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

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1048777'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_RFACR01_2                   
;
RESPONSE: The data obtained from the UK EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. The high wR-factor
is unexpected, but is probably a reflection that the crystal 
examined was poor quality. 
However, the structure refinement confirms the chemical entities
present and gives useful chemical information. 
;


_vrf_PLAT084_2                   
;
RESPONSE: The data obtained from the UK EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. The high wR-factor
is unexpected, but is probably a reflection that the crystal 
examined was poor quality. 
However, the structure refinement confirms the chemical entities
present and gives useful chemical information. 
;

_vrf_PLAT242_2                   
;
RESPONSE: This is central atom of a tButoxide group attached to
the metal centre. The peripheral carbon atoms have much greater 
displacement parameters than this carbon atom as expected 
chemically. This reflects the tendency of the tBu group to rock. 
It was not possible to model this using a disordered model. 
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C72 H104 O8 V2, 2(C2 H3 N)
;


_chemical_formula_sum            'C76 H110 N2 O8 V2'
_chemical_formula_weight         1281.53

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                   9.1413(7)
_cell_length_b                   11.0130(8)
_cell_length_c                   18.8731(13)
_cell_angle_alpha                74.468(8)
_cell_angle_beta                 89.494(9)
_cell_angle_gamma                85.010(9)
_cell_volume                     1823.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21499
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Plate
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             690
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.309
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_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            28762
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.822
_diffrn_reflns_theta_max         25.601
_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 0.999
_reflns_number_total             6855
_reflns_number_gt                3107
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;

_computing_structure_solution    SHELXS-2013
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6855
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2434
_refine_ls_R_factor_gt           0.1541
_refine_ls_wR_factor_ref         0.4724
_refine_ls_wR_factor_gt          0.4267
_refine_ls_goodness_of_fit_ref   1.431
_refine_ls_restrained_S_all      1.431
_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
C1 C 0.6804(9) 0.3476(7) 0.2570(4) 0.079(2) Uani 1 1 d . . . . .
C2 C 0.7991(10) 0.2628(7) 0.2909(4) 0.088(2) Uani 1 1 d . . . . .
C3 C 0.9257(9) 0.2785(7) 0.2532(5) 0.086(2) Uani 1 1 d . . . . .
H3 H 1.0101 0.2253 0.2747 0.104 Uiso 1 1 calc R U . . .
C4 C 0.9428(9) 0.3621(7) 0.1885(4) 0.082(2) Uani 1 1 d . . . . .
C5 C 0.8196(8) 0.4364(6) 0.1549(4) 0.0680(19) Uani 1 1 d . . . . .
H5 H 0.8277 0.4936 0.1077 0.082 Uiso 1 1 calc R U . . .
C6 C 0.6918(9) 0.4289(6) 0.1872(4) 0.0703(19) Uani 1 1 d . . . . .
C7 C 0.7791(12) 0.1596(10) 0.3684(6) 0.122(4) Uani 1 1 d . . . . .
C8 C 0.6555(13) 0.0782(10) 0.3558(7) 0.149(5) Uani 1 1 d . . . . .
H8A H 0.6824 0.0407 0.3154 0.224 Uiso 1 1 calc R U . . .
H8B H 0.6431 0.0107 0.4008 0.224 Uiso 1 1 calc R U . . .
H8C H 0.5631 0.1319 0.3434 0.224 Uiso 1 1 calc R U . . .
C9 C 0.9247(13) 0.0769(10) 0.3845(6) 0.145(4) Uani 1 1 d . . . . .
H9A H 0.9436 0.0340 0.3457 0.218 Uiso 1 1 calc R U . . .
H9B H 1.0044 0.1301 0.3863 0.218 Uiso 1 1 calc R U . . .
H9C H 0.9193 0.0138 0.4320 0.218 Uiso 1 1 calc R U . . .
C10 C 0.7547(14) 0.2215(13) 0.4268(6) 0.147(5) Uani 1 1 d . . . . .
H10A H 0.6619 0.2751 0.4177 0.220 Uiso 1 1 calc R U . . .
H10B H 0.7504 0.1574 0.4740 0.220 Uiso 1 1 calc R U . . .
H10C H 0.8355 0.2738 0.4283 0.220 Uiso 1 1 calc R U . . .
C11 C 1.0878(9) 0.3735(9) 0.1494(5) 0.095(3) Uani 1 1 d . . . . .
C12 C 1.2120(9) 0.3264(10) 0.2016(6) 0.120(3) Uani 1 1 d . . . . .
H12A H 1.2080 0.3736 0.2389 0.181 Uiso 1 1 calc R U . . .
H12B H 1.2060 0.2363 0.2255 0.181 Uiso 1 1 calc R U . . .
H12C H 1.3046 0.3379 0.1750 0.181 Uiso 1 1 calc R U . . .
C13 C 1.0932(13) 0.303(2) 0.0936(9) 0.224(7) Uani 1 1 d . . . . .
H13A H 1.0105 0.3350 0.0590 0.335 Uiso 1 1 calc R U . . .
H13B H 1.1857 0.3149 0.0670 0.335 Uiso 1 1 calc R U . . .
H13C H 1.0871 0.2133 0.1175 0.335 Uiso 1 1 calc R U . . .
C14 C 1.1132(11) 0.5174(10) 0.1180(7) 0.147(5) Uani 1 1 d . . . . .
H14A H 1.1081 0.5587 0.1580 0.221 Uiso 1 1 calc R U . . .
H14B H 1.2100 0.5250 0.0953 0.221 Uiso 1 1 calc R U . . .
H14C H 1.0371 0.5583 0.0809 0.221 Uiso 1 1 calc R U . . .
C15 C 0.5579(7) 0.5119(6) 0.1505(3) 0.0660(18) Uani 1 1 d . . . . .
H15 H 0.4715 0.4743 0.1780 0.079 Uiso 1 1 calc R U . . .
C16 C 0.5346(7) 0.5086(7) 0.0714(4) 0.071(2) Uani 1 1 d . . . . .
C17 C 0.5660(7) 0.3978(6) 0.0506(4) 0.0668(19) Uani 1 1 d . . . . .
H17 H 0.6130 0.3262 0.0851 0.080 Uiso 1 1 calc R U . . .
C18 C 0.4684(7) 0.6121(6) 0.0177(4) 0.0676(18) Uani 1 1 d . . . . .
H18 H 0.4470 0.6907 0.0292 0.081 Uiso 1 1 calc R U . . .
C19 C 0.4647(8) 0.6813(7) 0.2110(4) 0.075(2) Uani 1 1 d . . . . .
C20 C 0.5573(8) 0.6471(7) 0.1613(4) 0.0689(19) Uani 1 1 d . . . . .
C21 C 0.6474(7) 0.7299(7) 0.1221(4) 0.075(2) Uani 1 1 d . . . . .
H21 H 0.7124 0.7047 0.0881 0.090 Uiso 1 1 calc R U . . .
C22 C 0.6470(8) 0.8544(7) 0.1307(5) 0.083(2) Uani 1 1 d . . . . .
C23 C 0.5475(9) 0.8857(8) 0.1775(5) 0.085(2) Uani 1 1 d . . . . .
H23 H 0.5426 0.9692 0.1830 0.103 Uiso 1 1 calc R U . . .
C24 C 0.4517(8) 0.8034(8) 0.2182(4) 0.080(2) Uani 1 1 d . . . . .
C25 C 0.7497(10) 0.9442(8) 0.0885(6) 0.103(3) Uani 1 1 d . . . . .
C26 C 0.8976(9) 0.8796(10) 0.0910(7) 0.146(5) Uani 1 1 d . . . . .
H26A H 0.8934 0.8042 0.0731 0.219 Uiso 1 1 calc R U . . .
H26B H 0.9627 0.9369 0.0598 0.219 Uiso 1 1 calc R U . . .
H26C H 0.9353 0.8545 0.1418 0.219 Uiso 1 1 calc R U . . .
C27 C 0.7131(13) 0.9711(16) -0.0002(9) 0.261(10) Uani 1 1 d . . . . .
H27A H 0.7110 0.8903 -0.0125 0.392 Uiso 1 1 calc R U . . .
H27B H 0.6174 1.0198 -0.0119 0.392 Uiso 1 1 calc R U . . .
H27C H 0.7893 1.0191 -0.0287 0.392 Uiso 1 1 calc R U . . .
C28 C 0.756(2) 1.0528(15) 0.1143(15) 0.321(12) Uani 1 1 d . . . . .
H28A H 0.6577 1.0963 0.1127 0.481 Uiso 1 1 calc R U . . .
H28B H 0.7942 1.0276 0.1650 0.481 Uiso 1 1 calc R U . . .
H28C H 0.8217 1.1099 0.0830 0.481 Uiso 1 1 calc R U . . .
C29 C 0.3343(11) 0.8528(9) 0.2655(5) 0.106(3) Uani 1 1 d . . . . .
C30 C 0.3627(17) 0.7882(11) 0.3457(6) 0.153(5) Uani 1 1 d . . . . .
H30A H 0.4601 0.8051 0.3600 0.230 Uiso 1 1 calc R U . . .
H30B H 0.2879 0.8205 0.3752 0.230 Uiso 1 1 calc R U . . .
H30C H 0.3585 0.6967 0.3543 0.230 Uiso 1 1 calc R U . . .
C31 C 0.3388(14) 0.9938(10) 0.2572(8) 0.153(5) Uani 1 1 d . . . . .
H31A H 0.4356 1.0097 0.2729 0.229 Uiso 1 1 calc R U . . .
H31B H 0.3209 1.0404 0.2055 0.229 Uiso 1 1 calc R U . . .
H31C H 0.2630 1.0219 0.2877 0.229 Uiso 1 1 calc R U . . .
C32 C 0.1896(11) 0.8298(14) 0.2419(8) 0.163(5) Uani 1 1 d . . . . .
H32A H 0.1742 0.8729 0.1895 0.245 Uiso 1 1 calc R U . . .
H32B H 0.1842 0.7387 0.2497 0.245 Uiso 1 1 calc R U . . .
H32C H 0.1136 0.8625 0.2706 0.245 Uiso 1 1 calc R U . . .
C41 C 0.2666(14) 0.3633(12) 0.4540(8) 0.135(4) Uani 1 1 d . . . . .
C42 C 0.347(3) 0.259(2) 0.4957(10) 0.404(16) Uani 1 1 d . . . . .
H42A H 0.3387 0.1877 0.4746 0.605 Uiso 1 1 calc R U . . .
H42B H 0.4501 0.2764 0.4965 0.605 Uiso 1 1 calc R U . . .
H42C H 0.3096 0.2380 0.5459 0.605 Uiso 1 1 calc R U . . .
C43 C 0.1128(18) 0.355(3) 0.4471(11) 0.293(14) Uani 1 1 d . . . . .
H43A H 0.0674 0.4355 0.4160 0.439 Uiso 1 1 calc R U . . .
H43B H 0.0965 0.2868 0.4247 0.439 Uiso 1 1 calc R U . . .
H43C H 0.0686 0.3377 0.4959 0.439 Uiso 1 1 calc R U . . .
C44 C 0.280(4) 0.465(3) 0.4855(10) 0.421(19) Uani 1 1 d . . . . .
H44A H 0.2230 0.5407 0.4562 0.632 Uiso 1 1 calc R U . . .
H44B H 0.2433 0.4427 0.5359 0.632 Uiso 1 1 calc R U . . .
H44C H 0.3838 0.4811 0.4864 0.632 Uiso 1 1 calc R U . . .
C51 C 0.8699(16) 0.6956(17) 0.3226(9) 0.158(5) Uiso 1 1 d . . . . .
C52 C 0.8715(16) 0.6128(12) 0.2865(7) 0.151(4) Uani 1 1 d . . . . .
H52A H 0.8007 0.5515 0.3075 0.226 Uiso 1 1 calc R U . . .
H52B H 0.9701 0.5690 0.2892 0.226 Uiso 1 1 calc R U . . .
H52C H 0.8448 0.6544 0.2350 0.226 Uiso 1 1 calc R U . . .
N1 N 0.877(2) 0.761(2) 0.3578(12) 0.270(8) Uiso 1 1 d . . . . .
O1 O 0.5486(6) 0.3449(5) 0.2911(3) 0.0862(15) Uani 1 1 d . . . . .
O2 O 0.3824(5) 0.5918(5) 0.2542(3) 0.0807(14) Uani 1 1 d . . . . .
O3 O 0.5701(7) 0.5098(6) 0.3679(4) 0.123(2) Uani 1 1 d . . . . .
O4 O 0.3185(7) 0.3976(7) 0.3797(3) 0.115(2) Uani 1 1 d . . . . .
V1 V 0.45569(19) 0.45922(16) 0.32563(9) 0.1115(7) 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
C1 O1 1.360(9) . ?
C1 C6 1.389(10) . ?
C1 C2 1.405(10) . ?
C2 C3 1.353(11) . ?
C2 C7 1.614(12) . ?
C3 C4 1.335(10) . ?
C4 C5 1.383(10) . ?
C4 C11 1.510(11) . ?
C5 C6 1.313(10) . ?
C6 C15 1.515(9) . ?
C7 C10 1.450(16) . ?
C7 C9 1.530(14) . ?
C7 C8 1.559(15) . ?
C11 C13 1.461(16) . ?
C11 C12 1.473(11) . ?
C11 C14 1.573(14) . ?
C15 C16 1.519(10) . ?
C15 C20 1.557(10) . ?
C16 C17 1.385(10) . ?
C16 C18 1.402(9) . ?
C17 C18 1.365(9) 2_665 ?
C18 C17 1.365(9) 2_665 ?
C19 C20 1.363(10) . ?
C19 O2 1.374(9) . ?
C19 C24 1.382(11) . ?
C20 C21 1.348(10) . ?
C21 C22 1.422(11) . ?
C22 C23 1.351(11) . ?
C22 C25 1.490(11) . ?
C23 C24 1.389(11) . ?
C24 C29 1.545(13) . ?
C25 C28 1.412(19) . ?
C25 C26 1.467(13) . ?
C25 C27 1.65(2) . ?
C29 C32 1.463(14) . ?
C29 C30 1.505(14) . ?
C29 C31 1.523(14) . ?
C41 C42 1.363(18) . ?
C41 C44 1.41(2) . ?
C41 C43 1.426(18) . ?
C41 O4 1.438(14) . ?
C51 N1 1.11(2) . ?
C51 C52 1.275(19) . ?
O1 V1 1.725(6) . ?
O2 V1 1.786(5) . ?
O3 V1 1.547(6) . ?
O4 V1 1.682(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 118.9(7) . . ?
O1 C1 C2 119.5(7) . . ?
C6 C1 C2 121.5(8) . . ?
C3 C2 C1 113.9(7) . . ?
C3 C2 C7 125.5(7) . . ?
C1 C2 C7 120.7(8) . . ?
C4 C3 C2 125.9(7) . . ?
C3 C4 C5 117.8(8) . . ?
C3 C4 C11 122.8(7) . . ?
C5 C4 C11 119.3(7) . . ?
C6 C5 C4 121.0(7) . . ?
C5 C6 C1 119.6(7) . . ?
C5 C6 C15 120.6(6) . . ?
C1 C6 C15 119.7(7) . . ?
C10 C7 C9 108.0(9) . . ?
C10 C7 C8 115.9(11) . . ?
C9 C7 C8 109.5(10) . . ?
C10 C7 C2 110.4(9) . . ?
C9 C7 C2 106.1(9) . . ?
C8 C7 C2 106.4(8) . . ?
C13 C11 C12 109.7(9) . . ?
C13 C11 C4 110.2(8) . . ?
C12 C11 C4 111.2(8) . . ?
C13 C11 C14 113.7(11) . . ?
C12 C11 C14 102.5(8) . . ?
C4 C11 C14 109.4(7) . . ?
C6 C15 C16 113.2(6) . . ?
C6 C15 C20 110.8(5) . . ?
C16 C15 C20 114.6(5) . . ?
C17 C16 C18 116.4(6) . . ?
C17 C16 C15 120.9(6) . . ?
C18 C16 C15 122.5(7) . . ?
C18 C17 C16 122.3(6) 2_665 . ?
C17 C18 C16 121.2(6) 2_665 . ?
C20 C19 O2 118.7(7) . . ?
C20 C19 C24 121.3(7) . . ?
O2 C19 C24 120.0(8) . . ?
C21 C20 C19 120.1(7) . . ?
C21 C20 C15 120.5(7) . . ?
C19 C20 C15 119.4(7) . . ?
C20 C21 C22 121.3(8) . . ?
C23 C22 C21 116.2(7) . . ?
C23 C22 C25 122.9(8) . . ?
C21 C22 C25 120.9(8) . . ?
C22 C23 C24 124.1(8) . . ?
C19 C24 C23 116.7(8) . . ?
C19 C24 C29 123.8(8) . . ?
C23 C24 C29 119.5(8) . . ?
C28 C25 C26 109.2(12) . . ?
C28 C25 C22 113.3(10) . . ?
C26 C25 C22 109.8(7) . . ?
C28 C25 C27 115.8(13) . . ?
C26 C25 C27 99.1(10) . . ?
C22 C25 C27 108.7(7) . . ?
C32 C29 C30 111.3(11) . . ?
C32 C29 C31 109.1(9) . . ?
C30 C29 C31 106.2(10) . . ?
C32 C29 C24 108.4(9) . . ?
C30 C29 C24 110.2(8) . . ?
C31 C29 C24 111.6(9) . . ?
C42 C41 C44 108(2) . . ?
C42 C41 C43 117.1(19) . . ?
C44 C41 C43 106(2) . . ?
C42 C41 O4 111.1(12) . . ?
C44 C41 O4 109.0(11) . . ?
C43 C41 O4 105.0(12) . . ?
N1 C51 C52 174(2) . . ?
C1 O1 V1 129.0(5) . . ?
C19 O2 V1 124.6(4) . . ?
C41 O4 V1 144.6(7) . . ?
O3 V1 O4 112.4(4) . . ?
O3 V1 O1 106.8(3) . . ?
O4 V1 O1 110.1(3) . . ?
O3 V1 O2 106.1(3) . . ?
O4 V1 O2 109.3(3) . . ?
O1 V1 O2 112.0(2) . . ?

_refine_diff_density_max         0.514
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.108

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1404522'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;


_vrf_PLAT220_1                   
;
RESPONSE: The thermal motion of the tertiary butyl groups
around the outside of the molecule is considerably 
larger than that of the core carbon atoms. 
Inspection of the ORTEP shows there is no serious 
problem.
;

_vrf_PLAT243_1                   
;
RESPONSE: The THF molecule is crystallographically 
well determined. It is entirely reasonable on chemical 
grounds that the displacement parameter of the 
oxygen atom is great than that of the carbons of THF. 
Inspection of the ORTEP shows there is no serious 
problem.
;



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C78 H116 O10 V2, 2(C4 H8 O)
;
_chemical_formula_sum            'C86 H132 O12 V2'
_chemical_formula_weight         1459.80

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'


_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   23.8164(16)
_cell_length_b                   18.9585(7)
_cell_length_c                   18.6002(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8398.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    34672
_cell_measurement_theta_min      27.5
_cell_measurement_theta_max      3.0


_exptl_crystal_description       chip
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3160
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_process_details   
;
A multi-scan absorption correction was implemented
within Rigaku CrystalClear. 

Tmax = 1; Tmin = 0.511
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_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_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57655
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.46
_reflns_number_total             9280
_reflns_number_gt                5352
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;

_computing_structure_solution    'SHELXS-86 (Shldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9280
_refine_ls_number_parameters     464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1110
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.338045(16) 0.253793(19) 0.006378(17) 0.01355(10) Uani 1 1 d . . .
O3 O 0.33517(7) 0.26537(7) 0.09080(7) 0.0181(4) Uani 1 1 d . . .
C1 C 0.44978(9) 0.24534(11) 0.05005(10) 0.0131(5) Uani 1 1 d . . .
O1 O 0.41391(6) 0.25882(7) -0.00669(7) 0.0141(3) Uani 1 1 d . . .
C2 C 0.48274(10) 0.30003(11) 0.07892(11) 0.0144(5) Uani 1 1 d . . .
C3 C 0.51474(10) 0.28379(12) 0.13944(11) 0.0164(5) Uani 1 1 d . . .
H3 H 0.5372 0.3199 0.1601 0.020 Uiso 1 1 calc R . .
C4 C 0.51547(10) 0.21668(12) 0.17140(11) 0.0154(5) Uani 1 1 d . . .
C5 C 0.48466(10) 0.16400(11) 0.13838(11) 0.0156(5) Uani 1 1 d . . .
H5 H 0.4854 0.1178 0.1581 0.019 Uiso 1 1 calc R . .
C6 C 0.45254(10) 0.17678(11) 0.07688(10) 0.0132(5) Uani 1 1 d . . .
C7 C 0.48489(10) 0.37312(11) 0.04338(11) 0.0170(5) Uani 1 1 d . . .
C8 C 0.42658(10) 0.40835(11) 0.04232(12) 0.0212(6) Uani 1 1 d . . .
H8A H 0.4031 0.3857 0.0057 0.032 Uiso 1 1 calc R . .
H8B H 0.4307 0.4586 0.0310 0.032 Uiso 1 1 calc R . .
H8C H 0.4088 0.4032 0.0896 0.032 Uiso 1 1 calc R . .
C9 C 0.50703(11) 0.36430(12) -0.03411(11) 0.0202(6) Uani 1 1 d . . .
H9A H 0.5446 0.3433 -0.0328 0.030 Uiso 1 1 calc R . .
H9B H 0.5089 0.4105 -0.0575 0.030 Uiso 1 1 calc R . .
H9C H 0.4817 0.3334 -0.0612 0.030 Uiso 1 1 calc R . .
C10 C 0.52549(11) 0.42290(12) 0.08277(12) 0.0238(6) Uani 1 1 d . . .
H10A H 0.5126 0.4299 0.1323 0.036 Uiso 1 1 calc R . .
H10B H 0.5266 0.4685 0.0579 0.036 Uiso 1 1 calc R . .
H10C H 0.5632 0.4021 0.0832 0.036 Uiso 1 1 calc R . .
C11 C 0.55171(11) 0.20365(12) 0.23864(11) 0.0205(6) Uani 1 1 d . . .
C12 C 0.53902(12) 0.25929(13) 0.29634(11) 0.0300(6) Uani 1 1 d . . .
H12A H 0.5489 0.3062 0.2781 0.045 Uiso 1 1 calc R . .
H12B H 0.5611 0.2491 0.3396 0.045 Uiso 1 1 calc R . .
H12C H 0.4989 0.2581 0.3082 0.045 Uiso 1 1 calc R . .
C13 C 0.61399(11) 0.20817(16) 0.21800(13) 0.0344(7) Uani 1 1 d . . .
H13A H 0.6228 0.1711 0.1831 0.052 Uiso 1 1 calc R . .
H13B H 0.6372 0.2019 0.2611 0.052 Uiso 1 1 calc R . .
H13C H 0.6217 0.2544 0.1967 0.052 Uiso 1 1 calc R . .
C14 C 0.54021(12) 0.13093(12) 0.27109(12) 0.0267(6) Uani 1 1 d . . .
H14A H 0.5000 0.1262 0.2812 0.040 Uiso 1 1 calc R . .
H14B H 0.5615 0.1257 0.3159 0.040 Uiso 1 1 calc R . .
H14C H 0.5518 0.0943 0.2370 0.040 Uiso 1 1 calc R . .
C15 C 0.42217(10) 0.11576(11) 0.03852(10) 0.0133(5) Uani 1 1 d . . .
H15 H 0.4095 0.1347 -0.0090 0.016 Uiso 1 1 calc R . .
C16 C 0.46279(10) 0.05491(11) 0.02187(10) 0.0126(5) Uani 1 1 d . . .
C17 C 0.51944(10) 0.06786(11) 0.00756(11) 0.0151(5) Uani 1 1 d . . .
H17 H 0.5335 0.1145 0.0124 0.018 Uiso 1 1 calc R . .
C18 C 0.44423(10) -0.01447(11) 0.01351(11) 0.0151(5) Uani 1 1 d . . .
H18 H 0.4059 -0.0254 0.0224 0.018 Uiso 1 1 calc R . .
C19 C 0.31609(10) 0.11580(11) 0.05645(10) 0.0123(5) Uani 1 1 d . . .
O2 O 0.31266(6) 0.16350(7) 0.00057(7) 0.0143(3) Uani 1 1 d . . .
C20 C 0.36912(10) 0.09239(11) 0.07816(10) 0.0120(5) Uani 1 1 d . . .
C21 C 0.37266(10) 0.04665(11) 0.13696(10) 0.0146(5) Uani 1 1 d . . .
H21 H 0.4086 0.0316 0.1529 0.017 Uiso 1 1 calc R . .
C22 C 0.32550(10) 0.02259(11) 0.17268(11) 0.0157(5) Uani 1 1 d . . .
C23 C 0.27347(10) 0.04482(11) 0.14726(11) 0.0157(5) Uani 1 1 d . . .
H23 H 0.2408 0.0275 0.1706 0.019 Uiso 1 1 calc R . .
C24 C 0.26639(10) 0.09099(11) 0.08956(11) 0.0136(5) Uani 1 1 d . . .
C25 C 0.32881(10) -0.02849(12) 0.23680(11) 0.0210(6) Uani 1 1 d . . .
C26 C 0.30019(12) -0.09863(12) 0.21688(13) 0.0309(7) Uani 1 1 d . . .
H26A H 0.2607 -0.0899 0.2049 0.046 Uiso 1 1 calc R . .
H26B H 0.3024 -0.1312 0.2577 0.046 Uiso 1 1 calc R . .
H26C H 0.3192 -0.1195 0.1753 0.046 Uiso 1 1 calc R . .
C27 C 0.29861(13) 0.00378(14) 0.30196(12) 0.0359(7) Uani 1 1 d . . .
H27A H 0.3166 0.0485 0.3149 0.054 Uiso 1 1 calc R . .
H27B H 0.3008 -0.0289 0.3427 0.054 Uiso 1 1 calc R . .
H27C H 0.2591 0.0123 0.2898 0.054 Uiso 1 1 calc R . .
C28 C 0.38927(12) -0.04451(15) 0.25774(14) 0.0376(7) Uani 1 1 d . . .
H28A H 0.4089 -0.0655 0.2167 0.056 Uiso 1 1 calc R . .
H28B H 0.3897 -0.0776 0.2982 0.056 Uiso 1 1 calc R . .
H28C H 0.4082 -0.0007 0.2718 0.056 Uiso 1 1 calc R . .
C29 C 0.20796(10) 0.11311(11) 0.06360(11) 0.0163(5) Uani 1 1 d . . .
C30 C 0.16128(10) 0.07292(12) 0.10337(12) 0.0209(5) Uani 1 1 d . . .
H30A H 0.1666 0.0221 0.0967 0.031 Uiso 1 1 calc R . .
H30B H 0.1247 0.0868 0.0840 0.031 Uiso 1 1 calc R . .
H30C H 0.1628 0.0842 0.1547 0.031 Uiso 1 1 calc R . .
C31 C 0.20063(11) 0.09625(13) -0.01711(11) 0.0224(6) Uani 1 1 d . . .
H31A H 0.2294 0.1212 -0.0449 0.034 Uiso 1 1 calc R . .
H31B H 0.1633 0.1116 -0.0330 0.034 Uiso 1 1 calc R . .
H31C H 0.2045 0.0453 -0.0247 0.034 Uiso 1 1 calc R . .
C32 C 0.19819(11) 0.19234(12) 0.07677(13) 0.0238(6) Uani 1 1 d . . .
H32A H 0.2052 0.2033 0.1275 0.036 Uiso 1 1 calc R . .
H32B H 0.1593 0.2044 0.0647 0.036 Uiso 1 1 calc R . .
H32C H 0.2238 0.2198 0.0465 0.036 Uiso 1 1 calc R . .
O4 O 0.34241(7) 0.24079(8) -0.11810(7) 0.0175(4) Uani 1 1 d . . .
C41 C 0.37131(12) 0.29564(13) -0.15766(11) 0.0259(6) Uani 1 1 d . . .
H41A H 0.4125 0.2897 -0.1539 0.031 Uiso 1 1 calc R . .
H41B H 0.3611 0.3428 -0.1389 0.031 Uiso 1 1 calc R . .
C42 C 0.35213(12) 0.28730(14) -0.23477(12) 0.0316(7) Uani 1 1 d . . .
H42A H 0.3735 0.2499 -0.2598 0.038 Uiso 1 1 calc R . .
H42B H 0.3558 0.3320 -0.2618 0.038 Uiso 1 1 calc R . .
C43 C 0.29098(13) 0.26673(15) -0.22506(13) 0.0366(7) Uani 1 1 d . . .
H43A H 0.2772 0.2393 -0.2668 0.044 Uiso 1 1 calc R . .
H43B H 0.2670 0.3090 -0.2189 0.044 Uiso 1 1 calc R . .
C44 C 0.29141(11) 0.22169(13) -0.15686(12) 0.0262(6) Uani 1 1 d . . .
H44A H 0.2578 0.2316 -0.1272 0.031 Uiso 1 1 calc R . .
H44B H 0.2917 0.1709 -0.1692 0.031 Uiso 1 1 calc R . .
O5 O 0.29387(7) 0.32424(8) -0.02333(7) 0.0174(4) Uani 1 1 d . . .
C51 C 0.26845(11) 0.37898(12) 0.01890(12) 0.0247(6) Uani 1 1 d . . .
H51A H 0.2963 0.4166 0.0282 0.030 Uiso 1 1 calc R . .
H51B H 0.2564 0.3595 0.0658 0.030 Uiso 1 1 calc R . .
C52 C 0.21837(11) 0.40971(12) -0.01970(13) 0.0255(6) Uani 1 1 d . . .
H52A H 0.2304 0.4264 -0.0677 0.031 Uiso 1 1 calc R . .
H52B H 0.2046 0.4511 0.0076 0.031 Uiso 1 1 calc R . .
C53 C 0.17067(12) 0.35753(14) -0.02876(15) 0.0354(7) Uani 1 1 d . . .
H53A H 0.1840 0.3163 -0.0556 0.053 Uiso 1 1 calc R . .
H53B H 0.1399 0.3800 -0.0552 0.053 Uiso 1 1 calc R . .
H53C H 0.1573 0.3425 0.0186 0.053 Uiso 1 1 calc R . .
O6 O 0.15741(10) -0.04378(14) 0.29322(11) 0.0700(8) Uani 1 1 d . . .
C61 C 0.12750(15) -0.07350(17) 0.23563(14) 0.0495(9) Uani 1 1 d . . .
H61A H 0.1449 -0.1187 0.2209 0.059 Uiso 1 1 calc R . .
H61B H 0.1278 -0.0411 0.1939 0.059 Uiso 1 1 calc R . .
C62 C 0.06847(13) -0.08568(16) 0.26044(13) 0.0426(8) Uani 1 1 d . . .
H62A H 0.0434 -0.0472 0.2442 0.051 Uiso 1 1 calc R . .
H62B H 0.0539 -0.1312 0.2422 0.051 Uiso 1 1 calc R . .
C63 C 0.07320(13) -0.08654(18) 0.34060(14) 0.0469(8) Uani 1 1 d . . .
H63A H 0.0807 -0.1348 0.3586 0.056 Uiso 1 1 calc R . .
H63B H 0.0386 -0.0683 0.3634 0.056 Uiso 1 1 calc R . .
C64 C 0.12250(14) -0.03828(16) 0.35476(14) 0.0449(8) Uani 1 1 d . . .
H64A H 0.1096 0.0109 0.3614 0.054 Uiso 1 1 calc R . .
H64B H 0.1430 -0.0533 0.3984 0.054 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5871(14) . ?
V1 O5 1.7878(15) . ?
V1 O2 1.8187(15) . ?
V1 O1 1.8256(16) . ?
V1 O4 2.3307(13) . ?
C1 O1 1.382(2) . ?
C1 C6 1.394(3) . ?
C1 C2 1.407(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.536(3) . ?
C3 C4 1.404(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(3) . ?
C4 C11 1.540(3) . ?
C5 C6 1.397(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.540(3) . ?
C7 C10 1.537(3) . ?
C7 C8 1.541(3) . ?
C7 C9 1.544(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.530(3) . ?
C11 C13 1.534(3) . ?
C11 C12 1.535(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.528(3) . ?
C15 C16 1.537(3) . ?
C15 H15 1.0000 . ?
C16 C18 1.396(3) . ?
C16 C17 1.397(3) . ?
C17 C18 1.388(3) 5_655 ?
C17 H17 0.9500 . ?
C18 C17 1.388(3) 5_655 ?
C18 H18 0.9500 . ?
C19 O2 1.380(2) . ?
C19 C20 1.398(3) . ?
C19 C24 1.415(3) . ?
C20 C21 1.398(3) . ?
C21 C22 1.382(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(3) . ?
C22 C25 1.538(3) . ?
C23 C24 1.395(3) . ?
C23 H23 0.9500 . ?
C24 C29 1.532(3) . ?
C25 C28 1.522(3) . ?
C25 C27 1.536(3) . ?
C25 C26 1.539(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.537(3) . ?
C29 C32 1.540(3) . ?
C29 C31 1.545(3) . ?
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 . ?
O4 C41 1.448(3) . ?
O4 C44 1.458(3) . ?
C41 C42 1.514(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.519(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.529(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
O5 C51 1.435(3) . ?
C51 C52 1.509(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.516(4) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
O6 C61 1.404(3) . ?
O6 C64 1.419(3) . ?
C61 C62 1.498(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.495(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.512(4) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 V1 O5 100.20(7) . . ?
O3 V1 O2 100.05(7) . . ?
O5 V1 O2 119.29(7) . . ?
O3 V1 O1 99.63(7) . . ?
O5 V1 O1 120.16(7) . . ?
O2 V1 O1 111.73(7) . . ?
O3 V1 O4 178.12(7) . . ?
O5 V1 O4 78.36(6) . . ?
O2 V1 O4 81.73(6) . . ?
O1 V1 O4 80.16(6) . . ?
O1 C1 C6 118.37(19) . . ?
O1 C1 C2 120.02(18) . . ?
C6 C1 C2 121.61(19) . . ?
C1 O1 V1 120.04(12) . . ?
C3 C2 C1 116.78(19) . . ?
C3 C2 C7 121.9(2) . . ?
C1 C2 C7 121.27(19) . . ?
C2 C3 C4 123.3(2) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C5 C4 C3 117.37(19) . . ?
C5 C4 C11 122.84(19) . . ?
C3 C4 C11 119.7(2) . . ?
C4 C5 C6 121.9(2) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 118.7(2) . . ?
C1 C6 C15 120.83(18) . . ?
C5 C6 C15 120.42(18) . . ?
C2 C7 C10 111.71(18) . . ?
C2 C7 C8 111.50(19) . . ?
C10 C7 C8 107.86(18) . . ?
C2 C7 C9 108.39(18) . . ?
C10 C7 C9 107.25(19) . . ?
C8 C7 C9 110.04(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C11 C13 108.8(2) . . ?
C14 C11 C12 107.95(18) . . ?
C13 C11 C12 109.1(2) . . ?
C14 C11 C4 111.40(19) . . ?
C13 C11 C4 109.26(18) . . ?
C12 C11 C4 110.32(19) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 113.57(17) . . ?
C20 C15 C6 112.50(16) . . ?
C16 C15 C6 111.19(18) . . ?
C20 C15 H15 106.3 . . ?
C16 C15 H15 106.3 . . ?
C6 C15 H15 106.3 . . ?
C18 C16 C17 116.8(2) . . ?
C18 C16 C15 122.0(2) . . ?
C17 C16 C15 120.95(19) . . ?
C18 C17 C16 121.8(2) 5_655 . ?
C18 C17 H17 119.1 5_655 . ?
C16 C17 H17 119.1 . . ?
C17 C18 C16 121.4(2) 5_655 . ?
C17 C18 H18 119.3 5_655 . ?
C16 C18 H18 119.3 . . ?
O2 C19 C20 118.62(19) . . ?
O2 C19 C24 119.7(2) . . ?
C20 C19 C24 121.63(19) . . ?
C19 O2 V1 123.53(12) . . ?
C21 C20 C19 118.5(2) . . ?
C21 C20 C15 120.5(2) . . ?
C19 C20 C15 121.01(18) . . ?
C22 C21 C20 122.1(2) . . ?
C22 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C21 C22 C23 117.4(2) . . ?
C21 C22 C25 122.6(2) . . ?
C23 C22 C25 120.0(2) . . ?
C22 C23 C24 124.0(2) . . ?
C22 C23 H23 118.0 . . ?
C24 C23 H23 118.0 . . ?
C23 C24 C19 116.3(2) . . ?
C23 C24 C29 121.6(2) . . ?
C19 C24 C29 122.14(19) . . ?
C28 C25 C27 108.7(2) . . ?
C28 C25 C22 111.9(2) . . ?
C27 C25 C22 109.69(19) . . ?
C28 C25 C26 107.9(2) . . ?
C27 C25 C26 109.1(2) . . ?
C22 C25 C26 109.54(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 C30 111.70(18) . . ?
C24 C29 C32 110.74(19) . . ?
C30 C29 C32 107.33(19) . . ?
C24 C29 C31 110.63(18) . . ?
C30 C29 C31 106.46(18) . . ?
C32 C29 C31 109.84(18) . . ?
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 . . ?
C41 O4 C44 108.85(16) . . ?
C41 O4 V1 116.74(12) . . ?
C44 O4 V1 118.71(13) . . ?
O4 C41 C42 105.25(19) . . ?
O4 C41 H41A 110.7 . . ?
C42 C41 H41A 110.7 . . ?
O4 C41 H41B 110.7 . . ?
C42 C41 H41B 110.7 . . ?
H41A C41 H41B 108.8 . . ?
C41 C42 C43 101.74(19) . . ?
C41 C42 H42A 111.4 . . ?
C43 C42 H42A 111.4 . . ?
C41 C42 H42B 111.4 . . ?
C43 C42 H42B 111.4 . . ?
H42A C42 H42B 109.3 . . ?
C42 C43 C44 103.6(2) . . ?
C42 C43 H43A 111.0 . . ?
C44 C43 H43A 111.0 . . ?
C42 C43 H43B 111.0 . . ?
C44 C43 H43B 111.0 . . ?
H43A C43 H43B 109.0 . . ?
O4 C44 C43 106.1(2) . . ?
O4 C44 H44A 110.5 . . ?
C43 C44 H44A 110.5 . . ?
O4 C44 H44B 110.5 . . ?
C43 C44 H44B 110.5 . . ?
H44A C44 H44B 108.7 . . ?
C51 O5 V1 128.26(13) . . ?
O5 C51 C52 110.62(18) . . ?
O5 C51 H51A 109.5 . . ?
C52 C51 H51A 109.5 . . ?
O5 C51 H51B 109.5 . . ?
C52 C51 H51B 109.5 . . ?
H51A C51 H51B 108.1 . . ?
C51 C52 C53 113.2(2) . . ?
C51 C52 H52A 108.9 . . ?
C53 C52 H52A 108.9 . . ?
C51 C52 H52B 108.9 . . ?
C53 C52 H52B 108.9 . . ?
H52A C52 H52B 107.8 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C61 O6 C64 110.3(2) . . ?
O6 C61 C62 107.6(2) . . ?
O6 C61 H61A 110.2 . . ?
C62 C61 H61A 110.2 . . ?
O6 C61 H61B 110.2 . . ?
C62 C61 H61B 110.2 . . ?
H61A C61 H61B 108.5 . . ?
C63 C62 C61 103.8(2) . . ?
C63 C62 H62A 111.0 . . ?
C61 C62 H62A 111.0 . . ?
C63 C62 H62B 111.0 . . ?
C61 C62 H62B 111.0 . . ?
H62A C62 H62B 109.0 . . ?
C62 C63 C64 103.0(2) . . ?
C62 C63 H63A 111.2 . . ?
C64 C63 H63A 111.2 . . ?
C62 C63 H63B 111.2 . . ?
C64 C63 H63B 111.2 . . ?
H63A C63 H63B 109.1 . . ?
O6 C64 C63 105.7(2) . . ?
O6 C64 H64A 110.6 . . ?
C63 C64 H64A 110.6 . . ?
O6 C64 H64B 110.6 . . ?
C63 C64 H64B 110.6 . . ?
H64A C64 H64B 108.7 . . ?

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
C6 C1 O1 V1 67.8(2) . . . . ?
C2 C1 O1 V1 -112.72(18) . . . . ?
O3 V1 O1 C1 22.72(15) . . . . ?
O5 V1 O1 C1 130.55(14) . . . . ?
O2 V1 O1 C1 -82.25(15) . . . . ?
O4 V1 O1 C1 -159.17(14) . . . . ?
O1 C1 C2 C3 175.33(19) . . . . ?
C6 C1 C2 C3 -5.2(3) . . . . ?
O1 C1 C2 C7 -7.0(3) . . . . ?
C6 C1 C2 C7 172.4(2) . . . . ?
C1 C2 C3 C4 0.4(3) . . . . ?
C7 C2 C3 C4 -177.3(2) . . . . ?
C2 C3 C4 C5 3.1(3) . . . . ?
C2 C3 C4 C11 -179.5(2) . . . . ?
C3 C4 C5 C6 -1.9(3) . . . . ?
C11 C4 C5 C6 -179.2(2) . . . . ?
O1 C1 C6 C5 -174.11(18) . . . . ?
C2 C1 C6 C5 6.4(3) . . . . ?
O1 C1 C6 C15 7.5(3) . . . . ?
C2 C1 C6 C15 -171.93(19) . . . . ?
C4 C5 C6 C1 -2.7(3) . . . . ?
C4 C5 C6 C15 175.6(2) . . . . ?
C3 C2 C7 C10 -0.1(3) . . . . ?
C1 C2 C7 C10 -177.6(2) . . . . ?
C3 C2 C7 C8 -120.9(2) . . . . ?
C1 C2 C7 C8 61.6(3) . . . . ?
C3 C2 C7 C9 117.9(2) . . . . ?
C1 C2 C7 C9 -59.7(3) . . . . ?
C5 C4 C11 C14 -10.8(3) . . . . ?
C3 C4 C11 C14 171.9(2) . . . . ?
C5 C4 C11 C13 109.4(2) . . . . ?
C3 C4 C11 C13 -67.9(3) . . . . ?
C5 C4 C11 C12 -130.7(2) . . . . ?
C3 C4 C11 C12 52.0(3) . . . . ?
C1 C6 C15 C20 -105.2(2) . . . . ?
C5 C6 C15 C20 76.5(3) . . . . ?
C1 C6 C15 C16 126.1(2) . . . . ?
C5 C6 C15 C16 -52.2(3) . . . . ?
C20 C15 C16 C18 26.9(3) . . . . ?
C6 C15 C16 C18 154.99(18) . . . . ?
C20 C15 C16 C17 -159.34(18) . . . . ?
C6 C15 C16 C17 -31.3(3) . . . . ?
C18 C16 C17 C18 -0.4(3) . . . 5_655 ?
C15 C16 C17 C18 -174.47(18) . . . 5_655 ?
C17 C16 C18 C17 0.4(3) . . . 5_655 ?
C15 C16 C18 C17 174.40(18) . . . 5_655 ?
C20 C19 O2 V1 -67.2(2) . . . . ?
C24 C19 O2 V1 113.72(19) . . . . ?
O3 V1 O2 C19 -24.24(17) . . . . ?
O5 V1 O2 C19 -132.04(15) . . . . ?
O1 V1 O2 C19 80.44(16) . . . . ?
O4 V1 O2 C19 156.34(16) . . . . ?
O2 C19 C20 C21 177.03(17) . . . . ?
C24 C19 C20 C21 -3.9(3) . . . . ?
O2 C19 C20 C15 -3.3(3) . . . . ?
C24 C19 C20 C15 175.75(18) . . . . ?
C16 C15 C20 C21 46.0(3) . . . . ?
C6 C15 C20 C21 -81.4(2) . . . . ?
C16 C15 C20 C19 -133.68(19) . . . . ?
C6 C15 C20 C19 98.9(2) . . . . ?
C19 C20 C21 C22 1.8(3) . . . . ?
C15 C20 C21 C22 -177.88(18) . . . . ?
C20 C21 C22 C23 0.9(3) . . . . ?
C20 C21 C22 C25 179.18(19) . . . . ?
C21 C22 C23 C24 -1.7(3) . . . . ?
C25 C22 C23 C24 179.96(19) . . . . ?
C22 C23 C24 C19 -0.3(3) . . . . ?
C22 C23 C24 C29 179.49(19) . . . . ?
O2 C19 C24 C23 -177.83(17) . . . . ?
C20 C19 C24 C23 3.2(3) . . . . ?
O2 C19 C24 C29 2.4(3) . . . . ?
C20 C19 C24 C29 -176.59(18) . . . . ?
C21 C22 C25 C28 3.6(3) . . . . ?
C23 C22 C25 C28 -178.2(2) . . . . ?
C21 C22 C25 C27 124.3(2) . . . . ?
C23 C22 C25 C27 -57.5(3) . . . . ?
C21 C22 C25 C26 -116.1(2) . . . . ?
C23 C22 C25 C26 62.1(3) . . . . ?
C23 C24 C29 C30 -5.7(3) . . . . ?
C19 C24 C29 C30 174.05(18) . . . . ?
C23 C24 C29 C32 113.9(2) . . . . ?
C19 C24 C29 C32 -66.4(2) . . . . ?
C23 C24 C29 C31 -124.1(2) . . . . ?
C19 C24 C29 C31 55.6(3) . . . . ?
O3 V1 O4 C41 28(2) . . . . ?
O5 V1 O4 C41 68.33(16) . . . . ?
O2 V1 O4 C41 -169.36(16) . . . . ?
O1 V1 O4 C41 -55.47(16) . . . . ?
O3 V1 O4 C44 -105(2) . . . . ?
O5 V1 O4 C44 -65.17(15) . . . . ?
O2 V1 O4 C44 57.14(15) . . . . ?
O1 V1 O4 C44 171.03(15) . . . . ?
C44 O4 C41 C42 -24.5(3) . . . . ?
V1 O4 C41 C42 -162.26(16) . . . . ?
O4 C41 C42 C43 37.0(3) . . . . ?
C41 C42 C43 C44 -35.2(3) . . . . ?
C41 O4 C44 C43 1.7(3) . . . . ?
V1 O4 C44 C43 138.54(17) . . . . ?
C42 C43 C44 O4 21.4(3) . . . . ?
O3 V1 O5 C51 5.5(2) . . . . ?
O2 V1 O5 C51 113.21(18) . . . . ?
O1 V1 O5 C51 -102.02(18) . . . . ?
O4 V1 O5 C51 -173.28(19) . . . . ?
V1 O5 C51 C52 -158.24(16) . . . . ?
O5 C51 C52 C53 65.6(3) . . . . ?
C64 O6 C61 C62 2.3(4) . . . . ?
O6 C61 C62 C63 -20.6(3) . . . . ?
C61 C62 C63 C64 29.6(3) . . . . ?
C61 O6 C64 C63 16.9(3) . . . . ?
C62 C63 C64 O6 -29.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.30
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1404523'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;


_vrf_RFACR01_3                   
;
RESPONSE: The data obtained from the UK Synchrotron DLS I19
via the EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. The high wR-factor
is unexpected, but is probably a reflection that the crystal 
examined was poor quality. 
However, the structure refinement confirms the chemical entities
present and gives useful chemical information. 
;


_vrf_PLAT084_3                   
;
RESPONSE: The data obtained from the UK Synchrotron DLS I19
via the EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. The high wR-factor
is unexpected, but is probably a reflection that the crystal 
examined was poor quality. 
However, the structure refinement confirms the chemical entities
present and gives useful chemical information. 
;

_vrf_PLAT082_3                   
;
RESPONSE: The data obtained from the UK Synchrotron DLS I19
via the EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. The high wR-factor
is unexpected, but is probably a reflection that the crystal 
examined was poor quality. 
However, the structure refinement confirms the chemical entities
present and gives useful chemical information. 
;





_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C79.5 H4 N4 O10 V2'
_chemical_formula_weight         1216.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3080 0.5120 '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           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   20.18(2)
_cell_length_b                   15.820(16)
_cell_length_c                   26.50(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.686(11)
_cell_angle_gamma                90
_cell_volume                     7915(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7631
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      24.3

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_F_000             2412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.264
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           synchrotron
_diffrn_source                   'DLS beamline I19'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            30414
_diffrn_reflns_av_unetI/netI     0.1646
_diffrn_reflns_av_R_equivalents  0.2574
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.067
_diffrn_reflns_theta_max         18.060
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.422
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.422
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.422
_reflns_number_total             6040
_reflns_number_gt                3038
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;

_computing_structure_solution    SHEXLS-86
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6040
_refine_ls_number_parameters     578
_refine_ls_number_restraints     214
_refine_ls_R_factor_all          0.2851
_refine_ls_R_factor_gt           0.2176
_refine_ls_wR_factor_ref         0.5275
_refine_ls_wR_factor_gt          0.4767
_refine_ls_goodness_of_fit_ref   1.522
_refine_ls_restrained_S_all      1.505
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.008

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
C1 C 0.5830(12) 0.2349(14) 0.3482(9) 0.089(6) Uani 1 1 d . U . . .
C2 C 0.6568(12) 0.2258(13) 0.3487(9) 0.093(7) Uani 1 1 d . U . . .
C3 C 0.7092(10) 0.2635(12) 0.3892(8) 0.076(6) Uani 1 1 d . U . . .
C4 C 0.6930(11) 0.3155(13) 0.4259(8) 0.087(6) Uani 1 1 d . U . . .
C5 C 0.6243(12) 0.3327(13) 0.4222(9) 0.094(7) Uani 1 1 d . U . . .
C6 C 0.5709(12) 0.2893(14) 0.3823(9) 0.094(7) Uani 1 1 d . U . . .
C7 C 0.4887(14) 0.3070(16) 0.3739(10) 0.127(9) Uiso 1 1 d . . . . .
C8 C 0.4479(15) 0.2262(17) 0.3792(11) 0.137(9) Uiso 1 1 d . . . . .
C9 C 0.4477(13) 0.3532(15) 0.3148(10) 0.119(8) Uiso 1 1 d . . . . .
C10 C 0.4859(15) 0.3695(17) 0.4180(11) 0.139(9) Uiso 1 1 d . . . . .
C11 C 0.7547(12) 0.3615(13) 0.4696(9) 0.107(7) Uiso 1 1 d D . . . .
C12A C 0.7372(18) 0.397(2) 0.5184(12) 0.116(5) Uiso 0.659(18) 1 d D U P A 1
C13A C 0.8218(18) 0.2974(18) 0.4947(13) 0.116(5) Uiso 0.659(18) 1 d D U P A 1
C14A C 0.7851(18) 0.4371(18) 0.4449(13) 0.116(5) Uiso 0.659(18) 1 d D U P A 1
C12B C 0.736(3) 0.457(2) 0.466(2) 0.116(5) Uiso 0.341(18) 1 d D U P A 2
C14B C 0.829(2) 0.348(4) 0.467(3) 0.116(5) Uiso 0.341(18) 1 d D U P A 2
C13B C 0.750(3) 0.323(3) 0.5223(19) 0.116(5) Uiso 0.341(18) 1 d D U P A 2
C15 C 0.6686(11) 0.1724(12) 0.3034(8) 0.082(6) Uani 1 1 d . U . . .
C16 C 0.7137(9) 0.2211(11) 0.2762(7) 0.067(5) Uiso 1 1 d . . . . .
C17 C 0.7500 0.1755(17) 0.2500 0.082(8) Uiso 1 2 d S . P . .
C18 C 0.7116(12) 0.3136(14) 0.2767(9) 0.106(7) Uiso 1 1 d . . . . .
C19 C 0.7500 0.352(2) 0.2500 0.105(10) Uiso 1 2 d S . P . .
C20 C 0.6572(12) 0.0146(13) 0.3049(8) 0.077(6) Uani 1 1 d . U . . .
C21 C 0.7016(11) 0.0862(13) 0.3234(8) 0.080(6) Uani 1 1 d . U . . .
C22 C 0.7697(11) 0.0797(13) 0.3567(8) 0.084(6) Uani 1 1 d . U . . .
C23 C 0.7995(12) 0.0007(15) 0.3753(9) 0.098(7) Uani 1 1 d . U . . .
C24 C 0.7599(12) -0.0713(14) 0.3581(9) 0.099(7) Uani 1 1 d . U . . .
C25 C 0.6883(12) -0.0614(15) 0.3227(9) 0.099(7) Uani 1 1 d . U . . .
C26 C 0.6450(13) -0.1452(15) 0.2978(10) 0.117(8) Uiso 1 1 d . . . . .
C27 C 0.6939(13) -0.2299(15) 0.3146(10) 0.117(8) Uiso 1 1 d . . . . .
C28 C 0.6138(13) -0.1441(14) 0.2385(10) 0.112(8) Uiso 1 1 d . . . . .
C29 C 0.5874(16) -0.1545(17) 0.3288(11) 0.145(10) Uiso 1 1 d . . . . .
C30 C 0.8785(13) -0.0055(12) 0.4151(9) 0.109(7) Uiso 1 1 d D . . . .
C31A C 0.904(2) -0.0985(17) 0.4271(15) 0.116(5) Uiso 0.545(18) 1 d D U P B 1
C32A C 0.885(2) 0.043(2) 0.4680(13) 0.116(5) Uiso 0.545(18) 1 d D U P B 1
C33A C 0.923(2) 0.042(2) 0.3856(15) 0.116(5) Uiso 0.545(18) 1 d D U P B 1
C31B C 0.868(2) -0.040(3) 0.4674(14) 0.116(5) Uiso 0.455(18) 1 d D U P B 2
C32B C 0.920(2) -0.074(2) 0.3951(18) 0.116(5) Uiso 0.455(18) 1 d D U P B 2
C33B C 0.923(2) 0.078(2) 0.4291(18) 0.116(5) Uiso 0.455(18) 1 d D U P B 2
C34 C 0.1682(13) 0.6164(15) 0.3205(8) 0.091(7) Uani 1 1 d . U . . .
C35 C 0.2093(10) 0.5444(13) 0.3299(8) 0.078(6) Uani 1 1 d . U . . .
C36 C 0.2852(12) 0.5556(14) 0.3564(8) 0.093(7) Uani 1 1 d . U . . .
C37 C 0.3133(12) 0.6365(16) 0.3689(9) 0.102(7) Uani 1 1 d . U . . .
C38 C 0.2735(11) 0.7082(14) 0.3572(8) 0.093(7) Uani 1 1 d . U . . .
C39 C 0.1976(12) 0.6972(15) 0.3302(9) 0.098(7) Uani 1 1 d . U . . .
C40 C 0.1535(15) 0.7777(17) 0.3193(11) 0.131(9) Uiso 1 1 d . . . . .
C41 C 0.1126(14) 0.7811(16) 0.2580(11) 0.131(9) Uiso 1 1 d . . . . .
C42 C 0.2028(16) 0.8617(19) 0.3325(11) 0.151(10) Uiso 1 1 d . . . . .
C43 C 0.1019(15) 0.7843(17) 0.3508(11) 0.142(9) Uiso 1 1 d . . . . .
C44 C 0.4026(16) 0.6355(19) 0.4003(12) 0.147(10) Uiso 1 1 d . . . . .
C45 C 0.4275(17) 0.578(2) 0.4479(13) 0.167(12) Uiso 1 1 d . . . . .
C46 C 0.4334(16) 0.5959(18) 0.3526(12) 0.157(11) Uiso 1 1 d . . . . .
C47 C 0.4206(17) 0.730(2) 0.4071(12) 0.163(11) Uiso 1 1 d . . . . .
C48 C 0.1780(9) 0.4618(11) 0.3132(7) 0.067(5) Uani 1 1 d . U . . .
C49 C 0.2186(10) 0.4105(12) 0.2832(8) 0.079(6) Uiso 1 1 d . . . . .
C50 C 0.2500 0.4575(17) 0.2500 0.084(9) Uiso 1 2 d S . P . .
C51 C 0.2215(10) 0.3238(13) 0.2819(8) 0.085(6) Uiso 1 1 d . . . . .
C52 C 0.2500 0.2786(17) 0.2500 0.084(9) Uiso 1 2 d S . P . .
C53 C 0.1038(12) 0.4004(14) 0.3657(9) 0.086(6) Uani 1 1 d . U . . .
C54 C 0.1729(12) 0.4126(13) 0.3610(9) 0.090(6) Uani 1 1 d . U . . .
C55 C 0.2308(10) 0.3717(13) 0.3978(9) 0.081(6) Uani 1 1 d . U . . .
C56 C 0.2266(11) 0.3312(14) 0.4408(9) 0.095(7) Uani 1 1 d . U . . .
C57 C 0.1585(14) 0.3144(15) 0.4478(10) 0.114(8) Uani 1 1 d . U . . .
C58 C 0.1014(12) 0.3545(14) 0.4091(10) 0.098(7) Uani 1 1 d . U . . .
C59 C 0.0199(17) 0.3407(19) 0.4110(12) 0.153(10) Uiso 1 1 d . . . . .
C60 C 0.0269(15) 0.2782(16) 0.4624(11) 0.139(9) Uiso 1 1 d . . . . .
C61 C -0.0290(14) 0.2993(15) 0.3589(10) 0.127(9) Uiso 1 1 d . . . . .
C62 C -0.0057(14) 0.4241(17) 0.4266(11) 0.136(9) Uiso 1 1 d . . . . .
C63 C 0.2909(13) 0.2895(15) 0.4866(10) 0.110(8) Uiso 1 1 d . . . . .
C64 C 0.2753(19) 0.248(2) 0.5331(15) 0.197(14) Uiso 1 1 d . . . . .
C65 C 0.349(2) 0.357(2) 0.5069(15) 0.204(14) Uiso 1 1 d . . . . .
C66 C 0.3249(15) 0.2265(17) 0.4593(11) 0.141(9) Uiso 1 1 d . . . . .
C71 C 0.4486(18) 0.042(2) 0.1850(14) 0.165(12) Uiso 1 1 d . . . . .
C72 C 0.3991(18) 0.084(2) 0.1259(14) 0.171(12) Uiso 1 1 d . . . . .
C73 C 0.3511(16) 0.1354(18) 0.1514(12) 0.151(10) Uiso 1 1 d . . . . .
C74 C 0.4082(17) 0.1653(19) 0.2062(12) 0.148(10) Uiso 1 1 d . . . . .
C81 C -0.0827(16) 0.4680(18) 0.2359(12) 0.142(10) Uiso 1 1 d . . . . .
C82 C -0.1449(16) 0.4980(18) 0.1834(12) 0.144(10) Uiso 1 1 d . . . . .
C83 C -0.1090(14) 0.5615(16) 0.1600(11) 0.130(9) Uiso 1 1 d . . . . .
C84 C -0.0540(16) 0.6018(19) 0.2114(12) 0.141(10) Uiso 1 1 d . . . . .
C91 C 0.4344(19) -0.014(2) 0.3407(14) 0.169(12) Uiso 1 1 d . . . . .
C92 C 0.359(2) -0.032(3) 0.3311(16) 0.211(15) Uiso 1 1 d . . . . .
C93 C 0.317(2) 0.052(2) 0.3252(16) 0.209(15) Uiso 1 1 d . . . . .
C101 C -0.0449(17) 0.6477(19) 0.3739(13) 0.154(11) Uiso 1 1 d . . . . .
C102 C -0.127(2) 0.672(2) 0.3634(14) 0.189(13) Uiso 1 1 d . . . . .
C103 C -0.156(2) 0.594(2) 0.3683(15) 0.200(14) Uiso 1 1 d . . . . .
O1 O 0.5312(7) 0.1899(10) 0.3064(6) 0.110(5) Uani 1 1 d . . . . .
O2 O 0.5892(6) 0.0250(9) 0.2795(6) 0.100(5) Uani 1 1 d . . . . .
O3 O 0.0960(6) 0.6101(9) 0.2976(6) 0.094(4) Uani 1 1 d . . . . .
O4 O 0.0493(7) 0.4433(8) 0.3305(6) 0.092(4) Uani 1 1 d . . . . .
O5 O 0.5713(8) 0.0594(10) 0.3700(7) 0.124(5) Uani 1 1 d . . . . .
O6 O 0.0938(7) 0.5750(11) 0.3937(6) 0.126(6) Uani 1 1 d . . . . .
O7 O 0.4679(7) 0.1022(10) 0.2190(7) 0.124(6) Uani 1 1 d . . . . .
O8 O -0.0267(7) 0.5317(11) 0.2459(8) 0.137(6) Uani 1 1 d . . . . .
O10 O -0.0374(7) 0.6069(10) 0.3292(6) 0.114(5) Uani 1 1 d . . . . .
O90 O 0.4465(8) 0.0250(11) 0.2986(7) 0.136(6) Uani 1 1 d . . . . .
V1 V 0.5258(2) 0.0753(3) 0.3050(2) 0.1188(19) Uani 1 1 d . . . . .
V2 V 0.04269(18) 0.5584(3) 0.33066(19) 0.1095(18) Uani 1 1 d . . . . .
C112 C 0.659(3) 0.111(3) 0.501(3) 0.18(3) Uiso 0.5 1 d D . P . .
C113 C 0.711(3) 0.061(4) 0.489(3) 0.17(2) Uiso 0.5 1 d D . P . .
C111 C 0.609(3) 0.049(5) 0.508(3) 0.22(3) Uiso 0.5 1 d D . 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
C1 C6 1.33(3) . ?
C1 O1 1.42(2) . ?
C1 C2 1.49(3) . ?
C2 C3 1.35(3) . ?
C2 C15 1.55(3) . ?
C3 C4 1.40(2) . ?
C4 C5 1.38(3) . ?
C4 C11 1.55(3) . ?
C5 C6 1.39(3) . ?
C6 C7 1.62(3) . ?
C7 C10 1.55(3) . ?
C7 C8 1.55(3) . ?
C7 C9 1.66(3) . ?
C11 C14B 1.55(2) . ?
C11 C12B 1.56(2) . ?
C11 C13B 1.56(2) . ?
C11 C12A 1.56(2) . ?
C11 C14A 1.59(2) . ?
C11 C13A 1.63(3) . ?
C15 C21 1.53(3) . ?
C15 C16 1.55(2) . ?
C16 C17 1.38(2) . ?
C16 C18 1.46(2) . ?
C17 C16 1.38(2) 2_655 ?
C18 C19 1.36(2) . ?
C19 C18 1.36(2) 2_655 ?
C20 O2 1.31(2) . ?
C20 C25 1.36(3) . ?
C20 C21 1.42(3) . ?
C21 C22 1.35(2) . ?
C22 C23 1.40(3) . ?
C23 C24 1.37(3) . ?
C23 C30 1.57(3) . ?
C24 C25 1.43(3) . ?
C25 C26 1.60(3) . ?
C26 C28 1.47(3) . ?
C26 C27 1.63(3) . ?
C26 C29 1.65(4) . ?
C30 C31A 1.55(2) . ?
C30 C32A 1.56(2) . ?
C30 C33B 1.57(2) . ?
C30 C33A 1.57(2) . ?
C30 C32B 1.58(2) . ?
C30 C31B 1.58(2) . ?
C34 O3 1.37(2) . ?
C34 C35 1.38(3) . ?
C34 C39 1.39(3) . ?
C35 C48 1.45(2) . ?
C35 C36 1.45(3) . ?
C36 C37 1.39(3) . ?
C37 C38 1.36(3) . ?
C37 C44 1.70(3) . ?
C38 C39 1.45(3) . ?
C39 C40 1.52(3) . ?
C40 C41 1.54(3) . ?
C40 C43 1.55(4) . ?
C40 C42 1.62(3) . ?
C44 C45 1.49(4) . ?
C44 C47 1.53(4) . ?
C44 C46 1.71(4) . ?
C48 C54 1.52(3) . ?
C48 C49 1.56(2) . ?
C49 C51 1.37(2) . ?
C49 C50 1.46(2) . ?
C50 C49 1.46(2) 2 ?
C51 C52 1.38(2) . ?
C52 C51 1.38(2) 2 ?
C53 O4 1.35(2) . ?
C53 C58 1.38(3) . ?
C53 C54 1.46(3) . ?
C54 C55 1.39(3) . ?
C55 C56 1.34(2) . ?
C56 C57 1.47(3) . ?
C56 C63 1.57(3) . ?
C57 C58 1.40(3) . ?
C58 C59 1.68(4) . ?
C59 C61 1.53(3) . ?
C59 C62 1.53(3) . ?
C59 C60 1.65(4) . ?
C63 C64 1.52(4) . ?
C63 C66 1.53(3) . ?
C63 C65 1.54(4) . ?
C71 O7 1.27(3) . ?
C71 C72 1.67(4) . ?
C72 C73 1.59(4) . ?
C73 C74 1.57(4) . ?
C74 O7 1.51(3) . ?
C81 O8 1.47(3) . ?
C81 C82 1.58(4) . ?
C82 C83 1.49(3) . ?
C83 C84 1.56(3) . ?
C84 O8 1.42(3) . ?
C91 O90 1.37(4) . ?
C91 C92 1.49(5) . ?
C92 C93 1.55(4) . ?
C101 O10 1.40(3) . ?
C101 C102 1.62(4) . ?
C102 C103 1.39(4) . ?
O1 V1 1.816(16) . ?
O2 V1 1.828(13) . ?
O3 V2 1.806(13) . ?
O4 V2 1.826(14) . ?
O5 V1 1.661(18) . ?
O6 V2 1.644(16) . ?
O7 V1 2.204(18) . ?
O8 V2 2.23(2) . ?
O10 V2 1.777(15) . ?
O90 V1 1.741(16) . ?
C112 C113 1.45(2) . ?
C112 C111 1.45(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
C6 C1 O1 126(2) . . ?
C6 C1 C2 119(2) . . ?
O1 C1 C2 114.6(19) . . ?
C3 C2 C1 118(2) . . ?
C3 C2 C15 124(2) . . ?
C1 C2 C15 118(2) . . ?
C2 C3 C4 120(2) . . ?
C5 C4 C3 123(2) . . ?
C5 C4 C11 119(2) . . ?
C3 C4 C11 118.2(18) . . ?
C4 C5 C6 116(2) . . ?
C1 C6 C5 124(2) . . ?
C1 C6 C7 116(2) . . ?
C5 C6 C7 120(2) . . ?
C10 C7 C8 107(2) . . ?
C10 C7 C6 108(2) . . ?
C8 C7 C6 113(2) . . ?
C10 C7 C9 107(2) . . ?
C8 C7 C9 110(2) . . ?
C6 C7 C9 110.6(19) . . ?
C14B C11 C4 116(3) . . ?
C14B C11 C12B 110.9(18) . . ?
C4 C11 C12B 107(3) . . ?
C14B C11 C13B 111.0(17) . . ?
C4 C11 C13B 101(3) . . ?
C12B C11 C13B 109.9(17) . . ?
C4 C11 C12A 116(2) . . ?
C4 C11 C14A 112(2) . . ?
C12A C11 C14A 107.6(16) . . ?
C4 C11 C13A 110.2(19) . . ?
C12A C11 C13A 106.6(16) . . ?
C14A C11 C13A 104.5(16) . . ?
C21 C15 C16 110.5(16) . . ?
C21 C15 C2 112.6(16) . . ?
C16 C15 C2 111.4(16) . . ?
C17 C16 C18 123(2) . . ?
C17 C16 C15 118.5(16) . . ?
C18 C16 C15 117.9(17) . . ?
C16 C17 C16 117(2) 2_655 . ?
C19 C18 C16 114(2) . . ?
C18 C19 C18 127(3) 2_655 . ?
O2 C20 C25 124(2) . . ?
O2 C20 C21 119.8(18) . . ?
C25 C20 C21 115.4(19) . . ?
C22 C21 C20 122.5(19) . . ?
C22 C21 C15 120.8(19) . . ?
C20 C21 C15 116.6(18) . . ?
C21 C22 C23 121(2) . . ?
C24 C23 C22 120(2) . . ?
C24 C23 C30 120(2) . . ?
C22 C23 C30 120(2) . . ?
C23 C24 C25 118(2) . . ?
C20 C25 C24 124(2) . . ?
C20 C25 C26 118(2) . . ?
C24 C25 C26 117(2) . . ?
C28 C26 C25 113.4(19) . . ?
C28 C26 C27 106.9(19) . . ?
C25 C26 C27 112.3(19) . . ?
C28 C26 C29 115(2) . . ?
C25 C26 C29 104.3(19) . . ?
C27 C26 C29 104.8(19) . . ?
C31A C30 C32A 111.3(15) . . ?
C31A C30 C33A 110.2(15) . . ?
C32A C30 C33A 109.2(15) . . ?
C33B C30 C32B 109.2(16) . . ?
C33B C30 C31B 109.3(15) . . ?
C32B C30 C31B 108.1(15) . . ?
C31A C30 C23 112(2) . . ?
C32A C30 C23 109(2) . . ?
C33B C30 C23 118(2) . . ?
C33A C30 C23 105(2) . . ?
C32B C30 C23 111(2) . . ?
C31B C30 C23 101(2) . . ?
O3 C34 C35 119.9(19) . . ?
O3 C34 C39 118(2) . . ?
C35 C34 C39 122(2) . . ?
C34 C35 C48 121.2(18) . . ?
C34 C35 C36 116.8(19) . . ?
C48 C35 C36 121.9(19) . . ?
C37 C36 C35 120(2) . . ?
C38 C37 C36 124(2) . . ?
C38 C37 C44 124(2) . . ?
C36 C37 C44 112(2) . . ?
C37 C38 C39 117(2) . . ?
C34 C39 C38 120(2) . . ?
C34 C39 C40 123(2) . . ?
C38 C39 C40 116(2) . . ?
C39 C40 C41 107(2) . . ?
C39 C40 C43 114(2) . . ?
C41 C40 C43 111(2) . . ?
C39 C40 C42 112(2) . . ?
C41 C40 C42 105(2) . . ?
C43 C40 C42 108(2) . . ?
C45 C44 C47 120(3) . . ?
C45 C44 C37 114(2) . . ?
C47 C44 C37 102(2) . . ?
C45 C44 C46 107(2) . . ?
C47 C44 C46 108(2) . . ?
C37 C44 C46 104(2) . . ?
C35 C48 C54 111.0(16) . . ?
C35 C48 C49 112.0(15) . . ?
C54 C48 C49 111.2(16) . . ?
C51 C49 C50 118(2) . . ?
C51 C49 C48 124.5(18) . . ?
C50 C49 C48 117.5(16) . . ?
C49 C50 C49 119(2) 2 . ?
C49 C51 C52 124(2) . . ?
C51 C52 C51 118(3) . 2 ?
O4 C53 C58 126(2) . . ?
O4 C53 C54 116.4(19) . . ?
C58 C53 C54 117(2) . . ?
C55 C54 C53 118(2) . . ?
C55 C54 C48 122.4(19) . . ?
C53 C54 C48 119.2(19) . . ?
C56 C55 C54 122.1(19) . . ?
C55 C56 C57 122(2) . . ?
C55 C56 C63 125(2) . . ?
C57 C56 C63 112(2) . . ?
C58 C57 C56 113(2) . . ?
C53 C58 C57 126(2) . . ?
C53 C58 C59 115(2) . . ?
C57 C58 C59 119(2) . . ?
C61 C59 C62 116(2) . . ?
C61 C59 C60 109(2) . . ?
C62 C59 C60 103(2) . . ?
C61 C59 C58 111(2) . . ?
C62 C59 C58 109(2) . . ?
C60 C59 C58 108(2) . . ?
C64 C63 C66 111(2) . . ?
C64 C63 C65 111(3) . . ?
C66 C63 C65 102(2) . . ?
C64 C63 C56 117(2) . . ?
C66 C63 C56 107(2) . . ?
C65 C63 C56 107(2) . . ?
O7 C71 C72 107(3) . . ?
C73 C72 C71 93(2) . . ?
C74 C73 C72 101(2) . . ?
O7 C74 C73 106(2) . . ?
O8 C81 C82 106(2) . . ?
C83 C82 C81 102(2) . . ?
C82 C83 C84 102(2) . . ?
O8 C84 C83 104(2) . . ?
O90 C91 C92 115(3) . . ?
C91 C92 C93 110(3) . . ?
O10 C101 C102 112(3) . . ?
C103 C102 C101 103(3) . . ?
C1 O1 V1 122.6(13) . . ?
C20 O2 V1 127.5(13) . . ?
C34 O3 V2 122.7(13) . . ?
C53 O4 V2 122.8(13) . . ?
C71 O7 C74 108(2) . . ?
C71 O7 V1 120.3(19) . . ?
C74 O7 V1 116.8(15) . . ?
C84 O8 C81 109(2) . . ?
C84 O8 V2 117.7(16) . . ?
C81 O8 V2 118.9(15) . . ?
C101 O10 V2 123.3(17) . . ?
C91 O90 V1 123(2) . . ?
O5 V1 O90 100.6(8) . . ?
O5 V1 O1 97.1(8) . . ?
O90 V1 O1 120.3(7) . . ?
O5 V1 O2 96.6(7) . . ?
O90 V1 O2 120.3(8) . . ?
O1 V1 O2 113.4(6) . . ?
O5 V1 O7 177.3(7) . . ?
O90 V1 O7 81.6(7) . . ?
O1 V1 O7 80.4(7) . . ?
O2 V1 O7 83.5(6) . . ?
O6 V2 O10 101.1(8) . . ?
O6 V2 O3 98.8(7) . . ?
O10 V2 O3 119.1(7) . . ?
O6 V2 O4 98.2(8) . . ?
O10 V2 O4 119.9(6) . . ?
O3 V2 O4 113.2(6) . . ?
O6 V2 O8 178.2(8) . . ?
O10 V2 O8 79.4(7) . . ?
O3 V2 O8 82.3(6) . . ?
O4 V2 O8 80.1(6) . . ?
C113 C112 C111 104.9(19) . . ?

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
C6 C1 C2 C3 10(3) . . . . ?
O1 C1 C2 C3 -176.7(18) . . . . ?
C6 C1 C2 C15 -171.2(19) . . . . ?
O1 C1 C2 C15 2(3) . . . . ?
C1 C2 C3 C4 -6(3) . . . . ?
C15 C2 C3 C4 175.3(18) . . . . ?
C2 C3 C4 C5 -2(3) . . . . ?
C2 C3 C4 C11 -176.5(18) . . . . ?
C3 C4 C5 C6 5(3) . . . . ?
C11 C4 C5 C6 -179.8(19) . . . . ?
O1 C1 C6 C5 -179(2) . . . . ?
C2 C1 C6 C5 -6(3) . . . . ?
O1 C1 C6 C7 -1(3) . . . . ?
C2 C1 C6 C7 171.1(19) . . . . ?
C4 C5 C6 C1 -1(3) . . . . ?
C4 C5 C6 C7 -179(2) . . . . ?
C1 C6 C7 C10 178(2) . . . . ?
C5 C6 C7 C10 -4(3) . . . . ?
C1 C6 C7 C8 60(3) . . . . ?
C5 C6 C7 C8 -123(2) . . . . ?
C1 C6 C7 C9 -65(3) . . . . ?
C5 C6 C7 C9 113(2) . . . . ?
C5 C4 C11 C14B -172(3) . . . . ?
C3 C4 C11 C14B 3(3) . . . . ?
C5 C4 C11 C12B -48(3) . . . . ?
C3 C4 C11 C12B 127(3) . . . . ?
C5 C4 C11 C13B 67(3) . . . . ?
C3 C4 C11 C13B -118(3) . . . . ?
C5 C4 C11 C12A 22(3) . . . . ?
C3 C4 C11 C12A -163.4(19) . . . . ?
C5 C4 C11 C14A -102(2) . . . . ?
C3 C4 C11 C14A 73(2) . . . . ?
C5 C4 C11 C13A 142(2) . . . . ?
C3 C4 C11 C13A -43(2) . . . . ?
C3 C2 C15 C21 73(3) . . . . ?
C1 C2 C15 C21 -106(2) . . . . ?
C3 C2 C15 C16 -52(3) . . . . ?
C1 C2 C15 C16 129.6(19) . . . . ?
C21 C15 C16 C17 31(2) . . . . ?
C2 C15 C16 C17 157.2(15) . . . . ?
C21 C15 C16 C18 -152.7(17) . . . . ?
C2 C15 C16 C18 -27(2) . . . . ?
C18 C16 C17 C16 0.7(14) . . . 2_655 ?
C15 C16 C17 C16 176.6(18) . . . 2_655 ?
C17 C16 C18 C19 -1(3) . . . . ?
C15 C16 C18 C19 -177.3(15) . . . . ?
C16 C18 C19 C18 0.6(12) . . . 2_655 ?
O2 C20 C21 C22 169.8(19) . . . . ?
C25 C20 C21 C22 0(3) . . . . ?
O2 C20 C21 C15 -11(3) . . . . ?
C25 C20 C21 C15 179.0(18) . . . . ?
C16 C15 C21 C22 54(2) . . . . ?
C2 C15 C21 C22 -71(2) . . . . ?
C16 C15 C21 C20 -125.0(18) . . . . ?
C2 C15 C21 C20 110(2) . . . . ?
C20 C21 C22 C23 -1(3) . . . . ?
C15 C21 C22 C23 179.5(19) . . . . ?
C21 C22 C23 C24 2(3) . . . . ?
C21 C22 C23 C30 -178.6(19) . . . . ?
C22 C23 C24 C25 -2(3) . . . . ?
C30 C23 C24 C25 179.0(19) . . . . ?
O2 C20 C25 C24 -169(2) . . . . ?
C21 C20 C25 C24 1(3) . . . . ?
O2 C20 C25 C26 18(3) . . . . ?
C21 C20 C25 C26 -172.4(18) . . . . ?
C23 C24 C25 C20 0(3) . . . . ?
C23 C24 C25 C26 174(2) . . . . ?
C20 C25 C26 C28 48(3) . . . . ?
C24 C25 C26 C28 -125(2) . . . . ?
C20 C25 C26 C27 170(2) . . . . ?
C24 C25 C26 C27 -4(3) . . . . ?
C20 C25 C26 C29 -78(2) . . . . ?
C24 C25 C26 C29 109(2) . . . . ?
C24 C23 C30 C31A 4(3) . . . . ?
C22 C23 C30 C31A -175(2) . . . . ?
C24 C23 C30 C32A -119(2) . . . . ?
C22 C23 C30 C32A 62(2) . . . . ?
C24 C23 C30 C33B 175(2) . . . . ?
C22 C23 C30 C33B -5(3) . . . . ?
C24 C23 C30 C33A 124(2) . . . . ?
C22 C23 C30 C33A -55(2) . . . . ?
C24 C23 C30 C32B 48(3) . . . . ?
C22 C23 C30 C32B -131(2) . . . . ?
C24 C23 C30 C31B -67(3) . . . . ?
C22 C23 C30 C31B 114(2) . . . . ?
O3 C34 C35 C48 3(3) . . . . ?
C39 C34 C35 C48 -172.1(19) . . . . ?
O3 C34 C35 C36 -177.6(17) . . . . ?
C39 C34 C35 C36 7(3) . . . . ?
C34 C35 C36 C37 -3(3) . . . . ?
C48 C35 C36 C37 176.3(19) . . . . ?
C35 C36 C37 C38 -1(3) . . . . ?
C35 C36 C37 C44 179.2(18) . . . . ?
C36 C37 C38 C39 0(3) . . . . ?
C44 C37 C38 C39 -180(2) . . . . ?
O3 C34 C39 C38 176.6(18) . . . . ?
C35 C34 C39 C38 -8(3) . . . . ?
O3 C34 C39 C40 3(3) . . . . ?
C35 C34 C39 C40 179(2) . . . . ?
C37 C38 C39 C34 4(3) . . . . ?
C37 C38 C39 C40 178(2) . . . . ?
C34 C39 C40 C41 -63(3) . . . . ?
C38 C39 C40 C41 123(2) . . . . ?
C34 C39 C40 C43 59(3) . . . . ?
C38 C39 C40 C43 -114(2) . . . . ?
C34 C39 C40 C42 -178(2) . . . . ?
C38 C39 C40 C42 8(3) . . . . ?
C38 C37 C44 C45 128(3) . . . . ?
C36 C37 C44 C45 -52(3) . . . . ?
C38 C37 C44 C47 -3(3) . . . . ?
C36 C37 C44 C47 177(2) . . . . ?
C38 C37 C44 C46 -115(2) . . . . ?
C36 C37 C44 C46 65(2) . . . . ?
C34 C35 C48 C54 -103(2) . . . . ?
C36 C35 C48 C54 78(2) . . . . ?
C34 C35 C48 C49 132.5(19) . . . . ?
C36 C35 C48 C49 -46(2) . . . . ?
C35 C48 C49 C51 152.4(19) . . . . ?
C54 C48 C49 C51 28(3) . . . . ?
C35 C48 C49 C50 -34(2) . . . . ?
C54 C48 C49 C50 -158.5(15) . . . . ?
C51 C49 C50 C49 1.0(13) . . . 2 ?
C48 C49 C50 C49 -173.3(18) . . . 2 ?
C50 C49 C51 C52 -2(3) . . . . ?
C48 C49 C51 C52 171.7(15) . . . . ?
C49 C51 C52 C51 1.2(14) . . . 2 ?
O4 C53 C54 C55 177.9(18) . . . . ?
C58 C53 C54 C55 5(3) . . . . ?
O4 C53 C54 C48 -8(3) . . . . ?
C58 C53 C54 C48 179.1(19) . . . . ?
C35 C48 C54 C55 -79(2) . . . . ?
C49 C48 C54 C55 47(3) . . . . ?
C35 C48 C54 C53 108(2) . . . . ?
C49 C48 C54 C53 -127.2(19) . . . . ?
C53 C54 C55 C56 -9(3) . . . . ?
C48 C54 C55 C56 177(2) . . . . ?
C54 C55 C56 C57 11(3) . . . . ?
C54 C55 C56 C63 -175(2) . . . . ?
C55 C56 C57 C58 -8(3) . . . . ?
C63 C56 C57 C58 176.9(19) . . . . ?
O4 C53 C58 C57 -176(2) . . . . ?
C54 C53 C58 C57 -4(3) . . . . ?
O4 C53 C58 C59 10(3) . . . . ?
C54 C53 C58 C59 -178(2) . . . . ?
C56 C57 C58 C53 5(4) . . . . ?
C56 C57 C58 C59 179(2) . . . . ?
C53 C58 C59 C61 56(3) . . . . ?
C57 C58 C59 C61 -119(3) . . . . ?
C53 C58 C59 C62 -73(3) . . . . ?
C57 C58 C59 C62 112(3) . . . . ?
C53 C58 C59 C60 175(2) . . . . ?
C57 C58 C59 C60 0(3) . . . . ?
C55 C56 C63 C64 178(2) . . . . ?
C57 C56 C63 C64 -7(3) . . . . ?
C55 C56 C63 C66 -56(3) . . . . ?
C57 C56 C63 C66 119(2) . . . . ?
C55 C56 C63 C65 52(3) . . . . ?
C57 C56 C63 C65 -133(2) . . . . ?
O7 C71 C72 C73 -49(3) . . . . ?
C71 C72 C73 C74 39(3) . . . . ?
C72 C73 C74 O7 -25(3) . . . . ?
O8 C81 C82 C83 16(3) . . . . ?
C81 C82 C83 C84 -34(3) . . . . ?
C82 C83 C84 O8 42(3) . . . . ?
O90 C91 C92 C93 -65(4) . . . . ?
O10 C101 C102 C103 75(3) . . . . ?
C6 C1 O1 V1 -118(2) . . . . ?
C2 C1 O1 V1 70(2) . . . . ?
C25 C20 O2 V1 109(2) . . . . ?
C21 C20 O2 V1 -60(2) . . . . ?
C35 C34 O3 V2 65(2) . . . . ?
C39 C34 O3 V2 -119.1(18) . . . . ?
C58 C53 O4 V2 106(2) . . . . ?
C54 C53 O4 V2 -67(2) . . . . ?
C72 C71 O7 C74 36(3) . . . . ?
C72 C71 O7 V1 173.9(15) . . . . ?
C73 C74 O7 C71 -7(3) . . . . ?
C73 C74 O7 V1 -146.9(17) . . . . ?
C83 C84 O8 C81 -32(3) . . . . ?
C83 C84 O8 V2 -170.7(14) . . . . ?
C82 C81 O8 C84 10(3) . . . . ?
C82 C81 O8 V2 148.6(16) . . . . ?
C102 C101 O10 V2 -170.5(19) . . . . ?
C92 C91 O90 V1 164(2) . . . . ?
C91 O90 V1 O5 0(2) . . . . ?
C91 O90 V1 O1 -105(2) . . . . ?
C91 O90 V1 O2 104(2) . . . . ?
C91 O90 V1 O7 -178(2) . . . . ?
C1 O1 V1 O5 19.7(16) . . . . ?
C1 O1 V1 O90 126.4(15) . . . . ?
C1 O1 V1 O2 -80.7(16) . . . . ?
C1 O1 V1 O7 -159.2(15) . . . . ?
C20 O2 V1 O5 -24.3(18) . . . . ?
C20 O2 V1 O90 -130.7(17) . . . . ?
C20 O2 V1 O1 76.4(18) . . . . ?
C20 O2 V1 O7 153.0(18) . . . . ?
C101 O10 V2 O6 1(2) . . . . ?
C101 O10 V2 O3 -105.6(19) . . . . ?
C101 O10 V2 O4 107.4(19) . . . . ?
C101 O10 V2 O8 179(2) . . . . ?
C34 O3 V2 O6 28.3(17) . . . . ?
C34 O3 V2 O10 136.3(16) . . . . ?
C34 O3 V2 O4 -74.6(17) . . . . ?
C34 O3 V2 O8 -150.4(16) . . . . ?
C53 O4 V2 O6 -22.9(15) . . . . ?
C53 O4 V2 O10 -130.8(14) . . . . ?
C53 O4 V2 O3 80.4(15) . . . . ?
C53 O4 V2 O8 157.6(15) . . . . ?

_refine_diff_density_max         0.775
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.135

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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 1404524'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;


_vrf_PLAT201_4                   
;
RESPONSE: There is small-scale disorder in the ligand set. This 
is modelled using partially occupied atoms with isotropic 
displacement parameters.    
;


_vrf_PLAT220_4                   
;
RESPONSE: The carbon atoms of the aromatic rings at the core of the
molecule display considerably smaller displacement parameters than
the peripheral tButyl groups. This is entirely expected on 
chemical grounds.     
;

_vrf_PLAT222_4                   
;
RESPONSE: The hydrogen atoms of the aromatic rings at the core of the
molecule display considerably smaller displacement parameters than
the peripheral tButyl groups. This is entirely expected on 
chemical grounds.     
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C70 H100 O8 V2, 2(C H2 Cl2)
;

_chemical_formula_sum            'C72 H104 Cl4 O8 V2'
_chemical_formula_weight         1341.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0268(7)
_cell_length_b                   19.1028(13)
_cell_length_c                   70.103(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14766.7(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16405
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_F_000             5712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Absorption correction implemented within Rigaku CrystalClear suite. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device_type  
;
Rigaku Kappa 3 circle diffractometer with Saturn 724+ detector.
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            91884
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_limit_l_max       90
_diffrn_reflns_theta_min         2.429
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.300
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             16405
_reflns_number_gt                11323
_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 2.1 b31 (Rigaku, 2014)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;


_computing_structure_solution    ;SHELXS-86'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1236P)²+16.2408P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16405
_refine_ls_number_parameters     763
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2248
_refine_ls_wR_factor_gt          0.2001
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.053
_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 0.50620(5) 0.58841(3) 0.29251(2) 0.02517(14) Uani 1 1 d . . . . .
O1 O 0.6550(2) 0.55433(11) 0.29673(3) 0.0255(5) Uani 1 1 d . . . . .
O2 O 0.4273(2) 0.60089(11) 0.31457(3) 0.0252(5) Uani 1 1 d . . . . .
O3 O 0.4347(2) 0.53158(14) 0.28058(4) 0.0368(6) Uani 1 1 d . . . . .
C1 C 0.6787(3) 0.48561(16) 0.30205(4) 0.0230(6) Uani 1 1 d . . . . .
C2 C 0.7392(3) 0.43987(17) 0.28932(5) 0.0243(6) Uani 1 1 d . . . . .
C3 C 0.7559(3) 0.37173(17) 0.29568(5) 0.0271(7) Uani 1 1 d . . . . .
H3 H 0.7964 0.3398 0.2875 0.033 Uiso 1 1 calc R U . . .
C4 C 0.7167(3) 0.34723(17) 0.31345(5) 0.0272(7) Uani 1 1 d . . . . .
C5 C 0.6636(3) 0.39490(17) 0.32566(5) 0.0269(7) Uani 1 1 d . . . . .
H5 H 0.6390 0.3799 0.3380 0.032 Uiso 1 1 calc R U . . .
C6 C 0.6451(3) 0.46487(16) 0.32038(5) 0.0237(6) Uani 1 1 d . . . . .
C7 C 0.7886(3) 0.46406(17) 0.26990(5) 0.0261(7) Uani 1 1 d . . . . .
C8 C 0.6855(3) 0.4851(2) 0.25641(5) 0.0414(9) Uani 1 1 d . . . . .
H8A H 0.6302 0.4454 0.2547 0.062 Uiso 1 1 calc R U . . .
H8B H 0.7194 0.4987 0.2440 0.062 Uiso 1 1 calc R U . . .
H8C H 0.6409 0.5247 0.2619 0.062 Uiso 1 1 calc R U . . .
C9 C 0.8760(4) 0.5253(2) 0.27267(6) 0.0400(9) Uani 1 1 d . . . . .
H9A H 0.8338 0.5638 0.2791 0.060 Uiso 1 1 calc R U . . .
H9B H 0.9052 0.5413 0.2602 0.060 Uiso 1 1 calc R U . . .
H9C H 0.9450 0.5101 0.2804 0.060 Uiso 1 1 calc R U . . .
C10 C 0.8600(3) 0.4062(2) 0.25980(5) 0.0354(8) Uani 1 1 d . . . . .
H10A H 0.8071 0.3657 0.2577 0.053 Uiso 1 1 calc R U . . .
H10B H 0.9291 0.3923 0.2677 0.053 Uiso 1 1 calc R U . . .
H10C H 0.8895 0.4235 0.2475 0.053 Uiso 1 1 calc R U . . .
C11 C 0.7390(3) 0.27032(18) 0.31891(5) 0.0329(8) Uani 1 1 d . . . . .
C12 C 0.8743(4) 0.2602(2) 0.32277(7) 0.0516(11) Uani 1 1 d . . . . .
H12A H 0.8998 0.2915 0.3331 0.077 Uiso 1 1 calc R U . . .
H12B H 0.9205 0.2711 0.3112 0.077 Uiso 1 1 calc R U . . .
H12C H 0.8895 0.2115 0.3265 0.077 Uiso 1 1 calc R U . . .
C13 C 0.7000(4) 0.22171(18) 0.30272(6) 0.0394(9) Uani 1 1 d . . . . .
H13A H 0.6133 0.2279 0.3002 0.059 Uiso 1 1 calc R U . . .
H13B H 0.7156 0.1730 0.3064 0.059 Uiso 1 1 calc R U . . .
H13C H 0.7462 0.2330 0.2912 0.059 Uiso 1 1 calc R U . . .
C14 C 0.6664(4) 0.2497(2) 0.33676(6) 0.0427(9) Uani 1 1 d . . . . .
H14A H 0.6897 0.2801 0.3474 0.064 Uiso 1 1 calc R U . . .
H14B H 0.6836 0.2009 0.3400 0.064 Uiso 1 1 calc R U . . .
H14C H 0.5795 0.2552 0.3342 0.064 Uiso 1 1 calc R U . . .
C15 C 0.5922(3) 0.51650(16) 0.33470(4) 0.0231(6) Uani 1 1 d . . . . .
H15 H 0.6051 0.5641 0.3291 0.028 Uiso 1 1 calc R U . . .
C16 C 0.3772(3) 0.55017(16) 0.32610(4) 0.0232(6) Uani 1 1 d . . . . .
C17 C 0.4554(3) 0.50710(16) 0.33632(4) 0.0224(6) Uani 1 1 d . . . . .
C18 C 0.4066(3) 0.45299(16) 0.34723(4) 0.0234(6) Uani 1 1 d . . . . .
H18 H 0.4599 0.4229 0.3540 0.028 Uiso 1 1 calc R U . . .
C19 C 0.2832(3) 0.44188(16) 0.34843(5) 0.0257(7) Uani 1 1 d . . . . .
C20 C 0.2073(3) 0.48844(17) 0.33870(5) 0.0268(7) Uani 1 1 d . . . . .
H20 H 0.1221 0.4823 0.3398 0.032 Uiso 1 1 calc R U . . .
C21 C 0.2500(3) 0.54323(17) 0.32747(4) 0.0248(6) Uani 1 1 d . . . . .
C22 C 0.2338(3) 0.38080(18) 0.36033(5) 0.0319(7) Uani 1 1 d D . . . .
C23A C 0.1120(7) 0.3519(5) 0.35164(14) 0.0526(9) Uiso 0.536(6) 1 d D U P A 1
H23A H 0.1249 0.3392 0.3382 0.079 Uiso 0.536(6) 1 calc R U P A 1
H23B H 0.0491 0.3880 0.3525 0.079 Uiso 0.536(6) 1 calc R U P A 1
H23C H 0.0862 0.3104 0.3588 0.079 Uiso 0.536(6) 1 calc R U P A 1
C24A C 0.2155(9) 0.4000(5) 0.38016(12) 0.0526(9) Uiso 0.536(6) 1 d D U P A 1
H24A H 0.1791 0.4468 0.3808 0.079 Uiso 0.536(6) 1 calc R U P A 1
H24B H 0.2937 0.4002 0.3868 0.079 Uiso 0.536(6) 1 calc R U P A 1
H24C H 0.1613 0.3660 0.3862 0.079 Uiso 0.536(6) 1 calc R U P A 1
C25A C 0.2850(9) 0.3143(5) 0.35235(14) 0.0526(9) Uiso 0.536(6) 1 d D U P A 1
H25A H 0.2846 0.3166 0.3384 0.079 Uiso 0.536(6) 1 calc R U P A 1
H25B H 0.2356 0.2746 0.3566 0.079 Uiso 0.536(6) 1 calc R U P A 1
H25C H 0.3685 0.3083 0.3569 0.079 Uiso 0.536(6) 1 calc R U P A 1
C23B C 0.0966(8) 0.3794(6) 0.36048(16) 0.0526(9) Uiso 0.464(6) 1 d D U P A 2
H23D H 0.0685 0.3398 0.3682 0.079 Uiso 0.464(6) 1 calc R U P A 2
H23E H 0.0665 0.3743 0.3474 0.079 Uiso 0.464(6) 1 calc R U P A 2
H23F H 0.0659 0.4232 0.3660 0.079 Uiso 0.464(6) 1 calc R U P A 2
C24B C 0.2815(10) 0.3906(6) 0.38093(14) 0.0526(9) Uiso 0.464(6) 1 d D U P A 2
H24D H 0.3703 0.3921 0.3808 0.079 Uiso 0.464(6) 1 calc R U P A 2
H24E H 0.2544 0.3513 0.3889 0.079 Uiso 0.464(6) 1 calc R U P A 2
H24F H 0.2500 0.4345 0.3862 0.079 Uiso 0.464(6) 1 calc R U P A 2
C25B C 0.3221(10) 0.3166(5) 0.35911(17) 0.0526(9) Uiso 0.464(6) 1 d D U P A 2
H25D H 0.4062 0.3332 0.3596 0.079 Uiso 0.464(6) 1 calc R U P A 2
H25E H 0.3082 0.2915 0.3471 0.079 Uiso 0.464(6) 1 calc R U P A 2
H25F H 0.3071 0.2851 0.3699 0.079 Uiso 0.464(6) 1 calc R U P A 2
C26 C 0.1621(3) 0.59408(18) 0.31750(5) 0.0308(7) Uani 1 1 d . . . . .
C27 C 0.0300(3) 0.5785(2) 0.32296(6) 0.0392(9) Uani 1 1 d . . . . .
H27A H 0.0099 0.5303 0.3194 0.059 Uiso 1 1 calc R U . . .
H27B H -0.0239 0.6109 0.3162 0.059 Uiso 1 1 calc R U . . .
H27C H 0.0198 0.5843 0.3368 0.059 Uiso 1 1 calc R U . . .
C28 C 0.1891(4) 0.66952(19) 0.32341(6) 0.0420(9) Uani 1 1 d . . . . .
H28A H 0.1326 0.7012 0.3169 0.063 Uiso 1 1 calc R U . . .
H28B H 0.2725 0.6815 0.3198 0.063 Uiso 1 1 calc R U . . .
H28C H 0.1796 0.6742 0.3372 0.063 Uiso 1 1 calc R U . . .
C29 C 0.1706(3) 0.5877(2) 0.29570(5) 0.0400(9) Uani 1 1 d . . . . .
H29A H 0.1533 0.5393 0.2919 0.060 Uiso 1 1 calc R U . . .
H29B H 0.2525 0.6005 0.2915 0.060 Uiso 1 1 calc R U . . .
H29C H 0.1114 0.6191 0.2898 0.060 Uiso 1 1 calc R U . . .
C30 C 0.6627(3) 0.51537(16) 0.35355(4) 0.0238(6) Uani 1 1 d . . . . .
C31 C 0.7878(3) 0.5120(2) 0.35225(5) 0.0369(8) Uani 1 1 d . . . . .
H31 H 0.8249 0.5068 0.3401 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8595(3) 0.5162(3) 0.36837(6) 0.0436(10) Uani 1 1 d . . . . .
H32 H 0.9453 0.5140 0.3673 0.052 Uiso 1 1 calc R U . . .
C33 C 0.8065(3) 0.5237(2) 0.38609(5) 0.0348(8) Uani 1 1 d . . . . .
H33 H 0.8563 0.5260 0.3971 0.042 Uiso 1 1 calc R U . . .
C34 C 0.6809(3) 0.52778(16) 0.38800(4) 0.0237(6) Uani 1 1 d . . . . .
C35 C 0.6098(3) 0.52363(15) 0.37150(4) 0.0226(6) Uani 1 1 d . . . . .
H35 H 0.5240 0.5265 0.3725 0.027 Uiso 1 1 calc R U . . .
C36 C 0.6350(3) 0.53378(16) 0.40848(4) 0.0224(6) Uani 1 1 d . . . . .
H36 H 0.6689 0.4921 0.4153 0.027 Uiso 1 1 calc R U . . .
C37 C 0.6934(3) 0.59759(16) 0.41805(5) 0.0233(6) Uani 1 1 d . . . . .
C38 C 0.6897(3) 0.66268(16) 0.40910(5) 0.0258(7) Uani 1 1 d . . . . .
H38 H 0.6478 0.6672 0.3973 0.031 Uiso 1 1 calc R U . . .
C39 C 0.7452(3) 0.72086(16) 0.41690(5) 0.0263(6) Uani 1 1 d . . . . .
C40 C 0.8087(3) 0.71140(17) 0.43400(5) 0.0286(7) Uani 1 1 d . . . . .
H40 H 0.8486 0.7508 0.4394 0.034 Uiso 1 1 calc R U . . .
C41 C 0.8169(3) 0.64800(17) 0.44359(5) 0.0276(7) Uani 1 1 d . . . . .
C42 C 0.7531(3) 0.59095(16) 0.43546(4) 0.0240(6) Uani 1 1 d . . . . .
C43 C 0.7405(3) 0.79339(17) 0.40742(5) 0.0308(7) Uani 1 1 d . . . . .
C44 C 0.6593(4) 0.7940(2) 0.38967(6) 0.0447(10) Uani 1 1 d . . . . .
H44A H 0.6588 0.8411 0.3841 0.067 Uiso 1 1 calc R U . . .
H44B H 0.5765 0.7808 0.3933 0.067 Uiso 1 1 calc R U . . .
H44C H 0.6906 0.7606 0.3803 0.067 Uiso 1 1 calc R U . . .
C45 C 0.8681(3) 0.8155(2) 0.40125(6) 0.0397(9) Uani 1 1 d . . . . .
H45A H 0.8645 0.8618 0.3952 0.060 Uiso 1 1 calc R U . . .
H45B H 0.9003 0.7814 0.3921 0.060 Uiso 1 1 calc R U . . .
H45C H 0.9212 0.8175 0.4124 0.060 Uiso 1 1 calc R U . . .
C46 C 0.6903(4) 0.84679(18) 0.42172(6) 0.0395(9) Uani 1 1 d . . . . .
H46A H 0.6871 0.8931 0.4157 0.059 Uiso 1 1 calc R U . . .
H46B H 0.7431 0.8486 0.4329 0.059 Uiso 1 1 calc R U . . .
H46C H 0.6084 0.8328 0.4256 0.059 Uiso 1 1 calc R U . . .
C47 C 0.8910(3) 0.64106(19) 0.46211(5) 0.0342(8) Uani 1 1 d . . . . .
C48 C 0.9801(3) 0.5791(2) 0.46084(6) 0.0384(9) Uani 1 1 d . . . . .
H48A H 0.9349 0.5359 0.4584 0.058 Uiso 1 1 calc R U . . .
H48B H 1.0242 0.5747 0.4729 0.058 Uiso 1 1 calc R U . . .
H48C H 1.0378 0.5874 0.4505 0.058 Uiso 1 1 calc R U . . .
C49 C 0.8048(4) 0.6302(2) 0.47925(5) 0.0427(9) Uani 1 1 d . . . . .
H49A H 0.7557 0.5882 0.4771 0.064 Uiso 1 1 calc R U . . .
H49B H 0.7516 0.6710 0.4805 0.064 Uiso 1 1 calc R U . . .
H49C H 0.8527 0.6245 0.4909 0.064 Uiso 1 1 calc R U . . .
C50 C 0.9659(4) 0.7068(2) 0.46605(6) 0.0436(10) Uani 1 1 d . . . . .
H50A H 1.0119 0.7006 0.4779 0.065 Uiso 1 1 calc R U . . .
H50B H 0.9116 0.7472 0.4673 0.065 Uiso 1 1 calc R U . . .
H50C H 1.0221 0.7149 0.4554 0.065 Uiso 1 1 calc R U . . .
C51 C 0.4520(3) 0.48315(15) 0.42527(4) 0.0234(6) Uani 1 1 d . . . . .
C52 C 0.4989(3) 0.53122(15) 0.41194(4) 0.0214(6) Uani 1 1 d . . . . .
C53 C 0.4194(3) 0.57717(15) 0.40320(4) 0.0228(6) Uani 1 1 d . . . . .
H53 H 0.4504 0.6108 0.3945 0.027 Uiso 1 1 calc R U . . .
C54 C 0.2953(3) 0.57552(16) 0.40678(5) 0.0255(6) Uani 1 1 d . . . . .
C55 C 0.2523(3) 0.52328(17) 0.41889(5) 0.0277(7) Uani 1 1 d . . . . .
H55 H 0.1673 0.5204 0.4210 0.033 Uiso 1 1 calc R U . . .
C56 C 0.3268(3) 0.47503(16) 0.42815(5) 0.0255(6) Uani 1 1 d . . . . .
C57 C 0.2106(3) 0.62895(17) 0.39746(5) 0.0294(7) Uani 1 1 d . . . . .
C58 C 0.2103(6) 0.6193(3) 0.37634(7) 0.0673(15) Uani 1 1 d . . . . .
H58A H 0.1558 0.6537 0.3705 0.101 Uiso 1 1 calc R U . . .
H58B H 0.1821 0.5719 0.3733 0.101 Uiso 1 1 calc R U . . .
H58C H 0.2926 0.6258 0.3714 0.101 Uiso 1 1 calc R U . . .
C59 C 0.2542(6) 0.7027(2) 0.40199(10) 0.086(2) Uani 1 1 d . . . . .
H59A H 0.2542 0.7097 0.4158 0.129 Uiso 1 1 calc R U . . .
H59B H 0.1999 0.7368 0.3960 0.129 Uiso 1 1 calc R U . . .
H59C H 0.3366 0.7090 0.3970 0.129 Uiso 1 1 calc R U . . .
C60 C 0.0809(5) 0.6218(4) 0.40452(11) 0.118(3) Uani 1 1 d . . . . .
H60A H 0.0789 0.6280 0.4184 0.178 Uiso 1 1 calc R U . . .
H60B H 0.0499 0.5753 0.4013 0.178 Uiso 1 1 calc R U . . .
H60C H 0.0302 0.6576 0.3985 0.178 Uiso 1 1 calc R U . . .
C61 C 0.2716(3) 0.41815(18) 0.44101(5) 0.0319(7) Uani 1 1 d . . . . .
C62 C 0.2791(4) 0.4409(3) 0.46192(6) 0.0523(11) Uani 1 1 d . . . . .
H62A H 0.2439 0.4044 0.4700 0.078 Uiso 1 1 calc R U . . .
H62B H 0.2340 0.4846 0.4637 0.078 Uiso 1 1 calc R U . . .
H62C H 0.3642 0.4482 0.4654 0.078 Uiso 1 1 calc R U . . .
C63 C 0.1362(4) 0.4066(2) 0.43626(7) 0.0469(10) Uani 1 1 d . . . . .
H63A H 0.1030 0.3703 0.4446 0.070 Uiso 1 1 calc R U . . .
H63B H 0.1282 0.3919 0.4229 0.070 Uiso 1 1 calc R U . . .
H63C H 0.0916 0.4504 0.4382 0.070 Uiso 1 1 calc R U . . .
C64 C 0.3339(4) 0.34718(19) 0.43773(7) 0.0465(10) Uani 1 1 d . . . . .
H64A H 0.2972 0.3119 0.4461 0.070 Uiso 1 1 calc R U . . .
H64B H 0.4205 0.3513 0.4406 0.070 Uiso 1 1 calc R U . . .
H64C H 0.3235 0.3331 0.4244 0.070 Uiso 1 1 calc R U . . .
O4 O 0.5126(2) 0.66699(14) 0.28019(4) 0.0428(7) Uani 1 1 d D . . . .
C66A C 0.5870(10) 0.6879(6) 0.24995(16) 0.0520(11) Uiso 0.443(5) 1 d D U P B 1
H66A H 0.6704 0.6937 0.2545 0.078 Uiso 0.443(5) 1 calc R U P B 1
H66B H 0.5757 0.7152 0.2382 0.078 Uiso 0.443(5) 1 calc R U P B 1
H66C H 0.5716 0.6383 0.2473 0.078 Uiso 0.443(5) 1 calc R U P B 1
C65A C 0.4992(7) 0.7136(5) 0.26511(12) 0.0378(12) Uiso 0.443(5) 1 d D U P B 1
H65A H 0.5196 0.7624 0.2692 0.045 Uiso 0.443(5) 1 calc R U P B 1
C67A C 0.3680(8) 0.7073(6) 0.26046(16) 0.0520(11) Uiso 0.443(5) 1 d D U P B 1
H67A H 0.3196 0.7237 0.2713 0.078 Uiso 0.443(5) 1 calc R U P B 1
H67B H 0.3483 0.6582 0.2578 0.078 Uiso 0.443(5) 1 calc R U P B 1
H67C H 0.3495 0.7358 0.2492 0.078 Uiso 0.443(5) 1 calc R U P B 1
C66B C 0.5458(8) 0.6878(5) 0.24617(12) 0.0520(11) Uiso 0.557(5) 1 d D U P B 2
H66D H 0.5853 0.6421 0.2447 0.078 Uiso 0.557(5) 1 calc R U P B 2
H66E H 0.6063 0.7229 0.2499 0.078 Uiso 0.557(5) 1 calc R U P B 2
H66F H 0.5085 0.7014 0.2340 0.078 Uiso 0.557(5) 1 calc R U P B 2
C65B C 0.4522(6) 0.6833(4) 0.26092(9) 0.0378(12) Uiso 0.557(5) 1 d D U P B 2
H65B H 0.3932 0.6454 0.2576 0.045 Uiso 0.557(5) 1 calc R U P B 2
C67B C 0.3870(7) 0.7498(4) 0.26397(12) 0.0520(11) Uiso 0.557(5) 1 d D U P B 2
H67D H 0.3182 0.7419 0.2726 0.078 Uiso 0.557(5) 1 calc R U P B 2
H67E H 0.3572 0.7675 0.2517 0.078 Uiso 0.557(5) 1 calc R U P B 2
H67F H 0.4421 0.7842 0.2697 0.078 Uiso 0.557(5) 1 calc R U P B 2
V2 V 0.62916(5) 0.47791(3) 0.45406(2) 0.02683(15) Uani 1 1 d . . . . .
O5 O 0.7535(2) 0.52612(11) 0.44408(3) 0.0268(5) Uani 1 1 d . . . . .
O6 O 0.5335(2) 0.44377(11) 0.43564(3) 0.0258(5) Uani 1 1 d . . . . .
O7 O 0.5509(2) 0.53146(13) 0.46615(4) 0.0379(6) Uani 1 1 d . . . . .
O8 O 0.6826(3) 0.40880(14) 0.46771(4) 0.0399(6) Uani 1 1 d . . . . .
C68 C 0.6829(5) 0.3841(3) 0.48717(6) 0.0605(13) Uani 1 1 d . . . . .
H68 H 0.7138 0.3349 0.4873 0.073 Uiso 1 1 calc R U . . .
C69 C 0.7613(10) 0.4258(4) 0.49815(10) 0.149(4) Uani 1 1 d . . . . .
H69A H 0.8432 0.4240 0.4927 0.223 Uiso 1 1 calc R U . . .
H69B H 0.7631 0.4083 0.5113 0.223 Uiso 1 1 calc R U . . .
H69C H 0.7323 0.4743 0.4981 0.223 Uiso 1 1 calc R U . . .
C70 C 0.5519(6) 0.3842(3) 0.49489(8) 0.0810(18) Uani 1 1 d . . . . .
H70A H 0.5010 0.3543 0.4868 0.121 Uiso 1 1 calc R U . . .
H70B H 0.5201 0.4321 0.4948 0.121 Uiso 1 1 calc R U . . .
H70C H 0.5514 0.3663 0.5080 0.121 Uiso 1 1 calc R U . . .
C71 C 0.4967(6) 0.6971(3) 0.45302(11) 0.098(3) Uani 1 1 d D . . . .
H71A H 0.5183 0.7120 0.4399 0.118 Uiso 1 1 calc R U . . .
H71B H 0.5472 0.6560 0.4563 0.118 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5303(2) 0.76688(10) 0.46929(3) 0.1124(7) Uani 1 1 d D . . . .
Cl2 Cl 0.3486(2) 0.67370(11) 0.45352(3) 0.1084(7) Uani 1 1 d D . . . .
C72 C 0.3053(4) 0.3938(2) 0.29818(7) 0.0574(12) Uani 1 1 d D . . . .
H72A H 0.3161 0.4354 0.2899 0.069 Uiso 1 1 calc R U . . .
H72B H 0.3278 0.4075 0.3113 0.069 Uiso 1 1 calc R U . . .
Cl3 Cl 0.40407(13) 0.32936(7) 0.29059(2) 0.0650(3) Uani 1 1 d D . . . .
Cl4 Cl 0.15222(14) 0.37055(11) 0.29799(3) 0.0952(5) Uani 1 1 d 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 O3 1.581(3) . ?
V1 O4 1.733(3) . ?
V1 O1 1.790(2) . ?
V1 O2 1.790(2) . ?
O1 C1 1.390(4) . ?
O2 C16 1.378(4) . ?
C1 C6 1.395(4) . ?
C1 C2 1.416(4) . ?
C2 C3 1.388(4) . ?
C2 C7 1.537(4) . ?
C3 C4 1.399(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(5) . ?
C4 C11 1.538(5) . ?
C5 C6 1.402(4) . ?
C5 H5 0.9500 . ?
C6 C15 1.523(4) . ?
C7 C9 1.529(5) . ?
C7 C10 1.531(5) . ?
C7 C8 1.533(5) . ?
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 1.528(5) . ?
C11 C12 1.529(5) . ?
C11 C14 1.537(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(4) . ?
C15 C30 1.533(4) . ?
C15 H15 1.0000 . ?
C16 C17 1.391(4) . ?
C16 C21 1.411(4) . ?
C17 C18 1.394(4) . ?
C18 C19 1.380(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.398(4) . ?
C19 C22 1.534(4) . ?
C20 C21 1.392(4) . ?
C20 H20 0.9500 . ?
C21 C26 1.540(4) . ?
C22 C24A 1.452(9) . ?
C22 C25A 1.499(9) . ?
C22 C23B 1.513(9) . ?
C22 C24B 1.548(10) . ?
C22 C25B 1.568(10) . ?
C22 C23A 1.574(9) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C26 C28 1.529(5) . ?
C26 C27 1.535(5) . ?
C26 C29 1.536(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.384(5) . ?
C30 C35 1.396(4) . ?
C31 C32 1.381(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.399(4) . ?
C34 C36 1.527(4) . ?
C35 H35 0.9500 . ?
C36 C52 1.521(4) . ?
C36 C37 1.533(4) . ?
C36 H36 1.0000 . ?
C37 C42 1.392(4) . ?
C37 C38 1.394(4) . ?
C38 C39 1.382(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.400(5) . ?
C39 C43 1.538(4) . ?
C40 C41 1.388(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.417(4) . ?
C41 C47 1.539(5) . ?
C42 O5 1.378(4) . ?
C43 C45 1.532(5) . ?
C43 C44 1.533(5) . ?
C43 C46 1.534(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C50 1.528(5) . ?
C47 C48 1.540(5) . ?
C47 C49 1.546(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 O6 1.379(4) . ?
C51 C56 1.404(4) . ?
C51 C52 1.409(4) . ?
C52 C53 1.384(4) . ?
C53 C54 1.392(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.394(4) . ?
C54 C57 1.530(4) . ?
C55 C56 1.395(5) . ?
C55 H55 0.9500 . ?
C56 C61 1.537(4) . ?
C57 C58 1.492(6) . ?
C57 C60 1.520(6) . ?
C57 C59 1.521(6) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.531(6) . ?
C61 C64 1.537(5) . ?
C61 C63 1.546(5) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
O4 C65A 1.390(8) . ?
O4 C65B 1.538(7) . ?
C66A C65A 1.519(11) . ?
C66A H66A 0.9800 . ?
C66A H66B 0.9800 . ?
C66A H66C 0.9800 . ?
C65A C67A 1.488(10) . ?
C65A H65A 1.0000 . ?
C67A H67A 0.9800 . ?
C67A H67B 0.9800 . ?
C67A H67C 0.9800 . ?
C66B C65B 1.464(9) . ?
C66B H66D 0.9800 . ?
C66B H66E 0.9800 . ?
C66B H66F 0.9800 . ?
C65B C67B 1.476(9) . ?
C65B H65B 1.0000 . ?
C67B H67D 0.9800 . ?
C67B H67E 0.9800 . ?
C67B H67F 0.9800 . ?
V2 O7 1.584(3) . ?
V2 O8 1.734(3) . ?
V2 O6 1.790(2) . ?
V2 O5 1.793(2) . ?
O8 C68 1.444(5) . ?
C68 C69 1.406(8) . ?
C68 C70 1.542(8) . ?
C68 H68 1.0000 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 Cl2 1.694(6) . ?
C71 Cl1 1.793(7) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 Cl3 1.728(5) . ?
C72 Cl4 1.745(5) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 V1 O4 110.60(15) . . ?
O3 V1 O1 107.16(12) . . ?
O4 V1 O1 111.09(11) . . ?
O3 V1 O2 107.81(12) . . ?
O4 V1 O2 109.56(12) . . ?
O1 V1 O2 110.54(11) . . ?
C1 O1 V1 124.08(19) . . ?
C16 O2 V1 127.47(19) . . ?
O1 C1 C6 117.7(3) . . ?
O1 C1 C2 120.2(3) . . ?
C6 C1 C2 122.0(3) . . ?
C3 C2 C1 116.0(3) . . ?
C3 C2 C7 121.3(3) . . ?
C1 C2 C7 122.6(3) . . ?
C2 C3 C4 124.0(3) . . ?
C2 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
C5 C4 C3 117.6(3) . . ?
C5 C4 C11 122.9(3) . . ?
C3 C4 C11 119.5(3) . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 118.4(3) . . ?
C1 C6 C15 121.7(3) . . ?
C5 C6 C15 119.9(3) . . ?
C9 C7 C10 106.7(3) . . ?
C9 C7 C8 110.2(3) . . ?
C10 C7 C8 106.6(3) . . ?
C9 C7 C2 110.0(3) . . ?
C10 C7 C2 112.0(3) . . ?
C8 C7 C2 111.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 109.2(3) . . ?
C13 C11 C14 107.6(3) . . ?
C12 C11 C14 109.4(3) . . ?
C13 C11 C4 110.5(3) . . ?
C12 C11 C4 108.7(3) . . ?
C14 C11 C4 111.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 C17 110.6(2) . . ?
C6 C15 C30 111.4(3) . . ?
C17 C15 C30 115.9(3) . . ?
C6 C15 H15 106.1 . . ?
C17 C15 H15 106.1 . . ?
C30 C15 H15 106.1 . . ?
O2 C16 C17 118.0(3) . . ?
O2 C16 C21 120.3(3) . . ?
C17 C16 C21 121.7(3) . . ?
C16 C17 C18 118.8(3) . . ?
C16 C17 C15 120.4(3) . . ?
C18 C17 C15 120.7(3) . . ?
C19 C18 C17 121.9(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 117.5(3) . . ?
C18 C19 C22 120.0(3) . . ?
C20 C19 C22 122.5(3) . . ?
C21 C20 C19 123.5(3) . . ?
C21 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
C20 C21 C16 116.4(3) . . ?
C20 C21 C26 121.2(3) . . ?
C16 C21 C26 122.4(3) . . ?
C24A C22 C25A 128.6(6) . . ?
C24A C22 C19 112.2(4) . . ?
C25A C22 C19 107.9(4) . . ?
C23B C22 C19 111.9(5) . . ?
C23B C22 C24B 109.6(6) . . ?
C19 C22 C24B 107.1(5) . . ?
C23B C22 C25B 127.4(7) . . ?
C19 C22 C25B 110.1(5) . . ?
C24B C22 C25B 86.2(7) . . ?
C24A C22 C23A 109.9(5) . . ?
C25A C22 C23A 83.1(6) . . ?
C19 C22 C23A 111.1(4) . . ?
C22 C23A C25A 46.9(4) . . ?
C22 C23A H23A 109.5 . . ?
C25A C23A H23A 78.5 . . ?
C22 C23A H23B 109.5 . . ?
C25A C23A H23B 155.3 . . ?
H23A C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
C25A C23A H23C 88.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22 C25A C23A 50.0(4) . . ?
C22 C25A H25A 109.5 . . ?
C23A C25A H25A 87.5 . . ?
C22 C25A H25B 109.5 . . ?
C23A C25A H25B 76.1 . . ?
H25A C25A H25B 109.5 . . ?
C22 C25A H25C 109.5 . . ?
C23A C25A H25C 158.1 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22 C24B H24D 109.5 . . ?
C22 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C22 C25B H25D 109.5 . . ?
C22 C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C22 C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C28 C26 C27 107.5(3) . . ?
C28 C26 C29 109.4(3) . . ?
C27 C26 C29 106.9(3) . . ?
C28 C26 C21 110.4(3) . . ?
C27 C26 C21 111.2(3) . . ?
C29 C26 C21 111.3(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 118.7(3) . . ?
C31 C30 C15 116.7(3) . . ?
C35 C30 C15 124.3(3) . . ?
C32 C31 C30 121.0(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 120.0(3) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.9(3) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C35 118.3(3) . . ?
C33 C34 C36 115.0(3) . . ?
C35 C34 C36 126.6(3) . . ?
C30 C35 C34 121.2(3) . . ?
C30 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C52 C36 C34 118.3(3) . . ?
C52 C36 C37 111.7(2) . . ?
C34 C36 C37 109.4(2) . . ?
C52 C36 H36 105.5 . . ?
C34 C36 H36 105.5 . . ?
C37 C36 H36 105.5 . . ?
C42 C37 C38 119.4(3) . . ?
C42 C37 C36 120.6(3) . . ?
C38 C37 C36 120.0(3) . . ?
C39 C38 C37 121.7(3) . . ?
C39 C38 H38 119.1 . . ?
C37 C38 H38 119.1 . . ?
C38 C39 C40 117.2(3) . . ?
C38 C39 C43 122.6(3) . . ?
C40 C39 C43 120.2(3) . . ?
C41 C40 C39 124.1(3) . . ?
C41 C40 H40 118.0 . . ?
C39 C40 H40 118.0 . . ?
C40 C41 C42 116.3(3) . . ?
C40 C41 C47 121.2(3) . . ?
C42 C41 C47 122.5(3) . . ?
O5 C42 C37 117.9(3) . . ?
O5 C42 C41 120.9(3) . . ?
C37 C42 C41 121.2(3) . . ?
C45 C43 C44 107.8(3) . . ?
C45 C43 C46 109.5(3) . . ?
C44 C43 C46 108.3(3) . . ?
C45 C43 C39 109.9(3) . . ?
C44 C43 C39 112.2(3) . . ?
C46 C43 C39 109.2(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C50 C47 C41 111.6(3) . . ?
C50 C47 C48 107.3(3) . . ?
C41 C47 C48 110.9(3) . . ?
C50 C47 C49 107.6(3) . . ?
C41 C47 C49 109.9(3) . . ?
C48 C47 C49 109.5(3) . . ?
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 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O6 C51 C56 120.3(3) . . ?
O6 C51 C52 117.8(3) . . ?
C56 C51 C52 121.9(3) . . ?
C53 C52 C51 118.3(3) . . ?
C53 C52 C36 122.3(3) . . ?
C51 C52 C36 119.3(3) . . ?
C52 C53 C54 121.9(3) . . ?
C52 C53 H53 119.0 . . ?
C54 C53 H53 119.0 . . ?
C53 C54 C55 117.4(3) . . ?
C53 C54 C57 120.5(3) . . ?
C55 C54 C57 122.0(3) . . ?
C54 C55 C56 123.8(3) . . ?
C54 C55 H55 118.1 . . ?
C56 C55 H55 118.1 . . ?
C55 C56 C51 116.1(3) . . ?
C55 C56 C61 120.4(3) . . ?
C51 C56 C61 123.5(3) . . ?
C58 C57 C60 108.0(5) . . ?
C58 C57 C59 108.8(4) . . ?
C60 C57 C59 108.2(5) . . ?
C58 C57 C54 110.0(3) . . ?
C60 C57 C54 112.1(3) . . ?
C59 C57 C54 109.6(3) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 C64 111.7(4) . . ?
C62 C61 C56 109.9(3) . . ?
C64 C61 C56 111.1(3) . . ?
C62 C61 C63 107.4(3) . . ?
C64 C61 C63 105.9(3) . . ?
C56 C61 C63 110.9(3) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C65A O4 V1 158.3(4) . . ?
C65B O4 V1 126.5(3) . . ?
C65A C66A H66A 109.5 . . ?
C65A C66A H66B 109.5 . . ?
H66A C66A H66B 109.5 . . ?
C65A C66A H66C 109.5 . . ?
H66A C66A H66C 109.5 . . ?
H66B C66A H66C 109.5 . . ?
O4 C65A C67A 102.7(7) . . ?
O4 C65A C66A 104.9(7) . . ?
C67A C65A C66A 116.1(8) . . ?
O4 C65A H65A 110.9 . . ?
C67A C65A H65A 110.9 . . ?
C66A C65A H65A 110.9 . . ?
C65A C67A H67A 109.5 . . ?
C65A C67A H67B 109.5 . . ?
H67A C67A H67B 109.5 . . ?
C65A C67A H67C 109.5 . . ?
H67A C67A H67C 109.5 . . ?
H67B C67A H67C 109.5 . . ?
C65B C66B H66D 109.5 . . ?
C65B C66B H66E 109.5 . . ?
H66D C66B H66E 109.5 . . ?
C65B C66B H66F 109.5 . . ?
H66D C66B H66F 109.5 . . ?
H66E C66B H66F 109.5 . . ?
C66B C65B C67B 113.3(7) . . ?
C66B C65B O4 109.1(6) . . ?
C67B C65B O4 105.0(5) . . ?
C66B C65B H65B 109.8 . . ?
C67B C65B H65B 109.8 . . ?
O4 C65B H65B 109.8 . . ?
C65B C67B H67D 109.5 . . ?
C65B C67B H67E 109.5 . . ?
H67D C67B H67E 109.5 . . ?
C65B C67B H67F 109.5 . . ?
H67D C67B H67F 109.5 . . ?
H67E C67B H67F 109.5 . . ?
O7 V2 O8 112.43(14) . . ?
O7 V2 O6 107.45(12) . . ?
O8 V2 O6 108.71(12) . . ?
O7 V2 O5 107.08(12) . . ?
O8 V2 O5 110.27(12) . . ?
O6 V2 O5 110.88(10) . . ?
C42 O5 V2 129.0(2) . . ?
C51 O6 V2 124.44(19) . . ?
C68 O8 V2 140.5(3) . . ?
C69 C68 O8 109.5(5) . . ?
C69 C68 C70 112.5(7) . . ?
O8 C68 C70 109.2(4) . . ?
C69 C68 H68 108.5 . . ?
O8 C68 H68 108.5 . . ?
C70 C68 H68 108.5 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
Cl2 C71 Cl1 112.5(3) . . ?
Cl2 C71 H71A 109.1 . . ?
Cl1 C71 H71A 109.1 . . ?
Cl2 C71 H71B 109.1 . . ?
Cl1 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
Cl3 C72 Cl4 115.2(3) . . ?
Cl3 C72 H72A 108.5 . . ?
Cl4 C72 H72A 108.5 . . ?
Cl3 C72 H72B 108.5 . . ?
Cl4 C72 H72B 108.5 . . ?
H72A C72 H72B 107.5 . . ?

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
O3 V1 O1 C1 -43.0(3) . . . . ?
O4 V1 O1 C1 -163.9(2) . . . . ?
O2 V1 O1 C1 74.2(2) . . . . ?
O3 V1 O2 C16 42.3(3) . . . . ?
O4 V1 O2 C16 162.7(2) . . . . ?
O1 V1 O2 C16 -74.5(3) . . . . ?
V1 O1 C1 C6 -70.1(3) . . . . ?
V1 O1 C1 C2 112.2(3) . . . . ?
O1 C1 C2 C3 -178.3(3) . . . . ?
C6 C1 C2 C3 4.1(4) . . . . ?
O1 C1 C2 C7 4.1(4) . . . . ?
C6 C1 C2 C7 -173.5(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C7 C2 C3 C4 177.8(3) . . . . ?
C2 C3 C4 C5 -3.3(5) . . . . ?
C2 C3 C4 C11 179.3(3) . . . . ?
C3 C4 C5 C6 2.3(5) . . . . ?
C11 C4 C5 C6 179.5(3) . . . . ?
O1 C1 C6 C5 177.3(3) . . . . ?
C2 C1 C6 C5 -5.1(4) . . . . ?
O1 C1 C6 C15 -4.2(4) . . . . ?
C2 C1 C6 C15 173.4(3) . . . . ?
C4 C5 C6 C1 1.7(5) . . . . ?
C4 C5 C6 C15 -176.8(3) . . . . ?
C3 C2 C7 C9 -121.2(3) . . . . ?
C1 C2 C7 C9 56.3(4) . . . . ?
C3 C2 C7 C10 -2.7(4) . . . . ?
C1 C2 C7 C10 174.7(3) . . . . ?
C3 C2 C7 C8 116.5(4) . . . . ?
C1 C2 C7 C8 -66.1(4) . . . . ?
C5 C4 C11 C13 134.6(3) . . . . ?
C3 C4 C11 C13 -48.2(4) . . . . ?
C5 C4 C11 C12 -105.6(4) . . . . ?
C3 C4 C11 C12 71.7(4) . . . . ?
C5 C4 C11 C14 15.0(5) . . . . ?
C3 C4 C11 C14 -167.8(3) . . . . ?
C1 C6 C15 C17 103.1(3) . . . . ?
C5 C6 C15 C17 -78.4(4) . . . . ?
C1 C6 C15 C30 -126.5(3) . . . . ?
C5 C6 C15 C30 52.0(4) . . . . ?
V1 O2 C16 C17 71.6(4) . . . . ?
V1 O2 C16 C21 -108.9(3) . . . . ?
O2 C16 C17 C18 -176.5(3) . . . . ?
C21 C16 C17 C18 4.1(5) . . . . ?
O2 C16 C17 C15 0.2(4) . . . . ?
C21 C16 C17 C15 -179.3(3) . . . . ?
C6 C15 C17 C16 -97.3(3) . . . . ?
C30 C15 C17 C16 134.7(3) . . . . ?
C6 C15 C17 C18 79.3(4) . . . . ?
C30 C15 C17 C18 -48.7(4) . . . . ?
C16 C17 C18 C19 -1.2(5) . . . . ?
C15 C17 C18 C19 -177.8(3) . . . . ?
C17 C18 C19 C20 -1.9(5) . . . . ?
C17 C18 C19 C22 178.9(3) . . . . ?
C18 C19 C20 C21 2.3(5) . . . . ?
C22 C19 C20 C21 -178.4(3) . . . . ?
C19 C20 C21 C16 0.4(5) . . . . ?
C19 C20 C21 C26 -178.4(3) . . . . ?
O2 C16 C21 C20 176.9(3) . . . . ?
C17 C16 C21 C20 -3.6(5) . . . . ?
O2 C16 C21 C26 -4.3(5) . . . . ?
C17 C16 C21 C26 175.1(3) . . . . ?
C18 C19 C22 C24A 87.7(6) . . . . ?
C20 C19 C22 C24A -91.5(6) . . . . ?
C18 C19 C22 C25A -59.5(5) . . . . ?
C20 C19 C22 C25A 121.3(5) . . . . ?
C18 C19 C22 C23B 177.6(5) . . . . ?
C20 C19 C22 C23B -1.6(6) . . . . ?
C18 C19 C22 C24B 57.5(6) . . . . ?
C20 C19 C22 C24B -121.7(5) . . . . ?
C18 C19 C22 C25B -34.7(6) . . . . ?
C20 C19 C22 C25B 146.1(5) . . . . ?
C18 C19 C22 C23A -148.9(5) . . . . ?
C20 C19 C22 C23A 31.9(6) . . . . ?
C24A C22 C23A C25A -128.7(6) . . . . ?
C23B C22 C23A C25A -155.7(11) . . . . ?
C19 C22 C23A C25A 106.6(5) . . . . ?
C24B C22 C23A C25A -109.5(8) . . . . ?
C25B C22 C23A C25A -11.6(7) . . . . ?
C24A C22 C25A C23A 110.1(7) . . . . ?
C23B C22 C25A C23A 13.2(6) . . . . ?
C19 C22 C25A C23A -110.0(5) . . . . ?
C24B C22 C25A C23A 134.1(6) . . . . ?
C25B C22 C25A C23A 150.6(17) . . . . ?
C20 C21 C26 C28 123.4(3) . . . . ?
C16 C21 C26 C28 -55.3(4) . . . . ?
C20 C21 C26 C27 4.2(5) . . . . ?
C16 C21 C26 C27 -174.5(3) . . . . ?
C20 C21 C26 C29 -114.9(4) . . . . ?
C16 C21 C26 C29 66.4(4) . . . . ?
C6 C15 C30 C31 42.0(4) . . . . ?
C17 C15 C30 C31 169.5(3) . . . . ?
C6 C15 C30 C35 -143.9(3) . . . . ?
C17 C15 C30 C35 -16.3(4) . . . . ?
C35 C30 C31 C32 0.5(6) . . . . ?
C15 C30 C31 C32 175.0(4) . . . . ?
C30 C31 C32 C33 0.2(7) . . . . ?
C31 C32 C33 C34 -0.6(7) . . . . ?
C32 C33 C34 C35 0.5(6) . . . . ?
C32 C33 C34 C36 178.3(4) . . . . ?
C31 C30 C35 C34 -0.7(5) . . . . ?
C15 C30 C35 C34 -174.7(3) . . . . ?
C33 C34 C35 C30 0.2(5) . . . . ?
C36 C34 C35 C30 -177.3(3) . . . . ?
C33 C34 C36 C52 -174.0(3) . . . . ?
C35 C34 C36 C52 3.6(5) . . . . ?
C33 C34 C36 C37 56.5(4) . . . . ?
C35 C34 C36 C37 -125.9(3) . . . . ?
C52 C36 C37 C42 99.7(3) . . . . ?
C34 C36 C37 C42 -127.3(3) . . . . ?
C52 C36 C37 C38 -81.9(4) . . . . ?
C34 C36 C37 C38 51.1(4) . . . . ?
C42 C37 C38 C39 1.0(5) . . . . ?
C36 C37 C38 C39 -177.5(3) . . . . ?
C37 C38 C39 C40 1.7(5) . . . . ?
C37 C38 C39 C43 -179.0(3) . . . . ?
C38 C39 C40 C41 -1.2(5) . . . . ?
C43 C39 C40 C41 179.5(3) . . . . ?
C39 C40 C41 C42 -1.9(5) . . . . ?
C39 C40 C41 C47 178.5(3) . . . . ?
C38 C37 C42 O5 179.0(3) . . . . ?
C36 C37 C42 O5 -2.6(4) . . . . ?
C38 C37 C42 C41 -4.3(5) . . . . ?
C36 C37 C42 C41 174.1(3) . . . . ?
C40 C41 C42 O5 -178.7(3) . . . . ?
C47 C41 C42 O5 0.9(5) . . . . ?
C40 C41 C42 C37 4.7(5) . . . . ?
C47 C41 C42 C37 -175.7(3) . . . . ?
C38 C39 C43 C45 -115.0(4) . . . . ?
C40 C39 C43 C45 64.3(4) . . . . ?
C38 C39 C43 C44 4.9(5) . . . . ?
C40 C39 C43 C44 -175.9(3) . . . . ?
C38 C39 C43 C46 125.0(4) . . . . ?
C40 C39 C43 C46 -55.8(4) . . . . ?
C40 C41 C47 C50 -9.1(5) . . . . ?
C42 C41 C47 C50 171.3(3) . . . . ?
C40 C41 C47 C48 -128.7(4) . . . . ?
C42 C41 C47 C48 51.7(5) . . . . ?
C40 C41 C47 C49 110.2(4) . . . . ?
C42 C41 C47 C49 -69.4(4) . . . . ?
O6 C51 C52 C53 -172.0(3) . . . . ?
C56 C51 C52 C53 7.8(5) . . . . ?
O6 C51 C52 C36 4.6(4) . . . . ?
C56 C51 C52 C36 -175.6(3) . . . . ?
C34 C36 C52 C53 -56.3(4) . . . . ?
C37 C36 C52 C53 72.0(4) . . . . ?
C34 C36 C52 C51 127.2(3) . . . . ?
C37 C36 C52 C51 -104.4(3) . . . . ?
C51 C52 C53 C54 -2.0(4) . . . . ?
C36 C52 C53 C54 -178.5(3) . . . . ?
C52 C53 C54 C55 -3.1(5) . . . . ?
C52 C53 C54 C57 177.6(3) . . . . ?
C53 C54 C55 C56 2.8(5) . . . . ?
C57 C54 C55 C56 -177.9(3) . . . . ?
C54 C55 C56 C51 2.5(5) . . . . ?
C54 C55 C56 C61 -178.9(3) . . . . ?
O6 C51 C56 C55 171.9(3) . . . . ?
C52 C51 C56 C55 -7.9(5) . . . . ?
O6 C51 C56 C61 -6.7(5) . . . . ?
C52 C51 C56 C61 173.6(3) . . . . ?
C53 C54 C57 C58 64.6(5) . . . . ?
C55 C54 C57 C58 -114.7(4) . . . . ?
C53 C54 C57 C60 -175.2(5) . . . . ?
C55 C54 C57 C60 5.5(6) . . . . ?
C53 C54 C57 C59 -55.1(5) . . . . ?
C55 C54 C57 C59 125.6(4) . . . . ?
C55 C56 C61 C62 -98.3(4) . . . . ?
C51 C56 C61 C62 80.2(4) . . . . ?
C55 C56 C61 C64 137.6(3) . . . . ?
C51 C56 C61 C64 -43.9(5) . . . . ?
C55 C56 C61 C63 20.2(5) . . . . ?
C51 C56 C61 C63 -161.3(3) . . . . ?
O3 V1 O4 C65A -8.1(10) . . . . ?
O1 V1 O4 C65A 110.7(10) . . . . ?
O2 V1 O4 C65A -126.8(10) . . . . ?
O3 V1 O4 C65B 3.5(4) . . . . ?
O1 V1 O4 C65B 122.4(3) . . . . ?
O2 V1 O4 C65B -115.2(4) . . . . ?
C65B O4 C65A C67A 38.0(7) . . . . ?
V1 O4 C65A C67A 55.6(13) . . . . ?
C65B O4 C65A C66A -83.8(10) . . . . ?
V1 O4 C65A C66A -66.2(12) . . . . ?
C65A O4 C65B C66B 63.8(9) . . . . ?
V1 O4 C65B C66B -108.2(6) . . . . ?
C65A O4 C65B C67B -57.9(8) . . . . ?
V1 O4 C65B C67B 130.1(5) . . . . ?
C37 C42 O5 V2 -67.1(4) . . . . ?
C41 C42 O5 V2 116.2(3) . . . . ?
O7 V2 O5 C42 -44.2(3) . . . . ?
O8 V2 O5 C42 -166.8(2) . . . . ?
O6 V2 O5 C42 72.7(3) . . . . ?
C56 C51 O6 V2 -108.9(3) . . . . ?
C52 C51 O6 V2 70.9(3) . . . . ?
O7 V2 O6 C51 40.9(3) . . . . ?
O8 V2 O6 C51 162.8(2) . . . . ?
O5 V2 O6 C51 -75.8(2) . . . . ?
O7 V2 O8 C68 -2.8(5) . . . . ?
O6 V2 O8 C68 -121.6(4) . . . . ?
O5 V2 O8 C68 116.6(4) . . . . ?
V2 O8 C68 C69 -72.8(8) . . . . ?
V2 O8 C68 C70 50.8(7) . . . . ?

_refine_diff_density_max         0.625
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.086

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1404525'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_CHEMW03_5_2                 
;
RESPONSE: The composition calculated using the SQUEEZE
routine is reported rather than that derived from the 
point model. This explains the discrepancy. 
;

_vrf_PLAT051_5_2                 
;
RESPONSE: The composition calculated using the SQUEEZE
routine is reported rather than that derived from the 
point model. The total number of atoms in these two counts 
is different and hence the value of Mu is also different. 
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H104 O8 V2, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H108 Cl4 O8 V2'
_chemical_formula_weight         1369.28

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'
Cl Cl 0.1484 0.1585 '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                   21.4616(15)
_cell_length_b                   14.3723(10)
_cell_length_c                   25.6780(18)
_cell_angle_alpha                90
_cell_angle_beta                 104.2670(10)
_cell_angle_gamma                90
_cell_volume                     7676.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    81355
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Blade
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_F_000             2920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.432
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
A multi-scan absorption correction was implemented
within Rigaku CrystalClear.  
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_exptl_special_details           
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;

_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            91396
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.392
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             17489
_reflns_number_gt                13364
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0825P)²+5.3967P] 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         17489
_refine_ls_number_parameters     794
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1615
_refine_ls_wR_factor_gt          0.1439
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.040
_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 0.62741(2) 0.31419(3) 0.85523(2) 0.02478(9) Uani 1 1 d . . . . .
V2 V 0.28778(2) -0.05016(3) 0.57578(2) 0.02582(9) Uani 1 1 d . . . . .
O1 O 0.59101(7) 0.26977(10) 0.90609(6) 0.0250(3) Uani 1 1 d . . . . .
O2 O 0.58370(7) 0.27876(11) 0.78951(6) 0.0274(3) Uani 1 1 d . . . . .
O3 O 0.23796(7) -0.05796(10) 0.62221(6) 0.0272(3) Uani 1 1 d . . . . .
O4 O 0.35380(7) 0.02871(11) 0.59614(6) 0.0286(3) Uani 1 1 d . . . . .
O5 O 0.69720(8) 0.26991(12) 0.86513(7) 0.0336(4) Uani 1 1 d . . . . .
O7 O 0.24479(8) -0.01550(12) 0.51951(7) 0.0353(4) Uani 1 1 d . . . . .
C1 C 0.59164(10) 0.17891(14) 0.92347(8) 0.0230(4) Uani 1 1 d . . . . .
C2 C 0.62612(10) 0.15388(15) 0.97568(8) 0.0248(4) Uani 1 1 d . . . . .
C3 C 0.62631(10) 0.05941(15) 0.98864(8) 0.0262(4) Uani 1 1 d . . . . .
H3 H 0.6497 0.0404 1.0234 0.031 Uiso 1 1 calc R U . . .
C4 C 0.59394(10) -0.00881(15) 0.95314(8) 0.0253(4) Uani 1 1 d . . . . .
C5 C 0.55790(10) 0.02079(15) 0.90330(8) 0.0244(4) Uani 1 1 d . . . . .
H5 H 0.5341 -0.0238 0.8791 0.029 Uiso 1 1 calc R U . . .
C6 C 0.55561(9) 0.11352(15) 0.88778(8) 0.0231(4) Uani 1 1 d . . . . .
C7 C 0.66179(11) 0.22552(16) 1.01688(9) 0.0301(5) Uani 1 1 d . . . . .
C8 C 0.71861(13) 0.2681(2) 0.99926(11) 0.0425(6) Uani 1 1 d . . . . .
H8A H 0.7027 0.3031 0.9659 0.064 Uiso 1 1 calc R U . . .
H8B H 0.7473 0.2185 0.9933 0.064 Uiso 1 1 calc R U . . .
H8C H 0.7422 0.3101 1.0274 0.064 Uiso 1 1 calc R U . . .
C9 C 0.61584(13) 0.30341(18) 1.02510(10) 0.0395(6) Uani 1 1 d . . . . .
H9A H 0.5989 0.3359 0.9910 0.059 Uiso 1 1 calc R U . . .
H9B H 0.6392 0.3476 1.0520 0.059 Uiso 1 1 calc R U . . .
H9C H 0.5802 0.2763 1.0376 0.059 Uiso 1 1 calc R U . . .
C10 C 0.68932(14) 0.18054(19) 1.07195(10) 0.0427(6) Uani 1 1 d . . . . .
H10A H 0.7094 0.2285 1.0978 0.064 Uiso 1 1 calc R U . . .
H10B H 0.7216 0.1340 1.0689 0.064 Uiso 1 1 calc R U . . .
H10C H 0.6546 0.1504 1.0843 0.064 Uiso 1 1 calc R U . . .
C11 C 0.59431(11) -0.11170(16) 0.96844(9) 0.0298(5) Uani 1 1 d . . . . .
C12 C 0.64585(12) -0.13360(17) 1.01961(9) 0.0345(5) Uani 1 1 d . . . . .
H12A H 0.6878 -0.1122 1.0156 0.052 Uiso 1 1 calc R U . . .
H12B H 0.6474 -0.2009 1.0259 0.052 Uiso 1 1 calc R U . . .
H12C H 0.6355 -0.1018 1.0502 0.052 Uiso 1 1 calc R U . . .
C13 C 0.52813(12) -0.13705(18) 0.97738(11) 0.0395(6) Uani 1 1 d . . . . .
H13A H 0.5188 -0.0970 1.0054 0.059 Uiso 1 1 calc R U . . .
H13B H 0.5283 -0.2023 0.9886 0.059 Uiso 1 1 calc R U . . .
H13C H 0.4951 -0.1281 0.9438 0.059 Uiso 1 1 calc R U . . .
C14 C 0.60833(14) -0.17220(17) 0.92319(10) 0.0410(6) Uani 1 1 d . . . . .
H14A H 0.5744 -0.1629 0.8902 0.061 Uiso 1 1 calc R U . . .
H14B H 0.6095 -0.2379 0.9337 0.061 Uiso 1 1 calc R U . . .
H14C H 0.6499 -0.1544 0.9169 0.061 Uiso 1 1 calc R U . . .
C15 C 0.51513(9) 0.14353(15) 0.83278(8) 0.0228(4) Uani 1 1 d . . . . .
H15 H 0.5112 0.2128 0.8338 0.027 Uiso 1 1 calc R U . . .
C16 C 0.58202(10) 0.19103(15) 0.76755(8) 0.0263(4) Uani 1 1 d . . . . .
C17 C 0.60885(11) 0.17368(17) 0.72369(9) 0.0311(5) Uani 1 1 d . . . . .
C18 C 0.60494(12) 0.08266(18) 0.70449(10) 0.0370(5) Uani 1 1 d . . . . .
H18 H 0.6232 0.0690 0.6752 0.044 Uiso 1 1 calc R U . . .
C19 C 0.57572(12) 0.01070(17) 0.72581(10) 0.0343(5) Uani 1 1 d . . . . .
C20 C 0.54850(10) 0.03174(16) 0.76826(9) 0.0279(4) Uani 1 1 d . . . . .
H20 H 0.5282 -0.0164 0.7834 0.033 Uiso 1 1 calc R U . . .
C21 C 0.55017(9) 0.12089(15) 0.78905(8) 0.0243(4) Uani 1 1 d . . . . .
C22 C 0.64022(12) 0.25138(18) 0.69714(10) 0.0357(5) Uani 1 1 d . . . . .
C23 C 0.70273(13) 0.2844(2) 0.73568(11) 0.0450(6) Uani 1 1 d . . . . .
H23A H 0.7230 0.3318 0.7179 0.068 Uiso 1 1 calc R U . . .
H23B H 0.7320 0.2314 0.7458 0.068 Uiso 1 1 calc R U . . .
H23C H 0.6931 0.3109 0.7680 0.068 Uiso 1 1 calc R U . . .
C24 C 0.59374(14) 0.3327(2) 0.68064(11) 0.0448(6) Uani 1 1 d . . . . .
H24A H 0.5537 0.3102 0.6568 0.067 Uiso 1 1 calc R U . . .
H24B H 0.6132 0.3795 0.6618 0.067 Uiso 1 1 calc R U . . .
H24C H 0.5845 0.3606 0.7128 0.067 Uiso 1 1 calc R U . . .
C25 C 0.65762(15) 0.2164(2) 0.64596(11) 0.0487(7) Uani 1 1 d . . . . .
H25A H 0.6188 0.1931 0.6206 0.073 Uiso 1 1 calc R U . . .
H25B H 0.6892 0.1660 0.6552 0.073 Uiso 1 1 calc R U . . .
H25C H 0.6759 0.2676 0.6294 0.073 Uiso 1 1 calc R U . . .
C26 C 0.56876(15) -0.0883(2) 0.70276(12) 0.0478(7) Uani 1 1 d . U . . .
C27 C 0.6008(3) -0.0983(3) 0.65577(19) 0.0993(18) Uani 1 1 d . U . . .
H27A H 0.6476 -0.0947 0.6693 0.149 Uiso 1 1 calc R U . . .
H27B H 0.5861 -0.0481 0.6298 0.149 Uiso 1 1 calc R U . . .
H27C H 0.5891 -0.1585 0.6381 0.149 Uiso 1 1 calc R U . . .
C28 C 0.49642(17) -0.1094(2) 0.68072(12) 0.0550(8) Uani 1 1 d . U . . .
H28A H 0.4911 -0.1730 0.6666 0.082 Uiso 1 1 calc R U . . .
H28B H 0.4779 -0.0654 0.6519 0.082 Uiso 1 1 calc R U . . .
H28C H 0.4744 -0.1032 0.7097 0.082 Uiso 1 1 calc R U . . .
C29 C 0.59797(15) -0.1582(2) 0.74693(14) 0.0556(8) Uani 1 1 d . U . . .
H29A H 0.5929 -0.2213 0.7321 0.083 Uiso 1 1 calc R U . . .
H29B H 0.5759 -0.1534 0.7760 0.083 Uiso 1 1 calc R U . . .
H29C H 0.6438 -0.1445 0.7610 0.083 Uiso 1 1 calc R U . . .
C30 C 0.44670(10) 0.10454(14) 0.81879(8) 0.0232(4) Uani 1 1 d . . . . .
C31 C 0.41168(10) 0.10723(15) 0.76520(8) 0.0238(4) Uani 1 1 d . . . . .
H31 H 0.4322 0.1290 0.7387 0.029 Uiso 1 1 calc R U . . .
C32 C 0.34785(10) 0.07916(14) 0.74935(8) 0.0225(4) Uani 1 1 d . . . . .
C33 C 0.31825(10) 0.04626(15) 0.78816(8) 0.0257(4) Uani 1 1 d . . . . .
H33 H 0.2750 0.0253 0.7780 0.031 Uiso 1 1 calc R U . . .
C34 C 0.35197(11) 0.04410(17) 0.84167(9) 0.0301(5) Uani 1 1 d . . . . .
H34 H 0.3314 0.0224 0.8681 0.036 Uiso 1 1 calc R U . . .
C35 C 0.41558(10) 0.07335(16) 0.85706(8) 0.0276(4) Uani 1 1 d . . . . .
H35 H 0.4380 0.0721 0.8939 0.033 Uiso 1 1 calc R U . . .
C36 C 0.31455(9) 0.07395(14) 0.68948(8) 0.0222(4) Uani 1 1 d . . . . .
H36 H 0.3264 0.0122 0.6768 0.027 Uiso 1 1 calc R U . . .
C37 C 0.20507(10) 0.00745(14) 0.64433(8) 0.0233(4) Uani 1 1 d . . . . .
C38 C 0.13743(10) 0.00263(15) 0.63591(8) 0.0264(4) Uani 1 1 d . . . . .
C39 C 0.10896(10) 0.07294(16) 0.65946(8) 0.0268(4) Uani 1 1 d . . . . .
H39 H 0.0635 0.0722 0.6538 0.032 Uiso 1 1 calc R U . . .
C40 C 0.14336(10) 0.14480(15) 0.69098(8) 0.0257(4) Uani 1 1 d . . . . .
C41 C 0.20961(10) 0.14366(15) 0.69959(8) 0.0245(4) Uani 1 1 d . . . . .
H41 H 0.2342 0.1908 0.7212 0.029 Uiso 1 1 calc R U . . .
C42 C 0.24138(9) 0.07528(14) 0.67741(8) 0.0223(4) Uani 1 1 d . . . . .
C43 C 0.09717(11) -0.07605(18) 0.60380(9) 0.0336(5) Uani 1 1 d . . . . .
C44 C 0.09989(13) -0.0730(2) 0.54437(10) 0.0400(6) Uani 1 1 d . . . . .
H44A H 0.0724 -0.1222 0.5244 0.060 Uiso 1 1 calc R U . . .
H44B H 0.1443 -0.0827 0.5419 0.060 Uiso 1 1 calc R U . . .
H44C H 0.0847 -0.0123 0.5290 0.060 Uiso 1 1 calc R U . . .
C45 C 0.02614(12) -0.0680(2) 0.60467(12) 0.0477(7) Uani 1 1 d . . . . .
H45A H 0.0223 -0.0706 0.6419 0.072 Uiso 1 1 calc R U . . .
H45B H 0.0019 -0.1195 0.5842 0.072 Uiso 1 1 calc R U . . .
H45C H 0.0088 -0.0087 0.5885 0.072 Uiso 1 1 calc R U . . .
C46 C 0.12156(14) -0.17082(18) 0.62812(11) 0.0430(6) Uani 1 1 d . . . . .
H46A H 0.1183 -0.1735 0.6655 0.065 Uiso 1 1 calc R U . . .
H46B H 0.1665 -0.1790 0.6270 0.065 Uiso 1 1 calc R U . . .
H46C H 0.0954 -0.2205 0.6074 0.065 Uiso 1 1 calc R U . . .
C47 C 0.10830(11) 0.22040(16) 0.71530(9) 0.0305(5) Uani 1 1 d D U . . .
C48 C 0.0621(2) 0.2745(3) 0.66920(16) 0.0523(11) Uani 0.745(5) 1 d D U P A 1
H48A H 0.0868 0.3030 0.6460 0.078 Uiso 0.745(5) 1 calc R U P A 1
H48B H 0.0303 0.2315 0.6481 0.078 Uiso 0.745(5) 1 calc R U P A 1
H48C H 0.0400 0.3233 0.6845 0.078 Uiso 0.745(5) 1 calc R U P A 1
C49 C 0.0689(2) 0.1777(2) 0.75014(17) 0.0442(10) Uani 0.745(5) 1 d D U P A 1
H49A H 0.0471 0.2270 0.7652 0.066 Uiso 0.745(5) 1 calc R U P A 1
H49B H 0.0369 0.1356 0.7285 0.066 Uiso 0.745(5) 1 calc R U P A 1
H49C H 0.0972 0.1428 0.7794 0.066 Uiso 0.745(5) 1 calc R U P A 1
C50 C 0.15470(19) 0.2920(3) 0.7490(2) 0.0544(12) Uani 0.745(5) 1 d D U P A 1
H50A H 0.1807 0.3204 0.7268 0.082 Uiso 0.745(5) 1 calc R U P A 1
H50B H 0.1299 0.3404 0.7618 0.082 Uiso 0.745(5) 1 calc R U P A 1
H50C H 0.1830 0.2607 0.7798 0.082 Uiso 0.745(5) 1 calc R U P A 1
C48X C 0.1146(5) 0.3110(6) 0.6901(5) 0.042(3) Uani 0.255(5) 1 d D U P A 2
H48D H 0.0922 0.3588 0.7057 0.063 Uiso 0.255(5) 1 calc R U P A 2
H48E H 0.1602 0.3273 0.6965 0.063 Uiso 0.255(5) 1 calc R U P A 2
H48F H 0.0956 0.3070 0.6514 0.063 Uiso 0.255(5) 1 calc R U P A 2
C49X C 0.0368(4) 0.1953(8) 0.7078(5) 0.047(3) Uani 0.255(5) 1 d D U P A 2
H49D H 0.0334 0.1350 0.7247 0.071 Uiso 0.255(5) 1 calc R U P A 2
H49E H 0.0157 0.2432 0.7246 0.071 Uiso 0.255(5) 1 calc R U P A 2
H49F H 0.0159 0.1917 0.6694 0.071 Uiso 0.255(5) 1 calc R U P A 2
C50X C 0.1389(6) 0.2222(8) 0.7768(4) 0.049(3) Uani 0.255(5) 1 d D U P A 2
H50D H 0.1338 0.1610 0.7921 0.073 Uiso 0.255(5) 1 calc R U P A 2
H50E H 0.1847 0.2371 0.7833 0.073 Uiso 0.255(5) 1 calc R U P A 2
H50F H 0.1174 0.2695 0.7936 0.073 Uiso 0.255(5) 1 calc R U P A 2
C51 C 0.35964(10) 0.12087(15) 0.61073(8) 0.0245(4) Uani 1 1 d . . . . .
C52 C 0.38847(10) 0.18585(16) 0.58266(8) 0.0269(4) Uani 1 1 d . . . . .
C53 C 0.39381(10) 0.27678(16) 0.60169(9) 0.0280(4) Uani 1 1 d . . . . .
H53 H 0.4126 0.3217 0.5831 0.034 Uiso 1 1 calc R U . . .
C54 C 0.37311(10) 0.30584(15) 0.64658(8) 0.0259(4) Uani 1 1 d . . . . .
C55 C 0.34584(10) 0.23885(15) 0.67305(8) 0.0239(4) Uani 1 1 d . . . . .
H55 H 0.3310 0.2569 0.7035 0.029 Uiso 1 1 calc R U . . .
C56 C 0.33943(9) 0.14676(15) 0.65671(8) 0.0232(4) Uani 1 1 d . . . . .
C57 C 0.41682(11) 0.15683(18) 0.53555(9) 0.0332(5) Uani 1 1 d . . . . .
C58 C 0.36543(13) 0.1154(2) 0.48888(10) 0.0422(6) Uani 1 1 d . . . . .
H58A H 0.3326 0.1625 0.4747 0.063 Uiso 1 1 calc R U . . .
H58B H 0.3453 0.0617 0.5018 0.063 Uiso 1 1 calc R U . . .
H58C H 0.3855 0.0954 0.4604 0.063 Uiso 1 1 calc R U . . .
C59 C 0.44623(14) 0.2403(2) 0.51278(11) 0.0452(6) Uani 1 1 d . . . . .
H59A H 0.4617 0.2202 0.4817 0.068 Uiso 1 1 calc R U . . .
H59B H 0.4823 0.2651 0.5405 0.068 Uiso 1 1 calc R U . . .
H59C H 0.4135 0.2887 0.5017 0.068 Uiso 1 1 calc R U . . .
C60 C 0.47062(12) 0.08560(19) 0.55605(11) 0.0400(6) Uani 1 1 d . . . . .
H60A H 0.4522 0.0287 0.5671 0.060 Uiso 1 1 calc R U . . .
H60B H 0.5022 0.1117 0.5868 0.060 Uiso 1 1 calc R U . . .
H60C H 0.4918 0.0710 0.5273 0.060 Uiso 1 1 calc R U . . .
C61 C 0.38335(11) 0.40464(16) 0.66925(9) 0.0306(5) Uani 1 1 d . . . . .
C62 C 0.32133(15) 0.4456(2) 0.67592(19) 0.0713(12) Uani 1 1 d . . . . .
H62A H 0.2915 0.4534 0.6405 0.107 Uiso 1 1 calc R U . . .
H62B H 0.3298 0.5063 0.6937 0.107 Uiso 1 1 calc R U . . .
H62C H 0.3022 0.4039 0.6979 0.107 Uiso 1 1 calc R U . . .
C63 C 0.41504(19) 0.4683(2) 0.63547(13) 0.0595(9) Uani 1 1 d . . . . .
H63A H 0.3866 0.4750 0.5994 0.089 Uiso 1 1 calc R U . . .
H63B H 0.4560 0.4411 0.6327 0.089 Uiso 1 1 calc R U . . .
H63C H 0.4229 0.5296 0.6526 0.089 Uiso 1 1 calc R U . . .
C64 C 0.43084(16) 0.3991(2) 0.72502(12) 0.0523(7) Uani 1 1 d . . . . .
H64A H 0.4402 0.4619 0.7396 0.079 Uiso 1 1 calc R U . . .
H64B H 0.4708 0.3694 0.7217 0.079 Uiso 1 1 calc R U . . .
H64C H 0.4117 0.3622 0.7492 0.079 Uiso 1 1 calc R U . . .
O6 O 0.62844(8) 0.43453(11) 0.85617(6) 0.0307(3) Uani 1 1 d . . . . .
C65 C 0.66906(13) 0.51555(17) 0.85581(10) 0.0375(5) Uani 1 1 d . . . . .
C66 C 0.6611(2) 0.5411(2) 0.79690(13) 0.0698(11) Uani 1 1 d . . . . .
H66A H 0.6792 0.4917 0.7789 0.105 Uiso 1 1 calc R U . . .
H66B H 0.6836 0.5997 0.7945 0.105 Uiso 1 1 calc R U . . .
H66C H 0.6153 0.5485 0.7795 0.105 Uiso 1 1 calc R U . . .
C67 C 0.73738(13) 0.49003(18) 0.88339(12) 0.0418(6) Uani 1 1 d . . . . .
H67A H 0.7397 0.4716 0.9206 0.063 Uiso 1 1 calc R U . . .
H67B H 0.7654 0.5438 0.8832 0.063 Uiso 1 1 calc R U . . .
H67C H 0.7514 0.4381 0.8643 0.063 Uiso 1 1 calc R U . . .
C68 C 0.64306(16) 0.5904(2) 0.88564(15) 0.0567(8) Uani 1 1 d . . . . .
H68A H 0.5986 0.6046 0.8667 0.085 Uiso 1 1 calc R U . . .
H68B H 0.6694 0.6466 0.8876 0.085 Uiso 1 1 calc R U . . .
H68C H 0.6443 0.5688 0.9221 0.085 Uiso 1 1 calc R U . . .
O8 O 0.32070(8) -0.15867(11) 0.57025(6) 0.0327(3) Uani 1 1 d . . . . .
C69 C 0.33490(12) -0.22441(18) 0.53231(10) 0.0379(5) Uani 1 1 d . . . . .
C70 C 0.28053(13) -0.22518(18) 0.48225(10) 0.0389(5) Uani 1 1 d . . . . .
H70A H 0.2403 -0.2407 0.4918 0.058 Uiso 1 1 calc R U . . .
H70B H 0.2893 -0.2717 0.4571 0.058 Uiso 1 1 calc R U . . .
H70C H 0.2767 -0.1636 0.4654 0.058 Uiso 1 1 calc R U . . .
C71 C 0.39695(15) -0.1909(3) 0.51975(15) 0.0675(10) Uani 1 1 d . . . . .
H71A H 0.3899 -0.1297 0.5025 0.101 Uiso 1 1 calc R U . . .
H71B H 0.4101 -0.2352 0.4955 0.101 Uiso 1 1 calc R U . . .
H71C H 0.4308 -0.1862 0.5532 0.101 Uiso 1 1 calc R U . . .
C72 C 0.3425(2) -0.3170(2) 0.56082(14) 0.0685(10) Uani 1 1 d . . . . .
H72A H 0.3791 -0.3142 0.5923 0.103 Uiso 1 1 calc R U . . .
H72B H 0.3499 -0.3657 0.5363 0.103 Uiso 1 1 calc R U . . .
H72C H 0.3033 -0.3312 0.5724 0.103 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 O5 1.5890(16) . ?
V1 O6 1.7298(16) . ?
V1 O2 1.7908(15) . ?
V1 O1 1.7963(15) . ?
V2 O7 1.5908(17) . ?
V2 O8 1.7323(16) . ?
V2 O4 1.7891(16) . ?
V2 O3 1.7904(15) . ?
O1 C1 1.379(2) . ?
O2 C16 1.378(3) . ?
O3 C37 1.379(2) . ?
O4 C51 1.374(3) . ?
C1 C6 1.404(3) . ?
C1 C2 1.409(3) . ?
C2 C3 1.398(3) . ?
C2 C7 1.538(3) . ?
C3 C4 1.401(3) . ?
C4 C5 1.389(3) . ?
C4 C11 1.530(3) . ?
C5 C6 1.388(3) . ?
C6 C15 1.527(3) . ?
C7 C8 1.529(3) . ?
C7 C10 1.534(3) . ?
C7 C9 1.541(3) . ?
C11 C12 1.527(3) . ?
C11 C13 1.537(3) . ?
C11 C14 1.539(3) . ?
C15 C30 1.530(3) . ?
C15 C21 1.533(3) . ?
C16 C21 1.405(3) . ?
C16 C17 1.408(3) . ?
C17 C18 1.393(3) . ?
C17 C22 1.546(3) . ?
C18 C19 1.390(3) . ?
C19 C20 1.391(3) . ?
C19 C26 1.534(3) . ?
C20 C21 1.385(3) . ?
C22 C24 1.528(4) . ?
C22 C23 1.533(4) . ?
C22 C25 1.537(3) . ?
C26 C29 1.529(5) . ?
C26 C27 1.535(4) . ?
C26 C28 1.546(4) . ?
C30 C35 1.391(3) . ?
C30 C31 1.396(3) . ?
C31 C32 1.389(3) . ?
C32 C33 1.390(3) . ?
C32 C36 1.529(3) . ?
C33 C34 1.387(3) . ?
C34 C35 1.390(3) . ?
C36 C56 1.520(3) . ?
C36 C42 1.524(3) . ?
C37 C42 1.397(3) . ?
C37 C38 1.416(3) . ?
C38 C39 1.393(3) . ?
C38 C43 1.534(3) . ?
C39 C40 1.404(3) . ?
C40 C41 1.384(3) . ?
C40 C47 1.539(3) . ?
C41 C42 1.395(3) . ?
C43 C45 1.534(3) . ?
C43 C46 1.536(4) . ?
C43 C44 1.542(3) . ?
C47 C48X 1.474(9) . ?
C47 C49 1.504(4) . ?
C47 C50 1.541(4) . ?
C47 C49X 1.541(9) . ?
C47 C48 1.553(4) . ?
C47 C50X 1.553(9) . ?
C51 C56 1.405(3) . ?
C51 C52 1.412(3) . ?
C52 C53 1.390(3) . ?
C52 C57 1.540(3) . ?
C53 C54 1.398(3) . ?
C54 C55 1.388(3) . ?
C54 C61 1.530(3) . ?
C55 C56 1.385(3) . ?
C57 C58 1.535(3) . ?
C57 C60 1.536(4) . ?
C57 C59 1.536(4) . ?
C61 C62 1.503(4) . ?
C61 C63 1.531(4) . ?
C61 C64 1.542(4) . ?
O6 C65 1.456(3) . ?
C65 C68 1.505(4) . ?
C65 C67 1.508(4) . ?
C65 C66 1.525(4) . ?
O8 C69 1.443(3) . ?
C69 C72 1.508(4) . ?
C69 C70 1.508(4) . ?
C69 C71 1.524(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 V1 O6 112.95(8) . . ?
O5 V1 O2 106.92(8) . . ?
O6 V1 O2 107.42(7) . . ?
O5 V1 O1 107.64(8) . . ?
O6 V1 O1 110.58(7) . . ?
O2 V1 O1 111.31(7) . . ?
O7 V2 O8 111.37(8) . . ?
O7 V2 O4 107.89(8) . . ?
O8 V2 O4 106.54(8) . . ?
O7 V2 O3 108.46(8) . . ?
O8 V2 O3 108.72(8) . . ?
O4 V2 O3 113.89(7) . . ?
C1 O1 V1 126.91(13) . . ?
C16 O2 V1 126.91(13) . . ?
C37 O3 V2 132.98(13) . . ?
C51 O4 V2 134.67(13) . . ?
O1 C1 C6 117.55(18) . . ?
O1 C1 C2 120.71(18) . . ?
C6 C1 C2 121.72(19) . . ?
C3 C2 C1 116.40(18) . . ?
C3 C2 C7 120.97(19) . . ?
C1 C2 C7 122.63(19) . . ?
C2 C3 C4 123.57(19) . . ?
C5 C4 C3 117.35(19) . . ?
C5 C4 C11 119.95(19) . . ?
C3 C4 C11 122.62(19) . . ?
C6 C5 C4 122.05(19) . . ?
C5 C6 C1 118.70(19) . . ?
C5 C6 C15 120.56(18) . . ?
C1 C6 C15 120.74(19) . . ?
C8 C7 C10 106.7(2) . . ?
C8 C7 C2 111.25(19) . . ?
C10 C7 C2 111.42(19) . . ?
C8 C7 C9 109.5(2) . . ?
C10 C7 C9 107.1(2) . . ?
C2 C7 C9 110.72(18) . . ?
C12 C11 C4 112.15(19) . . ?
C12 C11 C13 108.83(19) . . ?
C4 C11 C13 108.72(18) . . ?
C12 C11 C14 107.34(19) . . ?
C4 C11 C14 109.99(19) . . ?
C13 C11 C14 109.8(2) . . ?
C6 C15 C30 114.10(17) . . ?
C6 C15 C21 110.35(16) . . ?
C30 C15 C21 111.48(16) . . ?
O2 C16 C21 117.52(18) . . ?
O2 C16 C17 120.98(19) . . ?
C21 C16 C17 121.4(2) . . ?
C18 C17 C16 116.7(2) . . ?
C18 C17 C22 121.1(2) . . ?
C16 C17 C22 122.2(2) . . ?
C19 C18 C17 123.6(2) . . ?
C18 C19 C20 117.7(2) . . ?
C18 C19 C26 123.3(2) . . ?
C20 C19 C26 119.0(2) . . ?
C21 C20 C19 121.8(2) . . ?
C20 C21 C16 118.77(19) . . ?
C20 C21 C15 120.53(19) . . ?
C16 C21 C15 120.64(19) . . ?
C24 C22 C23 110.5(2) . . ?
C24 C22 C25 107.1(2) . . ?
C23 C22 C25 107.2(2) . . ?
C24 C22 C17 110.5(2) . . ?
C23 C22 C17 110.2(2) . . ?
C25 C22 C17 111.4(2) . . ?
C29 C26 C19 109.9(2) . . ?
C29 C26 C27 109.9(3) . . ?
C19 C26 C27 111.7(2) . . ?
C29 C26 C28 109.5(2) . . ?
C19 C26 C28 108.5(2) . . ?
C27 C26 C28 107.3(3) . . ?
C35 C30 C31 117.99(18) . . ?
C35 C30 C15 123.52(18) . . ?
C31 C30 C15 118.28(18) . . ?
C32 C31 C30 122.22(19) . . ?
C31 C32 C33 118.72(18) . . ?
C31 C32 C36 119.44(17) . . ?
C33 C32 C36 121.42(18) . . ?
C34 C33 C32 119.93(19) . . ?
C33 C34 C35 120.75(19) . . ?
C34 C35 C30 120.37(19) . . ?
C56 C36 C42 111.33(16) . . ?
C56 C36 C32 112.46(16) . . ?
C42 C36 C32 113.99(16) . . ?
O3 C37 C42 117.42(18) . . ?
O3 C37 C38 120.89(18) . . ?
C42 C37 C38 121.61(19) . . ?
C39 C38 C37 116.17(19) . . ?
C39 C38 C43 121.24(19) . . ?
C37 C38 C43 122.6(2) . . ?
C38 C39 C40 123.99(19) . . ?
C41 C40 C39 117.17(19) . . ?
C41 C40 C47 121.96(19) . . ?
C39 C40 C47 120.87(19) . . ?
C40 C41 C42 121.96(19) . . ?
C41 C42 C37 118.96(18) . . ?
C41 C42 C36 120.57(18) . . ?
C37 C42 C36 120.47(18) . . ?
C38 C43 C45 111.5(2) . . ?
C38 C43 C46 110.18(19) . . ?
C45 C43 C46 107.6(2) . . ?
C38 C43 C44 110.94(19) . . ?
C45 C43 C44 107.0(2) . . ?
C46 C43 C44 109.6(2) . . ?
C48X C47 C40 109.8(4) . . ?
C49 C47 C40 110.9(2) . . ?
C49 C47 C50 108.6(3) . . ?
C40 C47 C50 112.7(2) . . ?
C48X C47 C49X 110.4(6) . . ?
C40 C47 C49X 110.8(4) . . ?
C49 C47 C48 108.1(3) . . ?
C40 C47 C48 109.2(2) . . ?
C50 C47 C48 107.2(3) . . ?
C48X C47 C50X 111.7(7) . . ?
C40 C47 C50X 107.3(4) . . ?
C49X C47 C50X 106.8(7) . . ?
O4 C51 C56 117.27(18) . . ?
O4 C51 C52 121.36(18) . . ?
C56 C51 C52 121.25(19) . . ?
C53 C52 C51 116.80(19) . . ?
C53 C52 C57 121.1(2) . . ?
C51 C52 C57 122.0(2) . . ?
C52 C53 C54 123.7(2) . . ?
C55 C54 C53 117.0(2) . . ?
C55 C54 C61 119.72(19) . . ?
C53 C54 C61 123.1(2) . . ?
C56 C55 C54 122.46(19) . . ?
C55 C56 C51 118.66(19) . . ?
C55 C56 C36 120.82(18) . . ?
C51 C56 C36 120.43(19) . . ?
C58 C57 C60 110.1(2) . . ?
C58 C57 C59 106.8(2) . . ?
C60 C57 C59 107.8(2) . . ?
C58 C57 C52 111.80(19) . . ?
C60 C57 C52 108.70(19) . . ?
C59 C57 C52 111.5(2) . . ?
C62 C61 C54 111.0(2) . . ?
C62 C61 C63 111.1(3) . . ?
C54 C61 C63 112.4(2) . . ?
C62 C61 C64 108.4(3) . . ?
C54 C61 C64 107.8(2) . . ?
C63 C61 C64 105.8(2) . . ?
C65 O6 V1 143.63(15) . . ?
O6 C65 C68 105.7(2) . . ?
O6 C65 C67 108.47(19) . . ?
C68 C65 C67 112.0(2) . . ?
O6 C65 C66 106.1(2) . . ?
C68 C65 C66 111.5(3) . . ?
C67 C65 C66 112.5(3) . . ?
C69 O8 V2 143.45(16) . . ?
O8 C69 C72 105.4(2) . . ?
O8 C69 C70 109.4(2) . . ?
C72 C69 C70 112.0(2) . . ?
O8 C69 C71 106.1(2) . . ?
C72 C69 C71 112.7(3) . . ?
C70 C69 C71 110.8(2) . . ?

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 V1 O1 C1 -44.15(17) . . . . ?
O6 V1 O1 C1 -167.96(15) . . . . ?
O2 V1 O1 C1 72.72(17) . . . . ?
O5 V1 O2 C16 44.32(18) . . . . ?
O6 V1 O2 C16 165.84(16) . . . . ?
O1 V1 O2 C16 -72.98(17) . . . . ?
O7 V2 O3 C37 -64.71(19) . . . . ?
O8 V2 O3 C37 174.04(17) . . . . ?
O4 V2 O3 C37 55.4(2) . . . . ?
O7 V2 O4 C51 65.9(2) . . . . ?
O8 V2 O4 C51 -174.45(18) . . . . ?
O3 V2 O4 C51 -54.6(2) . . . . ?
V1 O1 C1 C6 -69.7(2) . . . . ?
V1 O1 C1 C2 111.79(19) . . . . ?
O1 C1 C2 C3 -177.08(18) . . . . ?
C6 C1 C2 C3 4.5(3) . . . . ?
O1 C1 C2 C7 3.1(3) . . . . ?
C6 C1 C2 C7 -175.35(19) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C7 C2 C3 C4 179.0(2) . . . . ?
C2 C3 C4 C5 -2.6(3) . . . . ?
C2 C3 C4 C11 -179.4(2) . . . . ?
C3 C4 C5 C6 2.6(3) . . . . ?
C11 C4 C5 C6 179.44(19) . . . . ?
C4 C5 C6 C1 0.9(3) . . . . ?
C4 C5 C6 C15 -179.64(18) . . . . ?
O1 C1 C6 C5 176.94(18) . . . . ?
C2 C1 C6 C5 -4.6(3) . . . . ?
O1 C1 C6 C15 -2.5(3) . . . . ?
C2 C1 C6 C15 175.96(18) . . . . ?
C3 C2 C7 C8 113.4(2) . . . . ?
C1 C2 C7 C8 -66.8(3) . . . . ?
C3 C2 C7 C10 -5.5(3) . . . . ?
C1 C2 C7 C10 174.3(2) . . . . ?
C3 C2 C7 C9 -124.6(2) . . . . ?
C1 C2 C7 C9 55.2(3) . . . . ?
C5 C4 C11 C12 169.21(19) . . . . ?
C3 C4 C11 C12 -14.1(3) . . . . ?
C5 C4 C11 C13 -70.4(3) . . . . ?
C3 C4 C11 C13 106.3(2) . . . . ?
C5 C4 C11 C14 49.8(3) . . . . ?
C3 C4 C11 C14 -133.5(2) . . . . ?
C5 C6 C15 C30 47.8(3) . . . . ?
C1 C6 C15 C30 -132.7(2) . . . . ?
C5 C6 C15 C21 -78.6(2) . . . . ?
C1 C6 C15 C21 100.9(2) . . . . ?
V1 O2 C16 C21 69.3(2) . . . . ?
V1 O2 C16 C17 -113.4(2) . . . . ?
O2 C16 C17 C18 179.8(2) . . . . ?
C21 C16 C17 C18 -3.0(3) . . . . ?
O2 C16 C17 C22 -1.2(3) . . . . ?
C21 C16 C17 C22 176.0(2) . . . . ?
C16 C17 C18 C19 0.9(4) . . . . ?
C22 C17 C18 C19 -178.1(2) . . . . ?
C17 C18 C19 C20 0.7(4) . . . . ?
C17 C18 C19 C26 177.0(3) . . . . ?
C18 C19 C20 C21 -0.1(4) . . . . ?
C26 C19 C20 C21 -176.6(2) . . . . ?
C19 C20 C21 C16 -2.0(3) . . . . ?
C19 C20 C21 C15 175.1(2) . . . . ?
O2 C16 C21 C20 -179.12(18) . . . . ?
C17 C16 C21 C20 3.6(3) . . . . ?
O2 C16 C21 C15 3.8(3) . . . . ?
C17 C16 C21 C15 -173.47(19) . . . . ?
C6 C15 C21 C20 81.0(2) . . . . ?
C30 C15 C21 C20 -46.9(3) . . . . ?
C6 C15 C21 C16 -102.0(2) . . . . ?
C30 C15 C21 C16 130.1(2) . . . . ?
C18 C17 C22 C24 125.1(3) . . . . ?
C16 C17 C22 C24 -53.8(3) . . . . ?
C18 C17 C22 C23 -112.5(3) . . . . ?
C16 C17 C22 C23 68.6(3) . . . . ?
C18 C17 C22 C25 6.3(3) . . . . ?
C16 C17 C22 C25 -172.6(2) . . . . ?
C18 C19 C26 C29 125.1(3) . . . . ?
C20 C19 C26 C29 -58.6(3) . . . . ?
C18 C19 C26 C27 2.8(5) . . . . ?
C20 C19 C26 C27 179.1(3) . . . . ?
C18 C19 C26 C28 -115.2(3) . . . . ?
C20 C19 C26 C28 61.1(3) . . . . ?
C6 C15 C30 C35 21.7(3) . . . . ?
C21 C15 C30 C35 147.5(2) . . . . ?
C6 C15 C30 C31 -163.65(18) . . . . ?
C21 C15 C30 C31 -37.8(3) . . . . ?
C35 C30 C31 C32 -0.7(3) . . . . ?
C15 C30 C31 C32 -175.61(19) . . . . ?
C30 C31 C32 C33 -0.8(3) . . . . ?
C30 C31 C32 C36 -173.43(19) . . . . ?
C31 C32 C33 C34 1.6(3) . . . . ?
C36 C32 C33 C34 174.0(2) . . . . ?
C32 C33 C34 C35 -0.9(3) . . . . ?
C33 C34 C35 C30 -0.6(4) . . . . ?
C31 C30 C35 C34 1.4(3) . . . . ?
C15 C30 C35 C34 176.0(2) . . . . ?
C31 C32 C36 C56 -32.2(3) . . . . ?
C33 C32 C36 C56 155.39(19) . . . . ?
C31 C32 C36 C42 -160.13(19) . . . . ?
C33 C32 C36 C42 27.4(3) . . . . ?
V2 O3 C37 C42 -63.7(3) . . . . ?
V2 O3 C37 C38 119.6(2) . . . . ?
O3 C37 C38 C39 -179.14(18) . . . . ?
C42 C37 C38 C39 4.2(3) . . . . ?
O3 C37 C38 C43 2.1(3) . . . . ?
C42 C37 C38 C43 -174.6(2) . . . . ?
C37 C38 C39 C40 -1.3(3) . . . . ?
C43 C38 C39 C40 177.5(2) . . . . ?
C38 C39 C40 C41 -1.3(3) . . . . ?
C38 C39 C40 C47 179.6(2) . . . . ?
C39 C40 C41 C42 1.0(3) . . . . ?
C47 C40 C41 C42 -179.81(19) . . . . ?
C40 C41 C42 C37 1.8(3) . . . . ?
C40 C41 C42 C36 -177.62(19) . . . . ?
O3 C37 C42 C41 178.73(18) . . . . ?
C38 C37 C42 C41 -4.5(3) . . . . ?
O3 C37 C42 C36 -1.9(3) . . . . ?
C38 C37 C42 C36 174.88(19) . . . . ?
C56 C36 C42 C41 -77.7(2) . . . . ?
C32 C36 C42 C41 50.8(3) . . . . ?
C56 C36 C42 C37 102.9(2) . . . . ?
C32 C36 C42 C37 -128.6(2) . . . . ?
C39 C38 C43 C45 -3.1(3) . . . . ?
C37 C38 C43 C45 175.7(2) . . . . ?
C39 C38 C43 C46 -122.4(2) . . . . ?
C37 C38 C43 C46 56.3(3) . . . . ?
C39 C38 C43 C44 116.1(2) . . . . ?
C37 C38 C43 C44 -65.2(3) . . . . ?
C41 C40 C47 C48X 67.9(6) . . . . ?
C39 C40 C47 C48X -112.9(5) . . . . ?
C41 C40 C47 C49 -121.7(3) . . . . ?
C39 C40 C47 C49 57.4(3) . . . . ?
C41 C40 C47 C50 0.2(3) . . . . ?
C39 C40 C47 C50 179.3(3) . . . . ?
C41 C40 C47 C49X -169.9(5) . . . . ?
C39 C40 C47 C49X 9.2(6) . . . . ?
C41 C40 C47 C48 119.3(3) . . . . ?
C39 C40 C47 C48 -61.6(3) . . . . ?
C41 C40 C47 C50X -53.7(6) . . . . ?
C39 C40 C47 C50X 125.5(6) . . . . ?
V2 O4 C51 C56 62.2(3) . . . . ?
V2 O4 C51 C52 -121.7(2) . . . . ?
O4 C51 C52 C53 -178.06(19) . . . . ?
C56 C51 C52 C53 -2.1(3) . . . . ?
O4 C51 C52 C57 -2.0(3) . . . . ?
C56 C51 C52 C57 174.0(2) . . . . ?
C51 C52 C53 C54 0.7(3) . . . . ?
C57 C52 C53 C54 -175.3(2) . . . . ?
C52 C53 C54 C55 0.0(3) . . . . ?
C52 C53 C54 C61 175.8(2) . . . . ?
C53 C54 C55 C56 0.5(3) . . . . ?
C61 C54 C55 C56 -175.39(19) . . . . ?
C54 C55 C56 C51 -1.9(3) . . . . ?
C54 C55 C56 C36 174.77(19) . . . . ?
O4 C51 C56 C55 178.78(18) . . . . ?
C52 C51 C56 C55 2.6(3) . . . . ?
O4 C51 C56 C36 2.1(3) . . . . ?
C52 C51 C56 C36 -174.00(19) . . . . ?
C42 C36 C56 C55 81.6(2) . . . . ?
C32 C36 C56 C55 -47.7(3) . . . . ?
C42 C36 C56 C51 -101.8(2) . . . . ?
C32 C36 C56 C51 128.9(2) . . . . ?
C53 C52 C57 C58 -122.6(2) . . . . ?
C51 C52 C57 C58 61.5(3) . . . . ?
C53 C52 C57 C60 115.6(2) . . . . ?
C51 C52 C57 C60 -60.3(3) . . . . ?
C53 C52 C57 C59 -3.1(3) . . . . ?
C51 C52 C57 C59 -179.0(2) . . . . ?
C55 C54 C61 C62 -56.0(3) . . . . ?
C53 C54 C61 C62 128.4(3) . . . . ?
C55 C54 C61 C63 178.9(2) . . . . ?
C53 C54 C61 C63 3.2(3) . . . . ?
C55 C54 C61 C64 62.6(3) . . . . ?
C53 C54 C61 C64 -113.0(2) . . . . ?
O5 V1 O6 C65 11.7(3) . . . . ?
O2 V1 O6 C65 -106.0(2) . . . . ?
O1 V1 O6 C65 132.4(2) . . . . ?
V1 O6 C65 C68 -150.9(2) . . . . ?
V1 O6 C65 C67 -30.6(4) . . . . ?
V1 O6 C65 C66 90.6(3) . . . . ?
O7 V2 O8 C69 17.3(3) . . . . ?
O4 V2 O8 C69 -100.1(3) . . . . ?
O3 V2 O8 C69 136.8(3) . . . . ?
V2 O8 C69 C72 -159.7(2) . . . . ?
V2 O8 C69 C70 -39.0(4) . . . . ?
V2 O8 C69 C71 80.5(3) . . . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.069



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1404526'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_CHEMW03_5_3                 
;
RESPONSE: The composition calculated using the SQUEEZE
routine is reported rather than that derived from the 
point model. This explains the discrepancy. 
;

_vrf_PLAT051_5_3                 
;
RESPONSE: The composition calculated using the SQUEEZE
routine is reported rather than that derived from the 
point model. The total number of atoms in these two counts 
is different and hence the value of Mu is also different. 
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C71 H102 O8 V2, 3(C H2 Cl2)'
_chemical_formula_sum            'C74 H108 Cl6 O8 V2'
_chemical_formula_weight         1440.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0032 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2945 0.5062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1435 0.1514 '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                   21.479(15)
_cell_length_b                   14.382(9)
_cell_length_c                   25.952(18)
_cell_angle_alpha                90
_cell_angle_beta                 103.682(7)
_cell_angle_gamma                90
_cell_volume                     7789(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10927
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      26.7

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.460
_shelx_estimated_absorpt_T_min   0.947
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   
; 
 ? 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           synchrotron
_diffrn_source                   'DLS Station I19'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            50396
_diffrn_reflns_av_unetI/netI     0.1227
_diffrn_reflns_av_R_equivalents  0.1961
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.315
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        22.500
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             11066
_reflns_number_gt                6500
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_cell_refinement       
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_reduction        
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1902P)²+15.8389P] 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         11066
_refine_ls_number_parameters     889
_refine_ls_number_restraints     701
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_gt           0.1279
_refine_ls_wR_factor_ref         0.3700
_refine_ls_wR_factor_gt          0.3218
_refine_ls_goodness_of_fit_ref   1.034
_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 0.70848(7) 0.55085(10) 0.92170(5) 0.0583(5) Uani 1 1 d . . . . .
O1 O 0.7506(3) 0.5165(5) 0.9767(3) 0.0814(19) Uani 1 1 d . . . . .
V2 V 0.37170(7) 0.18373(10) 0.64611(6) 0.0600(5) Uani 1 1 d . . . . .
O7 O 0.3031(3) 0.2281(5) 0.6372(3) 0.0815(18) Uani 1 1 d . . . . .
O2 O 0.7593(3) 0.5579(4) 0.87548(19) 0.0570(14) Uani 1 1 d . . . . .
O3 O 0.6429(3) 0.4717(4) 0.9022(2) 0.0594(15) Uani 1 1 d . . . . .
O4 O 0.4148(2) 0.2188(4) 0.7110(2) 0.0595(15) Uani 1 1 d . . . . .
O5 O 0.4081(2) 0.2282(4) 0.5956(2) 0.0552(14) Uani 1 1 d . . . . .
C1 C 0.7935(4) 0.4894(5) 0.8545(3) 0.0473(18) Uani 1 1 d . . . . .
C2 C 0.8609(4) 0.4954(6) 0.8632(3) 0.057(2) Uani 1 1 d . . . . .
C3 C 0.8893(4) 0.4238(6) 0.8396(3) 0.055(2) Uani 1 1 d . . . . .
H3 H 0.9346 0.4238 0.8454 0.066 Uiso 1 1 calc R U . . .
C4 C 0.8557(4) 0.3532(5) 0.8085(3) 0.0485(19) Uani 1 1 d . . . . .
C5 C 0.7895(4) 0.3541(5) 0.7998(3) 0.0464(18) Uani 1 1 d . . . . .
H5 H 0.7653 0.3065 0.7787 0.056 Uiso 1 1 calc R U . . .
C6 C 0.7572(3) 0.4235(5) 0.8212(3) 0.0449(18) Uani 1 1 d . . . . .
C7 C 0.9007(5) 0.5759(7) 0.8946(4) 0.073(3) Uani 1 1 d . . . . .
C8 C 0.8746(6) 0.6712(8) 0.8698(4) 0.093(3) Uani 1 1 d . . . . .
H8A H 0.9036 0.7211 0.8864 0.140 Uiso 1 1 calc R U . . .
H8B H 0.8319 0.6820 0.8758 0.140 Uiso 1 1 calc R U . . .
H8C H 0.8721 0.6702 0.8316 0.140 Uiso 1 1 calc R U . . .
C9 C 0.8958(5) 0.5744(7) 0.9537(4) 0.084(3) Uani 1 1 d . . . . .
H9A H 0.9197 0.6271 0.9726 0.125 Uiso 1 1 calc R U . . .
H9B H 0.9138 0.5162 0.9704 0.125 Uiso 1 1 calc R U . . .
H9C H 0.8507 0.5791 0.9551 0.125 Uiso 1 1 calc R U . . .
C10 C 0.9721(5) 0.5718(9) 0.8933(4) 0.096(4) Uani 1 1 d . . . . .
H10A H 0.9760 0.5751 0.8565 0.143 Uiso 1 1 calc R U . . .
H10B H 0.9908 0.5133 0.9093 0.143 Uiso 1 1 calc R U . . .
H10C H 0.9949 0.6243 0.9134 0.143 Uiso 1 1 calc R U . . .
C11 C 0.8916(4) 0.2777(6) 0.7845(3) 0.062(2) Uani 1 1 d D U . . .
C12 C 0.9379(7) 0.2232(11) 0.8290(6) 0.087(4) Uani 0.674(11) 1 d D U P A 1
H12A H 0.9137 0.1949 0.8526 0.131 Uiso 0.674(11) 1 calc R U P A 1
H12B H 0.9592 0.1743 0.8132 0.131 Uiso 0.674(11) 1 calc R U P A 1
H12C H 0.9701 0.2657 0.8494 0.131 Uiso 0.674(11) 1 calc R U P A 1
C13 C 0.9296(7) 0.3210(9) 0.7483(6) 0.074(4) Uani 0.674(11) 1 d D U P A 1
H13A H 0.9585 0.3685 0.7679 0.111 Uiso 0.674(11) 1 calc R U P A 1
H13B H 0.9547 0.2728 0.7358 0.111 Uiso 0.674(11) 1 calc R U P A 1
H13C H 0.9001 0.3498 0.7179 0.111 Uiso 0.674(11) 1 calc R U P A 1
C14 C 0.8464(7) 0.2034(9) 0.7535(7) 0.085(4) Uani 0.674(11) 1 d D U P A 1
H14A H 0.8217 0.1751 0.7767 0.127 Uiso 0.674(11) 1 calc R U P A 1
H14B H 0.8170 0.2324 0.7230 0.127 Uiso 0.674(11) 1 calc R U P A 1
H14C H 0.8716 0.1554 0.7410 0.127 Uiso 0.674(11) 1 calc R U P A 1
C12X C 0.9630(8) 0.3023(18) 0.7948(11) 0.067(6) Uani 0.326(11) 1 d D U P A 2
H12D H 0.9679 0.3630 0.7791 0.100 Uiso 0.326(11) 1 calc R U P A 2
H12E H 0.9815 0.3047 0.8331 0.100 Uiso 0.326(11) 1 calc R U P A 2
H12F H 0.9853 0.2549 0.7788 0.100 Uiso 0.326(11) 1 calc R U P A 2
C13X C 0.8647(12) 0.2754(19) 0.7240(7) 0.071(6) Uani 0.326(11) 1 d D U P A 2
H13D H 0.8694 0.3370 0.7092 0.106 Uiso 0.326(11) 1 calc R U P A 2
H13E H 0.8884 0.2295 0.7083 0.106 Uiso 0.326(11) 1 calc R U P A 2
H13F H 0.8193 0.2584 0.7161 0.106 Uiso 0.326(11) 1 calc R U P A 2
C14X C 0.8853(13) 0.1844(13) 0.8090(11) 0.067(6) Uani 0.326(11) 1 d D U P A 2
H14D H 0.8399 0.1677 0.8028 0.100 Uiso 0.326(11) 1 calc R U P A 2
H14E H 0.9078 0.1374 0.7929 0.100 Uiso 0.326(11) 1 calc R U P A 2
H14F H 0.9041 0.1872 0.8472 0.100 Uiso 0.326(11) 1 calc R U P A 2
C15 C 0.6838(3) 0.4240(5) 0.8093(3) 0.0408(17) Uani 1 1 d . . . . .
H15 H 0.6717 0.4858 0.8217 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6375(3) 0.3777(5) 0.8886(3) 0.0489(19) Uani 1 1 d . . . . .
C17 C 0.6078(4) 0.3142(6) 0.9166(3) 0.056(2) Uani 1 1 d . . . . .
C18 C 0.6041(4) 0.2227(6) 0.8987(3) 0.056(2) Uani 1 1 d . . . . .
H18 H 0.5861 0.1776 0.9176 0.067 Uiso 1 1 calc R U . . .
C19 C 0.6257(4) 0.1926(6) 0.8538(3) 0.052(2) Uani 1 1 d . . . . .
C20 C 0.6534(4) 0.2591(5) 0.8279(3) 0.0469(18) Uani 1 1 d . . . . .
H20 H 0.6693 0.2405 0.7983 0.056 Uiso 1 1 calc R U . . .
C21 C 0.6588(3) 0.3506(6) 0.8429(3) 0.0453(18) Uani 1 1 d . . . . .
C22 C 0.5786(4) 0.3456(6) 0.9633(3) 0.064(2) Uani 1 1 d . . . . .
C23 C 0.6294(5) 0.3867(8) 1.0092(3) 0.081(3) Uani 1 1 d . . . . .
H23A H 0.6606 0.3385 1.0244 0.121 Uiso 1 1 calc R U . . .
H23B H 0.6088 0.4099 1.0366 0.121 Uiso 1 1 calc R U . . .
H23C H 0.6514 0.4380 0.9961 0.121 Uiso 1 1 calc R U . . .
C24 C 0.5482(5) 0.2616(7) 0.9855(4) 0.087(3) Uani 1 1 d . . . . .
H24A H 0.5810 0.2141 0.9978 0.131 Uiso 1 1 calc R U . . .
H24B H 0.5138 0.2356 0.9574 0.131 Uiso 1 1 calc R U . . .
H24C H 0.5306 0.2821 1.0151 0.131 Uiso 1 1 calc R U . . .
C25 C 0.5246(5) 0.4175(7) 0.9419(4) 0.073(3) Uani 1 1 d . . . . .
H25A H 0.5016 0.4310 0.9694 0.110 Uiso 1 1 calc R U . . .
H25B H 0.4947 0.3918 0.9106 0.110 Uiso 1 1 calc R U . . .
H25C H 0.5435 0.4749 0.9321 0.110 Uiso 1 1 calc R U . . .
C26 C 0.6152(4) 0.0935(6) 0.8325(4) 0.065(2) Uani 1 1 d . U . . .
C27 C 0.5796(6) 0.0311(7) 0.8647(4) 0.091(3) Uani 1 1 d . U . . .
H27A H 0.5721 -0.0302 0.8478 0.136 Uiso 1 1 calc R U . . .
H27B H 0.5385 0.0597 0.8656 0.136 Uiso 1 1 calc R U . . .
H27C H 0.6058 0.0241 0.9009 0.136 Uiso 1 1 calc R U . . .
C28 C 0.5690(5) 0.0979(7) 0.7757(4) 0.084(3) Uani 1 1 d . U . . .
H28A H 0.5889 0.1350 0.7522 0.126 Uiso 1 1 calc R U . . .
H28B H 0.5283 0.1265 0.7780 0.126 Uiso 1 1 calc R U . . .
H28C H 0.5610 0.0348 0.7614 0.126 Uiso 1 1 calc R U . . .
C29 C 0.6786(5) 0.0516(7) 0.8291(5) 0.099(3) Uani 1 1 d . U . . .
H29A H 0.6978 0.0894 0.8055 0.148 Uiso 1 1 calc R U . . .
H29B H 0.6717 -0.0118 0.8151 0.148 Uiso 1 1 calc R U . . .
H29C H 0.7075 0.0500 0.8645 0.148 Uiso 1 1 calc R U . . .
C30 C 0.6508(3) 0.4187(5) 0.7504(3) 0.0482(18) Uani 1 1 d . . . . .
C31 C 0.5868(3) 0.3914(5) 0.7350(3) 0.0429(17) Uani 1 1 d . . . . .
H31 H 0.5658 0.3710 0.7613 0.051 Uiso 1 1 calc R U . . .
C32 C 0.5525(3) 0.3930(5) 0.6819(3) 0.0451(18) Uani 1 1 d . . . . .
C33 C 0.5847(4) 0.4238(6) 0.6441(3) 0.058(2) Uani 1 1 d . . . . .
H33 H 0.5621 0.4274 0.6079 0.069 Uiso 1 1 calc R U . . .
C34 C 0.6492(4) 0.4493(6) 0.6582(3) 0.057(2) Uani 1 1 d . . . . .
H34 H 0.6711 0.4665 0.6319 0.069 Uiso 1 1 calc R U . . .
C35 C 0.6810(4) 0.4491(5) 0.7120(3) 0.054(2) Uani 1 1 d . . . . .
H35 H 0.7240 0.4703 0.7223 0.065 Uiso 1 1 calc R U . . .
C36 C 0.4839(3) 0.3558(6) 0.6682(3) 0.0499(19) Uani 1 1 d . . . . .
H36 H 0.4874 0.2865 0.6673 0.060 Uiso 1 1 calc R U . . .
C37 C 0.4168(4) 0.3072(6) 0.7337(3) 0.054(2) Uani 1 1 d . . . . .
C38 C 0.3892(4) 0.3238(6) 0.7768(4) 0.060(2) Uani 1 1 d . . . . .
C39 C 0.3914(4) 0.4145(7) 0.7945(3) 0.066(2) Uani 1 1 d . . . . .
H39 H 0.3721 0.4277 0.8231 0.080 Uiso 1 1 calc R U . . .
C40 C 0.4204(4) 0.4900(6) 0.7729(3) 0.062(2) Uani 1 1 d . . . . .
C41 C 0.4488(4) 0.4676(6) 0.7322(3) 0.055(2) Uani 1 1 d . . . . .
H41 H 0.4696 0.5156 0.7175 0.066 Uiso 1 1 calc R U . . .
C42 C 0.4487(3) 0.3781(6) 0.7114(3) 0.0503(19) Uani 1 1 d . . . . .
C43 C 0.3595(4) 0.2449(6) 0.8047(3) 0.066(2) Uani 1 1 d . . . . .
C44 C 0.2965(5) 0.2093(8) 0.7668(4) 0.086(3) Uani 1 1 d . . . . .
H44A H 0.2764 0.1628 0.7852 0.130 Uiso 1 1 calc R U . . .
H44B H 0.3065 0.1811 0.7353 0.130 Uiso 1 1 calc R U . . .
H44C H 0.2670 0.2615 0.7560 0.130 Uiso 1 1 calc R U . . .
C45 C 0.4073(5) 0.1669(7) 0.8221(4) 0.079(3) Uani 1 1 d . . . . .
H45A H 0.4448 0.1907 0.8479 0.119 Uiso 1 1 calc R U . . .
H45B H 0.4207 0.1423 0.7912 0.119 Uiso 1 1 calc R U . . .
H45C H 0.3873 0.1172 0.8383 0.119 Uiso 1 1 calc R U . . .
C46 C 0.3403(5) 0.2826(8) 0.8545(4) 0.087(3) Uani 1 1 d . . . . .
H46A H 0.3227 0.2319 0.8720 0.131 Uiso 1 1 calc R U . . .
H46B H 0.3078 0.3313 0.8441 0.131 Uiso 1 1 calc R U . . .
H46C H 0.3781 0.3086 0.8791 0.131 Uiso 1 1 calc R U . . .
C47 C 0.4260(6) 0.5891(7) 0.7953(4) 0.083(3) Uani 1 1 d . U . . .
C48 C 0.3886(8) 0.6018(9) 0.8383(6) 0.133(5) Uani 1 1 d . U . . .
H48A H 0.3425 0.5995 0.8221 0.199 Uiso 1 1 calc R U . . .
H48B H 0.3994 0.6621 0.8557 0.199 Uiso 1 1 calc R U . . .
H48C H 0.3999 0.5520 0.8647 0.199 Uiso 1 1 calc R U . . .
C49 C 0.3990(6) 0.6583(7) 0.7501(5) 0.094(3) Uani 1 1 d . U . . .
H49A H 0.4229 0.6524 0.7224 0.141 Uiso 1 1 calc R U . . .
H49B H 0.4033 0.7219 0.7641 0.141 Uiso 1 1 calc R U . . .
H49C H 0.3536 0.6446 0.7350 0.141 Uiso 1 1 calc R U . . .
C50 C 0.4964(6) 0.6124(7) 0.8180(4) 0.088(3) Uani 1 1 d . U . . .
H50A H 0.5162 0.5636 0.8428 0.132 Uiso 1 1 calc R U . . .
H50B H 0.4997 0.6721 0.8366 0.132 Uiso 1 1 calc R U . . .
H50C H 0.5185 0.6166 0.7891 0.132 Uiso 1 1 calc R U . . .
C51 C 0.4085(3) 0.3188(5) 0.5780(3) 0.0483(19) Uani 1 1 d . . . . .
C52 C 0.3730(4) 0.3450(6) 0.5257(3) 0.053(2) Uani 1 1 d . . . . .
C53 C 0.3734(4) 0.4402(6) 0.5142(3) 0.055(2) Uani 1 1 d . . . . .
H53 H 0.3498 0.4602 0.4803 0.066 Uiso 1 1 calc R U . . .
C54 C 0.4057(4) 0.5073(6) 0.5488(3) 0.055(2) Uani 1 1 d . . . . .
C55 C 0.4411(4) 0.4773(6) 0.5982(3) 0.053(2) Uani 1 1 d . . . . .
H55 H 0.4643 0.5218 0.6224 0.064 Uiso 1 1 calc R U . . .
C56 C 0.4433(3) 0.3855(6) 0.6129(3) 0.0479(19) Uani 1 1 d . . . . .
C57 C 0.3387(4) 0.2754(6) 0.4848(3) 0.068(2) Uani 1 1 d . . . . .
C58 C 0.2798(5) 0.2347(8) 0.5012(4) 0.094(3) Uani 1 1 d . . . . .
H58A H 0.2938 0.2003 0.5346 0.141 Uiso 1 1 calc R U . . .
H58B H 0.2569 0.1926 0.4735 0.141 Uiso 1 1 calc R U . . .
H58C H 0.2511 0.2854 0.5061 0.141 Uiso 1 1 calc R U . . .
C59 C 0.3127(6) 0.3181(8) 0.4306(4) 0.096(4) Uani 1 1 d . . . . .
H59A H 0.2811 0.3660 0.4330 0.144 Uiso 1 1 calc R U . . .
H59B H 0.2922 0.2696 0.4057 0.144 Uiso 1 1 calc R U . . .
H59C H 0.3479 0.3461 0.4179 0.144 Uiso 1 1 calc R U . . .
C60 C 0.3830(6) 0.1949(7) 0.4770(4) 0.093(3) Uani 1 1 d . . . . .
H60A H 0.4192 0.2197 0.4643 0.140 Uiso 1 1 calc R U . . .
H60B H 0.3589 0.1511 0.4508 0.140 Uiso 1 1 calc R U . . .
H60C H 0.3990 0.1627 0.5108 0.140 Uiso 1 1 calc R U . . .
C61 C 0.4058(4) 0.6110(6) 0.5329(3) 0.065(2) Uani 1 1 d . U . . .
C62 C 0.3557(5) 0.6326(7) 0.4824(4) 0.074(2) Uani 1 1 d . U . . .
H62A H 0.3135 0.6123 0.4864 0.111 Uiso 1 1 calc R U . . .
H62B H 0.3663 0.5997 0.4526 0.111 Uiso 1 1 calc R U . . .
H62C H 0.3548 0.6997 0.4758 0.111 Uiso 1 1 calc R U . . .
C63 C 0.4731(5) 0.6362(8) 0.5239(4) 0.086(3) Uani 1 1 d . U . . .
H63A H 0.4727 0.7005 0.5114 0.129 Uiso 1 1 calc R U . . .
H63B H 0.4834 0.5943 0.4974 0.129 Uiso 1 1 calc R U . . .
H63C H 0.5054 0.6296 0.5574 0.129 Uiso 1 1 calc R U . . .
C64 C 0.3916(6) 0.6711(7) 0.5776(4) 0.089(3) Uani 1 1 d . U . . .
H64A H 0.3927 0.7370 0.5682 0.134 Uiso 1 1 calc R U . . .
H64B H 0.4239 0.6592 0.6106 0.134 Uiso 1 1 calc R U . . .
H64C H 0.3490 0.6556 0.5828 0.134 Uiso 1 1 calc R U . . .
O6 O 0.6760(3) 0.6598(4) 0.9274(2) 0.0763(17) Uani 1 1 d D U . . .
C65 C 0.6660(6) 0.7249(8) 0.9676(4) 0.068(3) Uani 0.745(14) 1 d D U P B 1
C66 C 0.6627(9) 0.8199(9) 0.9404(6) 0.103(5) Uani 0.745(14) 1 d D U P B 1
H66A H 0.6560 0.8684 0.9651 0.155 Uiso 0.745(14) 1 calc R U P B 1
H66B H 0.7029 0.8317 0.9300 0.155 Uiso 0.745(14) 1 calc R U P B 1
H66C H 0.6270 0.8204 0.9089 0.155 Uiso 0.745(14) 1 calc R U P B 1
C67 C 0.6059(7) 0.6974(12) 0.9826(6) 0.106(5) Uani 0.745(14) 1 d D U P B 1
H67A H 0.5978 0.7400 1.0097 0.160 Uiso 0.745(14) 1 calc R U P B 1
H67B H 0.5700 0.7001 0.9512 0.160 Uiso 0.745(14) 1 calc R U P B 1
H67C H 0.6102 0.6338 0.9966 0.160 Uiso 0.745(14) 1 calc R U P B 1
C68 C 0.7221(7) 0.7231(11) 1.0153(5) 0.077(4) Uani 0.745(14) 1 d D U P B 1
H68A H 0.7145 0.7673 1.0419 0.115 Uiso 0.745(14) 1 calc R U P B 1
H68B H 0.7269 0.6603 1.0305 0.115 Uiso 0.745(14) 1 calc R U P B 1
H68C H 0.7613 0.7404 1.0045 0.115 Uiso 0.745(14) 1 calc R U P B 1
C65X C 0.6637(14) 0.7503(15) 0.9482(11) 0.088(6) Uani 0.255(14) 1 d D U P B 2
C66X C 0.7012(19) 0.8201(19) 0.9229(16) 0.086(8) Uani 0.255(14) 1 d D U P B 2
H66D H 0.6949 0.8829 0.9354 0.129 Uiso 0.255(14) 1 calc R U P B 2
H66E H 0.7469 0.8045 0.9327 0.129 Uiso 0.255(14) 1 calc R U P B 2
H66F H 0.6858 0.8177 0.8842 0.129 Uiso 0.255(14) 1 calc R U P B 2
C67X C 0.5939(15) 0.771(3) 0.9342(17) 0.098(8) Uani 0.255(14) 1 d D U P B 2
H67D H 0.5865 0.8324 0.9485 0.147 Uiso 0.255(14) 1 calc R U P B 2
H67E H 0.5782 0.7721 0.8955 0.147 Uiso 0.255(14) 1 calc R U P B 2
H67F H 0.5708 0.7237 0.9493 0.147 Uiso 0.255(14) 1 calc R U P B 2
C68X C 0.693(2) 0.749(3) 1.0073(11) 0.101(8) Uani 0.255(14) 1 d D U P B 2
H68D H 0.6858 0.8093 1.0227 0.151 Uiso 0.255(14) 1 calc R U P B 2
H68E H 0.6735 0.6997 1.0240 0.151 Uiso 0.255(14) 1 calc R U P B 2
H68F H 0.7394 0.7381 1.0136 0.151 Uiso 0.255(14) 1 calc R U P B 2
O8 O 0.3714(3) 0.0632(4) 0.6442(2) 0.0707(16) Uani 1 1 d D U . . .
C69 C 0.3291(6) -0.0172(8) 0.6436(4) 0.076(3) Uani 0.797(15) 1 d D U P C 1
C70 C 0.3566(7) -0.0930(9) 0.6134(7) 0.098(4) Uani 0.797(15) 1 d D U P C 1
H70A H 0.3306 -0.1495 0.6113 0.146 Uiso 0.797(15) 1 calc R U P C 1
H70B H 0.3558 -0.0711 0.5775 0.146 Uiso 0.797(15) 1 calc R U P C 1
H70C H 0.4008 -0.1067 0.6321 0.146 Uiso 0.797(15) 1 calc R U P C 1
C71 C 0.2619(6) 0.0087(11) 0.6114(6) 0.080(4) Uani 0.797(15) 1 d D U P C 1
H71A H 0.2330 -0.0443 0.6105 0.119 Uiso 0.797(15) 1 calc R U P C 1
H71B H 0.2459 0.0621 0.6280 0.119 Uiso 0.797(15) 1 calc R U P C 1
H71C H 0.2638 0.0249 0.5751 0.119 Uiso 0.797(15) 1 calc R U P C 1
C72 C 0.3324(8) -0.0427(10) 0.7012(5) 0.108(5) Uani 0.797(15) 1 d D U P C 1
H72A H 0.3046 -0.0964 0.7024 0.162 Uiso 0.797(15) 1 calc R U P C 1
H72B H 0.3766 -0.0584 0.7191 0.162 Uiso 0.797(15) 1 calc R U P C 1
H72C H 0.3180 0.0102 0.7192 0.162 Uiso 0.797(15) 1 calc R U P C 1
C69X C 0.3382(15) -0.0249(17) 0.6282(12) 0.084(6) Uani 0.203(15) 1 d D U P C 2
C70X C 0.351(3) -0.050(3) 0.5740(16) 0.097(9) Uani 0.203(15) 1 d D U P C 2
H70D H 0.3293 -0.1091 0.5617 0.145 Uiso 0.203(15) 1 calc R U P C 2
H70E H 0.3339 -0.0010 0.5484 0.145 Uiso 0.203(15) 1 calc R U P C 2
H70F H 0.3969 -0.0568 0.5774 0.145 Uiso 0.203(15) 1 calc R U P C 2
C71X C 0.2665(15) -0.013(4) 0.625(2) 0.089(9) Uani 0.203(15) 1 d D U P C 2
H71D H 0.2445 -0.0723 0.6138 0.133 Uiso 0.203(15) 1 calc R U P C 2
H71E H 0.2600 0.0053 0.6592 0.133 Uiso 0.203(15) 1 calc R U P C 2
H71F H 0.2491 0.0347 0.5982 0.133 Uiso 0.203(15) 1 calc R U P C 2
C72X C 0.368(2) -0.095(2) 0.6714(18) 0.093(9) Uani 0.203(15) 1 d D U P C 2
H72D H 0.3478 -0.1562 0.6627 0.140 Uiso 0.203(15) 1 calc R U P C 2
H72E H 0.4142 -0.1008 0.6734 0.140 Uiso 0.203(15) 1 calc R U P C 2
H72F H 0.3618 -0.0743 0.7057 0.140 Uiso 0.203(15) 1 calc R U P C 2
C73 C 0.2706(12) 0.4341(15) 0.6101(12) 0.239(9) Uani 1 1 d . U . . .
H73A H 0.2630 0.3662 0.6071 0.287 Uiso 1 1 calc R U . . .
H73B H 0.3151 0.4472 0.6078 0.287 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2124(5) 0.4976(9) 0.5581(6) 0.383(7) Uani 1 1 d . U . . .
Cl2 Cl 0.2567(7) 0.4757(11) 0.6674(6) 0.442(9) Uani 1 1 d . 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 1.577(6) . ?
V1 O6 1.736(6) . ?
V1 O3 1.790(6) . ?
V1 O2 1.806(5) . ?
V2 O7 1.572(7) . ?
V2 O8 1.735(6) . ?
V2 O4 1.792(6) . ?
V2 O5 1.796(5) . ?
O2 C1 1.413(9) . ?
O3 C16 1.394(9) . ?
O4 C37 1.397(9) . ?
O5 C51 1.382(9) . ?
C1 C6 1.390(10) . ?
C1 C2 1.413(11) . ?
C2 C3 1.409(12) . ?
C2 C7 1.551(12) . ?
C3 C4 1.388(11) . ?
C4 C5 1.387(10) . ?
C4 C11 1.545(11) . ?
C5 C6 1.403(10) . ?
C6 C15 1.533(10) . ?
C7 C10 1.542(14) . ?
C7 C8 1.560(15) . ?
C7 C9 1.563(13) . ?
C11 C14X 1.505(15) . ?
C11 C13 1.516(14) . ?
C11 C12X 1.536(15) . ?
C11 C14 1.538(13) . ?
C11 C13X 1.540(19) . ?
C11 C12 1.547(13) . ?
C15 C30 1.526(10) . ?
C15 C21 1.546(10) . ?
C16 C17 1.409(11) . ?
C16 C21 1.423(10) . ?
C17 C18 1.393(11) . ?
C17 C22 1.558(11) . ?
C18 C19 1.417(11) . ?
C19 C20 1.381(11) . ?
C19 C26 1.527(12) . ?
C20 C21 1.371(10) . ?
C22 C23 1.531(12) . ?
C22 C24 1.547(12) . ?
C22 C25 1.555(13) . ?
C26 C29 1.512(13) . ?
C26 C27 1.545(13) . ?
C26 C28 1.573(13) . ?
C30 C35 1.381(11) . ?
C30 C31 1.396(10) . ?
C31 C32 1.399(10) . ?
C32 C33 1.401(11) . ?
C32 C36 1.529(10) . ?
C33 C34 1.396(11) . ?
C34 C35 1.403(11) . ?
C36 C42 1.527(10) . ?
C36 C56 1.554(10) . ?
C37 C38 1.404(12) . ?
C37 C42 1.425(11) . ?
C38 C39 1.380(12) . ?
C38 C43 1.561(12) . ?
C39 C40 1.430(12) . ?
C40 C41 1.378(11) . ?
C40 C47 1.533(13) . ?
C41 C42 1.395(11) . ?
C43 C45 1.515(13) . ?
C43 C46 1.546(13) . ?
C43 C44 1.560(13) . ?
C47 C50 1.525(15) . ?
C47 C48 1.533(14) . ?
C47 C49 1.544(15) . ?
C51 C56 1.406(10) . ?
C51 C52 1.439(11) . ?
C52 C53 1.402(11) . ?
C52 C57 1.516(11) . ?
C53 C54 1.387(11) . ?
C54 C55 1.395(11) . ?
C54 C61 1.547(12) . ?
C55 C56 1.373(11) . ?
C57 C59 1.516(13) . ?
C57 C60 1.542(14) . ?
C57 C58 1.544(14) . ?
C61 C62 1.519(12) . ?
C61 C64 1.535(13) . ?
C61 C63 1.559(14) . ?
O6 C65 1.454(12) . ?
O6 C65X 1.46(2) . ?
C65 C67 1.489(18) . ?
C65 C68 1.510(13) . ?
C65 C66 1.532(15) . ?
C65X C67X 1.49(2) . ?
C65X C68X 1.515(18) . ?
C65X C66X 1.530(18) . ?
O8 C69X 1.46(2) . ?
O8 C69 1.468(12) . ?
C69 C72 1.526(13) . ?
C69 C71 1.533(16) . ?
C69 C70 1.539(14) . ?
C69X C71X 1.53(2) . ?
C69X C72X 1.536(18) . ?
C69X C70X 1.536(19) . ?
C73 Cl2 1.69(3) . ?
C73 Cl1 1.85(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O6 111.2(3) . . ?
O1 V1 O3 107.6(3) . . ?
O6 V1 O3 107.0(3) . . ?
O1 V1 O2 108.1(3) . . ?
O6 V1 O2 108.9(3) . . ?
O3 V1 O2 114.0(2) . . ?
O7 V2 O8 113.9(3) . . ?
O7 V2 O4 106.3(3) . . ?
O8 V2 O4 107.8(3) . . ?
O7 V2 O5 107.7(3) . . ?
O8 V2 O5 109.5(3) . . ?
O4 V2 O5 111.7(2) . . ?
C1 O2 V1 131.9(5) . . ?
C16 O3 V1 134.5(5) . . ?
C37 O4 V2 127.5(5) . . ?
C51 O5 V2 127.9(5) . . ?
C6 C1 O2 116.7(6) . . ?
C6 C1 C2 122.9(7) . . ?
O2 C1 C2 120.1(7) . . ?
C3 C2 C1 114.7(7) . . ?
C3 C2 C7 122.1(8) . . ?
C1 C2 C7 123.1(8) . . ?
C4 C3 C2 124.7(7) . . ?
C5 C4 C3 117.4(7) . . ?
C5 C4 C11 122.1(7) . . ?
C3 C4 C11 120.5(7) . . ?
C4 C5 C6 121.7(7) . . ?
C1 C6 C5 118.3(7) . . ?
C1 C6 C15 121.4(6) . . ?
C5 C6 C15 120.2(6) . . ?
C10 C7 C2 112.9(8) . . ?
C10 C7 C8 106.7(9) . . ?
C2 C7 C8 109.9(8) . . ?
C10 C7 C9 108.6(8) . . ?
C2 C7 C9 110.3(7) . . ?
C8 C7 C9 108.4(8) . . ?
C14X C11 C12X 108.5(14) . . ?
C13 C11 C14 109.1(9) . . ?
C14X C11 C13X 111.2(14) . . ?
C12X C11 C13X 107.4(13) . . ?
C14X C11 C4 110.8(11) . . ?
C13 C11 C4 110.7(8) . . ?
C12X C11 C4 110.0(12) . . ?
C14 C11 C4 112.7(8) . . ?
C13X C11 C4 108.9(11) . . ?
C13 C11 C12 109.0(9) . . ?
C14 C11 C12 104.7(10) . . ?
C4 C11 C12 110.5(8) . . ?
C30 C15 C6 114.5(6) . . ?
C30 C15 C21 113.0(6) . . ?
C6 C15 C21 111.2(5) . . ?
O3 C16 C17 121.3(7) . . ?
O3 C16 C21 116.8(7) . . ?
C17 C16 C21 121.7(7) . . ?
C18 C17 C16 115.9(7) . . ?
C18 C17 C22 122.2(7) . . ?
C16 C17 C22 121.8(7) . . ?
C17 C18 C19 124.0(8) . . ?
C20 C19 C18 116.8(7) . . ?
C20 C19 C26 120.9(7) . . ?
C18 C19 C26 122.2(7) . . ?
C21 C20 C19 122.9(7) . . ?
C20 C21 C16 118.5(7) . . ?
C20 C21 C15 120.9(6) . . ?
C16 C21 C15 120.5(7) . . ?
C23 C22 C24 107.3(8) . . ?
C23 C22 C25 110.9(8) . . ?
C24 C22 C25 107.9(8) . . ?
C23 C22 C17 111.9(7) . . ?
C24 C22 C17 110.2(7) . . ?
C25 C22 C17 108.6(7) . . ?
C29 C26 C19 109.6(7) . . ?
C29 C26 C27 111.6(9) . . ?
C19 C26 C27 113.4(7) . . ?
C29 C26 C28 109.8(9) . . ?
C19 C26 C28 108.0(7) . . ?
C27 C26 C28 104.3(8) . . ?
C35 C30 C31 118.7(7) . . ?
C35 C30 C15 121.3(7) . . ?
C31 C30 C15 119.6(7) . . ?
C30 C31 C32 122.1(7) . . ?
C31 C32 C33 117.6(7) . . ?
C31 C32 C36 118.5(6) . . ?
C33 C32 C36 123.8(7) . . ?
C34 C33 C32 121.5(7) . . ?
C33 C34 C35 118.7(7) . . ?
C30 C35 C34 121.2(7) . . ?
C42 C36 C32 111.9(6) . . ?
C42 C36 C56 110.8(6) . . ?
C32 C36 C56 114.7(6) . . ?
O4 C37 C38 120.9(8) . . ?
O4 C37 C42 116.8(7) . . ?
C38 C37 C42 122.3(8) . . ?
C39 C38 C37 116.0(8) . . ?
C39 C38 C43 121.2(8) . . ?
C37 C38 C43 122.8(8) . . ?
C38 C39 C40 124.8(8) . . ?
C41 C40 C39 115.8(8) . . ?
C41 C40 C47 119.9(8) . . ?
C39 C40 C47 124.1(8) . . ?
C40 C41 C42 123.5(8) . . ?
C41 C42 C37 117.5(7) . . ?
C41 C42 C36 121.4(7) . . ?
C37 C42 C36 121.0(7) . . ?
C45 C43 C46 107.9(8) . . ?
C45 C43 C44 111.7(8) . . ?
C46 C43 C44 106.2(8) . . ?
C45 C43 C38 110.7(7) . . ?
C46 C43 C38 110.7(8) . . ?
C44 C43 C38 109.6(7) . . ?
C50 C47 C48 109.6(10) . . ?
C50 C47 C40 109.4(9) . . ?
C48 C47 C40 112.3(8) . . ?
C50 C47 C49 108.1(8) . . ?
C48 C47 C49 108.1(10) . . ?
C40 C47 C49 109.2(8) . . ?
O5 C51 C56 118.3(7) . . ?
O5 C51 C52 121.0(6) . . ?
C56 C51 C52 120.7(7) . . ?
C53 C52 C51 115.3(7) . . ?
C53 C52 C57 121.4(7) . . ?
C51 C52 C57 123.3(7) . . ?
C54 C53 C52 124.7(7) . . ?
C53 C54 C55 117.4(7) . . ?
C53 C54 C61 122.0(7) . . ?
C55 C54 C61 120.5(7) . . ?
C56 C55 C54 121.9(7) . . ?
C55 C56 C51 119.9(7) . . ?
C55 C56 C36 119.7(7) . . ?
C51 C56 C36 120.3(7) . . ?
C59 C57 C52 113.3(8) . . ?
C59 C57 C60 106.5(8) . . ?
C52 C57 C60 112.0(8) . . ?
C59 C57 C58 105.3(8) . . ?
C52 C57 C58 110.6(8) . . ?
C60 C57 C58 108.8(9) . . ?
C62 C61 C64 108.0(8) . . ?
C62 C61 C54 112.4(7) . . ?
C64 C61 C54 109.2(7) . . ?
C62 C61 C63 108.5(7) . . ?
C64 C61 C63 109.9(8) . . ?
C54 C61 C63 108.9(7) . . ?
C65 O6 V1 140.5(6) . . ?
C65X O6 V1 161.7(12) . . ?
O6 C65 C67 107.5(10) . . ?
O6 C65 C68 110.7(9) . . ?
C67 C65 C68 110.8(11) . . ?
O6 C65 C66 104.1(9) . . ?
C67 C65 C66 114.1(12) . . ?
C68 C65 C66 109.5(11) . . ?
O6 C65X C67X 111(2) . . ?
O6 C65X C68X 107.4(19) . . ?
C67X C65X C68X 114(2) . . ?
O6 C65X C66X 105.4(17) . . ?
C67X C65X C66X 111(2) . . ?
C68X C65X C66X 108(2) . . ?
C69X O8 V2 150.6(14) . . ?
C69 O8 V2 141.8(7) . . ?
O8 C69 C72 107.0(9) . . ?
O8 C69 C71 108.3(9) . . ?
C72 C69 C71 114.3(11) . . ?
O8 C69 C70 104.7(9) . . ?
C72 C69 C70 113.2(12) . . ?
C71 C69 C70 108.7(10) . . ?
O8 C69X C71X 110(2) . . ?
O8 C69X C72X 105.8(19) . . ?
C71X C69X C72X 111(2) . . ?
O8 C69X C70X 106.6(19) . . ?
C71X C69X C70X 111(2) . . ?
C72X C69X C70X 112(3) . . ?
Cl2 C73 Cl1 103.7(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 O2 C1 63.4(7) . . . . ?
O6 V1 O2 C1 -175.6(6) . . . . ?
O3 V1 O2 C1 -56.1(7) . . . . ?
O1 V1 O3 C16 -64.6(7) . . . . ?
O6 V1 O3 C16 175.8(6) . . . . ?
O2 V1 O3 C16 55.3(7) . . . . ?
O7 V2 O4 C37 -44.2(7) . . . . ?
O8 V2 O4 C37 -166.7(6) . . . . ?
O5 V2 O4 C37 72.9(6) . . . . ?
O7 V2 O5 C51 44.1(6) . . . . ?
O8 V2 O5 C51 168.4(5) . . . . ?
O4 V2 O5 C51 -72.2(6) . . . . ?
V1 O2 C1 C6 66.6(9) . . . . ?
V1 O2 C1 C2 -119.7(7) . . . . ?
C6 C1 C2 C3 -5.8(11) . . . . ?
O2 C1 C2 C3 -179.0(7) . . . . ?
C6 C1 C2 C7 172.1(7) . . . . ?
O2 C1 C2 C7 -1.2(11) . . . . ?
C1 C2 C3 C4 2.0(11) . . . . ?
C7 C2 C3 C4 -175.9(7) . . . . ?
C2 C3 C4 C5 0.6(11) . . . . ?
C2 C3 C4 C11 -179.8(7) . . . . ?
C3 C4 C5 C6 0.3(10) . . . . ?
C11 C4 C5 C6 -179.3(7) . . . . ?
O2 C1 C6 C5 -179.7(6) . . . . ?
C2 C1 C6 C5 6.8(11) . . . . ?
O2 C1 C6 C15 -1.6(10) . . . . ?
C2 C1 C6 C15 -175.1(7) . . . . ?
C4 C5 C6 C1 -3.8(11) . . . . ?
C4 C5 C6 C15 178.0(6) . . . . ?
C3 C2 C7 C10 3.9(12) . . . . ?
C1 C2 C7 C10 -173.8(8) . . . . ?
C3 C2 C7 C8 122.9(9) . . . . ?
C1 C2 C7 C8 -54.9(10) . . . . ?
C3 C2 C7 C9 -117.8(9) . . . . ?
C1 C2 C7 C9 64.5(11) . . . . ?
C5 C4 C11 C14X -67.6(14) . . . . ?
C3 C4 C11 C14X 112.8(14) . . . . ?
C5 C4 C11 C13 119.4(9) . . . . ?
C3 C4 C11 C13 -60.2(11) . . . . ?
C5 C4 C11 C12X 172.5(12) . . . . ?
C3 C4 C11 C12X -7.1(14) . . . . ?
C5 C4 C11 C14 -3.0(12) . . . . ?
C3 C4 C11 C14 177.4(9) . . . . ?
C5 C4 C11 C13X 55.0(14) . . . . ?
C3 C4 C11 C13X -124.6(13) . . . . ?
C5 C4 C11 C12 -119.8(9) . . . . ?
C3 C4 C11 C12 60.6(11) . . . . ?
C1 C6 C15 C30 130.1(7) . . . . ?
C5 C6 C15 C30 -51.9(9) . . . . ?
C1 C6 C15 C21 -100.5(8) . . . . ?
C5 C6 C15 C21 77.6(8) . . . . ?
V1 O3 C16 C17 122.1(7) . . . . ?
V1 O3 C16 C21 -62.6(9) . . . . ?
O3 C16 C17 C18 178.7(6) . . . . ?
C21 C16 C17 C18 3.6(11) . . . . ?
O3 C16 C17 C22 1.0(11) . . . . ?
C21 C16 C17 C22 -174.1(7) . . . . ?
C16 C17 C18 C19 -2.7(11) . . . . ?
C22 C17 C18 C19 175.0(7) . . . . ?
C17 C18 C19 C20 1.7(11) . . . . ?
C17 C18 C19 C26 -174.2(8) . . . . ?
C18 C19 C20 C21 -1.7(11) . . . . ?
C26 C19 C20 C21 174.3(7) . . . . ?
C19 C20 C21 C16 2.7(11) . . . . ?
C19 C20 C21 C15 -173.7(7) . . . . ?
O3 C16 C21 C20 -179.0(6) . . . . ?
C17 C16 C21 C20 -3.7(11) . . . . ?
O3 C16 C21 C15 -2.5(9) . . . . ?
C17 C16 C21 C15 172.7(7) . . . . ?
C30 C15 C21 C20 48.7(9) . . . . ?
C6 C15 C21 C20 -81.6(8) . . . . ?
C30 C15 C21 C16 -127.7(7) . . . . ?
C6 C15 C21 C16 102.1(7) . . . . ?
C18 C17 C22 C23 120.6(9) . . . . ?
C16 C17 C22 C23 -61.8(11) . . . . ?
C18 C17 C22 C24 1.2(11) . . . . ?
C16 C17 C22 C24 178.8(8) . . . . ?
C18 C17 C22 C25 -116.7(9) . . . . ?
C16 C17 C22 C25 60.8(10) . . . . ?
C20 C19 C26 C29 58.5(11) . . . . ?
C18 C19 C26 C29 -125.7(9) . . . . ?
C20 C19 C26 C27 -176.1(8) . . . . ?
C18 C19 C26 C27 -0.3(12) . . . . ?
C20 C19 C26 C28 -61.0(10) . . . . ?
C18 C19 C26 C28 114.8(9) . . . . ?
C6 C15 C30 C35 -25.4(10) . . . . ?
C21 C15 C30 C35 -153.9(7) . . . . ?
C6 C15 C30 C31 161.2(6) . . . . ?
C21 C15 C30 C31 32.7(9) . . . . ?
C35 C30 C31 C32 0.7(11) . . . . ?
C15 C30 C31 C32 174.3(6) . . . . ?
C30 C31 C32 C33 -0.3(11) . . . . ?
C30 C31 C32 C36 176.0(7) . . . . ?
C31 C32 C33 C34 1.9(12) . . . . ?
C36 C32 C33 C34 -174.2(8) . . . . ?
C32 C33 C34 C35 -3.8(13) . . . . ?
C31 C30 C35 C34 -2.7(12) . . . . ?
C15 C30 C35 C34 -176.1(7) . . . . ?
C33 C34 C35 C30 4.2(12) . . . . ?
C31 C32 C36 C42 36.0(9) . . . . ?
C33 C32 C36 C42 -147.9(7) . . . . ?
C31 C32 C36 C56 163.3(6) . . . . ?
C33 C32 C36 C56 -20.7(11) . . . . ?
V2 O4 C37 C38 112.7(7) . . . . ?
V2 O4 C37 C42 -68.2(8) . . . . ?
O4 C37 C38 C39 -177.1(7) . . . . ?
C42 C37 C38 C39 3.9(11) . . . . ?
O4 C37 C38 C43 4.6(12) . . . . ?
C42 C37 C38 C43 -174.4(7) . . . . ?
C37 C38 C39 C40 -1.5(13) . . . . ?
C43 C38 C39 C40 176.8(8) . . . . ?
C38 C39 C40 C41 -1.2(13) . . . . ?
C38 C39 C40 C47 -176.0(9) . . . . ?
C39 C40 C41 C42 1.7(12) . . . . ?
C47 C40 C41 C42 176.7(8) . . . . ?
C40 C41 C42 C37 0.6(11) . . . . ?
C40 C41 C42 C36 -176.7(7) . . . . ?
O4 C37 C42 C41 177.5(6) . . . . ?
C38 C37 C42 C41 -3.5(11) . . . . ?
O4 C37 C42 C36 -5.2(10) . . . . ?
C38 C37 C42 C36 173.8(7) . . . . ?
C32 C36 C42 C41 48.8(9) . . . . ?
C56 C36 C42 C41 -80.5(9) . . . . ?
C32 C36 C42 C37 -128.4(7) . . . . ?
C56 C36 C42 C37 102.3(8) . . . . ?
C39 C38 C43 C45 -124.3(9) . . . . ?
C37 C38 C43 C45 53.9(11) . . . . ?
C39 C38 C43 C46 -4.7(11) . . . . ?
C37 C38 C43 C46 173.5(8) . . . . ?
C39 C38 C43 C44 112.0(9) . . . . ?
C37 C38 C43 C44 -69.8(10) . . . . ?
C41 C40 C47 C50 -60.9(11) . . . . ?
C39 C40 C47 C50 113.7(10) . . . . ?
C41 C40 C47 C48 177.2(10) . . . . ?
C39 C40 C47 C48 -8.3(15) . . . . ?
C41 C40 C47 C49 57.3(12) . . . . ?
C39 C40 C47 C49 -128.1(9) . . . . ?
V2 O5 C51 C56 67.8(8) . . . . ?
V2 O5 C51 C52 -110.8(7) . . . . ?
O5 C51 C52 C53 175.3(7) . . . . ?
C56 C51 C52 C53 -3.3(11) . . . . ?
O5 C51 C52 C57 -6.1(12) . . . . ?
C56 C51 C52 C57 175.2(8) . . . . ?
C51 C52 C53 C54 1.2(12) . . . . ?
C57 C52 C53 C54 -177.4(8) . . . . ?
C52 C53 C54 C55 1.0(12) . . . . ?
C52 C53 C54 C61 178.1(8) . . . . ?
C53 C54 C55 C56 -1.1(12) . . . . ?
C61 C54 C55 C56 -178.3(7) . . . . ?
C54 C55 C56 C51 -1.0(11) . . . . ?
C54 C55 C56 C36 179.5(7) . . . . ?
O5 C51 C56 C55 -175.4(7) . . . . ?
C52 C51 C56 C55 3.3(11) . . . . ?
O5 C51 C56 C36 4.1(10) . . . . ?
C52 C51 C56 C36 -177.2(7) . . . . ?
C42 C36 C56 C55 78.2(9) . . . . ?
C32 C36 C56 C55 -49.6(9) . . . . ?
C42 C36 C56 C51 -101.2(8) . . . . ?
C32 C36 C56 C51 131.0(7) . . . . ?
C53 C52 C57 C59 6.4(12) . . . . ?
C51 C52 C57 C59 -172.1(9) . . . . ?
C53 C52 C57 C60 126.9(9) . . . . ?
C51 C52 C57 C60 -51.5(11) . . . . ?
C53 C52 C57 C58 -111.5(9) . . . . ?
C51 C52 C57 C58 70.1(11) . . . . ?
C53 C54 C61 C62 13.3(12) . . . . ?
C55 C54 C61 C62 -169.7(8) . . . . ?
C53 C54 C61 C64 133.2(9) . . . . ?
C55 C54 C61 C64 -49.8(11) . . . . ?
C53 C54 C61 C63 -106.9(9) . . . . ?
C55 C54 C61 C63 70.2(10) . . . . ?
O1 V1 O6 C65 -13.2(11) . . . . ?
O3 V1 O6 C65 104.0(10) . . . . ?
O2 V1 O6 C65 -132.3(10) . . . . ?
O1 V1 O6 C65X 13(4) . . . . ?
O3 V1 O6 C65X 131(4) . . . . ?
O2 V1 O6 C65X -106(4) . . . . ?
V1 O6 C65 C67 -84.5(12) . . . . ?
V1 O6 C65 C68 36.6(16) . . . . ?
V1 O6 C65 C66 154.2(10) . . . . ?
V1 O6 C65X C67X -142(3) . . . . ?
V1 O6 C65X C68X -17(5) . . . . ?
V1 O6 C65X C66X 98(4) . . . . ?
O7 V2 O8 C69X 21(3) . . . . ?
O4 V2 O8 C69X 139(3) . . . . ?
O5 V2 O8 C69X -99(3) . . . . ?
O7 V2 O8 C69 -10.6(10) . . . . ?
O4 V2 O8 C69 107.1(9) . . . . ?
O5 V2 O8 C69 -131.2(9) . . . . ?
V2 O8 C69 C72 -88.4(13) . . . . ?
V2 O8 C69 C71 35.4(14) . . . . ?
V2 O8 C69 C70 151.2(9) . . . . ?
V2 O8 C69X C71X -29(4) . . . . ?
V2 O8 C69X C72X -149(3) . . . . ?
V2 O8 C69X C70X 92(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
C73 H73A O7 0.99 2.23 3.09(2) 143.8 .

_refine_diff_density_max         0.783
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.092



####################################################################### 
# 
# 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 1404527'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_PLAT201_6                   
;
RESPONSE: There is small scale disorder present. This is modelled
using partially occupied atoms with isotropic displacement parameters. 
;

_vrf_RFACR01_6                   
;
RESPONSE: Data were collected at the UK crystallography service
in Southampton using a rotating anode instrument. The crystal was 
weakly scattering. All observed data to 25.15 degrees theta were used 
in refinements. Due to the weak scattering, there are modest values
for wR2 and Rint, while 42% of the data are observed. 

This explains a numer of the C-alerts. 

The refinement is stable and gives valuble chemical 
information. 
;



_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C79 H111 N O7 V2, C H2 Cl2
;
_chemical_formula_sum            'C80 H113 Cl2 N O7 V2'
_chemical_formula_weight         1373.49

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.4460(6)
_cell_length_b                   11.1800(7)
_cell_length_c                   19.3754(13)
_cell_angle_alpha                77.635(4)
_cell_angle_beta                 81.522(4)
_cell_angle_gamma                85.307(5)
_cell_volume                     1974.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6954
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      25.0

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.354
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Implemented within Rigaku CrystalClear software. 
CrystalClear 2.1 b31
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku Kappa CCD with Saturn724+ detector.
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            21387
_diffrn_reflns_av_unetI/netI     0.1748
_diffrn_reflns_av_R_equivalents  0.1230
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.558
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6954
_reflns_number_gt                2929
_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 2.1 b31 (Rigaku, 2014)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_structure_solution    SHELXS-86
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1193P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6954
_refine_ls_number_parameters     480
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.2135
_refine_ls_R_factor_gt           0.0895
_refine_ls_wR_factor_ref         0.2553
_refine_ls_wR_factor_gt          0.1929
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.967
_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
C30 C 0.7432(7) 0.5431(5) 0.7542(3) 0.0426(15) Uani 1 1 d . . . . .
C31 C 0.8658(7) 0.4834(5) 0.7234(3) 0.0441(15) Uani 1 1 d . . . . .
C32 C 0.9868(7) 0.4738(5) 0.7580(3) 0.0482(16) Uani 1 1 d . . . . .
H32 H 1.0723 0.4371 0.7373 0.058 Uiso 1 1 calc R U . . .
C33 C 0.9911(7) 0.5144(5) 0.8209(3) 0.0467(16) Uani 1 1 d . . . . .
C34 C 0.8627(6) 0.5628(5) 0.8516(3) 0.0441(15) Uani 1 1 d . . . . .
H34 H 0.8598 0.5874 0.8958 0.053 Uiso 1 1 calc R U . . .
C35 C 0.7394(6) 0.5761(5) 0.8197(3) 0.0395(14) Uani 1 1 d . . . . .
C36 C 0.8689(7) 0.4323(6) 0.6556(3) 0.0507(17) Uani 1 1 d . . . . .
C37 C 0.7449(7) 0.3454(6) 0.6658(4) 0.065(2) Uani 1 1 d . . . . .
H37A H 0.7570 0.2768 0.7059 0.097 Uiso 1 1 calc R U . . .
H37B H 0.7459 0.3138 0.6223 0.097 Uiso 1 1 calc R U . . .
H37C H 0.6534 0.3904 0.6758 0.097 Uiso 1 1 calc R U . . .
C38 C 0.8572(8) 0.5375(7) 0.5908(3) 0.067(2) Uani 1 1 d . . . . .
H38A H 0.7647 0.5830 0.5973 0.101 Uiso 1 1 calc R U . . .
H38B H 0.8644 0.5038 0.5476 0.101 Uiso 1 1 calc R U . . .
H38C H 0.9350 0.5928 0.5860 0.101 Uiso 1 1 calc R U . . .
C39 C 1.0090(8) 0.3561(7) 0.6389(4) 0.071(2) Uani 1 1 d . . . . .
H39A H 1.0903 0.4091 0.6291 0.107 Uiso 1 1 calc R U . . .
H39B H 1.0035 0.3213 0.5972 0.107 Uiso 1 1 calc R U . . .
H39C H 1.0220 0.2897 0.6800 0.107 Uiso 1 1 calc R U . . .
C40 C 1.1276(7) 0.5023(6) 0.8573(4) 0.0542(17) Uani 1 1 d . . . . .
C41 C 1.2627(7) 0.4832(7) 0.8059(4) 0.073(2) Uani 1 1 d . . . . .
H41A H 1.3470 0.4756 0.8309 0.110 Uiso 1 1 calc R U . . .
H41B H 1.2711 0.5534 0.7657 0.110 Uiso 1 1 calc R U . . .
H41C H 1.2566 0.4082 0.7882 0.110 Uiso 1 1 calc R U . . .
C42 C 1.1148(9) 0.3962(9) 0.9202(5) 0.107(3) Uani 1 1 d . . . . .
H42A H 1.1106 0.3199 0.9035 0.161 Uiso 1 1 calc R U . . .
H42B H 1.0273 0.4087 0.9525 0.161 Uiso 1 1 calc R U . . .
H42C H 1.1982 0.3908 0.9456 0.161 Uiso 1 1 calc R U . . .
C43 C 1.1450(8) 0.6226(8) 0.8818(5) 0.089(3) Uani 1 1 d . . . . .
H43A H 1.2361 0.6174 0.9011 0.134 Uiso 1 1 calc R U . . .
H43B H 1.0657 0.6348 0.9188 0.134 Uiso 1 1 calc R U . . .
H43C H 1.1443 0.6918 0.8411 0.134 Uiso 1 1 calc R U . . .
C26 C 0.5999(6) 0.6299(5) 0.8544(3) 0.0403(14) Uani 1 1 d . . . . .
H26 H 0.5240 0.6137 0.8272 0.048 Uiso 1 1 calc R U . . .
C27 C 0.5540(6) 0.5659(5) 0.9317(3) 0.0408(15) Uani 1 1 d . . . . .
C28 C 0.5822(6) 0.4407(5) 0.9521(3) 0.0418(15) Uani 1 1 d . . . . .
H28 H 0.6395 0.3985 0.9194 0.050 Uiso 1 1 calc R U . . .
C29 C 0.4705(6) 0.6247(5) 0.9813(3) 0.0440(15) Uani 1 1 d . . . . .
H29 H 0.4496 0.7106 0.9693 0.053 Uiso 1 1 calc R U . . .
C12 C 0.5167(6) 0.8438(5) 0.7955(3) 0.0428(15) Uani 1 1 d . . . . .
C17 C 0.5980(6) 0.7701(5) 0.8441(3) 0.0410(15) Uani 1 1 d . . . . .
C16 C 0.6762(6) 0.8257(5) 0.8836(3) 0.0460(15) Uani 1 1 d . . . . .
H16 H 0.7338 0.7761 0.9161 0.055 Uiso 1 1 calc R U . . .
C15 C 0.6708(7) 0.9533(6) 0.8758(3) 0.0492(16) Uani 1 1 d . . . . .
C14 C 0.5796(7) 1.0213(6) 0.8307(3) 0.0490(16) Uani 1 1 d . . . . .
H14 H 0.5713 1.1076 0.8273 0.059 Uiso 1 1 calc R U . . .
C13 C 0.4994(6) 0.9719(6) 0.7901(3) 0.0479(16) Uani 1 1 d . . . . .
C22 C 0.7636(7) 1.0113(6) 0.9180(4) 0.0616(19) Uani 1 1 d . . . . .
C23A C 0.7172(12) 0.9595(12) 1.0021(6) 0.0784(19) Uiso 0.669(7) 1 d . U P A 1
H23A H 0.6157 0.9815 1.0149 0.118 Uiso 0.669(7) 1 calc R U P A 1
H23B H 0.7328 0.8701 1.0128 0.118 Uiso 0.669(7) 1 calc R U P A 1
H23C H 0.7752 0.9956 1.0296 0.118 Uiso 0.669(7) 1 calc R U P A 1
C24A C 0.7324(13) 1.1471(11) 0.9092(7) 0.0784(19) Uiso 0.669(7) 1 d . U P A 1
H24A H 0.6301 1.1637 0.9239 0.118 Uiso 0.669(7) 1 calc R U P A 1
H24B H 0.7888 1.1796 0.9390 0.118 Uiso 0.669(7) 1 calc R U P A 1
H24C H 0.7578 1.1868 0.8591 0.118 Uiso 0.669(7) 1 calc R U P A 1
C25A C 0.9129(12) 0.9804(12) 0.8973(7) 0.0784(19) Uiso 0.669(7) 1 d . U P A 1
H25A H 0.9282 0.8912 0.9038 0.118 Uiso 0.669(7) 1 calc R U P A 1
H25B H 0.9405 1.0182 0.8470 0.118 Uiso 0.669(7) 1 calc R U P A 1
H25C H 0.9715 1.0110 0.9269 0.118 Uiso 0.669(7) 1 calc R U P A 1
C24B C 0.845(3) 1.126(2) 0.8601(13) 0.0784(19) Uiso 0.331(7) 1 d . U P A 2
H24D H 0.9028 1.0937 0.8210 0.118 Uiso 0.331(7) 1 calc R U P A 2
H24E H 0.7733 1.1871 0.8409 0.118 Uiso 0.331(7) 1 calc R U P A 2
H24F H 0.9079 1.1639 0.8843 0.118 Uiso 0.331(7) 1 calc R U P A 2
C23B C 0.690(3) 1.070(2) 0.9678(13) 0.0784(19) Uiso 0.331(7) 1 d . U P A 2
H23D H 0.7576 1.1037 0.9916 0.118 Uiso 0.331(7) 1 calc R U P A 2
H23E H 0.6283 1.1371 0.9447 0.118 Uiso 0.331(7) 1 calc R U P A 2
H23F H 0.6305 1.0121 1.0032 0.118 Uiso 0.331(7) 1 calc R U P A 2
C5B C 0.901(2) 0.927(2) 0.9395(14) 0.0784(19) Uiso 0.331(7) 1 d . U P A 2
H5B1 H 0.9449 0.8895 0.8994 0.118 Uiso 0.331(7) 1 calc R U P A 2
H5B2 H 0.9711 0.9765 0.9515 0.118 Uiso 0.331(7) 1 calc R U P A 2
H5B3 H 0.8727 0.8617 0.9809 0.118 Uiso 0.331(7) 1 calc R U P A 2
C18 C 0.3934(7) 1.0525(6) 0.7442(4) 0.0557(18) Uani 1 1 d . . . . .
C19 C 0.2444(8) 1.0017(7) 0.7647(5) 0.092(3) Uani 1 1 d . . . . .
H19A H 0.1747 1.0600 0.7410 0.138 Uiso 1 1 calc R U . . .
H19B H 0.2181 0.9893 0.8165 0.138 Uiso 1 1 calc R U . . .
H19C H 0.2449 0.9233 0.7498 0.138 Uiso 1 1 calc R U . . .
C20 C 0.4457(10) 1.0587(7) 0.6653(4) 0.086(2) Uani 1 1 d . . . . .
H20A H 0.5450 1.0835 0.6545 0.128 Uiso 1 1 calc R U . . .
H20B H 0.3849 1.1187 0.6366 0.128 Uiso 1 1 calc R U . . .
H20C H 0.4408 0.9778 0.6540 0.128 Uiso 1 1 calc R U . . .
C21 C 0.3774(9) 1.1838(7) 0.7565(5) 0.086(3) Uani 1 1 d . . . . .
H21A H 0.4690 1.2229 0.7406 0.129 Uiso 1 1 calc R U . . .
H21B H 0.3494 1.1824 0.8074 0.129 Uiso 1 1 calc R U . . .
H21C H 0.3037 1.2301 0.7294 0.129 Uiso 1 1 calc R U . . .
C8 C 0.3871(9) 0.7215(8) 0.5546(4) 0.079(2) Uani 1 1 d . . . . .
C10 C 0.2499(12) 0.6594(12) 0.5574(5) 0.153(5) Uani 1 1 d . . . . .
H10A H 0.2657 0.5707 0.5736 0.229 Uiso 1 1 calc R U . . .
H10B H 0.2199 0.6764 0.5098 0.229 Uiso 1 1 calc R U . . .
H10C H 0.1750 0.6906 0.5907 0.229 Uiso 1 1 calc R U . . .
C9 C 0.5133(11) 0.6708(9) 0.5079(5) 0.109(3) Uani 1 1 d . . . . .
H9A H 0.5987 0.7158 0.5068 0.163 Uiso 1 1 calc R U . . .
H9B H 0.4896 0.6807 0.4593 0.163 Uiso 1 1 calc R U . . .
H9C H 0.5322 0.5836 0.5276 0.163 Uiso 1 1 calc R U . . .
C11 C 0.3739(11) 0.8573(8) 0.5322(5) 0.103(3) Uani 1 1 d . . . . .
H11A H 0.2997 0.8903 0.5651 0.155 Uiso 1 1 calc R U . . .
H11B H 0.3475 0.8794 0.4838 0.155 Uiso 1 1 calc R U . . .
H11C H 0.4658 0.8916 0.5328 0.155 Uiso 1 1 calc R U . . .
C2 C 0.8432(13) 0.8789(12) 0.5440(7) 0.073(5) Uani 0.5 1 d D . P B 2
C1 C 0.7847(14) 0.8693(12) 0.6145(6) 0.065(4) Uani 0.5 1 d D . P B 2
C6 C 0.8420(16) 0.9423(13) 0.6506(7) 0.082(5) Uani 0.5 1 d D . P B 2
H6 H 0.8092 0.9367 0.6999 0.098 Uiso 0.5 1 calc DR U P B 2
C5 C 0.9452(14) 1.0234(11) 0.6181(7) 0.057(4) Uani 0.5 1 d D . P B 2
H5 H 0.9775 1.0753 0.6448 0.069 Uiso 0.5 1 calc DR U P B 2
C4 C 1.0011(16) 1.0312(12) 0.5503(7) 0.080(5) Uani 0.5 1 d D . P B 2
C3 C 0.9503(16) 0.9571(13) 0.5128(9) 0.094(6) Uani 0.5 1 d D . P B 2
C7 C 1.1199(19) 1.1177(16) 0.5158(11) 0.095(6) Uani 0.5 1 d D . P B 2
O3 O 0.6210(4) 0.5650(4) 0.7209(2) 0.0470(11) Uani 1 1 d . . . . .
O2 O 0.4498(4) 0.7875(4) 0.7529(2) 0.0486(11) Uani 1 1 d . . . . .
O4 O 0.6664(5) 0.7956(4) 0.6426(3) 0.0613(14) Uani 0.5 1 d . . P . .
N1 N 0.6664(5) 0.7956(4) 0.6426(3) 0.0613(14) Uani 0.5 1 d . . P . .
O1 O 0.4197(5) 0.6910(4) 0.6281(2) 0.0623(13) Uani 1 1 d . . . . .
V1 V 0.53917(12) 0.71106(10) 0.68412(6) 0.0514(4) Uani 1 1 d . . . . .
C45 C 0.9190(15) 0.8705(12) 0.7188(9) 0.096(6) Uani 0.5 1 d D . P C 1
H45A H 0.9337 0.8616 0.7692 0.115 Uiso 0.5 1 calc R U P C 1
H45B H 0.8327 0.8260 0.7186 0.115 Uiso 0.5 1 calc R U P C 1
Cl1 Cl 0.8823(6) 1.0204(6) 0.6864(4) 0.135(2) Uani 0.5 1 d D . P C 1
Cl2 Cl 1.0522(9) 0.8025(5) 0.6803(4) 0.153(2) Uani 0.5 1 d D . P C 1
H2 H 0.808(5) 0.832(4) 0.5169(14) 0.184 Uiso 0.5 1 d D U P D 2
H3 H 0.987(5) 0.960(5) 0.4651(13) 0.184 Uiso 0.5 1 d D U P E 2
H7A H 1.181(12) 1.085(10) 0.479(7) 0.230 Uiso 0.5 1 d D U P F 2
H7B H 1.176(13) 1.125(14) 0.552(3) 0.230 Uiso 0.5 1 d D U P G 2
H7C H 1.080(7) 1.197(6) 0.495(9) 0.230 Uiso 0.5 1 d D U P H 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
C30 O3 1.383(7) . ?
C30 C35 1.390(8) . ?
C30 C31 1.409(8) . ?
C31 C32 1.393(8) . ?
C31 C36 1.535(8) . ?
C32 C33 1.396(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(8) . ?
C33 C40 1.541(9) . ?
C34 C35 1.381(8) . ?
C34 H34 0.9500 . ?
C35 C26 1.528(8) . ?
C36 C38 1.536(9) . ?
C36 C39 1.545(9) . ?
C36 C37 1.546(8) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
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 C42 1.507(10) . ?
C40 C41 1.529(9) . ?
C40 C43 1.547(9) . ?
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 . ?
C26 C27 1.530(8) . ?
C26 C17 1.536(8) . ?
C26 H26 1.0000 . ?
C27 C28 1.386(8) . ?
C27 C29 1.394(8) . ?
C28 C29 1.383(8) 2_667 ?
C28 H28 0.9500 . ?
C29 C28 1.383(8) 2_667 ?
C29 H29 0.9500 . ?
C12 O2 1.386(7) . ?
C12 C17 1.390(8) . ?
C12 C13 1.411(8) . ?
C17 C16 1.401(8) . ?
C16 C15 1.399(8) . ?
C16 H16 0.9500 . ?
C15 C14 1.384(9) . ?
C15 C22 1.545(9) . ?
C14 C13 1.389(8) . ?
C14 H14 0.9500 . ?
C13 C18 1.541(9) . ?
C22 C23B 1.36(2) . ?
C22 C25A 1.443(13) . ?
C22 C24A 1.501(13) . ?
C22 C5B 1.60(2) . ?
C22 C23A 1.616(13) . ?
C22 C24B 1.67(2) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C5B H5B1 0.9800 . ?
C5B H5B2 0.9800 . ?
C5B H5B3 0.9800 . ?
C18 C20 1.526(10) . ?
C18 C19 1.526(9) . ?
C18 C21 1.528(9) . ?
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 . ?
C8 O1 1.464(8) . ?
C8 C11 1.487(11) . ?
C8 C10 1.508(11) . ?
C8 C9 1.533(12) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C2 C7 1.15(2) 2_776 ?
C2 C3 1.376(13) . ?
C2 C1 1.381(12) . ?
C2 H2 0.930(10) . ?
C1 C6 1.370(10) . ?
C1 O4 1.415(13) . ?
C6 C5 1.374(11) . ?
C6 H6 0.9500 . ?
C5 C4 1.329(11) . ?
C5 H5 0.9500 . ?
C4 C3 1.22(2) 2_776 ?
C4 C3 1.367(12) . ?
C4 C7 1.52(2) . ?
C3 C4 1.22(2) 2_776 ?
C3 C7 1.36(2) 2_776 ?
C3 C3 1.36(3) 2_776 ?
C3 H3 0.933(10) . ?
C7 C2 1.15(2) 2_776 ?
C7 C3 1.36(2) 2_776 ?
C7 H7A 0.961(10) . ?
C7 H7B 0.961(10) . ?
C7 H7C 0.960(10) . ?
O3 V1 1.797(4) . ?
O2 V1 1.805(4) . ?
O4 V1 1.600(5) . ?
O1 V1 1.735(4) . ?
C45 Cl2 1.590(12) . ?
C45 Cl1 1.686(13) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C30 C35 118.6(5) . . ?
O3 C30 C31 120.0(5) . . ?
C35 C30 C31 121.3(5) . . ?
C32 C31 C30 115.8(5) . . ?
C32 C31 C36 121.3(5) . . ?
C30 C31 C36 123.0(5) . . ?
C31 C32 C33 124.6(6) . . ?
C31 C32 H32 117.7 . . ?
C33 C32 H32 117.7 . . ?
C34 C33 C32 116.4(6) . . ?
C34 C33 C40 120.7(5) . . ?
C32 C33 C40 122.8(6) . . ?
C35 C34 C33 121.9(6) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C30 119.6(5) . . ?
C34 C35 C26 120.8(5) . . ?
C30 C35 C26 119.5(5) . . ?
C31 C36 C38 110.4(5) . . ?
C31 C36 C39 112.5(5) . . ?
C38 C36 C39 107.1(6) . . ?
C31 C36 C37 109.4(5) . . ?
C38 C36 C37 110.7(6) . . ?
C39 C36 C37 106.6(5) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C42 C40 C41 110.1(6) . . ?
C42 C40 C33 108.7(5) . . ?
C41 C40 C33 111.8(5) . . ?
C42 C40 C43 110.5(7) . . ?
C41 C40 C43 106.1(6) . . ?
C33 C40 C43 109.6(5) . . ?
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 . . ?
C35 C26 C27 114.2(5) . . ?
C35 C26 C17 112.5(4) . . ?
C27 C26 C17 113.2(5) . . ?
C35 C26 H26 105.3 . . ?
C27 C26 H26 105.3 . . ?
C17 C26 H26 105.3 . . ?
C28 C27 C29 117.3(5) . . ?
C28 C27 C26 119.3(5) . . ?
C29 C27 C26 123.0(5) . . ?
C29 C28 C27 122.0(5) 2_667 . ?
C29 C28 H28 119.0 2_667 . ?
C27 C28 H28 119.0 . . ?
C28 C29 C27 120.7(5) 2_667 . ?
C28 C29 H29 119.7 2_667 . ?
C27 C29 H29 119.7 . . ?
O2 C12 C17 118.0(5) . . ?
O2 C12 C13 120.3(6) . . ?
C17 C12 C13 121.7(5) . . ?
C12 C17 C16 119.0(5) . . ?
C12 C17 C26 120.0(5) . . ?
C16 C17 C26 121.0(5) . . ?
C15 C16 C17 121.0(6) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C14 C15 C16 117.4(6) . . ?
C14 C15 C22 123.2(6) . . ?
C16 C15 C22 119.4(6) . . ?
C15 C14 C13 124.4(6) . . ?
C15 C14 H14 117.8 . . ?
C13 C14 H14 117.8 . . ?
C14 C13 C12 116.1(6) . . ?
C14 C13 C18 121.5(6) . . ?
C12 C13 C18 122.3(6) . . ?
C25A C22 C24A 112.4(8) . . ?
C23B C22 C15 115.5(11) . . ?
C25A C22 C15 109.3(7) . . ?
C24A C22 C15 112.0(7) . . ?
C23B C22 C5B 117.3(15) . . ?
C15 C22 C5B 113.2(10) . . ?
C25A C22 C23A 110.9(8) . . ?
C24A C22 C23A 103.7(8) . . ?
C15 C22 C23A 108.4(6) . . ?
C23B C22 C24B 102.2(14) . . ?
C15 C22 C24B 106.7(9) . . ?
C5B C22 C24B 99.2(13) . . ?
C22 C23A H23A 109.5 . . ?
C22 C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22 C25A H25A 109.5 . . ?
C22 C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C22 C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C22 C24B H24D 109.5 . . ?
C22 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22 C5B H5B1 109.5 . . ?
C22 C5B H5B2 109.5 . . ?
H5B1 C5B H5B2 109.5 . . ?
C22 C5B H5B3 109.5 . . ?
H5B1 C5B H5B3 109.5 . . ?
H5B2 C5B H5B3 109.5 . . ?
C20 C18 C19 111.0(6) . . ?
C20 C18 C21 107.6(6) . . ?
C19 C18 C21 106.2(6) . . ?
C20 C18 C13 110.2(5) . . ?
C19 C18 C13 109.8(6) . . ?
C21 C18 C13 112.0(6) . . ?
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 . . ?
O1 C8 C11 108.3(6) . . ?
O1 C8 C10 104.4(7) . . ?
C11 C8 C10 113.8(9) . . ?
O1 C8 C9 107.5(7) . . ?
C11 C8 C9 109.5(8) . . ?
C10 C8 C9 112.9(8) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C2 C3 64.2(13) 2_776 . ?
C7 C2 C1 173.5(16) 2_776 . ?
C3 C2 C1 121.9(11) . . ?
C7 C2 H2 55.2(17) 2_776 . ?
C3 C2 H2 119.4(15) . . ?
C1 C2 H2 118.7(15) . . ?
C6 C1 C2 115.1(12) . . ?
C6 C1 O4 124.9(10) . . ?
C2 C1 O4 119.9(10) . . ?
C1 C6 C5 122.4(11) . . ?
C1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C4 C5 C6 121.8(11) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C3 C4 C5 177.4(17) 2_776 . ?
C3 C4 C3 63.2(13) 2_776 . ?
C5 C4 C3 117.7(14) . . ?
C3 C4 C7 58.0(12) 2_776 . ?
C5 C4 C7 121.3(13) . . ?
C3 C4 C7 121.0(14) . . ?
C4 C3 C7 72.2(15) 2_776 2_776 ?
C4 C3 C3 63.6(12) 2_776 2_776 ?
C7 C3 C3 136(2) 2_776 2_776 ?
C4 C3 C4 116.8(13) 2_776 . ?
C7 C3 C4 170.2(16) 2_776 . ?
C3 C3 C4 53.3(12) 2_776 . ?
C4 C3 C2 122.1(15) 2_776 . ?
C7 C3 C2 49.9(9) 2_776 . ?
C3 C3 C2 173.4(19) 2_776 . ?
C4 C3 C2 121.0(13) . . ?
C4 C3 H3 4(3) 2_776 . ?
C7 C3 H3 69.3(16) 2_776 . ?
C3 C3 H3 66.7(19) 2_776 . ?
C4 C3 H3 119.9(16) . . ?
C2 C3 H3 119.1(15) . . ?
C2 C7 C3 65.9(14) 2_776 2_776 ?
C2 C7 C4 115.8(18) 2_776 . ?
C3 C7 C4 49.9(11) 2_776 . ?
C2 C7 H7A 31(10) 2_776 . ?
C3 C7 H7A 68(6) 2_776 . ?
C4 C7 H7A 110(4) . . ?
C2 C7 H7B 129(7) 2_776 . ?
C3 C7 H7B 147(8) 2_776 . ?
C4 C7 H7B 108(4) . . ?
H7A C7 H7B 109(2) . . ?
C2 C7 H7C 79(10) 2_776 . ?
C3 C7 H7C 102(9) 2_776 . ?
C4 C7 H7C 111(4) . . ?
H7A C7 H7C 110(2) . . ?
H7B C7 H7C 110(2) . . ?
C30 O3 V1 127.5(3) . . ?
C12 O2 V1 125.7(4) . . ?
C1 O4 V1 172.7(6) . . ?
C8 O1 V1 144.4(4) . . ?
O4 V1 O1 112.1(2) . . ?
O4 V1 O3 106.7(2) . . ?
O1 V1 O3 109.5(2) . . ?
O4 V1 O2 106.1(2) . . ?
O1 V1 O2 110.5(2) . . ?
O3 V1 O2 111.81(18) . . ?
Cl2 C45 Cl1 118.8(10) . . ?
Cl2 C45 H45A 107.6 . . ?
Cl1 C45 H45A 107.6 . . ?
Cl2 C45 H45B 107.6 . . ?
Cl1 C45 H45B 107.6 . . ?
H45A C45 H45B 107.0 . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1404528'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_THETM01_7                   
;
RESPONSE: The data obtained from the UK EPSRC crystallography
service in Southampton were used without further processing. 
The solution obtained is chemically as expected. Refinement
proceeds normally and refinement is stable. 

Diffraction was weak at high angle and no useful data were 
available beyond 22.5 degrees 2theta. Therefore the data 
were truncated at this point.  
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C79 H106 F3 N O7 V2, C H2 Cl2'
_chemical_formula_sum            'C80 H108 Cl2 F3 N O7 V2'
_chemical_formula_weight         1425.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.413(7)
_cell_length_b                   11.244(8)
_cell_length_c                   19.369(13)
_cell_angle_alpha                79.20(4)
_cell_angle_beta                 80.90(3)
_cell_angle_gamma                84.40(4)
_cell_volume                     1983(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3444
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      25.1

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark Red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             758
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.360
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Absorption correction applied within 
CrystalClear-SM software.
;


_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_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            17204
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.299
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        22.499
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5167
_reflns_number_gt                3631
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_structure_solution    'SHELXS97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1285P)²+4.2139P] 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         5167
_refine_ls_number_parameters     527
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.1053
_refine_ls_wR_factor_ref         0.2815
_refine_ls_wR_factor_gt          0.2530
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45653(13) 0.30064(11) 0.81324(7) 0.0481(5) Uani 1 1 d . . . . .
N1 N 0.3253(6) 0.2228(5) 0.8548(3) 0.0593(15) Uani 0.5 1 d . U P A -1
C1 C 0.2129(10) 0.1431(9) 0.8866(6) 0.056(3) Uani 0.5 1 d D U P A -1
C2 C 0.1569(14) 0.0726(12) 0.8490(7) 0.059(4) Uani 0.5 1 d D U P A -1
H2 H 0.1894 0.0762 0.7997 0.071 Uiso 0.5 1 calc R U P A -1
C3 C 0.0518(14) -0.0043(12) 0.8840(7) 0.055(3) Uani 0.5 1 d D U P A -1
H3 H 0.0152 -0.0570 0.8590 0.066 Uiso 0.5 1 calc R U P A -1
C4 C 0.0017(13) -0.0050(12) 0.9521(7) 0.056(3) Uani 0.5 1 d D U P A -1
C5 C 0.0523(17) 0.0668(14) 0.9894(7) 0.068(4) Uani 0.5 1 d D U P A -1
H5 H 0.0139 0.0662 1.0379 0.082 Uiso 0.5 1 calc R U P A -1
C6 C 0.1614(18) 0.1422(16) 0.9566(8) 0.067(4) Uani 0.5 1 d D U P A -1
H6 H 0.1995 0.1923 0.9826 0.080 Uiso 0.5 1 calc R U P A -1
C7 C -0.1112(17) -0.0914(17) 0.9901(9) 0.073(3) Uani 0.5 1 d D U P A -1
F1 F -0.1964(10) -0.1194(9) 0.9459(6) 0.085(3) Uani 0.5 1 d D U P A -1
F2 F -0.1979(11) -0.0461(11) 1.0430(6) 0.097(3) Uani 0.5 1 d D U P A -1
F3 F -0.0511(11) -0.2003(9) 1.0185(6) 0.092(3) Uani 0.5 1 d D U P A -1
O4 O 0.3253(6) 0.2228(5) 0.8548(3) 0.0593(15) Uani 0.5 1 d . . P A 2
O1 O 0.5768(5) 0.3180(5) 0.8692(3) 0.0545(13) Uani 1 1 d . U . . .
C8 C 0.6083(10) 0.2876(8) 0.9419(5) 0.072(2) Uani 1 1 d . U . . .
C9 C 0.6252(14) 0.1493(9) 0.9621(5) 0.108(3) Uani 1 1 d . U . . .
H9A H 0.5308 0.1161 0.9675 0.162 Uiso 1 1 calc R U . . .
H9B H 0.6648 0.1272 1.0070 0.162 Uiso 1 1 calc R U . . .
H9C H 0.6908 0.1161 0.9247 0.162 Uiso 1 1 calc R U . . .
C10 C 0.4815(11) 0.3306(10) 0.9911(5) 0.095(3) Uani 1 1 d . U . . .
H10A H 0.4588 0.4175 0.9758 0.143 Uiso 1 1 calc R U . . .
H10B H 0.5054 0.3163 1.0396 0.143 Uiso 1 1 calc R U . . .
H10C H 0.3979 0.2858 0.9900 0.143 Uiso 1 1 calc R U . . .
C11 C 0.7439(12) 0.3448(12) 0.9418(6) 0.115(4) Uani 1 1 d . U . . .
H11A H 0.8198 0.3153 0.9070 0.173 Uiso 1 1 calc R U . . .
H11B H 0.7735 0.3238 0.9891 0.173 Uiso 1 1 calc R U . . .
H11C H 0.7281 0.4332 0.9293 0.173 Uiso 1 1 calc R U . . .
O2 O 0.3753(5) 0.4463(4) 0.7772(2) 0.0440(12) Uani 1 1 d . . . . .
C12 C 0.2521(6) 0.4660(6) 0.7447(3) 0.0390(16) Uani 1 1 d . . . . .
C13 C 0.1265(7) 0.5269(6) 0.7755(4) 0.0439(17) Uani 1 1 d . . . . .
C14 C 0.0063(7) 0.5348(6) 0.7427(4) 0.0475(18) Uani 1 1 d . . . . .
H14 H -0.0809 0.5707 0.7644 0.057 Uiso 1 1 calc R U . . .
C15 C 0.0040(7) 0.4935(6) 0.6796(4) 0.0443(17) Uani 1 1 d . . . . .
C16 C 0.1336(7) 0.4438(6) 0.6468(4) 0.0419(17) Uani 1 1 d . . . . .
H16 H 0.1371 0.4201 0.6020 0.050 Uiso 1 1 calc R U . . .
C17 C 0.2573(7) 0.4287(5) 0.6793(3) 0.0357(15) Uani 1 1 d . . . . .
C18 C 0.1218(7) 0.5811(6) 0.8436(4) 0.0493(18) Uani 1 1 d . . . . .
C19 C 0.1381(9) 0.4808(7) 0.9077(4) 0.062(2) Uani 1 1 d . . . . .
H19A H 0.1246 0.5165 0.9509 0.093 Uiso 1 1 calc R U . . .
H19B H 0.2347 0.4395 0.9015 0.093 Uiso 1 1 calc R U . . .
H19C H 0.0655 0.4221 0.9118 0.093 Uiso 1 1 calc R U . . .
C20 C -0.0208(8) 0.6547(7) 0.8617(4) 0.061(2) Uani 1 1 d . . . . .
H20A H -0.1009 0.6020 0.8694 0.091 Uiso 1 1 calc R U . . .
H20B H -0.0340 0.7216 0.8223 0.091 Uiso 1 1 calc R U . . .
H20C H -0.0185 0.6874 0.9049 0.091 Uiso 1 1 calc R U . . .
C21 C 0.2450(8) 0.6665(7) 0.8332(4) 0.062(2) Uani 1 1 d . . . . .
H21A H 0.2330 0.7325 0.7932 0.093 Uiso 1 1 calc R U . . .
H21B H 0.3379 0.6207 0.8234 0.093 Uiso 1 1 calc R U . . .
H21C H 0.2425 0.7005 0.8765 0.093 Uiso 1 1 calc R U . . .
C22 C -0.1311(7) 0.5042(7) 0.6428(4) 0.053(2) Uani 1 1 d . . . . .
C23 C -0.2682(7) 0.5214(7) 0.6944(4) 0.059(2) Uani 1 1 d . . . . .
H23A H -0.2748 0.4517 0.7334 0.089 Uiso 1 1 calc R U . . .
H23B H -0.3522 0.5278 0.6695 0.089 Uiso 1 1 calc R U . . .
H23C H -0.2658 0.5957 0.7136 0.089 Uiso 1 1 calc R U . . .
C24 C -0.1212(10) 0.6115(11) 0.5825(6) 0.114(4) Uani 1 1 d . . . . .
H24A H -0.1205 0.6862 0.6017 0.172 Uiso 1 1 calc R U . . .
H24B H -0.2045 0.6169 0.5572 0.172 Uiso 1 1 calc R U . . .
H24C H -0.0323 0.6010 0.5497 0.172 Uiso 1 1 calc R U . . .
C25 C -0.1468(9) 0.3845(9) 0.6174(6) 0.090(3) Uani 1 1 d . . . . .
H25A H -0.0667 0.3712 0.5800 0.135 Uiso 1 1 calc R U . . .
H25B H -0.2383 0.3895 0.5986 0.135 Uiso 1 1 calc R U . . .
H25C H -0.1452 0.3168 0.6574 0.135 Uiso 1 1 calc R U . . .
C26 C 0.4000(6) 0.3733(6) 0.6442(3) 0.0364(15) Uani 1 1 d . . . . .
C27 C 0.4440(6) 0.4373(6) 0.5676(3) 0.0368(16) Uani 1 1 d . . . . .
C28 C 0.4142(7) 0.5628(6) 0.5485(3) 0.0383(16) Uani 1 1 d . . . . .
H28 H 0.3554 0.6067 0.5812 0.046 Uiso 1 1 calc R U . . .
C29 C 0.5294(7) 0.3770(6) 0.5179(4) 0.0401(16) Uani 1 1 d . . . . .
H29 H 0.5498 0.2919 0.5297 0.048 Uiso 1 1 calc R U . . .
O3 O 0.5467(4) 0.2197(4) 0.7449(2) 0.0418(11) Uani 1 1 d . . . . .
C30 C 0.4784(7) 0.1637(6) 0.7025(3) 0.0421(17) Uani 1 1 d . . . . .
C31 C 0.4936(7) 0.0347(6) 0.7085(4) 0.0433(17) Uani 1 1 d . . . . .
C32 C 0.4134(7) -0.0139(6) 0.6674(4) 0.0457(18) Uani 1 1 d . . . . .
H32 H 0.4188 -0.0996 0.6714 0.055 Uiso 1 1 calc R U . . .
C33 C 0.3265(7) 0.0542(6) 0.6212(4) 0.0457(18) Uani 1 1 d . . . . .
C34 C 0.3245(7) 0.1805(6) 0.6135(4) 0.0450(18) Uani 1 1 d . . . . .
H34 H 0.2700 0.2302 0.5803 0.054 Uiso 1 1 calc R U . . .
C35 C 0.4009(7) 0.2346(6) 0.6537(3) 0.0394(16) Uani 1 1 d . . . . .
C36 C 0.5952(7) -0.0452(6) 0.7560(4) 0.0500(19) Uani 1 1 d . . . . .
C37 C 0.6108(9) -0.1764(7) 0.7429(5) 0.071(2) Uani 1 1 d . . . . .
H37A H 0.5193 -0.2141 0.7604 0.107 Uiso 1 1 calc R U . . .
H37B H 0.6869 -0.2221 0.7682 0.107 Uiso 1 1 calc R U . . .
H37C H 0.6361 -0.1769 0.6919 0.107 Uiso 1 1 calc R U . . .
C38 C 0.7457(8) 0.0013(8) 0.7375(6) 0.090(3) Uani 1 1 d . . . . .
H38A H 0.7816 -0.0008 0.6874 0.135 Uiso 1 1 calc R U . . .
H38B H 0.8107 -0.0504 0.7673 0.135 Uiso 1 1 calc R U . . .
H38C H 0.7416 0.0848 0.7460 0.135 Uiso 1 1 calc R U . . .
C39 C 0.5361(12) -0.0487(8) 0.8341(4) 0.091(3) Uani 1 1 d . . . . .
H39A H 0.5316 0.0332 0.8453 0.136 Uiso 1 1 calc R U . . .
H39B H 0.5995 -0.1032 0.8634 0.136 Uiso 1 1 calc R U . . .
H39C H 0.4391 -0.0782 0.8438 0.136 Uiso 1 1 calc R U . . .
C40 C 0.2338(7) -0.0028(6) 0.5793(4) 0.0558(18) Uani 1 1 d D U . . .
C41 C 0.2599(15) -0.1407(9) 0.5888(7) 0.085(4) Uani 0.791(12) 1 d D U P B 1
H41A H 0.3632 -0.1624 0.5775 0.127 Uiso 0.791(12) 1 calc R U P B 1
H41B H 0.2261 -0.1766 0.6381 0.127 Uiso 0.791(12) 1 calc R U P B 1
H41C H 0.2070 -0.1716 0.5570 0.127 Uiso 0.791(12) 1 calc R U P B 1
C42 C 0.2833(10) 0.0432(10) 0.4968(5) 0.062(3) Uani 0.791(12) 1 d D U P B 1
H42A H 0.3848 0.0165 0.4842 0.093 Uiso 0.791(12) 1 calc R U P B 1
H42B H 0.2239 0.0094 0.4690 0.093 Uiso 0.791(12) 1 calc R U P B 1
H42C H 0.2716 0.1321 0.4865 0.093 Uiso 0.791(12) 1 calc R U P B 1
C43 C 0.0781(10) 0.0407(13) 0.5953(8) 0.074(4) Uani 0.791(12) 1 d D U P B 1
H43A H 0.0695 0.1296 0.5881 0.111 Uiso 0.791(12) 1 calc R U P B 1
H43B H 0.0221 0.0129 0.5636 0.111 Uiso 0.791(12) 1 calc R U P B 1
H43C H 0.0411 0.0080 0.6447 0.111 Uiso 0.791(12) 1 calc R U P B 1
C41X C 0.162(4) -0.111(3) 0.6333(18) 0.075(9) Uani 0.209(12) 1 d D U P B 2
H41D H 0.1011 -0.1508 0.6091 0.112 Uiso 0.209(12) 1 calc R U P B 2
H41E H 0.2374 -0.1697 0.6511 0.112 Uiso 0.209(12) 1 calc R U P B 2
H41F H 0.1026 -0.0794 0.6731 0.112 Uiso 0.209(12) 1 calc R U P B 2
C42X C 0.313(4) -0.062(4) 0.5155(17) 0.083(10) Uani 0.209(12) 1 d D U P B 2
H42D H 0.2414 -0.0951 0.4935 0.124 Uiso 0.209(12) 1 calc R U P B 2
H42E H 0.3644 -0.0013 0.4803 0.124 Uiso 0.209(12) 1 calc R U P B 2
H42F H 0.3813 -0.1284 0.5327 0.124 Uiso 0.209(12) 1 calc R U P B 2
C43X C 0.104(3) 0.080(3) 0.555(2) 0.055(8) Uani 0.209(12) 1 d D U P B 2
H43D H 0.0501 0.0379 0.5291 0.082 Uiso 0.209(12) 1 calc R U P B 2
H43E H 0.0402 0.1016 0.5972 0.082 Uiso 0.209(12) 1 calc R U P B 2
H43F H 0.1380 0.1546 0.5246 0.082 Uiso 0.209(12) 1 calc R U P B 2
Cl1 Cl 0.0916(8) -0.0221(8) 0.8090(5) 0.145(3) Uani 0.5 1 d D U P C -2
C45 C 0.084(4) 0.1194(18) 0.7902(17) 0.177(9) Uani 0.5 1 d D U P C -2
H45A H 0.1517 0.1454 0.8178 0.212 Uiso 0.5 1 calc R U P C -2
H45B H 0.1270 0.1389 0.7397 0.212 Uiso 0.5 1 calc R U P C -2
Cl2 Cl -0.0523(15) 0.2051(8) 0.7984(7) 0.215(5) Uani 0.5 1 d D U P C -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O4 1.603(5) . ?
V1 N1 1.603(5) . ?
V1 O1 1.734(5) . ?
V1 O3 1.802(4) . ?
V1 O2 1.803(5) . ?
N1 C1 1.441(12) . ?
C1 C2 1.361(15) . ?
C1 C6 1.363(16) . ?
C2 C3 1.387(15) . ?
C3 C4 1.328(13) . ?
C4 C5 1.343(13) . ?
C4 C7 1.52(2) . ?
C5 C6 1.392(16) . ?
C7 F2 1.35(2) . ?
C7 F3 1.353(16) . ?
C7 F1 1.357(16) . ?
O1 C8 1.455(9) . ?
C8 C11 1.484(12) . ?
C8 C10 1.506(13) . ?
C8 C9 1.530(13) . ?
O2 C12 1.385(7) . ?
C12 C17 1.399(9) . ?
C12 C13 1.412(9) . ?
C13 C14 1.370(9) . ?
C13 C18 1.546(10) . ?
C14 C15 1.390(10) . ?
C15 C16 1.400(9) . ?
C15 C22 1.538(9) . ?
C16 C17 1.391(9) . ?
C17 C26 1.537(8) . ?
C18 C19 1.530(10) . ?
C18 C20 1.533(10) . ?
C18 C21 1.543(10) . ?
C22 C24 1.512(12) . ?
C22 C23 1.522(10) . ?
C22 C25 1.545(11) . ?
C26 C27 1.535(8) . ?
C26 C35 1.535(9) . ?
C27 C29 1.387(9) . ?
C27 C28 1.402(9) . ?
C28 C29 1.386(9) 2_666 ?
C29 C28 1.386(9) 2_666 ?
O3 C30 1.387(8) . ?
C30 C35 1.373(9) . ?
C30 C31 1.428(9) . ?
C31 C32 1.391(9) . ?
C31 C36 1.540(10) . ?
C32 C33 1.382(10) . ?
C33 C34 1.398(9) . ?
C33 C40 1.536(10) . ?
C34 C35 1.390(9) . ?
C36 C39 1.521(11) . ?
C36 C38 1.523(10) . ?
C36 C37 1.532(10) . ?
C40 C43 1.502(10) . ?
C40 C41 1.527(11) . ?
C40 C43X 1.544(16) . ?
C40 C42X 1.57(2) . ?
C40 C41X 1.578(17) . ?
C40 C42 1.593(12) . ?
Cl1 C45 1.56(2) . ?
C45 Cl2 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
O4 V1 O1 111.8(3) . . ?
N1 V1 O1 111.8(3) . . ?
O4 V1 O3 106.8(3) . . ?
N1 V1 O3 106.8(3) . . ?
O1 V1 O3 109.9(2) . . ?
O4 V1 O2 105.7(3) . . ?
N1 V1 O2 105.7(3) . . ?
O1 V1 O2 110.3(2) . . ?
O3 V1 O2 112.3(2) . . ?
C1 N1 V1 173.4(6) . . ?
C2 C1 C6 120.5(8) . . ?
C2 C1 N1 122.2(9) . . ?
C6 C1 N1 117.2(9) . . ?
C1 C2 C3 118.8(8) . . ?
C4 C3 C2 120.5(8) . . ?
C3 C4 C5 121.4(9) . . ?
C3 C4 C7 120.0(12) . . ?
C5 C4 C7 118.6(12) . . ?
C4 C5 C6 119.6(9) . . ?
C1 C6 C5 119.1(9) . . ?
F2 C7 F3 107.8(14) . . ?
F2 C7 F1 107.8(13) . . ?
F3 C7 F1 103.9(15) . . ?
F2 C7 C4 112.0(16) . . ?
F3 C7 C4 112.1(13) . . ?
F1 C7 C4 112.8(13) . . ?
C8 O1 V1 144.3(5) . . ?
O1 C8 C11 105.8(7) . . ?
O1 C8 C10 109.2(7) . . ?
C11 C8 C10 114.4(9) . . ?
O1 C8 C9 108.2(7) . . ?
C11 C8 C9 112.1(9) . . ?
C10 C8 C9 106.9(9) . . ?
C12 O2 V1 126.0(4) . . ?
O2 C12 C17 118.3(6) . . ?
O2 C12 C13 120.7(6) . . ?
C17 C12 C13 120.9(6) . . ?
C14 C13 C12 116.9(6) . . ?
C14 C13 C18 120.7(6) . . ?
C12 C13 C18 122.4(6) . . ?
C13 C14 C15 124.0(6) . . ?
C14 C15 C16 117.7(6) . . ?
C14 C15 C22 123.6(6) . . ?
C16 C15 C22 118.7(6) . . ?
C17 C16 C15 120.6(6) . . ?
C16 C17 C12 119.4(6) . . ?
C16 C17 C26 121.1(6) . . ?
C12 C17 C26 119.5(6) . . ?
C19 C18 C20 106.9(6) . . ?
C19 C18 C21 109.2(6) . . ?
C20 C18 C21 107.8(6) . . ?
C19 C18 C13 111.0(6) . . ?
C20 C18 C13 112.4(6) . . ?
C21 C18 C13 109.4(6) . . ?
C24 C22 C23 109.5(7) . . ?
C24 C22 C15 108.7(6) . . ?
C23 C22 C15 111.4(6) . . ?
C24 C22 C25 112.4(8) . . ?
C23 C22 C25 104.5(6) . . ?
C15 C22 C25 110.4(6) . . ?
C27 C26 C35 114.7(5) . . ?
C27 C26 C17 112.7(5) . . ?
C35 C26 C17 111.6(5) . . ?
C29 C27 C28 117.9(6) . . ?
C29 C27 C26 121.4(6) . . ?
C28 C27 C26 120.2(5) . . ?
C29 C28 C27 120.1(6) 2_666 . ?
C28 C29 C27 122.1(6) 2_666 . ?
C30 O3 V1 125.2(4) . . ?
C35 C30 O3 118.8(6) . . ?
C35 C30 C31 121.3(6) . . ?
O3 C30 C31 119.9(6) . . ?
C32 C31 C30 115.7(6) . . ?
C32 C31 C36 122.1(6) . . ?
C30 C31 C36 122.1(6) . . ?
C33 C32 C31 124.4(6) . . ?
C32 C33 C34 117.2(6) . . ?
C32 C33 C40 123.0(6) . . ?
C34 C33 C40 119.8(7) . . ?
C35 C34 C33 121.1(7) . . ?
C30 C35 C34 119.9(6) . . ?
C30 C35 C26 119.3(6) . . ?
C34 C35 C26 120.8(6) . . ?
C39 C36 C38 111.9(8) . . ?
C39 C36 C37 107.1(7) . . ?
C38 C36 C37 106.4(6) . . ?
C39 C36 C31 110.6(6) . . ?
C38 C36 C31 109.5(6) . . ?
C37 C36 C31 111.2(6) . . ?
C43 C40 C41 114.0(9) . . ?
C43 C40 C33 110.2(7) . . ?
C41 C40 C33 112.6(7) . . ?
C33 C40 C43X 114.3(15) . . ?
C33 C40 C42X 117.8(16) . . ?
C43X C40 C42X 109.1(18) . . ?
C33 C40 C41X 106.0(16) . . ?
C43X C40 C41X 103.6(18) . . ?
C42X C40 C41X 104.5(17) . . ?
C43 C40 C42 107.0(8) . . ?
C41 C40 C42 104.5(7) . . ?
C33 C40 C42 108.1(6) . . ?
Cl2 C45 Cl1 126(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.1(18) . . . . ?
N1 C1 C2 C3 178.2(10) . . . . ?
C1 C2 C3 C4 3(2) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C2 C3 C4 C7 -178.8(13) . . . . ?
C3 C4 C5 C6 -1(3) . . . . ?
C7 C4 C5 C6 176.6(15) . . . . ?
C2 C1 C6 C5 1(2) . . . . ?
N1 C1 C6 C5 179.7(13) . . . . ?
C4 C5 C6 C1 1(3) . . . . ?
C3 C4 C7 F2 -150.3(14) . . . . ?
C5 C4 C7 F2 32(2) . . . . ?
C3 C4 C7 F3 88.4(18) . . . . ?
C5 C4 C7 F3 -89(2) . . . . ?
C3 C4 C7 F1 -28(2) . . . . ?
C5 C4 C7 F1 153.7(14) . . . . ?
O4 V1 O1 C8 1.1(9) . . . . ?
N1 V1 O1 C8 1.1(9) . . . . ?
O3 V1 O1 C8 -117.3(8) . . . . ?
O2 V1 O1 C8 118.3(8) . . . . ?
V1 O1 C8 C11 179.8(8) . . . . ?
V1 O1 C8 C10 -56.6(12) . . . . ?
V1 O1 C8 C9 59.5(12) . . . . ?
O4 V1 O2 C12 -42.7(5) . . . . ?
N1 V1 O2 C12 -42.7(5) . . . . ?
O1 V1 O2 C12 -163.8(5) . . . . ?
O3 V1 O2 C12 73.3(5) . . . . ?
V1 O2 C12 C17 -67.3(7) . . . . ?
V1 O2 C12 C13 115.4(6) . . . . ?
O2 C12 C13 C14 -175.4(6) . . . . ?
C17 C12 C13 C14 7.4(10) . . . . ?
O2 C12 C13 C18 3.7(10) . . . . ?
C17 C12 C13 C18 -173.5(6) . . . . ?
C12 C13 C14 C15 -4.1(11) . . . . ?
C18 C13 C14 C15 176.8(6) . . . . ?
C13 C14 C15 C16 -1.7(11) . . . . ?
C13 C14 C15 C22 -179.3(7) . . . . ?
C14 C15 C16 C17 4.4(10) . . . . ?
C22 C15 C16 C17 -177.9(6) . . . . ?
C15 C16 C17 C12 -1.2(10) . . . . ?
C15 C16 C17 C26 179.5(6) . . . . ?
O2 C12 C17 C16 177.8(6) . . . . ?
C13 C12 C17 C16 -4.9(10) . . . . ?
O2 C12 C17 C26 -2.9(9) . . . . ?
C13 C12 C17 C26 174.4(6) . . . . ?
C14 C13 C18 C19 112.3(8) . . . . ?
C12 C13 C18 C19 -66.8(8) . . . . ?
C14 C13 C18 C20 -7.4(10) . . . . ?
C12 C13 C18 C20 173.6(6) . . . . ?
C14 C13 C18 C21 -127.2(7) . . . . ?
C12 C13 C18 C21 53.8(9) . . . . ?
C14 C15 C22 C24 100.3(9) . . . . ?
C16 C15 C22 C24 -77.3(9) . . . . ?
C14 C15 C22 C23 -20.4(10) . . . . ?
C16 C15 C22 C23 162.0(6) . . . . ?
C14 C15 C22 C25 -136.0(8) . . . . ?
C16 C15 C22 C25 46.4(9) . . . . ?
C16 C17 C26 C27 52.6(8) . . . . ?
C12 C17 C26 C27 -126.6(6) . . . . ?
C16 C17 C26 C35 -78.2(7) . . . . ?
C12 C17 C26 C35 102.6(7) . . . . ?
C35 C26 C27 C29 -24.0(8) . . . . ?
C17 C26 C27 C29 -153.2(6) . . . . ?
C35 C26 C27 C28 164.3(5) . . . . ?
C17 C26 C27 C28 35.1(8) . . . . ?
C29 C27 C28 C29 -0.6(10) . . . 2_666 ?
C26 C27 C28 C29 171.4(6) . . . 2_666 ?
C28 C27 C29 C28 0.6(10) . . . 2_666 ?
C26 C27 C29 C28 -171.3(6) . . . 2_666 ?
O4 V1 O3 C30 41.5(6) . . . . ?
N1 V1 O3 C30 41.5(6) . . . . ?
O1 V1 O3 C30 162.9(5) . . . . ?
O2 V1 O3 C30 -73.9(5) . . . . ?
V1 O3 C30 C35 68.2(7) . . . . ?
V1 O3 C30 C31 -114.0(6) . . . . ?
C35 C30 C31 C32 -6.4(9) . . . . ?
O3 C30 C31 C32 175.8(6) . . . . ?
C35 C30 C31 C36 172.1(6) . . . . ?
O3 C30 C31 C36 -5.7(9) . . . . ?
C30 C31 C32 C33 2.0(10) . . . . ?
C36 C31 C32 C33 -176.5(6) . . . . ?
C31 C32 C33 C34 2.8(10) . . . . ?
C31 C32 C33 C40 -177.0(6) . . . . ?
C32 C33 C34 C35 -3.4(10) . . . . ?
C40 C33 C34 C35 176.4(6) . . . . ?
O3 C30 C35 C34 -176.2(6) . . . . ?
C31 C30 C35 C34 6.0(9) . . . . ?
O3 C30 C35 C26 3.8(8) . . . . ?
C31 C30 C35 C26 -174.0(5) . . . . ?
C33 C34 C35 C30 -0.9(10) . . . . ?
C33 C34 C35 C26 179.1(6) . . . . ?
C27 C26 C35 C30 126.2(6) . . . . ?
C17 C26 C35 C30 -104.1(7) . . . . ?
C27 C26 C35 C34 -53.8(8) . . . . ?
C17 C26 C35 C34 75.9(7) . . . . ?
C32 C31 C36 C39 -110.7(8) . . . . ?
C30 C31 C36 C39 70.9(8) . . . . ?
C32 C31 C36 C38 125.6(8) . . . . ?
C30 C31 C36 C38 -52.9(9) . . . . ?
C32 C31 C36 C37 8.3(9) . . . . ?
C30 C31 C36 C37 -170.2(6) . . . . ?
C32 C33 C40 C43 122.9(9) . . . . ?
C34 C33 C40 C43 -56.9(11) . . . . ?
C32 C33 C40 C41 -5.6(11) . . . . ?
C34 C33 C40 C41 174.6(8) . . . . ?
C32 C33 C40 C43X 156.8(19) . . . . ?
C34 C33 C40 C43X -23(2) . . . . ?
C32 C33 C40 C42X -73(2) . . . . ?
C34 C33 C40 C42X 107.1(19) . . . . ?
C32 C33 C40 C41X 43.3(17) . . . . ?
C34 C33 C40 C41X -136.5(17) . . . . ?
C32 C33 C40 C42 -120.5(8) . . . . ?
C34 C33 C40 C42 59.7(8) . . . . ?

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1404529'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_PLAT201_8                   
;
RESPONSE: Small scale disorder in one of the tBu groups is
modelled using isotropic displacement parameters.  
;


_vrf_PLAT222_8                   
;
RESPONSE: The displacement parameters of the central phenyl 
ring are much smaller than those of the tBu groups on the 
periphery of the molecule. This is entirely reasonable on 
chemical grounds. 
;

_vrf_PLAT213_8                   
;
RESPONSE: This alert relates to the adp of a carbon atom 
on the edge of the molecule in a tBu group. As expected there 
is considerable rocking of these group and this is reflected 
in the adps. 
;


_vrf_PLAT220_8                   
;
RESPONSE: The displacement parameters of the central phenyl 
ring are much smaller than those of the tBu groups on the 
periphery of the molecule. This is entirely reasonable on 
chemical grounds. 
;

_vrf_PLAT242_8                   
;
RESPONSE: The displacement parameter of the central atom
of the tBu group is much smaller than those of the 
external carbon atoms. This is entirely reasonable on 
chemical grounds. 
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
'C86 H112 Cl2 N6 O4 V2' 
;

_chemical_formula_sum            'C86 H112 Cl2 N6 O4 V2'
_chemical_formula_weight         1466.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   10.6773(7)
_cell_length_b                   18.5913(13)
_cell_length_c                   21.2520(15)
_cell_angle_alpha                90
_cell_angle_beta                 96.0750(10)
_cell_angle_gamma                90
_cell_volume                     4194.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6499
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      27.5

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_F_000             1564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.337
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_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            14230
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         27.609
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14230
_reflns_number_gt                12276
_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.
;



_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    SHELXS-2013
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          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)+(0.0830P)²+7.3268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14230
_refine_ls_number_parameters     453
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.1911
_refine_ls_wR_factor_gt          0.1837
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.122
_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 0.42412(6) 0.17002(3) 0.15079(3) 0.02177(15) Uani 1 1 d . . . . .
Cl1 Cl 0.60754(9) 0.21843(6) 0.19411(5) 0.0348(2) Uani 1 1 d . . . . .
O1 O 0.3726(2) 0.08215(13) 0.17537(12) 0.0213(5) Uani 1 1 d . . . . .
O2 O 0.3541(2) 0.19280(13) 0.07092(11) 0.0196(5) Uani 1 1 d . . . . .
N1 N 0.3338(3) 0.22073(17) 0.19261(15) 0.0239(6) Uani 1 1 d . . . . .
C20 C 0.1339(3) 0.17622(18) 0.07282(15) 0.0172(6) Uani 1 1 d . . . . .
C6 C 0.1499(3) 0.07754(17) 0.15725(16) 0.0178(6) Uani 1 1 d . . . . .
C5 C 0.0338(3) 0.06760(18) 0.18067(16) 0.0191(7) Uani 1 1 d . . . . .
H5 H -0.0412 0.0739 0.1529 0.023 Uiso 1 1 calc R U . . .
C15 C 0.1553(3) 0.09576(18) 0.08793(16) 0.0177(7) Uani 1 1 d . . . . .
H15 H 0.2434 0.0850 0.0789 0.021 Uiso 1 1 calc R U . . .
C21 C 0.0145(3) 0.20548(19) 0.06919(17) 0.0223(7) Uani 1 1 d . . . . .
H21 H -0.0532 0.1765 0.0801 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2349(3) 0.22053(19) 0.06037(16) 0.0188(7) Uani 1 1 d . . . . .
C23 C 0.0913(3) 0.31675(19) 0.03343(17) 0.0224(7) Uani 1 1 d . . . . .
H23 H 0.0753 0.3645 0.0188 0.027 Uiso 1 1 calc R U . . .
N2 N 0.5503(3) 0.10087(19) 0.09569(16) 0.0293(7) Uani 1 1 d . . . . .
C3 C 0.1366(4) 0.0385(2) 0.28200(17) 0.0252(8) Uani 1 1 d . . . . .
H3 H 0.1314 0.0246 0.3247 0.030 Uiso 1 1 calc R U . . .
C17 C 0.0475(3) -0.02408(19) 0.05892(16) 0.0207(7) Uani 1 1 d . . . . .
H17 H 0.0800 -0.0416 0.0994 0.025 Uiso 1 1 calc R U . . .
C16 C 0.0696(3) 0.04753(18) 0.04322(16) 0.0169(6) Uani 1 1 d . . . . .
C24 C 0.2144(3) 0.29132(19) 0.03709(16) 0.0203(7) Uani 1 1 d . . . . .
C22 C -0.0098(3) 0.2763(2) 0.04999(18) 0.0253(8) Uani 1 1 d . . . . .
C7 C 0.3767(4) 0.0356(2) 0.30838(19) 0.0324(9) Uani 1 1 d . . . . .
C2 C 0.2553(3) 0.0471(2) 0.26240(17) 0.0230(7) Uani 1 1 d . . . . .
C29 C 0.3234(3) 0.3379(2) 0.01682(17) 0.0235(7) Uani 1 1 d . . . . .
C11 C -0.1037(4) 0.0409(2) 0.26926(18) 0.0293(9) Uani 1 1 d . . . . .
C31 C 0.4154(4) 0.3577(2) 0.07447(19) 0.0302(8) Uani 1 1 d . . . . .
H31A H 0.3705 0.3846 0.1048 0.045 Uiso 1 1 calc R U . . .
H31B H 0.4833 0.3875 0.0609 0.045 Uiso 1 1 calc R U . . .
H31C H 0.4510 0.3138 0.0945 0.045 Uiso 1 1 calc R U . . .
C4 C 0.0242(3) 0.04878(19) 0.24346(17) 0.0211(7) Uani 1 1 d . . . . .
C60 C 0.6117(4) 0.0633(3) 0.0698(2) 0.0342(9) Uani 1 1 d . . . . .
C18 C 0.0208(3) 0.07032(19) -0.01684(16) 0.0203(7) Uani 1 1 d . . . . .
H18 H 0.0345 0.1185 -0.0293 0.024 Uiso 1 1 calc R U . . .
C1 C 0.2598(3) 0.06930(19) 0.19873(17) 0.0204(7) Uani 1 1 d . . . . .
C30 C 0.3937(4) 0.2969(2) -0.03213(19) 0.0319(9) Uani 1 1 d . . . . .
H30A H 0.4624 0.3269 -0.0447 0.048 Uiso 1 1 calc R U . . .
H30B H 0.3350 0.2858 -0.0694 0.048 Uiso 1 1 calc R U . . .
H30C H 0.4285 0.2521 -0.0133 0.048 Uiso 1 1 calc R U . . .
C45 C 0.1705(4) 0.2383(2) 0.2615(2) 0.0383(10) Uani 1 1 d . . . . .
H45 H 0.1328 0.1936 0.2489 0.046 Uiso 1 1 calc R U . . .
C41 C 0.3289(4) 0.3296(2) 0.25126(19) 0.0305(8) Uani 1 1 d . . . . .
H41 H 0.3995 0.3469 0.2320 0.037 Uiso 1 1 calc R U . . .
C40 C 0.2766(4) 0.2628(2) 0.23428(18) 0.0265(8) Uani 1 1 d . . . . .
C32 C 0.2733(4) 0.4086(2) -0.01551(19) 0.0300(8) Uani 1 1 d . . . . .
H32A H 0.2314 0.4374 0.0147 0.045 Uiso 1 1 calc R U . . .
H32B H 0.2131 0.3971 -0.0522 0.045 Uiso 1 1 calc R U . . .
H32C H 0.3438 0.4359 -0.0295 0.045 Uiso 1 1 calc R U . . .
C9 C 0.4667(4) -0.0166(3) 0.2796(2) 0.0441(12) Uani 1 1 d . . . . .
H9A H 0.4274 -0.0642 0.2749 0.066 Uiso 1 1 calc R U . . .
H9B H 0.5455 -0.0201 0.3076 0.066 Uiso 1 1 calc R U . . .
H9C H 0.4843 0.0012 0.2381 0.066 Uiso 1 1 calc R U . . .
C12 C -0.1106(5) -0.0273(4) 0.3066(4) 0.100(3) Uani 1 1 d . . . . .
H12A H -0.0404 -0.0289 0.3402 0.151 Uiso 1 1 calc R U . . .
H12B H -0.1905 -0.0288 0.3254 0.151 Uiso 1 1 calc R U . . .
H12C H -0.1056 -0.0688 0.2785 0.151 Uiso 1 1 calc R U . . .
C10 C 0.3459(4) 0.0015(3) 0.3711(2) 0.0412(11) Uani 1 1 d . . . . .
H10A H 0.2916 0.0341 0.3922 0.062 Uiso 1 1 calc R U . . .
H10B H 0.4241 -0.0069 0.3985 0.062 Uiso 1 1 calc R U . . .
H10C H 0.3023 -0.0443 0.3622 0.062 Uiso 1 1 calc R U . . .
C43 C 0.1740(5) 0.3462(2) 0.3256(2) 0.0391(10) Uani 1 1 d . . . . .
C13 C -0.2135(4) 0.0428(3) 0.2171(2) 0.0454(12) Uani 1 1 d . . . . .
H13A H -0.2096 0.0872 0.1926 0.068 Uiso 1 1 calc R U . . .
H13B H -0.2083 0.0012 0.1892 0.068 Uiso 1 1 calc R U . . .
H13C H -0.2932 0.0412 0.2361 0.068 Uiso 1 1 calc R U . . .
C44 C 0.1211(5) 0.2801(3) 0.3070(2) 0.0445(11) Uani 1 1 d . . . . .
H44 H 0.0499 0.2632 0.3259 0.053 Uiso 1 1 calc R U . . .
C8 C 0.4407(5) 0.1083(3) 0.3232(2) 0.0473(13) Uani 1 1 d . . . . .
H8A H 0.4661 0.1293 0.2842 0.071 Uiso 1 1 calc R U . . .
H8B H 0.5152 0.1014 0.3537 0.071 Uiso 1 1 calc R U . . .
H8C H 0.3817 0.1408 0.3413 0.071 Uiso 1 1 calc R U . . .
C42 C 0.2774(4) 0.3706(2) 0.2962(2) 0.0357(9) Uani 1 1 d . . . . .
H42 H 0.3128 0.4163 0.3075 0.043 Uiso 1 1 calc R U . . .
C25 C -0.1430(4) 0.3073(2) 0.0490(3) 0.0416(11) Uani 1 1 d D . . . .
C14 C -0.1218(6) 0.1066(4) 0.3119(3) 0.080(2) Uani 1 1 d . . . . .
H14A H -0.1171 0.1508 0.2873 0.120 Uiso 1 1 calc R U . . .
H14B H -0.2042 0.1036 0.3281 0.120 Uiso 1 1 calc R U . . .
H14C H -0.0554 0.1069 0.3475 0.120 Uiso 1 1 calc R U . . .
C61 C 0.6916(5) 0.0147(3) 0.0373(3) 0.0539(14) Uani 1 1 d . . . . .
H61A H 0.7725 0.0381 0.0330 0.081 Uiso 1 1 calc R U . . .
H61B H 0.6498 0.0031 -0.0048 0.081 Uiso 1 1 calc R U . . .
H61C H 0.7060 -0.0297 0.0619 0.081 Uiso 1 1 calc R U . . .
C46 C 0.1197(6) 0.3903(3) 0.3763(3) 0.0541(14) Uani 1 1 d . . . . .
H46A H 0.1679 0.4350 0.3835 0.081 Uiso 1 1 calc R U . . .
H46B H 0.0315 0.4019 0.3625 0.081 Uiso 1 1 calc R U . . .
H46C H 0.1245 0.3626 0.4158 0.081 Uiso 1 1 calc R U . . .
C26A C -0.1628(7) 0.3198(5) 0.1221(3) 0.0563(11) Uiso 0.736(7) 1 d D U P A 1
H26A H -0.0990 0.3534 0.1411 0.085 Uiso 0.736(7) 1 calc R U P A 1
H26B H -0.2469 0.3397 0.1251 0.085 Uiso 0.736(7) 1 calc R U P A 1
H26C H -0.1546 0.2738 0.1446 0.085 Uiso 0.736(7) 1 calc R U P A 1
C27A C -0.2405(8) 0.2569(4) 0.0233(4) 0.0563(11) Uiso 0.736(7) 1 d D U P A 1
H27A H -0.2254 0.2097 0.0433 0.085 Uiso 0.736(7) 1 calc R U P A 1
H27B H -0.3233 0.2748 0.0319 0.085 Uiso 0.736(7) 1 calc R U P A 1
H27C H -0.2381 0.2523 -0.0225 0.085 Uiso 0.736(7) 1 calc R U P A 1
C28A C -0.1534(7) 0.3836(4) 0.0225(4) 0.0563(11) Uiso 0.736(7) 1 d D U P A 1
H28A H -0.0841 0.4129 0.0426 0.085 Uiso 0.736(7) 1 calc R U P A 1
H28B H -0.1487 0.3822 -0.0233 0.085 Uiso 0.736(7) 1 calc R U P A 1
H28C H -0.2340 0.4046 0.0311 0.085 Uiso 0.736(7) 1 calc R U P A 1
C26B C -0.166(2) 0.3631(10) 0.0940(9) 0.0563(11) Uiso 0.264(7) 1 d D U P A 2
H26D H -0.2550 0.3774 0.0876 0.085 Uiso 0.264(7) 1 calc R U P A 2
H26E H -0.1465 0.3447 0.1371 0.085 Uiso 0.264(7) 1 calc R U P A 2
H26F H -0.1130 0.4048 0.0876 0.085 Uiso 0.264(7) 1 calc R U P A 2
C27B C -0.2490(19) 0.2477(10) 0.0495(11) 0.0563(11) Uiso 0.264(7) 1 d D U P A 2
H27D H -0.2341 0.2097 0.0192 0.085 Uiso 0.264(7) 1 calc R U P A 2
H27E H -0.2468 0.2270 0.0920 0.085 Uiso 0.264(7) 1 calc R U P A 2
H27F H -0.3317 0.2695 0.0376 0.085 Uiso 0.264(7) 1 calc R U P A 2
C28B C -0.182(2) 0.3392(11) -0.0200(7) 0.0563(11) Uiso 0.264(7) 1 d D U P A 2
H28D H -0.1679 0.3029 -0.0519 0.085 Uiso 0.264(7) 1 calc R U P A 2
H28E H -0.2717 0.3524 -0.0241 0.085 Uiso 0.264(7) 1 calc R U P A 2
H28F H -0.1315 0.3820 -0.0264 0.085 Uiso 0.264(7) 1 calc R U P A 2
N3 N 0.2626(7) 0.1318(3) -0.1287(4) 0.098(2) Uani 1 1 d . . . . .
C71 C 0.1869(7) 0.1747(3) -0.1316(3) 0.0638(15) Uani 1 1 d . . . . .
C72 C 0.0903(6) 0.2303(4) -0.1351(3) 0.0632(16) Uani 1 1 d . . . . .
H72A H 0.0914 0.2541 -0.0938 0.095 Uiso 1 1 calc R U . . .
H72B H 0.0075 0.2084 -0.1464 0.095 Uiso 1 1 calc R U . . .
H72C H 0.1070 0.2658 -0.1672 0.095 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 N1 1.670(3) . ?
V1 O1 1.818(3) . ?
V1 O2 1.831(2) . ?
V1 Cl1 2.2609(11) . ?
V1 N2 2.274(3) . ?
O1 C1 1.372(4) . ?
O2 C19 1.369(4) . ?
N1 C40 1.373(5) . ?
C20 C21 1.380(5) . ?
C20 C19 1.405(5) . ?
C20 C15 1.542(5) . ?
C6 C5 1.396(5) . ?
C6 C1 1.399(5) . ?
C6 C15 1.519(5) . ?
C5 C4 1.393(5) . ?
C5 H5 0.9500 . ?
C15 C16 1.536(5) . ?
C15 H15 1.0000 . ?
C21 C22 1.395(5) . ?
C21 H21 0.9500 . ?
C19 C24 1.415(5) . ?
C23 C22 1.390(5) . ?
C23 C24 1.391(5) . ?
C23 H23 0.9500 . ?
N2 C60 1.140(5) . ?
C3 C2 1.385(5) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
C17 C18 1.390(5) 3 ?
C17 C16 1.399(5) . ?
C17 H17 0.9500 . ?
C16 C18 1.393(5) . ?
C24 C29 1.548(5) . ?
C22 C25 1.532(5) . ?
C7 C8 1.532(6) . ?
C7 C9 1.537(7) . ?
C7 C10 1.542(6) . ?
C7 C2 1.553(5) . ?
C2 C1 1.420(5) . ?
C29 C31 1.532(5) . ?
C29 C30 1.546(5) . ?
C29 C32 1.552(5) . ?
C11 C12 1.502(7) . ?
C11 C13 1.526(6) . ?
C11 C4 1.532(5) . ?
C11 C14 1.545(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C60 C61 1.464(6) . ?
C18 C17 1.390(5) 3 ?
C18 H18 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C45 C44 1.388(6) . ?
C45 C40 1.401(6) . ?
C45 H45 0.9500 . ?
C41 C42 1.381(6) . ?
C41 C40 1.394(6) . ?
C41 H41 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C43 C44 1.393(6) . ?
C43 C42 1.400(7) . ?
C43 C46 1.517(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C44 H44 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C42 H42 0.9500 . ?
C25 C26B 1.450(14) . ?
C25 C27A 1.463(8) . ?
C25 C28A 1.525(8) . ?
C25 C27B 1.585(14) . ?
C25 C28B 1.596(14) . ?
C25 C26A 1.607(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
N3 C71 1.133(8) . ?
C71 C72 1.456(9) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 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
N1 V1 O1 98.33(13) . . ?
N1 V1 O2 99.23(13) . . ?
O1 V1 O2 111.59(11) . . ?
N1 V1 Cl1 94.74(11) . . ?
O1 V1 Cl1 121.08(8) . . ?
O2 V1 Cl1 122.47(9) . . ?
N1 V1 N2 178.76(14) . . ?
O1 V1 N2 81.60(12) . . ?
O2 V1 N2 81.93(11) . . ?
Cl1 V1 N2 84.25(9) . . ?
C1 O1 V1 124.4(2) . . ?
C19 O2 V1 121.4(2) . . ?
C40 N1 V1 170.5(3) . . ?
C21 C20 C19 118.8(3) . . ?
C21 C20 C15 120.7(3) . . ?
C19 C20 C15 120.5(3) . . ?
C5 C6 C1 118.5(3) . . ?
C5 C6 C15 120.1(3) . . ?
C1 C6 C15 121.3(3) . . ?
C4 C5 C6 122.1(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C6 C15 C16 112.8(3) . . ?
C6 C15 C20 113.5(3) . . ?
C16 C15 C20 111.8(3) . . ?
C6 C15 H15 106.0 . . ?
C16 C15 H15 106.0 . . ?
C20 C15 H15 106.0 . . ?
C20 C21 C22 122.1(3) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
O2 C19 C20 117.9(3) . . ?
O2 C19 C24 121.0(3) . . ?
C20 C19 C24 121.2(3) . . ?
C22 C23 C24 123.8(3) . . ?
C22 C23 H23 118.1 . . ?
C24 C23 H23 118.1 . . ?
C60 N2 V1 176.5(3) . . ?
C2 C3 C4 124.5(3) . . ?
C2 C3 H3 117.8 . . ?
C4 C3 H3 117.8 . . ?
C18 C17 C16 121.7(3) 3 . ?
C18 C17 H17 119.2 3 . ?
C16 C17 H17 119.2 . . ?
C18 C16 C17 116.9(3) . . ?
C18 C16 C15 122.0(3) . . ?
C17 C16 C15 120.8(3) . . ?
C23 C24 C19 116.5(3) . . ?
C23 C24 C29 121.9(3) . . ?
C19 C24 C29 121.6(3) . . ?
C23 C22 C21 117.3(3) . . ?
C23 C22 C25 122.5(3) . . ?
C21 C22 C25 120.2(3) . . ?
C8 C7 C9 110.8(4) . . ?
C8 C7 C10 108.4(4) . . ?
C9 C7 C10 106.5(4) . . ?
C8 C7 C2 109.4(3) . . ?
C9 C7 C2 110.6(3) . . ?
C10 C7 C2 111.1(3) . . ?
C3 C2 C1 116.4(3) . . ?
C3 C2 C7 121.6(3) . . ?
C1 C2 C7 122.0(3) . . ?
C31 C29 C30 109.9(3) . . ?
C31 C29 C24 110.5(3) . . ?
C30 C29 C24 110.2(3) . . ?
C31 C29 C32 108.1(3) . . ?
C30 C29 C32 106.7(3) . . ?
C24 C29 C32 111.3(3) . . ?
C12 C11 C13 109.0(5) . . ?
C12 C11 C4 111.5(4) . . ?
C13 C11 C4 112.5(3) . . ?
C12 C11 C14 109.9(5) . . ?
C13 C11 C14 105.9(4) . . ?
C4 C11 C14 107.8(4) . . ?
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 . . ?
C3 C4 C5 116.9(3) . . ?
C3 C4 C11 121.4(3) . . ?
C5 C4 C11 121.7(3) . . ?
N2 C60 C61 179.2(5) . . ?
C17 C18 C16 121.4(3) 3 . ?
C17 C18 H18 119.3 3 . ?
C16 C18 H18 119.3 . . ?
O1 C1 C6 117.6(3) . . ?
O1 C1 C2 121.0(3) . . ?
C6 C1 C2 121.4(3) . . ?
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 . . ?
C44 C45 C40 119.3(4) . . ?
C44 C45 H45 120.4 . . ?
C40 C45 H45 120.4 . . ?
C42 C41 C40 119.5(4) . . ?
C42 C41 H41 120.3 . . ?
C40 C41 H41 120.3 . . ?
N1 C40 C41 118.8(4) . . ?
N1 C40 C45 121.0(4) . . ?
C41 C40 C45 120.2(4) . . ?
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 . . ?
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 . . ?
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 . . ?
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 . . ?
C44 C43 C42 118.3(4) . . ?
C44 C43 C46 120.4(5) . . ?
C42 C43 C46 121.4(4) . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C45 C44 C43 121.3(4) . . ?
C45 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C41 C42 C43 121.4(4) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C27A C25 C28A 115.9(5) . . ?
C26B C25 C22 118.9(9) . . ?
C27A C25 C22 112.8(5) . . ?
C28A C25 C22 112.7(4) . . ?
C26B C25 C27B 108.9(12) . . ?
C22 C25 C27B 113.6(9) . . ?
C26B C25 C28B 107.0(11) . . ?
C22 C25 C28B 107.8(9) . . ?
C27B C25 C28B 98.5(11) . . ?
C27A C25 C26A 107.0(5) . . ?
C28A C25 C26A 102.2(5) . . ?
C22 C25 C26A 104.9(4) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C25 C26A H26A 109.5 . . ?
C25 C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C25 C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C25 C27A H27A 109.5 . . ?
C25 C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
C25 C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C25 C28A H28A 109.5 . . ?
C25 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C25 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C25 C26B H26D 109.5 . . ?
C25 C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C25 C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C25 C27B H27D 109.5 . . ?
C25 C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C25 C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C25 C28B H28D 109.5 . . ?
C25 C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C25 C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
N3 C71 C72 179.5(9) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?

_refine_diff_density_max         0.808
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1404530'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_PLAT220_9                   
;
RESPONSE: Atoms at the core of the molecule have small displacement parameters.
Those of atoms around the edge (especially the tBu groups) are much larger.   
;

_vrf_PLAT222_9                   
;
RESPONSE: Atoms at the core of the molecule have small displacement parameters.
Those of atoms around the edge (especially the tBu groups) are much larger.   
;

_vrf_PLAT242_9                   
;
RESPONSE: C25 is the central atom of a tBu group. As expected, it has a smaller
displacement parameter than those of the carbon atoms attached.   
;

_vrf_GOODF01_9                   
;
RESPONSE: The crystal examined was weakly scattering and contained disordered
solvent. Each of these contributes to a rather low number of observed reflections
and a low GooF, but there is no serious problem with the refinement.    
;

_vrf_PLAT026_9                   
;
RESPONSE: The crystal examined was weakly scattering and contained disordered
solvent. Each of these contributes to a rather low number of observed reflections
and a low GooF, but there is no serious problem with the refinement.    
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H132 Cl2 N2 O6 V2'
_chemical_formula_weight         1798.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.8048(12)
_cell_length_b                   14.4744(13)
_cell_length_c                   18.3207(19)
_cell_angle_alpha                74.937(8)
_cell_angle_beta                 84.606(9)
_cell_angle_gamma                69.796(8)
_cell_volume                     2596.5(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6990
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      26.65

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_F_000             958
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.284
_shelx_estimated_absorpt_T_min   0.895
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            18330
_diffrn_reflns_av_unetI/netI     0.1889
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             9342
_reflns_number_gt                3813
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0738P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9342
_refine_ls_number_parameters     525
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.1661
_refine_ls_wR_factor_gt          0.1407
_refine_ls_goodness_of_fit_ref   0.785
_refine_ls_restrained_S_all      0.789
_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 0.16222(8) 0.37246(6) 0.33086(4) 0.0361(2) Uani 1 1 d . . . . .
O1 O 0.0353(3) 0.3393(2) 0.29562(15) 0.0336(7) Uani 1 1 d . . . . .
O2 O 0.2132(3) 0.4634(2) 0.25704(16) 0.0355(7) Uani 1 1 d . . . . .
O3 O -0.0078(3) 0.5037(2) 0.34431(18) 0.0494(9) Uani 1 1 d . U . . .
N1 N 0.2891(4) 0.2686(3) 0.32834(19) 0.0361(9) Uani 1 1 d . . . . .
Cl1 Cl 0.19331(13) 0.35733(10) 0.45545(7) 0.0530(4) Uani 1 1 d . . . . .
C1 C 0.0614(4) 0.2671(3) 0.2539(2) 0.0301(10) Uani 1 1 d . . . . .
C2 C 0.0350(4) 0.1755(3) 0.2850(2) 0.0358(11) Uani 1 1 d . . . . .
C3 C 0.0758(4) 0.1049(3) 0.2409(3) 0.0387(12) Uani 1 1 d . . . . .
H3 H 0.0628 0.0415 0.2611 0.046 Uiso 1 1 calc R U . . .
C4 C 0.1342(4) 0.1197(3) 0.1696(2) 0.0343(11) Uani 1 1 d . . . . .
C5 C 0.1449(4) 0.2160(3) 0.1395(2) 0.0319(10) Uani 1 1 d . . . . .
H5 H 0.1772 0.2315 0.0893 0.038 Uiso 1 1 calc R U . . .
C6 C 0.1102(4) 0.2893(3) 0.1804(2) 0.0292(10) Uani 1 1 d . . . . .
C7 C -0.0354(5) 0.1564(4) 0.3611(3) 0.0456(12) Uani 1 1 d . . . . .
C8 C 0.0513(6) 0.1485(4) 0.4262(3) 0.0608(16) Uani 1 1 d . . . . .
H8A H 0.0722 0.2113 0.4177 0.091 Uiso 1 1 calc R U . . .
H8B H 0.0036 0.1384 0.4742 0.091 Uiso 1 1 calc R U . . .
H8C H 0.1333 0.0909 0.4282 0.091 Uiso 1 1 calc R U . . .
C9 C -0.1681(5) 0.2417(4) 0.3607(3) 0.0550(14) Uani 1 1 d . . . . .
H9A H -0.1533 0.3070 0.3505 0.082 Uiso 1 1 calc R U . . .
H9B H -0.2247 0.2431 0.3214 0.082 Uiso 1 1 calc R U . . .
H9C H -0.2113 0.2296 0.4101 0.082 Uiso 1 1 calc R U . . .
C10 C -0.0648(6) 0.0568(4) 0.3773(3) 0.0677(17) Uani 1 1 d . . . . .
H10A H -0.1097 0.0468 0.4263 0.102 Uiso 1 1 calc R U . . .
H10B H -0.1215 0.0597 0.3375 0.102 Uiso 1 1 calc R U . . .
H10C H 0.0180 0.0002 0.3786 0.102 Uiso 1 1 calc R U . . .
C11 C 0.1828(5) 0.0374(3) 0.1249(3) 0.0431(12) Uani 1 1 d . . . . .
C12 C 0.2231(7) -0.0696(4) 0.1779(4) 0.085(2) Uani 1 1 d . . . . .
H12A H 0.2916 -0.0769 0.2126 0.127 Uiso 1 1 calc R U . . .
H12B H 0.1461 -0.0798 0.2071 0.127 Uiso 1 1 calc R U . . .
H12C H 0.2573 -0.1203 0.1479 0.127 Uiso 1 1 calc R U . . .
C13 C 0.0776(6) 0.0495(5) 0.0715(4) 0.091(2) Uani 1 1 d . . . . .
H13A H 0.1098 -0.0034 0.0434 0.137 Uiso 1 1 calc R U . . .
H13B H -0.0015 0.0435 0.1003 0.137 Uiso 1 1 calc R U . . .
H13C H 0.0562 0.1165 0.0360 0.137 Uiso 1 1 calc R U . . .
C14 C 0.3057(6) 0.0436(5) 0.0773(4) 0.0779(19) Uani 1 1 d . . . . .
H14A H 0.3766 0.0359 0.1104 0.117 Uiso 1 1 calc R U . . .
H14B H 0.3346 -0.0107 0.0504 0.117 Uiso 1 1 calc R U . . .
H14C H 0.2845 0.1096 0.0406 0.117 Uiso 1 1 calc R U . . .
C15 C 0.1284(4) 0.3919(3) 0.1480(2) 0.0286(10) Uani 1 1 d . . . . .
H15 H 0.0769 0.4361 0.1819 0.034 Uiso 1 1 calc R U . . .
C16 C 0.0677(4) 0.4446(3) 0.0690(2) 0.0266(10) Uani 1 1 d . . . . .
C17 C -0.0580(4) 0.4452(3) 0.0564(2) 0.0328(11) Uani 1 1 d . . . . .
H17 H -0.0996 0.4078 0.0950 0.039 Uiso 1 1 calc R U . . .
C18 C 0.1237(4) 0.5007(3) 0.0113(2) 0.0329(11) Uani 1 1 d . . . . .
H18 H 0.2090 0.5022 0.0181 0.040 Uiso 1 1 calc R U . . .
C19 C 0.3057(4) 0.4311(3) 0.2037(2) 0.0303(10) Uani 1 1 d . . . . .
C20 C 0.2721(4) 0.3868(3) 0.1524(2) 0.0283(10) Uani 1 1 d . . . . .
C21 C 0.3709(4) 0.3370(3) 0.1078(2) 0.0314(10) Uani 1 1 d . . . . .
H21 H 0.3489 0.3051 0.0741 0.038 Uiso 1 1 calc R U . . .
C22 C 0.5014(4) 0.3324(3) 0.1111(2) 0.0357(11) Uani 1 1 d . . . . .
C23 C 0.5262(5) 0.3872(3) 0.1567(2) 0.0381(11) Uani 1 1 d . . . . .
H23 H 0.6131 0.3893 0.1567 0.046 Uiso 1 1 calc R U . . .
C24 C 0.4328(5) 0.4390(3) 0.2022(2) 0.0360(11) Uani 1 1 d . . . . .
C25 C 0.6100(5) 0.2711(4) 0.0655(3) 0.0477(13) Uani 1 1 d . . . . .
C26 C 0.5906(9) 0.3258(8) -0.0178(4) 0.157(4) Uani 1 1 d . . . . .
H26A H 0.5961 0.3938 -0.0254 0.235 Uiso 1 1 calc R U . . .
H26B H 0.6595 0.2873 -0.0478 0.235 Uiso 1 1 calc R U . . .
H26C H 0.5039 0.3314 -0.0340 0.235 Uiso 1 1 calc R U . . .
C27 C 0.6006(8) 0.1711(7) 0.0722(7) 0.166(5) Uani 1 1 d . . . . .
H27A H 0.5112 0.1785 0.0591 0.249 Uiso 1 1 calc R U . . .
H27B H 0.6642 0.1370 0.0377 0.249 Uiso 1 1 calc R U . . .
H27C H 0.6202 0.1305 0.1243 0.249 Uiso 1 1 calc R U . . .
C28 C 0.7452(6) 0.2642(7) 0.0849(5) 0.119(3) Uani 1 1 d . . . . .
H28A H 0.7478 0.3326 0.0798 0.179 Uiso 1 1 calc R U . . .
H28B H 0.7660 0.2245 0.1371 0.179 Uiso 1 1 calc R U . . .
H28C H 0.8100 0.2310 0.0505 0.179 Uiso 1 1 calc R U . . .
C29 C 0.4680(5) 0.5006(4) 0.2497(3) 0.0455(13) Uani 1 1 d . . . . .
C30 C 0.3620(6) 0.6072(4) 0.2382(3) 0.0605(16) Uani 1 1 d . . . . .
H30A H 0.2756 0.6004 0.2536 0.091 Uiso 1 1 calc R U . . .
H30B H 0.3838 0.6457 0.2688 0.091 Uiso 1 1 calc R U . . .
H30C H 0.3594 0.6430 0.1847 0.091 Uiso 1 1 calc R U . . .
C31 C 0.6002(6) 0.5157(4) 0.2248(3) 0.0616(16) Uani 1 1 d . . . . .
H31A H 0.5965 0.5501 0.1710 0.092 Uiso 1 1 calc R U . . .
H31B H 0.6183 0.5572 0.2543 0.092 Uiso 1 1 calc R U . . .
H31C H 0.6704 0.4495 0.2332 0.092 Uiso 1 1 calc R U . . .
C32 C 0.4759(5) 0.4467(4) 0.3341(3) 0.0551(15) Uani 1 1 d . . . . .
H32A H 0.3917 0.4365 0.3509 0.083 Uiso 1 1 calc R U . . .
H32B H 0.5465 0.3807 0.3421 0.083 Uiso 1 1 calc R U . . .
H32C H 0.4945 0.4884 0.3632 0.083 Uiso 1 1 calc R U . . .
C42 C -0.2311(7) 0.5722(6) 0.3771(4) 0.101(2) Uani 1 1 d . U . . .
H42A H -0.2865 0.5410 0.3586 0.121 Uiso 1 1 calc R U . . .
H42B H -0.2799 0.6044 0.4175 0.121 Uiso 1 1 calc R U . . .
C43 C -0.0997(6) 0.4915(6) 0.4073(4) 0.084(2) Uani 1 1 d . U . . .
H43A H -0.0718 0.5038 0.4528 0.101 Uiso 1 1 calc R U . . .
H43B H -0.1063 0.4225 0.4200 0.101 Uiso 1 1 calc R U . . .
C50 C 0.3939(4) 0.1784(3) 0.3394(2) 0.0367(11) Uani 1 1 d . . . . .
C51 C 0.4803(5) 0.1545(4) 0.3997(3) 0.0609(16) Uani 1 1 d . . . . .
H51 H 0.4692 0.2012 0.4298 0.073 Uiso 1 1 calc R U . . .
C52 C 0.5807(6) 0.0627(4) 0.4142(3) 0.0651(17) Uani 1 1 d . . . . .
H52 H 0.6370 0.0465 0.4558 0.078 Uiso 1 1 calc R U . . .
C53 C 0.6033(5) -0.0068(4) 0.3712(3) 0.0544(14) Uani 1 1 d . . . . .
C54 C 0.5148(6) 0.0183(4) 0.3128(4) 0.0698(17) Uani 1 1 d . . . . .
H54 H 0.5262 -0.0285 0.2827 0.084 Uiso 1 1 calc R U . . .
C55 C 0.4101(6) 0.1097(4) 0.2971(3) 0.0622(16) Uani 1 1 d . . . . .
H55 H 0.3504 0.1241 0.2575 0.075 Uiso 1 1 calc R U . . .
C56 C 0.7136(6) -0.1057(4) 0.3878(4) 0.081(2) Uani 1 1 d . . . . .
H56A H 0.7129 -0.1440 0.3510 0.121 Uiso 1 1 calc R U . . .
H56B H 0.7978 -0.0933 0.3844 0.121 Uiso 1 1 calc R U . . .
H56C H 0.7026 -0.1449 0.4388 0.121 Uiso 1 1 calc R U . . .
C40 C -0.0768(7) 0.5755(5) 0.2826(4) 0.084(2) Uani 1 1 d . U . . .
H40A H -0.1037 0.5426 0.2488 0.101 Uiso 1 1 calc R U . . .
H40B H -0.0220 0.6151 0.2535 0.101 Uiso 1 1 calc R U . . .
C41 C -0.2001(7) 0.6455(5) 0.3169(4) 0.083(2) Uani 1 1 d . U . . .
H41A H -0.1783 0.6963 0.3356 0.100 Uiso 1 1 calc R U . . .
H41B H -0.2728 0.6806 0.2799 0.100 Uiso 1 1 calc R U . . .
C60 C 0.9044(8) 0.7667(6) 0.1221(4) 0.090(2) Uani 1 1 d . . . . .
C61 C 0.8563(7) 0.7066(5) 0.0988(4) 0.0780(19) Uani 1 1 d . . . . .
H61 H 0.9161 0.6504 0.0821 0.094 Uiso 1 1 calc R U . . .
C62 C 0.7256(9) 0.7219(6) 0.0980(4) 0.100(2) Uani 1 1 d . . . . .
H62 H 0.6966 0.6758 0.0815 0.120 Uiso 1 1 calc R U . . .
C63 C 0.6367(8) 0.8000(7) 0.1198(5) 0.099(2) Uani 1 1 d . . . . .
H63 H 0.5452 0.8101 0.1185 0.119 Uiso 1 1 calc R U . . .
C64 C 0.6805(11) 0.8668(6) 0.1446(4) 0.109(3) Uani 1 1 d . . . . .
H64 H 0.6177 0.9234 0.1595 0.131 Uiso 1 1 calc R U . . .
C65 C 0.8156(10) 0.8519(5) 0.1478(4) 0.100(2) Uani 1 1 d . . . . .
H65 H 0.8465 0.8958 0.1660 0.120 Uiso 1 1 calc R U . . .
C66 C 1.0476(8) 0.7488(8) 0.1246(5) 0.149(4) Uani 1 1 d . . . . .
H66A H 1.0616 0.8019 0.1434 0.223 Uiso 1 1 calc R U . . .
H66B H 1.0908 0.6823 0.1584 0.223 Uiso 1 1 calc R U . . .
H66C H 1.0852 0.7502 0.0737 0.223 Uiso 1 1 calc R U . . .
C70 C 0.2225(5) 0.7023(4) 0.4183(4) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C71 C 0.2106(5) 0.8015(4) 0.3804(3) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C72 C 0.3083(6) 0.8408(3) 0.3874(4) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C73 C 0.4179(5) 0.7809(4) 0.4323(4) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C74 C 0.4297(5) 0.6817(4) 0.4701(4) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C75 C 0.3320(6) 0.6424(3) 0.4631(4) 0.0663(8) Uiso 0.695(5) 1 d G U P A 1
C76 C 0.1120(10) 0.6625(8) 0.4064(6) 0.0796(10) Uiso 0.695(5) 1 d . U P A 1
C80 C 0.2093(11) 0.7293(10) 0.4047(8) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C81 C 0.2501(13) 0.8128(8) 0.3959(8) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C82 C 0.3696(14) 0.8007(8) 0.4260(9) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C83 C 0.4483(11) 0.7053(10) 0.4651(9) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C84 C 0.4075(13) 0.6218(8) 0.4739(9) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C85 C 0.2880(13) 0.6339(8) 0.4437(9) 0.0663(8) Uiso 0.305(5) 1 d G U P A 2
C86 C 0.077(2) 0.7410(17) 0.3688(12) 0.0796(10) Uiso 0.305(5) 1 d . U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.656(4) . ?
V1 O2 1.817(3) . ?
V1 O1 1.819(3) . ?
V1 O3 2.189(3) . ?
V1 Cl1 2.2814(14) . ?
O1 C1 1.388(5) . ?
O2 C19 1.380(5) . ?
O3 C40 1.388(6) . ?
O3 C43 1.467(7) . ?
N1 C50 1.383(6) . ?
C1 C6 1.398(6) . ?
C1 C2 1.415(6) . ?
C2 C3 1.393(6) . ?
C2 C7 1.531(6) . ?
C3 C4 1.394(6) . ?
C4 C5 1.401(6) . ?
C4 C11 1.536(6) . ?
C5 C6 1.383(6) . ?
C6 C15 1.522(6) . ?
C7 C10 1.531(7) . ?
C7 C9 1.536(7) . ?
C7 C8 1.543(7) . ?
C11 C13 1.504(7) . ?
C11 C14 1.536(8) . ?
C11 C12 1.537(7) . ?
C15 C20 1.537(6) . ?
C15 C16 1.539(5) . ?
C16 C18 1.384(6) . ?
C16 C17 1.395(5) . ?
C17 C18 1.390(5) 2_565 ?
C18 C17 1.390(5) 2_565 ?
C19 C20 1.402(5) . ?
C19 C24 1.414(6) . ?
C20 C21 1.391(6) . ?
C21 C22 1.394(6) . ?
C22 C23 1.390(6) . ?
C22 C25 1.531(7) . ?
C23 C24 1.385(7) . ?
C24 C29 1.549(6) . ?
C25 C27 1.460(9) . ?
C25 C28 1.499(8) . ?
C25 C26 1.523(9) . ?
C29 C31 1.529(7) . ?
C29 C32 1.536(7) . ?
C29 C30 1.547(7) . ?
C42 C41 1.422(10) . ?
C42 C43 1.534(9) . ?
C50 C55 1.369(7) . ?
C50 C51 1.409(6) . ?
C51 C52 1.374(7) . ?
C52 C53 1.378(7) . ?
C53 C54 1.395(7) . ?
C53 C56 1.492(7) . ?
C54 C55 1.394(7) . ?
C40 C41 1.560(9) . ?
C60 C61 1.325(9) . ?
C60 C65 1.436(10) . ?
C60 C66 1.482(10) . ?
C61 C62 1.353(9) . ?
C62 C63 1.332(11) . ?
C63 C64 1.396(11) . ?
C64 C65 1.405(11) . ?
C70 C71 1.3900 . ?
C70 C75 1.3900 . ?
C70 C76 1.546(10) . ?
C71 C72 1.3900 . ?
C72 C73 1.3900 . ?
C73 C74 1.3900 . ?
C74 C75 1.3900 . ?
C80 C81 1.3900 . ?
C80 C85 1.3900 . ?
C80 C86 1.56(2) . ?
C81 C82 1.3900 . ?
C82 C83 1.3900 . ?
C83 C84 1.3900 . ?
C84 C85 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O2 99.32(16) . . ?
N1 V1 O1 98.84(15) . . ?
O2 V1 O1 110.17(12) . . ?
N1 V1 O3 175.11(16) . . ?
O2 V1 O3 85.04(13) . . ?
O1 V1 O3 81.58(13) . . ?
N1 V1 Cl1 92.89(12) . . ?
O2 V1 Cl1 121.19(10) . . ?
O1 V1 Cl1 124.39(10) . . ?
O3 V1 Cl1 82.92(9) . . ?
C1 O1 V1 123.9(2) . . ?
C19 O2 V1 120.6(3) . . ?
C40 O3 C43 109.2(5) . . ?
C40 O3 V1 121.9(4) . . ?
C43 O3 V1 119.3(3) . . ?
C50 N1 V1 170.4(3) . . ?
O1 C1 C6 118.0(4) . . ?
O1 C1 C2 120.2(4) . . ?
C6 C1 C2 121.8(4) . . ?
C3 C2 C1 115.2(4) . . ?
C3 C2 C7 122.7(4) . . ?
C1 C2 C7 122.2(4) . . ?
C2 C3 C4 125.5(4) . . ?
C3 C4 C5 115.9(4) . . ?
C3 C4 C11 123.2(4) . . ?
C5 C4 C11 121.0(4) . . ?
C6 C5 C4 122.2(4) . . ?
C5 C6 C1 119.0(4) . . ?
C5 C6 C15 121.4(4) . . ?
C1 C6 C15 119.5(4) . . ?
C10 C7 C2 111.4(4) . . ?
C10 C7 C9 107.1(4) . . ?
C2 C7 C9 110.2(4) . . ?
C10 C7 C8 107.2(4) . . ?
C2 C7 C8 110.7(4) . . ?
C9 C7 C8 110.1(5) . . ?
C13 C11 C4 110.2(4) . . ?
C13 C11 C14 107.2(5) . . ?
C4 C11 C14 111.9(4) . . ?
C13 C11 C12 110.0(5) . . ?
C4 C11 C12 111.4(4) . . ?
C14 C11 C12 105.9(5) . . ?
C6 C15 C20 112.5(3) . . ?
C6 C15 C16 112.8(3) . . ?
C20 C15 C16 113.4(3) . . ?
C18 C16 C17 117.1(3) . . ?
C18 C16 C15 124.2(3) . . ?
C17 C16 C15 118.4(4) . . ?
C18 C17 C16 121.4(4) 2_565 . ?
C16 C18 C17 121.5(4) . 2_565 ?
O2 C19 C20 118.2(4) . . ?
O2 C19 C24 121.2(4) . . ?
C20 C19 C24 120.6(4) . . ?
C21 C20 C19 118.8(4) . . ?
C21 C20 C15 121.7(3) . . ?
C19 C20 C15 119.5(4) . . ?
C20 C21 C22 122.0(4) . . ?
C23 C22 C21 116.6(4) . . ?
C23 C22 C25 122.4(4) . . ?
C21 C22 C25 121.0(4) . . ?
C24 C23 C22 124.4(4) . . ?
C23 C24 C19 116.6(4) . . ?
C23 C24 C29 121.1(4) . . ?
C19 C24 C29 122.2(4) . . ?
C27 C25 C28 111.7(6) . . ?
C27 C25 C26 106.2(7) . . ?
C28 C25 C26 105.9(6) . . ?
C27 C25 C22 111.4(5) . . ?
C28 C25 C22 112.6(4) . . ?
C26 C25 C22 108.5(5) . . ?
C31 C29 C32 108.6(4) . . ?
C31 C29 C30 107.3(4) . . ?
C32 C29 C30 109.2(4) . . ?
C31 C29 C24 111.1(4) . . ?
C32 C29 C24 111.0(4) . . ?
C30 C29 C24 109.6(4) . . ?
C41 C42 C43 106.9(6) . . ?
O3 C43 C42 103.4(5) . . ?
C55 C50 N1 122.1(4) . . ?
C55 C50 C51 119.7(5) . . ?
N1 C50 C51 118.1(4) . . ?
C52 C51 C50 119.1(5) . . ?
C51 C52 C53 123.0(5) . . ?
C52 C53 C54 116.6(5) . . ?
C52 C53 C56 122.1(5) . . ?
C54 C53 C56 121.3(5) . . ?
C55 C54 C53 122.2(5) . . ?
C50 C55 C54 119.5(5) . . ?
O3 C40 C41 105.2(6) . . ?
C42 C41 C40 100.2(6) . . ?
C61 C60 C65 119.5(7) . . ?
C61 C60 C66 122.7(9) . . ?
C65 C60 C66 117.7(8) . . ?
C60 C61 C62 122.7(8) . . ?
C63 C62 C61 121.6(8) . . ?
C62 C63 C64 118.7(8) . . ?
C63 C64 C65 121.2(8) . . ?
C64 C65 C60 116.3(8) . . ?
C71 C70 C75 120.0 . . ?
C71 C70 C76 117.3(5) . . ?
C75 C70 C76 122.7(5) . . ?
C70 C71 C72 120.0 . . ?
C71 C72 C73 120.0 . . ?
C74 C73 C72 120.0 . . ?
C73 C74 C75 120.0 . . ?
C74 C75 C70 120.0 . . ?
C81 C80 C85 120.0 . . ?
C81 C80 C86 120.6(12) . . ?
C85 C80 C86 119.4(12) . . ?
C80 C81 C82 120.0 . . ?
C83 C82 C81 120.0 . . ?
C82 C83 C84 120.0 . . ?
C83 C84 C85 120.0 . . ?
C84 C85 C80 120.0 . . ?

_refine_diff_density_max         0.510
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1404531'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

_vrf_RFACR01_10                  
;
RESPONSE: Data were collected at the UK EPSRC
crystallography service using a Rigaku rotating anode
as the source. The crystals were weakly scattering.
A few red crystals were attempted and all showed 
signs of splitting with the one used producing the 
cleanest diffraction. The solution has a moderately 
high wR2 but produces a solution that gives excellent 
chemical information.    
;

_vrf_PLAT084_10                  
;
RESPONSE: Data were collected at the UK EPSRC
crystallography service using a Rigaku rotating anode
as the source. The crystals were weakly scattering.
A few red crystals were attempted and all showed 
signs of splitting with the one used producing the 
cleanest diffraction. The solution has a moderately 
high wR2 but produces a solution that gives excellent 
chemical information.    
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C86 H110 Cl2 F6 N2 O6 V2'
_chemical_formula_sum            'C86 H110 Cl2 F6 N2 O6 V2'
_chemical_formula_weight         1554.53

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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.5705(7)
_cell_length_b                   11.3001(8)
_cell_length_c                   17.4045(11)
_cell_angle_alpha                94.986(7)
_cell_angle_beta                 90.688(7)
_cell_angle_gamma                93.257(7)
_cell_volume                     2067.4(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8402
_cell_measurement_theta_min      2.167
_cell_measurement_theta_max      27.499

_exptl_crystal_description       blade
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_F_000             822
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.356
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_T_min  0.68837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            25769
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.277
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             9232
_reflns_number_gt                5672
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;

_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;

_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1508P)²+3.5228P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9232
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0942
_refine_ls_wR_factor_ref         0.2885
_refine_ls_wR_factor_gt          0.2536
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C1 C 1.0111(4) 0.7646(4) 0.2468(3) 0.0298(10) Uani 1 1 d . . . . .
C2 C 1.0715(4) 0.7631(4) 0.3199(3) 0.0342(11) Uani 1 1 d . . . . .
C3 C 1.0817(4) 0.6541(5) 0.3483(3) 0.0361(11) Uani 1 1 d . . . . .
H3 H 1.1221 0.6522 0.3972 0.043 Uiso 1 1 calc R U . . .
C4 C 1.0362(4) 0.5456(4) 0.3096(3) 0.0310(10) Uani 1 1 d . . . . .
C5 C 0.9807(4) 0.5511(4) 0.2363(2) 0.0267(9) Uani 1 1 d . . . . .
H5 H 0.9511 0.4792 0.2077 0.032 Uiso 1 1 calc R U . . .
C6 C 0.9679(4) 0.6573(4) 0.2048(2) 0.0246(9) Uani 1 1 d . . . . .
C7 C 1.1240(5) 0.8794(5) 0.3687(3) 0.0476(14) Uani 1 1 d . . . . .
C8 C 1.2055(8) 0.9561(6) 0.3217(4) 0.081(2) Uani 1 1 d . . . . .
H8A H 1.1592 0.9712 0.2748 0.122 Uiso 1 1 calc R U . . .
H8B H 1.2285 1.0318 0.3518 0.122 Uiso 1 1 calc R U . . .
H8C H 1.2826 0.9156 0.3077 0.122 Uiso 1 1 calc R U . . .
C9 C 1.1921(9) 0.8550(7) 0.4404(4) 0.087(3) Uani 1 1 d . . . . .
H9A H 1.1371 0.8046 0.4705 0.131 Uiso 1 1 calc R U . . .
H9B H 1.2692 0.8142 0.4268 0.131 Uiso 1 1 calc R U . . .
H9C H 1.2150 0.9303 0.4710 0.131 Uiso 1 1 calc R U . . .
C10 C 1.0136(8) 0.9591(7) 0.3941(4) 0.081(2) Uani 1 1 d . . . . .
H10A H 0.9658 0.9775 0.3485 0.121 Uiso 1 1 calc R U . . .
H10B H 0.9571 0.9167 0.4281 0.121 Uiso 1 1 calc R U . . .
H10C H 1.0484 1.0333 0.4219 0.121 Uiso 1 1 calc R U . . .
C11 C 1.0402(5) 0.4265(5) 0.3448(3) 0.0376(11) Uani 1 1 d . . . . .
C12 C 1.0879(6) 0.3298(5) 0.2857(3) 0.0487(13) Uani 1 1 d . . . . .
H12A H 1.0896 0.2543 0.3094 0.073 Uiso 1 1 calc R U . . .
H12B H 1.0308 0.3199 0.2405 0.073 Uiso 1 1 calc R U . . .
H12C H 1.1734 0.3538 0.2697 0.073 Uiso 1 1 calc R U . . .
C13 C 0.9037(5) 0.3879(5) 0.3670(3) 0.0446(13) Uani 1 1 d . . . . .
H13A H 0.9041 0.3115 0.3898 0.067 Uiso 1 1 calc R U . . .
H13B H 0.8718 0.4482 0.4046 0.067 Uiso 1 1 calc R U . . .
H13C H 0.8489 0.3794 0.3208 0.067 Uiso 1 1 calc R U . . .
C14 C 1.1268(7) 0.4340(6) 0.4166(3) 0.0582(16) Uani 1 1 d . . . . .
H14A H 1.1263 0.3559 0.4371 0.087 Uiso 1 1 calc R U . . .
H14B H 1.2134 0.4585 0.4027 0.087 Uiso 1 1 calc R U . . .
H14C H 1.0961 0.4924 0.4559 0.087 Uiso 1 1 calc R U . . .
C15 C 0.9012(4) 0.6594(4) 0.1255(2) 0.0202(8) Uani 1 1 d . . . . .
H15 H 0.9197 0.7408 0.1087 0.024 Uiso 1 1 calc R U . . .
C16 C 0.9512(4) 0.5719(3) 0.0625(2) 0.0208(8) Uani 1 1 d . . . . .
C17 C 1.0751(4) 0.5356(4) 0.0641(2) 0.0226(8) Uani 1 1 d . . . . .
H17 H 1.1280 0.5595 0.1079 0.027 Uiso 1 1 calc R U . . .
C18 C 0.8773(4) 0.5350(4) -0.0028(2) 0.0225(8) Uani 1 1 d . . . . .
H18 H 0.7927 0.5585 -0.0056 0.027 Uiso 1 1 calc R U . . .
C19 C 0.6821(4) 0.7422(4) 0.1337(2) 0.0255(9) Uani 1 1 d . . . . .
C20 C 0.7571(4) 0.6445(4) 0.1335(2) 0.0239(9) Uani 1 1 d . . . . .
C21 C 0.7003(4) 0.5327(4) 0.1420(2) 0.0251(9) Uani 1 1 d . . . . .
H21 H 0.7518 0.4664 0.1412 0.030 Uiso 1 1 calc R U . . .
C22 C 0.5703(4) 0.5147(4) 0.1515(2) 0.0280(9) Uani 1 1 d . . . . .
C23 C 0.4975(4) 0.6141(4) 0.1491(3) 0.0305(10) Uani 1 1 d . . . . .
H23 H 0.4085 0.6031 0.1548 0.037 Uiso 1 1 calc R U . . .
C24 C 0.5480(4) 0.7278(4) 0.1388(3) 0.0306(10) Uani 1 1 d . . . . .
C25 C 0.5086(4) 0.3929(4) 0.1657(3) 0.0390(12) Uani 1 1 d . . . . .
C26 C 0.5996(6) 0.2938(6) 0.1530(6) 0.087(3) Uani 1 1 d . . . . .
H26A H 0.6748 0.3123 0.1862 0.130 Uiso 1 1 calc R U . . .
H26B H 0.5576 0.2185 0.1656 0.130 Uiso 1 1 calc R U . . .
H26C H 0.6250 0.2867 0.0989 0.130 Uiso 1 1 calc R U . . .
C27 C 0.3936(5) 0.3627(5) 0.1140(4) 0.0563(16) Uani 1 1 d . . . . .
H27A H 0.3341 0.4260 0.1216 0.084 Uiso 1 1 calc R U . . .
H27B H 0.4197 0.3553 0.0600 0.084 Uiso 1 1 calc R U . . .
H27C H 0.3523 0.2872 0.1267 0.084 Uiso 1 1 calc R U . . .
C28 C 0.4668(8) 0.3977(7) 0.2503(4) 0.083(2) Uani 1 1 d . . . . .
H28A H 0.5409 0.4172 0.2844 0.125 Uiso 1 1 calc R U . . .
H28B H 0.4052 0.4587 0.2595 0.125 Uiso 1 1 calc R U . . .
H28C H 0.4279 0.3201 0.2608 0.125 Uiso 1 1 calc R U . . .
C29 C 0.4616(5) 0.8325(5) 0.1327(4) 0.0457(13) Uani 1 1 d . . . . .
C30 C 0.4869(6) 0.8875(6) 0.0574(5) 0.067(2) Uani 1 1 d . . . . .
H30A H 0.4709 0.8269 0.0141 0.101 Uiso 1 1 calc R U . . .
H30B H 0.4308 0.9527 0.0527 0.101 Uiso 1 1 calc R U . . .
H30C H 0.5754 0.9184 0.0569 0.101 Uiso 1 1 calc R U . . .
C31 C 0.3204(5) 0.7898(5) 0.1331(4) 0.0493(14) Uani 1 1 d . . . . .
H31A H 0.3020 0.7539 0.1813 0.074 Uiso 1 1 calc R U . . .
H31B H 0.2679 0.8578 0.1290 0.074 Uiso 1 1 calc R U . . .
H31C H 0.3018 0.7307 0.0893 0.074 Uiso 1 1 calc R U . . .
C32 C 0.4864(5) 0.9264(5) 0.2014(5) 0.068(2) Uani 1 1 d . . . . .
H32A H 0.4698 0.8899 0.2496 0.101 Uiso 1 1 calc R U . . .
H32B H 0.5749 0.9574 0.2013 0.101 Uiso 1 1 calc R U . . .
H32C H 0.4303 0.9917 0.1971 0.101 Uiso 1 1 calc R U . . .
C34 C 0.7032(5) 0.8183(5) 0.3424(3) 0.0382(11) Uani 1 1 d . . . . .
C35 C 0.6914(7) 0.6981(5) 0.3514(4) 0.0633(19) Uani 1 1 d . . . . .
H35 H 0.7261 0.6426 0.3144 0.076 Uiso 1 1 calc R U . . .
C36 C 0.6288(9) 0.6589(6) 0.4145(4) 0.081(2) Uani 1 1 d . . . . .
H36 H 0.6225 0.5766 0.4221 0.098 Uiso 1 1 calc R U . . .
C37 C 0.5745(6) 0.7412(6) 0.4674(3) 0.0547(15) Uani 1 1 d . . . . .
C38 C 0.5922(8) 0.8584(6) 0.4592(4) 0.074(2) Uani 1 1 d . . . . .
H38 H 0.5605 0.9145 0.4969 0.089 Uiso 1 1 calc R U . . .
C39 C 0.6557(8) 0.8978(6) 0.3971(4) 0.078(2) Uani 1 1 d . . . . .
H39 H 0.6667 0.9808 0.3919 0.094 Uiso 1 1 calc R U . . .
C40 C 0.4985(9) 0.6957(8) 0.5342(4) 0.080(2) Uani 1 1 d . . . . .
C41 C 0.8449(5) 1.0903(5) 0.0685(3) 0.0430(12) Uani 1 1 d . . . . .
H41A H 0.7612 1.1004 0.0924 0.052 Uiso 1 1 calc R U . . .
H41B H 0.8317 1.0511 0.0157 0.052 Uiso 1 1 calc R U . . .
C42 C 0.9178(5) 1.2100(5) 0.0666(4) 0.0500(14) Uani 1 1 d . . . . .
H42A H 0.8989 1.2474 0.0187 0.060 Uiso 1 1 calc R U . . .
H42B H 0.8983 1.2651 0.1117 0.060 Uiso 1 1 calc R U . . .
C43 C 1.0543(5) 1.1759(5) 0.0694(4) 0.0483(14) Uani 1 1 d . . . . .
H43A H 1.0824 1.1447 0.0179 0.058 Uiso 1 1 calc R U . . .
H43B H 1.1116 1.2446 0.0888 0.058 Uiso 1 1 calc R U . . .
C44 C 1.0497(5) 1.0803(4) 0.1250(3) 0.0387(11) Uani 1 1 d . . . . .
H44A H 1.1163 1.0235 0.1132 0.046 Uiso 1 1 calc R U . . .
H44B H 1.0626 1.1158 0.1788 0.046 Uiso 1 1 calc R U . . .
F1 F 0.5545(5) 0.6130(6) 0.5667(3) 0.112(2) Uani 1 1 d . . . . .
F2 F 0.3891(5) 0.6378(6) 0.5116(3) 0.115(2) Uani 1 1 d . . . . .
F3 F 0.4626(8) 0.7793(5) 0.5798(3) 0.155(3) Uani 1 1 d . . . . .
N1 N 0.7656(4) 0.8590(3) 0.2796(2) 0.0378(10) Uani 1 1 d . . . . .
V1 V 0.83593(8) 0.92702(7) 0.20899(5) 0.0337(3) Uani 1 1 d . . . . .
O1 O 0.9911(3) 0.8688(3) 0.21560(17) 0.0305(7) Uani 1 1 d . . . . .
O2 O 0.7409(3) 0.8529(3) 0.12916(18) 0.0291(7) Uani 1 1 d . . . . .
O3 O 0.9236(3) 1.0201(3) 0.1147(2) 0.0366(8) Uani 1 1 d . . . . .
Cl1 Cl 0.80140(14) 1.11349(11) 0.25948(8) 0.0484(4) 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
C1 O1 1.365(6) . ?
C1 C6 1.410(6) . ?
C1 C2 1.418(7) . ?
C2 C3 1.376(7) . ?
C2 C7 1.571(7) . ?
C3 C4 1.404(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.407(6) . ?
C4 C11 1.529(7) . ?
C5 C6 1.375(6) . ?
C5 H5 0.9500 . ?
C6 C15 1.544(6) . ?
C7 C9 1.487(9) . ?
C7 C8 1.489(9) . ?
C7 C10 1.559(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.534(7) . ?
C11 C12 1.545(8) . ?
C11 C13 1.546(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.531(5) . ?
C15 C20 1.532(5) . ?
C15 H15 1.0000 . ?
C16 C18 1.391(6) . ?
C16 C17 1.396(6) . ?
C17 C18 1.393(6) 2_765 ?
C17 H17 0.9500 . ?
C18 C17 1.393(6) 2_765 ?
C18 H18 0.9500 . ?
C19 O2 1.374(5) . ?
C19 C20 1.396(6) . ?
C19 C24 1.423(6) . ?
C20 C21 1.387(6) . ?
C21 C22 1.392(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.400(7) . ?
C22 C25 1.530(6) . ?
C23 C24 1.390(6) . ?
C23 H23 0.9500 . ?
C24 C29 1.544(7) . ?
C25 C27 1.509(7) . ?
C25 C26 1.520(9) . ?
C25 C28 1.540(9) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.518(9) . ?
C29 C32 1.538(9) . ?
C29 C31 1.542(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 . ?
C34 C39 1.371(8) . ?
C34 C35 1.380(8) . ?
C34 N1 1.383(6) . ?
C35 C36 1.382(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.401(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.347(9) . ?
C37 C40 1.531(9) . ?
C38 C39 1.373(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 F3 1.259(10) . ?
C40 F1 1.300(9) . ?
C40 F2 1.333(10) . ?
C41 O3 1.462(6) . ?
C41 C42 1.522(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.515(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.512(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 O3 1.464(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
N1 V1 1.666(4) . ?
V1 O1 1.808(3) . ?
V1 O2 1.819(3) . ?
V1 O3 2.210(3) . ?
V1 Cl1 2.2625(14) . ?

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 C1 C6 118.0(4) . . ?
O1 C1 C2 121.5(4) . . ?
C6 C1 C2 120.5(4) . . ?
C3 C2 C1 117.3(4) . . ?
C3 C2 C7 119.9(4) . . ?
C1 C2 C7 122.8(5) . . ?
C2 C3 C4 124.1(4) . . ?
C2 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
C3 C4 C5 116.6(4) . . ?
C3 C4 C11 123.2(4) . . ?
C5 C4 C11 120.2(4) . . ?
C6 C5 C4 122.0(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C1 119.5(4) . . ?
C5 C6 C15 120.1(4) . . ?
C1 C6 C15 120.3(4) . . ?
C9 C7 C8 110.6(6) . . ?
C9 C7 C10 106.7(6) . . ?
C8 C7 C10 104.0(6) . . ?
C9 C7 C2 113.0(5) . . ?
C8 C7 C2 111.5(4) . . ?
C10 C7 C2 110.6(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C11 C14 112.4(4) . . ?
C4 C11 C12 110.8(4) . . ?
C14 C11 C12 108.0(5) . . ?
C4 C11 C13 108.1(4) . . ?
C14 C11 C13 109.3(5) . . ?
C12 C11 C13 108.2(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 112.5(3) . . ?
C16 C15 C6 114.0(3) . . ?
C20 C15 C6 110.5(3) . . ?
C16 C15 H15 106.4 . . ?
C20 C15 H15 106.4 . . ?
C6 C15 H15 106.4 . . ?
C18 C16 C17 117.4(4) . . ?
C18 C16 C15 120.3(4) . . ?
C17 C16 C15 122.0(4) . . ?
C18 C17 C16 121.2(4) 2_765 . ?
C18 C17 H17 119.4 2_765 . ?
C16 C17 H17 119.4 . . ?
C16 C18 C17 121.4(4) . 2_765 ?
C16 C18 H18 119.3 . . ?
C17 C18 H18 119.3 2_765 . ?
O2 C19 C20 118.4(4) . . ?
O2 C19 C24 120.7(4) . . ?
C20 C19 C24 120.9(4) . . ?
C21 C20 C19 119.4(4) . . ?
C21 C20 C15 119.7(4) . . ?
C19 C20 C15 120.9(4) . . ?
C20 C21 C22 122.1(4) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C23 116.9(4) . . ?
C21 C22 C25 122.1(4) . . ?
C23 C22 C25 120.9(4) . . ?
C24 C23 C22 123.8(4) . . ?
C24 C23 H23 118.1 . . ?
C22 C23 H23 118.1 . . ?
C23 C24 C19 116.7(4) . . ?
C23 C24 C29 121.2(4) . . ?
C19 C24 C29 122.1(4) . . ?
C27 C25 C26 108.7(5) . . ?
C27 C25 C22 111.0(4) . . ?
C26 C25 C22 112.4(4) . . ?
C27 C25 C28 108.8(5) . . ?
C26 C25 C28 107.8(6) . . ?
C22 C25 C28 108.1(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C32 110.2(5) . . ?
C30 C29 C31 108.1(5) . . ?
C32 C29 C31 107.8(5) . . ?
C30 C29 C24 109.2(5) . . ?
C32 C29 C24 110.4(5) . . ?
C31 C29 C24 111.2(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 . . ?
C39 C34 C35 119.8(5) . . ?
C39 C34 N1 119.9(5) . . ?
C35 C34 N1 120.3(5) . . ?
C34 C35 C36 119.5(6) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C35 C36 C37 119.7(6) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C38 C37 C36 119.5(6) . . ?
C38 C37 C40 121.4(6) . . ?
C36 C37 C40 119.0(6) . . ?
C37 C38 C39 120.8(6) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C34 C39 C38 120.4(6) . . ?
C34 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
F3 C40 F1 115.1(7) . . ?
F3 C40 F2 102.3(8) . . ?
F1 C40 F2 100.8(7) . . ?
F3 C40 C37 112.2(7) . . ?
F1 C40 C37 112.3(6) . . ?
F2 C40 C37 113.2(6) . . ?
O3 C41 C42 105.4(4) . . ?
O3 C41 H41A 110.7 . . ?
C42 C41 H41A 110.7 . . ?
O3 C41 H41B 110.7 . . ?
C42 C41 H41B 110.7 . . ?
H41A C41 H41B 108.8 . . ?
C43 C42 C41 102.2(4) . . ?
C43 C42 H42A 111.3 . . ?
C41 C42 H42A 111.3 . . ?
C43 C42 H42B 111.3 . . ?
C41 C42 H42B 111.3 . . ?
H42A C42 H42B 109.2 . . ?
C44 C43 C42 102.7(4) . . ?
C44 C43 H43A 111.2 . . ?
C42 C43 H43A 111.2 . . ?
C44 C43 H43B 111.2 . . ?
C42 C43 H43B 111.2 . . ?
H43A C43 H43B 109.1 . . ?
O3 C44 C43 105.6(4) . . ?
O3 C44 H44A 110.6 . . ?
C43 C44 H44A 110.6 . . ?
O3 C44 H44B 110.6 . . ?
C43 C44 H44B 110.6 . . ?
H44A C44 H44B 108.7 . . ?
C34 N1 V1 172.0(4) . . ?
N1 V1 O1 99.05(18) . . ?
N1 V1 O2 97.55(17) . . ?
O1 V1 O2 112.47(14) . . ?
N1 V1 O3 178.16(18) . . ?
O1 V1 O3 82.79(14) . . ?
O2 V1 O3 81.75(13) . . ?
N1 V1 Cl1 95.29(14) . . ?
O1 V1 Cl1 120.60(11) . . ?
O2 V1 Cl1 122.21(11) . . ?
O3 V1 Cl1 83.68(10) . . ?
C1 O1 V1 122.7(3) . . ?
C19 O2 V1 121.5(3) . . ?
C41 O3 C44 108.9(4) . . ?
C41 O3 V1 119.1(3) . . ?
C44 O3 V1 120.5(3) . . ?

_refine_diff_density_max         1.376
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.133

####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1404532'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 522 53 ' '
_platon_squeeze_details          ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C76 H106 O8 V2
;
_chemical_formula_sum            'C76 H106 O8 V2'
_chemical_formula_weight         1249.49



_vrf_PLAT201_11                  
;
RESPONSE: Small scale disorder in one the methyl groups
was modelled using isotropic displacement parameters. 
;


_vrf_PLAT220_11                  
;
RESPONSE: It is completely reasonable that the tertiary 
butyl groups have larger displacement paramaters than the
central core of carbon atoms. This alert reflects this. 
;




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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   11.3476(8)
_cell_length_b                   12.2819(9)
_cell_length_c                   16.8097(11)
_cell_angle_alpha                100.861(4)
_cell_angle_beta                 99.097(4)
_cell_angle_gamma                108.087(5)
_cell_volume                     2127.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9756
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9818
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_process_details   
;
A multi-scan absorption correction was implemented
within Rigaku CrystalClear. 

Tma = 1; Tmin = 0.742
;

_exptl_special_details           
;
 An extremely disordered solvent molecule was located
but we were unable to model this effectively. The structure
was therefore treated with the SQUEEZE routine. 

Before squeeze: wR(F2) = 0.3306  R1 (all data) = 0.1380
After squeeze:  WR(F2) = 0.1587  R1 (all data) = 0.0848
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_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_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9683
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.49
_reflns_number_total             9683
_reflns_number_gt                6948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b22 (Rigaku, 20112)
;

_computing_structure_solution    'SHELXS-86 (Shldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0858P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9683
_refine_ls_number_parameters     392
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1587
_refine_ls_wR_factor_gt          0.1479
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0128(2) 0.44827(18) 0.25984(13) 0.0152(4) Uani 1 1 d . . .
C2 C 0.9000(2) 0.36620(18) 0.20628(13) 0.0149(4) Uani 1 1 d . . .
C3 C 0.9021(2) 0.31678(19) 0.12486(13) 0.0168(4) Uani 1 1 d . . .
H3 H 0.8260 0.2599 0.0887 0.020 Uiso 1 1 calc R . .
C4 C 1.0121(2) 0.34831(19) 0.09507(14) 0.0177(5) Uani 1 1 d . A .
C5 C 1.1210(2) 0.4352(2) 0.14922(14) 0.0181(5) Uani 1 1 d . . .
H5 H 1.1962 0.4586 0.1291 0.022 Uiso 1 1 calc R . .
C6 C 1.1261(2) 0.48983(19) 0.23104(14) 0.0170(4) Uani 1 1 d . . .
C7 C 1.2426(2) 0.5947(2) 0.28510(14) 0.0206(5) Uani 1 1 d . . .
C8 C 1.2994(2) 0.5690(2) 0.36596(16) 0.0300(6) Uani 1 1 d . . .
H8A H 1.3144 0.4939 0.3525 0.045 Uiso 1 1 calc R . .
H8B H 1.2398 0.5636 0.4026 0.045 Uiso 1 1 calc R . .
H8C H 1.3803 0.6331 0.3943 0.045 Uiso 1 1 calc R . .
C9 C 1.2019(3) 0.7034(2) 0.30669(16) 0.0283(6) Uani 1 1 d . . .
H9A H 1.2767 0.7728 0.3374 0.042 Uiso 1 1 calc R . .
H9B H 1.1395 0.6882 0.3412 0.042 Uiso 1 1 calc R . .
H9C H 1.1635 0.7183 0.2552 0.042 Uiso 1 1 calc R . .
C10 C 1.3493(2) 0.6281(2) 0.23837(16) 0.0299(6) Uani 1 1 d . . .
H10A H 1.3803 0.5621 0.2256 0.045 Uiso 1 1 calc R . .
H10B H 1.4197 0.6984 0.2733 0.045 Uiso 1 1 calc R . .
H10C H 1.3161 0.6450 0.1864 0.045 Uiso 1 1 calc R . .
C11 C 1.0095(2) 0.2884(2) 0.00522(14) 0.0198(5) Uani 1 1 d D . .
C12A C 0.9767(4) 0.1542(3) -0.0037(2) 0.0320(5) Uiso 0.717(3) 1 d PD A 1
H12A H 0.8948 0.1216 0.0109 0.048 Uiso 0.717(3) 1 calc PR A 1
H12B H 1.0435 0.1410 0.0338 0.048 Uiso 0.717(3) 1 calc PR A 1
H12C H 0.9709 0.1148 -0.0613 0.048 Uiso 0.717(3) 1 calc PR A 1
C13A C 0.9073(4) 0.3086(4) -0.0553(2) 0.0320(5) Uiso 0.717(3) 1 d PD A 1
H13A H 0.8247 0.2783 -0.0411 0.048 Uiso 0.717(3) 1 calc PR A 1
H13B H 0.9018 0.2670 -0.1123 0.048 Uiso 0.717(3) 1 calc PR A 1
H13C H 0.9298 0.3936 -0.0512 0.048 Uiso 0.717(3) 1 calc PR A 1
C14A C 1.1365(4) 0.3357(3) -0.0183(2) 0.0320(5) Uiso 0.717(3) 1 d PD A 1
H14A H 1.1295 0.2946 -0.0757 0.048 Uiso 0.717(3) 1 calc PR A 1
H14B H 1.2027 0.3222 0.0194 0.048 Uiso 0.717(3) 1 calc PR A 1
H14C H 1.1589 0.4208 -0.0136 0.048 Uiso 0.717(3) 1 calc PR A 1
C12B C 1.0675(9) 0.1934(8) 0.0096(6) 0.0320(5) Uiso 0.283(3) 1 d PD A 2
H12D H 1.0672 0.1535 -0.0468 0.048 Uiso 0.283(3) 1 calc PR A 2
H12E H 1.0174 0.1354 0.0354 0.048 Uiso 0.283(3) 1 calc PR A 2
H12F H 1.1553 0.2296 0.0430 0.048 Uiso 0.283(3) 1 calc PR A 2
C13B C 0.8773(8) 0.2333(8) -0.0535(6) 0.0320(5) Uiso 0.283(3) 1 d PD A 2
H13D H 0.8844 0.1971 -0.1089 0.048 Uiso 0.283(3) 1 calc PR A 2
H13E H 0.8403 0.2949 -0.0574 0.048 Uiso 0.283(3) 1 calc PR A 2
H13F H 0.8224 0.1726 -0.0319 0.048 Uiso 0.283(3) 1 calc PR A 2
C14B C 1.0905(9) 0.3785(8) -0.0383(6) 0.0320(5) Uiso 0.283(3) 1 d PD A 2
H14D H 1.0864 0.3370 -0.0951 0.048 Uiso 0.283(3) 1 calc PR A 2
H14E H 1.1793 0.4122 -0.0066 0.048 Uiso 0.283(3) 1 calc PR A 2
H14F H 1.0560 0.4421 -0.0403 0.048 Uiso 0.283(3) 1 calc PR A 2
C15 C 0.7770(2) 0.33293(18) 0.23664(13) 0.0150(4) Uani 1 1 d . . .
H15 H 0.7966 0.3878 0.2930 0.018 Uiso 1 1 calc R . .
C16 C 0.6676(2) 0.35425(19) 0.18365(13) 0.0162(4) Uani 1 1 d . . .
C17 C 0.5428(2) 0.3021(2) 0.18988(15) 0.0218(5) Uani 1 1 d . . .
H17 H 0.5236 0.2437 0.2204 0.026 Uiso 1 1 calc R . .
C18 C 0.4454(2) 0.3354(2) 0.15131(15) 0.0267(5) Uani 1 1 d . . .
H18 H 0.3606 0.3004 0.1566 0.032 Uiso 1 1 calc R . .
C19 C 0.4720(3) 0.4191(2) 0.10561(15) 0.0288(6) Uani 1 1 d . . .
H19 H 0.4059 0.4417 0.0796 0.035 Uiso 1 1 calc R . .
C20 C 0.5952(3) 0.4693(2) 0.09806(15) 0.0288(6) Uani 1 1 d . . .
H20 H 0.6135 0.5259 0.0661 0.035 Uiso 1 1 calc R . .
C21 C 0.6926(2) 0.4379(2) 0.13684(14) 0.0228(5) Uani 1 1 d . . .
H21 H 0.7771 0.4738 0.1315 0.027 Uiso 1 1 calc R . .
C22 C 0.7750(2) 0.19329(18) 0.33090(13) 0.0157(4) Uani 1 1 d . . .
C23 C 0.7462(2) 0.0784(2) 0.34490(14) 0.0198(5) Uani 1 1 d . . .
C24 C 0.6928(2) -0.01690(19) 0.27428(14) 0.0214(5) Uani 1 1 d . . .
H24 H 0.6752 -0.0946 0.2818 0.026 Uiso 1 1 calc R . .
C25 C 0.6638(2) -0.00460(19) 0.19315(14) 0.0184(5) Uani 1 1 d . . .
C26 C 0.6867(2) 0.11021(19) 0.18376(14) 0.0174(5) Uani 1 1 d . . .
H26 H 0.6625 0.1210 0.1299 0.021 Uiso 1 1 calc R . .
C27 C 0.7435(2) 0.20848(19) 0.25043(13) 0.0158(4) Uani 1 1 d . . .
C28 C 0.6063(2) -0.1099(2) 0.11588(15) 0.0248(5) Uani 1 1 d . . .
C29 C 0.6105(3) -0.2263(2) 0.13486(16) 0.0294(6) Uani 1 1 d . . .
H29A H 0.6989 -0.2174 0.1578 0.044 Uiso 1 1 calc R . .
H29B H 0.5759 -0.2900 0.0834 0.044 Uiso 1 1 calc R . .
H29C H 0.5594 -0.2459 0.1755 0.044 Uiso 1 1 calc R . .
C30 C 0.4678(3) -0.1247(3) 0.0816(2) 0.0470(8) Uani 1 1 d . . .
H30A H 0.4181 -0.1444 0.1229 0.071 Uiso 1 1 calc R . .
H30B H 0.4325 -0.1884 0.0303 0.071 Uiso 1 1 calc R . .
H30C H 0.4640 -0.0506 0.0697 0.071 Uiso 1 1 calc R . .
C31 C 0.6839(3) -0.0871(2) 0.04942(17) 0.0413(8) Uani 1 1 d . . .
H31A H 0.6796 -0.0157 0.0330 0.062 Uiso 1 1 calc R . .
H31B H 0.6484 -0.1550 0.0006 0.062 Uiso 1 1 calc R . .
H31C H 0.7729 -0.0762 0.0724 0.062 Uiso 1 1 calc R . .
C32 C 0.7630(3) 0.0578(2) 0.43308(15) 0.0263(5) Uani 1 1 d . . .
C33 C 0.7293(3) -0.0753(2) 0.42969(17) 0.0417(8) Uani 1 1 d . . .
H33A H 0.7451 -0.0852 0.4864 0.063 Uiso 1 1 calc R . .
H33B H 0.7822 -0.1071 0.3983 0.063 Uiso 1 1 calc R . .
H33C H 0.6392 -0.1178 0.4021 0.063 Uiso 1 1 calc R . .
C34 C 0.9008(3) 0.1219(2) 0.48489(16) 0.0348(6) Uani 1 1 d . . .
H34A H 0.9190 0.2075 0.4993 0.052 Uiso 1 1 calc R . .
H34B H 0.9599 0.1039 0.4523 0.052 Uiso 1 1 calc R . .
H34C H 0.9113 0.0949 0.5360 0.052 Uiso 1 1 calc R . .
C35 C 0.6721(3) 0.1021(2) 0.47655(17) 0.0368(7) Uani 1 1 d . . .
H35A H 0.6959 0.1878 0.4833 0.055 Uiso 1 1 calc R . .
H35B H 0.6772 0.0850 0.5314 0.055 Uiso 1 1 calc R . .
H35C H 0.5847 0.0621 0.4428 0.055 Uiso 1 1 calc R . .
C41 C 0.7859(2) 0.5363(2) 0.44504(14) 0.0197(5) Uani 1 1 d . . .
H41A H 0.7492 0.5639 0.4912 0.024 Uiso 1 1 calc R . .
H41B H 0.7266 0.4565 0.4130 0.024 Uiso 1 1 calc R . .
C42 C 0.7977(2) 0.6199(2) 0.38866(15) 0.0240(5) Uani 1 1 d . . .
H42A H 0.8427 0.5978 0.3459 0.029 Uiso 1 1 calc R . .
H42B H 0.8484 0.7018 0.4218 0.029 Uiso 1 1 calc R . .
C43 C 0.6655(3) 0.6146(2) 0.34613(16) 0.0312(6) Uani 1 1 d . . .
H43A H 0.6153 0.5335 0.3135 0.047 Uiso 1 1 calc R . .
H43B H 0.6745 0.6682 0.3092 0.047 Uiso 1 1 calc R . .
H43C H 0.6220 0.6387 0.3885 0.047 Uiso 1 1 calc R . .
O1 O 1.00981(14) 0.49084(13) 0.34115(9) 0.0164(3) Uani 1 1 d . . .
O2 O 0.83231(15) 0.29400(13) 0.39624(9) 0.0170(3) Uani 1 1 d . . .
O3 O 1.06457(16) 0.31441(14) 0.38207(10) 0.0213(4) Uani 1 1 d . . .
O4 O 0.90777(14) 0.52860(13) 0.47953(9) 0.0162(3) Uani 1 1 d . . .
V1 V 0.99278(4) 0.39974(3) 0.41474(2) 0.01455(11) 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
C1 O1 1.378(2) . ?
C1 C2 1.399(3) . ?
C1 C6 1.425(3) . ?
C2 C3 1.396(3) . ?
C2 C15 1.525(3) . ?
C3 C4 1.389(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(3) . ?
C4 C11 1.542(3) . ?
C5 C6 1.396(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.535(3) . ?
C7 C10 1.538(3) . ?
C7 C8 1.541(3) . ?
C7 C9 1.543(3) . ?
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 C12B 1.514(8) . ?
C11 C14A 1.522(4) . ?
C11 C13B 1.527(8) . ?
C11 C13A 1.530(4) . ?
C11 C12A 1.545(4) . ?
C11 C14B 1.578(8) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15 C27 1.528(3) . ?
C15 C16 1.531(3) . ?
C15 H15 1.0000 . ?
C16 C17 1.392(3) . ?
C16 C21 1.396(3) . ?
C17 C18 1.402(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.388(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O2 1.386(2) . ?
C22 C27 1.406(3) . ?
C22 C23 1.421(3) . ?
C23 C24 1.398(3) . ?
C23 C32 1.542(3) . ?
C24 C25 1.399(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(3) . ?
C25 C28 1.536(3) . ?
C26 C27 1.381(3) . ?
C26 H26 0.9500 . ?
C28 C30 1.527(4) . ?
C28 C29 1.536(3) . ?
C28 C31 1.542(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C35 1.527(4) . ?
C32 C34 1.540(4) . ?
C32 C33 1.546(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C41 O4 1.451(2) . ?
C41 C42 1.514(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.532(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O1 V1 1.8117(15) . ?
O2 V1 1.8165(16) . ?
O3 V1 1.5869(15) . ?
O4 V1 1.8348(15) 2_766 ?
O4 V1 2.2917(14) . ?
V1 O4 1.8348(15) 2_766 ?

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 C1 C2 117.72(19) . . ?
O1 C1 C6 120.83(19) . . ?
C2 C1 C6 121.41(19) . . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C15 121.0(2) . . ?
C1 C2 C15 120.16(19) . . ?
C4 C3 C2 122.0(2) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 117.3(2) . . ?
C3 C4 C11 119.7(2) . . ?
C5 C4 C11 123.1(2) . . ?
C6 C5 C4 124.1(2) . . ?
C6 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C5 C6 C1 116.0(2) . . ?
C5 C6 C7 122.4(2) . . ?
C1 C6 C7 121.42(19) . . ?
C6 C7 C10 111.72(19) . . ?
C6 C7 C8 112.35(19) . . ?
C10 C7 C8 107.4(2) . . ?
C6 C7 C9 108.47(19) . . ?
C10 C7 C9 107.1(2) . . ?
C8 C7 C9 109.60(19) . . ?
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 . . ?
C12B C11 C14A 75.6(4) . . ?
C12B C11 C13B 109.3(5) . . ?
C14A C11 C13B 127.1(4) . . ?
C12B C11 C13A 137.4(4) . . ?
C14A C11 C13A 108.5(2) . . ?
C13B C11 C13A 33.8(3) . . ?
C12B C11 C4 107.5(4) . . ?
C14A C11 C4 112.9(2) . . ?
C13B C11 C4 114.9(4) . . ?
C13A C11 C4 109.1(2) . . ?
C12B C11 C12A 36.6(4) . . ?
C14A C11 C12A 108.0(2) . . ?
C13B C11 C12A 76.4(4) . . ?
C13A C11 C12A 109.4(3) . . ?
C4 C11 C12A 108.9(2) . . ?
C12B C11 C14B 108.1(5) . . ?
C14A C11 C14B 34.4(3) . . ?
C13B C11 C14B 104.7(5) . . ?
C13A C11 C14B 77.1(4) . . ?
C4 C11 C14B 112.0(4) . . ?
C12A C11 C14B 133.4(4) . . ?
C11 C12A H12A 109.5 . . ?
C11 C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11 C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C11 C13A H13A 109.5 . . ?
C11 C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C11 C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C11 C14A H14A 109.5 . . ?
C11 C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C11 C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C11 C12B H12D 109.5 . . ?
C11 C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11 C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11 C13B H13D 109.5 . . ?
C11 C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11 C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C11 C14B H14D 109.5 . . ?
C11 C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C11 C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C2 C15 C27 110.35(16) . . ?
C2 C15 C16 113.66(17) . . ?
C27 C15 C16 114.45(18) . . ?
C2 C15 H15 105.9 . . ?
C27 C15 H15 105.9 . . ?
C16 C15 H15 105.9 . . ?
C17 C16 C21 118.6(2) . . ?
C17 C16 C15 120.27(19) . . ?
C21 C16 C15 120.6(2) . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 120.3(2) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.5(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C16 120.7(2) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
O2 C22 C27 117.84(18) . . ?
O2 C22 C23 121.18(19) . . ?
C27 C22 C23 121.0(2) . . ?
C24 C23 C22 116.4(2) . . ?
C24 C23 C32 121.0(2) . . ?
C22 C23 C32 122.5(2) . . ?
C23 C24 C25 123.9(2) . . ?
C23 C24 H24 118.0 . . ?
C25 C24 H24 118.0 . . ?
C26 C25 C24 117.1(2) . . ?
C26 C25 C28 119.4(2) . . ?
C24 C25 C28 123.5(2) . . ?
C27 C26 C25 122.0(2) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C26 C27 C22 119.47(19) . . ?
C26 C27 C15 120.41(19) . . ?
C22 C27 C15 120.07(19) . . ?
C30 C28 C29 108.8(2) . . ?
C30 C28 C25 109.3(2) . . ?
C29 C28 C25 112.52(19) . . ?
C30 C28 C31 110.1(2) . . ?
C29 C28 C31 106.7(2) . . ?
C25 C28 C31 109.4(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C35 C32 C34 109.8(2) . . ?
C35 C32 C23 108.3(2) . . ?
C34 C32 C23 112.1(2) . . ?
C35 C32 C33 108.0(2) . . ?
C34 C32 C33 107.2(2) . . ?
C23 C32 C33 111.3(2) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O4 C41 C42 112.29(19) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 C43 110.4(2) . . ?
C41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
C41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C1 O1 V1 122.64(12) . . ?
C22 O2 V1 126.04(13) . . ?
C41 O4 V1 127.10(12) . 2_766 ?
C41 O4 V1 124.08(12) . . ?
V1 O4 V1 108.23(6) 2_766 . ?
O3 V1 O1 100.19(7) . . ?
O3 V1 O2 100.58(8) . . ?
O1 V1 O2 113.14(7) . . ?
O3 V1 O4 100.35(7) . 2_766 ?
O1 V1 O4 115.74(7) . 2_766 ?
O2 V1 O4 121.56(7) . 2_766 ?
O3 V1 O4 172.06(7) . . ?
O1 V1 O4 84.55(6) . . ?
O2 V1 O4 83.19(6) . . ?
O4 V1 O4 71.77(6) 2_766 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -176.53(17) . . . . ?
C6 C1 C2 C3 5.6(3) . . . . ?
O1 C1 C2 C15 4.1(3) . . . . ?
C6 C1 C2 C15 -173.75(18) . . . . ?
C1 C2 C3 C4 -1.2(3) . . . . ?
C15 C2 C3 C4 178.07(18) . . . . ?
C2 C3 C4 C5 -2.1(3) . . . . ?
C2 C3 C4 C11 178.44(18) . . . . ?
C3 C4 C5 C6 1.3(3) . . . . ?
C11 C4 C5 C6 -179.3(2) . . . . ?
C4 C5 C6 C1 2.7(3) . . . . ?
C4 C5 C6 C7 -172.7(2) . . . . ?
O1 C1 C6 C5 175.97(18) . . . . ?
C2 C1 C6 C5 -6.2(3) . . . . ?
O1 C1 C6 C7 -8.5(3) . . . . ?
C2 C1 C6 C7 169.35(19) . . . . ?
C5 C6 C7 C10 -1.0(3) . . . . ?
C1 C6 C7 C10 -176.2(2) . . . . ?
C5 C6 C7 C8 -121.8(2) . . . . ?
C1 C6 C7 C8 62.9(3) . . . . ?
C5 C6 C7 C9 116.9(2) . . . . ?
C1 C6 C7 C9 -58.4(3) . . . . ?
C3 C4 C11 C12B -100.4(4) . . . . ?
C5 C4 C11 C12B 80.2(5) . . . . ?
C3 C4 C11 C14A 178.2(2) . . . . ?
C5 C4 C11 C14A -1.2(3) . . . . ?
C3 C4 C11 C13B 21.5(5) . . . . ?
C5 C4 C11 C13B -157.9(4) . . . . ?
C3 C4 C11 C13A 57.6(3) . . . . ?
C5 C4 C11 C13A -121.9(3) . . . . ?
C3 C4 C11 C12A -61.8(3) . . . . ?
C5 C4 C11 C12A 118.7(3) . . . . ?
C3 C4 C11 C14B 140.9(4) . . . . ?
C5 C4 C11 C14B -38.5(4) . . . . ?
C3 C2 C15 C27 74.0(2) . . . . ?
C1 C2 C15 C27 -106.7(2) . . . . ?
C3 C2 C15 C16 -56.1(2) . . . . ?
C1 C2 C15 C16 123.2(2) . . . . ?
C2 C15 C16 C17 163.90(19) . . . . ?
C27 C15 C16 C17 35.8(3) . . . . ?
C2 C15 C16 C21 -24.6(3) . . . . ?
C27 C15 C16 C21 -152.63(19) . . . . ?
C21 C16 C17 C18 -1.4(3) . . . . ?
C15 C16 C17 C18 170.3(2) . . . . ?
C16 C17 C18 C19 1.0(4) . . . . ?
C17 C18 C19 C20 0.2(4) . . . . ?
C18 C19 C20 C21 -0.9(4) . . . . ?
C19 C20 C21 C16 0.5(4) . . . . ?
C17 C16 C21 C20 0.7(3) . . . . ?
C15 C16 C21 C20 -171.0(2) . . . . ?
O2 C22 C23 C24 -177.7(2) . . . . ?
C27 C22 C23 C24 3.8(3) . . . . ?
O2 C22 C23 C32 6.8(3) . . . . ?
C27 C22 C23 C32 -171.8(2) . . . . ?
C22 C23 C24 C25 -1.9(4) . . . . ?
C32 C23 C24 C25 173.7(2) . . . . ?
C23 C24 C25 C26 -2.0(4) . . . . ?
C23 C24 C25 C28 179.4(2) . . . . ?
C24 C25 C26 C27 4.3(3) . . . . ?
C28 C25 C26 C27 -177.0(2) . . . . ?
C25 C26 C27 C22 -2.6(3) . . . . ?
C25 C26 C27 C15 174.87(19) . . . . ?
O2 C22 C27 C26 179.75(19) . . . . ?
C23 C22 C27 C26 -1.7(3) . . . . ?
O2 C22 C27 C15 2.3(3) . . . . ?
C23 C22 C27 C15 -179.12(19) . . . . ?
C2 C15 C27 C26 -79.2(2) . . . . ?
C16 C15 C27 C26 50.6(3) . . . . ?
C2 C15 C27 C22 98.3(2) . . . . ?
C16 C15 C27 C22 -132.0(2) . . . . ?
C26 C25 C28 C30 -69.7(3) . . . . ?
C24 C25 C28 C30 108.8(3) . . . . ?
C26 C25 C28 C29 169.4(2) . . . . ?
C24 C25 C28 C29 -12.1(3) . . . . ?
C26 C25 C28 C31 50.9(3) . . . . ?
C24 C25 C28 C31 -130.6(2) . . . . ?
C24 C23 C32 C35 -111.9(3) . . . . ?
C22 C23 C32 C35 63.5(3) . . . . ?
C24 C23 C32 C34 126.8(2) . . . . ?
C22 C23 C32 C34 -57.9(3) . . . . ?
C24 C23 C32 C33 6.7(3) . . . . ?
C22 C23 C32 C33 -177.9(2) . . . . ?
O4 C41 C42 C43 173.62(18) . . . . ?
C2 C1 O1 V1 69.6(2) . . . . ?
C6 C1 O1 V1 -112.53(19) . . . . ?
C27 C22 O2 V1 -69.5(2) . . . . ?
C23 C22 O2 V1 111.9(2) . . . . ?
C42 C41 O4 V1 102.56(19) . . . 2_766 ?
C42 C41 O4 V1 -87.3(2) . . . . ?
C1 O1 V1 O3 32.23(17) . . . . ?
C1 O1 V1 O2 -74.02(16) . . . . ?
C1 O1 V1 O4 139.05(15) . . . 2_766 ?
C1 O1 V1 O4 -154.21(16) . . . . ?
C22 O2 V1 O3 -34.08(17) . . . . ?
C22 O2 V1 O1 71.92(16) . . . . ?
C22 O2 V1 O4 -143.31(15) . . . 2_766 ?
C22 O2 V1 O4 153.00(16) . . . . ?
C41 O4 V1 O3 -164.1(5) . . . . ?
V1 O4 V1 O3 7.6(6) 2_766 . . . ?
C41 O4 V1 O1 68.84(16) . . . . ?
V1 O4 V1 O1 -119.39(8) 2_766 . . . ?
C41 O4 V1 O2 -45.31(15) . . . . ?
V1 O4 V1 O2 126.47(8) 2_766 . . . ?
C41 O4 V1 O4 -171.77(19) . . . 2_766 ?
V1 O4 V1 O4 0.0 2_766 . . 2_766 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.075
