# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Carl Redshaw'
_publ_contact_author_email       CARL.REDSHAW@UEA.AC.UK

_publ_section_title              
;
Vanadium-based imido-alkoxide procatalysts bearing
bisphenolate ligands for ethylene and \%a-caprolactone polymerisation.
;
loop_
_publ_author_name
'Carl Redshaw'
'Abdessamad Arbaoui'
'Mark Elsegood'
'Damien M Homden'
'Joseph Wright'

# Attachment 'Di-phenolates.cif.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 718351'

_chemical_name_common            'Compound 1'
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H60 N O3 V'
_chemical_formula_sum            'C41 H60 N O3 V'
_chemical_formula_weight         665.84

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   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   10.9243(7)
_cell_length_b                   18.3726(11)
_cell_length_c                   20.1620(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7902(11)
_cell_angle_gamma                90.00
_cell_volume                     4046.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7087
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      28.76

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   'SADABS v2.08, Sheldrick, G.M., (2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18044
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         29.03
_reflns_number_total             5043
_reflns_number_gt                4038
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0526P)^2^+4.6627P] where P=(Fo^2^+2Fc^2^)/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         5043
_refine_ls_number_parameters     249
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1175
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.44552(3) 0.0000 0.624720(18) 0.01999(11) Uani 1 2 d S . .
O1 O 0.34876(14) 0.0000 0.55476(8) 0.0260(3) Uani 1 2 d S . .
C1 C 0.2251(2) 0.0000 0.52865(11) 0.0289(5) Uani 1 2 d S . .
C2 C 0.21193(17) 0.06903(11) 0.48706(9) 0.0365(4) Uani 1 1 d . . .
H2A H 0.2201 0.1118 0.5159 0.055 Uiso 1 1 calc R . .
H2B H 0.1313 0.0696 0.4651 0.055 Uiso 1 1 calc R . .
H2C H 0.2759 0.0701 0.4535 0.055 Uiso 1 1 calc R . .
C3 C 0.1355(2) 0.0000 0.58597(14) 0.0427(7) Uani 1 2 d S . .
H3A H 0.1407 0.0466 0.6094 0.064 Uiso 0.50 1 calc PR . .
H3B H 0.1563 -0.0396 0.6167 0.064 Uiso 0.50 1 calc PR . .
H3C H 0.0521 -0.0070 0.5687 0.064 Uiso 0.50 1 calc PR . .
N1 N 0.37090(17) 0.0000 0.69569(10) 0.0258(4) Uani 1 2 d S . .
C5 C 0.3169(2) 0.0000 0.75740(12) 0.0291(5) Uani 1 2 d SU . .
C6 C 0.3805(4) -0.0259(3) 0.81223(19) 0.0524(13) Uani 0.50 1 d PU . .
H6 H 0.4617 -0.0436 0.8076 0.063 Uiso 0.50 1 calc PR . .
C7 C 0.3266(5) -0.0262(3) 0.8738(2) 0.0641(17) Uani 0.50 1 d PU . .
H7 H 0.3712 -0.0447 0.9109 0.077 Uiso 0.50 1 calc PR . .
C8 C 0.2087(3) 0.0000 0.88260(15) 0.0535(8) Uani 1 2 d SU . .
C9 C 0.1473(4) 0.0270(3) 0.8283(2) 0.0491(12) Uani 0.50 1 d PU . .
H9 H 0.0670 0.0457 0.8336 0.059 Uiso 0.50 1 calc PR . .
C10 C 0.1987(3) 0.0277(2) 0.76597(18) 0.0423(10) Uani 0.50 1 d PU . .
H10 H 0.1541 0.0469 0.7292 0.051 Uiso 0.50 1 calc PR . .
C11 C 0.1495(5) 0.0000 0.95072(19) 0.0905(16) Uani 1 2 d SU . .
H11A H 0.2064 0.0211 0.9834 0.136 Uiso 0.50 1 calc PR . .
H11B H 0.1300 -0.0501 0.9635 0.136 Uiso 0.50 1 calc PR . .
H11C H 0.0742 0.0289 0.9490 0.136 Uiso 0.50 1 calc PR . .
O2 O 0.54323(9) 0.07962(6) 0.62839(5) 0.0212(2) Uani 1 1 d . . .
C12 C 0.58743(13) 0.10960(8) 0.68647(7) 0.0204(3) Uani 1 1 d . . .
C13 C 0.54666(14) 0.17873(9) 0.70697(8) 0.0238(3) Uani 1 1 d . . .
C14 C 0.58841(15) 0.20297(9) 0.76883(8) 0.0277(3) Uani 1 1 d . . .
H14 H 0.5606 0.2489 0.7842 0.033 Uiso 1 1 calc R . .
C15 C 0.66925(15) 0.16316(9) 0.80947(8) 0.0266(3) Uani 1 1 d . . .
C16 C 0.71187(14) 0.09727(9) 0.78503(8) 0.0244(3) Uani 1 1 d . . .
H16 H 0.7685 0.0699 0.8111 0.029 Uiso 1 1 calc R . .
C17 C 0.67427(13) 0.07007(8) 0.72363(7) 0.0200(3) Uani 1 1 d . . .
C18 C 0.45664(16) 0.22445(9) 0.66442(9) 0.0298(4) Uani 1 1 d . . .
C19 C 0.50034(19) 0.23150(11) 0.59220(9) 0.0392(4) Uani 1 1 d . . .
H19A H 0.4429 0.2621 0.5670 0.059 Uiso 1 1 calc R . .
H19B H 0.5040 0.1831 0.5719 0.059 Uiso 1 1 calc R . .
H19C H 0.5819 0.2537 0.5919 0.059 Uiso 1 1 calc R . .
C20 C 0.32868(17) 0.18946(12) 0.66525(11) 0.0427(5) Uani 1 1 d . . .
H20A H 0.3020 0.1842 0.7112 0.064 Uiso 1 1 calc R . .
H20B H 0.3319 0.1414 0.6442 0.064 Uiso 1 1 calc R . .
H20C H 0.2706 0.2205 0.6409 0.064 Uiso 1 1 calc R . .
C21 C 0.4448(2) 0.30231(11) 0.69145(11) 0.0456(5) Uani 1 1 d . . .
H21A H 0.3915 0.3308 0.6618 0.068 Uiso 1 1 calc R . .
H21B H 0.5259 0.3250 0.6940 0.068 Uiso 1 1 calc R . .
H21C H 0.4093 0.3008 0.7358 0.068 Uiso 1 1 calc R . .
C22 C 0.70629(18) 0.19140(11) 0.87870(9) 0.0372(4) Uani 1 1 d . . .
C23 C 0.6052(3) 0.1743(3) 0.92605(12) 0.1048(15) Uani 1 1 d . . .
H23A H 0.5976 0.1214 0.9308 0.157 Uiso 1 1 calc R . .
H23B H 0.5280 0.1943 0.9089 0.157 Uiso 1 1 calc R . .
H23C H 0.6242 0.1960 0.9694 0.157 Uiso 1 1 calc R . .
C24 C 0.8251(2) 0.15740(16) 0.90353(12) 0.0616(7) Uani 1 1 d . . .
H24A H 0.8480 0.1787 0.9465 0.092 Uiso 1 1 calc R . .
H24B H 0.8900 0.1668 0.8716 0.092 Uiso 1 1 calc R . .
H24C H 0.8141 0.1048 0.9086 0.092 Uiso 1 1 calc R . .
C25 C 0.7295(4) 0.27385(15) 0.87685(15) 0.0896(12) Uani 1 1 d . . .
H25A H 0.6527 0.2992 0.8665 0.134 Uiso 1 1 calc R . .
H25B H 0.7898 0.2849 0.8427 0.134 Uiso 1 1 calc R . .
H25C H 0.7608 0.2900 0.9202 0.134 Uiso 1 1 calc R . .
C26 C 0.72948(19) 0.0000 0.69564(11) 0.0204(4) Uani 1 2 d S . .
H26 H 0.7110 0.0000 0.6469 0.024 Uiso 1 2 calc SR . .
C27 C 0.8701(2) 0.0000 0.70339(13) 0.0270(5) Uani 1 2 d S . .
H27A H 0.9026 0.0467 0.6881 0.040 Uiso 0.50 1 calc PR . .
H27B H 0.9044 -0.0395 0.6769 0.040 Uiso 0.50 1 calc PR . .
H27C H 0.8925 -0.0071 0.7502 0.040 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.01617(18) 0.0250(2) 0.01874(19) 0.000 -0.00114(13) 0.000
O1 0.0174(7) 0.0379(9) 0.0226(8) 0.000 -0.0030(6) 0.000
C1 0.0172(10) 0.0463(15) 0.0229(11) 0.000 -0.0030(8) 0.000
C2 0.0317(9) 0.0447(11) 0.0331(9) 0.0009(8) -0.0046(7) 0.0083(8)
C3 0.0183(11) 0.077(2) 0.0326(14) 0.000 -0.0007(10) 0.000
N1 0.0208(9) 0.0314(10) 0.0252(10) 0.000 0.0004(7) 0.000
C5 0.0273(12) 0.0362(13) 0.0238(11) 0.000 0.0043(9) 0.000
C6 0.044(2) 0.081(4) 0.0323(19) 0.0089(18) 0.0066(16) 0.028(2)
C7 0.071(3) 0.095(5) 0.0257(18) 0.014(2) 0.0065(18) 0.036(3)
C8 0.0576(19) 0.072(2) 0.0309(15) 0.000 0.0159(14) 0.000
C9 0.0300(18) 0.078(3) 0.039(2) -0.0115(18) 0.0111(15) 0.0025(17)
C10 0.0301(17) 0.069(3) 0.0282(17) -0.0020(16) 0.0014(14) 0.0095(16)
C11 0.093(3) 0.140(5) 0.040(2) 0.000 0.034(2) 0.000
O2 0.0201(5) 0.0226(5) 0.0208(5) -0.0012(4) -0.0012(4) 0.0014(4)
C12 0.0186(7) 0.0230(7) 0.0197(7) -0.0004(6) 0.0013(5) -0.0008(6)
C13 0.0227(7) 0.0228(8) 0.0259(8) -0.0002(6) 0.0006(6) 0.0020(6)
C14 0.0288(8) 0.0254(8) 0.0289(8) -0.0050(7) 0.0020(6) 0.0037(7)
C15 0.0275(8) 0.0300(9) 0.0221(8) -0.0048(6) -0.0013(6) -0.0009(7)
C16 0.0227(7) 0.0265(8) 0.0240(8) 0.0012(6) -0.0018(6) 0.0005(6)
C17 0.0173(7) 0.0197(7) 0.0231(7) -0.0006(6) 0.0016(5) -0.0014(5)
C18 0.0310(9) 0.0256(8) 0.0327(9) -0.0026(7) -0.0055(7) 0.0091(7)
C19 0.0483(11) 0.0353(10) 0.0336(10) 0.0061(8) -0.0062(8) 0.0107(9)
C20 0.0279(9) 0.0422(11) 0.0579(13) -0.0028(10) -0.0070(9) 0.0113(8)
C21 0.0554(13) 0.0301(10) 0.0509(12) -0.0069(9) -0.0134(10) 0.0190(9)
C22 0.0411(10) 0.0438(11) 0.0266(9) -0.0120(8) -0.0055(7) 0.0046(8)
C23 0.0674(18) 0.218(5) 0.0292(12) -0.0331(19) 0.0114(12) -0.038(2)
C24 0.0600(15) 0.0832(19) 0.0409(12) -0.0256(12) -0.0241(11) 0.0164(13)
C25 0.150(3) 0.0503(16) 0.0673(18) -0.0252(14) -0.057(2) 0.0071(18)
C26 0.0193(10) 0.0195(10) 0.0224(10) 0.000 -0.0008(8) 0.000
C27 0.0199(10) 0.0228(11) 0.0383(13) 0.000 0.0004(9) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.657(2) . ?
V1 O1 1.7509(15) . ?
V1 O2 1.8118(11) . ?
O1 C1 1.444(3) . ?
C1 C3 1.524(3) . ?
C1 C2 1.526(2) 6 ?
C1 C2 1.526(2) . ?
N1 C5 1.384(3) . ?
C5 C6 1.382(4) . ?
C5 C10 1.401(4) . ?
C6 C7 1.380(6) . ?
C7 C8 1.389(6) . ?
C8 C9 1.369(5) . ?
C8 C11 1.526(4) . ?
C9 C10 1.383(5) . ?
O2 C12 1.3756(18) . ?
C12 C17 1.403(2) . ?
C12 C13 1.410(2) . ?
C13 C14 1.395(2) . ?
C13 C18 1.544(2) . ?
C14 C15 1.402(2) . ?
C15 C16 1.390(2) . ?
C15 C22 1.538(2) . ?
C16 C17 1.392(2) . ?
C17 C26 1.5326(19) . ?
C18 C21 1.537(2) . ?
C18 C20 1.539(3) . ?
C18 C19 1.544(3) . ?
C22 C23 1.503(3) . ?
C22 C24 1.519(3) . ?
C22 C25 1.536(4) . ?
C26 C27 1.541(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O1 113.39(9) . . ?
N1 V1 O2 105.15(5) . . ?
O1 V1 O2 112.44(4) . . ?
O2 V1 O2 107.69(7) . 6 ?
C1 O1 V1 147.73(14) . . ?
O1 C1 C3 109.30(19) . . ?
O1 C1 C2 106.31(13) . 6 ?
C3 C1 C2 111.12(13) . 6 ?
O1 C1 C2 106.31(13) . . ?
C3 C1 C2 111.12(13) . . ?
C2 C1 C2 112.4(2) 6 . ?
C5 N1 V1 175.73(17) . . ?
N1 C5 C6 120.2(2) . . ?
N1 C5 C10 121.0(2) . . ?
C6 C5 C10 103.3(3) 6 . ?
C6 C5 C10 118.7(3) . . ?
C5 C6 C7 120.3(4) . . ?
C6 C7 C8 121.4(4) . . ?
C9 C8 C7 102.5(3) 6 . ?
C9 C8 C7 117.9(3) . . ?
C9 C8 C11 120.7(3) 6 . ?
C9 C8 C11 120.7(3) . . ?
C7 C8 C11 121.4(3) . . ?
C8 C9 C10 122.0(3) . . ?
C9 C10 C5 119.6(3) . . ?
C12 O2 V1 123.90(9) . . ?
O2 C12 C17 118.30(13) . . ?
O2 C12 C13 120.11(13) . . ?
C17 C12 C13 121.59(14) . . ?
C14 C13 C12 116.67(14) . . ?
C14 C13 C18 121.39(14) . . ?
C12 C13 C18 121.91(14) . . ?
C13 C14 C15 123.47(15) . . ?
C16 C15 C14 117.30(15) . . ?
C16 C15 C22 122.03(15) . . ?
C14 C15 C22 120.67(15) . . ?
C15 C16 C17 122.13(15) . . ?
C16 C17 C12 118.56(14) . . ?
C16 C17 C26 121.08(15) . . ?
C12 C17 C26 120.32(14) . . ?
C21 C18 C20 107.69(16) . . ?
C21 C18 C19 106.57(16) . . ?
C20 C18 C19 109.75(16) . . ?
C21 C18 C13 111.43(14) . . ?
C20 C18 C13 109.77(15) . . ?
C19 C18 C13 111.51(14) . . ?
C23 C22 C24 109.7(2) . . ?
C23 C22 C15 108.63(17) . . ?
C24 C22 C15 111.92(16) . . ?
C23 C22 C25 110.2(3) . . ?
C24 C22 C25 105.8(2) . . ?
C15 C22 C25 110.61(18) . . ?
C17 C26 C17 114.28(17) 6 . ?
C17 C26 C27 111.05(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 0.0 . . . . ?
O2 V1 O1 C1 -119.13(4) . . . . ?
O2 V1 O1 C1 119.13(4) 6 . . . ?
V1 O1 C1 C3 0.0 . . . . ?
V1 O1 C1 C2 -120.01(13) . . . 6 ?
V1 O1 C1 C2 120.01(13) . . . . ?
N1 C5 C6 C7 -179.8(4) . . . . ?
C6 C5 C6 C7 77.9(5) 6 . . . ?
C10 C5 C6 C7 -41.1(5) 6 . . . ?
C10 C5 C6 C7 1.8(6) . . . . ?
C5 C6 C7 C8 -0.7(7) . . . . ?
C6 C7 C8 C9 41.8(6) . . . 6 ?
C6 C7 C8 C9 -0.6(6) . . . . ?
C6 C7 C8 C7 -76.7(5) . . . 6 ?
C6 C7 C8 C11 -179.7(4) . . . . ?
C9 C8 C9 C10 -76.7(4) 6 . . . ?
C7 C8 C9 C10 41.1(5) 6 . . . ?
C7 C8 C9 C10 0.9(6) . . . . ?
C11 C8 C9 C10 179.9(3) . . . . ?
C8 C9 C10 C5 0.2(6) . . . . ?
N1 C5 C10 C9 -180.0(3) . . . . ?
C6 C5 C10 C9 -41.7(4) 6 . . . ?
C6 C5 C10 C9 -1.6(5) . . . . ?
C10 C5 C10 C9 76.4(4) 6 . . . ?
N1 V1 O2 C12 27.60(13) . . . . ?
O1 V1 O2 C12 151.44(11) . . . . ?
O2 V1 O2 C12 -84.15(12) 6 . . . ?
V1 O2 C12 C17 68.58(16) . . . . ?
V1 O2 C12 C13 -112.20(14) . . . . ?
O2 C12 C13 C14 175.20(14) . . . . ?
C17 C12 C13 C14 -5.6(2) . . . . ?
O2 C12 C13 C18 -2.7(2) . . . . ?
C17 C12 C13 C18 176.50(14) . . . . ?
C12 C13 C14 C15 1.5(2) . . . . ?
C18 C13 C14 C15 179.43(16) . . . . ?
C13 C14 C15 C16 2.1(3) . . . . ?
C13 C14 C15 C22 -176.80(17) . . . . ?
C14 C15 C16 C17 -1.7(2) . . . . ?
C22 C15 C16 C17 177.10(16) . . . . ?
C15 C16 C17 C12 -2.1(2) . . . . ?
C15 C16 C17 C26 175.61(15) . . . . ?
O2 C12 C17 C16 -174.82(13) . . . . ?
C13 C12 C17 C16 6.0(2) . . . . ?
O2 C12 C17 C26 7.4(2) . . . . ?
C13 C12 C17 C26 -171.80(14) . . . . ?
C14 C13 C18 C21 12.3(2) . . . . ?
C12 C13 C18 C21 -169.88(16) . . . . ?
C14 C13 C18 C20 -106.89(18) . . . . ?
C12 C13 C18 C20 70.9(2) . . . . ?
C14 C13 C18 C19 131.27(17) . . . . ?
C12 C13 C18 C19 -50.9(2) . . . . ?
C16 C15 C22 C23 -99.0(3) . . . . ?
C14 C15 C22 C23 79.8(3) . . . . ?
C16 C15 C22 C24 22.2(3) . . . . ?
C14 C15 C22 C24 -159.0(2) . . . . ?
C16 C15 C22 C25 139.9(2) . . . . ?
C14 C15 C22 C25 -41.3(3) . . . . ?
C16 C17 C26 C17 80.8(2) . . . 6 ?
C12 C17 C26 C17 -101.52(19) . . . 6 ?
C16 C17 C26 C27 -45.8(2) . . . . ?
C12 C17 C26 C27 131.90(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.051

data_2
_database_code_depnum_ccdc_archive 'CCDC 718352'

_chemical_name_common            'Compound 2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H54 F6 N O3 V'
_chemical_formula_sum            'C41 H54 F6 N O3 V'
_chemical_formula_weight         773.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   10.2039(6)
_cell_length_b                   19.5337(11)
_cell_length_c                   10.3267(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.0073(9)
_cell_angle_gamma                90.00
_cell_volume                     2058.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12813
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      30.56

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24199
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         30.59
_reflns_number_total             12114
_reflns_number_gt                11384
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. 5687 Friedel pairs.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.3491P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12114
_refine_ls_number_parameters     546
_refine_ls_number_restraints     279
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.044
_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 0.21888(2) 0.655189(13) 0.50016(2) 0.02091(6) Uani 1 1 d . . .
O1 O 0.09965(11) 0.65589(8) 0.36960(10) 0.0288(2) Uani 1 1 d . A .
C1 C 0.06913(19) 0.67746(11) 0.24434(17) 0.0328(4) Uani 1 1 d D . .
C2 C 0.1900(3) 0.6906(2) 0.1623(3) 0.0696(9) Uani 1 1 d D A .
H2A H 0.2467 0.7242 0.2059 0.104 Uiso 1 1 calc R . .
H2B H 0.1624 0.7082 0.0773 0.104 Uiso 1 1 calc R . .
H2C H 0.2382 0.6476 0.1512 0.104 Uiso 1 1 calc R . .
C3 C -0.0097(6) 0.6211(2) 0.1802(4) 0.0745(13) Uani 0.807(7) 1 d PDU A 1
F1 F 0.0585(6) 0.56518(14) 0.1748(3) 0.1161(18) Uani 0.807(7) 1 d PDU A 1
F2 F -0.1214(4) 0.6108(3) 0.2475(5) 0.1222(19) Uani 0.807(7) 1 d PDU A 1
F3 F -0.0434(6) 0.6374(3) 0.0579(3) 0.1155(18) Uani 0.807(7) 1 d PDU A 1
C3X C -0.0566(15) 0.6347(8) 0.2243(15) 0.084(4) Uani 0.193(7) 1 d PDU A 2
F1X F -0.0423(19) 0.5673(6) 0.2330(12) 0.089(4) Uani 0.193(7) 1 d PDU A 2
F2X F -0.1529(9) 0.6640(13) 0.3081(13) 0.110(3) Uani 0.193(7) 1 d PDU A 2
F3X F -0.1068(18) 0.6447(11) 0.1033(14) 0.098(4) Uani 0.193(7) 1 d PDU A 2
C4 C -0.0032(3) 0.74658(18) 0.2522(3) 0.0631(7) Uani 1 1 d DU A .
F4 F 0.0752(4) 0.79395(11) 0.3018(3) 0.1148(10) Uani 1 1 d DU . .
F5 F -0.0462(2) 0.76807(12) 0.13638(18) 0.0851(7) Uani 1 1 d DU . .
F6 F -0.1039(3) 0.74337(19) 0.3269(2) 0.1227(11) Uani 1 1 d DU . .
N1 N 0.33508(14) 0.71291(8) 0.48250(14) 0.0251(3) Uani 1 1 d . . .
C5 C 0.43869(16) 0.75803(8) 0.47310(15) 0.0240(3) Uani 1 1 d . . .
C6 C 0.41886(17) 0.82249(9) 0.41569(17) 0.0275(3) Uani 1 1 d . . .
H6 H 0.3337 0.8360 0.3872 0.033 Uiso 1 1 calc R . .
C7 C 0.52406(17) 0.86618(9) 0.40092(19) 0.0297(3) Uani 1 1 d . . .
H7 H 0.5104 0.9097 0.3621 0.036 Uiso 1 1 calc R . .
C8 C 0.65009(17) 0.84739(10) 0.44211(19) 0.0310(4) Uani 1 1 d . . .
C9 C 0.66723(19) 0.78416(11) 0.5022(2) 0.0333(4) Uani 1 1 d . . .
H9 H 0.7521 0.7714 0.5328 0.040 Uiso 1 1 calc R . .
C10 C 0.56351(18) 0.73927(10) 0.51853(18) 0.0313(3) Uani 1 1 d . . .
H10 H 0.5771 0.6964 0.5600 0.038 Uiso 1 1 calc R . .
C11 C 0.7644(2) 0.89467(11) 0.4193(3) 0.0447(5) Uani 1 1 d . . .
H11A H 0.7887 0.8926 0.3280 0.067 Uiso 1 1 calc R . .
H11B H 0.8391 0.8805 0.4739 0.067 Uiso 1 1 calc R . .
H11C H 0.7395 0.9417 0.4413 0.067 Uiso 1 1 calc R . .
O2 O 0.30234(12) 0.57432(6) 0.50992(11) 0.0244(2) Uani 1 1 d . . .
O3 O 0.15172(11) 0.67479(6) 0.65691(11) 0.0240(2) Uani 1 1 d . . .
C12 C 0.42510(16) 0.55758(8) 0.55720(16) 0.0236(3) Uani 1 1 d . . .
C13 C 0.52390(17) 0.53435(8) 0.47552(17) 0.0256(3) Uani 1 1 d . . .
C14 C 0.64726(19) 0.52254(9) 0.5323(2) 0.0299(3) Uani 1 1 d . . .
H14 H 0.7164 0.5081 0.4782 0.036 Uiso 1 1 calc R . .
C15 C 0.67409(18) 0.53092(9) 0.6647(2) 0.0319(4) Uani 1 1 d . B .
C16 C 0.56946(19) 0.54944(9) 0.74281(18) 0.0310(4) Uani 1 1 d . . .
H16 H 0.5839 0.5531 0.8337 0.037 Uiso 1 1 calc R . .
C17 C 0.44548(18) 0.56270(8) 0.69224(16) 0.0260(3) Uani 1 1 d . . .
C18 C 0.50267(18) 0.52557(9) 0.32791(17) 0.0286(3) Uani 1 1 d . . .
C19 C 0.4985(2) 0.59709(10) 0.26655(19) 0.0371(4) Uani 1 1 d . . .
H19A H 0.4263 0.6234 0.3034 0.056 Uiso 1 1 calc R . .
H19B H 0.4848 0.5928 0.1727 0.056 Uiso 1 1 calc R . .
H19C H 0.5816 0.6207 0.2844 0.056 Uiso 1 1 calc R . .
C20 C 0.3773(2) 0.48552(11) 0.29470(19) 0.0374(4) Uani 1 1 d . . .
H20A H 0.3800 0.4410 0.3383 0.056 Uiso 1 1 calc R . .
H20B H 0.3707 0.4786 0.2008 0.056 Uiso 1 1 calc R . .
H20C H 0.3009 0.5114 0.3238 0.056 Uiso 1 1 calc R . .
C21 C 0.6160(2) 0.48629(13) 0.2660(2) 0.0425(5) Uani 1 1 d . . .
H21A H 0.6978 0.5119 0.2790 0.064 Uiso 1 1 calc R . .
H21B H 0.5981 0.4808 0.1731 0.064 Uiso 1 1 calc R . .
H21C H 0.6245 0.4411 0.3066 0.064 Uiso 1 1 calc R . .
C22 C 0.8123(2) 0.52162(11) 0.7218(2) 0.0416(5) Uani 1 1 d DU . .
C23 C 0.9127(4) 0.4987(4) 0.6209(5) 0.086(2) Uani 0.725(6) 1 d PDU B 1
H23A H 0.9109 0.5306 0.5476 0.129 Uiso 0.725(6) 1 calc PR B 1
H23B H 0.8904 0.4526 0.5901 0.129 Uiso 0.725(6) 1 calc PR B 1
H23C H 1.0006 0.4982 0.6606 0.129 Uiso 0.725(6) 1 calc PR B 1
C24 C 0.8137(4) 0.4733(3) 0.8333(6) 0.084(2) Uani 0.725(6) 1 d PDU B 1
H24A H 0.9035 0.4686 0.8673 0.126 Uiso 0.725(6) 1 calc PR B 1
H24B H 0.7812 0.4285 0.8045 0.126 Uiso 0.725(6) 1 calc PR B 1
H24C H 0.7573 0.4911 0.9014 0.126 Uiso 0.725(6) 1 calc PR B 1
C25 C 0.8602(4) 0.5930(2) 0.7672(5) 0.0651(12) Uani 0.725(6) 1 d PDU B 1
H25A H 0.8601 0.6244 0.6933 0.098 Uiso 0.725(6) 1 calc PR B 1
H25B H 0.9494 0.5891 0.8034 0.098 Uiso 0.725(6) 1 calc PR B 1
H25C H 0.8016 0.6105 0.8336 0.098 Uiso 0.725(6) 1 calc PR B 1
C23X C 0.9085(12) 0.5616(9) 0.649(2) 0.115(5) Uani 0.275(6) 1 d PDU B 2
H23D H 0.9961 0.5548 0.6874 0.172 Uiso 0.275(6) 1 calc PR B 2
H23E H 0.8855 0.6102 0.6525 0.172 Uiso 0.275(6) 1 calc PR B 2
H23F H 0.9080 0.5463 0.5586 0.172 Uiso 0.275(6) 1 calc PR B 2
C24X C 0.8491(8) 0.4443(4) 0.7140(9) 0.044(2) Uani 0.275(6) 1 d PDU B 2
H24D H 0.7871 0.4175 0.7646 0.067 Uiso 0.275(6) 1 calc PR B 2
H24E H 0.9380 0.4376 0.7491 0.067 Uiso 0.275(6) 1 calc PR B 2
H24F H 0.8453 0.4294 0.6234 0.067 Uiso 0.275(6) 1 calc PR B 2
C25X C 0.8151(13) 0.5316(9) 0.8737(11) 0.102(5) Uani 0.275(6) 1 d PDU B 2
H25D H 0.7473 0.5030 0.9124 0.154 Uiso 0.275(6) 1 calc PR B 2
H25E H 0.7985 0.5798 0.8943 0.154 Uiso 0.275(6) 1 calc PR B 2
H25F H 0.9013 0.5182 0.9087 0.154 Uiso 0.275(6) 1 calc PR B 2
C26 C 0.33169(18) 0.58347(8) 0.77828(15) 0.0257(3) Uani 1 1 d . . .
H26 H 0.2488 0.5725 0.7295 0.031 Uiso 1 1 calc R . .
C27 C 0.3301(2) 0.54178(10) 0.90534(19) 0.0372(4) Uani 1 1 d . . .
H27A H 0.3308 0.4928 0.8851 0.056 Uiso 1 1 calc R . .
H27B H 0.2509 0.5529 0.9533 0.056 Uiso 1 1 calc R . .
H27C H 0.4077 0.5532 0.9583 0.056 Uiso 1 1 calc R . .
C28 C 0.23018(16) 0.70205(8) 0.75458(15) 0.0224(3) Uani 1 1 d . . .
C29 C 0.21294(16) 0.77000(8) 0.79746(15) 0.0230(3) Uani 1 1 d . . .
C30 C 0.31086(16) 0.79609(8) 0.87970(16) 0.0240(3) Uani 1 1 d . . .
H30 H 0.3026 0.8421 0.9084 0.029 Uiso 1 1 calc R . .
C31 C 0.42010(16) 0.75882(8) 0.92234(15) 0.0241(3) Uani 1 1 d . . .
C32 C 0.42417(17) 0.68968(8) 0.88829(16) 0.0249(3) Uani 1 1 d . . .
H32 H 0.4935 0.6620 0.9215 0.030 Uiso 1 1 calc R . .
C33 C 0.32957(15) 0.66012(9) 0.80705(13) 0.0238(3) Uani 1 1 d . . .
C34 C 0.09468(16) 0.81412(9) 0.75569(17) 0.0264(3) Uani 1 1 d . . .
C35 C -0.03287(18) 0.77366(11) 0.7675(2) 0.0366(4) Uani 1 1 d . . .
H35A H -0.0397 0.7557 0.8558 0.055 Uiso 1 1 calc R . .
H35B H -0.0331 0.7355 0.7058 0.055 Uiso 1 1 calc R . .
H35C H -0.1075 0.8038 0.7486 0.055 Uiso 1 1 calc R . .
C36 C 0.1114(2) 0.83813(11) 0.61522(19) 0.0362(4) Uani 1 1 d . . .
H36A H 0.1097 0.7984 0.5573 0.054 Uiso 1 1 calc R . .
H36B H 0.1954 0.8620 0.6075 0.054 Uiso 1 1 calc R . .
H36C H 0.0397 0.8693 0.5913 0.054 Uiso 1 1 calc R . .
C37 C 0.0819(2) 0.87786(10) 0.8418(2) 0.0366(4) Uani 1 1 d . . .
H37A H 0.0037 0.9038 0.8151 0.055 Uiso 1 1 calc R . .
H37B H 0.1598 0.9067 0.8327 0.055 Uiso 1 1 calc R . .
H37C H 0.0739 0.8637 0.9323 0.055 Uiso 1 1 calc R . .
C38 C 0.53371(17) 0.79192(9) 0.99763(17) 0.0275(3) Uani 1 1 d . . .
C39 C 0.6480(2) 0.80035(15) 0.9048(3) 0.0503(6) Uani 1 1 d . . .
H39A H 0.6741 0.7554 0.8721 0.075 Uiso 1 1 calc R . .
H39B H 0.7224 0.8215 0.9508 0.075 Uiso 1 1 calc R . .
H39C H 0.6207 0.8296 0.8320 0.075 Uiso 1 1 calc R . .
C40 C 0.4979(2) 0.86240(10) 1.0513(2) 0.0413(5) Uani 1 1 d . . .
H40A H 0.4830 0.8944 0.9794 0.062 Uiso 1 1 calc R . .
H40B H 0.5699 0.8793 1.1068 0.062 Uiso 1 1 calc R . .
H40C H 0.4181 0.8587 1.1022 0.062 Uiso 1 1 calc R . .
C41 C 0.5780(2) 0.74734(10) 1.1125(2) 0.0358(4) Uani 1 1 d . . .
H41A H 0.5031 0.7382 1.1680 0.054 Uiso 1 1 calc R . .
H41B H 0.6463 0.7714 1.1626 0.054 Uiso 1 1 calc R . .
H41C H 0.6130 0.7039 1.0804 0.054 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.02140(10) 0.02135(11) 0.01994(10) -0.00116(9) -0.00104(7) -0.00026(10)
O1 0.0271(5) 0.0359(6) 0.0233(5) -0.0012(6) -0.0043(4) -0.0023(6)
C1 0.0314(8) 0.0424(10) 0.0244(7) -0.0017(6) -0.0055(6) 0.0052(7)
C2 0.0514(14) 0.117(3) 0.0405(12) 0.0244(15) 0.0085(11) 0.0200(16)
C3 0.112(3) 0.067(2) 0.0426(19) -0.0033(15) -0.0346(19) -0.039(2)
F1 0.236(5) 0.0456(13) 0.0659(18) -0.0200(12) -0.030(3) -0.0118(19)
F2 0.087(2) 0.150(4) 0.128(3) 0.032(3) -0.042(2) -0.081(3)
F3 0.179(5) 0.117(3) 0.0483(15) -0.0026(18) -0.061(2) -0.043(3)
C3X 0.098(9) 0.103(6) 0.051(7) 0.028(5) -0.019(6) 0.019(8)
F1X 0.152(11) 0.067(4) 0.048(6) -0.001(4) -0.030(6) -0.069(5)
F2X 0.037(4) 0.209(6) 0.083(6) 0.040(7) -0.002(4) 0.021(5)
F3X 0.117(10) 0.112(9) 0.061(6) 0.001(7) -0.061(6) -0.038(9)
C4 0.0761(18) 0.0715(18) 0.0414(12) 0.0053(12) -0.0122(12) 0.0287(14)
F4 0.206(3) 0.0473(10) 0.0883(15) -0.0078(10) -0.0644(17) 0.0167(14)
F5 0.1046(16) 0.0969(15) 0.0529(10) 0.0144(10) -0.0224(10) 0.0476(13)
F6 0.1115(17) 0.179(3) 0.0791(14) 0.0198(17) 0.0304(14) 0.0992(18)
N1 0.0253(6) 0.0252(6) 0.0248(6) -0.0006(5) 0.0006(5) -0.0003(5)
C5 0.0245(7) 0.0250(7) 0.0224(7) -0.0027(5) 0.0019(5) -0.0015(6)
C6 0.0251(7) 0.0245(7) 0.0328(8) -0.0020(6) 0.0013(6) 0.0009(6)
C7 0.0293(8) 0.0217(7) 0.0380(9) -0.0029(6) 0.0034(7) -0.0008(6)
C8 0.0253(8) 0.0276(8) 0.0403(9) -0.0082(7) 0.0039(7) -0.0025(6)
C9 0.0231(8) 0.0357(9) 0.0410(10) -0.0024(7) -0.0031(7) 0.0021(7)
C10 0.0289(8) 0.0315(8) 0.0333(8) 0.0025(7) -0.0042(7) 0.0005(7)
C11 0.0291(9) 0.0326(10) 0.0728(16) -0.0069(9) 0.0076(9) -0.0077(7)
O2 0.0277(5) 0.0217(5) 0.0238(5) -0.0019(4) -0.0019(4) 0.0012(4)
O3 0.0250(5) 0.0248(5) 0.0221(5) -0.0022(4) 0.0002(4) -0.0010(4)
C12 0.0286(7) 0.0168(6) 0.0253(7) -0.0009(5) -0.0015(6) 0.0000(5)
C13 0.0292(8) 0.0192(7) 0.0284(7) -0.0024(5) -0.0001(6) -0.0005(6)
C14 0.0287(8) 0.0244(8) 0.0364(9) -0.0051(6) 0.0004(7) 0.0005(6)
C15 0.0305(8) 0.0229(8) 0.0420(10) -0.0073(7) -0.0097(7) 0.0023(6)
C16 0.0373(9) 0.0245(8) 0.0310(8) -0.0055(6) -0.0088(7) 0.0033(6)
C17 0.0332(8) 0.0196(7) 0.0250(7) -0.0014(5) -0.0028(6) 0.0018(6)
C18 0.0347(8) 0.0260(7) 0.0253(7) -0.0030(6) 0.0027(6) 0.0038(6)
C19 0.0533(11) 0.0305(9) 0.0276(8) 0.0026(7) 0.0048(8) 0.0040(8)
C20 0.0438(10) 0.0405(10) 0.0278(8) -0.0116(7) -0.0011(7) -0.0055(8)
C21 0.0456(11) 0.0446(11) 0.0377(10) -0.0110(8) 0.0077(9) 0.0110(9)
C22 0.0329(9) 0.0368(10) 0.0545(12) -0.0136(9) -0.0153(8) 0.0042(8)
C23 0.0361(18) 0.147(5) 0.074(3) -0.056(3) -0.0180(16) 0.029(2)
C24 0.045(2) 0.094(4) 0.111(4) 0.056(3) -0.028(2) -0.006(2)
C25 0.0386(17) 0.057(2) 0.099(3) -0.029(2) -0.0148(18) -0.0110(15)
C23X 0.055(6) 0.091(9) 0.196(11) 0.061(10) -0.045(7) -0.045(7)
C24X 0.033(4) 0.042(3) 0.058(5) -0.006(3) -0.021(3) 0.010(3)
C25X 0.077(7) 0.143(12) 0.085(4) -0.077(6) -0.055(5) 0.060(7)
C26 0.0360(8) 0.0200(7) 0.0211(7) -0.0002(5) 0.0006(6) 0.0007(6)
C27 0.0620(13) 0.0231(8) 0.0267(8) 0.0050(6) 0.0030(8) 0.0035(8)
C28 0.0250(7) 0.0222(7) 0.0202(6) -0.0006(5) 0.0022(5) -0.0013(5)
C29 0.0244(7) 0.0234(7) 0.0214(6) -0.0006(5) 0.0033(5) 0.0009(5)
C30 0.0271(7) 0.0200(7) 0.0249(7) -0.0013(5) 0.0028(6) -0.0015(6)
C31 0.0271(7) 0.0240(7) 0.0211(6) 0.0005(5) -0.0002(5) -0.0012(6)
C32 0.0280(7) 0.0234(7) 0.0231(7) 0.0012(5) -0.0013(6) 0.0019(6)
C33 0.0308(6) 0.0205(6) 0.0201(6) -0.0009(6) 0.0017(5) 0.0005(6)
C34 0.0246(7) 0.0261(7) 0.0286(7) -0.0013(6) 0.0007(6) 0.0020(6)
C35 0.0244(8) 0.0373(10) 0.0482(11) -0.0030(8) 0.0035(7) -0.0005(7)
C36 0.0375(9) 0.0388(10) 0.0324(9) 0.0074(7) 0.0003(7) 0.0091(8)
C37 0.0353(9) 0.0303(9) 0.0441(10) -0.0082(8) -0.0004(8) 0.0091(7)
C38 0.0289(7) 0.0253(7) 0.0282(7) 0.0010(6) -0.0031(6) -0.0035(6)
C39 0.0391(11) 0.0626(15) 0.0493(12) -0.0033(11) 0.0066(9) -0.0193(11)
C40 0.0499(11) 0.0266(9) 0.0469(11) -0.0050(8) -0.0182(9) -0.0012(8)
C41 0.0422(10) 0.0285(8) 0.0364(9) 0.0003(7) -0.0118(8) -0.0014(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.6487(15) . ?
V1 O2 1.7966(12) . ?
V1 O1 1.8001(11) . ?
V1 O3 1.8097(12) . ?
O1 C1 1.391(2) . ?
C1 C3 1.510(4) . ?
C1 C2 1.530(3) . ?
C1 C3X 1.541(15) . ?
C1 C4 1.542(4) . ?
C3 F1 1.296(6) . ?
C3 F3 1.342(5) . ?
C3 F2 1.361(7) . ?
C3X F1X 1.328(13) . ?
C3X F3X 1.357(13) . ?
C3X F2X 1.439(15) . ?
C4 F6 1.297(4) . ?
C4 F4 1.320(4) . ?
C4 F5 1.334(3) . ?
N1 C5 1.381(2) . ?
C5 C10 1.398(2) . ?
C5 C6 1.405(2) . ?
C6 C7 1.382(2) . ?
C7 C8 1.397(3) . ?
C8 C9 1.392(3) . ?
C8 C11 1.509(3) . ?
C9 C10 1.387(3) . ?
O2 C12 1.376(2) . ?
O3 C28 1.3833(19) . ?
C12 C13 1.401(2) . ?
C12 C17 1.410(2) . ?
C13 C14 1.398(3) . ?
C13 C18 1.545(2) . ?
C14 C15 1.400(3) . ?
C15 C16 1.397(3) . ?
C15 C22 1.530(3) . ?
C16 C17 1.385(3) . ?
C17 C26 1.529(2) . ?
C18 C20 1.534(3) . ?
C18 C19 1.534(3) . ?
C18 C21 1.537(3) . ?
C22 C23X 1.471(11) . ?
C22 C24 1.488(5) . ?
C22 C23 1.541(5) . ?
C22 C25 1.547(4) . ?
C22 C24X 1.558(8) . ?
C22 C25X 1.581(10) . ?
C26 C33 1.527(2) . ?
C26 C27 1.545(2) . ?
C28 C33 1.405(2) . ?
C28 C29 1.411(2) . ?
C29 C30 1.396(2) . ?
C29 C34 1.538(2) . ?
C30 C31 1.396(2) . ?
C31 C32 1.396(2) . ?
C31 C38 1.528(2) . ?
C32 C33 1.393(2) . ?
C34 C35 1.529(3) . ?
C34 C37 1.537(3) . ?
C34 C36 1.537(3) . ?
C38 C40 1.531(3) . ?
C38 C39 1.532(3) . ?
C38 C41 1.533(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O2 105.45(7) . . ?
N1 V1 O1 112.94(7) . . ?
O2 V1 O1 111.23(7) . . ?
N1 V1 O3 103.81(6) . . ?
O2 V1 O3 108.81(5) . . ?
O1 V1 O3 114.00(5) . . ?
C1 O1 V1 146.77(12) . . ?
O1 C1 C3 107.2(2) . . ?
O1 C1 C2 113.33(17) . . ?
C3 C1 C2 107.9(3) . . ?
O1 C1 C3X 97.6(5) . . ?
C2 C1 C3X 133.9(7) . . ?
O1 C1 C4 108.42(17) . . ?
C3 C1 C4 114.2(3) . . ?
C2 C1 C4 105.9(2) . . ?
C3X C1 C4 94.8(6) . . ?
F1 C3 F3 106.8(4) . . ?
F1 C3 F2 110.7(4) . . ?
F3 C3 F2 108.2(4) . . ?
F1 C3 C1 110.5(4) . . ?
F3 C3 C1 111.4(4) . . ?
F2 C3 C1 109.1(4) . . ?
F1X C3X F3X 104.1(14) . . ?
F1X C3X F2X 115.3(15) . . ?
F3X C3X F2X 104.2(13) . . ?
F1X C3X C1 116.0(11) . . ?
F3X C3X C1 110.2(12) . . ?
F2X C3X C1 106.3(11) . . ?
C3X F2X F6 103.7(10) . . ?
F6 C4 F4 106.5(3) . . ?
F6 C4 F5 107.3(3) . . ?
F4 C4 F5 108.3(3) . . ?
F6 C4 C1 112.0(3) . . ?
F4 C4 C1 110.3(2) . . ?
F5 C4 C1 112.2(2) . . ?
C4 F6 F2X 102.6(4) . . ?
C5 N1 V1 175.63(13) . . ?
N1 C5 C10 120.20(16) . . ?
N1 C5 C6 119.79(15) . . ?
C10 C5 C6 120.00(16) . . ?
C7 C6 C5 119.59(16) . . ?
C6 C7 C8 121.12(17) . . ?
C9 C8 C7 118.48(17) . . ?
C9 C8 C11 121.41(18) . . ?
C7 C8 C11 120.11(18) . . ?
C10 C9 C8 121.67(17) . . ?
C9 C10 C5 119.08(17) . . ?
C12 O2 V1 131.04(10) . . ?
C28 O3 V1 120.68(10) . . ?
O2 C12 C13 121.57(15) . . ?
O2 C12 C17 116.85(15) . . ?
C13 C12 C17 121.54(16) . . ?
C14 C13 C12 116.93(16) . . ?
C14 C13 C18 120.32(15) . . ?
C12 C13 C18 122.67(15) . . ?
C13 C14 C15 123.33(17) . . ?
C16 C15 C14 117.13(16) . . ?
C16 C15 C22 121.15(18) . . ?
C14 C15 C22 121.71(18) . . ?
C17 C16 C15 122.23(17) . . ?
C16 C17 C12 118.53(16) . . ?
C16 C17 C26 121.91(15) . . ?
C12 C17 C26 119.55(15) . . ?
C20 C18 C19 110.80(17) . . ?
C20 C18 C21 106.46(16) . . ?
C19 C18 C21 107.38(17) . . ?
C20 C18 C13 112.28(15) . . ?
C19 C18 C13 107.99(14) . . ?
C21 C18 C13 111.84(16) . . ?
C23X C22 C24 137.3(6) . . ?
C23X C22 C15 111.0(6) . . ?
C24 C22 C15 111.7(2) . . ?
C23X C22 C23 49.5(9) . . ?
C24 C22 C23 110.0(4) . . ?
C15 C22 C23 113.1(2) . . ?
C23X C22 C25 57.8(9) . . ?
C24 C22 C25 109.8(4) . . ?
C15 C22 C25 107.1(2) . . ?
C23 C22 C25 104.9(3) . . ?
C23X C22 C24X 108.9(9) . . ?
C24 C22 C24X 55.0(5) . . ?
C15 C22 C24X 108.4(3) . . ?
C23 C22 C24X 61.3(5) . . ?
C25 C22 C24X 144.4(4) . . ?
C23X C22 C25X 116.2(10) . . ?
C24 C22 C25X 46.4(7) . . ?
C15 C22 C25X 111.6(5) . . ?
C23 C22 C25X 135.0(5) . . ?
C25 C22 C25X 65.7(7) . . ?
C24X C22 C25X 99.8(7) . . ?
C33 C26 C17 112.75(14) . . ?
C33 C26 C27 110.57(13) . . ?
C17 C26 C27 111.89(15) . . ?
O3 C28 C33 117.48(14) . . ?
O3 C28 C29 121.14(14) . . ?
C33 C28 C29 121.36(15) . . ?
C30 C29 C28 116.26(15) . . ?
C30 C29 C34 121.03(14) . . ?
C28 C29 C34 122.71(14) . . ?
C31 C30 C29 124.08(15) . . ?
C30 C31 C32 116.87(15) . . ?
C30 C31 C38 122.29(15) . . ?
C32 C31 C38 120.78(15) . . ?
C33 C32 C31 121.95(15) . . ?
C32 C33 C28 118.59(15) . . ?
C32 C33 C26 120.78(15) . . ?
C28 C33 C26 120.62(14) . . ?
C35 C34 C37 106.94(15) . . ?
C35 C34 C36 109.98(16) . . ?
C37 C34 C36 108.10(16) . . ?
C35 C34 C29 110.64(14) . . ?
C37 C34 C29 111.47(14) . . ?
C36 C34 C29 109.65(14) . . ?
C31 C38 C40 112.42(15) . . ?
C31 C38 C39 107.84(15) . . ?
C40 C38 C39 108.61(18) . . ?
C31 C38 C41 111.35(14) . . ?
C40 C38 C41 107.42(16) . . ?
C39 C38 C41 109.15(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 15.5(3) . . . . ?
O2 V1 O1 C1 -102.9(2) . . . . ?
O3 V1 O1 C1 133.7(2) . . . . ?
V1 O1 C1 C3 143.9(3) . . . . ?
V1 O1 C1 C2 25.0(4) . . . . ?
V1 O1 C1 C3X 170.0(7) . . . . ?
V1 O1 C1 C4 -92.3(3) . . . . ?
O1 C1 C3 F1 -61.2(4) . . . . ?
C2 C1 C3 F1 61.2(4) . . . . ?
C3X C1 C3 F1 -133.8(13) . . . . ?
C4 C1 C3 F1 178.7(3) . . . . ?
O1 C1 C3 F3 -179.8(4) . . . . ?
C2 C1 C3 F3 -57.4(5) . . . . ?
C3X C1 C3 F3 107.6(14) . . . . ?
C4 C1 C3 F3 60.1(5) . . . . ?
O1 C1 C3 F2 60.8(4) . . . . ?
C2 C1 C3 F2 -176.8(3) . . . . ?
C3X C1 C3 F2 -11.9(11) . . . . ?
C4 C1 C3 F2 -59.4(4) . . . . ?
O1 C1 C3X F1X -60.1(12) . . . . ?
C3 C1 C3X F1X 53.0(12) . . . . ?
C2 C1 C3X F1X 73.0(14) . . . . ?
C4 C1 C3X F1X -169.4(11) . . . . ?
O1 C1 C3X F3X -178.1(12) . . . . ?
C3 C1 C3X F3X -65.0(16) . . . . ?
C2 C1 C3X F3X -45.0(16) . . . . ?
C4 C1 C3X F3X 72.6(13) . . . . ?
O1 C1 C3X F2X 69.6(9) . . . . ?
C3 C1 C3X F2X -177.3(19) . . . . ?
C2 C1 C3X F2X -157.3(8) . . . . ?
C4 C1 C3X F2X -39.8(9) . . . . ?
F1X C3X F2X F6 155.0(11) . . . . ?
F3X C3X F2X F6 -91.5(13) . . . . ?
C1 C3X F2X F6 25.0(10) . . . . ?
O1 C1 C4 F6 -53.8(3) . . . . ?
C3 C1 C4 F6 65.6(4) . . . . ?
C2 C1 C4 F6 -175.8(3) . . . . ?
C3X C1 C4 F6 45.9(6) . . . . ?
O1 C1 C4 F4 64.6(3) . . . . ?
C3 C1 C4 F4 -176.0(3) . . . . ?
C2 C1 C4 F4 -57.4(3) . . . . ?
C3X C1 C4 F4 164.2(6) . . . . ?
O1 C1 C4 F5 -174.6(3) . . . . ?
C3 C1 C4 F5 -55.1(4) . . . . ?
C2 C1 C4 F5 63.5(3) . . . . ?
C3X C1 C4 F5 -74.9(6) . . . . ?
F4 C4 F6 F2X -152.2(5) . . . . ?
F5 C4 F6 F2X 92.0(5) . . . . ?
C1 C4 F6 F2X -31.6(5) . . . . ?
C3X F2X F6 C4 3.4(8) . . . . ?
N1 C5 C6 C7 -176.93(16) . . . . ?
C10 C5 C6 C7 2.0(2) . . . . ?
C5 C6 C7 C8 0.0(3) . . . . ?
C6 C7 C8 C9 -1.9(3) . . . . ?
C6 C7 C8 C11 177.19(19) . . . . ?
C7 C8 C9 C10 1.8(3) . . . . ?
C11 C8 C9 C10 -177.3(2) . . . . ?
C8 C9 C10 C5 0.2(3) . . . . ?
N1 C5 C10 C9 176.85(17) . . . . ?
C6 C5 C10 C9 -2.1(3) . . . . ?
N1 V1 O2 C12 30.69(15) . . . . ?
O1 V1 O2 C12 153.46(13) . . . . ?
O3 V1 O2 C12 -80.15(14) . . . . ?
N1 V1 O3 C28 -31.45(13) . . . . ?
O2 V1 O3 C28 80.49(12) . . . . ?
O1 V1 O3 C28 -154.73(11) . . . . ?
V1 O2 C12 C13 -113.15(15) . . . . ?
V1 O2 C12 C17 68.92(19) . . . . ?
O2 C12 C13 C14 176.39(15) . . . . ?
C17 C12 C13 C14 -5.8(2) . . . . ?
O2 C12 C13 C18 -0.2(2) . . . . ?
C17 C12 C13 C18 177.59(15) . . . . ?
C12 C13 C14 C15 1.9(3) . . . . ?
C18 C13 C14 C15 178.60(17) . . . . ?
C13 C14 C15 C16 2.6(3) . . . . ?
C13 C14 C15 C22 -176.29(18) . . . . ?
C14 C15 C16 C17 -3.4(3) . . . . ?
C22 C15 C16 C17 175.51(18) . . . . ?
C15 C16 C17 C12 -0.3(3) . . . . ?
C15 C16 C17 C26 -179.53(16) . . . . ?
O2 C12 C17 C16 -176.97(15) . . . . ?
C13 C12 C17 C16 5.1(2) . . . . ?
O2 C12 C17 C26 2.3(2) . . . . ?
C13 C12 C17 C26 -175.68(14) . . . . ?
C14 C13 C18 C20 134.48(18) . . . . ?
C12 C13 C18 C20 -49.0(2) . . . . ?
C14 C13 C18 C19 -103.08(19) . . . . ?
C12 C13 C18 C19 73.4(2) . . . . ?
C14 C13 C18 C21 14.9(2) . . . . ?
C12 C13 C18 C21 -168.62(17) . . . . ?
C16 C15 C22 C23X -128.4(10) . . . . ?
C14 C15 C22 C23X 50.5(10) . . . . ?
C16 C15 C22 C24 53.2(4) . . . . ?
C14 C15 C22 C24 -128.0(4) . . . . ?
C16 C15 C22 C23 177.9(4) . . . . ?
C14 C15 C22 C23 -3.3(4) . . . . ?
C16 C15 C22 C25 -67.0(3) . . . . ?
C14 C15 C22 C25 111.8(3) . . . . ?
C16 C15 C22 C24X 112.0(4) . . . . ?
C14 C15 C22 C24X -69.2(5) . . . . ?
C16 C15 C22 C25X 3.0(8) . . . . ?
C14 C15 C22 C25X -178.2(8) . . . . ?
C16 C17 C26 C33 84.26(19) . . . . ?
C12 C17 C26 C33 -94.94(18) . . . . ?
C16 C17 C26 C27 -41.1(2) . . . . ?
C12 C17 C26 C27 139.67(17) . . . . ?
V1 O3 C28 C33 -67.18(16) . . . . ?
V1 O3 C28 C29 111.27(14) . . . . ?
O3 C28 C29 C30 -169.23(14) . . . . ?
C33 C28 C29 C30 9.2(2) . . . . ?
O3 C28 C29 C34 9.9(2) . . . . ?
C33 C28 C29 C34 -171.66(14) . . . . ?
C28 C29 C30 C31 -1.4(2) . . . . ?
C34 C29 C30 C31 179.43(15) . . . . ?
C29 C30 C31 C32 -5.5(2) . . . . ?
C29 C30 C31 C38 171.80(16) . . . . ?
C30 C31 C32 C33 5.0(2) . . . . ?
C38 C31 C32 C33 -172.36(15) . . . . ?
C31 C32 C33 C28 2.3(2) . . . . ?
C31 C32 C33 C26 -176.13(15) . . . . ?
O3 C28 C33 C32 168.71(14) . . . . ?
C29 C28 C33 C32 -9.7(2) . . . . ?
O3 C28 C33 C26 -12.8(2) . . . . ?
C29 C28 C33 C26 168.73(14) . . . . ?
C17 C26 C33 C32 -70.60(19) . . . . ?
C27 C26 C33 C32 55.5(2) . . . . ?
C17 C26 C33 C28 110.97(17) . . . . ?
C27 C26 C33 C28 -122.92(17) . . . . ?
C30 C29 C34 C35 -134.22(17) . . . . ?
C28 C29 C34 C35 46.6(2) . . . . ?
C30 C29 C34 C37 -15.4(2) . . . . ?
C28 C29 C34 C37 165.51(16) . . . . ?
C30 C29 C34 C36 104.31(18) . . . . ?
C28 C29 C34 C36 -74.8(2) . . . . ?
C30 C31 C38 C40 15.6(2) . . . . ?
C32 C31 C38 C40 -167.13(17) . . . . ?
C30 C31 C38 C39 -104.1(2) . . . . ?
C32 C31 C38 C39 73.2(2) . . . . ?
C30 C31 C38 C41 136.23(17) . . . . ?
C32 C31 C38 C41 -46.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        30.59
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.052

data_3
_database_code_depnum_ccdc_archive 'CCDC 718353'

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H57 Cl N O3 V'
_chemical_formula_sum            'C40 H57 Cl N O3 V'
_chemical_formula_weight         686.26

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           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   18.2831(8)
_cell_length_b                   11.0322(4)
_cell_length_c                   41.0433(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0783(12)
_cell_angle_gamma                90.00
_cell_volume                     8196.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    33012
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       tablet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28806
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6959
_reflns_number_gt                5804
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0000P)^2^+36.2525P] where P=(Fo^2^+2Fc^2^)/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         6959
_refine_ls_number_parameters     468
_refine_ls_number_restraints     181
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.103
_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 0.28000(3) 0.53445(5) 0.316909(12) 0.02573(15) Uani 1 1 d . . .
O1 O 0.26758(14) 0.6161(2) 0.28032(5) 0.0386(6) Uani 1 1 d . . .
C1 C 0.2613(3) 0.7281(4) 0.26225(9) 0.0513(11) Uani 1 1 d . . .
C2 C 0.2747(4) 0.8329(4) 0.28635(12) 0.093(2) Uani 1 1 d . . .
H2A H 0.2389 0.8293 0.3020 0.139 Uiso 1 1 calc R . .
H2B H 0.2691 0.9097 0.2743 0.139 Uiso 1 1 calc R . .
H2C H 0.3249 0.8273 0.2984 0.139 Uiso 1 1 calc R . .
C3 C 0.3199(3) 0.7215(5) 0.23934(11) 0.0704(15) Uani 1 1 d . . .
H3A H 0.3690 0.7163 0.2524 0.106 Uiso 1 1 calc R . .
H3B H 0.3172 0.7943 0.2256 0.106 Uiso 1 1 calc R . .
H3C H 0.3113 0.6496 0.2253 0.106 Uiso 1 1 calc R . .
C4 C 0.1841(3) 0.7308(5) 0.24320(11) 0.0709(15) Uani 1 1 d . . .
H4A H 0.1779 0.6625 0.2278 0.106 Uiso 1 1 calc R . .
H4B H 0.1766 0.8071 0.2310 0.106 Uiso 1 1 calc R . .
H4C H 0.1477 0.7244 0.2586 0.106 Uiso 1 1 calc R . .
N1 N 0.29135(15) 0.6164(2) 0.35095(6) 0.0301(6) Uani 1 1 d D A .
C5 C 0.29899(19) 0.6786(3) 0.38045(8) 0.0325(8) Uani 1 1 d DU . .
C6 C 0.3309(4) 0.7949(4) 0.38293(13) 0.0490(19) Uani 0.688(8) 1 d PDU A 1
H6 H 0.3481 0.8307 0.3644 0.059 Uiso 0.688(8) 1 calc PR A 1
C7 C 0.3370(5) 0.8570(5) 0.41241(13) 0.060(2) Uani 0.688(8) 1 d PDU A 1
H7 H 0.3578 0.9360 0.4142 0.072 Uiso 0.688(8) 1 calc PR A 1
C8 C 0.3121(3) 0.8022(3) 0.43944(9) 0.0551(11) Uani 1 1 d DU . .
C9 C 0.2868(4) 0.6858(6) 0.43815(15) 0.0474(17) Uani 0.688(8) 1 d PDU A 1
H9 H 0.2737 0.6479 0.4573 0.057 Uiso 0.688(8) 1 calc PR A 1
C10 C 0.2806(4) 0.6232(6) 0.40854(13) 0.0404(16) Uani 0.688(8) 1 d PDU A 1
H10 H 0.2635 0.5417 0.4075 0.048 Uiso 0.688(8) 1 calc PR A 1
Cl1 Cl 0.31916(10) 0.88231(12) 0.47628(3) 0.0953(5) Uani 1 1 d DU A .
C6X C 0.2705(8) 0.7975(8) 0.3816(2) 0.032(3) Uani 0.312(8) 1 d PDU A 2
H6X H 0.2480 0.8357 0.3620 0.038 Uiso 0.312(8) 1 calc PR A 2
C7X C 0.2754(8) 0.8578(9) 0.4113(2) 0.036(3) Uani 0.312(8) 1 d PDU A 2
H7X H 0.2542 0.9360 0.4125 0.043 Uiso 0.312(8) 1 calc PR A 2
C9X C 0.3306(13) 0.6830(11) 0.4386(3) 0.068(5) Uani 0.312(8) 1 d PDU A 2
H9X H 0.3479 0.6419 0.4586 0.082 Uiso 0.312(8) 1 calc PR A 2
C10X C 0.3248(12) 0.6214(11) 0.4093(3) 0.061(5) Uani 0.312(8) 1 d PDU A 2
H10X H 0.3387 0.5384 0.4091 0.073 Uiso 0.312(8) 1 calc PR A 2
O2 O 0.36039(12) 0.43874(18) 0.31907(5) 0.0262(5) Uani 1 1 d . . .
O3 O 0.20090(12) 0.43932(18) 0.31972(5) 0.0252(5) Uani 1 1 d . . .
C12 C 0.39999(17) 0.3974(3) 0.34800(7) 0.0245(7) Uani 1 1 d . . .
C13 C 0.47294(18) 0.4396(3) 0.35780(8) 0.0283(7) Uani 1 1 d . . .
C14 C 0.50717(19) 0.3996(3) 0.38826(8) 0.0325(8) Uani 1 1 d . . .
H14 H 0.5558 0.4274 0.3958 0.039 Uiso 1 1 calc R . .
C15 C 0.47403(18) 0.3203(3) 0.40863(7) 0.0300(7) Uani 1 1 d . . .
C16 C 0.40375(18) 0.2781(3) 0.39685(7) 0.0273(7) Uani 1 1 d . . .
H16 H 0.3805 0.2232 0.4100 0.033 Uiso 1 1 calc R . .
C17 C 0.36618(17) 0.3133(3) 0.36662(7) 0.0240(7) Uani 1 1 d . . .
C18 C 0.51143(19) 0.5257(3) 0.33623(8) 0.0353(8) Uani 1 1 d . . .
C19 C 0.4766(2) 0.6523(3) 0.33586(10) 0.0474(10) Uani 1 1 d . . .
H19A H 0.5041 0.7080 0.3235 0.071 Uiso 1 1 calc R . .
H19B H 0.4783 0.6817 0.3585 0.071 Uiso 1 1 calc R . .
H19C H 0.4251 0.6481 0.3254 0.071 Uiso 1 1 calc R . .
C20 C 0.5074(2) 0.4779(4) 0.30076(8) 0.0428(9) Uani 1 1 d . . .
H20A H 0.5330 0.5343 0.2878 0.064 Uiso 1 1 calc R . .
H20B H 0.4555 0.4709 0.2909 0.064 Uiso 1 1 calc R . .
H20C H 0.5310 0.3981 0.3011 0.064 Uiso 1 1 calc R . .
C21 C 0.5937(2) 0.5403(4) 0.34967(10) 0.0527(11) Uani 1 1 d . . .
H21A H 0.6175 0.4604 0.3514 0.079 Uiso 1 1 calc R . .
H21B H 0.5988 0.5781 0.3715 0.079 Uiso 1 1 calc R . .
H21C H 0.6175 0.5915 0.3347 0.079 Uiso 1 1 calc R . .
C22 C 0.5156(2) 0.2837(3) 0.44243(8) 0.0386(9) Uani 1 1 d . . .
C23 C 0.5961(2) 0.2506(5) 0.43938(11) 0.0768(16) Uani 1 1 d . . .
H23A H 0.6220 0.3226 0.4329 0.115 Uiso 1 1 calc R . .
H23B H 0.5968 0.1874 0.4226 0.115 Uiso 1 1 calc R . .
H23C H 0.6208 0.2206 0.4606 0.115 Uiso 1 1 calc R . .
C24 C 0.4816(2) 0.1732(4) 0.45665(9) 0.0529(11) Uani 1 1 d . . .
H24A H 0.5111 0.1509 0.4776 0.079 Uiso 1 1 calc R . .
H24B H 0.4807 0.1054 0.4412 0.079 Uiso 1 1 calc R . .
H24C H 0.4310 0.1922 0.4603 0.079 Uiso 1 1 calc R . .
C25 C 0.5140(3) 0.3888(4) 0.46618(10) 0.0801(17) Uani 1 1 d . . .
H25A H 0.4627 0.4092 0.4682 0.120 Uiso 1 1 calc R . .
H25B H 0.5383 0.4593 0.4579 0.120 Uiso 1 1 calc R . .
H25C H 0.5401 0.3658 0.4878 0.120 Uiso 1 1 calc R . .
C26 C 0.29169(17) 0.2577(3) 0.35284(7) 0.0245(7) Uani 1 1 d . . .
H26 H 0.2838 0.2753 0.3287 0.029 Uiso 1 1 calc R . .
C27 C 0.29299(18) 0.1185(3) 0.35636(8) 0.0317(8) Uani 1 1 d . . .
H27A H 0.3338 0.0853 0.3460 0.048 Uiso 1 1 calc R . .
H27B H 0.2462 0.0848 0.3455 0.048 Uiso 1 1 calc R . .
H27C H 0.2998 0.0967 0.3797 0.048 Uiso 1 1 calc R . .
C28 C 0.18031(17) 0.3971(3) 0.34865(7) 0.0241(7) Uani 1 1 d . . .
C29 C 0.11398(18) 0.4390(3) 0.35889(7) 0.0283(7) Uani 1 1 d . . .
C30 C 0.09955(19) 0.3976(3) 0.38934(8) 0.0306(7) Uani 1 1 d . . .
H30 H 0.0558 0.4249 0.3971 0.037 Uiso 1 1 calc R . .
C31 C 0.14564(19) 0.3184(3) 0.40921(7) 0.0294(7) Uani 1 1 d . . .
C32 C 0.20789(18) 0.2757(3) 0.39724(7) 0.0270(7) Uani 1 1 d . . .
H32 H 0.2393 0.2199 0.4101 0.032 Uiso 1 1 calc R . .
C33 C 0.22588(17) 0.3122(3) 0.36683(7) 0.0246(7) Uani 1 1 d . . .
C34 C 0.06197(19) 0.5271(3) 0.33778(8) 0.0358(8) Uani 1 1 d . . .
C35 C 0.0429(2) 0.4817(4) 0.30201(8) 0.0436(9) Uani 1 1 d . . .
H35A H 0.0073 0.5370 0.2897 0.065 Uiso 1 1 calc R . .
H35B H 0.0215 0.4003 0.3020 0.065 Uiso 1 1 calc R . .
H35C H 0.0880 0.4789 0.2916 0.065 Uiso 1 1 calc R . .
C36 C 0.0977(2) 0.6532(3) 0.33799(9) 0.0445(9) Uani 1 1 d . . .
H36A H 0.1417 0.6492 0.3269 0.067 Uiso 1 1 calc R . .
H36B H 0.1119 0.6800 0.3608 0.067 Uiso 1 1 calc R . .
H36C H 0.0624 0.7108 0.3265 0.067 Uiso 1 1 calc R . .
C37 C -0.0120(2) 0.5417(4) 0.35150(10) 0.0520(11) Uani 1 1 d . . .
H37A H -0.0438 0.5981 0.3376 0.078 Uiso 1 1 calc R . .
H37B H -0.0025 0.5735 0.3740 0.078 Uiso 1 1 calc R . .
H37C H -0.0364 0.4627 0.3516 0.078 Uiso 1 1 calc R . .
C38 C 0.1267(2) 0.2814(3) 0.44339(8) 0.0368(8) Uani 1 1 d . . .
C39 C 0.1432(3) 0.3894(4) 0.46662(9) 0.0629(13) Uani 1 1 d . . .
H39A H 0.1959 0.4091 0.4688 0.094 Uiso 1 1 calc R . .
H39B H 0.1300 0.3688 0.4883 0.094 Uiso 1 1 calc R . .
H39C H 0.1141 0.4596 0.4577 0.094 Uiso 1 1 calc R . .
C40 C 0.0446(2) 0.2470(4) 0.44105(10) 0.0589(12) Uani 1 1 d . . .
H40A H 0.0140 0.3173 0.4336 0.088 Uiso 1 1 calc R . .
H40B H 0.0339 0.2214 0.4627 0.088 Uiso 1 1 calc R . .
H40C H 0.0337 0.1804 0.4253 0.088 Uiso 1 1 calc R . .
C41 C 0.1717(3) 0.1723(4) 0.45766(9) 0.0556(11) Uani 1 1 d . . .
H41A H 0.1641 0.1044 0.4422 0.083 Uiso 1 1 calc R . .
H41B H 0.1556 0.1488 0.4786 0.083 Uiso 1 1 calc R . .
H41C H 0.2242 0.1937 0.4614 0.083 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0332(3) 0.0228(3) 0.0213(3) 0.0027(2) 0.0043(2) 0.0007(2)
O1 0.0509(16) 0.0371(13) 0.0282(12) 0.0124(10) 0.0066(11) 0.0046(12)
C1 0.070(3) 0.042(2) 0.042(2) 0.0241(18) 0.009(2) 0.006(2)
C2 0.168(6) 0.034(2) 0.073(3) 0.020(2) 0.006(4) 0.005(3)
C3 0.064(3) 0.084(3) 0.064(3) 0.050(3) 0.014(2) 0.000(3)
C4 0.066(3) 0.086(3) 0.062(3) 0.047(3) 0.015(2) 0.025(3)
N1 0.0355(17) 0.0244(13) 0.0302(14) 0.0008(11) 0.0041(12) -0.0022(12)
C5 0.042(2) 0.0251(16) 0.0300(17) -0.0024(13) 0.0031(15) 0.0024(15)
C6 0.077(6) 0.028(3) 0.038(3) 0.000(2) -0.005(3) -0.006(3)
C7 0.102(7) 0.024(3) 0.045(3) -0.009(2) -0.019(3) 0.002(3)
C8 0.081(3) 0.045(2) 0.0327(19) -0.0140(17) -0.0135(19) 0.018(2)
C9 0.047(4) 0.066(4) 0.028(3) -0.007(3) 0.001(3) -0.004(3)
C10 0.042(4) 0.045(3) 0.033(3) -0.004(2) 0.001(3) -0.015(3)
Cl1 0.1635(15) 0.0711(8) 0.0400(6) -0.0270(6) -0.0250(7) 0.0335(9)
C6X 0.048(9) 0.022(5) 0.026(5) 0.000(4) 0.005(5) 0.001(5)
C7X 0.054(9) 0.020(5) 0.036(5) -0.003(4) 0.017(5) -0.002(5)
C9X 0.111(14) 0.057(7) 0.030(6) -0.005(5) -0.020(9) 0.038(10)
C10X 0.107(13) 0.026(6) 0.039(6) -0.007(4) -0.026(9) 0.010(8)
O2 0.0288(13) 0.0261(11) 0.0239(11) 0.0002(9) 0.0048(9) -0.0027(9)
O3 0.0301(13) 0.0246(11) 0.0213(10) -0.0001(8) 0.0051(9) 0.0037(9)
C12 0.0274(18) 0.0221(15) 0.0242(15) -0.0013(12) 0.0036(13) 0.0020(13)
C13 0.0260(18) 0.0272(16) 0.0325(17) -0.0023(13) 0.0064(13) -0.0053(13)
C14 0.034(2) 0.0344(18) 0.0280(17) -0.0040(14) 0.0007(14) -0.0037(15)
C15 0.031(2) 0.0345(18) 0.0241(16) -0.0019(14) 0.0035(13) 0.0049(15)
C16 0.0263(19) 0.0280(16) 0.0289(16) 0.0008(13) 0.0082(13) -0.0018(13)
C17 0.0248(18) 0.0201(14) 0.0281(16) -0.0028(12) 0.0072(13) 0.0018(13)
C18 0.031(2) 0.0391(19) 0.0357(18) 0.0067(15) 0.0044(15) -0.0101(16)
C19 0.048(3) 0.033(2) 0.060(2) 0.0082(18) 0.0063(19) -0.0101(17)
C20 0.036(2) 0.053(2) 0.041(2) 0.0094(18) 0.0100(16) -0.0079(18)
C21 0.038(2) 0.066(3) 0.053(2) 0.017(2) 0.0027(18) -0.017(2)
C22 0.039(2) 0.049(2) 0.0265(17) 0.0045(15) 0.0002(15) -0.0015(17)
C23 0.042(3) 0.133(5) 0.053(3) 0.040(3) -0.005(2) 0.010(3)
C24 0.060(3) 0.056(3) 0.039(2) 0.0175(19) -0.0047(19) 0.001(2)
C25 0.140(5) 0.059(3) 0.035(2) -0.001(2) -0.013(3) -0.005(3)
C26 0.0260(18) 0.0230(15) 0.0251(15) -0.0001(12) 0.0054(13) 0.0015(13)
C27 0.0247(19) 0.0230(16) 0.047(2) -0.0013(14) 0.0053(15) 0.0020(14)
C28 0.0275(18) 0.0248(15) 0.0208(15) -0.0027(12) 0.0064(13) -0.0020(13)
C29 0.0294(19) 0.0262(16) 0.0297(17) -0.0017(13) 0.0057(13) 0.0021(14)
C30 0.030(2) 0.0333(18) 0.0310(17) -0.0041(14) 0.0111(14) 0.0009(14)
C31 0.035(2) 0.0292(17) 0.0248(16) -0.0014(13) 0.0052(14) -0.0036(14)
C32 0.0297(19) 0.0232(15) 0.0276(16) 0.0005(13) 0.0020(13) 0.0006(13)
C33 0.0259(18) 0.0209(15) 0.0267(16) -0.0045(12) 0.0028(13) -0.0018(13)
C34 0.035(2) 0.0386(19) 0.0349(18) 0.0059(15) 0.0095(15) 0.0113(16)
C35 0.039(2) 0.050(2) 0.040(2) 0.0078(17) -0.0024(16) 0.0113(18)
C36 0.050(3) 0.0296(19) 0.054(2) 0.0047(17) 0.0099(19) 0.0130(17)
C37 0.041(2) 0.060(3) 0.058(2) 0.014(2) 0.0171(19) 0.022(2)
C38 0.043(2) 0.0397(19) 0.0303(18) 0.0010(15) 0.0130(16) -0.0011(16)
C39 0.103(4) 0.058(3) 0.030(2) -0.0060(19) 0.019(2) -0.014(3)
C40 0.049(3) 0.085(3) 0.047(2) 0.017(2) 0.020(2) -0.008(2)
C41 0.071(3) 0.060(3) 0.040(2) 0.0222(19) 0.021(2) 0.012(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.653(3) . ?
V1 O1 1.738(2) . ?
V1 O2 1.802(2) . ?
V1 O3 1.804(2) . ?
O1 C1 1.437(4) . ?
C1 C4 1.516(6) . ?
C1 C2 1.519(6) . ?
C1 C3 1.523(6) . ?
N1 C5 1.382(4) . ?
C5 C10X 1.366(10) . ?
C5 C10 1.388(6) . ?
C5 C6 1.407(6) . ?
C5 C6X 1.415(9) . ?
C6 C7 1.381(7) . ?
C7 C8 1.395(7) . ?
C8 C9X 1.359(11) . ?
C8 C9 1.363(7) . ?
C8 C7X 1.394(10) . ?
C8 Cl1 1.741(4) . ?
C9 C10 1.388(7) . ?
C6X C7X 1.380(11) . ?
C9X C10X 1.372(12) . ?
O2 C12 1.379(3) . ?
O3 C28 1.377(3) . ?
C12 C17 1.400(4) . ?
C12 C13 1.417(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.535(4) . ?
C14 C15 1.405(5) . ?
C15 C16 1.388(4) . ?
C15 C22 1.539(4) . ?
C16 C17 1.386(4) . ?
C17 C26 1.528(4) . ?
C18 C19 1.535(5) . ?
C18 C21 1.537(5) . ?
C18 C20 1.540(5) . ?
C22 C25 1.518(5) . ?
C22 C24 1.522(5) . ?
C22 C23 1.539(6) . ?
C26 C33 1.527(4) . ?
C26 C27 1.543(4) . ?
C28 C33 1.398(4) . ?
C28 C29 1.416(4) . ?
C29 C30 1.390(4) . ?
C29 C34 1.539(4) . ?
C30 C31 1.395(5) . ?
C31 C32 1.384(4) . ?
C31 C38 1.546(4) . ?
C32 C33 1.394(4) . ?
C34 C36 1.537(5) . ?
C34 C37 1.544(5) . ?
C34 C35 1.544(5) . ?
C38 C41 1.527(5) . ?
C38 C39 1.529(5) . ?
C38 C40 1.538(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O1 115.61(12) . . ?
N1 V1 O2 105.92(12) . . ?
O1 V1 O2 110.67(10) . . ?
N1 V1 O3 105.72(11) . . ?
O1 V1 O3 110.38(11) . . ?
O2 V1 O3 108.16(9) . . ?
C1 O1 V1 151.9(2) . . ?
O1 C1 C4 106.5(3) . . ?
O1 C1 C2 108.9(3) . . ?
C4 C1 C2 112.0(4) . . ?
O1 C1 C3 105.4(3) . . ?
C4 C1 C3 111.6(3) . . ?
C2 C1 C3 112.1(4) . . ?
C5 N1 V1 176.2(2) . . ?
C10X C5 N1 120.7(6) . . ?
N1 C5 C10 120.2(4) . . ?
C10X C5 C6 105.7(7) . . ?
N1 C5 C6 120.4(3) . . ?
C10 C5 C6 119.2(4) . . ?
C10X C5 C6X 118.9(7) . . ?
N1 C5 C6X 119.8(5) . . ?
C10 C5 C6X 104.3(5) . . ?
C7 C6 C5 119.8(5) . . ?
C6 C7 C8 119.1(5) . . ?
C9X C8 C7X 119.9(7) . . ?
C9 C8 C7X 105.2(6) . . ?
C9X C8 C7 106.8(9) . . ?
C9 C8 C7 121.6(4) . . ?
C9X C8 Cl1 121.7(6) . . ?
C9 C8 Cl1 119.7(4) . . ?
C7X C8 Cl1 117.7(4) . . ?
C7 C8 Cl1 118.5(3) . . ?
C8 C9 C10 119.2(6) . . ?
C5 C10 C9 120.6(5) . . ?
C7X C6X C5 119.9(8) . . ?
C6X C7X C8 118.9(8) . . ?
C8 C9X C10X 120.8(10) . . ?
C5 C10X C9X 120.4(10) . . ?
C12 O2 V1 124.22(18) . . ?
C28 O3 V1 124.83(18) . . ?
O2 C12 C17 118.1(3) . . ?
O2 C12 C13 119.7(3) . . ?
C17 C12 C13 122.2(3) . . ?
C14 C13 C12 116.0(3) . . ?
C14 C13 C18 122.0(3) . . ?
C12 C13 C18 122.0(3) . . ?
C13 C14 C15 123.8(3) . . ?
C16 C15 C14 117.2(3) . . ?
C16 C15 C22 122.8(3) . . ?
C14 C15 C22 120.0(3) . . ?
C17 C16 C15 122.4(3) . . ?
C16 C17 C12 118.2(3) . . ?
C16 C17 C26 121.5(3) . . ?
C12 C17 C26 120.2(3) . . ?
C13 C18 C19 110.2(3) . . ?
C13 C18 C21 111.3(3) . . ?
C19 C18 C21 107.0(3) . . ?
C13 C18 C20 111.6(3) . . ?
C19 C18 C20 109.7(3) . . ?
C21 C18 C20 106.8(3) . . ?
C25 C22 C24 108.7(3) . . ?
C25 C22 C23 109.8(4) . . ?
C24 C22 C23 106.8(3) . . ?
C25 C22 C15 109.1(3) . . ?
C24 C22 C15 112.3(3) . . ?
C23 C22 C15 110.2(3) . . ?
C33 C26 C17 114.3(2) . . ?
C33 C26 C27 111.1(3) . . ?
C17 C26 C27 111.3(3) . . ?
O3 C28 C33 118.2(3) . . ?
O3 C28 C29 119.7(3) . . ?
C33 C28 C29 122.1(3) . . ?
C30 C29 C28 116.0(3) . . ?
C30 C29 C34 122.2(3) . . ?
C28 C29 C34 121.8(3) . . ?
C29 C30 C31 123.8(3) . . ?
C32 C31 C30 117.7(3) . . ?
C32 C31 C38 122.2(3) . . ?
C30 C31 C38 120.1(3) . . ?
C31 C32 C33 121.9(3) . . ?
C32 C33 C28 118.3(3) . . ?
C32 C33 C26 121.4(3) . . ?
C28 C33 C26 120.3(3) . . ?
C36 C34 C29 109.9(3) . . ?
C36 C34 C37 107.3(3) . . ?
C29 C34 C37 111.4(3) . . ?
C36 C34 C35 109.7(3) . . ?
C29 C34 C35 111.7(3) . . ?
C37 C34 C35 106.8(3) . . ?
C41 C38 C39 109.1(3) . . ?
C41 C38 C40 107.3(3) . . ?
C39 C38 C40 109.6(3) . . ?
C41 C38 C31 112.3(3) . . ?
C39 C38 C31 108.1(3) . . ?
C40 C38 C31 110.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 0.0(6) . . . . ?
O2 V1 O1 C1 -120.4(5) . . . . ?
O3 V1 O1 C1 119.9(5) . . . . ?
V1 O1 C1 C4 -117.0(5) . . . . ?
V1 O1 C1 C2 4.0(8) . . . . ?
V1 O1 C1 C3 124.4(5) . . . . ?
C10X C5 C6 C7 -40.0(11) . . . . ?
N1 C5 C6 C7 178.8(5) . . . . ?
C10 C5 C6 C7 -6.1(9) . . . . ?
C6X C5 C6 C7 75.3(8) . . . . ?
C5 C6 C7 C8 0.8(10) . . . . ?
C6 C7 C8 C9X 38.7(11) . . . . ?
C6 C7 C8 C9 4.8(10) . . . . ?
C6 C7 C8 C7X -76.7(8) . . . . ?
C6 C7 C8 Cl1 -179.2(5) . . . . ?
C9X C8 C9 C10 -77.2(12) . . . . ?
C7X C8 C9 C10 44.1(9) . . . . ?
C7 C8 C9 C10 -4.8(9) . . . . ?
Cl1 C8 C9 C10 179.2(5) . . . . ?
C10X C5 C10 C9 80.0(11) . . . . ?
N1 C5 C10 C9 -178.9(5) . . . . ?
C6 C5 C10 C9 6.1(8) . . . . ?
C6X C5 C10 C9 -40.9(9) . . . . ?
C8 C9 C10 C5 -0.7(10) . . . . ?
C10X C5 C6X C7X 6.0(17) . . . . ?
N1 C5 C6X C7X 177.4(9) . . . . ?
C10 C5 C6X C7X 39.2(13) . . . . ?
C6 C5 C6X C7X -77.8(12) . . . . ?
C5 C6X C7X C8 3.3(17) . . . . ?
C9X C8 C7X C6X -11.6(18) . . . . ?
C9 C8 C7X C6X -45.2(12) . . . . ?
C7 C8 C7X C6X 74.0(11) . . . . ?
Cl1 C8 C7X C6X 178.5(9) . . . . ?
C9 C8 C9X C10X 82.7(19) . . . . ?
C7X C8 C9X C10X 11(3) . . . . ?
C7 C8 C9X C10X -39(2) . . . . ?
Cl1 C8 C9X C10X -179.9(14) . . . . ?
N1 C5 C10X C9X -178.5(14) . . . . ?
C10 C5 C10X C9X -79.0(19) . . . . ?
C6 C5 C10X C9X 40(2) . . . . ?
C6X C5 C10X C9X -7(2) . . . . ?
C8 C9X C10X C5 -1(3) . . . . ?
N1 V1 O2 C12 29.8(2) . . . . ?
O1 V1 O2 C12 155.9(2) . . . . ?
O3 V1 O2 C12 -83.1(2) . . . . ?
N1 V1 O3 C28 -30.4(2) . . . . ?
O1 V1 O3 C28 -156.1(2) . . . . ?
O2 V1 O3 C28 82.7(2) . . . . ?
V1 O2 C12 C17 68.4(3) . . . . ?
V1 O2 C12 C13 -112.2(3) . . . . ?
O2 C12 C13 C14 176.0(3) . . . . ?
C17 C12 C13 C14 -4.7(4) . . . . ?
O2 C12 C13 C18 -3.3(4) . . . . ?
C17 C12 C13 C18 176.1(3) . . . . ?
C12 C13 C14 C15 1.2(5) . . . . ?
C18 C13 C14 C15 -179.6(3) . . . . ?
C13 C14 C15 C16 1.7(5) . . . . ?
C13 C14 C15 C22 -178.3(3) . . . . ?
C14 C15 C16 C17 -1.2(5) . . . . ?
C22 C15 C16 C17 178.8(3) . . . . ?
C15 C16 C17 C12 -2.1(5) . . . . ?
C15 C16 C17 C26 174.7(3) . . . . ?
O2 C12 C17 C16 -175.4(3) . . . . ?
C13 C12 C17 C16 5.2(4) . . . . ?
O2 C12 C17 C26 7.7(4) . . . . ?
C13 C12 C17 C26 -171.7(3) . . . . ?
C14 C13 C18 C19 -108.2(4) . . . . ?
C12 C13 C18 C19 71.0(4) . . . . ?
C14 C13 C18 C21 10.3(5) . . . . ?
C12 C13 C18 C21 -170.5(3) . . . . ?
C14 C13 C18 C20 129.6(3) . . . . ?
C12 C13 C18 C20 -51.2(4) . . . . ?
C16 C15 C22 C25 -104.7(4) . . . . ?
C14 C15 C22 C25 75.3(4) . . . . ?
C16 C15 C22 C24 15.8(5) . . . . ?
C14 C15 C22 C24 -164.3(3) . . . . ?
C16 C15 C22 C23 134.6(4) . . . . ?
C14 C15 C22 C23 -45.4(5) . . . . ?
C16 C17 C26 C33 80.8(3) . . . . ?
C12 C17 C26 C33 -102.4(3) . . . . ?
C16 C17 C26 C27 -46.0(4) . . . . ?
C12 C17 C26 C27 130.8(3) . . . . ?
V1 O3 C28 C33 -68.2(3) . . . . ?
V1 O3 C28 C29 112.6(3) . . . . ?
O3 C28 C29 C30 -176.2(3) . . . . ?
C33 C28 C29 C30 4.6(4) . . . . ?
O3 C28 C29 C34 2.7(4) . . . . ?
C33 C28 C29 C34 -176.6(3) . . . . ?
C28 C29 C30 C31 -0.8(5) . . . . ?
C34 C29 C30 C31 -179.6(3) . . . . ?
C29 C30 C31 C32 -2.3(5) . . . . ?
C29 C30 C31 C38 177.4(3) . . . . ?
C30 C31 C32 C33 1.7(5) . . . . ?
C38 C31 C32 C33 -178.0(3) . . . . ?
C31 C32 C33 C28 1.9(5) . . . . ?
C31 C32 C33 C26 -175.6(3) . . . . ?
O3 C28 C33 C32 175.6(3) . . . . ?
C29 C28 C33 C32 -5.2(4) . . . . ?
O3 C28 C33 C26 -6.9(4) . . . . ?
C29 C28 C33 C26 172.4(3) . . . . ?
C17 C26 C33 C32 -81.2(4) . . . . ?
C27 C26 C33 C32 45.8(4) . . . . ?
C17 C26 C33 C28 101.3(3) . . . . ?
C27 C26 C33 C28 -131.7(3) . . . . ?
C30 C29 C34 C36 108.0(4) . . . . ?
C28 C29 C34 C36 -70.8(4) . . . . ?
C30 C29 C34 C37 -10.7(5) . . . . ?
C28 C29 C34 C37 170.5(3) . . . . ?
C30 C29 C34 C35 -130.0(3) . . . . ?
C28 C29 C34 C35 51.2(4) . . . . ?
C32 C31 C38 C41 -14.4(5) . . . . ?
C30 C31 C38 C41 165.9(3) . . . . ?
C32 C31 C38 C39 106.0(4) . . . . ?
C30 C31 C38 C39 -73.7(4) . . . . ?
C32 C31 C38 C40 -134.1(4) . . . . ?
C30 C31 C38 C40 46.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.062

data_4
_database_code_depnum_ccdc_archive 'CCDC 718354'

_chemical_name_common            'Compound 4'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4Me)(diphenolate)(mu-O-i-Pr)]2'
_chemical_formula_moiety         'C80 H116 N2 O6 V2'
_chemical_formula_sum            'C80 H116 N2 O6 V2'
_chemical_formula_weight         1303.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   9.6738(7)
_cell_length_b                   17.4718(12)
_cell_length_c                   22.3216(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.642(7)
_cell_angle_gamma                90.00
_cell_volume                     3747.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    3753
_cell_measurement_theta_min      3.1416
_cell_measurement_theta_max      33.9540

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3947
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41164
_diffrn_reflns_av_R_equivalents  0.1726
_diffrn_reflns_av_sigmaI/netI    0.1933
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6590
_reflns_number_gt                2865
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/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         6590
_refine_ls_number_parameters     422
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_restrained_S_all      0.857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.56888(7) 0.43845(4) 0.05084(3) 0.0241(2) Uani 1 1 d . . .
N1 N 0.7091(3) 0.38350(17) 0.06482(14) 0.0255(8) Uani 1 1 d . . .
O1 O 0.6118(2) 0.48953(13) -0.01877(11) 0.0270(7) Uani 1 1 d . . .
O2 O 0.5810(2) 0.48883(13) 0.12355(11) 0.0218(6) Uani 1 1 d . . .
O3 O 0.4415(2) 0.35998(13) 0.04830(11) 0.0248(7) Uani 1 1 d . . .
C1 C 0.7430(4) 0.4812(2) -0.0460(2) 0.0435(12) Uani 1 1 d . . .
H1 H 0.8000 0.4472 -0.0167 0.052 Uiso 1 1 calc R . .
C2 C 0.7224(4) 0.4338(3) -0.1015(2) 0.0605(15) Uani 1 1 d . . .
H2A H 0.6662 0.4623 -0.1333 0.091 Uiso 1 1 calc R . .
H2B H 0.6745 0.3863 -0.0931 0.091 Uiso 1 1 calc R . .
H2C H 0.8131 0.4217 -0.1146 0.091 Uiso 1 1 calc R . .
C3 C 0.8288(4) 0.5500(3) -0.0469(2) 0.0556(14) Uani 1 1 d . . .
H3A H 0.7834 0.5865 -0.0762 0.083 Uiso 1 1 calc R . .
H3B H 0.9203 0.5362 -0.0584 0.083 Uiso 1 1 calc R . .
H3C H 0.8402 0.5734 -0.0067 0.083 Uiso 1 1 calc R . .
C5 C 0.8158(4) 0.3304(2) 0.07643(18) 0.0228(10) Uani 1 1 d . . .
C6 C 0.8841(4) 0.3200(2) 0.1342(2) 0.0444(13) Uani 1 1 d . . .
H6 H 0.8596 0.3506 0.1666 0.053 Uiso 1 1 calc R . .
C7 C 0.9876(4) 0.2653(3) 0.1448(2) 0.0490(14) Uani 1 1 d . . .
H7 H 1.0325 0.2592 0.1847 0.059 Uiso 1 1 calc R . .
C8 C 1.0273(4) 0.2199(2) 0.1004(2) 0.0338(11) Uani 1 1 d . . .
C9 C 0.9580(5) 0.2307(3) 0.0440(2) 0.0717(18) Uani 1 1 d . . .
H9 H 0.9812 0.1990 0.0120 0.086 Uiso 1 1 calc R . .
C10 C 0.8566(5) 0.2852(3) 0.0316(2) 0.0650(17) Uani 1 1 d . . .
H10 H 0.8142 0.2916 -0.0087 0.078 Uiso 1 1 calc R . .
C11 C 1.1414(4) 0.1616(2) 0.1132(2) 0.0465(13) Uani 1 1 d . . .
H11A H 1.2306 0.1845 0.1062 0.070 Uiso 1 1 calc R . .
H11B H 1.1221 0.1175 0.0864 0.070 Uiso 1 1 calc R . .
H11C H 1.1459 0.1449 0.1553 0.070 Uiso 1 1 calc R . .
C12 C 0.6527(4) 0.4624(2) 0.17630(17) 0.0212(9) Uani 1 1 d . . .
C13 C 0.7715(4) 0.5001(2) 0.20377(18) 0.0238(10) Uani 1 1 d . . .
C14 C 0.8418(4) 0.4667(2) 0.25512(17) 0.0260(10) Uani 1 1 d . . .
H14 H 0.9238 0.4911 0.2734 0.031 Uiso 1 1 calc R . .
C15 C 0.7995(4) 0.3998(2) 0.28127(18) 0.0273(10) Uani 1 1 d . . .
C16 C 0.6763(4) 0.3674(2) 0.25518(17) 0.0274(10) Uani 1 1 d . . .
H16 H 0.6415 0.3233 0.2733 0.033 Uiso 1 1 calc R . .
C17 C 0.6019(4) 0.3969(2) 0.20367(17) 0.0242(10) Uani 1 1 d . . .
C18 C 0.8226(4) 0.5765(2) 0.18061(17) 0.0269(10) Uani 1 1 d . . .
C19 C 0.8431(4) 0.5724(2) 0.11362(16) 0.0314(10) Uani 1 1 d . . .
H19A H 0.8881 0.6195 0.1019 0.047 Uiso 1 1 calc R . .
H19B H 0.7524 0.5669 0.0894 0.047 Uiso 1 1 calc R . .
H19C H 0.9018 0.5283 0.1067 0.047 Uiso 1 1 calc R . .
C20 C 0.7133(4) 0.6379(2) 0.19065(18) 0.0338(11) Uani 1 1 d . . .
H20A H 0.7425 0.6873 0.1756 0.051 Uiso 1 1 calc R . .
H20B H 0.7045 0.6421 0.2338 0.051 Uiso 1 1 calc R . .
H20C H 0.6233 0.6234 0.1689 0.051 Uiso 1 1 calc R . .
C21 C 0.9610(4) 0.6025(2) 0.21510(19) 0.0406(12) Uani 1 1 d . . .
H21A H 1.0330 0.5643 0.2104 0.061 Uiso 1 1 calc R . .
H21B H 0.9500 0.6082 0.2580 0.061 Uiso 1 1 calc R . .
H21C H 0.9883 0.6517 0.1990 0.061 Uiso 1 1 calc R . .
C22 C 0.8889(4) 0.3647(2) 0.33570(19) 0.0373(12) Uani 1 1 d . . .
C23 C 1.0346(4) 0.3467(3) 0.3169(2) 0.0564(14) Uani 1 1 d . . .
H23A H 1.0949 0.3268 0.3517 0.085 Uiso 1 1 calc R . .
H23B H 1.0754 0.3936 0.3024 0.085 Uiso 1 1 calc R . .
H23C H 1.0258 0.3084 0.2846 0.085 Uiso 1 1 calc R . .
C24 C 0.9088(5) 0.4228(3) 0.38713(19) 0.0629(15) Uani 1 1 d . . .
H24A H 0.8190 0.4329 0.4019 0.094 Uiso 1 1 calc R . .
H24B H 0.9461 0.4705 0.3725 0.094 Uiso 1 1 calc R . .
H24C H 0.9740 0.4021 0.4200 0.094 Uiso 1 1 calc R . .
C25 C 0.8304(5) 0.2904(3) 0.3567(2) 0.0568(15) Uani 1 1 d . . .
H25A H 0.8930 0.2698 0.3905 0.085 Uiso 1 1 calc R . .
H25B H 0.8216 0.2534 0.3235 0.085 Uiso 1 1 calc R . .
H25C H 0.7386 0.2998 0.3698 0.085 Uiso 1 1 calc R . .
C26 C 0.4655(4) 0.3592(2) 0.17687(17) 0.0259(10) Uani 1 1 d . . .
H26 H 0.4161 0.3974 0.1487 0.031 Uiso 1 1 calc R . .
C27 C 0.3676(4) 0.3408(2) 0.22446(18) 0.0348(11) Uani 1 1 d . . .
H27A H 0.2817 0.3178 0.2047 0.052 Uiso 1 1 calc R . .
H27B H 0.3452 0.3880 0.2449 0.052 Uiso 1 1 calc R . .
H27C H 0.4134 0.3048 0.2540 0.052 Uiso 1 1 calc R . .
C28 C 0.4681(4) 0.2908(2) 0.07647(18) 0.0238(10) Uani 1 1 d . . .
C29 C 0.4739(4) 0.2224(2) 0.04202(18) 0.0290(10) Uani 1 1 d . . .
C30 C 0.5166(4) 0.1567(2) 0.07338(19) 0.0326(11) Uani 1 1 d . . .
H30 H 0.5224 0.1108 0.0510 0.039 Uiso 1 1 calc R . .
C31 C 0.5515(4) 0.1535(2) 0.13572(18) 0.0255(10) Uani 1 1 d . . .
C32 C 0.5333(4) 0.2203(2) 0.16734(18) 0.0274(10) Uani 1 1 d . . .
H32 H 0.5500 0.2194 0.2101 0.033 Uiso 1 1 calc R . .
C33 C 0.4915(3) 0.2889(2) 0.13890(18) 0.0224(10) Uani 1 1 d . . .
C34 C 0.4232(5) 0.2201(2) -0.02579(19) 0.0386(12) Uani 1 1 d . . .
C35 C 0.2707(4) 0.2444(3) -0.0349(2) 0.0531(14) Uani 1 1 d . . .
H35A H 0.2614 0.2955 -0.0177 0.080 Uiso 1 1 calc R . .
H35B H 0.2149 0.2078 -0.0147 0.080 Uiso 1 1 calc R . .
H35C H 0.2381 0.2456 -0.0781 0.080 Uiso 1 1 calc R . .
C36 C 0.5083(5) 0.2726(3) -0.0624(2) 0.0498(13) Uani 1 1 d . . .
H36A H 0.4782 0.2658 -0.1055 0.075 Uiso 1 1 calc R . .
H36B H 0.6072 0.2598 -0.0539 0.075 Uiso 1 1 calc R . .
H36C H 0.4939 0.3260 -0.0512 0.075 Uiso 1 1 calc R . .
C37 C 0.4331(6) 0.1390(3) -0.0521(2) 0.086(2) Uani 1 1 d . . .
H37A H 0.3761 0.1038 -0.0312 0.129 Uiso 1 1 calc R . .
H37B H 0.5303 0.1220 -0.0466 0.129 Uiso 1 1 calc R . .
H37C H 0.3993 0.1398 -0.0952 0.129 Uiso 1 1 calc R . .
C38 C 0.6002(4) 0.0778(2) 0.16563(18) 0.0306(10) Uani 1 1 d . . .
C39 C 0.7280(4) 0.0491(2) 0.1377(2) 0.0461(12) Uani 1 1 d . . .
H39A H 0.7023 0.0389 0.0947 0.069 Uiso 1 1 calc R . .
H39B H 0.7622 0.0019 0.1579 0.069 Uiso 1 1 calc R . .
H39C H 0.8012 0.0881 0.1426 0.069 Uiso 1 1 calc R . .
C40 C 0.4819(4) 0.0189(2) 0.15577(19) 0.0412(12) Uani 1 1 d . . .
H40A H 0.4015 0.0373 0.1746 0.062 Uiso 1 1 calc R . .
H40B H 0.5135 -0.0300 0.1740 0.062 Uiso 1 1 calc R . .
H40C H 0.4552 0.0117 0.1124 0.062 Uiso 1 1 calc R . .
C41 C 0.6413(4) 0.0869(2) 0.23366(18) 0.0415(12) Uani 1 1 d . . .
H41A H 0.7115 0.1273 0.2409 0.062 Uiso 1 1 calc R . .
H41B H 0.6798 0.0385 0.2504 0.062 Uiso 1 1 calc R . .
H41C H 0.5591 0.1006 0.2531 0.062 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0257(4) 0.0209(4) 0.0254(4) 0.0006(4) 0.0015(3) 0.0011(3)
N1 0.0197(18) 0.028(2) 0.029(2) 0.0012(16) 0.0018(15) 0.0049(15)
O1 0.0302(16) 0.0206(15) 0.0315(17) 0.0049(13) 0.0093(13) 0.0026(12)
O2 0.0246(15) 0.0195(15) 0.0208(16) 0.0008(12) 0.0002(12) -0.0051(11)
O3 0.0271(16) 0.0203(16) 0.0272(17) 0.0004(13) 0.0039(12) 0.0025(12)
C1 0.049(3) 0.032(3) 0.056(3) -0.003(2) 0.035(3) 0.004(2)
C2 0.028(3) 0.107(4) 0.048(3) -0.028(3) 0.010(2) -0.004(3)
C3 0.036(3) 0.077(4) 0.055(3) -0.023(3) 0.012(2) -0.016(3)
C5 0.016(2) 0.024(2) 0.028(3) 0.0073(19) 0.0022(19) 0.0075(18)
C6 0.043(3) 0.051(3) 0.037(3) -0.018(2) -0.006(2) 0.026(2)
C7 0.046(3) 0.069(4) 0.030(3) -0.004(3) -0.007(2) 0.029(3)
C8 0.027(3) 0.034(3) 0.040(3) 0.002(2) 0.005(2) 0.008(2)
C9 0.067(4) 0.093(4) 0.051(4) -0.031(3) -0.010(3) 0.052(3)
C10 0.069(4) 0.084(4) 0.037(3) -0.026(3) -0.016(3) 0.055(3)
C11 0.029(3) 0.051(3) 0.059(3) 0.015(3) 0.004(2) 0.018(2)
C12 0.021(2) 0.024(2) 0.018(2) -0.0018(18) -0.0015(18) 0.0007(18)
C13 0.025(2) 0.018(2) 0.029(2) -0.0037(19) 0.0019(19) 0.0064(18)
C14 0.025(2) 0.028(2) 0.026(2) -0.005(2) 0.0032(19) -0.0042(18)
C15 0.030(2) 0.026(2) 0.025(2) 0.003(2) 0.000(2) 0.003(2)
C16 0.033(3) 0.020(2) 0.029(3) 0.006(2) 0.001(2) 0.0041(19)
C17 0.028(2) 0.019(2) 0.025(3) -0.004(2) 0.001(2) 0.0044(19)
C18 0.027(2) 0.028(3) 0.024(2) 0.000(2) -0.0040(19) -0.0042(19)
C19 0.033(2) 0.032(3) 0.029(3) 0.002(2) 0.0023(19) -0.006(2)
C20 0.042(3) 0.023(3) 0.036(3) -0.003(2) 0.004(2) -0.005(2)
C21 0.047(3) 0.032(3) 0.041(3) 0.005(2) -0.003(2) -0.011(2)
C22 0.051(3) 0.029(3) 0.029(3) 0.004(2) -0.011(2) 0.003(2)
C23 0.047(3) 0.063(3) 0.055(3) 0.020(3) -0.010(3) 0.011(3)
C24 0.098(4) 0.056(4) 0.031(3) 0.005(3) -0.010(3) 0.005(3)
C25 0.065(3) 0.055(3) 0.046(3) 0.028(3) -0.012(3) -0.009(3)
C26 0.028(2) 0.020(2) 0.030(3) -0.001(2) 0.0043(19) -0.0027(18)
C27 0.034(3) 0.035(3) 0.037(3) -0.003(2) 0.009(2) -0.003(2)
C28 0.021(2) 0.017(2) 0.032(3) 0.004(2) -0.0002(19) 0.0041(17)
C29 0.032(3) 0.026(3) 0.027(3) 0.005(2) -0.002(2) -0.0016(19)
C30 0.035(3) 0.023(2) 0.040(3) -0.001(2) 0.002(2) 0.001(2)
C31 0.023(2) 0.023(2) 0.030(3) 0.005(2) 0.0014(19) -0.0034(18)
C32 0.026(2) 0.025(3) 0.029(3) -0.001(2) -0.0027(19) -0.0006(19)
C33 0.015(2) 0.020(2) 0.031(3) 0.003(2) 0.0011(18) -0.0015(17)
C34 0.053(3) 0.029(3) 0.031(3) 0.001(2) -0.002(2) 0.003(2)
C35 0.060(3) 0.056(3) 0.038(3) 0.006(3) -0.017(3) -0.017(3)
C36 0.067(3) 0.049(3) 0.035(3) -0.001(3) 0.013(3) 0.011(3)
C37 0.175(6) 0.038(3) 0.037(3) -0.014(3) -0.022(3) 0.015(4)
C38 0.032(3) 0.025(3) 0.035(3) 0.008(2) 0.003(2) 0.0040(19)
C39 0.050(3) 0.037(3) 0.052(3) 0.005(2) 0.008(2) 0.020(2)
C40 0.046(3) 0.028(3) 0.048(3) 0.009(2) 0.001(2) 0.002(2)
C41 0.050(3) 0.035(3) 0.037(3) 0.007(2) -0.006(2) 0.011(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.662(3) . ?
V1 O2 1.838(2) . ?
V1 O3 1.840(2) . ?
V1 O1 1.879(3) . ?
V1 O1 2.205(2) 3_665 ?
N1 C5 1.390(4) . ?
O1 C1 1.476(4) . ?
O1 V1 2.205(2) 3_665 ?
O2 C12 1.376(4) . ?
O3 C28 1.373(4) . ?
C1 C3 1.463(5) . ?
C1 C2 1.483(5) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C10 1.370(5) . ?
C5 C6 1.392(5) . ?
C6 C7 1.384(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.358(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(6) . ?
C8 C11 1.505(5) . ?
C9 C10 1.372(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.402(5) . ?
C12 C17 1.412(5) . ?
C13 C14 1.392(5) . ?
C13 C18 1.535(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(5) . ?
C15 C22 1.535(5) . ?
C16 C17 1.384(5) . ?
C16 H16 0.9500 . ?
C17 C26 1.533(5) . ?
C18 C19 1.533(5) . ?
C18 C21 1.534(5) . ?
C18 C20 1.541(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.513(5) . ?
C22 C24 1.527(6) . ?
C22 C23 1.549(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.529(5) . ?
C26 C27 1.537(5) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.386(5) . ?
C28 C29 1.425(5) . ?
C29 C30 1.382(5) . ?
C29 C34 1.537(5) . ?
C30 C31 1.395(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(5) . ?
C31 C38 1.532(5) . ?
C32 C33 1.394(5) . ?
C32 H32 0.9500 . ?
C34 C35 1.526(5) . ?
C34 C36 1.531(6) . ?
C34 C37 1.541(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.533(5) . ?
C38 C41 1.533(5) . ?
C38 C40 1.536(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O2 98.25(13) . . ?
N1 V1 O3 96.00(13) . . ?
O2 V1 O3 110.98(11) . . ?
N1 V1 O1 100.15(13) . . ?
O2 V1 O1 120.33(10) . . ?
O3 V1 O1 122.65(11) . . ?
N1 V1 O1 171.87(14) . 3_665 ?
O2 V1 O1 88.88(10) . 3_665 ?
O3 V1 O1 84.97(10) . 3_665 ?
O1 V1 O1 72.73(11) . 3_665 ?
C5 N1 V1 173.3(3) . . ?
C1 O1 V1 125.1(2) . . ?
C1 O1 V1 127.6(2) . 3_665 ?
V1 O1 V1 107.27(11) . 3_665 ?
C12 O2 V1 124.7(2) . . ?
C28 O3 V1 123.5(2) . . ?
C3 C1 O1 116.2(3) . . ?
C3 C1 C2 117.9(4) . . ?
O1 C1 C2 111.1(3) . . ?
C3 C1 H1 103.0 . . ?
O1 C1 H1 103.0 . . ?
C2 C1 H1 103.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C5 N1 121.3(4) . . ?
C10 C5 C6 117.2(4) . . ?
N1 C5 C6 121.5(4) . . ?
C7 C6 C5 120.3(4) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 122.6(4) . . ?
C8 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C7 C8 C9 116.2(4) . . ?
C7 C8 C11 121.3(4) . . ?
C9 C8 C11 122.5(4) . . ?
C8 C9 C10 122.9(5) . . ?
C8 C9 H9 118.5 . . ?
C10 C9 H9 118.5 . . ?
C5 C10 C9 120.8(4) . . ?
C5 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 C13 121.6(3) . . ?
O2 C12 C17 118.4(3) . . ?
C13 C12 C17 120.0(3) . . ?
C14 C13 C12 117.5(3) . . ?
C14 C13 C18 119.7(3) . . ?
C12 C13 C18 122.7(3) . . ?
C15 C14 C13 124.0(3) . . ?
C15 C14 H14 118.0 . . ?
C13 C14 H14 118.0 . . ?
C16 C15 C14 116.6(3) . . ?
C16 C15 C22 123.2(4) . . ?
C14 C15 C22 120.1(3) . . ?
C17 C16 C15 122.4(4) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C12 119.2(3) . . ?
C16 C17 C26 120.3(3) . . ?
C12 C17 C26 120.5(3) . . ?
C19 C18 C21 107.4(3) . . ?
C19 C18 C13 111.8(3) . . ?
C21 C18 C13 112.7(3) . . ?
C19 C18 C20 110.0(3) . . ?
C21 C18 C20 107.1(3) . . ?
C13 C18 C20 107.7(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C24 110.8(4) . . ?
C25 C22 C15 113.0(3) . . ?
C24 C22 C15 109.9(3) . . ?
C25 C22 C23 107.2(4) . . ?
C24 C22 C23 107.4(4) . . ?
C15 C22 C23 108.2(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C33 C26 C17 111.9(3) . . ?
C33 C26 C27 111.7(3) . . ?
C17 C26 C27 113.1(3) . . ?
C33 C26 H26 106.6 . . ?
C17 C26 H26 106.6 . . ?
C27 C26 H26 106.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 118.7(3) . . ?
O3 C28 C29 120.5(4) . . ?
C33 C28 C29 120.7(3) . . ?
C30 C29 C28 116.8(4) . . ?
C30 C29 C34 121.3(4) . . ?
C28 C29 C34 121.7(3) . . ?
C29 C30 C31 124.2(4) . . ?
C29 C30 H30 117.9 . . ?
C31 C30 H30 117.9 . . ?
C32 C31 C30 116.4(4) . . ?
C32 C31 C38 123.8(4) . . ?
C30 C31 C38 119.7(4) . . ?
C31 C32 C33 122.6(4) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 H32 118.7 . . ?
C28 C33 C32 118.9(4) . . ?
C28 C33 C26 121.4(3) . . ?
C32 C33 C26 119.7(4) . . ?
C35 C34 C36 109.5(3) . . ?
C35 C34 C29 108.5(4) . . ?
C36 C34 C29 112.3(3) . . ?
C35 C34 C37 107.9(4) . . ?
C36 C34 C37 106.7(4) . . ?
C29 C34 C37 111.9(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C31 C38 C39 109.1(3) . . ?
C31 C38 C41 112.0(3) . . ?
C39 C38 C41 107.9(3) . . ?
C31 C38 C40 109.3(3) . . ?
C39 C38 C40 110.2(3) . . ?
C41 C38 C40 108.4(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 -3.6(3) . . . . ?
O2 V1 O1 C1 102.3(3) . . . . ?
O3 V1 O1 C1 -107.6(3) . . . . ?
O1 V1 O1 C1 -179.6(3) 3_665 . . . ?
N1 V1 O1 V1 175.98(13) . . . 3_665 ?
O2 V1 O1 V1 -78.14(13) . . . 3_665 ?
O3 V1 O1 V1 72.04(14) . . . 3_665 ?
O1 V1 O1 V1 0.0 3_665 . . 3_665 ?
N1 V1 O2 C12 -21.6(3) . . . . ?
O3 V1 O2 C12 78.1(3) . . . . ?
O1 V1 O2 C12 -128.5(3) . . . . ?
O1 V1 O2 C12 162.3(3) 3_665 . . . ?
N1 V1 O3 C28 23.8(3) . . . . ?
O2 V1 O3 C28 -77.4(3) . . . . ?
O1 V1 O3 C28 130.0(3) . . . . ?
O1 V1 O3 C28 -164.3(3) 3_665 . . . ?
V1 O1 C1 C3 -116.6(4) . . . . ?
V1 O1 C1 C3 63.9(5) 3_665 . . . ?
V1 O1 C1 C2 105.0(4) . . . . ?
V1 O1 C1 C2 -74.5(4) 3_665 . . . ?
C10 C5 C6 C7 -0.7(7) . . . . ?
N1 C5 C6 C7 178.3(4) . . . . ?
C5 C6 C7 C8 0.1(7) . . . . ?
C6 C7 C8 C9 -0.6(7) . . . . ?
C6 C7 C8 C11 179.2(4) . . . . ?
C7 C8 C9 C10 1.7(8) . . . . ?
C11 C8 C9 C10 -178.1(5) . . . . ?
N1 C5 C10 C9 -177.2(4) . . . . ?
C6 C5 C10 C9 1.8(7) . . . . ?
C8 C9 C10 C5 -2.4(9) . . . . ?
V1 O2 C12 C13 113.4(3) . . . . ?
V1 O2 C12 C17 -68.4(4) . . . . ?
O2 C12 C13 C14 -176.4(3) . . . . ?
C17 C12 C13 C14 5.4(5) . . . . ?
O2 C12 C13 C18 5.5(5) . . . . ?
C17 C12 C13 C18 -172.7(3) . . . . ?
C12 C13 C14 C15 -1.6(6) . . . . ?
C18 C13 C14 C15 176.6(3) . . . . ?
C13 C14 C15 C16 -2.8(6) . . . . ?
C13 C14 C15 C22 176.3(4) . . . . ?
C14 C15 C16 C17 3.6(6) . . . . ?
C22 C15 C16 C17 -175.5(4) . . . . ?
C15 C16 C17 C12 0.1(6) . . . . ?
C15 C16 C17 C26 -179.6(4) . . . . ?
O2 C12 C17 C16 177.0(3) . . . . ?
C13 C12 C17 C16 -4.8(5) . . . . ?
O2 C12 C17 C26 -3.3(5) . . . . ?
C13 C12 C17 C26 174.9(3) . . . . ?
C14 C13 C18 C19 127.8(4) . . . . ?
C12 C13 C18 C19 -54.1(5) . . . . ?
C14 C13 C18 C21 6.6(5) . . . . ?
C12 C13 C18 C21 -175.2(4) . . . . ?
C14 C13 C18 C20 -111.3(4) . . . . ?
C12 C13 C18 C20 66.9(4) . . . . ?
C16 C15 C22 C25 1.5(6) . . . . ?
C14 C15 C22 C25 -177.6(4) . . . . ?
C16 C15 C22 C24 -122.9(4) . . . . ?
C14 C15 C22 C24 58.0(5) . . . . ?
C16 C15 C22 C23 120.0(4) . . . . ?
C14 C15 C22 C23 -59.1(5) . . . . ?
C16 C17 C26 C33 -80.7(4) . . . . ?
C12 C17 C26 C33 99.6(4) . . . . ?
C16 C17 C26 C27 46.4(5) . . . . ?
C12 C17 C26 C27 -133.2(4) . . . . ?
V1 O3 C28 C33 64.9(4) . . . . ?
V1 O3 C28 C29 -114.0(3) . . . . ?
O3 C28 C29 C30 172.9(3) . . . . ?
C33 C28 C29 C30 -5.9(5) . . . . ?
O3 C28 C29 C34 -12.3(6) . . . . ?
C33 C28 C29 C34 168.8(4) . . . . ?
C28 C29 C30 C31 0.9(6) . . . . ?
C34 C29 C30 C31 -173.9(4) . . . . ?
C29 C30 C31 C32 4.0(6) . . . . ?
C29 C30 C31 C38 -178.8(3) . . . . ?
C30 C31 C32 C33 -4.3(5) . . . . ?
C38 C31 C32 C33 178.7(3) . . . . ?
O3 C28 C33 C32 -173.1(3) . . . . ?
C29 C28 C33 C32 5.8(5) . . . . ?
O3 C28 C33 C26 9.9(5) . . . . ?
C29 C28 C33 C26 -171.2(3) . . . . ?
C31 C32 C33 C28 -0.5(5) . . . . ?
C31 C32 C33 C26 176.5(3) . . . . ?
C17 C26 C33 C28 -106.2(4) . . . . ?
C27 C26 C33 C28 125.9(4) . . . . ?
C17 C26 C33 C32 76.9(4) . . . . ?
C27 C26 C33 C32 -51.0(4) . . . . ?
C30 C29 C34 C35 116.4(4) . . . . ?
C28 C29 C34 C35 -58.1(5) . . . . ?
C30 C29 C34 C36 -122.4(4) . . . . ?
C28 C29 C34 C36 63.1(5) . . . . ?
C30 C29 C34 C37 -2.5(6) . . . . ?
C28 C29 C34 C37 -177.0(4) . . . . ?
C32 C31 C38 C39 -125.6(4) . . . . ?
C30 C31 C38 C39 57.5(5) . . . . ?
C32 C31 C38 C41 -6.2(5) . . . . ?
C30 C31 C38 C41 176.8(3) . . . . ?
C32 C31 C38 C40 113.9(4) . . . . ?
C30 C31 C38 C40 -63.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.063

data_5
_database_code_depnum_ccdc_archive 'CCDC 718355'

_chemical_name_common            'Compound 5'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4Cl)(diphenolate)(mu-O-i-Pr)]2'
_chemical_formula_moiety         'C78 H110 Cl2 N2 O6 V2'
_chemical_formula_sum            'C78 H110 Cl2 N2 O6 V2'
_chemical_formula_weight         1344.46

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   9.8290(5)
_cell_length_b                   17.5429(9)
_cell_length_c                   21.4878(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.687(5)
_cell_angle_gamma                90.00
_cell_volume                     3692.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    5477
_cell_measurement_theta_min      3.5538
_cell_measurement_theta_max      27.4995

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.56
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42947
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_sigmaI/netI    0.2670
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         27.66
_reflns_number_total             8590
_reflns_number_gt                2881
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

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

The crystal was weakly diffracting and this meant that the ratio of
observed to unique reflections is low.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/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         8590
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0673
_refine_ls_goodness_of_fit_ref   0.691
_refine_ls_restrained_S_all      0.691
_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 0.57150(4) 0.43730(2) 0.04975(2) 0.02389(13) Uani 1 1 d . . .
Cl1 Cl 1.14748(8) 0.15767(5) 0.11961(4) 0.0567(3) Uani 1 1 d . . .
N1 N 0.70759(19) 0.38155(11) 0.06055(9) 0.0217(5) Uani 1 1 d . . .
O1 O 0.59943(15) 0.48556(9) -0.02632(7) 0.0244(4) Uani 1 1 d . . .
O2 O 0.58900(15) 0.48706(9) 0.12604(7) 0.0221(4) Uani 1 1 d . . .
O3 O 0.44253(15) 0.36215(9) 0.05136(7) 0.0225(4) Uani 1 1 d . . .
C1 C 0.7088(3) 0.48205(16) -0.06852(13) 0.0369(8) Uani 1 1 d . . .
H1 H 0.6762 0.5152 -0.1045 0.044 Uiso 1 1 calc R . .
C2 C 0.7235(3) 0.40617(17) -0.09622(13) 0.0500(9) Uani 1 1 d . . .
H2A H 0.7937 0.4080 -0.1261 0.075 Uiso 1 1 calc R . .
H2B H 0.6363 0.3906 -0.1179 0.075 Uiso 1 1 calc R . .
H2C H 0.7504 0.3693 -0.0632 0.075 Uiso 1 1 calc R . .
C3 C 0.8333(3) 0.51934(19) -0.04168(13) 0.0556(10) Uani 1 1 d . . .
H3A H 0.8116 0.5711 -0.0286 0.083 Uiso 1 1 calc R . .
H3B H 0.9001 0.5217 -0.0731 0.083 Uiso 1 1 calc R . .
H3C H 0.8715 0.4902 -0.0055 0.083 Uiso 1 1 calc R . .
C5 C 0.8120(3) 0.32887(15) 0.07453(12) 0.0232(7) Uani 1 1 d . . .
C6 C 0.8161(3) 0.26127(16) 0.04179(13) 0.0379(8) Uani 1 1 d . . .
H6 H 0.7478 0.2510 0.0090 0.045 Uiso 1 1 calc R . .
C7 C 0.9183(3) 0.20808(16) 0.05604(14) 0.0424(8) Uani 1 1 d . . .
H7 H 0.9193 0.1614 0.0337 0.051 Uiso 1 1 calc R . .
C8 C 1.0174(3) 0.22340(16) 0.10242(13) 0.0330(7) Uani 1 1 d . . .
C9 C 1.0158(3) 0.2897(2) 0.13510(14) 0.0578(10) Uani 1 1 d . . .
H9 H 1.0854 0.2997 0.1674 0.069 Uiso 1 1 calc R . .
C10 C 0.9136(3) 0.34243(17) 0.12149(14) 0.0475(9) Uani 1 1 d . . .
H10 H 0.9131 0.3885 0.1447 0.057 Uiso 1 1 calc R . .
C12 C 0.6613(3) 0.46054(14) 0.17920(11) 0.0206(6) Uani 1 1 d . . .
C13 C 0.7780(2) 0.49959(14) 0.20605(12) 0.0215(7) Uani 1 1 d . . .
C14 C 0.8488(2) 0.46580(14) 0.25677(12) 0.0236(7) Uani 1 1 d . . .
H14 H 0.9286 0.4909 0.2743 0.028 Uiso 1 1 calc R . .
C15 C 0.8126(3) 0.39819(15) 0.28405(12) 0.0249(7) Uani 1 1 d . . .
C16 C 0.6930(3) 0.36397(14) 0.25921(12) 0.0265(7) Uani 1 1 d . . .
H16 H 0.6631 0.3183 0.2776 0.032 Uiso 1 1 calc R . .
C17 C 0.6151(3) 0.39475(14) 0.20775(12) 0.0220(6) Uani 1 1 d . . .
C18 C 0.8237(2) 0.57712(14) 0.18211(11) 0.0248(7) Uani 1 1 d . . .
C19 C 0.8422(2) 0.57455(14) 0.11145(10) 0.0294(7) Uani 1 1 d . . .
H19A H 0.7525 0.5723 0.0880 0.044 Uiso 1 1 calc R . .
H19B H 0.8953 0.5293 0.1021 0.044 Uiso 1 1 calc R . .
H19C H 0.8906 0.6204 0.0995 0.044 Uiso 1 1 calc R . .
C20 C 0.7167(2) 0.63693(13) 0.19597(12) 0.0306(7) Uani 1 1 d . . .
H20A H 0.6281 0.6226 0.1750 0.046 Uiso 1 1 calc R . .
H20B H 0.7442 0.6868 0.1807 0.046 Uiso 1 1 calc R . .
H20C H 0.7094 0.6397 0.2411 0.046 Uiso 1 1 calc R . .
C21 C 0.9615(2) 0.60277(15) 0.21454(12) 0.0352(7) Uani 1 1 d . . .
H21A H 0.9866 0.6524 0.1980 0.053 Uiso 1 1 calc R . .
H21B H 1.0319 0.5652 0.2067 0.053 Uiso 1 1 calc R . .
H21C H 0.9539 0.6070 0.2596 0.053 Uiso 1 1 calc R . .
C22 C 0.9041(3) 0.36441(15) 0.33838(12) 0.0314(7) Uani 1 1 d . . .
C23 C 1.0437(3) 0.34566(17) 0.31520(14) 0.0488(8) Uani 1 1 d . . .
H23A H 1.0837 0.3920 0.2989 0.073 Uiso 1 1 calc R . .
H23B H 1.0325 0.3074 0.2820 0.073 Uiso 1 1 calc R . .
H23C H 1.1042 0.3256 0.3499 0.073 Uiso 1 1 calc R . .
C24 C 0.9223(3) 0.42149(16) 0.39215(13) 0.0562(9) Uani 1 1 d . . .
H24A H 0.8340 0.4307 0.4089 0.084 Uiso 1 1 calc R . .
H24B H 0.9580 0.4695 0.3769 0.084 Uiso 1 1 calc R . .
H24C H 0.9866 0.4008 0.4252 0.084 Uiso 1 1 calc R . .
C25 C 0.8453(3) 0.29070(16) 0.36323(12) 0.0458(8) Uani 1 1 d . . .
H25A H 0.9095 0.2694 0.3960 0.069 Uiso 1 1 calc R . .
H25B H 0.8305 0.2538 0.3291 0.069 Uiso 1 1 calc R . .
H25C H 0.7582 0.3017 0.3805 0.069 Uiso 1 1 calc R . .
C26 C 0.4816(2) 0.35640(13) 0.18394(11) 0.0202(6) Uani 1 1 d . . .
H26 H 0.4292 0.3949 0.1573 0.024 Uiso 1 1 calc R . .
C27 C 0.3931(2) 0.33683(14) 0.23752(11) 0.0275(7) Uani 1 1 d . . .
H27A H 0.3091 0.3116 0.2206 0.041 Uiso 1 1 calc R . .
H27B H 0.3700 0.3837 0.2591 0.041 Uiso 1 1 calc R . .
H27C H 0.4438 0.3026 0.2671 0.041 Uiso 1 1 calc R . .
C28 C 0.4674(2) 0.29120(15) 0.07813(12) 0.0223(6) Uani 1 1 d . . .
C29 C 0.4592(2) 0.22336(15) 0.04176(12) 0.0243(7) Uani 1 1 d . . .
C30 C 0.5018(2) 0.15679(14) 0.07179(12) 0.0248(7) Uani 1 1 d . . .
H30 H 0.5008 0.1114 0.0477 0.030 Uiso 1 1 calc R . .
C31 C 0.5461(2) 0.15169(15) 0.13490(12) 0.0225(6) Uani 1 1 d . . .
C32 C 0.5408(2) 0.21770(14) 0.16954(12) 0.0243(7) Uani 1 1 d . . .
H32 H 0.5666 0.2158 0.2131 0.029 Uiso 1 1 calc R . .
C33 C 0.4989(2) 0.28709(15) 0.14271(12) 0.0220(6) Uani 1 1 d . . .
C34 C 0.3978(3) 0.22265(15) -0.02589(12) 0.0286(7) Uani 1 1 d . . .
C35 C 0.2506(2) 0.25251(14) -0.02796(12) 0.0328(7) Uani 1 1 d . . .
H35A H 0.1960 0.2186 -0.0037 0.049 Uiso 1 1 calc R . .
H35B H 0.2114 0.2541 -0.0714 0.049 Uiso 1 1 calc R . .
H35C H 0.2505 0.3039 -0.0101 0.049 Uiso 1 1 calc R . .
C36 C 0.3940(3) 0.14183(15) -0.05391(13) 0.0534(9) Uani 1 1 d . . .
H36A H 0.4872 0.1220 -0.0538 0.080 Uiso 1 1 calc R . .
H36B H 0.3522 0.1436 -0.0969 0.080 Uiso 1 1 calc R . .
H36C H 0.3402 0.1084 -0.0289 0.080 Uiso 1 1 calc R . .
C37 C 0.4806(3) 0.27185(15) -0.06801(12) 0.0388(8) Uani 1 1 d . . .
H37A H 0.4753 0.3254 -0.0554 0.058 Uiso 1 1 calc R . .
H37B H 0.4433 0.2664 -0.1115 0.058 Uiso 1 1 calc R . .
H37C H 0.5761 0.2552 -0.0641 0.058 Uiso 1 1 calc R . .
C38 C 0.5924(3) 0.07497(14) 0.16267(12) 0.0276(7) Uani 1 1 d . . .
C39 C 0.7137(3) 0.04511(14) 0.12912(12) 0.0426(8) Uani 1 1 d . . .
H39A H 0.6866 0.0399 0.0844 0.064 Uiso 1 1 calc R . .
H39B H 0.7420 -0.0047 0.1464 0.064 Uiso 1 1 calc R . .
H39C H 0.7899 0.0811 0.1351 0.064 Uiso 1 1 calc R . .
C40 C 0.4726(3) 0.01825(14) 0.15371(12) 0.0371(8) Uani 1 1 d . . .
H40A H 0.3946 0.0380 0.1743 0.056 Uiso 1 1 calc R . .
H40B H 0.5005 -0.0310 0.1721 0.056 Uiso 1 1 calc R . .
H40C H 0.4466 0.0117 0.1090 0.056 Uiso 1 1 calc R . .
C41 C 0.6368(3) 0.08009(14) 0.23263(11) 0.0366(7) Uani 1 1 d . . .
H41A H 0.7147 0.1148 0.2392 0.055 Uiso 1 1 calc R . .
H41B H 0.6631 0.0294 0.2485 0.055 Uiso 1 1 calc R . .
H41C H 0.5608 0.0993 0.2550 0.055 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0256(3) 0.0226(3) 0.0234(3) 0.0012(2) 0.0012(2) 0.0017(2)
Cl1 0.0533(6) 0.0715(6) 0.0461(5) 0.0159(5) 0.0090(4) 0.0405(5)
N1 0.0205(13) 0.0260(13) 0.0181(13) 0.0014(10) -0.0006(10) -0.0007(11)
O1 0.0277(10) 0.0245(10) 0.0229(11) 0.0018(8) 0.0131(9) 0.0029(9)
O2 0.0241(10) 0.0177(10) 0.0238(11) 0.0008(8) -0.0023(9) 0.0007(8)
O3 0.0258(11) 0.0211(11) 0.0205(10) 0.0011(8) 0.0009(8) 0.0025(9)
C1 0.0380(19) 0.0329(19) 0.042(2) 0.0023(16) 0.0183(17) 0.0013(16)
C2 0.051(2) 0.060(2) 0.042(2) -0.0149(18) 0.0214(17) -0.0008(18)
C3 0.0320(19) 0.091(3) 0.046(2) -0.0232(19) 0.0156(17) -0.0117(19)
C5 0.0242(17) 0.0249(17) 0.0213(17) 0.0020(13) 0.0064(14) -0.0003(14)
C6 0.0358(19) 0.041(2) 0.035(2) -0.0063(16) -0.0097(15) 0.0112(17)
C7 0.044(2) 0.0330(19) 0.050(2) -0.0075(16) -0.0007(17) 0.0118(17)
C8 0.0337(19) 0.0374(19) 0.0286(19) 0.0026(16) 0.0063(15) 0.0146(16)
C9 0.038(2) 0.085(3) 0.047(2) -0.016(2) -0.0209(17) 0.027(2)
C10 0.0365(19) 0.048(2) 0.055(2) -0.0255(18) -0.0139(17) 0.0172(18)
C12 0.0242(16) 0.0218(16) 0.0158(16) -0.0005(13) 0.0014(13) 0.0053(13)
C13 0.0216(16) 0.0213(16) 0.0217(17) -0.0025(13) 0.0019(13) 0.0031(14)
C14 0.0212(16) 0.0249(17) 0.0247(17) -0.0021(13) 0.0010(13) -0.0035(13)
C15 0.0256(17) 0.0253(16) 0.0237(17) -0.0011(14) 0.0015(13) 0.0008(14)
C16 0.0264(17) 0.0186(16) 0.0349(19) -0.0024(14) 0.0052(15) -0.0035(14)
C17 0.0260(17) 0.0201(15) 0.0200(17) -0.0044(13) 0.0034(13) 0.0017(14)
C18 0.0227(16) 0.0272(17) 0.0243(17) 0.0023(13) 0.0012(13) 0.0007(14)
C19 0.0341(17) 0.0284(17) 0.0258(17) 0.0034(13) 0.0043(13) -0.0008(14)
C20 0.0355(18) 0.0226(17) 0.0344(18) -0.0049(14) 0.0079(14) -0.0018(14)
C21 0.0377(18) 0.0332(17) 0.0335(19) 0.0067(14) -0.0045(15) -0.0081(15)
C22 0.0383(19) 0.0262(17) 0.0282(18) 0.0095(14) -0.0068(15) -0.0037(15)
C23 0.0347(19) 0.056(2) 0.053(2) 0.0228(18) -0.0104(16) 0.0051(17)
C24 0.075(2) 0.053(2) 0.037(2) 0.0033(18) -0.0183(18) -0.0051(19)
C25 0.043(2) 0.050(2) 0.042(2) 0.0206(17) -0.0117(16) -0.0036(17)
C26 0.0205(15) 0.0177(15) 0.0220(16) 0.0028(13) -0.0011(13) -0.0006(13)
C27 0.0248(16) 0.0261(16) 0.0313(17) 0.0013(14) 0.0007(13) 0.0000(14)
C28 0.0173(16) 0.0238(17) 0.0260(18) 0.0033(14) 0.0026(13) 0.0039(13)
C29 0.0240(16) 0.0238(17) 0.0250(18) -0.0009(14) 0.0018(13) 0.0020(14)
C30 0.0321(17) 0.0186(16) 0.0237(17) -0.0048(13) 0.0016(14) -0.0008(14)
C31 0.0212(16) 0.0195(16) 0.0266(18) 0.0020(14) 0.0000(13) 0.0033(13)
C32 0.0242(16) 0.0249(17) 0.0229(17) 0.0042(14) -0.0042(13) 0.0030(14)
C33 0.0173(15) 0.0244(17) 0.0240(18) -0.0019(13) 0.0002(13) -0.0041(13)
C34 0.0394(19) 0.0232(17) 0.0227(17) 0.0009(14) -0.0003(14) 0.0024(15)
C35 0.0291(18) 0.0389(19) 0.0287(18) -0.0013(14) -0.0087(14) -0.0075(15)
C36 0.090(3) 0.0344(19) 0.0316(19) -0.0112(16) -0.0185(18) 0.0112(19)
C37 0.0419(19) 0.049(2) 0.0248(18) -0.0002(16) -0.0024(15) 0.0041(16)
C38 0.0298(17) 0.0206(16) 0.0316(18) 0.0047(14) -0.0018(14) 0.0026(14)
C39 0.0486(19) 0.0333(19) 0.046(2) 0.0096(15) 0.0069(17) 0.0127(16)
C40 0.0486(19) 0.0250(17) 0.0365(19) 0.0061(14) -0.0027(15) 0.0047(16)
C41 0.0442(19) 0.0277(18) 0.0362(19) 0.0106(14) -0.0077(15) 0.0063(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.658(2) . ?
V1 O3 1.8313(16) . ?
V1 O2 1.8527(16) . ?
V1 O1 1.8808(16) . ?
V1 O1 2.1838(16) 3_665 ?
Cl1 C8 1.739(3) . ?
N1 C5 1.395(3) . ?
O1 C1 1.464(3) . ?
O1 V1 2.1838(16) 3_665 ?
O2 C12 1.376(3) . ?
O3 C28 1.385(3) . ?
C1 C3 1.463(3) . ?
C1 C2 1.470(3) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.381(3) . ?
C5 C10 1.381(3) . ?
C6 C7 1.387(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.362(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.359(4) . ?
C9 C10 1.380(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 C17 1.400(3) . ?
C12 C13 1.418(3) . ?
C13 C14 1.378(3) . ?
C13 C18 1.534(3) . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 C22 1.534(3) . ?
C16 C17 1.401(3) . ?
C16 H16 0.9500 . ?
C17 C26 1.525(3) . ?
C18 C20 1.532(3) . ?
C18 C21 1.539(3) . ?
C18 C19 1.545(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.529(3) . ?
C22 C25 1.530(3) . ?
C22 C23 1.533(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.522(3) . ?
C26 C27 1.538(3) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.399(3) . ?
C28 C29 1.423(3) . ?
C29 C30 1.383(3) . ?
C29 C34 1.528(3) . ?
C30 C31 1.393(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.380(3) . ?
C31 C38 1.527(3) . ?
C32 C33 1.395(3) . ?
C32 H32 0.9500 . ?
C34 C37 1.532(3) . ?
C34 C35 1.536(3) . ?
C34 C36 1.540(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C41 1.533(3) . ?
C38 C39 1.535(3) . ?
C38 C40 1.542(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O3 97.15(8) . . ?
N1 V1 O2 97.97(9) . . ?
O3 V1 O2 109.68(7) . . ?
N1 V1 O1 102.34(8) . . ?
O3 V1 O1 119.40(7) . . ?
O2 V1 O1 123.19(7) . . ?
N1 V1 O1 173.97(8) . 3_665 ?
O3 V1 O1 85.97(6) . 3_665 ?
O2 V1 O1 85.76(7) . 3_665 ?
O1 V1 O1 71.63(7) . 3_665 ?
C5 N1 V1 172.54(17) . . ?
C1 O1 V1 133.34(15) . . ?
C1 O1 V1 118.27(14) . 3_665 ?
V1 O1 V1 108.37(7) . 3_665 ?
C12 O2 V1 125.42(14) . . ?
C28 O3 V1 123.78(15) . . ?
C3 C1 O1 111.7(2) . . ?
C3 C1 C2 117.3(3) . . ?
O1 C1 C2 113.0(2) . . ?
C3 C1 H1 104.5 . . ?
O1 C1 H1 104.5 . . ?
C2 C1 H1 104.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C6 C5 C10 118.1(3) . . ?
C6 C5 N1 120.7(3) . . ?
C10 C5 N1 121.2(2) . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 120.7(3) . . ?
C9 C8 Cl1 119.8(3) . . ?
C7 C8 Cl1 119.6(2) . . ?
C8 C9 C10 120.2(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C5 120.7(3) . . ?
C9 C10 H10 119.7 . . ?
C5 C10 H10 119.7 . . ?
O2 C12 C17 118.6(2) . . ?
O2 C12 C13 121.3(2) . . ?
C17 C12 C13 120.0(2) . . ?
C14 C13 C12 117.0(2) . . ?
C14 C13 C18 120.2(2) . . ?
C12 C13 C18 122.8(2) . . ?
C13 C14 C15 125.0(2) . . ?
C13 C14 H14 117.5 . . ?
C15 C14 H14 117.5 . . ?
C14 C15 C16 116.6(2) . . ?
C14 C15 C22 119.9(2) . . ?
C16 C15 C22 123.5(2) . . ?
C15 C16 C17 121.9(2) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C12 C17 C16 119.2(2) . . ?
C12 C17 C26 121.1(2) . . ?
C16 C17 C26 119.6(2) . . ?
C20 C18 C13 108.53(18) . . ?
C20 C18 C21 107.7(2) . . ?
C13 C18 C21 112.2(2) . . ?
C20 C18 C19 110.4(2) . . ?
C13 C18 C19 111.4(2) . . ?
C21 C18 C19 106.45(19) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C25 108.3(2) . . ?
C24 C22 C23 109.5(2) . . ?
C25 C22 C23 107.8(2) . . ?
C24 C22 C15 110.3(2) . . ?
C25 C22 C15 112.2(2) . . ?
C23 C22 C15 108.7(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C33 C26 C17 114.45(19) . . ?
C33 C26 C27 110.74(19) . . ?
C17 C26 C27 111.8(2) . . ?
C33 C26 H26 106.4 . . ?
C17 C26 H26 106.4 . . ?
C27 C26 H26 106.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 118.4(2) . . ?
O3 C28 C29 121.6(2) . . ?
C33 C28 C29 120.0(2) . . ?
C30 C29 C28 116.7(2) . . ?
C30 C29 C34 121.2(2) . . ?
C28 C29 C34 122.0(2) . . ?
C29 C30 C31 124.6(2) . . ?
C29 C30 H30 117.7 . . ?
C31 C30 H30 117.7 . . ?
C32 C31 C30 116.7(2) . . ?
C32 C31 C38 123.5(2) . . ?
C30 C31 C38 119.8(2) . . ?
C31 C32 C33 122.2(2) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
C32 C33 C28 119.3(2) . . ?
C32 C33 C26 120.0(2) . . ?
C28 C33 C26 120.7(2) . . ?
C29 C34 C37 111.7(2) . . ?
C29 C34 C35 108.8(2) . . ?
C37 C34 C35 109.6(2) . . ?
C29 C34 C36 112.0(2) . . ?
C37 C34 C36 106.6(2) . . ?
C35 C34 C36 108.1(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C31 C38 C41 112.5(2) . . ?
C31 C38 C39 109.6(2) . . ?
C41 C38 C39 108.1(2) . . ?
C31 C38 C40 108.6(2) . . ?
C41 C38 C40 108.3(2) . . ?
C39 C38 C40 109.6(2) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 -1.7(2) . . . . ?
O3 V1 O1 C1 -107.4(2) . . . . ?
O2 V1 O1 C1 106.5(2) . . . . ?
O1 V1 O1 C1 178.4(2) 3_665 . . . ?
N1 V1 O1 V1 179.85(9) . . . 3_665 ?
O3 V1 O1 V1 74.21(9) . . . 3_665 ?
O2 V1 O1 V1 -71.93(10) . . . 3_665 ?
O1 V1 O1 V1 0.0 3_665 . . 3_665 ?
N1 V1 O2 C12 -21.32(19) . . . . ?
O3 V1 O2 C12 79.26(18) . . . . ?
O1 V1 O2 C12 -131.78(17) . . . . ?
O1 V1 O2 C12 163.44(17) 3_665 . . . ?
N1 V1 O3 C28 20.84(19) . . . . ?
O2 V1 O3 C28 -80.31(18) . . . . ?
O1 V1 O3 C28 129.38(17) . . . . ?
O1 V1 O3 C28 -164.35(17) 3_665 . . . ?
V1 O1 C1 C3 -71.1(3) . . . . ?
V1 O1 C1 C3 107.1(2) 3_665 . . . ?
V1 O1 C1 C2 63.6(3) . . . . ?
V1 O1 C1 C2 -118.1(2) 3_665 . . . ?
C10 C5 C6 C7 0.7(4) . . . . ?
N1 C5 C6 C7 -179.0(2) . . . . ?
C5 C6 C7 C8 -1.0(4) . . . . ?
C6 C7 C8 C9 0.7(4) . . . . ?
C6 C7 C8 Cl1 -178.9(2) . . . . ?
C7 C8 C9 C10 -0.1(5) . . . . ?
Cl1 C8 C9 C10 179.5(2) . . . . ?
C8 C9 C10 C5 -0.2(5) . . . . ?
C6 C5 C10 C9 -0.1(4) . . . . ?
N1 C5 C10 C9 179.6(2) . . . . ?
V1 O2 C12 C17 -66.3(2) . . . . ?
V1 O2 C12 C13 115.5(2) . . . . ?
O2 C12 C13 C14 -175.7(2) . . . . ?
C17 C12 C13 C14 6.1(3) . . . . ?
O2 C12 C13 C18 6.1(3) . . . . ?
C17 C12 C13 C18 -172.1(2) . . . . ?
C12 C13 C14 C15 -1.7(4) . . . . ?
C18 C13 C14 C15 176.5(2) . . . . ?
C13 C14 C15 C16 -2.3(4) . . . . ?
C13 C14 C15 C22 176.9(2) . . . . ?
C14 C15 C16 C17 2.1(4) . . . . ?
C22 C15 C16 C17 -177.1(2) . . . . ?
O2 C12 C17 C16 175.4(2) . . . . ?
C13 C12 C17 C16 -6.3(3) . . . . ?
O2 C12 C17 C26 -4.8(3) . . . . ?
C13 C12 C17 C26 173.4(2) . . . . ?
C15 C16 C17 C12 2.1(4) . . . . ?
C15 C16 C17 C26 -177.6(2) . . . . ?
C14 C13 C18 C20 -110.8(2) . . . . ?
C12 C13 C18 C20 67.3(3) . . . . ?
C14 C13 C18 C21 8.1(3) . . . . ?
C12 C13 C18 C21 -173.7(2) . . . . ?
C14 C13 C18 C19 127.4(2) . . . . ?
C12 C13 C18 C19 -54.5(3) . . . . ?
C14 C15 C22 C24 57.8(3) . . . . ?
C16 C15 C22 C24 -123.0(3) . . . . ?
C14 C15 C22 C25 178.6(2) . . . . ?
C16 C15 C22 C25 -2.2(4) . . . . ?
C14 C15 C22 C23 -62.3(3) . . . . ?
C16 C15 C22 C23 116.9(3) . . . . ?
C12 C17 C26 C33 99.9(3) . . . . ?
C16 C17 C26 C33 -80.3(3) . . . . ?
C12 C17 C26 C27 -133.2(2) . . . . ?
C16 C17 C26 C27 46.6(3) . . . . ?
V1 O3 C28 C33 65.3(3) . . . . ?
V1 O3 C28 C29 -115.9(2) . . . . ?
O3 C28 C29 C30 172.5(2) . . . . ?
C33 C28 C29 C30 -8.7(3) . . . . ?
O3 C28 C29 C34 -11.4(4) . . . . ?
C33 C28 C29 C34 167.4(2) . . . . ?
C28 C29 C30 C31 2.8(4) . . . . ?
C34 C29 C30 C31 -173.4(2) . . . . ?
C29 C30 C31 C32 2.8(4) . . . . ?
C29 C30 C31 C38 -179.2(2) . . . . ?
C30 C31 C32 C33 -2.6(4) . . . . ?
C38 C31 C32 C33 179.5(2) . . . . ?
C31 C32 C33 C28 -3.2(4) . . . . ?
C31 C32 C33 C26 174.0(2) . . . . ?
O3 C28 C33 C32 -172.1(2) . . . . ?
C29 C28 C33 C32 9.1(4) . . . . ?
O3 C28 C33 C26 10.7(3) . . . . ?
C29 C28 C33 C26 -168.2(2) . . . . ?
C17 C26 C33 C32 77.0(3) . . . . ?
C27 C26 C33 C32 -50.5(3) . . . . ?
C17 C26 C33 C28 -105.8(3) . . . . ?
C27 C26 C33 C28 126.7(2) . . . . ?
C30 C29 C34 C37 -120.6(3) . . . . ?
C28 C29 C34 C37 63.4(3) . . . . ?
C30 C29 C34 C35 118.3(2) . . . . ?
C28 C29 C34 C35 -57.7(3) . . . . ?
C30 C29 C34 C36 -1.1(3) . . . . ?
C28 C29 C34 C36 -177.1(2) . . . . ?
C32 C31 C38 C41 -1.9(3) . . . . ?
C30 C31 C38 C41 -179.7(2) . . . . ?
C32 C31 C38 C39 -122.3(3) . . . . ?
C30 C31 C38 C39 60.0(3) . . . . ?
C32 C31 C38 C40 118.0(3) . . . . ?
C30 C31 C38 C40 -59.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.66
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.056

data_6
_database_code_depnum_ccdc_archive 'CCDC 718356'

_chemical_name_common            'Compound 6'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4CF3)(diphenolate)(mu-O-i-Pr]2'
_chemical_formula_moiety         'C80 H110 F6 N2 O6 V2'
_chemical_formula_sum            'C80 H110 F6 N2 O6 V2'
_chemical_formula_weight         1411.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   10.7533(8)
_cell_length_b                   18.7325(14)
_cell_length_c                   38.124(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.883(6)
_cell_angle_gamma                90.00
_cell_volume                     7675.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    4880
_cell_measurement_theta_min      3.1936
_cell_measurement_theta_max      33.8976

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_T_max  0.9408
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42244
_diffrn_reflns_av_R_equivalents  0.1339
_diffrn_reflns_av_sigmaI/netI    0.1737
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6733
_reflns_number_gt                2932
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
There is a short contact between H19B and H35B, which is not due to disorder.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0457P)^2^] where P=(Fo^2^+2Fc^2^)/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         6733
_refine_ls_number_parameters     565
_refine_ls_number_restraints     588
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1161
_refine_ls_wR_factor_gt          0.0968
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_restrained_S_all      0.848
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.49186(6) 0.48460(3) 0.042972(14) 0.02648(19) Uani 1 1 d . . .
N1 N 0.5360(3) 0.52104(15) 0.08078(6) 0.0305(7) Uani 1 1 d . . .
O1 O 0.5546(2) 0.55239(12) 0.01177(5) 0.0314(6) Uani 1 1 d . . .
O2 O 0.3263(2) 0.47866(12) 0.05117(5) 0.0279(6) Uani 1 1 d . . .
O3 O 0.5656(2) 0.39809(11) 0.05016(5) 0.0286(6) Uani 1 1 d . . .
C1 C 0.6214(5) 0.6175(2) 0.02189(10) 0.0526(13) Uani 1 1 d . A .
H1 H 0.6243 0.6164 0.0481 0.063 Uiso 1 1 calc R . .
C2 C 0.5526(5) 0.6839(2) 0.01297(11) 0.0705(15) Uani 1 1 d . . .
H2A H 0.5490 0.6903 -0.0126 0.106 Uiso 1 1 calc R A .
H2B H 0.5954 0.7248 0.0240 0.106 Uiso 1 1 calc R . .
H2C H 0.4679 0.6806 0.0216 0.106 Uiso 1 1 calc R . .
C3 C 0.7536(4) 0.6164(2) 0.01242(11) 0.0661(15) Uani 1 1 d . . .
H3A H 0.7922 0.5719 0.0208 0.099 Uiso 1 1 calc R A .
H3B H 0.7970 0.6571 0.0233 0.099 Uiso 1 1 calc R . .
H3C H 0.7592 0.6193 -0.0131 0.099 Uiso 1 1 calc R . .
C5 C 0.5824(5) 0.5439(3) 0.11388(12) 0.028(2) Uani 0.553(4) 1 d PGU A 1
C6 C 0.6912(4) 0.5838(3) 0.11701(10) 0.0322(18) Uani 0.553(4) 1 d PGU A 1
H6 H 0.7412 0.5905 0.0972 0.039 Uiso 0.553(4) 1 calc PR A 1
C7 C 0.7270(4) 0.6137(2) 0.14914(12) 0.040(2) Uani 0.553(4) 1 d PGU A 1
H7 H 0.8014 0.6410 0.1513 0.048 Uiso 0.553(4) 1 calc PR A 1
C8 C 0.6539(5) 0.6038(3) 0.17814(10) 0.041(2) Uani 0.553(4) 1 d PGU A 1
C9 C 0.5451(5) 0.5640(3) 0.17502(13) 0.049(3) Uani 0.553(4) 1 d PGU A 1
H9 H 0.4951 0.5572 0.1948 0.059 Uiso 0.553(4) 1 calc PR A 1
C10 C 0.5093(4) 0.5340(3) 0.14289(17) 0.049(3) Uani 0.553(4) 1 d PGU A 1
H10 H 0.4349 0.5068 0.1408 0.059 Uiso 0.553(4) 1 calc PR A 1
C11 C 0.6942(13) 0.6365(7) 0.2119(4) 0.060(3) Uani 0.553(4) 1 d PDU A 1
F7 F 0.8077(7) 0.6226(4) 0.2215(2) 0.078(2) Uani 0.553(4) 1 d PDU A 1
F8 F 0.6875(14) 0.7074(4) 0.2113(3) 0.130(5) Uani 0.553(4) 1 d PDU A 1
F9 F 0.6255(12) 0.6161(8) 0.2387(4) 0.111(5) Uani 0.553(4) 1 d PDU A 1
C5X C 0.5532(7) 0.5556(3) 0.11313(16) 0.030(3) Uani 0.447(4) 1 d PGU A 2
C6X C 0.5625(6) 0.6293(3) 0.11663(13) 0.037(2) Uani 0.447(4) 1 d PGU A 2
H6X H 0.5467 0.6593 0.0969 0.044 Uiso 0.447(4) 1 calc PR A 2
C7X C 0.5949(6) 0.6592(3) 0.14903(15) 0.042(3) Uani 0.447(4) 1 d PGU A 2
H7X H 0.6012 0.7096 0.1514 0.051 Uiso 0.447(4) 1 calc PR A 2
C8X C 0.6180(7) 0.6154(4) 0.17794(13) 0.045(3) Uani 0.447(4) 1 d PGU A 2
C9X C 0.6087(7) 0.5417(4) 0.17444(18) 0.057(3) Uani 0.447(4) 1 d PGU A 2
H9X H 0.6245 0.5117 0.1942 0.068 Uiso 0.447(4) 1 calc PR A 2
C10X C 0.5763(7) 0.5118(2) 0.1420(2) 0.048(3) Uani 0.447(4) 1 d PGU A 2
H10X H 0.5699 0.4615 0.1397 0.057 Uiso 0.447(4) 1 calc PR A 2
C11X C 0.6543(16) 0.6487(8) 0.2122(5) 0.061(4) Uani 0.447(4) 1 d PDU A 2
F7X F 0.7669(11) 0.6745(10) 0.2123(3) 0.134(6) Uani 0.447(4) 1 d PDU A 2
F8X F 0.5814(8) 0.7016(5) 0.2204(2) 0.071(3) Uani 0.447(4) 1 d PDU A 2
F9X F 0.6506(19) 0.6033(8) 0.2391(4) 0.112(6) Uani 0.447(4) 1 d PDU A 2
C12 C 0.2714(3) 0.47302(19) 0.08340(8) 0.0267(9) Uani 1 1 d . A .
C13 C 0.1971(3) 0.52898(19) 0.09628(9) 0.0323(9) Uani 1 1 d . . .
C14 C 0.1526(3) 0.5199(2) 0.12962(9) 0.0387(10) Uani 1 1 d . A .
H14 H 0.1052 0.5576 0.1391 0.046 Uiso 1 1 calc R . .
C15 C 0.1725(4) 0.4595(2) 0.15018(9) 0.0385(10) Uani 1 1 d . . .
C16 C 0.2402(3) 0.40513(19) 0.13552(9) 0.0339(10) Uani 1 1 d . A .
H16 H 0.2539 0.3626 0.1487 0.041 Uiso 1 1 calc R . .
C17 C 0.2892(3) 0.41012(19) 0.10230(9) 0.0273(9) Uani 1 1 d . . .
C18 C 0.1663(4) 0.5959(2) 0.07479(13) 0.0592(14) Uani 1 1 d . A .
C19 C 0.2815(5) 0.6416(2) 0.07059(17) 0.131(3) Uani 1 1 d . . .
H19A H 0.3129 0.6574 0.0937 0.196 Uiso 1 1 calc R A .
H19B H 0.2603 0.6833 0.0561 0.196 Uiso 1 1 calc R . .
H19C H 0.3457 0.6135 0.0592 0.196 Uiso 1 1 calc R . .
C20 C 0.1149(5) 0.5748(3) 0.03816(12) 0.106(2) Uani 1 1 d . . .
H20A H 0.0779 0.6167 0.0265 0.160 Uiso 1 1 calc R A .
H20B H 0.0514 0.5377 0.0404 0.160 Uiso 1 1 calc R . .
H20C H 0.1828 0.5565 0.0242 0.160 Uiso 1 1 calc R . .
C21 C 0.0667(4) 0.6419(2) 0.09186(12) 0.0787(17) Uani 1 1 d . . .
H21A H 0.0949 0.6548 0.1157 0.118 Uiso 1 1 calc R A .
H21B H -0.0112 0.6149 0.0927 0.118 Uiso 1 1 calc R . .
H21C H 0.0529 0.6854 0.0780 0.118 Uiso 1 1 calc R . .
C22 C 0.1224(5) 0.4539(2) 0.18757(10) 0.0566(12) Uani 0.353(13) 1 d PDU A 1
C23 C 0.074(2) 0.3846(9) 0.1998(8) 0.089(8) Uani 0.353(13) 1 d PDU A 1
H23A H 0.0401 0.3904 0.2231 0.134 Uiso 0.353(13) 1 calc PR A 1
H23B H 0.1417 0.3496 0.2009 0.134 Uiso 0.353(13) 1 calc PR A 1
H23C H 0.0083 0.3679 0.1834 0.134 Uiso 0.353(13) 1 calc PR A 1
C24 C 0.2502(15) 0.4651(13) 0.2109(5) 0.090(3) Uani 0.353(13) 1 d PDU A 1
H24A H 0.2310 0.4661 0.2359 0.135 Uiso 0.353(13) 1 calc PR A 1
H24B H 0.2891 0.5103 0.2045 0.135 Uiso 0.353(13) 1 calc PR A 1
H24C H 0.3074 0.4256 0.2066 0.135 Uiso 0.353(13) 1 calc PR A 1
C25 C 0.052(3) 0.5213(11) 0.1985(5) 0.125(8) Uani 0.353(13) 1 d PDU A 1
H25A H -0.0122 0.5328 0.1806 0.188 Uiso 0.353(13) 1 calc PR A 1
H25B H 0.1106 0.5612 0.2009 0.188 Uiso 0.353(13) 1 calc PR A 1
H25C H 0.0131 0.5128 0.2210 0.188 Uiso 0.353(13) 1 calc PR A 1
C22X C 0.1224(5) 0.4539(2) 0.18757(10) 0.0566(12) Uani 0.647(13) 1 d PDU A 2
C23X C 0.1206(11) 0.3764(4) 0.1991(4) 0.052(3) Uani 0.647(13) 1 d PDU A 2
H23D H 0.2062 0.3591 0.2025 0.079 Uiso 0.647(13) 1 calc PR A 2
H23E H 0.0774 0.3476 0.1810 0.079 Uiso 0.647(13) 1 calc PR A 2
H23F H 0.0771 0.3723 0.2212 0.079 Uiso 0.647(13) 1 calc PR A 2
C24X C 0.1964(13) 0.4998(6) 0.2125(2) 0.090(3) Uani 0.647(13) 1 d PDU A 2
H24D H 0.1628 0.4958 0.2360 0.135 Uiso 0.647(13) 1 calc PR A 2
H24E H 0.1917 0.5496 0.2047 0.135 Uiso 0.647(13) 1 calc PR A 2
H24F H 0.2834 0.4841 0.2132 0.135 Uiso 0.647(13) 1 calc PR A 2
C25X C -0.0185(7) 0.4783(6) 0.1866(2) 0.064(3) Uani 0.647(13) 1 d PDU A 2
H25D H -0.0533 0.4712 0.2098 0.095 Uiso 0.647(13) 1 calc PR A 2
H25E H -0.0657 0.4498 0.1692 0.095 Uiso 0.647(13) 1 calc PR A 2
H25F H -0.0239 0.5289 0.1802 0.095 Uiso 0.647(13) 1 calc PR A 2
C26 C 0.3601(3) 0.34701(17) 0.08717(8) 0.0260(9) Uani 1 1 d . A .
H26 H 0.3655 0.3559 0.0614 0.031 Uiso 1 1 calc R . .
C27 C 0.2906(3) 0.27638(18) 0.09117(9) 0.0365(10) Uani 1 1 d . . .
H27A H 0.3355 0.2383 0.0793 0.055 Uiso 1 1 calc R A .
H27B H 0.2066 0.2808 0.0806 0.055 Uiso 1 1 calc R . .
H27C H 0.2850 0.2648 0.1161 0.055 Uiso 1 1 calc R . .
C28 C 0.5935(4) 0.36660(17) 0.08222(8) 0.0250(9) Uani 1 1 d . A .
C29 C 0.7168(3) 0.35640(18) 0.09480(9) 0.0305(9) Uani 1 1 d . . .
C30 C 0.7329(4) 0.32855(19) 0.12837(9) 0.0366(10) Uani 1 1 d . A .
H30 H 0.8156 0.3238 0.1376 0.044 Uiso 1 1 calc R . .
C31 C 0.6371(4) 0.3072(2) 0.14933(9) 0.0381(10) Uani 1 1 d . . .
C32 C 0.5165(4) 0.31478(18) 0.13510(9) 0.0337(10) Uani 1 1 d . A .
H32 H 0.4484 0.3001 0.1486 0.040 Uiso 1 1 calc R . .
C33 C 0.4926(3) 0.34299(17) 0.10186(9) 0.0257(9) Uani 1 1 d . . .
C34 C 0.8278(4) 0.3734(2) 0.07173(12) 0.0553(13) Uani 1 1 d . A .
C35 C 0.8107(5) 0.3355(3) 0.03613(11) 0.0925(19) Uani 1 1 d . . .
H35A H 0.7415 0.3575 0.0227 0.139 Uiso 1 1 calc R A .
H35B H 0.7925 0.2849 0.0400 0.139 Uiso 1 1 calc R . .
H35C H 0.8872 0.3399 0.0230 0.139 Uiso 1 1 calc R . .
C36 C 0.8393(4) 0.4531(3) 0.06653(14) 0.098(2) Uani 1 1 d . . .
H36A H 0.8483 0.4766 0.0894 0.147 Uiso 1 1 calc R A .
H36B H 0.7646 0.4710 0.0541 0.147 Uiso 1 1 calc R . .
H36C H 0.9125 0.4632 0.0527 0.147 Uiso 1 1 calc R . .
C37 C 0.9505(4) 0.3466(3) 0.08879(12) 0.0797(16) Uani 1 1 d . . .
H37A H 1.0187 0.3554 0.0729 0.120 Uiso 1 1 calc R A .
H37B H 0.9441 0.2952 0.0934 0.120 Uiso 1 1 calc R . .
H37C H 0.9668 0.3720 0.1109 0.120 Uiso 1 1 calc R . .
C38 C 0.6629(4) 0.2793(3) 0.18652(10) 0.0597(13) Uani 0.604(11) 1 d PDU A 1
C39 C 0.5507(13) 0.2380(7) 0.2003(5) 0.064(4) Uani 0.604(11) 1 d PDU A 1
H39A H 0.5760 0.2120 0.2216 0.096 Uiso 0.604(11) 1 calc PR A 1
H39B H 0.5207 0.2040 0.1824 0.096 Uiso 0.604(11) 1 calc PR A 1
H39C H 0.4841 0.2716 0.2055 0.096 Uiso 0.604(11) 1 calc PR A 1
C40 C 0.7089(15) 0.3335(6) 0.2108(3) 0.094(3) Uani 0.604(11) 1 d PDU A 1
H40A H 0.7829 0.3561 0.2013 0.142 Uiso 0.604(11) 1 calc PR A 1
H40B H 0.7306 0.3114 0.2335 0.142 Uiso 0.604(11) 1 calc PR A 1
H40C H 0.6443 0.3696 0.2139 0.142 Uiso 0.604(11) 1 calc PR A 1
C41 C 0.7700(8) 0.2187(6) 0.1838(2) 0.066(3) Uani 0.604(11) 1 d PDU A 1
H41A H 0.8470 0.2407 0.1760 0.100 Uiso 0.604(11) 1 calc PR A 1
H41B H 0.7426 0.1821 0.1669 0.100 Uiso 0.604(11) 1 calc PR A 1
H41C H 0.7850 0.1966 0.2069 0.100 Uiso 0.604(11) 1 calc PR A 1
C38X C 0.6629(4) 0.2793(3) 0.18652(10) 0.0597(13) Uani 0.396(11) 1 d PDU A 2
C39X C 0.5774(19) 0.2184(10) 0.1954(7) 0.061(5) Uani 0.396(11) 1 d PDU A 2
H39D H 0.4908 0.2329 0.1909 0.092 Uiso 0.396(11) 1 calc PR A 2
H39E H 0.5898 0.2059 0.2203 0.092 Uiso 0.396(11) 1 calc PR A 2
H39F H 0.5963 0.1769 0.1809 0.092 Uiso 0.396(11) 1 calc PR A 2
C40X C 0.623(2) 0.3440(8) 0.2111(5) 0.094(3) Uani 0.396(11) 1 d PDU A 2
H40D H 0.5325 0.3482 0.2106 0.142 Uiso 0.396(11) 1 calc PR A 2
H40E H 0.6598 0.3884 0.2027 0.142 Uiso 0.396(11) 1 calc PR A 2
H40F H 0.6537 0.3349 0.2353 0.142 Uiso 0.396(11) 1 calc PR A 2
C41X C 0.7996(11) 0.2731(15) 0.1974(4) 0.109(6) Uani 0.396(11) 1 d PDU A 2
H41D H 0.8079 0.2462 0.2194 0.164 Uiso 0.396(11) 1 calc PR A 2
H41E H 0.8348 0.3210 0.2009 0.164 Uiso 0.396(11) 1 calc PR A 2
H41F H 0.8443 0.2483 0.1791 0.164 Uiso 0.396(11) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0235(4) 0.0293(4) 0.0266(3) -0.0011(3) -0.0002(3) 0.0022(3)
N1 0.0300(19) 0.0383(18) 0.0235(15) 0.0005(15) 0.0041(14) -0.0068(16)
O1 0.0339(17) 0.0314(15) 0.0286(13) -0.0032(12) -0.0021(12) -0.0072(13)
O2 0.0232(14) 0.0308(14) 0.0298(13) 0.0008(12) 0.0021(11) 0.0028(12)
O3 0.0308(16) 0.0316(15) 0.0234(13) 0.0040(11) 0.0026(12) 0.0060(12)
C1 0.080(4) 0.036(3) 0.041(3) -0.005(2) -0.004(2) -0.030(3)
C2 0.094(4) 0.031(3) 0.088(4) -0.019(3) 0.028(3) -0.019(3)
C3 0.062(4) 0.059(3) 0.076(3) 0.023(3) -0.031(3) -0.039(3)
C5 0.029(5) 0.033(5) 0.022(5) 0.004(4) 0.006(4) 0.003(4)
C6 0.030(4) 0.041(4) 0.026(4) -0.003(3) 0.001(3) -0.005(3)
C7 0.051(5) 0.032(4) 0.036(4) -0.002(3) -0.005(3) -0.013(4)
C8 0.059(6) 0.036(6) 0.027(4) -0.008(4) -0.004(4) -0.008(4)
C9 0.051(6) 0.079(7) 0.017(4) -0.008(4) 0.011(4) -0.016(5)
C10 0.044(6) 0.071(7) 0.033(4) -0.005(4) 0.010(4) -0.025(5)
C11 0.080(8) 0.056(6) 0.043(6) -0.020(7) -0.006(6) -0.014(7)
F7 0.074(5) 0.103(6) 0.054(4) -0.025(4) -0.023(3) -0.007(4)
F8 0.230(14) 0.058(4) 0.096(8) -0.039(4) -0.090(10) 0.028(8)
F9 0.092(6) 0.196(12) 0.046(7) -0.047(7) 0.015(5) -0.032(7)
C5X 0.027(6) 0.036(5) 0.028(6) -0.003(5) -0.006(5) -0.003(5)
C6X 0.057(7) 0.031(4) 0.023(4) 0.002(4) -0.004(4) -0.004(5)
C7X 0.054(7) 0.033(5) 0.040(5) -0.011(4) 0.001(5) -0.017(5)
C8X 0.063(7) 0.046(6) 0.026(5) -0.008(4) -0.008(5) -0.013(6)
C9X 0.082(9) 0.049(5) 0.037(5) 0.006(4) -0.017(6) 0.004(7)
C10X 0.067(8) 0.033(5) 0.043(6) 0.003(4) -0.019(6) -0.008(6)
C11X 0.073(9) 0.072(10) 0.036(7) -0.011(6) -0.014(9) -0.014(7)
F7X 0.072(8) 0.23(2) 0.098(12) -0.105(13) 0.000(8) -0.050(9)
F8X 0.089(6) 0.071(5) 0.051(4) -0.028(3) -0.011(5) -0.002(5)
F9X 0.227(16) 0.065(6) 0.038(7) -0.003(5) -0.063(8) 0.014(7)
C12 0.019(2) 0.034(2) 0.027(2) -0.0004(19) 0.0034(17) -0.0063(19)
C13 0.027(2) 0.032(2) 0.038(2) 0.000(2) 0.0090(19) 0.007(2)
C14 0.036(3) 0.030(2) 0.051(3) -0.003(2) 0.012(2) 0.005(2)
C15 0.040(3) 0.041(3) 0.034(2) -0.004(2) 0.004(2) 0.003(2)
C16 0.037(3) 0.034(2) 0.030(2) 0.0033(19) 0.0002(19) 0.007(2)
C17 0.025(2) 0.029(2) 0.028(2) -0.0033(19) -0.0030(18) -0.0006(19)
C18 0.046(3) 0.035(3) 0.098(4) 0.028(3) 0.040(3) 0.020(2)
C19 0.099(5) 0.038(3) 0.262(8) 0.031(4) 0.111(5) 0.012(3)
C20 0.105(5) 0.141(5) 0.076(4) 0.077(4) 0.035(4) 0.068(4)
C21 0.067(4) 0.054(3) 0.118(4) 0.034(3) 0.050(3) 0.032(3)
C22 0.073(4) 0.058(3) 0.040(3) -0.001(2) 0.017(2) 0.016(3)
C23 0.066(16) 0.096(9) 0.110(16) -0.011(11) 0.074(14) -0.008(10)
C24 0.136(8) 0.096(9) 0.039(3) -0.035(6) 0.026(5) -0.028(6)
C25 0.214(18) 0.107(12) 0.059(11) -0.002(11) 0.067(13) 0.082(15)
C22X 0.073(4) 0.058(3) 0.040(3) -0.001(2) 0.017(2) 0.016(3)
C23X 0.047(7) 0.075(5) 0.037(5) 0.008(4) 0.033(5) 0.007(4)
C24X 0.136(8) 0.096(9) 0.039(3) -0.035(6) 0.026(5) -0.028(6)
C25X 0.082(5) 0.058(6) 0.054(6) 0.011(4) 0.045(4) 0.029(5)
C26 0.023(2) 0.027(2) 0.028(2) 0.0001(17) -0.0032(17) 0.0053(19)
C27 0.023(2) 0.033(2) 0.053(2) 0.001(2) 0.000(2) -0.001(2)
C28 0.030(3) 0.024(2) 0.021(2) -0.0005(17) -0.0018(19) 0.0027(19)
C29 0.027(3) 0.033(2) 0.032(2) 0.0036(18) -0.001(2) 0.001(2)
C30 0.023(3) 0.046(3) 0.040(2) 0.008(2) -0.008(2) -0.002(2)
C31 0.034(3) 0.044(3) 0.036(2) 0.005(2) -0.005(2) -0.003(2)
C32 0.031(3) 0.040(2) 0.030(2) 0.0086(19) 0.0023(19) -0.002(2)
C33 0.030(2) 0.021(2) 0.026(2) -0.0046(17) -0.0014(19) -0.0002(19)
C34 0.023(3) 0.071(3) 0.072(3) 0.034(3) 0.009(2) 0.010(2)
C35 0.080(4) 0.146(5) 0.054(3) 0.035(3) 0.032(3) 0.050(4)
C36 0.040(3) 0.082(4) 0.173(5) 0.077(4) 0.004(3) -0.006(3)
C37 0.024(3) 0.120(4) 0.096(4) 0.055(3) 0.009(3) 0.015(3)
C38 0.041(3) 0.103(4) 0.034(3) 0.022(2) -0.007(2) 0.002(3)
C39 0.066(6) 0.078(7) 0.048(7) 0.017(6) 0.002(5) 0.004(5)
C40 0.110(10) 0.137(6) 0.034(3) -0.004(4) -0.037(8) -0.031(7)
C41 0.045(5) 0.101(6) 0.052(5) 0.045(4) -0.018(4) 0.004(4)
C38X 0.041(3) 0.103(4) 0.034(3) 0.022(2) -0.007(2) 0.002(3)
C39X 0.073(12) 0.088(10) 0.023(10) 0.036(9) -0.002(8) 0.009(10)
C40X 0.110(10) 0.137(6) 0.034(3) -0.004(4) -0.037(8) -0.031(7)
C41X 0.059(7) 0.198(19) 0.069(11) 0.050(12) -0.023(8) -0.014(9)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.651(3) . ?
V1 O3 1.821(2) . ?
V1 O2 1.821(2) . ?
V1 O1 1.880(2) . ?
V1 O1 2.240(2) 5_665 ?
N1 C5X 1.400(6) . ?
N1 C5 1.408(5) . ?
O1 C1 1.462(4) . ?
O1 V1 2.240(2) 5_665 ?
O2 C12 1.385(3) . ?
O3 C28 1.381(4) . ?
C1 C3 1.478(6) . ?
C1 C2 1.481(5) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 C9 1.3900 . ?
C8 C11 1.477(16) . ?
C9 C10 1.3900 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 F7 1.289(14) . ?
C11 F8 1.330(13) . ?
C11 F9 1.335(12) . ?
C5X C6X 1.3900 . ?
C5X C10X 1.3900 . ?
C6X C7X 1.3900 . ?
C6X H6X 0.9500 . ?
C7X C8X 1.3900 . ?
C7X H7X 0.9500 . ?
C8X C9X 1.3900 . ?
C8X C11X 1.49(2) . ?
C9X C10X 1.3900 . ?
C9X H9X 0.9500 . ?
C10X H10X 0.9500 . ?
C11X F7X 1.304(15) . ?
C11X F8X 1.307(16) . ?
C11X F9X 1.333(14) . ?
C12 C17 1.391(4) . ?
C12 C13 1.416(4) . ?
C13 C14 1.383(4) . ?
C13 C18 1.528(5) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(4) . ?
C15 C22 1.544(5) . ?
C16 C17 1.391(4) . ?
C16 H16 0.9500 . ?
C17 C26 1.530(4) . ?
C18 C19 1.518(6) . ?
C18 C21 1.536(5) . ?
C18 C20 1.536(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.480(14) . ?
C22 C25 1.535(12) . ?
C22 C24 1.627(14) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C23X H23D 0.9800 . ?
C23X H23E 0.9800 . ?
C23X H23F 0.9800 . ?
C24X H24D 0.9800 . ?
C24X H24E 0.9800 . ?
C24X H24F 0.9800 . ?
C25X H25D 0.9800 . ?
C25X H25E 0.9800 . ?
C25X H25F 0.9800 . ?
C26 C33 1.516(5) . ?
C26 C27 1.530(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.408(5) . ?
C28 C33 1.409(4) . ?
C29 C30 1.388(4) . ?
C29 C34 1.540(5) . ?
C30 C31 1.383(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.396(5) . ?
C31 C38 1.528(5) . ?
C32 C33 1.389(4) . ?
C32 H32 0.9500 . ?
C34 C36 1.511(6) . ?
C34 C37 1.536(5) . ?
C34 C35 1.538(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.449(8) . ?
C38 C39 1.540(10) . ?
C38 C41 1.623(8) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C39X H39D 0.9800 . ?
C39X H39E 0.9800 . ?
C39X H39F 0.9800 . ?
C40X H40D 0.9800 . ?
C40X H40E 0.9800 . ?
C40X H40F 0.9800 . ?
C41X H41D 0.9800 . ?
C41X H41E 0.9800 . ?
C41X H41F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O3 97.19(12) . . ?
N1 V1 O2 97.49(11) . . ?
O3 V1 O2 110.06(10) . . ?
N1 V1 O1 100.04(12) . . ?
O3 V1 O1 122.21(10) . . ?
O2 V1 O1 121.51(10) . . ?
N1 V1 O1 172.14(11) . 5_665 ?
O3 V1 O1 87.00(9) . 5_665 ?
O2 V1 O1 87.24(9) . 5_665 ?
O1 V1 O1 72.12(10) . 5_665 ?
C5X N1 V1 170.6(4) . . ?
C5 N1 V1 172.6(3) . . ?
C1 O1 V1 125.5(2) . . ?
C1 O1 V1 126.63(19) . 5_665 ?
V1 O1 V1 107.88(10) . 5_665 ?
C12 O2 V1 127.20(19) . . ?
C28 O3 V1 126.45(18) . . ?
O1 C1 C3 113.1(4) . . ?
O1 C1 C2 113.7(4) . . ?
C3 C1 C2 115.7(4) . . ?
O1 C1 H1 104.2 . . ?
C3 C1 H1 104.2 . . ?
C2 C1 H1 104.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C6 C5 C10 120.0 . . ?
C6 C5 N1 120.8(4) . . ?
C10 C5 N1 118.7(4) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 C11 118.7(6) . . ?
C9 C8 C11 121.3(6) . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C5 120.0 . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
F7 C11 F8 104.9(11) . . ?
F7 C11 F9 105.5(13) . . ?
F8 C11 F9 105.5(14) . . ?
F7 C11 C8 114.3(11) . . ?
F8 C11 C8 112.6(12) . . ?
F9 C11 C8 113.1(11) . . ?
C6X C5X C10X 120.0 . . ?
C6X C5X N1 123.4(5) . . ?
C10X C5X N1 116.1(5) . . ?
C5X C6X C7X 120.0 . . ?
C5X C6X H6X 120.0 . . ?
C7X C6X H6X 120.0 . . ?
C8X C7X C6X 120.0 . . ?
C8X C7X H7X 120.0 . . ?
C6X C7X H7X 120.0 . . ?
C7X C8X C9X 120.0 . . ?
C7X C8X C11X 118.9(7) . . ?
C9X C8X C11X 121.1(7) . . ?
C10X C9X C8X 120.0 . . ?
C10X C9X H9X 120.0 . . ?
C8X C9X H9X 120.0 . . ?
C9X C10X C5X 120.0 . . ?
C9X C10X H10X 120.0 . . ?
C5X C10X H10X 120.0 . . ?
F7X C11X F8X 106.4(13) . . ?
F7X C11X F9X 106.6(16) . . ?
F8X C11X F9X 105.6(14) . . ?
F7X C11X C8X 112.0(15) . . ?
F8X C11X C8X 112.5(12) . . ?
F9X C11X C8X 113.2(14) . . ?
O2 C12 C17 118.0(3) . . ?
O2 C12 C13 120.9(3) . . ?
C17 C12 C13 121.1(3) . . ?
C14 C13 C12 116.3(3) . . ?
C14 C13 C18 121.2(3) . . ?
C12 C13 C18 122.4(3) . . ?
C13 C14 C15 124.6(3) . . ?
C13 C14 H14 117.7 . . ?
C15 C14 H14 117.7 . . ?
C16 C15 C14 116.5(3) . . ?
C16 C15 C22 121.9(3) . . ?
C14 C15 C22 121.7(3) . . ?
C15 C16 C17 122.6(3) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C12 118.6(3) . . ?
C16 C17 C26 120.0(3) . . ?
C12 C17 C26 121.4(3) . . ?
C19 C18 C13 110.8(4) . . ?
C19 C18 C21 108.1(4) . . ?
C13 C18 C21 112.0(3) . . ?
C19 C18 C20 108.6(4) . . ?
C13 C18 C20 109.9(4) . . ?
C21 C18 C20 107.2(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C25 117.0(12) . . ?
C23 C22 C15 119.1(12) . . ?
C25 C22 C15 112.6(7) . . ?
C23 C22 C24 103.9(13) . . ?
C25 C22 C24 99.2(11) . . ?
C15 C22 C24 100.5(8) . . ?
H23D C23X H23E 109.5 . . ?
H23D C23X H23F 109.5 . . ?
H23E C23X H23F 109.5 . . ?
H24D C24X H24E 109.5 . . ?
H24D C24X H24F 109.5 . . ?
H24E C24X H24F 109.5 . . ?
H25D C25X H25E 109.5 . . ?
H25D C25X H25F 109.5 . . ?
H25E C25X H25F 109.5 . . ?
C33 C26 C17 111.9(3) . . ?
C33 C26 C27 112.1(3) . . ?
C17 C26 C27 112.3(3) . . ?
C33 C26 H26 106.7 . . ?
C17 C26 H26 106.7 . . ?
C27 C26 H26 106.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C29 122.3(3) . . ?
O3 C28 C33 117.1(3) . . ?
C29 C28 C33 120.6(3) . . ?
C30 C29 C28 116.9(3) . . ?
C30 C29 C34 121.9(3) . . ?
C28 C29 C34 121.1(3) . . ?
C31 C30 C29 124.6(4) . . ?
C31 C30 H30 117.7 . . ?
C29 C30 H30 117.7 . . ?
C30 C31 C32 116.5(3) . . ?
C30 C31 C38 121.2(4) . . ?
C32 C31 C38 122.2(4) . . ?
C33 C32 C31 122.3(4) . . ?
C33 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C32 C33 C28 118.8(3) . . ?
C32 C33 C26 120.0(3) . . ?
C28 C33 C26 121.2(3) . . ?
C36 C34 C37 107.8(4) . . ?
C36 C34 C35 110.4(4) . . ?
C37 C34 C35 107.4(4) . . ?
C36 C34 C29 110.3(4) . . ?
C37 C34 C29 111.2(3) . . ?
C35 C34 C29 109.6(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C31 113.6(6) . . ?
C40 C38 C39 112.9(8) . . ?
C31 C38 C39 111.5(9) . . ?
C40 C38 C41 107.7(6) . . ?
C31 C38 C41 106.7(4) . . ?
C39 C38 C41 103.6(7) . . ?
H39D C39X H39E 109.5 . . ?
H39D C39X H39F 109.5 . . ?
H39E C39X H39F 109.5 . . ?
H40D C40X H40E 109.5 . . ?
H40D C40X H40F 109.5 . . ?
H40E C40X H40F 109.5 . . ?
H41D C41X H41E 109.5 . . ?
H41D C41X H41F 109.5 . . ?
H41E C41X H41F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 -0.5(3) . . . . ?
O3 V1 O1 C1 -105.6(3) . . . . ?
O2 V1 O1 C1 104.8(3) . . . . ?
O1 V1 O1 C1 179.9(3) 5_665 . . . ?
N1 V1 O1 V1 179.61(13) . . . 5_665 ?
O3 V1 O1 V1 74.43(14) . . . 5_665 ?
O2 V1 O1 V1 -75.10(13) . . . 5_665 ?
O1 V1 O1 V1 0.0 5_665 . . 5_665 ?
N1 V1 O2 C12 -27.0(3) . . . . ?
O3 V1 O2 C12 73.5(3) . . . . ?
O1 V1 O2 C12 -133.7(2) . . . . ?
O1 V1 O2 C12 159.3(3) 5_665 . . . ?
N1 V1 O3 C28 25.8(3) . . . . ?
O2 V1 O3 C28 -74.9(3) . . . . ?
O1 V1 O3 C28 132.5(2) . . . . ?
O1 V1 O3 C28 -160.9(3) 5_665 . . . ?
V1 O1 C1 C3 112.3(3) . . . . ?
V1 O1 C1 C3 -67.8(4) 5_665 . . . ?
V1 O1 C1 C2 -113.0(3) . . . . ?
V1 O1 C1 C2 66.9(4) 5_665 . . . ?
C5X N1 C5 C6 -110.9(17) . . . . ?
C5X N1 C5 C10 60.8(15) . . . . ?
C10 C5 C6 C7 0.0 . . . . ?
N1 C5 C6 C7 171.6(5) . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C6 C7 C8 C11 -179.9(8) . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C11 C8 C9 C10 179.9(8) . . . . ?
C8 C9 C10 C5 0.0 . . . . ?
C6 C5 C10 C9 0.0 . . . . ?
N1 C5 C10 C9 -171.8(5) . . . . ?
C7 C8 C11 F7 -51.3(13) . . . . ?
C9 C8 C11 F7 128.8(9) . . . . ?
C7 C8 C11 F8 68.3(14) . . . . ?
C9 C8 C11 F8 -111.6(11) . . . . ?
C7 C8 C11 F9 -172.1(10) . . . . ?
C9 C8 C11 F9 8.0(15) . . . . ?
C5 N1 C5X C6X 122.2(17) . . . . ?
C10X C5X C6X C7X 0.0 . . . . ?
N1 C5X C6X C7X -172.0(6) . . . . ?
C5X C6X C7X C8X 0.0 . . . . ?
C6X C7X C8X C9X 0.0 . . . . ?
C6X C7X C8X C11X 179.1(10) . . . . ?
C7X C8X C9X C10X 0.0 . . . . ?
C11X C8X C9X C10X -179.1(10) . . . . ?
C8X C9X C10X C5X 0.0 . . . . ?
C6X C5X C10X C9X 0.0 . . . . ?
N1 C5X C10X C9X 172.5(6) . . . . ?
C7X C8X C11X F7X -71.5(16) . . . . ?
C9X C8X C11X F7X 107.6(13) . . . . ?
C7X C8X C11X F8X 48.3(15) . . . . ?
C9X C8X C11X F8X -132.6(10) . . . . ?
C7X C8X C11X F9X 167.8(12) . . . . ?
C9X C8X C11X F9X -13.1(18) . . . . ?
V1 O2 C12 C17 -68.2(4) . . . . ?
V1 O2 C12 C13 113.3(3) . . . . ?
O2 C12 C13 C14 -176.3(3) . . . . ?
C17 C12 C13 C14 5.2(5) . . . . ?
O2 C12 C13 C18 4.0(5) . . . . ?
C17 C12 C13 C18 -174.5(4) . . . . ?
C12 C13 C14 C15 -2.3(5) . . . . ?
C18 C13 C14 C15 177.4(4) . . . . ?
C13 C14 C15 C16 -0.9(6) . . . . ?
C13 C14 C15 C22 178.6(4) . . . . ?
C14 C15 C16 C17 1.5(5) . . . . ?
C22 C15 C16 C17 -178.1(4) . . . . ?
C15 C16 C17 C12 1.4(5) . . . . ?
C15 C16 C17 C26 -178.2(3) . . . . ?
O2 C12 C17 C16 176.6(3) . . . . ?
C13 C12 C17 C16 -4.9(5) . . . . ?
O2 C12 C17 C26 -3.8(5) . . . . ?
C13 C12 C17 C26 174.7(3) . . . . ?
C14 C13 C18 C19 111.3(4) . . . . ?
C12 C13 C18 C19 -69.0(5) . . . . ?
C14 C13 C18 C21 -9.6(6) . . . . ?
C12 C13 C18 C21 170.1(4) . . . . ?
C14 C13 C18 C20 -128.7(4) . . . . ?
C12 C13 C18 C20 51.1(5) . . . . ?
C16 C15 C22 C23 -38.3(14) . . . . ?
C14 C15 C22 C23 142.2(13) . . . . ?
C16 C15 C22 C25 178.9(16) . . . . ?
C14 C15 C22 C25 -0.6(17) . . . . ?
C16 C15 C22 C24 74.2(10) . . . . ?
C14 C15 C22 C24 -105.3(10) . . . . ?
C16 C17 C26 C33 -79.5(4) . . . . ?
C12 C17 C26 C33 101.0(4) . . . . ?
C16 C17 C26 C27 47.7(4) . . . . ?
C12 C17 C26 C27 -131.9(3) . . . . ?
V1 O3 C28 C29 -112.0(3) . . . . ?
V1 O3 C28 C33 69.5(4) . . . . ?
O3 C28 C29 C30 175.8(3) . . . . ?
C33 C28 C29 C30 -5.8(5) . . . . ?
O3 C28 C29 C34 -6.0(5) . . . . ?
C33 C28 C29 C34 172.4(3) . . . . ?
C28 C29 C30 C31 3.2(5) . . . . ?
C34 C29 C30 C31 -174.9(4) . . . . ?
C29 C30 C31 C32 0.0(6) . . . . ?
C29 C30 C31 C38 -178.0(4) . . . . ?
C30 C31 C32 C33 -0.8(5) . . . . ?
C38 C31 C32 C33 177.2(4) . . . . ?
C31 C32 C33 C28 -1.8(5) . . . . ?
C31 C32 C33 C26 177.4(3) . . . . ?
O3 C28 C33 C32 -176.4(3) . . . . ?
C29 C28 C33 C32 5.2(5) . . . . ?
O3 C28 C33 C26 4.5(4) . . . . ?
C29 C28 C33 C26 -174.0(3) . . . . ?
C17 C26 C33 C32 78.7(4) . . . . ?
C27 C26 C33 C32 -48.5(4) . . . . ?
C17 C26 C33 C28 -102.1(4) . . . . ?
C27 C26 C33 C28 130.7(3) . . . . ?
C30 C29 C34 C36 -112.2(4) . . . . ?
C28 C29 C34 C36 69.7(5) . . . . ?
C30 C29 C34 C37 7.4(6) . . . . ?
C28 C29 C34 C37 -170.7(4) . . . . ?
C30 C29 C34 C35 126.0(4) . . . . ?
C28 C29 C34 C35 -52.1(5) . . . . ?
C30 C31 C38 C40 68.6(9) . . . . ?
C32 C31 C38 C40 -109.3(8) . . . . ?
C30 C31 C38 C39 -162.4(7) . . . . ?
C32 C31 C38 C39 19.7(8) . . . . ?
C30 C31 C38 C41 -49.9(7) . . . . ?
C32 C31 C38 C41 132.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.051

data_7
_database_code_depnum_ccdc_archive 'CCDC 718357'

_chemical_name_common            'Compound 7'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4OMe)(diphenolate)(mu-O-i-Pr)]2'
_chemical_formula_moiety         'C80 H116 N2 O8 V2'
_chemical_formula_sum            'C80 H116 N2 O8 V2'
_chemical_formula_weight         1335.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   10.6184(3)
_cell_length_b                   10.6968(4)
_cell_length_c                   16.6833(7)
_cell_angle_alpha                91.325(3)
_cell_angle_beta                 95.727(3)
_cell_angle_gamma                91.217(3)
_cell_volume                     1884.45(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    5133
_cell_measurement_theta_min      3.2582
_cell_measurement_theta_max      33.9719

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6283
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25919
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.1673
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8611
_reflns_number_gt                3924
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkins <i>et al.</i>, 1999)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0337P)^2^] where P=(Fo^2^+2Fc^2^)/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         8611
_refine_ls_number_parameters     462
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_restrained_S_all      0.788
_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 0.00845(3) 0.43513(4) 0.58944(2) 0.02475(11) Uani 1 1 d . . .
N1 N -0.03537(14) 0.45541(15) 0.68133(10) 0.0251(4) Uani 1 1 d . . .
O1 O -0.05328(11) 0.57895(12) 0.53996(8) 0.0228(3) Uani 1 1 d . . .
O2 O -0.06978(11) 0.28103(12) 0.57000(8) 0.0244(3) Uani 1 1 d . . .
O3 O 0.17903(11) 0.42338(12) 0.61623(8) 0.0232(3) Uani 1 1 d . . .
O4 O -0.20076(14) 0.44628(17) 0.98634(10) 0.0547(5) Uani 1 1 d . . .
C1 C -0.1180(2) 0.6798(2) 0.57982(14) 0.0342(6) Uani 1 1 d . . .
H1 H -0.1149 0.6561 0.6376 0.041 Uiso 1 1 calc R . .
C2 C -0.25648(19) 0.6813(2) 0.55043(14) 0.0425(6) Uani 1 1 d . . .
H2A H -0.2667 0.7093 0.4947 0.064 Uiso 1 1 calc R . .
H2B H -0.2997 0.7386 0.5847 0.064 Uiso 1 1 calc R . .
H2C H -0.2934 0.5968 0.5528 0.064 Uiso 1 1 calc R . .
C3 C -0.0508(2) 0.8024(2) 0.58093(15) 0.0510(7) Uani 1 1 d . . .
H3A H 0.0383 0.7925 0.6007 0.076 Uiso 1 1 calc R . .
H3B H -0.0897 0.8611 0.6165 0.076 Uiso 1 1 calc R . .
H3C H -0.0566 0.8348 0.5263 0.076 Uiso 1 1 calc R . .
C5 C -0.07267(19) 0.4531(2) 0.75896(14) 0.0285(5) Uani 1 1 d . . .
C6 C -0.1796(2) 0.5191(2) 0.77833(14) 0.0362(6) Uani 1 1 d . . .
H6 H -0.2253 0.5671 0.7385 0.043 Uiso 1 1 calc R . .
C7 C -0.2179(2) 0.5142(2) 0.85427(14) 0.0399(6) Uani 1 1 d . . .
H7 H -0.2893 0.5601 0.8668 0.048 Uiso 1 1 calc R . .
C8 C -0.1543(2) 0.4437(2) 0.91260(14) 0.0363(6) Uani 1 1 d . . .
C9 C -0.0487(2) 0.3786(2) 0.89462(14) 0.0369(6) Uani 1 1 d . . .
H9 H -0.0040 0.3300 0.9345 0.044 Uiso 1 1 calc R . .
C10 C -0.00887(19) 0.3846(2) 0.81921(13) 0.0324(6) Uani 1 1 d . . .
H10 H 0.0644 0.3406 0.8078 0.039 Uiso 1 1 calc R . .
C11 C -0.1499(2) 0.3622(3) 1.04549(14) 0.0557(8) Uani 1 1 d . . .
H11A H -0.1623 0.2760 1.0244 0.084 Uiso 1 1 calc R . .
H11B H -0.1933 0.3722 1.0943 0.084 Uiso 1 1 calc R . .
H11C H -0.0593 0.3805 1.0584 0.084 Uiso 1 1 calc R . .
C12 C -0.09149(18) 0.20016(19) 0.63022(12) 0.0236(5) Uani 1 1 d . . .
C13 C -0.21548(17) 0.17047(19) 0.64892(12) 0.0252(5) Uani 1 1 d . . .
C14 C -0.22567(18) 0.09191(19) 0.71296(13) 0.0280(5) Uani 1 1 d . . .
H14 H -0.3080 0.0738 0.7278 0.034 Uiso 1 1 calc R . .
C15 C -0.12400(18) 0.03784(19) 0.75692(13) 0.0272(5) Uani 1 1 d . . .
C16 C -0.00524(18) 0.06579(19) 0.73377(13) 0.0286(5) Uani 1 1 d . . .
H16 H 0.0664 0.0294 0.7621 0.034 Uiso 1 1 calc R . .
C17 C 0.01364(17) 0.14409(19) 0.67136(13) 0.0244(5) Uani 1 1 d . . .
C18 C -0.33468(18) 0.2134(2) 0.59791(13) 0.0297(5) Uani 1 1 d . . .
C19 C -0.3370(2) 0.3547(2) 0.58795(15) 0.0434(7) Uani 1 1 d . . .
H19A H -0.2661 0.3813 0.5586 0.065 Uiso 1 1 calc R . .
H19B H -0.3296 0.3965 0.6412 0.065 Uiso 1 1 calc R . .
H19C H -0.4169 0.3771 0.5577 0.065 Uiso 1 1 calc R . .
C20 C -0.45642(19) 0.1755(3) 0.63398(16) 0.0656(9) Uani 1 1 d . . .
H20A H -0.5296 0.2058 0.6001 0.098 Uiso 1 1 calc R . .
H20B H -0.4551 0.2122 0.6884 0.098 Uiso 1 1 calc R . .
H20C H -0.4624 0.0841 0.6365 0.098 Uiso 1 1 calc R . .
C21 C -0.3371(2) 0.1492(2) 0.51530(14) 0.0485(7) Uani 1 1 d . . .
H21A H -0.4164 0.1678 0.4829 0.073 Uiso 1 1 calc R . .
H21B H -0.3314 0.0585 0.5217 0.073 Uiso 1 1 calc R . .
H21C H -0.2653 0.1798 0.4881 0.073 Uiso 1 1 calc R . .
C22 C -0.14240(19) -0.0488(2) 0.82735(14) 0.0352(6) Uani 1 1 d . . .
C23 C -0.2682(2) -0.1197(2) 0.81489(16) 0.0583(8) Uani 1 1 d . . .
H23A H -0.2749 -0.1651 0.7629 0.087 Uiso 1 1 calc R . .
H23B H -0.3374 -0.0606 0.8155 0.087 Uiso 1 1 calc R . .
H23C H -0.2736 -0.1792 0.8583 0.087 Uiso 1 1 calc R . .
C24 C -0.0396(2) -0.1455(3) 0.83706(19) 0.0838(12) Uani 1 1 d . . .
H24A H -0.0572 -0.2025 0.8800 0.126 Uiso 1 1 calc R . .
H24B H 0.0427 -0.1032 0.8511 0.126 Uiso 1 1 calc R . .
H24C H -0.0379 -0.1933 0.7863 0.126 Uiso 1 1 calc R . .
C25 C -0.1376(3) 0.0327(3) 0.90366(16) 0.0764(9) Uani 1 1 d . . .
H25A H -0.2029 0.0960 0.8970 0.115 Uiso 1 1 calc R . .
H25B H -0.0541 0.0740 0.9137 0.115 Uiso 1 1 calc R . .
H25C H -0.1528 -0.0196 0.9494 0.115 Uiso 1 1 calc R . .
C26 C 0.14670(17) 0.16704(19) 0.64675(13) 0.0252(5) Uani 1 1 d . . .
H26 H 0.1367 0.2085 0.5935 0.030 Uiso 1 1 calc R . .
C27 C 0.21262(19) 0.0432(2) 0.63364(14) 0.0392(6) Uani 1 1 d . . .
H27A H 0.2966 0.0602 0.6162 0.059 Uiso 1 1 calc R . .
H27B H 0.1619 -0.0077 0.5922 0.059 Uiso 1 1 calc R . .
H27C H 0.2215 -0.0021 0.6842 0.059 Uiso 1 1 calc R . .
C28 C 0.23873(17) 0.38323(19) 0.68738(12) 0.0217(5) Uani 1 1 d . . .
C29 C 0.31478(17) 0.46574(19) 0.74051(12) 0.0223(5) Uani 1 1 d . . .
C30 C 0.36727(18) 0.4167(2) 0.81216(13) 0.0287(5) Uani 1 1 d . . .
H30 H 0.4157 0.4715 0.8495 0.034 Uiso 1 1 calc R . .
C31 C 0.35350(18) 0.2919(2) 0.83298(13) 0.0278(5) Uani 1 1 d . A .
C32 C 0.28293(17) 0.2139(2) 0.77704(13) 0.0280(5) Uani 1 1 d . . .
H32 H 0.2740 0.1277 0.7885 0.034 Uiso 1 1 calc R . .
C33 C 0.22511(17) 0.2569(2) 0.70517(13) 0.0238(5) Uani 1 1 d . . .
C34 C 0.34263(18) 0.60130(19) 0.71892(12) 0.0270(5) Uani 1 1 d . . .
C35 C 0.2208(2) 0.6758(2) 0.70700(15) 0.0440(7) Uani 1 1 d . . .
H35A H 0.1756 0.6703 0.7552 0.066 Uiso 1 1 calc R . .
H35B H 0.1669 0.6412 0.6603 0.066 Uiso 1 1 calc R . .
H35C H 0.2421 0.7636 0.6978 0.066 Uiso 1 1 calc R . .
C36 C 0.4099(2) 0.6014(2) 0.64167(14) 0.0445(7) Uani 1 1 d . . .
H36A H 0.4274 0.6879 0.6271 0.067 Uiso 1 1 calc R . .
H36B H 0.3557 0.5592 0.5978 0.067 Uiso 1 1 calc R . .
H36C H 0.4898 0.5572 0.6508 0.067 Uiso 1 1 calc R . .
C37 C 0.4302(2) 0.6710(2) 0.78439(14) 0.0442(6) Uani 1 1 d . . .
H37A H 0.3904 0.6729 0.8349 0.066 Uiso 1 1 calc R . .
H37B H 0.4455 0.7568 0.7677 0.066 Uiso 1 1 calc R . .
H37C H 0.5109 0.6280 0.7925 0.066 Uiso 1 1 calc R . .
C38 C 0.4139(2) 0.2420(2) 0.91251(14) 0.0370(6) Uani 1 1 d U . .
C39 C 0.4709(5) 0.3499(5) 0.9727(3) 0.0524(17) Uani 0.575(6) 1 d PU A 1
H39A H 0.4047 0.4096 0.9819 0.079 Uiso 0.575(6) 1 calc PR A 1
H39B H 0.5404 0.3932 0.9494 0.079 Uiso 0.575(6) 1 calc PR A 1
H39C H 0.5029 0.3139 1.0240 0.079 Uiso 0.575(6) 1 calc PR A 1
C40 C 0.5188(6) 0.1586(7) 0.8963(3) 0.069(2) Uani 0.575(6) 1 d PU A 1
H40A H 0.5819 0.2054 0.8693 0.104 Uiso 0.575(6) 1 calc PR A 1
H40B H 0.4853 0.0879 0.8616 0.104 Uiso 0.575(6) 1 calc PR A 1
H40C H 0.5584 0.1273 0.9473 0.104 Uiso 0.575(6) 1 calc PR A 1
C41 C 0.3128(5) 0.1768(6) 0.9582(3) 0.066(2) Uani 0.575(6) 1 d PU A 1
H41A H 0.3533 0.1419 1.0078 0.098 Uiso 0.575(6) 1 calc PR A 1
H41B H 0.2707 0.1094 0.9241 0.098 Uiso 0.575(6) 1 calc PR A 1
H41C H 0.2501 0.2378 0.9716 0.098 Uiso 0.575(6) 1 calc PR A 1
C39X C 0.3962(8) 0.0974(6) 0.9159(4) 0.072(3) Uani 0.425(6) 1 d PU A 2
H39D H 0.4403 0.0676 0.9660 0.108 Uiso 0.425(6) 1 calc PR A 2
H39E H 0.4313 0.0578 0.8697 0.108 Uiso 0.425(6) 1 calc PR A 2
H39F H 0.3058 0.0757 0.9140 0.108 Uiso 0.425(6) 1 calc PR A 2
C40X C 0.3591(8) 0.3022(7) 0.9790(4) 0.069(3) Uani 0.425(6) 1 d PU A 2
H40D H 0.4046 0.2777 1.0300 0.103 Uiso 0.425(6) 1 calc PR A 2
H40E H 0.2697 0.2765 0.9777 0.103 Uiso 0.425(6) 1 calc PR A 2
H40F H 0.3657 0.3932 0.9742 0.103 Uiso 0.425(6) 1 calc PR A 2
C41X C 0.5579(6) 0.2702(10) 0.9177(5) 0.078(3) Uani 0.425(6) 1 d PU A 2
H41D H 0.5733 0.3609 0.9199 0.116 Uiso 0.425(6) 1 calc PR A 2
H41E H 0.5921 0.2340 0.8702 0.116 Uiso 0.425(6) 1 calc PR A 2
H41F H 0.5995 0.2335 0.9665 0.116 Uiso 0.425(6) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0207(2) 0.0258(2) 0.0275(2) 0.00128(17) 0.00150(16) -0.00316(16)
N1 0.0186(9) 0.0228(11) 0.0337(12) 0.0026(8) 0.0023(8) -0.0029(8)
O1 0.0224(8) 0.0194(8) 0.0265(9) -0.0013(7) 0.0031(6) -0.0003(6)
O2 0.0214(7) 0.0240(9) 0.0280(9) 0.0038(7) 0.0041(6) -0.0054(6)
O3 0.0201(7) 0.0234(8) 0.0256(9) 0.0027(7) 0.0004(6) -0.0033(6)
O4 0.0491(10) 0.0870(15) 0.0314(11) 0.0186(10) 0.0131(8) 0.0204(10)
C1 0.0366(14) 0.0271(14) 0.0404(15) -0.0020(11) 0.0120(11) 0.0011(11)
C2 0.0351(14) 0.0396(16) 0.0549(18) -0.0054(13) 0.0156(12) 0.0029(12)
C3 0.0435(15) 0.0420(17) 0.0648(19) -0.0148(14) -0.0040(13) 0.0037(13)
C5 0.0229(12) 0.0303(14) 0.0324(15) -0.0020(11) 0.0049(10) -0.0042(10)
C6 0.0334(14) 0.0441(16) 0.0314(16) 0.0108(12) 0.0008(11) 0.0059(12)
C7 0.0300(13) 0.0551(18) 0.0367(16) 0.0075(13) 0.0100(12) 0.0150(12)
C8 0.0348(14) 0.0462(17) 0.0288(15) 0.0051(12) 0.0066(12) 0.0043(12)
C9 0.0388(14) 0.0418(16) 0.0305(15) 0.0100(12) 0.0006(11) 0.0102(12)
C10 0.0301(13) 0.0358(15) 0.0314(15) 0.0029(12) 0.0014(11) 0.0078(11)
C11 0.0612(17) 0.080(2) 0.0280(16) 0.0192(15) 0.0068(13) 0.0074(15)
C12 0.0266(12) 0.0185(12) 0.0261(13) -0.0018(10) 0.0061(10) -0.0039(10)
C13 0.0206(12) 0.0275(13) 0.0277(13) 0.0003(10) 0.0032(9) -0.0010(10)
C14 0.0191(11) 0.0305(14) 0.0351(15) 0.0038(11) 0.0071(10) -0.0063(10)
C15 0.0253(12) 0.0245(13) 0.0321(14) 0.0048(11) 0.0049(10) -0.0051(10)
C16 0.0207(12) 0.0216(13) 0.0430(16) 0.0021(11) 0.0004(10) 0.0010(10)
C17 0.0205(12) 0.0179(12) 0.0346(14) -0.0021(10) 0.0028(10) -0.0030(9)
C18 0.0227(12) 0.0340(15) 0.0325(14) 0.0085(11) 0.0030(10) -0.0059(10)
C19 0.0328(14) 0.0390(16) 0.0565(18) 0.0020(13) -0.0052(12) 0.0050(12)
C20 0.0193(13) 0.103(3) 0.077(2) 0.0489(19) 0.0035(13) -0.0008(14)
C21 0.0518(16) 0.0428(17) 0.0471(18) -0.0002(13) -0.0121(13) -0.0029(13)
C22 0.0296(13) 0.0357(15) 0.0407(16) 0.0136(12) 0.0037(11) -0.0049(11)
C23 0.0510(17) 0.0552(19) 0.069(2) 0.0324(16) 0.0041(14) -0.0196(14)
C24 0.0606(19) 0.083(2) 0.116(3) 0.073(2) 0.0315(18) 0.0217(18)
C25 0.112(2) 0.076(2) 0.0402(19) 0.0133(17) 0.0118(17) -0.0328(19)
C26 0.0185(11) 0.0217(13) 0.0360(14) 0.0011(10) 0.0061(10) -0.0009(10)
C27 0.0319(13) 0.0289(15) 0.0585(18) -0.0045(12) 0.0147(12) -0.0015(11)
C28 0.0174(11) 0.0251(13) 0.0231(13) 0.0051(10) 0.0033(9) 0.0028(9)
C29 0.0190(11) 0.0252(13) 0.0228(13) 0.0026(10) 0.0028(9) -0.0022(10)
C30 0.0230(12) 0.0321(15) 0.0302(14) 0.0015(11) -0.0014(10) -0.0008(10)
C31 0.0193(12) 0.0348(15) 0.0299(14) 0.0088(11) 0.0039(10) 0.0009(10)
C32 0.0219(12) 0.0230(13) 0.0405(15) 0.0073(11) 0.0083(11) 0.0016(10)
C33 0.0150(11) 0.0256(13) 0.0316(14) 0.0017(11) 0.0058(9) 0.0007(9)
C34 0.0259(12) 0.0245(13) 0.0293(14) 0.0058(10) -0.0038(10) -0.0026(10)
C35 0.0448(15) 0.0251(14) 0.0579(18) 0.0009(12) -0.0146(12) -0.0013(12)
C36 0.0533(16) 0.0373(16) 0.0433(17) 0.0078(13) 0.0079(12) -0.0130(12)
C37 0.0442(14) 0.0329(15) 0.0516(17) 0.0084(13) -0.0136(12) -0.0107(12)
C38 0.0349(14) 0.0389(16) 0.0372(16) 0.0146(12) 0.0001(11) 0.0015(12)
C39 0.055(4) 0.064(3) 0.035(3) 0.017(2) -0.016(2) -0.002(3)
C40 0.074(4) 0.096(6) 0.038(3) 0.021(3) -0.006(3) 0.052(5)
C41 0.062(3) 0.092(6) 0.042(3) 0.025(3) 0.002(3) -0.018(3)
C39X 0.103(7) 0.046(4) 0.058(5) 0.026(4) -0.035(5) 0.001(4)
C40X 0.103(7) 0.064(6) 0.040(4) 0.022(4) 0.005(4) 0.005(5)
C41X 0.045(4) 0.103(8) 0.081(6) 0.044(6) -0.018(4) -0.009(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.6567(17) . ?
V1 O3 1.8295(12) . ?
V1 O2 1.8373(13) . ?
V1 O1 1.8632(12) . ?
V1 O1 2.2590(13) 2_566 ?
N1 C5 1.392(2) . ?
O1 C1 1.472(2) . ?
O1 V1 2.2590(13) 2_566 ?
O2 C12 1.374(2) . ?
O3 C28 1.371(2) . ?
O4 C8 1.370(2) . ?
O4 C11 1.425(2) . ?
C1 C3 1.478(3) . ?
C1 C2 1.504(3) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C10 1.388(3) . ?
C5 C6 1.410(3) . ?
C6 C7 1.370(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.377(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(3) . ?
C9 C10 1.369(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.404(3) . ?
C12 C13 1.414(3) . ?
C13 C14 1.386(3) . ?
C13 C18 1.538(3) . ?
C14 C15 1.388(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(3) . ?
C15 C22 1.538(3) . ?
C16 C17 1.379(3) . ?
C16 H16 0.9500 . ?
C17 C26 1.527(3) . ?
C18 C21 1.523(3) . ?
C18 C19 1.525(3) . ?
C18 C20 1.530(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.515(3) . ?
C22 C24 1.520(3) . ?
C22 C25 1.522(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.525(3) . ?
C26 C27 1.533(3) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.398(3) . ?
C28 C29 1.417(3) . ?
C29 C30 1.387(3) . ?
C29 C34 1.532(3) . ?
C30 C31 1.396(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(3) . ?
C31 C38 1.528(3) . ?
C32 C33 1.384(3) . ?
C32 H32 0.9500 . ?
C34 C37 1.531(3) . ?
C34 C35 1.532(3) . ?
C34 C36 1.535(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40X 1.447(7) . ?
C38 C40 1.483(5) . ?
C38 C41 1.541(5) . ?
C38 C41X 1.545(7) . ?
C38 C39X 1.557(7) . ?
C38 C39 1.582(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C39X H39D 0.9800 . ?
C39X H39E 0.9800 . ?
C39X H39F 0.9800 . ?
C40X H40D 0.9800 . ?
C40X H40E 0.9800 . ?
C40X H40F 0.9800 . ?
C41X H41D 0.9800 . ?
C41X H41E 0.9800 . ?
C41X H41F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O3 98.51(7) . . ?
N1 V1 O2 95.82(7) . . ?
O3 V1 O2 112.19(6) . . ?
N1 V1 O1 101.15(7) . . ?
O3 V1 O1 118.96(6) . . ?
O2 V1 O1 122.30(6) . . ?
N1 V1 O1 174.32(6) . 2_566 ?
O3 V1 O1 86.01(5) . 2_566 ?
O2 V1 O1 85.58(5) . 2_566 ?
O1 V1 O1 73.54(6) . 2_566 ?
C5 N1 V1 171.47(15) . . ?
C1 O1 V1 125.22(12) . . ?
C1 O1 V1 128.31(11) . 2_566 ?
V1 O1 V1 106.46(6) . 2_566 ?
C12 O2 V1 123.02(12) . . ?
C28 O3 V1 127.18(11) . . ?
C8 O4 C11 118.14(18) . . ?
O1 C1 C3 113.66(17) . . ?
O1 C1 C2 111.49(18) . . ?
C3 C1 C2 115.13(19) . . ?
O1 C1 H1 105.1 . . ?
C3 C1 H1 105.1 . . ?
C2 C1 H1 105.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C5 N1 121.88(19) . . ?
C10 C5 C6 117.7(2) . . ?
N1 C5 C6 120.44(19) . . ?
C7 C6 C5 120.3(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 120.9(2) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
O4 C8 C7 115.8(2) . . ?
O4 C8 C9 124.7(2) . . ?
C7 C8 C9 119.5(2) . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C5 121.7(2) . . ?
C9 C10 H10 119.1 . . ?
C5 C10 H10 119.1 . . ?
O4 C11 H11A 109.5 . . ?
O4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 C17 117.81(16) . . ?
O2 C12 C13 121.61(17) . . ?
C17 C12 C13 120.55(18) . . ?
C14 C13 C12 116.55(18) . . ?
C14 C13 C18 120.51(17) . . ?
C12 C13 C18 122.77(18) . . ?
C13 C14 C15 124.61(18) . . ?
C13 C14 H14 117.7 . . ?
C15 C14 H14 117.7 . . ?
C16 C15 C14 116.37(19) . . ?
C16 C15 C22 121.84(18) . . ?
C14 C15 C22 121.80(18) . . ?
C17 C16 C15 122.85(18) . . ?
C17 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
C16 C17 C12 118.92(17) . . ?
C16 C17 C26 120.21(17) . . ?
C12 C17 C26 120.86(18) . . ?
C21 C18 C19 109.28(18) . . ?
C21 C18 C20 107.9(2) . . ?
C19 C18 C20 106.99(19) . . ?
C21 C18 C13 107.31(17) . . ?
C19 C18 C13 113.00(17) . . ?
C20 C18 C13 112.25(17) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C24 107.1(2) . . ?
C23 C22 C25 109.5(2) . . ?
C24 C22 C25 109.5(2) . . ?
C23 C22 C15 111.61(18) . . ?
C24 C22 C15 111.58(18) . . ?
C25 C22 C15 107.5(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C33 C26 C17 112.18(16) . . ?
C33 C26 C27 112.88(16) . . ?
C17 C26 C27 110.98(17) . . ?
C33 C26 H26 106.8 . . ?
C17 C26 H26 106.8 . . ?
C27 C26 H26 106.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 117.88(18) . . ?
O3 C28 C29 121.44(18) . . ?
C33 C28 C29 120.66(18) . . ?
C30 C29 C28 116.80(19) . . ?
C30 C29 C34 121.19(18) . . ?
C28 C29 C34 121.97(18) . . ?
C29 C30 C31 124.2(2) . . ?
C29 C30 H30 117.9 . . ?
C31 C30 H30 117.9 . . ?
C32 C31 C30 116.55(19) . . ?
C32 C31 C38 121.2(2) . . ?
C30 C31 C38 122.3(2) . . ?
C33 C32 C31 122.5(2) . . ?
C33 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C32 C33 C28 119.2(2) . . ?
C32 C33 C26 120.06(19) . . ?
C28 C33 C26 120.72(18) . . ?
C37 C34 C29 112.58(17) . . ?
C37 C34 C35 106.80(18) . . ?
C29 C34 C35 111.30(16) . . ?
C37 C34 C36 107.05(18) . . ?
C29 C34 C36 108.91(17) . . ?
C35 C34 C36 110.08(17) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40X C38 C40 140.7(4) . . ?
C40X C38 C31 109.5(3) . . ?
C40 C38 C31 109.3(2) . . ?
C40X C38 C41 57.6(4) . . ?
C40 C38 C41 112.8(4) . . ?
C31 C38 C41 110.3(2) . . ?
C40X C38 C41X 110.7(5) . . ?
C40 C38 C41X 50.2(4) . . ?
C31 C38 C41X 108.1(3) . . ?
C41 C38 C41X 141.6(3) . . ?
C40X C38 C39X 110.2(5) . . ?
C40 C38 C39X 59.6(4) . . ?
C31 C38 C39X 111.4(3) . . ?
C41 C38 C39X 56.2(4) . . ?
C41X C38 C39X 107.0(5) . . ?
C40X C38 C39 50.5(3) . . ?
C40 C38 C39 107.6(3) . . ?
C31 C38 C39 112.6(2) . . ?
C41 C38 C39 104.2(3) . . ?
C41X C38 C39 61.9(4) . . ?
C39X C38 C39 135.9(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
C38 C39X H39D 109.5 . . ?
C38 C39X H39E 109.5 . . ?
H39D C39X H39E 109.5 . . ?
C38 C39X H39F 109.5 . . ?
H39D C39X H39F 109.5 . . ?
H39E C39X H39F 109.5 . . ?
C38 C40X H40D 109.5 . . ?
C38 C40X H40E 109.5 . . ?
H40D C40X H40E 109.5 . . ?
C38 C40X H40F 109.5 . . ?
H40D C40X H40F 109.5 . . ?
H40E C40X H40F 109.5 . . ?
C38 C41X H41D 109.5 . . ?
C38 C41X H41E 109.5 . . ?
H41D C41X H41E 109.5 . . ?
C38 C41X H41F 109.5 . . ?
H41D C41X H41F 109.5 . . ?
H41E C41X H41F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 2.14(15) . . . . ?
O3 V1 O1 C1 -104.21(14) . . . . ?
O2 V1 O1 C1 106.44(15) . . . . ?
O1 V1 O1 C1 -179.94(17) 2_566 . . . ?
N1 V1 O1 V1 -177.92(7) . . . 2_566 ?
O3 V1 O1 V1 75.73(7) . . . 2_566 ?
O2 V1 O1 V1 -73.63(7) . . . 2_566 ?
O1 V1 O1 V1 0.0 2_566 . . 2_566 ?
N1 V1 O2 C12 -27.44(14) . . . . ?
O3 V1 O2 C12 74.22(14) . . . . ?
O1 V1 O2 C12 -134.57(13) . . . . ?
O1 V1 O2 C12 158.08(13) 2_566 . . . ?
N1 V1 O3 C28 27.01(16) . . . . ?
O2 V1 O3 C28 -72.88(16) . . . . ?
O1 V1 O3 C28 134.85(15) . . . . ?
O1 V1 O3 C28 -156.46(15) 2_566 . . . ?
V1 O1 C1 C3 118.29(17) . . . . ?
V1 O1 C1 C3 -61.6(2) 2_566 . . . ?
V1 O1 C1 C2 -109.59(17) . . . . ?
V1 O1 C1 C2 70.5(2) 2_566 . . . ?
C10 C5 C6 C7 -0.2(3) . . . . ?
N1 C5 C6 C7 178.4(2) . . . . ?
C5 C6 C7 C8 -1.0(4) . . . . ?
C11 O4 C8 C7 171.6(2) . . . . ?
C11 O4 C8 C9 -10.0(3) . . . . ?
C6 C7 C8 O4 179.7(2) . . . . ?
C6 C7 C8 C9 1.2(4) . . . . ?
O4 C8 C9 C10 -178.6(2) . . . . ?
C7 C8 C9 C10 -0.2(3) . . . . ?
C8 C9 C10 C5 -1.0(3) . . . . ?
N1 C5 C10 C9 -177.4(2) . . . . ?
C6 C5 C10 C9 1.2(3) . . . . ?
V1 O2 C12 C17 -69.4(2) . . . . ?
V1 O2 C12 C13 112.66(19) . . . . ?
O2 C12 C13 C14 -177.42(19) . . . . ?
C17 C12 C13 C14 4.7(3) . . . . ?
O2 C12 C13 C18 7.2(3) . . . . ?
C17 C12 C13 C18 -170.69(19) . . . . ?
C12 C13 C14 C15 -2.6(3) . . . . ?
C18 C13 C14 C15 172.9(2) . . . . ?
C13 C14 C15 C16 -0.1(3) . . . . ?
C13 C14 C15 C22 -179.9(2) . . . . ?
C14 C15 C16 C17 0.8(3) . . . . ?
C22 C15 C16 C17 -179.4(2) . . . . ?
C15 C16 C17 C12 1.3(3) . . . . ?
C15 C16 C17 C26 -177.61(19) . . . . ?
O2 C12 C17 C16 177.90(18) . . . . ?
C13 C12 C17 C16 -4.1(3) . . . . ?
O2 C12 C17 C26 -3.2(3) . . . . ?
C13 C12 C17 C26 174.75(19) . . . . ?
C14 C13 C18 C21 -110.1(2) . . . . ?
C12 C13 C18 C21 65.1(3) . . . . ?
C14 C13 C18 C19 129.3(2) . . . . ?
C12 C13 C18 C19 -55.5(3) . . . . ?
C14 C13 C18 C20 8.2(3) . . . . ?
C12 C13 C18 C20 -176.6(2) . . . . ?
C16 C15 C22 C23 -149.4(2) . . . . ?
C14 C15 C22 C23 30.4(3) . . . . ?
C16 C15 C22 C24 -29.6(3) . . . . ?
C14 C15 C22 C24 150.2(2) . . . . ?
C16 C15 C22 C25 90.5(3) . . . . ?
C14 C15 C22 C25 -89.7(3) . . . . ?
C16 C17 C26 C33 -76.6(2) . . . . ?
C12 C17 C26 C33 104.6(2) . . . . ?
C16 C17 C26 C27 50.7(3) . . . . ?
C12 C17 C26 C27 -128.1(2) . . . . ?
V1 O3 C28 C33 68.4(2) . . . . ?
V1 O3 C28 C29 -113.27(17) . . . . ?
O3 C28 C29 C30 177.80(16) . . . . ?
C33 C28 C29 C30 -3.9(3) . . . . ?
O3 C28 C29 C34 -4.6(3) . . . . ?
C33 C28 C29 C34 173.68(17) . . . . ?
C28 C29 C30 C31 2.5(3) . . . . ?
C34 C29 C30 C31 -175.12(18) . . . . ?
C29 C30 C31 C32 0.4(3) . . . . ?
C29 C30 C31 C38 179.61(19) . . . . ?
C30 C31 C32 C33 -2.0(3) . . . . ?
C38 C31 C32 C33 178.75(18) . . . . ?
C31 C32 C33 C28 0.6(3) . . . . ?
C31 C32 C33 C26 -178.87(17) . . . . ?
O3 C28 C33 C32 -179.17(16) . . . . ?
C29 C28 C33 C32 2.5(3) . . . . ?
O3 C28 C33 C26 0.3(3) . . . . ?
C29 C28 C33 C26 -178.03(17) . . . . ?
C17 C26 C33 C32 80.4(2) . . . . ?
C27 C26 C33 C32 -45.9(2) . . . . ?
C17 C26 C33 C28 -99.1(2) . . . . ?
C27 C26 C33 C28 134.67(19) . . . . ?
C30 C29 C34 C37 -0.6(3) . . . . ?
C28 C29 C34 C37 -178.14(18) . . . . ?
C30 C29 C34 C35 -120.5(2) . . . . ?
C28 C29 C34 C35 62.0(2) . . . . ?
C30 C29 C34 C36 117.9(2) . . . . ?
C28 C29 C34 C36 -59.6(2) . . . . ?
C32 C31 C38 C40X -116.6(4) . . . . ?
C30 C31 C38 C40X 64.3(4) . . . . ?
C32 C31 C38 C40 69.6(4) . . . . ?
C30 C31 C38 C40 -109.6(4) . . . . ?
C32 C31 C38 C41 -55.0(4) . . . . ?
C30 C31 C38 C41 125.9(3) . . . . ?
C32 C31 C38 C41X 122.8(5) . . . . ?
C30 C31 C38 C41X -56.4(5) . . . . ?
C32 C31 C38 C39X 5.6(5) . . . . ?
C30 C31 C38 C39X -173.6(4) . . . . ?
C32 C31 C38 C39 -170.8(3) . . . . ?
C30 C31 C38 C39 10.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.047

data_8
_database_code_depnum_ccdc_archive 'CCDC 718358'

_chemical_name_common            'Compound 8'
_chemical_melting_point          ?
_chemical_formula_structural     
'[V(=NC6H4Me)(diphenolate)(mu-O-Pr)]2.2(CH2Cl2)'
_chemical_formula_moiety         'C80 H116 N2 O6 V2, 2(C H2 Cl2)'
_chemical_formula_sum            'C82 H120 Cl4 N2 O6 V2'
_chemical_formula_weight         1473.48

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61

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

_cell_length_a                   19.206(2)
_cell_length_b                   19.9382(17)
_cell_length_c                   21.798(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8347.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    5258
_cell_measurement_theta_min      3.0049
_cell_measurement_theta_max      24.9997

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3152
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7275
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            70865
_diffrn_reflns_av_R_equivalents  0.2251
_diffrn_reflns_av_sigmaI/netI    0.1755
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.14
_reflns_number_total             7425
_reflns_number_gt                3676
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'

_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
The crystal was weakly diffracting and this led to a high R~int~ value.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0335P)^2^] where P=(Fo^2^+2Fc^2^)/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         7425
_refine_ls_number_parameters     455
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1863
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.48372(3) 0.07580(3) 0.47450(3) 0.01631(17) Uani 1 1 d . . .
N1 N 0.43103(15) 0.13939(15) 0.49088(14) 0.0165(9) Uani 1 1 d . . .
O1 O 0.45947(12) 0.01722(12) 0.53892(12) 0.0150(7) Uani 1 1 d . . .
O2 O 0.56763(12) 0.11951(12) 0.48000(12) 0.0164(6) Uani 1 1 d . . .
O3 O 0.45858(12) 0.06450(13) 0.39294(12) 0.0178(7) Uani 1 1 d . . .
C1 C 0.4196(2) 0.0320(2) 0.59358(18) 0.0177(11) Uani 1 1 d . . .
H1A H 0.4150 0.0813 0.5979 0.021 Uiso 1 1 calc R . .
H1B H 0.4449 0.0150 0.6299 0.021 Uiso 1 1 calc R . .
C2 C 0.3478(2) 0.0008(2) 0.59169(18) 0.0206(11) Uani 1 1 d . . .
H2A H 0.3518 -0.0475 0.5817 0.025 Uiso 1 1 calc R . .
H2B H 0.3198 0.0225 0.5591 0.025 Uiso 1 1 calc R . .
C3 C 0.3104(2) 0.0091(2) 0.6542(2) 0.0374(13) Uani 1 1 d . . .
H3A H 0.3378 -0.0128 0.6864 0.056 Uiso 1 1 calc R . .
H3B H 0.2641 -0.0115 0.6521 0.056 Uiso 1 1 calc R . .
H3C H 0.3056 0.0570 0.6637 0.056 Uiso 1 1 calc R . .
C5 C 0.3879(2) 0.1939(2) 0.50586(19) 0.0199(11) Uani 1 1 d . . .
C6 C 0.4083(2) 0.2592(2) 0.4908(2) 0.0302(12) Uani 1 1 d . . .
H6 H 0.4497 0.2670 0.4681 0.036 Uiso 1 1 calc R . .
C7 C 0.3669(2) 0.3124(2) 0.5094(2) 0.0408(15) Uani 1 1 d . . .
H7 H 0.3810 0.3567 0.4995 0.049 Uiso 1 1 calc R . .
C8 C 0.3059(2) 0.3031(2) 0.5420(2) 0.0285(12) Uani 1 1 d . . .
C9 C 0.2850(2) 0.2380(2) 0.5537(2) 0.0262(12) Uani 1 1 d . . .
H9 H 0.2422 0.2303 0.5744 0.031 Uiso 1 1 calc R . .
C10 C 0.3245(2) 0.1844(2) 0.5363(2) 0.0227(11) Uani 1 1 d . . .
H10 H 0.3088 0.1402 0.5449 0.027 Uiso 1 1 calc R . .
C11 C 0.2645(2) 0.3623(2) 0.5661(2) 0.0465(15) Uani 1 1 d . . .
H11A H 0.2794 0.3725 0.6081 0.070 Uiso 1 1 calc R . .
H11B H 0.2148 0.3512 0.5660 0.070 Uiso 1 1 calc R . .
H11C H 0.2727 0.4014 0.5399 0.070 Uiso 1 1 calc R . .
C12 C 0.57771(19) 0.18740(19) 0.4719(2) 0.0179(10) Uani 1 1 d . . .
C13 C 0.59612(19) 0.2292(2) 0.5217(2) 0.0210(10) Uani 1 1 d . . .
C14 C 0.6014(2) 0.2981(2) 0.5090(2) 0.0272(12) Uani 1 1 d . . .
H14 H 0.6119 0.3275 0.5420 0.033 Uiso 1 1 calc R . .
C15 C 0.5924(2) 0.3262(2) 0.4510(2) 0.0268(12) Uani 1 1 d . . .
C16 C 0.5781(2) 0.2820(2) 0.4033(2) 0.0260(12) Uani 1 1 d . . .
H16 H 0.5732 0.2995 0.3629 0.031 Uiso 1 1 calc R . .
C17 C 0.57084(19) 0.2133(2) 0.4123(2) 0.0192(11) Uani 1 1 d . . .
C18 C 0.6126(2) 0.2021(2) 0.5859(2) 0.0255(12) Uani 1 1 d . . .
C19 C 0.5515(2) 0.1623(2) 0.6132(2) 0.0393(14) Uani 1 1 d . . .
H19A H 0.5089 0.1893 0.6108 0.059 Uiso 1 1 calc R . .
H19B H 0.5614 0.1517 0.6563 0.059 Uiso 1 1 calc R . .
H19C H 0.5451 0.1206 0.5901 0.059 Uiso 1 1 calc R . .
C20 C 0.6775(2) 0.1572(2) 0.5818(2) 0.0382(14) Uani 1 1 d . . .
H20A H 0.6678 0.1190 0.5548 0.057 Uiso 1 1 calc R . .
H20B H 0.6896 0.1408 0.6228 0.057 Uiso 1 1 calc R . .
H20C H 0.7165 0.1832 0.5652 0.057 Uiso 1 1 calc R . .
C21 C 0.6296(3) 0.2588(2) 0.6321(2) 0.0616(18) Uani 1 1 d . . .
H21A H 0.6709 0.2833 0.6181 0.092 Uiso 1 1 calc R . .
H21B H 0.6387 0.2394 0.6726 0.092 Uiso 1 1 calc R . .
H21C H 0.5901 0.2897 0.6347 0.092 Uiso 1 1 calc R . .
C22 C 0.5941(2) 0.4024(2) 0.4402(2) 0.0350(13) Uani 1 1 d . . .
C23 C 0.6320(3) 0.4394(2) 0.4927(3) 0.093(3) Uani 1 1 d . . .
H23A H 0.6340 0.4874 0.4834 0.140 Uiso 1 1 calc R . .
H23B H 0.6794 0.4217 0.4968 0.140 Uiso 1 1 calc R . .
H23C H 0.6066 0.4324 0.5312 0.140 Uiso 1 1 calc R . .
C24 C 0.5196(2) 0.4280(2) 0.4379(2) 0.0511(14) Uani 1 1 d . . .
H24A H 0.5197 0.4766 0.4311 0.077 Uiso 1 1 calc R . .
H24B H 0.4963 0.4180 0.4768 0.077 Uiso 1 1 calc R . .
H24C H 0.4946 0.4059 0.4043 0.077 Uiso 1 1 calc R . .
C25 C 0.6304(3) 0.4187(3) 0.3796(3) 0.110(3) Uani 1 1 d . . .
H25A H 0.6025 0.4014 0.3454 0.165 Uiso 1 1 calc R . .
H25B H 0.6765 0.3977 0.3790 0.165 Uiso 1 1 calc R . .
H25C H 0.6354 0.4674 0.3756 0.165 Uiso 1 1 calc R . .
C26 C 0.5546(2) 0.1672(2) 0.35797(19) 0.0201(11) Uani 1 1 d . . .
H26 H 0.5654 0.1205 0.3715 0.024 Uiso 1 1 calc R . .
C27 C 0.6014(2) 0.1818(2) 0.3016(2) 0.0327(13) Uani 1 1 d . . .
H27A H 0.5914 0.2269 0.2861 0.049 Uiso 1 1 calc R . .
H27B H 0.5919 0.1487 0.2695 0.049 Uiso 1 1 calc R . .
H27C H 0.6504 0.1791 0.3137 0.049 Uiso 1 1 calc R . .
C28 C 0.4318(2) 0.1164(2) 0.35825(18) 0.0167(10) Uani 1 1 d . . .
C29 C 0.3613(2) 0.1147(2) 0.33795(19) 0.0191(10) Uani 1 1 d . . .
C30 C 0.3376(2) 0.1715(2) 0.3061(2) 0.0248(12) Uani 1 1 d . . .
H30 H 0.2904 0.1725 0.2932 0.030 Uiso 1 1 calc R . .
C31 C 0.3795(2) 0.2267(2) 0.2922(2) 0.0229(11) Uani 1 1 d . . .
C32 C 0.4489(2) 0.2228(2) 0.30956(19) 0.0242(11) Uani 1 1 d . . .
H32 H 0.4790 0.2588 0.2990 0.029 Uiso 1 1 calc R . .
C33 C 0.4766(2) 0.1689(2) 0.34147(18) 0.0197(10) Uani 1 1 d . . .
C34 C 0.3130(2) 0.0536(2) 0.3474(2) 0.0242(11) Uani 1 1 d . . .
C35 C 0.3047(2) 0.0363(2) 0.4157(2) 0.0344(13) Uani 1 1 d . . .
H35A H 0.2921 0.0768 0.4386 0.052 Uiso 1 1 calc R . .
H35B H 0.3487 0.0185 0.4315 0.052 Uiso 1 1 calc R . .
H35C H 0.2680 0.0026 0.4205 0.052 Uiso 1 1 calc R . .
C36 C 0.3449(2) -0.0061(2) 0.3125(2) 0.0383(14) Uani 1 1 d . . .
H36A H 0.3915 -0.0155 0.3287 0.057 Uiso 1 1 calc R . .
H36B H 0.3482 0.0049 0.2688 0.057 Uiso 1 1 calc R . .
H36C H 0.3152 -0.0457 0.3179 0.057 Uiso 1 1 calc R . .
C37 C 0.2393(2) 0.0652(2) 0.3219(2) 0.0439(14) Uani 1 1 d . . .
H37A H 0.2115 0.0245 0.3273 0.066 Uiso 1 1 calc R . .
H37B H 0.2423 0.0761 0.2781 0.066 Uiso 1 1 calc R . .
H37C H 0.2173 0.1025 0.3439 0.066 Uiso 1 1 calc R . .
C38 C 0.3518(2) 0.2893(2) 0.2590(2) 0.0295(12) Uani 1 1 d . . .
C39 C 0.2763(3) 0.2805(3) 0.2362(3) 0.0640(19) Uani 1 1 d . . .
H39A H 0.2610 0.3217 0.2157 0.096 Uiso 1 1 calc R . .
H39B H 0.2457 0.2711 0.2711 0.096 Uiso 1 1 calc R . .
H39C H 0.2742 0.2431 0.2071 0.096 Uiso 1 1 calc R . .
C40 C 0.3969(3) 0.3053(3) 0.2039(3) 0.0644(19) Uani 1 1 d . . .
H40A H 0.3782 0.3447 0.1827 0.097 Uiso 1 1 calc R . .
H40B H 0.3972 0.2669 0.1759 0.097 Uiso 1 1 calc R . .
H40C H 0.4446 0.3147 0.2176 0.097 Uiso 1 1 calc R . .
C41 C 0.3522(3) 0.3475(3) 0.3044(3) 0.0693(19) Uani 1 1 d . . .
H41A H 0.4000 0.3559 0.3182 0.104 Uiso 1 1 calc R . .
H41B H 0.3230 0.3363 0.3398 0.104 Uiso 1 1 calc R . .
H41C H 0.3340 0.3878 0.2844 0.104 Uiso 1 1 calc R . .
C200 C 0.4649(3) 0.0821(4) 0.1975(3) 0.087(2) Uani 0.568(8) 1 d PD A 1
H20D H 0.4183 0.0625 0.2054 0.104 Uiso 0.568(8) 1 calc PR A 1
H20E H 0.4708 0.1195 0.2269 0.104 Uiso 0.568(8) 1 calc PR A 1
Cl1 Cl 0.463(2) 0.1156(19) 0.1269(9) 0.104(3) Uani 0.568(8) 1 d PD A 1
Cl2 Cl 0.5259(4) 0.0214(3) 0.2164(3) 0.0908(17) Uani 0.568(8) 1 d PD A 1
C201 C 0.4649(3) 0.0821(4) 0.1975(3) 0.087(2) Uani 0.432(8) 1 d PD A 2
H20F H 0.4280 0.0481 0.2040 0.104 Uiso 0.432(8) 1 calc PR A 2
H20G H 0.4643 0.1137 0.2325 0.104 Uiso 0.432(8) 1 calc PR A 2
Cl1X Cl 0.451(3) 0.124(3) 0.1305(12) 0.104(3) Uani 0.432(8) 1 d PD A 2
Cl2X Cl 0.5494(4) 0.0418(5) 0.1916(4) 0.0908(17) Uani 0.432(8) 1 d PD A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0195(4) 0.0135(4) 0.0159(4) 0.0009(4) 0.0008(4) 0.0010(4)
N1 0.0168(19) 0.017(2) 0.016(2) 0.0018(16) 0.0011(16) -0.0036(15)
O1 0.0178(15) 0.0131(16) 0.0142(17) -0.0009(13) 0.0035(12) 0.0015(12)
O2 0.0195(16) 0.0109(15) 0.0187(17) -0.0006(15) 0.0021(14) 0.0012(12)
O3 0.0232(16) 0.0158(17) 0.0145(16) 0.0003(14) 0.0001(12) 0.0017(13)
C1 0.019(3) 0.020(3) 0.014(3) 0.001(2) 0.004(2) 0.000(2)
C2 0.025(3) 0.016(3) 0.021(3) -0.001(2) 0.003(2) 0.001(2)
C3 0.031(3) 0.036(3) 0.045(4) -0.003(3) 0.018(3) -0.011(2)
C5 0.020(3) 0.023(3) 0.017(3) -0.002(2) -0.002(2) 0.005(2)
C6 0.026(3) 0.023(3) 0.043(3) 0.005(2) 0.014(2) 0.002(2)
C7 0.031(3) 0.016(3) 0.076(5) 0.003(3) 0.009(3) 0.003(2)
C8 0.019(3) 0.027(3) 0.039(3) -0.006(2) -0.001(2) 0.004(2)
C9 0.014(3) 0.028(3) 0.036(3) -0.005(2) 0.005(2) -0.001(2)
C10 0.023(3) 0.018(3) 0.027(3) 0.004(2) 0.004(2) 0.001(2)
C11 0.035(3) 0.029(3) 0.076(4) -0.015(3) 0.008(3) 0.009(2)
C12 0.016(2) 0.013(2) 0.025(3) 0.006(2) 0.006(2) 0.0016(18)
C13 0.017(2) 0.016(3) 0.030(3) 0.003(2) 0.002(2) 0.0007(19)
C14 0.023(3) 0.022(3) 0.037(3) -0.007(2) 0.001(2) -0.002(2)
C15 0.014(3) 0.018(3) 0.048(3) 0.011(3) 0.002(2) 0.000(2)
C16 0.019(3) 0.021(3) 0.038(3) 0.010(2) -0.003(2) -0.003(2)
C17 0.010(2) 0.020(3) 0.028(3) 0.005(2) 0.006(2) -0.001(2)
C18 0.030(3) 0.022(3) 0.025(3) -0.002(2) -0.006(2) -0.004(2)
C19 0.030(3) 0.070(4) 0.017(3) -0.003(3) 0.004(2) 0.002(3)
C20 0.036(3) 0.037(3) 0.041(4) 0.013(3) -0.009(3) -0.002(3)
C21 0.103(5) 0.040(4) 0.041(4) -0.008(3) -0.030(3) 0.000(3)
C22 0.027(3) 0.014(3) 0.064(4) 0.007(3) -0.001(3) -0.001(2)
C23 0.123(5) 0.021(4) 0.136(7) 0.016(4) -0.074(5) -0.026(3)
C24 0.047(3) 0.020(3) 0.086(4) 0.008(3) -0.003(3) 0.005(3)
C25 0.147(7) 0.025(4) 0.159(7) 0.027(5) 0.104(6) 0.003(4)
C26 0.022(3) 0.018(3) 0.021(3) 0.010(2) 0.005(2) 0.001(2)
C27 0.028(3) 0.038(3) 0.033(3) 0.008(3) 0.005(2) -0.004(2)
C28 0.025(3) 0.016(3) 0.010(2) -0.001(2) 0.000(2) 0.008(2)
C29 0.027(3) 0.015(3) 0.015(3) -0.002(2) 0.000(2) 0.003(2)
C30 0.022(3) 0.034(3) 0.018(3) 0.000(2) -0.002(2) 0.003(2)
C31 0.024(3) 0.026(3) 0.018(3) 0.007(2) 0.000(2) 0.004(2)
C32 0.029(3) 0.022(3) 0.021(3) 0.004(2) 0.006(2) -0.005(2)
C33 0.025(3) 0.020(3) 0.014(2) 0.002(2) -0.004(2) -0.001(2)
C34 0.025(3) 0.024(3) 0.024(3) 0.003(2) -0.009(2) 0.001(2)
C35 0.034(3) 0.032(3) 0.038(3) 0.000(3) 0.001(3) -0.014(2)
C36 0.056(3) 0.027(3) 0.032(3) 0.002(3) -0.010(3) -0.006(3)
C37 0.039(3) 0.031(3) 0.061(4) 0.008(3) -0.017(3) -0.012(3)
C38 0.023(3) 0.028(3) 0.038(3) 0.015(3) -0.002(2) 0.005(2)
C39 0.050(4) 0.058(4) 0.085(5) 0.046(4) -0.012(3) 0.005(3)
C40 0.059(4) 0.067(4) 0.067(4) 0.049(4) 0.021(3) 0.023(3)
C41 0.092(5) 0.034(4) 0.083(5) 0.010(4) -0.012(4) 0.029(3)
C200 0.074(5) 0.147(7) 0.039(4) -0.021(4) 0.010(3) 0.010(5)
Cl1 0.194(10) 0.056(8) 0.061(2) -0.011(4) 0.013(3) 0.005(5)
Cl2 0.102(4) 0.095(4) 0.076(4) -0.028(3) -0.032(3) 0.019(3)
C201 0.074(5) 0.147(7) 0.039(4) -0.021(4) 0.010(3) 0.010(5)
Cl1X 0.194(10) 0.056(8) 0.061(2) -0.011(4) 0.013(3) 0.005(5)
Cl2X 0.102(4) 0.095(4) 0.076(4) -0.028(3) -0.032(3) 0.019(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.661(3) . ?
V1 O2 1.836(2) . ?
V1 O3 1.856(3) . ?
V1 O1 1.885(3) . ?
V1 O1 2.171(2) 5_656 ?
N1 C5 1.405(5) . ?
O1 C1 1.447(4) . ?
O1 V1 2.171(2) 5_656 ?
O2 C12 1.379(4) . ?
O3 C28 1.381(4) . ?
C1 C2 1.514(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.550(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.398(5) . ?
C5 C10 1.400(5) . ?
C6 C7 1.386(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.384(5) . ?
C8 C11 1.516(6) . ?
C9 C10 1.363(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.406(6) . ?
C12 C13 1.413(6) . ?
C13 C14 1.407(5) . ?
C13 C18 1.534(6) . ?
C14 C15 1.393(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(6) . ?
C15 C22 1.537(6) . ?
C16 C17 1.392(5) . ?
C16 H16 0.9500 . ?
C17 C26 1.530(6) . ?
C18 C19 1.536(6) . ?
C18 C20 1.538(6) . ?
C18 C21 1.548(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.522(6) . ?
C22 C25 1.527(7) . ?
C22 C23 1.544(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.542(5) . ?
C26 C27 1.549(5) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.404(5) . ?
C28 C29 1.425(5) . ?
C29 C30 1.405(5) . ?
C29 C34 1.545(5) . ?
C30 C31 1.396(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.389(5) . ?
C31 C38 1.536(6) . ?
C32 C33 1.386(5) . ?
C32 H32 0.9500 . ?
C34 C35 1.535(6) . ?
C34 C37 1.538(5) . ?
C34 C36 1.540(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.515(6) . ?
C38 C41 1.526(7) . ?
C38 C39 1.544(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C200 Cl1 1.678(11) . ?
C200 Cl2 1.734(8) . ?
C200 H20D 0.9900 . ?
C200 H20E 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
N1 V1 O2 99.11(13) . . ?
N1 V1 O3 98.05(14) . . ?
O2 V1 O3 110.39(12) . . ?
N1 V1 O1 99.34(13) . . ?
O2 V1 O1 117.55(11) . . ?
O3 V1 O1 125.04(11) . . ?
N1 V1 O1 170.74(13) . 5_656 ?
O2 V1 O1 88.46(10) . 5_656 ?
O3 V1 O1 84.15(10) . 5_656 ?
O1 V1 O1 72.27(11) . 5_656 ?
C5 N1 V1 178.4(3) . . ?
C1 O1 V1 128.2(2) . . ?
C1 O1 V1 123.5(2) . 5_656 ?
V1 O1 V1 107.73(11) . 5_656 ?
C12 O2 V1 125.5(2) . . ?
C28 O3 V1 122.0(2) . . ?
O1 C1 C2 112.1(3) . . ?
O1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
O1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 110.7(3) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C6 C5 C10 118.7(4) . . ?
C6 C5 N1 120.1(4) . . ?
C10 C5 N1 121.2(4) . . ?
C7 C6 C5 118.9(4) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
C8 C7 C6 122.3(4) . . ?
C8 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C7 C8 C9 117.7(4) . . ?
C7 C8 C11 121.2(4) . . ?
C9 C8 C11 121.0(4) . . ?
C10 C9 C8 121.5(4) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C5 120.7(4) . . ?
C9 C10 H10 119.7 . . ?
C5 C10 H10 119.7 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O2 C12 C17 117.7(4) . . ?
O2 C12 C13 121.1(4) . . ?
C17 C12 C13 121.2(4) . . ?
C14 C13 C12 116.3(4) . . ?
C14 C13 C18 120.6(4) . . ?
C12 C13 C18 123.1(4) . . ?
C15 C14 C13 124.3(4) . . ?
C15 C14 H14 117.9 . . ?
C13 C14 H14 117.9 . . ?
C16 C15 C14 116.6(4) . . ?
C16 C15 C22 121.0(4) . . ?
C14 C15 C22 122.3(4) . . ?
C15 C16 C17 122.6(4) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C12 118.8(4) . . ?
C16 C17 C26 120.2(4) . . ?
C12 C17 C26 121.0(4) . . ?
C13 C18 C19 112.2(3) . . ?
C13 C18 C20 108.6(4) . . ?
C19 C18 C20 110.0(4) . . ?
C13 C18 C21 112.3(4) . . ?
C19 C18 C21 106.7(4) . . ?
C20 C18 C21 107.0(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C25 109.3(4) . . ?
C24 C22 C15 108.4(4) . . ?
C25 C22 C15 110.7(4) . . ?
C24 C22 C23 107.9(4) . . ?
C25 C22 C23 108.9(4) . . ?
C15 C22 C23 111.6(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C17 C26 C33 111.4(3) . . ?
C17 C26 C27 112.5(3) . . ?
C33 C26 C27 112.0(3) . . ?
C17 C26 H26 106.8 . . ?
C33 C26 H26 106.8 . . ?
C27 C26 H26 106.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 118.3(4) . . ?
O3 C28 C29 120.4(4) . . ?
C33 C28 C29 121.3(4) . . ?
C30 C29 C28 116.2(4) . . ?
C30 C29 C34 120.5(4) . . ?
C28 C29 C34 123.3(4) . . ?
C31 C30 C29 123.8(4) . . ?
C31 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C32 C31 C30 116.7(4) . . ?
C32 C31 C38 120.4(4) . . ?
C30 C31 C38 122.9(4) . . ?
C33 C32 C31 123.3(4) . . ?
C33 C32 H32 118.4 . . ?
C31 C32 H32 118.4 . . ?
C32 C33 C28 118.3(4) . . ?
C32 C33 C26 120.4(4) . . ?
C28 C33 C26 121.3(4) . . ?
C35 C34 C37 106.8(4) . . ?
C35 C34 C36 110.2(4) . . ?
C37 C34 C36 107.7(4) . . ?
C35 C34 C29 111.7(4) . . ?
C37 C34 C29 112.7(4) . . ?
C36 C34 C29 107.7(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C41 110.6(4) . . ?
C40 C38 C31 110.2(4) . . ?
C41 C38 C31 108.1(4) . . ?
C40 C38 C39 107.7(4) . . ?
C41 C38 C39 107.5(4) . . ?
C31 C38 C39 112.6(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Cl1 C200 Cl2 120.7(9) . . ?
Cl1 C200 H20D 107.2 . . ?
Cl2 C200 H20D 107.2 . . ?
Cl1 C200 H20E 107.2 . . ?
Cl2 C200 H20E 107.2 . . ?
H20D C200 H20E 106.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 -13.2(3) . . . . ?
O2 V1 O1 C1 92.3(3) . . . . ?
O3 V1 O1 C1 -119.9(3) . . . . ?
O1 V1 O1 C1 170.9(3) 5_656 . . . ?
N1 V1 O1 V1 175.98(14) . . . 5_656 ?
O2 V1 O1 V1 -78.55(14) . . . 5_656 ?
O3 V1 O1 V1 69.21(15) . . . 5_656 ?
O1 V1 O1 V1 0.0 5_656 . . 5_656 ?
N1 V1 O2 C12 -25.0(3) . . . . ?
O3 V1 O2 C12 77.2(3) . . . . ?
O1 V1 O2 C12 -130.6(3) . . . . ?
O1 V1 O2 C12 160.4(3) 5_656 . . . ?
N1 V1 O3 C28 25.9(3) . . . . ?
O2 V1 O3 C28 -77.0(3) . . . . ?
O1 V1 O3 C28 133.3(3) . . . . ?
O1 V1 O3 C28 -163.2(3) 5_656 . . . ?
V1 O1 C1 C2 108.2(3) . . . . ?
V1 O1 C1 C2 -82.3(3) 5_656 . . . ?
O1 C1 C2 C3 172.1(3) . . . . ?
C10 C5 C6 C7 3.6(6) . . . . ?
N1 C5 C6 C7 -176.0(4) . . . . ?
C5 C6 C7 C8 -0.6(7) . . . . ?
C6 C7 C8 C9 -2.5(7) . . . . ?
C6 C7 C8 C11 175.2(5) . . . . ?
C7 C8 C9 C10 2.8(7) . . . . ?
C11 C8 C9 C10 -174.9(4) . . . . ?
C8 C9 C10 C5 0.1(7) . . . . ?
C6 C5 C10 C9 -3.4(6) . . . . ?
N1 C5 C10 C9 176.2(4) . . . . ?
V1 O2 C12 C17 -70.6(4) . . . . ?
V1 O2 C12 C13 111.0(4) . . . . ?
O2 C12 C13 C14 -176.7(3) . . . . ?
C17 C12 C13 C14 5.0(6) . . . . ?
O2 C12 C13 C18 5.7(6) . . . . ?
C17 C12 C13 C18 -172.6(4) . . . . ?
C12 C13 C14 C15 -2.5(6) . . . . ?
C18 C13 C14 C15 175.1(4) . . . . ?
C13 C14 C15 C16 -0.9(6) . . . . ?
C13 C14 C15 C22 176.0(4) . . . . ?
C14 C15 C16 C17 2.0(6) . . . . ?
C22 C15 C16 C17 -174.9(4) . . . . ?
C15 C16 C17 C12 0.4(6) . . . . ?
C15 C16 C17 C26 179.6(4) . . . . ?
O2 C12 C17 C16 177.6(3) . . . . ?
C13 C12 C17 C16 -4.1(6) . . . . ?
O2 C12 C17 C26 -1.6(5) . . . . ?
C13 C12 C17 C26 176.8(3) . . . . ?
C14 C13 C18 C19 123.9(4) . . . . ?
C12 C13 C18 C19 -58.6(5) . . . . ?
C14 C13 C18 C20 -114.3(4) . . . . ?
C12 C13 C18 C20 63.2(5) . . . . ?
C14 C13 C18 C21 3.7(6) . . . . ?
C12 C13 C18 C21 -178.8(4) . . . . ?
C16 C15 C22 C24 78.6(5) . . . . ?
C14 C15 C22 C24 -98.1(5) . . . . ?
C16 C15 C22 C25 -41.2(6) . . . . ?
C14 C15 C22 C25 142.1(5) . . . . ?
C16 C15 C22 C23 -162.7(4) . . . . ?
C14 C15 C22 C23 20.6(6) . . . . ?
C16 C17 C26 C33 -80.0(5) . . . . ?
C12 C17 C26 C33 99.2(4) . . . . ?
C16 C17 C26 C27 46.7(5) . . . . ?
C12 C17 C26 C27 -134.1(4) . . . . ?
V1 O3 C28 C33 70.3(4) . . . . ?
V1 O3 C28 C29 -112.4(4) . . . . ?
O3 C28 C29 C30 176.3(4) . . . . ?
C33 C28 C29 C30 -6.5(6) . . . . ?
O3 C28 C29 C34 -6.0(6) . . . . ?
C33 C28 C29 C34 171.2(4) . . . . ?
C28 C29 C30 C31 2.1(6) . . . . ?
C34 C29 C30 C31 -175.6(4) . . . . ?
C29 C30 C31 C32 2.3(7) . . . . ?
C29 C30 C31 C38 -178.0(4) . . . . ?
C30 C31 C32 C33 -2.7(6) . . . . ?
C38 C31 C32 C33 177.6(4) . . . . ?
C31 C32 C33 C28 -1.5(6) . . . . ?
C31 C32 C33 C26 178.6(4) . . . . ?
O3 C28 C33 C32 -176.5(3) . . . . ?
C29 C28 C33 C32 6.3(6) . . . . ?
O3 C28 C33 C26 3.4(6) . . . . ?
C29 C28 C33 C26 -173.8(4) . . . . ?
C17 C26 C33 C32 76.7(5) . . . . ?
C27 C26 C33 C32 -50.3(5) . . . . ?
C17 C26 C33 C28 -103.2(4) . . . . ?
C27 C26 C33 C28 129.8(4) . . . . ?
C30 C29 C34 C35 -123.3(4) . . . . ?
C28 C29 C34 C35 59.1(5) . . . . ?
C30 C29 C34 C37 -3.1(6) . . . . ?
C28 C29 C34 C37 179.3(4) . . . . ?
C30 C29 C34 C36 115.5(4) . . . . ?
C28 C29 C34 C36 -62.1(5) . . . . ?
C32 C31 C38 C40 52.2(6) . . . . ?
C30 C31 C38 C40 -127.5(5) . . . . ?
C32 C31 C38 C41 -68.8(5) . . . . ?
C30 C31 C38 C41 111.6(5) . . . . ?
C32 C31 C38 C39 172.6(4) . . . . ?
C30 C31 C38 C39 -7.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.14
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.056

data_9
_database_code_depnum_ccdc_archive 'CCDC 718359'

_chemical_name_common            'Compound 9'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4CF3)(diphenolate)(mu-OPr)]2.MeCN'
_chemical_formula_moiety         'C80 H110 F6 N2 O6 V2, C2 H3 N'
_chemical_formula_sum            'C82 H113 F6 N3 O6 V2'
_chemical_formula_weight         1452.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   10.5771(10)
_cell_length_b                   10.9292(16)
_cell_length_c                   17.8899(15)
_cell_angle_alpha                100.193(10)
_cell_angle_beta                 94.794(7)
_cell_angle_gamma                96.548(10)
_cell_volume                     2010.7(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    7153
_cell_measurement_theta_min      3.1840
_cell_measurement_theta_max      27.4994

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7923
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26731
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.62
_reflns_number_total             9182
_reflns_number_gt                5674
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
The largest Q peak (2.080 electrons) is located in the disordered solvent
region, 0.78 \%A from C201.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1178P)^2^] where P=(Fo^2^+2Fc^2^)/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         9182
_refine_ls_number_parameters     506
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.1970
_refine_ls_wR_factor_gt          0.1795
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.009
_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 0.91079(5) 0.96543(5) 0.41762(3) 0.01581(16) Uani 1 1 d . . .
N1 N 0.9121(2) 0.8887(2) 0.32786(15) 0.0184(6) Uani 1 1 d . . .
O1 O 1.0717(2) 0.9450(2) 0.46155(12) 0.0172(5) Uani 1 1 d . . .
O3 O 0.8899(2) 1.1203(2) 0.39759(12) 0.0181(5) Uani 1 1 d . . .
O2 O 0.7588(2) 0.88279(19) 0.43727(13) 0.0186(5) Uani 1 1 d . . .
C1 C 1.1741(3) 0.8886(3) 0.42649(19) 0.0195(7) Uani 1 1 d . . .
H1A H 1.2569 0.9372 0.4502 0.023 Uiso 1 1 calc R . .
H1B H 1.1661 0.8933 0.3716 0.023 Uiso 1 1 calc R . .
C2 C 1.1746(3) 0.7530(3) 0.4344(2) 0.0251(8) Uani 1 1 d . . .
H2A H 1.1669 0.7455 0.4883 0.030 Uiso 1 1 calc R . .
H2B H 1.1000 0.7009 0.4025 0.030 Uiso 1 1 calc R . .
C3 C 1.2962(4) 0.7057(4) 0.4101(3) 0.0376(10) Uani 1 1 d . . .
H3A H 1.3049 0.7152 0.3572 0.056 Uiso 1 1 calc R . .
H3B H 1.2930 0.6169 0.4136 0.056 Uiso 1 1 calc R . .
H3C H 1.3697 0.7541 0.4436 0.056 Uiso 1 1 calc R . .
C5 C 0.9006(3) 0.8287(3) 0.25231(19) 0.0206(7) Uani 1 1 d . . .
C6 C 0.8235(4) 0.8710(3) 0.1971(2) 0.0285(8) Uani 1 1 d . . .
H6 H 0.7794 0.9410 0.2115 0.034 Uiso 1 1 calc R . .
C7 C 0.8119(4) 0.8106(4) 0.1215(2) 0.0309(9) Uani 1 1 d . . .
H7 H 0.7604 0.8402 0.0842 0.037 Uiso 1 1 calc R . .
C8 C 0.8745(4) 0.7075(4) 0.0997(2) 0.0283(8) Uani 1 1 d . . .
C11 C 0.8637(4) 0.6448(4) 0.0176(2) 0.0404(10) Uani 1 1 d . . .
F7 F 0.7645(4) 0.6723(4) -0.02382(16) 0.0965(14) Uani 1 1 d . . .
F8 F 0.8527(3) 0.5193(2) 0.00875(15) 0.0621(8) Uani 1 1 d . . .
F9 F 0.9656(3) 0.6742(3) -0.01720(16) 0.0723(9) Uani 1 1 d . . .
C9 C 0.9516(4) 0.6648(4) 0.1541(2) 0.0351(9) Uani 1 1 d . . .
H9 H 0.9949 0.5944 0.1391 0.042 Uiso 1 1 calc R . .
C10 C 0.9653(4) 0.7248(4) 0.2301(2) 0.0322(9) Uani 1 1 d . . .
H10 H 1.0181 0.6957 0.2670 0.039 Uiso 1 1 calc R . .
C12 C 0.6642(3) 0.8309(3) 0.37863(18) 0.0168(6) Uani 1 1 d . . .
C13 C 0.6339(3) 0.6998(3) 0.35519(19) 0.0193(7) Uani 1 1 d . . .
C14 C 0.5479(3) 0.6571(3) 0.28915(19) 0.0224(7) Uani 1 1 d . . .
H14 H 0.5304 0.5693 0.2704 0.027 Uiso 1 1 calc R . .
C15 C 0.4864(3) 0.7369(3) 0.24930(19) 0.0221(7) Uani 1 1 d . . .
C16 C 0.5100(3) 0.8640(3) 0.2791(2) 0.0231(7) Uani 1 1 d . . .
H16 H 0.4648 0.9195 0.2552 0.028 Uiso 1 1 calc R . .
C17 C 0.5979(3) 0.9140(3) 0.34334(19) 0.0195(7) Uani 1 1 d . . .
C18 C 0.6847(3) 0.6064(3) 0.4018(2) 0.0221(7) Uani 1 1 d . . .
C19 C 0.8316(3) 0.6146(3) 0.4057(2) 0.0304(8) Uani 1 1 d . . .
H19A H 0.8704 0.6989 0.4313 0.046 Uiso 1 1 calc R . .
H19B H 0.8571 0.5971 0.3538 0.046 Uiso 1 1 calc R . .
H19C H 0.8608 0.5528 0.4345 0.046 Uiso 1 1 calc R . .
C20 C 0.6438(4) 0.6361(3) 0.4828(2) 0.0289(8) Uani 1 1 d . . .
H20A H 0.6730 0.5757 0.5126 0.043 Uiso 1 1 calc R . .
H20B H 0.5503 0.6304 0.4799 0.043 Uiso 1 1 calc R . .
H20C H 0.6819 0.7211 0.5075 0.043 Uiso 1 1 calc R . .
C21 C 0.6309(4) 0.4697(3) 0.3673(2) 0.0359(10) Uani 1 1 d . . .
H21A H 0.6617 0.4146 0.4005 0.054 Uiso 1 1 calc R . .
H21B H 0.6595 0.4468 0.3166 0.054 Uiso 1 1 calc R . .
H21C H 0.5372 0.4605 0.3629 0.054 Uiso 1 1 calc R . .
C22 C 0.3965(4) 0.6829(3) 0.1757(2) 0.0293(8) Uani 1 1 d . . .
C23 C 0.3029(4) 0.5712(4) 0.1878(2) 0.0391(10) Uani 1 1 d . . .
H23A H 0.2605 0.5960 0.2338 0.059 Uiso 1 1 calc R . .
H23B H 0.3501 0.5009 0.1940 0.059 Uiso 1 1 calc R . .
H23C H 0.2385 0.5457 0.1435 0.059 Uiso 1 1 calc R . .
C24 C 0.4773(4) 0.6385(5) 0.1110(2) 0.0505(12) Uani 1 1 d . . .
H24A H 0.4207 0.6032 0.0641 0.076 Uiso 1 1 calc R . .
H24B H 0.5270 0.5742 0.1253 0.076 Uiso 1 1 calc R . .
H24C H 0.5357 0.7098 0.1025 0.076 Uiso 1 1 calc R . .
C25 C 0.3165(5) 0.7790(4) 0.1511(3) 0.0554(14) Uani 1 1 d . . .
H25A H 0.3728 0.8470 0.1371 0.083 Uiso 1 1 calc R . .
H25B H 0.2698 0.8132 0.1934 0.083 Uiso 1 1 calc R . .
H25C H 0.2554 0.7386 0.1071 0.083 Uiso 1 1 calc R . .
C26 C 0.6213(3) 1.0562(3) 0.3728(2) 0.0199(7) Uani 1 1 d . A .
H26 H 0.6753 1.0715 0.4230 0.024 Uiso 1 1 calc R . .
C27 C 0.4957(3) 1.1107(3) 0.3868(2) 0.0276(8) Uani 1 1 d . . .
H27A H 0.5135 1.2022 0.4014 0.041 Uiso 1 1 calc R . .
H27B H 0.4573 1.0765 0.4280 0.041 Uiso 1 1 calc R . .
H27C H 0.4362 1.0880 0.3401 0.041 Uiso 1 1 calc R . .
C28 C 0.8315(3) 1.1489(3) 0.33248(18) 0.0180(7) Uani 1 1 d . A .
C29 C 0.9036(3) 1.2087(3) 0.2826(2) 0.0231(7) Uani 1 1 d . . .
C30 C 0.8354(3) 1.2312(3) 0.2168(2) 0.0267(8) Uani 1 1 d . A .
H30 H 0.8820 1.2685 0.1816 0.032 Uiso 1 1 calc R . .
C31 C 0.7024(4) 1.2017(3) 0.2000(2) 0.0261(8) Uani 1 1 d . . .
C32 C 0.6362(3) 1.1485(3) 0.2526(2) 0.0228(7) Uani 1 1 d . A .
H32 H 0.5456 1.1306 0.2435 0.027 Uiso 1 1 calc R . .
C33 C 0.6973(3) 1.1203(3) 0.31797(19) 0.0194(7) Uani 1 1 d . . .
C34 C 1.0479(3) 1.2545(4) 0.3011(2) 0.0306(9) Uani 1 1 d D . .
C36 C 1.0681(4) 1.3510(4) 0.3766(3) 0.0489(12) Uani 1 1 d D . .
H36A H 1.0339 1.3120 0.4173 0.073 Uiso 1 1 calc R . .
H36B H 1.0235 1.4229 0.3704 0.073 Uiso 1 1 calc R . .
H36C H 1.1598 1.3794 0.3901 0.073 Uiso 1 1 calc R . .
C35 C 1.1256(4) 1.1457(4) 0.3082(3) 0.0462(12) Uani 1 1 d D . .
H35A H 1.2171 1.1761 0.3123 0.069 Uiso 1 1 calc R . .
H35B H 1.1028 1.0793 0.2630 0.069 Uiso 1 1 calc R . .
H35C H 1.1062 1.1124 0.3540 0.069 Uiso 1 1 calc R . .
C37 C 1.1002(4) 1.3216(5) 0.2394(3) 0.0567(15) Uani 1 1 d D . .
H37A H 1.1919 1.3495 0.2528 0.085 Uiso 1 1 calc R . .
H37B H 1.0553 1.3945 0.2360 0.085 Uiso 1 1 calc R . .
H37C H 1.0865 1.2638 0.1901 0.085 Uiso 1 1 calc R . .
C38 C 0.6366(15) 1.2290(13) 0.1251(11) 0.0356(10) Uani 0.51(2) 1 d PDU A 1
C39 C 0.4899(12) 1.200(2) 0.1194(11) 0.072(5) Uani 0.51(2) 1 d PDU A 1
H39A H 0.4517 1.2341 0.0768 0.108 Uiso 0.51(2) 1 calc PR A 1
H39B H 0.4597 1.2395 0.1671 0.108 Uiso 0.51(2) 1 calc PR A 1
H39C H 0.4649 1.1095 0.1107 0.108 Uiso 0.51(2) 1 calc PR A 1
C40 C 0.6808(18) 1.1444(17) 0.0575(7) 0.065(5) Uani 0.51(2) 1 d PDU A 1
H40A H 0.6493 1.1686 0.0098 0.098 Uiso 0.51(2) 1 calc PR A 1
H40B H 0.6469 1.0569 0.0569 0.098 Uiso 0.51(2) 1 calc PR A 1
H40C H 0.7745 1.1534 0.0623 0.098 Uiso 0.51(2) 1 calc PR A 1
C41 C 0.674(2) 1.3685(12) 0.1232(10) 0.073(5) Uani 0.51(2) 1 d PDU A 1
H41A H 0.7544 1.3787 0.0997 0.110 Uiso 0.51(2) 1 calc PR A 1
H41B H 0.6864 1.4171 0.1754 0.110 Uiso 0.51(2) 1 calc PR A 1
H41C H 0.6066 1.3985 0.0933 0.110 Uiso 0.51(2) 1 calc PR A 1
C38X C 0.6321(16) 1.2245(14) 0.1270(12) 0.0356(10) Uani 0.49(2) 1 d PDU A 2
C39X C 0.5047(15) 1.274(2) 0.1432(8) 0.065(5) Uani 0.49(2) 1 d PDU A 2
H39D H 0.4464 1.2092 0.1584 0.098 Uiso 0.49(2) 1 calc PR A 2
H39E H 0.4659 1.2979 0.0970 0.098 Uiso 0.49(2) 1 calc PR A 2
H39F H 0.5209 1.3482 0.1845 0.098 Uiso 0.49(2) 1 calc PR A 2
C40X C 0.603(2) 1.0995(12) 0.0709(8) 0.064(5) Uani 0.49(2) 1 d PDU A 2
H40D H 0.6815 1.0606 0.0659 0.097 Uiso 0.49(2) 1 calc PR A 2
H40E H 0.5693 1.1141 0.0209 0.097 Uiso 0.49(2) 1 calc PR A 2
H40F H 0.5391 1.0437 0.0899 0.097 Uiso 0.49(2) 1 calc PR A 2
C41X C 0.7101(16) 1.324(2) 0.0925(11) 0.079(6) Uani 0.49(2) 1 d PDU A 2
H41D H 0.7639 1.3834 0.1334 0.118 Uiso 0.49(2) 1 calc PR A 2
H41E H 0.6517 1.3688 0.0654 0.118 Uiso 0.49(2) 1 calc PR A 2
H41F H 0.7644 1.2829 0.0567 0.118 Uiso 0.49(2) 1 calc PR A 2
N200 N 0.0000 0.0000 0.0000 0.087(2) Uani 1 2 d SU . .
C201 C -0.0901(9) 0.0009(9) -0.0535(6) 0.062(3) Uani 0.50 1 d PDU B -1
C202 C -0.2120(7) -0.0717(6) -0.0885(4) 0.0291(16) Uani 0.50 1 d PDU B -1
H20D H -0.2219 -0.1524 -0.0715 0.044 Uiso 0.50 1 calc PR B -1
H20E H -0.2134 -0.0862 -0.1442 0.044 Uiso 0.50 1 calc PR B -1
H20F H -0.2824 -0.0251 -0.0731 0.044 Uiso 0.50 1 calc PR B -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0162(3) 0.0148(3) 0.0155(3) 0.0037(2) -0.0024(2) -0.00034(19)
N1 0.0143(13) 0.0236(14) 0.0169(15) 0.0038(11) -0.0028(11) 0.0033(11)
O1 0.0155(11) 0.0192(11) 0.0162(12) 0.0026(9) -0.0015(9) 0.0026(9)
O3 0.0202(12) 0.0168(11) 0.0166(12) 0.0061(9) -0.0037(9) -0.0011(9)
O2 0.0193(12) 0.0168(11) 0.0183(12) 0.0035(9) -0.0024(9) -0.0002(9)
C1 0.0159(16) 0.0248(16) 0.0178(17) 0.0028(13) 0.0015(13) 0.0049(13)
C2 0.0261(19) 0.0231(17) 0.027(2) 0.0045(14) 0.0068(15) 0.0047(14)
C3 0.033(2) 0.031(2) 0.050(3) 0.0045(18) 0.0103(19) 0.0125(17)
C5 0.0191(17) 0.0245(17) 0.0165(17) 0.0026(13) -0.0014(13) 0.0000(13)
C6 0.036(2) 0.0285(19) 0.022(2) 0.0035(15) 0.0000(16) 0.0105(16)
C7 0.036(2) 0.036(2) 0.021(2) 0.0035(15) -0.0017(16) 0.0109(17)
C8 0.029(2) 0.036(2) 0.0182(19) 0.0005(15) 0.0007(15) 0.0030(16)
C11 0.054(3) 0.040(2) 0.024(2) -0.0033(17) -0.002(2) 0.013(2)
F7 0.124(3) 0.122(3) 0.0340(17) -0.0332(17) -0.0355(18) 0.081(3)
F8 0.105(2) 0.0390(15) 0.0331(15) -0.0088(11) 0.0004(15) -0.0007(15)
F9 0.100(3) 0.072(2) 0.0393(17) -0.0051(14) 0.0338(17) -0.0051(17)
C9 0.038(2) 0.039(2) 0.028(2) -0.0021(17) 0.0016(17) 0.0168(18)
C10 0.033(2) 0.038(2) 0.025(2) 0.0012(16) -0.0043(16) 0.0131(17)
C12 0.0160(16) 0.0188(15) 0.0137(16) 0.0024(12) -0.0012(12) -0.0031(12)
C13 0.0192(17) 0.0165(15) 0.0218(18) 0.0044(13) 0.0012(13) -0.0003(12)
C14 0.0221(18) 0.0187(16) 0.0229(19) 0.0023(13) -0.0036(14) -0.0046(13)
C15 0.0232(18) 0.0213(16) 0.0205(18) 0.0060(13) -0.0026(14) -0.0026(13)
C16 0.0232(18) 0.0209(16) 0.0246(19) 0.0068(14) -0.0037(14) 0.0005(13)
C17 0.0209(17) 0.0171(15) 0.0191(18) 0.0026(12) 0.0006(13) -0.0011(13)
C18 0.0253(18) 0.0170(15) 0.0233(19) 0.0058(13) -0.0028(14) 0.0007(13)
C19 0.026(2) 0.0269(18) 0.041(2) 0.0111(16) 0.0033(17) 0.0076(15)
C20 0.029(2) 0.0277(18) 0.031(2) 0.0134(16) -0.0006(16) -0.0005(15)
C21 0.050(3) 0.0183(17) 0.037(2) 0.0091(16) -0.0089(19) -0.0012(16)
C22 0.032(2) 0.0277(18) 0.024(2) 0.0049(15) -0.0109(16) -0.0067(15)
C23 0.041(2) 0.037(2) 0.031(2) 0.0081(17) -0.0159(18) -0.0161(18)
C24 0.050(3) 0.070(3) 0.025(2) 0.004(2) -0.003(2) -0.008(2)
C25 0.062(3) 0.037(2) 0.056(3) 0.007(2) -0.040(3) -0.003(2)
C26 0.0191(17) 0.0172(15) 0.0223(18) 0.0031(13) -0.0011(13) 0.0011(12)
C27 0.0226(19) 0.0273(18) 0.034(2) 0.0077(15) 0.0039(15) 0.0040(14)
C28 0.0211(17) 0.0160(15) 0.0169(17) 0.0055(12) -0.0033(13) 0.0024(12)
C29 0.0255(19) 0.0197(16) 0.0254(19) 0.0100(14) 0.0004(15) 0.0014(13)
C30 0.030(2) 0.0276(18) 0.024(2) 0.0130(15) 0.0010(15) 0.0005(15)
C31 0.033(2) 0.0238(17) 0.0214(19) 0.0071(14) -0.0058(15) 0.0050(15)
C32 0.0228(18) 0.0189(16) 0.0257(19) 0.0052(13) -0.0058(14) 0.0032(13)
C33 0.0248(18) 0.0130(14) 0.0190(17) 0.0017(12) -0.0019(13) 0.0016(12)
C34 0.0243(19) 0.034(2) 0.037(2) 0.0206(17) 0.0016(16) -0.0019(15)
C36 0.032(2) 0.042(2) 0.066(3) 0.013(2) -0.016(2) -0.0148(19)
C35 0.025(2) 0.050(3) 0.072(3) 0.030(2) 0.011(2) 0.0071(19)
C37 0.032(2) 0.079(4) 0.067(4) 0.050(3) 0.001(2) -0.014(2)
C38 0.044(2) 0.041(2) 0.022(2) 0.0134(17) -0.0102(18) 0.0047(19)
C39 0.049(5) 0.126(13) 0.053(10) 0.051(10) -0.009(6) 0.020(7)
C40 0.074(9) 0.085(9) 0.033(6) -0.001(6) -0.015(6) 0.031(8)
C41 0.130(13) 0.048(6) 0.043(9) 0.031(5) -0.029(8) 0.004(7)
C38X 0.044(2) 0.041(2) 0.022(2) 0.0134(17) -0.0102(18) 0.0047(19)
C39X 0.068(7) 0.103(12) 0.035(7) 0.026(7) -0.014(6) 0.047(8)
C40X 0.098(13) 0.056(6) 0.029(6) -0.002(5) -0.034(7) 0.013(6)
C41X 0.078(9) 0.106(13) 0.051(11) 0.061(9) -0.034(7) -0.037(9)
N200 0.096(4) 0.049(3) 0.137(5) 0.057(3) 0.055(4) 0.005(3)
C201 0.071(5) 0.033(4) 0.071(5) -0.020(3) 0.040(4) -0.011(3)
C202 0.039(3) 0.029(3) 0.031(3) 0.013(3) 0.026(3) 0.026(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.677(3) . ?
V1 O3 1.824(2) . ?
V1 O2 1.844(2) . ?
V1 O1 1.868(2) . ?
V1 O1 2.193(2) 2_776 ?
N1 C5 1.383(4) . ?
O1 C1 1.441(4) . ?
O1 V1 2.193(2) 2_776 ?
O3 C28 1.374(4) . ?
O2 C12 1.381(4) . ?
C1 C2 1.514(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.510(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.403(5) . ?
C5 C10 1.406(5) . ?
C6 C7 1.384(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(5) . ?
C8 C11 1.496(5) . ?
C11 F9 1.325(5) . ?
C11 F7 1.327(5) . ?
C11 F8 1.342(5) . ?
C9 C10 1.389(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 C17 1.411(4) . ?
C12 C13 1.411(4) . ?
C13 C14 1.403(5) . ?
C13 C18 1.542(4) . ?
C14 C15 1.401(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(5) . ?
C15 C22 1.540(5) . ?
C16 C17 1.403(5) . ?
C16 H16 0.9500 . ?
C17 C26 1.534(4) . ?
C18 C21 1.535(5) . ?
C18 C20 1.537(5) . ?
C18 C19 1.542(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.522(6) . ?
C22 C24 1.539(6) . ?
C22 C23 1.539(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C33 1.532(5) . ?
C26 C27 1.538(5) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.410(5) . ?
C28 C29 1.418(5) . ?
C29 C30 1.403(5) . ?
C29 C34 1.541(5) . ?
C30 C31 1.402(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.387(5) . ?
C31 C38X 1.52(2) . ?
C31 C38 1.55(2) . ?
C32 C33 1.388(5) . ?
C32 H32 0.9500 . ?
C34 C37 1.536(5) . ?
C34 C35 1.537(5) . ?
C34 C36 1.542(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.528(13) . ?
C38 C41 1.538(12) . ?
C38 C39 1.538(13) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C38X C40X 1.528(13) . ?
C38X C41X 1.537(13) . ?
C38X C39X 1.541(13) . ?
C39X H39D 0.9800 . ?
C39X H39E 0.9800 . ?
C39X H39F 0.9800 . ?
C40X H40D 0.9800 . ?
C40X H40E 0.9800 . ?
C40X H40F 0.9800 . ?
C41X H41D 0.9800 . ?
C41X H41E 0.9800 . ?
C41X H41F 0.9800 . ?
N200 C201 1.296(12) 2 ?
N200 C201 1.296(12) . ?
C201 C202 1.462(8) . ?
C202 H20D 0.9800 . ?
C202 H20E 0.9800 . ?
C202 H20F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 O3 98.90(12) . . ?
N1 V1 O2 97.48(12) . . ?
O3 V1 O2 111.19(10) . . ?
N1 V1 O1 101.17(11) . . ?
O3 V1 O1 117.14(10) . . ?
O2 V1 O1 124.05(10) . . ?
N1 V1 O1 173.31(11) . 2_776 ?
O3 V1 O1 85.84(9) . 2_776 ?
O2 V1 O1 85.09(9) . 2_776 ?
O1 V1 O1 72.37(10) . 2_776 ?
C5 N1 V1 174.0(2) . . ?
C1 O1 V1 129.58(19) . . ?
C1 O1 V1 122.72(18) . 2_776 ?
V1 O1 V1 107.63(10) . 2_776 ?
C28 O3 V1 127.87(19) . . ?
C12 O2 V1 120.71(19) . . ?
O1 C1 C2 113.0(3) . . ?
O1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
O1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 110.8(3) . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C5 C6 120.0(3) . . ?
N1 C5 C10 120.6(3) . . ?
C6 C5 C10 119.4(3) . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.8(3) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 C11 120.3(3) . . ?
C9 C8 C11 119.9(3) . . ?
F9 C11 F7 106.0(4) . . ?
F9 C11 F8 104.0(3) . . ?
F7 C11 F8 107.2(4) . . ?
F9 C11 C8 113.6(4) . . ?
F7 C11 C8 113.0(3) . . ?
F8 C11 C8 112.5(4) . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C5 119.8(3) . . ?
C9 C10 H10 120.1 . . ?
C5 C10 H10 120.1 . . ?
O2 C12 C17 117.4(3) . . ?
O2 C12 C13 121.5(3) . . ?
C17 C12 C13 121.1(3) . . ?
C14 C13 C12 116.8(3) . . ?
C14 C13 C18 120.7(3) . . ?
C12 C13 C18 122.5(3) . . ?
C15 C14 C13 123.6(3) . . ?
C15 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
C16 C15 C14 117.1(3) . . ?
C16 C15 C22 122.4(3) . . ?
C14 C15 C22 120.4(3) . . ?
C15 C16 C17 122.5(3) . . ?
C15 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C16 C17 C12 118.4(3) . . ?
C16 C17 C26 119.9(3) . . ?
C12 C17 C26 121.7(3) . . ?
C21 C18 C20 107.7(3) . . ?
C21 C18 C19 106.7(3) . . ?
C20 C18 C19 110.0(3) . . ?
C21 C18 C13 112.5(3) . . ?
C20 C18 C13 108.5(3) . . ?
C19 C18 C13 111.4(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C24 108.6(4) . . ?
C25 C22 C23 107.3(3) . . ?
C24 C22 C23 109.3(3) . . ?
C25 C22 C15 112.3(3) . . ?
C24 C22 C15 108.9(3) . . ?
C23 C22 C15 110.4(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C33 C26 C17 109.8(3) . . ?
C33 C26 C27 112.5(3) . . ?
C17 C26 C27 111.8(3) . . ?
C33 C26 H26 107.5 . . ?
C17 C26 H26 107.5 . . ?
C27 C26 H26 107.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 117.9(3) . . ?
O3 C28 C29 121.0(3) . . ?
C33 C28 C29 121.0(3) . . ?
C30 C29 C28 116.6(3) . . ?
C30 C29 C34 120.9(3) . . ?
C28 C29 C34 122.4(3) . . ?
C31 C30 C29 123.7(3) . . ?
C31 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C32 C31 C30 117.1(3) . . ?
C32 C31 C38X 120.6(6) . . ?
C30 C31 C38X 122.2(6) . . ?
C32 C31 C38 123.3(6) . . ?
C30 C31 C38 119.6(6) . . ?
C31 C32 C33 122.5(3) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 H32 118.7 . . ?
C32 C33 C28 119.0(3) . . ?
C32 C33 C26 120.9(3) . . ?
C28 C33 C26 120.2(3) . . ?
C37 C34 C35 108.1(4) . . ?
C37 C34 C29 111.5(3) . . ?
C35 C34 C29 111.8(3) . . ?
C37 C34 C36 107.1(4) . . ?
C35 C34 C36 110.0(3) . . ?
C29 C34 C36 108.3(3) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C41 111.4(12) . . ?
C40 C38 C39 107.2(12) . . ?
C41 C38 C39 109.4(13) . . ?
C40 C38 C31 108.6(11) . . ?
C41 C38 C31 108.0(12) . . ?
C39 C38 C31 112.3(12) . . ?
C31 C38X C40X 108.2(12) . . ?
C31 C38X C41X 111.6(12) . . ?
C40X C38X C41X 111.4(14) . . ?
C31 C38X C39X 110.7(12) . . ?
C40X C38X C39X 108.6(13) . . ?
C41X C38X C39X 106.3(13) . . ?
C38X C39X H39D 109.5 . . ?
C38X C39X H39E 109.5 . . ?
H39D C39X H39E 109.5 . . ?
C38X C39X H39F 109.5 . . ?
H39D C39X H39F 109.5 . . ?
H39E C39X H39F 109.5 . . ?
C38X C40X H40D 109.5 . . ?
C38X C40X H40E 109.5 . . ?
H40D C40X H40E 109.5 . . ?
C38X C40X H40F 109.5 . . ?
H40D C40X H40F 109.5 . . ?
H40E C40X H40F 109.5 . . ?
C38X C41X H41D 109.5 . . ?
C38X C41X H41E 109.5 . . ?
H41D C41X H41E 109.5 . . ?
C38X C41X H41F 109.5 . . ?
H41D C41X H41F 109.5 . . ?
H41E C41X H41F 109.5 . . ?
C201 N200 C201 180.0(14) 2 . ?
N200 C201 C202 139.9(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 5.0(3) . . . . ?
O3 V1 O1 C1 -101.2(2) . . . . ?
O2 V1 O1 C1 112.1(2) . . . . ?
O1 V1 O1 C1 -176.8(3) 2_776 . . . ?
N1 V1 O1 V1 -178.22(12) . . . 2_776 ?
O3 V1 O1 V1 75.62(13) . . . 2_776 ?
O2 V1 O1 V1 -71.15(13) . . . 2_776 ?
O1 V1 O1 V1 0.0 2_776 . . 2_776 ?
N1 V1 O3 C28 27.6(3) . . . . ?
O2 V1 O3 C28 -74.1(3) . . . . ?
O1 V1 O3 C28 135.1(2) . . . . ?
O1 V1 O3 C28 -157.2(3) 2_776 . . . ?
N1 V1 O2 C12 -27.2(2) . . . . ?
O3 V1 O2 C12 75.4(2) . . . . ?
O1 V1 O2 C12 -136.2(2) . . . . ?
O1 V1 O2 C12 159.0(2) 2_776 . . . ?
V1 O1 C1 C2 -96.5(3) . . . . ?
V1 O1 C1 C2 87.2(3) 2_776 . . . ?
O1 C1 C2 C3 -169.5(3) . . . . ?
N1 C5 C6 C7 -179.8(3) . . . . ?
C10 C5 C6 C7 -0.1(5) . . . . ?
C5 C6 C7 C8 0.7(6) . . . . ?
C6 C7 C8 C9 -0.9(6) . . . . ?
C6 C7 C8 C11 -178.6(4) . . . . ?
C7 C8 C11 F9 102.1(5) . . . . ?
C9 C8 C11 F9 -75.6(5) . . . . ?
C7 C8 C11 F7 -18.6(6) . . . . ?
C9 C8 C11 F7 163.7(4) . . . . ?
C7 C8 C11 F8 -140.1(4) . . . . ?
C9 C8 C11 F8 42.2(5) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C11 C8 C9 C10 178.0(4) . . . . ?
C8 C9 C10 C5 0.3(6) . . . . ?
N1 C5 C10 C9 179.3(3) . . . . ?
C6 C5 C10 C9 -0.4(6) . . . . ?
V1 O2 C12 C17 -70.8(3) . . . . ?
V1 O2 C12 C13 109.8(3) . . . . ?
O2 C12 C13 C14 -172.3(3) . . . . ?
C17 C12 C13 C14 8.4(5) . . . . ?
O2 C12 C13 C18 11.6(5) . . . . ?
C17 C12 C13 C18 -167.7(3) . . . . ?
C12 C13 C14 C15 -4.0(5) . . . . ?
C18 C13 C14 C15 172.1(3) . . . . ?
C13 C14 C15 C16 -2.2(5) . . . . ?
C13 C14 C15 C22 178.1(3) . . . . ?
C14 C15 C16 C17 4.4(5) . . . . ?
C22 C15 C16 C17 -175.9(3) . . . . ?
C15 C16 C17 C12 -0.2(5) . . . . ?
C15 C16 C17 C26 179.0(3) . . . . ?
O2 C12 C17 C16 174.1(3) . . . . ?
C13 C12 C17 C16 -6.5(5) . . . . ?
O2 C12 C17 C26 -5.0(5) . . . . ?
C13 C12 C17 C26 174.4(3) . . . . ?
C14 C13 C18 C21 0.1(5) . . . . ?
C12 C13 C18 C21 176.1(3) . . . . ?
C14 C13 C18 C20 -119.0(3) . . . . ?
C12 C13 C18 C20 56.9(4) . . . . ?
C14 C13 C18 C19 119.8(4) . . . . ?
C12 C13 C18 C19 -64.3(4) . . . . ?
C16 C15 C22 C25 -12.7(5) . . . . ?
C14 C15 C22 C25 167.0(4) . . . . ?
C16 C15 C22 C24 107.6(4) . . . . ?
C14 C15 C22 C24 -72.7(4) . . . . ?
C16 C15 C22 C23 -132.4(4) . . . . ?
C14 C15 C22 C23 47.4(5) . . . . ?
C16 C17 C26 C33 -72.3(4) . . . . ?
C12 C17 C26 C33 106.8(4) . . . . ?
C16 C17 C26 C27 53.2(4) . . . . ?
C12 C17 C26 C27 -127.6(3) . . . . ?
V1 O3 C28 C33 71.0(4) . . . . ?
V1 O3 C28 C29 -110.9(3) . . . . ?
O3 C28 C29 C30 178.5(3) . . . . ?
C33 C28 C29 C30 -3.3(5) . . . . ?
O3 C28 C29 C34 -5.0(5) . . . . ?
C33 C28 C29 C34 173.1(3) . . . . ?
C28 C29 C30 C31 2.2(5) . . . . ?
C34 C29 C30 C31 -174.3(3) . . . . ?
C29 C30 C31 C32 0.6(5) . . . . ?
C29 C30 C31 C38X -178.4(7) . . . . ?
C29 C30 C31 C38 -179.3(6) . . . . ?
C30 C31 C32 C33 -2.4(5) . . . . ?
C38X C31 C32 C33 176.7(7) . . . . ?
C38 C31 C32 C33 177.5(6) . . . . ?
C31 C32 C33 C28 1.3(5) . . . . ?
C31 C32 C33 C26 -177.3(3) . . . . ?
O3 C28 C33 C32 179.9(3) . . . . ?
C29 C28 C33 C32 1.8(5) . . . . ?
O3 C28 C33 C26 -1.5(4) . . . . ?
C29 C28 C33 C26 -179.7(3) . . . . ?
C17 C26 C33 C32 82.8(4) . . . . ?
C27 C26 C33 C32 -42.4(4) . . . . ?
C17 C26 C33 C28 -95.7(3) . . . . ?
C27 C26 C33 C28 139.1(3) . . . . ?
C30 C29 C34 C37 -0.8(5) . . . . ?
C28 C29 C34 C37 -177.1(4) . . . . ?
C30 C29 C34 C35 -121.9(4) . . . . ?
C28 C29 C34 C35 61.8(5) . . . . ?
C30 C29 C34 C36 116.7(4) . . . . ?
C28 C29 C34 C36 -59.6(4) . . . . ?
C32 C31 C38 C40 -113.8(12) . . . . ?
C30 C31 C38 C40 66.2(13) . . . . ?
C38X C31 C38 C40 -99(21) . . . . ?
C32 C31 C38 C41 125.3(11) . . . . ?
C30 C31 C38 C41 -54.8(13) . . . . ?
C38X C31 C38 C41 140(21) . . . . ?
C32 C31 C38 C39 4.6(14) . . . . ?
C30 C31 C38 C39 -175.4(11) . . . . ?
C38X C31 C38 C39 20(20) . . . . ?
C32 C31 C38X C40X -77.9(13) . . . . ?
C30 C31 C38X C40X 101.2(12) . . . . ?
C38 C31 C38X C40X 117(21) . . . . ?
C32 C31 C38X C41X 159.2(12) . . . . ?
C30 C31 C38X C41X -21.7(15) . . . . ?
C38 C31 C38X C41X -6(20) . . . . ?
C32 C31 C38X C39X 41.0(15) . . . . ?
C30 C31 C38X C39X -140.0(12) . . . . ?
C38 C31 C38X C39X -124(21) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         2.080
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.098

data_10
_database_code_depnum_ccdc_archive 'CCDC 718360'

_chemical_name_common            'Compound 10'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=NC6H4Cl)(diphenolate)(mu-O-Et)]2.CH2Cl2'
_chemical_formula_moiety         'C76 H106 Cl2 N2 O6 V2, C H2 Cl2'
_chemical_formula_sum            'C77 H108 Cl4 N2 O6 V2'
_chemical_formula_weight         1401.33

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           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   19.0504(18)
_cell_length_b                   19.7366(19)
_cell_length_c                   20.978(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.969(8)
_cell_angle_gamma                90.00
_cell_volume                     7768.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    10491
_cell_measurement_theta_min      3.0259
_cell_measurement_theta_max      24.9999

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8764
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            83922
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1390
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.17
_reflns_number_total             13785
_reflns_number_gt                7264
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/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         13785
_refine_ls_number_parameters     907
_refine_ls_number_restraints     124
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_restrained_S_all      0.872
_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 0.50265(3) 0.86653(2) 0.72943(3) 0.02036(14) Uani 1 1 d . . .
N1 N 0.44998(11) 0.80056(12) 0.73640(11) 0.0206(6) Uani 1 1 d . . .
O1 O 0.45453(9) 0.93537(9) 0.76658(9) 0.0199(5) Uani 1 1 d . . .
O2 O 0.50042(9) 0.86355(9) 0.64213(9) 0.0214(5) Uani 1 1 d . . .
O3 O 0.58731(9) 0.83046(9) 0.77096(9) 0.0201(5) Uani 1 1 d . . .
C1 C 0.38612(14) 0.93273(15) 0.78760(15) 0.0255(8) Uani 1 1 d . . .
H1A H 0.3586 0.8939 0.7665 0.031 Uiso 1 1 calc R . .
H1B H 0.3592 0.9746 0.7736 0.031 Uiso 1 1 calc R . .
C2 C 0.39305(15) 0.92569(17) 0.85974(15) 0.0352(9) Uani 1 1 d . . .
H2A H 0.4139 0.8815 0.8732 0.053 Uiso 1 1 calc R . .
H2B H 0.3458 0.9293 0.8720 0.053 Uiso 1 1 calc R . .
H2C H 0.4240 0.9617 0.8810 0.053 Uiso 1 1 calc R . .
C5 C 0.40730(15) 0.74340(15) 0.73872(15) 0.0228(8) Uani 1 1 d . . .
C6 C 0.35800(15) 0.74043(15) 0.78073(15) 0.0286(8) Uani 1 1 d . . .
H6 H 0.3542 0.7773 0.8091 0.034 Uiso 1 1 calc R . .
C7 C 0.31450(16) 0.68400(16) 0.78139(16) 0.0340(9) Uani 1 1 d . . .
H7 H 0.2807 0.6825 0.8097 0.041 Uiso 1 1 calc R . .
C8 C 0.32051(16) 0.63050(16) 0.74113(17) 0.0322(9) Uani 1 1 d . . .
C9 C 0.36937(16) 0.63182(17) 0.69885(18) 0.0424(10) Uani 1 1 d . . .
H9 H 0.3733 0.5944 0.6711 0.051 Uiso 1 1 calc R . .
C10 C 0.41216(17) 0.68828(16) 0.69772(17) 0.0406(10) Uani 1 1 d . . .
H10 H 0.4453 0.6897 0.6687 0.049 Uiso 1 1 calc R . .
Cl1 Cl 0.26625(4) 0.55962(4) 0.74212(5) 0.0500(3) Uani 1 1 d . . .
C12 C 0.48757(15) 0.80859(15) 0.60114(15) 0.0225(8) Uani 1 1 d . A .
C13 C 0.42491(16) 0.80457(16) 0.55437(15) 0.0273(8) Uani 1 1 d . . .
C14 C 0.41611(18) 0.74683(16) 0.51592(16) 0.0383(10) Uani 1 1 d . A .
H14 H 0.3734 0.7427 0.4852 0.046 Uiso 1 1 calc R . .
C15 C 0.46600(19) 0.69460(16) 0.51958(16) 0.0400(10) Uani 1 1 d . . .
C16 C 0.52838(17) 0.70217(16) 0.56469(15) 0.0326(9) Uani 1 1 d . A .
H16 H 0.5639 0.6680 0.5677 0.039 Uiso 1 1 calc R . .
C17 C 0.54042(15) 0.75812(15) 0.60550(14) 0.0204(7) Uani 1 1 d . . .
C18 C 0.36969(16) 0.86235(16) 0.54315(16) 0.0309(8) Uani 1 1 d . . .
C19 C 0.33389(16) 0.87316(18) 0.60254(17) 0.0472(10) Uani 1 1 d . . .
H19A H 0.3696 0.8879 0.6393 0.071 Uiso 1 1 calc R . .
H19B H 0.3123 0.8306 0.6135 0.071 Uiso 1 1 calc R . .
H19C H 0.2968 0.9079 0.5928 0.071 Uiso 1 1 calc R . .
C20 C 0.40704(16) 0.92778(16) 0.52803(16) 0.0384(9) Uani 1 1 d . . .
H20A H 0.3715 0.9635 0.5163 0.058 Uiso 1 1 calc R . .
H20B H 0.4324 0.9198 0.4919 0.058 Uiso 1 1 calc R . .
H20C H 0.4411 0.9418 0.5663 0.058 Uiso 1 1 calc R . .
C21 C 0.31058(18) 0.84867(18) 0.48485(19) 0.0661(13) Uani 1 1 d . . .
H21A H 0.2792 0.8882 0.4772 0.099 Uiso 1 1 calc R . .
H21B H 0.2828 0.8091 0.4938 0.099 Uiso 1 1 calc R . .
H21C H 0.3320 0.8400 0.4464 0.099 Uiso 1 1 calc R . .
C22 C 0.4537(3) 0.6326(2) 0.4750(2) 0.0603(13) Uani 0.565(6) 1 d PDU A 1
C23 C 0.5272(4) 0.5890(4) 0.4794(4) 0.050(2) Uani 0.565(6) 1 d PDU A 1
H23A H 0.5398 0.5691 0.5227 0.075 Uiso 0.565(6) 1 calc PR A 1
H23B H 0.5658 0.6189 0.4712 0.075 Uiso 0.565(6) 1 calc PR A 1
H23C H 0.5203 0.5528 0.4469 0.075 Uiso 0.565(6) 1 calc PR A 1
C24 C 0.4526(4) 0.6647(3) 0.4006(3) 0.063(3) Uani 0.565(6) 1 d PDU A 1
H24A H 0.4486 0.6277 0.3690 0.095 Uiso 0.565(6) 1 calc PR A 1
H24B H 0.4967 0.6899 0.3998 0.095 Uiso 0.565(6) 1 calc PR A 1
H24C H 0.4117 0.6952 0.3896 0.095 Uiso 0.565(6) 1 calc PR A 1
C25 C 0.3967(4) 0.5948(4) 0.4788(4) 0.066(3) Uani 0.565(6) 1 d PDU A 1
H25A H 0.4001 0.5773 0.5229 0.098 Uiso 0.565(6) 1 calc PR A 1
H25B H 0.3945 0.5568 0.4484 0.098 Uiso 0.565(6) 1 calc PR A 1
H25C H 0.3536 0.6224 0.4678 0.098 Uiso 0.565(6) 1 calc PR A 1
C22X C 0.4537(3) 0.6326(2) 0.4750(2) 0.0603(13) Uani 0.435(6) 1 d PDU A 2
C25X C 0.4422(5) 0.5674(4) 0.5266(4) 0.045(3) Uani 0.435(6) 1 d PDU A 2
H25D H 0.4291 0.5260 0.5015 0.068 Uiso 0.435(6) 1 calc PR A 2
H25E H 0.4042 0.5792 0.5507 0.068 Uiso 0.435(6) 1 calc PR A 2
H25F H 0.4867 0.5598 0.5569 0.068 Uiso 0.435(6) 1 calc PR A 2
C24X C 0.3699(4) 0.6303(5) 0.4367(5) 0.059(3) Uani 0.435(6) 1 d PDU A 2
H24D H 0.3614 0.6683 0.4062 0.089 Uiso 0.435(6) 1 calc PR A 2
H24E H 0.3377 0.6339 0.4682 0.089 Uiso 0.435(6) 1 calc PR A 2
H24F H 0.3612 0.5875 0.4130 0.089 Uiso 0.435(6) 1 calc PR A 2
C23X C 0.5001(5) 0.6191(6) 0.4393(5) 0.061(4) Uani 0.435(6) 1 d PD A 2
H23D H 0.4979 0.6536 0.4054 0.091 Uiso 0.435(6) 1 calc PR A 2
H23E H 0.4900 0.5745 0.4192 0.091 Uiso 0.435(6) 1 calc PR A 2
H23F H 0.5477 0.6189 0.4658 0.091 Uiso 0.435(6) 1 calc PR A 2
C26 C 0.60965(14) 0.76451(15) 0.65421(14) 0.0220(8) Uani 1 1 d . A .
H26 H 0.6159 0.8136 0.6654 0.026 Uiso 1 1 calc R . .
C27 C 0.67538(15) 0.74259(16) 0.62534(15) 0.0334(9) Uani 1 1 d . . .
H27A H 0.6742 0.6934 0.6186 0.050 Uiso 1 1 calc R A .
H27B H 0.7189 0.7549 0.6553 0.050 Uiso 1 1 calc R . .
H27C H 0.6748 0.7655 0.5838 0.050 Uiso 1 1 calc R . .
C28 C 0.59885(14) 0.76122(14) 0.77435(15) 0.0190(7) Uani 1 1 d . A .
C29 C 0.60378(14) 0.72653(15) 0.83406(14) 0.0189(7) Uani 1 1 d . . .
C30 C 0.60872(14) 0.65576(15) 0.83178(15) 0.0225(8) Uani 1 1 d . . .
H30 H 0.6111 0.6314 0.8711 0.027 Uiso 1 1 calc R . .
C31 C 0.61033(14) 0.61863(15) 0.77491(15) 0.0198(7) Uani 1 1 d . . .
C32 C 0.61037(14) 0.65604(15) 0.71849(15) 0.0233(8) Uani 1 1 d . A .
H32 H 0.6134 0.6327 0.6795 0.028 Uiso 1 1 calc R . .
C33 C 0.60603(14) 0.72665(15) 0.71752(15) 0.0204(7) Uani 1 1 d . . .
C34 C 0.60674(15) 0.76289(15) 0.89945(15) 0.0241(8) Uani 1 1 d . . .
C35 C 0.54059(15) 0.80809(16) 0.89972(15) 0.0353(9) Uani 1 1 d . . .
H35A H 0.4973 0.7816 0.8849 0.053 Uiso 1 1 calc R . .
H35B H 0.5423 0.8467 0.8707 0.053 Uiso 1 1 calc R . .
H35C H 0.5403 0.8245 0.9437 0.053 Uiso 1 1 calc R . .
C36 C 0.67385(15) 0.80757(15) 0.91207(15) 0.0313(8) Uani 1 1 d . . .
H36A H 0.6766 0.8305 0.9539 0.047 Uiso 1 1 calc R . .
H36B H 0.6715 0.8414 0.8776 0.047 Uiso 1 1 calc R . .
H36C H 0.7162 0.7792 0.9128 0.047 Uiso 1 1 calc R . .
C37 C 0.60981(17) 0.71257(16) 0.95570(14) 0.0380(9) Uani 1 1 d . . .
H37A H 0.6530 0.6850 0.9590 0.057 Uiso 1 1 calc R . .
H37B H 0.5678 0.6831 0.9478 0.057 Uiso 1 1 calc R . .
H37C H 0.6105 0.7376 0.9962 0.057 Uiso 1 1 calc R . .
C38 C 0.61264(15) 0.54105(15) 0.77673(16) 0.0278(8) Uani 1 1 d D . .
C39 C 0.55269(17) 0.51418(17) 0.81097(18) 0.0483(10) Uani 1 1 d D . .
H39A H 0.5608 0.5298 0.8560 0.072 Uiso 1 1 calc R . .
H39B H 0.5526 0.4645 0.8101 0.072 Uiso 1 1 calc R . .
H39C H 0.5066 0.5311 0.7886 0.072 Uiso 1 1 calc R . .
C40 C 0.6018(2) 0.50984(17) 0.70851(17) 0.0563(11) Uani 1 1 d D . .
H40A H 0.5999 0.4604 0.7118 0.084 Uiso 1 1 calc R . .
H40B H 0.6415 0.5228 0.6870 0.084 Uiso 1 1 calc R . .
H40C H 0.5570 0.5265 0.6832 0.084 Uiso 1 1 calc R . .
C41 C 0.68389(16) 0.51733(16) 0.81449(18) 0.0479(11) Uani 1 1 d D . .
H41A H 0.6925 0.5391 0.8571 0.072 Uiso 1 1 calc R . .
H41B H 0.7221 0.5296 0.7908 0.072 Uiso 1 1 calc R . .
H41C H 0.6830 0.4680 0.8199 0.072 Uiso 1 1 calc R . .
V11 V 0.51368(3) 1.02994(2) 0.76160(3) 0.02019(14) Uani 1 1 d . . .
N11 N 0.56248(11) 1.09678(12) 0.74813(11) 0.0202(6) Uani 1 1 d . . .
O11 O 0.56049(9) 0.96056(9) 0.72445(9) 0.0192(5) Uani 1 1 d . . .
O12 O 0.53026(9) 1.03325(9) 0.85028(9) 0.0224(5) Uani 1 1 d . . .
O13 O 0.42507(9) 1.06487(9) 0.72952(9) 0.0205(5) Uani 1 1 d . . .
C101 C 0.62666(14) 0.96334(15) 0.69993(15) 0.0228(8) Uani 1 1 d . . .
H10A H 0.6495 0.9181 0.7046 0.027 Uiso 1 1 calc R . .
H10B H 0.6592 0.9958 0.7263 0.027 Uiso 1 1 calc R . .
C102 C 0.61654(15) 0.98455(17) 0.62982(15) 0.0374(9) Uani 1 1 d . . .
H10C H 0.5823 0.9541 0.6038 0.056 Uiso 1 1 calc R . .
H10D H 0.6623 0.9822 0.6146 0.056 Uiso 1 1 calc R . .
H10E H 0.5984 1.0311 0.6255 0.056 Uiso 1 1 calc R . .
C105 C 0.59964(15) 1.15615(15) 0.73960(14) 0.0198(7) Uani 1 1 d . . .
C106 C 0.66488(15) 1.15344(15) 0.71776(15) 0.0289(8) Uani 1 1 d . . .
H106 H 0.6828 1.1110 0.7063 0.035 Uiso 1 1 calc R . .
C107 C 0.70357(15) 1.21167(16) 0.71264(15) 0.0294(8) Uani 1 1 d . . .
H107 H 0.7483 1.2094 0.6985 0.035 Uiso 1 1 calc R . .
C108 C 0.67679(15) 1.27325(15) 0.72826(15) 0.0236(8) Uani 1 1 d . . .
C109 C 0.61192(16) 1.27774(16) 0.74865(16) 0.0301(9) Uani 1 1 d . . .
H109 H 0.5941 1.3206 0.7591 0.036 Uiso 1 1 calc R . .
C110 C 0.57275(15) 1.21932(15) 0.75389(15) 0.0263(8) Uani 1 1 d . . .
H110 H 0.5276 1.2222 0.7672 0.032 Uiso 1 1 calc R . .
Cl11 Cl 0.72685(4) 1.34676(4) 0.72462(4) 0.0375(2) Uani 1 1 d . . .
C112 C 0.54887(16) 1.09280(15) 0.88359(14) 0.0217(8) Uani 1 1 d . . .
C113 C 0.61839(16) 1.10332(15) 0.91824(15) 0.0242(8) Uani 1 1 d . . .
C114 C 0.63390(16) 1.16841(16) 0.94323(15) 0.0278(8) Uani 1 1 d . . .
H114 H 0.6811 1.1773 0.9647 0.033 Uiso 1 1 calc R . .
C115 C 0.58417(16) 1.22135(15) 0.93854(15) 0.0248(8) Uani 1 1 d . . .
C116 C 0.51483(16) 1.20575(15) 0.90977(14) 0.0251(8) Uani 1 1 d . . .
H116 H 0.4790 1.2395 0.9084 0.030 Uiso 1 1 calc R . .
C117 C 0.49573(15) 1.14217(15) 0.88272(14) 0.0203(7) Uani 1 1 d . . .
C118 C 0.67456(15) 1.04594(16) 0.93034(16) 0.0278(8) Uani 1 1 d . . .
C119 C 0.69457(16) 1.01972(17) 0.86710(15) 0.0390(9) Uani 1 1 d . . .
H11A H 0.7324 0.9857 0.8769 0.058 Uiso 1 1 calc R . .
H11B H 0.7115 1.0575 0.8435 0.058 Uiso 1 1 calc R . .
H11C H 0.6526 0.9992 0.8404 0.058 Uiso 1 1 calc R . .
C120 C 0.64341(17) 0.98784(16) 0.96578(16) 0.0396(9) Uani 1 1 d . . .
H12A H 0.6010 0.9696 0.9380 0.059 Uiso 1 1 calc R . .
H12B H 0.6304 1.0051 1.0060 0.059 Uiso 1 1 calc R . .
H12C H 0.6791 0.9519 0.9759 0.059 Uiso 1 1 calc R . .
C121 C 0.74401(16) 1.06975(16) 0.97424(16) 0.0416(10) Uani 1 1 d . . .
H12D H 0.7780 1.0321 0.9812 0.062 Uiso 1 1 calc R . .
H12E H 0.7332 1.0848 1.0160 0.062 Uiso 1 1 calc R . .
H12F H 0.7648 1.1074 0.9533 0.062 Uiso 1 1 calc R . .
C122 C 0.60742(16) 1.29221(16) 0.96466(16) 0.0287(8) Uani 1 1 d . . .
C123 C 0.67051(16) 1.31690(16) 0.93411(17) 0.0399(9) Uani 1 1 d . . .
H12G H 0.6567 1.3176 0.8869 0.060 Uiso 1 1 calc R . .
H12H H 0.7110 1.2861 0.9462 0.060 Uiso 1 1 calc R . .
H12I H 0.6841 1.3626 0.9497 0.060 Uiso 1 1 calc R . .
C124 C 0.54705(16) 1.34421(15) 0.94869(18) 0.0425(10) Uani 1 1 d . . .
H12J H 0.5640 1.3887 0.9653 0.064 Uiso 1 1 calc R . .
H12K H 0.5066 1.3303 0.9689 0.064 Uiso 1 1 calc R . .
H12L H 0.5319 1.3468 0.9017 0.064 Uiso 1 1 calc R . .
C125 C 0.63084(17) 1.28862(18) 1.03886(16) 0.0467(10) Uani 1 1 d . . .
H12M H 0.6481 1.3332 1.0553 0.070 Uiso 1 1 calc R . .
H12N H 0.6691 1.2552 1.0495 0.070 Uiso 1 1 calc R . .
H12O H 0.5902 1.2753 1.0589 0.070 Uiso 1 1 calc R . .
C126 C 0.41860(14) 1.12885(15) 0.85020(14) 0.0210(7) Uani 1 1 d . . .
H126 H 0.4145 1.0793 0.8405 0.025 Uiso 1 1 calc R . .
C127 C 0.36556(15) 1.14503(16) 0.89598(15) 0.0311(8) Uani 1 1 d . . .
H12P H 0.3681 1.1934 0.9068 0.047 Uiso 1 1 calc R . .
H12Q H 0.3778 1.1183 0.9357 0.047 Uiso 1 1 calc R . .
H12R H 0.3171 1.1337 0.8745 0.047 Uiso 1 1 calc R . .
C128 C 0.40552(14) 1.13279(15) 0.72694(15) 0.0204(7) Uani 1 1 d . . .
C129 C 0.38875(14) 1.16697(15) 0.66681(15) 0.0227(8) Uani 1 1 d . . .
C130 C 0.37134(14) 1.23588(15) 0.66931(16) 0.0274(8) Uani 1 1 d . . .
H130 H 0.3614 1.2601 0.6296 0.033 Uiso 1 1 calc R . .
C131 C 0.36764(15) 1.27104(15) 0.72595(16) 0.0239(8) Uani 1 1 d . . .
C132 C 0.38191(14) 1.23427(15) 0.78338(16) 0.0246(8) Uani 1 1 d . . .
H132 H 0.3786 1.2567 0.8228 0.030 Uiso 1 1 calc R . .
C133 C 0.40087(14) 1.16607(15) 0.78556(15) 0.0209(8) Uani 1 1 d . . .
C134 C 0.38353(15) 1.13036(16) 0.60113(15) 0.0278(8) Uani 1 1 d . . .
C135 C 0.32398(15) 1.07685(17) 0.59628(16) 0.0378(9) Uani 1 1 d . . .
H13A H 0.2798 1.0985 0.6035 0.057 Uiso 1 1 calc R . .
H13B H 0.3378 1.0418 0.6291 0.057 Uiso 1 1 calc R . .
H13C H 0.3165 1.0562 0.5531 0.057 Uiso 1 1 calc R . .
C136 C 0.36436(18) 1.17885(17) 0.54315(16) 0.0499(11) Uani 1 1 d . . .
H13D H 0.3606 1.1531 0.5027 0.075 Uiso 1 1 calc R . .
H13E H 0.4016 1.2133 0.5447 0.075 Uiso 1 1 calc R . .
H13F H 0.3187 1.2009 0.5451 0.075 Uiso 1 1 calc R . .
C137 C 0.45517(15) 1.09707(16) 0.59341(15) 0.0368(9) Uani 1 1 d . . .
H13G H 0.4657 1.0597 0.6244 0.055 Uiso 1 1 calc R . .
H13H H 0.4934 1.1309 0.6017 0.055 Uiso 1 1 calc R . .
H13I H 0.4518 1.0796 0.5493 0.055 Uiso 1 1 calc R . .
C138 C 0.35119(16) 1.34738(15) 0.72661(17) 0.0307(9) Uani 1 1 d . . .
C139 C 0.42068(17) 1.38602(17) 0.7420(2) 0.0633(13) Uani 1 1 d . . .
H13J H 0.4493 1.3773 0.7083 0.095 Uiso 1 1 calc R . .
H13K H 0.4470 1.3712 0.7840 0.095 Uiso 1 1 calc R . .
H13L H 0.4107 1.4346 0.7436 0.095 Uiso 1 1 calc R . .
C140 C 0.30553(19) 1.36359(18) 0.77843(19) 0.0603(12) Uani 1 1 d . . .
H14A H 0.3330 1.3539 0.8214 0.090 Uiso 1 1 calc R . .
H14B H 0.2624 1.3356 0.7711 0.090 Uiso 1 1 calc R . .
H14C H 0.2921 1.4116 0.7757 0.090 Uiso 1 1 calc R . .
C141 C 0.30921(19) 1.37135(17) 0.66144(18) 0.0567(11) Uani 1 1 d . . .
H14D H 0.2965 1.4192 0.6646 0.085 Uiso 1 1 calc R . .
H14E H 0.2657 1.3442 0.6503 0.085 Uiso 1 1 calc R . .
H14F H 0.3386 1.3659 0.6278 0.085 Uiso 1 1 calc R . .
C201 C 0.6559(5) 0.5190(8) 1.0781(5) 0.112(5) Uani 0.536(10) 1 d PDU B 1
H20D H 0.6722 0.5621 1.1000 0.135 Uiso 0.536(10) 1 calc PR B 1
H20E H 0.6926 0.4836 1.0904 0.135 Uiso 0.536(10) 1 calc PR B 1
Cl21 Cl 0.5747(3) 0.4946(4) 1.0947(3) 0.112(2) Uani 0.536(10) 1 d PDU B 1
Cl22 Cl 0.6367(5) 0.5281(4) 1.0018(4) 0.174(3) Uani 0.536(10) 1 d PDU B 1
C202 C 0.6083(13) 0.5277(9) 1.0542(8) 0.170(8) Uani 0.464(10) 1 d PDU B 2
H20F H 0.5585 0.5354 1.0325 0.204 Uiso 0.464(10) 1 calc PR B 2
H20G H 0.6249 0.5703 1.0768 0.204 Uiso 0.464(10) 1 calc PR B 2
Cl23 Cl 0.6064(5) 0.4642(3) 1.1148(3) 0.122(2) Uani 0.464(10) 1 d PDU B 2
Cl24 Cl 0.6600(2) 0.5148(2) 0.9929(2) 0.0489(13) Uani 0.464(10) 1 d PDU B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0230(3) 0.0183(3) 0.0200(3) -0.0020(3) 0.0044(2) 0.0004(2)
N1 0.0179(14) 0.0196(15) 0.0240(16) -0.0037(13) 0.0027(12) 0.0006(12)
O1 0.0162(11) 0.0189(12) 0.0261(13) -0.0024(10) 0.0079(9) -0.0002(9)
O2 0.0267(12) 0.0202(12) 0.0159(12) -0.0038(10) -0.0005(9) -0.0009(9)
O3 0.0243(12) 0.0162(12) 0.0201(13) -0.0007(10) 0.0044(10) 0.0016(9)
C1 0.0216(18) 0.0212(19) 0.037(2) -0.0029(17) 0.0139(16) -0.0022(14)
C2 0.032(2) 0.041(2) 0.037(2) -0.0073(19) 0.0171(17) -0.0062(16)
C5 0.0207(18) 0.0211(19) 0.026(2) 0.0013(16) 0.0015(16) 0.0002(15)
C6 0.036(2) 0.023(2) 0.029(2) -0.0053(17) 0.0115(17) -0.0048(16)
C7 0.036(2) 0.029(2) 0.042(2) 0.0024(19) 0.0194(18) -0.0054(17)
C8 0.030(2) 0.020(2) 0.046(2) 0.0017(19) 0.0028(17) -0.0040(16)
C9 0.045(2) 0.023(2) 0.064(3) -0.019(2) 0.021(2) -0.0111(18)
C10 0.043(2) 0.029(2) 0.056(3) -0.011(2) 0.0268(19) -0.0065(18)
Cl1 0.0421(6) 0.0267(5) 0.0829(8) 0.0022(5) 0.0158(5) -0.0129(4)
C12 0.029(2) 0.0196(19) 0.0188(19) -0.0025(16) 0.0048(15) -0.0042(15)
C13 0.031(2) 0.024(2) 0.024(2) -0.0012(17) -0.0042(16) 0.0012(15)
C14 0.050(2) 0.025(2) 0.033(2) -0.0031(18) -0.0133(18) 0.0006(18)
C15 0.066(3) 0.020(2) 0.028(2) -0.0024(18) -0.009(2) 0.0056(19)
C16 0.052(2) 0.024(2) 0.021(2) 0.0019(17) 0.0021(18) 0.0137(17)
C17 0.0275(19) 0.0208(19) 0.0137(18) 0.0025(15) 0.0059(15) 0.0030(15)
C18 0.031(2) 0.028(2) 0.030(2) -0.0066(18) -0.0065(17) 0.0052(16)
C19 0.036(2) 0.050(3) 0.058(3) 0.010(2) 0.015(2) 0.0083(18)
C20 0.050(2) 0.033(2) 0.032(2) 0.0003(19) 0.0075(18) 0.0143(18)
C21 0.053(3) 0.059(3) 0.071(3) -0.022(2) -0.033(2) 0.018(2)
C22 0.086(3) 0.030(2) 0.050(3) -0.015(2) -0.031(3) 0.020(2)
C23 0.074(5) 0.032(5) 0.040(5) -0.022(4) 0.001(4) 0.007(4)
C24 0.112(7) 0.037(5) 0.035(4) -0.020(3) -0.005(4) 0.018(4)
C25 0.072(6) 0.038(5) 0.086(8) -0.024(5) 0.011(6) 0.001(5)
C22X 0.086(3) 0.030(2) 0.050(3) -0.015(2) -0.031(3) 0.020(2)
C25X 0.055(6) 0.033(5) 0.044(6) -0.009(4) -0.002(5) 0.002(4)
C24X 0.068(6) 0.036(5) 0.062(7) -0.034(5) -0.025(5) 0.003(5)
C23X 0.073(9) 0.060(9) 0.053(9) -0.026(7) 0.022(8) -0.027(7)
C26 0.0235(19) 0.0241(19) 0.0200(19) 0.0010(16) 0.0080(15) 0.0070(14)
C27 0.038(2) 0.039(2) 0.027(2) 0.0058(18) 0.0159(17) 0.0074(16)
C28 0.0175(18) 0.0173(18) 0.023(2) -0.0026(16) 0.0055(14) 0.0027(14)
C29 0.0190(17) 0.0216(19) 0.0167(19) -0.0005(16) 0.0048(14) 0.0002(14)
C30 0.0234(18) 0.0236(19) 0.020(2) 0.0036(16) 0.0030(15) -0.0016(14)
C31 0.0197(18) 0.0199(19) 0.020(2) -0.0031(16) 0.0041(14) 0.0002(14)
C32 0.0231(18) 0.025(2) 0.021(2) -0.0057(17) 0.0040(15) 0.0012(14)
C33 0.0209(18) 0.022(2) 0.018(2) 0.0016(16) 0.0047(14) 0.0014(14)
C34 0.0270(19) 0.0245(19) 0.021(2) -0.0005(16) 0.0042(15) 0.0012(15)
C35 0.038(2) 0.045(2) 0.023(2) -0.0048(18) 0.0084(17) 0.0033(17)
C36 0.039(2) 0.031(2) 0.023(2) -0.0039(17) 0.0015(16) 0.0023(16)
C37 0.063(2) 0.036(2) 0.016(2) 0.0014(18) 0.0112(18) 0.0000(18)
C38 0.032(2) 0.020(2) 0.030(2) -0.0015(17) 0.0020(17) -0.0001(15)
C39 0.052(2) 0.033(2) 0.060(3) -0.001(2) 0.010(2) -0.0155(18)
C40 0.100(3) 0.025(2) 0.043(3) -0.008(2) 0.010(2) 0.001(2)
C41 0.046(2) 0.026(2) 0.069(3) 0.002(2) 0.002(2) 0.0048(17)
V11 0.0236(3) 0.0184(3) 0.0189(3) -0.0012(3) 0.0043(2) -0.0002(2)
N11 0.0183(14) 0.0218(15) 0.0194(16) 0.0003(12) 0.0006(12) 0.0003(11)
O11 0.0194(11) 0.0182(12) 0.0210(13) -0.0012(10) 0.0064(9) 0.0018(9)
O12 0.0286(12) 0.0201(12) 0.0180(13) -0.0036(11) 0.0027(10) -0.0012(10)
O13 0.0237(12) 0.0174(12) 0.0206(13) -0.0031(10) 0.0042(10) 0.0021(9)
C101 0.0173(17) 0.0231(19) 0.030(2) -0.0027(17) 0.0089(15) 0.0006(14)
C102 0.032(2) 0.050(2) 0.033(2) 0.000(2) 0.0104(17) -0.0030(17)
C105 0.0181(18) 0.0238(19) 0.0167(19) -0.0004(15) 0.0007(14) -0.0029(14)
C106 0.0265(19) 0.0193(19) 0.043(2) -0.0023(17) 0.0104(17) 0.0012(15)
C107 0.0202(18) 0.033(2) 0.037(2) 0.0004(18) 0.0085(16) -0.0032(16)
C108 0.0261(19) 0.0184(19) 0.025(2) 0.0039(16) -0.0005(16) -0.0077(15)
C109 0.033(2) 0.0172(19) 0.042(2) -0.0020(17) 0.0110(18) -0.0018(15)
C110 0.0243(19) 0.025(2) 0.032(2) -0.0016(17) 0.0118(16) -0.0002(15)
Cl11 0.0355(5) 0.0256(5) 0.0529(6) -0.0012(5) 0.0118(4) -0.0116(4)
C112 0.029(2) 0.0198(19) 0.0167(19) -0.0008(15) 0.0060(15) -0.0031(15)
C113 0.029(2) 0.0236(19) 0.020(2) 0.0016(16) 0.0034(15) -0.0006(15)
C114 0.029(2) 0.034(2) 0.020(2) 0.0002(17) 0.0021(16) -0.0037(16)
C115 0.031(2) 0.023(2) 0.022(2) -0.0031(16) 0.0080(16) -0.0045(15)
C116 0.031(2) 0.023(2) 0.024(2) -0.0015(16) 0.0118(16) 0.0005(15)
C117 0.0242(18) 0.0221(19) 0.0150(18) 0.0030(15) 0.0043(14) -0.0024(15)
C118 0.0279(19) 0.030(2) 0.024(2) 0.0015(16) -0.0003(16) 0.0000(16)
C119 0.040(2) 0.045(2) 0.031(2) 0.001(2) 0.0057(17) 0.0140(17)
C120 0.052(2) 0.030(2) 0.036(2) 0.0043(18) 0.0026(18) 0.0034(17)
C121 0.043(2) 0.035(2) 0.042(3) 0.0007(19) -0.0067(19) 0.0103(17)
C122 0.031(2) 0.024(2) 0.031(2) -0.0100(17) 0.0057(16) -0.0085(16)
C123 0.043(2) 0.032(2) 0.048(3) -0.0115(19) 0.0181(19) -0.0106(17)
C124 0.041(2) 0.025(2) 0.065(3) -0.015(2) 0.018(2) -0.0065(17)
C125 0.059(3) 0.046(3) 0.036(3) -0.011(2) 0.0106(19) -0.0143(19)
C126 0.0255(18) 0.0188(18) 0.0198(19) -0.0042(16) 0.0070(15) -0.0011(14)
C127 0.0288(19) 0.036(2) 0.031(2) -0.0038(18) 0.0113(16) -0.0032(15)
C128 0.0150(17) 0.0211(19) 0.025(2) -0.0018(17) 0.0040(14) -0.0001(14)
C129 0.0201(18) 0.025(2) 0.023(2) -0.0028(17) 0.0009(15) -0.0009(14)
C130 0.028(2) 0.027(2) 0.025(2) 0.0041(17) -0.0010(16) 0.0028(15)
C131 0.0247(19) 0.0170(19) 0.030(2) -0.0032(17) 0.0039(16) 0.0018(14)
C132 0.0231(19) 0.026(2) 0.025(2) -0.0042(17) 0.0049(15) 0.0001(14)
C133 0.0200(18) 0.0179(19) 0.025(2) -0.0032(16) 0.0056(15) -0.0008(14)
C134 0.032(2) 0.027(2) 0.021(2) -0.0019(17) -0.0028(16) 0.0058(16)
C135 0.033(2) 0.043(2) 0.034(2) -0.0149(19) -0.0021(17) 0.0038(17)
C136 0.077(3) 0.042(2) 0.027(2) -0.002(2) -0.001(2) 0.013(2)
C137 0.041(2) 0.046(2) 0.024(2) -0.0077(18) 0.0092(17) 0.0038(17)
C138 0.030(2) 0.021(2) 0.041(2) -0.0041(18) 0.0030(18) 0.0032(15)
C139 0.046(2) 0.024(2) 0.115(4) -0.007(2) -0.002(2) -0.0068(18)
C140 0.078(3) 0.033(2) 0.074(3) -0.004(2) 0.025(2) 0.024(2)
C141 0.084(3) 0.028(2) 0.052(3) 0.000(2) -0.004(2) 0.021(2)
C201 0.040(6) 0.192(13) 0.105(8) -0.085(9) 0.010(6) -0.030(7)
Cl21 0.060(3) 0.164(5) 0.124(4) -0.059(4) 0.048(2) -0.016(2)
Cl22 0.193(6) 0.142(5) 0.168(5) 0.096(4) -0.020(4) -0.076(4)
C202 0.27(2) 0.192(15) 0.061(12) -0.002(9) 0.052(12) 0.084(18)
Cl23 0.151(5) 0.152(4) 0.079(3) -0.009(3) 0.062(3) 0.067(4)
Cl24 0.067(2) 0.0415(19) 0.040(2) -0.0147(16) 0.0120(14) -0.0132(14)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N1 1.666(2) . ?
V1 O2 1.8255(19) . ?
V1 O3 1.8386(18) . ?
V1 O1 1.8818(19) . ?
V1 O11 2.1701(19) . ?
N1 C5 1.396(3) . ?
O1 C1 1.447(3) . ?
O1 V11 2.1921(19) . ?
O2 C12 1.380(3) . ?
O3 C28 1.384(3) . ?
C1 C2 1.503(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C5 C6 1.396(4) . ?
C5 C10 1.400(4) . ?
C6 C7 1.390(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.369(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(4) . ?
C8 Cl1 1.742(3) . ?
C9 C10 1.383(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 C17 1.408(4) . ?
C12 C13 1.410(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.542(4) . ?
C14 C15 1.395(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(4) . ?
C15 C22 1.534(5) . ?
C16 C17 1.392(4) . ?
C16 H16 0.9500 . ?
C17 C26 1.527(4) . ?
C18 C20 1.534(4) . ?
C18 C19 1.535(4) . ?
C18 C21 1.536(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.331(7) . ?
C22 C23 1.632(7) . ?
C22 C24 1.681(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25X H25D 0.9800 . ?
C25X H25E 0.9800 . ?
C25X H25F 0.9800 . ?
C24X H24D 0.9800 . ?
C24X H24E 0.9800 . ?
C24X H24F 0.9800 . ?
C23X H23D 0.9800 . ?
C23X H23E 0.9800 . ?
C23X H23F 0.9800 . ?
C26 C33 1.536(4) . ?
C26 C27 1.544(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.401(4) . ?
C28 C29 1.416(4) . ?
C29 C30 1.401(4) . ?
C29 C34 1.540(4) . ?
C30 C31 1.405(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(4) . ?
C31 C38 1.532(4) . ?
C32 C33 1.396(4) . ?
C32 H32 0.9500 . ?
C34 C37 1.536(4) . ?
C34 C36 1.538(4) . ?
C34 C35 1.545(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C41 1.522(4) . ?
C38 C40 1.539(4) . ?
C38 C39 1.544(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
V11 N11 1.666(2) . ?
V11 O12 1.8335(19) . ?
V11 O13 1.8395(18) . ?
V11 O11 1.8757(18) . ?
N11 C105 1.397(3) . ?
O11 C101 1.443(3) . ?
O12 C112 1.382(3) . ?
O13 C128 1.390(3) . ?
C101 C102 1.509(4) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C105 C106 1.398(4) . ?
C105 C110 1.400(4) . ?
C106 C107 1.380(4) . ?
C106 H106 0.9500 . ?
C107 C108 1.379(4) . ?
C107 H107 0.9500 . ?
C108 C109 1.379(4) . ?
C108 Cl11 1.745(3) . ?
C109 C110 1.388(4) . ?
C109 H109 0.9500 . ?
C110 H110 0.9500 . ?
C112 C117 1.403(4) . ?
C112 C113 1.411(4) . ?
C113 C114 1.400(4) . ?
C113 C118 1.549(4) . ?
C114 C115 1.402(4) . ?
C114 H114 0.9500 . ?
C115 C116 1.388(4) . ?
C115 C122 1.539(4) . ?
C116 C117 1.399(4) . ?
C116 H116 0.9500 . ?
C117 C126 1.532(4) . ?
C118 C119 1.532(4) . ?
C118 C120 1.540(4) . ?
C118 C121 1.548(4) . ?
C119 H11A 0.9800 . ?
C119 H11B 0.9800 . ?
C119 H11C 0.9800 . ?
C120 H12A 0.9800 . ?
C120 H12B 0.9800 . ?
C120 H12C 0.9800 . ?
C121 H12D 0.9800 . ?
C121 H12E 0.9800 . ?
C121 H12F 0.9800 . ?
C122 C124 1.534(4) . ?
C122 C123 1.536(4) . ?
C122 C125 1.545(4) . ?
C123 H12G 0.9800 . ?
C123 H12H 0.9800 . ?
C123 H12I 0.9800 . ?
C124 H12J 0.9800 . ?
C124 H12K 0.9800 . ?
C124 H12L 0.9800 . ?
C125 H12M 0.9800 . ?
C125 H12N 0.9800 . ?
C125 H12O 0.9800 . ?
C126 C133 1.528(4) . ?
C126 C127 1.543(4) . ?
C126 H126 1.0000 . ?
C127 H12P 0.9800 . ?
C127 H12Q 0.9800 . ?
C127 H12R 0.9800 . ?
C128 C133 1.410(4) . ?
C128 C129 1.417(4) . ?
C129 C130 1.403(4) . ?
C129 C134 1.544(4) . ?
C130 C131 1.388(4) . ?
C130 H130 0.9500 . ?
C131 C132 1.392(4) . ?
C131 C138 1.539(4) . ?
C132 C133 1.392(4) . ?
C132 H132 0.9500 . ?
C134 C135 1.540(4) . ?
C134 C136 1.541(4) . ?
C134 C137 1.548(4) . ?
C135 H13A 0.9800 . ?
C135 H13B 0.9800 . ?
C135 H13C 0.9800 . ?
C136 H13D 0.9800 . ?
C136 H13E 0.9800 . ?
C136 H13F 0.9800 . ?
C137 H13G 0.9800 . ?
C137 H13H 0.9800 . ?
C137 H13I 0.9800 . ?
C138 C139 1.513(4) . ?
C138 C141 1.534(4) . ?
C138 C140 1.539(4) . ?
C139 H13J 0.9800 . ?
C139 H13K 0.9800 . ?
C139 H13L 0.9800 . ?
C140 H14A 0.9800 . ?
C140 H14B 0.9800 . ?
C140 H14C 0.9800 . ?
C141 H14D 0.9800 . ?
C141 H14E 0.9800 . ?
C141 H14F 0.9800 . ?
C201 Cl22 1.588(10) . ?
C201 Cl21 1.712(9) . ?
C201 H20D 0.9900 . ?
C201 H20E 0.9900 . ?
C202 Cl24 1.767(13) . ?
C202 Cl23 1.790(14) . ?
C202 H20F 0.9900 . ?
C202 H20G 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
N1 V1 O2 98.81(10) . . ?
N1 V1 O3 98.51(10) . . ?
O2 V1 O3 109.21(8) . . ?
N1 V1 O1 100.61(10) . . ?
O2 V1 O1 120.68(9) . . ?
O3 V1 O1 122.25(9) . . ?
N1 V1 O11 172.48(10) . . ?
O2 V1 O11 84.44(8) . . ?
O3 V1 O11 86.72(7) . . ?
O1 V1 O11 71.95(7) . . ?
C5 N1 V1 176.3(2) . . ?
C1 O1 V1 128.98(17) . . ?
C1 O1 V11 122.87(16) . . ?
V1 O1 V11 107.68(8) . . ?
C12 O2 V1 128.43(18) . . ?
C28 O3 V1 121.68(16) . . ?
O1 C1 C2 112.5(2) . . ?
O1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C6 C5 N1 121.0(3) . . ?
C6 C5 C10 118.6(3) . . ?
N1 C5 C10 120.4(3) . . ?
C7 C6 C5 120.5(3) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 119.9(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 121.0(3) . . ?
C7 C8 Cl1 119.9(3) . . ?
C9 C8 Cl1 119.1(3) . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C5 120.9(3) . . ?
C9 C10 H10 119.5 . . ?
C5 C10 H10 119.5 . . ?
O2 C12 C17 117.9(3) . . ?
O2 C12 C13 121.0(3) . . ?
C17 C12 C13 121.0(3) . . ?
C14 C13 C12 116.9(3) . . ?
C14 C13 C18 120.5(3) . . ?
C12 C13 C18 122.5(3) . . ?
C13 C14 C15 124.2(3) . . ?
C13 C14 H14 117.9 . . ?
C15 C14 H14 117.9 . . ?
C16 C15 C14 116.8(3) . . ?
C16 C15 C22 121.4(3) . . ?
C14 C15 C22 121.7(3) . . ?
C17 C16 C15 122.2(3) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C12 118.8(3) . . ?
C16 C17 C26 120.6(3) . . ?
C12 C17 C26 120.7(3) . . ?
C20 C18 C19 109.8(3) . . ?
C20 C18 C21 106.6(3) . . ?
C19 C18 C21 107.6(3) . . ?
C20 C18 C13 109.0(2) . . ?
C19 C18 C13 111.5(3) . . ?
C21 C18 C13 112.2(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C15 116.7(5) . . ?
C25 C22 C23 113.7(5) . . ?
C15 C22 C23 110.3(4) . . ?
C25 C22 C24 112.8(5) . . ?
C15 C22 C24 104.0(4) . . ?
C23 C22 C24 97.2(5) . . ?
H25D C25X H25E 109.5 . . ?
H25D C25X H25F 109.5 . . ?
H25E C25X H25F 109.5 . . ?
H24D C24X H24E 109.5 . . ?
H24D C24X H24F 109.5 . . ?
H24E C24X H24F 109.5 . . ?
H23D C23X H23E 109.5 . . ?
H23D C23X H23F 109.5 . . ?
H23E C23X H23F 109.5 . . ?
C17 C26 C33 112.1(2) . . ?
C17 C26 C27 112.3(3) . . ?
C33 C26 C27 111.3(2) . . ?
C17 C26 H26 106.9 . . ?
C33 C26 H26 106.9 . . ?
C27 C26 H26 106.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 C28 C33 118.4(3) . . ?
O3 C28 C29 120.6(3) . . ?
C33 C28 C29 121.1(3) . . ?
C30 C29 C28 116.5(3) . . ?
C30 C29 C34 120.2(3) . . ?
C28 C29 C34 123.3(3) . . ?
C29 C30 C31 124.1(3) . . ?
C29 C30 H30 118.0 . . ?
C31 C30 H30 118.0 . . ?
C32 C31 C30 116.6(3) . . ?
C32 C31 C38 123.1(3) . . ?
C30 C31 C38 120.3(3) . . ?
C31 C32 C33 122.1(3) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
C32 C33 C28 119.2(3) . . ?
C32 C33 C26 119.1(3) . . ?
C28 C33 C26 121.6(3) . . ?
C37 C34 C36 108.6(2) . . ?
C37 C34 C29 111.9(2) . . ?
C36 C34 C29 108.8(2) . . ?
C37 C34 C35 107.1(3) . . ?
C36 C34 C35 108.8(2) . . ?
C29 C34 C35 111.6(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C41 C38 C31 109.8(2) . . ?
C41 C38 C40 109.0(3) . . ?
C31 C38 C40 112.2(3) . . ?
C41 C38 C39 108.5(3) . . ?
C31 C38 C39 109.5(2) . . ?
C40 C38 C39 107.7(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N11 V11 O12 98.09(10) . . ?
N11 V11 O13 98.33(10) . . ?
O12 V11 O13 110.11(9) . . ?
N11 V11 O11 100.85(10) . . ?
O12 V11 O11 115.89(9) . . ?
O13 V11 O11 126.42(8) . . ?
N11 V11 O1 171.45(10) . . ?
O12 V11 O1 88.95(8) . . ?
O13 V11 O1 83.67(8) . . ?
O11 V11 O1 71.55(8) . . ?
C105 N11 V11 175.1(2) . . ?
C101 O11 V11 128.91(17) . . ?
C101 O11 V1 122.14(16) . . ?
V11 O11 V1 108.81(8) . . ?
C112 O12 V11 121.82(18) . . ?
C128 O13 V11 126.75(16) . . ?
O11 C101 C102 112.7(2) . . ?
O11 C101 H10A 109.1 . . ?
C102 C101 H10A 109.0 . . ?
O11 C101 H10B 109.1 . . ?
C102 C101 H10B 109.1 . . ?
H10A C101 H10B 107.8 . . ?
C101 C102 H10C 109.5 . . ?
C101 C102 H10D 109.5 . . ?
H10C C102 H10D 109.5 . . ?
C101 C102 H10E 109.5 . . ?
H10C C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
N11 C105 C106 120.6(3) . . ?
N11 C105 C110 120.5(3) . . ?
C106 C105 C110 118.9(3) . . ?
C107 C106 C105 120.7(3) . . ?
C107 C106 H106 119.6 . . ?
C105 C106 H106 119.6 . . ?
C108 C107 C106 119.4(3) . . ?
C108 C107 H107 120.3 . . ?
C106 C107 H107 120.3 . . ?
C109 C108 C107 121.2(3) . . ?
C109 C108 Cl11 119.1(2) . . ?
C107 C108 Cl11 119.7(2) . . ?
C108 C109 C110 119.6(3) . . ?
C108 C109 H109 120.2 . . ?
C110 C109 H109 120.2 . . ?
C109 C110 C105 120.1(3) . . ?
C109 C110 H110 120.0 . . ?
C105 C110 H110 120.0 . . ?
O12 C112 C117 117.6(3) . . ?
O12 C112 C113 121.4(3) . . ?
C117 C112 C113 121.0(3) . . ?
C114 C113 C112 116.5(3) . . ?
C114 C113 C118 121.0(3) . . ?
C112 C113 C118 122.5(3) . . ?
C113 C114 C115 124.1(3) . . ?
C113 C114 H114 117.9 . . ?
C115 C114 H114 117.9 . . ?
C116 C115 C114 116.5(3) . . ?
C116 C115 C122 123.4(3) . . ?
C114 C115 C122 120.2(3) . . ?
C115 C116 C117 122.4(3) . . ?
C115 C116 H116 118.8 . . ?
C117 C116 H116 118.8 . . ?
C116 C117 C112 118.8(3) . . ?
C116 C117 C126 119.8(3) . . ?
C112 C117 C126 121.4(3) . . ?
C119 C118 C120 109.9(3) . . ?
C119 C118 C121 107.6(3) . . ?
C120 C118 C121 107.5(3) . . ?
C119 C118 C113 111.9(3) . . ?
C120 C118 C113 108.1(2) . . ?
C121 C118 C113 111.7(3) . . ?
C118 C119 H11A 109.5 . . ?
C118 C119 H11B 109.5 . . ?
H11A C119 H11B 109.5 . . ?
C118 C119 H11C 109.5 . . ?
H11A C119 H11C 109.5 . . ?
H11B C119 H11C 109.5 . . ?
C118 C120 H12A 109.5 . . ?
C118 C120 H12B 109.5 . . ?
H12A C120 H12B 109.5 . . ?
C118 C120 H12C 109.5 . . ?
H12A C120 H12C 109.5 . . ?
H12B C120 H12C 109.5 . . ?
C118 C121 H12D 109.5 . . ?
C118 C121 H12E 109.5 . . ?
H12D C121 H12E 109.5 . . ?
C118 C121 H12F 109.5 . . ?
H12D C121 H12F 109.5 . . ?
H12E C121 H12F 109.5 . . ?
C124 C122 C123 107.9(3) . . ?
C124 C122 C115 111.8(2) . . ?
C123 C122 C115 109.7(3) . . ?
C124 C122 C125 109.0(3) . . ?
C123 C122 C125 108.9(3) . . ?
C115 C122 C125 109.4(3) . . ?
C122 C123 H12G 109.5 . . ?
C122 C123 H12H 109.5 . . ?
H12G C123 H12H 109.5 . . ?
C122 C123 H12I 109.5 . . ?
H12G C123 H12I 109.5 . . ?
H12H C123 H12I 109.5 . . ?
C122 C124 H12J 109.5 . . ?
C122 C124 H12K 109.5 . . ?
H12J C124 H12K 109.5 . . ?
C122 C124 H12L 109.5 . . ?
H12J C124 H12L 109.5 . . ?
H12K C124 H12L 109.5 . . ?
C122 C125 H12M 109.5 . . ?
C122 C125 H12N 109.5 . . ?
H12M C125 H12N 109.5 . . ?
C122 C125 H12O 109.5 . . ?
H12M C125 H12O 109.5 . . ?
H12N C125 H12O 109.5 . . ?
C133 C126 C117 111.1(2) . . ?
C133 C126 C127 112.6(2) . . ?
C117 C126 C127 111.6(2) . . ?
C133 C126 H126 107.0 . . ?
C117 C126 H126 107.0 . . ?
C127 C126 H126 107.0 . . ?
C126 C127 H12P 109.5 . . ?
C126 C127 H12Q 109.5 . . ?
H12P C127 H12Q 109.5 . . ?
C126 C127 H12R 109.5 . . ?
H12P C127 H12R 109.5 . . ?
H12Q C127 H12R 109.5 . . ?
O13 C128 C133 118.2(3) . . ?
O13 C128 C129 120.8(3) . . ?
C133 C128 C129 121.0(3) . . ?
C130 C129 C128 116.5(3) . . ?
C130 C129 C134 120.5(3) . . ?
C128 C129 C134 122.8(3) . . ?
C131 C130 C129 124.3(3) . . ?
C131 C130 H130 117.8 . . ?
C129 C130 H130 117.8 . . ?
C130 C131 C132 116.7(3) . . ?
C130 C131 C138 122.5(3) . . ?
C132 C131 C138 120.8(3) . . ?
C131 C132 C133 122.9(3) . . ?
C131 C132 H132 118.6 . . ?
C133 C132 H132 118.6 . . ?
C132 C133 C128 118.5(3) . . ?
C132 C133 C126 120.7(3) . . ?
C128 C133 C126 120.8(3) . . ?
C135 C134 C136 107.6(3) . . ?
C135 C134 C129 108.2(3) . . ?
C136 C134 C129 112.6(3) . . ?
C135 C134 C137 110.8(3) . . ?
C136 C134 C137 105.9(3) . . ?
C129 C134 C137 111.7(2) . . ?
C134 C135 H13A 109.5 . . ?
C134 C135 H13B 109.5 . . ?
H13A C135 H13B 109.5 . . ?
C134 C135 H13C 109.5 . . ?
H13A C135 H13C 109.5 . . ?
H13B C135 H13C 109.5 . . ?
C134 C136 H13D 109.5 . . ?
C134 C136 H13E 109.5 . . ?
H13D C136 H13E 109.5 . . ?
C134 C136 H13F 109.5 . . ?
H13D C136 H13F 109.5 . . ?
H13E C136 H13F 109.5 . . ?
C134 C137 H13G 109.5 . . ?
C134 C137 H13H 109.5 . . ?
H13G C137 H13H 109.5 . . ?
C134 C137 H13I 109.5 . . ?
H13G C137 H13I 109.5 . . ?
H13H C137 H13I 109.5 . . ?
C139 C138 C141 109.7(3) . . ?
C139 C138 C140 109.0(3) . . ?
C141 C138 C140 107.1(3) . . ?
C139 C138 C131 108.9(2) . . ?
C141 C138 C131 111.7(3) . . ?
C140 C138 C131 110.5(3) . . ?
C138 C139 H13J 109.5 . . ?
C138 C139 H13K 109.5 . . ?
H13J C139 H13K 109.5 . . ?
C138 C139 H13L 109.5 . . ?
H13J C139 H13L 109.5 . . ?
H13K C139 H13L 109.5 . . ?
C138 C140 H14A 109.5 . . ?
C138 C140 H14B 109.5 . . ?
H14A C140 H14B 109.5 . . ?
C138 C140 H14C 109.5 . . ?
H14A C140 H14C 109.5 . . ?
H14B C140 H14C 109.5 . . ?
C138 C141 H14D 109.5 . . ?
C138 C141 H14E 109.5 . . ?
H14D C141 H14E 109.5 . . ?
C138 C141 H14F 109.5 . . ?
H14D C141 H14F 109.5 . . ?
H14E C141 H14F 109.5 . . ?
Cl22 C201 Cl21 100.3(9) . . ?
Cl22 C201 H20D 111.7 . . ?
Cl21 C201 H20D 111.7 . . ?
Cl22 C201 H20E 111.7 . . ?
Cl21 C201 H20E 111.7 . . ?
H20D C201 H20E 109.5 . . ?
Cl24 C202 Cl23 119.9(10) . . ?
Cl24 C202 H20F 107.3 . . ?
Cl23 C202 H20F 107.3 . . ?
Cl24 C202 H20G 107.3 . . ?
Cl23 C202 H20G 107.3 . . ?
H20F C202 H20G 106.9 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.17
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.048