# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_H3L2
_database_code_depnum_ccdc_archive 'CCDC 1575573'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H17 N2 O3'
_chemical_formula_weight         297.25

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pcab

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

_cell_length_a                   7.2782(14)
_cell_length_b                   12.8154(14)
_cell_length_c                   30.621(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2856.1(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7635
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none



_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         n/a
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            6376
_diffrn_reflns_av_R_equivalents  0.1168
_diffrn_reflns_av_sigmaI/netI    0.1314
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3214
_reflns_number_gt                1507
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)

_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)+(0.1203P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3214
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1524
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2703
_refine_ls_wR_factor_gt          0.2118
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_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
O1 O 0.5227(4) 0.88220(18) 0.14229(8) 0.0377(7) Uani 1 1 d D . .
HO1 H 0.572(6) 0.851(3) 0.1204(10) 0.057 Uiso 1 1 d D . .
O2 O 0.7455(4) 0.86341(16) 0.03275(8) 0.0358(7) Uani 1 1 d . . .
O3 O 0.7725(4) 0.54828(17) 0.00101(8) 0.0418(8) Uani 1 1 d D . .
HO3 H 0.786(6) 0.487(2) -0.0109(13) 0.050 Uiso 1 1 d D . .
N1 N 0.6133(5) 0.7333(2) 0.09193(10) 0.0319(7) Uani 1 1 d . . .
N2 N 0.6849(5) 0.69915(19) 0.05276(10) 0.0304(7) Uani 1 1 d D . .
HN2 H 0.687(5) 0.6304(16) 0.0473(12) 0.036 Uiso 1 1 d D . .
C1 C 0.4734(5) 0.8084(2) 0.17004(12) 0.0314(9) Uani 1 1 d . . .
C2 C 0.4864(5) 0.7038(2) 0.16075(12) 0.0307(8) Uani 1 1 d . . .
H2A H 0.3639 0.6751 0.1641 0.037 Uiso 1 1 calc R . .
H2B H 0.5610 0.6730 0.1836 0.037 Uiso 1 1 calc R . .
C3 C 0.5563(5) 0.6653(3) 0.12020(12) 0.0306(8) Uani 1 1 d . . .
C4 C 0.7491(5) 0.7685(2) 0.02385(11) 0.0260(8) Uani 1 1 d . . .
C5 C 0.8200(5) 0.7274(2) -0.01795(11) 0.0267(8) Uani 1 1 d . . .
C6 C 0.8300(5) 0.6202(2) -0.02874(12) 0.0308(9) Uani 1 1 d . . .
C7 C 0.8967(6) 0.5897(3) -0.06919(12) 0.0353(9) Uani 1 1 d . . .
H7 H 0.9054 0.5191 -0.0759 0.042 Uiso 1 1 calc R . .
C8 C 0.9499(5) 0.6626(3) -0.09942(12) 0.0336(9) Uani 1 1 d . . .
H8 H 0.9916 0.6412 -0.1267 0.040 Uiso 1 1 calc R . .
C9 C 0.9418(6) 0.7688(3) -0.08957(12) 0.0376(9) Uani 1 1 d . . .
H9 H 0.9789 0.8182 -0.1100 0.045 Uiso 1 1 calc R . .
C10 C 0.8781(6) 0.7992(2) -0.04916(12) 0.0346(9) Uani 1 1 d . . .
H10 H 0.8737 0.8700 -0.0425 0.042 Uiso 1 1 calc R . .
C11 C 0.4024(5) 0.8473(3) 0.21253(12) 0.0322(9) Uani 1 1 d . . .
C12 C 0.3317(6) 0.9489(3) 0.21474(14) 0.0391(10) Uani 1 1 d . . .
H12 H 0.3278 0.9903 0.1898 0.047 Uiso 1 1 calc R . .
C13 C 0.2675(6) 0.9876(3) 0.25412(14) 0.0442(10) Uani 1 1 d . . .
H13 H 0.2203 1.0549 0.2554 0.053 Uiso 1 1 calc R . .
C14 C 0.2730(6) 0.9276(3) 0.29120(14) 0.0465(11) Uani 1 1 d . . .
H14 H 0.2295 0.9541 0.3175 0.056 Uiso 1 1 calc R . .
C15 C 0.3435(6) 0.8274(3) 0.28920(13) 0.0428(10) Uani 1 1 d . . .
H15 H 0.3470 0.7867 0.3143 0.051 Uiso 1 1 calc R . .
C16 C 0.4089(6) 0.7871(3) 0.25027(12) 0.0387(10) Uani 1 1 d . . .
H16 H 0.4570 0.7199 0.2493 0.046 Uiso 1 1 calc R . .
C17 C 0.5605(6) 0.5495(2) 0.11157(12) 0.0370(10) Uani 1 1 d . . .
H17A H 0.4869 0.5340 0.0864 0.055 Uiso 1 1 calc R . .
H17B H 0.5124 0.5130 0.1364 0.055 Uiso 1 1 calc R . .
H17C H 0.6848 0.5278 0.1064 0.055 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
O1 C1 1.321(4) . ?
O1 HO1 0.859(19) . ?
O2 C4 1.247(4) . ?
O3 C6 1.361(4) . ?
O3 HO3 0.873(19) . ?
N1 C3 1.297(4) . ?
N1 N2 1.379(4) . ?
N2 C4 1.339(4) . ?
N2 HN2 0.897(18) . ?
C1 C2 1.373(4) . ?
C1 C11 1.486(5) . ?
C2 C3 1.430(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C17 1.508(4) . ?
C4 C5 1.477(5) . ?
C5 C10 1.392(5) . ?
C5 C6 1.416(4) . ?
C6 C7 1.386(5) . ?
C7 C8 1.371(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.394(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.378(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C16 1.390(5) . ?
C11 C12 1.401(5) . ?
C12 C13 1.385(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.383(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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
C1 O1 HO1 106(3) . . ?
C6 O3 HO3 107(3) . . ?
C3 N1 N2 119.2(3) . . ?
C4 N2 N1 119.7(2) . . ?
C4 N2 HN2 121(2) . . ?
N1 N2 HN2 119(2) . . ?
O1 C1 C2 123.2(3) . . ?
O1 C1 C11 114.7(3) . . ?
C2 C1 C11 122.2(3) . . ?
C1 C2 C3 122.8(3) . . ?
C1 C2 H2A 106.6 . . ?
C3 C2 H2A 106.6 . . ?
C1 C2 H2B 106.6 . . ?
C3 C2 H2B 106.6 . . ?
H2A C2 H2B 106.6 . . ?
N1 C3 C2 117.5(3) . . ?
N1 C3 C17 122.6(3) . . ?
C2 C3 C17 120.0(3) . . ?
O2 C4 N2 119.7(3) . . ?
O2 C4 C5 123.0(3) . . ?
N2 C4 C5 117.3(3) . . ?
C10 C5 C6 117.7(3) . . ?
C10 C5 C4 117.7(3) . . ?
C6 C5 C4 124.5(3) . . ?
O3 C6 C7 121.0(3) . . ?
O3 C6 C5 119.0(3) . . ?
C7 C6 C5 120.0(3) . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 120.5(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.0(3) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C5 122.1(3) . . ?
C9 C10 H10 118.9 . . ?
C5 C10 H10 118.9 . . ?
C16 C11 C12 119.2(3) . . ?
C16 C11 C1 122.0(3) . . ?
C12 C11 C1 118.8(3) . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.7(4) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 119.6(4) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 119.8(4) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 HO1 N1 0.859(19) 1.77(3) 2.540(4) 149(4) .
N2 HN2 O3 0.897(18) 1.87(3) 2.580(4) 135(3) .
O3 HO3 O2 0.873(19) 1.73(2) 2.588(3) 166(4) 4_645

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1575574'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H28 N4 O9 V2  '
_chemical_formula_weight         738.48

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'
O O 0.0106 0.0060 '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'
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                   7.3361(19)
_cell_length_b                   9.3756(18)
_cell_length_c                   11.919(2)
_cell_angle_alpha                77.072(16)
_cell_angle_beta                 77.405(19)
_cell_angle_gamma                83.703(19)
_cell_volume                     778.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5497
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      30.00

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             378
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_T_max  1.000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         n/a
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            5497
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         30.00
_reflns_number_total             4346
_reflns_number_gt                2999
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)


_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     
;
_refine_ls_weighting_details
  w=1/[σ²(Fo²)+(0.1027P)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         4346
_refine_ls_number_parameters     225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2200
_refine_ls_wR_factor_gt          0.1836
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
V V 0.60284(7) 0.92611(6) 0.62519(4) 0.0301(2) Uani 1 1 d . . .
O1 O 0.8262(3) 0.8602(3) 0.5435(2) 0.0369(6) Uani 1 1 d . . .
C1 C 0.9758(5) 0.7826(4) 0.5729(3) 0.0313(7) Uani 1 1 d . . .
C2 C 1.0296(5) 0.7862(4) 0.6748(3) 0.0348(7) Uani 1 1 d . . .
H2 H 1.1363 0.7295 0.6917 0.042 Uiso 1 1 calc R . .
C3 C 0.9324(5) 0.8714(4) 0.7570(3) 0.0337(7) Uani 1 1 d . . .
N1 N 0.7687(4) 0.9374(3) 0.7446(2) 0.0310(6) Uani 1 1 d . . .
N2 N 0.6935(4) 1.0283(3) 0.8233(2) 0.0325(6) Uani 1 1 d . . .
C4 C 0.5458(5) 1.1003(4) 0.7920(3) 0.0312(7) Uani 1 1 d . . .
O2 O 0.4888(3) 1.0824(3) 0.6989(2) 0.0363(6) Uani 1 1 d . . .
C5 C 0.4429(4) 1.2094(4) 0.8580(3) 0.0297(6) Uani 1 1 d . . .
C10 C 0.2976(5) 1.3001(4) 0.8155(3) 0.0367(8) Uani 1 1 d . . .
H10 H 0.2622 1.2863 0.7485 0.044 Uiso 1 1 calc R . .
C9 C 0.2060(5) 1.4097(4) 0.8710(3) 0.0402(8) Uani 1 1 d . . .
H9 H 0.1104 1.4699 0.8416 0.048 Uiso 1 1 calc R . .
C8 C 0.2593(5) 1.4286(4) 0.9722(3) 0.0402(8) Uani 1 1 d . . .
H8 H 0.1991 1.5025 1.0101 0.048 Uiso 1 1 calc R . .
C7 C 0.4008(5) 1.3385(4) 1.0167(3) 0.0392(8) Uani 1 1 d . . .
H7 H 0.4314 1.3499 1.0858 0.047 Uiso 1 1 calc R . .
C6 C 0.4974(5) 1.2312(4) 0.9587(3) 0.0338(7) Uani 1 1 d . . .
C11 C 1.0805(5) 0.6999(4) 0.4847(3) 0.0316(7) Uani 1 1 d . . .
C12 C 1.0422(5) 0.7308(4) 0.3710(3) 0.0333(7) Uani 1 1 d . . .
H12 H 0.9520 0.8045 0.3514 0.040 Uiso 1 1 calc R . .
C13 C 1.1368(5) 0.6530(4) 0.2877(3) 0.0400(8) Uani 1 1 d . . .
H13 H 1.1127 0.6759 0.2120 0.048 Uiso 1 1 calc R . .
C14 C 1.2691(5) 0.5396(4) 0.3180(3) 0.0408(9) Uani 1 1 d . . .
H14 H 1.3326 0.4867 0.2623 0.049 Uiso 1 1 calc R . .
C15 C 1.3058(5) 0.5056(4) 0.4301(3) 0.0382(8) Uani 1 1 d . . .
H15 H 1.3923 0.4289 0.4498 0.046 Uiso 1 1 calc R . .
C16 C 1.2138(5) 0.5859(4) 0.5145(3) 0.0355(7) Uani 1 1 d . . .
H16 H 1.2406 0.5640 0.5895 0.043 Uiso 1 1 calc R . .
C17 C 1.0243(5) 0.8873(4) 0.8543(3) 0.0394(8) Uani 1 1 d . . .
H17A H 1.0611 0.9859 0.8405 0.059 Uiso 1 1 calc R . .
H17B H 1.1328 0.8202 0.8564 0.059 Uiso 1 1 calc R . .
H17C H 0.9377 0.8660 0.9280 0.059 Uiso 1 1 calc R . .
O4 O 0.5000 1.0000 0.5000 0.0436(10) Uani 1 2 d S . .
O3 O 0.5017(3) 0.7850(3) 0.6991(2) 0.0385(6) Uani 1 1 d . . .
O5 O 0.6430(4) 1.1535(3) 1.0018(2) 0.0410(6) Uani 1 1 d . . .
H5 H 0.6946 1.0983 0.9582 0.062 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 O3 1.577(3) . ?
V O4 1.7859(6) . ?
V O1 1.835(2) . ?
V O2 1.898(2) . ?
V N1 2.090(3) . ?
O1 C1 1.317(4) . ?
C1 C2 1.365(5) . ?
C1 C11 1.476(4) . ?
C2 C3 1.424(4) . ?
C2 H2 0.9300 . ?
C3 N1 1.311(4) . ?
C3 C17 1.504(5) . ?
N1 N2 1.393(3) . ?
N2 C4 1.293(4) . ?
C4 O2 1.318(4) . ?
C4 C5 1.472(4) . ?
C5 C10 1.400(5) . ?
C5 C6 1.407(4) . ?
C10 C9 1.379(5) . ?
C10 H10 0.9300 . ?
C9 C8 1.400(5) . ?
C9 H9 0.9300 . ?
C8 C7 1.386(6) . ?
C8 H8 0.9300 . ?
C7 C6 1.390(4) . ?
C7 H7 0.9300 . ?
C6 O5 1.355(4) . ?
C11 C16 1.405(5) . ?
C11 C12 1.405(5) . ?
C12 C13 1.382(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.381(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.402(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O4 V 1.7859(6) 2_676 ?
O5 H5 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 V O4 109.59(10) . . ?
O3 V O1 106.14(13) . . ?
O4 V O1 96.21(8) . . ?
O3 V O2 105.82(12) . . ?
O4 V O2 91.25(8) . . ?
O1 V O2 142.42(13) . . ?
O3 V N1 96.45(12) . . ?
O4 V N1 153.14(9) . . ?
O1 V N1 82.35(11) . . ?
O2 V N1 74.91(10) . . ?
C1 O1 V 134.8(2) . . ?
O1 C1 C2 121.2(3) . . ?
O1 C1 C11 114.4(3) . . ?
C2 C1 C11 124.3(3) . . ?
C1 C2 C3 124.0(3) . . ?
C1 C2 H2 118.0 . . ?
C3 C2 H2 118.0 . . ?
N1 C3 C2 119.8(3) . . ?
N1 C3 C17 121.6(3) . . ?
C2 C3 C17 118.6(3) . . ?
C3 N1 N2 115.1(3) . . ?
C3 N1 V 129.9(2) . . ?
N2 N1 V 115.1(2) . . ?
C4 N2 N1 108.6(3) . . ?
N2 C4 O2 121.3(3) . . ?
N2 C4 C5 119.8(3) . . ?
O2 C4 C5 118.8(3) . . ?
C4 O2 V 118.6(2) . . ?
C10 C5 C6 119.3(3) . . ?
C10 C5 C4 119.7(3) . . ?
C6 C5 C4 120.8(3) . . ?
C9 C10 C5 121.3(3) . . ?
C9 C10 H10 119.4 . . ?
C5 C10 H10 119.4 . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C7 C8 C9 120.7(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C7 C6 120.5(3) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
O5 C6 C7 117.7(3) . . ?
O5 C6 C5 123.0(3) . . ?
C7 C6 C5 119.3(3) . . ?
C16 C11 C12 119.3(3) . . ?
C16 C11 C1 120.7(3) . . ?
C12 C11 C1 120.0(3) . . ?
C13 C12 C11 120.9(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 120.6(4) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 119.4(3) . . ?
C15 C16 H16 120.3 . . ?
C11 C16 H16 120.3 . . ?
C3 C17 H17A 109.5 . . ?
C3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
V O4 V 179.999(1) . 2_676 ?
C6 O5 H5 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.106
