# 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              
;
Synthesis, Structure and Ethylene Polymerisation
behaviour of Vanadium(IV and V) complexes bearing chelating aryloxide
ligands
;
loop_
_publ_author_name
'Carl Redshaw'
'Sophie H Dale'
'Mark Elsegood'
'Damien M Homden'
'David L Hughes'
'Lee Warford'
;
J.Wright
;

# Attachment 'cif1.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 718342'

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound 1'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(S-diphenolate)2]'
_chemical_formula_moiety         'C56 H80 O4 S2 V'
_chemical_formula_sum            'C56 H80 O4 S2 V'
_chemical_formula_weight         932.26

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_Int_Tables_number      56

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

_cell_length_a                   19.6406(6)
_cell_length_b                   15.4525(5)
_cell_length_c                   18.2289(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5532.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20504
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.80

_exptl_crystal_description       brick
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2012
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   '(SADABS v2.10; Sheldrick, 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 1K 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            46645
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         29.07
_reflns_number_total             6889
_reflns_number_gt                5487
_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    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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^)+(0.0563P)^2^+3.5257P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'all non-H atoms found by direct methods'
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6889
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1235
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 0.7500 0.7500 0.05008(2) 0.02613(10) Uani 1 2 d S . .
O1 O 0.78143(6) 0.86016(7) 0.07138(6) 0.0306(3) Uani 1 1 d . . .
O2 O 0.68462(6) 0.77560(8) -0.01946(6) 0.0301(2) Uani 1 1 d . . .
S1 S 0.65781(2) 0.80101(3) 0.13713(2) 0.02765(10) Uani 1 1 d . . .
C1 C 0.75734(8) 0.91947(10) 0.11914(8) 0.0276(3) Uani 1 1 d . . .
C2 C 0.79320(9) 0.99664(11) 0.13456(9) 0.0303(3) Uani 1 1 d . . .
C3 C 0.76152(9) 1.05425(11) 0.18286(9) 0.0324(4) Uani 1 1 d . . .
H3 H 0.7844 1.1069 0.1935 0.039 Uiso 1 1 calc R . .
C4 C 0.69837(9) 1.03998(11) 0.21679(9) 0.0311(3) Uani 1 1 d . . .
C5 C 0.66515(9) 0.96297(11) 0.20152(9) 0.0296(3) Uani 1 1 d . . .
H5 H 0.6226 0.9504 0.2239 0.036 Uiso 1 1 calc R . .
C6 C 0.69461(8) 0.90421(10) 0.15316(8) 0.0272(3) Uani 1 1 d . . .
C7 C 0.86257(9) 1.01533(12) 0.09904(10) 0.0368(4) Uani 1 1 d . . .
C8 C 0.85403(12) 1.02175(15) 0.01554(12) 0.0515(5) Uani 1 1 d . . .
H8A H 0.8357 0.9672 -0.0034 0.077 Uiso 1 1 calc R . .
H8B H 0.8984 1.0332 -0.0072 0.077 Uiso 1 1 calc R . .
H8C H 0.8226 1.0690 0.0038 0.077 Uiso 1 1 calc R . .
C9 C 0.91348(10) 0.94303(15) 0.11842(14) 0.0534(5) Uani 1 1 d . . .
H9A H 0.9169 0.9377 0.1719 0.080 Uiso 1 1 calc R . .
H9B H 0.9583 0.9573 0.0981 0.080 Uiso 1 1 calc R . .
H9C H 0.8977 0.8881 0.0976 0.080 Uiso 1 1 calc R . .
C10 C 0.89280(12) 1.10133(14) 0.12625(13) 0.0526(5) Uani 1 1 d . . .
H10A H 0.8614 1.1487 0.1147 0.079 Uiso 1 1 calc R . .
H10B H 0.9366 1.1116 0.1020 0.079 Uiso 1 1 calc R . .
H10C H 0.8997 1.0985 0.1794 0.079 Uiso 1 1 calc R . .
C11 C 0.66872(9) 1.10968(12) 0.26896(10) 0.0346(4) Uani 1 1 d . . .
C12 C 0.71922(11) 1.12686(15) 0.33048(12) 0.0484(5) Uani 1 1 d . . .
H12A H 0.7615 1.1502 0.3098 0.073 Uiso 1 1 calc R . .
H12B H 0.7290 1.0727 0.3563 0.073 Uiso 1 1 calc R . .
H12C H 0.6997 1.1688 0.3649 0.073 Uiso 1 1 calc R . .
C13 C 0.65448(10) 1.19104(13) 0.22501(12) 0.0440(5) Uani 1 1 d . . .
H13A H 0.6355 1.2355 0.2574 0.066 Uiso 1 1 calc R . .
H13B H 0.6218 1.1779 0.1859 0.066 Uiso 1 1 calc R . .
H13C H 0.6970 1.2122 0.2033 0.066 Uiso 1 1 calc R . .
C14 C 0.60135(10) 1.07792(14) 0.30391(12) 0.0449(5) Uani 1 1 d . . .
H14A H 0.5830 1.1232 0.3360 0.067 Uiso 1 1 calc R . .
H14B H 0.6101 1.0256 0.3328 0.067 Uiso 1 1 calc R . .
H14C H 0.5684 1.0649 0.2651 0.067 Uiso 1 1 calc R . .
C15 C 0.61964(8) 0.79758(10) -0.00662(9) 0.0265(3) Uani 1 1 d . . .
C16 C 0.57254(8) 0.80373(10) -0.06490(9) 0.0291(3) Uani 1 1 d . . .
C17 C 0.50656(9) 0.83030(11) -0.04762(9) 0.0315(3) Uani 1 1 d . . .
H17 H 0.4746 0.8351 -0.0865 0.038 Uiso 1 1 calc R . .
C18 C 0.48443(8) 0.85038(10) 0.02375(9) 0.0297(3) Uani 1 1 d . . .
C19 C 0.53121(9) 0.84120(10) 0.08019(9) 0.0298(3) Uani 1 1 d . . .
H19 H 0.5178 0.8522 0.1294 0.036 Uiso 1 1 calc R . .
C20 C 0.59766(8) 0.81592(10) 0.06500(9) 0.0272(3) Uani 1 1 d . . .
C21 C 0.59479(9) 0.78075(12) -0.14373(9) 0.0336(4) Uani 1 1 d . . .
C22 C 0.65280(10) 0.84100(14) -0.16892(10) 0.0409(4) Uani 1 1 d . . .
H22A H 0.6664 0.8257 -0.2190 0.061 Uiso 1 1 calc R . .
H22B H 0.6918 0.8345 -0.1359 0.061 Uiso 1 1 calc R . .
H22C H 0.6370 0.9011 -0.1679 0.061 Uiso 1 1 calc R . .
C23 C 0.61888(12) 0.68628(13) -0.14559(11) 0.0457(5) Uani 1 1 d . . .
H23A H 0.5809 0.6481 -0.1325 0.069 Uiso 1 1 calc R . .
H23B H 0.6561 0.6784 -0.1104 0.069 Uiso 1 1 calc R . .
H23C H 0.6350 0.6720 -0.1950 0.069 Uiso 1 1 calc R . .
C24 C 0.53594(11) 0.79010(17) -0.19822(10) 0.0500(5) Uani 1 1 d . . .
H24A H 0.4985 0.7520 -0.1835 0.075 Uiso 1 1 calc R . .
H24B H 0.5516 0.7741 -0.2474 0.075 Uiso 1 1 calc R . .
H24C H 0.5201 0.8502 -0.1986 0.075 Uiso 1 1 calc R . .
C25 C 0.41029(9) 0.87941(12) 0.03731(11) 0.0358(4) Uani 1 1 d . . .
C26 C 0.36330(12) 0.80304(15) 0.02276(17) 0.0596(6) Uani 1 1 d . . .
H26A H 0.3167 0.8184 0.0369 0.089 Uiso 1 1 calc R . .
H26B H 0.3784 0.7531 0.0516 0.089 Uiso 1 1 calc R . .
H26C H 0.3645 0.7884 -0.0295 0.089 Uiso 1 1 calc R . .
C27 C 0.39218(11) 0.95477(15) -0.01302(14) 0.0541(6) Uani 1 1 d . . .
H27A H 0.3960 0.9363 -0.0643 0.081 Uiso 1 1 calc R . .
H27B H 0.4235 1.0030 -0.0040 0.081 Uiso 1 1 calc R . .
H27C H 0.3454 0.9735 -0.0031 0.081 Uiso 1 1 calc R . .
C28 C 0.40087(11) 0.91003(18) 0.11670(13) 0.0583(6) Uani 1 1 d . . .
H28A H 0.4335 0.9564 0.1273 0.088 Uiso 1 1 calc R . .
H28B H 0.4087 0.8615 0.1502 0.088 Uiso 1 1 calc R . .
H28C H 0.3544 0.9318 0.1233 0.088 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 0.0299(2) 0.02359(18) 0.02486(19) 0.000 0.000 0.00687(15)
O1 0.0354(6) 0.0258(5) 0.0307(6) -0.0004(5) 0.0066(5) 0.0031(5)
O2 0.0301(6) 0.0351(6) 0.0253(5) 0.0008(5) 0.0011(4) 0.0108(5)
S1 0.0342(2) 0.02554(19) 0.02322(19) 0.00233(14) 0.00113(15) 0.00110(15)
C1 0.0334(8) 0.0247(7) 0.0247(7) 0.0019(6) 0.0010(6) 0.0057(6)
C2 0.0332(8) 0.0279(8) 0.0298(8) 0.0031(6) -0.0001(6) 0.0011(6)
C3 0.0387(9) 0.0265(8) 0.0321(8) -0.0011(7) -0.0021(7) 0.0004(7)
C4 0.0371(9) 0.0283(8) 0.0280(8) -0.0017(6) -0.0013(7) 0.0057(7)
C5 0.0329(8) 0.0311(8) 0.0248(7) 0.0010(6) 0.0009(6) 0.0030(7)
C6 0.0338(8) 0.0234(7) 0.0243(7) 0.0019(6) -0.0004(6) 0.0013(6)
C7 0.0371(9) 0.0342(9) 0.0393(9) -0.0002(7) 0.0066(8) -0.0033(7)
C8 0.0600(13) 0.0529(13) 0.0415(11) 0.0034(9) 0.0130(10) -0.0121(10)
C9 0.0350(10) 0.0510(12) 0.0742(15) 0.0028(11) 0.0052(10) 0.0036(9)
C10 0.0484(12) 0.0476(12) 0.0619(13) -0.0084(10) 0.0124(10) -0.0150(10)
C11 0.0352(9) 0.0362(9) 0.0323(8) -0.0090(7) 0.0022(7) 0.0074(7)
C12 0.0477(11) 0.0557(13) 0.0418(11) -0.0130(9) -0.0029(9) 0.0041(10)
C13 0.0436(10) 0.0351(10) 0.0534(12) -0.0060(9) -0.0015(9) 0.0034(8)
C14 0.0437(11) 0.0434(11) 0.0475(11) -0.0096(9) 0.0085(9) 0.0033(9)
C15 0.0296(8) 0.0234(7) 0.0267(7) 0.0013(6) 0.0033(6) 0.0045(6)
C16 0.0320(8) 0.0284(8) 0.0268(7) 0.0001(6) 0.0008(6) 0.0035(6)
C17 0.0310(8) 0.0319(8) 0.0315(8) 0.0004(7) -0.0011(7) 0.0033(7)
C18 0.0288(8) 0.0253(8) 0.0351(8) 0.0012(6) 0.0049(6) 0.0017(6)
C19 0.0350(8) 0.0268(8) 0.0277(8) 0.0000(6) 0.0065(6) -0.0007(6)
C20 0.0314(8) 0.0251(7) 0.0250(7) 0.0017(6) 0.0001(6) 0.0009(6)
C21 0.0337(9) 0.0421(9) 0.0250(8) -0.0028(7) 0.0001(6) 0.0062(7)
C22 0.0432(10) 0.0492(11) 0.0304(9) 0.0028(8) 0.0049(8) 0.0038(8)
C23 0.0570(12) 0.0416(10) 0.0384(10) -0.0119(8) 0.0021(9) 0.0048(9)
C24 0.0426(11) 0.0783(15) 0.0291(9) -0.0064(10) -0.0047(8) 0.0084(11)
C25 0.0292(8) 0.0347(9) 0.0434(10) -0.0008(8) 0.0057(7) 0.0029(7)
C26 0.0436(11) 0.0480(12) 0.0872(18) -0.0083(12) 0.0181(12) -0.0122(10)
C27 0.0414(11) 0.0484(12) 0.0726(15) 0.0127(11) 0.0073(10) 0.0129(9)
C28 0.0409(11) 0.0779(16) 0.0562(13) -0.0146(12) 0.0114(10) 0.0134(11)

_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 O2 1.8473(11) 2_665 ?
V1 O2 1.8473(11) . ?
V1 O1 1.8518(11) . ?
V1 O1 1.8518(11) 2_665 ?
V1 S1 2.5332(5) 2_665 ?
V1 S1 2.5332(5) . ?
O1 C1 1.3497(19) . ?
O2 C15 1.3413(19) . ?
S1 C6 1.7751(16) . ?
S1 C20 1.7827(16) . ?
C1 C6 1.399(2) . ?
C1 C2 1.413(2) . ?
C2 C3 1.398(2) . ?
C2 C7 1.536(2) . ?
C3 C4 1.403(2) . ?
C4 C5 1.385(2) . ?
C4 C11 1.550(2) . ?
C5 C6 1.392(2) . ?
C7 C8 1.534(3) . ?
C7 C10 1.538(3) . ?
C7 C9 1.540(3) . ?
C11 C13 1.517(3) . ?
C11 C12 1.521(3) . ?
C11 C14 1.548(3) . ?
C15 C20 1.404(2) . ?
C15 C16 1.412(2) . ?
C16 C17 1.396(2) . ?
C16 C21 1.543(2) . ?
C17 C18 1.406(2) . ?
C18 C19 1.387(2) . ?
C18 C25 1.544(2) . ?
C19 C20 1.390(2) . ?
C21 C24 1.531(3) . ?
C21 C23 1.535(3) . ?
C21 C22 1.541(3) . ?
C25 C26 1.521(3) . ?
C25 C27 1.525(3) . ?
C25 C28 1.534(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
O2 V1 O2 93.33(7) 2_665 . ?
O2 V1 O1 96.26(5) 2_665 . ?
O2 V1 O1 100.30(5) . . ?
O2 V1 O1 100.30(5) 2_665 2_665 ?
O2 V1 O1 96.26(5) . 2_665 ?
O1 V1 O1 155.79(7) . 2_665 ?
O2 V1 S1 82.32(4) 2_665 2_665 ?
O2 V1 S1 173.37(4) . 2_665 ?
O1 V1 S1 85.21(4) . 2_665 ?
O1 V1 S1 79.68(4) 2_665 2_665 ?
O2 V1 S1 173.37(4) 2_665 . ?
O2 V1 S1 82.32(4) . . ?
O1 V1 S1 79.68(4) . . ?
O1 V1 S1 85.21(4) 2_665 . ?
S1 V1 S1 102.43(2) 2_665 . ?
C1 O1 V1 129.99(10) . . ?
C15 O2 V1 126.58(10) . . ?
C6 S1 C20 105.96(7) . . ?
C6 S1 V1 95.26(5) . . ?
C20 S1 V1 92.97(5) . . ?
O1 C1 C6 118.69(15) . . ?
O1 C1 C2 121.78(15) . . ?
C6 C1 C2 119.53(14) . . ?
C3 C2 C1 116.16(15) . . ?
C3 C2 C7 122.72(15) . . ?
C1 C2 C7 121.12(15) . . ?
C2 C3 C4 124.80(16) . . ?
C5 C4 C3 117.56(15) . . ?
C5 C4 C11 122.89(16) . . ?
C3 C4 C11 119.55(15) . . ?
C4 C5 C6 119.47(16) . . ?
C5 C6 C1 122.47(15) . . ?
C5 C6 S1 121.42(13) . . ?
C1 C6 S1 115.90(12) . . ?
C8 C7 C2 109.47(16) . . ?
C8 C7 C10 107.84(17) . . ?
C2 C7 C10 111.65(15) . . ?
C8 C7 C9 110.21(18) . . ?
C2 C7 C9 110.04(15) . . ?
C10 C7 C9 107.59(17) . . ?
C13 C11 C12 111.42(17) . . ?
C13 C11 C14 108.82(16) . . ?
C12 C11 C14 108.02(16) . . ?
C13 C11 C4 108.73(15) . . ?
C12 C11 C4 109.18(15) . . ?
C14 C11 C4 110.68(15) . . ?
O2 C15 C20 120.40(14) . . ?
O2 C15 C16 120.60(14) . . ?
C20 C15 C16 119.00(14) . . ?
C17 C16 C15 117.28(15) . . ?
C17 C16 C21 122.74(15) . . ?
C15 C16 C21 119.98(14) . . ?
C16 C17 C18 124.11(16) . . ?
C19 C18 C17 117.33(15) . . ?
C19 C18 C25 122.41(15) . . ?
C17 C18 C25 120.25(15) . . ?
C18 C19 C20 120.20(15) . . ?
C19 C20 C15 122.05(15) . . ?
C19 C20 S1 120.77(12) . . ?
C15 C20 S1 117.13(12) . . ?
C24 C21 C23 107.94(17) . . ?
C24 C21 C22 107.93(16) . . ?
C23 C21 C22 109.88(16) . . ?
C24 C21 C16 111.63(14) . . ?
C23 C21 C16 109.06(15) . . ?
C22 C21 C16 110.35(15) . . ?
C26 C25 C27 110.25(19) . . ?
C26 C25 C28 109.30(18) . . ?
C27 C25 C28 107.70(18) . . ?
C26 C25 C18 108.60(16) . . ?
C27 C25 C18 110.23(15) . . ?
C28 C25 C18 110.76(16) . . ?

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
O2 V1 O1 C1 179.90(13) 2_665 . . . ?
O2 V1 O1 C1 85.34(14) . . . . ?
O1 V1 O1 C1 -47.06(13) 2_665 . . . ?
S1 V1 O1 C1 -98.39(13) 2_665 . . . ?
S1 V1 O1 C1 5.20(13) . . . . ?
O2 V1 O2 C15 177.28(15) 2_665 . . . ?
O1 V1 O2 C15 -85.73(13) . . . . ?
O1 V1 O2 C15 76.53(13) 2_665 . . . ?
S1 V1 O2 C15 -7.75(12) . . . . ?
O2 V1 S1 C6 -102.63(6) . . . . ?
O1 V1 S1 C6 -0.63(6) . . . . ?
O1 V1 S1 C6 160.38(6) 2_665 . . . ?
S1 V1 S1 C6 82.06(5) 2_665 . . . ?
O2 V1 S1 C20 3.71(6) . . . . ?
O1 V1 S1 C20 105.71(6) . . . . ?
O1 V1 S1 C20 -93.28(6) 2_665 . . . ?
S1 V1 S1 C20 -171.59(5) 2_665 . . . ?
V1 O1 C1 C6 -9.0(2) . . . . ?
V1 O1 C1 C2 172.05(11) . . . . ?
O1 C1 C2 C3 177.61(15) . . . . ?
C6 C1 C2 C3 -1.3(2) . . . . ?
O1 C1 C2 C7 -1.8(2) . . . . ?
C6 C1 C2 C7 179.30(15) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C7 C2 C3 C4 -179.81(16) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C2 C3 C4 C11 -179.61(16) . . . . ?
C3 C4 C5 C6 -0.9(2) . . . . ?
C11 C4 C5 C6 178.98(15) . . . . ?
C4 C5 C6 C1 0.4(2) . . . . ?
C4 C5 C6 S1 174.94(12) . . . . ?
O1 C1 C6 C5 -178.19(14) . . . . ?
C2 C1 C6 C5 0.8(2) . . . . ?
O1 C1 C6 S1 7.0(2) . . . . ?
C2 C1 C6 S1 -174.04(12) . . . . ?
C20 S1 C6 C5 87.49(14) . . . . ?
V1 S1 C6 C5 -177.89(13) . . . . ?
C20 S1 C6 C1 -97.63(13) . . . . ?
V1 S1 C6 C1 -3.01(12) . . . . ?
C3 C2 C7 C8 -116.55(19) . . . . ?
C1 C2 C7 C8 62.8(2) . . . . ?
C3 C2 C7 C10 2.8(3) . . . . ?
C1 C2 C7 C10 -177.90(17) . . . . ?
C3 C2 C7 C9 122.18(19) . . . . ?
C1 C2 C7 C9 -58.5(2) . . . . ?
C5 C4 C11 C13 -115.69(18) . . . . ?
C3 C4 C11 C13 64.2(2) . . . . ?
C5 C4 C11 C12 122.57(19) . . . . ?
C3 C4 C11 C12 -57.5(2) . . . . ?
C5 C4 C11 C14 3.8(2) . . . . ?
C3 C4 C11 C14 -176.32(16) . . . . ?
V1 O2 C15 C20 9.7(2) . . . . ?
V1 O2 C15 C16 -171.09(11) . . . . ?
O2 C15 C16 C17 -177.50(15) . . . . ?
C20 C15 C16 C17 1.7(2) . . . . ?
O2 C15 C16 C21 3.0(2) . . . . ?
C20 C15 C16 C21 -177.82(15) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C21 C16 C17 C18 178.97(16) . . . . ?
C16 C17 C18 C19 -1.4(3) . . . . ?
C16 C17 C18 C25 179.89(16) . . . . ?
C17 C18 C19 C20 2.2(2) . . . . ?
C25 C18 C19 C20 -179.17(15) . . . . ?
C18 C19 C20 C15 -1.0(2) . . . . ?
C18 C19 C20 S1 -178.31(12) . . . . ?
O2 C15 C20 C19 178.22(14) . . . . ?
C16 C15 C20 C19 -1.0(2) . . . . ?
O2 C15 C20 S1 -4.4(2) . . . . ?
C16 C15 C20 S1 176.40(12) . . . . ?
C6 S1 C20 C19 -86.97(14) . . . . ?
V1 S1 C20 C19 176.70(13) . . . . ?
C6 S1 C20 C15 95.62(13) . . . . ?
V1 S1 C20 C15 -0.71(12) . . . . ?
C17 C16 C21 C24 -0.6(3) . . . . ?
C15 C16 C21 C24 178.94(17) . . . . ?
C17 C16 C21 C23 -119.74(18) . . . . ?
C15 C16 C21 C23 59.7(2) . . . . ?
C17 C16 C21 C22 119.47(18) . . . . ?
C15 C16 C21 C22 -61.0(2) . . . . ?
C19 C18 C25 C26 -110.6(2) . . . . ?
C17 C18 C25 C26 68.1(2) . . . . ?
C19 C18 C25 C27 128.57(19) . . . . ?
C17 C18 C25 C27 -52.8(2) . . . . ?
C19 C18 C25 C28 9.5(2) . . . . ?
C17 C18 C25 C28 -171.88(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.931
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.055

# Attachment 'V_Dalton.cif.txt'

data_2
_database_code_depnum_ccdc_archive 'CCDC 718343'

_chemical_name_common            'Compound 2'
_chemical_melting_point          ?
_chemical_formula_structural     '[C7H10N][V(=O)(NCMe)2Cl3]'
_chemical_formula_moiety         'C7 H10 N, C4 H6 Cl3 N2 O V'
_chemical_formula_sum            'C11 H16 Cl3 N3 O V'
_chemical_formula_weight         363.56

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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

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

_cell_length_a                   8.6892(4)
_cell_length_b                   7.7891(4)
_cell_length_c                   11.8673(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2408(8)
_cell_angle_gamma                90.00
_cell_volume                     784.93(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5804
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.86

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             370
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 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            6978
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         28.86
_reflns_number_total             3610
_reflns_number_gt                3513
_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    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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^)+(0.0334P)^2^+0.1615P] 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   -0.029(17)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3610
_refine_ls_number_parameters     176
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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 0.73265(3) 0.33646(4) 0.74879(2) 0.01828(7) Uani 1 1 d . . .
O1 O 0.91743(14) 0.3387(2) 0.79869(11) 0.0255(3) Uani 1 1 d . . .
Cl1 Cl 0.66531(5) 0.09139(6) 0.84563(4) 0.02424(10) Uani 1 1 d . . .
Cl2 Cl 0.72718(5) 0.17019(6) 0.58188(4) 0.02242(10) Uani 1 1 d . . .
Cl3 Cl 0.71534(5) 0.59596(6) 0.63378(4) 0.02330(9) Uani 1 1 d . . .
N1 N 0.68611(19) 0.4887(2) 0.88762(13) 0.0220(3) Uani 1 1 d . . .
C1 C 0.6910(2) 0.5791(3) 0.96396(15) 0.0215(3) Uani 1 1 d . . .
C2 C 0.6987(3) 0.6999(3) 1.05863(18) 0.0296(4) Uani 1 1 d . . .
H2A H 0.8036 0.6953 1.1092 0.044 Uiso 1 1 calc R . .
H2B H 0.6192 0.6695 1.1027 0.044 Uiso 1 1 calc R . .
H2C H 0.6785 0.8163 1.0277 0.044 Uiso 1 1 calc R . .
N2 N 0.45203(18) 0.3557(2) 0.68551(14) 0.0251(3) Uani 1 1 d . . .
C3 C 0.3205(2) 0.3779(2) 0.65447(17) 0.0233(4) Uani 1 1 d . . .
C4 C 0.1512(2) 0.4074(3) 0.6163(2) 0.0321(5) Uani 1 1 d . . .
H4A H 0.1153 0.3617 0.5382 0.048 Uiso 1 1 calc R . .
H4B H 0.1297 0.5309 0.6162 0.048 Uiso 1 1 calc R . .
H4C H 0.0951 0.3493 0.6689 0.048 Uiso 1 1 calc R . .
C5 C 0.0043(2) 0.7739(3) 0.89339(18) 0.0322(5) Uani 1 1 d . . .
H5A H -0.0192 0.8812 0.9295 0.048 Uiso 1 1 calc R . .
H5B H 0.0496 0.6910 0.9534 0.048 Uiso 1 1 calc R . .
H5C H -0.0930 0.7269 0.8463 0.048 Uiso 1 1 calc R . .
C6 C 0.1200(2) 0.8087(3) 0.81821(16) 0.0234(4) Uani 1 1 d . . .
C7 C 0.2727(2) 0.7426(3) 0.84631(16) 0.0255(4) Uani 1 1 d . . .
H7 H 0.3032 0.6738 0.9134 0.031 Uiso 1 1 calc R . .
C8 C 0.3802(2) 0.7755(3) 0.77832(16) 0.0238(4) Uani 1 1 d . . .
H8 H 0.4837 0.7298 0.7984 0.029 Uiso 1 1 calc R . .
C9 C 0.3353(2) 0.8755(2) 0.68100(15) 0.0200(4) Uani 1 1 d . . .
C10 C 0.1846(2) 0.9413(3) 0.64922(16) 0.0243(4) Uani 1 1 d . . .
H10 H 0.1547 1.0085 0.5813 0.029 Uiso 1 1 calc R . .
C11 C 0.0775(2) 0.9076(3) 0.71821(17) 0.0259(4) Uani 1 1 d . . .
H11 H -0.0263 0.9524 0.6971 0.031 Uiso 1 1 calc R . .
N3 N 0.45369(19) 0.9139(2) 0.61249(13) 0.0226(3) Uani 1 1 d . . .
H3A H 0.5227 0.9934 0.6500 0.034 Uiso 1 1 calc R . .
H3B H 0.4049 0.9560 0.5425 0.034 Uiso 1 1 calc R . .
H3C H 0.5067 0.8162 0.6026 0.034 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 0.01829(13) 0.02026(14) 0.01618(13) -0.00092(12) 0.00339(10) 0.00028(13)
O1 0.0204(6) 0.0328(7) 0.0229(6) -0.0003(7) 0.0041(5) 0.0009(6)
Cl1 0.0303(2) 0.0232(2) 0.01898(18) 0.00088(17) 0.00466(16) -0.00227(19)
Cl2 0.0276(2) 0.0224(2) 0.01767(19) -0.00141(16) 0.00588(16) 0.00288(17)
Cl3 0.0286(2) 0.0210(2) 0.02039(19) -0.00051(17) 0.00527(15) -0.00090(18)
N1 0.0231(7) 0.0239(8) 0.0192(7) 0.0017(6) 0.0049(6) 0.0012(6)
C1 0.0212(8) 0.0216(9) 0.0216(8) 0.0013(7) 0.0045(6) -0.0004(7)
C2 0.0380(11) 0.0278(11) 0.0243(9) -0.0055(8) 0.0099(9) 0.0006(8)
N2 0.0235(7) 0.0268(8) 0.0248(7) 0.0008(7) 0.0046(6) 0.0007(7)
C3 0.0256(9) 0.0224(9) 0.0221(9) 0.0032(7) 0.0056(7) -0.0006(7)
C4 0.0197(9) 0.0398(12) 0.0358(11) 0.0098(9) 0.0041(8) 0.0016(8)
C5 0.0281(10) 0.0431(12) 0.0269(10) -0.0038(9) 0.0094(8) -0.0063(9)
C6 0.0239(8) 0.0242(10) 0.0220(8) -0.0048(7) 0.0044(7) -0.0032(7)
C7 0.0305(10) 0.0244(9) 0.0202(8) 0.0030(8) 0.0022(7) 0.0018(8)
C8 0.0236(9) 0.0236(9) 0.0232(9) 0.0016(7) 0.0023(7) 0.0030(7)
C9 0.0239(8) 0.0187(9) 0.0179(8) -0.0025(6) 0.0054(7) -0.0018(6)
C10 0.0265(9) 0.0251(10) 0.0186(8) 0.0013(7) -0.0011(7) 0.0010(8)
C11 0.0215(9) 0.0286(10) 0.0260(9) -0.0017(8) 0.0013(7) 0.0022(8)
N3 0.0237(7) 0.0246(8) 0.0191(8) -0.0005(6) 0.0034(6) -0.0025(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.5893(13) . ?
V1 N1 2.1369(16) . ?
V1 Cl2 2.3586(5) . ?
V1 Cl1 2.3647(6) . ?
V1 N2 2.3990(16) . ?
V1 Cl3 2.4257(6) . ?
N1 C1 1.141(2) . ?
C1 C2 1.456(3) . ?
N2 C3 1.138(2) . ?
C3 C4 1.462(3) . ?
C5 C6 1.504(3) . ?
C6 C7 1.396(3) . ?
C6 C11 1.397(3) . ?
C7 C8 1.381(3) . ?
C8 C9 1.379(3) . ?
C9 C10 1.382(3) . ?
C9 N3 1.471(2) . ?
C10 C11 1.389(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 N1 92.75(7) . . ?
O1 V1 Cl2 99.08(5) . . ?
N1 V1 Cl2 168.17(5) . . ?
O1 V1 Cl1 99.34(6) . . ?
N1 V1 Cl1 88.07(5) . . ?
Cl2 V1 Cl1 90.11(2) . . ?
O1 V1 N2 174.52(7) . . ?
N1 V1 N2 81.99(6) . . ?
Cl2 V1 N2 86.18(4) . . ?
Cl1 V1 N2 82.12(5) . . ?
O1 V1 Cl3 97.92(6) . . ?
N1 V1 Cl3 88.40(5) . . ?
Cl2 V1 Cl3 89.842(18) . . ?
Cl1 V1 Cl3 162.53(2) . . ?
N2 V1 Cl3 80.45(4) . . ?
C1 N1 V1 166.71(15) . . ?
N1 C1 C2 177.8(2) . . ?
C3 N2 V1 174.79(17) . . ?
N2 C3 C4 179.1(2) . . ?
C7 C6 C11 118.22(17) . . ?
C7 C6 C5 120.87(18) . . ?
C11 C6 C5 120.91(18) . . ?
C8 C7 C6 121.20(18) . . ?
C9 C8 C7 119.21(18) . . ?
C8 C9 C10 121.39(18) . . ?
C8 C9 N3 118.14(16) . . ?
C10 C9 N3 120.45(17) . . ?
C9 C10 C11 118.92(18) . . ?
C10 C11 C6 121.04(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
O1 V1 N1 C1 21.3(7) . . . . ?
Cl2 V1 N1 C1 -158.2(5) . . . . ?
Cl1 V1 N1 C1 120.5(7) . . . . ?
N2 V1 N1 C1 -157.2(7) . . . . ?
Cl3 V1 N1 C1 -76.6(7) . . . . ?
C11 C6 C7 C8 0.9(3) . . . . ?
C5 C6 C7 C8 -179.33(19) . . . . ?
C6 C7 C8 C9 0.0(3) . . . . ?
C7 C8 C9 C10 -1.0(3) . . . . ?
C7 C8 C9 N3 177.75(18) . . . . ?
C8 C9 C10 C11 1.0(3) . . . . ?
N3 C9 C10 C11 -177.68(17) . . . . ?
C9 C10 C11 C6 -0.1(3) . . . . ?
C7 C6 C11 C10 -0.8(3) . . . . ?
C5 C6 C11 C10 179.38(19) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A Cl1 0.91 2.51 3.2847(17) 143.7 1_565
N3 H3A Cl2 0.91 2.51 3.1826(17) 130.7 1_565
N3 H3B Cl3 0.91 2.39 3.2998(16) 174.0 2_656
N3 H3C Cl3 0.91 2.47 3.3352(17) 159.8 .

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.059

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 718344'

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound 3'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=O)(S-diphenolate)(mu-OH)]2.6MeCN'
_chemical_formula_moiety         'C56 H82 O8 S2 V2, 6(C2 H3 N)'
_chemical_formula_sum            'C68 H100 N6 O8 S2 V2'
_chemical_formula_weight         1295.54

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

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

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

_cell_length_a                   16.4675(5)
_cell_length_b                   15.2783(5)
_cell_length_c                   29.5448(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7433.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17022
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.46

_exptl_crystal_description       tablet
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2768
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   'SADABS v2.10, 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            61637
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8500
_reflns_number_gt                6221
_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    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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^)+(0.0472P)^2^+8.6736P] 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         8500
_refine_ls_number_parameters     442
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1309
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.002
_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 0.50909(2) 0.58984(2) 0.525990(13) 0.02036(10) Uani 1 1 d . . .
O1 O 0.43015(9) 0.67506(10) 0.52801(5) 0.0230(3) Uani 1 1 d . . .
O2 O 0.54658(10) 0.60456(10) 0.58442(5) 0.0252(3) Uani 1 1 d . . .
O3 O 0.54822(9) 0.46856(10) 0.52431(5) 0.0246(3) Uani 1 1 d . . .
H3 H 0.5872 0.4429 0.5439 0.029 Uiso 1 1 calc R . .
O4 O 0.57860(10) 0.64307(11) 0.50072(6) 0.0273(4) Uani 1 1 d . . .
S1 S 0.38894(3) 0.51348(3) 0.57791(2) 0.02241(13) Uani 1 1 d . . .
C1 C 0.35731(13) 0.67997(14) 0.54864(7) 0.0205(4) Uani 1 1 d . . .
C2 C 0.31146(13) 0.75783(14) 0.54561(8) 0.0218(4) Uani 1 1 d . . .
C3 C 0.23644(13) 0.75922(15) 0.56824(8) 0.0241(5) Uani 1 1 d . . .
H3A H 0.2047 0.8111 0.5666 0.029 Uiso 1 1 calc R . .
C4 C 0.20581(14) 0.68874(15) 0.59307(7) 0.0235(5) Uani 1 1 d . . .
C5 C 0.25283(13) 0.61295(14) 0.59551(7) 0.0223(4) Uani 1 1 d . . .
H5 H 0.2335 0.5638 0.6120 0.027 Uiso 1 1 calc R . .
C6 C 0.32765(13) 0.60906(14) 0.57397(7) 0.0207(4) Uani 1 1 d . . .
C7 C 0.34406(15) 0.83754(15) 0.51950(9) 0.0301(5) Uani 1 1 d . . .
C8 C 0.42590(16) 0.86675(17) 0.53968(11) 0.0417(7) Uani 1 1 d . . .
H8A H 0.4654 0.8191 0.5369 0.063 Uiso 1 1 calc R . .
H8B H 0.4186 0.8815 0.5717 0.063 Uiso 1 1 calc R . .
H8C H 0.4457 0.9183 0.5233 0.063 Uiso 1 1 calc R . .
C9 C 0.35484(18) 0.81496(19) 0.46911(10) 0.0422(7) Uani 1 1 d . . .
H9A H 0.3922 0.7653 0.4661 0.063 Uiso 1 1 calc R . .
H9B H 0.3771 0.8657 0.4531 0.063 Uiso 1 1 calc R . .
H9C H 0.3021 0.7994 0.4560 0.063 Uiso 1 1 calc R . .
C10 C 0.28578(17) 0.91553(17) 0.52290(13) 0.0495(8) Uani 1 1 d . . .
H10A H 0.3093 0.9661 0.5072 0.074 Uiso 1 1 calc R . .
H10B H 0.2769 0.9301 0.5548 0.074 Uiso 1 1 calc R . .
H10C H 0.2338 0.9002 0.5088 0.074 Uiso 1 1 calc R . .
C11 C 0.12426(15) 0.69224(16) 0.61840(9) 0.0303(5) Uani 1 1 d . . .
C12 C 0.06835(18) 0.6192(2) 0.60108(12) 0.0522(8) Uani 1 1 d . . .
H12A H 0.0174 0.6199 0.6182 0.078 Uiso 1 1 calc R . .
H12B H 0.0951 0.5624 0.6051 0.078 Uiso 1 1 calc R . .
H12C H 0.0569 0.6285 0.5689 0.078 Uiso 1 1 calc R . .
C13 C 0.14010(19) 0.6779(2) 0.66887(9) 0.0467(7) Uani 1 1 d . . .
H13A H 0.1778 0.7227 0.6799 0.070 Uiso 1 1 calc R . .
H13B H 0.1638 0.6198 0.6735 0.070 Uiso 1 1 calc R . .
H13C H 0.0888 0.6821 0.6855 0.070 Uiso 1 1 calc R . .
C14 C 0.0813(2) 0.7798(2) 0.61233(14) 0.0653(11) Uani 1 1 d . . .
H14A H 0.0695 0.7891 0.5802 0.098 Uiso 1 1 calc R . .
H14B H 0.1163 0.8270 0.6234 0.098 Uiso 1 1 calc R . .
H14C H 0.0304 0.7796 0.6295 0.098 Uiso 1 1 calc R . .
C15 C 0.51831(14) 0.57924(14) 0.62503(8) 0.0229(5) Uani 1 1 d . . .
C16 C 0.56255(15) 0.59978(16) 0.66489(8) 0.0276(5) Uani 1 1 d . . .
C17 C 0.53024(16) 0.57082(18) 0.70575(9) 0.0327(6) Uani 1 1 d . . .
H17 H 0.5593 0.5838 0.7327 0.039 Uiso 1 1 calc R . .
C18 C 0.45731(16) 0.52360(18) 0.70959(9) 0.0337(6) Uani 1 1 d . A .
C19 C 0.41449(15) 0.50643(16) 0.67000(9) 0.0293(5) Uani 1 1 d . . .
H19 H 0.3647 0.4752 0.6713 0.035 Uiso 1 1 calc R . .
C20 C 0.44416(14) 0.53466(14) 0.62861(8) 0.0234(5) Uani 1 1 d . . .
C21 C 0.64192(16) 0.65287(19) 0.66240(9) 0.0361(6) Uani 1 1 d . . .
C22 C 0.67698(19) 0.6696(2) 0.70985(10) 0.0506(8) Uani 1 1 d . . .
H22A H 0.6896 0.6136 0.7244 0.076 Uiso 1 1 calc R . .
H22B H 0.6370 0.7013 0.7282 0.076 Uiso 1 1 calc R . .
H22C H 0.7266 0.7046 0.7073 0.076 Uiso 1 1 calc R . .
C23 C 0.6246(2) 0.7426(2) 0.64094(11) 0.0533(9) Uani 1 1 d . . .
H23A H 0.6748 0.7769 0.6399 0.080 Uiso 1 1 calc R . .
H23B H 0.5839 0.7736 0.6591 0.080 Uiso 1 1 calc R . .
H23C H 0.6039 0.7343 0.6101 0.080 Uiso 1 1 calc R . .
C24 C 0.70617(17) 0.6034(2) 0.63461(11) 0.0520(8) Uani 1 1 d . . .
H24A H 0.7182 0.5473 0.6492 0.078 Uiso 1 1 calc R . .
H24B H 0.7559 0.6385 0.6329 0.078 Uiso 1 1 calc R . .
H24C H 0.6854 0.5928 0.6040 0.078 Uiso 1 1 calc R . .
C25 C 0.42550(19) 0.4947(3) 0.75588(11) 0.0571(9) Uani 1 1 d DU . .
C26 C 0.4057(4) 0.5876(4) 0.78391(18) 0.0585(18) Uani 0.581(6) 1 d PDU A 1
H26A H 0.4549 0.6236 0.7852 0.088 Uiso 0.581(6) 1 calc PR A 1
H26B H 0.3879 0.5736 0.8147 0.088 Uiso 0.581(6) 1 calc PR A 1
H26C H 0.3627 0.6198 0.7682 0.088 Uiso 0.581(6) 1 calc PR A 1
C27 C 0.3475(4) 0.4478(5) 0.7564(2) 0.0598(19) Uani 0.581(6) 1 d PDU A 1
H27A H 0.3088 0.4778 0.7365 0.090 Uiso 0.581(6) 1 calc PR A 1
H27B H 0.3261 0.4467 0.7874 0.090 Uiso 0.581(6) 1 calc PR A 1
H27C H 0.3556 0.3877 0.7457 0.090 Uiso 0.581(6) 1 calc PR A 1
C28 C 0.4918(6) 0.4565(7) 0.7846(3) 0.066(3) Uani 0.581(6) 1 d PDU A 1
H28A H 0.5409 0.4924 0.7817 0.099 Uiso 0.581(6) 1 calc PR A 1
H28B H 0.5034 0.3967 0.7745 0.099 Uiso 0.581(6) 1 calc PR A 1
H28C H 0.4744 0.4555 0.8163 0.099 Uiso 0.581(6) 1 calc PR A 1
C26X C 0.3409(5) 0.5249(7) 0.7613(3) 0.071(3) Uani 0.419(6) 1 d PDU A 2
H26D H 0.3128 0.5218 0.7321 0.107 Uiso 0.419(6) 1 calc PR A 2
H26E H 0.3407 0.5855 0.7722 0.107 Uiso 0.419(6) 1 calc PR A 2
H26F H 0.3129 0.4875 0.7833 0.107 Uiso 0.419(6) 1 calc PR A 2
C27X C 0.4104(8) 0.3865(5) 0.7481(3) 0.079(4) Uani 0.419(6) 1 d PDU A 2
H27D H 0.3733 0.3775 0.7226 0.118 Uiso 0.419(6) 1 calc PR A 2
H27E H 0.3866 0.3611 0.7756 0.118 Uiso 0.419(6) 1 calc PR A 2
H27F H 0.4624 0.3579 0.7417 0.118 Uiso 0.419(6) 1 calc PR A 2
C28X C 0.4837(8) 0.4974(9) 0.7929(4) 0.071(4) Uani 0.419(6) 1 d PDU A 2
H28D H 0.5369 0.4776 0.7820 0.106 Uiso 0.419(6) 1 calc PR A 2
H28E H 0.4653 0.4589 0.8174 0.106 Uiso 0.419(6) 1 calc PR A 2
H28F H 0.4883 0.5574 0.8043 0.106 Uiso 0.419(6) 1 calc PR A 2
N1 N 0.2009(2) 0.4129(2) 0.66294(14) 0.0821(11) Uani 1 1 d D . .
C29 C 0.1676(2) 0.3479(2) 0.66603(12) 0.0540(8) Uani 1 1 d D . .
C30 C 0.1255(2) 0.2649(2) 0.66894(13) 0.0610(9) Uani 1 1 d D . .
H30A H 0.0801 0.2644 0.6475 0.092 Uiso 1 1 calc R . .
H30B H 0.1047 0.2567 0.6997 0.092 Uiso 1 1 calc R . .
H30C H 0.1631 0.2173 0.6616 0.092 Uiso 1 1 calc R . .
N2 N 0.70579(17) 0.4120(2) 0.55058(12) 0.0639(8) Uani 1 1 d D . .
C31 C 0.76818(19) 0.3849(2) 0.54108(11) 0.0464(7) Uani 1 1 d D . .
C32 C 0.84618(19) 0.3525(2) 0.52900(11) 0.0516(8) Uani 1 1 d D . .
H32A H 0.8871 0.3773 0.5494 0.077 Uiso 1 1 calc R . .
H32B H 0.8586 0.3694 0.4978 0.077 Uiso 1 1 calc R . .
H32C H 0.8466 0.2886 0.5316 0.077 Uiso 1 1 calc R . .
N3 N 0.5764(7) 0.2585(8) 0.7169(3) 0.156(5) Uani 0.611(10) 1 d PDU B 1
C33 C 0.6009(5) 0.3081(6) 0.6911(3) 0.083(3) Uani 0.611(10) 1 d PDU B 1
C34 C 0.6252(8) 0.3675(8) 0.6572(5) 0.116(5) Uani 0.611(10) 1 d PDU B 1
H34A H 0.6247 0.3381 0.6277 0.174 Uiso 0.611(10) 1 calc PR B 1
H34B H 0.6802 0.3885 0.6638 0.174 Uiso 0.611(10) 1 calc PR B 1
H34C H 0.5876 0.4172 0.6566 0.174 Uiso 0.611(10) 1 calc PR B 1
N3X N 0.6474(12) 0.3289(12) 0.7231(5) 0.161(7) Uiso 0.389(10) 1 d PDU B 2
C33X C 0.6388(10) 0.3514(11) 0.6860(4) 0.069(4) Uiso 0.389(10) 1 d PDU B 2
C34X C 0.6280(13) 0.3666(13) 0.6384(4) 0.069(4) Uiso 0.389(10) 1 d PDU B 2
H34D H 0.6400 0.3128 0.6217 0.104 Uiso 0.389(10) 1 calc PR B 2
H34E H 0.6649 0.4132 0.6285 0.104 Uiso 0.389(10) 1 calc PR B 2
H34F H 0.5718 0.3843 0.6326 0.104 Uiso 0.389(10) 1 calc PR 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 0.01937(18) 0.02018(19) 0.02153(19) -0.00355(14) -0.00047(14) 0.00270(14)
O1 0.0219(8) 0.0187(7) 0.0284(8) -0.0009(6) 0.0042(6) 0.0025(6)
O2 0.0247(8) 0.0284(8) 0.0225(8) -0.0033(6) 0.0003(6) -0.0024(7)
O3 0.0240(8) 0.0236(8) 0.0260(8) -0.0042(6) -0.0066(7) 0.0074(6)
O4 0.0236(8) 0.0303(9) 0.0281(9) -0.0017(7) 0.0023(7) 0.0015(7)
S1 0.0224(3) 0.0166(2) 0.0283(3) -0.0016(2) -0.0034(2) 0.0012(2)
C1 0.0187(10) 0.0204(10) 0.0222(11) -0.0044(8) 0.0000(8) 0.0007(8)
C2 0.0226(11) 0.0183(10) 0.0246(11) 0.0000(8) 0.0012(9) 0.0011(8)
C3 0.0234(11) 0.0207(11) 0.0281(12) 0.0005(9) 0.0037(9) 0.0045(9)
C4 0.0236(11) 0.0249(11) 0.0220(11) -0.0012(9) 0.0024(9) 0.0011(9)
C5 0.0234(11) 0.0204(10) 0.0230(11) 0.0006(8) -0.0014(9) -0.0023(8)
C6 0.0217(10) 0.0179(10) 0.0226(11) -0.0024(8) -0.0036(8) 0.0013(8)
C7 0.0253(12) 0.0203(11) 0.0446(15) 0.0075(10) 0.0089(10) 0.0035(9)
C8 0.0325(14) 0.0249(13) 0.068(2) 0.0000(13) 0.0074(13) -0.0056(11)
C9 0.0437(16) 0.0412(16) 0.0417(16) 0.0179(13) 0.0096(13) 0.0018(12)
C10 0.0351(15) 0.0253(13) 0.088(2) 0.0211(14) 0.0226(15) 0.0088(11)
C11 0.0265(12) 0.0319(13) 0.0323(13) 0.0050(10) 0.0094(10) 0.0043(10)
C12 0.0291(15) 0.074(2) 0.0537(19) -0.0083(17) 0.0076(13) -0.0125(15)
C13 0.0433(16) 0.064(2) 0.0332(15) 0.0012(14) 0.0137(13) -0.0014(15)
C14 0.054(2) 0.059(2) 0.083(3) 0.0309(19) 0.0442(19) 0.0289(17)
C15 0.0247(11) 0.0210(11) 0.0231(11) -0.0013(8) -0.0010(9) 0.0020(9)
C16 0.0257(12) 0.0288(12) 0.0282(12) -0.0012(10) -0.0029(9) 0.0001(9)
C17 0.0321(13) 0.0407(14) 0.0254(12) 0.0005(10) -0.0050(10) 0.0006(11)
C18 0.0318(13) 0.0402(14) 0.0291(13) 0.0095(11) -0.0005(10) 0.0019(11)
C19 0.0263(12) 0.0262(12) 0.0353(13) 0.0076(10) -0.0011(10) 0.0005(9)
C20 0.0238(11) 0.0191(10) 0.0274(12) 0.0002(9) -0.0046(9) 0.0029(8)
C21 0.0349(14) 0.0472(16) 0.0263(13) -0.0042(11) -0.0057(11) -0.0144(12)
C22 0.0444(17) 0.073(2) 0.0345(15) -0.0052(15) -0.0099(13) -0.0196(16)
C23 0.066(2) 0.0469(18) 0.0468(18) 0.0039(14) -0.0165(16) -0.0294(16)
C24 0.0294(14) 0.085(2) 0.0412(17) -0.0089(16) 0.0020(12) -0.0128(15)
C25 0.0443(17) 0.089(2) 0.0381(17) 0.0264(17) 0.0026(13) -0.0036(17)
C26 0.046(3) 0.097(5) 0.033(3) -0.007(3) 0.011(2) 0.004(3)
C27 0.056(3) 0.083(5) 0.040(3) 0.020(3) 0.012(3) -0.014(3)
C28 0.067(4) 0.091(7) 0.039(5) 0.026(4) -0.002(3) 0.003(5)
C26X 0.069(5) 0.103(8) 0.043(5) 0.002(5) 0.026(4) -0.010(5)
C27X 0.141(10) 0.063(5) 0.032(4) 0.017(4) 0.006(5) -0.039(5)
C28X 0.096(8) 0.102(11) 0.015(4) 0.006(6) -0.004(5) -0.045(7)
N1 0.077(2) 0.063(2) 0.106(3) -0.014(2) 0.003(2) -0.0145(19)
C29 0.0477(18) 0.055(2) 0.059(2) -0.0153(16) 0.0095(15) -0.0005(16)
C30 0.063(2) 0.060(2) 0.060(2) -0.0165(17) 0.0208(18) -0.0095(18)
N2 0.0418(16) 0.0609(19) 0.089(2) -0.0146(17) -0.0163(15) 0.0139(14)
C31 0.0472(18) 0.0455(17) 0.0465(17) 0.0012(14) -0.0129(14) 0.0056(14)
C32 0.0502(18) 0.056(2) 0.0489(19) 0.0034(15) 0.0019(15) 0.0122(15)
N3 0.171(10) 0.192(11) 0.106(7) 0.052(6) -0.040(6) -0.018(8)
C33 0.069(5) 0.079(5) 0.100(6) -0.008(4) -0.028(4) 0.006(4)
C34 0.085(7) 0.076(6) 0.186(17) 0.018(9) 0.041(11) 0.014(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O4 1.5904(17) . ?
V1 O1 1.8409(15) . ?
V1 O2 1.8472(16) . ?
V1 O3 1.9624(15) . ?
V1 O3 1.9736(16) 5_666 ?
V1 S1 2.7620(7) . ?
O1 C1 1.348(3) . ?
O2 C15 1.344(3) . ?
O3 V1 1.9737(16) 5_666 ?
S1 C6 1.779(2) . ?
S1 C20 1.782(2) . ?
C1 C6 1.404(3) . ?
C1 C2 1.412(3) . ?
C2 C3 1.405(3) . ?
C2 C7 1.538(3) . ?
C3 C4 1.397(3) . ?
C4 C5 1.395(3) . ?
C4 C11 1.538(3) . ?
C5 C6 1.388(3) . ?
C7 C10 1.533(3) . ?
C7 C9 1.538(4) . ?
C7 C8 1.540(4) . ?
C11 C14 1.524(4) . ?
C11 C13 1.530(4) . ?
C11 C12 1.535(4) . ?
C15 C20 1.402(3) . ?
C15 C16 1.420(3) . ?
C16 C17 1.392(3) . ?
C16 C21 1.540(3) . ?
C17 C18 1.405(4) . ?
C18 C19 1.391(4) . ?
C18 C25 1.530(4) . ?
C19 C20 1.386(3) . ?
C21 C23 1.537(4) . ?
C21 C22 1.538(4) . ?
C21 C24 1.538(4) . ?
C25 C28X 1.456(9) . ?
C25 C27 1.471(6) . ?
C25 C26X 1.477(8) . ?
C25 C28 1.500(7) . ?
C25 C26 1.675(6) . ?
C25 C27X 1.688(8) . ?
N1 C29 1.139(4) . ?
C29 C30 1.448(5) . ?
N2 C31 1.143(4) . ?
C31 C32 1.422(4) . ?
N3 C33 1.148(10) . ?
C33 C34 1.409(11) . ?
N3X C33X 1.157(13) . ?
C33X C34X 1.436(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V1 O1 99.30(8) . . ?
O4 V1 O2 97.81(8) . . ?
O1 V1 O2 96.87(7) . . ?
O4 V1 O3 103.57(8) . . ?
O1 V1 O3 154.24(7) . . ?
O2 V1 O3 91.65(7) . . ?
O4 V1 O3 102.82(8) . 5_666 ?
O1 V1 O3 90.37(7) . 5_666 ?
O2 V1 O3 156.72(7) . 5_666 ?
O3 V1 O3 73.21(7) . 5_666 ?
O4 V1 S1 172.90(6) . . ?
O1 V1 S1 76.99(5) . . ?
O2 V1 S1 76.81(5) . . ?
O3 V1 S1 81.40(5) . . ?
O3 V1 S1 83.38(5) 5_666 . ?
C1 O1 V1 133.04(14) . . ?
C15 O2 V1 133.13(14) . . ?
V1 O3 V1 106.79(7) . 5_666 ?
C6 S1 C20 101.27(10) . . ?
C6 S1 V1 91.34(8) . . ?
C20 S1 V1 91.41(8) . . ?
O1 C1 C6 120.51(19) . . ?
O1 C1 C2 119.62(19) . . ?
C6 C1 C2 119.86(19) . . ?
C3 C2 C1 116.9(2) . . ?
C3 C2 C7 122.25(19) . . ?
C1 C2 C7 120.81(19) . . ?
C4 C3 C2 123.8(2) . . ?
C5 C4 C3 117.8(2) . . ?
C5 C4 C11 119.2(2) . . ?
C3 C4 C11 123.0(2) . . ?
C6 C5 C4 120.3(2) . . ?
C5 C6 C1 121.3(2) . . ?
C5 C6 S1 120.58(17) . . ?
C1 C6 S1 118.09(16) . . ?
C10 C7 C2 111.34(19) . . ?
C10 C7 C9 108.1(2) . . ?
C2 C7 C9 110.4(2) . . ?
C10 C7 C8 107.3(2) . . ?
C2 C7 C8 109.9(2) . . ?
C9 C7 C8 109.8(2) . . ?
C14 C11 C13 108.6(3) . . ?
C14 C11 C12 108.7(3) . . ?
C13 C11 C12 108.9(2) . . ?
C14 C11 C4 112.2(2) . . ?
C13 C11 C4 108.7(2) . . ?
C12 C11 C4 109.6(2) . . ?
O2 C15 C20 120.6(2) . . ?
O2 C15 C16 119.9(2) . . ?
C20 C15 C16 119.4(2) . . ?
C17 C16 C15 116.9(2) . . ?
C17 C16 C21 122.2(2) . . ?
C15 C16 C21 120.8(2) . . ?
C16 C17 C18 124.1(2) . . ?
C19 C18 C17 117.5(2) . . ?
C19 C18 C25 121.6(2) . . ?
C17 C18 C25 120.9(2) . . ?
C20 C19 C18 120.3(2) . . ?
C19 C20 C15 121.7(2) . . ?
C19 C20 S1 120.36(18) . . ?
C15 C20 S1 117.98(17) . . ?
C23 C21 C22 107.3(2) . . ?
C23 C21 C24 110.2(3) . . ?
C22 C21 C24 108.1(2) . . ?
C23 C21 C16 109.4(2) . . ?
C22 C21 C16 111.3(2) . . ?
C24 C21 C16 110.5(2) . . ?
C28X C25 C27 125.5(7) . . ?
C28X C25 C26X 122.1(8) . . ?
C27 C25 C28 116.1(6) . . ?
C28X C25 C18 116.0(7) . . ?
C27 C25 C18 116.7(3) . . ?
C26X C25 C18 109.3(4) . . ?
C28 C25 C18 111.6(5) . . ?
C27 C25 C26 103.7(4) . . ?
C28 C25 C26 101.1(5) . . ?
C18 C25 C26 105.3(3) . . ?
C28X C25 C27X 103.1(7) . . ?
C26X C25 C27X 100.5(6) . . ?
C18 C25 C27X 102.2(4) . . ?
N1 C29 C30 178.8(4) . . ?
N2 C31 C32 179.1(4) . . ?
N3 C33 C34 175.2(12) . . ?
N3X C33X C34X 172(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V1 O1 C1 -172.00(19) . . . . ?
O2 V1 O1 C1 -72.88(19) . . . . ?
O3 V1 O1 C1 35.6(3) . . . . ?
O3 V1 O1 C1 84.94(19) 5_666 . . . ?
S1 V1 O1 C1 1.83(18) . . . . ?
O4 V1 O2 C15 178.34(19) . . . . ?
O1 V1 O2 C15 77.9(2) . . . . ?
O3 V1 O2 C15 -77.7(2) . . . . ?
O3 V1 O2 C15 -29.3(3) 5_666 . . . ?
S1 V1 O2 C15 3.05(18) . . . . ?
O4 V1 O3 V1 -99.53(9) . . . 5_666 ?
O1 V1 O3 V1 52.44(19) . . . 5_666 ?
O2 V1 O3 V1 162.02(8) . . . 5_666 ?
O3 V1 O3 V1 0.0 5_666 . . 5_666 ?
S1 V1 O3 V1 85.63(7) . . . 5_666 ?
O1 V1 S1 C6 -1.15(9) . . . . ?
O2 V1 S1 C6 99.23(9) . . . . ?
O3 V1 S1 C6 -167.02(8) . . . . ?
O3 V1 S1 C6 -93.07(8) 5_666 . . . ?
O1 V1 S1 C20 -102.46(9) . . . . ?
O2 V1 S1 C20 -2.08(9) . . . . ?
O3 V1 S1 C20 91.67(8) . . . . ?
O3 V1 S1 C20 165.62(8) 5_666 . . . ?
V1 O1 C1 C6 -1.8(3) . . . . ?
V1 O1 C1 C2 176.64(15) . . . . ?
O1 C1 C2 C3 -179.3(2) . . . . ?
C6 C1 C2 C3 -0.9(3) . . . . ?
O1 C1 C2 C7 -0.7(3) . . . . ?
C6 C1 C2 C7 177.8(2) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C7 C2 C3 C4 -178.6(2) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C2 C3 C4 C11 178.7(2) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C11 C4 C5 C6 -178.2(2) . . . . ?
C4 C5 C6 C1 -1.2(3) . . . . ?
C4 C5 C6 S1 178.66(17) . . . . ?
O1 C1 C6 C5 179.9(2) . . . . ?
C2 C1 C6 C5 1.4(3) . . . . ?
O1 C1 C6 S1 0.0(3) . . . . ?
C2 C1 C6 S1 -178.42(16) . . . . ?
C20 S1 C6 C5 -87.32(19) . . . . ?
V1 S1 C6 C5 -179.03(18) . . . . ?
C20 S1 C6 C1 92.55(19) . . . . ?
V1 S1 C6 C1 0.84(17) . . . . ?
C3 C2 C7 C10 1.4(3) . . . . ?
C1 C2 C7 C10 -177.2(2) . . . . ?
C3 C2 C7 C9 -118.6(2) . . . . ?
C1 C2 C7 C9 62.8(3) . . . . ?
C3 C2 C7 C8 120.1(2) . . . . ?
C1 C2 C7 C8 -58.4(3) . . . . ?
C5 C4 C11 C14 179.6(3) . . . . ?
C3 C4 C11 C14 1.1(4) . . . . ?
C5 C4 C11 C13 59.4(3) . . . . ?
C3 C4 C11 C13 -119.1(3) . . . . ?
C5 C4 C11 C12 -59.4(3) . . . . ?
C3 C4 C11 C12 122.0(3) . . . . ?
V1 O2 C15 C20 -2.8(3) . . . . ?
V1 O2 C15 C16 178.96(16) . . . . ?
O2 C15 C16 C17 -179.4(2) . . . . ?
C20 C15 C16 C17 2.4(3) . . . . ?
O2 C15 C16 C21 1.5(3) . . . . ?
C20 C15 C16 C21 -176.8(2) . . . . ?
C15 C16 C17 C18 -0.3(4) . . . . ?
C21 C16 C17 C18 178.8(3) . . . . ?
C16 C17 C18 C19 -1.2(4) . . . . ?
C16 C17 C18 C25 -179.5(3) . . . . ?
C17 C18 C19 C20 0.6(4) . . . . ?
C25 C18 C19 C20 178.9(3) . . . . ?
C18 C19 C20 C15 1.4(4) . . . . ?
C18 C19 C20 S1 -179.49(19) . . . . ?
O2 C15 C20 C19 178.8(2) . . . . ?
C16 C15 C20 C19 -3.0(3) . . . . ?
O2 C15 C20 S1 -0.3(3) . . . . ?
C16 C15 C20 S1 177.90(17) . . . . ?
C6 S1 C20 C19 91.0(2) . . . . ?
V1 S1 C20 C19 -177.37(18) . . . . ?
C6 S1 C20 C15 -89.91(19) . . . . ?
V1 S1 C20 C15 1.73(17) . . . . ?
C17 C16 C21 C23 -119.5(3) . . . . ?
C15 C16 C21 C23 59.6(3) . . . . ?
C17 C16 C21 C22 -1.2(4) . . . . ?
C15 C16 C21 C22 178.0(2) . . . . ?
C17 C16 C21 C24 118.9(3) . . . . ?
C15 C16 C21 C24 -62.0(3) . . . . ?
C19 C18 C25 C28X 165.7(7) . . . . ?
C17 C18 C25 C28X -16.0(8) . . . . ?
C19 C18 C25 C27 0.1(5) . . . . ?
C17 C18 C25 C27 178.3(4) . . . . ?
C19 C18 C25 C26X -51.4(6) . . . . ?
C17 C18 C25 C26X 126.8(5) . . . . ?
C19 C18 C25 C28 136.9(5) . . . . ?
C17 C18 C25 C28 -44.9(6) . . . . ?
C19 C18 C25 C26 -114.3(3) . . . . ?
C17 C18 C25 C26 63.9(4) . . . . ?
C19 C18 C25 C27X 54.4(5) . . . . ?
C17 C18 C25 C27X -127.4(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 N2 0.95 2.02 2.843(3) 144.1 .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.062

#===END

data_4
_database_code_depnum_ccdc_archive 'CCDC 718345'

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound 4'
_chemical_melting_point          ?
_chemical_formula_structural     '[V(SO2-diphenolate)2)].MeCN'
_chemical_formula_moiety         'C56 H80 O8 S2 V, C2 H3 N'
_chemical_formula_sum            'C58 H83 N O8 S2 V'
_chemical_formula_weight         1037.31

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

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

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

_cell_length_a                   17.2685(19)
_cell_length_b                   19.079(2)
_cell_length_c                   19.842(2)
_cell_angle_alpha                112.4170(16)
_cell_angle_beta                 98.4624(17)
_cell_angle_gamma                98.2682(17)
_cell_volume                     5832.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8299
_cell_measurement_theta_min      3.91
_cell_measurement_theta_max      32.24

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2228
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.8462
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 16.2 SMX'
_diffrn_radiation_monochromator  'silicon 111'
_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_%        4
_diffrn_reflns_number            43293
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.87
_diffrn_reflns_theta_max         33.17
_reflns_number_total             23814
_reflns_number_gt                18131
_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    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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. Lattice contains small voids
but these only contain 6 electrons. No action taken.
;

_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^)+(0.0710P)^2^+3.6509P] 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         23814
_refine_ls_number_parameters     1386
_refine_ls_number_restraints     500
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1640
_refine_ls_wR_factor_gt          0.1513
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.123
_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 0.58351(3) 0.25590(3) 0.15820(2) 0.02023(11) Uani 1 1 d . . .
O1 O 0.46043(11) 0.24273(11) 0.12002(10) 0.0243(4) Uani 1 1 d . . .
O2 O 0.58193(11) 0.20224(12) 0.06005(11) 0.0293(5) Uani 1 1 d . . .
O3 O 0.60112(11) 0.35387(11) 0.15505(11) 0.0266(4) Uani 1 1 d . . .
O4 O 0.34738(11) 0.25641(12) 0.03782(11) 0.0296(5) Uani 1 1 d . . .
O5 O 0.69139(11) 0.26134(11) 0.19598(10) 0.0240(4) Uani 1 1 d . . .
O6 O 0.56153(11) 0.28957(11) 0.25265(10) 0.0240(4) Uani 1 1 d . . .
O7 O 0.55755(12) 0.14374(11) 0.15546(12) 0.0316(5) Uani 1 1 d . . .
O8 O 0.56547(13) 0.05355(12) 0.21563(12) 0.0357(5) Uani 1 1 d . . .
S1 S 0.43300(4) 0.26899(4) 0.06129(4) 0.02230(15) Uani 1 1 d . . .
S2 S 0.58027(4) 0.13285(4) 0.22289(4) 0.02645(16) Uani 1 1 d . . .
C1 C 0.55500(16) 0.39868(16) 0.13800(15) 0.0235(6) Uani 1 1 d . . .
C2 C 0.58703(16) 0.47981(16) 0.16240(15) 0.0246(6) Uani 1 1 d . . .
C3 C 0.53501(17) 0.52312(16) 0.14540(16) 0.0272(6) Uani 1 1 d . . .
H3 H 0.5553 0.5774 0.1626 0.033 Uiso 1 1 calc R . .
C4 C 0.45513(17) 0.49338(17) 0.10509(16) 0.0265(6) Uani 1 1 d . . .
C5 C 0.42651(16) 0.41469(16) 0.07920(15) 0.0243(6) Uani 1 1 d . . .
H5 H 0.3734 0.3916 0.0501 0.029 Uiso 1 1 calc R . .
C6 C 0.47567(16) 0.36854(15) 0.09568(15) 0.0220(6) Uani 1 1 d . . .
C7 C 0.67390(16) 0.51744(16) 0.20535(17) 0.0282(6) Uani 1 1 d . . .
C8 C 0.73172(18) 0.47746(19) 0.15975(19) 0.0362(7) Uani 1 1 d . . .
H8A H 0.7214 0.4225 0.1509 0.054 Uiso 1 1 calc R . .
H8B H 0.7872 0.5025 0.1875 0.054 Uiso 1 1 calc R . .
H8C H 0.7235 0.4819 0.1117 0.054 Uiso 1 1 calc R . .
C9 C 0.68545(19) 0.51233(19) 0.28117(17) 0.0366(7) Uani 1 1 d . . .
H9A H 0.6497 0.5403 0.3101 0.055 Uiso 1 1 calc R . .
H9B H 0.7413 0.5357 0.3085 0.055 Uiso 1 1 calc R . .
H9C H 0.6728 0.4577 0.2735 0.055 Uiso 1 1 calc R . .
C10 C 0.6961(2) 0.60421(19) 0.2210(2) 0.0451(9) Uani 1 1 d . . .
H10A H 0.6896 0.6099 0.1736 0.068 Uiso 1 1 calc R . .
H10B H 0.7520 0.6259 0.2487 0.068 Uiso 1 1 calc R . .
H10C H 0.6609 0.6320 0.2508 0.068 Uiso 1 1 calc R . .
C11 C 0.40332(17) 0.54845(17) 0.09210(17) 0.0294(6) Uani 1 1 d D . .
C12 C 0.3919(2) 0.6029(2) 0.16868(19) 0.0432(8) Uani 1 1 d D . .
H12A H 0.3594 0.6389 0.1620 0.065 Uiso 1 1 calc R . .
H12B H 0.4444 0.6325 0.2012 0.065 Uiso 1 1 calc R . .
H12C H 0.3646 0.5720 0.1915 0.065 Uiso 1 1 calc R . .
C13 C 0.32139(18) 0.50411(19) 0.04169(19) 0.0383(8) Uani 1 1 d D . .
H13A H 0.3281 0.4675 -0.0064 0.057 Uiso 1 1 calc R . .
H13B H 0.2909 0.5408 0.0336 0.057 Uiso 1 1 calc R . .
H13C H 0.2923 0.4755 0.0654 0.057 Uiso 1 1 calc R . .
C14 C 0.4454(2) 0.59682(19) 0.0562(2) 0.0399(8) Uani 1 1 d D . .
H14A H 0.4526 0.5622 0.0075 0.060 Uiso 1 1 calc R . .
H14B H 0.4979 0.6266 0.0887 0.060 Uiso 1 1 calc R . .
H14C H 0.4126 0.6326 0.0497 0.060 Uiso 1 1 calc R . .
C15 C 0.53913(16) 0.18729(16) -0.00768(15) 0.0239(6) Uani 1 1 d . . .
C16 C 0.56156(16) 0.13926(15) -0.07245(15) 0.0242(6) Uani 1 1 d . . .
C17 C 0.51958(17) 0.13185(16) -0.14079(16) 0.0277(6) Uani 1 1 d . . .
H17 H 0.5355 0.1009 -0.1845 0.033 Uiso 1 1 calc R . .
C18 C 0.45503(18) 0.16702(17) -0.14970(16) 0.0305(7) Uani 1 1 d . A .
C19 C 0.42991(17) 0.20902(16) -0.08571(16) 0.0279(6) Uani 1 1 d . . .
H19 H 0.3844 0.2310 -0.0896 0.033 Uiso 1 1 calc R . .
C20 C 0.47121(16) 0.21882(15) -0.01627(15) 0.0229(6) Uani 1 1 d . . .
C21 C 0.62760(17) 0.09431(17) -0.06672(16) 0.0284(6) Uani 1 1 d . . .
C22 C 0.5997(2) 0.03827(19) -0.03225(18) 0.0384(8) Uani 1 1 d . . .
H22A H 0.5949 0.0680 0.0190 0.058 Uiso 1 1 calc R . .
H22B H 0.6389 0.0060 -0.0316 0.058 Uiso 1 1 calc R . .
H22C H 0.5475 0.0049 -0.0621 0.058 Uiso 1 1 calc R . .
C23 C 0.70769(19) 0.1499(2) -0.0193(2) 0.0470(9) Uani 1 1 d . . .
H23A H 0.7218 0.1884 -0.0394 0.070 Uiso 1 1 calc R . .
H23B H 0.7498 0.1203 -0.0206 0.070 Uiso 1 1 calc R . .
H23C H 0.7026 0.1765 0.0324 0.070 Uiso 1 1 calc R . .
C24 C 0.6418(2) 0.0457(2) -0.14416(18) 0.0397(8) Uani 1 1 d . . .
H24A H 0.5916 0.0092 -0.1758 0.060 Uiso 1 1 calc R . .
H24B H 0.6829 0.0166 -0.1386 0.060 Uiso 1 1 calc R . .
H24C H 0.6598 0.0802 -0.1675 0.060 Uiso 1 1 calc R . .
C25 C 0.4115(2) 0.1550(2) -0.22776(18) 0.0488(9) Uani 1 1 d DU . .
C26 C 0.3263(4) 0.0978(4) -0.2398(5) 0.054(2) Uani 0.529(10) 1 d PDU A 1
H26A H 0.3361 0.0500 -0.2360 0.081 Uiso 0.529(10) 1 calc PR A 1
H26B H 0.2934 0.0849 -0.2894 0.081 Uiso 0.529(10) 1 calc PR A 1
H26C H 0.2979 0.1240 -0.2014 0.081 Uiso 0.529(10) 1 calc PR A 1
C27 C 0.3935(8) 0.2274(5) -0.2318(8) 0.047(3) Uani 0.529(10) 1 d PDU A 1
H27A H 0.3662 0.2159 -0.2829 0.071 Uiso 0.529(10) 1 calc PR A 1
H27B H 0.4437 0.2661 -0.2177 0.071 Uiso 0.529(10) 1 calc PR A 1
H27C H 0.3588 0.2479 -0.1975 0.071 Uiso 0.529(10) 1 calc PR A 1
C28 C 0.4443(6) 0.1016(6) -0.2897(4) 0.072(3) Uani 0.529(10) 1 d PDU A 1
H28A H 0.4565 0.0584 -0.2779 0.108 Uiso 0.529(10) 1 calc PR A 1
H28B H 0.4934 0.1305 -0.2944 0.108 Uiso 0.529(10) 1 calc PR A 1
H28C H 0.4043 0.0811 -0.3369 0.108 Uiso 0.529(10) 1 calc PR A 1
C26X C 0.3547(6) 0.0809(4) -0.2694(6) 0.059(3) Uani 0.471(10) 1 d PDU A 2
H26D H 0.3815 0.0386 -0.2712 0.088 Uiso 0.471(10) 1 calc PR A 2
H26E H 0.3345 0.0754 -0.3204 0.088 Uiso 0.471(10) 1 calc PR A 2
H26F H 0.3098 0.0789 -0.2448 0.088 Uiso 0.471(10) 1 calc PR A 2
C27X C 0.3754(7) 0.2245(5) -0.2222(7) 0.034(2) Uani 0.471(10) 1 d PDU A 2
H27D H 0.4168 0.2724 -0.1949 0.050 Uiso 0.471(10) 1 calc PR A 2
H27E H 0.3318 0.2257 -0.1956 0.050 Uiso 0.471(10) 1 calc PR A 2
H27F H 0.3543 0.2203 -0.2725 0.050 Uiso 0.471(10) 1 calc PR A 2
C28X C 0.4793(5) 0.1611(6) -0.2741(5) 0.053(3) Uani 0.471(10) 1 d PDU A 2
H28D H 0.5193 0.2098 -0.2456 0.080 Uiso 0.471(10) 1 calc PR A 2
H28E H 0.4544 0.1601 -0.3223 0.080 Uiso 0.471(10) 1 calc PR A 2
H28F H 0.5054 0.1170 -0.2827 0.080 Uiso 0.471(10) 1 calc PR A 2
C29 C 0.72522(16) 0.23180(15) 0.24147(15) 0.0217(6) Uani 1 1 d . . .
C30 C 0.80884(16) 0.25898(16) 0.27452(16) 0.0249(6) Uani 1 1 d . . .
C31 C 0.84167(16) 0.22862(17) 0.32283(16) 0.0268(6) Uani 1 1 d . . .
H31 H 0.8975 0.2469 0.3446 0.032 Uiso 1 1 calc R . .
C32 C 0.79938(17) 0.17351(16) 0.34207(15) 0.0244(6) Uani 1 1 d . . .
C33 C 0.71861(16) 0.14661(15) 0.30910(15) 0.0237(6) Uani 1 1 d . . .
H33 H 0.6873 0.1085 0.3198 0.028 Uiso 1 1 calc R . .
C34 C 0.68266(15) 0.17529(15) 0.25997(15) 0.0218(6) Uani 1 1 d . . .
C35 C 0.86006(17) 0.32190(19) 0.25940(18) 0.0340(7) Uani 1 1 d . . .
C36 C 0.8267(2) 0.39557(19) 0.2855(2) 0.0520(10) Uani 1 1 d . . .
H36A H 0.7720 0.3847 0.2563 0.078 Uiso 1 1 calc R . .
H36B H 0.8608 0.4367 0.2782 0.078 Uiso 1 1 calc R . .
H36C H 0.8259 0.4126 0.3386 0.078 Uiso 1 1 calc R . .
C37 C 0.8603(2) 0.2930(2) 0.1763(2) 0.0497(9) Uani 1 1 d . . .
H37A H 0.8801 0.2449 0.1603 0.074 Uiso 1 1 calc R . .
H37B H 0.8953 0.3326 0.1678 0.074 Uiso 1 1 calc R . .
H37C H 0.8056 0.2830 0.1475 0.074 Uiso 1 1 calc R . .
C38 C 0.9474(2) 0.3444(3) 0.3038(2) 0.0576(11) Uani 1 1 d . . .
H38A H 0.9483 0.3628 0.3573 0.086 Uiso 1 1 calc R . .
H38B H 0.9778 0.3858 0.2942 0.086 Uiso 1 1 calc R . .
H38C H 0.9716 0.2990 0.2880 0.086 Uiso 1 1 calc R . .
C39 C 0.84236(18) 0.14300(17) 0.39532(16) 0.0296(6) Uani 1 1 d . . .
C40 C 0.8963(2) 0.2110(2) 0.46520(18) 0.0463(9) Uani 1 1 d . . .
H40A H 0.9218 0.1908 0.4993 0.069 Uiso 1 1 calc R . .
H40B H 0.8637 0.2465 0.4905 0.069 Uiso 1 1 calc R . .
H40C H 0.9378 0.2390 0.4502 0.069 Uiso 1 1 calc R . .
C41 C 0.8925(3) 0.0895(3) 0.3535(2) 0.0671(13) Uani 1 1 d . . .
H41A H 0.8573 0.0452 0.3105 0.101 Uiso 1 1 calc R . .
H41B H 0.9218 0.0706 0.3870 0.101 Uiso 1 1 calc R . .
H41C H 0.9307 0.1179 0.3360 0.101 Uiso 1 1 calc R . .
C42 C 0.7832(2) 0.0989(2) 0.4233(2) 0.0487(9) Uani 1 1 d . . .
H42A H 0.7504 0.0524 0.3809 0.073 Uiso 1 1 calc R . .
H42B H 0.7484 0.1325 0.4473 0.073 Uiso 1 1 calc R . .
H42C H 0.8129 0.0835 0.4595 0.073 Uiso 1 1 calc R . .
C43 C 0.52276(15) 0.25965(16) 0.29267(15) 0.0230(6) Uani 1 1 d . . .
C44 C 0.48084(16) 0.30291(16) 0.34404(16) 0.0262(6) Uani 1 1 d . . .
C45 C 0.44547(17) 0.26574(18) 0.38411(17) 0.0311(7) Uani 1 1 d . . .
H45 H 0.4159 0.2934 0.4181 0.037 Uiso 1 1 calc R . .
C46 C 0.45013(17) 0.19116(18) 0.37827(17) 0.0326(7) Uani 1 1 d . . .
C47 C 0.49182(16) 0.15047(17) 0.32778(17) 0.0299(7) Uani 1 1 d . . .
H47 H 0.4966 0.0995 0.3217 0.036 Uiso 1 1 calc R . .
C48 C 0.52675(16) 0.18473(16) 0.28592(15) 0.0248(6) Uani 1 1 d . . .
C49 C 0.47744(18) 0.38682(17) 0.35691(16) 0.0300(7) Uani 1 1 d . . .
C50 C 0.4422(2) 0.3916(2) 0.28332(18) 0.0416(8) Uani 1 1 d . . .
H50A H 0.3901 0.3551 0.2601 0.062 Uiso 1 1 calc R . .
H50B H 0.4788 0.3782 0.2493 0.062 Uiso 1 1 calc R . .
H50C H 0.4353 0.4445 0.2937 0.062 Uiso 1 1 calc R . .
C51 C 0.4252(2) 0.4198(2) 0.4124(2) 0.0455(9) Uani 1 1 d . . .
H51A H 0.3701 0.3890 0.3922 0.068 Uiso 1 1 calc R . .
H51B H 0.4258 0.4739 0.4206 0.068 Uiso 1 1 calc R . .
H51C H 0.4465 0.4177 0.4600 0.068 Uiso 1 1 calc R . .
C52 C 0.56287(19) 0.43739(17) 0.38976(18) 0.0345(7) Uani 1 1 d . . .
H52A H 0.5623 0.4902 0.3941 0.041 Uiso 1 1 calc R . .
H52B H 0.5983 0.4153 0.3568 0.041 Uiso 1 1 calc R . .
H52C H 0.5825 0.4390 0.4393 0.041 Uiso 1 1 calc R . .
C53 C 0.4085(2) 0.1563(2) 0.4249(2) 0.0444(8) Uani 1 1 d . . .
C54 C 0.3182(2) 0.1376(3) 0.3949(3) 0.0815(16) Uani 1 1 d . . .
H54A H 0.3007 0.1853 0.3987 0.122 Uiso 1 1 calc R . .
H54B H 0.2908 0.1151 0.4242 0.122 Uiso 1 1 calc R . .
H54C H 0.3050 0.1003 0.3424 0.122 Uiso 1 1 calc R . .
C55 C 0.4284(3) 0.2131(3) 0.5067(2) 0.0889(18) Uani 1 1 d . . .
H55A H 0.4865 0.2256 0.5263 0.133 Uiso 1 1 calc R . .
H55B H 0.4011 0.1896 0.5354 0.133 Uiso 1 1 calc R . .
H55C H 0.4104 0.2608 0.5112 0.133 Uiso 1 1 calc R . .
C56 C 0.4329(4) 0.0809(3) 0.4203(4) 0.0976(19) Uani 1 1 d . . .
H56A H 0.4202 0.0433 0.3680 0.146 Uiso 1 1 calc R . .
H56B H 0.4035 0.0595 0.4493 0.146 Uiso 1 1 calc R . .
H56C H 0.4907 0.0916 0.4407 0.146 Uiso 1 1 calc R . .
V2 V 0.00094(3) 0.73857(3) 0.22504(2) 0.01987(11) Uani 1 1 d . . .
O9 O 0.00966(11) 0.83685(11) 0.22441(11) 0.0263(4) Uani 1 1 d . . .
O10 O 0.01160(11) 0.69378(11) 0.12863(10) 0.0262(4) Uani 1 1 d . . .
O11 O -0.12190(11) 0.71149(11) 0.17966(11) 0.0274(4) Uani 1 1 d . . .
O12 O -0.23755(11) 0.71233(12) 0.09121(11) 0.0305(5) Uani 1 1 d . . .
O13 O 0.10888(11) 0.75591(11) 0.27023(11) 0.0247(4) Uani 1 1 d . . .
O14 O -0.03027(11) 0.76550(11) 0.31452(10) 0.0246(4) Uani 1 1 d . . .
O15 O -0.01470(11) 0.62653(11) 0.22129(10) 0.0241(4) Uani 1 1 d . . .
O16 O 0.00116(12) 0.53750(11) 0.28249(11) 0.0304(5) Uani 1 1 d . . .
S3 S -0.15112(4) 0.73050(4) 0.11727(4) 0.02374(15) Uani 1 1 d . . .
S4 S 0.01002(4) 0.61647(4) 0.29062(4) 0.02186(15) Uani 1 1 d . . .
C57 C -0.03693(17) 0.87008(16) 0.19075(15) 0.0238(6) Uani 1 1 d . . .
C58 C -0.00917(17) 0.94800(16) 0.20250(15) 0.0261(6) Uani 1 1 d . . .
C59 C -0.06067(18) 0.98137(17) 0.16893(16) 0.0300(7) Uani 1 1 d . . .
H59 H -0.0422 1.0339 0.1770 0.036 Uiso 1 1 calc R . .
C60 C -0.13702(19) 0.94327(18) 0.12458(17) 0.0327(7) Uani 1 1 d . B .
C61 C -0.16223(17) 0.86601(17) 0.11117(16) 0.0284(6) Uani 1 1 d . . .
H61 H -0.2131 0.8373 0.0796 0.034 Uiso 1 1 calc R . .
C62 C -0.11331(16) 0.83011(16) 0.14373(15) 0.0231(6) Uani 1 1 d . . .
C63 C 0.07540(17) 0.99412(17) 0.24968(17) 0.0314(7) Uani 1 1 d . . .
C64 C 0.13861(19) 0.9521(2) 0.21341(19) 0.0390(8) Uani 1 1 d . . .
H64A H 0.1351 0.9511 0.1633 0.059 Uiso 1 1 calc R . .
H64B H 0.1284 0.8988 0.2098 0.059 Uiso 1 1 calc R . .
H64C H 0.1924 0.9799 0.2442 0.059 Uiso 1 1 calc R . .
C65 C 0.08290(19) 1.00138(19) 0.32970(18) 0.0395(8) Uani 1 1 d . . .
H65A H 0.1375 1.0288 0.3586 0.059 Uiso 1 1 calc R . .
H65B H 0.0717 0.9494 0.3295 0.059 Uiso 1 1 calc R . .
H65C H 0.0444 1.0306 0.3525 0.059 Uiso 1 1 calc R . .
C66 C 0.0930(2) 1.0764(2) 0.2527(2) 0.0532(10) Uani 1 1 d . . .
H66A H 0.0899 1.0736 0.2020 0.080 Uiso 1 1 calc R . .
H66B H 0.1470 1.1039 0.2833 0.080 Uiso 1 1 calc R . .
H66C H 0.0535 1.1045 0.2749 0.080 Uiso 1 1 calc R . .
C67 C -0.1919(2) 0.98362(19) 0.09014(19) 0.0449(9) Uani 1 1 d DU . .
C68 C -0.2764(3) 0.9740(3) 0.1140(3) 0.0575(15) Uani 0.774(6) 1 d PDU B 1
H68A H -0.3010 0.9187 0.0955 0.086 Uiso 0.774(6) 1 calc PR B 1
H68B H -0.3119 0.9994 0.0924 0.086 Uiso 0.774(6) 1 calc PR B 1
H68C H -0.2677 0.9982 0.1686 0.086 Uiso 0.774(6) 1 calc PR B 1
C69 C -0.1635(4) 1.0699(3) 0.1227(4) 0.0622(17) Uani 0.774(6) 1 d PDU B 1
H69A H -0.1543 1.0905 0.1773 0.093 Uiso 0.774(6) 1 calc PR B 1
H69B H -0.2042 1.0928 0.1039 0.093 Uiso 0.774(6) 1 calc PR B 1
H69C H -0.1133 1.0831 0.1084 0.093 Uiso 0.774(6) 1 calc PR B 1
C70 C -0.2085(4) 0.9440(3) 0.0079(2) 0.0596(18) Uani 0.774(6) 1 d PDU B 1
H70A H -0.2296 0.8883 -0.0079 0.089 Uiso 0.774(6) 1 calc PR B 1
H70B H -0.1588 0.9516 -0.0092 0.089 Uiso 0.774(6) 1 calc PR B 1
H70C H -0.2481 0.9658 -0.0140 0.089 Uiso 0.774(6) 1 calc PR B 1
C68X C -0.2652(10) 0.9254(9) 0.0319(10) 0.069(5) Uani 0.226(6) 1 d PDU B 2
H68D H -0.2525 0.8740 0.0108 0.104 Uiso 0.226(6) 1 calc PR B 2
H68E H -0.2792 0.9425 -0.0082 0.104 Uiso 0.226(6) 1 calc PR B 2
H68F H -0.3106 0.9225 0.0557 0.104 Uiso 0.226(6) 1 calc PR B 2
C69X C -0.2025(14) 1.0531(10) 0.1444(10) 0.070(6) Uani 0.226(6) 1 d PDU B 2
H69D H -0.2388 1.0761 0.1203 0.105 Uiso 0.226(6) 1 calc PR B 2
H69E H -0.1505 1.0897 0.1681 0.105 Uiso 0.226(6) 1 calc PR B 2
H69F H -0.2257 1.0419 0.1823 0.105 Uiso 0.226(6) 1 calc PR B 2
C70X C -0.1392(10) 1.0032(11) 0.0344(9) 0.060(4) Uani 0.226(6) 1 d PDU B 2
H70D H -0.1357 0.9545 -0.0054 0.090 Uiso 0.226(6) 1 calc PR B 2
H70E H -0.0851 1.0325 0.0631 0.090 Uiso 0.226(6) 1 calc PR B 2
H70F H -0.1654 1.0342 0.0123 0.090 Uiso 0.226(6) 1 calc PR B 2
C71 C -0.03030(16) 0.66763(15) 0.05824(15) 0.0225(6) Uani 1 1 d . . .
C72 C 0.00383(16) 0.62886(16) -0.00215(15) 0.0242(6) Uani 1 1 d . . .
C73 C -0.04251(17) 0.60607(17) -0.07347(16) 0.0285(6) Uani 1 1 d . . .
H73 H -0.0205 0.5795 -0.1147 0.034 Uiso 1 1 calc R . .
C74 C -0.11982(17) 0.61958(17) -0.08906(16) 0.0279(6) Uani 1 1 d . . .
C75 C -0.15200(16) 0.65757(16) -0.02892(15) 0.0243(6) Uani 1 1 d . . .
H75 H -0.2040 0.6679 -0.0370 0.029 Uiso 1 1 calc R . .
C76 C -0.10789(16) 0.68065(15) 0.04354(15) 0.0214(6) Uani 1 1 d . . .
C77 C 0.08994(17) 0.61605(18) 0.01055(17) 0.0303(7) Uani 1 1 d . . .
C78 C 0.10413(19) 0.5797(2) 0.06708(18) 0.0360(7) Uani 1 1 d . . .
H78A H 0.0996 0.6160 0.1162 0.054 Uiso 1 1 calc R . .
H78B H 0.1579 0.5686 0.0705 0.054 Uiso 1 1 calc R . .
H78C H 0.0639 0.5313 0.0506 0.054 Uiso 1 1 calc R . .
C79 C 0.1481(2) 0.6947(2) 0.0393(2) 0.0512(10) Uani 1 1 d . . .
H79A H 0.1435 0.7149 0.0006 0.077 Uiso 1 1 calc R . .
H79B H 0.2031 0.6885 0.0514 0.077 Uiso 1 1 calc R . .
H79C H 0.1351 0.7311 0.0842 0.077 Uiso 1 1 calc R . .
C80 C 0.1080(2) 0.5606(3) -0.06235(19) 0.0522(10) Uani 1 1 d . . .
H80A H 0.0691 0.5109 -0.0825 0.078 Uiso 1 1 calc R . .
H80B H 0.1623 0.5521 -0.0521 0.078 Uiso 1 1 calc R . .
H80C H 0.1041 0.5836 -0.0989 0.078 Uiso 1 1 calc R . .
C81 C -0.16593(19) 0.5889(2) -0.17071(17) 0.0380(8) Uani 1 1 d . . .
C82 C -0.2450(2) 0.6154(3) -0.17658(19) 0.0508(10) Uani 1 1 d . . .
H82A H -0.2790 0.5959 -0.1494 0.076 Uiso 1 1 calc R . .
H82B H -0.2725 0.5950 -0.2293 0.076 Uiso 1 1 calc R . .
H82C H -0.2342 0.6723 -0.1549 0.076 Uiso 1 1 calc R . .
C83 C -0.1148(2) 0.6178(3) -0.2152(2) 0.0573(11) Uani 1 1 d . . .
H83A H -0.1024 0.6747 -0.1935 0.086 Uiso 1 1 calc R . .
H83B H -0.1443 0.5979 -0.2673 0.086 Uiso 1 1 calc R . .
H83C H -0.0647 0.5993 -0.2136 0.086 Uiso 1 1 calc R . .
C84 C -0.1842(2) 0.4996(2) -0.20355(19) 0.0518(10) Uani 1 1 d . . .
H84A H -0.1338 0.4819 -0.2011 0.078 Uiso 1 1 calc R . .
H84B H -0.2135 0.4788 -0.2557 0.078 Uiso 1 1 calc R . .
H84C H -0.2170 0.4814 -0.1747 0.078 Uiso 1 1 calc R . .
C85 C 0.14758(15) 0.72698(16) 0.31386(15) 0.0223(6) Uani 1 1 d . . .
C86 C 0.23040(17) 0.76000(17) 0.34712(17) 0.0278(6) Uani 1 1 d . . .
C87 C 0.27006(17) 0.72922(17) 0.39155(17) 0.0296(7) Uani 1 1 d . . .
H87 H 0.3254 0.7514 0.4134 0.036 Uiso 1 1 calc R . .
C88 C 0.23418(18) 0.66786(16) 0.40640(16) 0.0293(7) Uani 1 1 d . C .
C89 C 0.15360(17) 0.63617(16) 0.37436(16) 0.0263(6) Uani 1 1 d . . .
H89 H 0.1269 0.5944 0.3832 0.032 Uiso 1 1 calc R . .
C90 C 0.11114(16) 0.66514(15) 0.32914(15) 0.0221(6) Uani 1 1 d . . .
C91 C 0.27485(18) 0.8281(2) 0.3347(2) 0.0389(8) Uani 1 1 d . . .
C92 C 0.2364(2) 0.89802(19) 0.3654(2) 0.0474(9) Uani 1 1 d . . .
H92A H 0.2622 0.9403 0.3541 0.071 Uiso 1 1 calc R . .
H92B H 0.2434 0.9156 0.4196 0.071 Uiso 1 1 calc R . .
H92C H 0.1790 0.8829 0.3420 0.071 Uiso 1 1 calc R . .
C93 C 0.2723(2) 0.8042(3) 0.2520(2) 0.0573(11) Uani 1 1 d . . .
H93A H 0.2960 0.7586 0.2334 0.086 Uiso 1 1 calc R . .
H93B H 0.3028 0.8471 0.2446 0.086 Uiso 1 1 calc R . .
H93C H 0.2165 0.7913 0.2247 0.086 Uiso 1 1 calc R . .
C94 C 0.3637(2) 0.8546(2) 0.3777(3) 0.0628(12) Uani 1 1 d . . .
H94A H 0.3914 0.8122 0.3583 0.094 Uiso 1 1 calc R . .
H94B H 0.3661 0.8684 0.4310 0.094 Uiso 1 1 calc R . .
H94C H 0.3896 0.9000 0.3710 0.094 Uiso 1 1 calc R . .
C95 C 0.2845(2) 0.63749(18) 0.45526(18) 0.0409(8) Uani 1 1 d DU . .
C96 C 0.3586(3) 0.6141(3) 0.4174(3) 0.0456(13) Uani 0.732(6) 1 d PDU C 1
H96A H 0.3890 0.6593 0.4135 0.068 Uiso 0.732(6) 1 calc PR C 1
H96B H 0.3381 0.5721 0.3674 0.068 Uiso 0.732(6) 1 calc PR C 1
H96C H 0.3937 0.5965 0.4482 0.068 Uiso 0.732(6) 1 calc PR C 1
C97 C 0.2408(3) 0.5690(3) 0.4598(3) 0.0563(17) Uani 0.732(6) 1 d PDU C 1
H97A H 0.2760 0.5525 0.4915 0.084 Uiso 0.732(6) 1 calc PR C 1
H97B H 0.2225 0.5270 0.4095 0.084 Uiso 0.732(6) 1 calc PR C 1
H97C H 0.1943 0.5814 0.4812 0.084 Uiso 0.732(6) 1 calc PR C 1
C98 C 0.3226(3) 0.7038(3) 0.5304(3) 0.0429(13) Uani 0.732(6) 1 d PDU C 1
H98A H 0.3508 0.7477 0.5230 0.064 Uiso 0.732(6) 1 calc PR C 1
H98B H 0.3608 0.6867 0.5592 0.064 Uiso 0.732(6) 1 calc PR C 1
H98C H 0.2808 0.7199 0.5578 0.064 Uiso 0.732(6) 1 calc PR C 1
C96X C 0.2770(8) 0.5501(5) 0.4155(7) 0.043(3) Uani 0.268(6) 1 d PDU C 2
H96D H 0.2231 0.5259 0.3836 0.064 Uiso 0.268(6) 1 calc PR C 2
H96E H 0.2861 0.5282 0.4526 0.064 Uiso 0.268(6) 1 calc PR C 2
H96F H 0.3170 0.5400 0.3846 0.064 Uiso 0.268(6) 1 calc PR C 2
C97X C 0.2333(7) 0.6353(8) 0.5197(6) 0.049(3) Uani 0.268(6) 1 d PDU C 2
H97D H 0.1788 0.6044 0.4950 0.073 Uiso 0.268(6) 1 calc PR C 2
H97E H 0.2310 0.6884 0.5518 0.073 Uiso 0.268(6) 1 calc PR C 2
H97F H 0.2602 0.6120 0.5501 0.073 Uiso 0.268(6) 1 calc PR C 2
C98X C 0.3626(8) 0.6868(9) 0.5028(11) 0.079(6) Uani 0.268(6) 1 d PDU C 2
H98D H 0.3880 0.6598 0.5302 0.119 Uiso 0.268(6) 1 calc PR C 2
H98E H 0.3543 0.7359 0.5385 0.119 Uiso 0.268(6) 1 calc PR C 2
H98F H 0.3974 0.6975 0.4715 0.119 Uiso 0.268(6) 1 calc PR C 2
C99 C -0.06460(15) 0.73260(15) 0.35456(15) 0.0216(6) Uani 1 1 d . . .
C100 C -0.11415(16) 0.76875(17) 0.40136(16) 0.0272(6) Uani 1 1 d . . .
C101 C -0.13891(17) 0.73374(18) 0.44676(16) 0.0320(7) Uani 1 1 d . . .
H101 H -0.1724 0.7573 0.4786 0.038 Uiso 1 1 calc R . .
C102 C -0.11825(18) 0.66661(19) 0.44899(16) 0.0327(7) Uani 1 1 d . . .
C103 C -0.07381(17) 0.62930(17) 0.39893(16) 0.0285(6) Uani 1 1 d . . .
H103 H -0.0611 0.5817 0.3964 0.034 Uiso 1 1 calc R . .
C104 C -0.04815(16) 0.66241(16) 0.35254(15) 0.0234(6) Uani 1 1 d . . .
C105 C -0.13412(18) 0.84636(18) 0.40641(17) 0.0340(7) Uani 1 1 d . . .
C106 C -0.1635(2) 0.8442(2) 0.32884(19) 0.0486(9) Uani 1 1 d . . .
H10D H -0.1828 0.8915 0.3340 0.073 Uiso 1 1 calc R . .
H10E H -0.2073 0.7986 0.3000 0.073 Uiso 1 1 calc R . .
H10F H -0.1192 0.8411 0.3029 0.073 Uiso 1 1 calc R . .
C107 C -0.0582(2) 0.91026(19) 0.4468(2) 0.0487(9) Uani 1 1 d . . .
H10G H -0.0160 0.8985 0.4188 0.073 Uiso 1 1 calc R . .
H10H H -0.0402 0.9130 0.4971 0.073 Uiso 1 1 calc R . .
H10I H -0.0697 0.9602 0.4505 0.073 Uiso 1 1 calc R . .
C108 C -0.1994(2) 0.8673(2) 0.4500(2) 0.0571(11) Uani 1 1 d . . .
H10J H -0.1805 0.8736 0.5015 0.086 Uiso 1 1 calc R . .
H10K H -0.2478 0.8256 0.4262 0.086 Uiso 1 1 calc R . .
H10L H -0.2117 0.9159 0.4504 0.086 Uiso 1 1 calc R . .
C109 C -0.1429(2) 0.6383(2) 0.50749(19) 0.0434(9) Uani 1 1 d . . .
C110 C -0.1127(2) 0.7055(2) 0.58530(18) 0.0495(9) Uani 1 1 d . . .
H11A H -0.1234 0.6869 0.6235 0.074 Uiso 1 1 calc R . .
H11B H -0.1406 0.7475 0.5883 0.074 Uiso 1 1 calc R . .
H11C H -0.0549 0.7249 0.5937 0.074 Uiso 1 1 calc R . .
C111 C -0.2344(2) 0.6134(3) 0.4919(2) 0.0661(13) Uani 1 1 d . . .
H11D H -0.2535 0.5677 0.4442 0.099 Uiso 1 1 calc R . .
H11E H -0.2585 0.6560 0.4893 0.099 Uiso 1 1 calc R . .
H11F H -0.2496 0.6006 0.5322 0.099 Uiso 1 1 calc R . .
C112 C -0.1053(3) 0.5712(2) 0.5083(2) 0.0580(11) Uani 1 1 d . . .
H11G H -0.1259 0.5263 0.4602 0.087 Uiso 1 1 calc R . .
H11H H -0.1188 0.5574 0.5485 0.087 Uiso 1 1 calc R . .
H11I H -0.0469 0.5868 0.5166 0.087 Uiso 1 1 calc R . .
N1 N 0.2488(2) 0.2704(3) 0.3012(3) 0.0886(14) Uani 1 1 d . . .
C113 C 0.2675(2) 0.2266(3) 0.2526(3) 0.0587(11) Uani 1 1 d . . .
C114 C 0.2924(3) 0.1711(3) 0.1922(3) 0.0834(15) Uani 1 1 d . . .
H11J H 0.3228 0.1402 0.2110 0.125 Uiso 1 1 calc R . .
H11K H 0.3265 0.1985 0.1705 0.125 Uiso 1 1 calc R . .
H11L H 0.2451 0.1367 0.1538 0.125 Uiso 1 1 calc R . .
N2 N -0.0779(6) 0.8475(7) -0.1100(5) 0.226(5) Uani 1 1 d . . .
C115 C -0.0363(5) 0.8428(5) -0.0609(4) 0.137(3) Uani 1 1 d . . .
C116 C 0.0093(3) 0.8335(3) -0.0033(3) 0.0783(14) Uani 1 1 d . . .
H11M H -0.0013 0.8673 0.0443 0.117 Uiso 1 1 calc R . .
H11N H 0.0663 0.8475 -0.0030 0.117 Uiso 1 1 calc R . .
H11O H -0.0046 0.7792 -0.0102 0.117 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 0.0202(2) 0.0216(2) 0.0192(2) 0.00923(19) -0.00012(18) 0.00776(18)
O1 0.0206(10) 0.0283(10) 0.0254(10) 0.0138(9) 0.0012(8) 0.0060(8)
O2 0.0256(10) 0.0378(12) 0.0221(10) 0.0094(9) -0.0004(8) 0.0141(9)
O3 0.0239(10) 0.0262(10) 0.0342(11) 0.0180(9) 0.0013(8) 0.0093(8)
O4 0.0206(10) 0.0336(11) 0.0353(12) 0.0164(10) 0.0003(9) 0.0078(8)
O5 0.0212(10) 0.0263(10) 0.0232(10) 0.0106(8) -0.0014(8) 0.0072(8)
O6 0.0218(10) 0.0260(10) 0.0225(10) 0.0090(8) 0.0007(8) 0.0073(8)
O7 0.0288(11) 0.0226(10) 0.0407(12) 0.0106(9) 0.0048(9) 0.0076(8)
O8 0.0338(12) 0.0254(11) 0.0441(13) 0.0144(10) -0.0003(10) 0.0044(9)
S1 0.0188(3) 0.0239(3) 0.0241(4) 0.0107(3) 0.0006(3) 0.0063(3)
S2 0.0201(3) 0.0208(3) 0.0312(4) 0.0048(3) 0.0004(3) 0.0048(3)
C1 0.0261(14) 0.0263(14) 0.0244(14) 0.0148(12) 0.0054(11) 0.0128(12)
C2 0.0249(14) 0.0273(14) 0.0238(14) 0.0119(12) 0.0030(11) 0.0104(12)
C3 0.0298(15) 0.0230(14) 0.0306(16) 0.0125(12) 0.0052(12) 0.0087(12)
C4 0.0283(15) 0.0299(15) 0.0270(15) 0.0141(13) 0.0073(12) 0.0152(12)
C5 0.0218(14) 0.0277(14) 0.0248(14) 0.0113(12) 0.0028(11) 0.0104(12)
C6 0.0239(14) 0.0225(13) 0.0200(13) 0.0088(11) 0.0035(11) 0.0069(11)
C7 0.0204(14) 0.0258(15) 0.0349(17) 0.0118(13) -0.0007(12) 0.0031(12)
C8 0.0258(16) 0.0434(19) 0.0441(19) 0.0227(16) 0.0066(14) 0.0092(14)
C9 0.0323(17) 0.0409(18) 0.0314(17) 0.0124(15) -0.0003(13) 0.0067(14)
C10 0.0312(18) 0.0312(17) 0.065(2) 0.0190(17) -0.0043(16) 0.0019(14)
C11 0.0286(15) 0.0277(15) 0.0374(17) 0.0161(13) 0.0072(13) 0.0149(12)
C12 0.042(2) 0.0431(19) 0.048(2) 0.0147(17) 0.0143(16) 0.0247(16)
C13 0.0294(17) 0.0414(18) 0.050(2) 0.0243(16) 0.0026(15) 0.0174(14)
C14 0.0380(18) 0.0399(18) 0.051(2) 0.0275(17) 0.0057(16) 0.0154(15)
C15 0.0215(14) 0.0241(14) 0.0236(14) 0.0103(12) -0.0025(11) 0.0036(11)
C16 0.0230(14) 0.0218(13) 0.0260(15) 0.0091(12) 0.0027(11) 0.0045(11)
C17 0.0314(16) 0.0250(14) 0.0243(15) 0.0087(12) 0.0022(12) 0.0072(12)
C18 0.0352(17) 0.0282(15) 0.0257(15) 0.0100(13) -0.0027(13) 0.0120(13)
C19 0.0258(15) 0.0262(15) 0.0297(16) 0.0119(13) -0.0037(12) 0.0088(12)
C20 0.0226(14) 0.0206(13) 0.0228(14) 0.0082(11) -0.0001(11) 0.0036(11)
C21 0.0224(14) 0.0290(15) 0.0308(16) 0.0087(13) 0.0021(12) 0.0106(12)
C22 0.047(2) 0.0388(18) 0.0372(18) 0.0198(15) 0.0078(15) 0.0211(15)
C23 0.0240(17) 0.047(2) 0.058(2) 0.0113(18) 0.0020(16) 0.0075(15)
C24 0.0379(18) 0.0441(19) 0.0413(19) 0.0159(16) 0.0132(15) 0.0225(15)
C25 0.063(2) 0.055(2) 0.0233(17) 0.0090(16) -0.0042(16) 0.0307(18)
C26 0.061(4) 0.032(3) 0.051(4) 0.009(3) -0.023(3) 0.017(3)
C27 0.054(5) 0.052(4) 0.038(4) 0.028(3) 0.000(4) 0.002(3)
C28 0.085(5) 0.083(5) 0.043(4) 0.020(3) 0.002(3) 0.036(4)
C26X 0.074(5) 0.044(4) 0.048(4) 0.016(3) -0.009(3) 0.013(3)
C27X 0.037(4) 0.041(4) 0.029(4) 0.024(3) 0.000(3) 0.006(3)
C28X 0.056(4) 0.077(5) 0.035(4) 0.027(3) 0.010(3) 0.027(3)
C29 0.0220(14) 0.0212(13) 0.0219(14) 0.0085(11) 0.0012(11) 0.0095(11)
C30 0.0237(14) 0.0268(14) 0.0259(15) 0.0124(12) 0.0034(11) 0.0077(12)
C31 0.0185(14) 0.0320(15) 0.0283(15) 0.0129(13) -0.0017(11) 0.0063(12)
C32 0.0262(14) 0.0246(14) 0.0232(14) 0.0092(12) 0.0042(11) 0.0113(12)
C33 0.0252(14) 0.0203(13) 0.0273(15) 0.0100(12) 0.0067(12) 0.0089(11)
C34 0.0169(13) 0.0192(13) 0.0245(14) 0.0047(11) 0.0003(11) 0.0063(10)
C35 0.0220(15) 0.0429(18) 0.0409(18) 0.0280(16) -0.0042(13) -0.0006(13)
C36 0.047(2) 0.0306(18) 0.071(3) 0.0241(18) -0.0059(19) -0.0036(16)
C37 0.041(2) 0.071(3) 0.053(2) 0.043(2) 0.0127(17) 0.0060(18)
C38 0.0257(18) 0.084(3) 0.076(3) 0.061(3) -0.0062(18) -0.0078(18)
C39 0.0320(16) 0.0335(16) 0.0273(15) 0.0157(13) 0.0034(12) 0.0130(13)
C40 0.047(2) 0.055(2) 0.0327(18) 0.0239(17) -0.0132(15) 0.0024(17)
C41 0.094(3) 0.092(3) 0.050(2) 0.042(2) 0.029(2) 0.074(3)
C42 0.048(2) 0.055(2) 0.053(2) 0.040(2) -0.0013(17) 0.0055(18)
C43 0.0161(13) 0.0274(14) 0.0212(14) 0.0082(12) -0.0033(10) 0.0048(11)
C44 0.0213(14) 0.0289(15) 0.0239(14) 0.0075(12) -0.0007(11) 0.0071(12)
C45 0.0223(15) 0.0390(17) 0.0277(16) 0.0087(14) 0.0049(12) 0.0079(13)
C46 0.0222(15) 0.0371(17) 0.0355(17) 0.0161(14) -0.0003(13) 0.0004(13)
C47 0.0210(14) 0.0273(15) 0.0368(17) 0.0125(13) -0.0007(12) 0.0003(12)
C48 0.0188(13) 0.0249(14) 0.0250(14) 0.0057(12) 0.0002(11) 0.0052(11)
C49 0.0319(16) 0.0299(16) 0.0264(15) 0.0075(13) 0.0042(12) 0.0156(13)
C50 0.050(2) 0.0404(19) 0.0374(19) 0.0161(15) 0.0014(16) 0.0275(16)
C51 0.050(2) 0.0391(19) 0.047(2) 0.0098(16) 0.0198(17) 0.0220(16)
C52 0.0428(19) 0.0271(16) 0.0335(17) 0.0113(14) 0.0079(14) 0.0107(14)
C53 0.0351(19) 0.051(2) 0.049(2) 0.0250(18) 0.0120(16) -0.0011(16)
C54 0.041(2) 0.122(4) 0.083(3) 0.058(3) 0.012(2) -0.017(3)
C55 0.113(4) 0.092(4) 0.047(3) 0.031(3) 0.017(3) -0.027(3)
C56 0.118(5) 0.094(4) 0.139(5) 0.088(4) 0.075(4) 0.037(3)
V2 0.0192(2) 0.0246(2) 0.0189(2) 0.01145(19) 0.00197(18) 0.00926(19)
O9 0.0246(10) 0.0272(10) 0.0318(11) 0.0185(9) 0.0002(8) 0.0081(8)
O10 0.0242(10) 0.0368(11) 0.0209(10) 0.0135(9) 0.0038(8) 0.0123(9)
O11 0.0224(10) 0.0332(11) 0.0278(11) 0.0131(9) 0.0043(8) 0.0089(8)
O12 0.0228(10) 0.0373(12) 0.0318(11) 0.0141(10) 0.0038(9) 0.0102(9)
O13 0.0188(9) 0.0310(10) 0.0295(11) 0.0192(9) 0.0004(8) 0.0068(8)
O14 0.0274(10) 0.0239(10) 0.0232(10) 0.0098(8) 0.0072(8) 0.0058(8)
O15 0.0252(10) 0.0242(10) 0.0208(10) 0.0076(8) 0.0007(8) 0.0083(8)
O16 0.0341(11) 0.0220(10) 0.0348(12) 0.0138(9) 0.0010(9) 0.0056(9)
S3 0.0243(4) 0.0240(3) 0.0257(4) 0.0109(3) 0.0085(3) 0.0085(3)
S4 0.0209(3) 0.0211(3) 0.0220(3) 0.0085(3) 0.0006(3) 0.0050(3)
C57 0.0277(15) 0.0267(14) 0.0213(14) 0.0126(12) 0.0044(11) 0.0127(12)
C58 0.0280(15) 0.0278(15) 0.0227(14) 0.0113(12) 0.0016(12) 0.0079(12)
C59 0.0378(17) 0.0224(14) 0.0305(16) 0.0131(13) 0.0013(13) 0.0083(13)
C60 0.0362(17) 0.0317(16) 0.0322(17) 0.0175(14) -0.0031(13) 0.0119(13)
C61 0.0276(15) 0.0286(15) 0.0250(15) 0.0091(12) -0.0025(12) 0.0080(12)
C62 0.0278(15) 0.0229(14) 0.0222(14) 0.0116(12) 0.0060(11) 0.0098(11)
C63 0.0235(15) 0.0282(15) 0.0367(17) 0.0119(14) -0.0039(13) 0.0034(12)
C64 0.0290(17) 0.047(2) 0.0429(19) 0.0224(16) 0.0050(14) 0.0058(15)
C65 0.0329(17) 0.0392(18) 0.0346(18) 0.0056(15) -0.0032(14) 0.0102(14)
C66 0.038(2) 0.0372(19) 0.076(3) 0.0256(19) -0.0088(19) -0.0021(16)
C67 0.048(2) 0.0364(18) 0.047(2) 0.0204(16) -0.0137(16) 0.0151(16)
C68 0.058(3) 0.073(4) 0.064(3) 0.040(3) 0.017(3) 0.044(3)
C69 0.077(5) 0.046(3) 0.066(4) 0.028(3) -0.009(3) 0.031(3)
C70 0.080(4) 0.083(4) 0.032(2) 0.027(2) 0.009(2) 0.059(3)
C68X 0.070(6) 0.066(6) 0.075(7) 0.037(5) -0.004(4) 0.021(4)
C69X 0.089(17) 0.069(11) 0.077(12) 0.040(7) 0.024(9) 0.061(11)
C70X 0.063(6) 0.062(6) 0.062(6) 0.031(5) 0.003(4) 0.032(4)
C71 0.0271(14) 0.0218(13) 0.0218(14) 0.0124(11) 0.0037(11) 0.0067(11)
C72 0.0231(14) 0.0291(15) 0.0266(15) 0.0157(12) 0.0064(11) 0.0116(12)
C73 0.0278(15) 0.0387(17) 0.0254(15) 0.0147(13) 0.0106(12) 0.0170(13)
C74 0.0242(15) 0.0370(16) 0.0247(15) 0.0129(13) 0.0054(12) 0.0128(13)
C75 0.0197(13) 0.0299(15) 0.0277(15) 0.0138(12) 0.0064(11) 0.0116(11)
C76 0.0245(14) 0.0223(13) 0.0222(14) 0.0111(11) 0.0084(11) 0.0106(11)
C77 0.0227(15) 0.0441(18) 0.0291(16) 0.0179(14) 0.0056(12) 0.0146(13)
C78 0.0314(17) 0.051(2) 0.0373(18) 0.0252(16) 0.0083(14) 0.0238(15)
C79 0.0253(17) 0.071(3) 0.068(3) 0.045(2) 0.0065(17) 0.0048(17)
C80 0.0370(19) 0.091(3) 0.040(2) 0.027(2) 0.0154(16) 0.040(2)
C81 0.0296(16) 0.064(2) 0.0218(15) 0.0153(15) 0.0044(13) 0.0231(16)
C82 0.040(2) 0.087(3) 0.0290(18) 0.0222(19) 0.0027(15) 0.034(2)
C83 0.046(2) 0.106(3) 0.0327(19) 0.038(2) 0.0098(16) 0.027(2)
C84 0.041(2) 0.067(3) 0.0303(18) 0.0030(18) -0.0021(15) 0.0193(18)
C85 0.0188(13) 0.0262(14) 0.0239(14) 0.0118(12) 0.0012(11) 0.0103(11)
C86 0.0232(14) 0.0297(15) 0.0333(16) 0.0164(13) 0.0016(12) 0.0092(12)
C87 0.0211(14) 0.0297(15) 0.0352(17) 0.0136(13) -0.0058(12) 0.0088(12)
C88 0.0321(16) 0.0245(14) 0.0281(15) 0.0108(13) -0.0068(12) 0.0104(12)
C89 0.0306(15) 0.0218(14) 0.0275(15) 0.0125(12) -0.0003(12) 0.0086(12)
C90 0.0194(13) 0.0233(14) 0.0216(14) 0.0082(11) -0.0005(11) 0.0069(11)
C91 0.0193(15) 0.0466(19) 0.060(2) 0.0360(18) 0.0002(14) 0.0022(14)
C92 0.041(2) 0.0342(18) 0.065(2) 0.0275(18) -0.0058(18) 0.0009(15)
C93 0.041(2) 0.081(3) 0.073(3) 0.052(2) 0.022(2) 0.016(2)
C94 0.0255(18) 0.069(3) 0.102(3) 0.058(3) -0.008(2) -0.0069(18)
C95 0.0441(19) 0.0332(16) 0.0383(18) 0.0141(14) -0.0148(14) 0.0134(14)
C96 0.051(3) 0.045(3) 0.044(3) 0.020(2) -0.001(2) 0.029(2)
C97 0.051(3) 0.051(3) 0.070(4) 0.043(3) -0.019(3) 0.003(2)
C98 0.048(3) 0.041(3) 0.031(2) 0.0123(19) -0.013(2) 0.015(2)
C96X 0.052(8) 0.047(4) 0.044(7) 0.026(5) 0.007(5) 0.037(5)
C97X 0.072(8) 0.050(8) 0.035(6) 0.024(6) -0.002(5) 0.038(6)
C98X 0.058(7) 0.067(8) 0.113(14) 0.067(9) -0.040(7) -0.008(7)
C99 0.0177(13) 0.0253(14) 0.0200(13) 0.0092(11) 0.0013(10) 0.0018(11)
C100 0.0217(14) 0.0292(15) 0.0231(14) 0.0050(12) 0.0025(11) 0.0017(12)
C101 0.0252(15) 0.0395(18) 0.0246(15) 0.0072(13) 0.0083(12) 0.0011(13)
C102 0.0255(15) 0.0430(18) 0.0237(15) 0.0134(14) 0.0018(12) -0.0060(13)
C103 0.0267(15) 0.0282(15) 0.0266(15) 0.0122(13) -0.0008(12) -0.0018(12)
C104 0.0192(13) 0.0269(14) 0.0210(14) 0.0087(12) 0.0020(11) 0.0018(11)
C105 0.0316(17) 0.0351(17) 0.0320(17) 0.0078(14) 0.0098(13) 0.0116(14)
C106 0.055(2) 0.051(2) 0.041(2) 0.0141(17) 0.0057(17) 0.0334(18)
C107 0.053(2) 0.0313(18) 0.049(2) 0.0070(16) 0.0021(18) 0.0068(16)
C108 0.059(2) 0.057(2) 0.064(3) 0.019(2) 0.035(2) 0.033(2)
C109 0.0395(19) 0.058(2) 0.0332(18) 0.0242(17) 0.0085(15) -0.0054(16)
C110 0.046(2) 0.069(3) 0.0304(18) 0.0216(18) 0.0070(16) 0.0008(18)
C111 0.042(2) 0.103(4) 0.047(2) 0.040(2) 0.0043(18) -0.022(2)
C112 0.078(3) 0.053(2) 0.047(2) 0.031(2) 0.017(2) -0.004(2)
N1 0.062(3) 0.106(4) 0.086(3) 0.023(3) 0.027(2) 0.017(2)
C113 0.041(2) 0.077(3) 0.055(3) 0.028(2) 0.0051(19) 0.009(2)
C114 0.096(4) 0.079(3) 0.056(3) 0.013(3) 0.013(3) 0.009(3)
N2 0.255(10) 0.357(13) 0.168(7) 0.171(8) 0.061(7) 0.184(10)
C115 0.151(7) 0.228(9) 0.125(6) 0.128(7) 0.076(5) 0.115(7)
C116 0.081(3) 0.100(4) 0.069(3) 0.055(3) 0.019(3) 0.008(3)

_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 O2 1.816(2) . ?
V1 O6 1.8520(19) . ?
V1 O5 1.8755(18) . ?
V1 O3 1.8765(19) . ?
V1 O1 2.0931(18) . ?
V1 O7 2.100(2) . ?
O1 S1 1.4781(19) . ?
O2 C15 1.337(3) . ?
O3 C1 1.348(3) . ?
O4 S1 1.4389(19) . ?
O5 C29 1.342(3) . ?
O6 C43 1.341(3) . ?
O7 S2 1.438(2) . ?
O8 S2 1.444(2) . ?
S1 C6 1.754(3) . ?
S1 C20 1.754(3) . ?
S2 C48 1.749(3) . ?
S2 C34 1.753(3) . ?
C1 C6 1.407(4) . ?
C1 C2 1.428(4) . ?
C2 C3 1.393(4) . ?
C2 C7 1.530(4) . ?
C3 C4 1.403(4) . ?
C4 C5 1.373(4) . ?
C4 C11 1.543(4) . ?
C5 C6 1.398(4) . ?
C7 C9 1.530(4) . ?
C7 C8 1.535(4) . ?
C7 C10 1.541(4) . ?
C11 C13 1.520(4) . ?
C11 C14 1.532(4) . ?
C11 C12 1.539(4) . ?
C15 C20 1.410(4) . ?
C15 C16 1.411(4) . ?
C16 C17 1.385(4) . ?
C16 C21 1.538(4) . ?
C17 C18 1.404(4) . ?
C18 C19 1.389(4) . ?
C18 C25 1.535(4) . ?
C19 C20 1.385(4) . ?
C21 C22 1.533(4) . ?
C21 C23 1.535(4) . ?
C21 C24 1.540(4) . ?
C25 C26X 1.454(6) . ?
C25 C27 1.487(7) . ?
C25 C28 1.513(6) . ?
C25 C27X 1.518(7) . ?
C25 C28X 1.609(6) . ?
C25 C26 1.627(6) . ?
C29 C34 1.411(4) . ?
C29 C30 1.425(4) . ?
C30 C31 1.391(4) . ?
C30 C35 1.536(4) . ?
C31 C32 1.397(4) . ?
C32 C33 1.381(4) . ?
C32 C39 1.539(4) . ?
C33 C34 1.400(4) . ?
C35 C37 1.527(5) . ?
C35 C36 1.530(5) . ?
C35 C38 1.538(4) . ?
C39 C41 1.517(4) . ?
C39 C42 1.527(4) . ?
C39 C40 1.541(4) . ?
C43 C48 1.397(4) . ?
C43 C44 1.411(4) . ?
C44 C45 1.399(4) . ?
C44 C49 1.533(4) . ?
C45 C46 1.398(4) . ?
C46 C47 1.380(4) . ?
C46 C53 1.531(4) . ?
C47 C48 1.389(4) . ?
C49 C51 1.533(4) . ?
C49 C52 1.536(4) . ?
C49 C50 1.538(4) . ?
C53 C55 1.522(6) . ?
C53 C54 1.523(5) . ?
C53 C56 1.529(6) . ?
V2 O10 1.8235(19) . ?
V2 O14 1.8365(19) . ?
V2 O9 1.8644(19) . ?
V2 O13 1.8687(18) . ?
V2 O11 2.0846(19) . ?
V2 O15 2.0868(19) . ?
O9 C57 1.344(3) . ?
O10 C71 1.338(3) . ?
O11 S3 1.459(2) . ?
O12 S3 1.450(2) . ?
O13 C85 1.342(3) . ?
O14 C99 1.337(3) . ?
O15 S4 1.4710(19) . ?
O16 S4 1.4355(19) . ?
S3 C76 1.751(3) . ?
S3 C62 1.759(3) . ?
S4 C104 1.755(3) . ?
S4 C90 1.759(3) . ?
C57 C58 1.411(4) . ?
C57 C62 1.413(4) . ?
C58 C59 1.397(4) . ?
C58 C63 1.544(4) . ?
C59 C60 1.391(4) . ?
C60 C61 1.384(4) . ?
C60 C67 1.543(4) . ?
C61 C62 1.394(4) . ?
C63 C65 1.524(4) . ?
C63 C66 1.532(4) . ?
C63 C64 1.547(4) . ?
C67 C69X 1.410(12) . ?
C67 C70 1.476(5) . ?
C67 C69 1.494(6) . ?
C67 C68X 1.535(12) . ?
C67 C68 1.604(6) . ?
C67 C70X 1.645(12) . ?
C71 C76 1.406(4) . ?
C71 C72 1.410(4) . ?
C72 C73 1.389(4) . ?
C72 C77 1.541(4) . ?
C73 C74 1.408(4) . ?
C74 C75 1.382(4) . ?
C74 C81 1.538(4) . ?
C75 C76 1.393(4) . ?
C77 C79 1.527(5) . ?
C77 C78 1.536(4) . ?
C77 C80 1.539(4) . ?
C81 C83 1.526(5) . ?
C81 C82 1.527(4) . ?
C81 C84 1.536(5) . ?
C85 C90 1.413(4) . ?
C85 C86 1.423(4) . ?
C86 C87 1.387(4) . ?
C86 C91 1.534(4) . ?
C87 C88 1.396(4) . ?
C88 C89 1.382(4) . ?
C88 C95 1.535(4) . ?
C89 C90 1.396(4) . ?
C91 C93 1.517(5) . ?
C91 C92 1.531(5) . ?
C91 C94 1.549(4) . ?
C95 C97 1.452(5) . ?
C95 C98X 1.476(10) . ?
C95 C98 1.513(5) . ?
C95 C96X 1.524(9) . ?
C95 C96 1.609(5) . ?
C95 C97X 1.668(10) . ?
C99 C104 1.396(4) . ?
C99 C100 1.409(4) . ?
C100 C101 1.389(4) . ?
C100 C105 1.538(4) . ?
C101 C102 1.393(4) . ?
C102 C103 1.387(4) . ?
C102 C109 1.542(4) . ?
C103 C104 1.388(4) . ?
C105 C108 1.526(4) . ?
C105 C107 1.527(5) . ?
C105 C106 1.531(5) . ?
C109 C112 1.519(5) . ?
C109 C111 1.531(5) . ?
C109 C110 1.536(5) . ?
N1 C113 1.135(5) . ?
C113 C114 1.434(6) . ?
N2 C115 1.163(9) . ?
C115 C116 1.374(8) . ?

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
O2 V1 O6 164.64(9) . . ?
O2 V1 O5 97.34(8) . . ?
O6 V1 O5 92.17(8) . . ?
O2 V1 O3 95.01(9) . . ?
O6 V1 O3 96.04(9) . . ?
O5 V1 O3 95.54(8) . . ?
O2 V1 O1 84.23(8) . . ?
O6 V1 O1 85.31(8) . . ?
O5 V1 O1 174.94(8) . . ?
O3 V1 O1 89.10(8) . . ?
O2 V1 O7 82.54(9) . . ?
O6 V1 O7 85.85(8) . . ?
O5 V1 O7 87.67(8) . . ?
O3 V1 O7 176.20(8) . . ?
O1 V1 O7 87.77(8) . . ?
S1 O1 V1 119.33(11) . . ?
C15 O2 V1 140.20(18) . . ?
C1 O3 V1 136.11(18) . . ?
C29 O5 V1 131.32(17) . . ?
C43 O6 V1 138.12(17) . . ?
S2 O7 V1 119.39(12) . . ?
O4 S1 O1 115.30(12) . . ?
O4 S1 C6 109.33(12) . . ?
O1 S1 C6 107.30(12) . . ?
O4 S1 C20 108.73(12) . . ?
O1 S1 C20 107.11(12) . . ?
C6 S1 C20 108.90(13) . . ?
O7 S2 O8 116.23(12) . . ?
O7 S2 C48 106.76(13) . . ?
O8 S2 C48 108.54(14) . . ?
O7 S2 C34 107.82(13) . . ?
O8 S2 C34 109.24(12) . . ?
C48 S2 C34 107.97(13) . . ?
O3 C1 C6 122.5(2) . . ?
O3 C1 C2 119.7(2) . . ?
C6 C1 C2 117.8(2) . . ?
C3 C2 C1 116.6(2) . . ?
C3 C2 C7 121.6(3) . . ?
C1 C2 C7 121.8(2) . . ?
C2 C3 C4 125.5(3) . . ?
C5 C4 C3 117.0(2) . . ?
C5 C4 C11 122.9(3) . . ?
C3 C4 C11 120.1(3) . . ?
C4 C5 C6 119.9(3) . . ?
C5 C6 C1 123.1(2) . . ?
C5 C6 S1 116.4(2) . . ?
C1 C6 S1 120.5(2) . . ?
C2 C7 C9 109.3(2) . . ?
C2 C7 C8 110.2(2) . . ?
C9 C7 C8 111.0(2) . . ?
C2 C7 C10 112.3(2) . . ?
C9 C7 C10 107.1(3) . . ?
C8 C7 C10 106.9(3) . . ?
C13 C11 C14 108.5(3) . . ?
C13 C11 C12 108.9(3) . . ?
C14 C11 C12 109.4(3) . . ?
C13 C11 C4 111.8(2) . . ?
C14 C11 C4 110.3(2) . . ?
C12 C11 C4 107.8(2) . . ?
O2 C15 C20 121.3(3) . . ?
O2 C15 C16 120.2(2) . . ?
C20 C15 C16 118.6(2) . . ?
C17 C16 C15 117.4(2) . . ?
C17 C16 C21 121.8(3) . . ?
C15 C16 C21 120.7(2) . . ?
C16 C17 C18 124.3(3) . . ?
C19 C18 C17 117.3(3) . . ?
C19 C18 C25 121.9(3) . . ?
C17 C18 C25 120.8(3) . . ?
C20 C19 C18 120.0(3) . . ?
C19 C20 C15 122.1(3) . . ?
C19 C20 S1 117.1(2) . . ?
C15 C20 S1 120.7(2) . . ?
C22 C21 C23 110.8(3) . . ?
C22 C21 C16 107.9(2) . . ?
C23 C21 C16 111.1(2) . . ?
C22 C21 C24 107.8(3) . . ?
C23 C21 C24 107.5(3) . . ?
C16 C21 C24 111.7(2) . . ?
C26X C25 C27 120.8(7) . . ?
C27 C25 C28 118.6(6) . . ?
C26X C25 C27X 113.4(6) . . ?
C26X C25 C18 114.8(5) . . ?
C27 C25 C18 113.5(6) . . ?
C28 C25 C18 112.9(4) . . ?
C27X C25 C18 109.6(5) . . ?
C26X C25 C28X 108.6(6) . . ?
C27X C25 C28X 102.6(6) . . ?
C18 C25 C28X 107.0(4) . . ?
C27 C25 C26 107.4(6) . . ?
C28 C25 C26 99.5(5) . . ?
C18 C25 C26 102.3(4) . . ?
C28X C25 C26 138.1(5) . . ?
O5 C29 C34 123.9(2) . . ?
O5 C29 C30 119.1(2) . . ?
C34 C29 C30 116.9(2) . . ?
C31 C30 C29 117.7(3) . . ?
C31 C30 C35 121.3(2) . . ?
C29 C30 C35 120.9(2) . . ?
C30 C31 C32 125.4(3) . . ?
C33 C32 C31 116.6(2) . . ?
C33 C32 C39 122.4(3) . . ?
C31 C32 C39 120.9(2) . . ?
C32 C33 C34 120.2(3) . . ?
C33 C34 C29 123.1(2) . . ?
C33 C34 S2 113.3(2) . . ?
C29 C34 S2 123.6(2) . . ?
C37 C35 C36 110.7(3) . . ?
C37 C35 C30 110.3(3) . . ?
C36 C35 C30 109.2(3) . . ?
C37 C35 C38 108.4(3) . . ?
C36 C35 C38 106.7(3) . . ?
C30 C35 C38 111.6(2) . . ?
C41 C39 C42 109.5(3) . . ?
C41 C39 C32 108.1(2) . . ?
C42 C39 C32 112.0(2) . . ?
C41 C39 C40 110.2(3) . . ?
C42 C39 C40 106.5(3) . . ?
C32 C39 C40 110.5(2) . . ?
O6 C43 C48 119.2(2) . . ?
O6 C43 C44 121.9(2) . . ?
C48 C43 C44 118.8(3) . . ?
C45 C44 C43 116.1(3) . . ?
C45 C44 C49 122.4(3) . . ?
C43 C44 C49 121.5(3) . . ?
C46 C45 C44 125.3(3) . . ?
C47 C46 C45 117.2(3) . . ?
C47 C46 C53 122.1(3) . . ?
C45 C46 C53 120.7(3) . . ?
C46 C47 C48 119.3(3) . . ?
C47 C48 C43 123.2(3) . . ?
C47 C48 S2 118.8(2) . . ?
C43 C48 S2 117.9(2) . . ?
C51 C49 C44 111.6(3) . . ?
C51 C49 C52 108.0(3) . . ?
C44 C49 C52 108.6(2) . . ?
C51 C49 C50 107.7(3) . . ?
C44 C49 C50 110.9(2) . . ?
C52 C49 C50 109.9(3) . . ?
C55 C53 C54 109.1(4) . . ?
C55 C53 C56 108.2(4) . . ?
C54 C53 C56 107.8(4) . . ?
C55 C53 C46 111.0(3) . . ?
C54 C53 C46 108.6(3) . . ?
C56 C53 C46 112.1(3) . . ?
O10 V2 O14 166.83(9) . . ?
O10 V2 O9 92.96(9) . . ?
O14 V2 O9 95.25(9) . . ?
O10 V2 O13 96.75(9) . . ?
O14 V2 O13 92.84(9) . . ?
O9 V2 O13 94.54(8) . . ?
O10 V2 O11 85.72(8) . . ?
O14 V2 O11 83.93(8) . . ?
O9 V2 O11 90.54(8) . . ?
O13 V2 O11 174.22(8) . . ?
O10 V2 O15 85.70(8) . . ?
O14 V2 O15 85.56(8) . . ?
O9 V2 O15 176.84(8) . . ?
O13 V2 O15 88.46(8) . . ?
O11 V2 O15 86.51(8) . . ?
C57 O9 V2 135.02(18) . . ?
C71 O10 V2 141.30(18) . . ?
S3 O11 V2 119.50(12) . . ?
C85 O13 V2 132.97(17) . . ?
C99 O14 V2 140.32(17) . . ?
S4 O15 V2 119.07(11) . . ?
O12 S3 O11 115.70(12) . . ?
O12 S3 C76 109.33(13) . . ?
O11 S3 C76 107.35(12) . . ?
O12 S3 C62 109.60(12) . . ?
O11 S3 C62 108.06(12) . . ?
C76 S3 C62 106.39(13) . . ?
O16 S4 O15 115.52(11) . . ?
O16 S4 C104 108.51(13) . . ?
O15 S4 C104 107.30(12) . . ?
O16 S4 C90 109.33(12) . . ?
O15 S4 C90 107.48(12) . . ?
C104 S4 C90 108.51(13) . . ?
O9 C57 C58 119.2(2) . . ?
O9 C57 C62 122.6(2) . . ?
C58 C57 C62 118.2(2) . . ?
C59 C58 C57 117.5(3) . . ?
C59 C58 C63 121.3(3) . . ?
C57 C58 C63 121.2(2) . . ?
C60 C59 C58 124.8(3) . . ?
C61 C60 C59 117.1(3) . . ?
C61 C60 C67 120.4(3) . . ?
C59 C60 C67 122.5(3) . . ?
C60 C61 C62 120.3(3) . . ?
C61 C62 C57 122.1(3) . . ?
C61 C62 S3 115.0(2) . . ?
C57 C62 S3 122.8(2) . . ?
C65 C63 C66 107.7(3) . . ?
C65 C63 C58 110.2(3) . . ?
C66 C63 C58 111.8(2) . . ?
C65 C63 C64 110.8(3) . . ?
C66 C63 C64 107.4(3) . . ?
C58 C63 C64 109.0(2) . . ?
C70 C67 C69 115.9(4) . . ?
C69X C67 C68X 119.4(12) . . ?
C69X C67 C60 112.2(9) . . ?
C70 C67 C60 109.5(3) . . ?
C69 C67 C60 113.2(3) . . ?
C68X C67 C60 111.9(7) . . ?
C70 C67 C68 107.0(4) . . ?
C69 C67 C68 102.1(4) . . ?
C60 C67 C68 108.6(3) . . ?
C69X C67 C70X 110.0(11) . . ?
C68X C67 C70X 99.8(10) . . ?
C60 C67 C70X 101.1(6) . . ?
O10 C71 C76 120.4(2) . . ?
O10 C71 C72 120.3(2) . . ?
C76 C71 C72 119.2(2) . . ?
C73 C72 C71 116.7(2) . . ?
C73 C72 C77 121.7(3) . . ?
C71 C72 C77 121.5(2) . . ?
C72 C73 C74 124.7(3) . . ?
C75 C74 C73 117.4(3) . . ?
C75 C74 C81 123.0(2) . . ?
C73 C74 C81 119.5(3) . . ?
C74 C75 C76 119.7(2) . . ?
C75 C76 C71 122.2(2) . . ?
C75 C76 S3 117.4(2) . . ?
C71 C76 S3 120.3(2) . . ?
C79 C77 C78 109.6(3) . . ?
C79 C77 C80 109.0(3) . . ?
C78 C77 C80 106.6(3) . . ?
C79 C77 C72 108.1(3) . . ?
C78 C77 C72 112.1(2) . . ?
C80 C77 C72 111.4(2) . . ?
C83 C81 C82 108.7(3) . . ?
C83 C81 C84 109.8(3) . . ?
C82 C81 C84 108.7(3) . . ?
C83 C81 C74 109.8(3) . . ?
C82 C81 C74 111.7(3) . . ?
C84 C81 C74 108.1(3) . . ?
O13 C85 C90 124.0(2) . . ?
O13 C85 C86 118.7(2) . . ?
C90 C85 C86 117.3(2) . . ?
C87 C86 C85 118.3(3) . . ?
C87 C86 C91 120.7(3) . . ?
C85 C86 C91 121.1(2) . . ?
C86 C87 C88 124.5(3) . . ?
C89 C88 C87 117.2(2) . . ?
C89 C88 C95 122.9(3) . . ?
C87 C88 C95 119.9(3) . . ?
C88 C89 C90 120.5(3) . . ?
C89 C90 C85 122.3(2) . . ?
C89 C90 S4 114.6(2) . . ?
C85 C90 S4 122.98(19) . . ?
C93 C91 C92 111.0(3) . . ?
C93 C91 C86 109.8(3) . . ?
C92 C91 C86 109.4(3) . . ?
C93 C91 C94 108.7(3) . . ?
C92 C91 C94 106.6(3) . . ?
C86 C91 C94 111.4(3) . . ?
C97 C95 C98X 126.7(7) . . ?
C97 C95 C98 114.1(4) . . ?
C98X C95 C98 37.5(9) . . ?
C97 C95 C96X 44.6(5) . . ?
C98X C95 C96X 119.0(9) . . ?
C98 C95 C96X 139.6(5) . . ?
C97 C95 C88 113.4(3) . . ?
C98X C95 C88 118.6(6) . . ?
C98 C95 C88 109.1(3) . . ?
C96X C95 C88 111.2(5) . . ?
C97 C95 C96 107.9(4) . . ?
C98X C95 C96 67.5(10) . . ?
C98 C95 C96 104.9(3) . . ?
C96X C95 C96 66.2(6) . . ?
C88 C95 C96 106.9(3) . . ?
C97 C95 C97X 53.0(5) . . ?
C98X C95 C97X 101.0(10) . . ?
C98 C95 C97X 68.7(5) . . ?
C96X C95 C97X 97.2(7) . . ?
C88 C95 C97X 105.5(4) . . ?
C96 C95 C97X 147.2(5) . . ?
O14 C99 C104 119.2(2) . . ?
O14 C99 C100 121.6(2) . . ?
C104 C99 C100 119.1(2) . . ?
C101 C100 C99 116.5(3) . . ?
C101 C100 C105 121.8(3) . . ?
C99 C100 C105 121.6(3) . . ?
C100 C101 C102 124.8(3) . . ?
C103 C102 C101 117.6(3) . . ?
C103 C102 C109 122.9(3) . . ?
C101 C102 C109 119.5(3) . . ?
C102 C103 C104 119.2(3) . . ?
C103 C104 C99 122.6(3) . . ?
C103 C104 S4 119.3(2) . . ?
C99 C104 S4 118.1(2) . . ?
C108 C105 C107 108.3(3) . . ?
C108 C105 C106 107.4(3) . . ?
C107 C105 C106 109.2(3) . . ?
C108 C105 C100 112.1(3) . . ?
C107 C105 C100 108.3(3) . . ?
C106 C105 C100 111.6(2) . . ?
C112 C109 C111 109.7(3) . . ?
C112 C109 C110 107.6(3) . . ?
C111 C109 C110 109.1(3) . . ?
C112 C109 C102 111.6(3) . . ?
C111 C109 C102 110.2(3) . . ?
C110 C109 C102 108.6(3) . . ?
N1 C113 C114 178.8(5) . . ?
N2 C115 C116 176.5(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
O2 V1 O1 S1 -54.67(13) . . . . ?
O6 V1 O1 S1 136.59(13) . . . . ?
O3 V1 O1 S1 40.45(13) . . . . ?
O7 V1 O1 S1 -137.40(13) . . . . ?
O6 V1 O2 C15 72.2(5) . . . . ?
O5 V1 O2 C15 -159.9(3) . . . . ?
O3 V1 O2 C15 -63.7(3) . . . . ?
O1 V1 O2 C15 24.9(3) . . . . ?
O7 V1 O2 C15 113.4(3) . . . . ?
O2 V1 O3 C1 86.0(3) . . . . ?
O6 V1 O3 C1 -83.3(3) . . . . ?
O5 V1 O3 C1 -176.1(3) . . . . ?
O1 V1 O3 C1 1.8(3) . . . . ?
O2 V1 O5 C29 -116.2(2) . . . . ?
O6 V1 O5 C29 51.7(2) . . . . ?
O3 V1 O5 C29 148.0(2) . . . . ?
O7 V1 O5 C29 -34.1(2) . . . . ?
O2 V1 O6 C43 21.4(5) . . . . ?
O5 V1 O6 C43 -107.0(2) . . . . ?
O3 V1 O6 C43 157.2(2) . . . . ?
O1 V1 O6 C43 68.6(2) . . . . ?
O7 V1 O6 C43 -19.5(2) . . . . ?
O2 V1 O7 S2 153.97(14) . . . . ?
O6 V1 O7 S2 -36.10(14) . . . . ?
O5 V1 O7 S2 56.25(14) . . . . ?
O1 V1 O7 S2 -121.56(14) . . . . ?
V1 O1 S1 O4 179.05(11) . . . . ?
V1 O1 S1 C6 -58.90(15) . . . . ?
V1 O1 S1 C20 57.90(15) . . . . ?
V1 O7 S2 O8 -175.88(12) . . . . ?
V1 O7 S2 C48 62.89(16) . . . . ?
V1 O7 S2 C34 -52.91(16) . . . . ?
V1 O3 C1 C6 -19.1(4) . . . . ?
V1 O3 C1 C2 161.8(2) . . . . ?
O3 C1 C2 C3 -177.5(2) . . . . ?
C6 C1 C2 C3 3.4(4) . . . . ?
O3 C1 C2 C7 2.3(4) . . . . ?
C6 C1 C2 C7 -176.9(3) . . . . ?
C1 C2 C3 C4 -1.6(4) . . . . ?
C7 C2 C3 C4 178.6(3) . . . . ?
C2 C3 C4 C5 -1.2(4) . . . . ?
C2 C3 C4 C11 178.3(3) . . . . ?
C3 C4 C5 C6 2.2(4) . . . . ?
C11 C4 C5 C6 -177.3(3) . . . . ?
C4 C5 C6 C1 -0.4(4) . . . . ?
C4 C5 C6 S1 179.0(2) . . . . ?
O3 C1 C6 C5 178.3(3) . . . . ?
C2 C1 C6 C5 -2.5(4) . . . . ?
O3 C1 C6 S1 -1.1(4) . . . . ?
C2 C1 C6 S1 178.1(2) . . . . ?
O4 S1 C6 C5 -14.5(3) . . . . ?
O1 S1 C6 C5 -140.2(2) . . . . ?
C20 S1 C6 C5 104.2(2) . . . . ?
O4 S1 C6 C1 165.0(2) . . . . ?
O1 S1 C6 C1 39.2(3) . . . . ?
C20 S1 C6 C1 -76.4(2) . . . . ?
C3 C2 C7 C9 114.6(3) . . . . ?
C1 C2 C7 C9 -65.2(3) . . . . ?
C3 C2 C7 C8 -123.2(3) . . . . ?
C1 C2 C7 C8 57.1(4) . . . . ?
C3 C2 C7 C10 -4.1(4) . . . . ?
C1 C2 C7 C10 176.2(3) . . . . ?
C5 C4 C11 C13 -5.5(4) . . . . ?
C3 C4 C11 C13 175.0(3) . . . . ?
C5 C4 C11 C14 -126.4(3) . . . . ?
C3 C4 C11 C14 54.1(4) . . . . ?
C5 C4 C11 C12 114.2(3) . . . . ?
C3 C4 C11 C12 -65.3(3) . . . . ?
V1 O2 C15 C20 0.3(5) . . . . ?
V1 O2 C15 C16 -179.9(2) . . . . ?
O2 C15 C16 C17 -174.0(2) . . . . ?
C20 C15 C16 C17 5.8(4) . . . . ?
O2 C15 C16 C21 8.7(4) . . . . ?
C20 C15 C16 C21 -171.5(2) . . . . ?
C15 C16 C17 C18 -2.0(4) . . . . ?
C21 C16 C17 C18 175.3(3) . . . . ?
C16 C17 C18 C19 -3.0(5) . . . . ?
C16 C17 C18 C25 -179.5(3) . . . . ?
C17 C18 C19 C20 3.9(4) . . . . ?
C25 C18 C19 C20 -179.7(3) . . . . ?
C18 C19 C20 C15 0.0(4) . . . . ?
C18 C19 C20 S1 -177.3(2) . . . . ?
O2 C15 C20 C19 174.8(3) . . . . ?
C16 C15 C20 C19 -5.0(4) . . . . ?
O2 C15 C20 S1 -8.0(4) . . . . ?
C16 C15 C20 S1 172.2(2) . . . . ?
O4 S1 C20 C19 29.6(3) . . . . ?
O1 S1 C20 C19 154.8(2) . . . . ?
C6 S1 C20 C19 -89.4(2) . . . . ?
O4 S1 C20 C15 -147.8(2) . . . . ?
O1 S1 C20 C15 -22.5(3) . . . . ?
C6 S1 C20 C15 93.2(2) . . . . ?
C17 C16 C21 C22 -115.7(3) . . . . ?
C15 C16 C21 C22 61.5(3) . . . . ?
C17 C16 C21 C23 122.7(3) . . . . ?
C15 C16 C21 C23 -60.2(4) . . . . ?
C17 C16 C21 C24 2.6(4) . . . . ?
C15 C16 C21 C24 179.8(3) . . . . ?
C19 C18 C25 C26X -98.1(6) . . . . ?
C17 C18 C25 C26X 78.3(7) . . . . ?
C19 C18 C25 C27 46.6(7) . . . . ?
C17 C18 C25 C27 -137.1(6) . . . . ?
C19 C18 C25 C28 -174.8(6) . . . . ?
C17 C18 C25 C28 1.6(6) . . . . ?
C19 C18 C25 C27X 30.9(7) . . . . ?
C17 C18 C25 C27X -152.8(6) . . . . ?
C19 C18 C25 C28X 141.4(5) . . . . ?
C17 C18 C25 C28X -42.2(5) . . . . ?
C19 C18 C25 C26 -68.8(5) . . . . ?
C17 C18 C25 C26 107.5(4) . . . . ?
V1 O5 C29 C34 12.9(4) . . . . ?
V1 O5 C29 C30 -166.23(19) . . . . ?
O5 C29 C30 C31 178.4(2) . . . . ?
C34 C29 C30 C31 -0.8(4) . . . . ?
O5 C29 C30 C35 0.7(4) . . . . ?
C34 C29 C30 C35 -178.5(3) . . . . ?
C29 C30 C31 C32 -0.2(4) . . . . ?
C35 C30 C31 C32 177.6(3) . . . . ?
C30 C31 C32 C33 1.0(4) . . . . ?
C30 C31 C32 C39 179.0(3) . . . . ?
C31 C32 C33 C34 -0.9(4) . . . . ?
C39 C32 C33 C34 -178.8(2) . . . . ?
C32 C33 C34 C29 0.0(4) . . . . ?
C32 C33 C34 S2 179.0(2) . . . . ?
O5 C29 C34 C33 -178.3(2) . . . . ?
C30 C29 C34 C33 0.9(4) . . . . ?
O5 C29 C34 S2 2.8(4) . . . . ?
C30 C29 C34 S2 -178.1(2) . . . . ?
O7 S2 C34 C33 -159.1(2) . . . . ?
O8 S2 C34 C33 -31.9(2) . . . . ?
C48 S2 C34 C33 85.9(2) . . . . ?
O7 S2 C34 C29 20.0(3) . . . . ?
O8 S2 C34 C29 147.1(2) . . . . ?
C48 S2 C34 C29 -95.0(3) . . . . ?
C31 C30 C35 C37 120.3(3) . . . . ?
C29 C30 C35 C37 -62.1(4) . . . . ?
C31 C30 C35 C36 -117.9(3) . . . . ?
C29 C30 C35 C36 59.7(4) . . . . ?
C31 C30 C35 C38 -0.3(4) . . . . ?
C29 C30 C35 C38 177.4(3) . . . . ?
C33 C32 C39 C41 105.1(4) . . . . ?
C31 C32 C39 C41 -72.8(4) . . . . ?
C33 C32 C39 C42 -15.7(4) . . . . ?
C31 C32 C39 C42 166.4(3) . . . . ?
C33 C32 C39 C40 -134.3(3) . . . . ?
C31 C32 C39 C40 47.8(4) . . . . ?
V1 O6 C43 C48 37.7(4) . . . . ?
V1 O6 C43 C44 -145.2(2) . . . . ?
O6 C43 C44 C45 -177.8(2) . . . . ?
C48 C43 C44 C45 -0.6(4) . . . . ?
O6 C43 C44 C49 0.0(4) . . . . ?
C48 C43 C44 C49 177.1(2) . . . . ?
C43 C44 C45 C46 1.5(4) . . . . ?
C49 C44 C45 C46 -176.2(3) . . . . ?
C44 C45 C46 C47 -1.3(4) . . . . ?
C44 C45 C46 C53 -179.8(3) . . . . ?
C45 C46 C47 C48 0.1(4) . . . . ?
C53 C46 C47 C48 178.6(3) . . . . ?
C46 C47 C48 C43 0.7(4) . . . . ?
C46 C47 C48 S2 179.3(2) . . . . ?
O6 C43 C48 C47 176.8(2) . . . . ?
C44 C43 C48 C47 -0.4(4) . . . . ?
O6 C43 C48 S2 -1.9(3) . . . . ?
C44 C43 C48 S2 -179.1(2) . . . . ?
O7 S2 C48 C47 136.8(2) . . . . ?
O8 S2 C48 C47 10.8(3) . . . . ?
C34 S2 C48 C47 -107.5(2) . . . . ?
O7 S2 C48 C43 -44.5(2) . . . . ?
O8 S2 C48 C43 -170.5(2) . . . . ?
C34 S2 C48 C43 71.2(2) . . . . ?
C45 C44 C49 C51 -5.1(4) . . . . ?
C43 C44 C49 C51 177.3(3) . . . . ?
C45 C44 C49 C52 113.8(3) . . . . ?
C43 C44 C49 C52 -63.7(3) . . . . ?
C45 C44 C49 C50 -125.2(3) . . . . ?
C43 C44 C49 C50 57.2(4) . . . . ?
C47 C46 C53 C55 132.5(4) . . . . ?
C45 C46 C53 C55 -49.1(5) . . . . ?
C47 C46 C53 C54 -107.5(4) . . . . ?
C45 C46 C53 C54 70.9(4) . . . . ?
C47 C46 C53 C56 11.4(5) . . . . ?
C45 C46 C53 C56 -170.1(4) . . . . ?
O10 V2 O9 C57 69.8(3) . . . . ?
O14 V2 O9 C57 -99.9(3) . . . . ?
O13 V2 O9 C57 166.8(2) . . . . ?
O11 V2 O9 C57 -16.0(3) . . . . ?
O14 V2 O10 C71 49.9(5) . . . . ?
O9 V2 O10 C71 -78.7(3) . . . . ?
O13 V2 O10 C71 -173.6(3) . . . . ?
O11 V2 O10 C71 11.6(3) . . . . ?
O15 V2 O10 C71 98.4(3) . . . . ?
O10 V2 O11 S3 -47.90(14) . . . . ?
O14 V2 O11 S3 140.25(14) . . . . ?
O9 V2 O11 S3 45.03(14) . . . . ?
O15 V2 O11 S3 -133.85(13) . . . . ?
O10 V2 O13 C85 -114.0(2) . . . . ?
O14 V2 O13 C85 56.9(2) . . . . ?
O9 V2 O13 C85 152.4(2) . . . . ?
O15 V2 O13 C85 -28.5(2) . . . . ?
O10 V2 O14 C99 34.7(5) . . . . ?
O9 V2 O14 C99 163.1(3) . . . . ?
O13 V2 O14 C99 -102.1(3) . . . . ?
O11 V2 O14 C99 73.1(3) . . . . ?
O15 V2 O14 C99 -13.9(3) . . . . ?
O10 V2 O15 S4 150.66(13) . . . . ?
O14 V2 O15 S4 -39.21(13) . . . . ?
O13 V2 O15 S4 53.77(13) . . . . ?
O11 V2 O15 S4 -123.38(13) . . . . ?
V2 O11 S3 O12 -177.69(11) . . . . ?
V2 O11 S3 C76 59.96(16) . . . . ?
V2 O11 S3 C62 -54.43(16) . . . . ?
V2 O15 S4 O16 -176.82(11) . . . . ?
V2 O15 S4 C104 62.04(15) . . . . ?
V2 O15 S4 C90 -54.49(15) . . . . ?
V2 O9 C57 C58 -178.6(2) . . . . ?
V2 O9 C57 C62 1.5(4) . . . . ?
O9 C57 C58 C59 -177.5(3) . . . . ?
C62 C57 C58 C59 2.4(4) . . . . ?
O9 C57 C58 C63 3.4(4) . . . . ?
C62 C57 C58 C63 -176.7(3) . . . . ?
C57 C58 C59 C60 -0.3(5) . . . . ?
C63 C58 C59 C60 178.8(3) . . . . ?
C58 C59 C60 C61 -2.1(5) . . . . ?
C58 C59 C60 C67 178.8(3) . . . . ?
C59 C60 C61 C62 2.4(4) . . . . ?
C67 C60 C61 C62 -178.5(3) . . . . ?
C60 C61 C62 C57 -0.3(4) . . . . ?
C60 C61 C62 S3 -176.6(2) . . . . ?
O9 C57 C62 C61 177.8(3) . . . . ?
C58 C57 C62 C61 -2.1(4) . . . . ?
O9 C57 C62 S3 -6.3(4) . . . . ?
C58 C57 C62 S3 173.8(2) . . . . ?
O12 S3 C62 C61 -22.7(3) . . . . ?
O11 S3 C62 C61 -149.6(2) . . . . ?
C76 S3 C62 C61 95.4(2) . . . . ?
O12 S3 C62 C57 161.0(2) . . . . ?
O11 S3 C62 C57 34.2(3) . . . . ?
C76 S3 C62 C57 -80.9(3) . . . . ?
C59 C58 C63 C65 119.0(3) . . . . ?
C57 C58 C63 C65 -62.0(4) . . . . ?
C59 C58 C63 C66 -0.7(4) . . . . ?
C57 C58 C63 C66 178.4(3) . . . . ?
C59 C58 C63 C64 -119.3(3) . . . . ?
C57 C58 C63 C64 59.8(4) . . . . ?
C61 C60 C67 C69X 127.2(12) . . . . ?
C59 C60 C67 C69X -53.7(12) . . . . ?
C61 C60 C67 C70 -61.2(5) . . . . ?
C59 C60 C67 C70 117.8(4) . . . . ?
C61 C60 C67 C69 167.8(4) . . . . ?
C59 C60 C67 C69 -13.2(6) . . . . ?
C61 C60 C67 C68X -10.2(10) . . . . ?
C59 C60 C67 C68X 168.8(10) . . . . ?
C61 C60 C67 C68 55.2(4) . . . . ?
C59 C60 C67 C68 -125.7(4) . . . . ?
C61 C60 C67 C70X -115.6(7) . . . . ?
C59 C60 C67 C70X 63.4(8) . . . . ?
V2 O10 C71 C76 8.1(4) . . . . ?
V2 O10 C71 C72 -173.9(2) . . . . ?
O10 C71 C72 C73 -177.7(2) . . . . ?
C76 C71 C72 C73 0.3(4) . . . . ?
O10 C71 C72 C77 -0.6(4) . . . . ?
C76 C71 C72 C77 177.4(3) . . . . ?
C71 C72 C73 C74 0.6(4) . . . . ?
C77 C72 C73 C74 -176.5(3) . . . . ?
C72 C73 C74 C75 -0.7(5) . . . . ?
C72 C73 C74 C81 -178.0(3) . . . . ?
C73 C74 C75 C76 -0.1(4) . . . . ?
C81 C74 C75 C76 177.1(3) . . . . ?
C74 C75 C76 C71 0.9(4) . . . . ?
C74 C75 C76 S3 178.6(2) . . . . ?
O10 C71 C76 C75 177.0(2) . . . . ?
C72 C71 C76 C75 -1.0(4) . . . . ?
O10 C71 C76 S3 -0.6(4) . . . . ?
C72 C71 C76 S3 -178.6(2) . . . . ?
O12 S3 C76 C75 22.9(3) . . . . ?
O11 S3 C76 C75 149.2(2) . . . . ?
C62 S3 C76 C75 -95.3(2) . . . . ?
O12 S3 C76 C71 -159.4(2) . . . . ?
O11 S3 C76 C71 -33.1(3) . . . . ?
C62 S3 C76 C71 82.4(2) . . . . ?
C73 C72 C77 C79 107.0(3) . . . . ?
C71 C72 C77 C79 -70.0(3) . . . . ?
C73 C72 C77 C78 -132.2(3) . . . . ?
C71 C72 C77 C78 50.8(4) . . . . ?
C73 C72 C77 C80 -12.9(4) . . . . ?
C71 C72 C77 C80 170.2(3) . . . . ?
C75 C74 C81 C83 128.7(3) . . . . ?
C73 C74 C81 C83 -54.2(4) . . . . ?
C75 C74 C81 C82 8.0(5) . . . . ?
C73 C74 C81 C82 -174.9(3) . . . . ?
C75 C74 C81 C84 -111.6(3) . . . . ?
C73 C74 C81 C84 65.5(4) . . . . ?
V2 O13 C85 C90 7.8(4) . . . . ?
V2 O13 C85 C86 -172.24(19) . . . . ?
O13 C85 C86 C87 -179.4(3) . . . . ?
C90 C85 C86 C87 0.6(4) . . . . ?
O13 C85 C86 C91 0.9(4) . . . . ?
C90 C85 C86 C91 -179.1(3) . . . . ?
C85 C86 C87 C88 -0.3(5) . . . . ?
C91 C86 C87 C88 179.4(3) . . . . ?
C86 C87 C88 C89 0.0(5) . . . . ?
C86 C87 C88 C95 178.8(3) . . . . ?
C87 C88 C89 C90 0.1(4) . . . . ?
C95 C88 C89 C90 -178.7(3) . . . . ?
C88 C89 C90 C85 0.2(4) . . . . ?
C88 C89 C90 S4 178.2(2) . . . . ?
O13 C85 C90 C89 179.4(3) . . . . ?
C86 C85 C90 C89 -0.5(4) . . . . ?
O13 C85 C90 S4 1.6(4) . . . . ?
C86 C85 C90 S4 -178.4(2) . . . . ?
O16 S4 C90 C89 -28.0(3) . . . . ?
O15 S4 C90 C89 -154.1(2) . . . . ?
C104 S4 C90 C89 90.2(2) . . . . ?
O16 S4 C90 C85 150.1(2) . . . . ?
O15 S4 C90 C85 24.0(3) . . . . ?
C104 S4 C90 C85 -91.8(3) . . . . ?
C87 C86 C91 C93 119.7(3) . . . . ?
C85 C86 C91 C93 -60.6(4) . . . . ?
C87 C86 C91 C92 -118.2(3) . . . . ?
C85 C86 C91 C92 61.5(4) . . . . ?
C87 C86 C91 C94 -0.7(5) . . . . ?
C85 C86 C91 C94 179.0(3) . . . . ?
C89 C88 C95 C97 4.3(5) . . . . ?
C87 C88 C95 C97 -174.5(4) . . . . ?
C89 C88 C95 C98X -163.9(11) . . . . ?
C87 C88 C95 C98X 17.4(12) . . . . ?
C89 C88 C95 C98 -124.0(4) . . . . ?
C87 C88 C95 C98 57.2(5) . . . . ?
C89 C88 C95 C96X 52.6(7) . . . . ?
C87 C88 C95 C96X -126.1(7) . . . . ?
C89 C88 C95 C96 123.0(3) . . . . ?
C87 C88 C95 C96 -55.7(4) . . . . ?
C89 C88 C95 C97X -51.6(6) . . . . ?
C87 C88 C95 C97X 129.6(6) . . . . ?
V2 O14 C99 C104 35.5(4) . . . . ?
V2 O14 C99 C100 -147.4(2) . . . . ?
O14 C99 C100 C101 -172.7(2) . . . . ?
C104 C99 C100 C101 4.4(4) . . . . ?
O14 C99 C100 C105 2.5(4) . . . . ?
C104 C99 C100 C105 179.6(3) . . . . ?
C99 C100 C101 C102 0.1(4) . . . . ?
C105 C100 C101 C102 -175.2(3) . . . . ?
C100 C101 C102 C103 -4.2(4) . . . . ?
C100 C101 C102 C109 174.0(3) . . . . ?
C101 C102 C103 C104 3.7(4) . . . . ?
C109 C102 C103 C104 -174.4(3) . . . . ?
C102 C103 C104 C99 0.6(4) . . . . ?
C102 C103 C104 S4 178.6(2) . . . . ?
O14 C99 C104 C103 172.3(2) . . . . ?
C100 C99 C104 C103 -4.9(4) . . . . ?
O14 C99 C104 S4 -5.6(3) . . . . ?
C100 C99 C104 S4 177.2(2) . . . . ?
O16 S4 C104 C103 17.6(3) . . . . ?
O15 S4 C104 C103 143.1(2) . . . . ?
C90 S4 C104 C103 -101.1(2) . . . . ?
O16 S4 C104 C99 -164.4(2) . . . . ?
O15 S4 C104 C99 -38.9(2) . . . . ?
C90 S4 C104 C99 76.9(2) . . . . ?
C101 C100 C105 C108 -14.6(4) . . . . ?
C99 C100 C105 C108 170.4(3) . . . . ?
C101 C100 C105 C107 104.8(3) . . . . ?
C99 C100 C105 C107 -70.2(3) . . . . ?
C101 C100 C105 C106 -135.0(3) . . . . ?
C99 C100 C105 C106 50.0(4) . . . . ?
C103 C102 C109 C112 6.0(4) . . . . ?
C101 C102 C109 C112 -172.1(3) . . . . ?
C103 C102 C109 C111 -116.2(4) . . . . ?
C101 C102 C109 C111 65.8(4) . . . . ?
C103 C102 C109 C110 124.4(3) . . . . ?
C101 C102 C109 C110 -53.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.902
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.066

#===END

data_5
_database_code_depnum_ccdc_archive 'CCDC 718346'

_chemical_name_common            'Compound 5'
_chemical_melting_point          ?
_chemical_formula_structural     '[{V(=O)(diphenolate)}2(mu-OH)(mu-OPr)]'
_chemical_formula_moiety         'C63 H96 O8 V2'
_chemical_formula_sum            'C63 H96 O8 V2'
_chemical_formula_weight         1083.28

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   I2/a
_symmetry_space_group_name_Hall  '-I 2ya'

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

_cell_length_a                   15.2469(7)
_cell_length_b                   24.3672(11)
_cell_length_c                   18.2970(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.4160(7)
_cell_angle_gamma                90.00
_cell_volume                     6449.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13303
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      29.10

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_process_details   'SADABS v2.03, Sheldrick, G.M., (2001)'

_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            28550
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         29.09
_reflns_number_total             7835
_reflns_number_gt                6188
_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    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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. I2/a gives lower beta angle.
;

_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^)+(0.0520P)^2^+5.5517P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'geom except OH coords freely refined'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7835
_refine_ls_number_parameters     387
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.046
_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 0.353882(17) 0.205037(11) 0.496020(16) 0.03161(9) Uani 1 1 d . . .
O2 O 0.35454(10) 0.19555(5) 0.41043(7) 0.0515(4) Uani 1 1 d . . .
O3 O 0.44382(7) 0.16143(4) 0.55577(6) 0.0285(2) Uani 1 1 d . . .
O4 O 0.42159(7) 0.26702(4) 0.52457(6) 0.0293(2) Uani 1 1 d . . .
O5 O 0.2500 0.25116(6) 0.5000 0.0341(4) Uani 1 2 d S . .
H5 H 0.2500 0.2815(12) 0.5000 0.041 Uiso 1 2 d S . .
C1 C 0.51194(9) 0.16807(6) 0.62423(8) 0.0253(3) Uani 1 1 d . . .
C2 C 0.59639(9) 0.13986(6) 0.63535(8) 0.0258(3) Uani 1 1 d . . .
C3 C 0.66357(10) 0.14504(6) 0.70697(9) 0.0293(3) Uani 1 1 d . . .
H3 H 0.7198 0.1254 0.7160 0.035 Uiso 1 1 calc R . .
C4 C 0.65277(10) 0.17753(7) 0.76626(8) 0.0301(3) Uani 1 1 d . . .
C5 C 0.57010(10) 0.20594(6) 0.75209(9) 0.0293(3) Uani 1 1 d . . .
H5A H 0.5616 0.2288 0.7913 0.035 Uiso 1 1 calc R . .
C6 C 0.49921(10) 0.20195(6) 0.68212(8) 0.0263(3) Uani 1 1 d . . .
C7 C 0.61524(10) 0.10730(6) 0.57016(9) 0.0296(3) Uani 1 1 d . . .
C8 C 0.71209(12) 0.08128(8) 0.59690(11) 0.0427(4) Uani 1 1 d . . .
H8A H 0.7588 0.1102 0.6136 0.064 Uiso 1 1 calc R . .
H8B H 0.7222 0.0608 0.5542 0.064 Uiso 1 1 calc R . .
H8C H 0.7169 0.0563 0.6399 0.064 Uiso 1 1 calc R . .
C9 C 0.61092(12) 0.14595(7) 0.50273(9) 0.0373(4) Uani 1 1 d . . .
H9A H 0.5492 0.1624 0.4834 0.056 Uiso 1 1 calc R . .
H9B H 0.6235 0.1251 0.4613 0.056 Uiso 1 1 calc R . .
H9C H 0.6573 0.1750 0.5205 0.056 Uiso 1 1 calc R . .
C10 C 0.54578(12) 0.06021(7) 0.54250(11) 0.0394(4) Uani 1 1 d . . .
H10A H 0.5471 0.0367 0.5863 0.059 Uiso 1 1 calc R . .
H10B H 0.5623 0.0385 0.5037 0.059 Uiso 1 1 calc R . .
H10C H 0.4835 0.0754 0.5199 0.059 Uiso 1 1 calc R . .
C11 C 0.73010(11) 0.17978(8) 0.84385(9) 0.0380(4) Uani 1 1 d . . .
C12 C 0.73015(14) 0.12563(10) 0.88595(11) 0.0579(6) Uani 1 1 d . . .
H12A H 0.7431 0.0953 0.8557 0.087 Uiso 1 1 calc R . .
H12B H 0.6695 0.1200 0.8927 0.087 Uiso 1 1 calc R . .
H12C H 0.7778 0.1268 0.9365 0.087 Uiso 1 1 calc R . .
C13 C 0.71507(17) 0.22694(12) 0.89400(13) 0.0697(7) Uani 1 1 d . . .
H13A H 0.7678 0.2291 0.9414 0.104 Uiso 1 1 calc R . .
H13B H 0.6584 0.2203 0.9071 0.104 Uiso 1 1 calc R . .
H13C H 0.7094 0.2616 0.8656 0.104 Uiso 1 1 calc R . .
C14 C 0.82431(12) 0.18817(11) 0.83235(11) 0.0552(6) Uani 1 1 d . . .
H14A H 0.8384 0.1566 0.8049 0.083 Uiso 1 1 calc R . .
H14B H 0.8720 0.1918 0.8826 0.083 Uiso 1 1 calc R . .
H14C H 0.8228 0.2216 0.8021 0.083 Uiso 1 1 calc R . .
C15 C 0.41004(10) 0.23426(6) 0.67039(9) 0.0289(3) Uani 1 1 d . . .
H15 H 0.3631 0.2174 0.6247 0.035 Uiso 1 1 calc R . .
C16 C 0.37214(12) 0.22720(8) 0.73824(11) 0.0411(4) Uani 1 1 d . . .
H16A H 0.3624 0.1881 0.7457 0.062 Uiso 1 1 calc R . .
H16B H 0.3133 0.2468 0.7272 0.062 Uiso 1 1 calc R . .
H16C H 0.4165 0.2422 0.7851 0.062 Uiso 1 1 calc R . .
C17 C 0.42097(10) 0.30786(6) 0.57486(9) 0.0282(3) Uani 1 1 d . . .
C18 C 0.41869(10) 0.29434(6) 0.64923(9) 0.0284(3) Uani 1 1 d . . .
C19 C 0.42315(11) 0.33663(7) 0.70087(9) 0.0345(3) Uani 1 1 d . . .
H19 H 0.4223 0.3280 0.7513 0.041 Uiso 1 1 calc R . .
C20 C 0.42883(12) 0.39148(7) 0.68096(10) 0.0380(4) Uani 1 1 d . A .
C21 C 0.42809(12) 0.40306(7) 0.60632(10) 0.0393(4) Uani 1 1 d . . .
H21 H 0.4308 0.4404 0.5921 0.047 Uiso 1 1 calc R . .
C22 C 0.42359(11) 0.36247(7) 0.55092(9) 0.0339(3) Uani 1 1 d . . .
C23 C 0.43651(15) 0.43751(8) 0.74027(11) 0.0478(5) Uani 1 1 d DU . .
C24 C 0.3630(7) 0.4298(4) 0.7799(7) 0.107(3) Uani 0.585(14) 1 d PDU A 1
H24A H 0.3691 0.3932 0.8031 0.160 Uiso 0.585(14) 1 calc PR A 1
H24B H 0.3015 0.4337 0.7420 0.160 Uiso 0.585(14) 1 calc PR A 1
H24C H 0.3714 0.4576 0.8203 0.160 Uiso 0.585(14) 1 calc PR A 1
C25 C 0.5304(5) 0.4333(3) 0.8010(4) 0.087(2) Uani 0.585(14) 1 d PDU A 1
H25A H 0.5385 0.3963 0.8233 0.130 Uiso 0.585(14) 1 calc PR A 1
H25B H 0.5349 0.4604 0.8416 0.130 Uiso 0.585(14) 1 calc PR A 1
H25C H 0.5788 0.4404 0.7774 0.130 Uiso 0.585(14) 1 calc PR A 1
C26 C 0.4266(9) 0.4948(2) 0.7061(4) 0.088(3) Uani 0.585(14) 1 d PDU A 1
H26A H 0.3657 0.4985 0.6672 0.132 Uiso 0.585(14) 1 calc PR A 1
H26B H 0.4749 0.5009 0.6821 0.132 Uiso 0.585(14) 1 calc PR A 1
H26C H 0.4329 0.5219 0.7470 0.132 Uiso 0.585(14) 1 calc PR A 1
C24X C 0.4188(15) 0.4166(4) 0.8123(6) 0.121(5) Uani 0.415(14) 1 d PDU A 2
H24D H 0.4655 0.3891 0.8373 0.182 Uiso 0.415(14) 1 calc PR A 2
H24E H 0.3572 0.4000 0.7984 0.182 Uiso 0.415(14) 1 calc PR A 2
H24F H 0.4223 0.4473 0.8478 0.182 Uiso 0.415(14) 1 calc PR A 2
C25X C 0.5326(7) 0.4609(7) 0.7618(11) 0.124(6) Uani 0.415(14) 1 d PDU A 2
H25D H 0.5777 0.4322 0.7852 0.186 Uiso 0.415(14) 1 calc PR A 2
H25E H 0.5385 0.4910 0.7987 0.186 Uiso 0.415(14) 1 calc PR A 2
H25F H 0.5443 0.4749 0.7155 0.186 Uiso 0.415(14) 1 calc PR A 2
C26X C 0.3664(11) 0.4812(5) 0.7043(5) 0.100(4) Uani 0.415(14) 1 d PDU A 2
H26D H 0.3708 0.5108 0.7415 0.150 Uiso 0.415(14) 1 calc PR A 2
H26E H 0.3042 0.4653 0.6892 0.150 Uiso 0.415(14) 1 calc PR A 2
H26F H 0.3786 0.4960 0.6586 0.150 Uiso 0.415(14) 1 calc PR A 2
C27 C 0.41899(13) 0.37686(7) 0.46784(10) 0.0413(4) Uani 1 1 d . . .
C28 C 0.4216(2) 0.43913(9) 0.45635(14) 0.0780(8) Uani 1 1 d . . .
H28A H 0.3684 0.4561 0.4666 0.117 Uiso 1 1 calc R . .
H28B H 0.4192 0.4469 0.4032 0.117 Uiso 1 1 calc R . .
H28C H 0.4789 0.4541 0.4919 0.117 Uiso 1 1 calc R . .
C29 C 0.50152(13) 0.35133(11) 0.44819(12) 0.0579(6) Uani 1 1 d . . .
H29A H 0.5595 0.3656 0.4836 0.087 Uiso 1 1 calc R . .
H29B H 0.4974 0.3608 0.3952 0.087 Uiso 1 1 calc R . .
H29C H 0.5000 0.3113 0.4533 0.087 Uiso 1 1 calc R . .
C30 C 0.32841(12) 0.35598(8) 0.41012(10) 0.0397(4) Uani 1 1 d . . .
H30A H 0.3277 0.3158 0.4108 0.059 Uiso 1 1 calc R . .
H30B H 0.3238 0.3688 0.3583 0.059 Uiso 1 1 calc R . .
H30C H 0.2759 0.3700 0.4245 0.059 Uiso 1 1 calc R . .
O1 O 0.2550(5) 0.15821(8) 0.4877(4) 0.0354(11) Uani 0.50 1 d PU . -1
C31 C 0.2628(3) 0.09910(14) 0.4794(2) 0.0455(8) Uani 0.50 1 d PDU B -1
H31 H 0.3273 0.0917 0.4794 0.055 Uiso 0.50 1 calc PR B -1
C32 C 0.1987(3) 0.07964(18) 0.4027(3) 0.0573(10) Uani 0.50 1 d PDU B -1
H32A H 0.2107 0.1006 0.3611 0.086 Uiso 0.50 1 calc PR B -1
H32B H 0.1344 0.0852 0.4009 0.086 Uiso 0.50 1 calc PR B -1
H32C H 0.2094 0.0405 0.3962 0.086 Uiso 0.50 1 calc PR B -1
C33 C 0.2519(4) 0.0710(2) 0.5479(3) 0.0744(12) Uani 0.50 1 d PDU B -1
H33A H 0.2975 0.0853 0.5946 0.112 Uiso 0.50 1 calc PR B -1
H33B H 0.2614 0.0315 0.5440 0.112 Uiso 0.50 1 calc PR B -1
H33C H 0.1895 0.0776 0.5504 0.112 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 0.02366(13) 0.02867(14) 0.03481(15) -0.00848(10) -0.00173(10) 0.00272(10)
O2 0.0605(8) 0.0461(7) 0.0330(7) -0.0133(5) -0.0063(6) 0.0158(6)
O3 0.0211(5) 0.0306(5) 0.0302(5) -0.0054(4) 0.0028(4) 0.0011(4)
O4 0.0267(5) 0.0331(6) 0.0293(5) -0.0079(4) 0.0104(4) -0.0038(4)
O5 0.0253(7) 0.0220(7) 0.0514(10) 0.000 0.0069(7) 0.000
C1 0.0195(6) 0.0292(7) 0.0261(7) -0.0008(5) 0.0056(5) -0.0028(5)
C2 0.0220(6) 0.0282(7) 0.0274(7) -0.0003(5) 0.0082(5) -0.0013(5)
C3 0.0212(6) 0.0356(8) 0.0304(7) 0.0029(6) 0.0071(6) -0.0005(5)
C4 0.0251(7) 0.0389(8) 0.0252(7) 0.0009(6) 0.0064(6) -0.0079(6)
C5 0.0311(7) 0.0336(8) 0.0252(7) -0.0033(6) 0.0117(6) -0.0062(6)
C6 0.0238(7) 0.0286(7) 0.0288(7) -0.0001(6) 0.0114(6) -0.0022(5)
C7 0.0253(7) 0.0314(7) 0.0319(7) -0.0038(6) 0.0088(6) 0.0028(6)
C8 0.0323(8) 0.0526(10) 0.0436(10) -0.0054(8) 0.0127(7) 0.0129(7)
C9 0.0394(9) 0.0438(9) 0.0324(8) -0.0010(7) 0.0165(7) 0.0026(7)
C10 0.0384(9) 0.0319(8) 0.0472(10) -0.0091(7) 0.0126(7) -0.0020(7)
C11 0.0303(8) 0.0545(10) 0.0255(7) 0.0018(7) 0.0036(6) -0.0124(7)
C12 0.0425(10) 0.0823(15) 0.0377(10) 0.0235(10) -0.0032(8) -0.0202(10)
C13 0.0594(14) 0.0956(18) 0.0404(11) -0.0277(12) -0.0036(10) -0.0099(13)
C14 0.0301(9) 0.0918(16) 0.0369(10) 0.0101(10) 0.0010(7) -0.0212(9)
C15 0.0260(7) 0.0322(8) 0.0316(7) -0.0026(6) 0.0133(6) 0.0000(6)
C16 0.0413(9) 0.0458(10) 0.0458(10) 0.0026(8) 0.0274(8) 0.0034(7)
C17 0.0241(7) 0.0318(7) 0.0292(7) -0.0072(6) 0.0092(6) -0.0041(5)
C18 0.0255(7) 0.0303(7) 0.0304(7) -0.0034(6) 0.0100(6) 0.0007(5)
C19 0.0360(8) 0.0372(8) 0.0295(8) -0.0045(6) 0.0091(6) 0.0048(6)
C20 0.0413(9) 0.0339(8) 0.0334(8) -0.0081(7) 0.0043(7) 0.0011(7)
C21 0.0453(9) 0.0295(8) 0.0384(9) -0.0043(7) 0.0065(7) -0.0061(7)
C22 0.0346(8) 0.0343(8) 0.0316(8) -0.0051(6) 0.0087(6) -0.0091(6)
C23 0.0628(12) 0.0358(9) 0.0372(9) -0.0117(7) 0.0048(8) 0.0052(8)
C24 0.137(6) 0.083(5) 0.142(8) -0.073(5) 0.103(6) -0.037(4)
C25 0.088(4) 0.078(4) 0.060(3) -0.040(3) -0.025(3) 0.021(3)
C26 0.158(8) 0.036(2) 0.052(3) -0.0141(18) 0.009(4) 0.014(3)
C24X 0.267(17) 0.053(4) 0.054(5) -0.022(3) 0.068(8) -0.004(7)
C25X 0.090(5) 0.114(10) 0.148(12) -0.096(9) 0.010(6) -0.026(6)
C26X 0.148(9) 0.062(6) 0.063(4) -0.030(4) -0.005(6) 0.050(6)
C27 0.0474(10) 0.0420(9) 0.0344(9) -0.0007(7) 0.0128(7) -0.0154(8)
C28 0.134(2) 0.0480(12) 0.0495(13) 0.0036(10) 0.0246(14) -0.0351(14)
C29 0.0384(10) 0.0970(17) 0.0414(10) 0.0051(11) 0.0170(8) -0.0159(10)
C30 0.0389(9) 0.0459(10) 0.0335(8) 0.0033(7) 0.0103(7) -0.0019(7)
O1 0.0179(16) 0.0249(8) 0.062(4) -0.0026(11) 0.010(2) 0.0001(11)
C31 0.0313(18) 0.0256(13) 0.073(2) -0.0079(15) 0.0068(15) -0.0007(13)
C32 0.0492(17) 0.0471(17) 0.0708(17) -0.0192(15) 0.0118(15) 0.0021(14)
C33 0.084(2) 0.0524(18) 0.0785(19) 0.0144(17) 0.0133(18) 0.0005(18)

_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 O2 1.5861(13) . ?
V1 O3 1.8048(10) . ?
V1 O4 1.8109(10) . ?
V1 O1 1.858(6) . ?
V1 O5 1.9621(9) . ?
V1 O1 2.112(5) 2_556 ?
O3 C1 1.3608(17) . ?
O4 C17 1.3573(17) . ?
O5 V1 1.9621(9) 2_556 ?
C1 C6 1.404(2) . ?
C1 C2 1.4165(19) . ?
C2 C3 1.391(2) . ?
C2 C7 1.534(2) . ?
C3 C4 1.394(2) . ?
C4 C5 1.389(2) . ?
C4 C11 1.533(2) . ?
C5 C6 1.394(2) . ?
C6 C15 1.526(2) . ?
C7 C10 1.535(2) . ?
C7 C9 1.537(2) . ?
C7 C8 1.538(2) . ?
C11 C12 1.528(3) . ?
C11 C14 1.530(2) . ?
C11 C13 1.532(3) . ?
C15 C18 1.531(2) . ?
C15 C16 1.536(2) . ?
C17 C22 1.405(2) . ?
C17 C18 1.411(2) . ?
C18 C19 1.385(2) . ?
C19 C20 1.395(2) . ?
C20 C21 1.391(2) . ?
C20 C23 1.539(2) . ?
C21 C22 1.402(2) . ?
C22 C27 1.540(2) . ?
C23 C25X 1.505(9) . ?
C23 C26X 1.505(7) . ?
C23 C25 1.513(5) . ?
C23 C24X 1.514(9) . ?
C23 C26 1.516(5) . ?
C23 C24 1.527(6) . ?
C27 C28 1.534(3) . ?
C27 C30 1.536(2) . ?
C27 C29 1.544(3) . ?
O1 C31 1.457(4) . ?
O1 V1 2.112(5) 2_556 ?
C31 C33 1.484(6) . ?
C31 C32 1.512(6) . ?

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
O2 V1 O3 105.77(6) . . ?
O2 V1 O4 103.03(7) . . ?
O3 V1 O4 93.53(5) . . ?
O2 V1 O1 95.02(17) . . ?
O3 V1 O1 97.4(2) . . ?
O4 V1 O1 155.47(11) . . ?
O2 V1 O5 112.15(5) . . ?
O3 V1 O5 141.49(4) . . ?
O4 V1 O5 84.54(5) . . ?
O1 V1 O5 73.23(14) . . ?
O2 V1 O1 108.12(17) . 2_556 ?
O3 V1 O1 94.43(18) . 2_556 ?
O4 V1 O1 144.28(10) . 2_556 ?
O1 V1 O1 13.1(3) . 2_556 ?
O5 V1 O1 67.93(12) . 2_556 ?
C1 O3 V1 134.47(9) . . ?
C17 O4 V1 132.97(9) . . ?
V1 O5 V1 110.11(8) 2_556 . ?
O3 C1 C6 121.14(12) . . ?
O3 C1 C2 118.00(12) . . ?
C6 C1 C2 120.86(13) . . ?
C3 C2 C1 117.19(13) . . ?
C3 C2 C7 121.10(13) . . ?
C1 C2 C7 121.64(12) . . ?
C2 C3 C4 123.49(14) . . ?
C5 C4 C3 117.45(13) . . ?
C5 C4 C11 122.83(14) . . ?
C3 C4 C11 119.71(14) . . ?
C4 C5 C6 122.11(14) . . ?
C5 C6 C1 118.82(13) . . ?
C5 C6 C15 119.40(13) . . ?
C1 C6 C15 121.77(13) . . ?
C2 C7 C10 111.34(13) . . ?
C2 C7 C9 109.65(12) . . ?
C10 C7 C9 110.08(13) . . ?
C2 C7 C8 111.27(13) . . ?
C10 C7 C8 106.85(14) . . ?
C9 C7 C8 107.54(13) . . ?
C12 C11 C14 109.50(17) . . ?
C12 C11 C13 108.80(18) . . ?
C14 C11 C13 107.86(17) . . ?
C12 C11 C4 108.27(14) . . ?
C14 C11 C4 110.99(14) . . ?
C13 C11 C4 111.38(16) . . ?
C6 C15 C18 112.63(12) . . ?
C6 C15 C16 112.00(13) . . ?
C18 C15 C16 113.34(13) . . ?
O4 C17 C22 118.42(14) . . ?
O4 C17 C18 119.35(13) . . ?
C22 C17 C18 122.22(14) . . ?
C19 C18 C17 118.25(14) . . ?
C19 C18 C15 121.90(14) . . ?
C17 C18 C15 119.84(13) . . ?
C18 C19 C20 121.88(15) . . ?
C21 C20 C19 117.96(15) . . ?
C21 C20 C23 121.31(16) . . ?
C19 C20 C23 120.73(16) . . ?
C20 C21 C22 123.36(16) . . ?
C21 C22 C17 116.26(15) . . ?
C21 C22 C27 121.97(15) . . ?
C17 C22 C27 121.75(14) . . ?
C25X C23 C26X 110.2(6) . . ?
C25X C23 C24X 109.1(7) . . ?
C26X C23 C24X 108.7(7) . . ?
C25 C23 C26 108.2(4) . . ?
C25 C23 C24 108.0(5) . . ?
C26 C23 C24 108.4(4) . . ?
C25X C23 C20 108.2(4) . . ?
C26X C23 C20 108.7(4) . . ?
C25 C23 C20 108.1(3) . . ?
C24X C23 C20 112.0(4) . . ?
C26 C23 C20 113.9(3) . . ?
C24 C23 C20 110.0(3) . . ?
C28 C27 C30 106.86(18) . . ?
C28 C27 C22 111.44(16) . . ?
C30 C27 C22 110.72(13) . . ?
C28 C27 C29 107.95(19) . . ?
C30 C27 C29 109.16(15) . . ?
C22 C27 C29 110.59(15) . . ?
C31 O1 V1 121.7(4) . . ?
C31 O1 V1 130.0(4) . 2_556 ?
V1 O1 V1 108.07(10) . 2_556 ?
O1 C31 C33 109.5(3) . . ?
O1 C31 C32 110.9(4) . . ?
C33 C31 C32 115.3(4) . . ?

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
O2 V1 O3 C1 136.08(13) . . . . ?
O4 V1 O3 C1 31.47(13) . . . . ?
O1 V1 O3 C1 -126.54(18) . . . . ?
O5 V1 O3 C1 -54.19(16) . . . . ?
O1 V1 O3 C1 -113.67(18) 2_556 . . . ?
O2 V1 O4 C17 151.42(13) . . . . ?
O3 V1 O4 C17 -101.50(13) . . . . ?
O1 V1 O4 C17 15.1(5) . . . . ?
O5 V1 O4 C17 39.91(13) . . . . ?
O1 V1 O4 C17 1.1(4) 2_556 . . . ?
O2 V1 O5 V1 95.31(6) . . . 2_556 ?
O3 V1 O5 V1 -74.02(7) . . . 2_556 ?
O4 V1 O5 V1 -162.82(4) . . . 2_556 ?
O1 V1 O5 V1 6.7(2) . . . 2_556 ?
O1 V1 O5 V1 -6.1(2) 2_556 . . 2_556 ?
V1 O3 C1 C6 33.2(2) . . . . ?
V1 O3 C1 C2 -146.61(11) . . . . ?
O3 C1 C2 C3 -177.00(13) . . . . ?
C6 C1 C2 C3 3.2(2) . . . . ?
O3 C1 C2 C7 6.0(2) . . . . ?
C6 C1 C2 C7 -173.82(13) . . . . ?
C1 C2 C3 C4 -2.1(2) . . . . ?
C7 C2 C3 C4 174.93(14) . . . . ?
C2 C3 C4 C5 0.0(2) . . . . ?
C2 C3 C4 C11 178.84(14) . . . . ?
C3 C4 C5 C6 1.1(2) . . . . ?
C11 C4 C5 C6 -177.73(14) . . . . ?
C4 C5 C6 C1 0.0(2) . . . . ?
C4 C5 C6 C15 179.93(13) . . . . ?
O3 C1 C6 C5 177.96(13) . . . . ?
C2 C1 C6 C5 -2.2(2) . . . . ?
O3 C1 C6 C15 -1.9(2) . . . . ?
C2 C1 C6 C15 177.89(13) . . . . ?
C3 C2 C7 C10 121.49(15) . . . . ?
C1 C2 C7 C10 -61.64(18) . . . . ?
C3 C2 C7 C9 -116.44(15) . . . . ?
C1 C2 C7 C9 60.43(18) . . . . ?
C3 C2 C7 C8 2.4(2) . . . . ?
C1 C2 C7 C8 179.28(14) . . . . ?
C5 C4 C11 C12 105.31(19) . . . . ?
C3 C4 C11 C12 -73.45(19) . . . . ?
C5 C4 C11 C14 -134.48(18) . . . . ?
C3 C4 C11 C14 46.8(2) . . . . ?
C5 C4 C11 C13 -14.3(2) . . . . ?
C3 C4 C11 C13 166.96(17) . . . . ?
C5 C6 C15 C18 80.91(17) . . . . ?
C1 C6 C15 C18 -99.20(16) . . . . ?
C5 C6 C15 C16 -48.24(19) . . . . ?
C1 C6 C15 C16 131.65(15) . . . . ?
V1 O4 C17 C22 -133.77(13) . . . . ?
V1 O4 C17 C18 46.86(19) . . . . ?
O4 C17 C18 C19 176.57(13) . . . . ?
C22 C17 C18 C19 -2.8(2) . . . . ?
O4 C17 C18 C15 -4.3(2) . . . . ?
C22 C17 C18 C15 176.34(14) . . . . ?
C6 C15 C18 C19 -107.44(16) . . . . ?
C16 C15 C18 C19 21.0(2) . . . . ?
C6 C15 C18 C17 73.47(17) . . . . ?
C16 C15 C18 C17 -158.07(14) . . . . ?
C17 C18 C19 C20 0.7(2) . . . . ?
C15 C18 C19 C20 -178.45(15) . . . . ?
C18 C19 C20 C21 1.2(3) . . . . ?
C18 C19 C20 C23 -178.24(16) . . . . ?
C19 C20 C21 C22 -1.2(3) . . . . ?
C23 C20 C21 C22 178.32(17) . . . . ?
C20 C21 C22 C17 -0.8(3) . . . . ?
C20 C21 C22 C27 177.52(16) . . . . ?
O4 C17 C22 C21 -176.53(14) . . . . ?
C18 C17 C22 C21 2.8(2) . . . . ?
O4 C17 C22 C27 5.1(2) . . . . ?
C18 C17 C22 C27 -175.52(14) . . . . ?
C21 C20 C23 C25X -70.0(10) . . . . ?
C19 C20 C23 C25X 109.4(10) . . . . ?
C21 C20 C23 C26X 49.6(9) . . . . ?
C19 C20 C23 C26X -131.0(9) . . . . ?
C21 C20 C23 C25 -110.5(5) . . . . ?
C19 C20 C23 C25 68.9(5) . . . . ?
C21 C20 C23 C24X 169.8(9) . . . . ?
C19 C20 C23 C24X -10.8(9) . . . . ?
C21 C20 C23 C26 9.8(6) . . . . ?
C19 C20 C23 C26 -170.7(5) . . . . ?
C21 C20 C23 C24 131.7(6) . . . . ?
C19 C20 C23 C24 -48.8(6) . . . . ?
C21 C22 C27 C28 0.9(3) . . . . ?
C17 C22 C27 C28 179.13(19) . . . . ?
C21 C22 C27 C30 -117.90(18) . . . . ?
C17 C22 C27 C30 60.3(2) . . . . ?
C21 C22 C27 C29 120.97(19) . . . . ?
C17 C22 C27 C29 -60.8(2) . . . . ?
O2 V1 O1 C31 67.9(5) . . . . ?
O3 V1 O1 C31 -38.7(5) . . . . ?
O4 V1 O1 C31 -154.5(2) . . . . ?
O5 V1 O1 C31 179.6(5) . . . . ?
O1 V1 O1 C31 -116.2(18) 2_556 . . . ?
O2 V1 O1 V1 -117.8(2) . . . 2_556 ?
O3 V1 O1 V1 135.6(2) . . . 2_556 ?
O4 V1 O1 V1 19.7(7) . . . 2_556 ?
O5 V1 O1 V1 -6.13(19) . . . 2_556 ?
O1 V1 O1 V1 58.1(12) 2_556 . . 2_556 ?
V1 O1 C31 C33 115.4(4) . . . . ?
V1 O1 C31 C33 -57.5(7) 2_556 . . . ?
V1 O1 C31 C32 -116.2(5) . . . . ?
V1 O1 C31 C32 70.9(6) 2_556 . . . ?

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.047

#===END

data_6
_database_code_depnum_ccdc_archive 'CCDC 718347'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '[V(=O)(diphenolate)(mu-OH)]2.4MeCN'
_chemical_formula_moiety         'C60 H90 O8 V2, 4(C2 H3 N)'
_chemical_formula_sum            'C68 H102 N4 O8 V2'
_chemical_formula_weight         1205.42

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'

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

_cell_length_a                   10.5991(7)
_cell_length_b                   12.9675(8)
_cell_length_c                   14.7112(9)
_cell_angle_alpha                71.2558(10)
_cell_angle_beta                 74.5933(10)
_cell_angle_gamma                68.2679(10)
_cell_volume                     1753.73(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9175
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.76

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.98
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_process_details   'SADABS, 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            15504
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         29.00
_reflns_number_total             8073
_reflns_number_gt                6816
_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    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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^)+(0.0503P)^2^+0.7320P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'geom except H1 coords freely refined'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8073
_refine_ls_number_parameters     413
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1038
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_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 1.00338(2) 0.47374(2) 0.112259(17) 0.02024(8) Uani 1 1 d . . .
O1 O 1.01228(12) 0.40450(9) 0.00822(8) 0.0244(2) Uani 1 1 d . . .
H1 H 1.065(2) 0.3471(18) 0.0081(15) 0.037 Uiso 1 1 d . . .
O2 O 1.15829(11) 0.43945(10) 0.12580(8) 0.0297(2) Uani 1 1 d . . .
O3 O 0.90986(10) 0.58057(9) 0.18135(7) 0.0231(2) Uani 1 1 d . . .
O4 O 0.93894(10) 0.36302(9) 0.19993(7) 0.0220(2) Uani 1 1 d . . .
C1 C 0.78541(14) 0.60824(12) 0.23849(10) 0.0196(3) Uani 1 1 d . . .
C2 C 0.77270(14) 0.65954(12) 0.31352(10) 0.0211(3) Uani 1 1 d . . .
C3 C 0.64376(15) 0.68960(12) 0.37061(10) 0.0221(3) Uani 1 1 d . . .
H3 H 0.6336 0.7237 0.4215 0.026 Uiso 1 1 calc R . .
C4 C 0.52812(14) 0.67217(12) 0.35691(10) 0.0208(3) Uani 1 1 d . . .
C5 C 0.54580(14) 0.61996(12) 0.28352(10) 0.0205(3) Uani 1 1 d . . .
H5 H 0.4692 0.6058 0.2738 0.025 Uiso 1 1 calc R . .
C6 C 0.67278(14) 0.58755(11) 0.22349(10) 0.0192(3) Uani 1 1 d . . .
C7 C 0.89694(15) 0.67990(14) 0.33156(11) 0.0276(3) Uani 1 1 d . . .
C8 C 1.01308(17) 0.56479(17) 0.35285(15) 0.0406(4) Uani 1 1 d . . .
H8A H 0.9766 0.5093 0.4059 0.061 Uiso 1 1 calc R . .
H8B H 1.0876 0.5765 0.3719 0.061 Uiso 1 1 calc R . .
H8C H 1.0487 0.5355 0.2943 0.061 Uiso 1 1 calc R . .
C9 C 0.9477(2) 0.76473(18) 0.24235(14) 0.0418(4) Uani 1 1 d . . .
H9A H 0.9733 0.7340 0.1849 0.063 Uiso 1 1 calc R . .
H9B H 1.0280 0.7761 0.2537 0.063 Uiso 1 1 calc R . .
H9C H 0.8740 0.8382 0.2314 0.063 Uiso 1 1 calc R . .
C10 C 0.86028(18) 0.73081(18) 0.41951(13) 0.0372(4) Uani 1 1 d . . .
H10A H 0.7866 0.8042 0.4084 0.056 Uiso 1 1 calc R . .
H10B H 0.9417 0.7430 0.4283 0.056 Uiso 1 1 calc R . .
H10C H 0.8291 0.6778 0.4781 0.056 Uiso 1 1 calc R . .
C11 C 0.38936(15) 0.71098(13) 0.42244(11) 0.0252(3) Uani 1 1 d . . .
C12 C 0.35191(18) 0.83957(15) 0.41412(15) 0.0383(4) Uani 1 1 d . . .
H12A H 0.3448 0.8824 0.3464 0.057 Uiso 1 1 calc R . .
H12B H 0.4236 0.8534 0.4348 0.057 Uiso 1 1 calc R . .
H12C H 0.2634 0.8650 0.4559 0.057 Uiso 1 1 calc R . .
C13 C 0.39883(18) 0.64655(15) 0.52905(12) 0.0355(4) Uani 1 1 d . . .
H13A H 0.3119 0.6767 0.5704 0.053 Uiso 1 1 calc R . .
H13B H 0.4742 0.6570 0.5482 0.053 Uiso 1 1 calc R . .
H13C H 0.4165 0.5647 0.5367 0.053 Uiso 1 1 calc R . .
C14 C 0.27413(18) 0.6907(2) 0.39387(16) 0.0471(5) Uani 1 1 d . . .
H14A H 0.2646 0.7334 0.3264 0.071 Uiso 1 1 calc R . .
H14B H 0.1875 0.7171 0.4370 0.071 Uiso 1 1 calc R . .
H14C H 0.2961 0.6087 0.3998 0.071 Uiso 1 1 calc R . .
C15 C 0.68601(14) 0.52796(12) 0.14558(10) 0.0200(3) Uani 1 1 d . . .
H15 H 0.7737 0.5320 0.0999 0.024 Uiso 1 1 calc R . .
C16 C 0.56985(16) 0.58925(13) 0.08463(11) 0.0268(3) Uani 1 1 d . . .
H16A H 0.5840 0.5486 0.0351 0.040 Uiso 1 1 calc R . .
H16B H 0.5703 0.6681 0.0527 0.040 Uiso 1 1 calc R . .
H16C H 0.4811 0.5902 0.1271 0.040 Uiso 1 1 calc R . .
C17 C 0.82920(14) 0.32481(12) 0.21863(10) 0.0194(3) Uani 1 1 d . . .
C18 C 0.70267(14) 0.40110(12) 0.19117(10) 0.0197(3) Uani 1 1 d . . .
C19 C 0.59284(15) 0.35921(13) 0.21145(11) 0.0229(3) Uani 1 1 d . . .
H19 H 0.5076 0.4098 0.1923 0.028 Uiso 1 1 calc R . .
C20 C 0.60341(16) 0.24498(13) 0.25910(11) 0.0249(3) Uani 1 1 d . A .
C21 C 0.72901(16) 0.17306(13) 0.28609(11) 0.0244(3) Uani 1 1 d . . .
H21 H 0.7370 0.0952 0.3187 0.029 Uiso 1 1 calc R . .
C22 C 0.84449(15) 0.20912(12) 0.26778(10) 0.0214(3) Uani 1 1 d . . .
C23 C 0.47852(18) 0.20333(15) 0.27903(13) 0.0343(4) Uani 1 1 d DU . .
C24 C 0.4459(5) 0.2139(4) 0.1780(3) 0.0346(8) Uani 0.707(13) 1 d PDU A 1
H24A H 0.3663 0.1879 0.1882 0.052 Uiso 0.707(13) 1 calc PR A 1
H24B H 0.5259 0.1664 0.1422 0.052 Uiso 0.707(13) 1 calc PR A 1
H24C H 0.4251 0.2941 0.1405 0.052 Uiso 0.707(13) 1 calc PR A 1
C25 C 0.3539(7) 0.2766(6) 0.3332(5) 0.0528(14) Uani 0.707(13) 1 d PDU A 1
H25A H 0.2758 0.2482 0.3449 0.079 Uiso 0.707(13) 1 calc PR A 1
H25B H 0.3309 0.3561 0.2942 0.079 Uiso 0.707(13) 1 calc PR A 1
H25C H 0.3742 0.2730 0.3956 0.079 Uiso 0.707(13) 1 calc PR A 1
C26 C 0.5092(6) 0.0774(4) 0.3329(6) 0.0623(15) Uani 0.707(13) 1 d PDU A 1
H26A H 0.4270 0.0542 0.3442 0.094 Uiso 0.707(13) 1 calc PR A 1
H26B H 0.5351 0.0657 0.3955 0.094 Uiso 0.707(13) 1 calc PR A 1
H26C H 0.5852 0.0310 0.2937 0.094 Uiso 0.707(13) 1 calc PR A 1
C24X C 0.4610(19) 0.1726(18) 0.1991(11) 0.071(3) Uani 0.293(13) 1 d PDU A 2
H24D H 0.3798 0.1465 0.2179 0.106 Uiso 0.293(13) 1 calc PR A 2
H24E H 0.5428 0.1108 0.1816 0.106 Uiso 0.293(13) 1 calc PR A 2
H24F H 0.4484 0.2394 0.1432 0.106 Uiso 0.293(13) 1 calc PR A 2
C25X C 0.3454(15) 0.3023(11) 0.3100(11) 0.042(2) Uani 0.293(13) 1 d PDU A 2
H25D H 0.3556 0.3182 0.3680 0.062 Uiso 0.293(13) 1 calc PR A 2
H25E H 0.2638 0.2776 0.3244 0.062 Uiso 0.293(13) 1 calc PR A 2
H25F H 0.3351 0.3718 0.2566 0.062 Uiso 0.293(13) 1 calc PR A 2
C26X C 0.4778(11) 0.1076(12) 0.3799(11) 0.062(3) Uani 0.293(13) 1 d PDU A 2
H26D H 0.4919 0.1346 0.4303 0.093 Uiso 0.293(13) 1 calc PR A 2
H26E H 0.5520 0.0367 0.3721 0.093 Uiso 0.293(13) 1 calc PR A 2
H26F H 0.3890 0.0927 0.3991 0.093 Uiso 0.293(13) 1 calc PR A 2
C27 C 0.98085(15) 0.12613(13) 0.30077(11) 0.0259(3) Uani 1 1 d . . .
C28 C 0.96868(19) 0.00670(14) 0.35513(14) 0.0378(4) Uani 1 1 d . . .
H28A H 1.0568 -0.0439 0.3754 0.057 Uiso 1 1 calc R . .
H28B H 0.9448 -0.0248 0.3120 0.057 Uiso 1 1 calc R . .
H28C H 0.8966 0.0125 0.4127 0.057 Uiso 1 1 calc R . .
C29 C 1.09595(18) 0.11270(16) 0.21218(13) 0.0393(4) Uani 1 1 d . . .
H29A H 1.1813 0.0574 0.2339 0.059 Uiso 1 1 calc R . .
H29B H 1.1106 0.1870 0.1785 0.059 Uiso 1 1 calc R . .
H29C H 1.0694 0.0851 0.1676 0.059 Uiso 1 1 calc R . .
C30 C 1.02104(17) 0.17080(15) 0.37039(12) 0.0335(4) Uani 1 1 d . . .
H30A H 0.9478 0.1784 0.4271 0.050 Uiso 1 1 calc R . .
H30B H 1.0338 0.2457 0.3366 0.050 Uiso 1 1 calc R . .
H30C H 1.1071 0.1167 0.3918 0.050 Uiso 1 1 calc R . .
N1 N 1.2202(2) 0.20315(14) -0.02115(12) 0.0534(5) Uani 1 1 d . . .
C31 C 1.3175(2) 0.15476(15) -0.06383(13) 0.0405(4) Uani 1 1 d . . .
C32 C 1.4421(2) 0.09467(18) -0.12050(16) 0.0496(5) Uani 1 1 d . . .
H32A H 1.5224 0.1040 -0.1069 0.074 Uiso 1 1 calc R . .
H32B H 1.4370 0.1265 -0.1900 0.074 Uiso 1 1 calc R . .
H32C H 1.4509 0.0130 -0.1028 0.074 Uiso 1 1 calc R . .
N2 N 0.2826(3) 0.8750(3) 0.0519(2) 0.0983(9) Uani 1 1 d . . .
C33 C 0.2310(3) 0.8302(3) 0.0267(2) 0.0681(7) Uani 1 1 d . . .
C34 C 0.1706(4) 0.7674(4) -0.0047(2) 0.0979(12) Uani 1 1 d . . .
H34A H 0.2161 0.7598 -0.0707 0.147 Uiso 1 1 calc R . .
H34B H 0.0721 0.8085 -0.0047 0.147 Uiso 1 1 calc R . .
H34C H 0.1823 0.6910 0.0398 0.147 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 0.01924(13) 0.02263(13) 0.01889(12) -0.00553(9) 0.00236(9) -0.01011(10)
O1 0.0302(6) 0.0197(5) 0.0215(5) -0.0056(4) 0.0028(4) -0.0104(4)
O2 0.0210(5) 0.0345(6) 0.0330(6) -0.0090(5) 0.0009(4) -0.0114(5)
O3 0.0216(5) 0.0285(5) 0.0218(5) -0.0099(4) 0.0038(4) -0.0127(4)
O4 0.0201(5) 0.0257(5) 0.0201(5) -0.0029(4) -0.0006(4) -0.0113(4)
C1 0.0197(6) 0.0199(6) 0.0175(6) -0.0032(5) 0.0009(5) -0.0082(5)
C2 0.0203(7) 0.0244(7) 0.0202(7) -0.0054(5) -0.0020(5) -0.0099(6)
C3 0.0226(7) 0.0246(7) 0.0207(7) -0.0075(5) -0.0012(5) -0.0093(6)
C4 0.0191(6) 0.0215(7) 0.0209(7) -0.0043(5) -0.0018(5) -0.0072(5)
C5 0.0193(6) 0.0209(7) 0.0225(7) -0.0038(5) -0.0041(5) -0.0087(5)
C6 0.0221(7) 0.0179(6) 0.0176(6) -0.0022(5) -0.0040(5) -0.0076(5)
C7 0.0219(7) 0.0404(9) 0.0289(8) -0.0169(7) 0.0011(6) -0.0156(7)
C8 0.0251(8) 0.0570(12) 0.0478(11) -0.0257(9) -0.0117(7) -0.0072(8)
C9 0.0462(10) 0.0569(12) 0.0386(10) -0.0205(9) 0.0081(8) -0.0374(9)
C10 0.0283(8) 0.0611(12) 0.0377(9) -0.0286(9) 0.0009(7) -0.0218(8)
C11 0.0190(7) 0.0288(8) 0.0288(8) -0.0115(6) 0.0010(6) -0.0083(6)
C12 0.0271(8) 0.0290(8) 0.0497(11) -0.0103(8) 0.0023(7) -0.0042(7)
C13 0.0318(8) 0.0359(9) 0.0289(8) -0.0092(7) 0.0064(7) -0.0065(7)
C14 0.0222(8) 0.0776(15) 0.0569(12) -0.0420(11) 0.0062(8) -0.0199(9)
C15 0.0223(7) 0.0208(7) 0.0179(6) -0.0040(5) -0.0037(5) -0.0083(5)
C16 0.0326(8) 0.0249(7) 0.0245(7) -0.0032(6) -0.0116(6) -0.0086(6)
C17 0.0204(6) 0.0232(7) 0.0159(6) -0.0047(5) 0.0001(5) -0.0107(5)
C18 0.0230(7) 0.0211(7) 0.0162(6) -0.0050(5) -0.0021(5) -0.0088(5)
C19 0.0225(7) 0.0251(7) 0.0234(7) -0.0059(6) -0.0049(5) -0.0091(6)
C20 0.0272(7) 0.0282(7) 0.0245(7) -0.0049(6) -0.0047(6) -0.0157(6)
C21 0.0306(8) 0.0214(7) 0.0228(7) -0.0022(5) -0.0044(6) -0.0129(6)
C22 0.0231(7) 0.0233(7) 0.0173(6) -0.0050(5) -0.0011(5) -0.0083(6)
C23 0.0335(8) 0.0354(8) 0.0413(9) -0.0015(7) -0.0106(7) -0.0226(7)
C24 0.0333(15) 0.0351(18) 0.0458(15) -0.0137(13) -0.0106(12) -0.0166(15)
C25 0.049(2) 0.085(3) 0.045(3) -0.029(3) 0.016(2) -0.049(2)
C26 0.065(3) 0.0524(17) 0.080(3) 0.0250(18) -0.037(2) -0.0464(17)
C24X 0.078(7) 0.095(8) 0.077(5) -0.042(5) -0.001(5) -0.059(7)
C25X 0.025(3) 0.051(4) 0.040(6) 0.004(3) 0.008(3) -0.024(2)
C26X 0.041(4) 0.054(5) 0.082(5) 0.029(4) -0.020(5) -0.037(4)
C27 0.0241(7) 0.0236(7) 0.0243(7) 0.0001(6) -0.0024(6) -0.0074(6)
C28 0.0341(9) 0.0243(8) 0.0455(10) 0.0055(7) -0.0116(8) -0.0073(7)
C29 0.0302(9) 0.0364(9) 0.0344(9) -0.0045(7) 0.0029(7) -0.0010(7)
C30 0.0298(8) 0.0375(9) 0.0311(8) 0.0008(7) -0.0108(7) -0.0124(7)
N1 0.0691(12) 0.0324(8) 0.0347(9) -0.0038(7) 0.0082(8) -0.0047(8)
C31 0.0563(12) 0.0281(9) 0.0323(9) -0.0033(7) -0.0042(8) -0.0137(8)
C32 0.0526(12) 0.0405(11) 0.0480(12) -0.0159(9) 0.0022(9) -0.0093(9)
N2 0.0869(19) 0.099(2) 0.140(3) -0.062(2) -0.0154(18) -0.0379(16)
C33 0.0645(16) 0.0890(19) 0.0682(16) -0.0390(15) 0.0085(12) -0.0404(15)
C34 0.113(3) 0.168(3) 0.0613(17) -0.064(2) 0.0293(16) -0.099(3)

_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 O2 1.5840(11) . ?
V1 O4 1.8054(10) . ?
V1 O3 1.8131(10) . ?
V1 O1 1.9559(11) 2_765 ?
V1 O1 1.9752(11) . ?
O3 C1 1.3526(16) . ?
O4 C17 1.3576(16) . ?
C1 C6 1.4002(19) . ?
C1 C2 1.4162(19) . ?
C2 C3 1.3896(19) . ?
C2 C7 1.5370(19) . ?
C3 C4 1.400(2) . ?
C4 C5 1.388(2) . ?
C4 C11 1.5350(19) . ?
C5 C6 1.3986(19) . ?
C6 C15 1.5278(19) . ?
C7 C10 1.534(2) . ?
C7 C9 1.535(2) . ?
C7 C8 1.544(2) . ?
C11 C14 1.522(2) . ?
C11 C13 1.532(2) . ?
C11 C12 1.535(2) . ?
C15 C18 1.5251(19) . ?
C15 C16 1.5347(19) . ?
C17 C22 1.4089(19) . ?
C17 C18 1.410(2) . ?
C18 C19 1.3852(19) . ?
C19 C20 1.396(2) . ?
C20 C21 1.387(2) . ?
C20 C23 1.534(2) . ?
C21 C22 1.399(2) . ?
C22 C27 1.539(2) . ?
C23 C24X 1.430(10) . ?
C23 C25 1.510(6) . ?
C23 C26 1.521(4) . ?
C23 C24 1.566(4) . ?
C23 C25X 1.593(10) . ?
C23 C26X 1.601(8) . ?
C27 C28 1.534(2) . ?
C27 C29 1.536(2) . ?
C27 C30 1.537(2) . ?
N1 C31 1.132(2) . ?
C31 C32 1.455(3) . ?
N2 C33 1.121(3) . ?
C33 C34 1.440(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O4 104.92(5) . . ?
O2 V1 O3 104.13(5) . . ?
O4 V1 O3 94.26(5) . . ?
O2 V1 O1 104.35(5) . 2_765 ?
O4 V1 O1 148.59(5) . 2_765 ?
O3 V1 O1 89.44(5) . 2_765 ?
O2 V1 O1 105.07(5) . . ?
O4 V1 O1 88.85(4) . . ?
O3 V1 O1 148.73(5) . . ?
O1 V1 O1 72.72(5) 2_765 . ?
V1 O1 V1 107.28(5) 2_765 . ?
C1 O3 V1 136.01(9) . . ?
C17 O4 V1 138.07(9) . . ?
O3 C1 C6 121.10(12) . . ?
O3 C1 C2 117.73(12) . . ?
C6 C1 C2 121.17(12) . . ?
C3 C2 C1 117.26(13) . . ?
C3 C2 C7 121.48(13) . . ?
C1 C2 C7 121.26(12) . . ?
C2 C3 C4 123.32(13) . . ?
C5 C4 C3 117.46(13) . . ?
C5 C4 C11 123.23(13) . . ?
C3 C4 C11 119.30(13) . . ?
C4 C5 C6 122.09(13) . . ?
C5 C6 C1 118.68(12) . . ?
C5 C6 C15 119.44(12) . . ?
C1 C6 C15 121.87(12) . . ?
C10 C7 C9 107.51(14) . . ?
C10 C7 C2 111.95(12) . . ?
C9 C7 C2 109.82(13) . . ?
C10 C7 C8 107.34(14) . . ?
C9 C7 C8 110.52(14) . . ?
C2 C7 C8 109.65(13) . . ?
C14 C11 C13 108.34(15) . . ?
C14 C11 C4 112.03(13) . . ?
C13 C11 C4 110.54(12) . . ?
C14 C11 C12 108.66(15) . . ?
C13 C11 C12 108.22(14) . . ?
C4 C11 C12 108.96(12) . . ?
C18 C15 C6 110.13(11) . . ?
C18 C15 C16 113.69(12) . . ?
C6 C15 C16 112.73(12) . . ?
O4 C17 C22 118.44(12) . . ?
O4 C17 C18 119.99(12) . . ?
C22 C17 C18 121.55(12) . . ?
C19 C18 C17 118.45(13) . . ?
C19 C18 C15 121.17(13) . . ?
C17 C18 C15 120.29(12) . . ?
C18 C19 C20 122.07(14) . . ?
C21 C20 C19 117.73(13) . . ?
C21 C20 C23 122.54(14) . . ?
C19 C20 C23 119.73(14) . . ?
C20 C21 C22 123.41(13) . . ?
C21 C22 C17 116.77(13) . . ?
C21 C22 C27 121.29(13) . . ?
C17 C22 C27 121.93(13) . . ?
C24X C23 C25 118.4(8) . . ?
C24X C23 C26 87.4(7) . . ?
C25 C23 C26 111.0(3) . . ?
C24X C23 C20 114.6(7) . . ?
C25 C23 C20 111.2(3) . . ?
C26 C23 C20 112.0(2) . . ?
C25 C23 C24 108.6(3) . . ?
C26 C23 C24 106.5(3) . . ?
C20 C23 C24 107.3(2) . . ?
C24X C23 C25X 110.3(10) . . ?
C20 C23 C25X 107.5(7) . . ?
C24X C23 C26X 114.6(7) . . ?
C20 C23 C26X 109.8(4) . . ?
C25X C23 C26X 98.8(7) . . ?
C28 C27 C29 107.63(14) . . ?
C28 C27 C30 107.54(13) . . ?
C29 C27 C30 109.73(14) . . ?
C28 C27 C22 111.46(13) . . ?
C29 C27 C22 110.27(13) . . ?
C30 C27 C22 110.13(13) . . ?
N1 C31 C32 178.8(2) . . ?
N2 C33 C34 177.0(4) . . ?

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
O2 V1 O1 V1 -100.67(6) . . . 2_765 ?
O4 V1 O1 V1 154.19(6) . . . 2_765 ?
O3 V1 O1 V1 57.86(10) . . . 2_765 ?
O1 V1 O1 V1 -0.002(2) 2_765 . . 2_765 ?
O2 V1 O3 C1 -142.60(13) . . . . ?
O4 V1 O3 C1 -36.04(13) . . . . ?
O1 V1 O3 C1 112.73(13) 2_765 . . . ?
O1 V1 O3 C1 58.77(17) . . . . ?
O2 V1 O4 C17 -165.60(13) . . . . ?
O3 V1 O4 C17 88.54(14) . . . . ?
O1 V1 O4 C17 -7.39(19) 2_765 . . . ?
O1 V1 O4 C17 -60.30(14) . . . . ?
V1 O3 C1 C6 -29.1(2) . . . . ?
V1 O3 C1 C2 151.38(11) . . . . ?
O3 C1 C2 C3 178.81(12) . . . . ?
C6 C1 C2 C3 -0.8(2) . . . . ?
O3 C1 C2 C7 -1.8(2) . . . . ?
C6 C1 C2 C7 178.63(13) . . . . ?
C1 C2 C3 C4 -0.4(2) . . . . ?
C7 C2 C3 C4 -179.75(14) . . . . ?
C2 C3 C4 C5 1.4(2) . . . . ?
C2 C3 C4 C11 -178.59(13) . . . . ?
C3 C4 C5 C6 -1.3(2) . . . . ?
C11 C4 C5 C6 178.65(13) . . . . ?
C4 C5 C6 C1 0.3(2) . . . . ?
C4 C5 C6 C15 178.62(13) . . . . ?
O3 C1 C6 C5 -178.74(12) . . . . ?
C2 C1 C6 C5 0.8(2) . . . . ?
O3 C1 C6 C15 2.9(2) . . . . ?
C2 C1 C6 C15 -177.51(12) . . . . ?
C3 C2 C7 C10 2.2(2) . . . . ?
C1 C2 C7 C10 -177.15(14) . . . . ?
C3 C2 C7 C9 -117.14(16) . . . . ?
C1 C2 C7 C9 63.50(18) . . . . ?
C3 C2 C7 C8 121.24(16) . . . . ?
C1 C2 C7 C8 -58.12(18) . . . . ?
C5 C4 C11 C14 -2.8(2) . . . . ?
C3 C4 C11 C14 177.12(15) . . . . ?
C5 C4 C11 C13 118.11(16) . . . . ?
C3 C4 C11 C13 -61.95(18) . . . . ?
C5 C4 C11 C12 -123.09(16) . . . . ?
C3 C4 C11 C12 56.86(18) . . . . ?
C5 C6 C15 C18 -80.21(15) . . . . ?
C1 C6 C15 C18 98.10(15) . . . . ?
C5 C6 C15 C16 47.93(17) . . . . ?
C1 C6 C15 C16 -133.76(14) . . . . ?
V1 O4 C17 C22 153.46(11) . . . . ?
V1 O4 C17 C18 -28.1(2) . . . . ?
O4 C17 C18 C19 -179.94(12) . . . . ?
C22 C17 C18 C19 -1.6(2) . . . . ?
O4 C17 C18 C15 -3.41(19) . . . . ?
C22 C17 C18 C15 174.95(13) . . . . ?
C6 C15 C18 C19 101.33(15) . . . . ?
C16 C15 C18 C19 -26.28(19) . . . . ?
C6 C15 C18 C17 -75.11(16) . . . . ?
C16 C15 C18 C17 157.28(13) . . . . ?
C17 C18 C19 C20 0.9(2) . . . . ?
C15 C18 C19 C20 -175.60(13) . . . . ?
C18 C19 C20 C21 0.0(2) . . . . ?
C18 C19 C20 C23 -179.62(14) . . . . ?
C19 C20 C21 C22 -0.2(2) . . . . ?
C23 C20 C21 C22 179.38(15) . . . . ?
C20 C21 C22 C17 -0.5(2) . . . . ?
C20 C21 C22 C27 179.02(14) . . . . ?
O4 C17 C22 C21 179.74(12) . . . . ?
C18 C17 C22 C21 1.4(2) . . . . ?
O4 C17 C22 C27 0.3(2) . . . . ?
C18 C17 C22 C27 -178.12(13) . . . . ?
C21 C20 C23 C24X -96.2(10) . . . . ?
C19 C20 C23 C24X 83.4(10) . . . . ?
C21 C20 C23 C25 126.2(4) . . . . ?
C19 C20 C23 C25 -54.2(4) . . . . ?
C21 C20 C23 C26 1.4(4) . . . . ?
C19 C20 C23 C26 -179.0(4) . . . . ?
C21 C20 C23 C24 -115.1(2) . . . . ?
C19 C20 C23 C24 64.4(2) . . . . ?
C21 C20 C23 C25X 140.9(6) . . . . ?
C19 C20 C23 C25X -39.6(6) . . . . ?
C21 C20 C23 C26X 34.5(8) . . . . ?
C19 C20 C23 C26X -146.0(8) . . . . ?
C21 C22 C27 C28 -1.2(2) . . . . ?
C17 C22 C27 C28 178.27(14) . . . . ?
C21 C22 C27 C29 118.29(16) . . . . ?
C17 C22 C27 C29 -62.25(19) . . . . ?
C21 C22 C27 C30 -120.46(15) . . . . ?
C17 C22 C27 C30 58.99(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N1 0.75(2) 2.06(2) 2.796(2) 168(2) .

_diffrn_measured_fraction_theta_max 0.864
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.050

#===END

data_7b
_database_code_depnum_ccdc_archive 'CCDC 718348'

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '[{V(O)(diphenolate)(\m-OPr)}2].2MeCN'
_chemical_formula_moiety         'C66 H102 O8 V2, 2(C2 H3 N)'
_chemical_formula_sum            'C70 H108 N2 O8 V2'
_chemical_formula_weight         1207.46

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'
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                   12.5074(4)
_cell_length_b                   15.8414(7)
_cell_length_c                   17.6437(7)
_cell_angle_alpha                88.361(3)
_cell_angle_beta                 84.915(3)
_cell_angle_gamma                87.381(3)
_cell_volume                     3477.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    11414
_cell_measurement_theta_min      3.0416
_cell_measurement_theta_max      28.5989

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2008)'

_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         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55721
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_sigmaI/netI    0.1328
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12205
_reflns_number_gt                7084
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2008)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2008)'
_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>, 1996)'
_computing_publication_material  
;
SHELXL-97 (Sheldrick, 2008), 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.

Crystals of 7b were weakly diffracting, leading to a high Rint value.
;

_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^)+(0.1474P)^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         12205
_refine_ls_number_parameters     831
_refine_ls_number_restraints     954
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.0974
_refine_ls_wR_factor_ref         0.2569
_refine_ls_wR_factor_gt          0.2274
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.83151(7) 0.22871(6) 0.20676(5) 0.0199(3) Uani 1 1 d U . .
V2 V 0.82561(7) 0.07009(6) 0.32364(5) 0.0187(3) Uani 1 1 d U . .
O1 O 0.7361(3) 0.1489(2) 0.2644(2) 0.0244(9) Uani 1 1 d U . .
O2 O 0.9180(3) 0.1561(2) 0.2725(2) 0.0260(9) Uani 1 1 d U . .
O3 O 0.7285(3) -0.0102(2) 0.31755(19) 0.0221(8) Uani 1 1 d U . .
O4 O 0.9406(3) -0.0040(2) 0.32350(19) 0.0209(8) Uani 1 1 d U . .
O5 O 0.8061(3) 0.0979(2) 0.4084(2) 0.0248(9) Uani 1 1 d U . .
O6 O 0.7195(3) 0.3005(2) 0.1918(2) 0.0217(8) Uani 1 1 d U . .
O7 O 0.9231(3) 0.3124(2) 0.2125(2) 0.0239(9) Uani 1 1 d U . .
O8 O 0.8615(3) 0.1918(2) 0.1258(2) 0.0277(9) Uani 1 1 d U . .
C1 C 1.0291(4) 0.1705(4) 0.2861(3) 0.0298(14) Uani 1 1 d U . .
H1A H 1.0639 0.2017 0.2419 0.036 Uiso 1 1 calc R . .
H1B H 1.0687 0.1153 0.2911 0.036 Uiso 1 1 calc R . .
C2 C 1.0359(5) 0.2202(4) 0.3574(3) 0.0311(14) Uani 1 1 d U . .
H2A H 1.0039 0.1880 0.4020 0.037 Uiso 1 1 calc R . .
H2B H 0.9943 0.2745 0.3533 0.037 Uiso 1 1 calc R . .
C3 C 1.1518(6) 0.2372(5) 0.3689(4) 0.052(2) Uani 1 1 d U . .
H3A H 1.1924 0.1835 0.3747 0.078 Uiso 1 1 calc R . .
H3B H 1.1540 0.2704 0.4147 0.078 Uiso 1 1 calc R . .
H3C H 1.1836 0.2689 0.3246 0.078 Uiso 1 1 calc R . .
C4 C 0.7205(4) -0.0822(3) 0.2793(3) 0.0202(11) Uani 1 1 d U . .
C5 C 0.6510(4) -0.1435(3) 0.3113(3) 0.0214(12) Uani 1 1 d U . .
C6 C 0.6425(4) -0.2155(3) 0.2693(3) 0.0228(12) Uani 1 1 d U . .
H6 H 0.5945 -0.2569 0.2896 0.027 Uiso 1 1 calc R . .
C7 C 0.6994(4) -0.2308(4) 0.1998(3) 0.0246(12) Uani 1 1 d U . .
C8 C 0.7691(4) -0.1692(3) 0.1721(3) 0.0237(12) Uani 1 1 d U . .
H8 H 0.8105 -0.1778 0.1249 0.028 Uiso 1 1 calc R . .
C9 C 0.7805(4) -0.0961(3) 0.2102(3) 0.0204(12) Uani 1 1 d U . .
C10 C 0.8646(4) -0.0328(3) 0.1775(3) 0.0203(12) Uani 1 1 d U . .
H10 H 0.8465 0.0221 0.2032 0.024 Uiso 1 1 calc R . .
C11 C 0.9744(4) -0.0644(3) 0.2008(3) 0.0212(12) Uani 1 1 d U . .
C12 C 1.0031(4) -0.0533(3) 0.2744(3) 0.0197(11) Uani 1 1 d U . .
C13 C 1.0969(4) -0.0945(3) 0.3008(3) 0.0201(11) Uani 1 1 d U . .
C14 C 1.1601(4) -0.1415(3) 0.2477(3) 0.0231(12) Uani 1 1 d U A .
H14 H 1.2236 -0.1691 0.2637 0.028 Uiso 1 1 calc R . .
C15 C 1.1383(5) -0.1512(3) 0.1737(3) 0.0249(12) Uani 1 1 d U . .
C16 C 1.0429(5) -0.1128(3) 0.1515(3) 0.0244(12) Uani 1 1 d U A .
H16 H 1.0243 -0.1201 0.1012 0.029 Uiso 1 1 calc R . .
C17A C 1.2100(6) -0.2028(4) 0.1171(3) 0.0430(15) Uani 0.431(15) 1 d PDU A 1
C18A C 1.2555(13) -0.2864(8) 0.1575(7) 0.026(3) Uani 0.431(15) 1 d PDU A 1
H18A H 1.3029 -0.2711 0.1959 0.039 Uiso 0.431(15) 1 calc PR A 1
H18B H 1.2960 -0.3219 0.1194 0.039 Uiso 0.431(15) 1 calc PR A 1
H18C H 1.1956 -0.3176 0.1822 0.039 Uiso 0.431(15) 1 calc PR A 1
C19A C 1.1689(18) -0.2223(17) 0.0442(10) 0.068(6) Uani 0.431(15) 1 d PDU A 1
H19A H 1.1036 -0.2542 0.0539 0.102 Uiso 0.431(15) 1 calc PR A 1
H19B H 1.2234 -0.2560 0.0136 0.102 Uiso 0.431(15) 1 calc PR A 1
H19C H 1.1522 -0.1694 0.0165 0.102 Uiso 0.431(15) 1 calc PR A 1
C20A C 1.3124(13) -0.1485(10) 0.0985(12) 0.055(5) Uani 0.431(15) 1 d PDU A 1
H20A H 1.2900 -0.0886 0.0946 0.083 Uiso 0.431(15) 1 calc PR A 1
H20B H 1.3502 -0.1663 0.0502 0.083 Uiso 0.431(15) 1 calc PR A 1
H20C H 1.3604 -0.1571 0.1393 0.083 Uiso 0.431(15) 1 calc PR A 1
C17B C 1.2100(6) -0.2028(4) 0.1171(3) 0.0430(15) Uani 0.569(15) 1 d PDU A 2
C18B C 1.2919(12) -0.2599(10) 0.1530(8) 0.056(4) Uani 0.569(15) 1 d PDU A 2
H18D H 1.3462 -0.2257 0.1726 0.085 Uiso 0.569(15) 1 calc PR A 2
H18E H 1.3266 -0.2983 0.1148 0.085 Uiso 0.569(15) 1 calc PR A 2
H18F H 1.2562 -0.2929 0.1950 0.085 Uiso 0.569(15) 1 calc PR A 2
C19B C 1.1368(11) -0.2590(8) 0.0737(8) 0.040(3) Uani 0.569(15) 1 d PDU A 2
H19D H 1.0885 -0.2895 0.1106 0.061 Uiso 0.569(15) 1 calc PR A 2
H19E H 1.1818 -0.2996 0.0428 0.061 Uiso 0.569(15) 1 calc PR A 2
H19F H 1.0942 -0.2229 0.0406 0.061 Uiso 0.569(15) 1 calc PR A 2
C20B C 1.2600(11) -0.1444(8) 0.0544(7) 0.047(4) Uani 0.569(15) 1 d PDU A 2
H20D H 1.2031 -0.1173 0.0262 0.070 Uiso 0.569(15) 1 calc PR A 2
H20E H 1.3096 -0.1776 0.0195 0.070 Uiso 0.569(15) 1 calc PR A 2
H20F H 1.2994 -0.1010 0.0773 0.070 Uiso 0.569(15) 1 calc PR A 2
C21 C 1.1249(4) -0.0893(3) 0.3834(3) 0.0220(12) Uani 1 1 d U . .
C22 C 1.1590(5) 0.0000(4) 0.3998(3) 0.0308(14) Uani 1 1 d U . .
H22A H 1.2182 0.0157 0.3627 0.046 Uiso 1 1 calc R . .
H22B H 1.1826 0.0007 0.4513 0.046 Uiso 1 1 calc R . .
H22C H 1.0979 0.0403 0.3958 0.046 Uiso 1 1 calc R . .
C23 C 1.2184(5) -0.1510(4) 0.3998(3) 0.0322(14) Uani 1 1 d U . .
H23A H 1.2824 -0.1367 0.3666 0.048 Uiso 1 1 calc R . .
H23B H 1.1992 -0.2087 0.3901 0.048 Uiso 1 1 calc R . .
H23C H 1.2334 -0.1469 0.4531 0.048 Uiso 1 1 calc R . .
C24 C 1.0298(5) -0.1123(4) 0.4407(3) 0.0299(14) Uani 1 1 d U . .
H24A H 1.0531 -0.1142 0.4924 0.045 Uiso 1 1 calc R . .
H24B H 1.0048 -0.1677 0.4288 0.045 Uiso 1 1 calc R . .
H24C H 0.9712 -0.0695 0.4375 0.045 Uiso 1 1 calc R . .
C25 C 0.8611(5) -0.0157(4) 0.0918(3) 0.0285(14) Uani 1 1 d U . .
H25A H 0.9187 0.0217 0.0736 0.043 Uiso 1 1 calc R . .
H25B H 0.7915 0.0112 0.0820 0.043 Uiso 1 1 calc R . .
H25C H 0.8711 -0.0693 0.0651 0.043 Uiso 1 1 calc R . .
C26 C 0.6847(5) -0.3127(4) 0.1576(3) 0.0304(14) Uani 1 1 d U . .
C27 C 0.5653(6) -0.3135(5) 0.1397(5) 0.060(2) Uani 1 1 d U . .
H27A H 0.5500 -0.2669 0.1040 0.090 Uiso 1 1 calc R . .
H27B H 0.5185 -0.3069 0.1869 0.090 Uiso 1 1 calc R . .
H27C H 0.5522 -0.3674 0.1168 0.090 Uiso 1 1 calc R . .
C28 C 0.7033(6) -0.3909(4) 0.2081(4) 0.0521(19) Uani 1 1 d U . .
H28A H 0.6880 -0.4416 0.1810 0.078 Uiso 1 1 calc R . .
H28B H 0.6557 -0.3869 0.2551 0.078 Uiso 1 1 calc R . .
H28C H 0.7783 -0.3945 0.2205 0.078 Uiso 1 1 calc R . .
C29 C 0.7559(7) -0.3202(5) 0.0856(4) 0.069(3) Uani 1 1 d U . .
H29A H 0.7455 -0.2696 0.0534 0.104 Uiso 1 1 calc R . .
H29B H 0.7380 -0.3702 0.0587 0.104 Uiso 1 1 calc R . .
H29C H 0.8310 -0.3258 0.0975 0.104 Uiso 1 1 calc R . .
C30 C 0.5870(5) -0.1306(4) 0.3896(3) 0.0292(13) Uani 1 1 d U . .
C31 C 0.5240(5) -0.2090(4) 0.4159(4) 0.0385(16) Uani 1 1 d U . .
H31A H 0.4887 -0.2002 0.4671 0.058 Uiso 1 1 calc R . .
H31B H 0.5735 -0.2587 0.4168 0.058 Uiso 1 1 calc R . .
H31C H 0.4696 -0.2180 0.3805 0.058 Uiso 1 1 calc R . .
C32 C 0.6635(6) -0.1168(4) 0.4513(3) 0.0431(17) Uani 1 1 d U . .
H32A H 0.7049 -0.0667 0.4379 0.065 Uiso 1 1 calc R . .
H32B H 0.7127 -0.1664 0.4552 0.065 Uiso 1 1 calc R . .
H32C H 0.6215 -0.1085 0.5004 0.065 Uiso 1 1 calc R . .
C33 C 0.5061(5) -0.0555(4) 0.3841(4) 0.0434(17) Uani 1 1 d U . .
H33A H 0.4597 -0.0518 0.4317 0.065 Uiso 1 1 calc R . .
H33B H 0.4621 -0.0635 0.3418 0.065 Uiso 1 1 calc R . .
H33C H 0.5448 -0.0032 0.3752 0.065 Uiso 1 1 calc R . .
C34 C 0.6184(4) 0.1470(4) 0.2675(3) 0.0298(14) Uani 1 1 d U . .
H34A H 0.5976 0.0888 0.2587 0.036 Uiso 1 1 calc R . .
H34B H 0.5921 0.1843 0.2265 0.036 Uiso 1 1 calc R . .
C35 C 0.5662(5) 0.1757(4) 0.3435(4) 0.0364(15) Uani 1 1 d U . .
H35A H 0.5962 0.2295 0.3569 0.044 Uiso 1 1 calc R . .
H35B H 0.5808 0.1328 0.3836 0.044 Uiso 1 1 calc R . .
C36 C 0.4457(6) 0.1881(5) 0.3385(4) 0.0542(19) Uani 1 1 d U . .
H36A H 0.4315 0.2338 0.3017 0.081 Uiso 1 1 calc R . .
H36B H 0.4106 0.2026 0.3885 0.081 Uiso 1 1 calc R . .
H36C H 0.4172 0.1357 0.3219 0.081 Uiso 1 1 calc R . .
C37 C 0.6466(4) 0.3534(3) 0.2309(3) 0.0166(11) Uani 1 1 d U . .
C38 C 0.5567(4) 0.3855(3) 0.1934(3) 0.0198(11) Uani 1 1 d U . .
C39 C 0.4801(4) 0.4324(3) 0.2372(3) 0.0206(12) Uani 1 1 d U . .
H39 H 0.4186 0.4541 0.2138 0.025 Uiso 1 1 calc R . .
C40 C 0.4868(4) 0.4496(4) 0.3116(3) 0.0268(13) Uani 1 1 d U . .
C41 C 0.5801(4) 0.4230(3) 0.3453(3) 0.0208(12) Uani 1 1 d U . .
H41 H 0.5885 0.4383 0.3961 0.025 Uiso 1 1 calc R . .
C42 C 0.6608(4) 0.3743(3) 0.3055(3) 0.0195(11) Uani 1 1 d U . .
C43 C 0.7648(4) 0.3490(3) 0.3409(3) 0.0186(11) Uani 1 1 d U . .
H43 H 0.7872 0.2915 0.3218 0.022 Uiso 1 1 calc R . .
C44 C 0.8540(4) 0.4073(3) 0.3106(3) 0.0207(12) Uani 1 1 d U . .
C45 C 0.9230(4) 0.3890(3) 0.2456(3) 0.0208(12) Uani 1 1 d U . .
C46 C 0.9990(4) 0.4477(3) 0.2138(3) 0.0228(12) Uani 1 1 d U . .
C47 C 1.0030(4) 0.5229(3) 0.2525(3) 0.0244(12) Uani 1 1 d U B .
H47 H 1.0543 0.5626 0.2337 0.029 Uiso 1 1 calc R . .
C48 C 0.9360(5) 0.5429(4) 0.3172(3) 0.0264(12) Uani 1 1 d U . .
C49 C 0.8614(4) 0.4845(3) 0.3442(3) 0.0223(12) Uani 1 1 d U B .
H49 H 0.8136 0.4980 0.3875 0.027 Uiso 1 1 calc R . .
C50A C 0.9454(5) 0.6266(4) 0.3588(3) 0.0340(14) Uani 0.56(3) 1 d PDU B 1
C51A C 0.8366(11) 0.6656(18) 0.3868(13) 0.051(5) Uani 0.56(3) 1 d PDU B 1
H51A H 0.7996 0.6266 0.4233 0.076 Uiso 0.56(3) 1 calc PR B 1
H51B H 0.7934 0.6765 0.3435 0.076 Uiso 0.56(3) 1 calc PR B 1
H51C H 0.8463 0.7189 0.4116 0.076 Uiso 0.56(3) 1 calc PR B 1
C52A C 1.0075(16) 0.6041(13) 0.4288(10) 0.052(5) Uani 0.56(3) 1 d PDU B 1
H52A H 1.0180 0.6557 0.4561 0.078 Uiso 0.56(3) 1 calc PR B 1
H52B H 1.0775 0.5774 0.4122 0.078 Uiso 0.56(3) 1 calc PR B 1
H52C H 0.9663 0.5649 0.4627 0.078 Uiso 0.56(3) 1 calc PR B 1
C53A C 1.010(3) 0.6904(12) 0.3095(11) 0.077(7) Uani 0.56(3) 1 d PDU B 1
H53A H 0.9724 0.7052 0.2641 0.115 Uiso 0.56(3) 1 calc PR B 1
H53B H 1.0812 0.6656 0.2942 0.115 Uiso 0.56(3) 1 calc PR B 1
H53C H 1.0166 0.7414 0.3385 0.115 Uiso 0.56(3) 1 calc PR B 1
C50B C 0.9454(5) 0.6266(4) 0.3588(3) 0.0340(14) Uani 0.44(3) 1 d PDU B 2
C51B C 0.849(2) 0.6475(19) 0.4149(17) 0.053(7) Uani 0.44(3) 1 d PDU B 2
H51D H 0.8474 0.6068 0.4578 0.079 Uiso 0.44(3) 1 calc PR B 2
H51E H 0.7826 0.6444 0.3893 0.079 Uiso 0.44(3) 1 calc PR B 2
H51F H 0.8539 0.7047 0.4337 0.079 Uiso 0.44(3) 1 calc PR B 2
C52B C 1.0490(19) 0.6263(15) 0.3984(19) 0.055(7) Uani 0.44(3) 1 d PDU B 2
H52D H 1.0507 0.6783 0.4269 0.083 Uiso 0.44(3) 1 calc PR B 2
H52E H 1.1108 0.6229 0.3602 0.083 Uiso 0.44(3) 1 calc PR B 2
H52F H 1.0520 0.5773 0.4335 0.083 Uiso 0.44(3) 1 calc PR B 2
C53B C 0.947(2) 0.7010(11) 0.2999(10) 0.041(5) Uani 0.44(3) 1 d PDU B 2
H53D H 0.9511 0.7544 0.3261 0.061 Uiso 0.44(3) 1 calc PR B 2
H53E H 0.8819 0.7021 0.2731 0.061 Uiso 0.44(3) 1 calc PR B 2
H53F H 1.0103 0.6936 0.2631 0.061 Uiso 0.44(3) 1 calc PR B 2
C54 C 1.0685(5) 0.4294(4) 0.1398(3) 0.0297(13) Uani 1 1 d U . .
C55 C 1.1471(5) 0.3531(4) 0.1508(4) 0.0423(16) Uani 1 1 d U . .
H55A H 1.1932 0.3649 0.1910 0.063 Uiso 1 1 calc R . .
H55B H 1.1917 0.3431 0.1031 0.063 Uiso 1 1 calc R . .
H55C H 1.1064 0.3029 0.1652 0.063 Uiso 1 1 calc R . .
C56 C 0.9950(6) 0.4138(4) 0.0770(3) 0.0425(17) Uani 1 1 d U . .
H56A H 0.9599 0.3601 0.0876 0.064 Uiso 1 1 calc R . .
H56B H 1.0378 0.4112 0.0278 0.064 Uiso 1 1 calc R . .
H56C H 0.9402 0.4599 0.0755 0.064 Uiso 1 1 calc R . .
C57 C 1.1367(5) 0.5053(4) 0.1140(4) 0.0393(16) Uani 1 1 d U . .
H57A H 1.0893 0.5553 0.1067 0.059 Uiso 1 1 calc R . .
H57B H 1.1790 0.4925 0.0659 0.059 Uiso 1 1 calc R . .
H57C H 1.1852 0.5163 0.1529 0.059 Uiso 1 1 calc R . .
C58 C 0.7548(5) 0.3406(4) 0.4277(3) 0.0268(13) Uani 1 1 d U . .
H58A H 0.7335 0.3956 0.4495 0.040 Uiso 1 1 calc R . .
H58B H 0.8241 0.3209 0.4451 0.040 Uiso 1 1 calc R . .
H58C H 0.7004 0.2998 0.4441 0.040 Uiso 1 1 calc R . .
C59 C 0.3987(5) 0.4997(4) 0.3589(3) 0.0400(16) Uani 1 1 d U . .
C60 C 0.4396(8) 0.5793(5) 0.3871(6) 0.088(3) Uani 1 1 d U . .
H60A H 0.4975 0.5651 0.4199 0.132 Uiso 1 1 calc R . .
H60B H 0.3810 0.6105 0.4162 0.132 Uiso 1 1 calc R . .
H60C H 0.4673 0.6143 0.3437 0.132 Uiso 1 1 calc R . .
C61 C 0.3566(8) 0.4473(6) 0.4286(5) 0.084(3) Uani 1 1 d U . .
H61A H 0.3279 0.3951 0.4119 0.127 Uiso 1 1 calc R . .
H61B H 0.2996 0.4800 0.4579 0.127 Uiso 1 1 calc R . .
H61C H 0.4155 0.4333 0.4605 0.127 Uiso 1 1 calc R . .
C62 C 0.3042(9) 0.5266(8) 0.3137(6) 0.115(3) Uani 1 1 d U . .
H62A H 0.3307 0.5538 0.2655 0.172 Uiso 1 1 calc R . .
H62B H 0.2561 0.5664 0.3432 0.172 Uiso 1 1 calc R . .
H62C H 0.2648 0.4767 0.3032 0.172 Uiso 1 1 calc R . .
C63 C 0.5476(4) 0.3711(3) 0.1091(3) 0.0226(12) Uani 1 1 d U . .
C64 C 0.5384(5) 0.2766(4) 0.0929(3) 0.0342(14) Uani 1 1 d U . .
H64A H 0.4809 0.2532 0.1274 0.051 Uiso 1 1 calc R . .
H64B H 0.6066 0.2461 0.1010 0.051 Uiso 1 1 calc R . .
H64C H 0.5221 0.2705 0.0401 0.051 Uiso 1 1 calc R . .
C65 C 0.4484(5) 0.4184(4) 0.0810(3) 0.0352(15) Uani 1 1 d U . .
H65A H 0.3833 0.3944 0.1062 0.053 Uiso 1 1 calc R . .
H65B H 0.4489 0.4129 0.0258 0.053 Uiso 1 1 calc R . .
H65C H 0.4496 0.4784 0.0932 0.053 Uiso 1 1 calc R . .
C66 C 0.6467(5) 0.4048(4) 0.0614(3) 0.0299(14) Uani 1 1 d U . .
H66A H 0.6389 0.3976 0.0073 0.045 Uiso 1 1 calc R . .
H66B H 0.7115 0.3734 0.0756 0.045 Uiso 1 1 calc R . .
H66C H 0.6526 0.4650 0.0712 0.045 Uiso 1 1 calc R . .
C67 C 0.5764(11) 0.9369(10) 0.0540(9) 0.144(6) Uani 1 1 d DU . .
C68 C 0.5281(13) 0.9819(9) 0.1298(8) 0.173(7) Uani 1 1 d U . .
H68A H 0.5214 0.9399 0.1716 0.259 Uiso 1 1 calc R . .
H68B H 0.4571 1.0078 0.1220 0.259 Uiso 1 1 calc R . .
H68C H 0.5759 1.0257 0.1424 0.259 Uiso 1 1 calc R . .
C69 C 0.2519(12) 0.0864(10) 0.1682(9) 0.152(6) Uani 1 1 d DU . .
C70 C 0.1761(11) 0.0992(7) 0.1095(7) 0.129(5) Uani 1 1 d U . .
H70A H 0.2139 0.1215 0.0627 0.194 Uiso 1 1 calc R . .
H70B H 0.1182 0.1395 0.1273 0.194 Uiso 1 1 calc R . .
H70C H 0.1457 0.0451 0.0994 0.194 Uiso 1 1 calc R . .
N1 N 0.6045(14) 0.9021(10) -0.0031(9) 0.208(7) Uani 1 1 d DU . .
N2 N 0.3161(15) 0.0679(13) 0.2111(10) 0.253(9) Uani 1 1 d DU . .

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 0.0109(5) 0.0196(5) 0.0282(5) 0.0000(4) 0.0014(4) 0.0049(4)
V2 0.0080(5) 0.0210(5) 0.0265(5) -0.0006(4) -0.0007(4) 0.0034(4)
O1 0.0115(19) 0.025(2) 0.036(2) 0.0017(17) -0.0024(16) 0.0028(16)
O2 0.0102(19) 0.030(2) 0.038(2) 0.0066(17) -0.0030(16) -0.0002(17)
O3 0.012(2) 0.025(2) 0.028(2) -0.0030(16) 0.0038(16) -0.0015(16)
O4 0.0108(19) 0.027(2) 0.0241(19) -0.0019(16) 0.0012(15) 0.0031(16)
O5 0.012(2) 0.028(2) 0.033(2) -0.0007(17) -0.0029(16) 0.0048(17)
O6 0.015(2) 0.021(2) 0.029(2) -0.0007(16) 0.0009(16) 0.0060(16)
O7 0.014(2) 0.025(2) 0.032(2) -0.0036(16) 0.0026(16) 0.0019(17)
O8 0.022(2) 0.026(2) 0.034(2) -0.0014(17) -0.0016(17) 0.0087(18)
C1 0.009(3) 0.037(4) 0.043(3) 0.011(3) -0.001(2) -0.001(3)
C2 0.021(3) 0.034(4) 0.039(3) 0.004(3) -0.008(3) 0.002(3)
C3 0.037(4) 0.050(5) 0.073(5) 0.002(4) -0.021(4) -0.012(4)
C4 0.009(3) 0.023(3) 0.028(3) -0.003(2) -0.003(2) 0.005(2)
C5 0.009(3) 0.023(3) 0.032(3) 0.000(2) -0.002(2) 0.007(2)
C6 0.009(3) 0.021(3) 0.038(3) -0.002(2) -0.005(2) 0.001(2)
C7 0.012(3) 0.031(3) 0.031(3) -0.004(2) -0.006(2) 0.000(2)
C8 0.016(3) 0.030(3) 0.025(3) -0.003(2) -0.003(2) 0.003(2)
C9 0.014(3) 0.023(3) 0.024(3) 0.002(2) -0.002(2) 0.004(2)
C10 0.011(3) 0.025(3) 0.025(3) -0.003(2) -0.002(2) 0.007(2)
C11 0.016(3) 0.024(3) 0.023(3) 0.005(2) 0.001(2) -0.003(2)
C12 0.014(3) 0.026(3) 0.017(3) 0.002(2) 0.004(2) 0.002(2)
C13 0.014(3) 0.018(3) 0.028(3) 0.000(2) 0.000(2) 0.001(2)
C14 0.011(3) 0.026(3) 0.030(3) 0.000(2) 0.005(2) 0.007(2)
C15 0.022(3) 0.024(3) 0.027(3) 0.004(2) 0.007(2) 0.002(2)
C16 0.022(3) 0.028(3) 0.023(3) -0.002(2) -0.002(2) 0.002(2)
C17A 0.047(4) 0.045(4) 0.034(3) -0.007(3) 0.010(3) 0.014(3)
C18A 0.019(5) 0.029(5) 0.031(5) -0.014(4) -0.001(4) 0.002(4)
C19A 0.059(13) 0.105(19) 0.037(9) -0.019(9) -0.007(9) 0.052(10)
C20A 0.053(6) 0.055(6) 0.054(6) 0.002(4) 0.016(4) 0.005(4)
C17B 0.047(4) 0.045(4) 0.034(3) -0.007(3) 0.010(3) 0.014(3)
C18B 0.056(4) 0.057(4) 0.057(4) -0.0018(10) -0.0048(11) -0.0014(10)
C19B 0.054(8) 0.033(7) 0.030(7) -0.005(5) 0.006(6) 0.027(5)
C20B 0.033(8) 0.072(8) 0.032(7) -0.015(5) 0.018(5) 0.006(6)
C21 0.014(3) 0.023(3) 0.028(3) 0.000(2) -0.001(2) 0.008(2)
C22 0.027(4) 0.030(3) 0.036(3) -0.005(3) -0.008(3) 0.000(3)
C23 0.019(3) 0.042(4) 0.034(3) -0.003(3) -0.002(3) 0.012(3)
C24 0.019(3) 0.047(4) 0.023(3) 0.003(3) 0.002(2) -0.001(3)
C25 0.018(3) 0.034(3) 0.034(3) -0.001(3) -0.006(2) 0.006(3)
C26 0.022(3) 0.031(3) 0.040(3) -0.008(3) -0.005(3) -0.001(3)
C27 0.037(4) 0.067(5) 0.079(5) -0.033(4) -0.017(4) -0.003(4)
C28 0.054(5) 0.034(4) 0.070(5) -0.011(3) -0.010(4) -0.007(4)
C29 0.080(6) 0.049(5) 0.076(5) -0.031(4) 0.028(5) -0.021(5)
C30 0.023(3) 0.022(3) 0.041(3) -0.008(3) 0.009(3) 0.000(3)
C31 0.035(4) 0.031(3) 0.046(4) -0.007(3) 0.017(3) -0.007(3)
C32 0.047(4) 0.049(4) 0.033(3) -0.005(3) 0.005(3) -0.013(4)
C33 0.024(4) 0.033(4) 0.070(5) -0.005(3) 0.018(3) 0.005(3)
C34 0.008(3) 0.035(4) 0.045(3) 0.008(3) -0.003(2) 0.001(3)
C35 0.018(3) 0.035(4) 0.053(4) 0.007(3) 0.009(3) 0.001(3)
C36 0.031(3) 0.062(4) 0.066(4) 0.012(3) 0.006(3) 0.012(3)
C37 0.010(2) 0.014(2) 0.025(2) 0.001(2) 0.0033(19) 0.004(2)
C38 0.013(3) 0.015(3) 0.030(3) 0.003(2) -0.002(2) 0.004(2)
C39 0.009(3) 0.023(3) 0.029(3) 0.000(2) 0.003(2) 0.003(2)
C40 0.013(3) 0.035(3) 0.031(3) -0.006(3) 0.007(2) 0.001(2)
C41 0.011(3) 0.028(3) 0.023(3) -0.003(2) 0.002(2) 0.005(2)
C42 0.009(3) 0.023(3) 0.026(3) 0.002(2) 0.000(2) 0.002(2)
C43 0.013(3) 0.020(3) 0.022(3) 0.001(2) 0.001(2) 0.003(2)
C44 0.010(3) 0.028(3) 0.024(3) 0.000(2) 0.000(2) 0.002(2)
C45 0.012(3) 0.021(3) 0.029(3) -0.001(2) -0.002(2) 0.003(2)
C46 0.017(3) 0.023(3) 0.028(3) 0.006(2) 0.001(2) 0.001(2)
C47 0.017(3) 0.023(3) 0.033(3) 0.003(2) -0.001(2) 0.000(2)
C48 0.020(3) 0.027(3) 0.032(3) 0.000(2) -0.004(2) 0.000(2)
C49 0.012(3) 0.026(3) 0.029(3) -0.006(2) -0.001(2) 0.006(2)
C50A 0.030(3) 0.032(3) 0.041(3) -0.011(3) -0.002(3) -0.004(3)
C51A 0.023(6) 0.045(13) 0.086(14) -0.021(10) -0.018(6) 0.011(6)
C52A 0.026(9) 0.057(13) 0.077(10) -0.030(7) -0.025(8) 0.012(8)
C53A 0.101(17) 0.056(10) 0.073(10) -0.022(7) 0.024(11) -0.046(12)
C50B 0.030(3) 0.032(3) 0.041(3) -0.011(3) -0.002(3) -0.004(3)
C51B 0.058(12) 0.025(13) 0.074(16) -0.028(10) 0.019(12) -0.010(10)
C52B 0.054(11) 0.027(10) 0.090(17) -0.008(10) -0.034(11) -0.005(10)
C53B 0.042(13) 0.028(7) 0.056(9) -0.011(6) -0.009(8) -0.010(9)
C54 0.025(3) 0.028(3) 0.035(3) 0.002(3) 0.007(2) -0.003(3)
C55 0.035(4) 0.034(4) 0.053(4) 0.002(3) 0.018(3) 0.002(3)
C56 0.048(4) 0.050(4) 0.030(3) -0.001(3) 0.004(3) -0.016(4)
C57 0.034(4) 0.037(4) 0.044(4) 0.004(3) 0.013(3) -0.007(3)
C58 0.017(3) 0.032(3) 0.030(3) 0.000(3) 0.002(2) 0.003(3)
C59 0.025(4) 0.057(4) 0.036(3) -0.014(3) 0.002(3) 0.023(3)
C60 0.070(6) 0.053(5) 0.131(8) -0.039(5) 0.052(5) 0.007(5)
C61 0.069(7) 0.076(6) 0.097(6) -0.005(5) 0.053(5) 0.004(5)
C62 0.096(5) 0.135(5) 0.112(5) -0.017(4) -0.020(4) 0.042(4)
C63 0.0216(15) 0.0231(15) 0.0228(14) -0.0005(9) -0.0021(9) 0.0009(9)
C64 0.033(4) 0.041(3) 0.029(3) -0.006(3) -0.003(3) 0.003(3)
C65 0.025(3) 0.053(4) 0.027(3) 0.002(3) -0.005(3) 0.013(3)
C66 0.024(3) 0.035(3) 0.028(3) 0.006(3) 0.005(2) 0.008(3)
C67 0.116(12) 0.154(14) 0.178(14) 0.004(10) -0.091(11) -0.037(10)
C68 0.188(16) 0.173(13) 0.179(12) -0.043(10) -0.144(12) 0.033(11)
C69 0.118(13) 0.205(16) 0.135(13) -0.068(12) 0.009(8) -0.034(12)
C70 0.171(14) 0.105(9) 0.114(10) -0.054(7) -0.006(8) -0.008(9)
N1 0.275(19) 0.179(14) 0.189(14) -0.038(10) -0.104(12) -0.057(13)
N2 0.238(16) 0.354(18) 0.185(13) 0.008(12) -0.077(10) -0.116(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 O8 1.568(4) . ?
V1 O6 1.797(4) . ?
V1 O7 1.802(4) . ?
V1 O2 1.967(4) . ?
V1 O1 1.976(4) . ?
V2 O5 1.567(4) . ?
V2 O3 1.810(3) . ?
V2 O4 1.814(4) . ?
V2 O2 1.974(4) . ?
V2 O1 1.977(4) . ?
O1 C34 1.471(6) . ?
O2 C1 1.460(6) . ?
O3 C4 1.353(6) . ?
O4 C12 1.354(6) . ?
O6 C37 1.363(6) . ?
O7 C45 1.362(6) . ?
C1 C2 1.513(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.518(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.392(7) . ?
C4 C5 1.406(7) . ?
C5 C6 1.392(7) . ?
C5 C30 1.546(8) . ?
C6 C7 1.383(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(7) . ?
C7 C26 1.541(8) . ?
C8 C9 1.375(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.549(7) . ?
C10 C11 1.526(7) . ?
C10 C25 1.533(7) . ?
C10 H10 1.0000 . ?
C11 C16 1.387(8) . ?
C11 C12 1.395(7) . ?
C12 C13 1.426(7) . ?
C13 C14 1.381(7) . ?
C13 C21 1.535(7) . ?
C14 C15 1.372(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(8) . ?
C15 C17A 1.513(8) . ?
C16 H16 0.9500 . ?
C17A C19A 1.474(14) . ?
C17A C20A 1.580(14) . ?
C17A C18A 1.591(12) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21 C23 1.531(7) . ?
C21 C22 1.537(7) . ?
C21 C24 1.541(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C29 1.489(9) . ?
C26 C28 1.526(9) . ?
C26 C27 1.554(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C33 1.533(8) . ?
C30 C32 1.539(8) . ?
C30 C31 1.539(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.511(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.521(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C42 1.395(7) . ?
C37 C38 1.422(7) . ?
C38 C39 1.379(7) . ?
C38 C63 1.527(7) . ?
C39 C40 1.358(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.400(8) . ?
C40 C59 1.528(8) . ?
C41 C42 1.394(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.524(7) . ?
C43 C58 1.527(7) . ?
C43 C44 1.531(7) . ?
C43 H43 1.0000 . ?
C44 C49 1.384(7) . ?
C44 C45 1.402(7) . ?
C45 C46 1.428(7) . ?
C46 C47 1.396(8) . ?
C46 C54 1.530(8) . ?
C47 C48 1.390(8) . ?
C47 H47 0.9500 . ?
C48 C49 1.389(7) . ?
C48 C50A 1.548(8) . ?
C49 H49 0.9500 . ?
C50A C51A 1.517(13) . ?
C50A C53A 1.524(12) . ?
C50A C52A 1.541(13) . ?
C51A H51A 0.9800 . ?
C51A H51B 0.9800 . ?
C51A H51C 0.9800 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C51B H51D 0.9800 . ?
C51B H51E 0.9800 . ?
C51B H51F 0.9800 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C53B H53D 0.9800 . ?
C53B H53E 0.9800 . ?
C53B H53F 0.9800 . ?
C54 C56 1.534(8) . ?
C54 C57 1.540(8) . ?
C54 C55 1.541(8) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.496(10) . ?
C59 C62 1.522(11) . ?
C59 C61 1.531(10) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C65 1.533(8) . ?
C63 C66 1.542(7) . ?
C63 C64 1.544(8) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 N1 1.181(9) . ?
C67 C68 1.59(2) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 N2 1.174(9) . ?
C69 C70 1.468(17) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 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
O8 V1 O6 102.91(18) . . ?
O8 V1 O7 104.24(18) . . ?
O6 V1 O7 93.47(17) . . ?
O8 V1 O2 103.12(18) . . ?
O6 V1 O2 152.04(16) . . ?
O7 V1 O2 89.89(16) . . ?
O8 V1 O1 107.55(18) . . ?
O6 V1 O1 91.16(16) . . ?
O7 V1 O1 145.93(16) . . ?
O2 V1 O1 71.35(15) . . ?
O5 V2 O3 103.23(18) . . ?
O5 V2 O4 104.03(17) . . ?
O3 V2 O4 94.91(16) . . ?
O5 V2 O2 105.08(18) . . ?
O3 V2 O2 149.18(16) . . ?
O4 V2 O2 89.89(16) . . ?
O5 V2 O1 106.15(18) . . ?
O3 V2 O1 89.43(16) . . ?
O4 V2 O1 147.61(16) . . ?
O2 V2 O1 71.21(15) . . ?
C34 O1 V1 128.1(3) . . ?
C34 O1 V2 123.5(3) . . ?
V1 O1 V2 108.29(17) . . ?
C1 O2 V1 124.4(3) . . ?
C1 O2 V2 126.5(3) . . ?
V1 O2 V2 108.79(17) . . ?
C4 O3 V2 137.9(3) . . ?
C12 O4 V2 139.5(3) . . ?
C37 O6 V1 140.8(3) . . ?
C45 O7 V1 137.7(3) . . ?
O2 C1 C2 111.8(5) . . ?
O2 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O2 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 111.0(5) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
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 . . ?
O3 C4 C9 121.0(5) . . ?
O3 C4 C5 118.6(5) . . ?
C9 C4 C5 120.4(5) . . ?
C6 C5 C4 116.9(5) . . ?
C6 C5 C30 122.0(5) . . ?
C4 C5 C30 121.1(5) . . ?
C7 C6 C5 124.3(5) . . ?
C7 C6 H6 117.9 . . ?
C5 C6 H6 117.9 . . ?
C6 C7 C8 116.3(5) . . ?
C6 C7 C26 120.4(5) . . ?
C8 C7 C26 123.3(5) . . ?
C9 C8 C7 122.5(5) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C8 C9 C4 119.6(5) . . ?
C8 C9 C10 119.2(5) . . ?
C4 C9 C10 121.0(5) . . ?
C11 C10 C25 114.2(4) . . ?
C11 C10 C9 108.1(4) . . ?
C25 C10 C9 112.8(4) . . ?
C11 C10 H10 107.1 . . ?
C25 C10 H10 107.1 . . ?
C9 C10 H10 107.1 . . ?
C16 C11 C12 118.5(5) . . ?
C16 C11 C10 120.2(5) . . ?
C12 C11 C10 120.9(5) . . ?
O4 C12 C11 120.5(5) . . ?
O4 C12 C13 118.1(4) . . ?
C11 C12 C13 121.4(5) . . ?
C14 C13 C12 115.9(5) . . ?
C14 C13 C21 121.8(5) . . ?
C12 C13 C21 122.3(5) . . ?
C15 C14 C13 125.0(5) . . ?
C15 C14 H14 117.5 . . ?
C13 C14 H14 117.5 . . ?
C14 C15 C16 117.0(5) . . ?
C14 C15 C17A 123.4(5) . . ?
C16 C15 C17A 119.6(5) . . ?
C11 C16 C15 122.1(5) . . ?
C11 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C19A C17A C15 118.5(10) . . ?
C19A C17A C20A 107.5(12) . . ?
C15 C17A C20A 104.6(8) . . ?
C19A C17A C18A 110.9(11) . . ?
C15 C17A C18A 110.3(6) . . ?
C20A C17A C18A 103.9(9) . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C23 C21 C13 111.4(4) . . ?
C23 C21 C22 107.3(5) . . ?
C13 C21 C22 110.7(4) . . ?
C23 C21 C24 106.4(5) . . ?
C13 C21 C24 111.9(4) . . ?
C22 C21 C24 108.9(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C10 C25 H25A 109.5 . . ?
C10 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C10 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 C26 C28 109.0(6) . . ?
C29 C26 C7 113.0(5) . . ?
C28 C26 C7 111.5(5) . . ?
C29 C26 C27 109.5(6) . . ?
C28 C26 C27 105.7(5) . . ?
C7 C26 C27 107.8(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 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C33 C30 C32 110.9(5) . . ?
C33 C30 C31 107.9(5) . . ?
C32 C30 C31 106.0(5) . . ?
C33 C30 C5 109.6(5) . . ?
C32 C30 C5 110.7(5) . . ?
C31 C30 C5 111.7(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O1 C34 C35 111.4(5) . . ?
O1 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
O1 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 C36 109.0(5) . . ?
C34 C35 H35A 109.9 . . ?
C36 C35 H35A 109.9 . . ?
C34 C35 H35B 109.9 . . ?
C36 C35 H35B 109.9 . . ?
H35A C35 H35B 108.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O6 C37 C42 120.3(4) . . ?
O6 C37 C38 118.0(4) . . ?
C42 C37 C38 121.7(5) . . ?
C39 C38 C37 116.1(5) . . ?
C39 C38 C63 122.2(5) . . ?
C37 C38 C63 121.7(5) . . ?
C40 C39 C38 124.2(5) . . ?
C40 C39 H39 117.9 . . ?
C38 C39 H39 117.9 . . ?
C39 C40 C41 118.5(5) . . ?
C39 C40 C59 122.7(5) . . ?
C41 C40 C59 118.7(5) . . ?
C42 C41 C40 120.9(5) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C37 118.3(5) . . ?
C41 C42 C43 120.8(5) . . ?
C37 C42 C43 120.8(5) . . ?
C42 C43 C58 115.2(4) . . ?
C42 C43 C44 110.2(4) . . ?
C58 C43 C44 112.5(4) . . ?
C42 C43 H43 106.1 . . ?
C58 C43 H43 106.1 . . ?
C44 C43 H43 106.1 . . ?
C49 C44 C45 118.2(5) . . ?
C49 C44 C43 119.1(5) . . ?
C45 C44 C43 122.4(5) . . ?
O7 C45 C44 120.7(5) . . ?
O7 C45 C46 117.5(5) . . ?
C44 C45 C46 121.7(5) . . ?
C47 C46 C45 116.2(5) . . ?
C47 C46 C54 122.6(5) . . ?
C45 C46 C54 121.1(5) . . ?
C48 C47 C46 123.5(5) . . ?
C48 C47 H47 118.3 . . ?
C46 C47 H47 118.3 . . ?
C49 C48 C47 117.7(5) . . ?
C49 C48 C50A 121.0(5) . . ?
C47 C48 C50A 121.3(5) . . ?
C44 C49 C48 122.6(5) . . ?
C44 C49 H49 118.7 . . ?
C48 C49 H49 118.7 . . ?
C51A C50A C53A 110.2(12) . . ?
C51A C50A C52A 108.0(10) . . ?
C53A C50A C52A 107.8(10) . . ?
C51A C50A C48 112.3(12) . . ?
C53A C50A C48 111.9(8) . . ?
C52A C50A C48 106.4(9) . . ?
H51D C51B H51E 109.5 . . ?
H51D C51B H51F 109.5 . . ?
H51E C51B H51F 109.5 . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
H53D C53B H53E 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
C46 C54 C56 108.9(5) . . ?
C46 C54 C57 111.1(5) . . ?
C56 C54 C57 107.7(5) . . ?
C46 C54 C55 110.8(5) . . ?
C56 C54 C55 111.2(5) . . ?
C57 C54 C55 107.1(5) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C43 C58 H58A 109.5 . . ?
C43 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C43 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 C62 106.2(7) . . ?
C60 C59 C40 111.5(6) . . ?
C62 C59 C40 112.6(6) . . ?
C60 C59 C61 107.5(6) . . ?
C62 C59 C61 108.4(7) . . ?
C40 C59 C61 110.5(6) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C38 C63 C65 111.4(5) . . ?
C38 C63 C66 109.9(4) . . ?
C65 C63 C66 107.1(4) . . ?
C38 C63 C64 111.7(4) . . ?
C65 C63 C64 107.4(5) . . ?
C66 C63 C64 109.1(5) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N1 C67 C68 174.9(14) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N2 C69 C70 172.4(19) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.099

#===END

data_8
_database_code_depnum_ccdc_archive 'CCDC 718349'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '[{VO(tBu-(C6H2-tBu,O-CH2-)3-tBu)}2].3(MeCN)'
_chemical_formula_moiety         'C80 H110 O8 V2, 3(C2 H3 N)'
_chemical_formula_sum            'C86 H119 N3 O8 V2'
_chemical_formula_weight         1424.72

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/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                   15.5098(8)
_cell_length_b                   19.2536(11)
_cell_length_c                   28.7880(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.323(4)
_cell_angle_gamma                90.00
_cell_volume                     8582.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(1)
_cell_measurement_reflns_used    52327
_cell_measurement_theta_min      3.69
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            'very dark'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.48
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3064
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_process_details   '(SADABS V2.10; Sheldrick, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(1)
_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_reflns_number            52327
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.69
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9782
_reflns_number_gt                7118
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material  
;
SHELXL-97 (Sheldrick, 2008), 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^ > 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.

The disordered t-Bu groups in 8 show a high degree of disorder, and the
minor components were modelled isotropically.
;

_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^)+(0.0802P)^2^+10.1069P] 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         9782
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1634
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.017
_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
O1A O 0.54511(10) 0.39541(9) 0.12746(6) 0.0307(4) Uani 1 1 d . . .
C1A C 0.37218(14) 0.37034(12) 0.37432(8) 0.0270(5) Uani 1 1 d . . .
C2A C 0.33128(15) 0.36933(13) 0.41673(8) 0.0321(5) Uani 1 1 d . . .
C3A C 0.24496(17) 0.34797(14) 0.41431(9) 0.0376(6) Uani 1 1 d . . .
H3A H 0.2164 0.3463 0.4418 0.045 Uiso 1 1 calc R . .
C4A C 0.19886(16) 0.32892(13) 0.37307(10) 0.0361(6) Uani 1 1 d . A .
C5A C 0.24230(15) 0.33095(12) 0.33217(9) 0.0307(5) Uani 1 1 d . . .
H5A H 0.2133 0.3181 0.3043 0.037 Uiso 1 1 calc R . .
C6A C 0.32847(14) 0.35182(11) 0.33206(8) 0.0266(5) Uani 1 1 d . . .
C41A C 0.10204(18) 0.31135(18) 0.37263(11) 0.0500(8) Uani 1 1 d . . .
C42A C 0.0537(3) 0.3807(3) 0.3826(2) 0.0724(14) Uani 0.80 1 d P A 1
H42A H 0.0649 0.4142 0.3590 0.109 Uiso 0.80 1 calc PR A 1
H42B H 0.0737 0.3985 0.4125 0.109 Uiso 0.80 1 calc PR A 1
H42C H -0.0073 0.3721 0.3825 0.109 Uiso 0.80 1 calc PR A 1
C43A C 0.0837(3) 0.2586(3) 0.4089(2) 0.0744(15) Uani 0.80 1 d P A 1
H43A H 0.0229 0.2492 0.4080 0.112 Uiso 0.80 1 calc PR A 1
H43B H 0.1022 0.2761 0.4391 0.112 Uiso 0.80 1 calc PR A 1
H43C H 0.1144 0.2165 0.4030 0.112 Uiso 0.80 1 calc PR A 1
C44A C 0.0658(3) 0.2865(4) 0.32461(17) 0.0871(19) Uani 0.80 1 d P A 1
H44A H 0.0791 0.3200 0.3014 0.131 Uiso 0.80 1 calc PR A 1
H44B H 0.0043 0.2812 0.3250 0.131 Uiso 0.80 1 calc PR A 1
H44C H 0.0913 0.2426 0.3174 0.131 Uiso 0.80 1 calc PR A 1
C42Y C 0.097(2) 0.2331(19) 0.3546(14) 0.149(13) Uiso 0.20 1 d P A 2
H42Z H 0.1380 0.2053 0.3727 0.223 Uiso 0.20 1 calc PR A 2
H42Y H 0.1107 0.2316 0.3225 0.223 Uiso 0.20 1 calc PR A 2
H42X H 0.0400 0.2153 0.3577 0.223 Uiso 0.20 1 calc PR A 2
C43Y C 0.050(3) 0.359(2) 0.3532(14) 0.140(14) Uiso 0.20 1 d P A 2
H43Z H 0.0092 0.3737 0.3749 0.210 Uiso 0.20 1 calc PR A 2
H43Y H 0.0203 0.3405 0.3259 0.210 Uiso 0.20 1 calc PR A 2
H43X H 0.0840 0.3987 0.3446 0.210 Uiso 0.20 1 calc PR A 2
C44Y C 0.077(2) 0.2938(16) 0.4253(10) 0.098(9) Uiso 0.20 1 d P A 2
H44Z H 0.1170 0.2600 0.4386 0.147 Uiso 0.20 1 calc PR A 2
H44Y H 0.0196 0.2755 0.4248 0.147 Uiso 0.20 1 calc PR A 2
H44X H 0.0806 0.3354 0.4437 0.147 Uiso 0.20 1 calc PR A 2
C21A C 0.37744(18) 0.39432(16) 0.46266(9) 0.0420(6) Uani 1 1 d . . .
C22A C 0.4570(2) 0.35026(19) 0.47600(10) 0.0539(8) Uani 1 1 d . . .
H22A H 0.4839 0.3671 0.5047 0.081 Uiso 1 1 calc R . .
H22B H 0.4971 0.3532 0.4519 0.081 Uiso 1 1 calc R . .
H22C H 0.4399 0.3028 0.4798 0.081 Uiso 1 1 calc R . .
C23A C 0.4036(2) 0.47132(17) 0.45691(11) 0.0606(9) Uani 1 1 d . . .
H23A H 0.4323 0.4876 0.4853 0.091 Uiso 1 1 calc R . .
H23B H 0.3529 0.4988 0.4499 0.091 Uiso 1 1 calc R . .
H23C H 0.4419 0.4753 0.4320 0.091 Uiso 1 1 calc R . .
C24A C 0.3174(2) 0.3908(2) 0.50354(11) 0.0646(10) Uani 1 1 d . . .
H24A H 0.3480 0.4066 0.5315 0.097 Uiso 1 1 calc R . .
H24B H 0.2988 0.3437 0.5076 0.097 Uiso 1 1 calc R . .
H24C H 0.2679 0.4199 0.4969 0.097 Uiso 1 1 calc R . .
C7A C 0.36972(14) 0.36077(12) 0.28600(8) 0.0271(5) Uani 1 1 d . . .
H7A1 H 0.3396 0.3317 0.2628 0.032 Uiso 1 1 calc R . .
H7A2 H 0.4292 0.3451 0.2893 0.032 Uiso 1 1 calc R . .
O1B O 0.41254(11) 0.39308(9) 0.19714(6) 0.0310(4) Uani 1 1 d . . .
C1B C 0.39000(13) 0.44907(11) 0.22314(8) 0.0259(5) Uani 1 1 d . . .
C2B C 0.36804(14) 0.43568(12) 0.26886(8) 0.0265(5) Uani 1 1 d . . .
C3B C 0.34190(16) 0.49124(13) 0.29570(9) 0.0337(5) Uani 1 1 d . . .
H3B H 0.3271 0.4829 0.3260 0.040 Uiso 1 1 calc R . .
C4B C 0.33724(18) 0.55891(13) 0.27861(9) 0.0369(6) Uani 1 1 d . B .
C5B C 0.36039(17) 0.57012(13) 0.23309(9) 0.0348(5) Uani 1 1 d . . .
H5B H 0.3588 0.6151 0.2214 0.042 Uiso 1 1 calc R . .
C6B C 0.38593(14) 0.51604(12) 0.20440(8) 0.0278(5) Uani 1 1 d . . .
C7B C 0.39970(15) 0.52950(12) 0.15328(8) 0.0288(5) Uani 1 1 d . . .
H7B1 H 0.4182 0.5772 0.1494 0.035 Uiso 1 1 calc R . .
H7B2 H 0.4450 0.4993 0.1432 0.035 Uiso 1 1 calc R . .
C41B C 0.3073(2) 0.61966(14) 0.30897(11) 0.0523(8) Uani 1 1 d . . .
C42B C 0.2767(8) 0.5972(5) 0.3548(4) 0.103(3) Uiso 0.537(7) 1 d P B 1
H42D H 0.2282 0.5665 0.3499 0.155 Uiso 0.537(7) 1 calc PR B 1
H42E H 0.2597 0.6372 0.3720 0.155 Uiso 0.537(7) 1 calc PR B 1
H42F H 0.3225 0.5734 0.3721 0.155 Uiso 0.537(7) 1 calc PR B 1
C43B C 0.3845(5) 0.6689(4) 0.3175(3) 0.076(2) Uiso 0.537(7) 1 d P B 1
H43D H 0.4072 0.6813 0.2883 0.115 Uiso 0.537(7) 1 calc PR B 1
H43E H 0.4286 0.6462 0.3367 0.115 Uiso 0.537(7) 1 calc PR B 1
H43F H 0.3661 0.7101 0.3329 0.115 Uiso 0.537(7) 1 calc PR B 1
C44B C 0.2381(4) 0.6628(3) 0.2808(2) 0.0515(16) Uiso 0.537(7) 1 d P B 1
H44D H 0.2610 0.6781 0.2523 0.077 Uiso 0.537(7) 1 calc PR B 1
H443 H 0.2225 0.7024 0.2987 0.077 Uiso 0.537(7) 1 calc PR B 1
H44F H 0.1879 0.6346 0.2739 0.077 Uiso 0.537(7) 1 calc PR B 1
C42Z C 0.3720(6) 0.6321(5) 0.3486(3) 0.077(3) Uiso 0.463(7) 1 d P B 2
H42W H 0.3854 0.5889 0.3641 0.116 Uiso 0.463(7) 1 calc PR B 2
H42V H 0.3485 0.6639 0.3702 0.116 Uiso 0.463(7) 1 calc PR B 2
H42U H 0.4236 0.6514 0.3371 0.116 Uiso 0.463(7) 1 calc PR B 2
C43Z C 0.2926(10) 0.6860(7) 0.2829(4) 0.115(4) Uiso 0.463(7) 1 d P B 2
H43W H 0.2749 0.7214 0.3039 0.173 Uiso 0.463(7) 1 calc PR B 2
H43V H 0.2483 0.6794 0.2586 0.173 Uiso 0.463(7) 1 calc PR B 2
H43U H 0.3452 0.7000 0.2696 0.173 Uiso 0.463(7) 1 calc PR B 2
C44Z C 0.2245(6) 0.5954(4) 0.3352(3) 0.065(2) Uiso 0.463(7) 1 d P B 2
H44W H 0.2387 0.5550 0.3536 0.098 Uiso 0.463(7) 1 calc PR B 2
H44V H 0.1784 0.5846 0.3127 0.098 Uiso 0.463(7) 1 calc PR B 2
H44U H 0.2068 0.6321 0.3551 0.098 Uiso 0.463(7) 1 calc PR B 2
O1C O 0.36365(11) 0.40392(9) 0.09964(6) 0.0339(4) Uani 1 1 d . . .
C1C C 0.30181(15) 0.45512(12) 0.09791(8) 0.0282(5) Uani 1 1 d . . .
C2C C 0.31743(14) 0.51674(12) 0.12310(8) 0.0266(5) Uani 1 1 d . . .
C3C C 0.25259(15) 0.56730(12) 0.12181(8) 0.0297(5) Uani 1 1 d . . .
H3C H 0.2623 0.6084 0.1383 0.036 Uiso 1 1 calc R . .
C4C C 0.17450(15) 0.55818(13) 0.09688(9) 0.0324(5) Uani 1 1 d . . .
C5C C 0.16263(16) 0.49660(13) 0.07140(9) 0.0340(5) Uani 1 1 d . . .
H5C H 0.1108 0.4905 0.0540 0.041 Uiso 1 1 calc R . .
C6C C 0.22445(16) 0.44393(12) 0.07082(8) 0.0309(5) Uani 1 1 d . . .
C7C C 0.20836(18) 0.37661(14) 0.04250(10) 0.0420(6) Uani 1 1 d . . .
C41C C 0.10240(17) 0.61356(14) 0.09582(10) 0.0414(6) Uani 1 1 d . . .
C42C C 0.0915(2) 0.64375(19) 0.04658(13) 0.0653(10) Uani 1 1 d . . .
H42G H 0.0471 0.6785 0.0455 0.098 Uiso 1 1 calc R . .
H42H H 0.0758 0.6073 0.0249 0.098 Uiso 1 1 calc R . .
H42I H 0.1450 0.6644 0.0384 0.098 Uiso 1 1 calc R . .
C43C C 0.01616(19) 0.58036(18) 0.10783(13) 0.0582(9) Uani 1 1 d . . .
H43G H -0.0281 0.6153 0.1070 0.087 Uiso 1 1 calc R . .
H43H H 0.0221 0.5604 0.1384 0.087 Uiso 1 1 calc R . .
H43I H 0.0007 0.5447 0.0855 0.087 Uiso 1 1 calc R . .
C44C C 0.1231(2) 0.67237(18) 0.13040(16) 0.0740(12) Uani 1 1 d . . .
H44G H 0.0771 0.7058 0.1285 0.111 Uiso 1 1 calc R . .
H44H H 0.1761 0.6944 0.1230 0.111 Uiso 1 1 calc R . .
H44I H 0.1291 0.6538 0.1614 0.111 Uiso 1 1 calc R . .
C71C C 0.2062(2) 0.31347(15) 0.07572(12) 0.0555(8) Uani 1 1 d . . .
H71A H 0.1962 0.2718 0.0579 0.083 Uiso 1 1 calc R . .
H71B H 0.1607 0.3195 0.0965 0.083 Uiso 1 1 calc R . .
H71C H 0.2605 0.3099 0.0933 0.083 Uiso 1 1 calc R . .
C72C C 0.2785(2) 0.36709(19) 0.00736(12) 0.0612(9) Uani 1 1 d . . .
H72A H 0.2675 0.3252 -0.0101 0.092 Uiso 1 1 calc R . .
H72B H 0.3341 0.3641 0.0237 0.092 Uiso 1 1 calc R . .
H72C H 0.2777 0.4060 -0.0135 0.092 Uiso 1 1 calc R . .
C73C C 0.1209(2) 0.37856(19) 0.01448(13) 0.0626(9) Uani 1 1 d . . .
H73A H 0.1131 0.3362 -0.0028 0.094 Uiso 1 1 calc R . .
H73B H 0.1199 0.4172 -0.0066 0.094 Uiso 1 1 calc R . .
H73C H 0.0753 0.3835 0.0354 0.094 Uiso 1 1 calc R . .
V1 V 0.44004(2) 0.36704(2) 0.140886(14) 0.02803(12) Uani 1 1 d . . .
O1 O 0.43503(12) 0.28434(9) 0.13857(6) 0.0392(4) Uani 1 1 d . . .
N81 N 0.3017(5) 0.8437(3) 0.3033(2) 0.167(3) Uani 1 1 d . . .
C82 C 0.3275(3) 0.8969(2) 0.29514(15) 0.0804(13) Uani 1 1 d . . .
C83 C 0.3534(3) 0.9645(2) 0.28804(18) 0.0881(13) Uani 1 1 d . . .
H83A H 0.3072 0.9898 0.2722 0.132 Uiso 1 1 calc R . .
H83B H 0.4029 0.9646 0.2695 0.132 Uiso 1 1 calc R . .
H83C H 0.3682 0.9861 0.3175 0.132 Uiso 1 1 calc R . .
N91 N 0.5000 0.0729(3) 0.2500 0.110(2) Uani 1 2 d S . .
C92 C 0.5000 0.1320(3) 0.2500 0.0647(13) Uani 1 2 d S . .
C93 C 0.5000 0.2063(3) 0.2500 0.0814(17) Uani 1 2 d S . .
H93A H 0.5119 0.2229 0.2196 0.122 Uiso 0.50 1 calc PR . .
H93B H 0.5436 0.2229 0.2723 0.122 Uiso 0.50 1 calc PR . .
H93C H 0.4445 0.2229 0.2581 0.122 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
O1A 0.0259(8) 0.0370(9) 0.0298(9) 0.0044(7) 0.0070(7) 0.0078(7)
C1A 0.0235(10) 0.0271(11) 0.0308(12) -0.0025(9) 0.0052(9) -0.0043(9)
C2A 0.0305(12) 0.0357(13) 0.0308(12) -0.0060(10) 0.0066(10) -0.0046(10)
C3A 0.0342(13) 0.0446(15) 0.0355(14) -0.0053(11) 0.0146(11) -0.0070(11)
C4A 0.0267(12) 0.0358(13) 0.0465(15) -0.0068(11) 0.0081(11) -0.0070(10)
C5A 0.0305(12) 0.0282(12) 0.0331(12) -0.0047(10) -0.0004(10) -0.0037(9)
C6A 0.0281(11) 0.0231(11) 0.0291(12) -0.0018(9) 0.0051(9) -0.0010(9)
C41A 0.0299(14) 0.066(2) 0.0555(18) -0.0096(15) 0.0106(13) -0.0152(13)
C42A 0.0268(19) 0.092(4) 0.100(4) -0.001(3) 0.016(2) 0.005(2)
C43A 0.047(2) 0.086(4) 0.091(4) 0.015(3) 0.012(2) -0.037(3)
C44A 0.035(2) 0.161(6) 0.066(3) -0.032(3) 0.006(2) -0.046(3)
C21A 0.0385(14) 0.0579(17) 0.0304(13) -0.0120(12) 0.0086(11) -0.0100(13)
C22A 0.0493(17) 0.080(2) 0.0326(15) 0.0007(14) 0.0039(13) -0.0036(16)
C23A 0.070(2) 0.060(2) 0.0515(19) -0.0256(16) 0.0020(16) -0.0178(17)
C24A 0.0543(19) 0.105(3) 0.0360(16) -0.0202(17) 0.0166(14) -0.0149(19)
C7A 0.0274(11) 0.0263(11) 0.0276(11) -0.0030(9) 0.0028(9) 0.0011(9)
O1B 0.0331(9) 0.0308(8) 0.0299(9) 0.0012(7) 0.0083(7) 0.0076(7)
C1B 0.0203(10) 0.0258(11) 0.0314(12) -0.0030(9) 0.0008(9) 0.0016(8)
C2B 0.0228(10) 0.0267(11) 0.0299(12) -0.0017(9) 0.0004(9) 0.0001(9)
C3B 0.0391(14) 0.0313(13) 0.0308(13) -0.0041(10) 0.0026(10) 0.0021(10)
C4B 0.0441(14) 0.0298(13) 0.0367(14) -0.0069(11) -0.0005(11) 0.0028(11)
C5B 0.0400(13) 0.0243(12) 0.0394(14) 0.0002(10) -0.0042(11) 0.0001(10)
C6B 0.0230(10) 0.0293(12) 0.0307(12) 0.0003(9) -0.0008(9) -0.0015(9)
C7B 0.0258(11) 0.0277(12) 0.0333(12) 0.0042(10) 0.0034(9) -0.0011(9)
C41B 0.081(2) 0.0291(14) 0.0466(17) -0.0102(12) 0.0049(16) 0.0107(14)
O1C 0.0314(9) 0.0331(9) 0.0371(9) -0.0026(7) 0.0021(7) 0.0114(7)
C1C 0.0281(11) 0.0288(12) 0.0283(12) 0.0047(9) 0.0052(9) 0.0067(9)
C2C 0.0259(11) 0.0271(11) 0.0271(11) 0.0055(9) 0.0047(9) 0.0022(9)
C3C 0.0319(12) 0.0262(12) 0.0312(12) 0.0006(10) 0.0039(10) 0.0030(9)
C4C 0.0291(12) 0.0331(13) 0.0351(13) 0.0039(10) 0.0041(10) 0.0085(10)
C5C 0.0264(12) 0.0392(14) 0.0360(13) 0.0014(11) -0.0028(10) 0.0044(10)
C6C 0.0315(12) 0.0314(12) 0.0300(12) -0.0008(10) 0.0027(10) 0.0020(10)
C7C 0.0410(14) 0.0414(15) 0.0432(15) -0.0133(12) -0.0020(12) 0.0054(12)
C41C 0.0313(13) 0.0369(14) 0.0558(17) 0.0007(12) 0.0009(12) 0.0122(11)
C42C 0.0470(18) 0.070(2) 0.079(2) 0.0277(19) 0.0041(17) 0.0261(16)
C43C 0.0344(15) 0.060(2) 0.081(2) 0.0061(17) 0.0119(15) 0.0161(14)
C44C 0.0510(19) 0.053(2) 0.117(3) -0.029(2) -0.007(2) 0.0265(16)
C71C 0.0592(19) 0.0366(16) 0.070(2) -0.0073(15) -0.0024(16) -0.0036(14)
C72C 0.061(2) 0.070(2) 0.0538(19) -0.0301(17) 0.0109(16) 0.0034(17)
C73C 0.058(2) 0.065(2) 0.063(2) -0.0243(17) -0.0168(17) 0.0001(16)
V1 0.0256(2) 0.0288(2) 0.0303(2) -0.00046(17) 0.00683(15) 0.00780(16)
O1 0.0414(10) 0.0319(9) 0.0447(10) -0.0022(8) 0.0070(8) 0.0096(8)
N81 0.202(6) 0.097(4) 0.190(6) 0.045(4) -0.091(5) -0.032(4)
C82 0.095(3) 0.066(3) 0.076(3) -0.001(2) -0.037(2) -0.001(2)
C83 0.062(2) 0.073(3) 0.129(4) -0.018(3) 0.001(2) -0.009(2)
N91 0.103(4) 0.059(3) 0.171(6) 0.000 0.041(4) 0.000
C92 0.067(3) 0.050(3) 0.080(4) 0.000 0.027(3) 0.000
C93 0.111(5) 0.044(3) 0.090(4) 0.000 0.017(4) 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
O1A C1A 1.374(3) 2_655 ?
O1A V1 1.7823(16) . ?
C1A O1A 1.374(3) 2_655 ?
C1A C6A 1.404(3) . ?
C1A C2A 1.408(3) . ?
C2A C3A 1.398(3) . ?
C2A C21A 1.544(4) . ?
C3A C4A 1.399(4) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.391(3) . ?
C4A C41A 1.539(3) . ?
C5A C6A 1.396(3) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.515(3) . ?
C41A C43Y 1.33(4) . ?
C41A C43A 1.497(6) . ?
C41A C44A 1.538(5) . ?
C41A C42A 1.567(6) . ?
C41A C42Y 1.59(4) . ?
C41A C44Y 1.62(3) . ?
C42A H42A 0.9600 . ?
C42A H42B 0.9600 . ?
C42A H42C 0.9600 . ?
C43A H43A 0.9600 . ?
C43A H43B 0.9600 . ?
C43A H43C 0.9600 . ?
C44A H44A 0.9600 . ?
C44A H44B 0.9600 . ?
C44A H44C 0.9600 . ?
C42Y H42Z 0.9600 . ?
C42Y H42Y 0.9600 . ?
C42Y H42X 0.9600 . ?
C43Y H43Z 0.9600 . ?
C43Y H43Y 0.9600 . ?
C43Y H43X 0.9600 . ?
C44Y H44Z 0.9600 . ?
C44Y H44Y 0.9600 . ?
C44Y H44X 0.9600 . ?
C21A C22A 1.527(4) . ?
C21A C24A 1.544(4) . ?
C21A C23A 1.548(4) . ?
C22A H22A 0.9600 . ?
C22A H22B 0.9600 . ?
C22A H22C 0.9600 . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C7A C2B 1.524(3) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
O1B C1B 1.369(3) . ?
O1B V1 1.7707(16) . ?
C1B C6B 1.398(3) . ?
C1B C2B 1.403(3) . ?
C2B C3B 1.394(3) . ?
C3B C4B 1.393(4) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.395(4) . ?
C4B C41B 1.548(4) . ?
C5B C6B 1.400(3) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.521(3) . ?
C7B C2C 1.521(3) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C41B C43Z 1.492(13) . ?
C41B C42B 1.492(10) . ?
C41B C42Z 1.495(10) . ?
C41B C43B 1.537(8) . ?
C41B C44B 1.549(7) . ?
C41B C44Z 1.596(9) . ?
C42B H42D 0.9600 . ?
C42B H42E 0.9600 . ?
C42B H42F 0.9600 . ?
C43B H43D 0.9600 . ?
C43B H43E 0.9600 . ?
C43B H43F 0.9600 . ?
C44B H44D 0.9600 . ?
C44B H443 0.9600 . ?
C44B H44F 0.9600 . ?
C42Z H42W 0.9600 . ?
C42Z H42V 0.9600 . ?
C42Z H42U 0.9600 . ?
C43Z H43W 0.9600 . ?
C43Z H43V 0.9600 . ?
C43Z H43U 0.9600 . ?
C44Z H44W 0.9600 . ?
C44Z H44V 0.9600 . ?
C44Z H44U 0.9600 . ?
O1C C1C 1.374(3) . ?
O1C V1 1.7760(17) . ?
C1C C2C 1.404(3) . ?
C1C C6C 1.409(3) . ?
C2C C3C 1.399(3) . ?
C3C C4C 1.383(3) . ?
C3C H3C 0.9300 . ?
C4C C5C 1.401(4) . ?
C4C C41C 1.544(3) . ?
C5C C6C 1.396(3) . ?
C5C H5C 0.9300 . ?
C6C C7C 1.544(3) . ?
C7C C73C 1.537(4) . ?
C7C C72C 1.539(4) . ?
C7C C71C 1.548(4) . ?
C41C C44C 1.529(4) . ?
C41C C42C 1.532(4) . ?
C41C C43C 1.540(4) . ?
C42C H42G 0.9600 . ?
C42C H42H 0.9600 . ?
C42C H42I 0.9600 . ?
C43C H43G 0.9600 . ?
C43C H43H 0.9600 . ?
C43C H43I 0.9600 . ?
C44C H44G 0.9600 . ?
C44C H44H 0.9600 . ?
C44C H44I 0.9600 . ?
C71C H71A 0.9600 . ?
C71C H71B 0.9600 . ?
C71C H71C 0.9600 . ?
C72C H72A 0.9600 . ?
C72C H72B 0.9600 . ?
C72C H72C 0.9600 . ?
C73C H73A 0.9600 . ?
C73C H73B 0.9600 . ?
C73C H73C 0.9600 . ?
V1 O1 1.5954(18) . ?
N81 C82 1.130(6) . ?
C82 C83 1.380(6) . ?
C83 H83A 0.9600 . ?
C83 H83B 0.9600 . ?
C83 H83C 0.9600 . ?
N91 C92 1.138(7) . ?
C92 C93 1.429(7) . ?
C93 H93A 0.9600 . ?
C93 H93B 0.9600 . ?
C93 H93C 0.9600 . ?

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
C1A O1A V1 140.15(15) 2_655 . ?
O1A C1A C6A 117.50(19) 2_655 . ?
O1A C1A C2A 120.4(2) 2_655 . ?
C6A C1A C2A 121.9(2) . . ?
C3A C2A C1A 116.0(2) . . ?
C3A C2A C21A 122.0(2) . . ?
C1A C2A C21A 121.9(2) . . ?
C2A C3A C4A 124.1(2) . . ?
C2A C3A H3A 118.0 . . ?
C4A C3A H3A 118.0 . . ?
C5A C4A C3A 117.5(2) . . ?
C5A C4A C41A 121.3(2) . . ?
C3A C4A C41A 121.0(2) . . ?
C4A C5A C6A 121.4(2) . . ?
C4A C5A H5A 119.3 . . ?
C6A C5A H5A 119.3 . . ?
C5A C6A C1A 119.0(2) . . ?
C5A C6A C7A 119.2(2) . . ?
C1A C6A C7A 121.5(2) . . ?
C43Y C41A C43A 129.3(18) . . ?
C43Y C41A C44A 69.9(18) . . ?
C43A C41A C44A 110.0(4) . . ?
C43Y C41A C4A 114.6(18) . . ?
C43A C41A C4A 111.6(3) . . ?
C44A C41A C4A 112.4(3) . . ?
C43A C41A C42A 109.8(4) . . ?
C44A C41A C42A 106.0(4) . . ?
C4A C41A C42A 106.8(3) . . ?
C43Y C41A C42Y 120(2) . . ?
C43A C41A C42Y 65.1(14) . . ?
C44A C41A C42Y 53.5(14) . . ?
C4A C41A C42Y 103.8(14) . . ?
C42A C41A C42Y 148.4(14) . . ?
C43Y C41A C44Y 112(2) . . ?
C44A C41A C44Y 133.0(11) . . ?
C4A C41A C44Y 108.8(11) . . ?
C42A C41A C44Y 82.3(11) . . ?
C42Y C41A C44Y 95.6(18) . . ?
C41A C42A H42A 109.5 . . ?
C41A C42A H42B 109.5 . . ?
H42A C42A H42B 109.5 . . ?
C41A C42A H42C 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C41A C43A H43A 109.5 . . ?
C41A C43A H43B 109.5 . . ?
H43A C43A H43B 109.5 . . ?
C41A C43A H43C 109.5 . . ?
H43A C43A H43C 109.5 . . ?
H43B C43A H43C 109.5 . . ?
C41A C44A H44A 109.5 . . ?
C41A C44A H44B 109.5 . . ?
H44A C44A H44B 109.5 . . ?
C41A C44A H44C 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C41A C42Y H42Z 109.5 . . ?
C41A C42Y H42Y 109.5 . . ?
H42Z C42Y H42Y 109.5 . . ?
C41A C42Y H42X 109.5 . . ?
H42Z C42Y H42X 109.5 . . ?
H42Y C42Y H42X 109.5 . . ?
C41A C43Y H43Z 109.5 . . ?
C41A C43Y H43Y 109.5 . . ?
H43Z C43Y H43Y 109.5 . . ?
C41A C43Y H43X 109.5 . . ?
H43Z C43Y H43X 109.5 . . ?
H43Y C43Y H43X 109.5 . . ?
C41A C44Y H44Z 109.5 . . ?
C41A C44Y H44Y 109.5 . . ?
H44Z C44Y H44Y 109.5 . . ?
C41A C44Y H44X 109.5 . . ?
H44Z C44Y H44X 109.5 . . ?
H44Y C44Y H44X 109.5 . . ?
C22A C21A C2A 111.7(2) . . ?
C22A C21A C24A 107.3(3) . . ?
C2A C21A C24A 111.6(2) . . ?
C22A C21A C23A 110.2(3) . . ?
C2A C21A C23A 108.6(2) . . ?
C24A C21A C23A 107.3(3) . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21A C23A H23A 109.5 . . ?
C21A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C21A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C21A C24A H24A 109.5 . . ?
C21A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C21A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C6A C7A C2B 113.00(18) . . ?
C6A C7A H7A1 109.0 . . ?
C2B C7A H7A1 109.0 . . ?
C6A C7A H7A2 109.0 . . ?
C2B C7A H7A2 109.0 . . ?
H7A1 C7A H7A2 107.8 . . ?
C1B O1B V1 143.66(15) . . ?
O1B C1B C6B 121.5(2) . . ?
O1B C1B C2B 116.9(2) . . ?
C6B C1B C2B 121.6(2) . . ?
C3B C2B C1B 118.3(2) . . ?
C3B C2B C7A 123.2(2) . . ?
C1B C2B C7A 118.50(19) . . ?
C4B C3B C2B 122.2(2) . . ?
C4B C3B H3B 118.9 . . ?
C2B C3B H3B 118.9 . . ?
C3B C4B C5B 117.7(2) . . ?
C3B C4B C41B 121.2(2) . . ?
C5B C4B C41B 121.0(2) . . ?
C4B C5B C6B 122.4(2) . . ?
C4B C5B H5B 118.8 . . ?
C6B C5B H5B 118.8 . . ?
C1B C6B C5B 117.8(2) . . ?
C1B C6B C7B 121.6(2) . . ?
C5B C6B C7B 120.3(2) . . ?
C2C C7B C6B 111.39(18) . . ?
C2C C7B H7B1 109.3 . . ?
C6B C7B H7B1 109.3 . . ?
C2C C7B H7B2 109.3 . . ?
C6B C7B H7B2 109.3 . . ?
H7B1 C7B H7B2 108.0 . . ?
C43Z C41B C42B 130.2(7) . . ?
C43Z C41B C42Z 108.8(7) . . ?
C42B C41B C42Z 66.7(6) . . ?
C43Z C41B C43B 69.3(6) . . ?
C42B C41B C43B 108.8(6) . . ?
C42Z C41B C43B 45.3(4) . . ?
C43Z C41B C4B 113.9(6) . . ?
C42B C41B C4B 113.7(5) . . ?
C42Z C41B C4B 110.0(4) . . ?
C43B C41B C4B 107.5(4) . . ?
C42B C41B C44B 111.9(5) . . ?
C42Z C41B C44B 136.7(5) . . ?
C43B C41B C44B 105.3(4) . . ?
C4B C41B C44B 109.3(3) . . ?
C43Z C41B C44Z 112.6(7) . . ?
C42Z C41B C44Z 102.0(5) . . ?
C43B C41B C44Z 138.2(5) . . ?
C4B C41B C44Z 108.8(4) . . ?
C44B C41B C44Z 81.6(4) . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41B C43B H43D 109.5 . . ?
C41B C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C41B C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C41B C44B H44D 109.5 . . ?
C41B C44B H443 109.5 . . ?
H44D C44B H443 109.5 . . ?
C41B C44B H44F 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H443 C44B H44F 109.5 . . ?
C41B C42Z H42W 109.5 . . ?
C41B C42Z H42V 109.5 . . ?
H42W C42Z H42V 109.5 . . ?
C41B C42Z H42U 109.5 . . ?
H42W C42Z H42U 109.5 . . ?
H42V C42Z H42U 109.5 . . ?
C41B C43Z H43W 109.5 . . ?
C41B C43Z H43V 109.5 . . ?
H43W C43Z H43V 109.5 . . ?
C41B C43Z H43U 109.5 . . ?
H43W C43Z H43U 109.5 . . ?
H43V C43Z H43U 109.5 . . ?
C41B C44Z H44W 109.5 . . ?
C41B C44Z H44V 109.5 . . ?
H44W C44Z H44V 109.5 . . ?
C41B C44Z H44U 109.5 . . ?
H44W C44Z H44U 109.5 . . ?
H44V C44Z H44U 109.5 . . ?
C1C O1C V1 138.42(15) . . ?
O1C C1C C2C 119.2(2) . . ?
O1C C1C C6C 118.7(2) . . ?
C2C C1C C6C 122.1(2) . . ?
C3C C2C C1C 118.2(2) . . ?
C3C C2C C7B 118.7(2) . . ?
C1C C2C C7B 123.0(2) . . ?
C4C C3C C2C 122.2(2) . . ?
C4C C3C H3C 118.9 . . ?
C2C C3C H3C 118.9 . . ?
C3C C4C C5C 117.6(2) . . ?
C3C C4C C41C 122.3(2) . . ?
C5C C4C C41C 120.1(2) . . ?
C6C C5C C4C 123.5(2) . . ?
C6C C5C H5C 118.3 . . ?
C4C C5C H5C 118.3 . . ?
C5C C6C C1C 116.5(2) . . ?
C5C C6C C7C 121.7(2) . . ?
C1C C6C C7C 121.8(2) . . ?
C73C C7C C72C 107.1(3) . . ?
C73C C7C C6C 111.5(2) . . ?
C72C C7C C6C 110.4(2) . . ?
C73C C7C C71C 107.1(3) . . ?
C72C C7C C71C 110.7(3) . . ?
C6C C7C C71C 110.0(2) . . ?
C44C C41C C42C 109.2(3) . . ?
C44C C41C C43C 108.3(3) . . ?
C42C C41C C43C 108.4(3) . . ?
C44C C41C C4C 112.0(2) . . ?
C42C C41C C4C 108.7(2) . . ?
C43C C41C C4C 110.3(2) . . ?
C41C C42C H42G 109.5 . . ?
C41C C42C H42H 109.5 . . ?
H42G C42C H42H 109.5 . . ?
C41C C42C H42I 109.5 . . ?
H42G C42C H42I 109.5 . . ?
H42H C42C H42I 109.5 . . ?
C41C C43C H43G 109.5 . . ?
C41C C43C H43H 109.5 . . ?
H43G C43C H43H 109.5 . . ?
C41C C43C H43I 109.5 . . ?
H43G C43C H43I 109.5 . . ?
H43H C43C H43I 109.5 . . ?
C41C C44C H44G 109.5 . . ?
C41C C44C H44H 109.5 . . ?
H44G C44C H44H 109.5 . . ?
C41C C44C H44I 109.5 . . ?
H44G C44C H44I 109.5 . . ?
H44H C44C H44I 109.5 . . ?
C7C C71C H71A 109.5 . . ?
C7C C71C H71B 109.5 . . ?
H71A C71C H71B 109.5 . . ?
C7C C71C H71C 109.5 . . ?
H71A C71C H71C 109.5 . . ?
H71B C71C H71C 109.5 . . ?
C7C C72C H72A 109.5 . . ?
C7C C72C H72B 109.5 . . ?
H72A C72C H72B 109.5 . . ?
C7C C72C H72C 109.5 . . ?
H72A C72C H72C 109.5 . . ?
H72B C72C H72C 109.5 . . ?
C7C C73C H73A 109.5 . . ?
C7C C73C H73B 109.5 . . ?
H73A C73C H73B 109.5 . . ?
C7C C73C H73C 109.5 . . ?
H73A C73C H73C 109.5 . . ?
H73B C73C H73C 109.5 . . ?
O1 V1 O1B 107.89(9) . . ?
O1 V1 O1C 110.00(9) . . ?
O1B V1 O1C 108.15(8) . . ?
O1 V1 O1A 109.85(9) . . ?
O1B V1 O1A 112.53(8) . . ?
O1C V1 O1A 108.39(8) . . ?
N81 C82 C83 174.5(7) . . ?
C82 C83 H83A 109.5 . . ?
C82 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C82 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
N91 C92 C93 180.000(1) . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 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
O1A C1A C2A C3A 175.2(2) 2_655 . . . ?
C6A C1A C2A C3A 0.8(4) . . . . ?
O1A C1A C2A C21A -1.4(4) 2_655 . . . ?
C6A C1A C2A C21A -175.9(2) . . . . ?
C1A C2A C3A C4A -0.6(4) . . . . ?
C21A C2A C3A C4A 176.0(3) . . . . ?
C2A C3A C4A C5A 0.6(4) . . . . ?
C2A C3A C4A C41A -175.3(3) . . . . ?
C3A C4A C5A C6A -0.6(4) . . . . ?
C41A C4A C5A C6A 175.2(2) . . . . ?
C4A C5A C6A C1A 0.7(4) . . . . ?
C4A C5A C6A C7A -173.3(2) . . . . ?
O1A C1A C6A C5A -175.4(2) 2_655 . . . ?
C2A C1A C6A C5A -0.8(3) . . . . ?
O1A C1A C6A C7A -1.6(3) 2_655 . . . ?
C2A C1A C6A C7A 173.0(2) . . . . ?
C5A C4A C41A C43Y -69(2) . . . . ?
C3A C4A C41A C43Y 107(2) . . . . ?
C5A C4A C41A C43A 132.8(4) . . . . ?
C3A C4A C41A C43A -51.5(4) . . . . ?
C5A C4A C41A C44A 8.7(5) . . . . ?
C3A C4A C41A C44A -175.6(4) . . . . ?
C5A C4A C41A C42A -107.2(4) . . . . ?
C3A C4A C41A C42A 68.5(4) . . . . ?
C5A C4A C41A C42Y 64.5(15) . . . . ?
C3A C4A C41A C42Y -119.8(15) . . . . ?
C5A C4A C41A C44Y 165.5(12) . . . . ?
C3A C4A C41A C44Y -18.9(12) . . . . ?
C3A C2A C21A C22A 121.3(3) . . . . ?
C1A C2A C21A C22A -62.2(3) . . . . ?
C3A C2A C21A C24A 1.1(4) . . . . ?
C1A C2A C21A C24A 177.6(3) . . . . ?
C3A C2A C21A C23A -116.9(3) . . . . ?
C1A C2A C21A C23A 59.5(3) . . . . ?
C5A C6A C7A C2B 96.0(2) . . . . ?
C1A C6A C7A C2B -77.8(3) . . . . ?
V1 O1B C1B C6B -2.6(4) . . . . ?
V1 O1B C1B C2B 175.03(18) . . . . ?
O1B C1B C2B C3B -177.8(2) . . . . ?
C6B C1B C2B C3B -0.2(3) . . . . ?
O1B C1B C2B C7A -0.7(3) . . . . ?
C6B C1B C2B C7A 176.9(2) . . . . ?
C6A C7A C2B C3B 8.1(3) . . . . ?
C6A C7A C2B C1B -168.84(19) . . . . ?
C1B C2B C3B C4B -0.2(4) . . . . ?
C7A C2B C3B C4B -177.1(2) . . . . ?
C2B C3B C4B C5B -0.4(4) . . . . ?
C2B C3B C4B C41B 179.5(3) . . . . ?
C3B C4B C5B C6B 1.3(4) . . . . ?
C41B C4B C5B C6B -178.6(3) . . . . ?
O1B C1B C6B C5B 178.6(2) . . . . ?
C2B C1B C6B C5B 1.0(3) . . . . ?
O1B C1B C6B C7B 4.7(3) . . . . ?
C2B C1B C6B C7B -172.9(2) . . . . ?
C4B C5B C6B C1B -1.6(4) . . . . ?
C4B C5B C6B C7B 172.4(2) . . . . ?
C1B C6B C7B C2C 82.6(3) . . . . ?
C5B C6B C7B C2C -91.2(3) . . . . ?
C3B C4B C41B C43Z -170.7(7) . . . . ?
C5B C4B C41B C43Z 9.2(8) . . . . ?
C3B C4B C41B C42B -5.7(7) . . . . ?
C5B C4B C41B C42B 174.2(6) . . . . ?
C3B C4B C41B C42Z 66.8(5) . . . . ?
C5B C4B C41B C42Z -113.3(5) . . . . ?
C3B C4B C41B C43B 114.7(4) . . . . ?
C5B C4B C41B C43B -65.4(5) . . . . ?
C3B C4B C41B C44B -131.5(4) . . . . ?
C5B C4B C41B C44B 48.3(4) . . . . ?
C3B C4B C41B C44Z -44.1(5) . . . . ?
C5B C4B C41B C44Z 135.8(4) . . . . ?
V1 O1C C1C C2C 37.2(3) . . . . ?
V1 O1C C1C C6C -142.7(2) . . . . ?
O1C C1C C2C C3C -178.3(2) . . . . ?
C6C C1C C2C C3C 1.6(3) . . . . ?
O1C C1C C2C C7B -1.1(3) . . . . ?
C6C C1C C2C C7B 178.9(2) . . . . ?
C6B C7B C2C C3C 77.8(3) . . . . ?
C6B C7B C2C C1C -99.4(3) . . . . ?
C1C C2C C3C C4C 0.3(3) . . . . ?
C7B C2C C3C C4C -177.1(2) . . . . ?
C2C C3C C4C C5C -1.8(4) . . . . ?
C2C C3C C4C C41C 179.3(2) . . . . ?
C3C C4C C5C C6C 1.5(4) . . . . ?
C41C C4C C5C C6C -179.6(2) . . . . ?
C4C C5C C6C C1C 0.3(4) . . . . ?
C4C C5C C6C C7C 179.5(2) . . . . ?
O1C C1C C6C C5C 178.0(2) . . . . ?
C2C C1C C6C C5C -1.9(3) . . . . ?
O1C C1C C6C C7C -1.2(3) . . . . ?
C2C C1C C6C C7C 178.9(2) . . . . ?
C5C C6C C7C C73C 3.2(4) . . . . ?
C1C C6C C7C C73C -177.7(3) . . . . ?
C5C C6C C7C C72C 122.1(3) . . . . ?
C1C C6C C7C C72C -58.7(3) . . . . ?
C5C C6C C7C C71C -115.5(3) . . . . ?
C1C C6C C7C C71C 63.7(3) . . . . ?
C3C C4C C41C C44C -8.2(4) . . . . ?
C5C C4C C41C C44C 172.9(3) . . . . ?
C3C C4C C41C C42C 112.5(3) . . . . ?
C5C C4C C41C C42C -66.4(3) . . . . ?
C3C C4C C41C C43C -128.8(3) . . . . ?
C5C C4C C41C C43C 52.3(3) . . . . ?
C1B O1B V1 O1 -166.3(2) . . . . ?
C1B O1B V1 O1C -47.3(3) . . . . ?
C1B O1B V1 O1A 72.4(3) . . . . ?
C1C O1C V1 O1 133.1(2) . . . . ?
C1C O1C V1 O1B 15.5(3) . . . . ?
C1C O1C V1 O1A -106.7(2) . . . . ?
C1A O1A V1 O1 -19.1(3) 2_655 . . . ?
C1A O1A V1 O1B 101.1(2) 2_655 . . . ?
C1A O1A V1 O1C -139.3(2) 2_655 . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.054

#===END

data_9
_database_code_depnum_ccdc_archive 'CCDC 718350'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     
'[{V(=NC6H4Me)}2(mu-triphenolate)2{V(=O)(mu-O)(O-i-Pr)}2].1.5MeCN'
_chemical_formula_moiety         'C94 H126 N2 O12 V4, 1.5(C2 H3 N)'
_chemical_formula_sum            'C97 H130.50 N3.50 O12 V4'
_chemical_formula_weight         1741.31

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'

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

_cell_length_a                   14.821(3)
_cell_length_b                   17.649(3)
_cell_length_c                   22.129(4)
_cell_angle_alpha                80.787(3)
_cell_angle_beta                 76.259(3)
_cell_angle_gamma                68.612(3)
_cell_volume                     5218.1(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14418
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      28.71

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1850
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   'SADABS v.2.03, Sheldrick, G.M., (2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6892
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART 1K 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_%        18
_diffrn_reflns_number            50900
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         27.50
_reflns_number_total             25941
_reflns_number_gt                17505
_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    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'CAMERON (Watkins <i>et al.</i>, 1996)'
_computing_publication_material  
;
Bruker SHELXTL (Sheldrick, 2008), 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^ > 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. Platon squeeze recovered
27 el in one void. MeCN has 22 el, so added one MeCN per cell.
;

_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^)+(0.0603P)^2^+0.0000P] 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         25941
_refine_ls_number_parameters     1106
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1181
_refine_ls_wR_factor_gt          0.1095
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.002
_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 0.76562(2) 0.168280(18) 0.792292(14) 0.01808(7) Uani 1 1 d . B .
V2 V 0.75107(2) 0.312833(19) 0.674263(14) 0.01968(7) Uani 1 1 d . C .
O1 O 0.96936(9) 0.23518(8) 0.88779(6) 0.0261(3) Uani 1 1 d . . .
O2 O 0.83947(8) 0.23914(7) 0.72423(5) 0.0193(3) Uani 1 1 d . . .
O3 O 0.75788(9) 0.25466(8) 0.61292(6) 0.0234(3) Uani 1 1 d . . .
C1 C 0.99080(13) 0.30601(11) 0.87360(9) 0.0219(4) Uani 1 1 d . . .
C2 C 1.04022(13) 0.32770(11) 0.91153(9) 0.0237(4) Uani 1 1 d . . .
C3 C 1.06202(14) 0.39943(12) 0.89226(9) 0.0263(4) Uani 1 1 d . . .
H3 H 1.0946 0.4155 0.9174 0.032 Uiso 1 1 calc R . .
C4 C 1.03919(14) 0.44828(12) 0.83910(9) 0.0276(4) Uani 1 1 d . . .
C5 C 0.99054(14) 0.42427(12) 0.80323(9) 0.0266(4) Uani 1 1 d . . .
H5 H 0.9737 0.4569 0.7663 0.032 Uiso 1 1 calc R . .
C6 C 0.96584(13) 0.35425(11) 0.81958(9) 0.0236(4) Uani 1 1 d . . .
C7 C 1.06631(15) 0.27654(13) 0.97211(10) 0.0312(4) Uani 1 1 d . . .
C8 C 1.12654(18) 0.30964(15) 1.00189(11) 0.0426(6) Uani 1 1 d . . .
H8A H 1.1880 0.3084 0.9726 0.064 Uiso 1 1 calc R . .
H8B H 1.1421 0.2757 1.0402 0.064 Uiso 1 1 calc R . .
H8C H 1.0880 0.3660 1.0119 0.064 Uiso 1 1 calc R . .
C9 C 1.12859(18) 0.18767(14) 0.95946(12) 0.0454(6) Uani 1 1 d . . .
H9A H 1.0908 0.1636 0.9425 0.068 Uiso 1 1 calc R . .
H9B H 1.1454 0.1566 0.9985 0.068 Uiso 1 1 calc R . .
H9C H 1.1894 0.1861 0.9293 0.068 Uiso 1 1 calc R . .
C10 C 0.97097(17) 0.28037(15) 1.01928(10) 0.0412(5) Uani 1 1 d . . .
H10A H 0.9336 0.3371 1.0286 0.062 Uiso 1 1 calc R . .
H10B H 0.9873 0.2472 1.0577 0.062 Uiso 1 1 calc R . .
H10C H 0.9310 0.2592 1.0017 0.062 Uiso 1 1 calc R . .
C11 C 1.06553(19) 0.52595(14) 0.81842(11) 0.0412(6) Uani 1 1 d . . .
C12 C 0.9703(3) 0.59822(16) 0.81294(16) 0.0758(10) Uani 1 1 d . . .
H12A H 0.9256 0.6045 0.8537 0.114 Uiso 1 1 calc R . .
H12B H 0.9382 0.5881 0.7826 0.114 Uiso 1 1 calc R . .
H12C H 0.9863 0.6482 0.7989 0.114 Uiso 1 1 calc R . .
C13 C 1.1136(3) 0.54464(18) 0.86495(13) 0.0668(9) Uani 1 1 d . . .
H13A H 1.1787 0.5027 0.8655 0.100 Uiso 1 1 calc R . .
H13B H 1.0719 0.5451 0.9066 0.100 Uiso 1 1 calc R . .
H13C H 1.1212 0.5982 0.8527 0.100 Uiso 1 1 calc R . .
C14 C 1.1352(3) 0.5164(2) 0.75492(13) 0.0757(10) Uani 1 1 d . . .
H14A H 1.1502 0.5668 0.7408 0.114 Uiso 1 1 calc R . .
H14B H 1.1036 0.5055 0.7247 0.114 Uiso 1 1 calc R . .
H14C H 1.1966 0.4709 0.7585 0.114 Uiso 1 1 calc R . .
C15 C 0.91379(13) 0.33061(11) 0.77910(8) 0.0228(4) Uani 1 1 d . . .
H15A H 0.8783 0.3803 0.7549 0.027 Uiso 1 1 calc R . .
H15B H 0.8638 0.3089 0.8063 0.027 Uiso 1 1 calc R . .
C16 C 0.93976(12) 0.22517(11) 0.70688(8) 0.0221(4) Uani 1 1 d . . .
C17 C 0.98101(13) 0.26765(12) 0.73407(8) 0.0249(4) Uani 1 1 d . . .
C18 C 1.08093(15) 0.25483(16) 0.71419(10) 0.0414(6) Uani 1 1 d . . .
H18 H 1.1103 0.2834 0.7319 0.050 Uiso 1 1 calc R . .
C19 C 1.13945(16) 0.20138(19) 0.66918(12) 0.0527(7) Uani 1 1 d . . .
C20 C 1.09548(15) 0.16128(16) 0.64326(11) 0.0440(6) Uani 1 1 d . . .
H20 H 1.1352 0.1244 0.6126 0.053 Uiso 1 1 calc R . .
C21 C 0.99463(14) 0.17285(12) 0.66029(9) 0.0276(4) Uani 1 1 d . . .
C22 C 1.24844(18) 0.1885(3) 0.64846(17) 0.0969(14) Uani 1 1 d . . .
H22A H 1.2597 0.2395 0.6498 0.145 Uiso 1 1 calc R . .
H22B H 1.2709 0.1718 0.6057 0.145 Uiso 1 1 calc R . .
H22C H 1.2854 0.1458 0.6764 0.145 Uiso 1 1 calc R . .
C23 C 0.94657(14) 0.13463(12) 0.62620(9) 0.0280(4) Uani 1 1 d . . .
H23A H 0.9913 0.0785 0.6174 0.034 Uiso 1 1 calc R . .
H23B H 0.8847 0.1308 0.6535 0.034 Uiso 1 1 calc R . .
C24 C 0.83000(14) 0.23866(12) 0.55951(8) 0.0252(4) Uani 1 1 d . . .
C25 C 0.92342(14) 0.18279(12) 0.56559(9) 0.0260(4) Uani 1 1 d . . .
C26 C 0.99854(15) 0.17130(13) 0.51289(9) 0.0329(5) Uani 1 1 d . . .
H26 H 1.0622 0.1333 0.5163 0.039 Uiso 1 1 calc R . .
C27 C 0.98397(16) 0.21316(14) 0.45578(9) 0.0354(5) Uani 1 1 d . . .
C28 C 0.88813(16) 0.26345(14) 0.45118(9) 0.0347(5) Uani 1 1 d . . .
H28 H 0.8763 0.2900 0.4115 0.042 Uiso 1 1 calc R . .
C29 C 0.80847(15) 0.27714(12) 0.50139(9) 0.0286(4) Uani 1 1 d . . .
C30 C 1.07278(19) 0.20288(17) 0.40138(11) 0.0501(6) Uani 1 1 d . . .
C31 C 1.1451(2) 0.2356(2) 0.41922(13) 0.0759(10) Uani 1 1 d . . .
H31A H 1.1103 0.2919 0.4306 0.114 Uiso 1 1 calc R . .
H31B H 1.1994 0.2343 0.3837 0.114 Uiso 1 1 calc R . .
H31C H 1.1715 0.2014 0.4548 0.114 Uiso 1 1 calc R . .
C32 C 1.1232(2) 0.1126(2) 0.38939(13) 0.0747(10) Uani 1 1 d . . .
H32A H 1.1495 0.0819 0.4261 0.112 Uiso 1 1 calc R . .
H32B H 1.1773 0.1067 0.3531 0.112 Uiso 1 1 calc R . .
H32C H 1.0750 0.0913 0.3813 0.112 Uiso 1 1 calc R . .
C33 C 1.0421(2) 0.25216(19) 0.34104(11) 0.0599(8) Uani 1 1 d . . .
H33A H 0.9965 0.2321 0.3282 0.090 Uiso 1 1 calc R . .
H33B H 1.1009 0.2457 0.3079 0.090 Uiso 1 1 calc R . .
H33C H 1.0094 0.3100 0.3486 0.090 Uiso 1 1 calc R . .
C34 C 0.70369(16) 0.32974(14) 0.49251(9) 0.0342(5) Uani 1 1 d . . .
C35 C 0.63287(17) 0.28138(16) 0.51860(11) 0.0465(6) Uani 1 1 d . . .
H35A H 0.6306 0.2679 0.5635 0.070 Uiso 1 1 calc R . .
H35B H 0.6564 0.2309 0.4976 0.070 Uiso 1 1 calc R . .
H35C H 0.5665 0.3145 0.5113 0.070 Uiso 1 1 calc R . .
C36 C 0.69855(19) 0.35414(17) 0.42314(11) 0.0487(6) Uani 1 1 d . . .
H36A H 0.6299 0.3846 0.4192 0.073 Uiso 1 1 calc R . .
H36B H 0.7233 0.3049 0.4005 0.073 Uiso 1 1 calc R . .
H36C H 0.7392 0.3884 0.4055 0.073 Uiso 1 1 calc R . .
C37 C 0.66650(16) 0.40956(14) 0.52466(11) 0.0399(5) Uani 1 1 d . . .
H37A H 0.6639 0.3969 0.5697 0.060 Uiso 1 1 calc R . .
H37B H 0.6003 0.4424 0.5170 0.060 Uiso 1 1 calc R . .
H37C H 0.7116 0.4402 0.5078 0.060 Uiso 1 1 calc R . .
O4 O 0.47337(9) 0.50716(8) 0.77268(6) 0.0275(3) Uani 1 1 d . . .
O5 O 0.67450(8) 0.25057(7) 0.74902(5) 0.0195(3) Uani 1 1 d . . .
O6 O 0.80204(8) 0.08192(7) 0.74831(5) 0.0195(2) Uani 1 1 d . . .
C38 C 0.43658(13) 0.50279(11) 0.83541(9) 0.0240(4) Uani 1 1 d . . .
C39 C 0.36907(14) 0.57232(11) 0.86488(9) 0.0268(4) Uani 1 1 d . . .
C40 C 0.33235(14) 0.56063(12) 0.92836(10) 0.0302(4) Uani 1 1 d . . .
H40 H 0.2866 0.6067 0.9492 0.036 Uiso 1 1 calc R . .
C41 C 0.35843(14) 0.48554(12) 0.96335(9) 0.0273(4) Uani 1 1 d . A .
C42 C 0.42670(13) 0.41917(12) 0.93214(9) 0.0263(4) Uani 1 1 d . . .
H42 H 0.4466 0.3672 0.9547 0.032 Uiso 1 1 calc R . .
C43 C 0.46654(13) 0.42686(11) 0.86902(9) 0.0239(4) Uani 1 1 d . . .
C44 C 0.34213(15) 0.65706(12) 0.82925(11) 0.0356(5) Uani 1 1 d . . .
C45 C 0.2605(2) 0.72142(14) 0.86983(13) 0.0603(8) Uani 1 1 d . . .
H45A H 0.2448 0.7747 0.8458 0.090 Uiso 1 1 calc R . .
H45B H 0.2835 0.7247 0.9070 0.090 Uiso 1 1 calc R . .
H45C H 0.2013 0.7058 0.8825 0.090 Uiso 1 1 calc R . .
C46 C 0.30455(18) 0.65896(14) 0.77018(12) 0.0459(6) Uani 1 1 d . . .
H46A H 0.2883 0.7142 0.7493 0.069 Uiso 1 1 calc R . .
H46B H 0.2453 0.6433 0.7814 0.069 Uiso 1 1 calc R . .
H46C H 0.3559 0.6206 0.7420 0.069 Uiso 1 1 calc R . .
C47 C 0.43342(18) 0.68393(14) 0.81245(12) 0.0463(6) Uani 1 1 d . . .
H47A H 0.4169 0.7380 0.7896 0.069 Uiso 1 1 calc R . .
H47B H 0.4873 0.6446 0.7863 0.069 Uiso 1 1 calc R . .
H47C H 0.4542 0.6863 0.8508 0.069 Uiso 1 1 calc R . .
C48 C 0.31686(15) 0.47742(13) 1.03363(10) 0.0335(5) Uani 1 1 d DU . .
C49 C 0.2035(2) 0.5161(3) 1.04523(14) 0.0578(11) Uani 0.816(5) 1 d PDU A 1
H49A H 0.1768 0.4881 1.0229 0.087 Uiso 0.816(5) 1 calc PR A 1
H49B H 0.1849 0.5740 1.0301 0.087 Uiso 0.816(5) 1 calc PR A 1
H49C H 0.1766 0.5110 1.0900 0.087 Uiso 0.816(5) 1 calc PR A 1
C50 C 0.3581(3) 0.5211(2) 1.06778(14) 0.0546(10) Uani 0.816(5) 1 d PDU A 1
H50A H 0.3314 0.5162 1.1126 0.082 Uiso 0.816(5) 1 calc PR A 1
H50B H 0.3395 0.5790 1.0525 0.082 Uiso 0.816(5) 1 calc PR A 1
H50C H 0.4303 0.4965 1.0603 0.082 Uiso 0.816(5) 1 calc PR A 1
C51 C 0.3408(3) 0.38892(17) 1.06038(14) 0.0518(10) Uani 0.816(5) 1 d PDU A 1
H51A H 0.3136 0.3605 1.0387 0.078 Uiso 0.816(5) 1 calc PR A 1
H51B H 0.3116 0.3870 1.1050 0.078 Uiso 0.816(5) 1 calc PR A 1
H51C H 0.4126 0.3622 1.0547 0.078 Uiso 0.816(5) 1 calc PR A 1
C49X C 0.2547(14) 0.4230(12) 1.0437(10) 0.106(8) Uani 0.184(5) 1 d PDU A 2
H49D H 0.2281 0.4156 1.0884 0.160 Uiso 0.184(5) 1 calc PR A 2
H49E H 0.2958 0.3697 1.0280 0.160 Uiso 0.184(5) 1 calc PR A 2
H49F H 0.2001 0.4484 1.0212 0.160 Uiso 0.184(5) 1 calc PR A 2
C50X C 0.2615(13) 0.5584(7) 1.0617(7) 0.097(8) Uani 0.184(5) 1 d PDU A 2
H50D H 0.2378 0.5488 1.1065 0.145 Uiso 0.184(5) 1 calc PR A 2
H50E H 0.2051 0.5888 1.0415 0.145 Uiso 0.184(5) 1 calc PR A 2
H50F H 0.3058 0.5901 1.0552 0.145 Uiso 0.184(5) 1 calc PR A 2
C51X C 0.4053(8) 0.4312(10) 1.0663(6) 0.068(5) Uani 0.184(5) 1 d PDU A 2
H51D H 0.3812 0.4253 1.1115 0.101 Uiso 0.184(5) 1 calc PR A 2
H51E H 0.4508 0.4620 1.0576 0.101 Uiso 0.184(5) 1 calc PR A 2
H51F H 0.4398 0.3771 1.0507 0.101 Uiso 0.184(5) 1 calc PR A 2
C52 C 0.54390(13) 0.35447(11) 0.83797(9) 0.0234(4) Uani 1 1 d . . .
H52A H 0.5768 0.3161 0.8704 0.028 Uiso 1 1 calc R . .
H52B H 0.5945 0.3735 0.8086 0.028 Uiso 1 1 calc R . .
C53 C 0.57697(12) 0.25412(11) 0.76030(8) 0.0200(4) Uani 1 1 d . . .
C54 C 0.50812(13) 0.30799(11) 0.80261(8) 0.0209(4) Uani 1 1 d . . .
C55 C 0.41091(13) 0.30987(12) 0.81408(9) 0.0276(4) Uani 1 1 d . . .
H55 H 0.3624 0.3460 0.8426 0.033 Uiso 1 1 calc R . .
C56 C 0.38298(14) 0.26032(13) 0.78493(10) 0.0318(5) Uani 1 1 d . . .
C57 C 0.45480(14) 0.20613(12) 0.74451(9) 0.0294(4) Uani 1 1 d . . .
H57 H 0.4361 0.1716 0.7248 0.035 Uiso 1 1 calc R . .
C58 C 0.55351(13) 0.20082(11) 0.73197(8) 0.0222(4) Uani 1 1 d . . .
C59 C 0.27639(16) 0.26523(17) 0.79666(14) 0.0553(7) Uani 1 1 d . . .
H59A H 0.2419 0.2876 0.8369 0.083 Uiso 1 1 calc R . .
H59B H 0.2736 0.2105 0.7973 0.083 Uiso 1 1 calc R . .
H59C H 0.2446 0.3008 0.7634 0.083 Uiso 1 1 calc R . .
C60 C 0.63198(13) 0.13672(11) 0.69134(8) 0.0231(4) Uani 1 1 d . . .
H60A H 0.6887 0.1557 0.6734 0.028 Uiso 1 1 calc R . .
H60B H 0.6044 0.1315 0.6562 0.028 Uiso 1 1 calc R . .
C61 C 0.75442(13) 0.02678(11) 0.75180(8) 0.0202(4) Uani 1 1 d . . .
C62 C 0.66919(13) 0.05290(11) 0.72601(8) 0.0218(4) Uani 1 1 d . . .
C63 C 0.61821(14) -0.00129(12) 0.73161(9) 0.0275(4) Uani 1 1 d . . .
H63 H 0.5604 0.0156 0.7143 0.033 Uiso 1 1 calc R . .
C64 C 0.64886(15) -0.07853(12) 0.76143(9) 0.0304(4) Uani 1 1 d . . .
C65 C 0.73602(15) -0.10290(12) 0.78398(9) 0.0283(4) Uani 1 1 d . . .
H65 H 0.7590 -0.1566 0.8033 0.034 Uiso 1 1 calc R . .
C66 C 0.79156(13) -0.05225(11) 0.77956(8) 0.0229(4) Uani 1 1 d . . .
C67 C 0.88711(15) -0.08263(12) 0.80576(9) 0.0279(4) Uani 1 1 d . . .
C68 C 0.97292(15) -0.06557(14) 0.75839(11) 0.0408(5) Uani 1 1 d . . .
H68A H 0.9575 -0.0065 0.7495 0.061 Uiso 1 1 calc R . .
H68B H 0.9828 -0.0905 0.7197 0.061 Uiso 1 1 calc R . .
H68C H 1.0333 -0.0888 0.7757 0.061 Uiso 1 1 calc R . .
C69 C 0.92047(18) -0.17532(13) 0.82270(11) 0.0409(5) Uani 1 1 d . . .
H69A H 0.9843 -0.1935 0.8358 0.061 Uiso 1 1 calc R . .
H69B H 0.9272 -0.2033 0.7862 0.061 Uiso 1 1 calc R . .
H69C H 0.8713 -0.1882 0.8569 0.061 Uiso 1 1 calc R . .
C70 C 0.86863(17) -0.04196(13) 0.86576(10) 0.0361(5) Uani 1 1 d . . .
H70A H 0.9263 -0.0669 0.8856 0.054 Uiso 1 1 calc R . .
H70B H 0.8104 -0.0495 0.8944 0.054 Uiso 1 1 calc R . .
H70C H 0.8574 0.0165 0.8557 0.054 Uiso 1 1 calc R . .
C71 C 0.58689(17) -0.13445(14) 0.77018(11) 0.0397(5) Uani 1 1 d . . .
C72 C 0.5605(3) -0.1381(2) 0.70956(14) 0.0780(10) Uani 1 1 d . . .
H72A H 0.5159 -0.0843 0.6968 0.117 Uiso 1 1 calc R . .
H72B H 0.5275 -0.1785 0.7148 0.117 Uiso 1 1 calc R . .
H72C H 0.6207 -0.1538 0.6774 0.117 Uiso 1 1 calc R . .
C73 C 0.6420(2) -0.22148(18) 0.7944(2) 0.0893(12) Uani 1 1 d . . .
H73A H 0.7020 -0.2454 0.7638 0.134 Uiso 1 1 calc R . .
H73B H 0.5993 -0.2546 0.8010 0.134 Uiso 1 1 calc R . .
H73C H 0.6600 -0.2202 0.8340 0.134 Uiso 1 1 calc R . .
C74 C 0.4933(2) -0.1009(2) 0.81900(14) 0.0670(9) Uani 1 1 d . . .
H74A H 0.5114 -0.1022 0.8591 0.100 Uiso 1 1 calc R . .
H74B H 0.4515 -0.1344 0.8237 0.100 Uiso 1 1 calc R . .
H74C H 0.4570 -0.0444 0.8055 0.100 Uiso 1 1 calc R . .
N1 N 0.68025(11) 0.14878(9) 0.85011(7) 0.0217(3) Uani 1 1 d . . .
C75 C 0.60265(13) 0.14040(11) 0.89620(8) 0.0232(4) Uani 1 1 d . . .
C76 C 0.54740(15) 0.09532(13) 0.88728(10) 0.0324(5) Uani 1 1 d . . .
H76 H 0.5638 0.0694 0.8497 0.039 Uiso 1 1 calc R . .
C77 C 0.46855(16) 0.08848(15) 0.93331(10) 0.0395(5) Uani 1 1 d . . .
H77 H 0.4311 0.0577 0.9270 0.047 Uiso 1 1 calc R . .
C78 C 0.44330(15) 0.12550(14) 0.98824(10) 0.0359(5) Uani 1 1 d . . .
C79 C 0.49920(15) 0.17013(13) 0.99666(10) 0.0356(5) Uani 1 1 d . . .
H79 H 0.4824 0.1961 1.0342 0.043 Uiso 1 1 calc R . .
C80 C 0.57864(15) 0.17758(12) 0.95161(9) 0.0306(4) Uani 1 1 d . . .
H80 H 0.6165 0.2077 0.9584 0.037 Uiso 1 1 calc R . .
C81 C 0.35699(17) 0.11739(18) 1.03824(11) 0.0526(7) Uani 1 1 d . . .
H81A H 0.3194 0.0929 1.0215 0.079 Uiso 1 1 calc R . .
H81B H 0.3141 0.1715 1.0514 0.079 Uiso 1 1 calc R . .
H81C H 0.3817 0.0825 1.0741 0.079 Uiso 1 1 calc R . .
N2 N 0.82745(11) 0.36314(10) 0.63926(7) 0.0242(3) Uani 1 1 d . . .
C82 C 0.89669(14) 0.40152(12) 0.61874(9) 0.0272(4) Uani 1 1 d . . .
C83 C 0.88342(16) 0.47362(13) 0.64323(10) 0.0336(5) Uani 1 1 d . . .
H83 H 0.8257 0.4975 0.6730 0.040 Uiso 1 1 calc R . .
C84 C 0.95481(17) 0.51019(14) 0.62392(11) 0.0409(5) Uani 1 1 d . . .
H84 H 0.9451 0.5596 0.6406 0.049 Uiso 1 1 calc R . .
C85 C 1.03968(17) 0.47676(15) 0.58111(11) 0.0429(6) Uani 1 1 d . . .
C86 C 1.05175(17) 0.40469(16) 0.55687(12) 0.0481(6) Uani 1 1 d . . .
H86 H 1.1099 0.3808 0.5274 0.058 Uiso 1 1 calc R . .
C87 C 0.98146(16) 0.36729(15) 0.57459(10) 0.0395(5) Uani 1 1 d . . .
H87 H 0.9906 0.3187 0.5570 0.047 Uiso 1 1 calc R . .
C88 C 1.1177(2) 0.51666(19) 0.56111(14) 0.0638(8) Uani 1 1 d . . .
H88A H 1.1833 0.4746 0.5583 0.096 Uiso 1 1 calc R . .
H88B H 1.1089 0.5543 0.5918 0.096 Uiso 1 1 calc R . .
H88C H 1.1115 0.5469 0.5202 0.096 Uiso 1 1 calc R . .
V3 V 0.87037(2) 0.195644(19) 0.903674(15) 0.02352(8) Uani 1 1 d . B .
O7 O 0.76892(11) 0.26312(9) 0.93000(7) 0.0386(4) Uani 1 1 d . . .
O8 O 0.89135(11) 0.11498(8) 0.96149(6) 0.0339(3) Uani 1 1 d DU . .
C89 C 0.83113(18) 0.10376(14) 1.02190(10) 0.0326(6) Uani 0.920(5) 1 d PDU B 1
H89 H 0.7755 0.1559 1.0317 0.039 Uiso 0.920(5) 1 calc PR B 1
C90 C 0.8975(2) 0.08164(17) 1.06945(12) 0.0559(7) Uani 1 1 d DU . .
H90A H 0.9519 0.0304 1.0599 0.084 Uiso 0.920(5) 1 calc PR B 1
H90B H 0.8590 0.0750 1.1113 0.084 Uiso 0.920(5) 1 calc PR B 1
H90C H 0.9244 0.1253 1.0678 0.084 Uiso 0.920(5) 1 calc PR B 1
H90D H 0.9621 0.0882 1.0629 0.084 Uiso 0.080(5) 1 calc PR B 2
H90E H 0.8905 0.0430 1.1058 0.084 Uiso 0.080(5) 1 calc PR B 2
H90F H 0.8451 0.1346 1.0767 0.084 Uiso 0.080(5) 1 calc PR B 2
C91 C 0.7906(2) 0.03816(16) 1.01973(12) 0.0491(6) Uani 1 1 d DU . .
H91A H 0.7465 0.0561 0.9896 0.074 Uiso 0.920(5) 1 calc PR B 1
H91B H 0.7537 0.0272 1.0612 0.074 Uiso 0.920(5) 1 calc PR B 1
H91C H 0.8452 -0.0117 1.0070 0.074 Uiso 0.920(5) 1 calc PR B 1
H91D H 0.7866 0.0173 0.9823 0.074 Uiso 0.080(5) 1 calc PR B 2
H91E H 0.7379 0.0909 1.0267 0.074 Uiso 0.080(5) 1 calc PR B 2
H91F H 0.7831 -0.0007 1.0559 0.074 Uiso 0.080(5) 1 calc PR B 2
C89X C 0.8892(14) 0.0487(11) 1.0109(7) 0.031(4) Uani 0.080(5) 1 d PDU B 2
H89X H 0.9449 -0.0031 1.0001 0.037 Uiso 0.080(5) 1 calc PR B 2
V4 V 0.58513(2) 0.49662(2) 0.717154(15) 0.02678(8) Uani 1 1 d . C .
O9 O 0.66359(11) 0.51066(10) 0.74784(7) 0.0414(4) Uani 1 1 d . . .
O10 O 0.55926(11) 0.57158(9) 0.65596(7) 0.0404(4) Uani 1 1 d DU . .
C92 C 0.5977(2) 0.63899(16) 0.63089(14) 0.0409(8) Uani 0.868(7) 1 d PDU C 1
H92 H 0.6321 0.6477 0.6616 0.049 Uiso 0.868(7) 1 calc PR C 1
C93 C 0.6690(2) 0.6151(2) 0.57226(15) 0.0782(10) Uani 1 1 d DU . .
H93A H 0.7246 0.5665 0.5811 0.117 Uiso 0.868(7) 1 calc PR C 1
H93B H 0.6934 0.6600 0.5536 0.117 Uiso 0.868(7) 1 calc PR C 1
H93C H 0.6364 0.6030 0.5432 0.117 Uiso 0.868(7) 1 calc PR C 1
H93D H 0.7008 0.5590 0.5601 0.117 Uiso 0.132(7) 1 calc PR C 2
H93E H 0.7035 0.6242 0.6017 0.117 Uiso 0.132(7) 1 calc PR C 2
H93F H 0.6719 0.6534 0.5351 0.117 Uiso 0.132(7) 1 calc PR C 2
C94 C 0.5097(2) 0.71425(15) 0.62280(13) 0.0572(7) Uani 1 1 d DU . .
H94A H 0.4664 0.7271 0.6635 0.086 Uiso 0.868(7) 1 calc PR C 1
H94B H 0.4733 0.7044 0.5950 0.086 Uiso 0.868(7) 1 calc PR C 1
H94C H 0.5323 0.7602 0.6046 0.086 Uiso 0.868(7) 1 calc PR C 1
H94D H 0.4417 0.7179 0.6421 0.086 Uiso 0.132(7) 1 calc PR C 2
H94E H 0.5094 0.7545 0.5867 0.086 Uiso 0.132(7) 1 calc PR C 2
H94F H 0.5409 0.7252 0.6533 0.086 Uiso 0.132(7) 1 calc PR C 2
C92X C 0.5682(10) 0.6279(8) 0.6013(7) 0.037(4) Uani 0.132(7) 1 d PDU C 2
H92X H 0.5348 0.6182 0.5705 0.045 Uiso 0.132(7) 1 calc PR C 2
O11 O 0.85899(9) 0.16336(8) 0.83647(6) 0.0253(3) Uani 1 1 d . . .
O12 O 0.63420(9) 0.39929(8) 0.68979(6) 0.0272(3) Uani 1 1 d . . .
N3 N 0.3323(4) 0.3659(4) 0.5985(3) 0.200(3) Uani 1 1 d . . .
C95 C 0.3717(3) 0.3899(3) 0.6255(2) 0.0924(12) Uani 1 1 d . . .
C96 C 0.4190(2) 0.4196(2) 0.65660(15) 0.0727(9) Uani 1 1 d . . .
H96A H 0.4592 0.4476 0.6266 0.109 Uiso 1 1 calc R . .
H96B H 0.4618 0.3744 0.6800 0.109 Uiso 1 1 calc R . .
H96C H 0.3701 0.4582 0.6856 0.109 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 0.01831(14) 0.02037(15) 0.01773(15) -0.00386(12) -0.00157(11) -0.00934(12)
V2 0.01912(15) 0.02412(16) 0.01720(15) -0.00301(12) -0.00037(12) -0.01041(12)
O1 0.0307(7) 0.0259(7) 0.0287(7) -0.0020(6) -0.0093(6) -0.0158(6)
O2 0.0169(6) 0.0252(6) 0.0174(6) -0.0035(5) -0.0006(5) -0.0100(5)
O3 0.0236(6) 0.0318(7) 0.0183(6) -0.0052(5) -0.0005(5) -0.0142(6)
C1 0.0208(9) 0.0222(9) 0.0253(9) -0.0057(7) -0.0025(7) -0.0101(7)
C2 0.0210(9) 0.0268(10) 0.0254(10) -0.0066(8) -0.0045(7) -0.0086(7)
C3 0.0261(9) 0.0291(10) 0.0292(10) -0.0111(8) -0.0020(8) -0.0145(8)
C4 0.0300(10) 0.0263(10) 0.0289(10) -0.0085(8) 0.0026(8) -0.0149(8)
C5 0.0302(10) 0.0264(10) 0.0244(10) -0.0023(8) -0.0017(8) -0.0131(8)
C6 0.0213(9) 0.0285(10) 0.0236(9) -0.0058(8) -0.0016(7) -0.0117(8)
C7 0.0356(11) 0.0354(11) 0.0303(11) -0.0015(9) -0.0133(9) -0.0172(9)
C8 0.0504(14) 0.0482(14) 0.0432(13) 0.0020(11) -0.0239(11) -0.0261(12)
C9 0.0548(15) 0.0347(12) 0.0540(15) 0.0022(11) -0.0323(12) -0.0126(11)
C10 0.0546(14) 0.0567(15) 0.0264(11) 0.0037(10) -0.0127(10) -0.0351(12)
C11 0.0646(16) 0.0353(12) 0.0359(12) -0.0041(10) -0.0021(11) -0.0358(12)
C12 0.112(3) 0.0329(15) 0.091(2) 0.0039(15) -0.028(2) -0.0328(17)
C13 0.113(2) 0.0719(19) 0.0492(16) -0.0052(14) -0.0084(16) -0.076(2)
C14 0.121(3) 0.093(2) 0.0433(16) -0.0125(15) 0.0161(16) -0.088(2)
C15 0.0244(9) 0.0290(10) 0.0190(9) -0.0014(7) -0.0041(7) -0.0140(8)
C16 0.0162(8) 0.0319(10) 0.0183(9) -0.0020(7) -0.0008(7) -0.0101(7)
C17 0.0205(9) 0.0374(11) 0.0191(9) -0.0062(8) -0.0007(7) -0.0131(8)
C18 0.0267(11) 0.0694(16) 0.0367(12) -0.0178(11) -0.0025(9) -0.0231(11)
C19 0.0206(11) 0.096(2) 0.0466(14) -0.0350(14) 0.0043(10) -0.0204(12)
C20 0.0222(10) 0.0713(17) 0.0375(12) -0.0277(12) 0.0033(9) -0.0108(11)
C21 0.0224(9) 0.0370(11) 0.0237(10) -0.0081(8) -0.0027(8) -0.0092(8)
C22 0.0254(13) 0.181(4) 0.098(3) -0.090(3) 0.0175(15) -0.0378(19)
C23 0.0267(10) 0.0324(11) 0.0240(10) -0.0100(8) -0.0014(8) -0.0081(8)
C24 0.0262(9) 0.0340(11) 0.0194(9) -0.0088(8) 0.0018(7) -0.0162(8)
C25 0.0268(10) 0.0340(11) 0.0207(9) -0.0115(8) 0.0007(8) -0.0138(8)
C26 0.0321(11) 0.0439(12) 0.0244(10) -0.0148(9) 0.0023(8) -0.0148(9)
C27 0.0391(12) 0.0504(13) 0.0199(10) -0.0135(9) 0.0041(9) -0.0205(10)
C28 0.0451(13) 0.0476(13) 0.0173(9) -0.0051(9) -0.0016(9) -0.0244(11)
C29 0.0349(11) 0.0359(11) 0.0218(9) -0.0055(8) -0.0050(8) -0.0188(9)
C30 0.0489(14) 0.0726(18) 0.0239(11) -0.0125(11) 0.0099(10) -0.0221(13)
C31 0.0513(17) 0.135(3) 0.0439(16) -0.0121(18) 0.0160(13) -0.0488(19)
C32 0.076(2) 0.087(2) 0.0315(14) -0.0190(15) 0.0135(14) -0.0030(18)
C33 0.0595(17) 0.088(2) 0.0247(12) -0.0095(13) 0.0109(11) -0.0265(16)
C34 0.0389(12) 0.0455(13) 0.0247(10) 0.0039(9) -0.0095(9) -0.0226(10)
C35 0.0431(13) 0.0655(17) 0.0435(14) 0.0078(12) -0.0182(11) -0.0322(13)
C36 0.0513(15) 0.0663(17) 0.0325(13) 0.0047(12) -0.0175(11) -0.0224(13)
C37 0.0367(12) 0.0448(13) 0.0370(12) 0.0007(10) -0.0074(10) -0.0141(10)
O4 0.0267(7) 0.0271(7) 0.0263(7) -0.0028(6) 0.0021(6) -0.0108(6)
O5 0.0159(6) 0.0219(6) 0.0211(6) -0.0029(5) 0.0003(5) -0.0088(5)
O6 0.0200(6) 0.0206(6) 0.0204(6) -0.0049(5) -0.0020(5) -0.0097(5)
C38 0.0200(9) 0.0274(10) 0.0259(10) -0.0073(8) 0.0029(7) -0.0120(7)
C39 0.0245(9) 0.0245(10) 0.0325(11) -0.0062(8) 0.0005(8) -0.0118(8)
C40 0.0260(10) 0.0268(10) 0.0367(11) -0.0124(9) 0.0050(8) -0.0106(8)
C41 0.0251(9) 0.0313(10) 0.0265(10) -0.0087(8) 0.0016(8) -0.0124(8)
C42 0.0238(9) 0.0281(10) 0.0276(10) -0.0037(8) -0.0026(8) -0.0104(8)
C43 0.0203(9) 0.0261(10) 0.0273(10) -0.0075(8) -0.0024(7) -0.0094(7)
C44 0.0339(11) 0.0226(10) 0.0443(13) -0.0053(9) 0.0064(10) -0.0103(9)
C45 0.0672(18) 0.0236(12) 0.0616(18) -0.0025(11) 0.0216(14) -0.0039(12)
C46 0.0409(13) 0.0342(12) 0.0551(15) 0.0072(11) -0.0042(11) -0.0119(10)
C47 0.0537(15) 0.0371(13) 0.0543(15) -0.0083(11) 0.0041(12) -0.0299(12)
C48 0.0333(11) 0.0362(11) 0.0286(11) -0.0098(9) 0.0036(9) -0.0120(9)
C49 0.0342(16) 0.086(3) 0.0333(17) 0.0016(17) 0.0103(13) -0.0103(16)
C50 0.077(2) 0.067(2) 0.0315(16) -0.0144(15) -0.0051(16) -0.037(2)
C51 0.070(2) 0.0426(17) 0.0280(15) -0.0020(13) 0.0090(15) -0.0139(16)
C49X 0.106(15) 0.160(19) 0.088(14) -0.008(14) 0.003(12) -0.100(16)
C50X 0.130(18) 0.066(9) 0.036(9) -0.023(8) 0.021(10) 0.017(9)
C51X 0.058(8) 0.099(13) 0.021(6) 0.001(7) 0.005(6) -0.009(7)
C52 0.0208(9) 0.0244(9) 0.0251(9) -0.0050(7) -0.0005(7) -0.0089(7)
C53 0.0161(8) 0.0231(9) 0.0203(9) -0.0001(7) -0.0021(7) -0.0078(7)
C54 0.0203(9) 0.0209(9) 0.0206(9) -0.0014(7) -0.0025(7) -0.0071(7)
C55 0.0185(9) 0.0292(10) 0.0319(11) -0.0068(8) 0.0010(8) -0.0063(8)
C56 0.0175(9) 0.0365(11) 0.0425(12) -0.0079(9) -0.0031(8) -0.0103(8)
C57 0.0234(9) 0.0352(11) 0.0352(11) -0.0080(9) -0.0075(8) -0.0130(8)
C58 0.0196(8) 0.0249(9) 0.0222(9) -0.0020(7) -0.0047(7) -0.0072(7)
C59 0.0213(11) 0.0688(18) 0.083(2) -0.0361(15) 0.0008(11) -0.0179(11)
C60 0.0217(9) 0.0288(10) 0.0217(9) -0.0067(8) -0.0040(7) -0.0104(8)
C61 0.0228(9) 0.0230(9) 0.0174(8) -0.0072(7) 0.0027(7) -0.0125(7)
C62 0.0228(9) 0.0258(9) 0.0191(9) -0.0083(7) 0.0006(7) -0.0110(7)
C63 0.0254(9) 0.0351(11) 0.0266(10) -0.0115(8) 0.0005(8) -0.0154(8)
C64 0.0350(11) 0.0324(11) 0.0294(10) -0.0107(9) 0.0039(9) -0.0210(9)
C65 0.0389(11) 0.0258(10) 0.0230(10) -0.0050(8) 0.0011(8) -0.0176(9)
C66 0.0276(9) 0.0243(9) 0.0178(9) -0.0064(7) 0.0020(7) -0.0119(8)
C67 0.0326(10) 0.0248(10) 0.0253(10) -0.0018(8) -0.0061(8) -0.0084(8)
C68 0.0274(11) 0.0403(13) 0.0481(14) 0.0023(11) -0.0071(10) -0.0065(9)
C69 0.0545(14) 0.0282(11) 0.0394(13) -0.0004(9) -0.0174(11) -0.0091(10)
C70 0.0469(13) 0.0344(12) 0.0323(11) -0.0040(9) -0.0169(10) -0.0137(10)
C71 0.0439(13) 0.0413(13) 0.0456(13) -0.0092(10) -0.0008(10) -0.0306(11)
C72 0.114(3) 0.104(3) 0.0614(19) -0.0147(18) -0.0132(18) -0.088(2)
C73 0.073(2) 0.0472(18) 0.165(4) 0.006(2) -0.027(2) -0.0442(17)
C74 0.0649(18) 0.089(2) 0.0678(19) -0.0232(17) 0.0138(15) -0.0602(18)
N1 0.0216(7) 0.0224(8) 0.0211(8) -0.0024(6) -0.0015(6) -0.0089(6)
C75 0.0227(9) 0.0229(9) 0.0208(9) 0.0009(7) -0.0002(7) -0.0077(7)
C76 0.0327(11) 0.0423(12) 0.0265(10) -0.0029(9) -0.0004(8) -0.0211(9)
C77 0.0340(11) 0.0548(14) 0.0354(12) 0.0041(10) -0.0037(9) -0.0268(11)
C78 0.0235(10) 0.0485(13) 0.0281(11) 0.0084(9) -0.0002(8) -0.0114(9)
C79 0.0353(11) 0.0403(12) 0.0243(10) -0.0032(9) 0.0046(9) -0.0111(10)
C80 0.0358(11) 0.0321(11) 0.0241(10) -0.0023(8) 0.0005(8) -0.0156(9)
C81 0.0320(12) 0.0798(19) 0.0371(14) 0.0097(13) 0.0039(10) -0.0214(13)
N2 0.0258(8) 0.0300(9) 0.0189(8) -0.0014(6) -0.0012(6) -0.0142(7)
C82 0.0288(10) 0.0334(11) 0.0224(10) 0.0038(8) -0.0030(8) -0.0180(8)
C83 0.0369(11) 0.0345(11) 0.0317(11) -0.0010(9) 0.0015(9) -0.0206(9)
C84 0.0490(14) 0.0420(13) 0.0416(13) -0.0015(10) -0.0032(11) -0.0312(11)
C85 0.0404(13) 0.0545(15) 0.0419(13) 0.0086(11) -0.0045(10) -0.0327(12)
C86 0.0372(13) 0.0625(16) 0.0461(14) -0.0104(12) 0.0122(11) -0.0289(12)
C87 0.0375(12) 0.0483(14) 0.0356(12) -0.0095(10) 0.0065(10) -0.0241(11)
C88 0.0589(17) 0.082(2) 0.0675(19) 0.0031(16) -0.0004(14) -0.0546(16)
V3 0.02751(17) 0.02382(16) 0.02367(16) -0.00320(13) -0.00504(13) -0.01334(13)
O7 0.0349(8) 0.0343(8) 0.0456(9) -0.0112(7) -0.0006(7) -0.0117(7)
O8 0.0459(9) 0.0321(8) 0.0286(8) 0.0024(6) -0.0102(6) -0.0193(7)
C89 0.0464(14) 0.0265(13) 0.0238(11) -0.0017(9) -0.0050(10) -0.0123(11)
C90 0.086(2) 0.0538(16) 0.0354(13) 0.0030(12) -0.0248(14) -0.0273(15)
C91 0.0638(16) 0.0505(15) 0.0396(13) 0.0014(11) -0.0045(12) -0.0326(13)
C89X 0.044(10) 0.010(10) 0.035(9) 0.002(7) -0.008(10) -0.005(9)
V4 0.02549(17) 0.02657(17) 0.02665(18) -0.00286(14) 0.00198(13) -0.01109(14)
O9 0.0347(8) 0.0528(10) 0.0417(9) -0.0128(8) -0.0014(7) -0.0208(7)
O10 0.0436(9) 0.0332(8) 0.0366(9) 0.0042(7) 0.0000(7) -0.0117(7)
C92 0.0553(17) 0.0404(15) 0.0340(16) 0.0120(12) -0.0133(13) -0.0276(13)
C93 0.078(2) 0.067(2) 0.071(2) 0.0112(16) 0.0173(17) -0.0288(17)
C94 0.0770(19) 0.0371(14) 0.0592(17) 0.0042(12) -0.0185(15) -0.0216(13)
C92X 0.040(7) 0.046(7) 0.020(8) 0.006(6) -0.005(6) -0.010(7)
O11 0.0292(7) 0.0295(7) 0.0242(7) -0.0005(5) -0.0079(5) -0.0173(6)
O12 0.0259(7) 0.0266(7) 0.0246(7) -0.0020(5) 0.0022(5) -0.0083(6)
N3 0.204(5) 0.215(6) 0.245(7) 0.000(5) -0.144(5) -0.089(5)
C95 0.075(2) 0.104(3) 0.104(3) 0.017(2) -0.045(2) -0.032(2)
C96 0.0545(18) 0.097(3) 0.066(2) 0.0170(18) -0.0215(15) -0.0291(18)

_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 1.6625(15) . ?
V1 O6 1.7853(12) . ?
V1 O11 1.8456(13) . ?
V1 O5 1.8944(12) . ?
V1 O2 2.1547(12) . ?
V2 N2 1.6631(15) . ?
V2 O3 1.7924(12) . ?
V2 O12 1.8450(13) . ?
V2 O2 1.9015(12) . ?
V2 O5 2.1604(12) . ?
O1 C1 1.371(2) . ?
O1 V3 1.7850(13) . ?
O2 C16 1.382(2) . ?
O3 C24 1.380(2) . ?
C1 C6 1.395(3) . ?
C1 C2 1.410(2) . ?
C2 C3 1.396(3) . ?
C2 C7 1.538(3) . ?
C3 C4 1.376(3) . ?
C4 C5 1.390(3) . ?
C4 C11 1.532(3) . ?
C5 C6 1.384(3) . ?
C6 C15 1.502(2) . ?
C7 C10 1.531(3) . ?
C7 C9 1.534(3) . ?
C7 C8 1.535(3) . ?
C11 C13 1.518(3) . ?
C11 C14 1.526(3) . ?
C11 C12 1.534(4) . ?
C15 C17 1.515(2) . ?
C16 C21 1.391(3) . ?
C16 C17 1.397(2) . ?
C17 C18 1.384(3) . ?
C18 C19 1.388(3) . ?
C19 C20 1.378(3) . ?
C19 C22 1.511(3) . ?
C20 C21 1.397(3) . ?
C21 C23 1.517(3) . ?
C23 C25 1.510(3) . ?
C24 C25 1.399(3) . ?
C24 C29 1.405(3) . ?
C25 C26 1.391(3) . ?
C26 C27 1.380(3) . ?
C27 C28 1.391(3) . ?
C27 C30 1.535(3) . ?
C28 C29 1.393(3) . ?
C29 C34 1.532(3) . ?
C30 C32 1.530(4) . ?
C30 C31 1.537(4) . ?
C30 C33 1.541(4) . ?
C34 C37 1.537(3) . ?
C34 C36 1.539(3) . ?
C34 C35 1.540(3) . ?
O4 C38 1.366(2) . ?
O4 V4 1.7803(13) . ?
O5 C53 1.3866(19) . ?
O6 C61 1.379(2) . ?
C38 C43 1.396(3) . ?
C38 C39 1.408(3) . ?
C39 C40 1.392(3) . ?
C39 C44 1.534(3) . ?
C40 C41 1.395(3) . ?
C41 C42 1.391(3) . ?
C41 C48 1.535(3) . ?
C42 C43 1.387(3) . ?
C43 C52 1.503(2) . ?
C44 C46 1.529(3) . ?
C44 C47 1.538(3) . ?
C44 C45 1.539(3) . ?
C48 C50X 1.513(8) . ?
C48 C50 1.514(3) . ?
C48 C49X 1.517(7) . ?
C48 C51 1.522(3) . ?
C48 C49 1.540(3) . ?
C48 C51X 1.545(7) . ?
C52 C54 1.512(2) . ?
C53 C58 1.389(2) . ?
C53 C54 1.395(2) . ?
C54 C55 1.391(2) . ?
C55 C56 1.387(3) . ?
C56 C57 1.388(3) . ?
C56 C59 1.511(3) . ?
C57 C58 1.393(2) . ?
C58 C60 1.520(2) . ?
C60 C62 1.524(3) . ?
C61 C66 1.397(3) . ?
C61 C62 1.403(2) . ?
C62 C63 1.395(2) . ?
C63 C64 1.380(3) . ?
C64 C65 1.391(3) . ?
C64 C71 1.540(3) . ?
C65 C66 1.399(2) . ?
C66 C67 1.538(3) . ?
C67 C70 1.530(3) . ?
C67 C68 1.534(3) . ?
C67 C69 1.537(3) . ?
C71 C72 1.501(3) . ?
C71 C74 1.528(3) . ?
C71 C73 1.531(4) . ?
N1 C75 1.380(2) . ?
C75 C80 1.393(3) . ?
C75 C76 1.395(3) . ?
C76 C77 1.384(3) . ?
C77 C78 1.380(3) . ?
C78 C79 1.392(3) . ?
C78 C81 1.514(3) . ?
C79 C80 1.382(3) . ?
N2 C82 1.380(2) . ?
C82 C83 1.392(3) . ?
C82 C87 1.396(3) . ?
C83 C84 1.383(3) . ?
C84 C85 1.378(3) . ?
C85 C86 1.394(3) . ?
C85 C88 1.509(3) . ?
C86 C87 1.378(3) . ?
V3 O7 1.5869(15) . ?
V3 O11 1.7394(13) . ?
V3 O8 1.7446(14) . ?
O8 C89 1.449(3) . ?
O8 C89X 1.472(15) . ?
C89 C91 1.497(3) . ?
C89 C90 1.519(3) . ?
C90 C89X 1.550(16) . ?
C91 C89X 1.502(16) . ?
V4 O9 1.5855(15) . ?
V4 O10 1.7419(15) . ?
V4 O12 1.7490(13) . ?
O10 C92X 1.450(12) . ?
O10 C92 1.476(3) . ?
C92 C93 1.475(4) . ?
C92 C94 1.506(4) . ?
C93 C92X 1.428(13) . ?
C94 C92X 1.540(14) . ?
N3 C95 1.141(5) . ?
C95 C96 1.362(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 O6 101.08(6) . . ?
N1 V1 O11 100.30(7) . . ?
O6 V1 O11 112.82(6) . . ?
N1 V1 O5 95.27(6) . . ?
O6 V1 O5 103.29(5) . . ?
O11 V1 O5 136.67(6) . . ?
N1 V1 O2 158.47(6) . . ?
O6 V1 O2 97.25(5) . . ?
O11 V1 O2 82.69(5) . . ?
O5 V1 O2 69.39(5) . . ?
N2 V2 O3 101.35(7) . . ?
N2 V2 O12 99.99(7) . . ?
O3 V2 O12 113.62(6) . . ?
N2 V2 O2 94.82(7) . . ?
O3 V2 O2 104.74(6) . . ?
O12 V2 O2 134.81(6) . . ?
N2 V2 O5 158.26(6) . . ?
O3 V2 O5 97.04(5) . . ?
O12 V2 O5 82.93(5) . . ?
O2 V2 O5 69.15(5) . . ?
C1 O1 V3 143.12(12) . . ?
C16 O2 V2 120.36(11) . . ?
C16 O2 V1 127.86(11) . . ?
V2 O2 V1 110.36(5) . . ?
C24 O3 V2 126.57(11) . . ?
O1 C1 C6 118.34(15) . . ?
O1 C1 C2 120.60(16) . . ?
C6 C1 C2 121.02(16) . . ?
C3 C2 C1 116.59(17) . . ?
C3 C2 C7 121.46(16) . . ?
C1 C2 C7 121.93(16) . . ?
C4 C3 C2 124.06(17) . . ?
C3 C4 C5 117.18(17) . . ?
C3 C4 C11 123.00(18) . . ?
C5 C4 C11 119.82(19) . . ?
C6 C5 C4 122.06(18) . . ?
C5 C6 C1 119.09(17) . . ?
C5 C6 C15 120.08(17) . . ?
C1 C6 C15 120.84(16) . . ?
C10 C7 C9 110.28(19) . . ?
C10 C7 C8 107.55(18) . . ?
C9 C7 C8 107.24(18) . . ?
C10 C7 C2 109.25(17) . . ?
C9 C7 C2 110.98(17) . . ?
C8 C7 C2 111.47(17) . . ?
C13 C11 C14 109.5(2) . . ?
C13 C11 C4 112.30(19) . . ?
C14 C11 C4 109.21(19) . . ?
C13 C11 C12 107.7(2) . . ?
C14 C11 C12 109.4(2) . . ?
C4 C11 C12 108.7(2) . . ?
C6 C15 C17 114.55(15) . . ?
O2 C16 C21 118.52(16) . . ?
O2 C16 C17 118.84(15) . . ?
C21 C16 C17 122.53(16) . . ?
C18 C17 C16 117.70(17) . . ?
C18 C17 C15 123.01(17) . . ?
C16 C17 C15 119.06(15) . . ?
C17 C18 C19 121.9(2) . . ?
C20 C19 C18 118.38(19) . . ?
C20 C19 C22 120.8(2) . . ?
C18 C19 C22 120.8(2) . . ?
C19 C20 C21 122.5(2) . . ?
C16 C21 C20 116.89(18) . . ?
C16 C21 C23 121.83(16) . . ?
C20 C21 C23 121.15(17) . . ?
C25 C23 C21 112.52(17) . . ?
O3 C24 C25 117.72(16) . . ?
O3 C24 C29 120.26(17) . . ?
C25 C24 C29 122.02(17) . . ?
C26 C25 C24 117.99(18) . . ?
C26 C25 C23 118.61(18) . . ?
C24 C25 C23 123.40(16) . . ?
C27 C26 C25 122.4(2) . . ?
C26 C27 C28 117.23(18) . . ?
C26 C27 C30 119.2(2) . . ?
C28 C27 C30 123.6(2) . . ?
C27 C28 C29 123.8(2) . . ?
C28 C29 C24 116.10(19) . . ?
C28 C29 C34 121.19(18) . . ?
C24 C29 C34 122.70(17) . . ?
C32 C30 C27 109.8(2) . . ?
C32 C30 C31 110.2(3) . . ?
C27 C30 C31 108.03(19) . . ?
C32 C30 C33 109.2(2) . . ?
C27 C30 C33 111.9(2) . . ?
C31 C30 C33 107.7(2) . . ?
C29 C34 C37 111.53(17) . . ?
C29 C34 C36 111.88(18) . . ?
C37 C34 C36 106.67(19) . . ?
C29 C34 C35 109.84(18) . . ?
C37 C34 C35 109.77(18) . . ?
C36 C34 C35 107.01(18) . . ?
C38 O4 V4 142.31(12) . . ?
C53 O5 V1 119.78(10) . . ?
C53 O5 V2 128.75(10) . . ?
V1 O5 V2 110.40(5) . . ?
C61 O6 V1 128.53(10) . . ?
O4 C38 C43 117.83(16) . . ?
O4 C38 C39 120.99(17) . . ?
C43 C38 C39 121.17(17) . . ?
C40 C39 C38 116.52(18) . . ?
C40 C39 C44 122.09(17) . . ?
C38 C39 C44 121.32(17) . . ?
C39 C40 C41 124.15(18) . . ?
C42 C41 C40 116.93(18) . . ?
C42 C41 C48 121.63(18) . . ?
C40 C41 C48 121.39(17) . . ?
C43 C42 C41 121.74(18) . . ?
C42 C43 C38 119.45(17) . . ?
C42 C43 C52 119.90(17) . . ?
C38 C43 C52 120.61(16) . . ?
C46 C44 C39 112.71(17) . . ?
C46 C44 C47 109.98(19) . . ?
C39 C44 C47 108.88(18) . . ?
C46 C44 C45 106.9(2) . . ?
C39 C44 C45 111.41(18) . . ?
C47 C44 C45 106.80(19) . . ?
C50X C48 C49X 113.0(8) . . ?
C50 C48 C51 109.1(2) . . ?
C50X C48 C41 113.7(6) . . ?
C50 C48 C41 109.43(19) . . ?
C49X C48 C41 107.4(8) . . ?
C51 C48 C41 112.66(18) . . ?
C50 C48 C49 109.5(2) . . ?
C51 C48 C49 106.9(2) . . ?
C41 C48 C49 109.18(19) . . ?
C50X C48 C51X 108.1(8) . . ?
C49X C48 C51X 106.8(9) . . ?
C41 C48 C51X 107.4(5) . . ?
C49 C48 C51X 143.4(5) . . ?
C43 C52 C54 116.27(15) . . ?
O5 C53 C58 118.72(15) . . ?
O5 C53 C54 118.04(15) . . ?
C58 C53 C54 123.12(16) . . ?
C55 C54 C53 117.27(16) . . ?
C55 C54 C52 123.50(16) . . ?
C53 C54 C52 118.93(15) . . ?
C56 C55 C54 121.74(18) . . ?
C55 C56 C57 118.77(17) . . ?
C55 C56 C59 120.79(19) . . ?
C57 C56 C59 120.44(19) . . ?
C56 C57 C58 121.94(18) . . ?
C53 C58 C57 117.05(17) . . ?
C53 C58 C60 121.97(15) . . ?
C57 C58 C60 120.92(16) . . ?
C58 C60 C62 113.89(15) . . ?
O6 C61 C66 120.36(16) . . ?
O6 C61 C62 117.59(16) . . ?
C66 C61 C62 122.05(16) . . ?
C63 C62 C61 117.99(17) . . ?
C63 C62 C60 119.29(16) . . ?
C61 C62 C60 122.71(16) . . ?
C64 C63 C62 122.24(18) . . ?
C63 C64 C65 117.66(18) . . ?
C63 C64 C71 120.55(19) . . ?
C65 C64 C71 121.79(19) . . ?
C64 C65 C66 123.29(19) . . ?
C61 C66 C65 116.63(17) . . ?
C61 C66 C67 122.54(16) . . ?
C65 C66 C67 120.82(17) . . ?
C70 C67 C68 110.16(17) . . ?
C70 C67 C69 107.12(17) . . ?
C68 C67 C69 106.72(17) . . ?
C70 C67 C66 109.42(16) . . ?
C68 C67 C66 111.88(16) . . ?
C69 C67 C66 111.41(17) . . ?
C72 C71 C74 110.2(2) . . ?
C72 C71 C73 108.4(2) . . ?
C74 C71 C73 107.2(2) . . ?
C72 C71 C64 110.54(19) . . ?
C74 C71 C64 108.50(18) . . ?
C73 C71 C64 111.9(2) . . ?
C75 N1 V1 174.01(14) . . ?
N1 C75 C80 120.11(17) . . ?
N1 C75 C76 120.13(17) . . ?
C80 C75 C76 119.76(17) . . ?
C77 C76 C75 119.7(2) . . ?
C78 C77 C76 121.2(2) . . ?
C77 C78 C79 118.50(18) . . ?
C77 C78 C81 120.7(2) . . ?
C79 C78 C81 120.8(2) . . ?
C80 C79 C78 121.5(2) . . ?
C79 C80 C75 119.30(19) . . ?
C82 N2 V2 170.99(14) . . ?
N2 C82 C83 120.00(17) . . ?
N2 C82 C87 120.29(18) . . ?
C83 C82 C87 119.69(18) . . ?
C84 C83 C82 119.6(2) . . ?
C85 C84 C83 121.6(2) . . ?
C84 C85 C86 118.1(2) . . ?
C84 C85 C88 121.1(2) . . ?
C86 C85 C88 120.8(2) . . ?
C87 C86 C85 121.7(2) . . ?
C86 C87 C82 119.3(2) . . ?
O7 V3 O11 108.61(7) . . ?
O7 V3 O8 106.90(8) . . ?
O11 V3 O8 110.44(7) . . ?
O7 V3 O1 110.64(7) . . ?
O11 V3 O1 110.92(6) . . ?
O8 V3 O1 109.25(7) . . ?
C89 O8 V3 130.38(14) . . ?
C89X O8 V3 169.0(7) . . ?
O8 C89 C91 108.66(18) . . ?
O8 C89 C90 106.76(19) . . ?
C91 C89 C90 112.5(2) . . ?
O8 C89X C91 107.2(11) . . ?
O8 C89X C90 104.1(10) . . ?
C91 C89X C90 110.5(11) . . ?
O9 V4 O10 108.08(8) . . ?
O9 V4 O12 109.26(7) . . ?
O10 V4 O12 110.66(7) . . ?
O9 V4 O4 110.21(7) . . ?
O10 V4 O4 108.17(7) . . ?
O12 V4 O4 110.42(6) . . ?
C92X O10 V4 163.5(6) . . ?
C92 O10 V4 131.59(17) . . ?
C93 C92 O10 107.8(2) . . ?
C93 C92 C94 113.9(3) . . ?
O10 C92 C94 106.8(2) . . ?
C93 C92X O10 112.0(10) . . ?
C93 C92X C94 114.6(11) . . ?
O10 C92X C94 106.4(9) . . ?
V3 O11 V1 141.62(8) . . ?
V4 O12 V2 141.72(8) . . ?
N3 C95 C96 178.8(6) . . ?

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
N2 V2 O2 C16 -21.58(13) . . . . ?
O3 V2 O2 C16 81.50(12) . . . . ?
O12 V2 O2 C16 -130.80(12) . . . . ?
O5 V2 O2 C16 173.54(13) . . . . ?
N2 V2 O2 V1 170.98(7) . . . . ?
O3 V2 O2 V1 -85.94(6) . . . . ?
O12 V2 O2 V1 61.76(9) . . . . ?
O5 V2 O2 V1 6.10(5) . . . . ?
N1 V1 O2 C16 140.10(18) . . . . ?
O6 V1 O2 C16 -71.68(13) . . . . ?
O11 V1 O2 C16 40.52(13) . . . . ?
O5 V1 O2 C16 -173.20(14) . . . . ?
N1 V1 O2 V2 -53.65(18) . . . . ?
O6 V1 O2 V2 94.57(6) . . . . ?
O11 V1 O2 V2 -153.22(7) . . . . ?
O5 V1 O2 V2 -6.95(5) . . . . ?
N2 V2 O3 C24 17.32(16) . . . . ?
O12 V2 O3 C24 123.63(14) . . . . ?
O2 V2 O3 C24 -80.81(15) . . . . ?
O5 V2 O3 C24 -151.03(14) . . . . ?
V3 O1 C1 C6 -58.9(3) . . . . ?
V3 O1 C1 C2 123.49(19) . . . . ?
O1 C1 C2 C3 177.82(16) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
O1 C1 C2 C7 -3.9(3) . . . . ?
C6 C1 C2 C7 178.54(17) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C7 C2 C3 C4 -178.99(18) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C2 C3 C4 C11 -178.93(19) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C11 C4 C5 C6 179.44(19) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
C4 C5 C6 C15 -179.66(17) . . . . ?
O1 C1 C6 C5 -177.42(16) . . . . ?
C2 C1 C6 C5 0.2(3) . . . . ?
O1 C1 C6 C15 2.0(3) . . . . ?
C2 C1 C6 C15 179.60(16) . . . . ?
C3 C2 C7 C10 112.6(2) . . . . ?
C1 C2 C7 C10 -65.6(2) . . . . ?
C3 C2 C7 C9 -125.5(2) . . . . ?
C1 C2 C7 C9 56.3(2) . . . . ?
C3 C2 C7 C8 -6.1(3) . . . . ?
C1 C2 C7 C8 175.73(18) . . . . ?
C3 C4 C11 C13 -3.3(3) . . . . ?
C5 C4 C11 C13 177.1(2) . . . . ?
C3 C4 C11 C14 118.4(2) . . . . ?
C5 C4 C11 C14 -61.2(3) . . . . ?
C3 C4 C11 C12 -122.4(2) . . . . ?
C5 C4 C11 C12 58.0(3) . . . . ?
C5 C6 C15 C17 97.5(2) . . . . ?
C1 C6 C15 C17 -81.9(2) . . . . ?
V2 O2 C16 C21 -78.64(19) . . . . ?
V1 O2 C16 C21 86.40(19) . . . . ?
V2 O2 C16 C17 97.64(17) . . . . ?
V1 O2 C16 C17 -97.32(18) . . . . ?
O2 C16 C17 C18 -177.64(18) . . . . ?
C21 C16 C17 C18 -1.5(3) . . . . ?
O2 C16 C17 C15 -3.1(3) . . . . ?
C21 C16 C17 C15 173.06(18) . . . . ?
C6 C15 C17 C18 -23.0(3) . . . . ?
C6 C15 C17 C16 162.68(17) . . . . ?
C16 C17 C18 C19 -0.5(4) . . . . ?
C15 C17 C18 C19 -174.8(2) . . . . ?
C17 C18 C19 C20 1.0(4) . . . . ?
C17 C18 C19 C22 -179.9(3) . . . . ?
C18 C19 C20 C21 0.4(4) . . . . ?
C22 C19 C20 C21 -178.7(3) . . . . ?
O2 C16 C21 C20 178.95(19) . . . . ?
C17 C16 C21 C20 2.8(3) . . . . ?
O2 C16 C21 C23 3.1(3) . . . . ?
C17 C16 C21 C23 -172.99(18) . . . . ?
C19 C20 C21 C16 -2.2(4) . . . . ?
C19 C20 C21 C23 173.6(2) . . . . ?
C16 C21 C23 C25 95.1(2) . . . . ?
C20 C21 C23 C25 -80.6(3) . . . . ?
V2 O3 C24 C25 72.7(2) . . . . ?
V2 O3 C24 C29 -108.02(17) . . . . ?
O3 C24 C25 C26 -174.94(16) . . . . ?
C29 C24 C25 C26 5.8(3) . . . . ?
O3 C24 C25 C23 5.1(3) . . . . ?
C29 C24 C25 C23 -174.24(17) . . . . ?
C21 C23 C25 C26 82.1(2) . . . . ?
C21 C23 C25 C24 -97.9(2) . . . . ?
C24 C25 C26 C27 0.4(3) . . . . ?
C23 C25 C26 C27 -179.57(18) . . . . ?
C25 C26 C27 C28 -5.0(3) . . . . ?
C25 C26 C27 C30 174.5(2) . . . . ?
C26 C27 C28 C29 3.8(3) . . . . ?
C30 C27 C28 C29 -175.6(2) . . . . ?
C27 C28 C29 C24 1.9(3) . . . . ?
C27 C28 C29 C34 -176.79(19) . . . . ?
O3 C24 C29 C28 173.92(17) . . . . ?
C25 C24 C29 C28 -6.8(3) . . . . ?
O3 C24 C29 C34 -7.4(3) . . . . ?
C25 C24 C29 C34 171.87(18) . . . . ?
C26 C27 C30 C32 57.0(3) . . . . ?
C28 C27 C30 C32 -123.6(3) . . . . ?
C26 C27 C30 C31 -63.2(3) . . . . ?
C28 C27 C30 C31 116.2(3) . . . . ?
C26 C27 C30 C33 178.4(2) . . . . ?
C28 C27 C30 C33 -2.1(3) . . . . ?
C28 C29 C34 C37 -112.5(2) . . . . ?
C24 C29 C34 C37 68.9(2) . . . . ?
C28 C29 C34 C36 6.9(3) . . . . ?
C24 C29 C34 C36 -171.74(19) . . . . ?
C28 C29 C34 C35 125.6(2) . . . . ?
C24 C29 C34 C35 -53.1(3) . . . . ?
N1 V1 O5 C53 -20.27(13) . . . . ?
O6 V1 O5 C53 82.45(12) . . . . ?
O11 V1 O5 C53 -131.34(12) . . . . ?
O2 V1 O5 C53 175.29(13) . . . . ?
N1 V1 O5 V2 170.56(7) . . . . ?
O6 V1 O5 V2 -86.73(6) . . . . ?
O11 V1 O5 V2 59.48(10) . . . . ?
O2 V1 O5 V2 6.11(5) . . . . ?
N2 V2 O5 C53 140.56(19) . . . . ?
O3 V2 O5 C53 -71.75(14) . . . . ?
O12 V2 O5 C53 41.30(13) . . . . ?
O2 V2 O5 C53 -174.88(14) . . . . ?
N2 V2 O5 V1 -51.50(19) . . . . ?
O3 V2 O5 V1 96.19(7) . . . . ?
O12 V2 O5 V1 -150.77(7) . . . . ?
O2 V2 O5 V1 -6.94(5) . . . . ?
N1 V1 O6 C61 15.36(15) . . . . ?
O11 V1 O6 C61 121.63(14) . . . . ?
O5 V1 O6 C61 -82.83(14) . . . . ?
O2 V1 O6 C61 -153.29(14) . . . . ?
V4 O4 C38 C43 -65.7(3) . . . . ?
V4 O4 C38 C39 115.6(2) . . . . ?
O4 C38 C39 C40 176.99(17) . . . . ?
C43 C38 C39 C40 -1.7(3) . . . . ?
O4 C38 C39 C44 -6.1(3) . . . . ?
C43 C38 C39 C44 175.20(18) . . . . ?
C38 C39 C40 C41 0.1(3) . . . . ?
C44 C39 C40 C41 -176.76(19) . . . . ?
C39 C40 C41 C42 1.0(3) . . . . ?
C39 C40 C41 C48 178.53(18) . . . . ?
C40 C41 C42 C43 -0.6(3) . . . . ?
C48 C41 C42 C43 -178.09(17) . . . . ?
C41 C42 C43 C38 -0.9(3) . . . . ?
C41 C42 C43 C52 176.89(17) . . . . ?
O4 C38 C43 C42 -176.59(16) . . . . ?
C39 C38 C43 C42 2.1(3) . . . . ?
O4 C38 C43 C52 5.6(3) . . . . ?
C39 C38 C43 C52 -175.70(16) . . . . ?
C40 C39 C44 C46 -128.4(2) . . . . ?
C38 C39 C44 C46 54.9(2) . . . . ?
C40 C39 C44 C47 109.3(2) . . . . ?
C38 C39 C44 C47 -67.4(2) . . . . ?
C40 C39 C44 C45 -8.3(3) . . . . ?
C38 C39 C44 C45 175.0(2) . . . . ?
C42 C41 C48 C50X 167.5(9) . . . . ?
C40 C41 C48 C50X -9.9(9) . . . . ?
C42 C41 C48 C50 109.4(2) . . . . ?
C40 C41 C48 C50 -68.0(3) . . . . ?
C42 C41 C48 C49X -66.6(9) . . . . ?
C40 C41 C48 C49X 115.9(9) . . . . ?
C42 C41 C48 C51 -12.2(3) . . . . ?
C40 C41 C48 C51 170.4(2) . . . . ?
C42 C41 C48 C49 -130.8(2) . . . . ?
C40 C41 C48 C49 51.8(3) . . . . ?
C42 C41 C48 C51X 47.9(7) . . . . ?
C40 C41 C48 C51X -129.5(7) . . . . ?
C42 C43 C52 C54 98.3(2) . . . . ?
C38 C43 C52 C54 -83.9(2) . . . . ?
V1 O5 C53 C58 -79.45(18) . . . . ?
V2 O5 C53 C58 87.51(19) . . . . ?
V1 O5 C53 C54 96.83(17) . . . . ?
V2 O5 C53 C54 -96.22(17) . . . . ?
O5 C53 C54 C55 -179.05(16) . . . . ?
C58 C53 C54 C55 -2.9(3) . . . . ?
O5 C53 C54 C52 -5.0(2) . . . . ?
C58 C53 C54 C52 171.08(17) . . . . ?
C43 C52 C54 C55 -22.4(3) . . . . ?
C43 C52 C54 C53 164.00(17) . . . . ?
C53 C54 C55 C56 0.1(3) . . . . ?
C52 C54 C55 C56 -173.63(19) . . . . ?
C54 C55 C56 C57 1.6(3) . . . . ?
C54 C55 C56 C59 -178.2(2) . . . . ?
C55 C56 C57 C58 -0.7(3) . . . . ?
C59 C56 C57 C58 179.1(2) . . . . ?
O5 C53 C58 C57 179.90(16) . . . . ?
C54 C53 C58 C57 3.8(3) . . . . ?
O5 C53 C58 C60 2.6(3) . . . . ?
C54 C53 C58 C60 -173.50(17) . . . . ?
C56 C57 C58 C53 -1.9(3) . . . . ?
C56 C57 C58 C60 175.43(19) . . . . ?
C53 C58 C60 C62 95.3(2) . . . . ?
C57 C58 C60 C62 -82.0(2) . . . . ?
V1 O6 C61 C66 -106.50(17) . . . . ?
V1 O6 C61 C62 74.22(19) . . . . ?
O6 C61 C62 C63 -177.38(15) . . . . ?
C66 C61 C62 C63 3.4(3) . . . . ?
O6 C61 C62 C60 3.9(2) . . . . ?
C66 C61 C62 C60 -175.37(16) . . . . ?
C58 C60 C62 C63 86.2(2) . . . . ?
C58 C60 C62 C61 -95.1(2) . . . . ?
C61 C62 C63 C64 0.1(3) . . . . ?
C60 C62 C63 C64 178.86(17) . . . . ?
C62 C63 C64 C65 -2.7(3) . . . . ?
C62 C63 C64 C71 176.16(18) . . . . ?
C63 C64 C65 C66 2.1(3) . . . . ?
C71 C64 C65 C66 -176.77(18) . . . . ?
O6 C61 C66 C65 176.86(15) . . . . ?
C62 C61 C66 C65 -3.9(2) . . . . ?
O6 C61 C66 C67 -1.6(2) . . . . ?
C62 C61 C66 C67 177.61(16) . . . . ?
C64 C65 C66 C61 1.1(3) . . . . ?
C64 C65 C66 C67 179.64(17) . . . . ?
C61 C66 C67 C70 71.9(2) . . . . ?
C65 C66 C67 C70 -106.5(2) . . . . ?
C61 C66 C67 C68 -50.4(2) . . . . ?
C65 C66 C67 C68 131.13(19) . . . . ?
C61 C66 C67 C69 -169.81(17) . . . . ?
C65 C66 C67 C69 11.8(2) . . . . ?
C63 C64 C71 C72 49.7(3) . . . . ?
C65 C64 C71 C72 -131.5(2) . . . . ?
C63 C64 C71 C74 -71.3(3) . . . . ?
C65 C64 C71 C74 107.5(2) . . . . ?
C63 C64 C71 C73 170.6(2) . . . . ?
C65 C64 C71 C73 -10.6(3) . . . . ?
N1 C75 C76 C77 -178.82(19) . . . . ?
C80 C75 C76 C77 0.6(3) . . . . ?
C75 C76 C77 C78 -0.1(3) . . . . ?
C76 C77 C78 C79 -0.1(3) . . . . ?
C76 C77 C78 C81 -179.9(2) . . . . ?
C77 C78 C79 C80 -0.2(3) . . . . ?
C81 C78 C79 C80 179.5(2) . . . . ?
C78 C79 C80 C75 0.8(3) . . . . ?
N1 C75 C80 C79 178.48(18) . . . . ?
C76 C75 C80 C79 -0.9(3) . . . . ?
N2 C82 C83 C84 177.84(19) . . . . ?
C87 C82 C83 C84 -0.5(3) . . . . ?
C82 C83 C84 C85 -0.4(3) . . . . ?
C83 C84 C85 C86 0.6(4) . . . . ?
C83 C84 C85 C88 -179.1(2) . . . . ?
C84 C85 C86 C87 0.2(4) . . . . ?
C88 C85 C86 C87 179.9(2) . . . . ?
C85 C86 C87 C82 -1.1(4) . . . . ?
N2 C82 C87 C86 -177.1(2) . . . . ?
C83 C82 C87 C86 1.3(3) . . . . ?
C1 O1 V3 O7 -25.0(2) . . . . ?
C1 O1 V3 O11 95.6(2) . . . . ?
C1 O1 V3 O8 -142.47(19) . . . . ?
O7 V3 O8 C89 2.65(18) . . . . ?
O11 V3 O8 C89 -115.33(16) . . . . ?
O1 V3 O8 C89 122.41(16) . . . . ?
O7 V3 O8 C89X 47(4) . . . . ?
O11 V3 O8 C89X -71(4) . . . . ?
O1 V3 O8 C89X 167(4) . . . . ?
C89X O8 C89 C91 -59.2(9) . . . . ?
V3 O8 C89 C91 109.4(2) . . . . ?
C89X O8 C89 C90 62.5(9) . . . . ?
V3 O8 C89 C90 -128.95(18) . . . . ?
O8 C89 C90 C89X -61.5(9) . . . . ?
C91 C89 C90 C89X 57.6(9) . . . . ?
O8 C89 C91 C89X 59.4(9) . . . . ?
C90 C89 C91 C89X -58.7(9) . . . . ?
C89 O8 C89X C91 58.1(9) . . . . ?
V3 O8 C89X C91 6(5) . . . . ?
C89 O8 C89X C90 -59.1(9) . . . . ?
V3 O8 C89X C90 -111(3) . . . . ?
C89 C91 C89X O8 -57.1(9) . . . . ?
C89 C91 C89X C90 55.7(9) . . . . ?
C89 C90 C89X O8 58.7(8) . . . . ?
C89 C90 C89X C91 -56.1(9) . . . . ?
C38 O4 V4 O9 -23.3(2) . . . . ?
C38 O4 V4 O10 -141.22(19) . . . . ?
C38 O4 V4 O12 97.5(2) . . . . ?
O9 V4 O10 C92X 44(2) . . . . ?
O12 V4 O10 C92X -76(2) . . . . ?
O4 V4 O10 C92X 163(2) . . . . ?
O9 V4 O10 C92 0.8(2) . . . . ?
O12 V4 O10 C92 -118.8(2) . . . . ?
O4 V4 O10 C92 120.1(2) . . . . ?
C92X O10 C92 C93 -57.7(8) . . . . ?
V4 O10 C92 C93 103.8(3) . . . . ?
C92X O10 C92 C94 65.1(8) . . . . ?
V4 O10 C92 C94 -133.4(2) . . . . ?
O10 C92 C93 C92X 58.6(8) . . . . ?
C94 C92 C93 C92X -59.8(8) . . . . ?
C93 C92 C94 C92X 56.7(8) . . . . ?
O10 C92 C94 C92X -62.2(8) . . . . ?
C92 C93 C92X O10 -63.1(10) . . . . ?
C92 C93 C92X C94 58.2(10) . . . . ?
C92 O10 C92X C93 63.7(11) . . . . ?
V4 O10 C92X C93 7(3) . . . . ?
C92 O10 C92X C94 -62.2(9) . . . . ?
V4 O10 C92X C94 -119.1(18) . . . . ?
C92 C94 C92X C93 -60.3(11) . . . . ?
C92 C94 C92X O10 64.0(9) . . . . ?
O7 V3 O11 V1 -13.11(14) . . . . ?
O8 V3 O11 V1 103.81(13) . . . . ?
O1 V3 O11 V1 -134.92(11) . . . . ?
N1 V1 O11 V3 -44.79(13) . . . . ?
O6 V1 O11 V3 -151.55(11) . . . . ?
O5 V1 O11 V3 64.40(15) . . . . ?
O2 V1 O11 V3 113.63(12) . . . . ?
O9 V4 O12 V2 -11.85(15) . . . . ?
O10 V4 O12 V2 107.04(13) . . . . ?
O4 V4 O12 V2 -133.22(12) . . . . ?
N2 V2 O12 V4 -44.19(14) . . . . ?
O3 V2 O12 V4 -151.35(11) . . . . ?
O2 V2 O12 V4 62.99(15) . . . . ?
O5 V2 O12 V4 114.02(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.055

#==END