# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global

_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
# SUBMISSION DETAILS

_publ_contact_author_name        'Professor Yi Pinggui'
_publ_contact_author_address     
;Department of Chemical and Environmental Engineering
Changsha University of Science and Technology
Hunan 411201
P. R. China
;
_publ_contact_author_email       pgyi@hnust.cn
_publ_contact_author_fax         86-0731-58290509
_publ_contact_author_phone       86-0731-58290187

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

# TITLE AND AUTHOR LIST

_publ_section_title              
;
NMR and Theoretical Study on the Coordination
and Solution Structures of the Interaction between
Diperoxovanadate Complexes and 4-(Pyridin-2-yl)pyrimidine-like ligands
;
_publ_section_title_footnote     
; ?
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Xianyong Yu' .
;
School of Chemistry and Chemical Engineering
Hunan University of Science and Technology
Hunan 411201
P. R. China
;
'Danhong Ji' .
;
School of Chemistry and Chemical Engineering
Hunan University of Science and Technology
Hunan 411201
P. R. China
;
'Xiaofang Li' .
;
School of Chemistry and Chemical Engineering
Hunan University of Science and Technology
Hunan 411201
P. R. China
;
'Pinggui Yi' .
;
School of Chemistry and Chemical Engineering
Hunan University of Science and Technology
Hunan 411201
P. R. China
;

#==============================================================================
data_a
_database_code_depnum_ccdc_archive 'CCDC 801327'
#TrackingRef 'a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H18 N5 O8 V'
_chemical_formula_weight         375.22

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           ?
_symmetry_space_group_name_H-M   'P 21/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                   7.2721(16)
_cell_length_b                   16.236(4)
_cell_length_c                   12.963(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.622(4)
_cell_angle_gamma                90.00
_cell_volume                     1513.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12607
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         28.26
_reflns_number_total             3537
_reflns_number_gt                3314
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0895P)^2^+4.1539P] 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         3537
_refine_ls_number_parameters     238
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0916
_refine_ls_wR_factor_ref         0.2211
_refine_ls_wR_factor_gt          0.2173
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_restrained_S_all      1.360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.28394(11) 0.28867(4) 0.45660(6) 0.0193(3) Uani 1 1 d . . .
O1 O 0.3389(5) 0.2158(2) 0.5393(3) 0.0300(8) Uani 1 1 d . . .
O2 O 0.5257(5) 0.3235(2) 0.4366(3) 0.0261(7) Uani 1 1 d . . .
O3 O 0.0203(5) 0.2923(2) 0.4533(3) 0.0381(9) Uani 1 1 d . . .
O4 O 0.4376(5) 0.2679(2) 0.3548(3) 0.0288(8) Uani 1 1 d . . .
N1 N 0.3012(5) 0.3801(2) 0.5753(3) 0.0226(8) Uani 1 1 d . . .
O5 O 0.0804(6) 0.2431(2) 0.3689(3) 0.0374(9) Uani 1 1 d . . .
N2 N 0.2163(5) 0.4200(2) 0.3749(3) 0.0218(8) Uani 1 1 d . . .
N3 N 0.1750(8) 0.3766(3) 0.2048(4) 0.0422(12) Uani 1 1 d . . .
H3A H 0.1949 0.3269 0.2266 0.051 Uiso 1 1 calc R . .
H3B H 0.1519 0.3865 0.1390 0.051 Uiso 1 1 calc R . .
N6 N 0.1471(8) 0.5148(3) 0.2345(4) 0.0392(11) Uani 1 1 d . . .
C12 C 0.1798(7) 0.4380(3) 0.2729(4) 0.0255(10) Uani 1 1 d . . .
C13 C 0.2660(6) 0.4606(3) 0.5529(4) 0.0204(9) Uani 1 1 d . . .
C14 C 0.2762(8) 0.5190(3) 0.6324(4) 0.0309(11) Uani 1 1 d . . .
H14A H 0.2505 0.5740 0.6163 0.037 Uiso 1 1 calc R . .
C15 C 0.2229(6) 0.4827(3) 0.4423(4) 0.0215(9) Uani 1 1 d . . .
C17 C 0.1916(8) 0.5633(3) 0.4092(4) 0.0317(11) Uani 1 1 d . . .
H17A H 0.1965 0.6070 0.4560 0.038 Uiso 1 1 calc R . .
C18 C 0.3464(8) 0.3582(3) 0.6750(4) 0.0325(11) Uani 1 1 d . . .
H18A H 0.3689 0.3028 0.6903 0.039 Uiso 1 1 calc R . .
C19 C 0.3612(10) 0.4127(4) 0.7558(4) 0.0408(14) Uani 1 1 d . . .
H19A H 0.3956 0.3948 0.8242 0.049 Uiso 1 1 calc R . .
C20 C 0.3242(9) 0.4952(3) 0.7345(4) 0.0392(14) Uani 1 1 d . . .
H20A H 0.3318 0.5336 0.7882 0.047 Uiso 1 1 calc R . .
C21 C 0.1531(10) 0.5747(3) 0.3033(5) 0.0427(15) Uani 1 1 d . . .
H21A H 0.1298 0.6280 0.2786 0.051 Uiso 1 1 calc R . .
O3W O 0.0704(8) 0.0824(3) 0.4570(4) 0.0518(12) Uani 1 1 d D . .
N8 N 0.7452(6) 0.2923(3) 0.2448(3) 0.0311(10) Uani 1 1 d D . .
H108 H 0.662(5) 0.289(4) 0.273(4) 0.037 Uiso 1 1 d D . .
O2W O -0.2474(6) 0.1946(3) 0.5335(4) 0.0449(11) Uani 1 1 d D . .
H102 H -0.163(6) 0.211(4) 0.505(5) 0.054 Uiso 1 1 d D . .
H202 H -0.326(6) 0.225(4) 0.504(5) 0.054 Uiso 1 1 d D . .
O4W O 0.3392(11) -0.0279(4) 0.5244(6) 0.089(2) Uani 1 1 d D . .
H308 H 0.815(7) 0.259(3) 0.263(6) 0.107 Uiso 1 1 d D . .
H208 H 0.791(9) 0.334(2) 0.257(6) 0.107 Uiso 1 1 d D . .
H408 H 0.715(8) 0.289(5) 0.1867(11) 0.107 Uiso 1 1 d D . .
H103 H 0.089(15) 0.126(4) 0.423(6) 0.107 Uiso 1 1 d D . .
H203 H 0.006(14) 0.062(6) 0.402(5) 0.107 Uiso 1 1 d D . .
H104 H 0.321(13) -0.0788(16) 0.511(9) 0.107 Uiso 1 1 d D . .
H204 H 0.232(6) -0.006(5) 0.511(9) 0.107 Uiso 1 1 d 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 0.0190(4) 0.0135(4) 0.0240(4) 0.0002(3) -0.0009(3) -0.0023(3)
O1 0.037(2) 0.0181(16) 0.0342(19) 0.0050(13) 0.0028(16) 0.0003(14)
O2 0.0196(16) 0.0237(16) 0.0340(19) -0.0001(14) 0.0003(14) -0.0049(13)
O3 0.0260(19) 0.039(2) 0.048(2) 0.0054(18) 0.0030(17) -0.0071(16)
O4 0.0341(19) 0.0219(16) 0.0318(18) -0.0065(14) 0.0092(15) 0.0009(14)
N1 0.0235(19) 0.0184(18) 0.0249(19) 0.0007(15) 0.0003(16) -0.0003(15)
O5 0.034(2) 0.036(2) 0.038(2) 0.0025(17) -0.0099(17) -0.0144(17)
N2 0.0207(18) 0.0191(18) 0.0250(19) 0.0029(15) 0.0016(15) 0.0016(14)
N3 0.071(4) 0.030(2) 0.024(2) 0.0024(18) 0.003(2) 0.014(2)
N6 0.058(3) 0.027(2) 0.030(2) 0.0076(18) -0.001(2) -0.004(2)
C12 0.026(2) 0.023(2) 0.026(2) 0.0021(18) 0.0018(19) 0.0024(18)
C13 0.017(2) 0.017(2) 0.027(2) -0.0007(17) 0.0006(17) -0.0032(16)
C14 0.040(3) 0.020(2) 0.032(3) -0.0044(19) 0.003(2) -0.006(2)
C15 0.018(2) 0.017(2) 0.028(2) 0.0007(17) 0.0001(17) -0.0013(16)
C17 0.038(3) 0.016(2) 0.038(3) -0.0022(19) -0.005(2) -0.001(2)
C18 0.044(3) 0.023(2) 0.028(3) 0.003(2) -0.003(2) 0.001(2)
C19 0.066(4) 0.033(3) 0.021(2) 0.001(2) -0.001(2) -0.006(3)
C20 0.061(4) 0.025(3) 0.030(3) -0.007(2) 0.003(3) -0.010(2)
C21 0.063(4) 0.021(2) 0.040(3) 0.008(2) -0.006(3) -0.002(2)
O3W 0.085(4) 0.031(2) 0.040(2) -0.0005(18) 0.009(2) -0.011(2)
N8 0.0187(19) 0.053(3) 0.0211(19) -0.0003(19) 0.0003(16) 0.0007(19)
O2W 0.039(2) 0.041(2) 0.054(3) 0.010(2) 0.002(2) 0.0059(19)
O4W 0.127(6) 0.036(3) 0.089(4) 0.006(3) -0.033(4) -0.014(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 1.606(3) . ?
V1 O5 1.878(4) . ?
V1 O4 1.882(4) . ?
V1 O2 1.901(3) . ?
V1 O3 1.912(4) . ?
V1 N1 2.128(4) . ?
V1 N2 2.399(4) . ?
O2 O4 1.465(5) . ?
O3 O5 1.472(6) . ?
N1 C18 1.334(6) . ?
N1 C13 1.355(6) . ?
N2 C15 1.337(6) . ?
N2 C12 1.341(6) . ?
N3 C12 1.329(7) . ?
N6 C21 1.317(8) . ?
N6 C12 1.350(6) . ?
C13 C14 1.394(7) . ?
C13 C15 1.465(7) . ?
C14 C20 1.373(8) . ?
C15 C17 1.387(6) . ?
C17 C21 1.372(8) . ?
C18 C19 1.363(8) . ?
C19 C20 1.387(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 O5 102.03(18) . . ?
O1 V1 O4 102.78(18) . . ?
O5 V1 O4 90.12(18) . . ?
O1 V1 O2 99.62(18) . . ?
O5 V1 O2 134.12(18) . . ?
O4 V1 O2 45.56(15) . . ?
O1 V1 O3 100.73(19) . . ?
O5 V1 O3 45.71(19) . . ?
O4 V1 O3 133.48(18) . . ?
O2 V1 O3 158.81(17) . . ?
O1 V1 N1 92.84(17) . . ?
O5 V1 N1 131.92(18) . . ?
O4 V1 N1 130.90(16) . . ?
O2 V1 N1 86.30(15) . . ?
O3 V1 N1 86.85(17) . . ?
O1 V1 N2 164.44(16) . . ?
O5 V1 N2 89.57(16) . . ?
O4 V1 N2 87.36(15) . . ?
O2 V1 N2 78.94(14) . . ?
O3 V1 N2 79.87(15) . . ?
N1 V1 N2 71.63(14) . . ?
O4 O2 V1 66.56(19) . . ?
O5 O3 V1 65.9(2) . . ?
O2 O4 V1 67.88(19) . . ?
C18 N1 C13 118.4(4) . . ?
C18 N1 V1 119.6(3) . . ?
C13 N1 V1 122.0(3) . . ?
O3 O5 V1 68.4(2) . . ?
C15 N2 C12 117.5(4) . . ?
C15 N2 V1 113.7(3) . . ?
C12 N2 V1 128.7(3) . . ?
C21 N6 C12 116.5(5) . . ?
N3 C12 N2 118.3(4) . . ?
N3 C12 N6 117.5(5) . . ?
N2 C12 N6 124.2(5) . . ?
N1 C13 C14 120.7(4) . . ?
N1 C13 C15 116.8(4) . . ?
C14 C13 C15 122.5(4) . . ?
C20 C14 C13 119.9(5) . . ?
N2 C15 C17 121.9(4) . . ?
N2 C15 C13 115.8(4) . . ?
C17 C15 C13 122.3(4) . . ?
C21 C17 C15 115.8(5) . . ?
N1 C18 C19 123.4(5) . . ?
C18 C19 C20 118.9(5) . . ?
C14 C20 C19 118.6(5) . . ?
N6 C21 C17 124.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.140


#==============================================================================
data_a
_database_code_depnum_ccdc_archive 'CCDC 801329'
#TrackingRef 'xiugai8-a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H11 N4 O7 V'
_chemical_formula_weight         338.16

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           ?
_symmetry_space_group_name_H-M   'P n m a'

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

_cell_length_a                   12.9276(14)
_cell_length_b                   6.9044(6)
_cell_length_c                   15.8482(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1414.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3638
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         24.98
_reflns_number_total             1363
_reflns_number_gt                1022
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1363
_refine_ls_number_parameters     121
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.03080(5) 0.2500 -0.22121(4) 0.0263(2) Uani 1 2 d S . .
O1 O 0.04277(17) -0.0184(3) -0.19805(13) 0.0375(5) Uani 1 1 d . . .
O2 O 0.12581(17) 0.0556(3) -0.25275(13) 0.0383(5) Uani 1 1 d . . .
O3 O -0.0530(2) 0.2500 -0.29648(17) 0.0401(8) Uani 1 2 d S . .
N1 N 0.2653(3) 0.2500 -0.0049(2) 0.0431(10) Uani 1 2 d S . .
N2 N 0.1165(3) 0.2500 -0.0917(2) 0.0290(8) Uani 1 2 d S . .
N3 N -0.0843(3) 0.2500 -0.12405(19) 0.0281(8) Uani 1 2 d S . .
C1 C 0.2028(4) 0.2500 0.0630(3) 0.0431(12) Uani 1 2 d S . .
H1A H 0.2327 0.2500 0.1164 0.052 Uiso 1 2 calc SR . .
C2 C 0.0974(4) 0.2500 0.0570(2) 0.0321(10) Uani 1 2 d S . .
H2A H 0.0558 0.2500 0.1049 0.039 Uiso 1 2 calc SR . .
C3 C 0.0548(3) 0.2500 -0.0237(2) 0.0269(9) Uani 1 2 d S . .
C4 C -0.0576(3) 0.2500 -0.0415(2) 0.0266(9) Uani 1 2 d S . .
C5 C -0.1317(3) 0.2500 0.0214(3) 0.0337(10) Uani 1 2 d S . .
H5A H -0.1124 0.2500 0.0779 0.040 Uiso 1 2 calc SR . .
C6 C -0.2347(4) 0.2500 -0.0009(3) 0.0428(12) Uani 1 2 d S . .
H6A H -0.2852 0.2500 0.0409 0.051 Uiso 1 2 calc SR . .
C7 C -0.2631(4) 0.2500 -0.0837(3) 0.0437(12) Uani 1 2 d S . .
H7A H -0.3325 0.2500 -0.0993 0.052 Uiso 1 2 calc SR . .
C8 C -0.1859(4) 0.2500 -0.1436(3) 0.0371(11) Uani 1 2 d S . .
H8A H -0.2047 0.2500 -0.2003 0.045 Uiso 1 2 calc SR . .
C9 C 0.2183(4) 0.2500 -0.0792(3) 0.0356(10) Uani 1 2 d S . .
H9A H 0.2602 0.2500 -0.1269 0.043 Uiso 1 2 calc SR . .
O1W O -0.2399(2) 0.7500 -0.2850(2) 0.0482(9) Uani 1 2 d SD . .
H101 H -0.2840 0.6608 -0.2783 0.072 Uiso 1 1 d RD . .
O2W O -0.5191(4) 0.2500 -0.0013(4) 0.226(5) Uani 1 2 d SD . .
H102 H -0.5369 0.1310 -0.0188 0.339 Uiso 1 1 d RD . .
N4 N -0.0315(3) 0.7500 -0.3265(2) 0.0438(10) Uani 1 2 d S . .

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 0.0279(4) 0.0284(4) 0.0227(4) 0.000 -0.0014(3) 0.000
O1 0.0404(13) 0.0314(11) 0.0407(12) 0.0025(9) 0.0022(10) -0.0041(10)
O2 0.0390(13) 0.0358(12) 0.0399(12) 0.0005(9) 0.0087(10) 0.0035(10)
O3 0.0394(19) 0.0543(19) 0.0268(16) 0.000 -0.0065(14) 0.000
N1 0.036(2) 0.055(2) 0.038(2) 0.000 -0.012(2) 0.000
N2 0.031(2) 0.0291(18) 0.0268(18) 0.000 -0.0030(17) 0.000
N3 0.026(2) 0.0337(18) 0.0248(17) 0.000 -0.0039(16) 0.000
C1 0.050(3) 0.050(3) 0.029(2) 0.000 -0.016(2) 0.000
C2 0.036(3) 0.035(2) 0.025(2) 0.000 -0.003(2) 0.000
C3 0.032(2) 0.0220(19) 0.026(2) 0.000 -0.005(2) 0.000
C4 0.032(2) 0.0237(19) 0.024(2) 0.000 -0.0006(18) 0.000
C5 0.036(3) 0.037(2) 0.028(2) 0.000 0.002(2) 0.000
C6 0.036(3) 0.054(3) 0.039(3) 0.000 0.010(2) 0.000
C7 0.029(3) 0.061(3) 0.041(3) 0.000 0.000(2) 0.000
C8 0.031(3) 0.050(3) 0.030(2) 0.000 -0.005(2) 0.000
C9 0.030(3) 0.040(3) 0.037(2) 0.000 -0.001(2) 0.000
O1W 0.0349(18) 0.0466(19) 0.063(2) 0.000 0.0039(17) 0.000
O2W 0.045(3) 0.552(17) 0.080(4) 0.000 -0.004(3) 0.000
N4 0.035(2) 0.053(2) 0.044(2) 0.000 -0.009(2) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.611(3) . ?
V1 O2 1.887(2) 8_565 ?
V1 O2 1.887(2) . ?
V1 O1 1.895(2) 8_565 ?
V1 O1 1.895(2) . ?
V1 N3 2.141(3) . ?
V1 N2 2.332(3) . ?
O1 O2 1.471(3) . ?
N1 C9 1.325(5) . ?
N1 C1 1.346(6) . ?
N2 C9 1.331(6) . ?
N2 C3 1.342(5) . ?
N3 C8 1.349(6) . ?
N3 C4 1.354(5) . ?
C1 C2 1.365(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.393(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.479(6) . ?
C4 C5 1.383(6) . ?
C5 C6 1.377(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.363(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.378(6) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
O1W H101 0.8457 . ?
O2W H102 0.8974 . ?

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
O3 V1 O2 103.97(10) . 8_565 ?
O3 V1 O2 103.97(10) . . ?
O2 V1 O2 90.70(13) 8_565 . ?
O3 V1 O1 101.43(7) . 8_565 ?
O2 V1 O1 45.78(9) 8_565 8_565 ?
O2 V1 O1 133.92(10) . 8_565 ?
O3 V1 O1 101.43(7) . . ?
O2 V1 O1 133.92(10) 8_565 . ?
O2 V1 O1 45.78(9) . . ?
O1 V1 O1 155.74(13) 8_565 . ?
O3 V1 N3 93.73(15) . . ?
O2 V1 N3 130.00(7) 8_565 . ?
O2 V1 N3 130.00(7) . . ?
O1 V1 N3 85.27(7) 8_565 . ?
O1 V1 N3 85.27(7) . . ?
O3 V1 N2 166.13(15) . . ?
O2 V1 N2 85.63(9) 8_565 . ?
O2 V1 N2 85.63(9) . . ?
O1 V1 N2 77.93(7) 8_565 . ?
O1 V1 N2 77.93(7) . . ?
N3 V1 N2 72.40(13) . . ?
O2 O1 V1 66.81(11) . . ?
O1 O2 V1 67.41(11) . . ?
C9 N1 C1 115.8(4) . . ?
C9 N2 C3 117.9(4) . . ?
C9 N2 V1 126.9(3) . . ?
C3 N2 V1 115.1(3) . . ?
C8 N3 C4 118.1(4) . . ?
C8 N3 V1 120.7(3) . . ?
C4 N3 V1 121.2(3) . . ?
N1 C1 C2 122.9(4) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C1 C2 C3 117.3(4) . . ?
C1 C2 H2A 121.3 . . ?
C3 C2 H2A 121.3 . . ?
N2 C3 C2 120.2(4) . . ?
N2 C3 C4 115.5(3) . . ?
C2 C3 C4 124.3(4) . . ?
N3 C4 C5 121.3(4) . . ?
N3 C4 C3 115.8(4) . . ?
C5 C4 C3 122.9(4) . . ?
C6 C5 C4 119.1(4) . . ?
C6 C5 H5A 120.5 . . ?
C4 C5 H5A 120.5 . . ?
C7 C6 C5 120.5(4) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 H7A 121.0 . . ?
C6 C7 H7A 121.0 . . ?
N3 C8 C7 123.1(4) . . ?
N3 C8 H8A 118.4 . . ?
C7 C8 H8A 118.4 . . ?
N1 C9 N2 125.9(4) . . ?
N1 C9 H9A 117.1 . . ?
N2 C9 H9A 117.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 V1 O1 O2 98.45(16) . . . . ?
O2 V1 O1 O2 -24.02(14) 8_565 . . . ?
O1 V1 O1 O2 -101.3(3) 8_565 . . . ?
N3 V1 O1 O2 -168.69(15) . . . . ?
N2 V1 O1 O2 -95.71(15) . . . . ?
O3 V1 O2 O1 -92.46(14) . . . . ?
O2 V1 O2 O1 162.95(10) 8_565 . . . ?
O1 V1 O2 O1 145.99(18) 8_565 . . . ?
N3 V1 O2 O1 14.78(19) . . . . ?
N2 V1 O2 O1 77.39(13) . . . . ?
O3 V1 N2 C9 180.0 . . . . ?
O2 V1 N2 C9 -45.52(6) 8_565 . . . ?
O2 V1 N2 C9 45.52(6) . . . . ?
O1 V1 N2 C9 -91.18(7) 8_565 . . . ?
O1 V1 N2 C9 91.18(7) . . . . ?
N3 V1 N2 C9 180.0 . . . . ?
O3 V1 N2 C3 0.0 . . . . ?
O2 V1 N2 C3 134.48(6) 8_565 . . . ?
O2 V1 N2 C3 -134.48(6) . . . . ?
O1 V1 N2 C3 88.82(7) 8_565 . . . ?
O1 V1 N2 C3 -88.82(7) . . . . ?
N3 V1 N2 C3 0.0 . . . . ?
O3 V1 N3 C8 0.0 . . . . ?
O2 V1 N3 C8 111.76(12) 8_565 . . . ?
O2 V1 N3 C8 -111.76(12) . . . . ?
O1 V1 N3 C8 101.18(7) 8_565 . . . ?
O1 V1 N3 C8 -101.18(7) . . . . ?
N2 V1 N3 C8 180.0 . . . . ?
O3 V1 N3 C4 180.0 . . . . ?
O2 V1 N3 C4 -68.24(12) 8_565 . . . ?
O2 V1 N3 C4 68.24(12) . . . . ?
O1 V1 N3 C4 -78.82(7) 8_565 . . . ?
O1 V1 N3 C4 78.82(7) . . . . ?
N2 V1 N3 C4 0.0 . . . . ?
C9 N1 C1 C2 0.0 . . . . ?
N1 C1 C2 C3 0.0 . . . . ?
C9 N2 C3 C2 0.0 . . . . ?
V1 N2 C3 C2 180.0 . . . . ?
C9 N2 C3 C4 180.0 . . . . ?
V1 N2 C3 C4 0.0 . . . . ?
C1 C2 C3 N2 0.0 . . . . ?
C1 C2 C3 C4 180.0 . . . . ?
C8 N3 C4 C5 0.0 . . . . ?
V1 N3 C4 C5 180.0 . . . . ?
C8 N3 C4 C3 180.0 . . . . ?
V1 N3 C4 C3 0.0 . . . . ?
N2 C3 C4 N3 0.0 . . . . ?
C2 C3 C4 N3 180.0 . . . . ?
N2 C3 C4 C5 180.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
N3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C6 180.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C4 N3 C8 C7 0.0 . . . . ?
V1 N3 C8 C7 180.0 . . . . ?
C6 C7 C8 N3 0.0 . . . . ?
C1 N1 C9 N2 0.0 . . . . ?
C3 N2 C9 N1 0.0 . . . . ?
V1 N2 C9 N1 180.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.084