# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_l
_database_code_depnum_ccdc_archive 'CCDC 1845249'
_audit_update_record             
;
2018-05-25 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H10 N2 O6 V'
_chemical_formula_weight         329.16

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   7.5535(4)
_cell_length_b                   14.0883(7)
_cell_length_c                   12.5319(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.707(4)
_cell_angle_gamma                90
_cell_volume                     1324.47(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    446(2)
_cell_measurement_reflns_used    1052
_cell_measurement_theta_min      3.3190
_cell_measurement_theta_max      24.3170

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.779
_shelx_estimated_absorpt_T_min   0.860
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 ?
;

_diffrn_ambient_temperature      446(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5817
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.076
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2846
_reflns_number_gt                2156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0476P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2846
_refine_ls_number_parameters     198
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1197
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.04009(7) 0.54981(4) 0.30866(4) 0.01909(17) Uani 1 1 d . . . . .
O1 O 0.2563(3) 0.54977(16) 0.23100(16) 0.0247(5) Uani 1 1 d . . . . .
N1 N -0.1166(3) 0.59811(18) 0.16678(19) 0.0182(6) Uani 1 1 d . . . . .
O2 O 0.1995(3) 0.46843(16) 0.40924(15) 0.0230(5) Uani 1 1 d . . . . .
O1W O -0.1678(3) 0.4985(2) 0.38080(18) 0.0326(6) Uani 1 1 d D . . . .
O5 O 0.0487(4) 0.65223(18) 0.36057(19) 0.0378(7) Uani 1 1 d . . . . .
N2 N -0.0382(4) 0.41888(19) 0.20660(19) 0.0198(6) Uani 1 1 d . . . . .
C2 C 0.3606(4) 0.4546(2) 0.3835(2) 0.0211(7) Uani 1 1 d . . . . .
O4 O 0.4769(3) 0.40872(18) 0.43350(19) 0.0353(6) Uani 1 1 d . . . . .
C9 C -0.1933(5) 0.3613(2) 0.0421(3) 0.0288(8) Uani 1 1 d . . . . .
H9A H -0.2594 0.3740 -0.0237 0.035 Uiso 1 1 calc R U . . .
C8 C -0.1377(4) 0.4345(2) 0.1121(2) 0.0189(7) Uani 1 1 d . . . . .
O3 O 0.5364(3) 0.49762(19) 0.24241(17) 0.0342(6) Uani 1 1 d . . . . .
C5 C -0.3200(5) 0.6609(3) -0.0179(3) 0.0310(9) Uani 1 1 d . . . . .
H5B H -0.3897 0.6817 -0.0795 0.037 Uiso 1 1 calc R U . . .
C4 C -0.2512(5) 0.7254(3) 0.0588(3) 0.0303(8) Uani 1 1 d . . . . .
H4A H -0.2720 0.7901 0.0497 0.036 Uiso 1 1 calc R U . . .
C1 C 0.3903(4) 0.5039(2) 0.2761(2) 0.0212(7) Uani 1 1 d . . . . .
C6 C -0.2854(5) 0.5660(3) -0.0031(2) 0.0257(8) Uani 1 1 d . . . . .
H6A H -0.3307 0.5223 -0.0548 0.031 Uiso 1 1 calc R U . . .
C7 C -0.1824(4) 0.5354(2) 0.0898(2) 0.0178(7) Uani 1 1 d . . . . .
C3 C -0.1502(5) 0.6908(2) 0.1498(3) 0.0266(8) Uani 1 1 d . . . . .
H3A H -0.1033 0.7339 0.2018 0.032 Uiso 1 1 calc R U . . .
C12 C 0.0033(5) 0.3293(3) 0.2334(3) 0.0308(8) Uani 1 1 d . . . . .
H12A H 0.0716 0.3180 0.2989 0.037 Uiso 1 1 calc R U . . .
C11 C -0.0493(6) 0.2528(3) 0.1697(3) 0.0384(10) Uani 1 1 d . . . . .
H11A H -0.0189 0.1913 0.1917 0.046 Uiso 1 1 calc R U . . .
C10 C -0.1491(6) 0.2698(3) 0.0718(3) 0.0376(10) Uani 1 1 d . . . . .
H10A H -0.1858 0.2196 0.0263 0.045 Uiso 1 1 calc R U . . .
H1WA H -0.272(2) 0.488(3) 0.350(3) 0.052(13) Uiso 1 1 d D . . . .
H1WB H -0.173(5) 0.522(3) 0.4424(17) 0.077(17) Uiso 1 1 d 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 O5 1.581(2) . ?
V1 O1 1.996(2) . ?
V1 O2 1.999(2) . ?
V1 O1W 2.034(2) . ?
V1 N1 2.129(3) . ?
V1 N2 2.283(3) . ?
O1 C1 1.276(4) . ?
N1 C3 1.342(4) . ?
N1 C7 1.359(4) . ?
O2 C2 1.309(4) . ?
N2 C12 1.335(4) . ?
N2 C8 1.344(4) . ?
C2 O4 1.206(4) . ?
C2 C1 1.555(4) . ?
C9 C10 1.372(5) . ?
C9 C8 1.387(4) . ?
C8 C7 1.480(4) . ?
O3 C1 1.229(4) . ?
C5 C6 1.371(5) . ?
C5 C4 1.380(5) . ?
C4 C3 1.384(5) . ?
C6 C7 1.391(4) . ?
C12 C11 1.372(5) . ?
C11 C10 1.384(5) . ?

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 O1 101.78(12) . . ?
O5 V1 O2 105.73(11) . . ?
O1 V1 O2 80.83(9) . . ?
O5 V1 O1W 97.96(13) . . ?
O1 V1 O1W 159.14(11) . . ?
O2 V1 O1W 87.43(10) . . ?
O5 V1 N1 92.53(12) . . ?
O1 V1 N1 89.97(9) . . ?
O2 V1 N1 160.85(9) . . ?
O1W V1 N1 95.86(10) . . ?
O5 V1 N2 164.48(12) . . ?
O1 V1 N2 84.24(9) . . ?
O2 V1 N2 89.27(9) . . ?
O1W V1 N2 78.40(10) . . ?
N1 V1 N2 73.03(10) . . ?
C1 O1 V1 115.88(19) . . ?
C3 N1 C7 118.2(3) . . ?
C3 N1 V1 121.3(2) . . ?
C7 N1 V1 120.4(2) . . ?
C2 O2 V1 116.04(19) . . ?
C12 N2 C8 117.9(3) . . ?
C12 N2 V1 125.9(2) . . ?
C8 N2 V1 116.3(2) . . ?
O4 C2 O2 126.5(3) . . ?
O4 C2 C1 121.3(3) . . ?
O2 C2 C1 112.3(3) . . ?
C10 C9 C8 118.7(3) . . ?
N2 C8 C9 122.2(3) . . ?
N2 C8 C7 114.5(3) . . ?
C9 C8 C7 123.3(3) . . ?
C6 C5 C4 119.9(3) . . ?
C5 C4 C3 117.9(3) . . ?
O3 C1 O1 125.6(3) . . ?
O3 C1 C2 119.4(3) . . ?
O1 C1 C2 115.0(3) . . ?
C5 C6 C7 119.6(3) . . ?
N1 C7 C6 121.0(3) . . ?
N1 C7 C8 115.7(3) . . ?
C6 C7 C8 123.3(3) . . ?
N1 C3 C4 123.4(3) . . ?
N2 C12 C11 123.6(3) . . ?
C12 C11 C10 118.1(4) . . ?
C9 C10 C11 119.6(4) . . ?

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.080

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_l_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1845251'
_audit_update_record             
;
2018-05-25 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H21 N3 O10 V'
_chemical_formula_weight         490.32

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.1624(3)
_cell_length_b                   23.3551(8)
_cell_length_c                   11.0452(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.358(4)
_cell_angle_gamma                90
_cell_volume                     2020.35(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1052
_cell_measurement_theta_min      3.3190
_cell_measurement_theta_max      24.3170

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             1012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8402
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.899
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3960
_reflns_number_gt                3292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0301P)²+0.9520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3960
_refine_ls_number_parameters     309
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0895
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.25329(5) 0.69007(2) 0.48098(3) 0.01277(11) Uani 1 1 d . . . . .
O3 O 0.17609(19) 0.69125(7) 0.63766(13) 0.0164(3) Uani 1 1 d . . . . .
O5 O 0.28833(19) 0.60480(7) 0.49630(15) 0.0184(4) Uani 1 1 d . . . . .
O1 O 0.20316(19) 0.68241(7) 0.29247(14) 0.0170(4) Uani 1 1 d . . . . .
O4 O -0.0360(2) 0.69548(7) 0.72636(14) 0.0215(4) Uani 1 1 d . . . . .
O6 O 0.1843(2) 0.51643(7) 0.45718(16) 0.0242(4) Uani 1 1 d . . . . .
O2 O 0.0130(2) 0.67387(8) 0.10343(14) 0.0230(4) Uani 1 1 d . . . . .
N1 N -0.0237(2) 0.65527(8) 0.41815(16) 0.0125(4) Uani 1 1 d . . . . .
N2 N 0.4085(2) 1.12503(9) 0.48612(18) 0.0193(4) Uani 1 1 d . . . . .
H2A H 0.4255 1.1208 0.4133 0.023 Uiso 1 1 calc R U . . .
C2 C 0.0508(3) 0.67547(10) 0.2202(2) 0.0155(5) Uani 1 1 d . . . . .
C17 C 0.2949(3) 1.02878(11) 0.4644(2) 0.0182(5) Uani 1 1 d . . . . .
C3 C -0.1100(3) 0.68355(10) 0.50266(19) 0.0151(5) Uani 1 1 d . . . . .
H3A H -0.2064 0.6606 0.5091 0.018 Uiso 1 1 calc R U . . .
H3B H -0.1523 0.7208 0.4690 0.018 Uiso 1 1 calc R U . . .
C6 C 0.1651(3) 0.56843(10) 0.4637(2) 0.0163(5) Uani 1 1 d . . . . .
C4 C 0.0173(3) 0.69038(10) 0.6325(2) 0.0151(5) Uani 1 1 d . . . . .
C1 C -0.0910(3) 0.67024(11) 0.2836(2) 0.0180(5) Uani 1 1 d . . . . .
H1A H -0.1521 0.7063 0.2760 0.022 Uiso 1 1 calc R U . . .
H1B H -0.1710 0.6410 0.2411 0.022 Uiso 1 1 calc R U . . .
C5 C -0.0143(3) 0.59242(10) 0.4377(2) 0.0187(5) Uani 1 1 d . . . . .
H5A H -0.0869 0.5739 0.3631 0.022 Uiso 1 1 calc R U . . .
H5B H -0.0586 0.5831 0.5081 0.022 Uiso 1 1 calc R U . . .
C10 C 0.3142(3) 1.08730(11) 0.6550(2) 0.0220(5) Uani 1 1 d . . . . .
C8 C 0.4287(3) 1.18266(12) 0.6647(3) 0.0299(6) Uani 1 1 d . . . . .
H8A H 0.4587 1.2172 0.7068 0.036 Uiso 1 1 calc R U . . .
C15 C 0.2223(3) 0.92929(12) 0.3342(3) 0.0352(7) Uani 1 1 d . . . . .
H15A H 0.2003 0.8957 0.2872 0.042 Uiso 1 1 calc R U . . .
N3 N 0.3198(3) 1.02687(9) 0.34810(18) 0.0234(5) Uani 1 1 d . . . . .
C13 C 0.2318(3) 0.98271(11) 0.5206(2) 0.0250(6) Uani 1 1 d . . . . .
C18 C 0.3384(3) 1.08092(11) 0.5347(2) 0.0174(5) Uani 1 1 d . . . . .
C14 C 0.1948(3) 0.93208(12) 0.4502(3) 0.0328(6) Uani 1 1 d . . . . .
H14A H 0.1517 0.9005 0.4825 0.039 Uiso 1 1 calc R U . . .
C9 C 0.3608(3) 1.13917(12) 0.7189(2) 0.0277(6) Uani 1 1 d . . . . .
H9A H 0.3457 1.1442 0.7985 0.033 Uiso 1 1 calc R U . . .
C16 C 0.2843(3) 0.97781(12) 0.2867(2) 0.0311(6) Uani 1 1 d . . . . .
H16A H 0.3015 0.9753 0.2072 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2096(3) 0.99011(13) 0.6439(3) 0.0326(7) Uani 1 1 d . . . . .
H12A H 0.1683 0.9597 0.6811 0.039 Uiso 1 1 calc R U . . .
C7 C 0.4518(3) 1.17437(11) 0.5463(2) 0.0266(6) Uani 1 1 d . . . . .
H7A H 0.4979 1.2035 0.5088 0.032 Uiso 1 1 calc R U . . .
C11 C 0.2466(3) 1.03946(13) 0.7071(2) 0.0301(6) Uani 1 1 d . . . . .
H11A H 0.2283 1.0429 0.7861 0.036 Uiso 1 1 calc R U . . .
O1W O 0.1552(2) 0.77038(7) 0.44778(14) 0.0178(4) Uani 1 1 d D . . . .
H1WA H 0.0993 0.7731 0.3737 0.027 Uiso 1 1 calc DR U . . .
O7 O 0.45299(19) 0.70464(7) 0.52696(15) 0.0207(4) Uani 1 1 d . . . . .
O3W O 0.5030(3) 1.13906(10) 0.27198(18) 0.0376(5) Uani 1 1 d D . . . .
O2W O 0.5945(2) 0.57441(9) 0.44902(19) 0.0337(5) Uani 1 1 d D . . . .
H1WB H 0.117(3) 0.7896(12) 0.4984(13) 0.057(11) Uiso 1 1 d D . . . .
H3WB H 0.597(2) 1.1547(12) 0.273(3) 0.055(11) Uiso 1 1 d D . . . .
H2WB H 0.636(3) 0.5414(7) 0.472(3) 0.046(10) Uiso 1 1 d D . . . .
H3WA H 0.476(4) 1.1142(12) 0.213(3) 0.072(13) Uiso 1 1 d D . . . .
H2WA H 0.502(2) 0.5785(11) 0.468(3) 0.044(9) Uiso 1 1 d 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 O7 1.6013(16) . ?
V1 O3 2.0018(15) . ?
V1 O5 2.0122(16) . ?
V1 O1 2.0136(15) . ?
V1 O1W 2.0317(17) . ?
V1 N1 2.3172(18) . ?
O3 C4 1.282(3) . ?
O5 C6 1.288(3) . ?
O1 C2 1.285(3) . ?
O4 C4 1.238(3) . ?
O6 C6 1.229(3) . ?
O2 C2 1.240(3) . ?
N1 C1 1.474(3) . ?
N1 C3 1.475(3) . ?
N1 C5 1.483(3) . ?
N2 C7 1.328(3) . ?
N2 C18 1.360(3) . ?
C2 C1 1.517(3) . ?
C17 N3 1.357(3) . ?
C17 C13 1.410(3) . ?
C17 C18 1.434(3) . ?
C3 C4 1.524(3) . ?
C6 C5 1.518(3) . ?
C10 C9 1.399(4) . ?
C10 C18 1.405(3) . ?
C10 C11 1.436(4) . ?
C8 C9 1.372(4) . ?
C8 C7 1.386(4) . ?
C15 C14 1.364(4) . ?
C15 C16 1.401(4) . ?
N3 C16 1.321(3) . ?
C13 C14 1.401(4) . ?
C13 C12 1.434(4) . ?
C12 C11 1.337(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
O7 V1 O3 105.25(7) . . ?
O7 V1 O5 94.34(8) . . ?
O3 V1 O5 90.73(6) . . ?
O7 V1 O1 103.83(7) . . ?
O3 V1 O1 150.85(6) . . ?
O5 V1 O1 88.95(7) . . ?
O7 V1 O1W 100.08(8) . . ?
O3 V1 O1W 86.53(6) . . ?
O5 V1 O1W 165.53(7) . . ?
O1 V1 O1W 86.58(6) . . ?
O7 V1 N1 171.73(8) . . ?
O3 V1 N1 75.26(6) . . ?
O5 V1 N1 77.39(6) . . ?
O1 V1 N1 76.24(6) . . ?
O1W V1 N1 88.18(7) . . ?
C4 O3 V1 121.49(13) . . ?
C6 O5 V1 123.22(14) . . ?
C2 O1 V1 122.18(13) . . ?
C1 N1 C3 115.03(18) . . ?
C1 N1 C5 111.76(18) . . ?
C3 N1 C5 111.46(17) . . ?
C1 N1 V1 105.89(12) . . ?
C3 N1 V1 104.67(13) . . ?
C5 N1 V1 107.31(13) . . ?
C7 N2 C18 122.8(2) . . ?
O2 C2 O1 124.3(2) . . ?
O2 C2 C1 118.7(2) . . ?
O1 C2 C1 117.02(19) . . ?
N3 C17 C13 124.2(2) . . ?
N3 C17 C18 117.4(2) . . ?
C13 C17 C18 118.4(2) . . ?
N1 C3 C4 108.77(18) . . ?
O6 C6 O5 124.4(2) . . ?
O6 C6 C5 119.1(2) . . ?
O5 C6 C5 116.4(2) . . ?
O4 C4 O3 123.5(2) . . ?
O4 C4 C3 119.4(2) . . ?
O3 C4 C3 117.14(18) . . ?
N1 C1 C2 111.63(18) . . ?
N1 C5 C6 113.62(18) . . ?
C9 C10 C18 118.5(2) . . ?
C9 C10 C11 123.6(2) . . ?
C18 C10 C11 117.9(2) . . ?
C9 C8 C7 119.1(2) . . ?
C14 C15 C16 119.0(3) . . ?
C16 N3 C17 116.4(2) . . ?
C14 C13 C17 116.7(2) . . ?
C14 C13 C12 124.3(2) . . ?
C17 C13 C12 119.0(2) . . ?
N2 C18 C10 118.7(2) . . ?
N2 C18 C17 119.8(2) . . ?
C10 C18 C17 121.5(2) . . ?
C15 C14 C13 119.7(3) . . ?
C8 C9 C10 120.5(2) . . ?
N3 C16 C15 124.0(2) . . ?
C11 C12 C13 121.9(2) . . ?
N2 C7 C8 120.4(2) . . ?
C12 C11 C10 121.2(2) . . ?

_refine_diff_density_max         0.301
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.060

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_l_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1845250'
_audit_update_record             
;
2018-05-25 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H29 N5 O9 V'
_chemical_formula_weight         630.50

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.1555(5)
_cell_length_b                   19.6759(12)
_cell_length_c                   19.8619(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.826(7)
_cell_angle_gamma                90
_cell_volume                     2781.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1052
_cell_measurement_theta_min      3.3190
_cell_measurement_theta_max      24.3170

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.421
_shelx_estimated_absorpt_T_min   0.920
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12451
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.922
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5452
_reflns_number_gt                3929
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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     
'w=1/[σ²(Fo²)+(0.0328P)²+0.1396P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5452
_refine_ls_number_parameters     412
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.32440(7) 0.26413(3) 0.21963(2) 0.01582(15) Uani 1 1 d . . . . .
O1 O 0.2679(3) 0.18142(10) 0.27192(10) 0.0197(5) Uani 1 1 d . . . . .
O2 O 0.0653(3) 0.10612(10) 0.30568(10) 0.0245(5) Uani 1 1 d . . . . .
O3 O 0.2641(3) 0.32931(10) 0.29214(9) 0.0194(5) Uani 1 1 d . . . . .
O4 O 0.0684(3) 0.40111(10) 0.33533(10) 0.0263(5) Uani 1 1 d . . . . .
O5 O 0.5462(3) 0.26905(11) 0.23531(10) 0.0243(5) Uani 1 1 d . . . . .
N1 N -0.0041(3) 0.26520(12) 0.21383(12) 0.0169(5) Uani 1 1 d . . . . .
H1 H -0.0586 0.2616 0.1667 0.020 Uiso 1 1 calc R U . . .
N2 N 0.3149(3) 0.20400(12) 0.13120(12) 0.0181(6) Uani 1 1 d . . . . .
N3 N 0.2707(3) 0.33813(12) 0.14186(12) 0.0175(6) Uani 1 1 d . . . . .
C1 C -0.0602(4) 0.20628(15) 0.25326(15) 0.0204(7) Uani 1 1 d . . . . .
H1A H -0.1521 0.1797 0.2252 0.024 Uiso 1 1 calc R U . . .
H1B H -0.1203 0.2227 0.2918 0.024 Uiso 1 1 calc R U . . .
C2 C 0.1005(4) 0.16097(15) 0.27832(14) 0.0181(7) Uani 1 1 d . . . . .
C3 C -0.0534(4) 0.33085(14) 0.24259(15) 0.0200(7) Uani 1 1 d . . . . .
H3A H -0.1693 0.3261 0.2636 0.024 Uiso 1 1 calc R U . . .
H3B H -0.0740 0.3641 0.2066 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1011(4) 0.35580(15) 0.29495(14) 0.0186(7) Uani 1 1 d . . . . .
C5 C 0.3565(4) 0.13816(15) 0.12677(16) 0.0226(7) Uani 1 1 d . . . . .
H5A H 0.3912 0.1139 0.1663 0.027 Uiso 1 1 calc R U . . .
C6 C 0.3497(4) 0.10446(17) 0.06459(17) 0.0283(8) Uani 1 1 d . . . . .
H6A H 0.3840 0.0589 0.0632 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2932(4) 0.13802(16) 0.00619(16) 0.0262(8) Uani 1 1 d . . . . .
H7A H 0.2839 0.1153 -0.0351 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2486(4) 0.20816(16) 0.00897(15) 0.0203(7) Uani 1 1 d . . . . .
C9 C 0.1918(4) 0.24880(17) -0.04954(15) 0.0276(8) Uani 1 1 d . . . . .
H9A H 0.1780 0.2286 -0.0921 0.033 Uiso 1 1 calc R U . . .
C10 C 0.1579(4) 0.31628(17) -0.04364(15) 0.0273(8) Uani 1 1 d . . . . .
H10A H 0.1174 0.3414 -0.0820 0.033 Uiso 1 1 calc R U . . .
C11 C 0.1836(4) 0.34935(16) 0.02079(15) 0.0202(7) Uani 1 1 d . . . . .
C12 C 0.1632(4) 0.41986(17) 0.02985(16) 0.0271(8) Uani 1 1 d . . . . .
H12A H 0.1244 0.4475 -0.0069 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2006(4) 0.44756(16) 0.09291(16) 0.0268(8) Uani 1 1 d . . . . .
H13A H 0.1902 0.4942 0.0991 0.032 Uiso 1 1 calc R U . . .
C14 C 0.2547(4) 0.40514(15) 0.14797(15) 0.0219(7) Uani 1 1 d . . . . .
H14A H 0.2805 0.4246 0.1906 0.026 Uiso 1 1 calc R U . . .
C15 C 0.2660(4) 0.23862(15) 0.07274(14) 0.0168(7) Uani 1 1 d . . . . .
C16 C 0.2373(4) 0.31060(15) 0.07860(14) 0.0167(7) Uani 1 1 d . . . . .
O1W O 0.3652(4) 0.01673(11) 0.32754(14) 0.0378(6) Uani 1 1 d D . . . .
O2W O -0.3010(4) 0.05442(14) 0.27636(14) 0.0471(7) Uani 1 1 d D . . . .
O3W O 0.3823(4) 0.48833(12) 0.34850(15) 0.0453(7) Uani 1 1 d D . . . .
O4W O -0.2655(4) 0.47307(16) 0.30949(13) 0.0516(8) Uani 1 1 d D . . . .
H1WA H 0.462(3) 0.0346(16) 0.3130(19) 0.062 Uiso 1 1 d D U . . .
H1WB H 0.277(3) 0.0461(13) 0.324(2) 0.062 Uiso 1 1 d D U . . .
H2WA H -0.195(3) 0.0744(17) 0.2836(16) 0.062 Uiso 1 1 d D U . . .
H2WB H -0.309(5) 0.0366(18) 0.2371(10) 0.062 Uiso 1 1 d D U . . .
H3WA H 0.486(3) 0.4715(16) 0.338(2) 0.062 Uiso 1 1 d D U . . .
H3WB H 0.298(3) 0.4579(13) 0.346(2) 0.062 Uiso 1 1 d D U . . .
H4WA H -0.281(5) 0.4823(19) 0.2675(7) 0.062 Uiso 1 1 d D U . . .
H4WB H -0.166(3) 0.4499(17) 0.3180(16) 0.062 Uiso 1 1 d D U . . .
N4 N 0.2396(3) 0.81273(12) 0.41692(12) 0.0204(6) Uani 1 1 d . . . . .
N5 N 0.1588(3) 0.67603(12) 0.40995(12) 0.0201(6) Uani 1 1 d . . . . .
C17 C 0.2845(4) 0.87816(16) 0.42125(17) 0.0266(8) Uani 1 1 d . . . . .
H17A H 0.2691 0.9041 0.3819 0.032 Uiso 1 1 calc R U . . .
C18 C 0.3539(4) 0.91049(18) 0.48153(18) 0.0333(9) Uani 1 1 d . . . . .
H18A H 0.3830 0.9566 0.4818 0.040 Uiso 1 1 calc R U . . .
C19 C 0.3778(5) 0.87366(18) 0.53938(18) 0.0334(9) Uani 1 1 d . . . . .
H19A H 0.4216 0.8944 0.5800 0.040 Uiso 1 1 calc R U . . .
C20 C 0.3357(4) 0.80344(18) 0.53761(16) 0.0254(8) Uani 1 1 d . . . . .
C21 C 0.3646(4) 0.7610(2) 0.59655(16) 0.0335(9) Uani 1 1 d . . . . .
H21A H 0.4097 0.7801 0.6379 0.040 Uiso 1 1 calc R U . . .
C22 C 0.3275(5) 0.6944(2) 0.59283(16) 0.0335(9) Uani 1 1 d . . . . .
H22A H 0.3487 0.6678 0.6316 0.040 Uiso 1 1 calc R U . . .
C23 C 0.2559(4) 0.66334(17) 0.53034(16) 0.0260(8) Uani 1 1 d . . . . .
C24 C 0.2169(5) 0.59310(18) 0.52480(18) 0.0337(9) Uani 1 1 d . . . . .
H24A H 0.2336 0.5653 0.5628 0.040 Uiso 1 1 calc R U . . .
C25 C 0.1546(5) 0.56644(18) 0.46328(18) 0.0340(9) Uani 1 1 d . . . . .
H25A H 0.1309 0.5201 0.4585 0.041 Uiso 1 1 calc R U . . .
C26 C 0.1270(5) 0.60991(15) 0.40753(18) 0.0281(8) Uani 1 1 d . . . . .
H26A H 0.0834 0.5910 0.3660 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2674(4) 0.77544(16) 0.47476(14) 0.0187(7) Uani 1 1 d . . . . .
C28 C 0.2254(4) 0.70289(16) 0.47139(15) 0.0201(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 O5 1.589(2) . ?
V1 O1 1.994(2) . ?
V1 O3 2.008(2) . ?
V1 N2 2.113(2) . ?
V1 N3 2.129(2) . ?
V1 N1 2.342(2) . ?
O1 C2 1.282(3) . ?
O2 C2 1.245(3) . ?
O3 C4 1.284(3) . ?
O4 C4 1.237(3) . ?
N1 C3 1.470(3) . ?
N1 C1 1.477(4) . ?
N2 C5 1.334(4) . ?
N2 C15 1.361(4) . ?
N3 C14 1.330(4) . ?
N3 C16 1.367(3) . ?
C1 C2 1.499(4) . ?
C3 C4 1.520(4) . ?
C5 C6 1.398(4) . ?
C6 C7 1.360(4) . ?
C7 C8 1.419(4) . ?
C8 C15 1.395(4) . ?
C8 C9 1.435(4) . ?
C9 C10 1.357(5) . ?
C10 C11 1.431(4) . ?
C11 C16 1.399(4) . ?
C11 C12 1.408(4) . ?
C12 C13 1.367(4) . ?
C13 C14 1.399(4) . ?
C15 C16 1.437(4) . ?
N4 C17 1.328(4) . ?
N4 C27 1.361(4) . ?
N5 C26 1.321(4) . ?
N5 C28 1.370(4) . ?
C17 C18 1.401(4) . ?
C18 C19 1.355(5) . ?
C19 C20 1.414(5) . ?
C20 C27 1.406(4) . ?
C20 C21 1.436(4) . ?
C21 C22 1.338(5) . ?
C22 C23 1.431(4) . ?
C23 C28 1.404(4) . ?
C23 C24 1.412(5) . ?
C24 C25 1.362(5) . ?
C25 C26 1.397(4) . ?
C27 C28 1.459(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
O5 V1 O1 101.48(9) . . ?
O5 V1 O3 95.95(9) . . ?
O1 V1 O3 94.47(8) . . ?
O5 V1 N2 98.29(10) . . ?
O1 V1 N2 89.13(9) . . ?
O3 V1 N2 164.31(9) . . ?
O5 V1 N3 101.74(10) . . ?
O1 V1 N3 154.81(9) . . ?
O3 V1 N3 92.72(9) . . ?
N2 V1 N3 77.98(9) . . ?
O5 V1 N1 170.64(10) . . ?
O1 V1 N1 77.13(8) . . ?
O3 V1 N1 75.03(8) . . ?
N2 V1 N1 90.96(9) . . ?
N3 V1 N1 81.49(9) . . ?
C2 O1 V1 123.27(18) . . ?
C4 O3 V1 123.57(18) . . ?
C3 N1 C1 113.3(2) . . ?
C3 N1 V1 105.55(16) . . ?
C1 N1 V1 107.00(16) . . ?
C5 N2 C15 118.0(3) . . ?
C5 N2 V1 127.6(2) . . ?
C15 N2 V1 114.37(19) . . ?
C14 N3 C16 117.9(3) . . ?
C14 N3 V1 128.5(2) . . ?
C16 N3 V1 113.43(18) . . ?
N1 C1 C2 113.7(2) . . ?
O2 C2 O1 123.2(3) . . ?
O2 C2 C1 118.5(3) . . ?
O1 C2 C1 118.2(3) . . ?
N1 C3 C4 111.3(2) . . ?
O4 C4 O3 123.6(3) . . ?
O4 C4 C3 120.2(3) . . ?
O3 C4 C3 116.1(3) . . ?
N2 C5 C6 122.1(3) . . ?
C7 C6 C5 120.2(3) . . ?
C6 C7 C8 119.2(3) . . ?
C15 C8 C7 117.0(3) . . ?
C15 C8 C9 119.2(3) . . ?
C7 C8 C9 123.8(3) . . ?
C10 C9 C8 120.9(3) . . ?
C9 C10 C11 121.0(3) . . ?
C16 C11 C12 117.1(3) . . ?
C16 C11 C10 119.1(3) . . ?
C12 C11 C10 123.8(3) . . ?
C13 C12 C11 119.8(3) . . ?
C12 C13 C14 119.4(3) . . ?
N3 C14 C13 122.7(3) . . ?
N2 C15 C8 123.4(3) . . ?
N2 C15 C16 116.8(3) . . ?
C8 C15 C16 119.8(3) . . ?
N3 C16 C11 123.1(3) . . ?
N3 C16 C15 116.9(3) . . ?
C11 C16 C15 120.0(3) . . ?
C17 N4 C27 117.0(3) . . ?
C26 N5 C28 117.1(3) . . ?
N4 C17 C18 123.9(3) . . ?
C19 C18 C17 119.0(3) . . ?
C18 C19 C20 119.6(3) . . ?
C27 C20 C19 117.3(3) . . ?
C27 C20 C21 120.3(3) . . ?
C19 C20 C21 122.4(3) . . ?
C22 C21 C20 120.9(3) . . ?
C21 C22 C23 121.2(3) . . ?
C28 C23 C24 117.7(3) . . ?
C28 C23 C22 119.9(3) . . ?
C24 C23 C22 122.4(3) . . ?
C25 C24 C23 119.4(3) . . ?
C24 C25 C26 118.8(3) . . ?
N5 C26 C25 124.4(3) . . ?
N4 C27 C20 123.1(3) . . ?
N4 C27 C28 118.5(3) . . ?
C20 C27 C28 118.4(3) . . ?
N5 C28 C23 122.6(3) . . ?
N5 C28 C27 118.0(3) . . ?
C23 C28 C27 119.4(3) . . ?

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.071

