# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_3-mepy
_database_code_depnum_ccdc_archive 'CCDC 615632'
#TrackingRef 'structures.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(1,3-diphenylpropane-1,3-dionato)(3-methylpyridine)oxovanadium(IV)
;
_chemical_name_common            
;bis(1,3-diphenylpropane-1,3-dionato)(3-
methylpyridine)oxovanadium(IV)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H29 N O5 V'
_chemical_formula_sum            'C36 H29 N O5 V'
_chemical_formula_weight         606.54

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/a'
_symmetry_space_group_name_Hall  '-P 2yab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   10.8327(11)
_cell_length_b                   20.919(3)
_cell_length_c                   13.3107(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.117(9)
_cell_angle_gamma                90.00
_cell_volume                     2925.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1260
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur3 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26116
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.81
_diffrn_reflns_theta_max         27.08
_reflns_number_total             6384
_reflns_number_gt                5371
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
Oxford Diffraction (2003). CrysAlis CCD. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_cell_refinement       
;
Oxford Diffraction (2003). CrysAlis RED. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_data_reduction        
;
Oxford Diffraction (2003). CrysAlis RED. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0218P)^2^+3.2076P] 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         6384
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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
V V 0.64619(4) 0.470989(19) 0.17239(3) 0.01453(10) Uani 1 1 d . . .
O1 O 0.54437(15) 0.43081(8) 0.08912(13) 0.0198(4) Uani 1 1 d . . .
O2 O 0.58638(15) 0.44631(8) 0.29712(12) 0.0169(3) Uani 1 1 d . . .
O3 O 0.55468(15) 0.55370(8) 0.17303(12) 0.0167(3) Uani 1 1 d . . .
O4 O 0.79552(14) 0.52450(7) 0.27396(12) 0.0165(3) Uani 1 1 d . . .
O5 O 0.77784(14) 0.40136(7) 0.20456(12) 0.0164(3) Uani 1 1 d . . .
N N 0.73494(18) 0.50828(9) 0.05608(15) 0.0172(4) Uani 1 1 d . . .
C1 C 0.9109(2) 0.51050(11) 0.31188(17) 0.0142(5) Uani 1 1 d . . .
C2 C 0.9656(2) 0.45050(11) 0.30201(17) 0.0156(5) Uani 1 1 d . . .
H2 H 1.0516 0.4446 0.3330 0.019 Uiso 1 1 calc R . .
C3 C 0.8972(2) 0.39969(11) 0.24814(17) 0.0144(5) Uani 1 1 d . . .
C4 C 0.9631(2) 0.33875(11) 0.23363(18) 0.0160(5) Uani 1 1 d . . .
C5 C 1.0826(2) 0.32223(12) 0.2944(2) 0.0228(5) Uani 1 1 d . . .
H5 H 1.1233 0.3487 0.3485 0.027 Uiso 1 1 calc R . .
C6 C 1.1413(3) 0.26614(12) 0.2743(2) 0.0264(6) Uani 1 1 d . . .
H6 H 1.2213 0.2555 0.3151 0.032 Uiso 1 1 calc R . .
C7 C 1.0821(2) 0.22613(12) 0.1946(2) 0.0246(6) Uani 1 1 d . . .
H7 H 1.1215 0.1886 0.1819 0.029 Uiso 1 1 calc R . .
C8 C 0.9636(2) 0.24239(12) 0.1338(2) 0.0256(6) Uani 1 1 d . . .
H8 H 0.9236 0.2159 0.0795 0.031 Uiso 1 1 calc R . .
C9 C 0.9046(2) 0.29783(12) 0.1535(2) 0.0215(5) Uani 1 1 d . . .
H9 H 0.8244 0.3080 0.1127 0.026 Uiso 1 1 calc R . .
C10 C 0.9938(2) 0.56285(11) 0.36782(17) 0.0145(5) Uani 1 1 d . . .
C11 C 1.1015(2) 0.55092(11) 0.44785(18) 0.0164(5) Uani 1 1 d . . .
H11 H 1.1218 0.5091 0.4695 0.020 Uiso 1 1 calc R . .
C12 C 1.1784(2) 0.60072(12) 0.49526(19) 0.0200(5) Uani 1 1 d . . .
H12 H 1.2492 0.5924 0.5492 0.024 Uiso 1 1 calc R . .
C13 C 1.1494(2) 0.66287(12) 0.46211(19) 0.0220(5) Uani 1 1 d . . .
H13 H 1.2019 0.6962 0.4929 0.026 Uiso 1 1 calc R . .
C14 C 1.0422(2) 0.67557(12) 0.3831(2) 0.0239(6) Uani 1 1 d . . .
H14 H 1.0230 0.7173 0.3608 0.029 Uiso 1 1 calc R . .
C15 C 0.9640(2) 0.62574(11) 0.33759(19) 0.0191(5) Uani 1 1 d . . .
H15 H 0.8907 0.6345 0.2863 0.023 Uiso 1 1 calc R . .
C16 C 0.4862(2) 0.46725(11) 0.32145(17) 0.0148(5) Uani 1 1 d . . .
C17 C 0.4243(2) 0.52412(11) 0.28446(18) 0.0164(5) Uani 1 1 d . . .
H17 H 0.3507 0.5346 0.3050 0.020 Uiso 1 1 calc R . .
C18 C 0.4665(2) 0.56625(11) 0.21839(17) 0.0149(5) Uani 1 1 d . . .
C19 C 0.4073(2) 0.63092(11) 0.19647(18) 0.0155(5) Uani 1 1 d . . .
C20 C 0.3416(2) 0.66013(11) 0.26199(19) 0.0206(5) Uani 1 1 d . . .
H20 H 0.3350 0.6395 0.3224 0.025 Uiso 1 1 calc R . .
C21 C 0.2863(2) 0.71945(12) 0.2378(2) 0.0247(6) Uani 1 1 d . . .
H21 H 0.2422 0.7384 0.2819 0.030 Uiso 1 1 calc R . .
C22 C 0.2958(3) 0.75087(12) 0.1488(2) 0.0265(6) Uani 1 1 d . . .
H22 H 0.2574 0.7905 0.1323 0.032 Uiso 1 1 calc R . .
C23 C 0.3630(3) 0.72279(12) 0.0840(2) 0.0244(6) Uani 1 1 d . . .
H23 H 0.3713 0.7442 0.0248 0.029 Uiso 1 1 calc R . .
C24 C 0.4180(2) 0.66321(11) 0.10706(18) 0.0190(5) Uani 1 1 d . . .
H24 H 0.4621 0.6446 0.0629 0.023 Uiso 1 1 calc R . .
C25 C 0.4387(2) 0.42599(11) 0.39516(17) 0.0148(5) Uani 1 1 d . . .
C26 C 0.3665(2) 0.44926(12) 0.46057(18) 0.0173(5) Uani 1 1 d . . .
H26 H 0.3444 0.4923 0.4577 0.021 Uiso 1 1 calc R . .
C27 C 0.3272(2) 0.40943(12) 0.52968(18) 0.0203(5) Uani 1 1 d . . .
H27 H 0.2796 0.4256 0.5734 0.024 Uiso 1 1 calc R . .
C28 C 0.3594(2) 0.34494(12) 0.53327(19) 0.0230(6) Uani 1 1 d . . .
H28 H 0.3324 0.3178 0.5789 0.028 Uiso 1 1 calc R . .
C29 C 0.4315(2) 0.32113(12) 0.4689(2) 0.0233(6) Uani 1 1 d . . .
H29 H 0.4531 0.2780 0.4715 0.028 Uiso 1 1 calc R . .
C30 C 0.4715(2) 0.36142(11) 0.40087(19) 0.0193(5) Uani 1 1 d . . .
H30 H 0.5207 0.3453 0.3584 0.023 Uiso 1 1 calc R . .
C31 C 0.7918(2) 0.46757(12) 0.00381(18) 0.0184(5) Uani 1 1 d . . .
H31 H 0.7949 0.4245 0.0218 0.022 Uiso 1 1 calc R . .
C32 C 0.8465(2) 0.48634(12) -0.07583(18) 0.0211(5) Uani 1 1 d . . .
C33 C 0.8396(2) 0.55062(13) -0.1016(2) 0.0255(6) Uani 1 1 d . . .
H33 H 0.8746 0.5652 -0.1546 0.031 Uiso 1 1 calc R . .
C34 C 0.7815(2) 0.59281(13) -0.0492(2) 0.0257(6) Uani 1 1 d . . .
H34 H 0.7767 0.6360 -0.0662 0.031 Uiso 1 1 calc R . .
C35 C 0.7298(2) 0.57022(12) 0.02956(19) 0.0215(5) Uani 1 1 d . . .
H35 H 0.6904 0.5989 0.0651 0.026 Uiso 1 1 calc R . .
C36 C 0.9089(2) 0.43826(13) -0.1305(2) 0.0264(6) Uani 1 1 d . . .
H36A H 0.8650 0.4368 -0.2025 0.040 Uiso 1 1 calc R . .
H36C H 0.9058 0.3969 -0.1001 0.040 Uiso 1 1 calc R . .
H36B H 0.9960 0.4502 -0.1242 0.040 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
V 0.01256(19) 0.0154(2) 0.0160(2) 0.00001(17) 0.00426(14) 0.00004(15)
O1 0.0164(8) 0.0216(9) 0.0217(9) -0.0009(7) 0.0053(7) -0.0018(7)
O2 0.0144(8) 0.0185(8) 0.0194(8) 0.0033(7) 0.0069(7) 0.0040(6)
O3 0.0158(8) 0.0174(8) 0.0180(8) 0.0021(7) 0.0065(7) 0.0020(6)
O4 0.0142(8) 0.0161(8) 0.0188(8) -0.0015(7) 0.0034(6) 0.0009(6)
O5 0.0130(8) 0.0154(8) 0.0210(9) -0.0018(7) 0.0046(7) 0.0001(6)
N 0.0127(9) 0.0218(11) 0.0170(10) -0.0018(8) 0.0031(8) -0.0012(8)
C1 0.0162(11) 0.0162(12) 0.0118(11) 0.0010(9) 0.0063(9) -0.0009(9)
C2 0.0126(11) 0.0169(12) 0.0170(12) -0.0016(9) 0.0030(9) 0.0015(9)
C3 0.0148(11) 0.0160(12) 0.0145(11) 0.0013(9) 0.0078(9) -0.0007(9)
C4 0.0159(11) 0.0144(12) 0.0202(12) 0.0010(9) 0.0088(9) -0.0002(9)
C5 0.0242(13) 0.0161(12) 0.0258(14) 0.0009(10) 0.0017(10) 0.0024(10)
C6 0.0231(13) 0.0214(14) 0.0332(15) 0.0034(12) 0.0039(11) 0.0070(10)
C7 0.0284(14) 0.0151(12) 0.0350(15) 0.0013(11) 0.0170(12) 0.0037(10)
C8 0.0265(14) 0.0188(13) 0.0334(15) -0.0083(11) 0.0109(12) 0.0003(10)
C9 0.0162(12) 0.0198(13) 0.0290(14) -0.0050(11) 0.0067(10) 0.0000(10)
C10 0.0157(11) 0.0153(12) 0.0150(11) -0.0016(9) 0.0084(9) -0.0006(9)
C11 0.0167(11) 0.0161(11) 0.0185(12) 0.0025(10) 0.0081(9) 0.0028(9)
C12 0.0163(12) 0.0254(13) 0.0181(12) -0.0037(10) 0.0034(10) 0.0009(10)
C13 0.0201(13) 0.0193(13) 0.0268(14) -0.0087(11) 0.0058(10) -0.0037(10)
C14 0.0266(14) 0.0138(12) 0.0302(14) -0.0023(11) 0.0048(11) 0.0013(10)
C15 0.0195(12) 0.0169(12) 0.0198(12) -0.0013(10) 0.0025(10) 0.0022(9)
C16 0.0130(11) 0.0161(12) 0.0142(11) -0.0014(9) 0.0015(9) -0.0011(9)
C17 0.0129(11) 0.0183(12) 0.0194(12) 0.0022(10) 0.0064(9) 0.0023(9)
C18 0.0118(11) 0.0163(12) 0.0152(11) -0.0020(9) 0.0007(9) -0.0003(9)
C19 0.0128(11) 0.0137(11) 0.0189(12) -0.0020(9) 0.0016(9) -0.0015(9)
C20 0.0241(13) 0.0177(12) 0.0207(13) 0.0010(10) 0.0067(10) 0.0016(10)
C21 0.0274(14) 0.0199(13) 0.0273(14) -0.0041(11) 0.0079(11) 0.0047(10)
C22 0.0311(15) 0.0154(13) 0.0292(14) -0.0002(11) 0.0000(11) 0.0067(11)
C23 0.0336(15) 0.0184(13) 0.0195(13) 0.0039(10) 0.0034(11) 0.0010(11)
C24 0.0207(13) 0.0177(12) 0.0189(12) 0.0003(10) 0.0054(10) 0.0021(10)
C25 0.0147(11) 0.0158(11) 0.0132(11) -0.0001(9) 0.0020(9) -0.0015(9)
C26 0.0160(11) 0.0172(12) 0.0186(12) -0.0002(10) 0.0042(9) 0.0002(9)
C27 0.0172(12) 0.0273(14) 0.0181(12) -0.0008(10) 0.0073(10) -0.0005(10)
C28 0.0243(13) 0.0244(13) 0.0216(13) 0.0076(11) 0.0081(11) -0.0031(10)
C29 0.0249(13) 0.0158(12) 0.0301(14) 0.0043(11) 0.0085(11) 0.0027(10)
C30 0.0199(12) 0.0190(12) 0.0208(12) 0.0000(10) 0.0082(10) 0.0014(10)
C31 0.0144(11) 0.0224(13) 0.0186(12) -0.0028(10) 0.0043(9) -0.0021(10)
C32 0.0145(11) 0.0315(15) 0.0171(12) -0.0062(11) 0.0033(9) -0.0039(10)
C33 0.0234(13) 0.0332(15) 0.0213(13) 0.0053(11) 0.0081(11) -0.0062(11)
C34 0.0236(14) 0.0237(14) 0.0308(15) 0.0068(11) 0.0087(11) -0.0004(11)
C35 0.0181(12) 0.0212(13) 0.0253(13) 0.0006(11) 0.0056(10) -0.0016(10)
C36 0.0240(14) 0.0316(15) 0.0255(14) -0.0038(12) 0.0099(11) -0.0010(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
V O1 1.5985(16) . ?
V O2 1.9919(16) . ?
V O3 1.9952(16) . ?
V O5 2.0102(16) . ?
V O4 2.1519(16) . ?
V N 2.158(2) . ?
O2 C16 1.283(3) . ?
O3 C18 1.275(3) . ?
O4 C1 1.262(3) . ?
O5 C3 1.282(3) . ?
N C31 1.341(3) . ?
N C35 1.341(3) . ?
C16 C17 1.395(3) . ?
C16 C25 1.490(3) . ?
C11 C12 1.386(3) . ?
C11 C10 1.397(3) . ?
C11 H11 0.9300 . ?
C10 C15 1.391(3) . ?
C10 C1 1.495(3) . ?
C3 C2 1.391(3) . ?
C3 C4 1.497(3) . ?
C17 C18 1.398(3) . ?
C17 H17 0.9300 . ?
C19 C20 1.394(3) . ?
C19 C24 1.397(3) . ?
C19 C18 1.495(3) . ?
C4 C9 1.393(3) . ?
C4 C5 1.392(3) . ?
C25 C26 1.392(3) . ?
C25 C30 1.394(3) . ?
C9 C8 1.380(3) . ?
C9 H9 0.9300 . ?
C1 C2 1.408(3) . ?
C26 C27 1.383(3) . ?
C26 H26 0.9300 . ?
C31 C32 1.391(3) . ?
C31 H31 0.9300 . ?
C15 C14 1.387(3) . ?
C15 H15 0.9300 . ?
C30 C29 1.381(3) . ?
C30 H30 0.9300 . ?
C24 C23 1.383(3) . ?
C24 H24 0.9300 . ?
C2 H2 0.9300 . ?
C12 C13 1.384(3) . ?
C12 H12 0.9300 . ?
C27 C28 1.391(4) . ?
C27 H27 0.9300 . ?
C7 C6 1.381(4) . ?
C7 C8 1.382(4) . ?
C7 H7 0.9300 . ?
C13 C14 1.389(3) . ?
C13 H13 0.9300 . ?
C32 C33 1.385(4) . ?
C32 C36 1.496(3) . ?
C20 C21 1.382(3) . ?
C20 H20 0.9300 . ?
C5 C6 1.391(3) . ?
C5 H5 0.9300 . ?
C8 H8 0.9300 . ?
C28 C29 1.386(4) . ?
C28 H28 0.9300 . ?
C34 C33 1.370(4) . ?
C34 C35 1.386(3) . ?
C34 H34 0.9300 . ?
C22 C21 1.381(4) . ?
C22 C23 1.387(4) . ?
C22 H22 0.9300 . ?
C21 H21 0.9300 . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36C 0.9600 . ?
C36 H36B 0.9600 . ?
C35 H35 0.9300 . ?
C6 H6 0.9300 . ?
C23 H23 0.9300 . ?
C33 H33 0.9300 . ?

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 V O2 97.58(8) . . ?
O1 V O3 101.51(8) . . ?
O2 V O3 87.60(7) . . ?
O1 V O5 95.76(8) . . ?
O2 V O5 89.59(7) . . ?
O3 V O5 162.73(7) . . ?
O1 V O4 174.26(8) . . ?
O2 V O4 87.63(6) . . ?
O3 V O4 81.05(6) . . ?
O5 V O4 81.81(6) . . ?
O1 V N 92.61(8) . . ?
O2 V N 169.80(7) . . ?
O3 V N 89.90(7) . . ?
O5 V N 89.87(7) . . ?
O4 V N 82.21(7) . . ?
C16 O2 V 126.09(14) . . ?
C18 O3 V 127.64(15) . . ?
C1 O4 V 130.50(15) . . ?
C3 O5 V 134.50(15) . . ?
C31 N C35 118.2(2) . . ?
C31 N V 118.96(16) . . ?
C35 N V 122.77(16) . . ?
O2 C16 C17 124.4(2) . . ?
O2 C16 C25 114.7(2) . . ?
C17 C16 C25 120.9(2) . . ?
C12 C11 C10 120.7(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C15 C10 C11 118.8(2) . . ?
C15 C10 C1 118.7(2) . . ?
C11 C10 C1 122.5(2) . . ?
O5 C3 C2 124.4(2) . . ?
O5 C3 C4 115.2(2) . . ?
C2 C3 C4 120.4(2) . . ?
C16 C17 C18 123.9(2) . . ?
C16 C17 H17 118.1 . . ?
C18 C17 H17 118.1 . . ?
C20 C19 C24 118.8(2) . . ?
C20 C19 C18 122.3(2) . . ?
C24 C19 C18 118.9(2) . . ?
C9 C4 C5 118.5(2) . . ?
C9 C4 C3 118.7(2) . . ?
C5 C4 C3 122.8(2) . . ?
O3 C18 C17 124.4(2) . . ?
O3 C18 C19 115.4(2) . . ?
C17 C18 C19 120.2(2) . . ?
C26 C25 C30 118.6(2) . . ?
C26 C25 C16 123.1(2) . . ?
C30 C25 C16 118.2(2) . . ?
C8 C9 C4 121.1(2) . . ?
C8 C9 H9 119.5 . . ?
C4 C9 H9 119.5 . . ?
O4 C1 C2 124.6(2) . . ?
O4 C1 C10 116.4(2) . . ?
C2 C1 C10 118.9(2) . . ?
C27 C26 C25 121.1(2) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
N C31 C32 123.4(2) . . ?
N C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C14 C15 C10 120.7(2) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
C29 C30 C25 120.7(2) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?
C23 C24 C19 120.3(2) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C3 C2 C1 123.1(2) . . ?
C3 C2 H2 118.5 . . ?
C1 C2 H2 118.5 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C26 C27 C28 119.4(2) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C6 C7 C8 119.5(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C33 C32 C31 117.1(2) . . ?
C33 C32 C36 122.4(2) . . ?
C31 C32 C36 120.5(2) . . ?
C21 C20 C19 120.4(2) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C6 C5 C4 120.1(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C9 C8 C7 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C29 C28 C27 120.1(2) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C33 C34 C35 119.1(2) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C21 C22 C23 119.5(2) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C21 C20 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C30 C29 C28 120.0(2) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36C C36 H36B 109.5 . . ?
N C35 C34 122.0(2) . . ?
N C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
C7 C6 C5 120.7(2) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C24 C23 C22 120.5(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.08
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.059


data_44-bipy
_database_code_depnum_ccdc_archive 'CCDC 615633'
#TrackingRef 'structures.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(1,3-diphenylpropane-1,3-dionato)(4,4'-bipyridine)oxovanadium(IV)
dimethylsulphoxyde solvate
;
_chemical_name_common            
;
bis(1,3-diphenylpropane-1,3-dionato)(4,4'-
bipyridine)oxovanadium(IV) dimethylsulphoxyde solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H30 N2 O5 V, C2 H6 O S'
_chemical_formula_sum            'C42 H36 N2 O6 S V'
_chemical_formula_weight         747.74

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'
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'
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 '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                   10.333(2)
_cell_length_b                   14.007(2)
_cell_length_c                   14.251(3)
_cell_angle_alpha                77.356(15)
_cell_angle_beta                 70.407(18)
_cell_angle_gamma                77.535(16)
_cell_volume                     1873.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             778
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   
;
Alcock, N. W. (1970). Crystallographic Computing, edited by F. R. Ahmed,
S. R. Hall & C. P. Huber, pp. 271-276. Copenhagen: Munksgaard.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur3 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20063
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         25.07
_reflns_number_total             6513
_reflns_number_gt                4572
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
Oxford Diffraction (2003). CrysAlis CCD. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_cell_refinement       
;
Oxford Diffraction (2003). CrysAlis RED. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_data_reduction        
;
Oxford Diffraction (2003). CrysAlis RED. Version
1.171.26 beta. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.1994P)^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         6513
_refine_ls_number_parameters     501
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0973
_refine_ls_wR_factor_ref         0.3113
_refine_ls_wR_factor_gt          0.2747
_refine_ls_goodness_of_fit_ref   1.122
_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
V V 0.56539(7) 0.46641(5) 0.18307(5) 0.0694(4) Uani 1 1 d . . .
O1 O 0.4460(3) 0.4818(2) 0.1316(2) 0.0789(9) Uani 1 1 d . . .
O3 O 0.7022(3) 0.3684(2) 0.1033(2) 0.0722(8) Uani 1 1 d . . .
O2 O 0.5044(3) 0.3533(2) 0.2903(2) 0.0741(8) Uani 1 1 d . . .
O4 O 0.4615(3) 0.5615(2) 0.2797(2) 0.0739(8) Uani 1 1 d . . .
O5 O 0.7247(3) 0.4613(2) 0.2471(2) 0.0714(8) Uani 1 1 d . . .
N1 N 0.6688(4) 0.5796(3) 0.0703(3) 0.0685(9) Uani 1 1 d . . .
N2 N 0.9893(5) 0.9593(3) -0.2979(3) 0.0918(12) Uani 1 1 d . . .
C1 C 0.6885(4) 0.2792(3) 0.1078(3) 0.0651(10) Uani 1 1 d . . .
C2 C 0.5981(4) 0.2283(3) 0.1883(3) 0.0696(11) Uani 1 1 d . . .
H2 H 0.5921 0.1644 0.1831 0.083 Uiso 1 1 calc R . .
C3 C 0.5150(4) 0.2645(3) 0.2769(3) 0.0672(10) Uani 1 1 d . . .
C4 C 0.4275(5) 0.2008(4) 0.3627(3) 0.0739(12) Uani 1 1 d . . .
C5 C 0.4474(6) 0.1004(4) 0.3705(4) 0.1053(18) Uani 1 1 d . . .
H5 H 0.5184 0.0690 0.3219 0.126 Uiso 1 1 calc R . .
C6 C 0.3607(8) 0.0442(5) 0.4518(5) 0.124(2) Uani 1 1 d . . .
H6 H 0.3793 -0.0245 0.4587 0.149 Uiso 1 1 calc R . .
C7 C 0.2518(8) 0.0873(6) 0.5197(5) 0.123(2) Uani 1 1 d . . .
H7 H 0.1906 0.0501 0.5704 0.148 Uiso 1 1 calc R . .
C8 C 0.2349(8) 0.1862(6) 0.5113(5) 0.132(2) Uani 1 1 d . . .
H8 H 0.1617 0.2174 0.5588 0.158 Uiso 1 1 calc R . .
C9 C 0.3213(6) 0.2431(5) 0.4357(4) 0.1054(18) Uani 1 1 d . . .
H9 H 0.3073 0.3112 0.4341 0.126 Uiso 1 1 calc R . .
C10 C 0.7759(4) 0.2335(3) 0.0174(3) 0.0688(11) Uani 1 1 d . . .
C11 C 0.8042(6) 0.1315(4) 0.0186(4) 0.0923(15) Uani 1 1 d . . .
H11 H 0.7664 0.0891 0.0771 0.111 Uiso 1 1 calc R . .
C12 C 0.8884(7) 0.0934(4) -0.0671(5) 0.1087(19) Uani 1 1 d . . .
H12 H 0.9057 0.0252 -0.0659 0.130 Uiso 1 1 calc R . .
C13 C 0.9469(7) 0.1540(5) -0.1539(4) 0.1080(18) Uani 1 1 d . . .
H13 H 1.0045 0.1271 -0.2107 0.130 Uiso 1 1 calc R . .
C14 C 0.9202(6) 0.2538(5) -0.1566(4) 0.1031(17) Uani 1 1 d . . .
H14 H 0.9589 0.2954 -0.2154 0.124 Uiso 1 1 calc R . .
C15 C 0.8348(5) 0.2936(4) -0.0710(4) 0.0858(14) Uani 1 1 d . . .
H15 H 0.8171 0.3619 -0.0735 0.103 Uiso 1 1 calc R . .
C16 C 0.4900(4) 0.5933(3) 0.3473(3) 0.0643(10) Uani 1 1 d . . .
C17 C 0.6178(4) 0.5701(4) 0.3651(3) 0.0741(12) Uani 1 1 d . . .
H17 H 0.6288 0.5972 0.4155 0.089 Uiso 1 1 calc R . .
C18 C 0.7309(4) 0.5084(3) 0.3120(3) 0.0670(10) Uani 1 1 d . . .
C19 C 0.8706(4) 0.5016(3) 0.3240(3) 0.0685(11) Uani 1 1 d . . .
C20 C 0.9836(5) 0.4436(5) 0.2684(5) 0.114(2) Uani 1 1 d . . .
H20 H 0.9702 0.4053 0.2277 0.137 Uiso 1 1 calc R . .
C21 C 1.1149(5) 0.4410(6) 0.2718(5) 0.121(2) Uani 1 1 d . . .
H21 H 1.1889 0.4003 0.2344 0.145 Uiso 1 1 calc R . .
C22 C 1.1387(5) 0.4963(5) 0.3282(4) 0.0977(16) Uani 1 1 d . . .
H22 H 1.2287 0.4949 0.3290 0.117 Uiso 1 1 calc R . .
C23 C 1.0301(5) 0.5545(4) 0.3842(4) 0.0902(15) Uani 1 1 d . . .
H23 H 1.0454 0.5923 0.4245 0.108 Uiso 1 1 calc R . .
C24 C 0.8991(5) 0.5573(4) 0.3813(4) 0.0831(13) Uani 1 1 d . . .
H24 H 0.8261 0.5981 0.4193 0.100 Uiso 1 1 calc R . .
C25 C 0.3772(4) 0.6644(3) 0.4033(3) 0.0655(10) Uani 1 1 d . . .
C26 C 0.2742(4) 0.7139(3) 0.3606(4) 0.0751(12) Uani 1 1 d . . .
H26 H 0.2744 0.7005 0.2995 0.090 Uiso 1 1 calc R . .
C27 C 0.1696(5) 0.7840(4) 0.4097(4) 0.0904(15) Uani 1 1 d . . .
H27 H 0.1020 0.8186 0.3799 0.108 Uiso 1 1 calc R . .
C28 C 0.1659(5) 0.8020(4) 0.5007(5) 0.0995(17) Uani 1 1 d . . .
H28 H 0.0954 0.8482 0.5332 0.119 Uiso 1 1 calc R . .
C29 C 0.2656(6) 0.7521(5) 0.5445(4) 0.1022(17) Uani 1 1 d . . .
H29 H 0.2621 0.7641 0.6070 0.123 Uiso 1 1 calc R . .
C30 C 0.3725(5) 0.6834(4) 0.4960(4) 0.0848(13) Uani 1 1 d . . .
H30 H 0.4406 0.6504 0.5258 0.102 Uiso 1 1 calc R . .
C31 C 0.6023(5) 0.6450(4) 0.0127(4) 0.0844(14) Uani 1 1 d . . .
H31 H 0.5100 0.6408 0.0223 0.101 Uiso 1 1 calc R . .
C32 C 0.6602(5) 0.7179(4) -0.0593(4) 0.0860(14) Uani 1 1 d . . .
H32 H 0.6068 0.7620 -0.0960 0.103 Uiso 1 1 calc R . .
C33 C 0.7980(4) 0.7271(3) -0.0786(3) 0.0657(10) Uani 1 1 d . . .
C34 C 0.8680(5) 0.6577(4) -0.0218(4) 0.0967(17) Uani 1 1 d . . .
H34 H 0.9614 0.6588 -0.0318 0.116 Uiso 1 1 calc R . .
C35 C 0.8028(5) 0.5869(4) 0.0490(4) 0.0959(16) Uani 1 1 d . . .
H35 H 0.8549 0.5406 0.0851 0.115 Uiso 1 1 calc R . .
C36 C 0.8647(5) 0.8070(3) -0.1568(3) 0.0730(11) Uani 1 1 d . . .
C37 C 0.7946(6) 0.8746(5) -0.2134(5) 0.120(2) Uani 1 1 d . . .
H37 H 0.7025 0.8717 -0.2060 0.144 Uiso 1 1 calc R . .
C38 C 0.8614(7) 0.9476(5) -0.2820(6) 0.128(2) Uani 1 1 d . . .
H38 H 0.8109 0.9925 -0.3204 0.153 Uiso 1 1 calc R . .
C39 C 1.0549(6) 0.8936(4) -0.2436(5) 0.1044(18) Uani 1 1 d . . .
H39 H 1.1470 0.8981 -0.2529 0.125 Uiso 1 1 calc R . .
C40 C 0.9981(6) 0.8175(4) -0.1730(5) 0.1019(18) Uani 1 1 d . . .
H40 H 1.0514 0.7733 -0.1363 0.122 Uiso 1 1 calc R . .
O6 O 0.5539(7) 0.0082(4) 0.1487(6) 0.191(3) Uani 1 1 d D . .
S1 S 0.5998(4) -0.0915(3) 0.1164(3) 0.167(2) Uani 0.612(6) 1 d PD A 1
C41 C 0.456(2) -0.1454(16) 0.129(2) 0.192(9) Uani 0.612(6) 1 d PDU A 1
H41A H 0.3751 -0.1157 0.1764 0.288 Uiso 0.612(6) 1 calc PR A 1
H41B H 0.4732 -0.2152 0.1521 0.288 Uiso 0.612(6) 1 calc PR A 1
H41C H 0.4394 -0.1349 0.0644 0.288 Uiso 0.612(6) 1 calc PR A 1
C42 C 0.646(2) -0.1538(19) 0.2272(16) 0.235(11) Uani 0.612(6) 1 d PDU A 1
H42A H 0.7175 -0.2095 0.2108 0.353 Uiso 0.612(6) 1 calc PR A 1
H42B H 0.5661 -0.1762 0.2780 0.353 Uiso 0.612(6) 1 calc PR A 1
H42C H 0.6805 -0.1089 0.2521 0.353 Uiso 0.612(6) 1 calc PR A 1
S1A S 0.5136(7) -0.0948(5) 0.2110(5) 0.150(3) Uani 0.388(6) 1 d PD A 2
C41A C 0.423(3) -0.104(2) 0.128(3) 0.169(12) Uani 0.388(6) 1 d PDU A 2
H41D H 0.3269 -0.1047 0.1651 0.253 Uiso 0.388(6) 1 calc PR A 2
H41E H 0.4619 -0.1636 0.1000 0.253 Uiso 0.388(6) 1 calc PR A 2
H41F H 0.4324 -0.0477 0.0753 0.253 Uiso 0.388(6) 1 calc PR A 2
C42A C 0.658(2) -0.1923(15) 0.182(2) 0.156(9) Uani 0.388(6) 1 d PDU A 2
H42D H 0.7431 -0.1648 0.1546 0.235 Uiso 0.388(6) 1 calc PR A 2
H42E H 0.6485 -0.2256 0.1328 0.235 Uiso 0.388(6) 1 calc PR A 2
H42F H 0.6602 -0.2387 0.2419 0.235 Uiso 0.388(6) 1 calc PR A 2


loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12






V 0.0624(5) 0.0714(6) 0.0733(6) -0.0243(4) -0.0087(4) -0.0144(4)
O1 0.0699(18) 0.089(2) 0.082(2) -0.0255(16) -0.0175(15) -0.0190(16)
O2 0.0738(18) 0.078(2) 0.0689(18) -0.0253(14) -0.0056(14) -0.0209(15)
O3 0.0685(17) 0.0692(18) 0.0744(18) -0.0238(14) -0.0052(13) -0.0155(14)
O4 0.0538(16) 0.0798(19) 0.089(2) -0.0336(16) -0.0125(14) -0.0061(14)
O5 0.0556(16) 0.0748(18) 0.0809(18) -0.0278(15) -0.0092(13) -0.0072(14)
N1 0.069(2) 0.065(2) 0.073(2) -0.0222(17) -0.0195(17) -0.0048(17)
N2 0.086(3) 0.083(3) 0.092(3) -0.012(2) -0.005(2) -0.022(2)
C1 0.058(2) 0.071(3) 0.069(2) -0.022(2) -0.0215(19) -0.002(2)
C2 0.068(2) 0.064(2) 0.076(3) -0.013(2) -0.022(2) -0.006(2)
C3 0.059(2) 0.080(3) 0.062(2) -0.013(2) -0.0175(18) -0.009(2)
C4 0.067(3) 0.081(3) 0.076(3) -0.012(2) -0.019(2) -0.020(2)
C5 0.109(4) 0.095(4) 0.092(4) -0.010(3) 0.001(3) -0.028(3)
C6 0.150(6) 0.098(4) 0.117(5) -0.001(4) -0.020(5) -0.053(4)
C7 0.117(5) 0.131(6) 0.105(5) 0.014(4) -0.011(4) -0.053(5)
C8 0.119(5) 0.137(6) 0.106(5) -0.015(4) 0.020(4) -0.044(5)
C9 0.097(4) 0.098(4) 0.096(4) -0.016(3) 0.009(3) -0.023(3)
C10 0.065(2) 0.069(3) 0.072(3) -0.024(2) -0.015(2) -0.005(2)
C11 0.115(4) 0.076(3) 0.077(3) -0.028(2) -0.012(3) -0.006(3)
C12 0.136(5) 0.078(3) 0.104(4) -0.040(3) -0.020(4) 0.003(3)
C13 0.125(5) 0.101(4) 0.080(3) -0.037(3) -0.005(3) 0.003(4)
C14 0.112(4) 0.106(4) 0.073(3) -0.018(3) -0.006(3) -0.011(3)
C15 0.097(3) 0.078(3) 0.072(3) -0.022(2) -0.011(2) -0.006(3)
C16 0.058(2) 0.066(2) 0.068(2) -0.0171(19) -0.0146(18) -0.0096(19)
C17 0.060(2) 0.088(3) 0.078(3) -0.037(2) -0.017(2) -0.001(2)
C18 0.053(2) 0.067(2) 0.079(3) -0.014(2) -0.0135(19) -0.0102(19)
C19 0.061(2) 0.072(3) 0.072(3) -0.020(2) -0.016(2) -0.010(2)
C20 0.068(3) 0.140(5) 0.154(5) -0.087(4) -0.037(3) 0.013(3)
C21 0.058(3) 0.166(6) 0.150(6) -0.087(5) -0.025(3) 0.011(3)
C22 0.055(3) 0.126(5) 0.114(4) -0.024(3) -0.022(3) -0.018(3)
C23 0.073(3) 0.103(4) 0.105(4) -0.023(3) -0.027(3) -0.028(3)
C24 0.057(3) 0.098(3) 0.092(3) -0.031(3) -0.013(2) -0.008(2)
C25 0.051(2) 0.065(2) 0.078(3) -0.018(2) -0.0112(19) -0.0105(19)
C26 0.064(3) 0.075(3) 0.086(3) -0.027(2) -0.018(2) -0.003(2)
C27 0.075(3) 0.084(3) 0.114(4) -0.030(3) -0.033(3) 0.006(3)
C28 0.077(3) 0.097(4) 0.112(4) -0.045(3) -0.012(3) 0.015(3)
C29 0.086(3) 0.117(4) 0.100(4) -0.050(3) -0.018(3) 0.007(3)
C30 0.067(3) 0.093(3) 0.086(3) -0.028(3) -0.014(2) 0.004(2)
C31 0.064(3) 0.088(3) 0.107(4) -0.015(3) -0.026(3) -0.023(3)
C32 0.079(3) 0.094(3) 0.092(3) -0.003(3) -0.038(3) -0.021(3)
C33 0.064(2) 0.067(2) 0.068(2) -0.023(2) -0.0168(19) -0.004(2)
C34 0.057(3) 0.098(4) 0.120(4) 0.002(3) -0.016(3) -0.016(3)
C35 0.059(3) 0.106(4) 0.111(4) -0.002(3) -0.020(3) -0.013(3)
C36 0.069(3) 0.065(3) 0.084(3) -0.026(2) -0.018(2) -0.002(2)
C37 0.085(4) 0.119(5) 0.141(5) 0.033(4) -0.043(4) -0.027(4)
C38 0.109(5) 0.120(5) 0.142(6) 0.036(4) -0.054(4) -0.023(4)
C39 0.082(3) 0.104(4) 0.122(4) 0.008(4) -0.032(3) -0.028(3)
C40 0.086(4) 0.093(4) 0.126(5) 0.017(3) -0.048(3) -0.022(3)
O6 0.190(6) 0.121(4) 0.239(7) -0.063(4) 0.005(5) -0.055(4)
S1 0.175(4) 0.114(3) 0.171(4) -0.054(2) 0.040(3) -0.056(2)
C41 0.197(12) 0.179(12) 0.204(12) -0.047(9) -0.041(8) -0.051(9)
C42 0.229(13) 0.241(14) 0.238(14) -0.032(9) -0.088(9) -0.018(9)
S1A 0.161(5) 0.137(4) 0.138(5) -0.052(3) 0.017(4) -0.065(4)
C41A 0.164(14) 0.167(15) 0.182(15) -0.028(9) -0.053(9) -0.038(9)
C42A 0.166(12) 0.147(12) 0.159(12) -0.028(9) -0.053(9) -0.021(9)

_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
O6 S1 1.496(6) . ?
O6 S1A 1.580(8) . ?
S1 C41 1.754(13) . ?
S1 C42 1.792(14) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
S1A C41A 1.766(15) . ?
S1A C42A 1.795(15) . ?
C41A H41D 0.9600 . ?
C41A H41E 0.9600 . ?
C41A H41F 0.9600 . ?
C42A H42D 0.9600 . ?
C42A H42E 0.9600 . ?
C42A H42F 0.9600 . ?
V O1 1.590(3) . ?
V O3 1.986(3) . ?
V O2 1.991(3) . ?
V O4 2.004(3) . ?
V O5 2.115(3) . ?
V N1 2.168(4) . ?
O4 C16 1.284(5) . ?
O5 C18 1.273(5) . ?
O3 C1 1.273(5) . ?
O2 C3 1.276(5) . ?
N1 C31 1.328(6) . ?
N1 C35 1.336(6) . ?
C25 C26 1.383(6) . ?
C25 C30 1.387(7) . ?
C25 C16 1.486(6) . ?
C16 C17 1.385(6) . ?
C2 C1 1.381(6) . ?
C2 C3 1.398(6) . ?
C2 H2 0.9300 . ?
C18 C17 1.394(6) . ?
C18 C19 1.489(6) . ?
C1 C10 1.489(6) . ?
C17 H17 0.9300 . ?
C33 C34 1.366(7) . ?
C33 C32 1.386(6) . ?
C33 C36 1.497(6) . ?
C3 C4 1.495(6) . ?
C19 C24 1.379(7) . ?
C19 C20 1.380(7) . ?
C36 C37 1.354(7) . ?
C36 C40 1.355(7) . ?
N2 C39 1.296(7) . ?
N2 C38 1.305(7) . ?
C28 C27 1.361(8) . ?
C28 C29 1.366(8) . ?
C28 H28 0.9300 . ?
C10 C15 1.381(6) . ?
C10 C11 1.393(6) . ?
C26 C27 1.399(6) . ?
C26 H26 0.9300 . ?
C15 C14 1.392(7) . ?
C15 H15 0.9300 . ?
C4 C5 1.363(7) . ?
C4 C9 1.363(7) . ?
C31 C32 1.359(7) . ?
C31 H31 0.9300 . ?
C12 C13 1.371(8) . ?
C12 C11 1.380(7) . ?
C12 H12 0.9300 . ?
C30 C29 1.394(7) . ?
C30 H30 0.9300 . ?
C24 C23 1.361(6) . ?
C24 H24 0.9300 . ?
C35 C34 1.360(7) . ?
C35 H35 0.9300 . ?
C34 H34 0.9300 . ?
C23 C22 1.361(8) . ?
C23 H23 0.9300 . ?
C11 H11 0.9300 . ?
C21 C22 1.338(8) . ?
C21 C20 1.366(7) . ?
C21 H21 0.9300 . ?
C27 H27 0.9300 . ?
C32 H32 0.9300 . ?
C9 C8 1.371(8) . ?
C9 H9 0.9300 . ?
C5 C6 1.404(8) . ?
C5 H5 0.9300 . ?
C14 C13 1.359(8) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C7 C6 1.341(10) . ?
C7 C8 1.343(10) . ?
C7 H7 0.9300 . ?
C40 C39 1.377(7) . ?
C40 H40 0.9300 . ?
C22 H22 0.9300 . ?
C38 C37 1.376(8) . ?
C38 H38 0.9300 . ?
C20 H20 0.9300 . ?
C37 H37 0.9300 . ?
C39 H39 0.9300 . ?
C8 H8 0.9300 . ?
C29 H29 0.9300 . ?
C6 H6 0.9300 . ?

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
S1 O6 S1A 51.6(3) . . ?
O6 S1 C41 110.6(9) . . ?
O6 S1 C42 95.7(9) . . ?
C41 S1 C42 101.7(11) . . ?
O6 S1A C41A 91.2(12) . . ?
O6 S1A C42A 110.7(9) . . ?
C41A S1A C42A 100.7(12) . . ?
S1A C41A H41D 109.5 . . ?
S1A C41A H41E 109.5 . . ?
H41D C41A H41E 109.5 . . ?
S1A C41A H41F 109.5 . . ?
H41D C41A H41F 109.5 . . ?
H41E C41A H41F 109.5 . . ?
S1A C42A H42D 109.5 . . ?
S1A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
S1A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
O1 V O3 98.84(14) . . ?
O1 V O2 98.03(15) . . ?
O3 V O2 87.84(12) . . ?
O1 V O4 94.63(14) . . ?
O3 V O4 166.53(12) . . ?
O2 V O4 90.24(13) . . ?
O1 V O5 174.30(14) . . ?
O3 V O5 84.16(12) . . ?
O2 V O5 86.90(12) . . ?
O4 V O5 82.43(11) . . ?
O1 V N1 91.63(15) . . ?
O3 V N1 86.69(12) . . ?
O2 V N1 169.53(13) . . ?
O4 V N1 93.01(13) . . ?
O5 V N1 83.67(13) . . ?
C16 O4 V 134.1(3) . . ?
C18 O5 V 131.5(3) . . ?
C1 O3 V 125.8(3) . . ?
C3 O2 V 125.9(3) . . ?
C31 N1 C35 114.6(4) . . ?
C31 N1 V 121.0(3) . . ?
C35 N1 V 124.3(3) . . ?
C26 C25 C30 119.0(4) . . ?
C26 C25 C16 118.6(4) . . ?
C30 C25 C16 122.4(4) . . ?
O4 C16 C17 124.3(4) . . ?
O4 C16 C25 115.1(4) . . ?
C17 C16 C25 120.4(4) . . ?
C1 C2 C3 125.6(4) . . ?
C1 C2 H2 117.2 . . ?
C3 C2 H2 117.2 . . ?
O5 C18 C17 123.5(4) . . ?
O5 C18 C19 116.6(4) . . ?
C17 C18 C19 119.7(4) . . ?
O3 C1 C2 123.6(4) . . ?
O3 C1 C10 114.6(4) . . ?
C2 C1 C10 121.8(4) . . ?
C16 C17 C18 123.8(4) . . ?
C16 C17 H17 118.1 . . ?
C18 C17 H17 118.1 . . ?
C34 C33 C32 115.2(4) . . ?
C34 C33 C36 122.9(4) . . ?
C32 C33 C36 122.0(4) . . ?
O2 C3 C2 123.6(4) . . ?
O2 C3 C4 115.0(4) . . ?
C2 C3 C4 121.4(4) . . ?
C24 C19 C20 115.9(4) . . ?
C24 C19 C18 124.1(4) . . ?
C20 C19 C18 119.8(4) . . ?
C37 C36 C40 116.1(5) . . ?
C37 C36 C33 122.3(4) . . ?
C40 C36 C33 121.6(4) . . ?
C39 N2 C38 114.3(5) . . ?
C27 C28 C29 120.1(5) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C15 C10 C11 118.0(4) . . ?
C15 C10 C1 119.4(4) . . ?
C11 C10 C1 122.6(4) . . ?
C25 C26 C27 119.9(5) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C10 C15 C14 121.3(5) . . ?
C10 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C5 C4 C9 117.5(5) . . ?
C5 C4 C3 122.4(4) . . ?
C9 C4 C3 120.1(5) . . ?
N1 C31 C32 124.3(4) . . ?
N1 C31 H31 117.9 . . ?
C32 C31 H31 117.9 . . ?
C13 C12 C11 121.3(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C25 C30 C29 120.0(5) . . ?
C25 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C23 C24 C19 122.3(5) . . ?
C23 C24 H24 118.8 . . ?
C19 C24 H24 118.8 . . ?
N1 C35 C34 124.4(5) . . ?
N1 C35 H35 117.8 . . ?
C34 C35 H35 117.8 . . ?
C35 C34 C33 120.8(4) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C24 C23 C22 119.9(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C22 C21 C20 121.0(5) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C28 C27 C26 120.5(5) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C31 C32 C33 120.6(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C4 C9 C8 120.7(6) . . ?
C4 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C13 C14 C15 119.9(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C13 C12 119.6(5) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C6 C7 C8 117.3(6) . . ?
C6 C7 H7 121.4 . . ?
C8 C7 H7 121.4 . . ?
C36 C40 C39 120.1(5) . . ?
C36 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C21 C22 C23 119.4(5) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
N2 C38 C37 125.7(5) . . ?
N2 C38 H38 117.2 . . ?
C37 C38 H38 117.2 . . ?
C21 C20 C19 121.5(5) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C36 C37 C38 119.1(5) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.5 . . ?
N2 C39 C40 124.8(5) . . ?
N2 C39 H39 117.6 . . ?
C40 C39 H39 117.6 . . ?
C7 C8 C9 122.6(7) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C28 C29 C30 120.4(5) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C7 C6 C5 121.6(7) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.072