# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_w

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H48 Cl0 N3 O4 V'
_chemical_formula_sum            'C33 H48 Cl0 N3 O4 V'
_chemical_formula_weight         601.68

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

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   40.3177(11)
_cell_length_b                   40.3177(11)
_cell_length_c                   11.1035(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     15630.8(10)
_cell_formula_units_Z            18
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    3780
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      20.68

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5796
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8846
_exptl_absorpt_correction_T_max  0.9413
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31181
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6143
_reflns_number_gt                4687
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.012 565 41 ' '
2 0.029 0.412 0.750 7 0 ' '
3 0.049 0.304 0.083 7 0 ' '
4 0.078 0.716 0.583 7 0 ' '
5 0.333 0.667 0.164 566 41 ' '
6 0.255 0.951 0.083 7 0 ' '
7 0.284 0.363 0.583 7 0 ' '
8 0.304 0.255 0.917 7 0 ' '
9 0.363 0.078 0.417 7 0 ' '
10 0.382 0.971 0.750 7 0 ' '
11 0.412 0.382 0.250 7 0 ' '
12 0.667 0.333 0.831 566 41 ' '
13 0.588 0.618 0.750 7 0 ' '
14 0.618 0.029 0.250 7 0 ' '
15 0.637 0.922 0.583 7 0 ' '
16 0.696 0.745 0.083 7 0 ' '
17 0.716 0.637 0.417 7 0 ' '
18 0.745 0.049 0.917 7 0 ' '
19 0.922 0.284 0.417 7 0 ' '
20 0.951 0.696 0.917 7 0 ' '
21 0.971 0.588 0.250 7 0 ' '
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0684P)²+23.2861P] 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         6143
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1479
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.053812(14) 0.801081(14) 0.72331(4) 0.02789(16) Uani 1 1 d . . .
O2 O 0.07604(6) 0.85052(5) 0.79441(17) 0.0297(5) Uani 1 1 d . . .
O3 O 0.03429(6) 0.74924(6) 0.71645(18) 0.0328(5) Uani 1 1 d . . .
O4 O 0.09635(6) 0.81170(6) 0.63822(18) 0.0354(5) Uani 1 1 d . . .
N1 N 0.08148(7) 0.78880(7) 0.9004(2) 0.0263(5) Uani 1 1 d . . .
O1 O 0.02526(6) 0.80354(6) 0.62854(19) 0.0376(5) Uani 1 1 d . . .
N2 N 0.01154(7) 0.78536(7) 0.8691(2) 0.0276(6) Uani 1 1 d . . .
N3 N 0.09646(7) 0.71936(7) 0.9895(2) 0.0316(6) Uani 1 1 d . . .
C5 C 0.07669(8) 0.86291(8) 0.9074(3) 0.0282(7) Uani 1 1 d . . .
C15 C 0.11955(8) 0.75541(8) 0.9520(3) 0.0276(7) Uani 1 1 d . . .
C10 C 0.01656(8) 0.77144(8) 0.9728(3) 0.0280(7) Uani 1 1 d . . .
C3 C 0.10739(9) 0.82463(9) 0.9669(3) 0.0321(7) Uani 1 1 d . . .
H3A H 0.1302 0.8405 0.9165 0.039 Uiso 1 1 calc R . .
H3B H 0.1163 0.8179 1.0413 0.039 Uiso 1 1 calc R . .
C1 C 0.10329(9) 0.77035(9) 0.8576(3) 0.0305(7) Uani 1 1 d . . .
H1A H 0.1248 0.7891 0.8073 0.037 Uiso 1 1 calc R . .
H1B H 0.0863 0.7487 0.8047 0.037 Uiso 1 1 calc R . .
C14 C -0.01874(9) 0.79061(9) 0.8595(3) 0.0360(8) Uani 1 1 d . . .
H14 H -0.0225 0.8002 0.7857 0.043 Uiso 1 1 calc R . .
C31 C -0.00369(8) 0.72033(8) 0.6932(3) 0.0322(7) Uani 1 1 d . . .
H31A H -0.0162 0.7304 0.6394 0.039 Uiso 1 1 calc R . .
H31B H -0.0183 0.7122 0.7696 0.039 Uiso 1 1 calc R . .
C9 C 0.08549(8) 0.85599(9) 1.1197(3) 0.0332(7) Uani 1 1 d . . .
H9 H 0.0937 0.8455 1.1817 0.040 Uiso 1 1 calc R . .
C4 C 0.08901(8) 0.84798(8) 1.0004(3) 0.0293(7) Uani 1 1 d . . .
C32 C -0.00376(10) 0.68652(9) 0.6347(3) 0.0423(8) Uani 1 1 d . . .
H32A H 0.0115 0.6950 0.5596 0.051 Uiso 1 1 calc R . .
H32B H 0.0085 0.6764 0.6895 0.051 Uiso 1 1 calc R . .
C6 C 0.06526(8) 0.88978(8) 0.9342(3) 0.0318(7) Uani 1 1 d . . .
C20 C 0.05821(10) 0.91188(9) 0.8345(3) 0.0399(8) Uani 1 1 d . . .
C12 C -0.03866(10) 0.76933(10) 1.0583(3) 0.0474(9) Uani 1 1 d . . .
H12 H -0.0555 0.7643 1.1243 0.057 Uiso 1 1 calc R . .
C16 C 0.15711(9) 0.77707(9) 0.9914(3) 0.0323(7) Uani 1 1 d . . .
H16 H 0.1728 0.8026 0.9635 0.039 Uiso 1 1 calc R . .
C2 C 0.04874(8) 0.76274(8) 0.9761(3) 0.0292(7) Uani 1 1 d . . .
H2A H 0.0576 0.7646 1.0603 0.035 Uiso 1 1 calc R . .
H2B H 0.0390 0.7361 0.9486 0.035 Uiso 1 1 calc R . .
C11 C -0.00803(10) 0.76332(10) 1.0686(3) 0.0398(8) Uani 1 1 d . . .
H11 H -0.0039 0.7536 1.1415 0.048 Uiso 1 1 calc R . .
C7 C 0.06187(9) 0.89638(9) 1.0559(3) 0.0350(8) Uani 1 1 d . . .
H7 H 0.0533 0.9138 1.0753 0.042 Uiso 1 1 calc R . .
C19 C 0.11113(9) 0.70478(9) 1.0669(3) 0.0366(8) Uani 1 1 d . . .
H19 H 0.0951 0.6792 1.0936 0.044 Uiso 1 1 calc R . .
C13 C -0.04443(9) 0.78280(10) 0.9509(3) 0.0435(9) Uani 1 1 d . . .
H13 H -0.0657 0.7866 0.9405 0.052 Uiso 1 1 calc R . .
C17 C 0.17130(10) 0.76118(10) 1.0716(3) 0.0408(8) Uani 1 1 d . . .
H17 H 0.1969 0.7755 1.0997 0.049 Uiso 1 1 calc R . .
C8 C 0.07020(8) 0.87911(9) 1.1505(3) 0.0333(7) Uani 1 1 d . . .
C18 C 0.14799(10) 0.72447(10) 1.1103(3) 0.0399(8) Uani 1 1 d . . .
H18 H 0.1570 0.7128 1.1658 0.048 Uiso 1 1 calc R . .
C33 C -0.04389(12) 0.65512(10) 0.6057(4) 0.0616(12) Uani 1 1 d . . .
H33A H -0.0586 0.6457 0.6804 0.092 Uiso 1 1 calc R . .
H33B H -0.0429 0.6341 0.5652 0.092 Uiso 1 1 calc R . .
H33C H -0.0562 0.6652 0.5528 0.092 Uiso 1 1 calc R . .
C24 C 0.06360(10) 0.88503(10) 1.2831(3) 0.0409(8) Uani 1 1 d . . .
C22 C 0.09363(11) 0.93157(11) 0.7537(3) 0.0539(10) Uani 1 1 d . . .
H22A H 0.1157 0.9499 0.8014 0.081 Uiso 1 1 calc R . .
H22B H 0.0890 0.9451 0.6883 0.081 Uiso 1 1 calc R . .
H22C H 0.0990 0.9123 0.7196 0.081 Uiso 1 1 calc R . .
C28 C 0.09608(12) 0.79398(12) 0.5286(3) 0.0590(11) Uani 1 1 d . . .
H28A H 0.0881 0.8052 0.4631 0.071 Uiso 1 1 calc R . .
H28B H 0.0769 0.7664 0.5335 0.071 Uiso 1 1 calc R . .
C21 C 0.02337(12) 0.88500(11) 0.7581(4) 0.0581(11) Uani 1 1 d . . .
H21A H 0.0191 0.8999 0.6964 0.087 Uiso 1 1 calc R . .
H21B H 0.0007 0.8721 0.8098 0.087 Uiso 1 1 calc R . .
H21C H 0.0280 0.8659 0.7192 0.087 Uiso 1 1 calc R . .
C25 C 0.04510(12) 0.91049(13) 1.2969(4) 0.0610(11) Uani 1 1 d . . .
H25A H 0.0408 0.9130 1.3825 0.091 Uiso 1 1 calc R . .
H25B H 0.0206 0.8987 1.2541 0.091 Uiso 1 1 calc R . .
H25C H 0.0622 0.9359 1.2629 0.091 Uiso 1 1 calc R . .
C23 C 0.05127(13) 0.94353(11) 0.8851(4) 0.0622(11) Uani 1 1 d . . .
H23A H 0.0728 0.9606 0.9369 0.093 Uiso 1 1 calc R . .
H23B H 0.0275 0.9318 0.9323 0.093 Uiso 1 1 calc R . .
H23C H 0.0491 0.9582 0.8184 0.093 Uiso 1 1 calc R . .
C26 C 0.10161(12) 0.90563(15) 1.3489(4) 0.0756(15) Uani 1 1 d . . .
H26A H 0.1146 0.8907 1.3424 0.113 Uiso 1 1 calc R . .
H26B H 0.0971 0.9086 1.4340 0.113 Uiso 1 1 calc R . .
H26C H 0.1176 0.9310 1.3129 0.113 Uiso 1 1 calc R . .
C27 C 0.03539(14) 0.84606(13) 1.3378(4) 0.0728(13) Uani 1 1 d . . .
H27A H 0.0469 0.8296 1.3377 0.109 Uiso 1 1 calc R . .
H27B H 0.0118 0.8340 1.2900 0.109 Uiso 1 1 calc R . .
H27C H 0.0294 0.8496 1.4207 0.109 Uiso 1 1 calc R . .
C29 C 0.13404(14) 0.79838(16) 0.4980(5) 0.0923(18) Uani 1 1 d . . .
H29A H 0.1527 0.8261 0.4901 0.111 Uiso 1 1 calc R . .
H29B H 0.1424 0.7887 0.5667 0.111 Uiso 1 1 calc R . .
C30 C 0.13613(14) 0.77915(15) 0.3881(5) 0.0918(17) Uani 1 1 d . . .
H30A H 0.1223 0.7514 0.4008 0.138 Uiso 1 1 calc R . .
H30B H 0.1630 0.7878 0.3693 0.138 Uiso 1 1 calc R . .
H30C H 0.1245 0.7854 0.3210 0.138 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.599(2) . ?
V1 O4 1.812(2) . ?
V1 O3 1.830(2) . ?
V1 O2 1.901(2) . ?
V1 N2 2.201(2) . ?
V1 N1 2.430(2) . ?
O2 C5 1.346(3) . ?
O3 C31 1.409(3) . ?
O4 C28 1.409(4) . ?
N1 C2 1.472(4) . ?
N1 C1 1.486(4) . ?
N1 C3 1.488(4) . ?
N2 C10 1.340(4) . ?
N2 C14 1.343(4) . ?
N3 C19 1.334(4) . ?
N3 C15 1.341(4) . ?
C5 C4 1.405(4) . ?
C5 C6 1.405(4) . ?
C15 C16 1.388(4) . ?
C15 C1 1.512(4) . ?
C10 C11 1.377(4) . ?
C10 C2 1.505(4) . ?
C3 C4 1.507(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C14 C13 1.370(5) . ?
C14 H14 0.9500 . ?
C31 C32 1.509(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C9 C4 1.388(4) . ?
C9 C8 1.393(4) . ?
C9 H9 0.9500 . ?
C32 C33 1.508(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C6 C7 1.397(4) . ?
C6 C20 1.534(4) . ?
C20 C22 1.530(5) . ?
C20 C21 1.531(5) . ?
C20 C23 1.543(5) . ?
C12 C13 1.378(5) . ?
C12 C11 1.377(5) . ?
C12 H12 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H16 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C11 H11 0.9500 . ?
C7 C8 1.391(4) . ?
C7 H7 0.9500 . ?
C19 C18 1.375(5) . ?
C19 H19 0.9500 . ?
C13 H13 0.9500 . ?
C17 C18 1.367(5) . ?
C17 H17 0.9500 . ?
C8 C24 1.536(4) . ?
C18 H18 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C24 C26 1.517(5) . ?
C24 C27 1.531(5) . ?
C24 C25 1.549(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C28 C29 1.490(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 C30 1.470(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O4 105.55(11) . . ?
O1 V1 O3 97.56(10) . . ?
O4 V1 O3 93.66(10) . . ?
O1 V1 O2 100.66(10) . . ?
O4 V1 O2 94.27(9) . . ?
O3 V1 O2 157.37(9) . . ?
O1 V1 N2 91.36(10) . . ?
O4 V1 N2 163.05(9) . . ?
O3 V1 N2 82.70(9) . . ?
O2 V1 N2 83.56(9) . . ?
O1 V1 N1 164.37(10) . . ?
O4 V1 N1 89.62(9) . . ?
O3 V1 N1 77.29(9) . . ?
O2 V1 N1 81.60(8) . . ?
N2 V1 N1 73.43(8) . . ?
C5 O2 V1 133.46(17) . . ?
C31 O3 V1 128.42(18) . . ?
C28 O4 V1 124.4(2) . . ?
C2 N1 C1 111.7(2) . . ?
C2 N1 C3 110.7(2) . . ?
C1 N1 C3 109.9(2) . . ?
C2 N1 V1 105.58(16) . . ?
C1 N1 V1 106.88(17) . . ?
C3 N1 V1 112.00(17) . . ?
C10 N2 C14 118.2(3) . . ?
C10 N2 V1 119.68(19) . . ?
C14 N2 V1 122.0(2) . . ?
C19 N3 C15 117.2(3) . . ?
O2 C5 C4 118.1(3) . . ?
O2 C5 C6 122.1(3) . . ?
C4 C5 C6 119.8(3) . . ?
N3 C15 C16 122.1(3) . . ?
N3 C15 C1 116.3(3) . . ?
C16 C15 C1 121.5(3) . . ?
N2 C10 C11 121.5(3) . . ?
N2 C10 C2 116.5(3) . . ?
C11 C10 C2 121.9(3) . . ?
N1 C3 C4 113.8(2) . . ?
N1 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N1 C1 C15 117.5(2) . . ?
N1 C1 H1A 107.9 . . ?
C15 C1 H1A 107.9 . . ?
N1 C1 H1B 107.9 . . ?
C15 C1 H1B 107.9 . . ?
H1A C1 H1B 107.2 . . ?
N2 C14 C13 123.2(3) . . ?
N2 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
O3 C31 C32 109.7(3) . . ?
O3 C31 H31A 109.7 . . ?
C32 C31 H31A 109.7 . . ?
O3 C31 H31B 109.7 . . ?
C32 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C4 C9 C8 121.4(3) . . ?
C4 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C4 C5 120.2(3) . . ?
C9 C4 C3 121.4(3) . . ?
C5 C4 C3 118.4(3) . . ?
C33 C32 C31 111.5(3) . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C7 C6 C5 116.9(3) . . ?
C7 C6 C20 121.5(3) . . ?
C5 C6 C20 121.5(3) . . ?
C22 C20 C21 109.3(3) . . ?
C22 C20 C6 109.2(3) . . ?
C21 C20 C6 111.1(3) . . ?
C22 C20 C23 107.0(3) . . ?
C21 C20 C23 107.8(3) . . ?
C6 C20 C23 112.3(3) . . ?
C13 C12 C11 119.0(3) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C17 C16 C15 119.2(3) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
N1 C2 C10 112.9(2) . . ?
N1 C2 H2A 109.0 . . ?
C10 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C10 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C8 C7 C6 124.3(3) . . ?
C8 C7 H7 117.8 . . ?
C6 C7 H7 117.8 . . ?
N3 C19 C18 124.1(3) . . ?
N3 C19 H19 118.0 . . ?
C18 C19 H19 118.0 . . ?
C14 C13 C12 118.3(3) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C9 C8 C7 116.6(3) . . ?
C9 C8 C24 120.6(3) . . ?
C7 C8 C24 122.8(3) . . ?
C17 C18 C19 118.3(3) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C24 C27 113.5(4) . . ?
C26 C24 C8 109.9(3) . . ?
C27 C24 C8 108.6(3) . . ?
C26 C24 C25 106.2(3) . . ?
C27 C24 C25 106.5(3) . . ?
C8 C24 C25 112.1(3) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C28 C29 112.9(3) . . ?
O4 C28 H28A 109.0 . . ?
C29 C28 H28A 109.0 . . ?
O4 C28 H28B 109.0 . . ?
C29 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 C29 C28 116.9(4) . . ?
C30 C29 H29A 108.1 . . ?
C28 C29 H29A 108.1 . . ?
C30 C29 H29B 108.1 . . ?
C28 C29 H29B 108.1 . . ?
H29A C29 H29B 107.3 . . ?
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 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.058

_database_code_depnum_ccdc_archive 'CCDC 994166'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_w2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H37 N2 O5 V'
_chemical_formula_sum            'C28 H37 N2 O5 V'
_chemical_formula_weight         532.54

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   14.0405(7)
_cell_length_b                   16.1686(8)
_cell_length_c                   25.3609(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.070(1)
_cell_angle_gamma                90.00
_cell_volume                     5532.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    5246
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      22.70

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_T_max  0.9355
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33307
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         26.05
_reflns_number_total             10929
_reflns_number_gt                7309
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0774P)²+2.4526P] 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         10929
_refine_ls_number_parameters     729
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1695
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V -0.01956(4) 0.19553(4) 0.87759(2) 0.04015(17) Uani 1 1 d . A .
V2 V 0.49715(4) 0.32698(4) 0.89115(2) 0.04256(18) Uani 1 1 d . B .
N1 N 0.11321(18) 0.13040(16) 0.84825(11) 0.0376(6) Uani 1 1 d . . .
N2 N 0.05265(18) 0.29454(15) 0.84350(11) 0.0366(6) Uani 1 1 d . . .
N3 N 0.61622(18) 0.40348(15) 0.85662(10) 0.0340(6) Uani 1 1 d . . .
N4 N 0.56654(18) 0.23607(16) 0.85018(10) 0.0366(6) Uani 1 1 d . . .
O1 O -0.09704(17) 0.25534(15) 0.89431(10) 0.0511(6) Uani 1 1 d . . .
O2 O -0.08769(15) 0.18747(14) 0.80070(9) 0.0415(5) Uani 1 1 d . . .
O3 O 0.08380(17) 0.21056(15) 0.93834(9) 0.0478(6) Uani 1 1 d D . .
O4 O -0.05570(18) 0.09340(15) 0.89313(10) 0.0542(6) Uani 1 1 d . . .
O5 O -0.17139(17) 0.30333(15) 0.72745(10) 0.0511(6) Uani 1 1 d . . .
O6 O 0.42701(18) 0.26221(16) 0.90982(11) 0.0586(7) Uani 1 1 d . . .
O7 O 0.41712(15) 0.33694(14) 0.81569(9) 0.0442(6) Uani 1 1 d . . .
O8 O 0.45996(17) 0.42534(15) 0.91123(10) 0.0549(7) Uani 1 1 d D . .
O9 O 0.60885(17) 0.31160(14) 0.94768(9) 0.0461(6) Uani 1 1 d . . .
O10 O 0.33576(17) 0.22161(15) 0.74130(10) 0.0527(6) Uani 1 1 d . . .
C1 C 0.1582(2) 0.0665(2) 0.89000(14) 0.0443(8) Uani 1 1 d . . .
H1A H 0.1078 0.0232 0.8888 0.053 Uiso 1 1 calc R . .
H1B H 0.1732 0.0927 0.9267 0.053 Uiso 1 1 calc R . .
C2 C 0.1852(2) 0.19704(18) 0.84687(14) 0.0372(7) Uani 1 1 d . . .
H2A H 0.2243 0.1809 0.8215 0.045 Uiso 1 1 calc R . .
H2B H 0.2316 0.2035 0.8839 0.045 Uiso 1 1 calc R . .
C3 C 0.0738(2) 0.0907(2) 0.79341(14) 0.0429(8) Uani 1 1 d . . .
H3A H 0.0262 0.0469 0.7964 0.051 Uiso 1 1 calc R . .
H3B H 0.1293 0.0638 0.7831 0.051 Uiso 1 1 calc R . .
C4 C 0.0231(2) 0.14914(19) 0.74864(13) 0.0378(7) Uani 1 1 d . . .
C5 C -0.0556(2) 0.1959(2) 0.75628(13) 0.0385(7) Uani 1 1 d . . .
C6 C -0.0992(2) 0.2552(2) 0.71593(14) 0.0427(8) Uani 1 1 d . . .
C7 C -0.0697(2) 0.2615(2) 0.66815(14) 0.0469(8) Uani 1 1 d . . .
H7 H -0.1005 0.3011 0.6411 0.056 Uiso 1 1 calc R . .
C8 C 0.0043(3) 0.2105(2) 0.65941(15) 0.0479(9) Uani 1 1 d . . .
C9 C 0.0507(2) 0.1560(2) 0.70011(14) 0.0456(8) Uani 1 1 d . . .
H9 H 0.1028 0.1222 0.6950 0.055 Uiso 1 1 calc R . .
C10 C 0.1353(2) 0.27802(19) 0.82878(13) 0.0352(7) Uani 1 1 d . . .
C11 C 0.1760(2) 0.3359(2) 0.80104(14) 0.0448(8) Uani 1 1 d . . .
H11 H 0.2349 0.3235 0.7911 0.054 Uiso 1 1 calc R . .
C12 C 0.1303(3) 0.4116(2) 0.78792(15) 0.0516(9) Uani 1 1 d . . .
H12 H 0.1571 0.4518 0.7687 0.062 Uiso 1 1 calc R . .
C13 C 0.0456(3) 0.4280(2) 0.80302(15) 0.0490(9) Uani 1 1 d . . .
H13 H 0.0132 0.4799 0.7946 0.059 Uiso 1 1 calc R . .
C14 C 0.0085(2) 0.3685(2) 0.83038(14) 0.0432(8) Uani 1 1 d . . .
H14 H -0.0506 0.3799 0.8404 0.052 Uiso 1 1 calc R . .
C15 C 0.2515(2) 0.0246(2) 0.88490(14) 0.0434(8) Uani 1 1 d . . .
C16 C 0.2468(3) -0.0457(2) 0.85290(16) 0.0585(10) Uani 1 1 d . . .
H16 H 0.1841 -0.0672 0.8331 0.070 Uiso 1 1 calc R . .
C17 C 0.3326(4) -0.0847(3) 0.8497(2) 0.0792(14) Uani 1 1 d . . .
H17 H 0.3289 -0.1318 0.8268 0.095 Uiso 1 1 calc R . .
C18 C 0.4232(4) -0.0554(3) 0.8794(2) 0.0842(16) Uani 1 1 d . . .
H18 H 0.4820 -0.0825 0.8772 0.101 Uiso 1 1 calc R . .
C19 C 0.4294(3) 0.0129(3) 0.9125(2) 0.0730(13) Uani 1 1 d . . .
H19 H 0.4922 0.0328 0.9333 0.088 Uiso 1 1 calc R . .
C20 C 0.3435(3) 0.0526(2) 0.91518(16) 0.0558(10) Uani 1 1 d . . .
H20 H 0.3477 0.0997 0.9381 0.067 Uiso 1 1 calc R . .
C21 C -0.2023(3) 0.3745(3) 0.69397(19) 0.0751(13) Uani 1 1 d . . .
H21A H -0.2390 0.3571 0.6569 0.113 Uiso 1 1 calc R . .
H21B H -0.1441 0.4066 0.6923 0.113 Uiso 1 1 calc R . .
H21C H -0.2452 0.4087 0.7097 0.113 Uiso 1 1 calc R . .
C22 C 0.0328(3) 0.2145(3) 0.60577(16) 0.0693(12) Uani 1 1 d . . .
H22A H 0.0087 0.1648 0.5840 0.104 Uiso 1 1 calc R . .
H22B H 0.1051 0.2175 0.6137 0.104 Uiso 1 1 calc R . .
H22C H 0.0030 0.2636 0.5851 0.104 Uiso 1 1 calc R . .
C23 C 0.0885(11) 0.2532(8) 0.9870(5) 0.095(5) Uani 0.50 1 d PDU A 1
H23A H 0.0940 0.2137 1.0175 0.114 Uiso 0.50 1 calc PR A 1
H23B H 0.0281 0.2870 0.9828 0.114 Uiso 0.50 1 calc PR A 1
C23' C 0.0916(8) 0.2829(7) 0.9729(4) 0.062(3) Uani 0.50 1 d PDU A 2
H23C H 0.0288 0.2932 0.9824 0.074 Uiso 0.50 1 calc PR A 2
H23D H 0.1087 0.3326 0.9547 0.074 Uiso 0.50 1 calc PR A 2
C24 C 0.1825(10) 0.3100(7) 0.9989(5) 0.118(5) Uani 0.50 1 d PD A 1
H24A H 0.1941 0.3331 0.9650 0.142 Uiso 0.50 1 calc PR A 1
H24B H 0.1809 0.3550 1.0251 0.142 Uiso 0.50 1 calc PR A 1
C24' C 0.1769(6) 0.2602(8) 1.0252(3) 0.082(3) Uani 0.50 1 d PD A 2
H24C H 0.1742 0.2969 1.0560 0.098 Uiso 0.50 1 calc PR A 2
H24D H 0.1689 0.2023 1.0361 0.098 Uiso 0.50 1 calc PR A 2
C25 C 0.2566(13) 0.2412(10) 1.0246(8) 0.135(7) Uani 0.50 1 d PDU A 1
H25A H 0.3215 0.2658 1.0419 0.203 Uiso 0.50 1 calc PR A 1
H25B H 0.2624 0.2025 0.9959 0.203 Uiso 0.50 1 calc PR A 1
H25C H 0.2329 0.2116 1.0522 0.203 Uiso 0.50 1 calc PR A 1
C25' C 0.2752(9) 0.2701(13) 1.0127(7) 0.114(5) Uani 0.50 1 d PDU A 2
H25D H 0.3079 0.3204 1.0303 0.171 Uiso 0.50 1 calc PR A 2
H25E H 0.2644 0.2741 0.9729 0.171 Uiso 0.50 1 calc PR A 2
H25F H 0.3172 0.2221 1.0267 0.171 Uiso 0.50 1 calc PR A 2
C26 C -0.1464(8) 0.0677(7) 0.8984(5) 0.089(4) Uani 0.50 1 d PD A 1
H26A H -0.1769 0.0313 0.8668 0.107 Uiso 0.50 1 calc PR A 1
H26B H -0.1892 0.1171 0.8952 0.107 Uiso 0.50 1 calc PR A 1
C26' C -0.0875(7) 0.0689(6) 0.9365(4) 0.072(3) Uani 0.50 1 d PD A 2
H26C H -0.0784 0.1147 0.9634 0.087 Uiso 0.50 1 calc PR A 2
H26D H -0.0469 0.0215 0.9548 0.087 Uiso 0.50 1 calc PR A 2
C27 C -0.1489(9) 0.0227(8) 0.9495(5) 0.100(4) Uani 0.50 1 d PD A 1
H27A H -0.1230 0.0591 0.9817 0.120 Uiso 0.50 1 calc PR A 1
H27B H -0.1060 -0.0268 0.9541 0.120 Uiso 0.50 1 calc PR A 1
C27' C -0.1939(7) 0.0441(10) 0.9194(4) 0.100(4) Uani 0.50 1 d PD A 2
H27C H -0.2027 -0.0019 0.8927 0.120 Uiso 0.50 1 calc PR A 2
H27D H -0.2342 0.0914 0.9006 0.120 Uiso 0.50 1 calc PR A 2
C28 C -0.2559(11) -0.0037(13) 0.9465(7) 0.118(7) Uani 0.50 1 d PD A 1
H28A H -0.2568 -0.0314 0.9807 0.177 Uiso 0.50 1 calc PR A 1
H28B H -0.2803 -0.0417 0.9156 0.177 Uiso 0.50 1 calc PR A 1
H28C H -0.2986 0.0453 0.9413 0.177 Uiso 0.50 1 calc PR A 1
C28' C -0.2317(10) 0.0172(10) 0.9675(6) 0.088(5) Uani 0.50 1 d PDU A 2
H28D H -0.1756 0.0000 0.9981 0.131 Uiso 0.50 1 calc PR A 2
H28E H -0.2776 -0.0293 0.9562 0.131 Uiso 0.50 1 calc PR A 2
H28F H -0.2661 0.0635 0.9792 0.131 Uiso 0.50 1 calc PR A 2
C29 C 0.6651(2) 0.46553(19) 0.89884(13) 0.0377(7) Uani 1 1 d . . .
H29A H 0.6875 0.4369 0.9347 0.045 Uiso 1 1 calc R . .
H29B H 0.6147 0.5068 0.9018 0.045 Uiso 1 1 calc R . .
C30 C 0.6891(2) 0.34163(18) 0.84879(13) 0.0334(7) Uani 1 1 d . . .
H30A H 0.7423 0.3356 0.8836 0.040 Uiso 1 1 calc R . .
H30B H 0.7198 0.3622 0.8206 0.040 Uiso 1 1 calc R . .
C31 C 0.5658(2) 0.44641(19) 0.80444(13) 0.0399(8) Uani 1 1 d . . .
H31A H 0.6155 0.4789 0.7921 0.048 Uiso 1 1 calc R . .
H31B H 0.5165 0.4856 0.8114 0.048 Uiso 1 1 calc R . .
C32 C 0.5147(2) 0.38843(19) 0.75964(13) 0.0377(7) Uani 1 1 d . . .
C33 C 0.4426(2) 0.33491(19) 0.76860(13) 0.0383(7) Uani 1 1 d . . .
C34 C 0.4004(2) 0.2768(2) 0.72801(14) 0.0417(8) Uani 1 1 d . . .
C35 C 0.4244(2) 0.2771(2) 0.67825(14) 0.0467(8) Uani 1 1 d . . .
H35 H 0.3940 0.2381 0.6507 0.056 Uiso 1 1 calc R . .
C36 C 0.4919(3) 0.3333(2) 0.66815(14) 0.0471(8) Uani 1 1 d . . .
C37 C 0.5375(2) 0.3870(2) 0.70950(13) 0.0422(8) Uani 1 1 d . . .
H37 H 0.5859 0.4242 0.7037 0.051 Uiso 1 1 calc R . .
C38 C 0.6436(2) 0.25819(18) 0.83153(12) 0.0323(7) Uani 1 1 d . . .
C39 C 0.6832(2) 0.20501(19) 0.80044(13) 0.0391(8) Uani 1 1 d . . .
H39 H 0.7370 0.2221 0.7871 0.047 Uiso 1 1 calc R . .
C40 C 0.6434(3) 0.1266(2) 0.78904(14) 0.0473(9) Uani 1 1 d . . .
H40 H 0.6701 0.0888 0.7683 0.057 Uiso 1 1 calc R . .
C41 C 0.5640(3) 0.1042(2) 0.80833(14) 0.0487(9) Uani 1 1 d . . .
H41 H 0.5353 0.0508 0.8009 0.058 Uiso 1 1 calc R . .
C42 C 0.5278(3) 0.1601(2) 0.83814(14) 0.0443(8) Uani 1 1 d . . .
H42 H 0.4727 0.1447 0.8509 0.053 Uiso 1 1 calc R . .
C43 C 0.7529(2) 0.51155(19) 0.88912(13) 0.0383(7) Uani 1 1 d . . .
C44 C 0.8491(3) 0.4851(2) 0.91361(15) 0.0488(9) Uani 1 1 d . . .
H44 H 0.8600 0.4372 0.9362 0.059 Uiso 1 1 calc R . .
C45 C 0.9294(3) 0.5277(3) 0.90549(19) 0.0649(12) Uani 1 1 d . . .
H45 H 0.9949 0.5093 0.9227 0.078 Uiso 1 1 calc R . .
C46 C 0.9143(3) 0.5970(3) 0.87236(19) 0.0683(12) Uani 1 1 d . . .
H46 H 0.9694 0.6256 0.8662 0.082 Uiso 1 1 calc R . .
C47 C 0.8198(3) 0.6245(2) 0.84829(17) 0.0621(11) Uani 1 1 d . . .
H47 H 0.8095 0.6722 0.8255 0.075 Uiso 1 1 calc R . .
C48 C 0.7398(3) 0.5830(2) 0.85716(14) 0.0476(9) Uani 1 1 d . . .
H48 H 0.6748 0.6034 0.8412 0.057 Uiso 1 1 calc R . .
C49 C 0.3147(3) 0.1485(2) 0.70920(19) 0.0698(12) Uani 1 1 d . . .
H49A H 0.3767 0.1251 0.7050 0.105 Uiso 1 1 calc R . .
H49B H 0.2705 0.1617 0.6730 0.105 Uiso 1 1 calc R . .
H49C H 0.2826 0.1081 0.7275 0.105 Uiso 1 1 calc R . .
C50 C 0.5142(3) 0.3350(3) 0.61314(15) 0.0663(11) Uani 1 1 d . . .
H50A H 0.5695 0.3729 0.6149 0.099 Uiso 1 1 calc R . .
H50B H 0.4555 0.3540 0.5849 0.099 Uiso 1 1 calc R . .
H50C H 0.5320 0.2793 0.6040 0.099 Uiso 1 1 calc R . .
C51 C 0.3636(7) 0.4536(9) 0.9016(5) 0.092(4) Uani 0.40 1 d PDU B 1
H51A H 0.3174 0.4062 0.8920 0.110 Uiso 0.40 1 calc PR B 1
H51B H 0.3486 0.4921 0.8700 0.110 Uiso 0.40 1 calc PR B 1
C51' C 0.3942(6) 0.4396(6) 0.9440(4) 0.102(3) Uani 0.60 1 d PDU B 2
H51C H 0.4300 0.4643 0.9797 0.122 Uiso 0.60 1 calc PR B 2
H51D H 0.3632 0.3871 0.9508 0.122 Uiso 0.60 1 calc PR B 2
C52 C 0.3474(9) 0.4978(8) 0.9513(4) 0.086(4) Uani 0.40 1 d PDU B 1
H52A H 0.3961 0.5430 0.9634 0.103 Uiso 0.40 1 calc PR B 1
H52B H 0.3541 0.4587 0.9822 0.103 Uiso 0.40 1 calc PR B 1
C52' C 0.3136(7) 0.5009(7) 0.9102(4) 0.112(3) Uani 0.60 1 d PDU B 2
H52C H 0.3424 0.5569 0.9111 0.134 Uiso 0.60 1 calc PR B 2
H52D H 0.2910 0.4826 0.8715 0.134 Uiso 0.60 1 calc PR B 2
C53 C 0.2403(11) 0.5329(13) 0.9322(9) 0.117(4) Uani 0.40 1 d PDU B 1
H53A H 0.2221 0.5563 0.9637 0.175 Uiso 0.40 1 calc PR B 1
H53B H 0.1940 0.4884 0.9160 0.175 Uiso 0.40 1 calc PR B 1
H53C H 0.2371 0.5762 0.9047 0.175 Uiso 0.40 1 calc PR B 1
C53' C 0.2280(8) 0.5033(8) 0.9341(6) 0.117(4) Uani 0.60 1 d PDU B 2
H53D H 0.2432 0.5404 0.9659 0.175 Uiso 0.60 1 calc PR B 2
H53E H 0.2152 0.4475 0.9457 0.175 Uiso 0.60 1 calc PR B 2
H53F H 0.1691 0.5235 0.9064 0.175 Uiso 0.60 1 calc PR B 2
C54 C 0.6349(4) 0.2382(3) 0.98046(16) 0.0711(12) Uani 1 1 d . B .
H54A H 0.6483 0.1928 0.9574 0.085 Uiso 1 1 calc R . .
H54B H 0.5784 0.2214 0.9943 0.085 Uiso 1 1 calc R . .
C55 C 0.7235(4) 0.2516(3) 1.02760(19) 0.0811(14) Uani 1 1 d . . .
H55A H 0.7071 0.2932 1.0524 0.097 Uiso 1 1 calc R B .
H55B H 0.7395 0.1992 1.0484 0.097 Uiso 1 1 calc R . .
C56 C 0.8131(4) 0.2799(4) 1.0121(2) 0.1030(19) Uani 1 1 d . B .
H56A H 0.7982 0.3318 0.9915 0.154 Uiso 1 1 calc R . .
H56B H 0.8323 0.2377 0.9892 0.154 Uiso 1 1 calc R . .
H56C H 0.8676 0.2887 1.0454 0.154 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.598(2) . ?
V1 O4 1.803(2) . ?
V1 O3 1.817(2) . ?
V1 O2 1.924(2) . ?
V1 N2 2.196(3) . ?
V1 N1 2.430(2) . ?
V2 O6 1.596(2) . ?
V2 O8 1.791(2) . ?
V2 O9 1.825(2) . ?
V2 O7 1.939(2) . ?
V2 N4 2.179(2) . ?
V2 N3 2.429(2) . ?
N1 C2 1.484(4) . ?
N1 C1 1.489(4) . ?
N1 C3 1.492(4) . ?
N2 C10 1.341(4) . ?
N2 C14 1.346(4) . ?
N3 C30 1.483(4) . ?
N3 C31 1.488(4) . ?
N3 C29 1.489(4) . ?
N4 C38 1.344(4) . ?
N4 C42 1.344(4) . ?
O2 C5 1.331(4) . ?
O3 C23 1.398(8) . ?
O3 C23' 1.449(9) . ?
O4 C26' 1.356(8) . ?
O4 C26 1.381(10) . ?
O5 C6 1.372(4) . ?
O5 C21 1.424(4) . ?
O7 C33 1.339(4) . ?
O8 C51 1.384(8) . ?
O8 C51' 1.422(6) . ?
O9 C54 1.436(5) . ?
O10 C34 1.379(4) . ?
O10 C49 1.420(4) . ?
C1 C15 1.511(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C10 1.495(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.497(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.393(4) . ?
C4 C5 1.396(4) . ?
C5 C6 1.412(5) . ?
C6 C7 1.388(4) . ?
C7 C8 1.392(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(5) . ?
C8 C22 1.522(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(4) . ?
C11 C12 1.380(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.372(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.371(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.383(5) . ?
C15 C16 1.387(5) . ?
C16 C17 1.383(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.376(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.568(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23' C24' 1.564(9) . ?
C23' H23C 0.9900 . ?
C23' H23D 0.9900 . ?
C24 C25 1.539(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24' C25' 1.508(9) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25' H25D 0.9800 . ?
C25' H25E 0.9800 . ?
C25' H25F 0.9800 . ?
C26 C27 1.495(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26' C27' 1.491(8) . ?
C26' H26C 0.9900 . ?
C26' H26D 0.9900 . ?
C27 C28 1.543(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27' C28' 1.522(9) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28' H28D 0.9800 . ?
C28' H28E 0.9800 . ?
C28' H28F 0.9800 . ?
C29 C43 1.518(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C38 1.505(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.494(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C37 1.394(4) . ?
C32 C33 1.397(4) . ?
C33 C34 1.399(4) . ?
C34 C35 1.394(5) . ?
C35 C36 1.387(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.375(5) . ?
C36 C50 1.512(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.383(4) . ?
C39 C40 1.383(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.383(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.364(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.389(5) . ?
C43 C48 1.394(5) . ?
C44 C45 1.384(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.381(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.372(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.379(5) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
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 C52 1.519(9) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51' C52' 1.568(8) . ?
C51' H51C 0.9900 . ?
C51' H51D 0.9900 . ?
C52 C53 1.555(10) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52' C53' 1.488(9) . ?
C52' H52C 0.9900 . ?
C52' H52D 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C53' H53D 0.9800 . ?
C53' H53E 0.9800 . ?
C53' H53F 0.9800 . ?
C54 C55 1.483(6) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.489(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O4 104.05(12) . . ?
O1 V1 O3 97.86(11) . . ?
O4 V1 O3 98.29(11) . . ?
O1 V1 O2 97.24(11) . . ?
O4 V1 O2 93.92(11) . . ?
O3 V1 O2 157.64(10) . . ?
O1 V1 N2 94.92(11) . . ?
O4 V1 N2 160.43(10) . . ?
O3 V1 N2 83.62(10) . . ?
O2 V1 N2 78.74(9) . . ?
O1 V1 N1 168.44(11) . . ?
O4 V1 N1 87.49(10) . . ?
O3 V1 N1 79.47(9) . . ?
O2 V1 N1 82.45(9) . . ?
N2 V1 N1 73.65(9) . . ?
O6 V2 O8 104.23(12) . . ?
O6 V2 O9 98.29(12) . . ?
O8 V2 O9 98.76(11) . . ?
O6 V2 O7 96.35(12) . . ?
O8 V2 O7 94.13(11) . . ?
O9 V2 O7 157.45(9) . . ?
O6 V2 N4 95.32(11) . . ?
O8 V2 N4 159.78(11) . . ?
O9 V2 N4 83.24(10) . . ?
O7 V2 N4 78.40(9) . . ?
O6 V2 N3 169.54(11) . . ?
O8 V2 N3 86.23(10) . . ?
O9 V2 N3 79.93(9) . . ?
O7 V2 N3 82.56(9) . . ?
N4 V2 N3 74.25(9) . . ?
C2 N1 C1 111.3(2) . . ?
C2 N1 C3 111.7(2) . . ?
C1 N1 C3 109.8(3) . . ?
C2 N1 V1 106.11(17) . . ?
C1 N1 V1 107.09(17) . . ?
C3 N1 V1 110.71(18) . . ?
C10 N2 C14 118.9(3) . . ?
C10 N2 V1 119.6(2) . . ?
C14 N2 V1 120.9(2) . . ?
C30 N3 C31 111.8(2) . . ?
C30 N3 C29 110.7(2) . . ?
C31 N3 C29 109.6(2) . . ?
C30 N3 V2 105.91(17) . . ?
C31 N3 V2 110.66(17) . . ?
C29 N3 V2 108.06(17) . . ?
C38 N4 C42 118.6(3) . . ?
C38 N4 V2 119.9(2) . . ?
C42 N4 V2 121.2(2) . . ?
C5 O2 V1 131.37(19) . . ?
C23 O3 V1 130.2(6) . . ?
C23' O3 V1 122.0(4) . . ?
C26' O4 V1 128.4(5) . . ?
C26 O4 V1 128.3(5) . . ?
C6 O5 C21 116.9(3) . . ?
C33 O7 V2 130.77(19) . . ?
C51 O8 V2 126.2(6) . . ?
C51' O8 V2 126.7(4) . . ?
C54 O9 V2 126.4(2) . . ?
C34 O10 C49 116.4(3) . . ?
N1 C1 C15 117.3(3) . . ?
N1 C1 H1A 108.0 . . ?
C15 C1 H1A 108.0 . . ?
N1 C1 H1B 108.0 . . ?
C15 C1 H1B 108.0 . . ?
H1A C1 H1B 107.2 . . ?
N1 C2 C10 112.3(2) . . ?
N1 C2 H2A 109.1 . . ?
C10 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
C10 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C4 114.3(3) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C9 C4 C5 120.2(3) . . ?
C9 C4 C3 122.0(3) . . ?
C5 C4 C3 117.7(3) . . ?
O2 C5 C4 121.9(3) . . ?
O2 C5 C6 120.2(3) . . ?
C4 C5 C6 117.9(3) . . ?
O5 C6 C7 124.1(3) . . ?
O5 C6 C5 115.3(3) . . ?
C7 C6 C5 120.5(3) . . ?
C8 C7 C6 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C7 118.6(3) . . ?
C9 C8 C22 120.7(3) . . ?
C7 C8 C22 120.6(4) . . ?
C8 C9 C4 121.6(3) . . ?
C8 C9 H9 119.2 . . ?
C4 C9 H9 119.2 . . ?
N2 C10 C11 121.2(3) . . ?
N2 C10 C2 117.2(3) . . ?
C11 C10 C2 121.6(3) . . ?
C10 C11 C12 119.5(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 119.0(3) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
N2 C14 C13 122.3(3) . . ?
N2 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C20 C15 C16 118.6(3) . . ?
C20 C15 C1 120.2(3) . . ?
C16 C15 C1 121.0(3) . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.3(4) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 119.6(4) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 120.9(4) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C8 C22 H22A 109.5 . . ?
C8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C24 106.9(8) . . ?
O3 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
O3 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.6 . . ?
O3 C23' C24' 103.6(7) . . ?
O3 C23' H23C 111.0 . . ?
C24' C23' H23C 111.0 . . ?
O3 C23' H23D 111.0 . . ?
C24' C23' H23D 111.0 . . ?
H23C C23' H23D 109.0 . . ?
C25 C24 C23 95.3(13) . . ?
C25 C24 H24A 112.7 . . ?
C23 C24 H24A 112.7 . . ?
C25 C24 H24B 112.7 . . ?
C23 C24 H24B 112.7 . . ?
H24A C24 H24B 110.2 . . ?
C25' C24' C23' 109.1(11) . . ?
C25' C24' H24C 109.8 . . ?
C23' C24' H24C 109.8 . . ?
C25' C24' H24D 109.9 . . ?
C23' C24' H24D 109.9 . . ?
H24C C24' H24D 108.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24' C25' H25D 109.5 . . ?
C24' C25' H25E 109.5 . . ?
H25D C25' H25E 109.5 . . ?
C24' C25' H25F 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
O4 C26 C27 118.3(9) . . ?
O4 C26 H26A 107.7 . . ?
C27 C26 H26A 107.7 . . ?
O4 C26 H26B 107.7 . . ?
C27 C26 H26B 107.7 . . ?
H26A C26 H26B 107.1 . . ?
O4 C26' C27' 111.7(8) . . ?
O4 C26' H26C 109.3 . . ?
C27' C26' H26C 109.3 . . ?
O4 C26' H26D 109.3 . . ?
C27' C26' H26D 109.3 . . ?
H26C C26' H26D 107.9 . . ?
C26 C27 C28 110.4(12) . . ?
C26 C27 H27A 109.6 . . ?
C28 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C28 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C26' C27' C28' 112.7(8) . . ?
C26' C27' H27C 109.0 . . ?
C28' C27' H27C 109.0 . . ?
C26' C27' H27D 109.0 . . ?
C28' C27' H27D 109.0 . . ?
H27C C27' H27D 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27' C28' H28D 109.5 . . ?
C27' C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C27' C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
N3 C29 C43 116.6(2) . . ?
N3 C29 H29A 108.2 . . ?
C43 C29 H29A 108.2 . . ?
N3 C29 H29B 108.2 . . ?
C43 C29 H29B 108.2 . . ?
H29A C29 H29B 107.3 . . ?
N3 C30 C38 113.0(2) . . ?
N3 C30 H30A 109.0 . . ?
C38 C30 H30A 109.0 . . ?
N3 C30 H30B 109.0 . . ?
C38 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
N3 C31 C32 113.2(3) . . ?
N3 C31 H31A 108.9 . . ?
C32 C31 H31A 108.9 . . ?
N3 C31 H31B 108.9 . . ?
C32 C31 H31B 108.9 . . ?
H31A C31 H31B 107.8 . . ?
C37 C32 C33 119.8(3) . . ?
C37 C32 C31 121.4(3) . . ?
C33 C32 C31 118.8(3) . . ?
O7 C33 C32 121.0(3) . . ?
O7 C33 C34 120.6(3) . . ?
C32 C33 C34 118.4(3) . . ?
O10 C34 C35 124.3(3) . . ?
O10 C34 C33 115.4(3) . . ?
C35 C34 C33 120.3(3) . . ?
C36 C35 C34 121.2(3) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C37 C36 C35 118.1(3) . . ?
C37 C36 C50 121.4(3) . . ?
C35 C36 C50 120.6(3) . . ?
C36 C37 C32 122.0(3) . . ?
C36 C37 H37 119.0 . . ?
C32 C37 H37 119.0 . . ?
N4 C38 C39 121.7(3) . . ?
N4 C38 C30 117.0(3) . . ?
C39 C38 C30 121.2(3) . . ?
C38 C39 C40 119.0(3) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
C41 C40 C39 119.0(3) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C42 C41 C40 118.9(3) . . ?
C42 C41 H41 120.5 . . ?
C40 C41 H41 120.5 . . ?
N4 C42 C41 122.8(3) . . ?
N4 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C44 C43 C48 118.1(3) . . ?
C44 C43 C29 120.6(3) . . ?
C48 C43 C29 121.2(3) . . ?
C45 C44 C43 120.7(4) . . ?
C45 C44 H44 119.6 . . ?
C43 C44 H44 119.6 . . ?
C46 C45 C44 120.1(4) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C47 C46 C45 120.0(4) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C47 C48 120.0(4) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 C43 121.1(4) . . ?
C47 C48 H48 119.5 . . ?
C43 C48 H48 119.5 . . ?
O10 C49 H49A 109.5 . . ?
O10 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O10 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C36 C50 H50A 109.5 . . ?
C36 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C36 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O8 C51 C52 111.9(8) . . ?
O8 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O8 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
O8 C51' C52' 105.7(7) . . ?
O8 C51' H51C 110.6 . . ?
C52' C51' H51C 110.6 . . ?
O8 C51' H51D 110.6 . . ?
C52' C51' H51D 110.6 . . ?
H51C C51' H51D 108.7 . . ?
C51 C52 C53 105.5(8) . . ?
C51 C52 H52A 110.6 . . ?
C53 C52 H52A 110.6 . . ?
C51 C52 H52B 110.6 . . ?
C53 C52 H52B 110.6 . . ?
H52A C52 H52B 108.8 . . ?
C53' C52' C51' 109.6(7) . . ?
C53' C52' H52C 109.7 . . ?
C51' C52' H52C 109.7 . . ?
C53' C52' H52D 109.7 . . ?
C51' C52' H52D 109.7 . . ?
H52C C52' H52D 108.2 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52' C53' H53D 109.5 . . ?
C52' C53' H53E 109.5 . . ?
H53D C53' H53E 109.5 . . ?
C52' C53' H53F 109.5 . . ?
H53D C53' H53F 109.5 . . ?
H53E C53' H53F 109.5 . . ?
O9 C54 C55 111.6(4) . . ?
O9 C54 H54A 109.3 . . ?
C55 C54 H54A 109.3 . . ?
O9 C54 H54B 109.3 . . ?
C55 C54 H54B 109.3 . . ?
H54A C54 H54B 108.0 . . ?
C56 C55 C54 114.4(4) . . ?
C56 C55 H55A 108.7 . . ?
C54 C55 H55A 108.7 . . ?
C56 C55 H55B 108.7 . . ?
C54 C55 H55B 108.7 . . ?
H55A C55 H55B 107.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 994167'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wjb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H33 N2 O5 V, C H2 Cl2'
_chemical_formula_sum            'C23 H35 Cl2 N2 O5 V'
_chemical_formula_weight         541.37

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   13.2554(5)
_cell_length_b                   19.2889(8)
_cell_length_c                   23.4680(9)
_cell_angle_alpha                110.703(1)
_cell_angle_beta                 102.623(1)
_cell_angle_gamma                91.396(1)
_cell_volume                     5443.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    4234
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2272
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29328
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.75
_reflns_number_total             20425
_reflns_number_gt                12242
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0970P)²+0.6395P] 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         20425
_refine_ls_number_parameters     1228
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_ref         0.2128
_refine_ls_wR_factor_gt          0.1860
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.58273(6) 0.36064(4) 0.05746(4) 0.0396(2) Uani 1 1 d . . .
V2 V 0.02246(6) 0.12687(5) 0.91436(4) 0.0479(2) Uani 1 1 d . . .
V3 V 0.89431(6) 0.27873(5) 0.40729(4) 0.0459(2) Uani 1 1 d . . .
V4 V 0.50483(7) 0.79024(5) 0.37987(4) 0.0464(2) Uani 1 1 d . . .
Cl1 Cl 0.3583(2) 0.00711(14) 1.03652(12) 0.1431(10) Uani 1 1 d . . .
Cl2 Cl 0.30348(18) 0.00409(14) 0.91062(12) 0.1320(9) Uani 1 1 d . . .
Cl3 Cl 0.8526(2) 0.48067(17) -0.04413(14) 0.0951(9) Uani 0.75 1 d P A 1
Cl3' Cl 0.8061(8) 0.5209(4) -0.0345(4) 0.100(3) Uani 0.25 1 d PD A 2
Cl4 Cl 0.87232(14) 0.50189(14) 0.08531(9) 0.1076(7) Uani 1 1 d . A .
Cl5 Cl 0.62128(16) 0.38694(13) 0.34249(9) 0.1086(7) Uani 1 1 d . . .
Cl6 Cl 0.60430(13) 0.46886(9) 0.46832(10) 0.0910(6) Uani 1 1 d . . .
Cl7 Cl 0.1243(2) 0.0980(2) 0.59049(18) 0.1864(14) Uani 1 1 d . . .
Cl8 Cl 0.1943(3) -0.01936(15) 0.49709(16) 0.1774(13) Uani 1 1 d . . .
N1 N 0.5031(3) 0.2376(2) 0.03215(17) 0.0423(9) Uani 1 1 d . . .
N2 N 0.4443(3) 0.3435(2) -0.01867(17) 0.0397(9) Uani 1 1 d . . .
N3 N -0.0382(3) 0.2471(2) 0.93085(18) 0.0456(10) Uani 1 1 d . . .
N4 N -0.0577(3) 0.1492(2) 0.99021(18) 0.0412(9) Uani 1 1 d . . .
N5 N 0.9651(3) 0.1972(2) 0.45871(18) 0.0496(10) Uani 1 1 d . . .
N6 N 1.0374(3) 0.3405(2) 0.47664(18) 0.0440(9) Uani 1 1 d . . .
N7 N 0.4385(3) 0.6826(2) 0.39385(17) 0.0449(10) Uani 1 1 d . . .
N8 N 0.4490(3) 0.8326(2) 0.46561(17) 0.0439(9) Uani 1 1 d . . .
O1 O 0.6100(2) 0.44533(17) 0.06566(15) 0.0495(8) Uani 1 1 d . . .
O2 O 0.6412(2) 0.31198(16) -0.01233(13) 0.0401(7) Uani 1 1 d . . .
O3 O 0.4895(2) 0.37909(17) 0.10650(15) 0.0483(8) Uani 1 1 d . . .
O4 O 0.6880(2) 0.34442(18) 0.11323(14) 0.0479(8) Uani 1 1 d . . .
O5 O 0.6518(3) 0.33459(18) -0.11672(15) 0.0531(9) Uani 1 1 d . . .
O6 O 0.0415(3) 0.04500(18) 0.91377(16) 0.0577(9) Uani 1 1 d . . .
O7 O 0.1353(2) 0.18471(17) 0.98397(14) 0.0443(8) Uani 1 1 d . . .
O8 O 0.0892(3) 0.1363(2) 0.85778(16) 0.0610(10) Uani 1 1 d . . .
O9 O -0.1076(3) 0.10315(19) 0.86303(15) 0.0569(9) Uani 1 1 d . . .
O10 O 0.2246(3) 0.1732(2) 1.09229(17) 0.0629(10) Uani 1 1 d . . .
O11 O 0.8753(3) 0.34537(19) 0.38237(15) 0.0548(9) Uani 1 1 d . . .
O12 O 0.8375(2) 0.31733(17) 0.47938(13) 0.0434(8) Uani 1 1 d . . .
O13 O 0.7809(3) 0.2117(2) 0.36395(15) 0.0570(9) Uani 1 1 d U . .
O14 O 0.9808(3) 0.23364(18) 0.35844(15) 0.0537(9) Uani 1 1 d . . .
O15 O 0.8323(3) 0.45177(19) 0.56227(15) 0.0580(9) Uani 1 1 d . . .
O16 O 0.5396(3) 0.87220(19) 0.38320(15) 0.0568(9) Uani 1 1 d . . .
O17 O 0.6261(2) 0.78551(17) 0.44252(14) 0.0458(8) Uani 1 1 d . . .
O18 O 0.5533(3) 0.7291(2) 0.31681(15) 0.0576(9) Uani 1 1 d . C .
O19 O 0.3692(3) 0.7811(2) 0.33980(15) 0.0555(9) Uani 1 1 d . . .
O20 O 0.7242(3) 0.8836(2) 0.55467(16) 0.0619(10) Uani 1 1 d . . .
C1 C 0.5147(4) 0.2212(3) 0.0903(2) 0.0557(13) Uani 1 1 d . . .
H1B H 0.4782 0.1720 0.0801 0.084 Uiso 1 1 calc R . .
H1C H 0.4849 0.2592 0.1203 0.084 Uiso 1 1 calc R . .
H1D H 0.5887 0.2217 0.1088 0.084 Uiso 1 1 calc R . .
C2 C 0.3919(3) 0.2369(3) 0.0045(2) 0.0468(12) Uani 1 1 d . . .
H2A H 0.3553 0.2552 0.0386 0.056 Uiso 1 1 calc R . .
H2B H 0.3618 0.1850 -0.0219 0.056 Uiso 1 1 calc R . .
C3 C 0.5514(4) 0.1796(3) -0.0114(2) 0.0448(12) Uani 1 1 d . . .
H3A H 0.5138 0.1302 -0.0213 0.054 Uiso 1 1 calc R . .
H3B H 0.6243 0.1793 0.0105 0.054 Uiso 1 1 calc R . .
C4 C 0.5512(3) 0.1902(3) -0.0714(2) 0.0419(11) Uani 1 1 d . . .
C5 C 0.5992(3) 0.2567(3) -0.0683(2) 0.0400(11) Uani 1 1 d . . .
C6 C 0.6025(4) 0.2668(3) -0.1242(2) 0.0468(12) Uani 1 1 d . . .
C7 C 0.5579(4) 0.2108(3) -0.1822(2) 0.0543(13) Uani 1 1 d . . .
H7A H 0.5602 0.2181 -0.2198 0.065 Uiso 1 1 calc R . .
C8 C 0.5101(4) 0.1444(3) -0.1850(2) 0.0547(13) Uani 1 1 d . . .
C9 C 0.5067(4) 0.1349(3) -0.1299(2) 0.0517(13) Uani 1 1 d . . .
H9A H 0.4734 0.0897 -0.1317 0.062 Uiso 1 1 calc R . .
C10 C 0.3747(3) 0.2843(2) -0.0344(2) 0.0403(11) Uani 1 1 d . . .
C11 C 0.2862(4) 0.2694(3) -0.0842(2) 0.0503(12) Uani 1 1 d . . .
H11B H 0.2376 0.2269 -0.0955 0.060 Uiso 1 1 calc R . .
C12 C 0.2708(4) 0.3168(3) -0.1163(2) 0.0598(15) Uani 1 1 d . . .
H12A H 0.2106 0.3082 -0.1495 0.072 Uiso 1 1 calc R . .
C13 C 0.3440(4) 0.3777(3) -0.0998(2) 0.0498(12) Uani 1 1 d . . .
H13A H 0.3351 0.4111 -0.1216 0.060 Uiso 1 1 calc R . .
C14 C 0.4289(4) 0.3885(3) -0.0516(2) 0.0447(12) Uani 1 1 d . . .
H14A H 0.4795 0.4296 -0.0407 0.054 Uiso 1 1 calc R . .
C15 C 0.6523(5) 0.3477(3) -0.1724(2) 0.0683(16) Uani 1 1 d . . .
H15A H 0.6905 0.3966 -0.1615 0.102 Uiso 1 1 calc R . .
H15B H 0.5806 0.3467 -0.1952 0.102 Uiso 1 1 calc R . .
H15C H 0.6863 0.3088 -0.1989 0.102 Uiso 1 1 calc R . .
C16 C 0.4597(5) 0.0845(3) -0.2481(2) 0.0787(19) Uani 1 1 d . . .
H16B H 0.5110 0.0711 -0.2735 0.118 Uiso 1 1 calc R . .
H16C H 0.4015 0.1033 -0.2699 0.118 Uiso 1 1 calc R . .
H16D H 0.4339 0.0404 -0.2418 0.118 Uiso 1 1 calc R . .
C17 C 0.4435(4) 0.4455(3) 0.1269(3) 0.0628(15) Uani 1 1 d . . .
H17A H 0.3997 0.4532 0.0902 0.075 Uiso 1 1 calc R . .
H17B H 0.4985 0.4881 0.1485 0.075 Uiso 1 1 calc R . .
C18 C 0.3784(5) 0.4428(3) 0.1706(3) 0.0736(18) Uani 1 1 d . . .
H18A H 0.3194 0.4034 0.1471 0.088 Uiso 1 1 calc R . .
H18B H 0.3490 0.4910 0.1848 0.088 Uiso 1 1 calc R . .
C19 C 0.4341(6) 0.4282(4) 0.2273(3) 0.091(2) Uani 1 1 d . . .
H19A H 0.3850 0.4256 0.2524 0.136 Uiso 1 1 calc R . .
H19B H 0.4899 0.4686 0.2526 0.136 Uiso 1 1 calc R . .
H19C H 0.4639 0.3808 0.2140 0.136 Uiso 1 1 calc R . .
C20 C 0.7299(5) 0.3982(3) 0.1734(3) 0.0777(19) Uani 1 1 d . . .
H20A H 0.6728 0.4124 0.1948 0.093 Uiso 1 1 calc R . .
H20B H 0.7587 0.4432 0.1688 0.093 Uiso 1 1 calc R . .
C21 C 0.8104(5) 0.3751(4) 0.2130(3) 0.088(2) Uani 1 1 d . . .
H21A H 0.8674 0.3602 0.1916 0.105 Uiso 1 1 calc R . .
H21B H 0.7815 0.3306 0.2184 0.105 Uiso 1 1 calc R . .
C22 C 0.8549(5) 0.4342(4) 0.2768(3) 0.0761(18) Uani 1 1 d . . .
H22A H 0.9185 0.4191 0.2974 0.114 Uiso 1 1 calc R . .
H22B H 0.8039 0.4404 0.3023 0.114 Uiso 1 1 calc R . .
H22C H 0.8713 0.4814 0.2722 0.114 Uiso 1 1 calc R . .
C23 C -0.0702(5) 0.2583(3) 0.8705(2) 0.0692(16) Uani 1 1 d . . .
H23A H -0.0999 0.3058 0.8776 0.104 Uiso 1 1 calc R . .
H23B H -0.1225 0.2175 0.8409 0.104 Uiso 1 1 calc R . .
H23C H -0.0095 0.2591 0.8532 0.104 Uiso 1 1 calc R . .
C24 C -0.1302(4) 0.2457(3) 0.9565(2) 0.0503(13) Uani 1 1 d . . .
H24A H -0.1916 0.2201 0.9216 0.060 Uiso 1 1 calc R . .
H24B H -0.1443 0.2975 0.9779 0.060 Uiso 1 1 calc R . .
C25 C 0.0426(4) 0.3099(3) 0.9737(2) 0.0480(12) Uani 1 1 d . . .
H25A H 0.1002 0.3111 0.9532 0.058 Uiso 1 1 calc R . .
H25B H 0.0117 0.3575 0.9804 0.058 Uiso 1 1 calc R . .
C26 C 0.0856(3) 0.3041(3) 1.0356(2) 0.0417(11) Uani 1 1 d . . .
C27 C 0.1337(3) 0.2411(3) 1.0371(2) 0.0420(11) Uani 1 1 d . . .
C28 C 0.1781(3) 0.2369(3) 1.0957(2) 0.0461(12) Uani 1 1 d . . .
C29 C 0.1704(4) 0.2934(3) 1.1502(2) 0.0536(13) Uani 1 1 d . . .
H29A H 0.1997 0.2894 1.1895 0.064 Uiso 1 1 calc R . .
C30 C 0.1219(4) 0.3550(3) 1.1492(2) 0.0541(13) Uani 1 1 d . . .
C31 C 0.0807(4) 0.3602(3) 1.0919(2) 0.0515(13) Uani 1 1 d . . .
H31A H 0.0481 0.4032 1.0906 0.062 Uiso 1 1 calc R . .
C32 C -0.1143(3) 0.2067(3) 1.0021(2) 0.0419(11) Uani 1 1 d . . .
C33 C -0.1589(4) 0.2262(3) 1.0531(2) 0.0532(13) Uani 1 1 d . . .
H33A H -0.1981 0.2677 1.0614 0.064 Uiso 1 1 calc R . .
C34 C -0.1467(4) 0.1863(3) 1.0913(3) 0.0586(14) Uani 1 1 d . . .
H34A H -0.1780 0.1989 1.1259 0.070 Uiso 1 1 calc R . .
C35 C -0.0881(4) 0.1271(3) 1.0786(2) 0.0545(13) Uani 1 1 d . . .
H35A H -0.0781 0.0981 1.1043 0.065 Uiso 1 1 calc R . .
C36 C -0.0445(4) 0.1108(3) 1.0284(2) 0.0503(13) Uani 1 1 d . . .
H36A H -0.0031 0.0705 1.0202 0.060 Uiso 1 1 calc R . .
C37 C 0.2696(6) 0.1655(4) 1.1504(3) 0.102(3) Uani 1 1 d . . .
H37A H 0.2987 0.1177 1.1423 0.153 Uiso 1 1 calc R . .
H37B H 0.2161 0.1673 1.1737 0.153 Uiso 1 1 calc R . .
H37C H 0.3251 0.2063 1.1752 0.153 Uiso 1 1 calc R . .
C38 C 0.1161(5) 0.4171(4) 1.2101(3) 0.083(2) Uani 1 1 d . . .
H38A H 0.1076 0.3955 1.2410 0.125 Uiso 1 1 calc R . .
H38B H 0.0567 0.4444 1.2019 0.125 Uiso 1 1 calc R . .
H38C H 0.1804 0.4514 1.2265 0.125 Uiso 1 1 calc R . .
C39 C 0.0952(6) 0.0749(4) 0.8047(3) 0.091(2) Uani 1 1 d . . .
H39A H 0.0253 0.0585 0.7757 0.109 Uiso 1 1 calc R . .
H39B H 0.1180 0.0331 0.8177 0.109 Uiso 1 1 calc R . .
C40 C 0.1698(7) 0.0930(5) 0.7706(4) 0.131(3) Uani 1 1 d U . .
H40A H 0.1464 0.1335 0.7560 0.157 Uiso 1 1 calc R . .
H40B H 0.2400 0.1101 0.7993 0.157 Uiso 1 1 calc R . .
C41 C 0.1737(9) 0.0264(6) 0.7173(4) 0.192(6) Uani 1 1 d U . .
H41A H 0.2259 0.0365 0.6966 0.289 Uiso 1 1 calc R . .
H41B H 0.1054 0.0122 0.6875 0.289 Uiso 1 1 calc R . .
H41C H 0.1925 -0.0144 0.7319 0.289 Uiso 1 1 calc R . .
C42 C -0.1811(4) 0.0427(3) 0.8499(3) 0.0684(16) Uani 1 1 d . . .
H42A H -0.2197 0.0544 0.8832 0.082 Uiso 1 1 calc R . .
H42B H -0.1451 -0.0018 0.8494 0.082 Uiso 1 1 calc R . .
C43 C -0.2572(5) 0.0259(4) 0.7867(3) 0.0779(18) Uani 1 1 d . . .
H43A H -0.2921 0.0709 0.7875 0.094 Uiso 1 1 calc R . .
H43B H -0.2178 0.0148 0.7537 0.094 Uiso 1 1 calc R . .
C44 C -0.3376(5) -0.0376(4) 0.7697(3) 0.091(2) Uani 1 1 d . . .
H44A H -0.3847 -0.0448 0.7291 0.136 Uiso 1 1 calc R . .
H44B H -0.3773 -0.0270 0.8019 0.136 Uiso 1 1 calc R . .
H44C H -0.3039 -0.0829 0.7669 0.136 Uiso 1 1 calc R . .
C45 C 0.9480(5) 0.1194(3) 0.4136(2) 0.0622(15) Uani 1 1 d . . .
H45A H 0.9827 0.0872 0.4342 0.093 Uiso 1 1 calc R . .
H45B H 0.9767 0.1164 0.3778 0.093 Uiso 1 1 calc R . .
H45C H 0.8732 0.1028 0.3988 0.093 Uiso 1 1 calc R . .
C46 C 1.0786(4) 0.2218(3) 0.4821(2) 0.0523(13) Uani 1 1 d . . .
H46A H 1.1131 0.2000 0.4474 0.063 Uiso 1 1 calc R . .
H46B H 1.1078 0.2029 0.5157 0.063 Uiso 1 1 calc R . .
C47 C 0.9183(4) 0.1995(3) 0.5115(2) 0.0541(13) Uani 1 1 d . . .
H47A H 0.9548 0.1675 0.5324 0.065 Uiso 1 1 calc R . .
H47B H 0.8446 0.1777 0.4939 0.065 Uiso 1 1 calc R . .
C48 C 0.9221(4) 0.2757(3) 0.5602(2) 0.0499(12) Uani 1 1 d . . .
C49 C 0.8780(4) 0.3303(3) 0.5404(2) 0.0444(11) Uani 1 1 d . . .
C50 C 0.8756(4) 0.4010(3) 0.5856(2) 0.0509(13) Uani 1 1 d . . .
C51 C 0.9146(4) 0.4140(3) 0.6489(2) 0.0590(14) Uani 1 1 d . . .
H51A H 0.9114 0.4613 0.6794 0.071 Uiso 1 1 calc R . .
C52 C 0.9584(5) 0.3587(3) 0.6684(2) 0.0655(16) Uani 1 1 d . . .
C53 C 0.9625(4) 0.2900(3) 0.6235(2) 0.0577(14) Uani 1 1 d . . .
H53A H 0.9933 0.2522 0.6361 0.069 Uiso 1 1 calc R . .
C54 C 1.1011(4) 0.3045(3) 0.5071(2) 0.0454(12) Uani 1 1 d . . .
C55 C 1.1856(4) 0.3429(3) 0.5558(2) 0.0502(13) Uani 1 1 d . . .
H55A H 1.2303 0.3167 0.5765 0.060 Uiso 1 1 calc R . .
C56 C 1.2048(4) 0.4191(3) 0.5744(3) 0.0587(14) Uani 1 1 d . . .
H56A H 1.2622 0.4461 0.6081 0.070 Uiso 1 1 calc R . .
C57 C 1.1393(4) 0.4557(3) 0.5432(3) 0.0601(15) Uani 1 1 d . . .
H57A H 1.1509 0.5082 0.5547 0.072 Uiso 1 1 calc R . .
C58 C 1.0574(4) 0.4145(3) 0.4953(2) 0.0491(12) Uani 1 1 d . . .
H58A H 1.0121 0.4398 0.4740 0.059 Uiso 1 1 calc R . .
C59 C 0.8228(5) 0.5233(3) 0.6058(3) 0.0741(18) Uani 1 1 d . . .
H59A H 0.7895 0.5537 0.5828 0.111 Uiso 1 1 calc R . .
H59B H 0.8920 0.5479 0.6310 0.111 Uiso 1 1 calc R . .
H59C H 0.7802 0.5175 0.6334 0.111 Uiso 1 1 calc R . .
C60 C 1.0006(6) 0.3750(4) 0.7386(3) 0.097(2) Uani 1 1 d . . .
H60A H 0.9442 0.3877 0.7601 0.146 Uiso 1 1 calc R . .
H60B H 1.0558 0.4168 0.7563 0.146 Uiso 1 1 calc R . .
H60C H 1.0289 0.3307 0.7442 0.146 Uiso 1 1 calc R . .
C61 C 0.7387(5) 0.1963(4) 0.2996(3) 0.0769(18) Uani 1 1 d U . .
H61A H 0.7847 0.1657 0.2752 0.092 Uiso 1 1 calc R . .
H61B H 0.7371 0.2438 0.2923 0.092 Uiso 1 1 calc R . .
C62 C 0.6326(6) 0.1565(5) 0.2764(3) 0.115(3) Uani 1 1 d . . .
H62A H 0.6360 0.1063 0.2787 0.138 Uiso 1 1 calc R . .
H62B H 0.5892 0.1838 0.3046 0.138 Uiso 1 1 calc R . .
C63 C 0.5827(7) 0.1485(7) 0.2132(4) 0.172(5) Uani 1 1 d . . .
H63A H 0.5101 0.1274 0.2031 0.257 Uiso 1 1 calc R . .
H63B H 0.6189 0.1151 0.1841 0.257 Uiso 1 1 calc R . .
H63C H 0.5849 0.1974 0.2093 0.257 Uiso 1 1 calc R . .
C64 C 1.0343(5) 0.2647(3) 0.3261(3) 0.0684(16) Uani 1 1 d . . .
H64A H 1.1097 0.2733 0.3464 0.082 Uiso 1 1 calc R . .
H64B H 1.0098 0.3133 0.3281 0.082 Uiso 1 1 calc R . .
C65 C 1.0162(6) 0.2128(4) 0.2582(3) 0.085(2) Uani 1 1 d . . .
H65A H 0.9412 0.2076 0.2379 0.102 Uiso 1 1 calc R . .
H65B H 1.0544 0.2361 0.2366 0.102 Uiso 1 1 calc R . .
C66 C 1.0484(6) 0.1376(4) 0.2487(3) 0.094(2) Uani 1 1 d . . .
H66A H 1.0409 0.1098 0.2038 0.141 Uiso 1 1 calc R . .
H66B H 1.0045 0.1111 0.2648 0.141 Uiso 1 1 calc R . .
H66C H 1.1213 0.1419 0.2712 0.141 Uiso 1 1 calc R . .
C67 C 0.3839(4) 0.6258(3) 0.3322(2) 0.0596(14) Uani 1 1 d . . .
H67A H 0.3562 0.5822 0.3385 0.089 Uiso 1 1 calc R . .
H67B H 0.4329 0.6108 0.3054 0.089 Uiso 1 1 calc R . .
H67C H 0.3266 0.6469 0.3121 0.089 Uiso 1 1 calc R . .
C68 C 0.3635(4) 0.7077(3) 0.4334(2) 0.0484(12) Uani 1 1 d . . .
H68A H 0.3567 0.6726 0.4549 0.058 Uiso 1 1 calc R . .
H68B H 0.2945 0.7065 0.4061 0.058 Uiso 1 1 calc R . .
C69 C 0.5232(4) 0.6480(3) 0.4229(2) 0.0478(12) Uani 1 1 d . . .
H69A H 0.5720 0.6329 0.3954 0.057 Uiso 1 1 calc R . .
H69B H 0.4929 0.6023 0.4259 0.057 Uiso 1 1 calc R . .
C70 C 0.5831(3) 0.6989(3) 0.4876(2) 0.0423(11) Uani 1 1 d . . .
C71 C 0.6303(3) 0.7665(3) 0.4926(2) 0.0420(11) Uani 1 1 d . . .
C72 C 0.6818(4) 0.8172(3) 0.5530(2) 0.0500(12) Uani 1 1 d . . .
C73 C 0.6857(4) 0.7979(3) 0.6043(2) 0.0530(13) Uani 1 1 d . . .
H73A H 0.7199 0.8325 0.6448 0.064 Uiso 1 1 calc R . .
C74 C 0.6412(4) 0.7294(3) 0.5986(2) 0.0538(13) Uani 1 1 d . . .
C75 C 0.5894(4) 0.6809(3) 0.5401(2) 0.0484(12) Uani 1 1 d . . .
H75A H 0.5573 0.6340 0.5356 0.058 Uiso 1 1 calc R . .
C76 C 0.3956(4) 0.7845(3) 0.4813(2) 0.0472(12) Uani 1 1 d . . .
C77 C 0.3681(4) 0.8078(3) 0.5384(2) 0.0557(13) Uani 1 1 d . . .
H77A H 0.3304 0.7737 0.5492 0.067 Uiso 1 1 calc R . .
C78 C 0.3958(5) 0.8806(3) 0.5792(3) 0.0650(16) Uani 1 1 d . . .
H78A H 0.3766 0.8972 0.6182 0.078 Uiso 1 1 calc R . .
C79 C 0.4511(5) 0.9291(3) 0.5635(2) 0.0638(15) Uani 1 1 d . . .
H79A H 0.4714 0.9794 0.5913 0.077 Uiso 1 1 calc R . .
C80 C 0.4765(4) 0.9027(3) 0.5059(2) 0.0528(13) Uani 1 1 d . . .
H80A H 0.5150 0.9359 0.4946 0.063 Uiso 1 1 calc R . .
C81 C 0.7649(6) 0.9394(3) 0.6151(3) 0.094(2) Uani 1 1 d . . .
H81A H 0.7928 0.9842 0.6106 0.141 Uiso 1 1 calc R . .
H81B H 0.8205 0.9208 0.6390 0.141 Uiso 1 1 calc R . .
H81C H 0.7093 0.9516 0.6374 0.141 Uiso 1 1 calc R . .
C82 C 0.6502(5) 0.7090(4) 0.6569(3) 0.0802(19) Uani 1 1 d . . .
H82A H 0.6342 0.6549 0.6439 0.120 Uiso 1 1 calc R . .
H82B H 0.6010 0.7346 0.6807 0.120 Uiso 1 1 calc R . .
H82C H 0.7212 0.7244 0.6834 0.120 Uiso 1 1 calc R . .
C83 C 0.6421(6) 0.7435(4) 0.2997(4) 0.108(3) Uani 1 1 d D . .
H83A H 0.6986 0.7638 0.3385 0.130 Uiso 1 1 calc R B 1
H83B H 0.6303 0.7837 0.2828 0.130 Uiso 1 1 calc R B 1
C84 C 0.6799(11) 0.6849(7) 0.2553(5) 0.122(7) Uani 0.55 1 d PD C 1
H84A H 0.7456 0.7049 0.2503 0.146 Uiso 0.55 1 calc PR C 1
H84B H 0.6289 0.6692 0.2141 0.146 Uiso 0.55 1 calc PR C 1
C84' C 0.7343(10) 0.7017(6) 0.2964(8) 0.115(7) Uani 0.45 1 d PD C 2
H84C H 0.7820 0.7170 0.3386 0.139 Uiso 0.45 1 calc PR C 2
H84D H 0.7722 0.7129 0.2681 0.139 Uiso 0.45 1 calc PR C 2
C85 C 0.6994(8) 0.6184(4) 0.2717(4) 0.132(4) Uani 1 1 d D . .
H85A H 0.7117 0.5779 0.2354 0.199 Uiso 1 1 calc R C 1
H85B H 0.6388 0.6028 0.2835 0.199 Uiso 1 1 calc R C 1
H85C H 0.7607 0.6305 0.3070 0.199 Uiso 1 1 calc R C 1
C86 C 0.3045(5) 0.8384(4) 0.3385(3) 0.094(2) Uani 1 1 d . . .
H86A H 0.3320 0.8692 0.3181 0.113 Uiso 1 1 calc R . .
H86B H 0.3055 0.8711 0.3820 0.113 Uiso 1 1 calc R . .
C87 C 0.1970(6) 0.8073(5) 0.3041(3) 0.114(3) Uani 1 1 d DU . .
H87A H 0.1974 0.7797 0.2597 0.137 Uiso 1 1 calc R . .
H87B H 0.1759 0.7701 0.3208 0.137 Uiso 1 1 calc R . .
C88 C 0.1152(5) 0.8575(4) 0.3047(4) 0.110(3) Uani 1 1 d DU . .
H88A H 0.0489 0.8286 0.2785 0.164 Uiso 1 1 calc R . .
H88B H 0.1336 0.8948 0.2880 0.164 Uiso 1 1 calc R . .
H88C H 0.1088 0.8827 0.3478 0.164 Uiso 1 1 calc R . .
C89 C 0.2725(4) 0.0326(3) 0.9825(3) 0.0785(19) Uani 1 1 d . . .
H89A H 0.2013 0.0103 0.9771 0.094 Uiso 1 1 calc R . .
H89B H 0.2731 0.0875 0.9989 0.094 Uiso 1 1 calc R . .
C90 C 0.7885(5) 0.4712(3) 0.0103(3) 0.0710(16) Uani 1 1 d D . .
H90A H 0.7619 0.4182 -0.0023 0.085 Uiso 1 1 calc R A 1
H90B H 0.7283 0.5006 0.0110 0.085 Uiso 1 1 calc R A 1
C91 C 0.6437(5) 0.3892(3) 0.4190(3) 0.0719(17) Uani 1 1 d . . .
H91A H 0.6055 0.3445 0.4191 0.086 Uiso 1 1 calc R . .
H91B H 0.7188 0.3877 0.4350 0.086 Uiso 1 1 calc R . .
C92 C 0.2269(5) 0.0669(4) 0.5579(4) 0.108(3) Uani 1 1 d . . .
H92A H 0.2852 0.0634 0.5909 0.130 Uiso 1 1 calc R . .
H92B H 0.2511 0.1037 0.5418 0.130 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.598(3) . ?
V1 O4 1.809(3) . ?
V1 O3 1.825(3) . ?
V1 O2 1.915(3) . ?
V1 N2 2.188(4) . ?
V1 N1 2.388(4) . ?
V2 O6 1.601(3) . ?
V2 O8 1.804(4) . ?
V2 O9 1.816(3) . ?
V2 O7 1.927(3) . ?
V2 N4 2.189(4) . ?
V2 N3 2.401(4) . ?
V3 O11 1.594(3) . ?
V3 O13 1.808(3) . ?
V3 O14 1.817(3) . ?
V3 O12 1.917(3) . ?
V3 N6 2.198(4) . ?
V3 N5 2.393(4) . ?
V4 O16 1.606(4) . ?
V4 O18 1.792(3) . ?
V4 O19 1.809(3) . ?
V4 O17 1.955(3) . ?
V4 N8 2.187(4) . ?
V4 N7 2.389(4) . ?
Cl1 C89 1.725(7) . ?
Cl2 C89 1.725(7) . ?
Cl3 C90 1.737(6) . ?
Cl3' C90 1.699(7) . ?
Cl4 C90 1.750(6) . ?
Cl5 C91 1.739(6) . ?
Cl6 C91 1.738(6) . ?
Cl7 C92 1.722(8) . ?
Cl8 C92 1.734(8) . ?
N1 C2 1.472(5) . ?
N1 C1 1.484(6) . ?
N1 C3 1.490(5) . ?
N2 C10 1.339(5) . ?
N2 C14 1.343(6) . ?
N3 C24 1.478(6) . ?
N3 C23 1.480(6) . ?
N3 C25 1.494(6) . ?
N4 C32 1.334(5) . ?
N4 C36 1.338(6) . ?
N5 C45 1.477(6) . ?
N5 C46 1.487(6) . ?
N5 C47 1.491(6) . ?
N6 C58 1.337(6) . ?
N6 C54 1.350(6) . ?
N7 C68 1.480(6) . ?
N7 C67 1.483(5) . ?
N7 C69 1.483(6) . ?
N8 C80 1.333(6) . ?
N8 C76 1.349(6) . ?
O2 C5 1.354(5) . ?
O3 C17 1.405(6) . ?
O4 C20 1.403(6) . ?
O5 C6 1.383(6) . ?
O5 C15 1.417(6) . ?
O7 C27 1.338(5) . ?
O8 C39 1.403(6) . ?
O9 C42 1.401(6) . ?
O10 C28 1.373(6) . ?
O10 C37 1.424(7) . ?
O12 C49 1.345(5) . ?
O13 C61 1.409(6) . ?
O14 C64 1.404(6) . ?
O15 C50 1.364(6) . ?
O15 C59 1.425(6) . ?
O17 C71 1.340(5) . ?
O18 C83 1.376(7) . ?
O19 C86 1.421(7) . ?
O20 C72 1.371(6) . ?
O20 C81 1.420(6) . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C2 C10 1.495(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.493(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.389(6) . ?
C4 C9 1.396(6) . ?
C5 C6 1.404(7) . ?
C6 C7 1.394(6) . ?
C7 C8 1.388(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.380(7) . ?
C8 C16 1.515(7) . ?
C9 H9A 0.9500 . ?
C10 C11 1.404(6) . ?
C11 C12 1.370(7) . ?
C11 H11B 0.9500 . ?
C12 C13 1.389(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.362(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 H16D 0.9800 . ?
C17 C18 1.490(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.495(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.444(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.504(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C32 1.495(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.485(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.393(6) . ?
C26 C31 1.397(6) . ?
C27 C28 1.404(7) . ?
C28 C29 1.383(7) . ?
C29 C30 1.371(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.376(7) . ?
C30 C38 1.525(7) . ?
C31 H31A 0.9500 . ?
C32 C33 1.387(6) . ?
C33 C34 1.361(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.379(7) . ?
C34 H34A 0.9500 . ?
C35 C36 1.365(7) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.504(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.454(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.520(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.484(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
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 C54 1.488(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.502(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.387(7) . ?
C48 C53 1.387(7) . ?
C49 C50 1.406(7) . ?
C50 C51 1.391(7) . ?
C51 C52 1.392(8) . ?
C51 H51A 0.9500 . ?
C52 C53 1.383(7) . ?
C52 C60 1.533(7) . ?
C53 H53A 0.9500 . ?
C54 C55 1.382(6) . ?
C55 C56 1.378(7) . ?
C55 H55A 0.9500 . ?
C56 C57 1.380(7) . ?
C56 H56A 0.9500 . ?
C57 C58 1.367(7) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
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 1.476(8) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.437(9) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.515(8) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.476(9) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C76 1.491(7) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.511(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C75 1.380(6) . ?
C70 C71 1.388(6) . ?
C71 C72 1.412(6) . ?
C72 C73 1.370(7) . ?
C73 C74 1.383(7) . ?
C73 H73A 0.9500 . ?
C74 C75 1.372(7) . ?
C74 C82 1.535(7) . ?
C75 H75A 0.9500 . ?
C76 C77 1.388(7) . ?
C77 C78 1.377(7) . ?
C77 H77A 0.9500 . ?
C78 C79 1.370(8) . ?
C78 H78A 0.9500 . ?
C79 C80 1.386(7) . ?
C79 H79A 0.9500 . ?
C80 H80A 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C84 1.429(8) . ?
C83 C84' 1.482(9) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 C85 1.476(9) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84' C85 1.522(9) . ?
C84' H84C 0.9900 . ?
C84' H84D 0.9900 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 C87 1.469(9) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C87 C88 1.470(7) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9900 . ?
C92 H92B 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
O1 V1 O4 104.10(16) . . ?
O1 V1 O3 96.39(16) . . ?
O4 V1 O3 96.72(14) . . ?
O1 V1 O2 99.12(15) . . ?
O4 V1 O2 93.30(13) . . ?
O3 V1 O2 158.89(14) . . ?
O1 V1 N2 93.23(15) . . ?
O4 V1 N2 162.47(15) . . ?
O3 V1 N2 83.71(14) . . ?
O2 V1 N2 81.20(13) . . ?
O1 V1 N1 166.56(15) . . ?
O4 V1 N1 88.96(14) . . ?
O3 V1 N1 78.64(14) . . ?
O2 V1 N1 83.03(13) . . ?
N2 V1 N1 73.90(13) . . ?
O6 V2 O8 103.58(18) . . ?
O6 V2 O9 97.38(17) . . ?
O8 V2 O9 96.94(16) . . ?
O6 V2 O7 99.78(16) . . ?
O8 V2 O7 92.25(15) . . ?
O9 V2 O7 158.05(14) . . ?
O6 V2 N4 92.01(17) . . ?
O8 V2 N4 163.90(16) . . ?
O9 V2 N4 84.82(15) . . ?
O7 V2 N4 81.01(13) . . ?
O6 V2 N3 164.92(17) . . ?
O8 V2 N3 91.23(16) . . ?
O9 V2 N3 77.67(14) . . ?
O7 V2 N3 82.26(13) . . ?
N4 V2 N3 73.46(14) . . ?
O11 V3 O13 104.09(17) . . ?
O11 V3 O14 97.01(17) . . ?
O13 V3 O14 96.76(15) . . ?
O11 V3 O12 98.13(16) . . ?
O13 V3 O12 91.98(14) . . ?
O14 V3 O12 160.13(15) . . ?
O11 V3 N6 91.84(16) . . ?
O13 V3 N6 163.52(16) . . ?
O14 V3 N6 85.27(15) . . ?
O12 V3 N6 81.45(13) . . ?
O11 V3 N5 165.29(17) . . ?
O13 V3 N5 90.55(16) . . ?
O14 V3 N5 79.54(15) . . ?
O12 V3 N5 82.57(14) . . ?
N6 V3 N5 73.68(14) . . ?
O16 V4 O18 104.04(17) . . ?
O16 V4 O19 98.99(17) . . ?
O18 V4 O19 99.52(16) . . ?
O16 V4 O17 96.30(16) . . ?
O18 V4 O17 91.80(14) . . ?
O19 V4 O17 158.13(15) . . ?
O16 V4 N8 93.44(16) . . ?
O18 V4 N8 161.01(16) . . ?
O19 V4 N8 84.76(15) . . ?
O17 V4 N8 78.78(13) . . ?
O16 V4 N7 167.62(16) . . ?
O18 V4 N7 88.33(15) . . ?
O19 V4 N7 79.01(15) . . ?
O17 V4 N7 82.70(13) . . ?
N8 V4 N7 74.24(14) . . ?
C2 N1 C1 109.3(4) . . ?
C2 N1 C3 111.6(4) . . ?
C1 N1 C3 107.4(4) . . ?
C2 N1 V1 106.5(3) . . ?
C1 N1 V1 109.6(3) . . ?
C3 N1 V1 112.3(3) . . ?
C10 N2 C14 119.1(4) . . ?
C10 N2 V1 118.5(3) . . ?
C14 N2 V1 122.4(3) . . ?
C24 N3 C23 109.1(4) . . ?
C24 N3 C25 111.7(4) . . ?
C23 N3 C25 107.2(4) . . ?
C24 N3 V2 105.4(3) . . ?
C23 N3 V2 110.5(3) . . ?
C25 N3 V2 113.0(3) . . ?
C32 N4 C36 118.9(4) . . ?
C32 N4 V2 119.2(3) . . ?
C36 N4 V2 121.7(3) . . ?
C45 N5 C46 109.5(4) . . ?
C45 N5 C47 107.7(4) . . ?
C46 N5 C47 110.5(4) . . ?
C45 N5 V3 110.3(3) . . ?
C46 N5 V3 105.8(3) . . ?
C47 N5 V3 113.1(3) . . ?
C58 N6 C54 118.2(4) . . ?
C58 N6 V3 122.0(3) . . ?
C54 N6 V3 119.2(3) . . ?
C68 N7 C67 109.5(4) . . ?
C68 N7 C69 111.7(4) . . ?
C67 N7 C69 107.5(4) . . ?
C68 N7 V4 106.6(3) . . ?
C67 N7 V4 110.1(3) . . ?
C69 N7 V4 111.5(3) . . ?
C80 N8 C76 119.3(4) . . ?
C80 N8 V4 121.2(3) . . ?
C76 N8 V4 119.0(3) . . ?
C5 O2 V1 130.9(3) . . ?
C17 O3 V1 126.0(3) . . ?
C20 O4 V1 122.2(3) . . ?
C6 O5 C15 116.5(4) . . ?
C27 O7 V2 130.0(3) . . ?
C39 O8 V2 121.5(4) . . ?
C42 O9 V2 129.2(4) . . ?
C28 O10 C37 116.6(4) . . ?
C49 O12 V3 131.6(3) . . ?
C61 O13 V3 121.1(3) . . ?
C64 O14 V3 127.0(3) . . ?
C50 O15 C59 118.1(4) . . ?
C71 O17 V4 129.4(3) . . ?
C83 O18 V4 126.5(4) . . ?
C86 O19 V4 128.4(4) . . ?
C72 O20 C81 116.5(4) . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N1 C2 C10 112.1(4) . . ?
N1 C2 H2A 109.2 . . ?
C10 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C10 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C4 114.4(4) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C9 119.7(4) . . ?
C5 C4 C3 118.3(4) . . ?
C9 C4 C3 122.0(4) . . ?
O2 C5 C4 121.1(4) . . ?
O2 C5 C6 119.8(4) . . ?
C4 C5 C6 119.1(4) . . ?
O5 C6 C7 124.4(4) . . ?
O5 C6 C5 115.2(4) . . ?
C7 C6 C5 120.3(5) . . ?
C8 C7 C6 120.3(5) . . ?
C8 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C9 C8 C7 119.2(5) . . ?
C9 C8 C16 120.8(5) . . ?
C7 C8 C16 120.0(5) . . ?
C8 C9 C4 121.4(5) . . ?
C8 C9 H9A 119.3 . . ?
C4 C9 H9A 119.3 . . ?
N2 C10 C11 120.9(4) . . ?
N2 C10 C2 117.8(4) . . ?
C11 C10 C2 121.2(4) . . ?
C12 C11 C10 119.1(5) . . ?
C12 C11 H11B 120.4 . . ?
C10 C11 H11B 120.4 . . ?
C11 C12 C13 119.4(5) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
N2 C14 C13 123.0(5) . . ?
N2 C14 H14A 118.5 . . ?
C13 C14 H14A 118.5 . . ?
O5 C15 H15A 109.5 . . ?
O5 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O5 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C8 C16 H16B 109.5 . . ?
C8 C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C16 H16D 109.5 . . ?
H16B C16 H16D 109.5 . . ?
H16C C16 H16D 109.5 . . ?
O3 C17 C18 111.0(5) . . ?
O3 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
O3 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 C19 115.1(5) . . ?
C17 C18 H18A 108.5 . . ?
C19 C18 H18A 108.5 . . ?
C17 C18 H18B 108.5 . . ?
C19 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 C21 115.2(5) . . ?
O4 C20 H20A 108.5 . . ?
C21 C20 H20A 108.5 . . ?
O4 C20 H20B 108.5 . . ?
C21 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 C22 114.0(6) . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 C32 111.6(4) . . ?
N3 C24 H24A 109.3 . . ?
C32 C24 H24A 109.3 . . ?
N3 C24 H24B 109.3 . . ?
C32 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C26 C25 N3 113.1(4) . . ?
C26 C25 H25A 109.0 . . ?
N3 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
N3 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C27 C26 C31 119.6(4) . . ?
C27 C26 C25 118.5(4) . . ?
C31 C26 C25 121.9(4) . . ?
O7 C27 C26 121.0(4) . . ?
O7 C27 C28 120.4(4) . . ?
C26 C27 C28 118.5(4) . . ?
O10 C28 C29 125.8(5) . . ?
O10 C28 C27 114.3(4) . . ?
C29 C28 C27 119.9(5) . . ?
C30 C29 C28 121.9(5) . . ?
C30 C29 H29A 119.0 . . ?
C28 C29 H29A 119.0 . . ?
C29 C30 C31 118.3(5) . . ?
C29 C30 C38 120.8(5) . . ?
C31 C30 C38 120.9(5) . . ?
C30 C31 C26 121.7(5) . . ?
C30 C31 H31A 119.2 . . ?
C26 C31 H31A 119.2 . . ?
N4 C32 C33 120.7(5) . . ?
N4 C32 C24 116.7(4) . . ?
C33 C32 C24 122.6(4) . . ?
C34 C33 C32 120.4(5) . . ?
C34 C33 H33A 119.8 . . ?
C32 C33 H33A 119.8 . . ?
C33 C34 C35 118.5(5) . . ?
C33 C34 H34A 120.8 . . ?
C35 C34 H34A 120.8 . . ?
C36 C35 C34 118.9(5) . . ?
C36 C35 H35A 120.6 . . ?
C34 C35 H35A 120.6 . . ?
N4 C36 C35 122.7(5) . . ?
N4 C36 H36A 118.6 . . ?
C35 C36 H36A 118.6 . . ?
O10 C37 H37A 109.5 . . ?
O10 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O10 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C30 C38 H38A 109.5 . . ?
C30 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C30 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O8 C39 C40 112.0(6) . . ?
O8 C39 H39A 109.2 . . ?
C40 C39 H39A 109.2 . . ?
O8 C39 H39B 109.2 . . ?
C40 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C41 C40 C39 108.8(8) . . ?
C41 C40 H40A 109.9 . . ?
C39 C40 H40A 109.9 . . ?
C41 C40 H40B 109.9 . . ?
C39 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O9 C42 C43 110.7(5) . . ?
O9 C42 H42A 109.5 . . ?
C43 C42 H42A 109.5 . . ?
O9 C42 H42B 109.5 . . ?
C43 C42 H42B 109.5 . . ?
H42A C42 H42B 108.1 . . ?
C44 C43 C42 113.6(6) . . ?
C44 C43 H43A 108.8 . . ?
C42 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C42 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
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 . . ?
N5 C45 H45A 109.5 . . ?
N5 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N5 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N5 C46 C54 112.1(4) . . ?
N5 C46 H46A 109.2 . . ?
C54 C46 H46A 109.2 . . ?
N5 C46 H46B 109.2 . . ?
C54 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
N5 C47 C48 115.1(4) . . ?
N5 C47 H47A 108.5 . . ?
C48 C47 H47A 108.5 . . ?
N5 C47 H47B 108.5 . . ?
C48 C47 H47B 108.5 . . ?
H47A C47 H47B 107.5 . . ?
C49 C48 C53 120.8(5) . . ?
C49 C48 C47 117.9(4) . . ?
C53 C48 C47 121.1(5) . . ?
O12 C49 C48 121.7(4) . . ?
O12 C49 C50 119.3(5) . . ?
C48 C49 C50 119.0(5) . . ?
O15 C50 C51 125.2(5) . . ?
O15 C50 C49 115.3(4) . . ?
C51 C50 C49 119.5(5) . . ?
C50 C51 C52 121.1(5) . . ?
C50 C51 H51A 119.4 . . ?
C52 C51 H51A 119.4 . . ?
C53 C52 C51 118.9(5) . . ?
C53 C52 C60 121.4(6) . . ?
C51 C52 C60 119.8(5) . . ?
C52 C53 C48 120.7(5) . . ?
C52 C53 H53A 119.7 . . ?
C48 C53 H53A 119.7 . . ?
N6 C54 C55 121.0(4) . . ?
N6 C54 C46 115.8(4) . . ?
C55 C54 C46 123.0(5) . . ?
C56 C55 C54 119.8(5) . . ?
C56 C55 H55A 120.1 . . ?
C54 C55 H55A 120.1 . . ?
C55 C56 C57 118.9(5) . . ?
C55 C56 H56A 120.5 . . ?
C57 C56 H56A 120.5 . . ?
C58 C57 C56 118.3(5) . . ?
C58 C57 H57A 120.9 . . ?
C56 C57 H57A 120.9 . . ?
N6 C58 C57 123.7(5) . . ?
N6 C58 H58A 118.2 . . ?
C57 C58 H58A 118.2 . . ?
O15 C59 H59A 109.5 . . ?
O15 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
O15 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C52 C60 H60A 109.5 . . ?
C52 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C52 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O13 C61 C62 113.2(5) . . ?
O13 C61 H61A 108.9 . . ?
C62 C61 H61A 108.9 . . ?
O13 C61 H61B 108.9 . . ?
C62 C61 H61B 108.9 . . ?
H61A C61 H61B 107.7 . . ?
C63 C62 C61 114.3(7) . . ?
C63 C62 H62A 108.7 . . ?
C61 C62 H62A 108.7 . . ?
C63 C62 H62B 108.7 . . ?
C61 C62 H62B 108.7 . . ?
H62A C62 H62B 107.6 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O14 C64 C65 110.3(5) . . ?
O14 C64 H64A 109.6 . . ?
C65 C64 H64A 109.6 . . ?
O14 C64 H64B 109.6 . . ?
C65 C64 H64B 109.6 . . ?
H64A C64 H64B 108.1 . . ?
C66 C65 C64 115.1(5) . . ?
C66 C65 H65A 108.5 . . ?
C64 C65 H65A 108.5 . . ?
C66 C65 H65B 108.5 . . ?
C64 C65 H65B 108.5 . . ?
H65A C65 H65B 107.5 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N7 C67 H67A 109.5 . . ?
N7 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N7 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N7 C68 C76 112.6(4) . . ?
N7 C68 H68A 109.1 . . ?
C76 C68 H68A 109.1 . . ?
N7 C68 H68B 109.1 . . ?
C76 C68 H68B 109.1 . . ?
H68A C68 H68B 107.8 . . ?
N7 C69 C70 113.4(4) . . ?
N7 C69 H69A 108.9 . . ?
C70 C69 H69A 108.9 . . ?
N7 C69 H69B 108.9 . . ?
C70 C69 H69B 108.9 . . ?
H69A C69 H69B 107.7 . . ?
C75 C70 C71 120.7(4) . . ?
C75 C70 C69 122.3(4) . . ?
C71 C70 C69 116.9(4) . . ?
O17 C71 C70 122.1(4) . . ?
O17 C71 C72 119.7(4) . . ?
C70 C71 C72 118.2(4) . . ?
C73 C72 O20 125.3(5) . . ?
C73 C72 C71 119.7(5) . . ?
O20 C72 C71 115.0(4) . . ?
C72 C73 C74 121.7(5) . . ?
C72 C73 H73A 119.1 . . ?
C74 C73 H73A 119.1 . . ?
C75 C74 C73 118.6(5) . . ?
C75 C74 C82 121.3(5) . . ?
C73 C74 C82 120.2(5) . . ?
C74 C75 C70 121.1(5) . . ?
C74 C75 H75A 119.5 . . ?
C70 C75 H75A 119.5 . . ?
N8 C76 C77 120.6(5) . . ?
N8 C76 C68 116.9(4) . . ?
C77 C76 C68 122.5(5) . . ?
C78 C77 C76 119.4(5) . . ?
C78 C77 H77A 120.3 . . ?
C76 C77 H77A 120.3 . . ?
C79 C78 C77 119.9(5) . . ?
C79 C78 H78A 120.0 . . ?
C77 C78 H78A 120.0 . . ?
C78 C79 C80 118.1(5) . . ?
C78 C79 H79A 121.0 . . ?
C80 C79 H79A 121.0 . . ?
N8 C80 C79 122.7(5) . . ?
N8 C80 H80A 118.7 . . ?
C79 C80 H80A 118.7 . . ?
O20 C81 H81A 109.5 . . ?
O20 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O20 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C74 C82 H82A 109.5 . . ?
C74 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C74 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O18 C83 C84 119.9(9) . . ?
O18 C83 C84' 128.9(9) . . ?
O18 C83 H83A 107.4 . . ?
C84 C83 H83A 107.4 . . ?
C84' C83 H83A 67.1 . . ?
O18 C83 H83B 107.4 . . ?
C84 C83 H83B 107.4 . . ?
C84' C83 H83B 123.1 . . ?
H83A C83 H83B 106.9 . . ?
C83 C84 C85 115.2(9) . . ?
C83 C84 H84A 108.5 . . ?
C85 C84 H84A 108.5 . . ?
C83 C84 H84B 108.5 . . ?
C85 C84 H84B 108.5 . . ?
H84A C84 H84B 107.5 . . ?
C83 C84' C85 109.5(9) . . ?
C83 C84' H84C 109.8 . . ?
C85 C84' H84C 109.8 . . ?
C83 C84' H84D 109.8 . . ?
C85 C84' H84D 109.8 . . ?
H84C C84' H84D 108.2 . . ?
C84 C85 H85A 109.5 . . ?
C84' C85 H85A 130.2 . . ?
C84 C85 H85B 109.5 . . ?
C84' C85 H85B 117.2 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
C84' C85 H85C 70.8 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O19 C86 C87 111.3(6) . . ?
O19 C86 H86A 109.4 . . ?
C87 C86 H86A 109.4 . . ?
O19 C86 H86B 109.4 . . ?
C87 C86 H86B 109.4 . . ?
H86A C86 H86B 108.0 . . ?
C88 C87 C86 119.4(7) . . ?
C88 C87 H87A 107.5 . . ?
C86 C87 H87A 107.5 . . ?
C88 C87 H87B 107.5 . . ?
C86 C87 H87B 107.5 . . ?
H87A C87 H87B 107.0 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
Cl2 C89 Cl1 112.2(3) . . ?
Cl2 C89 H89A 109.2 . . ?
Cl1 C89 H89A 109.2 . . ?
Cl2 C89 H89B 109.2 . . ?
Cl1 C89 H89B 109.2 . . ?
H89A C89 H89B 107.9 . . ?
Cl3' C90 Cl4 115.2(4) . . ?
Cl3 C90 Cl4 110.8(3) . . ?
Cl3' C90 H90A 130.2 . . ?
Cl3 C90 H90A 109.5 . . ?
Cl4 C90 H90A 109.5 . . ?
Cl3' C90 H90B 77.0 . . ?
Cl3 C90 H90B 109.5 . . ?
Cl4 C90 H90B 109.5 . . ?
H90A C90 H90B 108.1 . . ?
Cl6 C91 Cl5 111.7(3) . . ?
Cl6 C91 H91A 109.3 . . ?
Cl5 C91 H91A 109.3 . . ?
Cl6 C91 H91B 109.3 . . ?
Cl5 C91 H91B 109.3 . . ?
H91A C91 H91B 107.9 . . ?
Cl7 C92 Cl8 112.7(4) . . ?
Cl7 C92 H92A 109.1 . . ?
Cl8 C92 H92A 109.1 . . ?
Cl7 C92 H92B 109.1 . . ?
Cl8 C92 H92B 109.1 . . ?
H92A C92 H92B 107.8 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.75
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 994168'
