O20 S3 O18 110.46(16) . . ?
O21 S3 O18 107.55(15) . . ?
O19 S3 O18 107.93(14) . . ?
S3 O18 V3 130.55(15) . . ?
S3 O19 V4 134.06(16) . . ?
O25 S4 O24 111.40(15) . . ?
O25 S4 O23 108.50(15) . . ?
O24 S4 O23 110.60(16) . . ?
O25 S4 O22 108.20(15) . . ?
O24 S4 O22 109.94(15) . . ?
O23 S4 O22 108.10(14) . . ?
S4 O22 V4 128.07(15) . . ?
S4 O23 V1 128.74(16) . . ?
C1 N1 C3 115.0(3) . . ?
C1 N1 C5 111.5(4) . . ?
C3 N1 C5 111.7(3) . . ?
C1 N1 H1 103(3) . . ?
C3 N1 H1 111(3) . . ?
C5 N1 H1 104(3) . . ?
N1 C1 C2 112.8(4) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 113.1(4) . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 114.3(4) . . ?
C6 C5 H5A 108.7 . . ?
N1 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
N1 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9X N2 C7X 115.5(8) . . ?
C7 N2 C11 112.6(5) . . ?
C7 N2 C9 109.2(5) . . ?
C11 N2 C9 107.1(4) . . ?
C9X N2 C11X 117.2(8) . . ?
C7X N2 C11X 113.3(7) . . ?
C9X N2 H2 110(3) . . ?
C7X N2 H2 93(3) . . ?
C7 N2 H2 107(3) . . ?
C11 N2 H2 116(3) . . ?
C9 N2 H2 105(3) . . ?
C11X N2 H2 104(3) . . ?
N2 C7 C8 112.7(6) . . ?
N2 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7X C8 H8D 109.5 . . ?
C7X C8 H8E 109.5 . . ?
H8D C8 H8E 109.5 . . ?
C7X C8 H8F 109.5 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
C10 C9 N2 112.5(5) . . ?
C10 C9 H9A 109.1 . . ?
N2 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9X C10 H10D 109.5 . . ?
C9X C10 H10E 109.5 . . ?
H10D C10 H10E 109.5 . . ?
C9X C10 H10F 109.5 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
N2 C11 C12 113.1(5) . . ?
N2 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11X C12 H12D 109.5 . . ?
C11X C12 H12E 109.5 . . ?
H12D C12 H12E 109.5 . . ?
C11X C12 H12F 109.5 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
C8 C7X N2 121.1(9) . . ?
C8 C7X H7C 107.0 . . ?
N2 C7X H7C 107.0 . . ?
C8 C7X H7D 107.0 . . ?
N2 C7X H7D 107.0 . . ?
H7C C7X H7D 106.8 . . ?
N2 C9X C10 115.2(9) . . ?
N2 C9X H9C 108.5 . . ?
C10 C9X H9C 108.5 . . ?
N2 C9X H9D 108.5 . . ?
C10 C9X H9D 108.5 . . ?
H9C C9X H9D 107.5 . . ?
C12 C11X N2 114.3(9) . . ?
C12 C11X H11C 108.7 . . ?
N2 C11X H11C 108.7 . . ?
C12 C11X H11D 108.7 . . ?
N2 C11X H11D 108.7 . . ?
H11C C11X H11D 107.6 . . ?
C17 N3 C15 109.5(3) . . ?
C17 N3 C13 112.8(3) . . ?
C15 N3 C13 114.0(3) . . ?
C17 N3 H3 105(3) . . ?
C15 N3 H3 109(3) . . ?
C13 N3 H3 106(3) . . ?
N3 C13 C14 113.5(3) . . ?
N3 C13 H13A 108.9 . . ?
C14 C13 H13A 108.9 . . ?
N3 C13 H13B 108.9 . . ?
C14 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C16 112.7(4) . . ?
N3 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
N3 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N3 113.2(4) . . ?
C18 C17 H17A 108.9 . . ?
N3 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
N3 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 N4 C21 114.6(4) . . ?
C19 N4 C23 111.2(3) . . ?
C21 N4 C23 111.7(4) . . ?
C19 N4 H4 106(3) . . ?
C21 N4 H4 108(3) . . ?
C23 N4 H4 104(3) . . ?
N4 C19 C20 112.0(4) . . ?
N4 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N4 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N4 114.1(4) . . ?
C22 C21 H21A 108.7 . . ?
N4 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
N4 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N4 112.0(4) . . ?
C24 C23 H23A 109.2 . . ?
N4 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
N4 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C29 N5 C27 111.5(3) . . ?
C29 N5 C25 110.8(3) . . ?
C27 N5 C25 110.9(3) . . ?
C29 N5 H5 110(3) . . ?
C27 N5 H5 109(3) . . ?
C25 N5 H5 105(3) . . ?
C26 C25 N5 114.9(3) . . ?
C26 C25 H25A 108.5 . . ?
N5 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
N5 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 C28 112.4(4) . . ?
N5 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
N5 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 113.1(3) . . ?
N5 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
N5 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N6 C31 C32 178.0(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N7 C33 C34 178.9(6) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C36 179.1(10) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 178.7(7) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 V5 O6 V1 -111.75(13) . . . . ?
O9 V5 O6 V1 -3.43(10) . . . . ?
O7 V5 O6 V1 138.95(11) . . . . ?
O8 V5 O6 V1 68.48(17) . . . . ?
V2 V5 O6 V1 139.19(15) . . . . ?
V4 V5 O6 V1 23.20(11) . . . . ?
V3 V5 O6 V1 111.51(7) . . . . ?
O5 V5 O6 V2 109.06(13) . . . . ?
O9 V5 O6 V2 -142.62(11) . . . . ?
O7 V5 O6 V2 -0.23(10) . . . . ?
O8 V5 O6 V2 -70.71(17) . . . . ?
V1 V5 O6 V2 -139.19(15) . . . . ?
V4 V5 O6 V2 -115.99(8) . . . . ?
V3 V5 O6 V2 -27.68(11) . . . . ?
O5 V5 O7 V2 -107.88(13) . . . . ?
O6 V5 O7 V2 0.23(10) . . . . ?
O9 V5 O7 V2 72.60(17) . . . . ?
O8 V5 O7 V2 143.05(11) . . . . ?
V1 V5 O7 V2 29.21(11) . . . . ?
V4 V5 O7 V2 117.00(7) . . . . ?
V3 V5 O7 V2 141.00(15) . . . . ?
O5 V5 O7 V3 111.11(13) . . . . ?
O6 V5 O7 V3 -140.77(11) . . . . ?
O9 V5 O7 V3 -68.40(18) . . . . ?
O8 V5 O7 V3 2.04(10) . . . . ?
V1 V5 O7 V3 -111.79(8) . . . . ?
V2 V5 O7 V3 -141.00(15) . . . . ?
V4 V5 O7 V3 -24.00(11) . . . . ?
O5 V5 O8 V4 107.45(13) . . . . ?
O6 V5 O8 V4 -72.78(17) . . . . ?
O9 V5 O8 V4 -0.64(10) . . . . ?
O7 V5 O8 V4 -143.46(11) . . . . ?
V1 V5 O8 V4 -29.50(11) . . . . ?
V2 V5 O8 V4 -117.10(7) . . . . ?
V3 V5 O8 V4 -141.43(15) . . . . ?
O5 V5 O8 V3 -111.12(13) . . . . ?
O6 V5 O8 V3 68.65(17) . . . . ?
O9 V5 O8 V3 140.80(11) . . . . ?
O7 V5 O8 V3 -2.03(10) . . . . ?
V1 V5 O8 V3 111.94(8) . . . . ?
V2 V5 O8 V3 24.33(11) . . . . ?
V4 V5 O8 V3 141.43(15) . . . . ?
O5 V5 O9 V1 111.73(12) . . . . ?
O6 V5 O9 V1 3.44(10) . . . . ?
O7 V5 O9 V1 -68.76(17) . . . . ?
O8 V5 O9 V1 -139.04(11) . . . . ?
V2 V5 O9 V1 -23.49(11) . . . . ?
V4 V5 O9 V1 -139.68(15) . . . . ?
V3 V5 O9 V1 -111.44(8) . . . . ?
O5 V5 O9 V4 -108.59(13) . . . . ?
O6 V5 O9 V4 143.12(11) . . . . ?
O7 V5 O9 V4 70.92(17) . . . . ?
O8 V5 O9 V4 0.64(10) . . . . ?
V1 V5 O9 V4 139.68(15) . . . . ?
V2 V5 O9 V4 116.19(7) . . . . ?
V3 V5 O9 V4 28.24(11) . . . . ?
O13 S1 O10 V1 167.9(2) . . . . ?
O12 S1 O10 V1 -68.6(2) . . . . ?
O11 S1 O10 V1 49.5(2) . . . . ?
O13 S1 O11 V2 -168.4(2) . . . . ?
O12 S1 O11 V2 68.0(3) . . . . ?
O10 S1 O11 V2 -50.3(3) . . . . ?
O17 S2 O14 V2 175.43(19) . . . . ?
O16 S2 O14 V2 -60.0(2) . . . . ?
O15 S2 O14 V2 59.0(2) . . . . ?
O17 S2 O15 V3 179.15(18) . . . . ?
O16 S2 O15 V3 55.1(2) . . . . ?
O14 S2 O15 V3 -64.3(2) . . . . ?
O20 S3 O18 V3 -59.7(2) . . . . ?
O21 S3 O18 V3 176.46(18) . . . . ?
O19 S3 O18 V3 62.2(2) . . . . ?
O20 S3 O19 V4 70.9(3) . . . . ?
O21 S3 O19 V4 -165.6(2) . . . . ?
O18 S3 O19 V4 -50.5(3) . . . . ?
O25 S4 O22 V4 -176.14(17) . . . . ?
O24 S4 O22 V4 -54.3(2) . . . . ?
O23 S4 O22 V4 66.5(2) . . . . ?
O25 S4 O23 V1 -179.27(18) . . . . ?
O24 S4 O23 V1 58.3(2) . . . . ?
O22 S4 O23 V1 -62.1(2) . . . . ?
C3 N1 C1 C2 -52.8(5) . . . . ?
C5 N1 C1 C2 178.6(4) . . . . ?
C1 N1 C3 C4 -57.7(5) . . . . ?
C5 N1 C3 C4 70.8(5) . . . . ?
C1 N1 C5 C6 -55.4(5) . . . . ?
C3 N1 C5 C6 174.3(4) . . . . ?
C11 N2 C7 C8 -178.5(5) . . . . ?
C9 N2 C7 C8 62.7(7) . . . . ?
C7 N2 C9 C10 -178.9(5) . . . . ?
C11 N2 C9 C10 58.9(6) . . . . ?
C7 N2 C11 C12 53.6(6) . . . . ?
C9 N2 C11 C12 173.7(4) . . . . ?
C9X N2 C7X C8 -173.0(10) . . . . ?
C11X N2 C7X C8 -33.9(14) . . . . ?
C7X N2 C9X C10 -50.3(13) . . . . ?
C11X N2 C9X C10 172.3(9) . . . . ?
C9X N2 C11X C12 -33.5(13) . . . . ?
C7X N2 C11X C12 -171.8(8) . . . . ?
C17 N3 C13 C14 -64.7(5) . . . . ?
C15 N3 C13 C14 61.1(5) . . . . ?
C17 N3 C15 C16 -172.7(4) . . . . ?
C13 N3 C15 C16 59.9(5) . . . . ?
C15 N3 C17 C18 170.8(4) . . . . ?
C13 N3 C17 C18 -61.1(5) . . . . ?
C21 N4 C19 C20 -58.9(5) . . . . ?
C23 N4 C19 C20 173.1(4) . . . . ?
C19 N4 C21 C22 -60.7(6) . . . . ?
C23 N4 C21 C22 67.0(6) . . . . ?
C19 N4 C23 C24 -71.4(5) . . . . ?
C21 N4 C23 C24 159.1(4) . . . . ?
C29 N5 C25 C26 175.6(3) . . . . ?
C27 N5 C25 C26 -60.0(4) . . . . ?
C29 N5 C27 C28 -71.7(4) . . . . ?
C25 N5 C27 C28 164.4(3) . . . . ?
C27 N5 C29 C30 164.3(4) . . . . ?
C25 N5 C29 C30 -71.6(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O12 0.86(3) 1.87(3) 2.734(4) 174(5) .
N2 H2 O16 0.93(5) 1.87(5) 2.768(5) 162(5) .
N3 H3 O21 0.95(5) 1.88(5) 2.818(4) 171(4) .
N4 H4 O24 0.86(5) 1.93(5) 2.771(4) 166(5) .
N5 H5 O25 0.93(5) 1.92(5) 2.820(4) 165(4) .

_refine_diff_density_max         0.615
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.066

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1574243'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C82 H96 O28 S8 V2 4-), 2(C6 H16 N 1+), 2(C4 H12 N 1+)'
_chemical_formula_sum            'C102 H152 N4 O28 S8 V2'
_chemical_formula_weight         2240.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 '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 0.0082 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0139 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1451 0.1494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3281 0.6302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.459(2)
_cell_length_b                   14.920(3)
_cell_length_c                   16.674(3)
_cell_angle_alpha                95.233(3)
_cell_angle_beta                 111.125(3)
_cell_angle_gamma                112.613(3)
_cell_volume                     2778.6(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3977
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      29.43

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             1190
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.493
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'ALS Station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            82846
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.939
_diffrn_reflns_theta_max         33.673
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16757
_reflns_number_gt                11681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0074P)²+7.7856P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16757
_refine_ls_number_parameters     679
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1502
_refine_ls_wR_factor_gt          0.1276
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.93691(4) 0.88492(4) 0.48464(3) 0.01939(11) Uani 1 1 d . . . . .
O1 O 0.92439(19) 0.79911(16) 0.57246(14) 0.0231(4) Uani 1 1 d . . . . .
C1 C 0.8718(3) 0.7792(2) 0.62503(19) 0.0210(5) Uani 1 1 d . . . . .
C2 C 0.9050(3) 0.7286(2) 0.6907(2) 0.0220(6) Uani 1 1 d . . . . .
C3 C 0.8525(3) 0.7056(2) 0.7489(2) 0.0247(6) Uani 1 1 d . . . . .
H3 H 0.8799 0.6730 0.7921 0.030 Uiso 1 1 calc R U . . .
C4 C 0.7609(3) 0.7292(2) 0.7455(2) 0.0249(6) Uani 1 1 d . . . . .
C5 C 0.7251(3) 0.7778(2) 0.68119(19) 0.0229(6) Uani 1 1 d . . . . .
H5 H 0.6625 0.7948 0.6770 0.028 Uiso 1 1 calc R U . . .
C6 C 0.7776(3) 0.8025(2) 0.62297(19) 0.0208(5) Uani 1 1 d . . . . .
C7 C 0.7003(3) 0.7040(3) 0.8080(2) 0.0318(7) Uani 1 1 d . . . . .
C8 C 0.7553(4) 0.6553(3) 0.8763(3) 0.0470(10) Uani 1 1 d . . . . .
H8A H 0.7430 0.5902 0.8453 0.071 Uiso 1 1 calc R U . . .
H8B H 0.7173 0.6450 0.9172 0.071 Uiso 1 1 calc R U . . .
H8C H 0.8410 0.6994 0.9102 0.071 Uiso 1 1 calc R U . . .
C9 C 0.5685(4) 0.6285(3) 0.7510(3) 0.0483(10) Uani 1 1 d . . . . .
H9B H 0.5297 0.6593 0.7087 0.072 Uiso 1 1 calc R U . . .
H9C H 0.5282 0.6102 0.7899 0.072 Uiso 1 1 calc R U . . .
H9A H 0.5636 0.5679 0.7181 0.072 Uiso 1 1 calc R U . . .
C10 C 0.7086(5) 0.7996(3) 0.8583(3) 0.0510(11) Uani 1 1 d . . . . .
H10A H 0.6729 0.8315 0.8154 0.076 Uiso 1 1 calc R U . . .
H10B H 0.7925 0.8464 0.8961 0.076 Uiso 1 1 calc R U . . .
H10C H 0.6658 0.7820 0.8956 0.076 Uiso 1 1 calc R U . . .
O2 O 0.77168(17) 0.78285(15) 0.39525(14) 0.0220(4) Uani 1 1 d . . . . .
C11 C 0.6620(3) 0.7569(2) 0.3808(2) 0.0205(5) Uani 1 1 d . . . . .
C12 C 0.6235(3) 0.7856(2) 0.44433(19) 0.0203(5) Uani 1 1 d . . . . .
C13 C 0.5042(3) 0.7538(2) 0.4249(2) 0.0223(6) Uani 1 1 d . . . . .
H13 H 0.4840 0.7751 0.4697 0.027 Uiso 1 1 calc R U . . .
C14 C 0.4125(3) 0.6917(2) 0.3420(2) 0.0229(6) Uani 1 1 d . . . . .
C15 C 0.4471(3) 0.6627(2) 0.2790(2) 0.0228(6) Uani 1 1 d . . . . .
H15 H 0.3875 0.6206 0.2216 0.027 Uiso 1 1 calc R U . . .
C16 C 0.5665(3) 0.6933(2) 0.2972(2) 0.0212(6) Uani 1 1 d . . . . .
C17 C 0.2825(3) 0.6588(3) 0.3259(2) 0.0276(7) Uani 1 1 d . . . . .
C18 C 0.2627(3) 0.7529(3) 0.3417(3) 0.0443(10) Uani 1 1 d . . . . .
H18A H 0.1798 0.7319 0.3319 0.066 Uiso 1 1 calc R U . . .
H18B H 0.2796 0.7922 0.3002 0.066 Uiso 1 1 calc R U . . .
H18C H 0.3162 0.7943 0.4032 0.066 Uiso 1 1 calc R U . . .
C19 C 0.2572(3) 0.5986(3) 0.3918(3) 0.0437(10) Uani 1 1 d . . . . .
H19A H 0.2689 0.5383 0.3817 0.066 Uiso 1 1 calc R U . . .
H19B H 0.1748 0.5785 0.3829 0.066 Uiso 1 1 calc R U . . .
H19C H 0.3119 0.6404 0.4529 0.066 Uiso 1 1 calc R U . . .
C20 C 0.1943(3) 0.5937(3) 0.2315(2) 0.0376(8) Uani 1 1 d . . . . .
H20A H 0.2040 0.5325 0.2208 0.056 Uiso 1 1 calc R U . . .
H20B H 0.2095 0.6314 0.1886 0.056 Uiso 1 1 calc R U . . .
H20C H 0.1129 0.5752 0.2244 0.056 Uiso 1 1 calc R U . . .
O3 O 0.52325(19) 0.78602(16) 0.13287(14) 0.0236(4) Uani 1 1 d . . . . .
C21 C 0.6230(3) 0.7948(2) 0.13528(19) 0.0208(5) Uani 1 1 d . . . . .
C22 C 0.6794(3) 0.7371(2) 0.17825(19) 0.0208(5) Uani 1 1 d . . . . .
C23 C 0.7915(3) 0.7508(2) 0.1886(2) 0.0230(6) Uani 1 1 d . . . . .
H23 H 0.8252 0.7124 0.2208 0.028 Uiso 1 1 calc R U . . .
C24 C 0.8566(3) 0.8194(2) 0.1533(2) 0.0239(6) Uani 1 1 d . . . . .
C25 C 0.8027(3) 0.8738(2) 0.1072(2) 0.0237(6) Uani 1 1 d . . . . .
H25 H 0.8434 0.9200 0.0810 0.028 Uiso 1 1 calc R U . . .
C26 C 0.6912(3) 0.8627(2) 0.09810(19) 0.0206(5) Uani 1 1 d . . . . .
C27 C 0.9834(3) 0.8376(3) 0.1701(2) 0.0285(7) Uani 1 1 d . . . . .
C28 C 1.0646(3) 0.8856(4) 0.2693(3) 0.0504(11) Uani 1 1 d . . . . .
H28A H 1.0355 0.8406 0.3036 0.076 Uiso 1 1 calc R U . . .
H28B H 1.0648 0.9501 0.2872 0.076 Uiso 1 1 calc R U . . .
H28C H 1.1459 0.8971 0.2809 0.076 Uiso 1 1 calc R U . . .
C29 C 0.9831(3) 0.7370(3) 0.1416(3) 0.0409(9) Uani 1 1 d . . . . .
H29A H 0.9541 0.6918 0.1757 0.061 Uiso 1 1 calc R U . . .
H29B H 1.0643 0.7485 0.1529 0.061 Uiso 1 1 calc R U . . .
H29C H 0.9307 0.7063 0.0778 0.061 Uiso 1 1 calc R U . . .
C30 C 1.0319(4) 0.9065(4) 0.1165(4) 0.0556(12) Uani 1 1 d . . . . .
H30A H 0.9774 0.8777 0.0530 0.083 Uiso 1 1 calc R U . . .
H30B H 1.1107 0.9126 0.1259 0.083 Uiso 1 1 calc R U . . .
H30C H 1.0387 0.9733 0.1365 0.083 Uiso 1 1 calc R U . . .
O4 O 0.8808(2) 1.14347(17) 0.13787(15) 0.0284(5) Uani 1 1 d D . . . .
H4 H 0.845(3) 1.099(2) 0.0893(18) 0.043 Uiso 1 1 d D U . . .
C31 C 0.8068(3) 1.1275(2) 0.1784(2) 0.0221(6) Uani 1 1 d . . . . .
C32 C 0.6934(3) 1.0450(2) 0.14616(19) 0.0225(6) Uani 1 1 d . . . . .
C33 C 0.6230(3) 1.0339(2) 0.1922(2) 0.0257(6) Uani 1 1 d . . . . .
H33 H 0.5458 0.9785 0.1680 0.031 Uiso 1 1 calc R U . . .
C34 C 0.6634(3) 1.1022(2) 0.2730(2) 0.0268(6) Uani 1 1 d . . . . .
C35 C 0.7763(3) 1.1835(2) 0.3053(2) 0.0251(6) Uani 1 1 d . . . . .
H35 H 0.8063 1.2307 0.3606 0.030 Uiso 1 1 calc R U . . .
C36 C 0.8462(3) 1.1975(2) 0.2589(2) 0.0212(6) Uani 1 1 d . . . . .
C37 C 0.5895(4) 1.0874(3) 0.3266(3) 0.0400(9) Uani 1 1 d . . . . .
C38 C 0.6473(7) 1.0558(7) 0.4085(5) 0.118(3) Uani 1 1 d . . . . .
H38A H 0.7330 1.1010 0.4384 0.177 Uiso 1 1 calc R U . . .
H38B H 0.6346 0.9865 0.3901 0.177 Uiso 1 1 calc R U . . .
H38C H 0.6114 1.0595 0.4496 0.177 Uiso 1 1 calc R U . . .
C39 C 0.5915(5) 1.1879(4) 0.3601(5) 0.085(2) Uani 1 1 d . . . . .
H39A H 0.6727 1.2358 0.4030 0.128 Uiso 1 1 calc R U . . .
H39B H 0.5376 1.1766 0.3891 0.128 Uiso 1 1 calc R U . . .
H39C H 0.5653 1.2152 0.3095 0.128 Uiso 1 1 calc R U . . .
C40 C 0.4620(5) 1.0137(6) 0.2723(4) 0.115(3) Uani 1 1 d . . . . .
H40A H 0.4178 1.0094 0.3086 0.172 Uiso 1 1 calc R U . . .
H40B H 0.4565 0.9473 0.2527 0.172 Uiso 1 1 calc R U . . .
H40C H 0.4280 1.0360 0.2201 0.172 Uiso 1 1 calc R U . . .
S1 S 0.72746(6) 0.86968(5) 0.54957(5) 0.01993(14) Uani 1 1 d . . . . .
O5 O 0.82951(18) 0.93834(15) 0.53863(14) 0.0227(4) Uani 1 1 d . . . . .
O6 O 0.66613(19) 0.91172(17) 0.58376(15) 0.0259(5) Uani 1 1 d . . . . .
S2 S 0.59817(6) 0.64049(5) 0.21572(5) 0.02064(14) Uani 1 1 d . . . . .
O7 O 0.67462(19) 0.59552(15) 0.25869(14) 0.0241(4) Uani 1 1 d . . . . .
O8 O 0.48549(19) 0.57385(16) 0.14123(14) 0.0261(5) Uani 1 1 d . . . . .
S3 S 0.64344(7) 0.94727(5) 0.05109(5) 0.02275(15) Uani 1 1 d . . . . .
O9 O 0.5165(2) 0.90251(16) 0.00343(15) 0.0290(5) Uani 1 1 d . . . . .
O10 O 0.7127(2) 0.99099(16) 0.00227(15) 0.0277(5) Uani 1 1 d . . . . .
S4 S 0.98235(7) 1.30854(5) 0.29921(5) 0.02186(15) Uani 1 1 d . . . . .
O11 O 1.0040(2) 1.35965(16) 0.38634(14) 0.0255(5) Uani 1 1 d . . . . .
O12 O 0.9728(2) 1.36290(16) 0.23174(15) 0.0271(5) Uani 1 1 d . . . . .
O13 O 1.00506(19) 0.83553(16) 0.44847(15) 0.0258(5) Uani 1 1 d . . . . .
O14 O 0.93388(18) 0.99079(15) 0.42370(14) 0.0224(4) Uani 1 1 d . . . . .
C41 C 0.8603(4) 0.9816(3) 0.3360(3) 0.0439(10) Uani 1 1 d . . . . .
H41A H 0.8807 1.0486 0.3254 0.066 Uiso 1 1 calc R U . . .
H41B H 0.8720 0.9400 0.2946 0.066 Uiso 1 1 calc R U . . .
H41C H 0.7768 0.9498 0.3264 0.066 Uiso 1 1 calc R U . . .
C42 C 0.6721(3) 0.5462(3) 0.4591(3) 0.0375(8) Uani 1 1 d . . . . .
H42A H 0.6101 0.4828 0.4571 0.056 Uiso 1 1 calc R U . . .
H42B H 0.6352 0.5791 0.4180 0.056 Uiso 1 1 calc R U . . .
H42C H 0.7154 0.5906 0.5199 0.056 Uiso 1 1 calc R U . . .
C43 C 0.7582(3) 0.5247(2) 0.4316(2) 0.0330(7) Uani 1 1 d . . . . .
H43A H 0.7975 0.4936 0.4743 0.040 Uiso 1 1 calc R U . . .
H43B H 0.7136 0.4763 0.3718 0.040 Uiso 1 1 calc R U . . .
N1 N 0.8511(3) 0.6194(2) 0.42922(18) 0.0271(6) Uani 1 1 d D . . . .
H1A H 0.812(3) 0.647(3) 0.388(2) 0.033 Uiso 1 1 d D U . . .
H1B H 0.891(3) 0.661(3) 0.4866(18) 0.033 Uiso 1 1 d D U . . .
C44 C 0.9448(3) 0.6055(3) 0.4090(2) 0.0349(8) Uani 1 1 d . . . . .
H44A H 0.9842 0.5766 0.4541 0.042 Uiso 1 1 calc R U . . .
H44B H 1.0060 0.6721 0.4140 0.042 Uiso 1 1 calc R U . . .
C45 C 0.8956(4) 0.5375(3) 0.3173(3) 0.0443(9) Uani 1 1 d . . . . .
H45A H 0.8392 0.4699 0.3134 0.066 Uiso 1 1 calc R U . . .
H45B H 0.9611 0.5339 0.3067 0.066 Uiso 1 1 calc R U . . .
H45C H 0.8545 0.5647 0.2724 0.066 Uiso 1 1 calc R U . . .
N2 N 0.3154(2) 0.6841(2) -0.00827(19) 0.0313(6) Uani 1 1 d D . . . .
H2 H 0.389(3) 0.712(3) 0.039(2) 0.038 Uiso 1 1 d D U . . .
C46 C 0.1205(4) 0.5304(3) -0.0533(3) 0.0489(10) Uani 1 1 d . . . . .
H46A H 0.0812 0.4735 -0.0325 0.073 Uiso 1 1 calc R U . . .
H46B H 0.1168 0.5051 -0.1111 0.073 Uiso 1 1 calc R U . . .
H46C H 0.0798 0.5733 -0.0596 0.073 Uiso 1 1 calc R U . . .
C47 C 0.2489(3) 0.5909(3) 0.0134(3) 0.0361(8) Uani 1 1 d . . . . .
H47A H 0.2517 0.6101 0.0729 0.043 Uiso 1 1 calc R U . . .
H47B H 0.2900 0.5477 0.0171 0.043 Uiso 1 1 calc R U . . .
C48 C 0.2618(3) 0.7555(3) -0.0139(2) 0.0337(7) Uani 1 1 d . . . . .
H48A H 0.1819 0.7238 -0.0650 0.040 Uiso 1 1 calc R U . . .
H48B H 0.3121 0.8169 -0.0253 0.040 Uiso 1 1 calc R U . . .
C49 C 0.2501(4) 0.7852(3) 0.0700(3) 0.0443(9) Uani 1 1 d . . . . .
H49A H 0.1840 0.7290 0.0729 0.066 Uiso 1 1 calc R U . . .
H49B H 0.2343 0.8441 0.0695 0.066 Uiso 1 1 calc R U . . .
H49C H 0.3243 0.8017 0.1222 0.066 Uiso 1 1 calc R U . . .
C50 C 0.3317(4) 0.6620(3) -0.0905(3) 0.0483(11) Uani 1 1 d . . . . .
H50A H 0.3767 0.7263 -0.1010 0.058 Uiso 1 1 calc R U . . .
H50B H 0.2524 0.6264 -0.1421 0.058 Uiso 1 1 calc R U . . .
C51 C 0.3974(5) 0.5981(5) -0.0848(4) 0.080(2) Uani 1 1 d . . . . .
H51A H 0.3487 0.5311 -0.0817 0.121 Uiso 1 1 calc R U . . .
H51B H 0.4734 0.6303 -0.0312 0.121 Uiso 1 1 calc R U . . .
H51C H 0.4126 0.5916 -0.1377 0.121 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O13 1.608(2) . ?
V1 O14 1.960(2) . ?
V1 O14 1.971(2) 2_776 ?
V1 O2 2.020(2) . ?
V1 O1 2.041(2) . ?
V1 O5 2.287(2) . ?
V1 V1 3.0833(11) 2_776 ?
O1 C1 1.300(3) . ?
C1 C2 1.424(4) . ?
C1 C6 1.428(4) . ?
C2 C3 1.387(4) . ?
C2 S4 1.765(3) 2_776 ?
C3 C4 1.391(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(4) . ?
C4 C7 1.529(4) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 S1 1.763(3) . ?
C7 C8 1.526(5) . ?
C7 C10 1.530(5) . ?
C7 C9 1.541(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9A 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O2 C11 1.294(3) . ?
C11 C16 1.422(4) . ?
C11 C12 1.435(4) . ?
C12 C13 1.386(4) . ?
C12 S1 1.758(3) . ?
C13 C14 1.396(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(4) . ?
C14 C17 1.534(4) . ?
C15 C16 1.392(4) . ?
C15 H15 0.9500 . ?
C16 S2 1.769(3) . ?
C17 C20 1.523(5) . ?
C17 C19 1.531(5) . ?
C17 C18 1.542(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O3 C21 1.283(4) . ?
C21 C22 1.433(4) . ?
C21 C26 1.436(4) . ?
C22 C23 1.384(4) . ?
C22 S2 1.763(3) . ?
C23 C24 1.398(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(4) . ?
C24 C27 1.534(4) . ?
C25 C26 1.395(4) . ?
C25 H25 0.9500 . ?
C26 S3 1.749(3) . ?
C27 C28 1.524(5) . ?
C27 C29 1.530(5) . ?
C27 C30 1.534(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O4 C31 1.355(4) . ?
O4 H4 0.836(18) . ?
C31 C32 1.406(4) . ?
C31 C36 1.407(4) . ?
C32 C33 1.392(4) . ?
C32 S3 1.774(3) . ?
C33 C34 1.395(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.394(4) . ?
C34 C37 1.531(5) . ?
C35 C36 1.390(4) . ?
C35 H35 0.9500 . ?
C36 S4 1.769(3) . ?
C37 C40 1.489(6) . ?
C37 C38 1.526(8) . ?
C37 C39 1.538(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
S1 O6 1.439(2) . ?
S1 O5 1.450(2) . ?
S2 O8 1.445(2) . ?
S2 O7 1.452(2) . ?
S3 O9 1.430(2) . ?
S3 O10 1.461(2) . ?
S4 O12 1.443(2) . ?
S4 O11 1.449(2) . ?
S4 C2 1.764(3) 2_776 ?
O14 C41 1.397(4) . ?
O14 V1 1.971(2) 2_776 ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.516(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N1 1.499(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
N1 C44 1.497(5) . ?
N1 H1A 0.94(2) . ?
N1 H1B 0.93(2) . ?
C44 C45 1.508(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
N2 C48 1.491(5) . ?
N2 C50 1.492(5) . ?
N2 C47 1.495(5) . ?
N2 H2 0.91(2) . ?
C46 C47 1.508(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.511(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.518(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 V1 O14 104.92(11) . . ?
O13 V1 O14 104.19(10) . 2_776 ?
O14 V1 O14 76.70(10) . 2_776 ?
O13 V1 O2 95.06(10) . . ?
O14 V1 O2 93.42(9) . . ?
O14 V1 O2 160.03(9) 2_776 . ?
O13 V1 O1 93.21(10) . . ?
O14 V1 O1 161.37(9) . . ?
O14 V1 O1 94.95(9) 2_776 . ?
O2 V1 O1 89.15(9) . . ?
O13 V1 O5 173.68(10) . . ?
O14 V1 O5 80.73(9) . . ?
O14 V1 O5 79.69(8) 2_776 . ?
O2 V1 O5 81.63(8) . . ?
O1 V1 O5 81.40(8) . . ?
O13 V1 V1 108.69(8) . 2_776 ?
O14 V1 V1 38.48(6) . 2_776 ?
O14 V1 V1 38.22(6) 2_776 2_776 ?
O2 V1 V1 129.71(7) . 2_776 ?
O1 V1 V1 131.12(7) . 2_776 ?
O5 V1 V1 77.48(6) . 2_776 ?
C1 O1 V1 138.4(2) . . ?
O1 C1 C2 120.7(3) . . ?
O1 C1 C6 125.4(3) . . ?
C2 C1 C6 113.9(3) . . ?
C3 C2 C1 123.3(3) . . ?
C3 C2 S4 116.8(2) . 2_776 ?
C1 C2 S4 120.0(2) . 2_776 ?
C2 C3 C4 121.7(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 116.6(3) . . ?
C3 C4 C7 123.0(3) . . ?
C5 C4 C7 120.4(3) . . ?
C6 C5 C4 122.4(3) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C1 122.0(3) . . ?
C5 C6 S1 116.8(2) . . ?
C1 C6 S1 121.1(2) . . ?
C8 C7 C4 112.7(3) . . ?
C8 C7 C10 108.4(3) . . ?
C4 C7 C10 110.2(3) . . ?
C8 C7 C9 107.7(3) . . ?
C4 C7 C9 108.1(3) . . ?
C10 C7 C9 109.7(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 O2 V1 138.75(19) . . ?
O2 C11 C16 121.0(3) . . ?
O2 C11 C12 125.3(3) . . ?
C16 C11 C12 113.6(3) . . ?
C13 C12 C11 122.4(3) . . ?
C13 C12 S1 116.6(2) . . ?
C11 C12 S1 120.9(2) . . ?
C12 C13 C14 122.6(3) . . ?
C12 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C15 C14 C13 116.3(3) . . ?
C15 C14 C17 124.3(3) . . ?
C13 C14 C17 119.4(3) . . ?
C14 C15 C16 122.1(3) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C11 123.0(3) . . ?
C15 C16 S2 117.6(2) . . ?
C11 C16 S2 119.1(2) . . ?
C20 C17 C19 108.6(3) . . ?
C20 C17 C14 112.5(3) . . ?
C19 C17 C14 108.9(3) . . ?
C20 C17 C18 108.3(3) . . ?
C19 C17 C18 109.1(3) . . ?
C14 C17 C18 109.4(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 C22 122.1(3) . . ?
O3 C21 C26 125.2(3) . . ?
C22 C21 C26 112.7(3) . . ?
C23 C22 C21 123.5(3) . . ?
C23 C22 S2 118.7(2) . . ?
C21 C22 S2 117.7(2) . . ?
C22 C23 C24 122.0(3) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
C25 C24 C23 116.4(3) . . ?
C25 C24 C27 122.4(3) . . ?
C23 C24 C27 121.1(3) . . ?
C24 C25 C26 122.3(3) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C25 C26 C21 122.9(3) . . ?
C25 C26 S3 117.1(2) . . ?
C21 C26 S3 119.5(2) . . ?
C28 C27 C29 109.7(3) . . ?
C28 C27 C30 109.3(3) . . ?
C29 C27 C30 107.6(3) . . ?
C28 C27 C24 108.8(3) . . ?
C29 C27 C24 109.5(3) . . ?
C30 C27 C24 111.9(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 O4 H4 108(3) . . ?
O4 C31 C32 124.6(3) . . ?
O4 C31 C36 118.0(3) . . ?
C32 C31 C36 117.4(3) . . ?
C33 C32 C31 121.0(3) . . ?
C33 C32 S3 118.7(2) . . ?
C31 C32 S3 120.0(2) . . ?
C32 C33 C34 121.5(3) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C35 C34 C33 117.4(3) . . ?
C35 C34 C37 120.7(3) . . ?
C33 C34 C37 121.8(3) . . ?
C36 C35 C34 121.8(3) . . ?
C36 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
C35 C36 C31 120.8(3) . . ?
C35 C36 S4 119.0(2) . . ?
C31 C36 S4 120.1(2) . . ?
C40 C37 C38 111.6(6) . . ?
C40 C37 C34 112.6(3) . . ?
C38 C37 C34 108.5(4) . . ?
C40 C37 C39 106.9(5) . . ?
C38 C37 C39 107.3(5) . . ?
C34 C37 C39 109.8(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O6 S1 O5 118.03(13) . . ?
O6 S1 C12 107.52(14) . . ?
O5 S1 C12 107.18(13) . . ?
O6 S1 C6 107.49(14) . . ?
O5 S1 C6 107.11(13) . . ?
C12 S1 C6 109.31(14) . . ?
S1 O5 V1 122.80(12) . . ?
O8 S2 O7 116.60(13) . . ?
O8 S2 C22 108.34(14) . . ?
O7 S2 C22 107.32(14) . . ?
O8 S2 C16 107.38(14) . . ?
O7 S2 C16 107.61(14) . . ?
C22 S2 C16 109.46(14) . . ?
O9 S3 O10 117.07(14) . . ?
O9 S3 C26 111.57(14) . . ?
O10 S3 C26 107.91(14) . . ?
O9 S3 C32 110.31(15) . . ?
O10 S3 C32 106.25(14) . . ?
C26 S3 C32 102.64(14) . . ?
O12 S4 O11 117.04(13) . . ?
O12 S4 C2 107.83(14) . 2_776 ?
O11 S4 C2 109.88(14) . 2_776 ?
O12 S4 C36 107.22(14) . . ?
O11 S4 C36 107.13(14) . . ?
C2 S4 C36 107.33(14) 2_776 . ?
C41 O14 V1 129.0(2) . . ?
C41 O14 V1 127.7(2) . 2_776 ?
V1 O14 V1 103.30(9) . 2_776 ?
O14 C41 H41A 109.5 . . ?
O14 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O14 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C43 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 C42 111.1(3) . . ?
N1 C43 H43A 109.4 . . ?
C42 C43 H43A 109.4 . . ?
N1 C43 H43B 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C44 N1 C43 114.3(3) . . ?
C44 N1 H1A 112(2) . . ?
C43 N1 H1A 108(2) . . ?
C44 N1 H1B 106(2) . . ?
C43 N1 H1B 106(2) . . ?
H1A N1 H1B 111(3) . . ?
N1 C44 C45 113.0(3) . . ?
N1 C44 H44A 109.0 . . ?
C45 C44 H44A 109.0 . . ?
N1 C44 H44B 109.0 . . ?
C45 C44 H44B 109.0 . . ?
H44A C44 H44B 107.8 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 N2 C50 110.6(3) . . ?
C48 N2 C47 113.1(3) . . ?
C50 N2 C47 112.7(3) . . ?
C48 N2 H2 110(3) . . ?
C50 N2 H2 108(3) . . ?
C47 N2 H2 102(3) . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N2 C47 C46 114.0(3) . . ?
N2 C47 H47A 108.7 . . ?
C46 C47 H47A 108.7 . . ?
N2 C47 H47B 108.7 . . ?
C46 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
N2 C48 C49 112.6(3) . . ?
N2 C48 H48A 109.1 . . ?
C49 C48 H48A 109.1 . . ?
N2 C48 H48B 109.1 . . ?
C49 C48 H48B 109.1 . . ?
H48A C48 H48B 107.8 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N2 C50 C51 113.0(4) . . ?
N2 C50 H50A 109.0 . . ?
C51 C50 H50A 109.0 . . ?
N2 C50 H50B 109.0 . . ?
C51 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

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
V1 O1 C1 C2 -167.3(2) . . . . ?
V1 O1 C1 C6 13.9(5) . . . . ?
O1 C1 C2 C3 179.7(3) . . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
O1 C1 C2 S4 -0.5(4) . . . 2_776 ?
C6 C1 C2 S4 178.5(2) . . . 2_776 ?
C1 C2 C3 C4 1.3(5) . . . . ?
S4 C2 C3 C4 -178.5(2) 2_776 . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C2 C3 C4 C7 179.4(3) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C7 C4 C5 C6 179.9(3) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C4 C5 C6 S1 -176.7(2) . . . . ?
O1 C1 C6 C5 179.5(3) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
O1 C1 C6 S1 -3.7(4) . . . . ?
C2 C1 C6 S1 177.3(2) . . . . ?
C3 C4 C7 C8 2.7(5) . . . . ?
C5 C4 C7 C8 -177.4(3) . . . . ?
C3 C4 C7 C10 123.9(4) . . . . ?
C5 C4 C7 C10 -56.3(4) . . . . ?
C3 C4 C7 C9 -116.2(4) . . . . ?
C5 C4 C7 C9 63.6(4) . . . . ?
V1 O2 C11 C16 165.8(2) . . . . ?
V1 O2 C11 C12 -15.5(5) . . . . ?
O2 C11 C12 C13 -179.0(3) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
O2 C11 C12 S1 4.7(4) . . . . ?
C16 C11 C12 S1 -176.4(2) . . . . ?
C11 C12 C13 C14 -0.2(5) . . . . ?
S1 C12 C13 C14 176.2(2) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C12 C13 C14 C17 179.3(3) . . . . ?
C13 C14 C15 C16 0.2(4) . . . . ?
C17 C14 C15 C16 -178.9(3) . . . . ?
C14 C15 C16 C11 -0.5(5) . . . . ?
C14 C15 C16 S2 173.5(2) . . . . ?
O2 C11 C16 C15 179.4(3) . . . . ?
C12 C11 C16 C15 0.5(4) . . . . ?
O2 C11 C16 S2 5.5(4) . . . . ?
C12 C11 C16 S2 -173.4(2) . . . . ?
C15 C14 C17 C20 -2.3(4) . . . . ?
C13 C14 C17 C20 178.6(3) . . . . ?
C15 C14 C17 C19 118.1(4) . . . . ?
C13 C14 C17 C19 -61.0(4) . . . . ?
C15 C14 C17 C18 -122.7(4) . . . . ?
C13 C14 C17 C18 58.2(4) . . . . ?
O3 C21 C22 C23 -174.3(3) . . . . ?
C26 C21 C22 C23 4.6(4) . . . . ?
O3 C21 C22 S2 8.2(4) . . . . ?
C26 C21 C22 S2 -172.9(2) . . . . ?
C21 C22 C23 C24 -3.5(5) . . . . ?
S2 C22 C23 C24 174.0(2) . . . . ?
C22 C23 C24 C25 0.2(4) . . . . ?
C22 C23 C24 C27 176.6(3) . . . . ?
C23 C24 C25 C26 1.5(4) . . . . ?
C27 C24 C25 C26 -174.8(3) . . . . ?
C24 C25 C26 C21 0.0(5) . . . . ?
C24 C25 C26 S3 172.0(2) . . . . ?
O3 C21 C26 C25 176.0(3) . . . . ?
C22 C21 C26 C25 -2.9(4) . . . . ?
O3 C21 C26 S3 4.2(4) . . . . ?
C22 C21 C26 S3 -174.6(2) . . . . ?
C25 C24 C27 C28 110.5(4) . . . . ?
C23 C24 C27 C28 -65.6(4) . . . . ?
C25 C24 C27 C29 -129.6(3) . . . . ?
C23 C24 C27 C29 54.3(4) . . . . ?
C25 C24 C27 C30 -10.3(5) . . . . ?
C23 C24 C27 C30 173.6(3) . . . . ?
O4 C31 C32 C33 179.6(3) . . . . ?
C36 C31 C32 C33 0.4(4) . . . . ?
O4 C31 C32 S3 5.4(4) . . . . ?
C36 C31 C32 S3 -173.9(2) . . . . ?
C31 C32 C33 C34 -1.8(5) . . . . ?
S3 C32 C33 C34 172.5(3) . . . . ?
C32 C33 C34 C35 1.2(5) . . . . ?
C32 C33 C34 C37 -176.5(3) . . . . ?
C33 C34 C35 C36 0.9(5) . . . . ?
C37 C34 C35 C36 178.6(3) . . . . ?
C34 C35 C36 C31 -2.3(5) . . . . ?
C34 C35 C36 S4 174.3(3) . . . . ?
O4 C31 C36 C35 -177.7(3) . . . . ?
C32 C31 C36 C35 1.6(4) . . . . ?
O4 C31 C36 S4 5.8(4) . . . . ?
C32 C31 C36 S4 -174.9(2) . . . . ?
C35 C34 C37 C40 165.4(5) . . . . ?
C33 C34 C37 C40 -17.0(6) . . . . ?
C35 C34 C37 C38 -70.5(5) . . . . ?
C33 C34 C37 C38 107.1(5) . . . . ?
C35 C34 C37 C39 46.5(5) . . . . ?
C33 C34 C37 C39 -135.9(4) . . . . ?
C13 C12 S1 O6 -17.2(3) . . . . ?
C11 C12 S1 O6 159.3(2) . . . . ?
C13 C12 S1 O5 -145.0(2) . . . . ?
C11 C12 S1 O5 31.5(3) . . . . ?
C13 C12 S1 C6 99.2(3) . . . . ?
C11 C12 S1 C6 -84.3(3) . . . . ?
C5 C6 S1 O6 17.1(3) . . . . ?
C1 C6 S1 O6 -159.9(2) . . . . ?
C5 C6 S1 O5 144.9(2) . . . . ?
C1 C6 S1 O5 -32.1(3) . . . . ?
C5 C6 S1 C12 -99.3(2) . . . . ?
C1 C6 S1 C12 83.7(3) . . . . ?
O6 S1 O5 V1 -179.69(13) . . . . ?
C12 S1 O5 V1 -58.24(17) . . . . ?
C6 S1 O5 V1 58.97(17) . . . . ?
C23 C22 S2 O8 -122.7(2) . . . . ?
C21 C22 S2 O8 54.9(3) . . . . ?
C23 C22 S2 O7 4.0(3) . . . . ?
C21 C22 S2 O7 -178.4(2) . . . . ?
C23 C22 S2 C16 120.5(2) . . . . ?
C21 C22 S2 C16 -61.9(3) . . . . ?
C15 C16 S2 O8 1.4(3) . . . . ?
C11 C16 S2 O8 175.7(2) . . . . ?
C15 C16 S2 O7 -124.8(2) . . . . ?
C11 C16 S2 O7 49.4(3) . . . . ?
C15 C16 S2 C22 118.9(2) . . . . ?
C11 C16 S2 C22 -66.9(3) . . . . ?
C25 C26 S3 O9 149.6(2) . . . . ?
C21 C26 S3 O9 -38.2(3) . . . . ?
C25 C26 S3 O10 19.6(3) . . . . ?
C21 C26 S3 O10 -168.1(2) . . . . ?
C25 C26 S3 C32 -92.3(3) . . . . ?
C21 C26 S3 C32 79.9(3) . . . . ?
C33 C32 S3 O9 35.3(3) . . . . ?
C31 C32 S3 O9 -150.2(2) . . . . ?
C33 C32 S3 O10 163.2(2) . . . . ?
C31 C32 S3 O10 -22.4(3) . . . . ?
C33 C32 S3 C26 -83.6(3) . . . . ?
C31 C32 S3 C26 90.8(3) . . . . ?
C35 C36 S4 O12 -117.5(3) . . . . ?
C31 C36 S4 O12 59.1(3) . . . . ?
C35 C36 S4 O11 8.9(3) . . . . ?
C31 C36 S4 O11 -174.5(2) . . . . ?
C35 C36 S4 C2 126.9(3) . . . 2_776 ?
C31 C36 S4 C2 -56.5(3) . . . 2_776 ?
C42 C43 N1 C44 175.8(3) . . . . ?
C43 N1 C44 C45 63.6(4) . . . . ?
C48 N2 C47 C46 59.4(4) . . . . ?
C50 N2 C47 C46 -67.0(4) . . . . ?
C50 N2 C48 C49 -176.6(3) . . . . ?
C47 N2 C48 C49 55.9(4) . . . . ?
C48 N2 C50 C51 174.2(4) . . . . ?
C47 N2 C50 C51 -58.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O10 0.836(18) 1.84(3) 2.612(3) 153(4) .
N2 H2 O3 0.91(2) 1.74(3) 2.647(3) 169(4) .
N1 H1A O7 0.94(2) 2.09(3) 2.855(4) 137(3) .
N1 H1A O2 0.94(2) 2.29(3) 3.038(4) 136(3) .
N1 H1B O1 0.93(2) 2.18(3) 2.994(3) 146(3) .
N1 H1B O11 0.93(2) 2.21(3) 2.897(4) 130(3) 2_776

_refine_diff_density_max         0.816
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.093

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
####################################################################### 
# 
# 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_5_4MeCN
_database_code_depnum_ccdc_archive 'CCDC 1574244'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H109 O10 V 2-, 2(C6 H16 N 1+), 4(C2 H3 N)'
_chemical_formula_sum            'C108 H153 N6 O10 V'
_chemical_formula_weight         1746.29

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   16.7286(7)
_cell_length_b                   18.2453(8)
_cell_length_c                   18.7113(13)
_cell_angle_alpha                101.228(7)
_cell_angle_beta                 105.150(7)
_cell_angle_gamma                105.573(7)
_cell_volume                     5090.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    36379
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.1

_exptl_crystal_description       tablet
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             1892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.156
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'confocal mirrors'
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            55764
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             17887
_reflns_number_gt                10295
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_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     
'w=1/[σ²(Fo²)+(0.1082P)²+4.1350P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         17887
_refine_ls_number_parameters     1222
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2372
_refine_ls_wR_factor_gt          0.2060
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.64050(5) 0.57830(5) 0.39539(4) 0.0363(2) Uani 1 1 d . . . . .
O9 O 0.5903(2) 0.59933(18) 0.31907(17) 0.0449(8) Uani 1 1 d . . . . .
O10 O 0.56984(18) 0.54037(17) 0.43543(16) 0.0361(7) Uani 1 1 d . . . . .
O1 O 0.69435(19) 0.50921(19) 0.36601(16) 0.0405(8) Uani 1 1 d . . . . .
O2 O 0.72958(19) 0.66530(18) 0.46003(17) 0.0430(8) Uani 1 1 d . . . . .
O3 O 0.6154(2) 0.76054(17) 0.42262(18) 0.0416(8) Uani 1 1 d D . . . .
H3 H 0.590(3) 0.763(3) 0.3795(15) 0.043(14) Uiso 1 1 d D . . . .
O4 O 0.4990(2) 0.76497(17) 0.29469(17) 0.0339(7) Uani 1 1 d . . . . .
H4 H 0.452(3) 0.740(3) 0.257(3) 0.052(15) Uiso 1 1 d . . . . .
O5 O 0.35767(18) 0.67408(17) 0.17985(16) 0.0312(7) Uani 1 1 d . . . . .
H5 H 0.346(4) 0.625(4) 0.144(3) 0.076(18) Uiso 1 1 d . . . . .
O6 O 0.32631(17) 0.53992(16) 0.09855(15) 0.0301(7) Uani 1 1 d . . . . .
O7 O 0.40269(18) 0.43806(16) 0.10991(15) 0.0308(7) Uani 1 1 d . . . . .
H7 H 0.378(4) 0.479(4) 0.103(3) 0.09(2) Uiso 1 1 d . . . . .
O8 O 0.5195(2) 0.41014(17) 0.22422(16) 0.0337(7) Uani 1 1 d D . . . .
H8 H 0.490(3) 0.420(3) 0.186(2) 0.062(17) Uiso 1 1 d D . . . .
C1 C 0.7314(3) 0.4695(3) 0.4131(2) 0.0357(11) Uani 1 1 d . . . . .
C2 C 0.6853(3) 0.3901(3) 0.4014(2) 0.0354(11) Uani 1 1 d . . . . .
C3 C 0.7264(3) 0.3475(3) 0.4441(2) 0.0377(11) Uani 1 1 d . . . . .
H3A H 0.695788 0.293074 0.436411 0.045 Uiso 1 1 calc R U . . .
C4 C 0.8117(3) 0.3831(3) 0.4981(2) 0.0387(11) Uani 1 1 d . . . . .
C5 C 0.8531(3) 0.4628(3) 0.5104(3) 0.0446(12) Uani 1 1 d . . . . .
H5A H 0.909767 0.488099 0.548481 0.054 Uiso 1 1 calc R U . . .
C6 C 0.8151(3) 0.5082(3) 0.4692(2) 0.0407(11) Uani 1 1 d . . . . .
C7 C 0.8547(3) 0.3311(3) 0.5390(3) 0.0459(12) Uani 1 1 d . . . . .
C8 C 0.7996(3) 0.2956(3) 0.5864(3) 0.0445(12) Uani 1 1 d . . . . .
H8A H 0.740407 0.262107 0.551679 0.067 Uiso 1 1 calc R U . . .
H8B H 0.795562 0.338613 0.624311 0.067 Uiso 1 1 calc R U . . .
H8C H 0.827878 0.263457 0.613375 0.067 Uiso 1 1 calc R U . . .
C9 C 0.8598(4) 0.2647(4) 0.4785(3) 0.0674(17) Uani 1 1 d . . . . .
H9A H 0.887901 0.287581 0.444259 0.101 Uiso 1 1 calc R U . . .
H9B H 0.800326 0.228045 0.448051 0.101 Uiso 1 1 calc R U . . .
H9C H 0.894505 0.235966 0.504236 0.101 Uiso 1 1 calc R U . . .
C10 C 0.9477(3) 0.3799(4) 0.5952(3) 0.0573(15) Uani 1 1 d . . . . .
H10A H 0.974070 0.345111 0.619325 0.086 Uiso 1 1 calc R U . . .
H10B H 0.944570 0.421542 0.635178 0.086 Uiso 1 1 calc R U . . .
H10C H 0.983899 0.404325 0.566836 0.086 Uiso 1 1 calc R U . . .
C11 C 0.8642(3) 0.5955(3) 0.4866(3) 0.0506(13) Uani 1 1 d . . . . .
H11A H 0.846608 0.611963 0.439177 0.061 Uiso 1 1 calc R U . . .
H11B H 0.927957 0.603994 0.500802 0.061 Uiso 1 1 calc R U . . .
C12 C 0.7814(3) 0.6802(3) 0.5353(3) 0.0391(11) Uani 1 1 d . . . . .
C13 C 0.8484(3) 0.6479(3) 0.5509(3) 0.0416(11) Uani 1 1 d . . . . .
C14 C 0.9036(3) 0.6676(3) 0.6271(3) 0.0509(14) Uani 1 1 d . . . . .
H14 H 0.949461 0.645895 0.638147 0.061 Uiso 1 1 calc R U . . .
C15 C 0.8932(3) 0.7183(3) 0.6873(3) 0.0481(13) Uani 1 1 d . . . . .
C16 C 0.8259(3) 0.7490(3) 0.6686(3) 0.0445(12) Uani 1 1 d . . . . .
H16 H 0.818759 0.784792 0.708761 0.053 Uiso 1 1 calc R U . . .
C17 C 0.7686(3) 0.7300(3) 0.5942(3) 0.0400(11) Uani 1 1 d . . . . .
C18 C 0.9562(3) 0.7430(3) 0.7701(3) 0.0552(13) Uani 1 1 d D U . . .
C19 C 0.9014(6) 0.7122(7) 0.8167(4) 0.088(4) Uani 0.688(9) 1 d D U P A 1
H19A H 0.873086 0.654531 0.795130 0.133 Uiso 0.688(9) 1 calc R U P A 1
H19B H 0.939118 0.724532 0.870316 0.133 Uiso 0.688(9) 1 calc R U P A 1
H19C H 0.856313 0.737299 0.815039 0.133 Uiso 0.688(9) 1 calc R U P A 1
C20 C 1.0252(6) 0.6990(5) 0.7757(5) 0.075(3) Uani 0.688(9) 1 d D U P A 1
H20A H 0.994602 0.641497 0.759720 0.112 Uiso 0.688(9) 1 calc R U P A 1
H20B H 1.059283 0.712383 0.741861 0.112 Uiso 0.688(9) 1 calc R U P A 1
H20C H 1.065003 0.715473 0.829175 0.112 Uiso 0.688(9) 1 calc R U P A 1
C21 C 1.0037(6) 0.8287(4) 0.7943(4) 0.059(3) Uani 0.688(9) 1 d D U P A 1
H21A H 1.036957 0.841675 0.759766 0.088 Uiso 0.688(9) 1 calc R U P A 1
H21B H 0.961546 0.857233 0.792061 0.088 Uiso 0.688(9) 1 calc R U P A 1
H21C H 1.044351 0.844465 0.847338 0.088 Uiso 0.688(9) 1 calc R U P A 1
C19X C 0.9254(12) 0.7944(10) 0.8306(9) 0.063(5) Uiso 0.312(9) 1 d D U P A 2
H19D H 0.916856 0.840162 0.813748 0.094 Uiso 0.312(9) 1 calc R U P A 2
H19E H 0.869956 0.761425 0.833249 0.094 Uiso 0.312(9) 1 calc R U P A 2
H19F H 0.970584 0.812975 0.881767 0.094 Uiso 0.312(9) 1 calc R U P A 2
C20X C 0.9668(11) 0.6772(8) 0.8006(9) 0.045(4) Uiso 0.312(9) 1 d D U P A 2
H20D H 1.008021 0.698144 0.853646 0.067 Uiso 0.312(9) 1 calc R U P A 2
H20E H 0.909680 0.644315 0.800202 0.067 Uiso 0.312(9) 1 calc R U P A 2
H20F H 0.989804 0.645042 0.768405 0.067 Uiso 0.312(9) 1 calc R U P A 2
C21X C 1.0429(10) 0.8040(10) 0.7747(11) 0.057(5) Uiso 0.312(9) 1 d D U P A 2
H21D H 1.029957 0.846020 0.753117 0.086 Uiso 0.312(9) 1 calc R U P A 2
H21E H 1.080948 0.827347 0.828788 0.086 Uiso 0.312(9) 1 calc R U P A 2
H21F H 1.072820 0.777554 0.745164 0.086 Uiso 0.312(9) 1 calc R U P A 2
C22 C 0.6985(3) 0.7673(3) 0.5761(3) 0.0404(11) Uani 1 1 d . . . . .
H22A H 0.687187 0.787910 0.624137 0.048 Uiso 1 1 calc R U . . .
H22B H 0.643221 0.726315 0.539553 0.048 Uiso 1 1 calc R U . . .
C23 C 0.6835(3) 0.8292(3) 0.4648(2) 0.0338(10) Uani 1 1 d . . . . .
C24 C 0.7250(3) 0.8344(3) 0.5412(2) 0.0352(10) Uani 1 1 d . . . . .
C25 C 0.7926(3) 0.9047(3) 0.5879(3) 0.0377(11) Uani 1 1 d . . . . .
H25 H 0.820380 0.908655 0.640443 0.045 Uiso 1 1 calc R U . . .
C26 C 0.8202(3) 0.9685(2) 0.5605(2) 0.0336(10) Uani 1 1 d . . . . .
C27 C 0.7781(3) 0.9611(2) 0.4839(2) 0.0328(10) Uani 1 1 d . . . . .
H27 H 0.797005 1.004107 0.463758 0.039 Uiso 1 1 calc R U . . .
C28 C 0.7089(3) 0.8929(2) 0.4348(2) 0.0315(10) Uani 1 1 d . . . . .
C29 C 0.8891(3) 1.0468(3) 0.6138(3) 0.0456(12) Uani 1 1 d . . . . .
C30 C 0.9455(3) 1.0373(3) 0.6879(3) 0.0556(14) Uani 1 1 d . . . . .
H30A H 0.908156 1.019165 0.717939 0.083 Uiso 1 1 calc R U . . .
H30B H 0.990869 1.088494 0.718551 0.083 Uiso 1 1 calc R U . . .
H30C H 0.973499 0.998251 0.674700 0.083 Uiso 1 1 calc R U . . .
C31 C 0.9512(4) 1.0833(4) 0.5740(3) 0.095(2) Uani 1 1 d . . . . .
H31A H 0.983198 1.047632 0.561100 0.142 Uiso 1 1 calc R U . . .
H31B H 0.993189 1.134478 0.608636 0.142 Uiso 1 1 calc R U . . .
H31C H 0.917345 1.091217 0.526611 0.142 Uiso 1 1 calc R U . . .
C32 C 0.8406(4) 1.1025(3) 0.6373(3) 0.0698(18) Uani 1 1 d . . . . .
H32A H 0.804826 1.110928 0.591104 0.105 Uiso 1 1 calc R U . . .
H32B H 0.883472 1.153556 0.671548 0.105 Uiso 1 1 calc R U . . .
H32C H 0.802397 1.078771 0.664482 0.105 Uiso 1 1 calc R U . . .
C33 C 0.6616(3) 0.8905(3) 0.3532(2) 0.0339(10) Uani 1 1 d . . . . .
H33A H 0.651517 0.838535 0.317629 0.041 Uiso 1 1 calc R U . . .
H33B H 0.699003 0.932359 0.337834 0.041 Uiso 1 1 calc R U . . .
C34 C 0.4953(3) 0.8398(2) 0.3193(2) 0.0299(10) Uani 1 1 d . . . . .
C35 C 0.5735(3) 0.9030(3) 0.3460(2) 0.0315(10) Uani 1 1 d . . . . .
C36 C 0.5722(3) 0.9796(2) 0.3708(2) 0.0320(10) Uani 1 1 d . . . . .
H36 H 0.625679 1.023062 0.388299 0.038 Uiso 1 1 calc R U . . .
C37 C 0.4953(3) 0.9942(2) 0.3707(2) 0.0319(10) Uani 1 1 d . . . . .
C38 C 0.4183(3) 0.9287(3) 0.3467(2) 0.0346(10) Uani 1 1 d . . . . .
H38 H 0.365004 0.937292 0.347872 0.042 Uiso 1 1 calc R U . . .
C39 C 0.4169(3) 0.8516(2) 0.3213(2) 0.0310(10) Uani 1 1 d . . . . .
C40 C 0.4922(3) 1.0783(3) 0.3963(2) 0.0411(11) Uani 1 1 d . . . . .
C41 C 0.5848(4) 1.1398(3) 0.4312(4) 0.0751(19) Uani 1 1 d . . . . .
H41A H 0.617940 1.128002 0.476520 0.113 Uiso 1 1 calc R U . . .
H41B H 0.580940 1.192848 0.446823 0.113 Uiso 1 1 calc R U . . .
H41C H 0.614863 1.137853 0.392805 0.113 Uiso 1 1 calc R U . . .
C42 C 0.4456(3) 1.0842(3) 0.4555(3) 0.0490(13) Uani 1 1 d . . . . .
H42A H 0.384509 1.048199 0.432243 0.074 Uiso 1 1 calc R U . . .
H42B H 0.446382 1.138836 0.472384 0.074 Uiso 1 1 calc R U . . .
H42C H 0.475619 1.069497 0.499985 0.074 Uiso 1 1 calc R U . . .
C43 C 0.4431(5) 1.0984(3) 0.3251(3) 0.0715(19) Uani 1 1 d . . . . .
H43A H 0.473434 1.094838 0.286992 0.107 Uiso 1 1 calc R U . . .
H43B H 0.441743 1.152451 0.340667 0.107 Uiso 1 1 calc R U . . .
H43C H 0.382771 1.060799 0.302381 0.107 Uiso 1 1 calc R U . . .
C44 C 0.3303(3) 0.7834(2) 0.2927(2) 0.0311(10) Uani 1 1 d . . . . .
H44A H 0.340997 0.735191 0.303269 0.037 Uiso 1 1 calc R U . . .
H44B H 0.291099 0.796779 0.320712 0.037 Uiso 1 1 calc R U . . .
C45 C 0.3039(3) 0.7149(2) 0.1534(2) 0.0276(9) Uani 1 1 d . . . . .
C46 C 0.2863(2) 0.7673(2) 0.2072(2) 0.0266(9) Uani 1 1 d . . . . .
C47 C 0.2325(3) 0.8096(2) 0.1816(2) 0.0311(10) Uani 1 1 d . . . . .
H47 H 0.219462 0.843866 0.218669 0.037 Uiso 1 1 calc R U . . .
C48 C 0.1973(3) 0.8040(2) 0.1045(2) 0.0329(10) Uani 1 1 d . . . . .
C49 C 0.2164(3) 0.7516(2) 0.0519(2) 0.0312(10) Uani 1 1 d . . . . .
H49 H 0.192997 0.746476 -0.001546 0.037 Uiso 1 1 calc R U . . .
C50 C 0.2684(3) 0.7064(2) 0.0744(2) 0.0282(9) Uani 1 1 d . . . . .
C51 C 0.1393(3) 0.8527(3) 0.0770(3) 0.0374(11) Uani 1 1 d . . . . .
C52 C 0.1356(5) 0.9122(4) 0.1422(3) 0.084(2) Uani 1 1 d . . . . .
H52A H 0.193578 0.953467 0.167649 0.126 Uiso 1 1 calc R U . . .
H52B H 0.118801 0.885773 0.179485 0.126 Uiso 1 1 calc R U . . .
H52C H 0.092101 0.936441 0.122184 0.126 Uiso 1 1 calc R U . . .
C53 C 0.1705(5) 0.8927(4) 0.0217(4) 0.084(2) Uani 1 1 d . . . . .
H53A H 0.132524 0.922735 0.004045 0.127 Uiso 1 1 calc R U . . .
H53B H 0.168079 0.852528 -0.022767 0.127 Uiso 1 1 calc R U . . .
H53C H 0.231134 0.928907 0.047689 0.127 Uiso 1 1 calc R U . . .
C54 C 0.0451(3) 0.7962(3) 0.0332(4) 0.0703(18) Uani 1 1 d . . . . .
H54A H 0.021210 0.771475 0.068626 0.105 Uiso 1 1 calc R U . . .
H54B H 0.045082 0.755006 -0.009070 0.105 Uiso 1 1 calc R U . . .
H54C H 0.008609 0.826062 0.012107 0.105 Uiso 1 1 calc R U . . .
C55 C 0.2854(3) 0.6488(2) 0.0149(2) 0.0284(9) Uani 1 1 d . . . . .
H55A H 0.277057 0.665345 -0.033165 0.034 Uiso 1 1 calc R U . . .
H55B H 0.347201 0.650977 0.034365 0.034 Uiso 1 1 calc R U . . .
C56 C 0.2480(3) 0.5141(2) 0.0398(2) 0.0280(9) Uani 1 1 d . . . . .
C57 C 0.2254(3) 0.5650(2) -0.0033(2) 0.0267(9) Uani 1 1 d . . . . .
C58 C 0.1445(3) 0.5366(2) -0.0630(2) 0.0273(9) Uani 1 1 d . . . . .
H58 H 0.129649 0.570911 -0.092379 0.033 Uiso 1 1 calc R U . . .
C59 C 0.0854(3) 0.4610(2) -0.0813(2) 0.0274(9) Uani 1 1 d . . . . .
C60 C 0.1104(3) 0.4120(2) -0.0368(2) 0.0276(9) Uani 1 1 d . . . . .
H60 H 0.071380 0.359450 -0.048050 0.033 Uiso 1 1 calc R U . . .
C61 C 0.1899(3) 0.4374(2) 0.0227(2) 0.0259(9) Uani 1 1 d . . . . .
C62 C -0.0053(3) 0.4295(2) -0.1441(2) 0.0317(10) Uani 1 1 d . . . . .
C63 C -0.0133(3) 0.3535(3) -0.2024(3) 0.0458(12) Uani 1 1 d . . . . .
H63A H -0.005626 0.313536 -0.175590 0.069 Uiso 1 1 calc R U . . .
H63B H 0.032051 0.365627 -0.226671 0.069 Uiso 1 1 calc R U . . .
H63C H -0.071611 0.332994 -0.242189 0.069 Uiso 1 1 calc R U . . .
C64 C -0.0767(3) 0.4115(3) -0.1069(3) 0.0408(11) Uani 1 1 d . . . . .
H64A H -0.069355 0.372010 -0.079327 0.061 Uiso 1 1 calc R U . . .
H64B H -0.134660 0.390639 -0.147121 0.061 Uiso 1 1 calc R U . . .
H64C H -0.071821 0.460324 -0.070520 0.061 Uiso 1 1 calc R U . . .
C65 C -0.0202(3) 0.4902(3) -0.1872(2) 0.0387(11) Uani 1 1 d . . . . .
H65A H -0.079183 0.468500 -0.226009 0.058 Uiso 1 1 calc R U . . .
H65B H 0.023895 0.502143 -0.212798 0.058 Uiso 1 1 calc R U . . .
H65C H -0.015019 0.539000 -0.150503 0.058 Uiso 1 1 calc R U . . .
C66 C 0.2120(3) 0.3817(2) 0.0693(2) 0.0291(9) Uani 1 1 d . . . . .
H66A H 0.246553 0.413535 0.123399 0.035 Uiso 1 1 calc R U . . .
H66B H 0.156460 0.345136 0.069612 0.035 Uiso 1 1 calc R U . . .
C67 C 0.3542(3) 0.3631(2) 0.0617(2) 0.0268(9) Uani 1 1 d . . . . .
C68 C 0.2632(3) 0.3327(2) 0.0404(2) 0.0281(9) Uani 1 1 d . . . . .
C69 C 0.2194(3) 0.2554(2) -0.0072(2) 0.0300(9) Uani 1 1 d . . . . .
H69 H 0.157226 0.234820 -0.021147 0.036 Uiso 1 1 calc R U . . .
C70 C 0.2626(3) 0.2066(2) -0.0355(2) 0.0323(10) Uani 1 1 d . . . . .
C71 C 0.3536(3) 0.2391(2) -0.0122(2) 0.0309(10) Uani 1 1 d . . . . .
H71 H 0.385230 0.207590 -0.030048 0.037 Uiso 1 1 calc R U . . .
C72 C 0.4006(3) 0.3155(2) 0.0359(2) 0.0289(9) Uani 1 1 d . . . . .
C73 C 0.2136(3) 0.1218(3) -0.0885(3) 0.0415(11) Uani 1 1 d . . . . .
C74 C 0.2205(5) 0.1191(4) -0.1690(3) 0.098(2) Uani 1 1 d . . . . .
H74A H 0.186637 0.149575 -0.192690 0.147 Uiso 1 1 calc R U . . .
H74B H 0.196924 0.063883 -0.201256 0.147 Uiso 1 1 calc R U . . .
H74C H 0.282305 0.142145 -0.164483 0.147 Uiso 1 1 calc R U . . .
C75 C 0.1190(4) 0.0927(4) -0.0958(5) 0.104(3) Uani 1 1 d . . . . .
H75A H 0.113715 0.091366 -0.045110 0.156 Uiso 1 1 calc R U . . .
H75B H 0.090656 0.039136 -0.131788 0.156 Uiso 1 1 calc R U . . .
H75C H 0.090162 0.128407 -0.115421 0.156 Uiso 1 1 calc R U . . .
C76 C 0.2573(4) 0.0652(3) -0.0612(4) 0.087(2) Uani 1 1 d . . . . .
H76A H 0.318693 0.082572 -0.059513 0.130 Uiso 1 1 calc R U . . .
H76B H 0.226241 0.011722 -0.096815 0.130 Uiso 1 1 calc R U . . .
H76C H 0.255414 0.064592 -0.009370 0.130 Uiso 1 1 calc R U . . .
C77 C 0.5002(3) 0.3464(3) 0.0611(2) 0.0311(10) Uani 1 1 d . . . . .
H77A H 0.521070 0.405141 0.077830 0.037 Uiso 1 1 calc R U . . .
H77B H 0.518898 0.329502 0.016423 0.037 Uiso 1 1 calc R U . . .
C78 C 0.5493(3) 0.3494(2) 0.2037(2) 0.0300(9) Uani 1 1 d . . . . .
C79 C 0.5431(3) 0.3168(2) 0.1270(2) 0.0307(10) Uani 1 1 d . . . . .
C80 C 0.5741(3) 0.2544(3) 0.1108(2) 0.0351(10) Uani 1 1 d . . . . .
H80 H 0.569811 0.232510 0.058950 0.042 Uiso 1 1 calc R U . . .
C81 C 0.6113(3) 0.2228(3) 0.1675(3) 0.0410(11) Uani 1 1 d . . . . .
C82 C 0.6165(3) 0.2568(3) 0.2425(2) 0.0417(12) Uani 1 1 d . . . . .
H82 H 0.641540 0.236410 0.282477 0.050 Uiso 1 1 calc R U . . .
C83 C 0.5862(3) 0.3198(3) 0.2612(2) 0.0350(10) Uani 1 1 d . . . . .
C84 C 0.6431(3) 0.1526(3) 0.1473(3) 0.0524(13) Uani 1 1 d D U . . .
C85 C 0.5616(6) 0.0828(4) 0.0867(5) 0.077(3) Uani 0.711(10) 1 d D U P B 1
H85A H 0.515986 0.067418 0.110044 0.115 Uiso 0.711(10) 1 calc R U P B 1
H85B H 0.538281 0.100176 0.041661 0.115 Uiso 0.711(10) 1 calc R U P B 1
H85C H 0.579731 0.037240 0.070375 0.115 Uiso 0.711(10) 1 calc R U P B 1
C86 C 0.6729(9) 0.1230(7) 0.2158(5) 0.095(4) Uani 0.711(10) 1 d D U P B 1
H86A H 0.625146 0.109069 0.237172 0.143 Uiso 0.711(10) 1 calc R U P B 1
H86B H 0.688686 0.075999 0.199501 0.143 Uiso 0.711(10) 1 calc R U P B 1
H86C H 0.724217 0.164674 0.255237 0.143 Uiso 0.711(10) 1 calc R U P B 1
C87 C 0.7120(6) 0.1753(5) 0.1108(6) 0.074(3) Uani 0.711(10) 1 d D U P B 1
H87A H 0.688925 0.194035 0.066726 0.111 Uiso 0.711(10) 1 calc R U P B 1
H87B H 0.763964 0.217751 0.148745 0.111 Uiso 0.711(10) 1 calc R U P B 1
H87C H 0.728433 0.129076 0.093010 0.111 Uiso 0.711(10) 1 calc R U P B 1
C85X C 0.6239(13) 0.1182(11) 0.0594(7) 0.053(5) Uani 0.289(10) 1 d D U P B 2
H85D H 0.642329 0.161640 0.037225 0.079 Uiso 0.289(10) 1 calc R U P B 2
H85E H 0.656491 0.081704 0.051627 0.079 Uiso 0.289(10) 1 calc R U P B 2
H85F H 0.560700 0.089495 0.033962 0.079 Uiso 0.289(10) 1 calc R U P B 2
C86X C 0.616(2) 0.0885(13) 0.1826(15) 0.099(9) Uani 0.289(10) 1 d D U P B 2
H86D H 0.639083 0.046341 0.166585 0.149 Uiso 0.289(10) 1 calc R U P B 2
H86E H 0.639240 0.109794 0.238980 0.149 Uiso 0.289(10) 1 calc R U P B 2
H86F H 0.551608 0.066736 0.165595 0.149 Uiso 0.289(10) 1 calc R U P B 2
C87X C 0.7478(9) 0.1861(11) 0.1775(12) 0.063(5) Uani 0.289(10) 1 d D U P B 2
H87D H 0.768130 0.228939 0.155144 0.095 Uiso 0.289(10) 1 calc R U P B 2
H87E H 0.769439 0.206681 0.233954 0.095 Uiso 0.289(10) 1 calc R U P B 2
H87F H 0.770265 0.143359 0.161980 0.095 Uiso 0.289(10) 1 calc R U P B 2
C88 C 0.5924(3) 0.3508(3) 0.3449(2) 0.0358(10) Uani 1 1 d . . . . .
H88A H 0.560904 0.389472 0.347732 0.043 Uiso 1 1 calc R U . . .
H88B H 0.561790 0.305846 0.361177 0.043 Uiso 1 1 calc R U . . .
N1 N 0.6773(3) 0.6400(2) 0.2212(2) 0.0458(10) Uani 1 1 d D . . . .
H1 H 0.649(3) 0.629(3) 0.259(2) 0.055 Uiso 1 1 d D U . . .
C89 C 0.7730(3) 0.6808(4) 0.2635(3) 0.0679(17) Uani 1 1 d . . . . .
H89A H 0.802532 0.695936 0.226533 0.082 Uiso 1 1 calc R U . . .
H89B H 0.797692 0.643066 0.285135 0.082 Uiso 1 1 calc R U . . .
C90 C 0.7934(4) 0.7535(3) 0.3279(3) 0.0649(16) Uani 1 1 d . . . . .
H90A H 0.781590 0.795780 0.306196 0.097 Uiso 1 1 calc R U . . .
H90B H 0.855493 0.771141 0.359756 0.097 Uiso 1 1 calc R U . . .
H90C H 0.756397 0.741153 0.359787 0.097 Uiso 1 1 calc R U . . .
C91 C 0.6562(4) 0.5574(3) 0.1771(3) 0.0620(15) Uani 1 1 d . . . . .
H91A H 0.681320 0.529043 0.212193 0.074 Uiso 1 1 calc R U . . .
H91B H 0.591527 0.531284 0.157230 0.074 Uiso 1 1 calc R U . . .
C92 C 0.6894(4) 0.5503(4) 0.1128(4) 0.0700(17) Uani 1 1 d . . . . .
H92A H 0.657814 0.570549 0.073652 0.105 Uiso 1 1 calc R U . . .
H92B H 0.680514 0.494333 0.090061 0.105 Uiso 1 1 calc R U . . .
H92C H 0.752346 0.581062 0.131087 0.105 Uiso 1 1 calc R U . . .
C93 C 0.6362(3) 0.6876(3) 0.1763(3) 0.0476(12) Uani 1 1 d . . . . .
H93A H 0.661802 0.694475 0.134985 0.057 Uiso 1 1 calc R U . . .
H93B H 0.649243 0.740904 0.211005 0.057 Uiso 1 1 calc R U . . .
C94 C 0.5383(3) 0.6473(4) 0.1411(3) 0.0592(15) Uani 1 1 d . . . . .
H94A H 0.525239 0.600234 0.098655 0.089 Uiso 1 1 calc R U . . .
H94B H 0.511455 0.684081 0.121295 0.089 Uiso 1 1 calc R U . . .
H94C H 0.514413 0.631451 0.180462 0.089 Uiso 1 1 calc R U . . .
N2 N 0.3926(2) 0.51808(19) 0.37070(18) 0.0276(8) Uani 1 1 d D . . . .
H2 H 0.4522(14) 0.525(2) 0.385(2) 0.033 Uiso 1 1 d D U . . .
C95 C 0.3828(3) 0.5699(3) 0.4384(2) 0.0354(10) Uani 1 1 d . . . . .
H95A H 0.404976 0.553685 0.485144 0.042 Uiso 1 1 calc R U . . .
H95B H 0.319688 0.562188 0.428969 0.042 Uiso 1 1 calc R U . . .
C96 C 0.4328(3) 0.6573(3) 0.4524(3) 0.0397(11) Uani 1 1 d . . . . .
H96A H 0.492568 0.663648 0.451491 0.060 Uiso 1 1 calc R U . . .
H96B H 0.435720 0.687689 0.502928 0.060 Uiso 1 1 calc R U . . .
H96C H 0.402356 0.676748 0.411939 0.060 Uiso 1 1 calc R U . . .
C97 C 0.3465(3) 0.4327(2) 0.3633(2) 0.0341(10) Uani 1 1 d . . . . .
H97A H 0.283432 0.424271 0.355190 0.041 Uiso 1 1 calc R U . . .
H97B H 0.371466 0.421110 0.412189 0.041 Uiso 1 1 calc R U . . .
C98 C 0.3545(3) 0.3755(3) 0.2976(2) 0.0377(11) Uani 1 1 d . . . . .
H98A H 0.317297 0.377287 0.248370 0.057 Uiso 1 1 calc R U . . .
H98B H 0.335457 0.321630 0.302651 0.057 Uiso 1 1 calc R U . . .
H98C H 0.415885 0.390495 0.299254 0.057 Uiso 1 1 calc R U . . .
C99 C 0.3671(3) 0.5409(3) 0.2970(2) 0.0326(10) Uani 1 1 d . . . . .
H99A H 0.378436 0.505826 0.256204 0.039 Uiso 1 1 calc R U . . .
H99B H 0.404629 0.596037 0.305269 0.039 Uiso 1 1 calc R U . . .
C100 C 0.2712(3) 0.5352(3) 0.2694(2) 0.0406(11) Uani 1 1 d . . . . .
H10D H 0.233522 0.481010 0.262125 0.061 Uiso 1 1 calc R U . . .
H10E H 0.257790 0.548347 0.220260 0.061 Uiso 1 1 calc R U . . .
H10F H 0.260312 0.572466 0.307963 0.061 Uiso 1 1 calc R U . . .
N3 N 0.9145(5) 0.3988(6) 0.3455(5) 0.147(3) Uani 1 1 d . . . . .
C101 C 0.8600(5) 0.4126(4) 0.3015(4) 0.084(2) Uani 1 1 d . . . . .
C102 C 0.7974(5) 0.4313(6) 0.2511(4) 0.108(3) Uani 1 1 d . . . . .
H10G H 0.743733 0.420602 0.265083 0.161 Uiso 1 1 calc R U . . .
H10H H 0.783971 0.398961 0.198294 0.161 Uiso 1 1 calc R U . . .
H10I H 0.819937 0.487639 0.254096 0.161 Uiso 1 1 calc R U . . .
N4 N 1.1406(4) 0.9320(4) 0.6506(3) 0.0867(17) Uani 1 1 d . . . . .
C103 C 1.0693(4) 0.8938(4) 0.6165(3) 0.0599(15) Uani 1 1 d . . . . .
C104 C 0.9786(4) 0.8435(3) 0.5716(3) 0.0636(15) Uani 1 1 d . . . . .
H10J H 0.978487 0.798603 0.533041 0.095 Uiso 1 1 calc R U . . .
H10K H 0.947631 0.874530 0.545530 0.095 Uiso 1 1 calc R U . . .
H10L H 0.948928 0.823657 0.606242 0.095 Uiso 1 1 calc R U . . .
N5 N 0.2306(5) 0.1230(4) 0.2038(4) 0.124(3) Uani 1 1 d . . . . .
C105 C 0.2880(5) 0.1529(4) 0.1850(4) 0.0764(18) Uani 1 1 d . . . . .
C106 C 0.3585(4) 0.1902(4) 0.1645(3) 0.0711(17) Uani 1 1 d . . . . .
H10M H 0.341255 0.223052 0.131795 0.107 Uiso 1 1 calc R U . . .
H10N H 0.376670 0.150251 0.136103 0.107 Uiso 1 1 calc R U . . .
H10O H 0.407593 0.223906 0.211243 0.107 Uiso 1 1 calc R U . . .
N6 N 0.5143(4) 0.8258(4) 0.1066(4) 0.100(2) Uani 1 1 d . . . . .
C107 C 0.4792(4) 0.8655(3) 0.1281(3) 0.0538(14) Uani 1 1 d . . . . .
C108 C 0.4341(3) 0.9156(3) 0.1550(3) 0.0457(12) Uani 1 1 d . . . . .
H10P H 0.428789 0.952048 0.123315 0.069 Uiso 1 1 calc R U . . .
H10Q H 0.467260 0.946115 0.208982 0.069 Uiso 1 1 calc R U . . .
H10R H 0.375261 0.882839 0.151168 0.069 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O9 1.628(3) . ?
V1 O10 1.632(3) . ?
V1 O2 1.801(3) . ?
V1 O1 1.817(3) . ?
O1 C1 1.375(5) . ?
O2 C12 1.377(5) . ?
O3 C23 1.368(5) . ?
O3 H3 0.823(19) . ?
O4 C34 1.377(5) . ?
O4 H4 0.84(5) . ?
O5 C45 1.370(4) . ?
O5 H5 0.95(6) . ?
O6 C56 1.364(4) . ?
O7 C67 1.373(5) . ?
O7 H7 0.96(6) . ?
O8 C78 1.363(5) . ?
O8 H8 0.835(19) . ?
C1 C2 1.389(6) . ?
C1 C6 1.404(6) . ?
C2 C3 1.398(6) . ?
C2 C88 1.515(6) . ?
C3 C4 1.404(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.376(7) . ?
C4 C7 1.539(6) . ?
C5 C6 1.400(6) . ?
C5 H5A 0.9500 . ?
C6 C11 1.508(7) . ?
C7 C9 1.526(7) . ?
C7 C10 1.534(7) . ?
C7 C8 1.545(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.511(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.387(7) . ?
C12 C13 1.393(6) . ?
C13 C14 1.396(6) . ?
C14 C15 1.391(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(7) . ?
C15 C18 1.527(7) . ?
C16 C17 1.384(6) . ?
C16 H16 0.9500 . ?
C17 C22 1.505(6) . ?
C18 C20X 1.457(13) . ?
C18 C21 1.467(8) . ?
C18 C19 1.499(9) . ?
C18 C21X 1.543(12) . ?
C18 C20 1.567(9) . ?
C18 C19X 1.606(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19X H19D 0.9800 . ?
C19X H19E 0.9800 . ?
C19X H19F 0.9800 . ?
C20X H20D 0.9800 . ?
C20X H20E 0.9800 . ?
C20X H20F 0.9800 . ?
C21X H21D 0.9800 . ?
C21X H21E 0.9800 . ?
C21X H21F 0.9800 . ?
C22 C24 1.515(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.388(6) . ?
C23 C28 1.399(6) . ?
C24 C25 1.399(6) . ?
C25 C26 1.379(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(6) . ?
C26 C29 1.524(6) . ?
C27 C28 1.399(6) . ?
C27 H27 0.9500 . ?
C28 C33 1.511(6) . ?
C29 C31 1.516(8) . ?
C29 C30 1.530(7) . ?
C29 C32 1.531(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.527(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.385(6) . ?
C34 C39 1.392(6) . ?
C35 C36 1.391(6) . ?
C36 C37 1.381(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.397(6) . ?
C37 C40 1.535(6) . ?
C38 C39 1.387(6) . ?
C38 H38 0.9500 . ?
C39 C44 1.517(6) . ?
C40 C42 1.515(6) . ?
C40 C41 1.528(7) . ?
C40 C43 1.537(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C46 1.507(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.395(5) . ?
C45 C50 1.401(5) . ?
C46 C47 1.388(5) . ?
C47 C48 1.381(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.395(6) . ?
C48 C51 1.542(6) . ?
C49 C50 1.393(5) . ?
C49 H49 0.9500 . ?
C50 C55 1.515(5) . ?
C51 C52 1.493(7) . ?
C51 C53 1.497(7) . ?
C51 C54 1.530(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C57 1.503(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C61 1.391(5) . ?
C56 C57 1.406(5) . ?
C57 C58 1.398(5) . ?
C58 C59 1.379(5) . ?
C58 H58 0.9500 . ?
C59 C60 1.407(5) . ?
C59 C62 1.532(5) . ?
C60 C61 1.385(5) . ?
C60 H60 0.9500 . ?
C61 C66 1.520(5) . ?
C62 C64 1.527(6) . ?
C62 C65 1.528(6) . ?
C62 C63 1.537(6) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C68 1.513(5) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.388(6) . ?
C67 C72 1.408(5) . ?
C68 C69 1.390(5) . ?
C69 C70 1.400(6) . ?
C69 H69 0.9500 . ?
C70 C71 1.389(6) . ?
C70 C73 1.532(6) . ?
C71 C72 1.387(6) . ?
C71 H71 0.9500 . ?
C72 C77 1.515(6) . ?
C73 C75 1.488(8) . ?
C73 C76 1.509(7) . ?
C73 C74 1.532(8) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 C79 1.528(6) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 C83 1.374(6) . ?
C78 C79 1.406(5) . ?
C79 C80 1.386(6) . ?
C80 C81 1.391(6) . ?
C80 H80 0.9500 . ?
C81 C82 1.389(6) . ?
C81 C84 1.533(6) . ?
C82 C83 1.397(6) . ?
C82 H82 0.9500 . ?
C83 C88 1.523(6) . ?
C84 C86X 1.476(15) . ?
C84 C87 1.495(8) . ?
C84 C86 1.503(9) . ?
C84 C85X 1.555(12) . ?
C84 C85 1.569(9) . ?
C84 C87X 1.592(13) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C85X H85D 0.9800 . ?
C85X H85E 0.9800 . ?
C85X H85F 0.9800 . ?
C86X H86D 0.9800 . ?
C86X H86E 0.9800 . ?
C86X H86F 0.9800 . ?
C87X H87D 0.9800 . ?
C87X H87E 0.9800 . ?
C87X H87F 0.9800 . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
N1 C91 1.467(6) . ?
N1 C89 1.487(6) . ?
N1 C93 1.495(6) . ?
N1 H1 0.970(19) . ?
C89 C90 1.499(8) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 C92 1.450(7) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 C94 1.502(7) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
N2 C95 1.499(5) . ?
N2 C97 1.501(5) . ?
N2 C99 1.506(5) . ?
N2 H2 0.928(19) . ?
C95 C96 1.522(6) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C97 C98 1.509(6) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C99 C100 1.519(6) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 H10D 0.9800 . ?
C100 H10E 0.9800 . ?
C100 H10F 0.9800 . ?
N3 C101 1.176(9) . ?
C101 C102 1.380(9) . ?
C102 H10G 0.9800 . ?
C102 H10H 0.9800 . ?
C102 H10I 0.9800 . ?
N4 C103 1.139(7) . ?
C103 C104 1.462(8) . ?
C104 H10J 0.9800 . ?
C104 H10K 0.9800 . ?
C104 H10L 0.9800 . ?
N5 C105 1.147(8) . ?
C105 C106 1.380(9) . ?
C106 H10M 0.9800 . ?
C106 H10N 0.9800 . ?
C106 H10O 0.9800 . ?
N6 C107 1.127(7) . ?
C107 C108 1.431(7) . ?
C108 H10P 0.9800 . ?
C108 H10Q 0.9800 . ?
C108 H10R 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 V1 O10 109.84(16) . . ?
O9 V1 O2 109.78(15) . . ?
O10 V1 O2 113.25(15) . . ?
O9 V1 O1 108.25(15) . . ?
O10 V1 O1 111.23(14) . . ?
O2 V1 O1 104.28(14) . . ?
C1 O1 V1 123.9(3) . . ?
C12 O2 V1 131.0(3) . . ?
C23 O3 H3 112(3) . . ?
C34 O4 H4 106(3) . . ?
C45 O5 H5 113(3) . . ?
C67 O7 H7 116(4) . . ?
C78 O8 H8 113(4) . . ?
O1 C1 C2 118.1(4) . . ?
O1 C1 C6 120.2(4) . . ?
C2 C1 C6 121.6(4) . . ?
C1 C2 C3 118.3(4) . . ?
C1 C2 C88 121.1(4) . . ?
C3 C2 C88 120.7(4) . . ?
C2 C3 C4 121.7(4) . . ?
C2 C3 H3A 119.1 . . ?
C4 C3 H3A 119.1 . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C7 123.4(4) . . ?
C3 C4 C7 118.7(4) . . ?
C4 C5 C6 122.6(4) . . ?
C4 C5 H5A 118.7 . . ?
C6 C5 H5A 118.7 . . ?
C5 C6 C1 117.7(5) . . ?
C5 C6 C11 119.5(4) . . ?
C1 C6 C11 122.8(4) . . ?
C9 C7 C10 109.2(4) . . ?
C9 C7 C4 109.0(4) . . ?
C10 C7 C4 111.2(4) . . ?
C9 C7 C8 110.1(5) . . ?
C10 C7 C8 107.6(4) . . ?
C4 C7 C8 109.7(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C13 114.1(4) . . ?
C6 C11 H11A 108.7 . . ?
C13 C11 H11A 108.7 . . ?
C6 C11 H11B 108.7 . . ?
C13 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
O2 C12 C17 119.5(4) . . ?
O2 C12 C13 119.5(4) . . ?
C17 C12 C13 120.9(4) . . ?
C12 C13 C14 118.6(5) . . ?
C12 C13 C11 121.1(4) . . ?
C14 C13 C11 120.3(4) . . ?
C15 C14 C13 121.9(5) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C16 C15 C14 117.2(4) . . ?
C16 C15 C18 120.8(5) . . ?
C14 C15 C18 121.9(5) . . ?
C15 C16 C17 123.0(5) . . ?
C15 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C16 C17 C12 118.4(4) . . ?
C16 C17 C22 121.1(4) . . ?
C12 C17 C22 120.3(4) . . ?
C21 C18 C19 116.9(7) . . ?
C20X C18 C15 114.7(7) . . ?
C21 C18 C15 109.5(4) . . ?
C19 C18 C15 105.9(5) . . ?
C20X C18 C21X 114.7(10) . . ?
C15 C18 C21X 107.8(8) . . ?
C21 C18 C20 108.4(5) . . ?
C19 C18 C20 105.5(6) . . ?
C15 C18 C20 110.6(5) . . ?
C20X C18 C19X 104.8(9) . . ?
C15 C18 C19X 112.7(7) . . ?
C21X C18 C19X 101.5(10) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C19X H19D 109.5 . . ?
C18 C19X H19E 109.5 . . ?
H19D C19X H19E 109.5 . . ?
C18 C19X H19F 109.5 . . ?
H19D C19X H19F 109.5 . . ?
H19E C19X H19F 109.5 . . ?
C18 C20X H20D 109.5 . . ?
C18 C20X H20E 109.5 . . ?
H20D C20X H20E 109.5 . . ?
C18 C20X H20F 109.5 . . ?
H20D C20X H20F 109.5 . . ?
H20E C20X H20F 109.5 . . ?
C18 C21X H21D 109.5 . . ?
C18 C21X H21E 109.5 . . ?
H21D C21X H21E 109.5 . . ?
C18 C21X H21F 109.5 . . ?
H21D C21X H21F 109.5 . . ?
H21E C21X H21F 109.5 . . ?
C17 C22 C24 111.8(4) . . ?
C17 C22 H22A 109.3 . . ?
C24 C22 H22A 109.3 . . ?
C17 C22 H22B 109.3 . . ?
C24 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
O3 C23 C24 116.3(4) . . ?
O3 C23 C28 122.8(4) . . ?
C24 C23 C28 120.8(4) . . ?
C23 C24 C25 118.7(4) . . ?
C23 C24 C22 122.4(4) . . ?
C25 C24 C22 118.8(4) . . ?
C26 C25 C24 122.3(4) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 117.5(4) . . ?
C25 C26 C29 121.5(4) . . ?
C27 C26 C29 120.9(4) . . ?
C26 C27 C28 122.8(4) . . ?
C26 C27 H27 118.6 . . ?
C28 C27 H27 118.6 . . ?
C23 C28 C27 117.9(4) . . ?
C23 C28 C33 121.9(4) . . ?
C27 C28 C33 120.2(4) . . ?
C31 C29 C26 111.1(4) . . ?
C31 C29 C30 107.2(4) . . ?
C26 C29 C30 112.7(4) . . ?
C31 C29 C32 110.7(5) . . ?
C26 C29 C32 107.7(4) . . ?
C30 C29 C32 107.3(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 C35 111.4(3) . . ?
C28 C33 H33A 109.3 . . ?
C35 C33 H33A 109.3 . . ?
C28 C33 H33B 109.3 . . ?
C35 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
O4 C34 C35 117.4(4) . . ?
O4 C34 C39 121.7(4) . . ?
C35 C34 C39 120.9(4) . . ?
C34 C35 C36 119.0(4) . . ?
C34 C35 C33 121.7(4) . . ?
C36 C35 C33 119.2(4) . . ?
C37 C36 C35 121.9(4) . . ?
C37 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C36 C37 C38 117.5(4) . . ?
C36 C37 C40 122.7(4) . . ?
C38 C37 C40 119.8(4) . . ?
C39 C38 C37 122.2(4) . . ?
C39 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C38 C39 C34 118.4(4) . . ?
C38 C39 C44 119.5(4) . . ?
C34 C39 C44 122.1(4) . . ?
C42 C40 C41 108.7(4) . . ?
C42 C40 C37 110.9(4) . . ?
C41 C40 C37 111.1(4) . . ?
C42 C40 C43 109.5(4) . . ?
C41 C40 C43 107.7(5) . . ?
C37 C40 C43 108.8(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C46 C44 C39 110.5(3) . . ?
C46 C44 H44A 109.5 . . ?
C39 C44 H44A 109.5 . . ?
C46 C44 H44B 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
O5 C45 C46 118.5(3) . . ?
O5 C45 C50 121.6(3) . . ?
C46 C45 C50 119.8(3) . . ?
C47 C46 C45 119.4(3) . . ?
C47 C46 C44 119.4(3) . . ?
C45 C46 C44 121.0(3) . . ?
C48 C47 C46 122.6(4) . . ?
C48 C47 H47 118.7 . . ?
C46 C47 H47 118.7 . . ?
C47 C48 C49 116.8(4) . . ?
C47 C48 C51 122.1(4) . . ?
C49 C48 C51 121.1(4) . . ?
C50 C49 C48 122.9(4) . . ?
C50 C49 H49 118.6 . . ?
C48 C49 H49 118.6 . . ?
C49 C50 C45 118.5(4) . . ?
C49 C50 C55 120.8(3) . . ?
C45 C50 C55 120.8(3) . . ?
C52 C51 C53 110.4(5) . . ?
C52 C51 C54 107.1(5) . . ?
C53 C51 C54 107.3(5) . . ?
C52 C51 C48 112.8(4) . . ?
C53 C51 C48 110.3(4) . . ?
C54 C51 C48 108.8(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C57 C55 C50 112.4(3) . . ?
C57 C55 H55A 109.1 . . ?
C50 C55 H55A 109.1 . . ?
C57 C55 H55B 109.1 . . ?
C50 C55 H55B 109.1 . . ?
H55A C55 H55B 107.9 . . ?
O6 C56 C61 120.1(3) . . ?
O6 C56 C57 120.1(4) . . ?
C61 C56 C57 119.8(3) . . ?
C58 C57 C56 118.6(4) . . ?
C58 C57 C55 120.1(3) . . ?
C56 C57 C55 121.3(3) . . ?
C59 C58 C57 123.1(4) . . ?
C59 C58 H58 118.5 . . ?
C57 C58 H58 118.5 . . ?
C58 C59 C60 116.6(3) . . ?
C58 C59 C62 124.3(3) . . ?
C60 C59 C62 119.1(4) . . ?
C61 C60 C59 122.4(4) . . ?
C61 C60 H60 118.8 . . ?
C59 C60 H60 118.8 . . ?
C60 C61 C56 119.6(4) . . ?
C60 C61 C66 119.6(4) . . ?
C56 C61 C66 120.9(3) . . ?
C64 C62 C65 107.5(3) . . ?
C64 C62 C59 109.4(3) . . ?
C65 C62 C59 111.8(3) . . ?
C64 C62 C63 109.9(4) . . ?
C65 C62 C63 108.8(3) . . ?
C59 C62 C63 109.5(3) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C68 C66 C61 115.1(3) . . ?
C68 C66 H66A 108.5 . . ?
C61 C66 H66A 108.5 . . ?
C68 C66 H66B 108.5 . . ?
C61 C66 H66B 108.5 . . ?
H66A C66 H66B 107.5 . . ?
O7 C67 C68 122.5(3) . . ?
O7 C67 C72 117.4(4) . . ?
C68 C67 C72 120.0(4) . . ?
C67 C68 C69 118.8(4) . . ?
C67 C68 C66 121.1(4) . . ?
C69 C68 C66 120.1(4) . . ?
C68 C69 C70 123.2(4) . . ?
C68 C69 H69 118.4 . . ?
C70 C69 H69 118.4 . . ?
C71 C70 C69 116.1(4) . . ?
C71 C70 C73 121.2(4) . . ?
C69 C70 C73 122.7(4) . . ?
C72 C71 C70 123.1(4) . . ?
C72 C71 H71 118.4 . . ?
C70 C71 H71 118.4 . . ?
C71 C72 C67 118.8(4) . . ?
C71 C72 C77 120.3(4) . . ?
C67 C72 C77 120.8(4) . . ?
C75 C73 C76 109.5(5) . . ?
C75 C73 C74 108.7(5) . . ?
C76 C73 C74 105.6(5) . . ?
C75 C73 C70 113.1(4) . . ?
C76 C73 C70 110.8(4) . . ?
C74 C73 C70 108.8(4) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C73 C75 H75A 109.5 . . ?
C73 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C73 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C73 C76 H76A 109.5 . . ?
C73 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C73 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C72 C77 C79 112.7(3) . . ?
C72 C77 H77A 109.0 . . ?
C79 C77 H77A 109.0 . . ?
C72 C77 H77B 109.0 . . ?
C79 C77 H77B 109.0 . . ?
H77A C77 H77B 107.8 . . ?
O8 C78 C83 117.4(4) . . ?
O8 C78 C79 122.5(4) . . ?
C83 C78 C79 120.1(4) . . ?
C80 C79 C78 118.9(4) . . ?
C80 C79 C77 119.3(4) . . ?
C78 C79 C77 121.7(4) . . ?
C79 C80 C81 122.4(4) . . ?
C79 C80 H80 118.8 . . ?
C81 C80 H80 118.8 . . ?
C82 C81 C80 116.9(4) . . ?
C82 C81 C84 122.0(4) . . ?
C80 C81 C84 121.2(4) . . ?
C81 C82 C83 122.4(4) . . ?
C81 C82 H82 118.8 . . ?
C83 C82 H82 118.8 . . ?
C78 C83 C82 119.2(4) . . ?
C78 C83 C88 122.7(4) . . ?
C82 C83 C88 118.0(4) . . ?
C87 C84 C86 113.2(6) . . ?
C86X C84 C81 115.2(13) . . ?
C87 C84 C81 109.0(5) . . ?
C86 C84 C81 112.3(5) . . ?
C86X C84 C85X 110.8(12) . . ?
C81 C84 C85X 114.1(7) . . ?
C87 C84 C85 108.8(6) . . ?
C86 C84 C85 106.5(7) . . ?
C81 C84 C85 106.8(5) . . ?
C86X C84 C87X 107.3(13) . . ?
C81 C84 C87X 107.4(7) . . ?
C85X C84 C87X 100.8(10) . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C84 C86 H86A 109.5 . . ?
C84 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C84 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C84 C87 H87A 109.5 . . ?
C84 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C84 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C85X H85D 109.5 . . ?
C84 C85X H85E 109.5 . . ?
H85D C85X H85E 109.5 . . ?
C84 C85X H85F 109.5 . . ?
H85D C85X H85F 109.5 . . ?
H85E C85X H85F 109.5 . . ?
C84 C86X H86D 109.5 . . ?
C84 C86X H86E 109.5 . . ?
H86D C86X H86E 109.5 . . ?
C84 C86X H86F 109.5 . . ?
H86D C86X H86F 109.5 . . ?
H86E C86X H86F 109.5 . . ?
C84 C87X H87D 109.5 . . ?
C84 C87X H87E 109.5 . . ?
H87D C87X H87E 109.5 . . ?
C84 C87X H87F 109.5 . . ?
H87D C87X H87F 109.5 . . ?
H87E C87X H87F 109.5 . . ?
C2 C88 C83 114.8(4) . . ?
C2 C88 H88A 108.6 . . ?
C83 C88 H88A 108.6 . . ?
C2 C88 H88B 108.6 . . ?
C83 C88 H88B 108.6 . . ?
H88A C88 H88B 107.5 . . ?
C91 N1 C89 113.0(4) . . ?
C91 N1 C93 114.3(4) . . ?
C89 N1 C93 113.1(4) . . ?
C91 N1 H1 98(3) . . ?
C89 N1 H1 108(3) . . ?
C93 N1 H1 109(3) . . ?
N1 C89 C90 113.7(5) . . ?
N1 C89 H89A 108.8 . . ?
C90 C89 H89A 108.8 . . ?
N1 C89 H89B 108.8 . . ?
C90 C89 H89B 108.8 . . ?
H89A C89 H89B 107.7 . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C92 C91 N1 113.3(5) . . ?
C92 C91 H91A 108.9 . . ?
N1 C91 H91A 108.9 . . ?
C92 C91 H91B 108.9 . . ?
N1 C91 H91B 108.9 . . ?
H91A C91 H91B 107.7 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
N1 C93 C94 110.9(4) . . ?
N1 C93 H93A 109.5 . . ?
C94 C93 H93A 109.5 . . ?
N1 C93 H93B 109.5 . . ?
C94 C93 H93B 109.5 . . ?
H93A C93 H93B 108.1 . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C95 N2 C97 109.1(3) . . ?
C95 N2 C99 114.1(3) . . ?
C97 N2 C99 114.0(3) . . ?
C95 N2 H2 105(3) . . ?
C97 N2 H2 106(3) . . ?
C99 N2 H2 108(3) . . ?
N2 C95 C96 112.0(3) . . ?
N2 C95 H95A 109.2 . . ?
C96 C95 H95A 109.2 . . ?
N2 C95 H95B 109.2 . . ?
C96 C95 H95B 109.2 . . ?
H95A C95 H95B 107.9 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
N2 C97 C98 113.1(3) . . ?
N2 C97 H97A 109.0 . . ?
C98 C97 H97A 109.0 . . ?
N2 C97 H97B 109.0 . . ?
C98 C97 H97B 109.0 . . ?
H97A C97 H97B 107.8 . . ?
C97 C98 H98A 109.5 . . ?
C97 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C97 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N2 C99 C100 113.2(3) . . ?
N2 C99 H99A 108.9 . . ?
C100 C99 H99A 108.9 . . ?
N2 C99 H99B 108.9 . . ?
C100 C99 H99B 108.9 . . ?
H99A C99 H99B 107.8 . . ?
C99 C100 H10D 109.5 . . ?
C99 C100 H10E 109.5 . . ?
H10D C100 H10E 109.5 . . ?
C99 C100 H10F 109.5 . . ?
H10D C100 H10F 109.5 . . ?
H10E C100 H10F 109.5 . . ?
N3 C101 C102 178.1(10) . . ?
C101 C102 H10G 109.5 . . ?
C101 C102 H10H 109.5 . . ?
H10G C102 H10H 109.5 . . ?
C101 C102 H10I 109.5 . . ?
H10G C102 H10I 109.5 . . ?
H10H C102 H10I 109.5 . . ?
N4 C103 C104 178.6(7) . . ?
C103 C104 H10J 109.5 . . ?
C103 C104 H10K 109.5 . . ?
H10J C104 H10K 109.5 . . ?
C103 C104 H10L 109.5 . . ?
H10J C104 H10L 109.5 . . ?
H10K C104 H10L 109.5 . . ?
N5 C105 C106 178.3(8) . . ?
C105 C106 H10M 109.5 . . ?
C105 C106 H10N 109.5 . . ?
H10M C106 H10N 109.5 . . ?
C105 C106 H10O 109.5 . . ?
H10M C106 H10O 109.5 . . ?
H10N C106 H10O 109.5 . . ?
N6 C107 C108 179.7(8) . . ?
C107 C108 H10P 109.5 . . ?
C107 C108 H10Q 109.5 . . ?
H10P C108 H10Q 109.5 . . ?
C107 C108 H10R 109.5 . . ?
H10P C108 H10R 109.5 . . ?
H10Q C108 H10R 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 V1 O1 C1 -169.6(3) . . . . ?
O10 V1 O1 C1 -48.9(4) . . . . ?
O2 V1 O1 C1 73.5(4) . . . . ?
O9 V1 O2 C12 168.9(4) . . . . ?
O10 V1 O2 C12 45.8(4) . . . . ?
O1 V1 O2 C12 -75.3(4) . . . . ?
V1 O1 C1 C2 102.8(4) . . . . ?
V1 O1 C1 C6 -79.6(5) . . . . ?
O1 C1 C2 C3 173.9(3) . . . . ?
C6 C1 C2 C3 -3.7(6) . . . . ?
O1 C1 C2 C88 -7.0(6) . . . . ?
C6 C1 C2 C88 175.4(4) . . . . ?
C1 C2 C3 C4 0.5(6) . . . . ?
C88 C2 C3 C4 -178.6(4) . . . . ?
C2 C3 C4 C5 2.7(6) . . . . ?
C2 C3 C4 C7 -176.2(4) . . . . ?
C3 C4 C5 C6 -2.8(7) . . . . ?
C7 C4 C5 C6 176.0(4) . . . . ?
C4 C5 C6 C1 -0.2(7) . . . . ?
C4 C5 C6 C11 179.4(4) . . . . ?
O1 C1 C6 C5 -174.0(4) . . . . ?
C2 C1 C6 C5 3.5(6) . . . . ?
O1 C1 C6 C11 6.4(6) . . . . ?
C2 C1 C6 C11 -176.0(4) . . . . ?
C5 C4 C7 C9 -119.7(5) . . . . ?
C3 C4 C7 C9 59.1(6) . . . . ?
C5 C4 C7 C10 0.7(6) . . . . ?
C3 C4 C7 C10 179.6(4) . . . . ?
C5 C4 C7 C8 119.7(5) . . . . ?
C3 C4 C7 C8 -61.5(5) . . . . ?
C5 C6 C11 C13 -87.4(5) . . . . ?
C1 C6 C11 C13 92.1(5) . . . . ?
V1 O2 C12 C17 -106.3(4) . . . . ?
V1 O2 C12 C13 76.5(5) . . . . ?
O2 C12 C13 C14 176.2(4) . . . . ?
C17 C12 C13 C14 -1.0(7) . . . . ?
O2 C12 C13 C11 -1.1(6) . . . . ?
C17 C12 C13 C11 -178.3(4) . . . . ?
C6 C11 C13 C12 -91.4(5) . . . . ?
C6 C11 C13 C14 91.4(5) . . . . ?
C12 C13 C14 C15 0.1(7) . . . . ?
C11 C13 C14 C15 177.4(4) . . . . ?
C13 C14 C15 C16 -0.4(7) . . . . ?
C13 C14 C15 C18 -177.1(4) . . . . ?
C14 C15 C16 C17 1.6(7) . . . . ?
C18 C15 C16 C17 178.3(4) . . . . ?
C15 C16 C17 C12 -2.5(7) . . . . ?
C15 C16 C17 C22 -177.7(4) . . . . ?
O2 C12 C17 C16 -175.0(4) . . . . ?
C13 C12 C17 C16 2.1(6) . . . . ?
O2 C12 C17 C22 0.2(6) . . . . ?
C13 C12 C17 C22 177.4(4) . . . . ?
C16 C15 C18 C20X 128.9(9) . . . . ?
C14 C15 C18 C20X -54.5(9) . . . . ?
C16 C15 C18 C21 -61.3(7) . . . . ?
C14 C15 C18 C21 115.2(7) . . . . ?
C16 C15 C18 C19 65.5(7) . . . . ?
C14 C15 C18 C19 -117.9(7) . . . . ?
C16 C15 C18 C21X -101.9(9) . . . . ?
C14 C15 C18 C21X 74.6(10) . . . . ?
C16 C15 C18 C20 179.3(5) . . . . ?
C14 C15 C18 C20 -4.1(7) . . . . ?
C16 C15 C18 C19X 9.2(10) . . . . ?
C14 C15 C18 C19X -174.2(8) . . . . ?
C16 C17 C22 C24 100.4(5) . . . . ?
C12 C17 C22 C24 -74.7(5) . . . . ?
O3 C23 C24 C25 -177.2(4) . . . . ?
C28 C23 C24 C25 0.3(6) . . . . ?
O3 C23 C24 C22 1.6(6) . . . . ?
C28 C23 C24 C22 179.0(4) . . . . ?
C17 C22 C24 C23 111.5(5) . . . . ?
C17 C22 C24 C25 -69.8(5) . . . . ?
C23 C24 C25 C26 -1.0(7) . . . . ?
C22 C24 C25 C26 -179.8(4) . . . . ?
C24 C25 C26 C27 0.3(6) . . . . ?
C24 C25 C26 C29 175.3(4) . . . . ?
C25 C26 C27 C28 1.1(6) . . . . ?
C29 C26 C27 C28 -174.0(4) . . . . ?
O3 C23 C28 C27 178.4(4) . . . . ?
C24 C23 C28 C27 1.1(6) . . . . ?
O3 C23 C28 C33 0.7(6) . . . . ?
C24 C23 C28 C33 -176.6(4) . . . . ?
C26 C27 C28 C23 -1.8(6) . . . . ?
C26 C27 C28 C33 175.9(4) . . . . ?
C25 C26 C29 C31 141.4(5) . . . . ?
C27 C26 C29 C31 -43.7(6) . . . . ?
C25 C26 C29 C30 21.1(6) . . . . ?
C27 C26 C29 C30 -164.0(4) . . . . ?
C25 C26 C29 C32 -97.1(5) . . . . ?
C27 C26 C29 C32 77.7(5) . . . . ?
C23 C28 C33 C35 76.0(5) . . . . ?
C27 C28 C33 C35 -101.6(5) . . . . ?
O4 C34 C35 C36 179.5(3) . . . . ?
C39 C34 C35 C36 -3.7(6) . . . . ?
O4 C34 C35 C33 -4.1(6) . . . . ?
C39 C34 C35 C33 172.7(4) . . . . ?
C28 C33 C35 C34 -97.3(4) . . . . ?
C28 C33 C35 C36 79.0(5) . . . . ?
C34 C35 C36 C37 1.0(6) . . . . ?
C33 C35 C36 C37 -175.5(4) . . . . ?
C35 C36 C37 C38 1.8(6) . . . . ?
C35 C36 C37 C40 -178.7(4) . . . . ?
C36 C37 C38 C39 -2.1(6) . . . . ?
C40 C37 C38 C39 178.4(4) . . . . ?
C37 C38 C39 C34 -0.5(6) . . . . ?
C37 C38 C39 C44 -177.3(4) . . . . ?
O4 C34 C39 C38 -179.9(4) . . . . ?
C35 C34 C39 C38 3.4(6) . . . . ?
O4 C34 C39 C44 -3.2(6) . . . . ?
C35 C34 C39 C44 -179.9(4) . . . . ?
C36 C37 C40 C42 -129.0(4) . . . . ?
C38 C37 C40 C42 50.5(5) . . . . ?
C36 C37 C40 C41 -7.9(6) . . . . ?
C38 C37 C40 C41 171.6(4) . . . . ?
C36 C37 C40 C43 110.6(5) . . . . ?
C38 C37 C40 C43 -70.0(6) . . . . ?
C38 C39 C44 C46 89.5(4) . . . . ?
C34 C39 C44 C46 -87.2(5) . . . . ?
O5 C45 C46 C47 179.6(4) . . . . ?
C50 C45 C46 C47 1.0(6) . . . . ?
O5 C45 C46 C44 4.3(6) . . . . ?
C50 C45 C46 C44 -174.2(4) . . . . ?
C39 C44 C46 C47 -86.5(5) . . . . ?
C39 C44 C46 C45 88.7(5) . . . . ?
C45 C46 C47 C48 -2.0(6) . . . . ?
C44 C46 C47 C48 173.3(4) . . . . ?
C46 C47 C48 C49 1.5(6) . . . . ?
C46 C47 C48 C51 -178.6(4) . . . . ?
C47 C48 C49 C50 0.0(6) . . . . ?
C51 C48 C49 C50 -179.9(4) . . . . ?
C48 C49 C50 C45 -0.9(6) . . . . ?
C48 C49 C50 C55 178.5(4) . . . . ?
O5 C45 C50 C49 -178.1(4) . . . . ?
C46 C45 C50 C49 0.4(6) . . . . ?
O5 C45 C50 C55 2.5(6) . . . . ?
C46 C45 C50 C55 -179.0(4) . . . . ?
C47 C48 C51 C52 7.1(7) . . . . ?
C49 C48 C51 C52 -173.0(5) . . . . ?
C47 C48 C51 C53 131.1(5) . . . . ?
C49 C48 C51 C53 -49.0(6) . . . . ?
C47 C48 C51 C54 -111.5(5) . . . . ?
C49 C48 C51 C54 68.4(6) . . . . ?
C49 C50 C55 C57 -98.0(4) . . . . ?
C45 C50 C55 C57 81.4(4) . . . . ?
O6 C56 C57 C58 -179.9(3) . . . . ?
C61 C56 C57 C58 -0.4(6) . . . . ?
O6 C56 C57 C55 -1.2(6) . . . . ?
C61 C56 C57 C55 178.4(4) . . . . ?
C50 C55 C57 C58 90.3(4) . . . . ?
C50 C55 C57 C56 -88.4(4) . . . . ?
C56 C57 C58 C59 0.6(6) . . . . ?
C55 C57 C58 C59 -178.2(4) . . . . ?
C57 C58 C59 C60 -0.5(6) . . . . ?
C57 C58 C59 C62 177.2(4) . . . . ?
C58 C59 C60 C61 0.3(6) . . . . ?
C62 C59 C60 C61 -177.6(4) . . . . ?
C59 C60 C61 C56 -0.1(6) . . . . ?
C59 C60 C61 C66 178.9(3) . . . . ?
O6 C56 C61 C60 179.7(3) . . . . ?
C57 C56 C61 C60 0.2(6) . . . . ?
O6 C56 C61 C66 0.7(6) . . . . ?
C57 C56 C61 C66 -178.9(4) . . . . ?
C58 C59 C62 C64 -115.6(4) . . . . ?
C60 C59 C62 C64 62.1(5) . . . . ?
C58 C59 C62 C65 3.3(5) . . . . ?
C60 C59 C62 C65 -179.0(4) . . . . ?
C58 C59 C62 C63 123.9(4) . . . . ?
C60 C59 C62 C63 -58.4(5) . . . . ?
C60 C61 C66 C68 92.6(5) . . . . ?
C56 C61 C66 C68 -88.3(5) . . . . ?
O7 C67 C68 C69 -178.4(3) . . . . ?
C72 C67 C68 C69 -0.7(6) . . . . ?
O7 C67 C68 C66 0.3(6) . . . . ?
C72 C67 C68 C66 178.0(4) . . . . ?
C61 C66 C68 C67 84.6(5) . . . . ?
C61 C66 C68 C69 -96.7(5) . . . . ?
C67 C68 C69 C70 -0.6(6) . . . . ?
C66 C68 C69 C70 -179.4(4) . . . . ?
C68 C69 C70 C71 1.1(6) . . . . ?
C68 C69 C70 C73 -179.3(4) . . . . ?
C69 C70 C71 C72 -0.3(6) . . . . ?
C73 C70 C71 C72 -179.8(4) . . . . ?
C70 C71 C72 C67 -1.0(6) . . . . ?
C70 C71 C72 C77 178.1(4) . . . . ?
O7 C67 C72 C71 179.3(3) . . . . ?
C68 C67 C72 C71 1.5(6) . . . . ?
O7 C67 C72 C77 0.2(5) . . . . ?
C68 C67 C72 C77 -177.6(4) . . . . ?
C71 C70 C73 C75 169.9(5) . . . . ?
C69 C70 C73 C75 -9.6(7) . . . . ?
C71 C70 C73 C76 46.4(6) . . . . ?
C69 C70 C73 C76 -133.1(5) . . . . ?
C71 C70 C73 C74 -69.2(6) . . . . ?
C69 C70 C73 C74 111.3(5) . . . . ?
C71 C72 C77 C79 -79.5(5) . . . . ?
C67 C72 C77 C79 99.6(4) . . . . ?
O8 C78 C79 C80 -179.3(4) . . . . ?
C83 C78 C79 C80 0.5(6) . . . . ?
O8 C78 C79 C77 -1.5(6) . . . . ?
C83 C78 C79 C77 178.3(4) . . . . ?
C72 C77 C79 C80 100.9(4) . . . . ?
C72 C77 C79 C78 -76.9(5) . . . . ?
C78 C79 C80 C81 -0.1(7) . . . . ?
C77 C79 C80 C81 -177.9(4) . . . . ?
C79 C80 C81 C82 -0.1(7) . . . . ?
C79 C80 C81 C84 178.5(4) . . . . ?
C80 C81 C82 C83 -0.1(7) . . . . ?
C84 C81 C82 C83 -178.8(5) . . . . ?
O8 C78 C83 C82 179.1(4) . . . . ?
C79 C78 C83 C82 -0.7(7) . . . . ?
O8 C78 C83 C88 1.7(6) . . . . ?
C79 C78 C83 C88 -178.1(4) . . . . ?
C81 C82 C83 C78 0.5(7) . . . . ?
C81 C82 C83 C88 178.0(4) . . . . ?
C82 C81 C84 C86X 44.8(15) . . . . ?
C80 C81 C84 C86X -133.8(14) . . . . ?
C82 C81 C84 C87 -122.1(6) . . . . ?
C80 C81 C84 C87 59.3(7) . . . . ?
C82 C81 C84 C86 4.1(9) . . . . ?
C80 C81 C84 C86 -174.5(7) . . . . ?
C82 C81 C84 C85X 174.7(9) . . . . ?
C80 C81 C84 C85X -3.9(10) . . . . ?
C82 C81 C84 C85 120.6(6) . . . . ?
C80 C81 C84 C85 -58.1(7) . . . . ?
C82 C81 C84 C87X -74.6(10) . . . . ?
C80 C81 C84 C87X 106.8(10) . . . . ?
C1 C2 C88 C83 84.3(5) . . . . ?
C3 C2 C88 C83 -96.6(5) . . . . ?
C78 C83 C88 C2 -116.1(5) . . . . ?
C82 C83 C88 C2 66.5(6) . . . . ?
C91 N1 C89 C90 -161.0(5) . . . . ?
C93 N1 C89 C90 67.2(6) . . . . ?
C89 N1 C91 C92 -67.5(6) . . . . ?
C93 N1 C91 C92 63.8(6) . . . . ?
C91 N1 C93 C94 54.3(6) . . . . ?
C89 N1 C93 C94 -174.5(4) . . . . ?
C97 N2 C95 C96 176.5(3) . . . . ?
C99 N2 C95 C96 -54.7(5) . . . . ?
C95 N2 C97 C98 -178.6(3) . . . . ?
C99 N2 C97 C98 52.6(5) . . . . ?
C95 N2 C99 C100 -61.7(5) . . . . ?
C97 N2 C99 C100 64.6(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O4 0.823(19) 1.90(2) 2.692(4) 160(4) . yes
O4 H4 O5 0.84(5) 1.78(5) 2.610(4) 172(5) . yes
O5 H5 O6 0.95(6) 1.52(6) 2.454(4) 170(5) . yes
O7 H7 O6 0.96(6) 1.58(6) 2.534(4) 171(6) . yes
O8 H8 O7 0.835(19) 1.91(2) 2.725(4) 167(5) . yes
N1 H1 O9 0.970(19) 1.75(2) 2.714(5) 173(5) . yes
N2 H2 O10 0.928(19) 1.86(2) 2.776(4) 167(4) . yes

_refine_diff_density_max         0.753
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.067

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

data_6
_database_code_depnum_ccdc_archive 'CCDC 1574245'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 O19 V6 2-, 2(C6 H16 N 1+)'
_chemical_formula_sum            'C20 H56 N2 O19 V6'
_chemical_formula_weight         934.30

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.3807(2)
_cell_length_b                   10.7803(2)
_cell_length_c                   15.5914(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.0588(10)
_cell_angle_gamma                90
_cell_volume                     1883.46(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    24467
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.500
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_reflns_number            16623
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.079
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4310
_reflns_number_gt                3816
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.5572P] 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         4310
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0890
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 1.05343(4) 0.30231(4) 0.48263(3) 0.01176(11) Uani 1 1 d . . . . .
O1 O 1.08130(17) 0.15580(17) 0.48248(12) 0.0174(4) Uani 1 1 d . . . . .
V2 V 0.83491(4) 0.47357(4) 0.39171(3) 0.01257(11) Uani 1 1 d . . . . .
O2 O 0.72102(17) 0.45610(18) 0.31683(12) 0.0196(4) Uani 1 1 d . . . . .
V3 V 1.10756(4) 0.55648(4) 0.40012(3) 0.01153(11) Uani 1 1 d . . . . .
O3 O 1.18942(17) 0.58180(17) 0.32702(12) 0.0167(4) Uani 1 1 d . . . . .
O4 O 1.12772(16) 0.36786(16) 0.40809(11) 0.0143(4) Uani 1 1 d . . . . .
O5 O 1.17462(16) 0.34542(16) 0.58314(11) 0.0140(4) Uani 1 1 d . . . . .
C5 C 1.2069(3) 0.2610(3) 0.65391(18) 0.0209(6) Uani 1 1 d . . . . .
H5A H 1.148670 0.266732 0.693248 0.031 Uiso 1 1 calc R U . . .
H5B H 1.286368 0.282197 0.685764 0.031 Uiso 1 1 calc R U . . .
H5C H 1.207676 0.176286 0.631300 0.031 Uiso 1 1 calc R U . . .
O6 O 0.94202(16) 0.29842(16) 0.57672(11) 0.0129(4) Uani 1 1 d . . . . .
O7 O 0.89897(16) 0.29996(16) 0.40256(11) 0.0139(4) Uani 1 1 d . . . . .
C7 C 0.8175(3) 0.1984(3) 0.40188(18) 0.0201(6) Uani 1 1 d . . . . .
H7A H 0.862509 0.120802 0.413012 0.030 Uiso 1 1 calc R U . . .
H7B H 0.765326 0.193851 0.344893 0.030 Uiso 1 1 calc R U . . .
H7C H 0.769043 0.210998 0.447287 0.030 Uiso 1 1 calc R U . . .
O8 O 0.76265(15) 0.44347(16) 0.49833(11) 0.0136(4) Uani 1 1 d . . . . .
C8 C 0.6521(2) 0.5027(3) 0.50417(18) 0.0203(6) Uani 1 1 d . . . . .
H8A H 0.620160 0.468290 0.553557 0.030 Uiso 1 1 calc R U . . .
H8B H 0.595143 0.488335 0.450267 0.030 Uiso 1 1 calc R U . . .
H8C H 0.665208 0.591995 0.512703 0.030 Uiso 1 1 calc R U . . .
O9 O 0.95997(16) 0.51548(16) 0.32040(11) 0.0131(4) Uani 1 1 d . . . . .
C9 C 0.9631(3) 0.4465(3) 0.24267(17) 0.0186(6) Uani 1 1 d . . . . .
H9A H 1.022477 0.482831 0.211563 0.028 Uiso 1 1 calc R U . . .
H9B H 0.884316 0.449070 0.205367 0.028 Uiso 1 1 calc R U . . .
H9C H 0.984562 0.360186 0.257738 0.028 Uiso 1 1 calc R U . . .
O10 O 1.000000 0.500000 0.500000 0.0117(5) Uani 1 2 d S . P . .
N1 N 0.8597(2) 0.1192(2) 0.67744(14) 0.0159(5) Uani 1 1 d . . . . .
H1 H 0.880143 0.194980 0.646064 0.019 Uiso 1 1 calc R U . . .
C10 C 0.7500(3) 0.0641(3) 0.62325(19) 0.0222(6) Uani 1 1 d . . . . .
H10A H 0.717663 -0.000834 0.657482 0.027 Uiso 1 1 calc R U . . .
H10B H 0.772264 0.024175 0.571188 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6541(3) 0.1603(3) 0.5943(2) 0.0279(7) Uani 1 1 d . . . . .
H11A H 0.687191 0.227702 0.563709 0.042 Uiso 1 1 calc R U . . .
H11B H 0.625545 0.193755 0.645412 0.042 Uiso 1 1 calc R U . . .
H11C H 0.587440 0.121635 0.555121 0.042 Uiso 1 1 calc R U . . .
C12 C 0.8368(3) 0.1614(3) 0.76492(18) 0.0225(6) Uani 1 1 d . . . . .
H12A H 0.812383 0.089130 0.796829 0.027 Uiso 1 1 calc R U . . .
H12B H 0.770069 0.221523 0.756405 0.027 Uiso 1 1 calc R U . . .
C13 C 0.9450(3) 0.2212(3) 0.8193(2) 0.0308(7) Uani 1 1 d . . . . .
H13A H 0.974971 0.287118 0.785559 0.046 Uiso 1 1 calc R U . . .
H13B H 1.007424 0.158648 0.835534 0.046 Uiso 1 1 calc R U . . .
H13C H 0.922828 0.256682 0.872121 0.046 Uiso 1 1 calc R U . . .
C14 C 0.9645(2) 0.0315(2) 0.68295(18) 0.0185(6) Uani 1 1 d . . . . .
H14A H 0.978330 0.013716 0.623210 0.022 Uiso 1 1 calc R U . . .
H14B H 1.036709 0.073361 0.714580 0.022 Uiso 1 1 calc R U . . .
C15 C 0.9485(3) -0.0900(3) 0.72795(19) 0.0235(6) Uani 1 1 d . . . . .
H15A H 0.881584 -0.135828 0.694220 0.035 Uiso 1 1 calc R U . . .
H15B H 0.931882 -0.073473 0.786481 0.035 Uiso 1 1 calc R U . . .
H15C H 1.021549 -0.139415 0.732312 0.035 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6111(18) . ?
V1 O4 1.7054(18) . ?
V1 O5 1.9543(18) . ?
V1 O7 1.9704(18) . ?
V1 O6 2.1002(18) . ?
V1 O10 2.2455(4) . ?
V2 O2 1.5969(19) . ?
V2 O5 1.9970(18) 3_766 ?
V2 O9 2.0047(18) . ?
V2 O7 2.0050(18) . ?
V2 O8 2.0056(18) . ?
V2 O10 2.3138(4) . ?
V3 O3 1.6163(18) . ?
V3 O6 1.7225(18) 3_766 ?
V3 O9 1.9577(18) . ?
V3 O8 1.9676(17) 3_766 ?
V3 O4 2.0476(18) . ?
V3 O10 2.2271(4) . ?
O5 C5 1.428(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
O7 C7 1.434(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
O8 C8 1.427(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O9 C9 1.428(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N1 C10 1.502(3) . ?
N1 C12 1.503(3) . ?
N1 C14 1.513(3) . ?
N1 H1 1.0000 . ?
C10 C11 1.516(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.512(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.512(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O4 106.50(9) . . ?
O1 V1 O5 97.05(9) . . ?
O4 V1 O5 94.79(8) . . ?
O1 V1 O7 98.08(9) . . ?
O4 V1 O7 93.85(8) . . ?
O5 V1 O7 159.67(8) . . ?
O1 V1 O6 97.15(8) . . ?
O4 V1 O6 156.34(8) . . ?
O5 V1 O6 82.66(7) . . ?
O7 V1 O6 82.05(7) . . ?
O1 V1 O10 171.17(7) . . ?
O4 V1 O10 82.29(6) . . ?
O5 V1 O10 81.12(5) . . ?
O7 V1 O10 81.85(5) . . ?
O6 V1 O10 74.07(5) . . ?
O2 V2 O5 101.17(9) . 3_766 ?
O2 V2 O9 100.68(9) . . ?
O5 V2 O9 87.53(7) 3_766 . ?
O2 V2 O7 100.86(9) . . ?
O5 V2 O7 157.97(7) 3_766 . ?
O9 V2 O7 88.53(7) . . ?
O2 V2 O8 100.89(9) . . ?
O5 V2 O8 87.20(7) 3_766 . ?
O9 V2 O8 158.40(7) . . ?
O7 V2 O8 88.55(7) . . ?
O2 V2 O10 179.69(8) . . ?
O5 V2 O10 78.55(5) 3_766 . ?
O9 V2 O10 79.18(5) . . ?
O7 V2 O10 79.42(5) . . ?
O8 V2 O10 79.24(5) . . ?
O3 V3 O6 104.17(9) . 3_766 ?
O3 V3 O9 97.28(9) . . ?
O6 V3 O9 93.55(8) 3_766 . ?
O3 V3 O8 97.08(9) . 3_766 ?
O6 V3 O8 93.35(8) 3_766 3_766 ?
O9 V3 O8 162.03(8) . 3_766 ?
O3 V3 O4 97.95(8) . . ?
O6 V3 O4 157.89(8) 3_766 . ?
O9 V3 O4 83.62(7) . . ?
O8 V3 O4 83.75(7) 3_766 . ?
O3 V3 O10 173.79(7) . . ?
O6 V3 O10 82.04(6) 3_766 . ?
O9 V3 O10 82.35(5) . . ?
O8 V3 O10 82.21(5) 3_766 . ?
O4 V3 O10 75.85(5) . . ?
V1 O4 V3 112.91(9) . . ?
C5 O5 V1 121.22(16) . . ?
C5 O5 V2 119.09(16) . 3_766 ?
V1 O5 V2 109.56(8) . 3_766 ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
V3 O6 V1 112.84(9) 3_766 . ?
C7 O7 V1 121.24(16) . . ?
C7 O7 V2 119.17(16) . . ?
V1 O7 V2 108.21(8) . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 O8 V3 119.64(16) . 3_766 ?
C8 O8 V2 118.30(15) . . ?
V3 O8 V2 107.94(8) 3_766 . ?
O8 C8 H8A 109.5 . . ?
O8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O8 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 O9 V3 120.72(16) . . ?
C9 O9 V2 118.60(16) . . ?
V3 O9 V2 108.20(8) . . ?
O9 C9 H9A 109.5 . . ?
O9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O9 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
V3 O10 V3 180.0 3_766 . ?
V3 O10 V1 91.050(16) 3_766 . ?
V3 O10 V1 88.949(15) . . ?
V3 O10 V1 88.951(16) 3_766 3_766 ?
V3 O10 V1 91.050(15) . 3_766 ?
V1 O10 V1 180.00(2) . 3_766 ?
V3 O10 V2 89.934(15) 3_766 3_766 ?
V3 O10 V2 90.065(15) . 3_766 ?
V1 O10 V2 90.138(15) . 3_766 ?
V1 O10 V2 89.864(15) 3_766 3_766 ?
V3 O10 V2 90.065(15) 3_766 . ?
V3 O10 V2 89.935(15) . . ?
V1 O10 V2 89.863(15) . . ?
V1 O10 V2 90.136(15) 3_766 . ?
V2 O10 V2 180.0 3_766 . ?
C10 N1 C12 111.8(2) . . ?
C10 N1 C14 110.7(2) . . ?
C12 N1 C14 113.4(2) . . ?
C10 N1 H1 106.8 . . ?
C12 N1 H1 106.8 . . ?
C14 N1 H1 106.8 . . ?
N1 C10 C11 112.4(2) . . ?
N1 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C13 112.6(2) . . ?
N1 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
N1 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 114.2(2) . . ?
C15 C14 H14A 108.7 . . ?
N1 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
N1 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 O4 V3 -178.52(9) . . . . ?
O5 V1 O4 V3 -79.70(10) . . . . ?
O7 V1 O4 V3 81.87(10) . . . . ?
O6 V1 O4 V3 2.9(3) . . . . ?
O10 V1 O4 V3 0.65(7) . . . . ?
C12 N1 C10 C11 68.9(3) . . . . ?
C14 N1 C10 C11 -163.5(2) . . . . ?
C10 N1 C12 C13 -178.0(2) . . . . ?
C14 N1 C12 C13 55.9(3) . . . . ?
C10 N1 C14 C15 -63.4(3) . . . . ?
C12 N1 C14 C15 63.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O6 1.00 1.78 2.755(3) 163.4 . yes

_refine_diff_density_max         0.441
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.094


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

data_2_H2O
_database_code_depnum_ccdc_archive 'CCDC 1574241'
_audit_update_record             
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O25 S4 V5 5-, 5(C6 H16 N 1+), H2 O'
_chemical_formula_sum            'C30 H82 N5 O26 S4 V5'
_chemical_formula_weight         1311.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   13.2439(4)
_cell_length_b                   13.3679(4)
_cell_length_c                   31.3605(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.4436(5)
_cell_angle_gamma                90
_cell_volume                     5460.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    24188
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      30.07

_exptl_crystal_description       tablet
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_F_000             2736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.830
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.060
_shelx_estimated_absorpt_T_min   0.473
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62632
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         0.660
_diffrn_reflns_theta_max         30.239
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             30874
_reflns_number_gt                27570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_max     0.906
_reflns_Friedel_fraction_full    0.992

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

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          
'Disorder: two fold disorder modelled for the Et groups in 5 of the 10 unique cations.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+2.3635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 11479 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.006(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         30874
_refine_ls_number_parameters     1479
_refine_ls_number_restraints     786
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.75355(5) 0.24335(4) 0.10011(2) 0.01733(12) Uani 1 1 d . . . . .
O1 O 0.7172(2) 0.1567(2) 0.06606(10) 0.0291(6) Uani 1 1 d . . . . .
V2 V 0.99315(5) 0.38716(4) 0.09953(2) 0.01649(12) Uani 1 1 d . . . . .
O2 O 1.0686(2) 0.3689(2) 0.06645(9) 0.0252(6) Uani 1 1 d . . . . .
V3 V 0.84716(5) 0.62381(5) 0.09667(2) 0.02365(14) Uani 1 1 d . . . . .
O3 O 0.8520(3) 0.7083(2) 0.06134(13) 0.0401(8) Uani 1 1 d . . . . .
V4 V 0.61109(5) 0.48122(5) 0.09928(2) 0.01941(13) Uani 1 1 d . . . . .
O4 O 0.5085(2) 0.5000(2) 0.06529(10) 0.0291(6) Uani 1 1 d . . . . .
V5 V 0.78400(5) 0.43042(5) 0.05706(2) 0.01818(12) Uani 1 1 d . . . . .
O5 O 0.7620(2) 0.4272(2) 0.00517(9) 0.0289(6) Uani 1 1 d . . . . .
O6 O 0.86180(19) 0.31978(19) 0.07917(8) 0.0179(5) Uani 1 1 d . . . . .
O7 O 0.9051(2) 0.5005(2) 0.07759(9) 0.0203(5) Uani 1 1 d . . . . .
O8 O 0.7240(2) 0.5442(2) 0.07671(9) 0.0230(6) Uani 1 1 d . . . . .
O9 O 0.6802(2) 0.3651(2) 0.07914(9) 0.0192(5) Uani 1 1 d . . . . .
S1 S 0.97569(7) 0.17856(7) 0.14591(3) 0.01960(17) Uani 1 1 d . . . . .
O10 O 0.8637(2) 0.1908(2) 0.14656(9) 0.0243(6) Uani 1 1 d . . . . .
O11 O 1.0213(2) 0.2815(2) 0.14487(9) 0.0228(6) Uani 1 1 d . . . . .
O12 O 0.9905(2) 0.1218(3) 0.10826(10) 0.0309(7) Uani 1 1 d . . . . .
O13 O 1.0239(2) 0.1331(2) 0.18667(9) 0.0303(7) Uani 1 1 d . . . . .
S2 S 1.07505(7) 0.58789(7) 0.14663(3) 0.02195(18) Uani 1 1 d . . . . .
O14 O 1.0615(2) 0.4759(2) 0.14646(9) 0.0228(6) Uani 1 1 d . . . . .
O15 O 0.9703(2) 0.6348(2) 0.14367(10) 0.0287(6) Uani 1 1 d . . . . .
O16 O 1.1185(2) 0.6178(2) 0.10922(10) 0.0295(6) Uani 1 1 d . . . . .
O17 O 1.1375(2) 0.6155(2) 0.18747(10) 0.0338(7) Uani 1 1 d . . . . .
S3 S 0.66848(9) 0.69169(8) 0.14557(5) 0.0410(3) Uani 1 1 d . . . . .
O18 O 0.7813(2) 0.6801(2) 0.14312(13) 0.0396(9) Uani 1 1 d . . . . .
O19 O 0.6250(2) 0.5870(2) 0.14423(11) 0.0307(7) Uani 1 1 d . . . . .
O20 O 0.6161(3) 0.7500(3) 0.11007(18) 0.0624(13) Uani 1 1 d . . . . .
O21 O 0.6645(3) 0.7320(3) 0.18785(17) 0.0634(14) Uani 1 1 d . . . . .
S4 S 0.56779(7) 0.28470(7) 0.15014(3) 0.02113(18) Uani 1 1 d . . . . .
O22 O 0.5809(2) 0.3962(2) 0.14735(9) 0.0226(5) Uani 1 1 d . . . . .
O23 O 0.6684(2) 0.2366(2) 0.14602(10) 0.0262(6) Uani 1 1 d . . . . .
O24 O 0.4870(2) 0.2521(3) 0.11557(11) 0.0349(7) Uani 1 1 d . . . . .
O25 O 0.5476(3) 0.2623(2) 0.19310(10) 0.0332(7) Uani 1 1 d . . . . .
N1 N 0.9247(3) 0.0132(3) 0.03252(12) 0.0286(7) Uani 1 1 d D U . . .
H1 H 0.9178 0.0491 0.0598 0.034 Uiso 0.719(7) 1 calc R U P A 1
H1X H 0.9251 0.0523 0.0597 0.034 Uiso 0.281(7) 1 calc R U P A 2
C1 C 0.8195(5) 0.0105(5) 0.0027(2) 0.0420(17) Uani 0.719(7) 1 d D U P A 1
H1A H 0.8257 -0.0200 -0.0255 0.050 Uiso 0.719(7) 1 calc R U P A 1
H1B H 0.7925 0.0793 -0.0027 0.050 Uiso 0.719(7) 1 calc R U P A 1
C2 C 0.7440(5) -0.0534(5) 0.0253(4) 0.098(3) Uani 1 1 d D U . . .
H2A H 0.6763 -0.0558 0.0066 0.148 Uiso 0.719(7) 1 calc R U P A 1
H2B H 0.7710 -0.1215 0.0304 0.148 Uiso 0.719(7) 1 calc R U P A 1
H2C H 0.7380 -0.0225 0.0531 0.148 Uiso 0.719(7) 1 calc R U P A 1
H2D H 0.7034 -0.1135 0.0281 0.148 Uiso 0.281(7) 1 calc R U P A 2
H2E H 0.7279 -0.0018 0.0452 0.148 Uiso 0.281(7) 1 calc R U P A 2
H2F H 0.7276 -0.0285 -0.0045 0.148 Uiso 0.281(7) 1 calc R U P A 2
C3 C 0.9627(6) -0.0892(5) 0.0438(2) 0.0386(16) Uani 0.719(7) 1 d D U P A 1
H3A H 0.9660 -0.1266 0.0168 0.046 Uiso 0.719(7) 1 calc R U P A 1
H3B H 0.9138 -0.1242 0.0590 0.046 Uiso 0.719(7) 1 calc R U P A 1
C4 C 1.0705(5) -0.0884(5) 0.07300(19) 0.0574(16) Uani 1 1 d D U . . .
H4A H 1.0931 -0.1574 0.0798 0.086 Uiso 0.719(7) 1 calc R U P A 1
H4B H 1.1194 -0.0549 0.0578 0.086 Uiso 0.719(7) 1 calc R U P A 1
H4C H 1.0672 -0.0525 0.1000 0.086 Uiso 0.719(7) 1 calc R U P A 1
H4D H 1.1418 -0.1091 0.0737 0.086 Uiso 0.281(7) 1 calc R U P A 2
H4E H 1.0655 -0.0525 0.0998 0.086 Uiso 0.281(7) 1 calc R U P A 2
H4F H 1.0262 -0.1477 0.0705 0.086 Uiso 0.281(7) 1 calc R U P A 2
C5 C 0.9978(5) 0.0708(4) 0.0102(2) 0.0322(14) Uani 0.719(7) 1 d D U P A 1
H5A H 1.0057 0.0355 -0.0168 0.039 Uiso 0.719(7) 1 calc R U P A 1
H5B H 1.0660 0.0737 0.0293 0.039 Uiso 0.719(7) 1 calc R U P A 1
C6 C 0.9596(5) 0.1768(4) -0.00092(17) 0.0445(12) Uani 1 1 d D U . . .
H6A H 1.0087 0.2122 -0.0154 0.067 Uiso 0.719(7) 1 calc R U P A 1
H6B H 0.8926 0.1741 -0.0203 0.067 Uiso 0.719(7) 1 calc R U P A 1
H6C H 0.9528 0.2123 0.0258 0.067 Uiso 0.719(7) 1 calc R U P A 1
H6D H 0.9327 0.2214 -0.0251 0.067 Uiso 0.281(7) 1 calc R U P A 2
H6E H 0.9608 0.2121 0.0265 0.067 Uiso 0.281(7) 1 calc R U P A 2
H6F H 1.0293 0.1559 -0.0031 0.067 Uiso 0.281(7) 1 calc R U P A 2
C1X C 0.8633(12) -0.0801(13) 0.0370(7) 0.049(4) Uani 0.281(7) 1 d D U P A 2
H1C H 0.8804 -0.1058 0.0670 0.059 Uiso 0.281(7) 1 calc R U P A 2
H1D H 0.8802 -0.1326 0.0171 0.059 Uiso 0.281(7) 1 calc R U P A 2
C3X C 1.0359(12) -0.0191(13) 0.0337(5) 0.041(4) Uani 0.281(7) 1 d D U P A 2
H3C H 1.0809 0.0406 0.0359 0.049 Uiso 0.281(7) 1 calc R U P A 2
H3D H 1.0416 -0.0548 0.0066 0.049 Uiso 0.281(7) 1 calc R U P A 2
C5X C 0.8879(14) 0.0812(11) -0.0027(5) 0.039(4) Uani 0.281(7) 1 d D U P A 2
H5C H 0.8172 0.1025 -0.0010 0.047 Uiso 0.281(7) 1 calc R U P A 2
H5D H 0.8858 0.0462 -0.0307 0.047 Uiso 0.281(7) 1 calc R U P A 2
N2 N 1.1961(3) 0.2341(3) 0.23027(12) 0.0365(9) Uani 1 1 d D . . . .
H2 H 1.148(4) 0.195(4) 0.2138(16) 0.044 Uiso 1 1 d D U . . .
C7 C 1.2714(5) 0.2400(6) 0.20016(19) 0.066(2) Uani 1 1 d D . . . .
H7A H 1.3366 0.2689 0.2158 0.079 Uiso 1 1 calc R U . . .
H7B H 1.2442 0.2852 0.1758 0.079 Uiso 1 1 calc R U . . .
C8 C 1.2928(6) 0.1373(7) 0.1822(3) 0.089(3) Uani 1 1 d D . . . .
H8A H 1.3284 0.0952 0.2058 0.133 Uiso 1 1 calc R U . . .
H8B H 1.3359 0.1452 0.1601 0.133 Uiso 1 1 calc R U . . .
H8C H 1.2277 0.1057 0.1692 0.133 Uiso 1 1 calc R U . . .
C9 C 1.1491(5) 0.3361(4) 0.23787(17) 0.0472(14) Uani 1 1 d D . . . .
H9A H 1.1114 0.3617 0.2099 0.057 Uiso 1 1 calc R U . . .
H9B H 1.0989 0.3269 0.2574 0.057 Uiso 1 1 calc R U . . .
C10 C 1.2266(5) 0.4120(4) 0.2571(2) 0.0605(17) Uani 1 1 d D . . . .
H10A H 1.2612 0.3893 0.2858 0.091 Uiso 1 1 calc R U . . .
H10B H 1.1922 0.4759 0.2600 0.091 Uiso 1 1 calc R U . . .
H10C H 1.2774 0.4208 0.2383 0.091 Uiso 1 1 calc R U . . .
C11 C 1.2399(4) 0.1800(4) 0.27133(14) 0.0339(10) Uani 1 1 d D . . . .
H11A H 1.2985 0.2188 0.2872 0.041 Uiso 1 1 calc R U . . .
H11B H 1.2662 0.1141 0.2640 0.041 Uiso 1 1 calc R U . . .
C12 C 1.1624(4) 0.1647(4) 0.30022(15) 0.0359(10) Uani 1 1 d D . . . .
H12A H 1.1404 0.2298 0.3096 0.054 Uiso 1 1 calc R U . . .
H12B H 1.1934 0.1254 0.3256 0.054 Uiso 1 1 calc R U . . .
H12C H 1.1028 0.1288 0.2842 0.054 Uiso 1 1 calc R U . . .
N3 N 1.3274(3) 0.6543(3) 0.13409(16) 0.0423(10) Uani 1 1 d D U . . .
H3 H 1.2536 0.6367 0.1240 0.051 Uiso 0.664(14) 1 calc R U P B 1
H3X H 1.2510 0.6581 0.1309 0.051 Uiso 0.336(14) 1 calc R U P B 2
C13 C 1.3209(7) 0.7437(7) 0.1634(4) 0.068(3) Uani 0.664(14) 1 d D U P B 1
H13A H 1.2761 0.7953 0.1471 0.081 Uiso 0.664(14) 1 calc R U P B 1
H13B H 1.2895 0.7226 0.1883 0.081 Uiso 0.664(14) 1 calc R U P B 1
C14 C 1.4260(7) 0.7883(9) 0.1800(5) 0.081(4) Uani 0.664(14) 1 d D U P B 1
H14A H 1.4191 0.8456 0.1987 0.121 Uiso 0.664(14) 1 calc R U P B 1
H14B H 1.4701 0.7377 0.1966 0.121 Uiso 0.664(14) 1 calc R U P B 1
H14C H 1.4567 0.8104 0.1554 0.121 Uiso 0.664(14) 1 calc R U P B 1
C15 C 1.3636(4) 0.6739(5) 0.0927(2) 0.0543(16) Uani 1 1 d D . . . .
H15A H 1.3525 0.6132 0.0744 0.065 Uiso 1 1 calc R U . . .
H15B H 1.4383 0.6873 0.0991 0.065 Uiso 1 1 calc R U . . .
C16 C 1.3101(4) 0.7613(5) 0.0675(3) 0.065(2) Uani 1 1 d . . . . .
H16A H 1.2362 0.7574 0.0674 0.098 Uiso 1 1 calc R U . . .
H16B H 1.3222 0.7589 0.0376 0.098 Uiso 1 1 calc R U . . .
H16C H 1.3372 0.8241 0.0811 0.098 Uiso 1 1 calc R U . . .
C17 C 1.3704(4) 0.5601(4) 0.15543(18) 0.0405(11) Uani 1 1 d D . . . .
H17A H 1.3527 0.5565 0.1847 0.049 Uiso 1 1 calc R U . . .
H17B H 1.4462 0.5623 0.1590 0.049 Uiso 1 1 calc R U . . .
C18 C 1.3322(4) 0.4673(4) 0.13081(19) 0.0399(11) Uani 1 1 d . . . . .
H18A H 1.2570 0.4659 0.1260 0.060 Uiso 1 1 calc R U . . .
H18B H 1.3594 0.4082 0.1476 0.060 Uiso 1 1 calc R U . . .
H18C H 1.3552 0.4670 0.1028 0.060 Uiso 1 1 calc R U . . .
C13X C 1.3834(11) 0.7392(12) 0.1635(7) 0.054(5) Uani 0.336(14) 1 d D U P B 2
H13C H 1.4186 0.7110 0.1915 0.064 Uiso 0.336(14) 1 calc R U P B 2
H13D H 1.4356 0.7715 0.1491 0.064 Uiso 0.336(14) 1 calc R U P B 2
C14X C 1.3046(14) 0.8148(15) 0.1712(8) 0.069(7) Uani 0.336(14) 1 d D U P B 2
H14D H 1.3384 0.8687 0.1897 0.103 Uiso 0.336(14) 1 calc R U P B 2
H14E H 1.2705 0.8426 0.1434 0.103 Uiso 0.336(14) 1 calc R U P B 2
H14F H 1.2536 0.7823 0.1856 0.103 Uiso 0.336(14) 1 calc R U P B 2
N4 N 0.9368(10) 0.8056(8) 0.2088(4) 0.040(2) Uani 0.560(7) 1 d D U P C 1
H4 H 0.9173 0.7510 0.1871 0.048 Uiso 0.560(7) 1 calc R U P C 1
C19 C 0.9221(8) 0.7644(7) 0.2518(3) 0.043(2) Uani 0.560(7) 1 d D U P C 1
H19A H 0.8506 0.7404 0.2494 0.052 Uiso 0.560(7) 1 calc R U P C 1
H19B H 0.9332 0.8184 0.2737 0.052 Uiso 0.560(7) 1 calc R U P C 1
C20 C 0.9947(11) 0.6798(9) 0.2664(4) 0.068(4) Uani 0.560(7) 1 d D U P C 1
H20A H 0.9829 0.6549 0.2945 0.102 Uiso 0.560(7) 1 calc R U P C 1
H20B H 0.9831 0.6257 0.2450 0.102 Uiso 0.560(7) 1 calc R U P C 1
H20C H 1.0656 0.7037 0.2694 0.102 Uiso 0.560(7) 1 calc R U P C 1
C21 C 0.8618(7) 0.8899(8) 0.1958(3) 0.0362(19) Uani 0.560(7) 1 d D U P C 1
H21A H 0.7928 0.8681 0.2000 0.043 Uiso 0.560(7) 1 calc R U P C 1
H21B H 0.8822 0.9476 0.2152 0.043 Uiso 0.560(7) 1 calc R U P C 1
C22 C 0.8552(10) 0.9230(8) 0.1501(4) 0.051(3) Uani 0.560(7) 1 d D U P C 1
H22A H 0.8054 0.9776 0.1439 0.077 Uiso 0.560(7) 1 calc R U P C 1
H22B H 0.9228 0.9464 0.1458 0.077 Uiso 0.560(7) 1 calc R U P C 1
H22C H 0.8333 0.8668 0.1306 0.077 Uiso 0.560(7) 1 calc R U P C 1
C23 C 1.0463(7) 0.8334(7) 0.2068(3) 0.040(2) Uani 0.560(7) 1 d D U P C 1
H23A H 1.0904 0.7736 0.2137 0.048 Uiso 0.560(7) 1 calc R U P C 1
H23B H 1.0502 0.8543 0.1769 0.048 Uiso 0.560(7) 1 calc R U P C 1
C24 C 1.0870(18) 0.9161(17) 0.2375(8) 0.057(6) Uani 0.560(7) 1 d D U P C 1
H24A H 1.1580 0.9309 0.2348 0.086 Uiso 0.560(7) 1 calc R U P C 1
H24B H 1.0446 0.9760 0.2304 0.086 Uiso 0.560(7) 1 calc R U P C 1
H24C H 1.0848 0.8953 0.2673 0.086 Uiso 0.560(7) 1 calc R U P C 1
N4X N 0.9807(7) 0.8512(6) 0.2454(3) 0.033(2) Uani 0.440(7) 1 d D U P C 2
H4X H 0.9418 0.8906 0.2641 0.040 Uiso 0.440(7) 1 calc R U P C 2
C19X C 1.0136(9) 0.7572(8) 0.2691(4) 0.039(3) Uani 0.440(7) 1 d D U P C 2
H19C H 1.0703 0.7724 0.2935 0.047 Uiso 0.440(7) 1 calc R U P C 2
H19D H 1.0404 0.7105 0.2493 0.047 Uiso 0.440(7) 1 calc R U P C 2
C20X C 0.9280(12) 0.7065(10) 0.2867(6) 0.064(5) Uani 0.440(7) 1 d D U P C 2
H20D H 0.9540 0.6452 0.3020 0.097 Uiso 0.440(7) 1 calc R U P C 2
H20E H 0.9021 0.7517 0.3069 0.097 Uiso 0.440(7) 1 calc R U P C 2
H20F H 0.8722 0.6897 0.2628 0.097 Uiso 0.440(7) 1 calc R U P C 2
C21X C 0.9082(15) 0.8318(14) 0.2039(6) 0.042(4) Uani 0.440(7) 1 d D U P C 2
H21C H 0.9399 0.7810 0.1875 0.050 Uiso 0.440(7) 1 calc R U P C 2
H21D H 0.8452 0.8015 0.2112 0.050 Uiso 0.440(7) 1 calc R U P C 2
C22X C 0.8768(13) 0.9166(11) 0.1748(6) 0.060(4) Uani 0.440(7) 1 d D U P C 2
H22D H 0.8295 0.8931 0.1490 0.090 Uiso 0.440(7) 1 calc R U P C 2
H22E H 0.8425 0.9669 0.1898 0.090 Uiso 0.440(7) 1 calc R U P C 2
H22F H 0.9376 0.9463 0.1660 0.090 Uiso 0.440(7) 1 calc R U P C 2
C23X C 1.0724(17) 0.9157(17) 0.2389(5) 0.030(4) Uani 0.440(7) 1 d D U P C 2
H23C H 1.0465 0.9812 0.2268 0.036 Uiso 0.440(7) 1 calc R U P C 2
H23D H 1.1161 0.9282 0.2675 0.036 Uiso 0.440(7) 1 calc R U P C 2
C24X C 1.1365(10) 0.8709(11) 0.2098(4) 0.052(3) Uani 0.440(7) 1 d D U P C 2
H24D H 1.1932 0.9163 0.2072 0.078 Uiso 0.440(7) 1 calc R U P C 2
H24E H 1.1641 0.8068 0.2218 0.078 Uiso 0.440(7) 1 calc R U P C 2
H24F H 1.0945 0.8600 0.1811 0.078 Uiso 0.440(7) 1 calc R U P C 2
N5 N 0.4102(3) 0.1372(3) 0.04507(13) 0.0323(8) Uani 1 1 d D . . . .
H5 H 0.445(4) 0.172(4) 0.0643(15) 0.039 Uiso 1 1 d D U . . .
C25 C 0.3996(4) 0.1892(4) 0.00256(17) 0.0457(12) Uani 1 1 d . . . . .
H25A H 0.3915 0.1387 -0.0209 0.055 Uiso 1 1 calc R U . . .
H25B H 0.3368 0.2309 -0.0018 0.055 Uiso 1 1 calc R U . . .
C26 C 0.4888(6) 0.2534(7) -0.0007(2) 0.078(3) Uani 1 1 d . . . . .
H26A H 0.5013 0.2995 0.0240 0.117 Uiso 1 1 calc R U . . .
H26B H 0.4746 0.2918 -0.0277 0.117 Uiso 1 1 calc R U . . .
H26C H 0.5496 0.2115 -0.0005 0.117 Uiso 1 1 calc R U . . .
C27 C 0.3082(4) 0.1155(4) 0.05796(19) 0.0446(12) Uani 1 1 d . . . . .
H27A H 0.3199 0.0756 0.0850 0.054 Uiso 1 1 calc R U . . .
H27B H 0.2661 0.0747 0.0350 0.054 Uiso 1 1 calc R U . . .
C28 C 0.2485(4) 0.2107(5) 0.0651(2) 0.0545(16) Uani 1 1 d . . . . .
H28A H 0.2928 0.2554 0.0850 0.082 Uiso 1 1 calc R U . . .
H28B H 0.1882 0.1927 0.0775 0.082 Uiso 1 1 calc R U . . .
H28C H 0.2263 0.2446 0.0373 0.082 Uiso 1 1 calc R U . . .
C29 C 0.4719(4) 0.0423(4) 0.04476(16) 0.0352(10) Uani 1 1 d . . . . .
H29A H 0.5300 0.0551 0.0296 0.042 Uiso 1 1 calc R U . . .
H29B H 0.4280 -0.0098 0.0283 0.042 Uiso 1 1 calc R U . . .
C30 C 0.5134(4) 0.0036(4) 0.08988(17) 0.0403(11) Uani 1 1 d . . . . .
H30A H 0.5542 0.0560 0.1068 0.060 Uiso 1 1 calc R U . . .
H30B H 0.5567 -0.0551 0.0880 0.060 Uiso 1 1 calc R U . . .
H30C H 0.4561 -0.0152 0.1041 0.060 Uiso 1 1 calc R U . . .
V6 V 0.15165(5) -0.04754(4) 0.38940(2) 0.01638(12) Uani 1 1 d . . . . .
O26 O 0.1403(2) -0.1418(2) 0.41913(9) 0.0249(6) Uani 1 1 d . . . . .
V7 V 0.00809(5) 0.18712(5) 0.39781(2) 0.01743(12) Uani 1 1 d . . . . .
O27 O -0.0673(2) 0.1999(2) 0.43171(10) 0.0294(6) Uani 1 1 d . . . . .
V8 V 0.24985(5) 0.33012(4) 0.40722(2) 0.01792(12) Uani 1 1 d . . . . .
O28 O 0.2840(2) 0.4124(2) 0.44374(9) 0.0269(6) Uani 1 1 d . . . . .
V9 V 0.39439(5) 0.09613(5) 0.40119(3) 0.02642(15) Uani 1 1 d . . . . .
O29 O 0.4944(3) 0.0658(3) 0.43495(15) 0.0479(10) Uani 1 1 d . . . . .
V10 V 0.21558(5) 0.13126(5) 0.44075(2) 0.01897(12) Uani 1 1 d . . . . .
O30 O 0.2314(3) 0.1196(2) 0.49228(9) 0.0304(7) Uani 1 1 d . . . . .
O31 O 0.0941(2) 0.06907(19) 0.41378(8) 0.0180(5) Uani 1 1 d . . . . .
O32 O 0.1407(2) 0.2471(2) 0.42363(8) 0.0192(5) Uani 1 1 d . . . . .
O33 O 0.3230(2) 0.2047(2) 0.42507(10) 0.0237(6) Uani 1 1 d . . . . .
O34 O 0.2764(2) 0.0244(2) 0.41641(9) 0.0207(5) Uani 1 1 d . . . . .
S5 S -0.07737(7) -0.00372(7) 0.34295(3) 0.01791(17) Uani 1 1 d . . . . .
O35 O 0.02664(19) -0.0480(2) 0.34234(8) 0.0206(5) Uani 1 1 d . . . . .
O36 O -0.0654(2) 0.1076(2) 0.34760(9) 0.0219(5) Uani 1 1 d . . . . .
O37 O -0.1207(2) -0.0445(2) 0.37859(9) 0.0283(6) Uani 1 1 d . . . . .
O38 O -0.1410(2) -0.0241(2) 0.30067(9) 0.0255(6) Uani 1 1 d . . . . .
S6 S 0.03201(7) 0.40378(7) 0.35997(3) 0.02085(18) Uani 1 1 d . . . . .
O39 O -0.0149(2) 0.3001(2) 0.35658(9) 0.0242(6) Uani 1 1 d . . . . .
O40 O 0.1458(2) 0.3900(2) 0.36121(9) 0.0221(5) Uani 1 1 d . . . . .
O41 O 0.0135(2) 0.4540(3) 0.39825(10) 0.0332(7) Uani 1 1 d . . . . .
O42 O -0.0086(2) 0.4554(2) 0.31955(10) 0.0317(7) Uani 1 1 d . . . . .
S7 S 0.44432(7) 0.30646(7) 0.36093(3) 0.02146(18) Uani 1 1 d . . . . .
O43 O 0.3385(2) 0.3455(2) 0.36256(9) 0.0238(6) Uani 1 1 d . . . . .
O44 O 0.4387(3) 0.1957(2) 0.36091(14) 0.0413(9) Uani 1 1 d . . . . .
O45 O 0.5147(3) 0.3436(3) 0.39802(12) 0.0463(9) Uani 1 1 d . . . . .
O46 O 0.4708(3) 0.3375(3) 0.32021(11) 0.0397(8) Uani 1 1 d . . . . .
S8 S 0.33570(7) -0.09097(7) 0.33827(3) 0.0252(2) Uani 1 1 d . . . . .
O47 O 0.3812(2) 0.0103(2) 0.34916(12) 0.0324(7) Uani 1 1 d . . . . .
O48 O 0.2238(2) -0.0862(2) 0.34189(9) 0.0259(6) Uani 1 1 d . . . . .
O49 O 0.3878(2) -0.1636(2) 0.36900(12) 0.0349(7) Uani 1 1 d . . . . .
O50 O 0.3423(3) -0.1120(3) 0.29385(12) 0.0476(9) Uani 1 1 d . . . . .
N6 N -0.1229(3) -0.1561(3) 0.45434(12) 0.0338(8) Uani 1 1 d D . . . .
H6 H -0.109(4) -0.126(4) 0.4302(14) 0.041 Uiso 1 1 d D U . . .
C31 C -0.2362(4) -0.1747(4) 0.44571(18) 0.0410(11) Uani 1 1 d D . . . .
H31A H -0.2545 -0.2156 0.4695 0.049 Uiso 1 1 calc R U . . .
H31B H -0.2550 -0.2132 0.4185 0.049 Uiso 1 1 calc R U . . .
C32 C -0.2971(5) -0.0782(5) 0.4420(2) 0.0545(15) Uani 1 1 d D . . . .
H32A H -0.2917 -0.0477 0.4707 0.082 Uiso 1 1 calc R U . . .
H32B H -0.3693 -0.0924 0.4301 0.082 Uiso 1 1 calc R U . . .
H32C H -0.2696 -0.0320 0.4226 0.082 Uiso 1 1 calc R U . . .
C33 C -0.0637(4) -0.2514(4) 0.45231(18) 0.0423(12) Uani 1 1 d D . . . .
H33A H -0.0854 -0.3007 0.4724 0.051 Uiso 1 1 calc R U . . .
H33B H 0.0102 -0.2377 0.4624 0.051 Uiso 1 1 calc R U . . .
C34 C -0.0779(5) -0.2967(4) 0.4077(2) 0.0574(16) Uani 1 1 d D . . . .
H34A H -0.1507 -0.3122 0.3977 0.086 Uiso 1 1 calc R U . . .
H34B H -0.0374 -0.3583 0.4087 0.086 Uiso 1 1 calc R U . . .
H34C H -0.0549 -0.2492 0.3877 0.086 Uiso 1 1 calc R U . . .
C35 C -0.0870(4) -0.1040(4) 0.49711(15) 0.0432(12) Uani 1 1 d D . . . .
H35A H -0.1458 -0.0689 0.5059 0.052 Uiso 1 1 calc R U . . .
H35B H -0.0618 -0.1546 0.5196 0.052 Uiso 1 1 calc R U . . .
C36 C -0.0049(4) -0.0316(5) 0.49495(17) 0.0469(13) Uani 1 1 d D . . . .
H36A H 0.0532 -0.0657 0.4859 0.070 Uiso 1 1 calc R U . . .
H36B H 0.0176 -0.0015 0.5236 0.070 Uiso 1 1 calc R U . . .
H36C H -0.0306 0.0209 0.4739 0.070 Uiso 1 1 calc R U . . .
N7 N -0.3610(3) -0.0239(4) 0.28764(13) 0.0422(10) Uani 1 1 d D . . . .
H7 H -0.2845 -0.0193 0.2916 0.051 Uiso 0.623(11) 1 calc R U P D 1
H7X H -0.2846 -0.0176 0.2917 0.051 Uiso 0.377(11) 1 calc R U P D 2
C37 C -0.4004(10) -0.0528(12) 0.2424(3) 0.106(7) Uani 0.623(11) 1 d D . P D 1
H37A H -0.3793 -0.1226 0.2384 0.128 Uiso 0.623(11) 1 calc R U P D 1
H37B H -0.4763 -0.0516 0.2377 0.128 Uiso 0.623(11) 1 calc R U P D 1
C38 C -0.3673(12) 0.0089(9) 0.2092(3) 0.154(6) Uani 1 1 d D . . . .
H38A H -0.3977 -0.0167 0.1804 0.231 Uiso 0.623(11) 1 calc R U P D 1
H38B H -0.3896 0.0781 0.2120 0.231 Uiso 0.623(11) 1 calc R U P D 1
H38C H -0.2922 0.0068 0.2127 0.231 Uiso 0.623(11) 1 calc R U P D 1
H38D H -0.4014 0.0492 0.1846 0.231 Uiso 0.377(11) 1 calc R U P D 2
H38E H -0.2934 0.0227 0.2144 0.231 Uiso 0.377(11) 1 calc R U P D 2
H38F H -0.3790 -0.0622 0.2025 0.231 Uiso 0.377(11) 1 calc R U P D 2
C39 C -0.3869(9) -0.0993(8) 0.3189(4) 0.080(4) Uani 0.623(11) 1 d D . P D 1
H39A H -0.4619 -0.1110 0.3128 0.096 Uiso 0.623(11) 1 calc R U P D 1
H39B H -0.3691 -0.0715 0.3486 0.096 Uiso 0.623(11) 1 calc R U P D 1
C40 C -0.3326(6) -0.1984(5) 0.3176(2) 0.0633(17) Uani 1 1 d D . . . .
H40A H -0.3533 -0.2440 0.3390 0.095 Uiso 0.623(11) 1 calc R U P D 1
H40B H -0.3512 -0.2276 0.2886 0.095 Uiso 0.623(11) 1 calc R U P D 1
H40C H -0.2582 -0.1880 0.3245 0.095 Uiso 0.623(11) 1 calc R U P D 1
H40D H -0.3518 -0.2688 0.3126 0.095 Uiso 0.377(11) 1 calc R U P D 2
H40E H -0.2585 -0.1909 0.3192 0.095 Uiso 0.377(11) 1 calc R U P D 2
H40F H -0.3511 -0.1763 0.3450 0.095 Uiso 0.377(11) 1 calc R U P D 2
C41 C -0.4014(7) 0.0773(8) 0.2992(3) 0.058(3) Uani 0.623(11) 1 d D . P D 1
H41A H -0.3974 0.1250 0.2754 0.070 Uiso 0.623(11) 1 calc R U P D 1
H41B H -0.4746 0.0701 0.3015 0.070 Uiso 0.623(11) 1 calc R U P D 1
C42 C -0.3457(4) 0.1193(5) 0.3398(2) 0.0503(13) Uani 1 1 d D . . . .
H42A H -0.3756 0.1841 0.3452 0.075 Uiso 0.623(11) 1 calc R U P D 1
H42B H -0.3507 0.0735 0.3637 0.075 Uiso 0.623(11) 1 calc R U P D 1
H42C H -0.2733 0.1284 0.3376 0.075 Uiso 0.623(11) 1 calc R U P D 1
H42D H -0.3716 0.1433 0.3653 0.075 Uiso 0.377(11) 1 calc R U P D 2
H42E H -0.2709 0.1115 0.3471 0.075 Uiso 0.377(11) 1 calc R U P D 2
H42F H -0.3629 0.1677 0.3161 0.075 Uiso 0.377(11) 1 calc R U P D 2
C37X C -0.4078(14) 0.0338(13) 0.2468(4) 0.065(6) Uani 0.377(11) 1 d D . P D 2
H37C H -0.4828 0.0214 0.2407 0.078 Uiso 0.377(11) 1 calc R U P D 2
H37D H -0.3973 0.1062 0.2526 0.078 Uiso 0.377(11) 1 calc R U P D 2
C39X C -0.3891(10) -0.1353(9) 0.2808(4) 0.042(4) Uani 0.377(11) 1 d D . P D 2
H39C H -0.4641 -0.1437 0.2790 0.050 Uiso 0.377(11) 1 calc R U P D 2
H39D H -0.3713 -0.1583 0.2531 0.050 Uiso 0.377(11) 1 calc R U P D 2
C41X C -0.3945(13) 0.0191(11) 0.3257(5) 0.055(5) Uani 0.377(11) 1 d D . P D 2
H41C H -0.3782 -0.0287 0.3501 0.066 Uiso 0.377(11) 1 calc R U P D 2
H41D H -0.4700 0.0275 0.3192 0.066 Uiso 0.377(11) 1 calc R U P D 2
N8 N -0.1841(5) 0.3801(5) 0.26991(16) 0.0699(15) Uani 1 1 d D U . . .
H8 H -0.1162 0.3990 0.2876 0.084 Uiso 0.565(9) 1 calc R U P E 1
H8X H -0.1092 0.3903 0.2810 0.084 Uiso 0.435(9) 1 calc R U P E 2
C43 C -0.2493(8) 0.3468(9) 0.2976(4) 0.055(2) Uani 0.565(9) 1 d D U P E 1
H43A H -0.2152 0.2957 0.3182 0.066 Uiso 0.565(9) 1 calc R U P E 1
H43B H -0.3137 0.3186 0.2810 0.066 Uiso 0.565(9) 1 calc R U P E 1
C44 C -0.2696(9) 0.4402(10) 0.3208(4) 0.054(3) Uani 0.565(9) 1 d D U P E 1
H44A H -0.3151 0.4251 0.3413 0.082 Uiso 0.565(9) 1 calc R U P E 1
H44B H -0.2046 0.4671 0.3366 0.082 Uiso 0.565(9) 1 calc R U P E 1
H44C H -0.3023 0.4898 0.2997 0.082 Uiso 0.565(9) 1 calc R U P E 1
C45 C -0.2174(13) 0.4613(13) 0.2349(4) 0.070(4) Uani 0.565(9) 1 d D U P E 1
H45A H -0.2843 0.4428 0.2171 0.084 Uiso 0.565(9) 1 calc R U P E 1
H45B H -0.2258 0.5262 0.2491 0.084 Uiso 0.565(9) 1 calc R U P E 1
C46 C -0.1384(17) 0.472(2) 0.2063(6) 0.119(8) Uani 0.565(9) 1 d D U P E 1
H46A H -0.1604 0.5233 0.1844 0.179 Uiso 0.565(9) 1 calc R U P E 1
H46B H -0.0724 0.4910 0.2240 0.179 Uiso 0.565(9) 1 calc R U P E 1
H46C H -0.1308 0.4078 0.1920 0.179 Uiso 0.565(9) 1 calc R U P E 1
C47 C -0.1667(15) 0.3071(12) 0.2338(4) 0.106(4) Uani 0.565(9) 1 d D U P E 1
H47A H -0.2321 0.2845 0.2160 0.128 Uiso 0.565(9) 1 calc R U P E 1
H47B H -0.1222 0.3363 0.2149 0.128 Uiso 0.565(9) 1 calc R U P E 1
C48 C -0.1220(8) 0.2376(12) 0.2575(3) 0.069(3) Uani 0.565(9) 1 d D U P E 1
H48A H -0.1048 0.1832 0.2391 0.104 Uiso 0.565(9) 1 calc R U P E 1
H48B H -0.0589 0.2636 0.2753 0.104 Uiso 0.565(9) 1 calc R U P E 1
H48C H -0.1676 0.2123 0.2764 0.104 Uiso 0.565(9) 1 calc R U P E 1
C43X C -0.2611(17) 0.4274(16) 0.3014(6) 0.089(5) Uani 0.435(9) 1 d D U P E 2
H43C H -0.3327 0.4170 0.2863 0.107 Uiso 0.435(9) 1 calc R U P E 2
H43D H -0.2519 0.3865 0.3282 0.107 Uiso 0.435(9) 1 calc R U P E 2
C44X C -0.2511(19) 0.5348(18) 0.3149(9) 0.118(8) Uani 0.435(9) 1 d D U P E 2
H44D H -0.3017 0.5503 0.3332 0.177 Uiso 0.435(9) 1 calc R U P E 2
H44E H -0.1818 0.5469 0.3313 0.177 Uiso 0.435(9) 1 calc R U P E 2
H44F H -0.2632 0.5776 0.2891 0.177 Uiso 0.435(9) 1 calc R U P E 2
C45X C -0.2222(15) 0.4268(12) 0.2283(4) 0.043(3) Uani 0.435(9) 1 d D U P E 2
H45C H -0.2517 0.4928 0.2334 0.052 Uiso 0.435(9) 1 calc R U P E 2
H45D H -0.2782 0.3850 0.2123 0.052 Uiso 0.435(9) 1 calc R U P E 2
C46X C -0.1429(11) 0.4410(10) 0.2010(5) 0.028(2) Uiso 0.435(9) 1 d D U P E 2
H46D H -0.1740 0.4727 0.1735 0.042 Uiso 0.435(9) 1 calc R U P E 2
H46E H -0.0879 0.4837 0.2162 0.042 Uiso 0.435(9) 1 calc R U P E 2
H46F H -0.1144 0.3758 0.1950 0.042 Uiso 0.435(9) 1 calc R U P E 2
C47X C -0.2177(14) 0.2778(10) 0.2701(6) 0.075(4) Uani 0.435(9) 1 d D U P E 2
H47C H -0.2936 0.2801 0.2627 0.090 Uiso 0.435(9) 1 calc R U P E 2
H47D H -0.2009 0.2558 0.3008 0.090 Uiso 0.435(9) 1 calc R U P E 2
C48X C -0.1868(15) 0.1968(12) 0.2450(4) 0.069(4) Uani 0.435(9) 1 d D U P E 2
H48D H -0.2212 0.1350 0.2514 0.104 Uiso 0.435(9) 1 calc R U P E 2
H48E H -0.2060 0.2123 0.2141 0.104 Uiso 0.435(9) 1 calc R U P E 2
H48F H -0.1123 0.1878 0.2525 0.104 Uiso 0.435(9) 1 calc R U P E 2
N9 N 0.6527(3) 0.3003(4) 0.47108(15) 0.0497(12) Uani 1 1 d D . . . .
H9 H 0.604(4) 0.314(5) 0.4461(15) 0.060 Uiso 1 1 d D U . . .
C49 C 0.5941(6) 0.2795(10) 0.5084(2) 0.107(4) Uani 1 1 d D . . . .
H49A H 0.5673 0.2103 0.5057 0.129 Uiso 1 1 calc R U . . .
H49B H 0.6426 0.2845 0.5364 0.129 Uiso 1 1 calc R U . . .
C50 C 0.5111(8) 0.3465(9) 0.5091(3) 0.112(4) Uani 1 1 d D . . . .
H50A H 0.4771 0.3296 0.5334 0.168 Uiso 1 1 calc R U . . .
H50B H 0.5372 0.4151 0.5125 0.168 Uiso 1 1 calc R U . . .
H50C H 0.4619 0.3408 0.4818 0.168 Uiso 1 1 calc R U . . .
C51 C 0.7040(5) 0.2065(4) 0.4638(2) 0.0607(17) Uani 1 1 d D . . . .
H51A H 0.7421 0.2166 0.4397 0.073 Uiso 1 1 calc R U . . .
H51B H 0.6511 0.1549 0.4545 0.073 Uiso 1 1 calc R U . . .
C52 C 0.7770(5) 0.1683(5) 0.5023(2) 0.0592(16) Uani 1 1 d D . . . .
H52A H 0.8079 0.1057 0.4948 0.089 Uiso 1 1 calc R U . . .
H52B H 0.8310 0.2180 0.5114 0.089 Uiso 1 1 calc R U . . .
H52C H 0.7398 0.1562 0.5261 0.089 Uiso 1 1 calc R U . . .
C53 C 0.7129(7) 0.3901(5) 0.4781(2) 0.082(3) Uani 1 1 d D . . . .
H53A H 0.7702 0.3800 0.5028 0.098 Uiso 1 1 calc R U . . .
H53B H 0.6697 0.4455 0.4856 0.098 Uiso 1 1 calc R U . . .
C54 C 0.7563(5) 0.4181(7) 0.4375(2) 0.074(2) Uani 1 1 d D . . . .
H54A H 0.7971 0.4795 0.4430 0.110 Uiso 1 1 calc R U . . .
H54B H 0.7999 0.3637 0.4303 0.110 Uiso 1 1 calc R U . . .
H54C H 0.6996 0.4291 0.4131 0.110 Uiso 1 1 calc R U . . .
N10 N 0.3763(4) -0.3679(3) 0.35557(17) 0.0447(11) Uani 1 1 d D . . . .
H10 H 0.386(5) -0.302(3) 0.361(2) 0.054 Uiso 1 1 d D U . . .
C55 C 0.4244(5) -0.4084(4) 0.3999(3) 0.0651(19) Uani 1 1 d . . . . .
H55A H 0.4247 -0.4824 0.3991 0.078 Uiso 1 1 calc R U . . .
H55B H 0.3830 -0.3871 0.4216 0.078 Uiso 1 1 calc R U . . .
C56 C 0.5345(6) -0.3699(7) 0.4133(4) 0.116(4) Uani 1 1 d . . . . .
H56A H 0.5800 -0.4073 0.3977 0.174 Uiso 1 1 calc R U . . .
H56B H 0.5570 -0.3792 0.4446 0.174 Uiso 1 1 calc R U . . .
H56C H 0.5369 -0.2987 0.4062 0.174 Uiso 1 1 calc R U . . .
C57 C 0.4359(7) -0.3989(5) 0.3221(4) 0.104(4) Uani 1 1 d . . . . .
H57A H 0.4357 -0.4728 0.3200 0.124 Uiso 1 1 calc R U . . .
H57B H 0.5079 -0.3766 0.3308 0.124 Uiso 1 1 calc R U . . .
C58 C 0.3911(11) -0.3548(6) 0.2781(3) 0.145(6) Uani 1 1 d . . . . .
H58A H 0.3284 -0.3911 0.2656 0.217 Uiso 1 1 calc R U . . .
H58B H 0.4412 -0.3607 0.2588 0.217 Uiso 1 1 calc R U . . .
H58C H 0.3748 -0.2840 0.2815 0.217 Uiso 1 1 calc R U . . .
C59 C 0.2668(5) -0.3985(4) 0.3447(2) 0.0501(13) Uani 1 1 d . . . . .
H59A H 0.2377 -0.3730 0.3155 0.060 Uiso 1 1 calc R U . . .
H59B H 0.2636 -0.4725 0.3435 0.060 Uiso 1 1 calc R U . . .
C60 C 0.2015(4) -0.3633(4) 0.3754(2) 0.0473(13) Uani 1 1 d . . . . .
H60A H 0.2186 -0.4008 0.4027 0.071 Uiso 1 1 calc R U . . .
H60B H 0.1291 -0.3741 0.3628 0.071 Uiso 1 1 calc R U . . .
H60C H 0.2136 -0.2919 0.3812 0.071 Uiso 1 1 calc R U . . .
O51 O 0.4922(3) 0.4274(3) 0.24104(13) 0.0569(10) Uani 1 1 d . . . . .
O52 O 0.6010(8) 0.6139(7) 0.2468(3) 0.144(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.590(3) . ?
V1 O9 1.948(3) . ?
V1 O6 1.968(3) . ?
V1 O23 1.986(3) . ?
V1 O10 1.993(3) . ?
V1 V5 2.9044(9) . ?
V2 O2 1.584(3) . ?
V2 O7 1.959(3) . ?
V2 O6 1.960(3) . ?
V2 O14 1.977(3) . ?
V2 O11 1.991(3) . ?
V2 V5 2.9058(9) . ?
V3 O3 1.592(3) . ?
V3 O8 1.953(3) . ?
V3 O7 1.958(3) . ?
V3 O18 1.977(3) . ?
V3 O15 1.995(3) . ?
V3 V5 2.9240(9) . ?
V4 O4 1.588(3) . ?
V4 O8 1.957(3) . ?
V4 O9 1.964(3) . ?
V4 O19 1.982(3) . ?
V4 O22 1.986(3) . ?
V4 V5 2.9252(9) . ?
V5 O5 1.601(3) . ?
V5 O6 1.863(3) . ?
V5 O9 1.865(3) . ?
V5 O7 1.868(3) . ?
V5 O8 1.872(3) . ?
S1 O12 1.447(3) . ?
S1 O13 1.454(3) . ?
S1 O10 1.496(3) . ?
S1 O11 1.506(3) . ?
S2 O17 1.441(3) . ?
S2 O16 1.453(3) . ?
S2 O14 1.508(3) . ?
S2 O15 1.510(3) . ?
S3 O20 1.431(5) . ?
S3 O21 1.441(4) . ?
S3 O19 1.511(3) . ?
S3 O18 1.518(3) . ?
S4 O24 1.446(3) . ?
S4 O25 1.451(3) . ?
S4 O22 1.505(3) . ?
S4 O23 1.506(3) . ?
N1 C5X 1.445(15) . ?
N1 C3 1.478(7) . ?
N1 C5 1.505(7) . ?
N1 C1X 1.509(15) . ?
N1 C3X 1.529(15) . ?
N1 C1 1.533(8) . ?
N1 H1 1.0000 . ?
N1 H1X 1.0000 . ?
C1 C2 1.577(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C1X 1.596(17) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C2 H2F 0.9800 . ?
C3 C4 1.551(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C3X 1.545(16) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
C4 H4F 0.9800 . ?
C5 C6 1.524(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C5X 1.587(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6D 0.9800 . ?
C6 H6E 0.9800 . ?
C6 H6F 0.9800 . ?
C1X H1C 0.9900 . ?
C1X H1D 0.9900 . ?
C3X H3C 0.9900 . ?
C3X H3D 0.9900 . ?
C5X H5C 0.9900 . ?
C5X H5D 0.9900 . ?
N2 C7 1.494(7) . ?
N2 C11 1.498(6) . ?
N2 C9 1.535(7) . ?
N2 H2 0.91(3) . ?
C7 C8 1.530(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.492(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.501(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N3 C15 1.486(7) . ?
N3 C17 1.489(7) . ?
N3 C13 1.520(10) . ?
N3 C13X 1.563(14) . ?
N3 H3 1.0000 . ?
N3 H3X 1.0000 . ?
C13 C14 1.517(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.512(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.500(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C13X C14X 1.503(18) . ?
C13X H13C 0.9900 . ?
C13X H13D 0.9900 . ?
C14X H14D 0.9800 . ?
C14X H14E 0.9800 . ?
C14X H14F 0.9800 . ?
N4 C19 1.499(13) . ?
N4 C23 1.508(14) . ?
N4 C21 1.509(12) . ?
N4 H4 1.0000 . ?
C19 C20 1.501(13) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.487(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.500(16) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N4X C19X 1.485(12) . ?
N4X C21X 1.492(17) . ?
N4X C23X 1.534(19) . ?
N4X H4X 1.0000 . ?
C19X C20X 1.509(14) . ?
C19X H19C 0.9900 . ?
C19X H19D 0.9900 . ?
C20X H20D 0.9800 . ?
C20X H20E 0.9800 . ?
C20X H20F 0.9800 . ?
C21X C22X 1.468(16) . ?
C21X H21C 0.9900 . ?
C21X H21D 0.9900 . ?
C22X H22D 0.9800 . ?
C22X H22E 0.9800 . ?
C22X H22F 0.9800 . ?
C23X C24X 1.480(18) . ?
C23X H23C 0.9900 . ?
C23X H23D 0.9900 . ?
C24X H24D 0.9800 . ?
C24X H24E 0.9800 . ?
C24X H24F 0.9800 . ?
N5 C25 1.488(7) . ?
N5 C27 1.507(6) . ?
N5 C29 1.510(6) . ?
N5 H5 0.83(3) . ?
C25 C26 1.478(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.536(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.513(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
V6 O26 1.590(3) . ?
V6 O31 1.951(3) . ?
V6 O34 1.966(3) . ?
V6 O48 1.979(3) . ?
V6 O35 2.008(3) . ?
V6 V10 2.9205(9) . ?
V7 O27 1.594(3) . ?
V7 O31 1.958(3) . ?
V7 O32 1.967(3) . ?
V7 O39 1.975(3) . ?
V7 O36 2.000(3) . ?
V7 V10 2.9293(9) . ?
V8 O28 1.593(3) . ?
V8 O32 1.963(3) . ?
V8 O33 1.966(3) . ?
V8 O40 1.975(3) . ?
V8 O43 1.995(3) . ?
V8 V10 2.9242(9) . ?
V9 O29 1.591(3) . ?
V9 O33 1.954(3) . ?
V9 O34 1.965(3) . ?
V9 O47 1.976(3) . ?
V9 O44 1.995(3) . ?
V9 V10 2.9040(10) . ?
V10 O30 1.599(3) . ?
V10 O32 1.864(3) . ?
V10 O33 1.866(3) . ?
V10 O34 1.869(3) . ?
V10 O31 1.871(3) . ?
S5 O37 1.452(3) . ?
S5 O38 1.462(3) . ?
S5 O36 1.501(3) . ?
S5 O35 1.503(3) . ?
S6 O41 1.435(3) . ?
S6 O42 1.458(3) . ?
S6 O40 1.511(3) . ?
S6 O39 1.515(3) . ?
S7 O45 1.441(3) . ?
S7 O46 1.445(3) . ?
S7 O44 1.482(3) . ?
S7 O43 1.504(3) . ?
S8 O50 1.439(4) . ?
S8 O49 1.451(3) . ?
S8 O47 1.496(3) . ?
S8 O48 1.508(3) . ?
N6 C31 1.496(6) . ?
N6 C33 1.504(6) . ?
N6 C35 1.510(6) . ?
N6 H6 0.90(3) . ?
C31 C32 1.515(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.505(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.466(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N7 C41X 1.463(12) . ?
N7 C37 1.471(10) . ?
N7 C39 1.490(11) . ?
N7 C41 1.523(10) . ?
N7 C37X 1.526(12) . ?
N7 C39X 1.541(12) . ?
N7 H7 1.0000 . ?
N7 H7X 1.0000 . ?
C37 C38 1.458(16) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C37X 1.423(16) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 H38D 0.9800 . ?
C38 H38E 0.9800 . ?
C38 H38F 0.9800 . ?
C39 C40 1.512(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C39X 1.514(13) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 H40D 0.9800 . ?
C40 H40E 0.9800 . ?
C40 H40F 0.9800 . ?
C41 C42 1.461(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C41X 1.518(13) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 H42D 0.9800 . ?
C42 H42E 0.9800 . ?
C42 H42F 0.9800 . ?
C37X H37C 0.9900 . ?
C37X H37D 0.9900 . ?
C39X H39C 0.9900 . ?
C39X H39D 0.9900 . ?
C41X H41C 0.9900 . ?
C41X H41D 0.9900 . ?
N8 C43 1.404(10) . ?
N8 C47X 1.439(14) . ?
N8 C45X 1.451(14) . ?
N8 C47 1.543(14) . ?
N8 C45 1.549(13) . ?
N8 C43X 1.667(16) . ?
N8 H8 1.0000 . ?
N8 H8X 1.0000 . ?
C43 C44 1.494(15) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.504(15) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.267(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C43X C44X 1.50(2) . ?
C43X H43C 0.9900 . ?
C43X H43D 0.9900 . ?
C44X H44D 0.9800 . ?
C44X H44E 0.9800 . ?
C44X H44F 0.9800 . ?
C45X C46X 1.484(15) . ?
C45X H45C 0.9900 . ?
C45X H45D 0.9900 . ?
C46X H46D 0.9800 . ?
C46X H46E 0.9800 . ?
C46X H46F 0.9800 . ?
C47X C48X 1.442(16) . ?
C47X H47C 0.9900 . ?
C47X H47D 0.9900 . ?
C48X H48D 0.9800 . ?
C48X H48E 0.9800 . ?
C48X H48F 0.9800 . ?
N9 C53 1.436(8) . ?
N9 C51 1.464(8) . ?
N9 C49 1.543(8) . ?
N9 H9 0.94(4) . ?
C49 C50 1.420(11) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.494(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.537(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N10 C57 1.482(8) . ?
N10 C59 1.485(7) . ?
N10 C55 1.521(9) . ?
N10 H10 0.90(4) . ?
C55 C56 1.531(10) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.520(15) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.482(8) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O9 108.07(14) . . ?
O1 V1 O6 107.70(14) . . ?
O9 V1 O6 78.63(11) . . ?
O1 V1 O23 108.15(15) . . ?
O9 V1 O23 88.20(12) . . ?
O6 V1 O23 144.08(12) . . ?
O1 V1 O10 109.05(15) . . ?
O9 V1 O10 142.70(12) . . ?
O6 V1 O10 86.89(11) . . ?
O23 V1 O10 83.73(12) . . ?
O1 V1 V5 111.45(12) . . ?
O9 V1 V5 39.34(8) . . ?
O6 V1 V5 39.37(7) . . ?
O23 V1 V5 121.42(9) . . ?
O10 V1 V5 119.87(9) . . ?
O2 V2 O7 107.17(14) . . ?
O2 V2 O6 110.09(14) . . ?
O7 V2 O6 78.72(11) . . ?
O2 V2 O14 108.79(14) . . ?
O7 V2 O14 87.74(12) . . ?
O6 V2 O14 141.05(12) . . ?
O2 V2 O11 107.44(14) . . ?
O7 V2 O11 145.28(12) . . ?
O6 V2 O11 86.95(11) . . ?
O14 V2 O11 83.84(11) . . ?
O2 V2 V5 113.11(11) . . ?
O7 V2 V5 39.45(8) . . ?
O6 V2 V5 39.30(8) . . ?
O14 V2 V5 119.44(9) . . ?
O11 V2 V5 120.53(9) . . ?
O3 V3 O8 107.46(16) . . ?
O3 V3 O7 108.49(16) . . ?
O8 V3 O7 78.13(11) . . ?
O3 V3 O18 108.78(18) . . ?
O8 V3 O18 89.37(13) . . ?
O7 V3 O18 142.69(14) . . ?
O3 V3 O15 109.34(16) . . ?
O8 V3 O15 143.15(13) . . ?
O7 V3 O15 88.55(12) . . ?
O18 V3 O15 80.70(13) . . ?
O3 V3 V5 112.10(15) . . ?
O8 V3 V5 39.12(8) . . ?
O7 V3 V5 39.04(8) . . ?
O18 V3 V5 121.25(9) . . ?
O15 V3 V5 120.77(9) . . ?
O4 V4 O8 107.84(14) . . ?
O4 V4 O9 107.54(15) . . ?
O8 V4 O9 78.06(11) . . ?
O4 V4 O19 108.79(16) . . ?
O8 V4 O19 88.37(12) . . ?
O9 V4 O19 143.56(13) . . ?
O4 V4 O22 109.54(14) . . ?
O8 V4 O22 142.48(12) . . ?
O9 V4 O22 87.78(11) . . ?
O19 V4 O22 82.76(12) . . ?
O4 V4 V5 112.22(12) . . ?
O8 V4 V5 39.11(8) . . ?
O9 V4 V5 38.96(8) . . ?
O19 V4 V5 120.55(9) . . ?
O22 V4 V5 119.52(9) . . ?
O5 V5 O6 110.09(14) . . ?
O5 V5 O9 110.77(15) . . ?
O6 V5 O9 83.42(12) . . ?
O5 V5 O7 110.48(14) . . ?
O6 V5 O7 83.53(12) . . ?
O9 V5 O7 138.74(12) . . ?
O5 V5 O8 110.27(14) . . ?
O6 V5 O8 139.64(12) . . ?
O9 V5 O8 82.71(12) . . ?
O7 V5 O8 82.43(12) . . ?
O5 V5 V1 115.77(12) . . ?
O6 V5 V1 42.06(8) . . ?
O9 V5 V1 41.44(8) . . ?
O7 V5 V1 117.02(9) . . ?
O8 V5 V1 116.36(9) . . ?
O5 V5 V2 116.29(11) . . ?
O6 V5 V2 41.79(8) . . ?
O9 V5 V2 116.26(9) . . ?
O7 V5 V2 41.77(8) . . ?
O8 V5 V2 115.92(9) . . ?
V1 V5 V2 79.44(2) . . ?
O5 V5 V3 116.14(12) . . ?
O6 V5 V3 116.58(8) . . ?
O9 V5 V3 115.46(9) . . ?
O7 V5 V3 41.30(8) . . ?
O8 V5 V3 41.17(9) . . ?
V1 V5 V3 128.09(3) . . ?
V2 V5 V3 78.80(2) . . ?
O5 V5 V4 116.96(11) . . ?
O6 V5 V4 116.20(8) . . ?
O9 V5 V4 41.45(8) . . ?
O7 V5 V4 114.93(9) . . ?
O8 V5 V4 41.28(9) . . ?
V1 V5 V4 78.67(2) . . ?
V2 V5 V4 126.75(3) . . ?
V3 V5 V4 77.86(2) . . ?
V5 O6 V2 98.91(12) . . ?
V5 O6 V1 98.57(12) . . ?
V2 O6 V1 141.92(14) . . ?
V5 O7 V3 99.66(12) . . ?
V5 O7 V2 98.77(12) . . ?
V3 O7 V2 141.75(15) . . ?
V5 O8 V3 99.71(13) . . ?
V5 O8 V4 99.61(13) . . ?
V3 O8 V4 140.09(16) . . ?
V5 O9 V1 99.21(12) . . ?
V5 O9 V4 99.60(12) . . ?
V1 O9 V4 141.73(15) . . ?
O12 S1 O13 113.3(2) . . ?
O12 S1 O10 110.52(18) . . ?
O13 S1 O10 108.18(18) . . ?
O12 S1 O11 110.31(19) . . ?
O13 S1 O11 106.70(17) . . ?
O10 S1 O11 107.60(17) . . ?
S1 O10 V1 128.67(17) . . ?
S1 O11 V2 129.80(17) . . ?
O17 S2 O16 113.55(19) . . ?
O17 S2 O14 107.83(18) . . ?
O16 S2 O14 109.53(18) . . ?
O17 S2 O15 108.74(19) . . ?
O16 S2 O15 109.26(18) . . ?
O14 S2 O15 107.76(17) . . ?
S2 O14 V2 129.53(17) . . ?
S2 O15 V3 129.31(18) . . ?
O20 S3 O21 114.7(3) . . ?
O20 S3 O19 110.7(2) . . ?
O21 S3 O19 107.2(2) . . ?
O20 S3 O18 111.0(2) . . ?
O21 S3 O18 106.6(2) . . ?
O19 S3 O18 106.11(18) . . ?
S3 O18 V3 130.2(2) . . ?
S3 O19 V4 131.8(2) . . ?
O24 S4 O25 113.5(2) . . ?
O24 S4 O22 109.42(19) . . ?
O25 S4 O22 107.52(17) . . ?
O24 S4 O23 110.68(19) . . ?
O25 S4 O23 107.80(19) . . ?
O22 S4 O23 107.77(17) . . ?
S4 O22 V4 130.70(17) . . ?
S4 O23 V1 132.10(19) . . ?
C3 N1 C5 111.4(4) . . ?
C5X N1 C1X 118.5(10) . . ?
C5X N1 C3X 112.7(10) . . ?
C1X N1 C3X 107.3(10) . . ?
C3 N1 C1 110.8(4) . . ?
C5 N1 C1 108.5(5) . . ?
C3 N1 H1 108.7 . . ?
C5 N1 H1 108.7 . . ?
C1 N1 H1 108.7 . . ?
C5X N1 H1X 105.8 . . ?
C1X N1 H1X 105.8 . . ?
C3X N1 H1X 105.8 . . ?
N1 C1 C2 108.5(6) . . ?
N1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
N1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1X C2 H2D 109.5 . . ?
C1X C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
C1X C2 H2F 109.5 . . ?
H2D C2 H2F 109.5 . . ?
H2E C2 H2F 109.5 . . ?
N1 C3 C4 111.8(5) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3X C4 H4D 109.5 . . ?
C3X C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
C3X C4 H4F 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
N1 C5 C6 111.5(5) . . ?
N1 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N1 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5X C6 H6D 109.5 . . ?
C5X C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
C5X C6 H6F 109.5 . . ?
H6D C6 H6F 109.5 . . ?
H6E C6 H6F 109.5 . . ?
N1 C1X C2 108.8(11) . . ?
N1 C1X H1C 109.9 . . ?
C2 C1X H1C 109.9 . . ?
N1 C1X H1D 109.9 . . ?
C2 C1X H1D 109.9 . . ?
H1C C1X H1D 108.3 . . ?
N1 C3X C4 109.5(10) . . ?
N1 C3X H3C 109.8 . . ?
C4 C3X H3C 109.8 . . ?
N1 C3X H3D 109.8 . . ?
C4 C3X H3D 109.8 . . ?
H3C C3X H3D 108.2 . . ?
N1 C5X C6 111.3(10) . . ?
N1 C5X H5C 109.4 . . ?
C6 C5X H5C 109.4 . . ?
N1 C5X H5D 109.4 . . ?
C6 C5X H5D 109.4 . . ?
H5C C5X H5D 108.0 . . ?
C7 N2 C11 111.7(4) . . ?
C7 N2 C9 112.7(5) . . ?
C11 N2 C9 113.5(4) . . ?
C7 N2 H2 99(4) . . ?
C11 N2 H2 110(4) . . ?
C9 N2 H2 109(4) . . ?
N2 C7 C8 111.9(5) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 113.5(5) . . ?
C10 C9 H9A 108.9 . . ?
N2 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
N2 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 112.6(4) . . ?
N2 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 N3 C17 112.6(4) . . ?
C15 N3 C13 116.8(6) . . ?
C17 N3 C13 116.9(6) . . ?
C15 N3 C13X 101.2(9) . . ?
C17 N3 C13X 104.3(8) . . ?
C15 N3 H3 102.5 . . ?
C17 N3 H3 102.5 . . ?
C13 N3 H3 102.5 . . ?
C15 N3 H3X 112.6 . . ?
C17 N3 H3X 112.6 . . ?
C13X N3 H3X 112.6 . . ?
C14 C13 N3 111.6(7) . . ?
C14 C13 H13A 109.3 . . ?
N3 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
N3 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C16 113.5(5) . . ?
N3 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
N3 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 113.7(4) . . ?
N3 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
N3 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14X C13X N3 108.3(11) . . ?
C14X C13X H13C 110.0 . . ?
N3 C13X H13C 110.0 . . ?
C14X C13X H13D 110.0 . . ?
N3 C13X H13D 110.0 . . ?
H13C C13X H13D 108.4 . . ?
C13X C14X H14D 109.5 . . ?
C13X C14X H14E 109.5 . . ?
H14D C14X H14E 109.5 . . ?
C13X C14X H14F 109.5 . . ?
H14D C14X H14F 109.5 . . ?
H14E C14X H14F 109.5 . . ?
C19 N4 C23 114.2(9) . . ?
C19 N4 C21 109.3(10) . . ?
C23 N4 C21 113.3(9) . . ?
C19 N4 H4 106.5 . . ?
C23 N4 H4 106.5 . . ?
C21 N4 H4 106.5 . . ?
N4 C19 C20 111.8(9) . . ?
N4 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N4 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N4 113.8(9) . . ?
C22 C21 H21A 108.8 . . ?
N4 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
N4 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N4 113.0(11) . . ?
C24 C23 H23A 109.0 . . ?
N4 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
N4 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19X N4X C21X 111.9(10) . . ?
C19X N4X C23X 112.0(12) . . ?
C21X N4X C23X 112.5(11) . . ?
C19X N4X H4X 106.6 . . ?
C21X N4X H4X 106.6 . . ?
C23X N4X H4X 106.6 . . ?
N4X C19X C20X 113.1(9) . . ?
N4X C19X H19C 109.0 . . ?
C20X C19X H19C 109.0 . . ?
N4X C19X H19D 109.0 . . ?
C20X C19X H19D 109.0 . . ?
H19C C19X H19D 107.8 . . ?
C19X C20X H20D 109.5 . . ?
C19X C20X H20E 109.5 . . ?
H20D C20X H20E 109.5 . . ?
C19X C20X H20F 109.5 . . ?
H20D C20X H20F 109.5 . . ?
H20E C20X H20F 109.5 . . ?
C22X C21X N4X 118.2(14) . . ?
C22X C21X H21C 107.8 . . ?
N4X C21X H21C 107.8 . . ?
C22X C21X H21D 107.8 . . ?
N4X C21X H21D 107.8 . . ?
H21C C21X H21D 107.1 . . ?
C21X C22X H22D 109.5 . . ?
C21X C22X H22E 109.5 . . ?
H22D C22X H22E 109.5 . . ?
C21X C22X H22F 109.5 . . ?
H22D C22X H22F 109.5 . . ?
H22E C22X H22F 109.5 . . ?
C24X C23X N4X 114.2(13) . . ?
C24X C23X H23C 108.7 . . ?
N4X C23X H23C 108.7 . . ?
C24X C23X H23D 108.7 . . ?
N4X C23X H23D 108.7 . . ?
H23C C23X H23D 107.6 . . ?
C23X C24X H24D 109.5 . . ?
C23X C24X H24E 109.5 . . ?
H24D C24X H24E 109.5 . . ?
C23X C24X H24F 109.5 . . ?
H24D C24X H24F 109.5 . . ?
H24E C24X H24F 109.5 . . ?
C25 N5 C27 112.8(4) . . ?
C25 N5 C29 110.5(4) . . ?
C27 N5 C29 110.6(4) . . ?
C25 N5 H5 110(4) . . ?
C27 N5 H5 109(4) . . ?
C29 N5 H5 104(4) . . ?
C26 C25 N5 112.7(4) . . ?
C26 C25 H25A 109.0 . . ?
N5 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
N5 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 C28 113.0(5) . . ?
N5 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
N5 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 112.7(4) . . ?
N5 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
N5 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O26 V6 O31 108.52(13) . . ?
O26 V6 O34 107.23(13) . . ?
O31 V6 O34 78.33(11) . . ?
O26 V6 O48 110.15(14) . . ?
O31 V6 O48 141.27(12) . . ?
O34 V6 O48 88.25(12) . . ?
O26 V6 O35 105.99(14) . . ?
O31 V6 O35 87.82(11) . . ?
O34 V6 O35 146.57(12) . . ?
O48 V6 O35 83.82(11) . . ?
O26 V6 V10 111.94(11) . . ?
O31 V6 V10 39.18(8) . . ?
O34 V6 V10 39.19(8) . . ?
O48 V6 V10 119.84(9) . . ?
O35 V6 V10 121.72(8) . . ?
O27 V7 O31 108.76(14) . . ?
O27 V7 O32 107.60(15) . . ?
O31 V7 O32 77.79(11) . . ?
O27 V7 O39 108.26(15) . . ?
O31 V7 O39 142.88(12) . . ?
O32 V7 O39 88.75(12) . . ?
O27 V7 O36 107.94(15) . . ?
O31 V7 O36 87.16(11) . . ?
O32 V7 O36 144.23(12) . . ?
O39 V7 O36 84.01(12) . . ?
O27 V7 V10 111.69(12) . . ?
O31 V7 V10 39.01(8) . . ?
O32 V7 V10 38.86(8) . . ?
O39 V7 V10 121.09(9) . . ?
O36 V7 V10 120.55(8) . . ?
O28 V8 O32 109.17(14) . . ?
O28 V8 O33 108.83(14) . . ?
O32 V8 O33 77.96(11) . . ?
O28 V8 O40 108.37(14) . . ?
O32 V8 O40 88.34(11) . . ?
O33 V8 O40 142.76(12) . . ?
O28 V8 O43 107.89(14) . . ?
O32 V8 O43 142.86(12) . . ?
O33 V8 O43 88.00(12) . . ?
O40 V8 O43 82.38(11) . . ?
O28 V8 V10 114.29(11) . . ?
O32 V8 V10 38.95(8) . . ?
O33 V8 V10 39.02(8) . . ?
O40 V8 V10 119.85(9) . . ?
O43 V8 V10 119.70(9) . . ?
O29 V9 O33 109.66(18) . . ?
O29 V9 O34 108.50(17) . . ?
O33 V9 O34 78.92(12) . . ?
O29 V9 O47 109.89(19) . . ?
O33 V9 O47 140.45(13) . . ?
O34 V9 O47 87.83(12) . . ?
O29 V9 O44 106.64(19) . . ?
O33 V9 O44 88.00(13) . . ?
O34 V9 O44 144.83(14) . . ?
O47 V9 O44 81.77(14) . . ?
O29 V9 V10 113.70(17) . . ?
O33 V9 V10 39.41(8) . . ?
O34 V9 V10 39.55(8) . . ?
O47 V9 V10 119.32(9) . . ?
O44 V9 V10 121.23(9) . . ?
O30 V10 O32 109.72(14) . . ?
O30 V10 O33 110.58(15) . . ?
O32 V10 O33 82.99(12) . . ?
O30 V10 O34 110.55(15) . . ?
O32 V10 O34 139.73(12) . . ?
O33 V10 O34 83.63(12) . . ?
O30 V10 O31 110.95(15) . . ?
O32 V10 O31 82.54(12) . . ?
O33 V10 O31 138.47(12) . . ?
O34 V10 O31 82.80(12) . . ?
O30 V10 V9 116.65(12) . . ?
O32 V10 V9 116.33(9) . . ?
O33 V10 V9 41.67(9) . . ?
O34 V10 V9 42.00(9) . . ?
O31 V10 V9 115.84(8) . . ?
O30 V10 V6 116.68(12) . . ?
O32 V10 V6 115.79(9) . . ?
O33 V10 V6 116.35(9) . . ?
O34 V10 V6 41.64(8) . . ?
O31 V10 V6 41.20(8) . . ?
V9 V10 V6 79.01(2) . . ?
O30 V10 V8 116.86(12) . . ?
O32 V10 V8 41.46(8) . . ?
O33 V10 V8 41.54(9) . . ?
O34 V10 V8 116.19(9) . . ?
O31 V10 V8 114.72(8) . . ?
V9 V10 V8 78.56(2) . . ?
V6 V10 V8 126.45(3) . . ?
O30 V10 V7 115.43(12) . . ?
O32 V10 V7 41.44(8) . . ?
O33 V10 V7 116.17(9) . . ?
O34 V10 V7 116.40(9) . . ?
O31 V10 V7 41.19(8) . . ?
V9 V10 V7 127.92(3) . . ?
V6 V10 V7 78.53(2) . . ?
V8 V10 V7 78.27(2) . . ?
V10 O31 V6 99.62(12) . . ?
V10 O31 V7 99.80(12) . . ?
V6 O31 V7 142.59(14) . . ?
V10 O32 V8 99.59(12) . . ?
V10 O32 V7 99.71(13) . . ?
V8 O32 V7 140.12(14) . . ?
V10 O33 V9 98.92(13) . . ?
V10 O33 V8 99.44(13) . . ?
V9 O33 V8 140.53(17) . . ?
V10 O34 V9 98.45(12) . . ?
V10 O34 V6 99.17(12) . . ?
V9 O34 V6 141.03(15) . . ?
O37 S5 O38 112.61(18) . . ?
O37 S5 O36 110.32(18) . . ?
O38 S5 O36 107.86(17) . . ?
O37 S5 O35 110.67(17) . . ?
O38 S5 O35 107.11(16) . . ?
O36 S5 O35 108.09(16) . . ?
S5 O35 V6 128.68(16) . . ?
S5 O36 V7 129.14(16) . . ?
O41 S6 O42 114.5(2) . . ?
O41 S6 O40 110.88(18) . . ?
O42 S6 O40 106.80(18) . . ?
O41 S6 O39 110.85(19) . . ?
O42 S6 O39 106.87(17) . . ?
O40 S6 O39 106.55(16) . . ?
S6 O39 V7 129.86(17) . . ?
S6 O40 V8 128.96(17) . . ?
O45 S7 O46 112.9(2) . . ?
O45 S7 O44 111.7(2) . . ?
O46 S7 O44 107.8(2) . . ?
O45 S7 O43 108.9(2) . . ?
O46 S7 O43 107.91(18) . . ?
O44 S7 O43 107.38(18) . . ?
S7 O43 V8 131.19(18) . . ?
S7 O44 V9 133.4(2) . . ?
O50 S8 O49 114.0(2) . . ?
O50 S8 O47 107.8(2) . . ?
O49 S8 O47 109.28(19) . . ?
O50 S8 O48 108.30(19) . . ?
O49 S8 O48 109.51(19) . . ?
O47 S8 O48 107.77(18) . . ?
S8 O47 V9 133.3(2) . . ?
S8 O48 V6 133.08(18) . . ?
C31 N6 C33 111.4(4) . . ?
C31 N6 C35 112.5(4) . . ?
C33 N6 C35 110.2(4) . . ?
C31 N6 H6 106(4) . . ?
C33 N6 H6 99(4) . . ?
C35 N6 H6 117(4) . . ?
N6 C31 C32 112.0(4) . . ?
N6 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
N6 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N6 C33 C34 113.7(4) . . ?
N6 C33 H33A 108.8 . . ?
C34 C33 H33A 108.8 . . ?
N6 C33 H33B 108.8 . . ?
C34 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N6 112.4(4) . . ?
C36 C35 H35A 109.1 . . ?
N6 C35 H35A 109.1 . . ?
C36 C35 H35B 109.1 . . ?
N6 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37 N7 C39 112.0(9) . . ?
C37 N7 C41 112.7(7) . . ?
C39 N7 C41 108.1(6) . . ?
C41X N7 C37X 110.4(10) . . ?
C41X N7 C39X 113.0(8) . . ?
C37X N7 C39X 108.7(9) . . ?
C37 N7 H7 108.0 . . ?
C39 N7 H7 108.0 . . ?
C41 N7 H7 108.0 . . ?
C41X N7 H7X 108.2 . . ?
C37X N7 H7X 108.2 . . ?
C39X N7 H7X 108.2 . . ?
C38 C37 N7 116.2(11) . . ?
C38 C37 H37A 108.2 . . ?
N7 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
N7 C37 H37B 108.2 . . ?
H37A C37 H37B 107.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37X C38 H38D 109.5 . . ?
C37X C38 H38E 109.5 . . ?
H38D C38 H38E 109.5 . . ?
C37X C38 H38F 109.5 . . ?
H38D C38 H38F 109.5 . . ?
H38E C38 H38F 109.5 . . ?
N7 C39 C40 114.1(7) . . ?
N7 C39 H39A 108.7 . . ?
C40 C39 H39A 108.7 . . ?
N7 C39 H39B 108.7 . . ?
C40 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39X C40 H40D 109.5 . . ?
C39X C40 H40E 109.5 . . ?
H40D C40 H40E 109.5 . . ?
C39X C40 H40F 109.5 . . ?
H40D C40 H40F 109.5 . . ?
H40E C40 H40F 109.5 . . ?
C42 C41 N7 113.9(6) . . ?
C42 C41 H41A 108.8 . . ?
N7 C41 H41A 108.8 . . ?
C42 C41 H41B 108.8 . . ?
N7 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41X C42 H42D 109.5 . . ?
C41X C42 H42E 109.5 . . ?
H42D C42 H42E 109.5 . . ?
C41X C42 H42F 109.5 . . ?
H42D C42 H42F 109.5 . . ?
H42E C42 H42F 109.5 . . ?
C38 C37X N7 114.9(12) . . ?
C38 C37X H37C 108.5 . . ?
N7 C37X H37C 108.5 . . ?
C38 C37X H37D 108.5 . . ?
N7 C37X H37D 108.5 . . ?
H37C C37X H37D 107.5 . . ?
C40 C39X N7 111.1(8) . . ?
C40 C39X H39C 109.4 . . ?
N7 C39X H39C 109.4 . . ?
C40 C39X H39D 109.4 . . ?
N7 C39X H39D 109.4 . . ?
H39C C39X H39D 108.0 . . ?
N7 C41X C42 114.1(9) . . ?
N7 C41X H41C 108.7 . . ?
C42 C41X H41C 108.7 . . ?
N7 C41X H41D 108.7 . . ?
C42 C41X H41D 108.7 . . ?
H41C C41X H41D 107.6 . . ?
C47X N8 C45X 110.9(10) . . ?
C43 N8 C47 116.4(10) . . ?
C43 N8 C45 122.2(9) . . ?
C47 N8 C45 89.2(8) . . ?
C47X N8 C43X 97.7(11) . . ?
C45X N8 C43X 102.7(11) . . ?
C43 N8 H8 109.1 . . ?
C47 N8 H8 109.1 . . ?
C45 N8 H8 109.1 . . ?
C47X N8 H8X 114.6 . . ?
C45X N8 H8X 114.6 . . ?
C43X N8 H8X 114.6 . . ?
N8 C43 C44 102.8(8) . . ?
N8 C43 H43A 111.2 . . ?
C44 C43 H43A 111.2 . . ?
N8 C43 H43B 111.2 . . ?
C44 C43 H43B 111.2 . . ?
H43A C43 H43B 109.1 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N8 110.4(13) . . ?
C46 C45 H45A 109.6 . . ?
N8 C45 H45A 109.6 . . ?
C46 C45 H45B 109.6 . . ?
N8 C45 H45B 109.6 . . ?
H45A C45 H45B 108.1 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 N8 98.6(11) . . ?
C48 C47 H47A 112.0 . . ?
N8 C47 H47A 112.0 . . ?
C48 C47 H47B 112.0 . . ?
N8 C47 H47B 112.0 . . ?
H47A C47 H47B 109.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44X C43X N8 119.9(16) . . ?
C44X C43X H43C 107.3 . . ?
N8 C43X H43C 107.3 . . ?
C44X C43X H43D 107.3 . . ?
N8 C43X H43D 107.3 . . ?
H43C C43X H43D 106.9 . . ?
C43X C44X H44D 109.5 . . ?
C43X C44X H44E 109.5 . . ?
H44D C44X H44E 109.5 . . ?
C43X C44X H44F 109.5 . . ?
H44D C44X H44F 109.5 . . ?
H44E C44X H44F 109.5 . . ?
N8 C45X C46X 114.1(14) . . ?
N8 C45X H45C 108.7 . . ?
C46X C45X H45C 108.7 . . ?
N8 C45X H45D 108.7 . . ?
C46X C45X H45D 108.7 . . ?
H45C C45X H45D 107.6 . . ?
C45X C46X H46D 109.5 . . ?
C45X C46X H46E 109.5 . . ?
H46D C46X H46E 109.5 . . ?
C45X C46X H46F 109.5 . . ?
H46D C46X H46F 109.5 . . ?
H46E C46X H46F 109.5 . . ?
N8 C47X C48X 126.4(15) . . ?
N8 C47X H47C 105.7 . . ?
C48X C47X H47C 105.7 . . ?
N8 C47X H47D 105.7 . . ?
C48X C47X H47D 105.7 . . ?
H47C C47X H47D 106.2 . . ?
C47X C48X H48D 109.5 . . ?
C47X C48X H48E 109.5 . . ?
H48D C48X H48E 109.5 . . ?
C47X C48X H48F 109.5 . . ?
H48D C48X H48F 109.5 . . ?
H48E C48X H48F 109.5 . . ?
C53 N9 C51 118.6(5) . . ?
C53 N9 C49 112.0(7) . . ?
C51 N9 C49 106.1(6) . . ?
C53 N9 H9 104(4) . . ?
C51 N9 H9 108(4) . . ?
C49 N9 H9 108(4) . . ?
C50 C49 N9 113.3(8) . . ?
C50 C49 H49A 108.9 . . ?
N9 C49 H49A 108.9 . . ?
C50 C49 H49B 108.9 . . ?
N9 C49 H49B 108.9 . . ?
H49A C49 H49B 107.7 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N9 C51 C52 114.6(5) . . ?
N9 C51 H51A 108.6 . . ?
C52 C51 H51A 108.6 . . ?
N9 C51 H51B 108.6 . . ?
C52 C51 H51B 108.6 . . ?
H51A C51 H51B 107.6 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N9 C53 C54 110.9(6) . . ?
N9 C53 H53A 109.5 . . ?
C54 C53 H53A 109.5 . . ?
N9 C53 H53B 109.5 . . ?
C54 C53 H53B 109.5 . . ?
H53A C53 H53B 108.0 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C57 N10 C59 112.6(6) . . ?
C57 N10 C55 111.1(6) . . ?
C59 N10 C55 110.0(5) . . ?
C57 N10 H10 109(4) . . ?
C59 N10 H10 114(4) . . ?
C55 N10 H10 98(4) . . ?
N10 C55 C56 110.6(7) . . ?
N10 C55 H55A 109.5 . . ?
C56 C55 H55A 109.5 . . ?
N10 C55 H55B 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N10 C57 C58 111.4(7) . . ?
N10 C57 H57A 109.4 . . ?
C58 C57 H57A 109.4 . . ?
N10 C57 H57B 109.4 . . ?
C58 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 N10 115.1(5) . . ?
C60 C59 H59A 108.5 . . ?
N10 C59 H59A 108.5 . . ?
C60 C59 H59B 108.5 . . ?
N10 C59 H59B 108.5 . . ?
H59A C59 H59B 107.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 V5 O6 V2 107.37(15) . . . . ?
O9 V5 O6 V2 -142.88(13) . . . . ?
O7 V5 O6 V2 -2.11(12) . . . . ?
O8 V5 O6 V2 -72.3(2) . . . . ?
V1 V5 O6 V2 -146.03(17) . . . . ?
V3 V5 O6 V2 -27.66(13) . . . . ?
V4 V5 O6 V2 -116.75(8) . . . . ?
O5 V5 O6 V1 -106.60(15) . . . . ?
O9 V5 O6 V1 3.15(12) . . . . ?
O7 V5 O6 V1 143.93(13) . . . . ?
O8 V5 O6 V1 73.7(2) . . . . ?
V2 V5 O6 V1 146.03(17) . . . . ?
V3 V5 O6 V1 118.37(8) . . . . ?
V4 V5 O6 V1 29.29(13) . . . . ?
O5 V5 O7 V3 106.70(15) . . . . ?
O6 V5 O7 V3 -144.23(13) . . . . ?
O9 V5 O7 V3 -71.9(2) . . . . ?
O8 V5 O7 V3 -2.17(12) . . . . ?
V1 V5 O7 V3 -117.95(9) . . . . ?
V2 V5 O7 V3 -146.34(18) . . . . ?
V4 V5 O7 V3 -28.30(13) . . . . ?
O5 V5 O7 V2 -106.96(15) . . . . ?
O6 V5 O7 V2 2.11(12) . . . . ?
O9 V5 O7 V2 74.4(2) . . . . ?
O8 V5 O7 V2 144.17(13) . . . . ?
V1 V5 O7 V2 28.39(13) . . . . ?
V3 V5 O7 V2 146.34(18) . . . . ?
V4 V5 O7 V2 118.04(9) . . . . ?
O5 V5 O8 V3 -106.92(16) . . . . ?
O6 V5 O8 V3 72.8(2) . . . . ?
O9 V5 O8 V3 143.57(14) . . . . ?
O7 V5 O8 V3 2.17(12) . . . . ?
V1 V5 O8 V3 118.64(9) . . . . ?
V2 V5 O8 V3 27.87(14) . . . . ?
V4 V5 O8 V3 144.90(19) . . . . ?
O5 V5 O8 V4 108.17(16) . . . . ?
O6 V5 O8 V4 -72.1(2) . . . . ?
O9 V5 O8 V4 -1.33(12) . . . . ?
O7 V5 O8 V4 -142.73(14) . . . . ?
V1 V5 O8 V4 -26.27(14) . . . . ?
V2 V5 O8 V4 -117.04(9) . . . . ?
V3 V5 O8 V4 -144.90(19) . . . . ?
O5 V5 O9 V1 105.84(15) . . . . ?
O6 V5 O9 V1 -3.19(12) . . . . ?
O7 V5 O9 V1 -75.5(2) . . . . ?
O8 V5 O9 V1 -145.20(14) . . . . ?
V2 V5 O9 V1 -29.83(13) . . . . ?
V3 V5 O9 V1 -119.54(9) . . . . ?
V4 V5 O9 V1 -146.52(18) . . . . ?
O5 V5 O9 V4 -107.64(15) . . . . ?
O6 V5 O9 V4 143.33(13) . . . . ?
O7 V5 O9 V4 71.0(2) . . . . ?
O8 V5 O9 V4 1.33(12) . . . . ?
V1 V5 O9 V4 146.52(18) . . . . ?
V2 V5 O9 V4 116.69(9) . . . . ?
V3 V5 O9 V4 26.98(13) . . . . ?
O12 S1 O10 V1 -52.9(3) . . . . ?
O13 S1 O10 V1 -177.5(2) . . . . ?
O11 S1 O10 V1 67.6(3) . . . . ?
O12 S1 O11 V2 56.5(3) . . . . ?
O13 S1 O11 V2 179.9(2) . . . . ?
O10 S1 O11 V2 -64.1(3) . . . . ?
O17 S2 O14 V2 -175.4(2) . . . . ?
O16 S2 O14 V2 -51.4(3) . . . . ?
O15 S2 O14 V2 67.4(3) . . . . ?
O17 S2 O15 V3 -178.3(2) . . . . ?
O16 S2 O15 V3 57.3(3) . . . . ?
O14 S2 O15 V3 -61.7(3) . . . . ?
O20 S3 O18 V3 -57.6(3) . . . . ?
O21 S3 O18 V3 176.8(3) . . . . ?
O19 S3 O18 V3 62.8(3) . . . . ?
O20 S3 O19 V4 57.9(3) . . . . ?
O21 S3 O19 V4 -176.3(3) . . . . ?
O18 S3 O19 V4 -62.7(3) . . . . ?
O24 S4 O22 V4 -57.0(3) . . . . ?
O25 S4 O22 V4 179.4(2) . . . . ?
O23 S4 O22 V4 63.5(3) . . . . ?
O24 S4 O23 V1 62.0(3) . . . . ?
O25 S4 O23 V1 -173.4(2) . . . . ?
O22 S4 O23 V1 -57.6(3) . . . . ?
C3 N1 C1 C2 55.2(6) . . . . ?
C5 N1 C1 C2 177.9(5) . . . . ?
C5 N1 C3 C4 57.5(6) . . . . ?
C1 N1 C3 C4 178.5(5) . . . . ?
C3 N1 C5 C6 -179.2(5) . . . . ?
C1 N1 C5 C6 58.4(6) . . . . ?
C5X N1 C1X C2 -38.4(18) . . . . ?
C3X N1 C1X C2 -167.4(12) . . . . ?
C5X N1 C3X C4 178.0(10) . . . . ?
C1X N1 C3X C4 -49.7(15) . . . . ?
C1X N1 C5X C6 177.6(11) . . . . ?
C3X N1 C5X C6 -56.0(14) . . . . ?
C11 N2 C7 C8 68.0(7) . . . . ?
C9 N2 C7 C8 -162.8(6) . . . . ?
C7 N2 C9 C10 -60.0(6) . . . . ?
C11 N2 C9 C10 68.4(6) . . . . ?
C7 N2 C11 C12 -174.6(5) . . . . ?
C9 N2 C11 C12 56.6(5) . . . . ?
C15 N3 C13 C14 -64.6(12) . . . . ?
C17 N3 C13 C14 73.1(11) . . . . ?
C17 N3 C15 C16 172.2(5) . . . . ?
C13 N3 C15 C16 -48.4(8) . . . . ?
C13X N3 C15 C16 -77.0(8) . . . . ?
C15 N3 C17 C18 -67.3(5) . . . . ?
C13 N3 C17 C18 153.2(5) . . . . ?
C13X N3 C17 C18 -176.2(8) . . . . ?
C15 N3 C13X C14X 109.0(16) . . . . ?
C17 N3 C13X C14X -133.9(15) . . . . ?
C23 N4 C19 C20 -52.0(13) . . . . ?
C21 N4 C19 C20 179.9(10) . . . . ?
C19 N4 C21 C22 -168.6(9) . . . . ?
C23 N4 C21 C22 62.7(12) . . . . ?
C19 N4 C23 C24 -63.4(16) . . . . ?
C21 N4 C23 C24 62.6(16) . . . . ?
C21X N4X C19X C20X -68.5(16) . . . . ?
C23X N4X C19X C20X 164.1(12) . . . . ?
C19X N4X C21X C22X -174.1(16) . . . . ?
C23X N4X C21X C22X -47(2) . . . . ?
C19X N4X C23X C24X 66.5(18) . . . . ?
C21X N4X C23X C24X -61(2) . . . . ?
C27 N5 C25 C26 151.4(6) . . . . ?
C29 N5 C25 C26 -84.2(6) . . . . ?
C25 N5 C27 C28 -63.8(6) . . . . ?
C29 N5 C27 C28 171.9(4) . . . . ?
C25 N5 C29 C30 162.0(4) . . . . ?
C27 N5 C29 C30 -72.4(5) . . . . ?
O30 V10 O31 V6 -107.02(15) . . . . ?
O32 V10 O31 V6 144.66(13) . . . . ?
O33 V10 O31 V6 74.1(2) . . . . ?
O34 V10 O31 V6 2.28(12) . . . . ?
V9 V10 O31 V6 28.97(13) . . . . ?
V8 V10 O31 V6 117.84(9) . . . . ?
V7 V10 O31 V6 147.87(17) . . . . ?
O30 V10 O31 V7 105.11(15) . . . . ?
O32 V10 O31 V7 -3.20(12) . . . . ?
O33 V10 O31 V7 -73.7(2) . . . . ?
O34 V10 O31 V7 -145.59(13) . . . . ?
V9 V10 O31 V7 -118.90(9) . . . . ?
V6 V10 O31 V7 -147.87(17) . . . . ?
V8 V10 O31 V7 -30.03(13) . . . . ?
O30 V10 O32 V8 108.61(16) . . . . ?
O33 V10 O32 V8 -0.78(13) . . . . ?
O34 V10 O32 V8 -72.2(2) . . . . ?
O31 V10 O32 V8 -141.75(13) . . . . ?
V9 V10 O32 V8 -26.55(13) . . . . ?
V6 V10 O32 V8 -116.72(9) . . . . ?
V7 V10 O32 V8 -144.93(17) . . . . ?
O30 V10 O32 V7 -106.45(16) . . . . ?
O33 V10 O32 V7 144.15(13) . . . . ?
O34 V10 O32 V7 72.7(2) . . . . ?
O31 V10 O32 V7 3.19(11) . . . . ?
V9 V10 O32 V7 118.39(9) . . . . ?
V6 V10 O32 V7 28.22(13) . . . . ?
V8 V10 O32 V7 144.93(17) . . . . ?
O30 V10 O33 V9 107.39(16) . . . . ?
O32 V10 O33 V9 -144.12(13) . . . . ?
O34 V10 O33 V9 -2.20(13) . . . . ?
O31 V10 O33 V9 -73.8(2) . . . . ?
V6 V10 O33 V9 -28.77(14) . . . . ?
V8 V10 O33 V9 -144.91(19) . . . . ?
V7 V10 O33 V9 -118.54(9) . . . . ?
O30 V10 O33 V8 -107.70(16) . . . . ?
O32 V10 O33 V8 0.78(12) . . . . ?
O34 V10 O33 V8 142.71(14) . . . . ?
O31 V10 O33 V8 71.1(2) . . . . ?
V9 V10 O33 V8 144.91(19) . . . . ?
V6 V10 O33 V8 116.14(10) . . . . ?
V7 V10 O33 V8 26.37(15) . . . . ?
O30 V10 O34 V9 -107.44(16) . . . . ?
O32 V10 O34 V9 73.4(2) . . . . ?
O33 V10 O34 V9 2.19(12) . . . . ?
O31 V10 O34 V9 142.84(13) . . . . ?
V6 V10 O34 V9 145.10(18) . . . . ?
V8 V10 O34 V9 28.79(13) . . . . ?
V7 V10 O34 V9 118.29(9) . . . . ?
O30 V10 O34 V6 107.47(16) . . . . ?
O32 V10 O34 V6 -71.7(2) . . . . ?
O33 V10 O34 V6 -142.91(14) . . . . ?
O31 V10 O34 V6 -2.26(12) . . . . ?
V9 V10 O34 V6 -145.10(18) . . . . ?
V8 V10 O34 V6 -116.31(9) . . . . ?
V7 V10 O34 V6 -26.81(14) . . . . ?
O37 S5 O35 V6 -57.1(3) . . . . ?
O38 S5 O35 V6 179.8(2) . . . . ?
O36 S5 O35 V6 63.8(2) . . . . ?
O37 S5 O36 V7 54.5(3) . . . . ?
O38 S5 O36 V7 177.9(2) . . . . ?
O35 S5 O36 V7 -66.6(2) . . . . ?
O41 S6 O39 V7 -57.2(3) . . . . ?
O42 S6 O39 V7 177.5(2) . . . . ?
O40 S6 O39 V7 63.6(3) . . . . ?
O41 S6 O40 V8 52.4(3) . . . . ?
O42 S6 O40 V8 177.7(2) . . . . ?
O39 S6 O40 V8 -68.3(2) . . . . ?
O45 S7 O43 V8 -59.0(3) . . . . ?
O46 S7 O43 V8 178.2(2) . . . . ?
O44 S7 O43 V8 62.2(3) . . . . ?
O45 S7 O44 V9 62.3(4) . . . . ?
O46 S7 O44 V9 -173.1(3) . . . . ?
O43 S7 O44 V9 -57.0(4) . . . . ?
O50 S8 O47 V9 175.9(3) . . . . ?
O49 S8 O47 V9 -59.7(3) . . . . ?
O48 S8 O47 V9 59.2(3) . . . . ?
O50 S8 O48 V6 -172.5(3) . . . . ?
O49 S8 O48 V6 62.6(3) . . . . ?
O47 S8 O48 V6 -56.2(3) . . . . ?
C33 N6 C31 C32 -172.7(4) . . . . ?
C35 N6 C31 C32 62.9(5) . . . . ?
C31 N6 C33 C34 66.9(5) . . . . ?
C35 N6 C33 C34 -167.5(5) . . . . ?
C31 N6 C35 C36 -143.1(5) . . . . ?
C33 N6 C35 C36 91.9(5) . . . . ?
C39 N7 C37 C38 -171.9(10) . . . . ?
C41 N7 C37 C38 66.0(12) . . . . ?
C37 N7 C39 C40 67.7(11) . . . . ?
C41 N7 C39 C40 -167.7(8) . . . . ?
C37 N7 C41 C42 -165.9(9) . . . . ?
C39 N7 C41 C42 69.9(10) . . . . ?
C41X N7 C37X C38 170.1(13) . . . . ?
C39X N7 C37X C38 -65.4(16) . . . . ?
C41X N7 C39X C40 -65.0(13) . . . . ?
C37X N7 C39X C40 172.1(10) . . . . ?
C37X N7 C41X C42 -72.6(16) . . . . ?
C39X N7 C41X C42 165.4(10) . . . . ?
C47 N8 C43 C44 -167.1(9) . . . . ?
C45 N8 C43 C44 -60.0(12) . . . . ?
C43 N8 C45 C46 -172.3(14) . . . . ?
C47 N8 C45 C46 -51.2(17) . . . . ?
C43 N8 C47 C48 -64.0(16) . . . . ?
C45 N8 C47 C48 170.0(15) . . . . ?
C47X N8 C43X C44X 175(2) . . . . ?
C45X N8 C43X C44X -71(2) . . . . ?
C47X N8 C45X C46X -105.7(14) . . . . ?
C43X N8 C45X C46X 150.8(13) . . . . ?
C45X N8 C47X C48X 67(2) . . . . ?
C43X N8 C47X C48X 173.9(18) . . . . ?
C53 N9 C49 C50 71.7(10) . . . . ?
C51 N9 C49 C50 -157.4(8) . . . . ?
C53 N9 C51 C52 68.1(8) . . . . ?
C49 N9 C51 C52 -58.9(7) . . . . ?
C51 N9 C53 C54 65.0(7) . . . . ?
C49 N9 C53 C54 -170.8(6) . . . . ?
C57 N10 C55 C56 59.6(7) . . . . ?
C59 N10 C55 C56 -175.1(6) . . . . ?
C59 N10 C57 C58 58.8(7) . . . . ?
C55 N10 C57 C58 -177.3(6) . . . . ?
C57 N10 C59 C60 -175.8(6) . . . . ?
C55 N10 C59 C60 59.7(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1X O12 1.00 1.86 2.785(5) 152.8 .
N2 H2 O13 0.91(3) 1.90(4) 2.787(5) 166(5) .
N3 H3 O16 1.00 1.78 2.779(5) 173.5 .
N3 H3X O17 1.00 2.59 3.305(5) 128.6 .
N4 H4 O15 1.00 2.26 3.149(12) 147.3 .
N4 H4 O18 1.00 2.27 3.126(13) 143.0 .
N5 H5 O24 0.83(3) 1.93(4) 2.732(5) 162(5) .
N4X H4X O38 1.00 2.07 3.066(9) 177.5 1_665
N5 H5 O24 0.83(3) 1.93(4) 2.732(5) 162(5) .
N6 H6 O37 0.90(3) 1.93(4) 2.810(5) 162(5) .
N7 H7 O38 1.00 1.87 2.868(5) 174.3 .
N8 H8 O42 1.00 1.76 2.744(6) 168.6 .
N9 H9 O45 0.94(4) 1.78(4) 2.721(5) 178(6) .
N10 H10 O49 0.90(4) 1.87(4) 2.764(5) 172(6) .

_refine_diff_density_max         0.911
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.075

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichlormethane/toluene'
