Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Themistoklis Kabanos'
'Manolis J. Manos'
'Catherine Raptopoulou'
'Aris Terzis'
'Evangelos J. Tolis'

_publ_contact_author_name        'Dr Themistoklis Kabanos'
_publ_contact_author_address     
;
Department of Chemistry 
University of Ioannina 
Panepistimioupoli Douroutis 
Ioannina 
45110 
GREECE 
;

_publ_contact_author_email       TKAMPANO@CC.UOI.GR

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Mimicking the oxidized glutathione-V(IV)O(2+)
species 
;

data_kav1
_database_code_CSD               192413

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C33.68 H42.22 N6 O13.43 S2 V2'
_chemical_formula_weight         911.99
_chemical_melting_point          ?
_chemical_compound_source        ?

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

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

_cell_length_a                   13.974(4)
_cell_length_b                   12.581(3)
_cell_length_c                   15.157(4)
_cell_angle_alpha                110.694(8)
_cell_angle_beta                 92.144(9)
_cell_angle_gamma                116.050(8)
_cell_volume                     2180(1)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      5.3
_cell_measurement_theta_max      11.6

_exptl_crystal_description       parallelipiped
_exptl_crystal_colour            olive-yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.37
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             943
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        -2.9
_diffrn_reflns_number            6785
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         23.78
_reflns_number_total             6514
_reflns_number_observed          5062
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       
'Program COLLECT (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_cell_refinement       
'Program LEAST (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_data_reduction        
'Program REDUCE (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 136 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1593P)^2^+2.5385P] 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    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0146(25)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6378
_refine_ls_number_parameters     526
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_obs          0.0804
_refine_ls_wR_factor_all         0.2660
_refine_ls_wR_factor_obs         0.2352
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.116
_refine_ls_shift/esd_max         -0.030
_refine_ls_shift/esd_mean        0.004

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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.71516(8) 0.46483(9) 0.18334(7) 0.0646(4) Uani 1 d . .
V2 V 0.77345(8) 0.24788(9) 0.25021(6) 0.0623(3) Uani 1 d . .
O1 O 0.8197(4) 0.5971(4) 0.2541(3) 0.0915(14) Uani 1 d . .
O2 O 0.6652(4) 0.1132(5) 0.2182(3) 0.0914(14) Uani 1 d . .
O3 O 0.7522(3) 0.3264(4) 0.1673(3) 0.0686(10) Uani 1 d . .
O4 O 0.6346(4) 0.4239(5) 0.2850(3) 0.0844(13) Uani 1 d . .
O5 O 0.7283(4) 0.3586(5) 0.3541(3) 0.0829(12) Uani 1 d . .
O6 O 0.7518(3) 0.4414(4) 0.0543(3) 0.0718(10) Uani 1 d . .
O10 O 0.8581(3) 0.1787(3) 0.1629(3) 0.0636(9) Uani 1 d . .
N1 N 0.6296(4) 0.5670(4) 0.1729(3) 0.0699(12) Uani 1 d . .
N2 N 0.5427(4) 0.3152(4) 0.0923(3) 0.0658(12) Uani 1 d . .
N3 N 0.8427(4) 0.2201(4) 0.3646(3) 0.0694(12) Uani 1 d . .
N4 N 0.9507(4) 0.4150(4) 0.3177(3) 0.0621(11) Uani 1 d . .
C1 C 0.6802(6) 0.6968(6) 0.2118(5) 0.087(2) Uani 1 d . .
H1 H 0.7540(6) 0.7426(6) 0.2424(5) 0.115(13) Uiso 1 calc R .
C2 C 0.6269(8) 0.7645(8) 0.2080(7) 0.111(3) Uani 1 d . .
H2 H 0.6641(8) 0.8548(8) 0.2363(7) 0.115(13) Uiso 1 calc R .
C3 C 0.5206(9) 0.6998(10) 0.1631(8) 0.121(3) Uani 1 d . .
H3 H 0.4838(9) 0.7454(10) 0.1611(8) 0.115(13) Uiso 1 calc R .
C4 C 0.4663(6) 0.5672(8) 0.1203(6) 0.097(2) Uani 1 d . .
H4 H 0.3929(6) 0.5219(8) 0.0886(6) 0.115(13) Uiso 1 calc R .
C5 C 0.5227(5) 0.5013(6) 0.1252(4) 0.0726(15) Uani 1 d . .
C6 C 0.4737(5) 0.3592(6) 0.0809(4) 0.0684(14) Uani 1 d . .
C7 C 0.3660(6) 0.2767(7) 0.0304(6) 0.092(2) Uani 1 d . .
H7 H 0.3193(6) 0.3093(7) 0.0237(6) 0.131(15) Uiso 1 calc R .
C8 C 0.3299(7) 0.1463(8) -0.0094(7) 0.107(3) Uani 1 d . .
H8 H 0.2581(7) 0.0889(8) -0.0447(7) 0.131(15) Uiso 1 calc R .
C9 C 0.3994(7) 0.0998(7) 0.0026(6) 0.102(2) Uani 1 d . .
H9 H 0.3755(7) 0.0111(7) -0.0239(6) 0.131(15) Uiso 1 calc R .
C10 C 0.5042(6) 0.1861(6) 0.0541(5) 0.083(2) Uani 1 d . .
H10 H 0.5510(6) 0.1546(6) 0.0633(5) 0.131(15) Uiso 1 calc R .
C11 C 0.7797(7) 0.1260(6) 0.3913(5) 0.090(2) Uani 1 d . .
H11 H 0.7059(7) 0.0739(6) 0.3604(5) 0.102(12) Uiso 1 calc R .
C12 C 0.8208(9) 0.1038(9) 0.4631(6) 0.106(3) Uani 1 d . .
H12 H 0.7751(9) 0.0378(9) 0.4804(6) 0.102(12) Uiso 1 calc R .
C13 C 0.9257(10) 0.1770(11) 0.5074(7) 0.116(3) Uani 1 d . .
H13 H 0.9542(10) 0.1607(11) 0.5546(7) 0.102(12) Uiso 1 calc R .
C14 C 0.9942(7) 0.2789(9) 0.4838(5) 0.095(2) Uani 1 d . .
H14 H 1.0676(7) 0.3325(9) 0.5154(5) 0.102(12) Uiso 1 calc R .
C15 C 0.9476(5) 0.2970(6) 0.4105(4) 0.070(2) Uani 1 d . .
C16 C 1.0103(5) 0.4025(6) 0.3816(4) 0.0649(14) Uani 1 d . .
C17 C 1.1218(6) 0.4874(8) 0.4170(5) 0.091(2) Uani 1 d . .
H17 H 1.1622(6) 0.4793(8) 0.4620(5) 0.099(11) Uiso 1 calc R .
C18 C 1.1715(6) 0.5826(7) 0.3853(6) 0.096(2) Uani 1 d . .
H18 H 1.2462(6) 0.6397(7) 0.4085(6) 0.099(11) Uiso 1 calc R .
C19 C 1.1118(5) 0.5946(6) 0.3194(5) 0.080(2) Uani 1 d . .
H19 H 1.1451(5) 0.6590(6) 0.2969(5) 0.099(11) Uiso 1 calc R .
C20 C 1.0018(5) 0.5098(6) 0.2874(4) 0.0719(15) Uani 1 d . .
H20 H 0.9609(5) 0.5180(6) 0.2429(4) 0.099(11) Uiso 1 calc R .
C21 C 0.6545(5) 0.3872(7) 0.3484(4) 0.079(2) Uani 1 d . .
C22 C 0.5837(7) 0.3777(10) 0.4202(6) 0.107(3) Uani 1 d . .
H22A H 0.5233(36) 0.3883(77) 0.4012(32) 0.184(27) Uiso 1 calc R .
H22B H 0.6260(19) 0.4445(48) 0.4832(12) 0.184(27) Uiso 1 calc R .
H22C H 0.5565(52) 0.2942(30) 0.4222(41) 0.184(27) Uiso 1 calc R .
C23 C 0.7981(4) 0.5169(5) 0.0134(4) 0.0624(13) Uani 1 d . .
O7 O 0.8085(4) 0.6256(4) 0.0357(3) 0.0820(12) Uani 1 d . .
C24 C 0.8428(6) 0.4667(6) -0.0714(5) 0.079(2) Uani 1 d . .
H24A H 0.8140(6) 0.4754(6) -0.1261(5) 0.101(16) Uiso 1 calc R .
H24B H 0.9217(6) 0.5205(6) -0.0548(5) 0.101(16) Uiso 1 calc R .
N5 N 0.8166(5) 0.3317(5) -0.1005(4) 0.0740(13) Uani 1 d . .
HN5 H 0.8563(5) 0.3152(5) -0.0684(4) 0.131(32) Uiso 1 calc R .
C25 C 0.7359(5) 0.2334(6) -0.1732(5) 0.0718(15) Uani 1 d . .
O8 O 0.6792(4) 0.2497(5) -0.2256(4) 0.104(2) Uani 1 d . .
C26 C 0.7204(6) 0.1000(6) -0.1912(5) 0.081(2) Uani 1 d . .
H26 H 0.7573(6) 0.1032(6) -0.1334(5) 0.080(18) Uiso 1 calc R .
C27 C 0.6003(7) 0.0009(8) -0.2179(8) 0.115(3) Uani 1 d . .
H27A H 0.5929(7) -0.0826(17) -0.2291(55) 0.179(27) Uiso 1 calc R .
H27B H 0.5650(15) -0.0035(55) -0.2757(32) 0.179(27) Uiso 1 calc R .
H27C H 0.5668(15) 0.0260(40) -0.1659(24) 0.179(27) Uiso 1 calc R .
S1 S 0.7793(2) 0.0499(2) -0.29311(13) 0.0900(6) Uani 1 d . .
S2 S 0.9424(2) 0.1678(2) -0.24261(14) 0.0882(6) Uani 1 d . .
C28 C 0.9974(9) 0.0859(10) -0.1965(6) 0.105(3) Uani 1 d . .
H28 H 1.0745(9) 0.1508(10) -0.1668(6) 0.239(75) Uiso 1 calc R .
C29 C 1.0015(12) -0.0190(12) -0.2677(8) 0.161(5) Uani 1 d . .
H29A H 1.0267(65) 0.0036(31) -0.3198(29) 0.192(29) Uiso 1 calc R .
H29B H 0.9297(17) -0.0934(26) -0.2920(41) 0.192(29) Uiso 1 calc R .
H29C H 1.0507(50) -0.0391(51) -0.2398(17) 0.192(29) Uiso 1 calc R .
C30 C 0.9498(6) 0.0634(7) -0.1120(5) 0.074(2) Uani 1 d . .
O9 O 0.8645(5) -0.0352(5) -0.1225(4) 0.0952(14) Uani 1 d . .
N6 N 1.0069(5) 0.1557(5) -0.0266(4) 0.0722(13) Uani 1 d . .
HN6 H 1.0659(5) 0.2220(5) -0.0231(4) 0.077(20) Uiso 1 calc R .
C31 C 0.9756(5) 0.1511(6) 0.0608(4) 0.0684(14) Uani 1 d . .
H31A H 1.0411(5) 0.2023(6) 0.1127(4) 0.088(14) Uiso 1 calc R .
H31B H 0.9441(5) 0.0620(6) 0.0538(4) 0.088(14) Uiso 1 calc R .
C32 C 0.8949(4) 0.1992(5) 0.0913(4) 0.0601(13) Uani 1 d . .
O11 O 0.8724(4) 0.2571(5) 0.0495(3) 0.0810(12) Uani 1 d . .
HO3 H 0.7766(76) 0.3199(94) 0.1185(70) 0.133(34) Uiso 1 d . .
OM1 O 0.2899(12) 0.2711(15) 0.2888(11) 0.237(8) Uiso 0.91(2) d P .
CM1 C 0.3034(14) 0.3674(18) 0.2658(13) 0.183(7) Uiso 0.91(2) d P .
OM2 O 0.7524(14) 0.7659(17) 0.4769(13) 0.252(10) Uiso 0.78(3) d P .
CM2 C 0.7545(15) 0.6894(18) 0.5330(14) 0.168(8) Uiso 0.78(3) d P .
OW1 O 0.4803(21) 0.8278(26) 0.4253(19) 0.188(9) Uiso 0.41(2) d P .
OW2 O 0.5071(25) 0.9030(31) 0.3960(22) 0.183(10) Uiso 0.34(2) d P .

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 0.0609(6) 0.0639(6) 0.0572(6) 0.0099(4) 0.0061(4) 0.0328(5)
V2 0.0613(6) 0.0611(6) 0.0512(5) 0.0168(4) 0.0072(4) 0.0241(5)
O1 0.072(3) 0.082(3) 0.084(3) -0.001(2) 0.001(2) 0.037(2)
O2 0.075(3) 0.086(3) 0.073(3) 0.024(2) 0.011(2) 0.014(2)
O3 0.073(3) 0.082(3) 0.056(2) 0.023(2) 0.013(2) 0.046(2)
O4 0.086(3) 0.111(3) 0.065(2) 0.024(2) 0.015(2) 0.064(3)
O5 0.089(3) 0.106(3) 0.055(2) 0.020(2) 0.011(2) 0.058(3)
O6 0.079(3) 0.060(2) 0.079(3) 0.026(2) 0.022(2) 0.037(2)
O10 0.077(2) 0.058(2) 0.055(2) 0.023(2) 0.016(2) 0.031(2)
N1 0.072(3) 0.062(3) 0.066(3) 0.013(2) 0.016(2) 0.034(2)
N2 0.068(3) 0.060(3) 0.059(3) 0.014(2) 0.004(2) 0.031(2)
N3 0.088(4) 0.058(3) 0.059(3) 0.020(2) 0.015(2) 0.036(3)
N4 0.061(3) 0.059(3) 0.057(2) 0.017(2) 0.002(2) 0.028(2)
C1 0.092(5) 0.063(4) 0.090(4) 0.009(3) 0.024(4) 0.042(4)
C2 0.128(7) 0.066(4) 0.128(7) 0.021(4) 0.033(6) 0.054(5)
C3 0.136(8) 0.109(7) 0.150(8) 0.046(6) 0.043(7) 0.090(7)
C4 0.087(5) 0.097(5) 0.123(6) 0.042(5) 0.020(4) 0.060(4)
C5 0.074(4) 0.075(4) 0.073(4) 0.027(3) 0.021(3) 0.042(3)
C6 0.061(3) 0.072(3) 0.071(3) 0.026(3) 0.011(3) 0.034(3)
C7 0.067(4) 0.093(5) 0.106(5) 0.037(4) 0.000(4) 0.034(4)
C8 0.078(5) 0.088(5) 0.116(6) 0.036(5) -0.013(4) 0.015(4)
C9 0.095(5) 0.063(4) 0.108(6) 0.022(4) -0.007(4) 0.019(4)
C10 0.082(4) 0.061(4) 0.086(4) 0.020(3) 0.000(3) 0.029(3)
C11 0.125(6) 0.066(4) 0.078(4) 0.032(3) 0.035(4) 0.043(4)
C12 0.153(8) 0.098(6) 0.100(6) 0.060(5) 0.049(6) 0.073(6)
C13 0.186(10) 0.145(8) 0.092(6) 0.075(6) 0.059(6) 0.118(8)
C14 0.122(6) 0.125(6) 0.077(4) 0.049(4) 0.025(4) 0.084(5)
C15 0.093(4) 0.076(4) 0.051(3) 0.020(3) 0.014(3) 0.052(4)
C16 0.070(4) 0.067(3) 0.052(3) 0.015(2) 0.008(3) 0.037(3)
C17 0.072(4) 0.109(5) 0.079(4) 0.028(4) -0.002(3) 0.042(4)
C18 0.055(4) 0.085(5) 0.110(6) 0.025(4) -0.003(4) 0.017(3)
C19 0.070(4) 0.060(3) 0.092(4) 0.027(3) 0.022(3) 0.020(3)
C20 0.077(4) 0.063(3) 0.071(4) 0.025(3) 0.011(3) 0.033(3)
C21 0.072(4) 0.091(4) 0.061(3) 0.016(3) 0.007(3) 0.042(4)
C22 0.099(5) 0.168(8) 0.081(5) 0.060(5) 0.047(4) 0.078(6)
C23 0.059(3) 0.054(3) 0.069(3) 0.017(3) 0.005(3) 0.030(2)
O7 0.090(3) 0.068(3) 0.097(3) 0.034(2) 0.030(2) 0.045(2)
C24 0.108(5) 0.075(4) 0.081(4) 0.040(3) 0.040(4) 0.059(4)
N5 0.096(4) 0.079(3) 0.066(3) 0.030(3) 0.025(3) 0.058(3)
C25 0.067(4) 0.082(4) 0.082(4) 0.042(3) 0.025(3) 0.041(3)
O8 0.091(3) 0.114(4) 0.125(4) 0.064(3) 0.011(3) 0.055(3)
C26 0.086(4) 0.078(4) 0.079(4) 0.036(3) 0.014(3) 0.036(3)
C27 0.084(5) 0.102(6) 0.148(8) 0.062(6) 0.035(5) 0.028(4)
S1 0.1098(14) 0.0896(12) 0.0689(10) 0.0237(9) 0.0164(9) 0.0541(11)
S2 0.1078(14) 0.1062(13) 0.0883(11) 0.0559(10) 0.0421(10) 0.0687(11)
C28 0.150(8) 0.153(7) 0.084(5) 0.064(5) 0.063(5) 0.118(7)
C29 0.289(15) 0.196(11) 0.139(8) 0.101(8) 0.128(10) 0.202(12)
C30 0.095(5) 0.077(4) 0.078(4) 0.037(3) 0.034(4) 0.060(4)
O9 0.109(4) 0.089(3) 0.087(3) 0.032(3) 0.010(3) 0.052(3)
N6 0.090(4) 0.073(3) 0.080(3) 0.042(3) 0.042(3) 0.052(3)
C31 0.082(4) 0.076(4) 0.068(3) 0.033(3) 0.025(3) 0.052(3)
C32 0.067(3) 0.048(3) 0.058(3) 0.017(2) 0.002(2) 0.025(2)
O11 0.116(3) 0.107(3) 0.071(2) 0.050(2) 0.045(2) 0.084(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 O1 1.593(4) . ?
V1 O3 1.966(4) . ?
V1 O6 1.994(4) . ?
V1 O4 2.021(5) . ?
V1 N1 2.141(5) . ?
V1 N2 2.278(5) . ?
V2 O2 1.584(4) . ?
V2 O3 1.936(4) . ?
V2 O10 2.029(4) . ?
V2 O5 2.029(4) . ?
V2 N3 2.160(5) . ?
V2 N4 2.306(5) . ?
O4 C21 1.273(8) . ?
O5 C21 1.241(8) . ?
O6 C23 1.269(7) . ?
O10 C32 1.278(7) . ?
N1 C1 1.338(8) . ?
N1 C5 1.360(8) . ?
N2 C6 1.338(7) . ?
N2 C10 1.343(7) . ?
N3 C15 1.331(8) . ?
N3 C11 1.338(8) . ?
N4 C20 1.345(7) . ?
N4 C16 1.348(7) . ?
C1 C2 1.368(11) . ?
C2 C3 1.343(12) . ?
C3 C4 1.366(12) . ?
C4 C5 1.388(9) . ?
C5 C6 1.469(8) . ?
C6 C7 1.381(9) . ?
C7 C8 1.364(11) . ?
C8 C9 1.372(12) . ?
C9 C10 1.360(10) . ?
C11 C12 1.379(11) . ?
C12 C13 1.324(13) . ?
C13 C14 1.400(12) . ?
C14 C15 1.400(9) . ?
C15 C16 1.463(9) . ?
C16 C17 1.388(9) . ?
C17 C18 1.359(11) . ?
C18 C19 1.369(10) . ?
C19 C20 1.369(9) . ?
C21 C22 1.499(9) . ?
C23 O7 1.225(6) . ?
C23 C24 1.507(8) . ?
C24 N5 1.459(8) . ?
N5 C25 1.317(8) . ?
C25 O8 1.229(7) . ?
C25 C26 1.513(9) . ?
C26 C27 1.513(10) . ?
C26 S1 1.823(7) . ?
S1 S2 2.019(3) . ?
S2 C28 1.819(7) . ?
C28 C29 1.405(12) . ?
C28 C30 1.522(9) . ?
C30 O9 1.239(8) . ?
C30 N6 1.306(8) . ?
N6 C31 1.424(7) . ?
C31 C32 1.515(8) . ?
C32 O11 1.242(6) . ?
OM1 CM1 1.31(2) . ?
OM2 CM2 1.50(2) . ?
OW1 OW2 1.11(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 O3 106.1(2) . . ?
O1 V1 O6 102.3(2) . . ?
O3 V1 O6 82.3(2) . . ?
O1 V1 O4 98.0(2) . . ?
O3 V1 O4 89.1(2) . . ?
O6 V1 O4 159.5(2) . . ?
O1 V1 N1 91.1(2) . . ?
O3 V1 N1 162.8(2) . . ?
O6 V1 N1 94.5(2) . . ?
O4 V1 N1 88.2(2) . . ?
O1 V1 N2 162.8(2) . . ?
O3 V1 N2 90.7(2) . . ?
O6 V1 N2 83.2(2) . . ?
O4 V1 N2 78.3(2) . . ?
N1 V1 N2 72.1(2) . . ?
O2 V2 O3 105.9(2) . . ?
O2 V2 O10 96.5(2) . . ?
O3 V2 O10 90.9(2) . . ?
O2 V2 O5 98.1(2) . . ?
O3 V2 O5 88.6(2) . . ?
O10 V2 O5 164.9(2) . . ?
O2 V2 N3 92.2(2) . . ?
O3 V2 N3 161.8(2) . . ?
O10 V2 N3 89.4(2) . . ?
O5 V2 N3 86.5(2) . . ?
O2 V2 N4 162.9(2) . . ?
O3 V2 N4 90.5(2) . . ?
O10 V2 N4 78.0(2) . . ?
O5 V2 N4 87.0(2) . . ?
N3 V2 N4 71.7(2) . . ?
V2 O3 V1 134.9(2) . . ?
C21 O4 V1 131.1(4) . . ?
C21 O5 V2 130.8(4) . . ?
C23 O6 V1 134.9(4) . . ?
C32 O10 V2 132.2(3) . . ?
C1 N1 C5 118.3(5) . . ?
C1 N1 V1 121.0(4) . . ?
C5 N1 V1 120.8(4) . . ?
C6 N2 C10 118.1(5) . . ?
C6 N2 V1 117.3(4) . . ?
C10 N2 V1 124.5(4) . . ?
C15 N3 C11 119.0(6) . . ?
C15 N3 V2 120.9(4) . . ?
C11 N3 V2 120.1(5) . . ?
C20 N4 C16 118.7(5) . . ?
C20 N4 V2 124.9(4) . . ?
C16 N4 V2 115.6(4) . . ?
N1 C1 C2 122.2(7) . . ?
C3 C2 C1 119.6(7) . . ?
C2 C3 C4 120.2(8) . . ?
C3 C4 C5 118.8(8) . . ?
N1 C5 C4 120.9(6) . . ?
N1 C5 C6 115.3(5) . . ?
C4 C5 C6 123.8(6) . . ?
N2 C6 C7 122.2(6) . . ?
N2 C6 C5 114.4(5) . . ?
C7 C6 C5 123.4(6) . . ?
C8 C7 C6 118.4(7) . . ?
C7 C8 C9 120.0(7) . . ?
C10 C9 C8 118.7(7) . . ?
N2 C10 C9 122.6(7) . . ?
N3 C11 C12 122.0(8) . . ?
C13 C12 C11 119.5(8) . . ?
C12 C13 C14 120.5(8) . . ?
C15 C14 C13 117.3(8) . . ?
N3 C15 C14 121.6(7) . . ?
N3 C15 C16 116.2(5) . . ?
C14 C15 C16 122.2(7) . . ?
N4 C16 C17 120.7(6) . . ?
N4 C16 C15 114.7(5) . . ?
C17 C16 C15 124.5(6) . . ?
C18 C17 C16 119.5(6) . . ?
C17 C18 C19 120.1(6) . . ?
C18 C19 C20 118.5(6) . . ?
N4 C20 C19 122.5(6) . . ?
O5 C21 O4 124.2(6) . . ?
O5 C21 C22 118.2(7) . . ?
O4 C21 C22 117.6(6) . . ?
O7 C23 O6 126.1(5) . . ?
O7 C23 C24 117.2(5) . . ?
O6 C23 C24 116.7(5) . . ?
N5 C24 C23 114.2(5) . . ?
C25 N5 C24 123.9(6) . . ?
O8 C25 N5 121.8(6) . . ?
O8 C25 C26 122.0(6) . . ?
N5 C25 C26 116.1(6) . . ?
C25 C26 C27 111.3(6) . . ?
C25 C26 S1 108.4(4) . . ?
C27 C26 S1 107.7(5) . . ?
C26 S1 S2 104.8(2) . . ?
C28 S2 S1 107.7(4) . . ?
C29 C28 C30 116.8(8) . . ?
C29 C28 S2 115.1(7) . . ?
C30 C28 S2 110.9(5) . . ?
O9 C30 N6 122.1(6) . . ?
O9 C30 C28 123.1(7) . . ?
N6 C30 C28 114.8(7) . . ?
C30 N6 C31 122.8(6) . . ?
N6 C31 C32 116.1(5) . . ?
O11 C32 O10 125.6(5) . . ?
O11 C32 C31 120.1(5) . . ?
O10 C32 C31 114.3(5) . . ?

_refine_diff_density_max         0.795
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.090

data_kav
_database_code_CSD               192414

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C37.40 H42.22 N6 O13.21 S2 V2'
_chemical_formula_weight         953.15
_chemical_melting_point          ?
_chemical_compound_source        ?

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

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

_cell_length_a                   14.145(6)
_cell_length_b                   12.324(5)
_cell_length_c                   15.266(6)
_cell_angle_alpha                71.03(1)
_cell_angle_beta                 75.81(1)
_cell_angle_gamma                67.37(1)
_cell_volume                     2301(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      5.4
_cell_measurement_theta_max      11.6

_exptl_crystal_description       parallelipiped
_exptl_crystal_colour            green-brown
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      1.36
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             985
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  1.00

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        -2.9
_diffrn_reflns_number            5875
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         22.03
_reflns_number_total             5602
_reflns_number_observed          4050
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       
'Program COLLECT (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_cell_refinement       
'Program LEAST (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_data_reduction        
'Program REDUCE (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+6.0332P] 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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5601
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_obs          0.0709
_refine_ls_wR_factor_all         0.2199
_refine_ls_wR_factor_obs         0.1841
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.044
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.77853(9) 0.26447(10) 0.68625(8) 0.0616(4) Uani 1 d . .
V2 V 0.74978(8) 0.53810(10) 0.74288(7) 0.0580(4) Uani 1 d . .
O1 O 0.6798(4) 0.2383(5) 0.7543(3) 0.0832(15) Uani 1 d . .
O2 O 0.8546(4) 0.5699(5) 0.7128(4) 0.0802(14) Uani 1 d . .
O3 O 0.7567(3) 0.4373(4) 0.6653(3) 0.0618(11) Uani 1 d . .
O4 O 0.8676(4) 0.2236(5) 0.7856(3) 0.0785(14) Uani 1 d . .
O5 O 0.7965(4) 0.3855(5) 0.8458(3) 0.0728(13) Uani 1 d . .
O6 O 0.7313(3) 0.3223(4) 0.5610(3) 0.0645(12) Uani 1 d . .
O10 O 0.6664(3) 0.6913(4) 0.6546(3) 0.0605(11) Uani 1 d . .
N1 N 0.8488(5) 0.0789(5) 0.6768(4) 0.070(2) Uani 1 d . .
N2 N 0.9407(4) 0.2445(5) 0.6005(4) 0.0627(14) Uani 1 d . .
N3 N 0.6998(5) 0.6275(5) 0.8541(4) 0.069(2) Uani 1 d . .
N4 N 0.5805(4) 0.5434(5) 0.8024(3) 0.0584(13) Uani 1 d . .
C1 C 0.7979(8) -0.0013(8) 0.7095(6) 0.089(2) Uani 1 d . .
H1 H 0.7296(8) 0.0234(8) 0.7375(6) 0.087(14) Uiso 1 calc R .
C2 C 0.8450(10) -0.1207(9) 0.7025(7) 0.104(3) Uani 1 d . .
H2 H 0.8072(10) -0.1738(9) 0.7227(7) 0.087(14) Uiso 1 calc R .
C3 C 0.9470(9) -0.1600(8) 0.6658(7) 0.105(3) Uani 1 d . .
H3 H 0.9797(9) -0.2410(8) 0.6642(7) 0.087(14) Uiso 1 calc R .
C4 C 1.0009(7) -0.0800(7) 0.6314(6) 0.084(2) Uani 1 d . .
C5 C 1.1068(8) -0.1091(9) 0.5874(7) 0.105(3) Uani 1 d . .
H5 H 1.1431(8) -0.1889(9) 0.5840(7) 0.139(26) Uiso 1 calc R .
C6 C 1.1550(7) -0.0283(9) 0.5518(7) 0.099(3) Uani 1 d . .
H6 H 1.2241(7) -0.0527(9) 0.5257(7) 0.139(26) Uiso 1 calc R .
C7 C 1.1025(6) 0.0963(8) 0.5530(6) 0.080(2) Uani 1 d . .
C8 C 1.1439(6) 0.1892(9) 0.5135(7) 0.095(3) Uani 1 d . .
H8 H 1.2119(6) 0.1718(9) 0.4842(7) 0.096(15) Uiso 1 calc R .
C9 C 1.0875(7) 0.3037(9) 0.5169(6) 0.093(3) Uani 1 d . .
H9 H 1.1158(7) 0.3657(9) 0.4898(6) 0.096(15) Uiso 1 calc R .
C10 C 0.9860(6) 0.3285(7) 0.5615(6) 0.078(2) Uani 1 d . .
H10 H 0.9479(6) 0.4083(7) 0.5640(6) 0.096(15) Uiso 1 calc R .
C11 C 0.9965(5) 0.1290(6) 0.5973(4) 0.064(2) Uani 1 d . .
C12 C 0.9482(5) 0.0409(6) 0.6366(5) 0.064(2) Uani 1 d . .
C13 C 0.7627(8) 0.6601(8) 0.8849(5) 0.089(2) Uani 1 d . .
H13 H 0.8313(8) 0.6431(8) 0.8573(5) 0.100(16) Uiso 1 calc R .
C14 C 0.7304(11) 0.7178(9) 0.9556(7) 0.113(3) Uani 1 d . .
H14 H 0.7769(11) 0.7385(9) 0.9755(7) 0.100(16) Uiso 1 calc R .
C15 C 0.6300(12) 0.7446(9) 0.9964(7) 0.114(4) Uani 1 d . .
H15 H 0.6072(12) 0.7869(9) 1.0423(7) 0.100(16) Uiso 1 calc R .
C16 C 0.5621(8) 0.7093(7) 0.9702(5) 0.090(3) Uani 1 d . .
C17 C 0.4562(11) 0.7265(10) 1.0110(7) 0.125(4) Uani 1 d . .
H17 H 0.4292(11) 0.7659(10) 1.0587(7) 0.226(47) Uiso 1 calc R .
C18 C 0.3929(9) 0.6870(11) 0.9824(7) 0.122(4) Uani 1 d . .
H18 H 0.3247(9) 0.7003(11) 1.0109(7) 0.226(47) Uiso 1 calc R .
C19 C 0.4308(6) 0.6260(7) 0.9097(6) 0.083(2) Uani 1 d . .
C20 C 0.3752(7) 0.5801(9) 0.8788(7) 0.101(3) Uani 1 d . .
H20 H 0.3067(7) 0.5904(9) 0.9051(7) 0.098(15) Uiso 1 calc R .
C21 C 0.4174(6) 0.5192(8) 0.8101(7) 0.087(2) Uani 1 d . .
H21 H 0.3780(6) 0.4911(8) 0.7877(7) 0.098(15) Uiso 1 calc R .
C22 C 0.5222(6) 0.5008(7) 0.7749(5) 0.074(2) Uani 1 d . .
H22 H 0.5525(6) 0.4568(7) 0.7300(5) 0.098(15) Uiso 1 calc R .
C23 C 0.5355(5) 0.6062(6) 0.8681(4) 0.064(2) Uani 1 d . .
C24 C 0.6006(6) 0.6486(6) 0.8965(4) 0.069(2) Uani 1 d . .
C25 C 0.8595(6) 0.2805(7) 0.8427(5) 0.073(2) Uani 1 d . .
C26 C 0.9321(8) 0.2174(10) 0.9169(7) 0.123(4) Uani 1 d . .
H26A H 0.9238(52) 0.2728(29) 0.9525(43) 0.206(35) Uiso 1 calc R .
H26B H 1.0023(9) 0.1925(75) 0.8872(8) 0.206(35) Uiso 1 calc R .
H26C H 0.9158(47) 0.1473(49) 0.9579(39) 0.206(35) Uiso 1 calc R .
O7 O 0.6452(4) 0.2070(5) 0.5584(4) 0.0809(14) Uani 1 d . .
C27 C 0.6726(5) 0.2967(6) 0.5266(5) 0.061(2) Uani 1 d . .
C28 C 0.6354(6) 0.3854(6) 0.4368(5) 0.071(2) Uani 1 d . .
H28A H 0.6600(6) 0.3429(6) 0.3878(5) 0.058(12) Uiso 1 calc R .
H28B H 0.5605(6) 0.4129(6) 0.4453(5) 0.058(12) Uiso 1 calc R .
N5 N 0.6684(5) 0.4902(5) 0.4060(4) 0.070(2) Uani 1 d . .
H5A H 0.6343(5) 0.5507(5) 0.4302(4) 0.087(25) Uiso 1 calc R .
C29 C 0.7493(6) 0.4968(6) 0.3418(5) 0.067(2) Uani 1 d . .
O8 O 0.7984(4) 0.4179(5) 0.2998(4) 0.099(2) Uani 1 d . .
C30 C 0.7770(5) 0.6101(7) 0.3195(5) 0.075(2) Uani 1 d . .
H30 H 0.7500(5) 0.6463(7) 0.3728(5) 0.083(22) Uiso 1 calc R .
C31 C 0.8923(7) 0.5878(10) 0.2953(8) 0.118(3) Uani 1 d . .
H31A H 0.9047(8) 0.6637(13) 0.2787(53) 0.171(28) Uiso 1 calc R .
H31B H 0.9190(13) 0.5515(66) 0.2435(36) 0.171(28) Uiso 1 calc R .
H31C H 0.9261(10) 0.5340(56) 0.3484(19) 0.171(28) Uiso 1 calc R .
S1 S 0.7178(2) 0.7188(2) 0.21643(14) 0.0886(7) Uani 1 d . .
S2 S 0.5636(2) 0.7708(2) 0.2577(2) 0.0895(7) Uani 1 d . .
C32 C 0.5310(11) 0.9122(8) 0.2910(7) 0.121(4) Uani 1 d . .
H32 H 0.4587(11) 0.9230(8) 0.3183(7) 0.158(54) Uiso 1 calc R .
C33 C 0.5181(18) 1.0131(11) 0.2256(12) 0.265(13) Uani 1 d . .
H33A H 0.5017(76) 1.0038(29) 0.1717(27) 0.191(33) Uiso 1 calc R .
H33B H 0.5806(25) 1.0331(43) 0.2091(44) 0.191(33) Uiso 1 calc R .
H33C H 0.4626(45) 1.0773(21) 0.2477(26) 0.191(33) Uiso 1 calc R .
C34 C 0.5753(7) 0.8923(7) 0.3774(6) 0.077(2) Uani 1 d . .
O9 O 0.6532(5) 0.9152(6) 0.3721(5) 0.111(2) Uani 1 d . .
N6 N 0.5242(5) 0.8525(5) 0.4574(5) 0.072(2) Uani 1 d . .
H6A H 0.4692(5) 0.8385(5) 0.4572(5) 0.106(32) Uiso 1 calc R .
C35 C 0.5558(5) 0.8313(6) 0.5451(5) 0.068(2) Uani 1 d . .
H35A H 0.4945(5) 0.8470(6) 0.5909(5) 0.106(20) Uiso 1 calc R .
H35B H 0.5891(5) 0.8896(6) 0.5388(5) 0.106(20) Uiso 1 calc R .
C36 C 0.6292(5) 0.7038(6) 0.5828(4) 0.057(2) Uani 1 d . .
O11 O 0.6455(4) 0.6246(4) 0.5433(3) 0.0797(14) Uani 1 d . .
HO3 H 0.7171 0.5000 0.6071 0.050 Uiso 1 d . .
OM1 O 0.1928(12) 0.0450(16) 0.7945(11) 0.191(8) Uiso 0.70(2) d P .
CM1 C 0.1824(16) -0.0603(21) 0.7973(15) 0.159(8) Uiso 0.70(2) d P .
OM2 O 0.2103(17) 0.0118(22) 0.0364(17) 0.261(12) Uiso 0.70(2) d P .
CM2 C 0.1820(18) 0.1090(23) -0.0316(18) 0.175(10) Uiso 0.70(2) d P .
OW1 O 0.9069(24) 0.3483(29) 0.1232(21) 0.202(11) Uiso 0.41(2) d P .
OW2 O 0.9480(25) 0.4016(30) 0.1128(22) 0.201(12) Uiso 0.40(2) d P .

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 0.0584(7) 0.0613(7) 0.0533(7) -0.0140(5) -0.0014(5) -0.0118(5)
V2 0.0528(7) 0.0701(7) 0.0484(6) -0.0196(5) -0.0002(5) -0.0180(5)
O1 0.069(3) 0.088(3) 0.073(3) -0.013(3) 0.013(3) -0.027(3)
O2 0.058(3) 0.106(4) 0.079(3) -0.021(3) -0.002(2) -0.037(3)
O3 0.066(3) 0.058(3) 0.051(2) -0.018(2) -0.009(2) -0.006(2)
O4 0.084(3) 0.075(3) 0.064(3) -0.021(3) -0.022(3) -0.004(3)
O5 0.072(3) 0.081(3) 0.053(3) -0.015(2) -0.008(2) -0.014(3)
O6 0.067(3) 0.065(3) 0.061(3) -0.017(2) -0.009(2) -0.021(2)
O10 0.068(3) 0.061(3) 0.053(3) -0.022(2) -0.003(2) -0.019(2)
N1 0.080(4) 0.065(4) 0.060(3) -0.007(3) -0.008(3) -0.025(3)
N2 0.061(3) 0.059(3) 0.061(3) -0.018(3) -0.005(3) -0.012(3)
N3 0.082(4) 0.074(4) 0.056(3) -0.022(3) -0.009(3) -0.027(3)
N4 0.057(3) 0.064(3) 0.049(3) -0.016(3) -0.001(3) -0.018(3)
C1 0.109(7) 0.073(5) 0.080(5) -0.005(4) -0.012(5) -0.037(5)
C2 0.150(10) 0.079(6) 0.091(6) 0.001(5) -0.021(6) -0.063(7)
C3 0.136(9) 0.061(5) 0.108(7) -0.020(5) -0.026(7) -0.018(6)
C4 0.106(7) 0.060(5) 0.076(5) -0.021(4) -0.018(5) -0.010(5)
C5 0.107(8) 0.080(6) 0.100(7) -0.037(5) -0.022(6) 0.013(6)
C6 0.076(6) 0.099(7) 0.107(7) -0.051(6) -0.002(5) 0.003(5)
C7 0.065(5) 0.085(5) 0.084(5) -0.037(4) -0.005(4) -0.008(4)
C8 0.056(5) 0.117(7) 0.112(7) -0.048(6) 0.010(5) -0.027(5)
C9 0.075(6) 0.109(7) 0.106(7) -0.036(5) 0.009(5) -0.046(5)
C10 0.079(5) 0.070(5) 0.086(5) -0.022(4) -0.010(4) -0.025(4)
C11 0.063(4) 0.071(5) 0.054(4) -0.024(3) -0.011(3) -0.010(4)
C12 0.066(5) 0.061(4) 0.059(4) -0.018(3) -0.011(3) -0.012(4)
C13 0.120(7) 0.103(6) 0.068(5) -0.026(5) -0.019(5) -0.056(5)
C14 0.175(11) 0.109(7) 0.088(7) -0.028(6) -0.055(7) -0.057(8)
C15 0.175(11) 0.097(7) 0.078(6) -0.043(5) -0.031(7) -0.030(7)
C16 0.121(7) 0.072(5) 0.052(4) -0.011(4) -0.003(5) -0.014(5)
C17 0.149(11) 0.092(7) 0.069(6) -0.019(5) 0.020(7) 0.004(7)
C18 0.101(8) 0.119(8) 0.084(7) -0.024(6) 0.030(6) 0.002(6)
C19 0.067(5) 0.083(5) 0.077(5) -0.020(4) 0.017(4) -0.017(4)
C20 0.052(5) 0.106(7) 0.109(7) -0.009(6) 0.015(5) -0.020(5)
C21 0.060(5) 0.086(6) 0.106(7) -0.008(5) -0.013(5) -0.028(4)
C22 0.062(5) 0.076(5) 0.079(5) -0.020(4) -0.007(4) -0.019(4)
C23 0.064(4) 0.064(4) 0.048(4) -0.008(3) 0.003(3) -0.014(3)
C24 0.089(6) 0.062(4) 0.040(4) -0.015(3) -0.001(4) -0.011(4)
C25 0.066(5) 0.073(5) 0.063(5) -0.006(4) -0.011(4) -0.014(4)
C26 0.127(8) 0.121(8) 0.107(7) -0.031(6) -0.058(7) 0.000(6)
O7 0.073(3) 0.086(4) 0.088(4) -0.014(3) -0.013(3) -0.036(3)
C27 0.049(4) 0.063(4) 0.065(4) -0.024(4) 0.004(3) -0.013(3)
C28 0.071(5) 0.070(5) 0.076(5) -0.024(4) -0.015(4) -0.018(4)
N5 0.072(4) 0.066(4) 0.063(4) -0.024(3) -0.003(3) -0.011(3)
C29 0.065(4) 0.069(5) 0.064(4) -0.028(4) -0.014(4) -0.007(4)
O8 0.091(4) 0.101(4) 0.107(4) -0.060(4) 0.016(3) -0.024(3)
C30 0.065(5) 0.082(5) 0.072(5) -0.028(4) -0.008(4) -0.014(4)
C31 0.081(6) 0.151(9) 0.134(9) -0.067(7) 0.009(6) -0.042(6)
S1 0.095(2) 0.0968(15) 0.0622(12) -0.0174(10) -0.0005(10) -0.0282(12)
S2 0.0916(15) 0.0922(15) 0.0789(13) -0.0283(11) -0.0268(11) -0.0101(11)
C32 0.176(12) 0.075(6) 0.085(6) -0.025(5) -0.057(7) 0.014(6)
C33 0.526(35) 0.071(7) 0.231(17) 0.012(9) -0.265(22) -0.049(12)
C34 0.076(5) 0.069(5) 0.076(6) -0.021(4) -0.021(5) -0.006(4)
O9 0.095(5) 0.121(5) 0.103(5) -0.019(4) 0.001(4) -0.040(4)
N6 0.073(4) 0.066(4) 0.078(5) -0.017(3) -0.025(3) -0.018(3)
C35 0.066(4) 0.059(4) 0.077(5) -0.022(4) -0.011(4) -0.014(3)
C36 0.057(4) 0.058(4) 0.051(4) -0.017(3) 0.003(3) -0.018(3)
O11 0.103(4) 0.060(3) 0.068(3) -0.028(3) -0.028(3) 0.000(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 O1 1.597(5) . ?
V1 O3 1.958(4) . ?
V1 O6 1.996(5) . ?
V1 O4 2.023(5) . ?
V1 N1 2.153(6) . ?
V1 N2 2.311(6) . ?
V2 O2 1.599(5) . ?
V2 O3 1.939(4) . ?
V2 O5 2.018(5) . ?
V2 O10 2.046(4) . ?
V2 N3 2.151(6) . ?
V2 N4 2.327(5) . ?
O4 C25 1.246(9) . ?
O5 C25 1.265(9) . ?
O6 C27 1.261(8) . ?
O10 C36 1.268(8) . ?
N1 C1 1.340(10) . ?
N1 C12 1.352(9) . ?
N2 C10 1.326(9) . ?
N2 C11 1.347(8) . ?
N3 C13 1.332(9) . ?
N3 C24 1.355(9) . ?
N4 C22 1.335(9) . ?
N4 C23 1.350(8) . ?
C1 C2 1.390(13) . ?
C2 C3 1.369(13) . ?
C3 C4 1.368(12) . ?
C4 C12 1.406(10) . ?
C4 C5 1.441(13) . ?
C5 C6 1.320(13) . ?
C6 C7 1.428(12) . ?
C7 C8 1.382(12) . ?
C7 C11 1.444(10) . ?
C8 C9 1.338(12) . ?
C9 C10 1.393(11) . ?
C11 C12 1.396(10) . ?
C13 C14 1.374(13) . ?
C14 C15 1.361(14) . ?
C15 C16 1.376(14) . ?
C16 C24 1.434(11) . ?
C16 C17 1.436(15) . ?
C17 C18 1.38(2) . ?
C18 C19 1.423(14) . ?
C19 C20 1.363(13) . ?
C19 C23 1.421(10) . ?
C20 C21 1.372(13) . ?
C21 C22 1.402(10) . ?
C23 C24 1.422(10) . ?
C25 C26 1.525(11) . ?
O7 C27 1.223(8) . ?
C27 C28 1.513(10) . ?
C28 N5 1.438(9) . ?
N5 C29 1.321(9) . ?
C29 O8 1.227(8) . ?
C29 C30 1.505(10) . ?
C30 C31 1.516(11) . ?
C30 S1 1.839(8) . ?
S1 S2 2.019(3) . ?
S2 C32 1.829(9) . ?
C32 C33 1.298(15) . ?
C32 C34 1.506(12) . ?
C34 O9 1.217(9) . ?
C34 N6 1.306(10) . ?
N6 C35 1.427(9) . ?
C35 C36 1.525(9) . ?
C36 O11 1.229(7) . ?
OM1 CM1 1.35(2) . ?
OM2 CM2 1.30(3) . ?
OW1 OW2 0.99(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
O1 V1 O3 106.9(2) . . ?
O1 V1 O6 101.9(2) . . ?
O3 V1 O6 82.6(2) . . ?
O1 V1 O4 97.7(3) . . ?
O3 V1 O4 89.5(2) . . ?
O6 V1 O4 160.2(2) . . ?
O1 V1 N1 92.5(3) . . ?
O3 V1 N1 160.6(2) . . ?
O6 V1 N1 92.8(2) . . ?
O4 V1 N1 88.6(2) . . ?
O1 V1 N2 164.2(2) . . ?
O3 V1 N2 88.3(2) . . ?
O6 V1 N2 84.1(2) . . ?
O4 V1 N2 77.5(2) . . ?
N1 V1 N2 72.4(2) . . ?
O2 V2 O3 106.8(2) . . ?
O2 V2 O5 98.5(2) . . ?
O3 V2 O5 88.7(2) . . ?
O2 V2 O10 95.3(2) . . ?
O3 V2 O10 91.5(2) . . ?
O5 V2 O10 165.6(2) . . ?
O2 V2 N3 92.1(3) . . ?
O3 V2 N3 160.6(2) . . ?
O5 V2 N3 84.1(2) . . ?
O10 V2 N3 91.1(2) . . ?
O2 V2 N4 163.0(2) . . ?
O3 V2 N4 89.0(2) . . ?
O5 V2 N4 87.8(2) . . ?
O10 V2 N4 77.7(2) . . ?
N3 V2 N4 72.8(2) . . ?
V2 O3 V1 134.8(2) . . ?
C25 O4 V1 129.9(5) . . ?
C25 O5 V2 131.0(5) . . ?
C27 O6 V1 133.6(4) . . ?
C36 O10 V2 130.5(4) . . ?
C1 N1 C12 118.3(7) . . ?
C1 N1 V1 122.5(6) . . ?
C12 N1 V1 119.2(5) . . ?
C10 N2 C11 118.1(6) . . ?
C10 N2 V1 128.6(5) . . ?
C11 N2 V1 113.1(5) . . ?
C13 N3 C24 118.6(7) . . ?
C13 N3 V2 122.9(6) . . ?
C24 N3 V2 118.5(5) . . ?
C22 N4 C23 117.6(6) . . ?
C22 N4 V2 128.2(5) . . ?
C23 N4 V2 114.0(4) . . ?
N1 C1 C2 121.5(9) . . ?
C3 C2 C1 119.9(9) . . ?
C4 C3 C2 119.9(8) . . ?
C3 C4 C12 117.8(9) . . ?
C3 C4 C5 125.1(9) . . ?
C12 C4 C5 117.1(8) . . ?
C6 C5 C4 123.3(8) . . ?
C5 C6 C7 120.9(9) . . ?
C8 C7 C6 125.6(8) . . ?
C8 C7 C11 116.9(7) . . ?
C6 C7 C11 117.5(8) . . ?
C9 C8 C7 121.1(8) . . ?
C8 C9 C10 119.0(8) . . ?
N2 C10 C9 123.5(7) . . ?
N2 C11 C12 118.1(6) . . ?
N2 C11 C7 121.5(7) . . ?
C12 C11 C7 120.4(7) . . ?
N1 C12 C11 116.8(6) . . ?
N1 C12 C4 122.5(7) . . ?
C11 C12 C4 120.7(7) . . ?
N3 C13 C14 122.8(10) . . ?
C15 C14 C13 119.6(10) . . ?
C14 C15 C16 120.4(9) . . ?
C15 C16 C24 117.3(9) . . ?
C15 C16 C17 125.8(10) . . ?
C24 C16 C17 116.9(10) . . ?
C18 C17 C16 122.8(10) . . ?
C17 C18 C19 120.6(10) . . ?
C20 C19 C23 116.7(8) . . ?
C20 C19 C18 124.9(9) . . ?
C23 C19 C18 118.4(10) . . ?
C19 C20 C21 122.0(8) . . ?
C20 C21 C22 117.4(8) . . ?
N4 C22 C21 123.3(8) . . ?
N4 C23 C19 123.0(7) . . ?
N4 C23 C24 115.8(6) . . ?
C19 C23 C24 121.1(7) . . ?
N3 C24 C23 118.6(6) . . ?
N3 C24 C16 121.2(8) . . ?
C23 C24 C16 120.2(8) . . ?
O4 C25 O5 126.6(7) . . ?
O4 C25 C26 117.0(7) . . ?
O5 C25 C26 116.5(8) . . ?
O7 C27 O6 126.0(7) . . ?
O7 C27 C28 118.3(7) . . ?
O6 C27 C28 115.7(6) . . ?
N5 C28 C27 114.7(6) . . ?
C29 N5 C28 122.3(6) . . ?
O8 C29 N5 123.0(7) . . ?
O8 C29 C30 120.7(7) . . ?
N5 C29 C30 116.2(6) . . ?
C29 C30 C31 113.4(7) . . ?
C29 C30 S1 108.7(5) . . ?
C31 C30 S1 106.6(6) . . ?
C30 S1 S2 105.9(3) . . ?
C32 S2 S1 105.5(5) . . ?
C33 C32 C34 121.4(11) . . ?
C33 C32 S2 118.5(9) . . ?
C34 C32 S2 112.5(6) . . ?
O9 C34 N6 122.4(8) . . ?
O9 C34 C32 121.2(10) . . ?
N6 C34 C32 116.4(9) . . ?
C34 N6 C35 122.7(7) . . ?
N6 C35 C36 115.7(6) . . ?
O11 C36 O10 126.7(6) . . ?
O11 C36 C35 118.7(6) . . ?
O10 C36 C35 114.6(6) . . ?

_refine_diff_density_max         0.887
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.077


data_vobgsh
_database_code_CSD               200153

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C26 H26 N4 O9 V2'
_chemical_formula_weight         640.39
_chemical_melting_point          ?
_chemical_compound_source        ?

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           orthorhomibic
_symmetry_space_group_name_H-M   Pna21

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'

_cell_length_a                   20.38(1)
_cell_length_b                   8.235(4)
_cell_length_c                   16.64(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2794(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      5.4
_cell_measurement_theta_max      11.7

_exptl_crystal_description       parallelipiped
_exptl_crystal_colour            orange-brown
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.50
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        -2.4
_diffrn_reflns_number            4520
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         24.98
_reflns_number_total             4519
_reflns_number_observed          3982
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       
'Program COLLECT (UCLA Cryst.package, C.E.strouse 1994)'
_computing_cell_refinement       
'Program LEAST (UCLA Cryst.package, C.E.strouse 1994)'
_computing_data_reduction        
'Program REDUCE (UCLA Cryst.package, C.E.strouse 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.4451P] 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    ?
_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   0.28(3)
_refine_ls_number_reflns         4518
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_obs          0.0446
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.1000
_refine_ls_goodness_of_fit_all   1.215
_refine_ls_goodness_of_fit_obs   1.191
_refine_ls_restrained_S_all      1.216
_refine_ls_restrained_S_obs      1.191
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.71726(4) 0.22713(9) -0.74033(5) 0.0436(2) Uani 1 d . .
V2 V 0.55189(4) 0.24032(10) -0.81817(5) 0.0441(2) Uani 1 d . .
O1 O 0.7559(2) 0.1447(4) -0.8129(2) 0.0548(9) Uani 1 d . .
O2 O 0.5098(2) 0.2460(5) -0.7387(3) 0.0663(10) Uani 1 d . .
O3 O 0.6390(2) 0.3217(5) -0.7880(2) 0.0497(9) Uani 1 d . .
O4 O 0.6640(2) 0.0293(4) -0.7056(2) 0.0527(9) Uani 1 d . .
O5 O 0.5853(2) 0.0088(4) -0.7987(2) 0.0553(10) Uani 1 d . .
O6 O 0.7613(2) 0.4478(4) -0.7385(2) 0.0538(9) Uani 1 d . .
O8 O 0.5379(2) 0.4574(5) -0.8680(2) 0.0523(9) Uani 1 d . .
N1 N 0.7922(2) 0.1553(5) -0.6557(3) 0.0458(10) Uani 1 d . .
N2 N 0.6854(2) 0.3115(5) -0.6161(3) 0.0509(11) Uani 1 d . .
N3 N 0.4718(2) 0.1504(5) -0.8918(3) 0.0472(10) Uani 1 d . .
N4 N 0.5924(2) 0.1707(6) -0.9441(3) 0.0500(11) Uani 1 d . .
C1 C 0.8471(3) 0.0790(7) -0.6800(4) 0.0512(14) Uani 1 d . .
C2 C 0.8945(3) 0.0271(8) -0.6285(4) 0.064(2) Uani 1 d . .
C3 C 0.8862(3) 0.0486(9) -0.5484(4) 0.069(2) Uani 1 d . .
C4 C 0.8310(3) 0.1291(9) -0.5211(4) 0.065(2) Uani 1 d . .
C5 C 0.7850(3) 0.1834(6) -0.5766(3) 0.0484(13) Uani 1 d . .
C6 C 0.7266(3) 0.2797(7) -0.5546(3) 0.0529(14) Uani 1 d . .
C7 C 0.7145(3) 0.3371(9) -0.4778(3) 0.065(2) Uani 1 d . .
C8 C 0.6612(4) 0.4306(9) -0.4650(4) 0.073(2) Uani 1 d . .
C9 C 0.6185(4) 0.4626(9) -0.5252(4) 0.070(2) Uani 1 d . .
C10 C 0.6319(4) 0.3988(8) -0.6017(4) 0.061(2) Uani 1 d . .
C11 C 0.4096(3) 0.1561(8) -0.8645(4) 0.062(2) Uani 1 d . .
C12 C 0.3571(4) 0.1144(10) -0.9122(5) 0.074(2) Uani 1 d . .
C13 C 0.3672(3) 0.0632(9) -0.9878(5) 0.076(2) Uani 1 d . .
C14 C 0.4301(3) 0.0519(8) -1.0155(4) 0.061(2) Uani 1 d . .
C15 C 0.4816(3) 0.0983(6) -0.9677(3) 0.0473(12) Uani 1 d . .
C16 C 0.5501(3) 0.0982(6) -0.9950(3) 0.0508(13) Uani 1 d . .
C17 C 0.5702(4) 0.0327(8) -1.0685(4) 0.065(2) Uani 1 d . .
C18 C 0.6354(4) 0.0464(10) -1.0887(5) 0.079(2) Uani 1 d . .
C19 C 0.6786(4) 0.1242(10) -1.0388(5) 0.079(2) Uani 1 d . .
C20 C 0.6547(3) 0.1819(9) -0.9663(4) 0.065(2) Uani 1 d . .
C21 C 0.6184(3) -0.0457(6) -0.7424(4) 0.0499(12) Uani 1 d . .
C22 C 0.6052(3) -0.2161(7) -0.7154(4) 0.064(2) Uani 1 d . .
H22A H 0.6301(16) -0.2386(18) -0.6678(15) 0.091(13) Uiso 1 calc R .
H22B H 0.6177(19) -0.2905(7) -0.7571(10) 0.091(13) Uiso 1 calc R .
H22C H 0.5592(5) -0.2283(15) -0.7041(24) 0.091(13) Uiso 1 calc R .
C23 C 0.7501(3) 0.5723(6) -0.7823(3) 0.0524(14) Uani 1 d . .
O7 O 0.7097(2) 0.5779(5) -0.8364(2) 0.0642(11) Uani 1 d . .
C24 C 0.7915(4) 0.7200(7) -0.7649(4) 0.080(2) Uani 1 d . .
H24A H 0.7976(17) 0.7304(30) -0.7079(4) 0.098(15) Uiso 1 calc R .
H24B H 0.7698(11) 0.8151(9) -0.7851(23) 0.098(15) Uiso 1 calc R .
H24C H 0.8334(9) 0.7086(24) -0.7905(21) 0.098(15) Uiso 1 calc R .
C25 C 0.4935(3) 0.5609(7) -0.8554(4) 0.0540(13) Uani 1 d . .
O9 O 0.4447(2) 0.5325(6) -0.8145(4) 0.097(2) Uani 1 d . .
C26 C 0.4999(4) 0.7207(7) -0.8950(5) 0.079(2) Uani 1 d . .
H26A H 0.5438(9) 0.7606(33) -0.8880(30) 0.137(21) Uiso 1 calc R .
H26B H 0.4694(20) 0.7956(20) -0.8715(24) 0.137(21) Uiso 1 calc R .
H26C H 0.4907(28) 0.7096(15) -0.9513(8) 0.137(21) Uiso 1 calc R .
HO3 H 0.6462(31) 0.4056(79) -0.8021(42) 0.071(22) Uiso 1 d . .
H1 H 0.8471(22) 0.0629(55) -0.7291(34) 0.037(13) Uiso 1 d . .
H2 H 0.9278(26) -0.0273(62) -0.6462(29) 0.037(14) Uiso 1 d . .
H3 H 0.9224(30) 0.0070(72) -0.5128(38) 0.070(18) Uiso 1 d . .
H4 H 0.8164(24) 0.1624(61) -0.4732(32) 0.041(14) Uiso 1 d . .
H7 H 0.7464(31) 0.3106(80) -0.4365(41) 0.074(19) Uiso 1 d . .
H8 H 0.6543(30) 0.4880(76) -0.4177(38) 0.066(19) Uiso 1 d . .
H9 H 0.5792(29) 0.5296(72) -0.5286(35) 0.059(17) Uiso 1 d . .
H10 H 0.6041(27) 0.4239(70) -0.6430(34) 0.054(17) Uiso 1 d . .
H11 H 0.4056(23) 0.1863(60) -0.8091(33) 0.042(13) Uiso 1 d . .
H12 H 0.3224(34) 0.1202(91) -0.9011(44) 0.080(25) Uiso 1 d . .
H13 H 0.3297(30) 0.0026(69) -1.0187(35) 0.060(16) Uiso 1 d . .
H14 H 0.4400(32) 0.0200(84) -1.0619(40) 0.075(24) Uiso 1 d . .
H17 H 0.5376(32) -0.0128(80) -1.1011(41) 0.072(21) Uiso 1 d . .
H18 H 0.6444(37) 0.0065(90) -1.1340(43) 0.086(24) Uiso 1 d . .
H19 H 0.7256(35) 0.1476(86) -1.0520(42) 0.087(22) Uiso 1 d . .
H20 H 0.6841(25) 0.2512(61) -0.9343(30) 0.042(14) Uiso 1 d . .

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 0.0550(5) 0.0397(4) 0.0361(4) 0.0055(4) -0.0042(4) -0.0040(4)
V2 0.0495(4) 0.0415(4) 0.0414(4) 0.0044(4) 0.0040(4) -0.0008(4)
O1 0.065(2) 0.056(2) 0.043(2) 0.002(2) -0.007(2) -0.001(2)
O2 0.071(2) 0.068(2) 0.059(2) 0.003(2) 0.014(2) -0.003(2)
O3 0.061(2) 0.041(2) 0.048(2) 0.012(2) -0.007(2) -0.008(2)
O4 0.068(2) 0.042(2) 0.048(2) 0.013(2) -0.009(2) -0.009(2)
O5 0.068(2) 0.042(2) 0.057(3) 0.006(2) -0.014(2) -0.003(2)
O6 0.067(2) 0.047(2) 0.048(2) 0.010(2) -0.013(2) -0.014(2)
O8 0.057(2) 0.045(2) 0.055(2) 0.010(2) 0.003(2) 0.002(2)
N1 0.054(3) 0.044(2) 0.040(2) 0.005(2) -0.001(2) -0.002(2)
N2 0.066(3) 0.039(2) 0.047(3) 0.005(2) 0.006(2) -0.003(2)
N3 0.047(2) 0.040(2) 0.055(3) 0.003(2) 0.002(2) 0.002(2)
N4 0.046(3) 0.061(3) 0.043(2) 0.008(2) 0.007(2) 0.009(2)
C1 0.061(4) 0.052(3) 0.041(3) 0.001(3) -0.003(3) -0.001(3)
C2 0.064(4) 0.067(4) 0.061(4) 0.005(3) -0.005(3) 0.005(4)
C3 0.069(4) 0.080(5) 0.057(4) 0.017(3) -0.017(3) 0.003(4)
C4 0.077(4) 0.078(4) 0.039(3) 0.013(3) -0.003(3) -0.007(4)
C5 0.063(3) 0.050(3) 0.033(3) 0.010(2) -0.005(2) -0.011(3)
C6 0.071(4) 0.056(3) 0.031(3) 0.007(2) 0.002(2) -0.016(3)
C7 0.075(4) 0.079(4) 0.041(3) -0.001(3) 0.010(3) -0.008(4)
C8 0.093(5) 0.075(5) 0.050(4) -0.008(4) 0.017(4) -0.008(4)
C9 0.076(5) 0.067(4) 0.068(4) -0.002(3) 0.016(4) 0.004(4)
C10 0.077(4) 0.054(4) 0.052(4) 0.007(3) 0.004(3) -0.003(3)
C11 0.061(4) 0.054(3) 0.071(4) -0.002(3) 0.011(3) -0.004(3)
C12 0.046(4) 0.077(5) 0.100(6) 0.006(4) 0.011(4) -0.006(4)
C13 0.064(4) 0.065(4) 0.098(6) -0.004(4) -0.015(4) -0.017(3)
C14 0.066(4) 0.058(4) 0.060(4) 0.002(3) -0.011(3) -0.005(3)
C15 0.057(3) 0.035(3) 0.050(3) 0.004(2) -0.004(3) 0.006(2)
C16 0.061(3) 0.046(3) 0.046(3) 0.005(2) 0.002(3) 0.011(3)
C17 0.084(5) 0.062(4) 0.050(4) 0.002(3) 0.004(4) 0.013(4)
C18 0.102(6) 0.082(5) 0.051(4) 0.003(4) 0.028(4) 0.030(5)
C19 0.065(4) 0.103(6) 0.068(5) 0.028(4) 0.020(4) 0.028(4)
C20 0.060(4) 0.084(4) 0.050(3) 0.013(3) 0.002(3) 0.008(4)
C21 0.062(3) 0.042(2) 0.046(3) -0.005(3) 0.004(3) 0.001(2)
C22 0.088(4) 0.043(3) 0.060(3) 0.006(2) -0.001(3) -0.011(3)
C23 0.073(4) 0.048(3) 0.036(3) 0.004(2) -0.006(3) -0.016(3)
O7 0.080(3) 0.061(2) 0.051(2) 0.017(2) -0.021(2) -0.017(2)
C24 0.124(6) 0.050(3) 0.067(4) 0.012(3) -0.028(4) -0.031(4)
C25 0.054(3) 0.051(3) 0.057(3) 0.004(3) -0.002(3) -0.002(3)
O9 0.086(3) 0.092(3) 0.112(4) 0.032(4) 0.027(3) 0.032(3)
C26 0.093(5) 0.044(3) 0.101(5) 0.013(4) -0.021(4) 0.003(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 O1 1.593(4) . ?
V1 O3 1.944(4) . ?
V1 O6 2.027(3) . ?
V1 O4 2.041(4) . ?
V1 N1 2.160(4) . ?
V1 N2 2.276(5) . ?
V2 O2 1.577(4) . ?
V2 O3 1.964(4) . ?
V2 O8 1.991(4) . ?
V2 O5 2.050(4) . ?
V2 N3 2.170(5) . ?
V2 N4 2.324(5) . ?
O4 C21 1.272(6) . ?
O5 C21 1.240(6) . ?
O6 C23 1.278(6) . ?
O8 C25 1.260(6) . ?
N1 C5 1.345(7) . ?
N1 C1 1.345(7) . ?
N2 C10 1.327(8) . ?
N2 C6 1.351(7) . ?
N3 C11 1.348(7) . ?
N3 C15 1.350(7) . ?
N4 C20 1.326(7) . ?
N4 C16 1.348(7) . ?
C1 C2 1.361(8) . ?
C2 C3 1.355(9) . ?
C3 C4 1.382(10) . ?
C4 C5 1.391(8) . ?
C5 C6 1.476(8) . ?
C6 C7 1.384(8) . ?
C7 C8 1.349(10) . ?
C8 C9 1.352(10) . ?
C9 C10 1.405(9) . ?
C11 C12 1.377(10) . ?
C12 C13 1.343(11) . ?
C13 C14 1.366(10) . ?
C14 C15 1.370(8) . ?
C15 C16 1.470(8) . ?
C16 C17 1.398(8) . ?
C17 C18 1.377(11) . ?
C18 C19 1.370(11) . ?
C19 C20 1.384(10) . ?
C21 C22 1.497(7) . ?
C23 O7 1.223(6) . ?
C23 C24 1.508(7) . ?
C25 O9 1.228(7) . ?
C25 C26 1.477(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
O1 V1 O3 105.4(2) . . ?
O1 V1 O6 100.1(2) . . ?
O3 V1 O6 90.6(2) . . ?
O1 V1 O4 97.9(2) . . ?
O3 V1 O4 89.9(2) . . ?
O6 V1 O4 161.2(2) . . ?
O1 V1 N1 91.6(2) . . ?
O3 V1 N1 162.9(2) . . ?
O6 V1 N1 85.5(2) . . ?
O4 V1 N1 88.5(2) . . ?
O1 V1 N2 163.7(2) . . ?
O3 V1 N2 90.8(2) . . ?
O6 V1 N2 80.7(2) . . ?
O4 V1 N2 80.5(2) . . ?
N1 V1 N2 72.1(2) . . ?
O2 V2 O3 105.6(2) . . ?
O2 V2 O8 104.1(2) . . ?
O3 V2 O8 86.0(2) . . ?
O2 V2 O5 94.3(2) . . ?
O3 V2 O5 88.7(2) . . ?
O8 V2 O5 161.5(2) . . ?
O2 V2 N3 94.2(2) . . ?
O3 V2 N3 160.2(2) . . ?
O8 V2 N3 87.9(2) . . ?
O5 V2 N3 91.2(2) . . ?
O2 V2 N4 163.1(2) . . ?
O3 V2 N4 89.6(2) . . ?
O8 V2 N4 84.1(2) . . ?
O5 V2 N4 78.2(2) . . ?
N3 V2 N4 71.0(2) . . ?
V1 O3 V2 135.2(2) . . ?
C21 O4 V1 129.8(3) . . ?
C21 O5 V2 129.6(3) . . ?
C23 O6 V1 129.2(3) . . ?
C25 O8 V2 129.9(4) . . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 V1 120.9(4) . . ?
C1 N1 V1 121.3(4) . . ?
C10 N2 C6 118.6(5) . . ?
C10 N2 V1 124.3(4) . . ?
C6 N2 V1 116.9(4) . . ?
C11 N3 C15 117.7(5) . . ?
C11 N3 V2 120.4(4) . . ?
C15 N3 V2 121.8(4) . . ?
C20 N4 C16 117.8(5) . . ?
C20 N4 V2 125.1(4) . . ?
C16 N4 V2 116.7(3) . . ?
N1 C1 C2 123.2(6) . . ?
C3 C2 C1 119.3(7) . . ?
C2 C3 C4 119.2(6) . . ?
C3 C4 C5 119.0(6) . . ?
N1 C5 C4 121.4(6) . . ?
N1 C5 C6 115.0(5) . . ?
C4 C5 C6 123.5(5) . . ?
N2 C6 C7 121.5(6) . . ?
N2 C6 C5 114.7(5) . . ?
C7 C6 C5 123.8(5) . . ?
C8 C7 C6 119.0(7) . . ?
C7 C8 C9 120.8(7) . . ?
C8 C9 C10 118.2(7) . . ?
N2 C10 C9 121.7(7) . . ?
N3 C11 C12 122.0(7) . . ?
C13 C12 C11 119.9(7) . . ?
C12 C13 C14 118.8(7) . . ?
C13 C14 C15 120.2(7) . . ?
N3 C15 C14 121.3(6) . . ?
N3 C15 C16 115.4(5) . . ?
C14 C15 C16 123.2(5) . . ?
N4 C16 C17 122.3(6) . . ?
N4 C16 C15 114.4(5) . . ?
C17 C16 C15 123.2(6) . . ?
C18 C17 C16 117.7(7) . . ?
C19 C18 C17 120.7(7) . . ?
C18 C19 C20 117.6(7) . . ?
N4 C20 C19 123.8(7) . . ?
O5 C21 O4 125.8(5) . . ?
O5 C21 C22 117.9(5) . . ?
O4 C21 C22 116.3(5) . . ?
O7 C23 O6 124.8(5) . . ?
O7 C23 C24 119.2(5) . . ?
O6 C23 C24 116.0(5) . . ?
O9 C25 O8 123.0(5) . . ?
O9 C25 C26 119.2(6) . . ?
O8 C25 C26 117.7(6) . . ?

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.052