# 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 
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data_p-CF3diol
_database_code_depnum_ccdc_archive 'CCDC 1040815'
_audit_update_record             
;
2015-02-12 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;


_vrf_RINTA01_p-CF3diol           
;
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 25.17 degrees theta were used 
in refinements. Due to the weak scattering, there is a poor values
for Rint, while 38% of the data are observed. 

The refinement is stable and gives valuble chemical 
information. 
;


_vrf_PLAT020_p-CF3diol           
;
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 25.17 degrees theta were used 
in refinements. Due to the weak scattering, there is a poor values
for Rint, while 38% of the data are observed. 

The refinement is stable and gives valuble chemical 
information. 
;



_vrf_PLAT026_p-CF3diol           
;
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 25.17 degrees theta were used 
in refinements. Due to the weak scattering, there is a poor values
for Rint, while 38% of the data are observed. 

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         
;
C34 H53 O4 V
;

_chemical_formula_sum            'C34 H53 O4 V'
_chemical_formula_weight         576.70

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'

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

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

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

_cell_length_a                   13.886(8)
_cell_length_b                   23.550(14)
_cell_length_c                   10.938(7)
_cell_angle_alpha                90
_cell_angle_beta                 110.492(8)
_cell_angle_gamma                90
_cell_volume                     3351(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3438
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      25.1

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             1248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.329
_shelx_estimated_absorpt_T_min   0.981
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.502
_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      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating anode'
_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            37155
_diffrn_reflns_av_unetI/netI     0.2660
_diffrn_reflns_av_R_equivalents  0.3338
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.168
_diffrn_reflns_theta_max         25.171
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             5977
_reflns_number_gt                2250
_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 b29 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_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)+(0.0515P)²+5.9908P] 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         5977
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2607
_refine_ls_R_factor_gt           0.0922
_refine_ls_wR_factor_ref         0.2193
_refine_ls_wR_factor_gt          0.1574
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.1476(5) 0.6934(3) 0.2954(7) 0.0254(17) Uani 1 1 d . . . . .
C2 C 0.2457(5) 0.7051(3) 0.3827(6) 0.0213(16) Uani 1 1 d . . . . .
C3 C 0.3248(5) 0.6679(3) 0.3852(7) 0.0281(18) Uani 1 1 d . . . . .
H3 H 0.3925 0.6755 0.4435 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3079(5) 0.6205(3) 0.3058(7) 0.0292(18) Uani 1 1 d . . . . .
C5 C 0.2079(6) 0.6098(3) 0.2246(7) 0.0341(19) Uani 1 1 d . . . . .
H5 H 0.1955 0.5769 0.1710 0.041 Uiso 1 1 calc R U . . .
C6 C 0.1245(5) 0.6440(3) 0.2165(7) 0.0284(18) Uani 1 1 d . . . . .
C7 C 0.0131(5) 0.6275(3) 0.1345(8) 0.036(2) Uani 1 1 d . . . . .
C8 C 0.0097(6) 0.5696(4) 0.0689(9) 0.060(3) Uani 1 1 d . . . . .
H8A H 0.0468 0.5719 0.0076 0.089 Uiso 1 1 calc R U . . .
H8B H -0.0620 0.5590 0.0216 0.089 Uiso 1 1 calc R U . . .
H8C H 0.0420 0.5409 0.1356 0.089 Uiso 1 1 calc R U . . .
C9 C -0.0475(6) 0.6220(3) 0.2267(8) 0.045(2) Uani 1 1 d . . . . .
H9A H -0.0159 0.5927 0.2921 0.068 Uiso 1 1 calc R U . . .
H9B H -0.1186 0.6113 0.1766 0.068 Uiso 1 1 calc R U . . .
H9C H -0.0468 0.6584 0.2704 0.068 Uiso 1 1 calc R U . . .
C10 C -0.0389(6) 0.6714(4) 0.0284(8) 0.054(3) Uani 1 1 d . . . . .
H10A H -0.0486 0.7069 0.0694 0.081 Uiso 1 1 calc R U . . .
H10B H -0.1059 0.6569 -0.0280 0.081 Uiso 1 1 calc R U . . .
H10C H 0.0045 0.6785 -0.0240 0.081 Uiso 1 1 calc R U . . .
C11 C 0.3946(5) 0.5794(3) 0.3065(7) 0.0318(19) Uani 1 1 d . . . . .
C12 C 0.3752(6) 0.5215(3) 0.3581(9) 0.053(2) Uani 1 1 d . . . . .
H12A H 0.3070 0.5075 0.3042 0.079 Uiso 1 1 calc R U . . .
H12B H 0.3784 0.5255 0.4486 0.079 Uiso 1 1 calc R U . . .
H12C H 0.4277 0.4944 0.3544 0.079 Uiso 1 1 calc R U . . .
C13 C 0.3963(6) 0.5726(4) 0.1702(8) 0.051(2) Uani 1 1 d . . . . .
H13A H 0.3292 0.5589 0.1123 0.076 Uiso 1 1 calc R U . . .
H13B H 0.4496 0.5452 0.1711 0.076 Uiso 1 1 calc R U . . .
H13C H 0.4113 0.6093 0.1387 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4997(6) 0.6008(3) 0.3958(9) 0.053(3) Uani 1 1 d . . . . .
H14A H 0.5532 0.5740 0.3935 0.079 Uiso 1 1 calc R U . . .
H14B H 0.5002 0.6039 0.4853 0.079 Uiso 1 1 calc R U . . .
H14C H 0.5132 0.6381 0.3656 0.079 Uiso 1 1 calc R U . . .
C15 C 0.2688(5) 0.7560(3) 0.4741(6) 0.0255(17) Uani 1 1 d . . . . .
H15 H 0.2012 0.7705 0.4742 0.031 Uiso 1 1 calc R U . . .
C16 C 0.3310(5) 0.7389(3) 0.6148(7) 0.0348(19) Uani 1 1 d . . . . .
H16A H 0.3982 0.7243 0.6192 0.052 Uiso 1 1 calc R U . . .
H16B H 0.2939 0.7094 0.6435 0.052 Uiso 1 1 calc R U . . .
H16C H 0.3406 0.7721 0.6718 0.052 Uiso 1 1 calc R U . . .
C17 C 0.2596(5) 0.8491(3) 0.3508(7) 0.0287(18) Uani 1 1 d . . . . .
C18 C 0.3188(5) 0.8041(3) 0.4260(6) 0.0247(16) Uani 1 1 d . . . . .
C19 C 0.4231(5) 0.8046(3) 0.4515(6) 0.0282(17) Uani 1 1 d . . . . .
H19 H 0.4630 0.7735 0.4973 0.034 Uiso 1 1 calc R U . . .
C20 C 0.4730(5) 0.8490(3) 0.4129(7) 0.0331(19) Uani 1 1 d . . . . .
C21 C 0.4129(5) 0.8933(3) 0.3456(7) 0.0341(19) Uani 1 1 d . . . . .
H21 H 0.4461 0.9239 0.3197 0.041 Uiso 1 1 calc R U . . .
C22 C 0.3047(5) 0.8963(3) 0.3124(7) 0.0296(18) Uani 1 1 d . . . . .
C23 C 0.5892(5) 0.8467(3) 0.4477(8) 0.037(2) Uani 1 1 d . . . . .
C24 C 0.6160(6) 0.7958(4) 0.3778(9) 0.059(3) Uani 1 1 d . . . . .
H24A H 0.5913 0.7607 0.4051 0.089 Uiso 1 1 calc R U . . .
H24B H 0.6907 0.7937 0.4004 0.089 Uiso 1 1 calc R U . . .
H24C H 0.5831 0.8004 0.2832 0.089 Uiso 1 1 calc R U . . .
C25 C 0.6420(6) 0.8394(4) 0.5944(8) 0.057(3) Uani 1 1 d . . . . .
H25A H 0.6245 0.8715 0.6398 0.086 Uiso 1 1 calc R U . . .
H25B H 0.7166 0.8380 0.6157 0.086 Uiso 1 1 calc R U . . .
H25C H 0.6187 0.8039 0.6221 0.086 Uiso 1 1 calc R U . . .
C26 C 0.6312(6) 0.8998(3) 0.4052(10) 0.058(3) Uani 1 1 d . . . . .
H26A H 0.6003 0.9040 0.3103 0.087 Uiso 1 1 calc R U . . .
H26B H 0.7060 0.8967 0.4305 0.087 Uiso 1 1 calc R U . . .
H26C H 0.6142 0.9331 0.4475 0.087 Uiso 1 1 calc R U . . .
C27 C 0.2427(5) 0.9467(3) 0.2359(8) 0.0341(19) Uani 1 1 d . . . . .
C28 C 0.1769(6) 0.9281(3) 0.0959(8) 0.049(2) Uani 1 1 d . . . . .
H28A H 0.2222 0.9159 0.0494 0.073 Uiso 1 1 calc R U . . .
H28B H 0.1347 0.9601 0.0495 0.073 Uiso 1 1 calc R U . . .
H28C H 0.1322 0.8965 0.1001 0.073 Uiso 1 1 calc R U . . .
C29 C 0.3134(6) 0.9952(3) 0.2226(9) 0.054(2) Uani 1 1 d . . . . .
H29A H 0.3575 1.0077 0.3096 0.080 Uiso 1 1 calc R U . . .
H29B H 0.2712 1.0271 0.1756 0.080 Uiso 1 1 calc R U . . .
H29C H 0.3562 0.9814 0.1741 0.080 Uiso 1 1 calc R U . . .
C30 C 0.1736(6) 0.9714(3) 0.3055(9) 0.051(2) Uani 1 1 d . . . . .
H30A H 0.1275 0.9417 0.3157 0.077 Uiso 1 1 calc R U . . .
H30B H 0.1327 1.0027 0.2536 0.077 Uiso 1 1 calc R U . . .
H30C H 0.2163 0.9856 0.3916 0.077 Uiso 1 1 calc R U . . .
C40 C -0.1529(6) 0.8551(4) 0.1042(8) 0.048(2) Uani 1 1 d . . . . .
C41 C -0.2407(7) 0.8362(7) 0.1438(11) 0.133(6) Uani 1 1 d . . . . .
H41A H -0.2456 0.7947 0.1396 0.200 Uiso 1 1 calc R U . . .
H41B H -0.3049 0.8527 0.0846 0.200 Uiso 1 1 calc R U . . .
H41C H -0.2292 0.8488 0.2333 0.200 Uiso 1 1 calc R U . . .
C42 C -0.1699(8) 0.8381(5) -0.0310(9) 0.094(4) Uani 1 1 d . . . . .
H42A H -0.1131 0.8519 -0.0564 0.142 Uiso 1 1 calc R U . . .
H42B H -0.2347 0.8543 -0.0891 0.142 Uiso 1 1 calc R U . . .
H42C H -0.1732 0.7966 -0.0375 0.142 Uiso 1 1 calc R U . . .
C43 C -0.1404(10) 0.9179(4) 0.1235(13) 0.143(7) Uani 1 1 d . . . . .
H43A H -0.1361 0.9275 0.2124 0.214 Uiso 1 1 calc R U . . .
H43B H -0.1995 0.9373 0.0607 0.214 Uiso 1 1 calc R U . . .
H43C H -0.0773 0.9300 0.1102 0.214 Uiso 1 1 calc R U . . .
O1 O 0.0696(3) 0.73209(19) 0.2883(5) 0.0310(12) Uani 1 1 d . . . . .
O2 O 0.1547(3) 0.84715(19) 0.3227(5) 0.0319(12) Uani 1 1 d . . . . .
O3 O 0.0796(3) 0.7961(2) 0.0850(5) 0.0394(13) Uani 1 1 d . . . . .
O4 O -0.0617(3) 0.8298(2) 0.1953(5) 0.0371(13) Uani 1 1 d . . . . .
V1 V 0.05890(9) 0.80140(6) 0.21778(13) 0.0342(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 C2 1.391(9) . ?
C1 O1 1.397(8) . ?
C1 C6 1.415(9) . ?
C2 C3 1.396(9) . ?
C2 C15 1.522(9) . ?
C3 C4 1.384(9) . ?
C4 C5 1.384(9) . ?
C4 C11 1.543(9) . ?
C5 C6 1.388(9) . ?
C6 C7 1.542(9) . ?
C7 C9 1.529(10) . ?
C7 C10 1.532(10) . ?
C7 C8 1.534(10) . ?
C11 C13 1.508(10) . ?
C11 C14 1.531(10) . ?
C11 C12 1.534(10) . ?
C15 C18 1.516(9) . ?
C15 C16 1.531(9) . ?
C17 O2 1.381(8) . ?
C17 C22 1.409(10) . ?
C17 C18 1.414(10) . ?
C18 C19 1.376(8) . ?
C19 C20 1.399(10) . ?
C20 C21 1.377(10) . ?
C20 C23 1.524(10) . ?
C21 C22 1.419(9) . ?
C22 C27 1.533(10) . ?
C23 C26 1.519(10) . ?
C23 C25 1.523(11) . ?
C23 C24 1.537(11) . ?
C27 C30 1.533(10) . ?
C27 C29 1.544(10) . ?
C27 C28 1.547(10) . ?
C40 O4 1.439(8) . ?
C40 C42 1.469(12) . ?
C40 C43 1.494(12) . ?
C40 C41 1.498(13) . ?
O1 V1 1.789(5) . ?
O2 V1 1.783(5) . ?
O3 V1 1.581(5) . ?
O4 V1 1.739(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 O1 117.6(6) . . ?
C2 C1 C6 122.6(6) . . ?
O1 C1 C6 119.8(6) . . ?
C1 C2 C3 117.6(6) . . ?
C1 C2 C15 122.5(6) . . ?
C3 C2 C15 119.8(6) . . ?
C4 C3 C2 122.3(6) . . ?
C3 C4 C5 117.5(6) . . ?
C3 C4 C11 122.9(6) . . ?
C5 C4 C11 119.6(6) . . ?
C4 C5 C6 124.2(7) . . ?
C5 C6 C1 115.6(6) . . ?
C5 C6 C7 122.3(6) . . ?
C1 C6 C7 121.9(6) . . ?
C9 C7 C10 109.5(6) . . ?
C9 C7 C8 107.3(6) . . ?
C10 C7 C8 108.4(7) . . ?
C9 C7 C6 108.1(6) . . ?
C10 C7 C6 112.4(6) . . ?
C8 C7 C6 110.9(6) . . ?
C13 C11 C14 108.8(6) . . ?
C13 C11 C12 109.6(7) . . ?
C14 C11 C12 108.0(6) . . ?
C13 C11 C4 110.1(6) . . ?
C14 C11 C4 111.4(6) . . ?
C12 C11 C4 108.8(6) . . ?
C18 C15 C2 112.2(5) . . ?
C18 C15 C16 112.3(5) . . ?
C2 C15 C16 111.6(6) . . ?
O2 C17 C22 120.3(6) . . ?
O2 C17 C18 117.2(6) . . ?
C22 C17 C18 122.4(6) . . ?
C19 C18 C17 117.8(7) . . ?
C19 C18 C15 120.9(7) . . ?
C17 C18 C15 121.3(6) . . ?
C18 C19 C20 122.9(7) . . ?
C21 C20 C19 117.2(6) . . ?
C21 C20 C23 123.4(7) . . ?
C19 C20 C23 119.4(7) . . ?
C20 C21 C22 124.3(7) . . ?
C17 C22 C21 115.2(6) . . ?
C17 C22 C27 123.4(6) . . ?
C21 C22 C27 121.3(6) . . ?
C26 C23 C25 108.7(7) . . ?
C26 C23 C20 112.3(6) . . ?
C25 C23 C20 110.1(6) . . ?
C26 C23 C24 107.7(7) . . ?
C25 C23 C24 108.9(7) . . ?
C20 C23 C24 108.9(6) . . ?
C22 C27 C30 110.6(6) . . ?
C22 C27 C29 111.7(6) . . ?
C30 C27 C29 107.2(6) . . ?
C22 C27 C28 110.2(6) . . ?
C30 C27 C28 110.1(6) . . ?
C29 C27 C28 106.9(7) . . ?
O4 C40 C42 112.0(7) . . ?
O4 C40 C43 106.4(7) . . ?
C42 C40 C43 112.5(10) . . ?
O4 C40 C41 106.5(7) . . ?
C42 C40 C41 110.5(9) . . ?
C43 C40 C41 108.7(11) . . ?
C1 O1 V1 124.4(4) . . ?
C17 O2 V1 130.9(4) . . ?
C40 O4 V1 145.9(5) . . ?
O3 V1 O4 112.1(2) . . ?
O3 V1 O2 107.7(2) . . ?
O4 V1 O2 108.9(2) . . ?
O3 V1 O1 108.0(2) . . ?
O4 V1 O1 110.0(2) . . ?
O2 V1 O1 110.1(2) . . ?

_refine_diff_density_max         0.323
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.080

_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.
2015-12-18 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.
2015-12-18 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.
2015-12-18 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_8
_database_code_depnum_ccdc_archive 'CCDC 1404529'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-12-18 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_spiro1
_database_code_depnum_ccdc_archive 'CCDC 1404533'
_audit_update_record             
;
2015-06-02 deposited with the CCDC.
2015-12-18 downloaded from the CCDC.
;

_vrf_PLAT201_spiro1              
;
RESPONSE: Small-scale disorder in the position of one of the 
tbutyl groups is modelled using two orientations. As is normal
the atoms that are disordered are modelled with isotropic
displacement parameters.     
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C 64 H86 O4'
_chemical_formula_sum            'C64 H86 O4'
_chemical_formula_weight         919.32

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'

_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                   10.9672(8)
_cell_length_b                   18.3003(13)
_cell_length_c                   14.5447(10)
_cell_angle_alpha                90
_cell_angle_beta                 97.721(14)
_cell_angle_gamma                90
_cell_volume                     2892.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31114
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       'Cut Block'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_F_000             1004
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.064
_shelx_estimated_absorpt_T_min   0.992
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Implemented within Rigaku CrystalClear software. 
CrystalClear 2.1 b31
;
_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 HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            36590
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.457
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6556
_reflns_number_gt                4404
_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    
;
Superflip (Palatinus L. & Chapuis G., 2007)
;
_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)+(0.0940P)²+1.9957P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6556
_refine_ls_number_parameters     314
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0709
_refine_ls_wR_factor_ref         0.2076
_refine_ls_wR_factor_gt          0.1824
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.4703(2) 0.35326(12) 0.23774(16) 0.0297(5) Uani 1 1 d . . . . .
C2 C 0.5094(2) 0.34067(11) 0.33045(16) 0.0285(5) Uani 1 1 d . . . . .
C3 C 0.4674(2) 0.28016(12) 0.37517(17) 0.0316(5) Uani 1 1 d D . . . .
H3 H 0.4956(5) 0.2714(2) 0.4422(12) 0.038 Uiso 1 1 calc DR U . . .
C4 C 0.3852(2) 0.23189(12) 0.32478(18) 0.0331(5) Uani 1 1 d . . . . .
C5 C 0.3468(2) 0.24791(13) 0.23093(17) 0.0340(5) Uani 1 1 d D . . . .
H5 H 0.2888(11) 0.2151(6) 0.1968(7) 0.041 Uiso 1 1 calc DR U . . .
C6 C 0.3864(2) 0.30783(12) 0.18356(16) 0.0318(5) Uani 1 1 d . . . . .
C11 C 0.3451(2) 0.32208(14) 0.07946(16) 0.0350(5) Uani 1 1 d . . . . .
C7 C 0.3380(2) 0.16298(12) 0.37022(19) 0.0374(6) Uani 1 1 d . . . . .
C9A C 0.3994(4) 0.1521(2) 0.4713(3) 0.0523(6) Uiso 0.657(3) 1 d . U P A 1
H9A H 0.3846 0.1952 0.5081 0.078 Uiso 0.657(3) 1 calc R U P A 1
H9B H 0.3643 0.1089 0.4977 0.078 Uiso 0.657(3) 1 calc R U P A 1
H9C H 0.4881 0.1453 0.4721 0.078 Uiso 0.657(3) 1 calc R U P A 1
C10A C 0.2011(4) 0.1726(3) 0.3741(3) 0.0523(6) Uiso 0.657(3) 1 d . U P A 1
H10A H 0.1879 0.2164 0.4103 0.078 Uiso 0.657(3) 1 calc R U P A 1
H10B H 0.1579 0.1779 0.3110 0.078 Uiso 0.657(3) 1 calc R U P A 1
H10C H 0.1695 0.1297 0.4035 0.078 Uiso 0.657(3) 1 calc R U P A 1
C8A C 0.3618(4) 0.0965(2) 0.3154(3) 0.0523(6) Uiso 0.657(3) 1 d . U P A 1
H8A H 0.4505 0.0915 0.3139 0.078 Uiso 0.657(3) 1 calc R U P A 1
H8B H 0.3311 0.0531 0.3445 0.078 Uiso 0.657(3) 1 calc R U P A 1
H8C H 0.3195 0.1014 0.2519 0.078 Uiso 0.657(3) 1 calc R U P A 1
C9B C 0.4494(8) 0.1119(5) 0.4017(6) 0.0523(6) Uiso 0.343(3) 1 d . U P A 2
H9D H 0.4922 0.1007 0.3484 0.078 Uiso 0.343(3) 1 calc R U P A 2
H9E H 0.5062 0.1365 0.4497 0.078 Uiso 0.343(3) 1 calc R U P A 2
H9F H 0.4200 0.0665 0.4267 0.078 Uiso 0.343(3) 1 calc R U P A 2
C8B C 0.2540(8) 0.1131(5) 0.2971(6) 0.0523(6) Uiso 0.343(3) 1 d . U P A 2
H8D H 0.2990 0.1014 0.2451 0.078 Uiso 0.343(3) 1 calc R U P A 2
H8E H 0.2330 0.0678 0.3273 0.078 Uiso 0.343(3) 1 calc R U P A 2
H8F H 0.1784 0.1396 0.2738 0.078 Uiso 0.343(3) 1 calc R U P A 2
C10B C 0.2729(8) 0.1806(5) 0.4468(6) 0.0523(6) Uiso 0.343(3) 1 d . U P A 2
H10D H 0.2447 0.1354 0.4734 0.078 Uiso 0.343(3) 1 calc R U P A 2
H10E H 0.3279 0.2069 0.4942 0.078 Uiso 0.343(3) 1 calc R U P A 2
H10F H 0.2018 0.2114 0.4249 0.078 Uiso 0.343(3) 1 calc R U P A 2
C12 C 0.2862(3) 0.39908(16) 0.06678(19) 0.0458(6) Uani 1 1 d . . . . .
H12A H 0.3458 0.4359 0.0932 0.069 Uiso 1 1 calc R U . . .
H12B H 0.2130 0.4011 0.0986 0.069 Uiso 1 1 calc R U . . .
H12C H 0.2627 0.4088 0.0005 0.069 Uiso 1 1 calc R U . . .
C13 C 0.2513(3) 0.26622(17) 0.03715(19) 0.0494(7) Uani 1 1 d . . . . .
H13A H 0.2262 0.2779 -0.0284 0.074 Uiso 1 1 calc R U . . .
H13B H 0.1791 0.2675 0.0702 0.074 Uiso 1 1 calc R U . . .
H13C H 0.2880 0.2173 0.0424 0.074 Uiso 1 1 calc R U . . .
C14 C 0.4591(2) 0.31920(16) 0.02818(19) 0.0455(6) Uani 1 1 d . . . . .
H14A H 0.4969 0.2707 0.0360 0.068 Uiso 1 1 calc R U . . .
H14B H 0.5187 0.3563 0.0539 0.068 Uiso 1 1 calc R U . . .
H14C H 0.4344 0.3288 -0.0380 0.068 Uiso 1 1 calc R U . . .
C15 C 0.5960(2) 0.40058(11) 0.36958(16) 0.0298(5) Uani 1 1 d . . . . .
H15 H 0.6749 0.3785 0.3995 0.036 Uiso 1 1 calc R U . . .
C16 C 0.5448(2) 0.45068(11) 0.43796(16) 0.0292(5) Uani 1 1 d . . . . .
C17 C 0.6204(2) 0.47585(12) 0.51606(17) 0.0320(5) Uani 1 1 d D . . . .
H17 H 0.7032 0.4595 0.5279 0.038 Uiso 1 1 calc DR U . . .
C18 C 0.4237(2) 0.47542(12) 0.42307(17) 0.0333(5) Uani 1 1 d D . . . .
H18 H 0.3703 0.4587 0.3704 0.040 Uiso 1 1 calc DR U . . .
C19 C 0.7419(2) 0.41072(12) 0.25247(17) 0.0328(5) Uani 1 1 d . . . . .
C20 C 0.6183(2) 0.44044(12) 0.27424(16) 0.0317(5) Uani 1 1 d . . . . .
C21 C 0.6160(2) 0.52194(12) 0.27926(16) 0.0332(5) Uani 1 1 d D . . . .
H21 H 0.5365(15) 0.5484(5) 0.2639(3) 0.040 Uiso 1 1 calc DR U . . .
C22 C 0.7198(2) 0.55984(11) 0.30414(16) 0.0324(5) Uani 1 1 d . . . . .
C23 C 0.8371(2) 0.52038(12) 0.32060(16) 0.0327(5) Uani 1 1 d D . . . .
H23 H 0.9093(13) 0.5477(5) 0.3492(6) 0.039 Uiso 1 1 calc DR U . . .
C24 C 0.8541(2) 0.44952(12) 0.29959(15) 0.0299(5) Uani 1 1 d . . . . .
C25 C 0.7241(2) 0.64306(12) 0.31689(18) 0.0369(6) Uani 1 1 d . . . . .
C26 C 0.5957(3) 0.67679(14) 0.2979(2) 0.0498(7) Uani 1 1 d . . . . .
H26A H 0.5431 0.6559 0.3406 0.075 Uiso 1 1 calc R U . . .
H26B H 0.5600 0.6663 0.2338 0.075 Uiso 1 1 calc R U . . .
H26C H 0.6015 0.7298 0.3071 0.075 Uiso 1 1 calc R U . . .
C27 C 0.7766(3) 0.66191(15) 0.4168(2) 0.0560(8) Uani 1 1 d . . . . .
H27A H 0.7240 0.6409 0.4594 0.084 Uiso 1 1 calc R U . . .
H27B H 0.7797 0.7151 0.4244 0.084 Uiso 1 1 calc R U . . .
H27C H 0.8598 0.6418 0.4308 0.084 Uiso 1 1 calc R U . . .
C28 C 0.8056(3) 0.67630(14) 0.2496(2) 0.0536(8) Uani 1 1 d . . . . .
H28A H 0.8067 0.7296 0.2561 0.080 Uiso 1 1 calc R U . . .
H28B H 0.7726 0.6631 0.1858 0.080 Uiso 1 1 calc R U . . .
H28C H 0.8896 0.6573 0.2641 0.080 Uiso 1 1 calc R U . . .
C29 C 0.9764(2) 0.40937(12) 0.31669(18) 0.0351(5) Uani 1 1 d . . . . .
C30 C 0.9578(2) 0.33977(13) 0.37286(19) 0.0398(6) Uani 1 1 d . . . . .
H30A H 0.9372 0.3535 0.4341 0.060 Uiso 1 1 calc R U . . .
H30B H 1.0337 0.3109 0.3803 0.060 Uiso 1 1 calc R U . . .
H30C H 0.8906 0.3107 0.3399 0.060 Uiso 1 1 calc R U . . .
C31 C 1.0222(3) 0.38974(15) 0.2252(2) 0.0475(7) Uani 1 1 d . . . . .
H31A H 0.9618 0.3582 0.1886 0.071 Uiso 1 1 calc R U . . .
H31B H 1.1010 0.3639 0.2379 0.071 Uiso 1 1 calc R U . . .
H31C H 1.0334 0.4345 0.1903 0.071 Uiso 1 1 calc R U . . .
C32 C 1.0751(2) 0.45584(14) 0.3746(2) 0.0438(6) Uani 1 1 d . . . . .
H32A H 1.0914 0.4998 0.3397 0.066 Uiso 1 1 calc R U . . .
H32B H 1.1510 0.4273 0.3883 0.066 Uiso 1 1 calc R U . . .
H32C H 1.0459 0.4701 0.4328 0.066 Uiso 1 1 calc R U . . .
O1 O 0.52033(15) 0.41580(8) 0.20463(11) 0.0340(4) Uani 1 1 d . . . . .
O2 O 0.74610(16) 0.35716(9) 0.20327(13) 0.0414(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 C2 1.378(3) . ?
C1 O1 1.383(3) . ?
C1 C6 1.402(3) . ?
C2 C3 1.394(3) . ?
C2 C15 1.511(3) . ?
C3 C4 1.397(3) . ?
C4 C5 1.404(3) . ?
C4 C7 1.545(3) . ?
C5 C6 1.395(3) . ?
C6 C11 1.543(3) . ?
C11 C13 1.521(3) . ?
C11 C14 1.541(4) . ?
C11 C12 1.551(4) . ?
C7 C10B 1.438(9) . ?
C7 C8A 1.497(5) . ?
C7 C10A 1.519(5) . ?
C7 C9A 1.545(5) . ?
C7 C9B 1.557(9) . ?
C7 C8B 1.597(9) . ?
C15 C16 1.515(3) . ?
C15 C20 1.614(3) . ?
C16 C17 1.391(3) . ?
C16 C18 1.393(3) . ?
C17 C18 1.388(3) 3_666 ?
C18 C17 1.388(3) 3_666 ?
C19 O2 1.218(3) . ?
C19 C24 1.504(3) . ?
C19 C20 1.533(3) . ?
C20 O1 1.446(3) . ?
C20 C21 1.494(3) . ?
C21 C22 1.341(3) . ?
C22 C23 1.467(3) . ?
C22 C25 1.534(3) . ?
C23 C24 1.351(3) . ?
C24 C29 1.520(3) . ?
C25 C26 1.528(4) . ?
C25 C27 1.529(4) . ?
C25 C28 1.537(4) . ?
C29 C31 1.528(4) . ?
C29 C32 1.536(3) . ?
C29 C30 1.541(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
C2 C1 O1 113.16(19) . . ?
C2 C1 C6 123.0(2) . . ?
O1 C1 C6 123.8(2) . . ?
C1 C2 C3 120.7(2) . . ?
C1 C2 C15 110.13(19) . . ?
C3 C2 C15 129.1(2) . . ?
C2 C3 C4 119.2(2) . . ?
C3 C4 C5 117.8(2) . . ?
C3 C4 C7 121.4(2) . . ?
C5 C4 C7 120.8(2) . . ?
C6 C5 C4 124.8(2) . . ?
C5 C6 C1 114.4(2) . . ?
C5 C6 C11 123.2(2) . . ?
C1 C6 C11 122.4(2) . . ?
C13 C11 C14 109.3(2) . . ?
C13 C11 C6 112.1(2) . . ?
C14 C11 C6 108.6(2) . . ?
C13 C11 C12 108.3(2) . . ?
C14 C11 C12 109.0(2) . . ?
C6 C11 C12 109.44(19) . . ?
C8A C7 C10A 111.0(3) . . ?
C8A C7 C9A 108.5(3) . . ?
C10A C7 C9A 106.6(3) . . ?
C10B C7 C4 112.2(4) . . ?
C8A C7 C4 110.0(3) . . ?
C10A C7 C4 108.1(2) . . ?
C9A C7 C4 112.6(2) . . ?
C10B C7 C9B 111.0(5) . . ?
C4 C7 C9B 108.7(4) . . ?
C10B C7 C8B 110.0(5) . . ?
C4 C7 C8B 112.2(4) . . ?
C9B C7 C8B 102.3(5) . . ?
C2 C15 C16 114.63(18) . . ?
C2 C15 C20 99.46(17) . . ?
C16 C15 C20 113.75(17) . . ?
C17 C16 C18 118.0(2) . . ?
C17 C16 C15 120.3(2) . . ?
C18 C16 C15 121.6(2) . . ?
C18 C17 C16 120.9(2) 3_666 . ?
C17 C18 C16 121.1(2) 3_666 . ?
O2 C19 C24 123.7(2) . . ?
O2 C19 C20 120.8(2) . . ?
C24 C19 C20 115.50(19) . . ?
O1 C20 C21 109.27(18) . . ?
O1 C20 C19 109.84(18) . . ?
C21 C20 C19 112.66(19) . . ?
O1 C20 C15 106.06(17) . . ?
C21 C20 C15 113.81(18) . . ?
C19 C20 C15 104.92(18) . . ?
C22 C21 C20 120.7(2) . . ?
C21 C22 C23 118.9(2) . . ?
C21 C22 C25 123.8(2) . . ?
C23 C22 C25 117.2(2) . . ?
C24 C23 C22 125.4(2) . . ?
C23 C24 C19 115.3(2) . . ?
C23 C24 C29 124.9(2) . . ?
C19 C24 C29 119.75(19) . . ?
C26 C25 C27 107.5(2) . . ?
C26 C25 C22 111.5(2) . . ?
C27 C25 C22 109.9(2) . . ?
C26 C25 C28 109.0(2) . . ?
C27 C25 C28 109.8(2) . . ?
C22 C25 C28 109.1(2) . . ?
C24 C29 C31 111.0(2) . . ?
C24 C29 C32 111.32(19) . . ?
C31 C29 C32 108.5(2) . . ?
C24 C29 C30 108.03(19) . . ?
C31 C29 C30 110.5(2) . . ?
C32 C29 C30 107.5(2) . . ?
C1 O1 C20 107.83(17) . . ?

_refine_diff_density_max         0.417
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.055

