# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a
_audit_creation_date             2013-09-24
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H7 N3 O5 V, 6(H2 O), H4 N'
_chemical_formula_sum            'C8 H23 N4 O11 V'
_chemical_formula_weight         402.24

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_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                   7.5216(17)
_cell_length_b                   26.293(6)
_cell_length_c                   9.411(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.488(4)
_cell_angle_gamma                90.00
_cell_volume                     1731.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4624
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.33

_exptl_crystal_description       block
_exptl_crystal_colour            yelllow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.765407
_exptl_absorpt_process_details   
;
SADABS v.2.03 (Bruker,2002) was used for absorption correction.
R(int) was 0.0773 before and 0.0400 after correction.
The Ratio of minimum to maximum transmission is 0.7654.
The \l/2 correction factor is 0.0015.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8593
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3029
_reflns_number_gt                3003
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_cell_refinement       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SMART v5.625 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;

_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^)+(0.0121P)^2^+11.3203P] 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         3029
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

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 0.92881(10) 0.14047(3) 0.79282(8) 0.0202(2) Uani 1 1 d . . .
O5 O 0.7847(4) 0.16474(12) 0.8633(4) 0.0302(7) Uani 1 1 d . . .
O2 O 1.1530(4) 0.17733(12) 0.8878(4) 0.0290(7) Uani 1 1 d . . .
O1 O 1.1507(4) 0.13217(12) 0.9756(3) 0.0260(7) Uani 1 1 d . . .
O4 O 0.7669(4) 0.13463(12) 0.5813(4) 0.0302(7) Uani 1 1 d . . .
O3 O 0.8889(4) 0.17948(12) 0.6167(4) 0.0293(7) Uani 1 1 d . . .
O007 O 1.2590(5) 0.22604(13) 0.6433(5) 0.0377(8) Uani 1 1 d G . .
H00A H 1.2616 0.2574 0.6225 0.057 Uiso 1 1 d G . .
H00B H 1.1437 0.2163 0.6172 0.057 Uiso 1 1 d G . .
O008 O 1.4176(6) 0.24625(14) 1.2036(4) 0.0412(9) Uani 1 1 d G . .
H00C H 1.4609 0.2762 1.2258 0.062 Uiso 1 1 d G . .
H00D H 1.4425 0.2291 1.2851 0.062 Uiso 1 1 d G . .
O009 O 0.4365(5) 0.18622(15) 0.4581(4) 0.0359(8) Uani 1 1 d G . .
H00E H 0.3828 0.1954 0.5193 0.054 Uiso 1 1 d G . .
H00F H 0.5388 0.1702 0.5072 0.054 Uiso 1 1 d G . .
O010 O 1.0968(5) 0.15623(16) 1.2391(4) 0.0407(9) Uani 1 1 d G . .
H01E H 1.1043 0.1495 1.1532 0.061 Uiso 1 1 d G . .
H01F H 1.2082 0.1611 1.3049 0.061 Uiso 1 1 d G . .
N011 N 1.0358(6) 0.27594(18) 0.9661(6) 0.0330(10) Uani 1 1 d . . .
H01A H 1.085(8) 0.244(2) 0.955(7) 0.049 Uiso 1 1 d . . .
H01B H 1.024(8) 0.277(2) 1.058(7) 0.049 Uiso 1 1 d . . .
H01C H 1.118(9) 0.298(2) 0.973(7) 0.049 Uiso 1 1 d . . .
H01D H 0.923(9) 0.281(2) 0.875(7) 0.049 Uiso 1 1 d . . .
O012 O 0.5133(5) 0.09628(16) 1.0182(4) 0.0417(9) Uani 1 1 d G . .
H01G H 0.5847 0.1049 1.1081 0.062 Uiso 1 1 d G . .
H01H H 0.4011 0.1076 0.9990 0.062 Uiso 1 1 d G . .
N1 N 1.1068(5) 0.08327(15) 0.7023(4) 0.0259(8) Uani 1 1 d . . .
N3 N 0.7305(5) 0.04842(15) 0.8841(4) 0.0250(8) Uani 1 1 d . . .
C6 C 1.2951(7) 0.0091(2) 0.6072(6) 0.0400(13) Uani 1 1 d . . .
H6 H 1.3586 -0.0160 0.5748 0.048 Uiso 1 1 calc R . .
O016 O 0.7708(6) 0.12828(18) 0.2844(5) 0.0581(12) Uani 1 1 d G . .
H01I H 0.7312 0.1588 0.2748 0.087 Uiso 1 1 d G . .
H01J H 0.8839 0.1275 0.2846 0.087 Uiso 1 1 d G . .
C2 C 0.8494(7) -0.01883(18) 0.8170(5) 0.0306(11) Uani 1 1 d . . .
H2 H 0.8757 -0.0523 0.8000 0.037 Uiso 1 1 calc R . .
N2 N 0.8547(5) 0.06599(13) 0.8241(4) 0.0223(8) Uani 1 1 d . . .
C3 C 0.9287(6) 0.02503(16) 0.7830(5) 0.0246(10) Uani 1 1 d . . .
C5 C 1.1661(7) -0.0038(2) 0.6721(5) 0.0343(12) Uani 1 1 d . . .
H5 H 1.1411 -0.0378 0.6852 0.041 Uiso 1 1 calc R . .
C1 C 0.7249(7) -0.00191(19) 0.8807(5) 0.0319(11) Uani 1 1 d . . .
H1 H 0.6486 -0.0222 0.9160 0.038 Uiso 1 1 calc R . .
C4 C 1.0739(6) 0.03431(17) 0.7176(5) 0.0261(10) Uani 1 1 d . . .
C8 C 1.2336(7) 0.0953(2) 0.6403(5) 0.0341(11) Uani 1 1 d . . .
H8 H 1.2586 0.1294 0.6302 0.041 Uiso 1 1 calc R . .
C7 C 1.3297(7) 0.0591(2) 0.5904(6) 0.0405(13) Uani 1 1 d . . .
H7 H 1.4166 0.0687 0.5460 0.049 Uiso 1 1 calc R . .
H3 H 0.668(6) 0.0682(17) 0.913(5) 0.013(11) 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 0.0192(4) 0.0207(4) 0.0220(4) -0.0008(3) 0.0093(3) 0.0020(3)
O5 0.0278(17) 0.0304(18) 0.0371(19) 0.0003(15) 0.0173(15) 0.0034(14)
O2 0.0262(17) 0.0291(17) 0.0333(18) -0.0031(14) 0.0126(14) -0.0053(14)
O1 0.0229(16) 0.0304(17) 0.0243(17) 0.0009(13) 0.0082(13) 0.0013(13)
O4 0.0304(17) 0.0306(18) 0.0274(18) 0.0017(14) 0.0080(14) 0.0020(14)
O3 0.0305(18) 0.0282(17) 0.0303(18) 0.0053(14) 0.0127(15) 0.0033(14)
O007 0.041(2) 0.0268(18) 0.051(2) 0.0000(17) 0.0231(19) -0.0022(15)
O008 0.051(2) 0.040(2) 0.036(2) 0.0024(17) 0.0201(18) -0.0018(18)
O009 0.0292(18) 0.049(2) 0.0294(19) 0.0060(16) 0.0110(15) 0.0084(16)
O010 0.0329(19) 0.062(2) 0.0278(19) -0.0082(18) 0.0126(16) -0.0045(18)
N011 0.027(2) 0.034(3) 0.043(3) 0.005(2) 0.019(2) 0.0009(19)
O012 0.0269(18) 0.062(3) 0.038(2) -0.0030(19) 0.0136(16) 0.0067(18)
N1 0.0235(19) 0.035(2) 0.0202(19) 0.0011(16) 0.0088(16) 0.0043(16)
N3 0.0187(19) 0.027(2) 0.029(2) -0.0005(17) 0.0081(17) 0.0013(16)
C6 0.032(3) 0.053(4) 0.031(3) -0.011(2) 0.006(2) 0.020(2)
O016 0.049(3) 0.080(3) 0.048(3) -0.025(2) 0.022(2) -0.018(2)
C2 0.035(3) 0.026(2) 0.020(2) -0.0029(19) -0.002(2) -0.002(2)
N2 0.0197(18) 0.0219(19) 0.0229(19) 0.0026(15) 0.0048(15) -0.0017(15)
C3 0.024(2) 0.025(2) 0.019(2) -0.0014(18) 0.0010(18) 0.0049(19)
C5 0.032(3) 0.037(3) 0.026(3) -0.005(2) 0.002(2) 0.012(2)
C1 0.031(3) 0.033(3) 0.026(3) 0.003(2) 0.004(2) -0.006(2)
C4 0.024(2) 0.034(3) 0.016(2) 0.0012(19) 0.0009(18) 0.0029(19)
C8 0.033(3) 0.045(3) 0.026(3) 0.001(2) 0.012(2) 0.003(2)
C7 0.031(3) 0.064(4) 0.032(3) -0.006(3) 0.017(2) 0.007(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 O5 1.597(3) . ?
V1 O2 1.865(3) . ?
V1 O3 1.877(3) . ?
V1 O1 1.920(3) . ?
V1 O4 1.922(3) . ?
V1 N2 2.086(4) . ?
V1 N1 2.370(4) . ?
O2 O1 1.451(4) . ?
O4 O3 1.456(4) . ?
N1 C8 1.325(6) . ?
N1 C4 1.329(6) . ?
N3 C1 1.324(6) . ?
N3 N2 1.338(5) . ?
C6 C7 1.360(8) . ?
C6 C5 1.365(7) . ?
C2 C1 1.359(7) . ?
C2 C3 1.389(6) . ?
N2 C3 1.333(6) . ?
C3 C4 1.457(6) . ?
C5 C4 1.373(6) . ?
C8 C7 1.377(7) . ?

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
O5 V1 O2 103.03(16) . . ?
O5 V1 O3 103.60(15) . . ?
O2 V1 O3 87.90(14) . . ?
O5 V1 O1 99.94(15) . . ?
O2 V1 O1 45.04(13) . . ?
O3 V1 O1 131.18(14) . . ?
O5 V1 O4 101.14(16) . . ?
O2 V1 O4 131.05(14) . . ?
O3 V1 O4 45.05(14) . . ?
O1 V1 O4 158.70(13) . . ?
O5 V1 N2 93.40(16) . . ?
O2 V1 N2 131.43(14) . . ?
O3 V1 N2 132.28(15) . . ?
O1 V1 N2 87.50(14) . . ?
O4 V1 N2 88.30(14) . . ?
O5 V1 N1 164.15(15) . . ?
O2 V1 N1 88.36(14) . . ?
O3 V1 N1 87.59(13) . . ?
O1 V1 N1 80.20(13) . . ?
O4 V1 N1 78.70(13) . . ?
N2 V1 N1 70.75(14) . . ?
O1 O2 V1 69.52(17) . . ?
O2 O1 V1 65.44(17) . . ?
O3 O4 V1 65.86(18) . . ?
O4 O3 V1 69.09(18) . . ?
C8 N1 C4 118.1(4) . . ?
C8 N1 V1 126.8(3) . . ?
C4 N1 V1 115.0(3) . . ?
C1 N3 N2 110.9(4) . . ?
C7 C6 C5 119.3(5) . . ?
C1 C2 C3 104.7(4) . . ?
C3 N2 N3 105.9(4) . . ?
C3 N2 V1 123.8(3) . . ?
N3 N2 V1 130.3(3) . . ?
N2 C3 C2 110.1(4) . . ?
N2 C3 C4 116.4(4) . . ?
C2 C3 C4 133.5(4) . . ?
C6 C5 C4 118.7(5) . . ?
N3 C1 C2 108.4(4) . . ?
N1 C4 C5 122.5(4) . . ?
N1 C4 C3 114.0(4) . . ?
C5 C4 C3 123.5(4) . . ?
N1 C8 C7 122.6(5) . . ?
C6 C7 C8 118.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 898554'