
data_global


data_123
#TrackingRef '893011.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H14 Cl0 N7 O3 V'
_chemical_formula_weight         367.25

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'
Cl Cl 0.1484 0.1585 '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)/n

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

_cell_length_a                   9.378(2)
_cell_length_b                   12.245(3)
_cell_length_c                   13.488(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.744(3)
_cell_angle_gamma                90.00
_cell_volume                     1547.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2726
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8247
_exptl_absorpt_correction_T_max  0.8770
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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 SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7548
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2726
_reflns_number_gt                2369
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0695P)²+1.5303P] where P=(Fo²+2Fc²)/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         2726
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.1293
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.20942(5) 0.05399(4) 0.07870(3) 0.03044(19) Uani 1 1 d . . .
C10 C 0.0181(3) -0.0808(2) 0.2047(2) 0.0309(6) Uani 1 1 d . . .
C12 C 0.0066(3) 0.0989(2) 0.2417(2) 0.0315(6) Uani 1 1 d . . .
C13 C 0.0586(3) -0.2654(2) 0.1254(2) 0.0357(7) Uani 1 1 d . . .
C14 C -0.1291(3) -0.0225(2) 0.3237(2) 0.0390(7) Uani 1 1 d . . .
C15 C 0.2062(3) -0.1952(2) 0.0166(2) 0.0384(7) Uani 1 1 d . . .
C16 C 0.0346(3) 0.3056(2) 0.2494(2) 0.0361(7) Uani 1 1 d . . .
C17 C 0.1183(3) 0.3715(2) 0.1944(2) 0.0408(7) Uani 1 1 d . . .
H17A H 0.1257 0.4470 0.1999 0.049 Uiso 1 1 calc R . .
C18 C 0.3019(4) -0.1774(3) -0.0672(3) 0.0514(9) Uani 1 1 d . . .
H18A H 0.3318 -0.1024 -0.0679 0.077 Uiso 1 1 calc R . .
H18B H 0.2514 -0.1945 -0.1288 0.077 Uiso 1 1 calc R . .
H18C H 0.3842 -0.2237 -0.0589 0.077 Uiso 1 1 calc R . .
C19 C 0.1900(3) 0.3066(2) 0.1292(2) 0.0356(7) Uani 1 1 d . . .
C20 C -0.0381(4) -0.3336(3) 0.1834(3) 0.0439(8) Uani 1 1 d . . .
H20A H -0.0772 -0.2902 0.2348 0.066 Uiso 1 1 calc R . .
H20B H 0.0144 -0.3937 0.2127 0.066 Uiso 1 1 calc R . .
H20C H -0.1142 -0.3611 0.1402 0.066 Uiso 1 1 calc R . .
C21 C 0.1380(3) -0.2909(2) 0.0461(2) 0.0424(7) Uani 1 1 d . . .
H21A H 0.1454 -0.3594 0.0170 0.051 Uiso 1 1 calc R . .
C22 C 0.2934(4) 0.3378(3) 0.0531(3) 0.0496(8) Uani 1 1 d . . .
H22A H 0.3242 0.2734 0.0195 0.074 Uiso 1 1 calc R . .
H22B H 0.3745 0.3733 0.0851 0.074 Uiso 1 1 calc R . .
H22C H 0.2479 0.3867 0.0058 0.074 Uiso 1 1 calc R . .
C24 C -0.0651(4) 0.3327(3) 0.3276(3) 0.0515(9) Uani 1 1 d . . .
H24A H -0.1079 0.2669 0.3509 0.077 Uiso 1 1 calc R . .
H24B H -0.1384 0.3805 0.3008 0.077 Uiso 1 1 calc R . .
H24C H -0.0138 0.3683 0.3818 0.077 Uiso 1 1 calc R . .
O2 O 0.3785(2) 0.05680(18) 0.10261(19) 0.0473(6) Uani 1 1 d . . .
O3 O 0.1757(3) 0.0819(2) -0.03661(16) 0.0490(6) Uani 1 1 d . . .
O1 O -0.2176(3) -0.04266(19) 0.3840(2) 0.0596(7) Uani 1 1 d . . .
N1 N 0.0663(3) 0.02114(19) 0.18594(18) 0.0327(5) Uani 1 1 d . . .
N2 N -0.0711(3) -0.1091(2) 0.26937(17) 0.0357(6) Uani 1 1 d . . .
N3 N -0.0863(3) 0.0860(2) 0.30798(19) 0.0389(6) Uani 1 1 d . . .
N4 N 0.0580(3) 0.20211(19) 0.21610(18) 0.0345(6) Uani 1 1 d . . .
N5 N 0.1539(3) 0.20243(19) 0.14165(17) 0.0343(6) Uani 1 1 d . . .
N6 N 0.1713(3) -0.1136(2) 0.07528(17) 0.0343(5) Uani 1 1 d . . .
N7 N 0.0816(2) -0.15676(19) 0.14312(17) 0.0315(5) Uani 1 1 d . . .


_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 O2 1.603(2) . ?
V1 O3 1.609(2) . ?
V1 N1 2.059(2) . ?
V1 N5 2.083(2) . ?
V1 N6 2.083(2) . ?
C10 N2 1.285(4) . ?
C10 N1 1.356(4) . ?
C10 N7 1.399(4) . ?
C12 N3 1.288(4) . ?
C12 N1 1.351(4) . ?
C12 N4 1.402(4) . ?
C13 N7 1.367(4) . ?
C13 C21 1.369(4) . ?
C13 C20 1.483(4) . ?
C14 O1 1.215(4) . ?
C14 N3 1.408(4) . ?
C14 N2 1.412(4) . ?
C15 N6 1.326(4) . ?
C15 C21 1.401(4) . ?
C15 C18 1.493(4) . ?
C16 N4 1.366(4) . ?
C16 C17 1.369(4) . ?
C16 C24 1.480(4) . ?
C17 C19 1.384(4) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N5 1.332(4) . ?
C19 C22 1.495(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
N4 N5 1.379(3) . ?
N6 N7 1.378(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
O2 V1 O3 109.67(13) . . ?
O2 V1 N1 122.30(12) . . ?
O3 V1 N1 128.02(11) . . ?
O2 V1 N5 99.41(11) . . ?
O3 V1 N5 99.62(11) . . ?
N1 V1 N5 72.55(9) . . ?
O2 V1 N6 101.10(11) . . ?
O3 V1 N6 99.35(11) . . ?
N1 V1 N6 72.92(9) . . ?
N5 V1 N6 145.37(9) . . ?
N2 C10 N1 127.5(3) . . ?
N2 C10 N7 122.2(3) . . ?
N1 C10 N7 110.2(2) . . ?
N3 C12 N1 127.7(3) . . ?
N3 C12 N4 122.3(3) . . ?
N1 C12 N4 110.0(2) . . ?
N7 C13 C21 105.7(3) . . ?
N7 C13 C20 123.5(3) . . ?
C21 C13 C20 130.8(3) . . ?
O1 C14 N3 120.1(3) . . ?
O1 C14 N2 119.2(3) . . ?
N3 C14 N2 120.7(3) . . ?
N6 C15 C21 109.4(3) . . ?
N6 C15 C18 121.1(3) . . ?
C21 C15 C18 129.5(3) . . ?
N4 C16 C17 105.3(3) . . ?
N4 C16 C24 124.0(3) . . ?
C17 C16 C24 130.7(3) . . ?
C16 C17 C19 108.3(3) . . ?
C16 C17 H17A 125.8 . . ?
C19 C17 H17A 125.8 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C17 109.6(3) . . ?
N5 C19 C22 120.6(3) . . ?
C17 C19 C22 129.8(3) . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C21 C15 107.7(3) . . ?
C13 C21 H21A 126.1 . . ?
C15 C21 H21A 126.1 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C24 H24A 109.5 . . ?
C16 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C16 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C12 N1 C10 113.2(2) . . ?
C12 N1 V1 123.67(19) . . ?
C10 N1 V1 123.07(18) . . ?
C10 N2 C14 115.5(2) . . ?
C12 N3 C14 115.4(2) . . ?
C16 N4 N5 110.9(2) . . ?
C16 N4 C12 133.9(2) . . ?
N5 N4 C12 115.2(2) . . ?
C19 N5 N4 105.8(2) . . ?
C19 N5 V1 135.6(2) . . ?
N4 N5 V1 118.59(17) . . ?
C15 N6 N7 106.4(2) . . ?
C15 N6 V1 135.2(2) . . ?
N7 N6 V1 118.21(17) . . ?
C13 N7 N6 110.7(2) . . ?
C13 N7 C10 133.1(2) . . ?
N6 N7 C10 115.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.069

data_global

# Attachment '893015.cif'


data_2
#TrackingRef '893015.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H24 N10 O S2 V'
_chemical_formula_weight         523.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.447(3)
_cell_length_b                   8.7943(18)
_cell_length_c                   22.021(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.599(3)
_cell_angle_gamma                90.00
_cell_volume                     2508.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1152
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      18.18

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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 SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9995
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         22.80
_reflns_number_total             3408
_reflns_number_gt                2206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0592P)²+1.3873P] where P=(Fo²+2Fc²)/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         3408
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.82298(6) 0.22398(10) 1.11863(4) 0.0402(3) Uani 1 1 d . . .
O O 0.8719(3) 0.1789(4) 1.19032(15) 0.0581(10) Uani 1 1 d . . .
C1 C 0.7952(5) 0.5321(7) 1.2236(2) 0.083(2) Uani 1 1 d . . .
H1A H 0.8296 0.4355 1.2310 0.124 Uiso 1 1 calc R . .
H1B H 0.7434 0.5366 1.2463 0.124 Uiso 1 1 calc R . .
H1C H 0.8445 0.6120 1.2379 0.124 Uiso 1 1 calc R . .
C2 C 0.6873(5) 0.6724(7) 1.1223(3) 0.0711(18) Uani 1 1 d . . .
H2A H 0.6704 0.7608 1.1404 0.085 Uiso 1 1 calc R . .
C3 C 0.6603(4) 0.6395(6) 1.0606(3) 0.0568(15) Uani 1 1 d . . .
C4 C 0.5984(5) 0.7268(7) 1.0055(3) 0.082(2) Uani 1 1 d . . .
H4A H 0.5796 0.8234 1.0195 0.124 Uiso 1 1 calc R . .
H4B H 0.5371 0.6708 0.9854 0.124 Uiso 1 1 calc R . .
H4C H 0.6387 0.7427 0.9761 0.124 Uiso 1 1 calc R . .
N4 N 0.6994(3) 0.4970(5) 1.05502(18) 0.0448(11) Uani 1 1 d . . .
C6 C 0.9502(5) -0.1443(7) 1.1374(3) 0.079(2) Uani 1 1 d . . .
H6A H 0.9426 -0.0678 1.1670 0.118 Uiso 1 1 calc R . .
H6B H 1.0222 -0.1630 1.1423 0.118 Uiso 1 1 calc R . .
H6C H 0.9174 -0.2365 1.1452 0.118 Uiso 1 1 calc R . .
C7 C 0.8939(4) -0.1632(6) 1.0149(3) 0.0642(17) Uani 1 1 d . . .
H7A H 0.9211 -0.2581 1.0098 0.077 Uiso 1 1 calc R . .
C8 C 0.8402(4) -0.0712(6) 0.9678(3) 0.0554(15) Uani 1 1 d . . .
C9 C 0.8097(5) -0.0904(7) 0.8980(2) 0.0761(19) Uani 1 1 d . . .
H9A H 0.7716 -0.0027 0.8786 0.114 Uiso 1 1 calc R . .
H9B H 0.7673 -0.1794 0.8869 0.114 Uiso 1 1 calc R . .
H9C H 0.8704 -0.1015 0.8834 0.114 Uiso 1 1 calc R . .
N1 N 0.8149(3) 0.0547(5) 0.99719(18) 0.0424(10) Uani 1 1 d . . .
C11 C 0.7584(3) 0.1852(6) 0.9747(2) 0.0387(12) Uani 1 1 d . . .
C12 C 0.7000(4) 0.4048(6) 1.0037(2) 0.0390(12) Uani 1 1 d . . .
C13 C 0.6621(4) 0.3399(6) 0.9026(2) 0.0441(13) Uani 1 1 d . . .
C14 C 0.6166(4) 0.2630(7) 0.7912(2) 0.0667(17) Uani 1 1 d . . .
H14A H 0.5533 0.2772 0.7580 0.080 Uiso 1 1 calc R . .
H14B H 0.6168 0.1597 0.8066 0.080 Uiso 1 1 calc R . .
C15 C 0.7052(6) 0.2826(9) 0.7644(3) 0.107(3) Uani 1 1 d . . .
H15A H 0.7008 0.2097 0.7313 0.160 Uiso 1 1 calc R . .
H15B H 0.7683 0.2674 0.7968 0.160 Uiso 1 1 calc R . .
H15C H 0.7043 0.3835 0.7476 0.160 Uiso 1 1 calc R . .
C16 C 0.5911(6) 0.5854(14) 0.8184(4) 0.162(5) Uani 1 1 d . . .
H16A H 0.5741 0.6895 0.8071 0.243 Uiso 1 1 calc R . .
H16B H 0.6160 0.5374 0.7861 0.243 Uiso 1 1 calc R . .
H16C H 0.6437 0.5816 0.8577 0.243 Uiso 1 1 calc R . .
C17 C 0.5123(10) 0.5171(14) 0.8239(4) 0.202(7) Uani 1 1 d . . .
H17A H 0.4582 0.5017 0.7852 0.242 Uiso 1 1 calc R . .
H17B H 0.4860 0.5489 0.8588 0.242 Uiso 1 1 calc R . .
C18 C 0.6034(4) 0.0780(6) 1.1137(2) 0.0435(13) Uani 1 1 d . . .
C19 C 1.0137(4) 0.4147(6) 1.1002(2) 0.0494(14) Uani 1 1 d . . .
C10 C 0.9010(4) -0.0910(6) 1.0721(3) 0.0539(14) Uani 1 1 d . . .
N2 N 0.8530(3) 0.0425(5) 1.06221(18) 0.0449(11) Uani 1 1 d . . .
N3 N 0.7523(3) 0.4407(5) 1.11412(18) 0.0434(11) Uani 1 1 d . . .
C5 C 0.7453(4) 0.5509(7) 1.1546(2) 0.0544(15) Uani 1 1 d . . .
N5 N 0.6814(3) 0.1317(5) 1.11230(19) 0.0509(12) Uani 1 1 d . . .
N6 N 0.9485(3) 0.3344(5) 1.1063(2) 0.0553(12) Uani 1 1 d . . .
N7 N 0.7548(3) 0.2796(5) 1.02124(17) 0.0386(10) Uani 1 1 d . . .
N8 N 0.6523(3) 0.4445(5) 0.94632(19) 0.0464(11) Uani 1 1 d . . .
N9 N 0.7160(3) 0.2065(5) 0.91498(18) 0.0404(10) Uani 1 1 d . . .
N10 N 0.6172(4) 0.3686(5) 0.8427(2) 0.0655(14) Uani 1 1 d . . .
S1 S 1.10489(12) 0.5236(2) 1.09121(10) 0.0849(6) Uani 1 1 d . . .
S2 S 0.49574(11) 0.00042(19) 1.11599(8) 0.0690(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V O 1.589(3) . ?
V N6 2.027(5) . ?
V N5 2.039(5) . ?
V N3 2.120(4) . ?
V N2 2.127(4) . ?
V N7 2.150(4) . ?
C1 C5 1.497(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.339(7) . ?
C2 C5 1.399(7) . ?
C2 H2A 0.9300 . ?
C3 N4 1.377(6) . ?
C3 C4 1.487(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
N4 C12 1.393(6) . ?
N4 N3 1.395(5) . ?
C6 C10 1.489(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.359(7) . ?
C7 C10 1.390(7) . ?
C7 H7A 0.9300 . ?
C8 N1 1.372(6) . ?
C8 C9 1.491(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N1 N2 1.389(5) . ?
N1 C11 1.392(6) . ?
C11 N9 1.298(6) . ?
C11 N7 1.330(6) . ?
C12 N8 1.301(6) . ?
C12 N7 1.324(6) . ?
C13 N10 1.320(6) . ?
C13 N8 1.362(6) . ?
C13 N9 1.368(6) . ?
C14 N10 1.464(7) . ?
C14 C15 1.475(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.251(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N10 1.885(15) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N5 1.158(6) . ?
C18 S2 1.613(6) . ?
C19 N6 1.162(6) . ?
C19 S1 1.610(6) . ?
C10 N2 1.329(6) . ?
N3 C5 1.337(6) . ?

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
O V N6 96.61(18) . . ?
O V N5 95.62(17) . . ?
N6 V N5 167.62(17) . . ?
O V N3 109.36(17) . . ?
N6 V N3 86.67(16) . . ?
N5 V N3 87.49(16) . . ?
O V N2 107.48(17) . . ?
N6 V N2 89.19(17) . . ?
N5 V N2 88.95(17) . . ?
N3 V N2 143.16(15) . . ?
O V N7 178.56(18) . . ?
N6 V N7 84.54(16) . . ?
N5 V N7 83.26(15) . . ?
N3 V N7 71.54(15) . . ?
N2 V N7 71.63(15) . . ?
C5 C1 H1A 109.5 . . ?
C5 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C5 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C5 108.2(5) . . ?
C3 C2 H2A 125.9 . . ?
C5 C2 H2A 125.9 . . ?
C2 C3 N4 106.3(5) . . ?
C2 C3 C4 130.9(5) . . ?
N4 C3 C4 122.7(5) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 N4 C12 133.5(4) . . ?
C3 N4 N3 110.5(4) . . ?
C12 N4 N3 116.0(4) . . ?
C10 C6 H6A 109.5 . . ?
C10 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C10 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C10 108.2(5) . . ?
C8 C7 H7A 125.9 . . ?
C10 C7 H7A 125.9 . . ?
C7 C8 N1 105.6(4) . . ?
C7 C8 C9 131.5(5) . . ?
N1 C8 C9 122.9(5) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 N1 N2 110.7(4) . . ?
C8 N1 C11 132.8(4) . . ?
N2 N1 C11 116.5(4) . . ?
N9 C11 N7 126.4(5) . . ?
N9 C11 N1 121.9(5) . . ?
N7 C11 N1 111.6(4) . . ?
N8 C12 N7 126.6(5) . . ?
N8 C12 N4 121.5(5) . . ?
N7 C12 N4 111.8(4) . . ?
N10 C13 N8 118.2(5) . . ?
N10 C13 N9 116.0(5) . . ?
N8 C13 N9 125.8(4) . . ?
N10 C14 C15 113.5(5) . . ?
N10 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
N10 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C16 C17 N10 75.6(10) . . ?
C16 C17 H17A 115.9 . . ?
N10 C17 H17A 115.9 . . ?
C16 C17 H17B 115.9 . . ?
N10 C17 H17B 115.9 . . ?
H17A C17 H17B 112.9 . . ?
N5 C18 S2 179.0(5) . . ?
N6 C19 S1 179.0(5) . . ?
N2 C10 C7 110.1(5) . . ?
N2 C10 C6 120.4(5) . . ?
C7 C10 C6 129.5(5) . . ?
C10 N2 N1 105.4(4) . . ?
C10 N2 V 136.7(4) . . ?
N1 N2 V 117.9(3) . . ?
C5 N3 N4 104.8(4) . . ?
C5 N3 V 137.0(3) . . ?
N4 N3 V 118.2(3) . . ?
N3 C5 C2 110.1(5) . . ?
N3 C5 C1 120.3(5) . . ?
C2 C5 C1 129.6(5) . . ?
C18 N5 V 174.7(4) . . ?
C19 N6 V 171.2(4) . . ?
C12 N7 C11 115.2(4) . . ?
C12 N7 V 122.3(3) . . ?
C11 N7 V 122.2(3) . . ?
C12 N8 C13 112.9(4) . . ?
C11 N9 C13 113.0(4) . . ?
C13 N10 C14 124.0(5) . . ?
C13 N10 C17 117.7(5) . . ?
C14 N10 C17 114.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        22.80
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.061



data_global

# Attachment '893012.cif'


data_1
#TrackingRef '893012.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H52 N16 O14 V2'
_chemical_formula_weight         1082.86

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.3562(10)
_cell_length_b                   11.9681(12)
_cell_length_c                   11.9868(12)
_cell_angle_alpha                60.215(2)
_cell_angle_beta                 84.303(2)
_cell_angle_gamma                81.998(2)
_cell_volume                     1152.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1884
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.11

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             562
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7984
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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 SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5645
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4010
_reflns_number_gt                3062
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0670P)²+1.2136P] where P=(Fo²+2Fc²)/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         4010
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1332
_refine_ls_wR_factor_gt          0.1240
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H1WB H 0.531(8) 0.859(7) 0.447(7) 0.11(3) Uiso 1 1 d . . .
V1 V 0.14374(6) 0.43096(5) 0.21811(6) 0.02291(18) Uani 1 1 d . . .
C8 C -0.0229(4) 0.6168(3) 0.3054(3) 0.0232(7) Uani 1 1 d . . .
C15 C 0.0277(4) 0.8152(3) 0.2521(3) 0.0263(8) Uani 1 1 d . . .
C16 C 0.0379(3) 0.5620(3) -0.0355(3) 0.0227(7) Uani 1 1 d . . .
C17 C 0.1922(4) 0.6809(3) 0.2146(3) 0.0227(7) Uani 1 1 d . . .
C18 C -0.1363(4) 0.3170(3) 0.4208(3) 0.0276(8) Uani 1 1 d . . .
C19 C -0.2335(4) 0.4912(3) 0.4346(3) 0.0260(8) Uani 1 1 d . . .
C20 C 0.4920(4) 0.4994(4) 0.1745(3) 0.0291(8) Uani 1 1 d . . .
C21 C 0.2898(4) 0.1808(4) 0.3547(4) 0.0345(9) Uani 1 1 d . . .
C22 C -0.2533(4) 0.3659(3) 0.4732(3) 0.0293(8) Uani 1 1 d . . .
H22A H -0.3316 0.3196 0.5267 0.035 Uiso 1 1 d R . .
C23 C 0.3127(4) 0.2189(4) 0.2116(4) 0.0314(8) Uani 1 1 d . . .
C24 C 0.0913(4) 1.0279(3) 0.1930(4) 0.0336(9) Uani 1 1 d . . .
H24A H 0.1861 0.9848 0.2246 0.040 Uiso 1 1 calc R . .
H24B H 0.0628 1.0866 0.2269 0.040 Uiso 1 1 calc R . .
C25 C -0.1125(4) 0.1839(3) 0.4353(4) 0.0366(9) Uani 1 1 d . . .
H25A H -0.0248 0.1760 0.3897 0.055 Uiso 1 1 d R . .
H25B H -0.1055 0.1205 0.5247 0.055 Uiso 1 1 d R . .
H25C H -0.1923 0.1703 0.4004 0.055 Uiso 1 1 d R . .
C26 C 0.4556(4) 0.7011(3) 0.1438(3) 0.0299(8) Uani 1 1 d . . .
C27 C 0.5580(4) 0.6114(4) 0.1407(4) 0.0359(9) Uani 1 1 d . . .
H27A H 0.6587 0.6218 0.1191 0.043 Uiso 1 1 d R . .
C28 C 0.1019(5) 1.1061(4) 0.0472(4) 0.0455(11) Uani 1 1 d . . .
H28A H 0.1711 1.1675 0.0217 0.068 Uiso 1 1 calc R . .
H28B H 0.0092 1.1513 0.0151 0.068 Uiso 1 1 calc R . .
H28C H 0.1320 1.0490 0.0127 0.068 Uiso 1 1 calc R . .
C29 C -0.3222(4) 0.5903(4) 0.4602(4) 0.0357(9) Uani 1 1 d . . .
H29A H -0.2774 0.6694 0.4176 0.054 Uiso 1 1 calc R . .
H29B H -0.3291 0.5595 0.5511 0.054 Uiso 1 1 calc R . .
H29C H -0.4172 0.6057 0.4283 0.054 Uiso 1 1 calc R . .
C30 C 0.5663(4) 0.3773(4) 0.1840(5) 0.0448(11) Uani 1 1 d . . .
H30A H 0.4973 0.3160 0.2087 0.067 Uiso 1 1 calc R . .
H30B H 0.6390 0.3425 0.2473 0.067 Uiso 1 1 calc R . .
H30C H 0.6108 0.3944 0.1021 0.067 Uiso 1 1 calc R . .
C32 C -0.1554(5) 0.9609(4) 0.2897(4) 0.0428(11) Uani 1 1 d . . .
H32A H -0.1427 0.9814 0.3566 0.051 Uiso 1 1 calc R . .
H32B H -0.2078 0.8851 0.3277 0.051 Uiso 1 1 calc R . .
C34 C 0.4688(5) 0.8351(4) 0.1173(5) 0.0472(11) Uani 1 1 d . . .
H34A H 0.5674 0.8536 0.0940 0.071 Uiso 1 1 calc R . .
H34B H 0.4395 0.8418 0.1930 0.071 Uiso 1 1 calc R . .
H34C H 0.4081 0.8959 0.0480 0.071 Uiso 1 1 calc R . .
C35 C -0.2436(6) 1.0719(6) 0.1868(6) 0.0792(18) Uani 1 1 d . . .
H35A H -0.3352 1.0873 0.2232 0.119 Uiso 1 1 calc R . .
H35B H -0.2587 1.0516 0.1210 0.119 Uiso 1 1 calc R . .
H35C H -0.1936 1.1480 0.1500 0.119 Uiso 1 1 calc R . .
O1 O -0.0195(3) 0.3715(2) 0.1536(2) 0.0296(6) Uani 1 1 d . . .
O1W O 0.4834(5) 0.8660(4) 0.3942(5) 0.0749(12) Uani 1 1 d . . .
H1WA H 0.4178 0.9192 0.4012 0.112 Uiso 1 1 d R . .
O2 O 0.1111(3) 0.5850(2) 0.0314(2) 0.0278(6) Uani 1 1 d . . .
O3 O 0.2581(3) 0.3363(2) 0.1352(2) 0.0343(6) Uani 1 1 d . . .
O4 O 0.2181(3) 0.2711(2) 0.3735(2) 0.0317(6) Uani 1 1 d . . .
O5 O 0.3769(3) 0.1442(3) 0.1788(3) 0.0444(7) Uani 1 1 d . . .
O6 O 0.3374(4) 0.0756(3) 0.4388(3) 0.0725(11) Uani 1 1 d . . .
N1 N 0.1029(3) 0.5886(3) 0.2561(3) 0.0241(6) Uani 1 1 d . . .
N2 N 0.1634(3) 0.7941(3) 0.2082(3) 0.0267(7) Uani 1 1 d . . .
N3 N -0.0692(3) 0.7241(3) 0.3063(3) 0.0272(7) Uani 1 1 d . . .
N4 N -0.1068(3) 0.5137(3) 0.3607(3) 0.0253(6) Uani 1 1 d . . .
N5 N -0.0464(3) 0.4050(3) 0.3532(3) 0.0259(7) Uani 1 1 d . . .
N6 N 0.3283(3) 0.6432(3) 0.1798(3) 0.0259(7) Uani 1 1 d . . .
N7 N 0.3506(3) 0.5177(3) 0.1982(3) 0.0260(7) Uani 1 1 d . . .
N8 N -0.0120(3) 0.9299(3) 0.2426(3) 0.0300(7) Uani 1 1 d . . .


_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 O4 1.990(2) . ?
V1 O3 1.996(2) . ?
V1 O2 2.094(2) . ?
V1 O1 2.127(2) . ?
V1 N1 2.129(3) . ?
V1 N5 2.229(3) . ?
V1 N7 2.259(3) . ?
C8 N3 1.302(4) . ?
C8 N1 1.341(4) . ?
C8 N4 1.390(4) . ?
C15 N8 1.321(4) . ?
C15 N2 1.364(4) . ?
C15 N3 1.374(4) . ?
C16 O1 1.249(4) 2_565 ?
C16 O2 1.253(4) . ?
C16 C16 1.532(6) 2_565 ?
C17 N2 1.309(4) . ?
C17 N1 1.340(4) . ?
C17 N6 1.386(4) . ?
C18 N5 1.317(4) . ?
C18 C22 1.410(5) . ?
C18 C25 1.500(5) . ?
C19 C22 1.366(5) . ?
C19 N4 1.380(4) . ?
C19 C29 1.493(5) . ?
C20 N7 1.336(4) . ?
C20 C27 1.407(5) . ?
C20 C30 1.484(5) . ?
C21 O6 1.213(5) . ?
C21 O4 1.296(4) . ?
C21 C23 1.541(5) . ?
C22 H22A 0.9600 . ?
C23 O5 1.211(4) . ?
C23 O3 1.299(4) . ?
C24 N8 1.474(4) . ?
C24 C28 1.519(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9599 . ?
C26 C27 1.349(5) . ?
C26 N6 1.384(4) . ?
C26 C34 1.493(5) . ?
C27 H27A 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 N8 1.475(5) . ?
C32 C35 1.495(7) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
O1 C16 1.249(4) 2_565 ?
O1W H1WB 0.78(7) . ?
O1W H1WA 0.8500 . ?
N4 N5 1.387(4) . ?
N6 N7 1.393(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
O4 V1 O3 79.97(10) . . ?
O4 V1 O2 165.19(10) . . ?
O3 V1 O2 86.26(10) . . ?
O4 V1 O1 104.53(10) . . ?
O3 V1 O1 77.34(10) . . ?
O2 V1 O1 77.44(9) . . ?
O4 V1 N1 110.30(11) . . ?
O3 V1 N1 152.20(11) . . ?
O2 V1 N1 79.81(10) . . ?
O1 V1 N1 122.03(10) . . ?
O4 V1 N5 79.96(10) . . ?
O3 V1 N5 138.58(11) . . ?
O2 V1 N5 114.34(10) . . ?
O1 V1 N5 73.22(10) . . ?
N1 V1 N5 69.20(10) . . ?
O4 V1 N7 89.62(11) . . ?
O3 V1 N7 85.10(10) . . ?
O2 V1 N7 83.76(10) . . ?
O1 V1 N7 154.94(10) . . ?
N1 V1 N7 69.64(10) . . ?
N5 V1 N7 130.47(10) . . ?
N3 C8 N1 127.9(3) . . ?
N3 C8 N4 120.4(3) . . ?
N1 C8 N4 111.8(3) . . ?
N8 C15 N2 117.8(3) . . ?
N8 C15 N3 118.2(3) . . ?
N2 C15 N3 123.9(3) . . ?
O1 C16 O2 127.4(3) 2_565 . ?
O1 C16 C16 116.2(4) 2_565 2_565 ?
O2 C16 C16 116.4(4) . 2_565 ?
N2 C17 N1 127.0(3) . . ?
N2 C17 N6 120.8(3) . . ?
N1 C17 N6 112.2(3) . . ?
N5 C18 C22 111.2(3) . . ?
N5 C18 C25 122.3(3) . . ?
C22 C18 C25 126.5(3) . . ?
C22 C19 N4 105.3(3) . . ?
C22 C19 C29 131.1(3) . . ?
N4 C19 C29 123.7(3) . . ?
N7 C20 C27 110.3(3) . . ?
N7 C20 C30 123.9(3) . . ?
C27 C20 C30 125.8(3) . . ?
O6 C21 O4 125.1(4) . . ?
O6 C21 C23 121.3(3) . . ?
O4 C21 C23 113.6(3) . . ?
C19 C22 C18 107.1(3) . . ?
C19 C22 H22A 126.5 . . ?
C18 C22 H22A 126.4 . . ?
O5 C23 O3 126.0(4) . . ?
O5 C23 C21 121.3(4) . . ?
O3 C23 C21 112.8(3) . . ?
N8 C24 C28 113.9(3) . . ?
N8 C24 H24A 108.8 . . ?
C28 C24 H24A 108.8 . . ?
N8 C24 H24B 108.8 . . ?
C28 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C18 C25 H25A 109.5 . . ?
C18 C25 H25B 109.6 . . ?
H25A C25 H25B 109.5 . . ?
C18 C25 H25C 109.3 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N6 105.5(3) . . ?
C27 C26 C34 129.7(3) . . ?
N6 C26 C34 124.7(3) . . ?
C26 C27 C20 108.2(3) . . ?
C26 C27 H27A 126.0 . . ?
C20 C27 H27A 125.8 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C19 C29 H29A 109.5 . . ?
C19 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C19 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C20 C30 H30A 109.5 . . ?
C20 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C20 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N8 C32 C35 113.4(4) . . ?
N8 C32 H32A 108.9 . . ?
C35 C32 H32A 108.9 . . ?
N8 C32 H32B 108.9 . . ?
C35 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C16 O1 V1 113.5(2) 2_565 . ?
H1WB O1W H1WA 95.8 . . ?
C16 O2 V1 114.3(2) . . ?
C23 O3 V1 116.7(2) . . ?
C21 O4 V1 116.6(2) . . ?
C17 N1 C8 112.9(3) . . ?
C17 N1 V1 122.7(2) . . ?
C8 N1 V1 123.7(2) . . ?
C17 N2 C15 114.3(3) . . ?
C8 N3 C15 113.6(3) . . ?
C19 N4 N5 111.6(3) . . ?
C19 N4 C8 132.9(3) . . ?
N5 N4 C8 115.1(3) . . ?
C18 N5 N4 104.9(3) . . ?
C18 N5 V1 138.0(2) . . ?
N4 N5 V1 116.41(19) . . ?
C26 N6 C17 131.9(3) . . ?
C26 N6 N7 111.3(3) . . ?
C17 N6 N7 116.2(3) . . ?
C20 N7 N6 104.6(3) . . ?
C20 N7 V1 140.4(2) . . ?
N6 N7 V1 113.5(2) . . ?
C15 N8 C24 120.3(3) . . ?
C15 N8 C32 121.8(3) . . ?
C24 N8 C32 117.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.071

data_global

# Attachment '893013.cif'


data_1a
#TrackingRef '893013.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H17 N5 O7 S V'
_chemical_formula_weight         438.32

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.0090(17)
_cell_length_b                   12.111(3)
_cell_length_c                   18.060(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.664(3)
_cell_angle_gamma                90.00
_cell_volume                     1749.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1395
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      21.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8090
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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 SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10503
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.90
_reflns_number_total             4108
_reflns_number_gt                2599
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0746P)²+0.0000P] where P=(Fo²+2Fc²)/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         4108
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1535
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.23560(8) 0.74153(5) 0.01966(3) 0.02677(19) Uani 1 1 d . . .
S S 0.24654(12) 0.95259(7) -0.08811(5) 0.0290(2) Uani 1 1 d . . .
C1 C 0.2293(5) 0.6105(3) 0.15924(19) 0.0321(8) Uani 1 1 d . . .
C2 C 0.1713(5) 0.5395(3) 0.2118(2) 0.0390(10) Uani 1 1 d . . .
H2A H 0.2350 0.5235 0.2548 0.047 Uiso 1 1 calc R . .
C3 C 0.0155(5) 0.4929(3) 0.1984(2) 0.0414(10) Uani 1 1 d . . .
H3A H -0.0262 0.4441 0.2327 0.050 Uiso 1 1 calc R . .
C4 C -0.0802(5) 0.5178(3) 0.1341(2) 0.0372(9) Uani 1 1 d . . .
H4A H -0.1846 0.4858 0.1247 0.045 Uiso 1 1 calc R . .
C5 C -0.0158(5) 0.5909(3) 0.0851(2) 0.0298(8) Uani 1 1 d . . .
C6 C 0.3903(5) 0.6698(3) 0.16394(19) 0.0297(8) Uani 1 1 d . . .
C7 C 0.5235(5) 0.6696(3) 0.2148(2) 0.0374(9) Uani 1 1 d . . .
H7A H 0.5348 0.6279 0.2580 0.045 Uiso 1 1 calc R . .
C8 C 0.6368(5) 0.7440(3) 0.1886(2) 0.0367(9) Uani 1 1 d . . .
C9 C 0.8022(5) 0.7808(3) 0.2207(2) 0.0424(10) Uani 1 1 d . . .
H9A H 0.8498 0.8338 0.1882 0.064 Uiso 1 1 calc R . .
H9B H 0.8755 0.7184 0.2263 0.064 Uiso 1 1 calc R . .
H9C H 0.7880 0.8140 0.2683 0.064 Uiso 1 1 calc R . .
C10 C -0.0991(5) 0.6344(3) 0.01663(19) 0.0297(8) Uani 1 1 d . . .
C11 C -0.2511(5) 0.6134(3) -0.0207(2) 0.0352(9) Uani 1 1 d . . .
H11A H -0.3327 0.5634 -0.0076 0.042 Uiso 1 1 calc R . .
C12 C -0.2554(5) 0.6826(3) -0.0817(2) 0.0362(9) Uani 1 1 d . . .
C13 C -0.3830(5) 0.6988(4) -0.1432(2) 0.0464(11) Uani 1 1 d . . .
H13A H -0.3451 0.7543 -0.1765 0.070 Uiso 1 1 calc R . .
H13B H -0.4864 0.7220 -0.1233 0.070 Uiso 1 1 calc R . .
H13C H -0.4000 0.6306 -0.1695 0.070 Uiso 1 1 calc R . .
O1W O 0.3010(3) 0.0440(2) 0.10435(15) 0.0440(7) Uani 1 1 d . . .
H1WA H 0.3547 0.0132 0.0705 0.066 Uiso 1 1 d R . .
H1WB H 0.3516 0.0332 0.1461 0.066 Uiso 1 1 d R . .
O1 O 0.3174(3) 0.6497(2) -0.03032(14) 0.0378(6) Uani 1 1 d . . .
O2 O 0.1097(3) 0.8635(2) 0.09026(14) 0.0382(6) Uani 1 1 d . . .
H2WA H 0.0187 0.8841 0.0684 0.057 Uiso 1 1 d R . .
H2WB H 0.0890 0.8336 0.1314 0.057 Uiso 1 1 d R . .
O3 O 0.3177(3) 0.8746(2) -0.02957(13) 0.0360(6) Uani 1 1 d . . .
O4 O 0.3619(4) 0.9581(2) -0.14738(14) 0.0434(7) Uani 1 1 d . . .
O5 O 0.2320(3) 1.06198(19) -0.05273(14) 0.0367(6) Uani 1 1 d . . .
O6 O 0.0827(3) 0.9147(2) -0.11463(15) 0.0435(7) Uani 1 1 d . . .
N1 N 0.1376(4) 0.6347(2) 0.09707(15) 0.0273(6) Uani 1 1 d . . .
N2 N 0.4177(4) 0.7411(2) 0.10792(16) 0.0287(7) Uani 1 1 d . . .
N3 N 0.5695(4) 0.7843(2) 0.12438(16) 0.0309(7) Uani 1 1 d . . .
H3B H 0.6178 0.8319 0.0972 0.037 Uiso 1 1 calc R . .
N4 N -0.0132(4) 0.7117(2) -0.01876(17) 0.0311(7) Uani 1 1 d . . .
N5 N -0.1101(4) 0.7395(2) -0.07828(18) 0.0342(7) Uani 1 1 d . . .
H5B H -0.0830 0.7878 -0.1105 0.041 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V O1 1.593(3) . ?
V O3 1.968(2) . ?
V N1 2.085(3) . ?
V N2 2.110(3) . ?
V N4 2.110(3) . ?
V O2 2.223(3) . ?
S O4 1.448(3) . ?
S O6 1.450(3) . ?
S O5 1.478(3) . ?
S O3 1.510(2) . ?
C1 N1 1.345(4) . ?
C1 C2 1.377(5) . ?
C1 C6 1.475(5) . ?
C2 C3 1.381(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.369(5) . ?
C4 H4A 0.9300 . ?
C5 N1 1.346(4) . ?
C5 C10 1.475(5) . ?
C6 N2 1.356(4) . ?
C6 C7 1.375(5) . ?
C7 C8 1.378(5) . ?
C7 H7A 0.9300 . ?
C8 N3 1.348(4) . ?
C8 C9 1.490(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N4 1.342(4) . ?
C10 C11 1.388(5) . ?
C11 C12 1.383(5) . ?
C11 H11A 0.9300 . ?
C12 N5 1.352(5) . ?
C12 C13 1.487(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2 H2WA 0.8500 . ?
O2 H2WB 0.8500 . ?
N2 N3 1.345(4) . ?
N3 H3B 0.8600 . ?
N4 N5 1.339(4) . ?
N5 H5B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V O3 99.26(13) . . ?
O1 V N1 97.15(12) . . ?
O3 V N1 162.76(11) . . ?
O1 V N2 97.95(13) . . ?
O3 V N2 96.30(11) . . ?
N1 V N2 76.13(11) . . ?
O1 V N4 95.82(13) . . ?
O3 V N4 108.75(11) . . ?
N1 V N4 74.65(12) . . ?
N2 V N4 148.97(12) . . ?
O1 V O2 176.86(12) . . ?
O3 V O2 83.39(11) . . ?
N1 V O2 80.37(11) . . ?
N2 V O2 83.36(11) . . ?
N4 V O2 81.70(11) . . ?
O4 S O6 111.66(17) . . ?
O4 S O5 110.13(17) . . ?
O6 S O5 109.79(17) . . ?
O4 S O3 108.28(16) . . ?
O6 S O3 109.84(15) . . ?
O5 S O3 107.03(15) . . ?
N1 C1 C2 121.5(3) . . ?
N1 C1 C6 112.6(3) . . ?
C2 C1 C6 125.9(3) . . ?
C1 C2 C3 117.8(4) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 H4A 121.0 . . ?
C3 C4 H4A 121.0 . . ?
N1 C5 C4 121.3(3) . . ?
N1 C5 C10 111.6(3) . . ?
C4 C5 C10 127.1(3) . . ?
N2 C6 C7 110.7(3) . . ?
N2 C6 C1 116.0(3) . . ?
C7 C6 C1 133.3(3) . . ?
C6 C7 C8 105.8(3) . . ?
C6 C7 H7A 127.1 . . ?
C8 C7 H7A 127.1 . . ?
N3 C8 C7 106.8(3) . . ?
N3 C8 C9 122.6(4) . . ?
C7 C8 C9 130.5(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 C11 110.7(3) . . ?
N4 C10 C5 115.3(3) . . ?
C11 C10 C5 134.0(3) . . ?
C12 C11 C10 105.4(3) . . ?
C12 C11 H11A 127.3 . . ?
C10 C11 H11A 127.3 . . ?
N5 C12 C11 106.4(3) . . ?
N5 C12 C13 121.8(4) . . ?
C11 C12 C13 131.7(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
V O2 H2WA 109.3 . . ?
V O2 H2WB 109.3 . . ?
H2WA O2 H2WB 109.5 . . ?
S O3 V 134.89(16) . . ?
C1 N1 C5 120.4(3) . . ?
C1 N1 V 119.2(2) . . ?
C5 N1 V 120.4(2) . . ?
N3 N2 C6 105.0(3) . . ?
N3 N2 V 138.8(2) . . ?
C6 N2 V 115.8(2) . . ?
N2 N3 C8 111.7(3) . . ?
N2 N3 H3B 124.1 . . ?
C8 N3 H3B 124.1 . . ?
N5 N4 C10 105.5(3) . . ?
N5 N4 V 136.4(2) . . ?
C10 N4 V 117.4(2) . . ?
N4 N5 C12 112.0(3) . . ?
N4 N5 H5B 124.0 . . ?
C12 N5 H5B 124.0 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.085

data_global

# Attachment '893014.cif'


data_1b
#TrackingRef '893014.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H19 N5 O6 S V'
_chemical_formula_weight         448.35

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           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                   12.260(2)
_cell_length_b                   8.0264(15)
_cell_length_c                   19.192(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.580(2)
_cell_angle_gamma                90.00
_cell_volume                     1843.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2715
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             924
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8273
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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 SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8938
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3239
_reflns_number_gt                2649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0600P)²+1.9910P] where P=(Fo²+2Fc²)/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         3239
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.79643(4) 0.97254(7) 0.12103(3) 0.02476(18) Uani 1 1 d . . .
S S 0.71880(7) 1.20708(11) 0.20198(5) 0.0331(2) Uani 1 1 d . . .
C1 C 0.8061(3) 1.0816(4) -0.02592(18) 0.0287(7) Uani 1 1 d . . .
C2 C 0.7712(3) 1.1016(4) -0.09866(18) 0.0365(8) Uani 1 1 d . . .
H2A H 0.8137 1.1627 -0.1242 0.044 Uiso 1 1 calc R . .
C3 C 0.6713(3) 1.0287(4) -0.13295(19) 0.0382(9) Uani 1 1 d . . .
H3A H 0.6465 1.0414 -0.1820 0.046 Uiso 1 1 calc R . .
C4 C 0.6082(3) 0.9374(4) -0.09499(18) 0.0331(8) Uani 1 1 d . . .
H4A H 0.5409 0.8894 -0.1177 0.040 Uiso 1 1 calc R . .
C5 C 0.6483(3) 0.9195(4) -0.02194(16) 0.0255(7) Uani 1 1 d . . .
C6 C 0.9049(3) 1.1563(4) 0.02064(17) 0.0286(7) Uani 1 1 d . . .
C7 C 0.9915(3) 1.2550(4) 0.00860(19) 0.0355(8) Uani 1 1 d . . .
H7A H 1.0038 1.2901 -0.0352 0.043 Uiso 1 1 calc R . .
C8 C 1.0555(3) 1.2902(4) 0.0752(2) 0.0352(8) Uani 1 1 d . . .
C9 C 1.1591(3) 1.3928(6) 0.0972(2) 0.0543(11) Uani 1 1 d . . .
H9A H 1.1830 1.3914 0.1483 0.081 Uiso 1 1 calc R . .
H9B H 1.1439 1.5054 0.0812 0.081 Uiso 1 1 calc R . .
H9C H 1.2170 1.3475 0.0763 0.081 Uiso 1 1 calc R . .
C14 C 1.0443(3) 1.2108(6) 0.2008(2) 0.0481(10) Uani 1 1 d . . .
H14A H 1.1113 1.2756 0.2149 0.072 Uiso 1 1 calc R . .
H14B H 1.0591 1.0976 0.2163 0.072 Uiso 1 1 calc R . .
H14C H 0.9871 1.2563 0.2223 0.072 Uiso 1 1 calc R . .
C10 C 0.5938(3) 0.8298(4) 0.02722(17) 0.0273(7) Uani 1 1 d . . .
C11 C 0.5038(3) 0.7218(4) 0.01910(18) 0.0314(8) Uani 1 1 d . . .
H11A H 0.4552 0.6919 -0.0234 0.038 Uiso 1 1 calc R . .
C12 C 0.5010(3) 0.6683(4) 0.08660(19) 0.0315(8) Uani 1 1 d . . .
C13 C 0.4262(3) 0.5457(5) 0.1114(2) 0.0463(10) Uani 1 1 d . . .
H13A H 0.4466 0.5368 0.1625 0.069 Uiso 1 1 calc R . .
H13B H 0.4336 0.4389 0.0905 0.069 Uiso 1 1 calc R . .
H13C H 0.3501 0.5827 0.0973 0.069 Uiso 1 1 calc R . .
C15 C 0.6185(3) 0.7277(5) 0.20963(19) 0.0420(9) Uani 1 1 d . . .
H15A H 0.6813 0.7990 0.2275 0.063 Uiso 1 1 calc R . .
H15B H 0.6390 0.6141 0.2215 0.063 Uiso 1 1 calc R . .
H15C H 0.5574 0.7586 0.2308 0.063 Uiso 1 1 calc R . .
N1 N 0.7450(2) 0.9901(3) 0.01096(13) 0.0241(6) Uani 1 1 d . . .
N2 N 0.6436(2) 0.8442(3) 0.09713(13) 0.0273(6) Uani 1 1 d . . .
N3 N 0.5851(2) 0.7451(3) 0.13228(14) 0.0296(6) Uani 1 1 d . . .
N4 N 0.9142(2) 1.1314(3) 0.09065(14) 0.0286(6) Uani 1 1 d . . .
N5 N 1.0073(2) 1.2150(3) 0.12378(15) 0.0322(7) Uani 1 1 d . . .
O1W O 0.7750(3) 0.5027(4) 0.06292(19) 0.0800(11) Uani 1 1 d . . .
H1WA H 0.8182 0.4850 0.0346 0.120 Uiso 1 1 d R . .
H1WB H 0.7944 0.4414 0.0996 0.120 Uiso 1 1 d R . .
O1 O 0.8750(2) 0.8131(3) 0.13806(13) 0.0393(6) Uani 1 1 d . . .
O3 O 0.79420(19) 1.0533(3) 0.21935(12) 0.0352(6) Uani 1 1 d . . .
O2 O 0.69570(19) 1.2032(3) 0.12213(12) 0.0334(6) Uani 1 1 d . . .
O4 O 0.7799(2) 1.3539(4) 0.22989(15) 0.0528(7) Uani 1 1 d . . .
O5 O 0.6179(2) 1.1836(4) 0.22752(15) 0.0556(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V O1 1.592(2) . ?
V O3 2.001(2) . ?
V N1 2.074(3) . ?
V N2 2.100(3) . ?
V N4 2.101(3) . ?
V O2 2.228(2) . ?
S O4 1.436(3) . ?
S O5 1.438(3) . ?
S O2 1.497(2) . ?
S O3 1.535(2) . ?
C1 N1 1.353(4) . ?
C1 C2 1.378(5) . ?
C1 C6 1.467(5) . ?
C2 C3 1.387(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.382(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(5) . ?
C4 H4A 0.9300 . ?
C5 N1 1.341(4) . ?
C5 C10 1.460(4) . ?
C6 N4 1.338(4) . ?
C6 C7 1.384(5) . ?
C7 C8 1.375(5) . ?
C7 H7A 0.9300 . ?
C8 N5 1.350(4) . ?
C8 C9 1.496(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 N5 1.449(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C10 N2 1.353(4) . ?
C10 C11 1.385(4) . ?
C11 C12 1.373(5) . ?
C11 H11A 0.9300 . ?
C12 N3 1.349(4) . ?
C12 C13 1.492(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 N3 1.458(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 N3 1.346(4) . ?
N4 N5 1.357(3) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V O3 101.45(12) . . ?
O1 V N1 107.45(12) . . ?
O3 V N1 151.06(10) . . ?
O1 V N2 96.99(12) . . ?
O3 V N2 99.79(10) . . ?
N1 V N2 75.65(10) . . ?
O1 V N4 97.08(12) . . ?
O3 V N4 102.51(10) . . ?
N1 V N4 75.56(10) . . ?
N2 V N4 150.62(10) . . ?
O1 V O2 167.86(11) . . ?
O3 V O2 66.45(9) . . ?
N1 V O2 84.67(9) . . ?
N2 V O2 86.53(10) . . ?
N4 V O2 85.08(10) . . ?
O4 S O5 113.43(18) . . ?
O4 S O2 111.48(16) . . ?
O5 S O2 111.17(15) . . ?
O4 S O3 109.80(15) . . ?
O5 S O3 110.01(17) . . ?
O2 S O3 100.15(13) . . ?
N1 C1 C2 120.5(3) . . ?
N1 C1 C6 112.4(3) . . ?
C2 C1 C6 127.0(3) . . ?
C1 C2 C3 118.6(3) . . ?
C1 C2 H2A 120.7 . . ?
C3 C2 H2A 120.7 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 120.9(3) . . ?
N1 C5 C10 112.7(3) . . ?
C4 C5 C10 126.3(3) . . ?
N4 C6 C7 110.6(3) . . ?
N4 C6 C1 115.4(3) . . ?
C7 C6 C1 133.9(3) . . ?
C8 C7 C6 105.4(3) . . ?
C8 C7 H7A 127.3 . . ?
C6 C7 H7A 127.3 . . ?
N5 C8 C7 107.7(3) . . ?
N5 C8 C9 121.5(3) . . ?
C7 C8 C9 130.8(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C10 C11 110.0(3) . . ?
N2 C10 C5 115.3(3) . . ?
C11 C10 C5 134.6(3) . . ?
C12 C11 C10 105.8(3) . . ?
C12 C11 H11A 127.1 . . ?
C10 C11 H11A 127.1 . . ?
N3 C12 C11 107.3(3) . . ?
N3 C12 C13 122.0(3) . . ?
C11 C12 C13 130.7(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 N1 C1 121.1(3) . . ?
C5 N1 V 119.5(2) . . ?
C1 N1 V 119.3(2) . . ?
N3 N2 C10 105.8(2) . . ?
N3 N2 V 136.7(2) . . ?
C10 N2 V 116.6(2) . . ?
N2 N3 C12 111.1(3) . . ?
N2 N3 C15 120.3(3) . . ?
C12 N3 C15 128.6(3) . . ?
C6 N4 N5 106.0(3) . . ?
C6 N4 V 117.1(2) . . ?
N5 N4 V 136.8(2) . . ?
C8 N5 N4 110.3(3) . . ?
C8 N5 C14 128.9(3) . . ?
N4 N5 C14 120.7(3) . . ?
H1WA O1W H1WB 109.5 . . ?
S O3 V 100.78(12) . . ?
S O2 V 92.60(11) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.071
