Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               'Dalton Trans.'
#======================================================================
_journal_coden_Cambridge         0222
# 1. SUBMISSION DETAILS

_publ_contact_author             
;
D Dieter Rehder
Department of Chemistry
University of Hamburg
Martin-Luther-King platz 6
Hamburg
D-20146
GERMANY
;

_publ_contact_author_email       DIETER.REHDER@CHEMIE.UNI-HAMBURG.DE
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
Dear Sir, dear Madam,
enclosed to this e-mail is a cif-file.
Sincerely yours,

Cerstin Bader

;

#======================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Synthesis, characterisation and catalytic potential
of hydrazonato-vanadium(V) model complexes with [VO]3+ and [VO2]+ cores
;

loop_
_publ_author_name
_publ_author_address
M.R.Maurya
;    Institut f\"ur Anorganische und Angewandte Chemie der
Universit\"at Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg
Bundesrepublik Deutschland
;
S.Agarwal
;    Institut f\"ur Anorganische und Angewandte Chemie der
Universit\"at Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg
Bundesrepublik Deutschland
;
C.Bader
;    Institut f\"ur Anorganische und Angewandte Chemie der
Universit\"at Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg
Bundesrepublik Deutschland
;
M.Ebel
;    Institut f\"ur Anorganische und Angewandte Chemie der
Universit\"at Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg
Bundesrepublik Deutschland
;
D.Rehder
;    Institut f\"ur Anorganische und Angewandte Chemie der
Universit\"at Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg
Bundesrepublik Deutschland
;

#======================================================================

# 4. TEXT
_publ_section_abstract           
;

;
_publ_section_comment            
;

;
_publ_section_experimental       
;

;
_publ_section_references         
;

;
_publ_section_figure_captions    
;

;
_publ_section_acknowledgements   
;

;
_publ_contact_author_name        'D Dieter Rehder'
#=END
#==========#eof
#======================================================================
data_marya12
_database_code_depnum_ccdc_archive 'CCDC 251548'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'Oxo-(2-furfurylamidosalicylaldimino)vanadium(V)'
;
_chemical_name_common            
Oxo-(2-furfurylamidosalicylaldimino)vanadium(V)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H30 N4 O12 V2'
_chemical_formula_weight         716.44

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.3650(3)
_cell_length_b                   16.0241(5)
_cell_length_c                   11.7780(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.4460(10)
_cell_angle_gamma                90.00
_cell_volume                     1528.83(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    22488
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      65.54

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_T_max  0.8217
_exptl_absorpt_process_details   'program SADABS (Bruker axs system)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15273
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2659
_reflns_number_gt                2462
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0914P)^2^+1.1280P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2659
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1505
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      1.214
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.27480(6) 0.98344(3) 0.76044(4) 0.0206(2) Uani 1 1 d . . .
O1 O 0.4454(3) 0.93531(13) 0.77538(18) 0.0274(5) Uani 1 1 d . . .
O2 O 0.1265(3) 0.88848(12) 0.70187(17) 0.0238(5) Uani 1 1 d . . .
O3 O 0.3451(3) 1.09231(12) 0.75242(17) 0.0255(5) Uani 1 1 d . . .
O4 O 0.2437(3) 0.97745(13) 0.90334(18) 0.0257(5) Uani 1 1 d . . .
O5 O 0.0252(3) 1.05096(13) 0.72392(17) 0.0262(5) Uani 1 1 d . . .
O6 O -0.0627(4) 0.7777(2) 0.4334(3) 0.0581(8) Uani 1 1 d . . .
N1 N 0.1256(3) 0.92658(14) 0.51369(19) 0.0195(5) Uani 1 1 d . . .
H1N H 0.0937 0.9219 0.4369 0.023 Uiso 1 1 calc R . .
N2 N 0.2290(3) 0.98850(14) 0.5750(2) 0.0190(5) Uani 1 1 d . . .
C1 C 0.0838(3) 0.87666(17) 0.5889(2) 0.0196(6) Uani 1 1 d . . .
C2 C -0.0165(4) 0.80398(18) 0.5458(2) 0.0227(6) Uani 1 1 d . . .
C3 C -0.0811(4) 0.7578(2) 0.6203(3) 0.0313(8) Uani 1 1 d . . .
H3 H -0.0676 0.7666 0.7019 0.038 Uiso 1 1 calc R . .
C4 C -0.1706(6) 0.6955(3) 0.5521(6) 0.0750(17) Uani 1 1 d . . .
H4 H -0.2292 0.6524 0.5798 0.090 Uiso 1 1 calc R . .
C5 C -0.1622(5) 0.7051(3) 0.4422(6) 0.0707(17) Uani 1 1 d . . .
H5 H -0.2134 0.6698 0.3788 0.085 Uiso 1 1 calc R . .
C6 C 0.2981(3) 1.03694(17) 0.5150(2) 0.0207(6) Uani 1 1 d . . .
H6 H 0.2743 1.0289 0.4325 0.025 Uiso 1 1 calc R . .
C7 C 0.4102(4) 1.10313(17) 0.5661(3) 0.0220(6) Uani 1 1 d . . .
C8 C 0.4986(4) 1.14451(17) 0.4969(3) 0.0246(6) Uani 1 1 d . . .
H8 H 0.4826 1.1293 0.4169 0.029 Uiso 1 1 calc R . .
C9 C 0.6091(4) 1.20733(19) 0.5431(3) 0.0293(7) Uani 1 1 d . . .
H9 H 0.6707 1.2341 0.4958 0.035 Uiso 1 1 calc R . .
C10 C 0.6291(4) 1.23098(19) 0.6592(3) 0.0313(7) Uani 1 1 d . . .
H10 H 0.7053 1.2739 0.6914 0.038 Uiso 1 1 calc R . .
C11 C 0.5397(4) 1.19283(18) 0.7282(3) 0.0287(7) Uani 1 1 d . . .
H11 H 0.5520 1.2110 0.8067 0.034 Uiso 1 1 calc R . .
C12 C 0.4312(4) 1.12772(17) 0.6840(3) 0.0226(6) Uani 1 1 d . . .
C13 C 0.3261(4) 0.9305(2) 1.0017(3) 0.0306(7) Uani 1 1 d . . .
H13A H 0.2551 0.8845 1.0141 0.046 Uiso 1 1 calc R . .
H13B H 0.3518 0.9664 1.0713 0.046 Uiso 1 1 calc R . .
H13C H 0.4287 0.9078 0.9883 0.046 Uiso 1 1 calc R . .
C14 C -0.0978(4) 1.0328(2) 0.7847(3) 0.0342(7) Uani 1 1 d . . .
H14A H -0.1268 0.9735 0.7755 0.051 Uiso 1 1 calc R . .
H14B H -0.1962 1.0666 0.7524 0.051 Uiso 1 1 calc R . .
H14C H -0.0552 1.0456 0.8682 0.051 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0249(4) 0.0220(3) 0.0132(3) 0.00021(17) 0.0016(2) 0.00203(18)
O1 0.0285(12) 0.0311(11) 0.0194(10) -0.0013(8) -0.0001(8) 0.0040(9)
O2 0.0282(11) 0.0237(10) 0.0175(10) 0.0027(8) 0.0019(8) -0.0013(8)
O3 0.0328(12) 0.0236(10) 0.0189(10) -0.0041(8) 0.0043(9) -0.0018(9)
O4 0.0308(12) 0.0291(12) 0.0155(11) 0.0007(8) 0.0026(9) 0.0056(8)
O5 0.0260(11) 0.0324(11) 0.0201(10) 0.0038(8) 0.0057(8) 0.0046(9)
O6 0.0543(18) 0.0650(19) 0.0486(17) -0.0107(14) 0.0008(14) 0.0006(15)
N1 0.0225(12) 0.0191(11) 0.0142(11) -0.0028(9) -0.0003(9) -0.0011(9)
N2 0.0197(12) 0.0190(12) 0.0171(12) -0.0014(9) 0.0023(9) 0.0016(9)
C1 0.0186(14) 0.0196(13) 0.0195(14) 0.0022(11) 0.0025(11) 0.0048(10)
C2 0.0244(15) 0.0217(14) 0.0201(14) 0.0029(11) 0.0017(11) 0.0014(11)
C3 0.0245(16) 0.0426(18) 0.0246(16) 0.0214(14) 0.0017(12) -0.0118(13)
C4 0.047(3) 0.051(3) 0.113(5) 0.042(3) -0.006(3) -0.016(2)
C5 0.038(2) 0.040(2) 0.114(4) -0.047(3) -0.019(3) 0.0006(18)
C6 0.0220(14) 0.0212(13) 0.0172(14) -0.0002(11) 0.0015(11) 0.0026(11)
C7 0.0217(14) 0.0183(13) 0.0239(15) -0.0015(11) 0.0020(11) 0.0021(11)
C8 0.0255(16) 0.0211(13) 0.0272(16) -0.0014(12) 0.0066(12) 0.0008(12)
C9 0.0257(16) 0.0237(15) 0.0376(18) 0.0048(13) 0.0062(13) -0.0014(12)
C10 0.0288(17) 0.0209(14) 0.0372(18) 0.0005(13) -0.0051(13) -0.0027(12)
C11 0.0317(17) 0.0235(15) 0.0249(15) -0.0047(12) -0.0039(12) 0.0012(12)
C12 0.0246(15) 0.0178(13) 0.0231(14) 0.0010(11) 0.0015(11) 0.0030(11)
C13 0.0373(18) 0.0342(17) 0.0187(15) 0.0055(12) 0.0039(13) 0.0057(13)
C14 0.0287(17) 0.0498(19) 0.0245(16) 0.0013(14) 0.0073(13) 0.0052(15)

_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(2) . ?
V1 O4 1.769(2) . ?
V1 O3 1.851(2) . ?
V1 O2 1.976(2) . ?
V1 N2 2.122(3) . ?
V1 O5 2.295(2) . ?
O2 C1 1.302(3) . ?
O3 C12 1.334(4) . ?
O4 C13 1.410(4) . ?
O5 C14 1.423(4) . ?
O6 C2 1.350(4) . ?
O6 C5 1.450(6) . ?
N1 C1 1.304(4) . ?
N1 N2 1.394(3) . ?
N1 H1N 0.8800 . ?
N2 C6 1.281(4) . ?
C1 C2 1.451(4) . ?
C2 C3 1.358(4) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.323(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.444(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(4) . ?
C7 C12 1.412(4) . ?
C8 C9 1.383(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(4) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O4 102.06(10) . . ?
O1 V1 O3 100.07(11) . . ?
O4 V1 O3 102.92(9) . . ?
O1 V1 O2 97.64(10) . . ?
O4 V1 O2 93.55(9) . . ?
O3 V1 O2 152.61(9) . . ?
O1 V1 N2 93.38(10) . . ?
O4 V1 N2 161.73(10) . . ?
O3 V1 N2 83.66(9) . . ?
O2 V1 N2 74.56(9) . . ?
O1 V1 O5 175.66(9) . . ?
O4 V1 O5 82.01(9) . . ?
O3 V1 O5 80.31(8) . . ?
O2 V1 O5 80.50(8) . . ?
N2 V1 O5 82.36(8) . . ?
C1 O2 V1 117.20(18) . . ?
C12 O3 V1 131.14(18) . . ?
C13 O4 V1 130.8(2) . . ?
C14 O5 V1 123.19(18) . . ?
C2 O6 C5 102.0(3) . . ?
C1 N1 N2 108.7(2) . . ?
C1 N1 H1N 125.6 . . ?
N2 N1 H1N 125.6 . . ?
C6 N2 N1 116.9(2) . . ?
C6 N2 V1 127.0(2) . . ?
N1 N2 V1 115.81(17) . . ?
O2 C1 N1 123.6(3) . . ?
O2 C1 C2 117.5(2) . . ?
N1 C1 C2 118.9(2) . . ?
O6 C2 C3 113.7(3) . . ?
O6 C2 C1 126.3(3) . . ?
C3 C2 C1 119.9(3) . . ?
C2 C3 C4 105.3(4) . . ?
C2 C3 H3 127.4 . . ?
C4 C3 H3 127.4 . . ?
C5 C4 C3 109.4(4) . . ?
C5 C4 H4 125.3 . . ?
C3 C4 H4 125.3 . . ?
C4 C5 O6 109.6(4) . . ?
C4 C5 H5 125.2 . . ?
O6 C5 H5 125.2 . . ?
N2 C6 C7 123.4(3) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C8 C7 C12 119.2(3) . . ?
C8 C7 C6 119.3(3) . . ?
C12 C7 C6 121.6(3) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 120.7(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
O3 C12 C11 119.5(3) . . ?
O3 C12 C7 121.5(3) . . ?
C11 C12 C7 119.0(3) . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.084
#=END
#==========#eof
#End of Crystallographic Information File


#======================================================================
data_7mary
_database_code_depnum_ccdc_archive 'CCDC 252201'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'Oxo-(2-nicotineamidosalicylaldimino)vanadium(V)'
;
_chemical_name_common            
Oxo-(2-nicotineamidosalicylaldimino)vanadium(V)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H32 N6 O10 V2'
_chemical_formula_weight         738.50

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.0161(2)
_cell_length_b                   14.9534(4)
_cell_length_c                   13.2937(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.9190(10)
_cell_angle_gamma                90.00
_cell_volume                     1591.42(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    43494
_cell_measurement_theta_min      0.793661
_cell_measurement_theta_max      1.000000

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.46
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6431
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS, 1998'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        0
_diffrn_reflns_number            41950
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         32.00
_reflns_number_total             5507
_reflns_number_gt                5246
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 1998)'
_computing_cell_refinement       'SAINT (Bruker AXS, 1998)'
_computing_data_reduction        'SAINT (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'

_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^)+(0.0444P)^2^+0.6611P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5507
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.95444(2) 0.109847(13) 0.327532(15) 0.01694(6) Uani 1 1 d . . .
N3 N 0.29027(13) 0.26313(7) 0.17722(8) 0.0212(2) Uani 1 1 d . . .
N1 N 0.83151(12) 0.14567(7) 0.11298(8) 0.01959(19) Uani 1 1 d . . .
N2 N 0.96791(13) 0.10966(7) 0.16806(8) 0.01773(18) Uani 1 1 d . . .
O1 O 0.89653(12) 0.00789(7) 0.32962(8) 0.02565(19) Uani 1 1 d . . .
O2 O 0.74684(10) 0.16492(6) 0.27446(6) 0.01933(16) Uani 1 1 d . . .
O3 O 1.18424(11) 0.09323(6) 0.32617(7) 0.02129(17) Uani 1 1 d . . .
O4 O 0.91556(11) 0.14325(7) 0.45242(7) 0.02268(18) Uani 1 1 d . . .
O5 O 1.04958(12) 0.25082(6) 0.31453(7) 0.02195(18) Uani 1 1 d . . .
H5O H 1.111(3) 0.2592(14) 0.2778(17) 0.036(5) Uiso 1 1 d . . .
C1 C 0.72318(14) 0.17167(8) 0.17726(8) 0.0171(2) Uani 1 1 d . . .
C2 C 0.56319(14) 0.21075(8) 0.13855(9) 0.0170(2) Uani 1 1 d . . .
C3 C 0.52854(16) 0.22834(10) 0.03690(10) 0.0248(2) Uani 1 1 d . . .
H3 H 0.611(2) 0.2182(13) -0.0109(15) 0.031(5) Uiso 1 1 d . . .
C4 C 0.37342(18) 0.26327(11) 0.00716(11) 0.0298(3) Uani 1 1 d . . .
H4 H 0.344(3) 0.2758(15) -0.0615(17) 0.042(6) Uiso 1 1 d . . .
C5 C 0.25811(16) 0.27891(10) 0.07923(11) 0.0256(3) Uani 1 1 d . . .
H5 H 0.152(2) 0.3005(13) 0.0625(15) 0.032(5) Uiso 1 1 d . . .
C6 C 0.44064(15) 0.23018(8) 0.20570(9) 0.0183(2) Uani 1 1 d . . .
H6 H 0.458(2) 0.2189(12) 0.2702(14) 0.025(4) Uiso 1 1 d . . .
C7 C 1.08319(15) 0.07365(8) 0.11670(9) 0.0198(2) Uani 1 1 d . . .
H7 H 1.072(2) 0.0753(12) 0.0463(14) 0.025(4) Uiso 1 1 d . . .
C8 C 1.23207(15) 0.03409(8) 0.16250(10) 0.0203(2) Uani 1 1 d . . .
C9 C 1.33981(17) -0.01354(9) 0.10157(12) 0.0276(3) Uani 1 1 d . . .
H9 H 1.308(3) -0.0233(14) 0.0319(17) 0.040(5) Uiso 1 1 d . . .
C10 C 1.48683(18) -0.04984(10) 0.14189(14) 0.0328(3) Uani 1 1 d . . .
H10 H 1.554(3) -0.0797(15) 0.1002(16) 0.038(5) Uiso 1 1 d . . .
C11 C 1.53021(17) -0.03829(9) 0.24354(13) 0.0309(3) Uani 1 1 d . . .
H11 H 1.625(3) -0.0611(14) 0.2685(16) 0.036(5) Uiso 1 1 d . . .
C12 C 1.42730(16) 0.00827(9) 0.30501(12) 0.0259(3) Uani 1 1 d . . .
H12 H 1.455(3) 0.0182(14) 0.3720(16) 0.036(5) Uiso 1 1 d . . .
C13 C 1.27677(14) 0.04468(8) 0.26581(10) 0.0199(2) Uani 1 1 d . . .
C14 C 0.8202(2) 0.09682(12) 0.52237(12) 0.0335(3) Uani 1 1 d . . .
H14A H 0.823(3) 0.0333(15) 0.5154(16) 0.041(6) Uiso 1 1 d . . .
H14B H 0.861(3) 0.1101(17) 0.588(2) 0.057(7) Uiso 1 1 d . . .
H14C H 0.705(4) 0.1095(17) 0.510(2) 0.060(8) Uiso 1 1 d . . .
C15 C 0.96113(19) 0.33152(10) 0.33187(12) 0.0286(3) Uani 1 1 d . . .
H15A H 0.912(3) 0.3257(14) 0.3955(17) 0.040(5) Uiso 1 1 d . . .
H15B H 0.867(3) 0.3401(16) 0.2800(18) 0.050(6) Uiso 1 1 d . . .
H15C H 1.033(3) 0.3808(14) 0.3335(16) 0.039(6) Uiso 1 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 0.01526(10) 0.01961(10) 0.01581(10) 0.00182(6) -0.00059(7) -0.00041(6)
N3 0.0168(4) 0.0208(5) 0.0262(5) 0.0016(4) 0.0029(4) 0.0007(4)
N1 0.0156(4) 0.0259(5) 0.0172(4) 0.0007(4) -0.0005(3) 0.0025(4)
N2 0.0146(4) 0.0199(4) 0.0185(4) -0.0004(3) -0.0003(3) 0.0011(3)
O1 0.0244(4) 0.0225(4) 0.0297(5) 0.0040(4) -0.0030(3) -0.0029(3)
O2 0.0161(4) 0.0269(4) 0.0149(4) 0.0011(3) 0.0006(3) 0.0023(3)
O3 0.0165(4) 0.0239(4) 0.0231(4) -0.0010(3) -0.0023(3) 0.0020(3)
O4 0.0211(4) 0.0318(5) 0.0152(4) 0.0032(3) 0.0013(3) -0.0005(4)
O5 0.0217(4) 0.0192(4) 0.0256(4) 0.0002(3) 0.0080(3) 0.0014(3)
C1 0.0155(4) 0.0190(5) 0.0168(5) 0.0012(4) -0.0002(4) -0.0003(4)
C2 0.0144(4) 0.0190(5) 0.0177(5) 0.0011(4) 0.0005(4) 0.0001(4)
C3 0.0210(5) 0.0347(7) 0.0186(5) 0.0026(5) 0.0012(4) 0.0049(5)
C4 0.0253(6) 0.0428(8) 0.0210(6) 0.0058(5) -0.0021(5) 0.0078(6)
C5 0.0179(5) 0.0294(6) 0.0291(6) 0.0037(5) -0.0017(4) 0.0042(5)
C6 0.0171(5) 0.0189(5) 0.0190(5) 0.0013(4) 0.0024(4) -0.0005(4)
C7 0.0176(5) 0.0206(5) 0.0211(5) -0.0032(4) 0.0021(4) 0.0000(4)
C8 0.0157(5) 0.0174(5) 0.0281(6) -0.0015(4) 0.0025(4) -0.0007(4)
C9 0.0212(6) 0.0241(6) 0.0379(7) -0.0072(5) 0.0063(5) 0.0007(5)
C10 0.0205(6) 0.0239(6) 0.0547(9) -0.0077(6) 0.0078(6) 0.0033(5)
C11 0.0164(5) 0.0196(6) 0.0565(9) 0.0026(6) -0.0008(5) 0.0022(4)
C12 0.0186(5) 0.0209(5) 0.0375(7) 0.0041(5) -0.0037(5) 0.0001(4)
C13 0.0155(5) 0.0157(5) 0.0284(6) 0.0015(4) 0.0004(4) -0.0010(4)
C14 0.0317(7) 0.0433(8) 0.0264(7) 0.0107(6) 0.0105(5) 0.0035(6)
C15 0.0311(7) 0.0218(6) 0.0334(7) -0.0027(5) 0.0079(5) 0.0035(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.5943(10) . ?
V1 O4 1.7764(9) . ?
V1 O3 1.8598(9) . ?
V1 O2 1.9559(9) . ?
V1 N2 2.1283(11) . ?
V1 O5 2.2514(10) . ?
N3 C5 1.3360(17) . ?
N3 C6 1.3389(15) . ?
N1 C1 1.3081(15) . ?
N1 N2 1.3929(14) . ?
N2 C7 1.2939(15) . ?
O2 C1 1.3004(14) . ?
O3 C13 1.3347(15) . ?
O4 C14 1.4156(17) . ?
O5 C15 1.4242(16) . ?
O5 H5O 0.72(2) . ?
C1 C2 1.4778(15) . ?
C2 C3 1.3907(16) . ?
C2 C6 1.3913(16) . ?
C3 C4 1.3876(18) . ?
C3 H3 0.95(2) . ?
C4 C5 1.385(2) . ?
C4 H4 0.95(2) . ?
C5 H5 0.93(2) . ?
C6 H6 0.878(19) . ?
C7 C8 1.4391(17) . ?
C7 H7 0.936(18) . ?
C8 C9 1.4073(18) . ?
C8 C13 1.4104(18) . ?
C9 C10 1.381(2) . ?
C9 H9 0.96(2) . ?
C10 C11 1.389(2) . ?
C10 H10 0.91(2) . ?
C11 C12 1.379(2) . ?
C11 H11 0.88(2) . ?
C12 C13 1.4001(17) . ?
C12 H12 0.92(2) . ?
C14 H14A 0.95(2) . ?
C14 H14B 0.93(3) . ?
C14 H14C 0.95(3) . ?
C15 H15A 0.95(2) . ?
C15 H15B 1.01(2) . ?
C15 H15C 0.94(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O4 100.81(5) . . ?
O1 V1 O3 99.31(5) . . ?
O4 V1 O3 105.53(4) . . ?
O1 V1 O2 99.54(4) . . ?
O4 V1 O2 91.84(4) . . ?
O3 V1 O2 151.36(4) . . ?
O1 V1 N2 92.62(5) . . ?
O4 V1 N2 162.09(4) . . ?
O3 V1 N2 83.66(4) . . ?
O2 V1 N2 74.14(4) . . ?
O1 V1 O5 175.39(5) . . ?
O4 V1 O5 83.38(4) . . ?
O3 V1 O5 77.57(4) . . ?
O2 V1 O5 82.15(4) . . ?
N2 V1 O5 83.70(4) . . ?
C5 N3 C6 117.84(11) . . ?
C1 N1 N2 107.52(9) . . ?
C7 N2 N1 116.50(10) . . ?
C7 N2 V1 126.87(9) . . ?
N1 N2 V1 116.41(7) . . ?
C1 O2 V1 118.00(7) . . ?
C13 O3 V1 131.26(8) . . ?
C14 O4 V1 127.04(10) . . ?
C15 O5 V1 127.41(8) . . ?
C15 O5 H5O 108.9(17) . . ?
V1 O5 H5O 117.4(17) . . ?
O2 C1 N1 123.92(10) . . ?
O2 C1 C2 117.18(10) . . ?
N1 C1 C2 118.90(10) . . ?
C3 C2 C6 118.12(11) . . ?
C3 C2 C1 122.68(11) . . ?
C6 C2 C1 119.19(10) . . ?
C4 C3 C2 118.67(12) . . ?
C4 C3 H3 120.7(12) . . ?
C2 C3 H3 120.6(12) . . ?
C5 C4 C3 119.12(12) . . ?
C5 C4 H4 119.4(13) . . ?
C3 C4 H4 121.5(13) . . ?
N3 C5 C4 122.85(12) . . ?
N3 C5 H5 115.2(12) . . ?
C4 C5 H5 122.0(12) . . ?
N3 C6 C2 123.39(11) . . ?
N3 C6 H6 116.2(12) . . ?
C2 C6 H6 120.4(12) . . ?
N2 C7 C8 123.16(11) . . ?
N2 C7 H7 118.9(11) . . ?
C8 C7 H7 117.8(11) . . ?
C9 C8 C13 118.97(12) . . ?
C9 C8 C7 118.98(12) . . ?
C13 C8 C7 122.00(11) . . ?
C10 C9 C8 120.81(14) . . ?
C10 C9 H9 119.6(13) . . ?
C8 C9 H9 119.6(13) . . ?
C9 C10 C11 119.69(13) . . ?
C9 C10 H10 118.5(14) . . ?
C11 C10 H10 121.8(14) . . ?
C12 C11 C10 120.78(13) . . ?
C12 C11 H11 120.2(14) . . ?
C10 C11 H11 119.1(14) . . ?
C11 C12 C13 120.40(14) . . ?
C11 C12 H12 122.4(13) . . ?
C13 C12 H12 117.2(13) . . ?
O3 C13 C12 118.85(12) . . ?
O3 C13 C8 121.67(11) . . ?
C12 C13 C8 119.35(12) . . ?
O4 C14 H14A 114.1(13) . . ?
O4 C14 H14B 109.2(16) . . ?
H14A C14 H14B 107(2) . . ?
O4 C14 H14C 109.8(16) . . ?
H14A C14 H14C 102.1(19) . . ?
H14B C14 H14C 115(2) . . ?
O5 C15 H15A 107.3(13) . . ?
O5 C15 H15B 111.1(14) . . ?
H15A C15 H15B 106.8(18) . . ?
O5 C15 H15C 111.1(14) . . ?
H15A C15 H15C 109.4(18) . . ?
H15B C15 H15C 111.0(19) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        32.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.069