# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_fz9_ba
_database_code_depnum_ccdc_archive 'CCDC 1911693'
loop_
_audit_author_name
_audit_author_address
'Robert Gyepes'
;Department of Inorganic Chemistry, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 O10 V2, 2(C4 H12 N), H2 O'
_chemical_formula_sum            'C24 H38 N2 O11 V2'
_chemical_formula_weight         632.44

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.7521(8)
_cell_length_b                   15.6443(11)
_cell_length_c                   18.2430(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3068.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    137
_cell_measurement_theta_min      3.9147
_cell_measurement_theta_max      22.4664

_exptl_crystal_description       prism
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.683
_exptl_crystal_size_mid          0.647
_exptl_crystal_size_min          0.388
_exptl_absorpt_coefficient_mu    0.664
_shelx_estimated_absorpt_T_min   0.660
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.78
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius KappaCCD with Bruker APEXII detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21743
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.715
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7004
_reflns_number_gt                5989
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.997

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0678P)²+2.7234P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7004
_refine_ls_number_parameters     367
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1335
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.055
_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_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 0.89168(7) 0.18557(5) 0.26177(4) 0.02616(19) Uani 1 1 d . . . . .
V2 V 0.65325(8) 0.30772(5) 0.23535(5) 0.0310(2) Uani 1 1 d . . . . .
O1 O 0.7317(3) 0.2290(2) 0.30567(17) 0.0276(7) Uani 1 1 d . . . . .
O2 O 0.7978(3) 0.2479(2) 0.18702(17) 0.0328(8) Uani 1 1 d . . . . .
O9 O 1.0212(3) 0.2380(3) 0.2546(2) 0.0448(9) Uani 1 1 d . . . . .
O7 O 0.9060(4) 0.1503(3) 0.3645(2) 0.0498(11) Uani 1 1 d . . . . .
O10 O 0.9088(4) 0.0940(2) 0.2219(2) 0.0455(9) Uani 1 1 d . . . . .
O3 O 0.6831(5) 0.3742(3) 0.1441(2) 0.0580(13) Uani 1 1 d . . . . .
O8 O 0.8296(4) 0.1526(4) 0.4777(2) 0.0598(13) Uani 1 1 d . . . . .
O5 O 0.5170(4) 0.2674(3) 0.2221(2) 0.0467(10) Uani 1 1 d . . . . .
O6 O 0.6406(5) 0.3882(2) 0.2905(2) 0.0577(12) Uani 1 1 d . . . . .
O4 O 0.8020(7) 0.3984(3) 0.0455(3) 0.084(2) Uani 1 1 d . . . . .
C10 C 0.8234(5) 0.1708(4) 0.4122(3) 0.0387(12) Uani 1 1 d . . . . .
C9 C 0.7109(4) 0.2197(3) 0.3816(2) 0.0272(9) Uani 1 1 d . . . . .
H12 H 0.706132 0.277424 0.405032 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5931(5) 0.1710(3) 0.3968(3) 0.0354(11) Uani 1 1 d . . . . .
C1 C 0.8423(6) 0.2756(4) 0.1177(3) 0.0424(13) Uani 1 1 d . . . . .
H6 H 0.933209 0.288293 0.121149 0.051 Uiso 1 1 calc R U . . .
C4 C 0.7042(6) 0.1707(4) 0.0503(3) 0.0485(15) Uani 1 1 d . . . . .
H5 H 0.637117 0.188266 0.080696 0.058 Uiso 1 1 calc R U . . .
C3 C 0.8204(5) 0.2070(4) 0.0595(3) 0.0378(12) Uani 1 1 d . . . . .
C8 C 0.9162(6) 0.1833(5) 0.0131(3) 0.0546(16) Uani 1 1 d . . . . .
H1 H 0.995312 0.209751 0.017773 0.066 Uiso 1 1 calc R U . . .
C12 C 0.5628(7) 0.1010(4) 0.3509(4) 0.0549(17) Uani 1 1 d . . . . .
H11 H 0.614648 0.090865 0.309607 0.066 Uiso 1 1 calc R U . . .
C7 C 0.8980(8) 0.1213(5) -0.0401(3) 0.0592(19) Uani 1 1 d . . . . .
H2 H 0.964520 0.105172 -0.071459 0.071 Uiso 1 1 calc R U . . .
C2 C 0.7736(8) 0.3549(4) 0.0986(3) 0.0579(19) Uani 1 1 d . . . . .
C15 C 0.4056(7) 0.1316(5) 0.4646(4) 0.066(2) Uani 1 1 d D U . . .
H8 H 0.347932 0.140680 0.503250 0.079 Uiso 1 1 calc R U . . .
C6 C 0.7831(9) 0.0832(4) -0.0475(4) 0.063(2) Uani 1 1 d . . . . .
H3 H 0.770852 0.039519 -0.082938 0.076 Uiso 1 1 calc R U . . .
C14 C 0.3914(8) 0.0673(5) 0.4172(5) 0.067(2) Uani 1 1 d . U . . .
H9 H 0.320587 0.031955 0.424128 0.080 Uiso 1 1 calc R U . . .
C5 C 0.6849(7) 0.1090(4) -0.0028(4) 0.0579(18) Uani 1 1 d . . . . .
H4 H 0.604867 0.084251 -0.008757 0.070 Uiso 1 1 calc R U . . .
C16 C 0.5183(6) 0.1898(5) 0.4543(4) 0.0574(18) Uani 1 1 d D . . . .
H7 H 0.534868 0.236364 0.486302 0.069 Uiso 1 1 calc R U . . .
C13 C 0.4651(7) 0.0475(5) 0.3615(4) 0.0631(19) Uani 1 1 d . . . . .
H10 H 0.450633 -0.000880 0.331191 0.076 Uiso 1 1 calc R U . . .
N1 N 0.2471(4) 0.3883(3) 0.3315(2) 0.0303(9) Uani 1 1 d . . . . .
C17 C 0.2262(6) 0.3977(3) 0.2506(3) 0.0407(12) Uani 1 1 d . . . . .
H13 H 0.158965 0.359483 0.235133 0.061 Uiso 1 1 calc R U . . .
H14 H 0.302673 0.382885 0.224241 0.061 Uiso 1 1 calc R U . . .
H15 H 0.203376 0.456986 0.239481 0.061 Uiso 1 1 calc R U . . .
C18 C 0.2812(6) 0.2978(3) 0.3488(3) 0.0399(12) Uani 1 1 d . . . . .
H16 H 0.292787 0.291534 0.401789 0.060 Uiso 1 1 calc R U . . .
H17 H 0.358635 0.282940 0.323464 0.060 Uiso 1 1 calc R U . . .
H18 H 0.214505 0.259625 0.332379 0.060 Uiso 1 1 calc R U . . .
C19 C 0.1338(6) 0.4121(4) 0.3721(3) 0.0505(16) Uani 1 1 d . . . . .
H19 H 0.148576 0.405618 0.424867 0.076 Uiso 1 1 calc R U . . .
H20 H 0.065105 0.374714 0.357245 0.076 Uiso 1 1 calc R U . . .
H21 H 0.112281 0.471616 0.361349 0.076 Uiso 1 1 calc R U . . .
C20 C 0.3514(7) 0.4456(4) 0.3534(4) 0.0588(18) Uani 1 1 d . . . . .
H22 H 0.363391 0.442388 0.406583 0.088 Uiso 1 1 calc R U . . .
H23 H 0.331592 0.504575 0.339500 0.088 Uiso 1 1 calc R U . . .
H24 H 0.427788 0.427572 0.328523 0.088 Uiso 1 1 calc R U . . .
N2 N 0.2635(4) 0.1035(2) 0.1505(2) 0.0272(8) Uani 1 1 d . . . . .
C21 C 0.3916(5) 0.0807(4) 0.1276(3) 0.0429(13) Uani 1 1 d . . . . .
H25 H 0.451371 0.117043 0.153564 0.064 Uiso 1 1 calc R U . . .
H26 H 0.400296 0.089452 0.074637 0.064 Uiso 1 1 calc R U . . .
H27 H 0.407839 0.020629 0.139385 0.064 Uiso 1 1 calc R U . . .
C22 C 0.2388(5) 0.1943(3) 0.1303(3) 0.0391(11) Uani 1 1 d . . . . .
H28 H 0.156297 0.211050 0.148096 0.059 Uiso 1 1 calc R U . . .
H29 H 0.241933 0.200503 0.076920 0.059 Uiso 1 1 calc R U . . .
H30 H 0.302028 0.231125 0.152757 0.059 Uiso 1 1 calc R U . . .
C23 C 0.2537(7) 0.0938(4) 0.2319(3) 0.0521(16) Uani 1 1 d . . . . .
H31 H 0.320478 0.126360 0.255570 0.078 Uiso 1 1 calc R U . . .
H32 H 0.261413 0.033277 0.245001 0.078 Uiso 1 1 calc R U . . .
H33 H 0.172974 0.115453 0.248502 0.078 Uiso 1 1 calc R U . . .
C24 C 0.1726(6) 0.0464(4) 0.1141(4) 0.0486(14) Uani 1 1 d . . . . .
H34 H 0.192387 -0.013195 0.125637 0.073 Uiso 1 1 calc R U . . .
H35 H 0.176655 0.054984 0.060899 0.073 Uiso 1 1 calc R U . . .
H36 H 0.088614 0.059815 0.131508 0.073 Uiso 1 1 calc R U . . .
O11 O 0.0764(6) 0.0707(5) 0.5057(4) 0.095(2) Uani 1 1 d D . . . .
H11A H 0.006(6) 0.079(8) 0.480(6) 0.114 Uiso 1 1 d D U . . .
H11B H 0.073(12) 0.033(6) 0.465(4) 0.114 Uiso 1 1 d D U . . .


_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 O10 1.617(4) . ?
V1 O9 1.621(4) . ?
V1 O2 1.957(3) . ?
V1 O7 1.960(4) . ?
V1 O1 2.015(3) . ?
V2 O5 1.613(4) . ?
V2 O6 1.617(4) . ?
V2 O1 1.969(3) . ?
V2 O3 1.989(4) . ?
V2 O2 2.017(3) . ?
O1 C9 1.411(5) . ?
O2 C1 1.420(6) . ?
O7 C10 1.283(7) . ?
O3 C2 1.314(9) . ?
O8 C10 1.231(6) . ?
O4 C2 1.224(7) . ?
C10 C9 1.536(7) . ?
C9 C11 1.504(7) . ?
C9 H12 1.0000 . ?
C11 C16 1.355(8) . ?
C11 C12 1.416(9) . ?
C1 C2 1.485(9) . ?
C1 C3 1.527(8) . ?
C1 H6 1.0000 . ?
C4 C3 1.383(9) . ?
C4 C5 1.383(9) . ?
C4 H5 0.9500 . ?
C3 C8 1.384(8) . ?
C8 C7 1.386(10) . ?
C8 H1 0.9500 . ?
C12 C13 1.358(10) . ?
C12 H11 0.9500 . ?
C7 C6 1.378(12) . ?
C7 H2 0.9500 . ?
C15 C14 1.334(11) . ?
C15 C16 1.527(11) . ?
C15 H8 0.9500 . ?
C6 C5 1.394(11) . ?
C6 H3 0.9500 . ?
C14 C13 1.325(11) . ?
C14 H9 0.9500 . ?
C5 H4 0.9500 . ?
C16 H7 0.9500 . ?
C13 H10 0.9500 . ?
N1 C19 1.474(7) . ?
N1 C20 1.490(7) . ?
N1 C18 1.496(6) . ?
N1 C17 1.501(6) . ?
C17 H13 0.9800 . ?
C17 H14 0.9800 . ?
C17 H15 0.9800 . ?
C18 H16 0.9800 . ?
C18 H17 0.9800 . ?
C18 H18 0.9800 . ?
C19 H19 0.9800 . ?
C19 H20 0.9800 . ?
C19 H21 0.9800 . ?
C20 H22 0.9800 . ?
C20 H23 0.9800 . ?
C20 H24 0.9800 . ?
N2 C24 1.481(7) . ?
N2 C21 1.484(7) . ?
N2 C22 1.492(6) . ?
N2 C23 1.496(6) . ?
C21 H25 0.9800 . ?
C21 H26 0.9800 . ?
C21 H27 0.9800 . ?
C22 H28 0.9800 . ?
C22 H29 0.9800 . ?
C22 H30 0.9800 . ?
C23 H31 0.9800 . ?
C23 H32 0.9800 . ?
C23 H33 0.9800 . ?
C24 H34 0.9800 . ?
C24 H35 0.9800 . ?
C24 H36 0.9800 . ?
O11 H11A 0.90(4) . ?
O11 H11B 0.95(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
O10 V1 O9 108.3(2) . . ?
O10 V1 O2 100.71(18) . . ?
O9 V1 O2 97.74(19) . . ?
O10 V1 O7 99.9(2) . . ?
O9 V1 O7 98.8(2) . . ?
O2 V1 O7 147.91(15) . . ?
O10 V1 O1 125.05(19) . . ?
O9 V1 O1 126.51(18) . . ?
O2 V1 O1 70.66(13) . . ?
O7 V1 O1 77.39(14) . . ?
O5 V2 O6 108.7(3) . . ?
O5 V2 O1 104.00(18) . . ?
O6 V2 O1 96.76(19) . . ?
O5 V2 O3 103.1(2) . . ?
O6 V2 O3 97.3(2) . . ?
O1 V2 O3 143.47(18) . . ?
O5 V2 O2 116.93(19) . . ?
O6 V2 O2 134.3(2) . . ?
O1 V2 O2 70.38(13) . . ?
O3 V2 O2 75.68(17) . . ?
C9 O1 V2 129.5(3) . . ?
C9 O1 V1 119.4(3) . . ?
V2 O1 V1 108.52(15) . . ?
C1 O2 V1 126.8(3) . . ?
C1 O2 V2 120.5(3) . . ?
V1 O2 V2 108.91(15) . . ?
C10 O7 V1 121.6(3) . . ?
C2 O3 V2 121.8(4) . . ?
O8 C10 O7 124.3(5) . . ?
O8 C10 C9 120.7(5) . . ?
O7 C10 C9 115.0(4) . . ?
O1 C9 C11 111.5(4) . . ?
O1 C9 C10 106.4(4) . . ?
C11 C9 C10 110.1(4) . . ?
O1 C9 H12 109.6 . . ?
C11 C9 H12 109.6 . . ?
C10 C9 H12 109.6 . . ?
C16 C11 C12 119.3(6) . . ?
C16 C11 C9 122.2(6) . . ?
C12 C11 C9 118.5(5) . . ?
O2 C1 C2 107.3(5) . . ?
O2 C1 C3 110.7(4) . . ?
C2 C1 C3 110.3(5) . . ?
O2 C1 H6 109.5 . . ?
C2 C1 H6 109.5 . . ?
C3 C1 H6 109.5 . . ?
C3 C4 C5 120.5(6) . . ?
C3 C4 H5 119.8 . . ?
C5 C4 H5 119.8 . . ?
C4 C3 C8 119.2(6) . . ?
C4 C3 C1 120.8(5) . . ?
C8 C3 C1 120.0(6) . . ?
C3 C8 C7 120.7(7) . . ?
C3 C8 H1 119.6 . . ?
C7 C8 H1 119.6 . . ?
C13 C12 C11 124.8(7) . . ?
C13 C12 H11 117.6 . . ?
C11 C12 H11 117.6 . . ?
C6 C7 C8 119.8(6) . . ?
C6 C7 H2 120.1 . . ?
C8 C7 H2 120.1 . . ?
O4 C2 O3 123.8(7) . . ?
O4 C2 C1 121.8(7) . . ?
O3 C2 C1 114.3(5) . . ?
C14 C15 C16 117.4(7) . . ?
C14 C15 H8 121.3 . . ?
C16 C15 H8 121.3 . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 H3 120.1 . . ?
C5 C6 H3 120.1 . . ?
C13 C14 C15 127.2(8) . . ?
C13 C14 H9 116.4 . . ?
C15 C14 H9 116.4 . . ?
C4 C5 C6 119.9(7) . . ?
C4 C5 H4 120.1 . . ?
C6 C5 H4 120.1 . . ?
C11 C16 C15 115.9(7) . . ?
C11 C16 H7 122.1 . . ?
C15 C16 H7 122.1 . . ?
C14 C13 C12 115.3(8) . . ?
C14 C13 H10 122.4 . . ?
C12 C13 H10 122.4 . . ?
C19 N1 C20 109.6(5) . . ?
C19 N1 C18 109.6(4) . . ?
C20 N1 C18 109.2(5) . . ?
C19 N1 C17 110.3(4) . . ?
C20 N1 C17 108.5(4) . . ?
C18 N1 C17 109.7(4) . . ?
N1 C17 H13 109.5 . . ?
N1 C17 H14 109.5 . . ?
H13 C17 H14 109.5 . . ?
N1 C17 H15 109.5 . . ?
H13 C17 H15 109.5 . . ?
H14 C17 H15 109.5 . . ?
N1 C18 H16 109.5 . . ?
N1 C18 H17 109.5 . . ?
H16 C18 H17 109.5 . . ?
N1 C18 H18 109.5 . . ?
H16 C18 H18 109.5 . . ?
H17 C18 H18 109.5 . . ?
N1 C19 H19 109.5 . . ?
N1 C19 H20 109.5 . . ?
H19 C19 H20 109.5 . . ?
N1 C19 H21 109.5 . . ?
H19 C19 H21 109.5 . . ?
H20 C19 H21 109.5 . . ?
N1 C20 H22 109.5 . . ?
N1 C20 H23 109.5 . . ?
H22 C20 H23 109.5 . . ?
N1 C20 H24 109.5 . . ?
H22 C20 H24 109.5 . . ?
H23 C20 H24 109.5 . . ?
C24 N2 C21 110.0(4) . . ?
C24 N2 C22 110.2(4) . . ?
C21 N2 C22 108.9(4) . . ?
C24 N2 C23 109.8(5) . . ?
C21 N2 C23 108.7(4) . . ?
C22 N2 C23 109.2(4) . . ?
N2 C21 H25 109.5 . . ?
N2 C21 H26 109.5 . . ?
H25 C21 H26 109.5 . . ?
N2 C21 H27 109.5 . . ?
H25 C21 H27 109.5 . . ?
H26 C21 H27 109.5 . . ?
N2 C22 H28 109.5 . . ?
N2 C22 H29 109.5 . . ?
H28 C22 H29 109.5 . . ?
N2 C22 H30 109.5 . . ?
H28 C22 H30 109.5 . . ?
H29 C22 H30 109.5 . . ?
N2 C23 H31 109.5 . . ?
N2 C23 H32 109.5 . . ?
H31 C23 H32 109.5 . . ?
N2 C23 H33 109.5 . . ?
H31 C23 H33 109.5 . . ?
H32 C23 H33 109.5 . . ?
N2 C24 H34 109.5 . . ?
N2 C24 H35 109.5 . . ?
H34 C24 H35 109.5 . . ?
N2 C24 H36 109.5 . . ?
H34 C24 H36 109.5 . . ?
H35 C24 H36 109.5 . . ?
H11A O11 H11B 70(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O7 C10 O8 -177.8(5) . . . . ?
V1 O7 C10 C9 3.4(7) . . . . ?
V2 O1 C9 C11 77.4(5) . . . . ?
V1 O1 C9 C11 -123.0(3) . . . . ?
V2 O1 C9 C10 -162.5(3) . . . . ?
V1 O1 C9 C10 -3.0(5) . . . . ?
O8 C10 C9 O1 -179.1(5) . . . . ?
O7 C10 C9 O1 -0.2(6) . . . . ?
O8 C10 C9 C11 -58.1(7) . . . . ?
O7 C10 C9 C11 120.8(5) . . . . ?
O1 C9 C11 C16 -144.0(5) . . . . ?
C10 C9 C11 C16 98.1(6) . . . . ?
O1 C9 C11 C12 38.5(6) . . . . ?
C10 C9 C11 C12 -79.3(5) . . . . ?
V1 O2 C1 C2 -149.4(4) . . . . ?
V2 O2 C1 C2 6.1(6) . . . . ?
V1 O2 C1 C3 90.2(5) . . . . ?
V2 O2 C1 C3 -114.3(4) . . . . ?
C5 C4 C3 C8 2.5(9) . . . . ?
C5 C4 C3 C1 179.6(5) . . . . ?
O2 C1 C3 C4 51.4(7) . . . . ?
C2 C1 C3 C4 -67.2(7) . . . . ?
O2 C1 C3 C8 -131.6(5) . . . . ?
C2 C1 C3 C8 109.9(6) . . . . ?
C4 C3 C8 C7 -2.7(9) . . . . ?
C1 C3 C8 C7 -179.8(5) . . . . ?
C16 C11 C12 C13 -2.9(9) . . . . ?
C9 C11 C12 C13 174.6(6) . . . . ?
C3 C8 C7 C6 0.5(10) . . . . ?
V2 O3 C2 O4 -173.3(6) . . . . ?
V2 O3 C2 C1 5.4(8) . . . . ?
O2 C1 C2 O4 171.9(7) . . . . ?
C3 C1 C2 O4 -67.5(9) . . . . ?
O2 C1 C2 O3 -6.9(8) . . . . ?
C3 C1 C2 O3 113.7(6) . . . . ?
C8 C7 C6 C5 1.9(10) . . . . ?
C16 C15 C14 C13 0.4(11) . . . . ?
C3 C4 C5 C6 -0.1(10) . . . . ?
C7 C6 C5 C4 -2.1(10) . . . . ?
C12 C11 C16 C15 0.4(8) . . . . ?
C9 C11 C16 C15 -177.0(5) . . . . ?
C14 C15 C16 C11 0.7(9) . . . . ?
C15 C14 C13 C12 -2.6(12) . . . . ?
C11 C12 C13 C14 3.9(10) . . . . ?

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
_geom_hbond_publ_flag
C17 H13 O9 0.98 2.44 3.333(7) 152 1_455 yes
C17 H15 O10 0.98 2.56 3.434(7) 149 3_655 yes
C18 H16 O8 0.98 2.40 3.300(7) 153 4_456 yes
C18 H17 O5 0.98 2.52 3.463(7) 160 . yes
C18 H18 O9 0.98 2.54 3.413(7) 148 1_455 yes
C19 H21 O10 0.98 2.45 3.355(7) 153 3_655 yes
C20 H24 O6 0.98 2.47 3.434(10) 168 . yes
C21 H26 O4 0.98 2.44 3.317(8) 149 4_455 yes
C21 H27 O6 0.98 2.49 3.380(7) 151 3_645 yes
C22 H28 O9 0.98 2.46 3.329(7) 147 1_455 yes
C23 H32 O6 0.98 2.59 3.436(7) 145 3_645 yes
C23 H33 O9 0.98 2.52 3.393(8) 148 1_455 yes
C24 H35 O4 0.98 2.47 3.339(8) 147 4_455 yes
C24 H36 O10 0.98 2.60 3.531(8) 159 1_455 yes
O11 H11A O8 0.90(4) 2.22(8) 2.990(8) 144(10) 1_455 yes
O11 H11B O4 0.95(4) 2.51(10) 3.138(9) 124(9) 3_645 yes

_refine_diff_density_max         1.045
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_fz5157
_database_code_depnum_ccdc_archive 'CCDC 1911695'
loop_
_audit_author_name
_audit_author_address
'Robert Gyepes'
;Department of Inorganic Chemistry, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C16 H12 O10 V2, 2(C24 H20 P), 2(C3 H6 O), 2(H2 O)'
_chemical_formula_sum            'C70 H68 O14 P2 V2'
_chemical_formula_weight         1297.06

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'
P P 0.1023 0.0942 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.8560(3)
_cell_length_b                   11.7821(4)
_cell_length_c                   13.1551(4)
_cell_angle_alpha                74.534(2)
_cell_angle_beta                 82.6910(10)
_cell_angle_gamma                71.7350(10)
_cell_volume                     1538.24(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9410
_cell_measurement_theta_min      2.2935
_cell_measurement_theta_max      29.0635

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.968
_exptl_crystal_size_mid          0.428
_exptl_crystal_size_min          0.276
_exptl_absorpt_coefficient_mu    0.424
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius KappaCCD with Bruker APEXII detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75879
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.608
_diffrn_reflns_theta_max         29.232
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8321
_reflns_number_gt                7496
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0360P)²+0.8523P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8321
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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 0.51730(2) 0.50808(2) 0.37337(2) 0.01406(5) Uani 1 1 d . . . . .
O1 O 0.64673(9) 0.54404(9) 0.31835(7) 0.02480(19) Uani 1 1 d . . . . .
O2 O 0.39932(9) 0.57990(9) 0.29386(7) 0.02334(18) Uani 1 1 d . . . . .
O3 O 0.53765(8) 0.39410(7) 0.52034(6) 0.01670(15) Uani 1 1 d . . . . .
O4 O 0.54953(8) 0.34334(8) 0.34709(7) 0.02151(17) Uani 1 1 d . . . . .
O5 O 0.59741(10) 0.14062(9) 0.41027(8) 0.0282(2) Uani 1 1 d . . . . .
C1 C 0.58225(11) 0.26604(10) 0.53118(9) 0.0172(2) Uani 1 1 d . . . . .
H1 H 0.524174 0.225633 0.583429 0.021 Uiso 1 1 calc R U . . .
C2 C 0.57571(11) 0.24471(11) 0.42203(9) 0.0190(2) Uani 1 1 d . . . . .
C3 C 0.72126(11) 0.20824(11) 0.56316(9) 0.0171(2) Uani 1 1 d . . . . .
C4 C 0.76032(12) 0.08708(11) 0.62171(10) 0.0229(2) Uani 1 1 d . . . . .
H4 H 0.697366 0.044851 0.649953 0.027 Uiso 1 1 calc R U . . .
C5 C 0.89114(13) 0.02714(12) 0.63928(12) 0.0286(3) Uani 1 1 d . . . . .
H5 H 0.917340 -0.056159 0.678482 0.034 Uiso 1 1 calc R U . . .
C6 C 0.98294(13) 0.08866(13) 0.59976(11) 0.0285(3) Uani 1 1 d . . . . .
H6 H 1.072435 0.047314 0.610426 0.034 Uiso 1 1 calc R U . . .
C7 C 0.94394(12) 0.21085(14) 0.54453(11) 0.0271(3) Uani 1 1 d . . . . .
H7 H 1.006703 0.253945 0.518982 0.033 Uiso 1 1 calc R U . . .
C8 C 0.81350(12) 0.27073(12) 0.52630(10) 0.0222(2) Uani 1 1 d . . . . .
H8 H 0.787354 0.354620 0.488524 0.027 Uiso 1 1 calc R U . . .
P1 P 0.14001(3) 0.41659(3) 0.20892(2) 0.01376(6) Uani 1 1 d . . . . .
C9 C 0.27545(10) 0.40746(10) 0.11581(8) 0.01518(19) Uani 1 1 d . . . . .
C10 C 0.40095(11) 0.34121(11) 0.14668(9) 0.0187(2) Uani 1 1 d . . . . .
H10 H 0.417378 0.304029 0.219078 0.022 Uiso 1 1 calc R U . . .
C11 C 0.50197(12) 0.33013(12) 0.07022(11) 0.0236(2) Uani 1 1 d . . . . .
H11 H 0.588028 0.285191 0.090523 0.028 Uiso 1 1 calc R U . . .
C12 C 0.47816(12) 0.38400(12) -0.03516(10) 0.0239(2) Uani 1 1 d . . . . .
H12 H 0.547700 0.374625 -0.086904 0.029 Uiso 1 1 calc R U . . .
C13 C 0.35330(13) 0.45170(13) -0.06586(9) 0.0243(2) Uani 1 1 d . . . . .
H13 H 0.337635 0.489133 -0.138341 0.029 Uiso 1 1 calc R U . . .
C14 C 0.25181(12) 0.46456(12) 0.00918(9) 0.0210(2) Uani 1 1 d . . . . .
H14 H 0.166428 0.511870 -0.011383 0.025 Uiso 1 1 calc R U . . .
C15 C 0.04983(11) 0.57508(10) 0.19689(8) 0.0160(2) Uani 1 1 d . . . . .
C16 C -0.08515(11) 0.61671(12) 0.19281(9) 0.0211(2) Uani 1 1 d . . . . .
H16 H -0.132598 0.561811 0.191275 0.025 Uiso 1 1 calc R U . . .
C17 C -0.14930(13) 0.73924(13) 0.19101(10) 0.0274(3) Uani 1 1 d . . . . .
H17 H -0.241119 0.768416 0.187392 0.033 Uiso 1 1 calc R U . . .
C18 C -0.08104(14) 0.81921(12) 0.19443(10) 0.0288(3) Uani 1 1 d . . . . .
H18 H -0.126064 0.902555 0.194463 0.035 Uiso 1 1 calc R U . . .
C19 C 0.05327(14) 0.77784(12) 0.19782(10) 0.0259(3) Uani 1 1 d . . . . .
H19 H 0.100027 0.833129 0.199804 0.031 Uiso 1 1 calc R U . . .
C20 C 0.11959(12) 0.65610(11) 0.19834(9) 0.0202(2) Uani 1 1 d . . . . .
H20 H 0.211639 0.628072 0.199669 0.024 Uiso 1 1 calc R U . . .
C21 C 0.04004(10) 0.33183(10) 0.18365(9) 0.0161(2) Uani 1 1 d . . . . .
C22 C 0.07000(11) 0.27380(12) 0.10067(9) 0.0206(2) Uani 1 1 d . . . . .
H22 H 0.144326 0.278898 0.055076 0.025 Uiso 1 1 calc R U . . .
C23 C -0.00952(13) 0.20823(13) 0.08482(10) 0.0253(3) Uani 1 1 d . . . . .
H23 H 0.010504 0.168879 0.027940 0.030 Uiso 1 1 calc R U . . .
C24 C -0.11745(12) 0.19989(12) 0.15118(11) 0.0249(2) Uani 1 1 d . . . . .
H24 H -0.171463 0.155227 0.139634 0.030 Uiso 1 1 calc R U . . .
C25 C -0.14682(12) 0.25655(13) 0.23439(11) 0.0268(3) Uani 1 1 d . . . . .
H25 H -0.220941 0.250590 0.279998 0.032 Uiso 1 1 calc R U . . .
C26 C -0.06845(12) 0.32200(12) 0.25142(10) 0.0230(2) Uani 1 1 d . . . . .
H26 H -0.088357 0.360163 0.309032 0.028 Uiso 1 1 calc R U . . .
C27 C 0.19258(10) 0.34830(10) 0.34090(8) 0.0155(2) Uani 1 1 d . . . . .
C28 C 0.24658(11) 0.22053(11) 0.36907(9) 0.0195(2) Uani 1 1 d . . . . .
H28 H 0.255256 0.173466 0.318718 0.023 Uiso 1 1 calc R U . . .
C29 C 0.28750(12) 0.16249(12) 0.47062(10) 0.0223(2) Uani 1 1 d . . . . .
H29 H 0.324977 0.075711 0.489924 0.027 Uiso 1 1 calc R U . . .
C30 C 0.27341(12) 0.23177(12) 0.54370(9) 0.0227(2) Uani 1 1 d . . . . .
H30 H 0.299965 0.191866 0.613641 0.027 Uiso 1 1 calc R U . . .
C31 C 0.22105(13) 0.35861(13) 0.51601(9) 0.0242(2) Uani 1 1 d . . . . .
H31 H 0.213038 0.405233 0.566591 0.029 Uiso 1 1 calc R U . . .
C32 C 0.18009(12) 0.41791(11) 0.41404(9) 0.0204(2) Uani 1 1 d . . . . .
H32 H 0.144062 0.504870 0.394706 0.024 Uiso 1 1 calc R U . . .
O0AA O 0.39165(14) 1.06565(11) 0.12834(12) 0.0505(3) Uani 1 1 d . . . . .
C33 C 0.39140(13) 0.96898(13) 0.11310(11) 0.0287(3) Uani 1 1 d . . . . .
C34 C 0.47926(15) 0.84939(14) 0.16801(13) 0.0344(3) Uani 1 1 d . . . . .
H34A H 0.527182 0.863033 0.219744 0.052 Uiso 1 1 calc R U . . .
H34B H 0.540715 0.812295 0.116241 0.052 Uiso 1 1 calc R U . . .
H34C H 0.427838 0.793960 0.204283 0.052 Uiso 1 1 calc R U . . .
C35 C 0.30276(17) 0.96475(18) 0.03661(14) 0.0429(4) Uani 1 1 d . . . . .
H35A H 0.241387 0.920447 0.074618 0.064 Uiso 1 1 calc R U . . .
H35B H 0.354163 0.922162 -0.016345 0.064 Uiso 1 1 calc R U . . .
H35C H 0.254747 1.048862 0.001516 0.064 Uiso 1 1 calc R U . . .
O1AA O 0.63315(12) 0.03987(11) 0.23544(9) 0.0404(3) Uani 1 1 d . . . . .
H7A H 0.617999 0.073015 0.284218 0.061 Uiso 1 1 d R U . . .
H7B H 0.561999 0.049015 0.216018 0.061 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6213(9) . ?
V1 O2 1.6248(8) . ?
V1 O3 1.9636(8) 2_666 ?
V1 O4 1.9775(9) . ?
V1 O3 2.0319(8) . ?
O3 C1 1.4057(13) . ?
O4 C2 1.2870(15) . ?
O5 C2 1.2224(15) . ?
C1 C3 1.5109(15) . ?
C1 C2 1.5361(16) . ?
C1 H1 1.0000 . ?
C3 C8 1.3885(16) . ?
C3 C4 1.3886(16) . ?
C4 C5 1.3917(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.3895(17) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
P1 C9 1.7851(11) . ?
P1 C15 1.7906(11) . ?
P1 C27 1.7908(11) . ?
P1 C21 1.7984(11) . ?
C9 C10 1.3912(15) . ?
C9 C14 1.4023(15) . ?
C10 C11 1.3896(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.3822(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.3880(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.3819(16) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.3950(15) . ?
C15 C20 1.3970(16) . ?
C16 C17 1.3876(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3872(17) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.3903(15) . ?
C21 C26 1.3995(16) . ?
C22 C23 1.3912(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3823(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.3831(19) . ?
C24 H24 0.9500 . ?
C25 C26 1.3858(18) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.3910(16) . ?
C27 C28 1.3970(16) . ?
C28 C29 1.3867(16) . ?
C28 H28 0.9500 . ?
C29 C30 1.3845(18) . ?
C29 H29 0.9500 . ?
C30 C31 1.3853(19) . ?
C30 H30 0.9500 . ?
C31 C32 1.3937(16) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
O0AA C33 1.2088(18) . ?
C33 C34 1.486(2) . ?
C33 C35 1.498(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O1AA H7A 0.8111 . ?
O1AA H7B 0.8104 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 108.41(5) . . ?
O1 V1 O3 102.57(4) . 2_666 ?
O2 V1 O3 98.98(4) . 2_666 ?
O1 V1 O4 101.65(4) . . ?
O2 V1 O4 96.87(4) . . ?
O3 V1 O4 145.01(4) 2_666 . ?
O1 V1 O3 115.48(4) . . ?
O2 V1 O3 136.07(4) . . ?
O3 V1 O3 70.36(4) 2_666 . ?
O4 V1 O3 76.57(3) . . ?
C1 O3 V1 131.11(7) . 2_666 ?
C1 O3 V1 119.23(6) . . ?
V1 O3 V1 109.64(4) 2_666 . ?
C2 O4 V1 121.82(7) . . ?
O3 C1 C3 113.87(9) . . ?
O3 C1 C2 106.52(9) . . ?
C3 C1 C2 107.31(9) . . ?
O3 C1 H1 109.7 . . ?
C3 C1 H1 109.7 . . ?
C2 C1 H1 109.7 . . ?
O5 C2 O4 124.63(11) . . ?
O5 C2 C1 120.77(11) . . ?
O4 C2 C1 114.57(10) . . ?
C8 C3 C4 119.26(11) . . ?
C8 C3 C1 120.71(10) . . ?
C4 C3 C1 119.75(10) . . ?
C3 C4 C5 120.39(12) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.07(12) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 119.72(12) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 120.33(12) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C3 C8 C7 120.15(12) . . ?
C3 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C9 P1 C15 108.90(5) . . ?
C9 P1 C27 110.93(5) . . ?
C15 P1 C27 109.77(5) . . ?
C9 P1 C21 109.32(5) . . ?
C15 P1 C21 110.71(5) . . ?
C27 P1 C21 107.21(5) . . ?
C10 C9 C14 120.36(10) . . ?
C10 C9 P1 121.33(8) . . ?
C14 C9 P1 118.26(8) . . ?
C11 C10 C9 119.13(11) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C12 C11 C10 120.49(11) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.42(11) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 119.89(11) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C9 119.68(11) . . ?
C13 C14 H14 120.2 . . ?
C9 C14 H14 120.2 . . ?
C16 C15 C20 120.34(11) . . ?
C16 C15 P1 122.43(9) . . ?
C20 C15 P1 117.11(8) . . ?
C17 C16 C15 119.23(12) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C18 C17 C16 120.68(12) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.01(12) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 120.30(12) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 119.42(11) . . ?
C19 C20 H20 120.3 . . ?
C15 C20 H20 120.3 . . ?
C22 C21 C26 119.73(11) . . ?
C22 C21 P1 121.64(9) . . ?
C26 C21 P1 118.61(9) . . ?
C21 C22 C23 119.60(11) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.51(12) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 120.02(12) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.20(12) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 119.93(11) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C32 C27 C28 120.38(10) . . ?
C32 C27 P1 122.19(9) . . ?
C28 C27 P1 117.42(8) . . ?
C29 C28 C27 119.93(11) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.60(11) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 120.76(11) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C30 C31 C32 120.10(11) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 119.23(11) . . ?
C27 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
O0AA C33 C34 121.92(14) . . ?
O0AA C33 C35 121.19(15) . . ?
C34 C33 C35 116.89(14) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
H7A O1AA H7B 104.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O3 C1 C3 -76.52(12) 2_666 . . . ?
V1 O3 C1 C3 105.48(9) . . . . ?
V1 O3 C1 C2 165.41(7) 2_666 . . . ?
V1 O3 C1 C2 -12.60(11) . . . . ?
V1 O4 C2 O5 -179.41(9) . . . . ?
V1 O4 C2 C1 -1.17(13) . . . . ?
O3 C1 C2 O5 -173.10(10) . . . . ?
C3 C1 C2 O5 64.59(14) . . . . ?
O3 C1 C2 O4 8.59(13) . . . . ?
C3 C1 C2 O4 -113.72(11) . . . . ?
O3 C1 C3 C8 -35.53(15) . . . . ?
C2 C1 C3 C8 82.09(13) . . . . ?
O3 C1 C3 C4 150.64(10) . . . . ?
C2 C1 C3 C4 -91.74(13) . . . . ?
C8 C3 C4 C5 -2.85(18) . . . . ?
C1 C3 C4 C5 171.06(11) . . . . ?
C3 C4 C5 C6 1.0(2) . . . . ?
C4 C5 C6 C7 1.3(2) . . . . ?
C5 C6 C7 C8 -1.7(2) . . . . ?
C4 C3 C8 C7 2.45(18) . . . . ?
C1 C3 C8 C7 -171.40(11) . . . . ?
C6 C7 C8 C3 -0.2(2) . . . . ?
C15 P1 C9 C10 128.10(10) . . . . ?
C27 P1 C9 C10 7.18(11) . . . . ?
C21 P1 C9 C10 -110.83(10) . . . . ?
C15 P1 C9 C14 -54.63(11) . . . . ?
C27 P1 C9 C14 -175.54(9) . . . . ?
C21 P1 C9 C14 66.44(11) . . . . ?
C14 C9 C10 C11 -1.42(18) . . . . ?
P1 C9 C10 C11 175.80(9) . . . . ?
C9 C10 C11 C12 -0.11(19) . . . . ?
C10 C11 C12 C13 1.11(19) . . . . ?
C11 C12 C13 C14 -0.6(2) . . . . ?
C12 C13 C14 C9 -0.96(19) . . . . ?
C10 C9 C14 C13 1.96(18) . . . . ?
P1 C9 C14 C13 -175.34(10) . . . . ?
C9 P1 C15 C16 133.70(9) . . . . ?
C27 P1 C15 C16 -104.68(10) . . . . ?
C21 P1 C15 C16 13.48(11) . . . . ?
C9 P1 C15 C20 -50.24(10) . . . . ?
C27 P1 C15 C20 71.38(10) . . . . ?
C21 P1 C15 C20 -170.46(8) . . . . ?
C20 C15 C16 C17 -0.48(17) . . . . ?
P1 C15 C16 C17 175.45(9) . . . . ?
C15 C16 C17 C18 -0.74(19) . . . . ?
C16 C17 C18 C19 1.1(2) . . . . ?
C17 C18 C19 C20 -0.3(2) . . . . ?
C18 C19 C20 C15 -0.88(18) . . . . ?
C16 C15 C20 C19 1.28(17) . . . . ?
P1 C15 C20 C19 -174.86(9) . . . . ?
C9 P1 C21 C22 -1.48(11) . . . . ?
C15 P1 C21 C22 118.49(10) . . . . ?
C27 P1 C21 C22 -121.80(10) . . . . ?
C9 P1 C21 C26 176.83(9) . . . . ?
C15 P1 C21 C26 -63.20(11) . . . . ?
C27 P1 C21 C26 56.51(11) . . . . ?
C26 C21 C22 C23 1.07(18) . . . . ?
P1 C21 C22 C23 179.36(10) . . . . ?
C21 C22 C23 C24 -0.34(19) . . . . ?
C22 C23 C24 C25 -0.3(2) . . . . ?
C23 C24 C25 C26 0.1(2) . . . . ?
C24 C25 C26 C21 0.6(2) . . . . ?
C22 C21 C26 C25 -1.21(18) . . . . ?
P1 C21 C26 C25 -179.56(10) . . . . ?
C9 P1 C27 C32 111.06(10) . . . . ?
C15 P1 C27 C32 -9.34(11) . . . . ?
C21 P1 C27 C32 -129.65(10) . . . . ?
C9 P1 C27 C28 -69.45(10) . . . . ?
C15 P1 C27 C28 170.15(9) . . . . ?
C21 P1 C27 C28 49.84(10) . . . . ?
C32 C27 C28 C29 0.29(17) . . . . ?
P1 C27 C28 C29 -179.21(9) . . . . ?
C27 C28 C29 C30 0.56(18) . . . . ?
C28 C29 C30 C31 -1.16(18) . . . . ?
C29 C30 C31 C32 0.90(19) . . . . ?
C28 C27 C32 C31 -0.55(18) . . . . ?
P1 C27 C32 C31 178.93(9) . . . . ?
C30 C31 C32 C27 -0.05(19) . . . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_fz3_ba
_database_code_depnum_ccdc_archive 'CCDC 1911697'
loop_
_audit_author_name
_audit_author_address
'Robert Gyepes'
;Department of Inorganic Chemistry, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 O10 V2, 2(C4 H12 N)'
_chemical_formula_sum            'C24 H36 N2 O10 V2'
_chemical_formula_weight         614.43

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                   12.3039(5)
_cell_length_b                   13.3030(4)
_cell_length_c                   18.5521(9)
_cell_angle_alpha                90
_cell_angle_beta                 109.3440(10)
_cell_angle_gamma                90
_cell_volume                     2865.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9734
_cell_measurement_theta_min      2.4049
_cell_measurement_theta_max      35.1134

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.749
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.295
_exptl_absorpt_coefficient_mu    0.707
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48284
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.329
_diffrn_reflns_theta_max         35.362
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             11633
_reflns_number_gt                10139
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+3.8341P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11633
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0971
_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_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 0.16358(2) 0.22734(2) 0.44712(2) 0.01300(5) Uani 1 1 d . . . . .
V2 V 0.28206(2) 0.35394(2) 0.34473(2) 0.01485(5) Uani 1 1 d . . . . .
O1 O 0.31179(9) 0.25006(8) 0.43026(6) 0.01523(19) Uani 1 1 d . . . . .
O3 O -0.00382(10) 0.25222(9) 0.41112(8) 0.0209(2) Uani 1 1 d . . . . .
O2 O 0.14791(9) 0.35064(8) 0.38015(7) 0.0164(2) Uani 1 1 d . . . . .
O9 O 0.15772(10) 0.10631(8) 0.43248(7) 0.0205(2) Uani 1 1 d . . . . .
O5 O 0.39825(11) 0.26586(9) 0.32538(7) 0.0218(2) Uani 1 1 d . . . . .
O10 O 0.19699(11) 0.24696(10) 0.53810(7) 0.0232(2) Uani 1 1 d . . . . .
O7 O 0.35104(11) 0.45796(9) 0.37436(9) 0.0278(3) Uani 1 1 d . . . . .
O6 O 0.49677(12) 0.12205(11) 0.35216(8) 0.0279(3) Uani 1 1 d . . . . .
O8 O 0.20342(11) 0.36756(11) 0.25527(7) 0.0267(3) Uani 1 1 d . . . . .
O4 O -0.15193(11) 0.34905(10) 0.34522(10) 0.0345(3) Uani 1 1 d . . . . .
C9 C 0.43569(13) 0.18648(12) 0.36658(9) 0.0186(3) Uani 1 1 d . . . . .
C11 C 0.50373(12) 0.19251(11) 0.50803(9) 0.0158(2) Uani 1 1 d . . . . .
C10 C 0.39901(12) 0.17694(11) 0.43766(9) 0.0153(2) Uani 1 1 d . . . . .
H12 H 0.366697 0.108308 0.439200 0.018 Uiso 1 1 calc R U . . .
C2 C -0.04974(13) 0.32709(11) 0.36598(11) 0.0207(3) Uani 1 1 d . . . . .
C3 C 0.02477(12) 0.49761(11) 0.34506(9) 0.0150(2) Uani 1 1 d . . . . .
C1 C 0.03562(12) 0.38589(11) 0.33763(9) 0.0161(2) Uani 1 1 d . . . . .
H6 H 0.019989 0.369454 0.282513 0.019 Uiso 1 1 calc R U . . .
C4 C -0.01443(15) 0.55733(13) 0.27997(10) 0.0228(3) Uani 1 1 d . . . . .
H5 H -0.031531 0.527919 0.230791 0.027 Uiso 1 1 calc R U . . .
C8 C 0.05108(14) 0.54183(12) 0.41680(10) 0.0211(3) Uani 1 1 d . . . . .
H1 H 0.078207 0.501416 0.461418 0.025 Uiso 1 1 calc R U . . .
C12 C 0.56450(14) 0.28303(13) 0.51853(10) 0.0222(3) Uani 1 1 d . . . . .
H11 H 0.537130 0.336230 0.482961 0.027 Uiso 1 1 calc R U . . .
C14 C 0.70454(16) 0.21869(18) 0.63282(11) 0.0321(4) Uani 1 1 d . . . . .
H9 H 0.773064 0.227505 0.675136 0.039 Uiso 1 1 calc R U . . .
C16 C 0.54415(15) 0.11596(13) 0.56134(10) 0.0225(3) Uani 1 1 d . . . . .
H7 H 0.502939 0.054414 0.555412 0.027 Uiso 1 1 calc R U . . .
C13 C 0.66437(15) 0.29601(15) 0.58036(12) 0.0283(4) Uani 1 1 d . . . . .
H10 H 0.705335 0.357738 0.586858 0.034 Uiso 1 1 calc R U . . .
C7 C 0.03790(16) 0.64469(14) 0.42352(13) 0.0293(4) Uani 1 1 d . . . . .
H2 H 0.056563 0.674634 0.472617 0.035 Uiso 1 1 calc R U . . .
C5 C -0.02855(19) 0.66037(14) 0.28709(13) 0.0323(4) Uani 1 1 d . . . . .
H4 H -0.056200 0.700947 0.242593 0.039 Uiso 1 1 calc R U . . .
C6 C -0.00266(18) 0.70380(13) 0.35823(14) 0.0333(4) Uani 1 1 d . . . . .
H3 H -0.012528 0.774089 0.362679 0.040 Uiso 1 1 calc R U . . .
C15 C 0.64489(17) 0.12907(17) 0.62346(11) 0.0316(4) Uani 1 1 d . . . . .
H8 H 0.672429 0.076247 0.659356 0.038 Uiso 1 1 calc R U . . .
N1 N 0.36708(11) 0.04677(11) 0.14907(8) 0.0194(2) Uani 1 1 d . . . . .
C17 C 0.26567(14) 0.08105(14) 0.17011(11) 0.0245(3) Uani 1 1 d . . . . .
H13 H 0.211203 0.025300 0.163699 0.037 Uiso 1 1 calc R U . . .
H14 H 0.227646 0.136979 0.136943 0.037 Uiso 1 1 calc R U . . .
H15 H 0.291744 0.103318 0.223478 0.037 Uiso 1 1 calc R U . . .
C18 C 0.44986(16) 0.13195(16) 0.15985(11) 0.0289(4) Uani 1 1 d . . . . .
H16 H 0.412640 0.187485 0.125951 0.043 Uiso 1 1 calc R U . . .
H17 H 0.517625 0.109548 0.147638 0.043 Uiso 1 1 calc R U . . .
H18 H 0.473697 0.154749 0.213054 0.043 Uiso 1 1 calc R U . . .
C19 C 0.42363(16) -0.03950(15) 0.19930(11) 0.0285(4) Uani 1 1 d . . . . .
H19 H 0.490181 -0.062253 0.185816 0.043 Uiso 1 1 calc R U . . .
H20 H 0.368461 -0.094827 0.192150 0.043 Uiso 1 1 calc R U . . .
H21 H 0.449270 -0.017909 0.252819 0.043 Uiso 1 1 calc R U . . .
C20 C 0.3289(2) 0.01397(18) 0.06764(11) 0.0372(5) Uani 1 1 d . . . . .
H22 H 0.285430 0.068355 0.035065 0.056 Uiso 1 1 calc R U . . .
H23 H 0.279650 -0.045561 0.061284 0.056 Uiso 1 1 calc R U . . .
H24 H 0.396403 -0.002451 0.053056 0.056 Uiso 1 1 calc R U . . .
N2 N 0.21587(11) 0.54071(10) 0.11523(7) 0.0151(2) Uani 1 1 d . . . . .
C21 C 0.30184(13) 0.45805(12) 0.12395(10) 0.0185(3) Uani 1 1 d . . . . .
H25 H 0.281351 0.418623 0.076706 0.028 Uiso 1 1 calc R U . . .
H26 H 0.301706 0.414341 0.166438 0.028 Uiso 1 1 calc R U . . .
H27 H 0.378741 0.487076 0.134401 0.028 Uiso 1 1 calc R U . . .
C22 C 0.09927(13) 0.49551(14) 0.10031(10) 0.0216(3) Uani 1 1 d . . . . .
H28 H 0.041944 0.549204 0.092283 0.032 Uiso 1 1 calc R U . . .
H29 H 0.099324 0.454593 0.144249 0.032 Uiso 1 1 calc R U . . .
H30 H 0.080091 0.453084 0.054612 0.032 Uiso 1 1 calc R U . . .
C23 C 0.21438(16) 0.60638(14) 0.04917(10) 0.0241(3) Uani 1 1 d . . . . .
H31 H 0.191468 0.566402 0.002151 0.036 Uiso 1 1 calc R U . . .
H32 H 0.291434 0.634322 0.058112 0.036 Uiso 1 1 calc R U . . .
H33 H 0.159261 0.661302 0.044108 0.036 Uiso 1 1 calc R U . . .
C24 C 0.24783(15) 0.60156(13) 0.18701(10) 0.0229(3) Uani 1 1 d . . . . .
H34 H 0.323353 0.632673 0.195883 0.034 Uiso 1 1 calc R U . . .
H35 H 0.251132 0.557782 0.230165 0.034 Uiso 1 1 calc R U . . .
H36 H 0.189968 0.654106 0.182008 0.034 Uiso 1 1 calc R U . . .


_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 O10 1.6206(12) . ?
V1 O9 1.6305(12) . ?
V1 O3 1.9714(11) . ?
V1 O1 1.9730(10) . ?
V1 O2 2.0280(11) . ?
V2 O7 1.6213(13) . ?
V2 O8 1.6308(13) . ?
V2 O2 1.9690(11) . ?
V2 O5 1.9711(12) . ?
V2 O1 2.0438(11) . ?
O1 C10 1.4210(17) . ?
O3 C2 1.303(2) . ?
O2 C1 1.4243(17) . ?
O5 C9 1.295(2) . ?
O6 C9 1.2265(19) . ?
O4 C2 1.2222(19) . ?
C9 C10 1.534(2) . ?
C11 C16 1.392(2) . ?
C11 C12 1.397(2) . ?
C11 C10 1.514(2) . ?
C10 H12 1.0000 . ?
C2 C1 1.535(2) . ?
C3 C4 1.391(2) . ?
C3 C8 1.392(2) . ?
C3 C1 1.503(2) . ?
C1 H6 1.0000 . ?
C4 C5 1.393(2) . ?
C4 H5 0.9500 . ?
C8 C7 1.388(2) . ?
C8 H1 0.9500 . ?
C12 C13 1.386(2) . ?
C12 H11 0.9500 . ?
C14 C15 1.381(3) . ?
C14 C13 1.390(3) . ?
C14 H9 0.9500 . ?
C16 C15 1.396(3) . ?
C16 H7 0.9500 . ?
C13 H10 0.9500 . ?
C7 C6 1.391(3) . ?
C7 H2 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H4 0.9500 . ?
C6 H3 0.9500 . ?
C15 H8 0.9500 . ?
N1 C20 1.491(2) . ?
N1 C18 1.492(2) . ?
N1 C19 1.497(2) . ?
N1 C17 1.497(2) . ?
C17 H13 0.9800 . ?
C17 H14 0.9800 . ?
C17 H15 0.9800 . ?
C18 H16 0.9800 . ?
C18 H17 0.9800 . ?
C18 H18 0.9800 . ?
C19 H19 0.9800 . ?
C19 H20 0.9800 . ?
C19 H21 0.9800 . ?
C20 H22 0.9800 . ?
C20 H23 0.9800 . ?
C20 H24 0.9800 . ?
N2 C24 1.495(2) . ?
N2 C22 1.494(2) . ?
N2 C21 1.4969(19) . ?
N2 C23 1.500(2) . ?
C21 H25 0.9800 . ?
C21 H26 0.9800 . ?
C21 H27 0.9800 . ?
C22 H28 0.9800 . ?
C22 H29 0.9800 . ?
C22 H30 0.9800 . ?
C23 H31 0.9800 . ?
C23 H32 0.9800 . ?
C23 H33 0.9800 . ?
C24 H34 0.9800 . ?
C24 H35 0.9800 . ?
C24 H36 0.9800 . ?

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
O10 V1 O9 108.34(7) . . ?
O10 V1 O3 101.65(6) . . ?
O9 V1 O3 97.22(5) . . ?
O10 V1 O1 102.21(6) . . ?
O9 V1 O1 96.72(5) . . ?
O3 V1 O1 146.86(5) . . ?
O10 V1 O2 116.59(6) . . ?
O9 V1 O2 134.96(6) . . ?
O3 V1 O2 77.29(4) . . ?
O1 V1 O2 71.59(4) . . ?
O7 V2 O8 108.52(8) . . ?
O7 V2 O2 107.96(6) . . ?
O8 V2 O2 93.54(6) . . ?
O7 V2 O5 103.85(6) . . ?
O8 V2 O5 95.88(6) . . ?
O2 V2 O5 141.84(5) . . ?
O7 V2 O1 112.02(6) . . ?
O8 V2 O1 139.34(6) . . ?
O2 V2 O1 71.34(4) . . ?
O5 V2 O1 77.61(5) . . ?
C10 O1 V1 126.01(9) . . ?
C10 O1 V2 118.23(9) . . ?
V1 O1 V2 106.83(5) . . ?
C2 O3 V1 121.86(10) . . ?
C1 O2 V2 125.05(9) . . ?
C1 O2 V1 118.91(9) . . ?
V2 O2 V1 107.60(5) . . ?
C9 O5 V2 120.98(10) . . ?
O6 C9 O5 124.39(15) . . ?
O6 C9 C10 120.38(15) . . ?
O5 C9 C10 115.23(13) . . ?
C16 C11 C12 118.88(15) . . ?
C16 C11 C10 120.95(14) . . ?
C12 C11 C10 120.11(14) . . ?
O1 C10 C11 112.91(12) . . ?
O1 C10 C9 106.75(12) . . ?
C11 C10 C9 108.74(12) . . ?
O1 C10 H12 109.5 . . ?
C11 C10 H12 109.5 . . ?
C9 C10 H12 109.5 . . ?
O4 C2 O3 124.53(15) . . ?
O4 C2 C1 121.29(15) . . ?
O3 C2 C1 114.16(13) . . ?
C4 C3 C8 119.51(14) . . ?
C4 C3 C1 120.06(14) . . ?
C8 C3 C1 120.41(14) . . ?
O2 C1 C3 111.97(12) . . ?
O2 C1 C2 106.90(12) . . ?
C3 C1 C2 112.38(12) . . ?
O2 C1 H6 108.5 . . ?
C3 C1 H6 108.5 . . ?
C2 C1 H6 108.5 . . ?
C3 C4 C5 119.85(18) . . ?
C3 C4 H5 120.1 . . ?
C5 C4 H5 120.1 . . ?
C7 C8 C3 120.35(17) . . ?
C7 C8 H1 119.8 . . ?
C3 C8 H1 119.8 . . ?
C13 C12 C11 120.65(16) . . ?
C13 C12 H11 119.7 . . ?
C11 C12 H11 119.7 . . ?
C15 C14 C13 120.02(17) . . ?
C15 C14 H9 120.0 . . ?
C13 C14 H9 120.0 . . ?
C11 C16 C15 120.39(17) . . ?
C11 C16 H7 119.8 . . ?
C15 C16 H7 119.8 . . ?
C12 C13 C14 119.96(18) . . ?
C12 C13 H10 120.0 . . ?
C14 C13 H10 120.0 . . ?
C8 C7 C6 119.87(18) . . ?
C8 C7 H2 120.1 . . ?
C6 C7 H2 120.1 . . ?
C6 C5 C4 120.44(18) . . ?
C6 C5 H4 119.8 . . ?
C4 C5 H4 119.8 . . ?
C5 C6 C7 119.97(17) . . ?
C5 C6 H3 120.0 . . ?
C7 C6 H3 120.0 . . ?
C14 C15 C16 120.09(18) . . ?
C14 C15 H8 120.0 . . ?
C16 C15 H8 120.0 . . ?
C20 N1 C18 109.28(16) . . ?
C20 N1 C19 109.39(15) . . ?
C18 N1 C19 110.06(14) . . ?
C20 N1 C17 110.07(14) . . ?
C18 N1 C17 108.95(14) . . ?
C19 N1 C17 109.09(14) . . ?
N1 C17 H13 109.5 . . ?
N1 C17 H14 109.5 . . ?
H13 C17 H14 109.5 . . ?
N1 C17 H15 109.5 . . ?
H13 C17 H15 109.5 . . ?
H14 C17 H15 109.5 . . ?
N1 C18 H16 109.5 . . ?
N1 C18 H17 109.5 . . ?
H16 C18 H17 109.5 . . ?
N1 C18 H18 109.5 . . ?
H16 C18 H18 109.5 . . ?
H17 C18 H18 109.5 . . ?
N1 C19 H19 109.5 . . ?
N1 C19 H20 109.5 . . ?
H19 C19 H20 109.5 . . ?
N1 C19 H21 109.5 . . ?
H19 C19 H21 109.5 . . ?
H20 C19 H21 109.5 . . ?
N1 C20 H22 109.5 . . ?
N1 C20 H23 109.5 . . ?
H22 C20 H23 109.5 . . ?
N1 C20 H24 109.5 . . ?
H22 C20 H24 109.5 . . ?
H23 C20 H24 109.5 . . ?
C24 N2 C22 109.63(13) . . ?
C24 N2 C21 109.48(12) . . ?
C22 N2 C21 108.97(12) . . ?
C24 N2 C23 109.92(13) . . ?
C22 N2 C23 109.38(12) . . ?
C21 N2 C23 109.45(12) . . ?
N2 C21 H25 109.5 . . ?
N2 C21 H26 109.5 . . ?
H25 C21 H26 109.5 . . ?
N2 C21 H27 109.5 . . ?
H25 C21 H27 109.5 . . ?
H26 C21 H27 109.5 . . ?
N2 C22 H28 109.5 . . ?
N2 C22 H29 109.5 . . ?
H28 C22 H29 109.5 . . ?
N2 C22 H30 109.5 . . ?
H28 C22 H30 109.5 . . ?
H29 C22 H30 109.5 . . ?
N2 C23 H31 109.5 . . ?
N2 C23 H32 109.5 . . ?
H31 C23 H32 109.5 . . ?
N2 C23 H33 109.5 . . ?
H31 C23 H33 109.5 . . ?
H32 C23 H33 109.5 . . ?
N2 C24 H34 109.5 . . ?
N2 C24 H35 109.5 . . ?
H34 C24 H35 109.5 . . ?
N2 C24 H36 109.5 . . ?
H34 C24 H36 109.5 . . ?
H35 C24 H36 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 O5 C9 O6 170.69(13) . . . . ?
V2 O5 C9 C10 -9.73(19) . . . . ?
V1 O1 C10 C11 -107.38(12) . . . . ?
V2 O1 C10 C11 109.81(12) . . . . ?
V1 O1 C10 C9 133.19(11) . . . . ?
V2 O1 C10 C9 -9.62(14) . . . . ?
C16 C11 C10 O1 124.73(15) . . . . ?
C12 C11 C10 O1 -58.21(18) . . . . ?
C16 C11 C10 C9 -117.00(15) . . . . ?
C12 C11 C10 C9 60.06(17) . . . . ?
O6 C9 C10 O1 -168.44(15) . . . . ?
O5 C9 C10 O1 11.96(18) . . . . ?
O6 C9 C10 C11 69.46(19) . . . . ?
O5 C9 C10 C11 -110.14(15) . . . . ?
V1 O3 C2 O4 -175.97(15) . . . . ?
V1 O3 C2 C1 5.9(2) . . . . ?
V2 O2 C1 C3 -82.70(15) . . . . ?
V1 O2 C1 C3 133.25(11) . . . . ?
V2 O2 C1 C2 153.82(10) . . . . ?
V1 O2 C1 C2 9.77(15) . . . . ?
C4 C3 C1 O2 126.28(15) . . . . ?
C8 C3 C1 O2 -55.27(18) . . . . ?
C4 C3 C1 C2 -113.38(16) . . . . ?
C8 C3 C1 C2 65.07(18) . . . . ?
O4 C2 C1 O2 172.20(17) . . . . ?
O3 C2 C1 O2 -9.63(19) . . . . ?
O4 C2 C1 C3 49.0(2) . . . . ?
O3 C2 C1 C3 -132.85(15) . . . . ?
C8 C3 C4 C5 -0.9(2) . . . . ?
C1 C3 C4 C5 177.55(16) . . . . ?
C4 C3 C8 C7 0.3(2) . . . . ?
C1 C3 C8 C7 -178.17(15) . . . . ?
C16 C11 C12 C13 1.0(2) . . . . ?
C10 C11 C12 C13 -176.16(15) . . . . ?
C12 C11 C16 C15 -1.1(2) . . . . ?
C10 C11 C16 C15 175.98(16) . . . . ?
C11 C12 C13 C14 -0.3(3) . . . . ?
C15 C14 C13 C12 -0.1(3) . . . . ?
C3 C8 C7 C6 0.5(3) . . . . ?
C3 C4 C5 C6 0.8(3) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C8 C7 C6 C5 -0.7(3) . . . . ?
C13 C14 C15 C16 0.0(3) . . . . ?
C11 C16 C15 C14 0.7(3) . . . . ?

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
_geom_hbond_publ_flag
C10 H12 O9 1.00 2.53 3.0850(18) 115 . yes
C17 H13 O4 0.98 2.44 3.362(2) 156 2_545 yes
C17 H14 O10 0.98 2.33 3.252(2) 156 4_565 yes
C18 H18 O6 0.98 2.54 3.423(2) 150 . yes
C19 H19 O7 0.98 2.57 3.473(2) 154 2_645 yes
C19 H21 O6 0.98 2.55 3.432(2) 150 . yes
C21 H25 O10 0.98 2.44 3.206(2) 135 4_565 yes
C21 H26 O8 0.98 2.43 3.287(2) 146 . yes
C21 H27 O6 0.98 2.32 3.220(2) 152 2_655 yes
C22 H28 O9 0.98 2.46 3.357(2) 151 2 yes
C22 H29 O8 0.98 2.34 3.219(2) 149 . yes
C23 H31 O9 0.98 2.60 3.490(2) 151 4_565 yes
C23 H32 O6 0.98 2.59 3.423(2) 143 2_655 yes

_refine_diff_density_max         0.802
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_m119_sq
_database_code_depnum_ccdc_archive 'CCDC 1911696'
loop_
_audit_author_name
_audit_author_address
'Robert Gyepes'
;Department of Inorganic Chemistry, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H36 N3 O8 V3'
_chemical_formula_sum            'C20 H36 N3 O8 V3'
_chemical_formula_weight         599.34

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      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, z'

_cell_length_a                   11.6214(4)
_cell_length_b                   13.4677(5)
_cell_length_c                   25.1952(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3943.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    193
_cell_measurement_theta_min      4.2361
_cell_measurement_theta_max      24.9185

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.202
_exptl_absorpt_coefficient_mu    0.727
_shelx_estimated_absorpt_T_min   0.772
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            97181
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.315
_diffrn_reflns_theta_max         29.050
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5373
_reflns_number_gt                4261
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²+4.1248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5373
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.17486(3) 0.50620(3) 0.250000 0.01519(10) Uani 1 2 d S T P . .
V2 V 0.39907(3) 0.51033(3) 0.17872(2) 0.02249(9) Uani 1 1 d . . . . .
O1 O 0.34425(15) 0.51386(15) 0.250000 0.0225(4) Uani 1 2 d S T P . .
O2 O 0.22612(11) 0.49773(9) 0.17588(5) 0.0201(3) Uani 1 1 d . . . . .
O3 O 0.36860(12) 0.46985(14) 0.10460(6) 0.0364(4) Uani 1 1 d . . . . .
O4 O 0.24286(14) 0.42002(14) 0.04368(6) 0.0418(4) Uani 1 1 d . . . . .
O5 O 0.50725(14) 0.43641(16) 0.18653(6) 0.0482(5) Uani 1 1 d . . . . .
O6 O 0.44575(18) 0.62416(14) 0.17005(7) 0.0530(5) Uani 1 1 d . . . . .
O7 O 0.08234(15) 0.41406(14) 0.250000 0.0229(4) Uani 1 2 d S T P . .
O8 O 0.10281(16) 0.60932(14) 0.250000 0.0254(4) Uani 1 2 d S T P . .
C1 C 0.17008(15) 0.47775(14) 0.12752(7) 0.0223(4) Uani 1 1 d . . . . .
H1 H 0.119255 0.418451 0.132107 0.027 Uiso 1 1 calc R U . . .
C2 C 0.26553(17) 0.45255(16) 0.08748(8) 0.0275(4) Uani 1 1 d . . . . .
C3 C 0.09860(15) 0.56375(15) 0.10797(7) 0.0227(4) Uani 1 1 d . . . . .
C4 C 0.01164(17) 0.54750(18) 0.07074(7) 0.0295(4) Uani 1 1 d . . . . .
H4 H -0.002128 0.482218 0.057951 0.035 Uiso 1 1 calc R U . . .
C5 C -0.05474(19) 0.6256(2) 0.05227(8) 0.0373(5) Uani 1 1 d . . . . .
H5 H -0.113419 0.613689 0.026807 0.045 Uiso 1 1 calc R U . . .
C6 C -0.0358(2) 0.72090(19) 0.07082(8) 0.0392(5) Uani 1 1 d . . . . .
H6 H -0.081758 0.774377 0.058350 0.047 Uiso 1 1 calc R U . . .
C7 C 0.0502(2) 0.73796(18) 0.10755(9) 0.0373(5) Uani 1 1 d . . . . .
H7 H 0.063142 0.803385 0.120319 0.045 Uiso 1 1 calc R U . . .
C8 C 0.11805(18) 0.66007(16) 0.12601(8) 0.0300(4) Uani 1 1 d . . . . .
H8 H 0.177660 0.672626 0.150922 0.036 Uiso 1 1 calc R U . . .


_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 O8 1.6217(19) . ?
V1 O7 1.6419(18) . ?
V1 O2 1.9634(12) . ?
V1 O2 1.9635(12) 6_556 ?
V1 O1 1.9712(18) . ?
V2 O5 1.6157(17) . ?
V2 O6 1.6407(18) . ?
V2 O1 1.9061(7) . ?
V2 O3 1.9775(15) . ?
V2 O2 2.0183(13) . ?
O2 C1 1.408(2) . ?
O3 C2 1.294(2) . ?
O4 C2 1.216(2) . ?
C1 C3 1.508(3) . ?
C1 C2 1.537(3) . ?
C1 H1 1.0000 . ?
C3 C8 1.393(3) . ?
C3 C4 1.396(2) . ?
C4 C5 1.385(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?

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
O8 V1 O7 108.00(10) . . ?
O8 V1 O2 101.91(4) . . ?
O7 V1 O2 98.91(4) . . ?
O8 V1 O2 101.91(4) . 6_556 ?
O7 V1 O2 98.91(4) . 6_556 ?
O2 V1 O2 144.01(8) . 6_556 ?
O8 V1 O1 118.09(9) . . ?
O7 V1 O1 133.91(9) . . ?
O2 V1 O1 72.55(4) . . ?
O2 V1 O1 72.55(4) 6_556 . ?
O5 V2 O6 109.55(11) . . ?
O5 V2 O1 99.25(8) . . ?
O6 V2 O1 102.28(9) . . ?
O5 V2 O3 94.84(8) . . ?
O6 V2 O3 101.01(8) . . ?
O1 V2 O3 146.81(7) . . ?
O5 V2 O2 136.67(9) . . ?
O6 V2 O2 113.77(9) . . ?
O1 V2 O2 72.70(6) . . ?
O3 V2 O2 76.41(5) . . ?
V2 O1 V2 140.83(10) 6_556 . ?
V2 O1 V1 109.42(5) 6_556 . ?
V2 O1 V1 109.42(5) . . ?
C1 O2 V1 133.95(11) . . ?
C1 O2 V2 120.50(11) . . ?
V1 O2 V2 105.28(6) . . ?
C2 O3 V2 122.00(13) . . ?
O2 C1 C3 113.00(15) . . ?
O2 C1 C2 106.04(14) . . ?
C3 C1 C2 110.66(16) . . ?
O2 C1 H1 109.0 . . ?
C3 C1 H1 109.0 . . ?
C2 C1 H1 109.0 . . ?
O4 C2 O3 124.58(19) . . ?
O4 C2 C1 121.24(18) . . ?
O3 C2 C1 114.18(16) . . ?
C8 C3 C4 118.86(19) . . ?
C8 C3 C1 121.29(16) . . ?
C4 C3 C1 119.85(18) . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C6 C5 C4 120.2(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C7 C6 C5 119.7(2) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C8 120.6(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C3 120.05(19) . . ?
C7 C8 H8 120.0 . . ?
C3 C8 H8 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O2 C1 C3 74.9(2) . . . . ?
V2 O2 C1 C3 -112.02(14) . . . . ?
V1 O2 C1 C2 -163.68(13) . . . . ?
V2 O2 C1 C2 9.38(19) . . . . ?
V2 O3 C2 O4 -173.91(18) . . . . ?
V2 O3 C2 C1 6.7(3) . . . . ?
O2 C1 C2 O4 170.8(2) . . . . ?
C3 C1 C2 O4 -66.3(3) . . . . ?
O2 C1 C2 O3 -9.7(2) . . . . ?
C3 C1 C2 O3 113.2(2) . . . . ?
O2 C1 C3 C8 20.2(2) . . . . ?
C2 C1 C3 C8 -98.6(2) . . . . ?
O2 C1 C3 C4 -160.39(16) . . . . ?
C2 C1 C3 C4 80.9(2) . . . . ?
C8 C3 C4 C5 -0.4(3) . . . . ?
C1 C3 C4 C5 -179.89(18) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C7 0.5(3) . . . . ?
C5 C6 C7 C8 0.1(4) . . . . ?
C6 C7 C8 C3 -0.8(3) . . . . ?
C4 C3 C8 C7 1.0(3) . . . . ?
C1 C3 C8 C7 -179.56(19) . . . . ?

_refine_diff_density_max         0.679
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.071



####################################################################### 
# 
# 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_fz_s35_sq
_database_code_depnum_ccdc_archive 'CCDC 1911694'
loop_
_audit_author_name
_audit_author_address
'Robert Gyepes'
;Department of Inorganic Chemistry, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 O10 V2, 2(C8 H20 N) [+ solvent]'
_chemical_formula_sum            'C16 H26 N O5.50 V'
_chemical_formula_weight         371.32

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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   7.4443(4)
_cell_length_b                   18.6609(12)
_cell_length_c                   13.3061(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.543(2)
_cell_angle_gamma                90
_cell_volume                     1839.80(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9942
_cell_measurement_theta_min      2.6703
_cell_measurement_theta_max      28.2661

_exptl_crystal_description       fragment
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.565
_shelx_estimated_absorpt_T_min   0.752
_shelx_estimated_absorpt_T_max   0.895
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54352
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.670
_diffrn_reflns_theta_max         34.832
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14165
_reflns_number_gt                11081
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.861
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0990P)²+1.6956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         14165
_refine_ls_number_parameters     424
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1760
_refine_ls_wR_factor_gt          0.1565
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.50885(8) 0.30779(3) 0.28670(5) 0.01451(13) Uani 1 1 d . . . . .
V2 V 0.44190(8) 0.47886(3) 0.30718(5) 0.01530(14) Uani 1 1 d . . . . .
O1 O 0.4446(4) 0.25835(16) 0.3782(2) 0.0204(6) Uani 1 1 d . . . . .
O2 O 0.5670(5) 0.53585(18) 0.2538(3) 0.0275(7) Uani 1 1 d . . . . .
O3 O 0.7019(4) 0.27834(17) 0.2582(3) 0.0231(6) Uani 1 1 d . . . . .
O4 O 0.2325(5) 0.5043(2) 0.2862(3) 0.0306(8) Uani 1 1 d . . . . .
O5 O 0.5692(4) 0.39224(15) 0.3736(2) 0.0136(5) Uani 1 1 d . . . . .
O6 O 0.4782(4) 0.50753(15) 0.4498(2) 0.0193(6) Uani 1 1 d . . . . .
O7 O 0.5546(4) 0.47601(19) 0.6099(2) 0.0244(6) Uani 1 1 d . . . . .
O8 O 0.4234(5) 0.39860(17) 0.2124(2) 0.0240(7) Uani 1 1 d . . . . .
O9 O 0.3378(5) 0.27145(19) 0.1777(3) 0.0287(7) Uani 1 1 d . . . . .
O10 O 0.1513(6) 0.2950(2) 0.0376(3) 0.0411(10) Uani 1 1 d . . . . .
C1 C 0.3225(8) 0.3927(3) 0.1171(4) 0.0320(12) Uani 1 1 d . . . . .
H1 H 0.214822 0.424916 0.114686 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2600(7) 0.3139(3) 0.1070(4) 0.0322(10) Uani 1 1 d . . . . .
C3 C 0.4357(11) 0.4112(3) 0.0297(4) 0.0404(15) Uani 1 1 d . . . . .
C4 C 0.6153(12) 0.4146(3) 0.0437(5) 0.0502(18) Uani 1 1 d . . . . .
H4 H 0.673213 0.408683 0.109930 0.060 Uiso 1 1 calc R U . . .
C5 C 0.7240(15) 0.4269(5) -0.0380(6) 0.069(3) Uani 1 1 d . . . . .
H5 H 0.852020 0.427600 -0.027622 0.083 Uiso 1 1 calc R U . . .
C6 C 0.6329(18) 0.4379(4) -0.1333(6) 0.077(3) Uani 1 1 d . . . . .
H6 H 0.700208 0.447563 -0.188851 0.092 Uiso 1 1 calc R U . . .
C7 C 0.4502(19) 0.4350(4) -0.1483(5) 0.077(3) Uani 1 1 d . . . . .
H7 H 0.391613 0.441633 -0.214307 0.093 Uiso 1 1 calc R U . . .
C8 C 0.3474(14) 0.4223(4) -0.0675(4) 0.059(2) Uani 1 1 d . . . . .
H8 H 0.219381 0.421204 -0.078038 0.071 Uiso 1 1 calc R U . . .
C9 C 0.6074(5) 0.39186(19) 0.4798(3) 0.0122(6) Uani 1 1 d . . . . .
H9 H 0.536599 0.352422 0.508142 0.015 Uiso 1 1 calc R U . . .
C10 C 0.5433(5) 0.46347(19) 0.5197(3) 0.0151(7) Uani 1 1 d . . . . .
C11 C 0.8052(5) 0.38077(19) 0.5142(3) 0.0136(6) Uani 1 1 d . . . . .
C12 C 0.9369(5) 0.3841(2) 0.4468(3) 0.0184(7) Uani 1 1 d . . . . .
H12 H 0.903502 0.392789 0.377127 0.022 Uiso 1 1 calc R U . . .
C13 C 1.1193(6) 0.3744(3) 0.4822(4) 0.0237(8) Uani 1 1 d . . . . .
H13 H 1.209293 0.376412 0.436281 0.028 Uiso 1 1 calc R U . . .
C14 C 1.1681(6) 0.3621(3) 0.5835(4) 0.0256(9) Uani 1 1 d . . . . .
H14 H 1.291636 0.355987 0.607094 0.031 Uiso 1 1 calc R U . . .
C15 C 1.0366(6) 0.3587(3) 0.6511(3) 0.0239(8) Uani 1 1 d . . . . .
H15 H 1.070516 0.350455 0.720813 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8560(5) 0.3675(2) 0.6163(3) 0.0186(7) Uani 1 1 d . . . . .
H16 H 0.766262 0.364392 0.662318 0.022 Uiso 1 1 calc R U . . .
N1 N 0.9621(5) 0.13493(19) 0.4408(3) 0.0215(7) Uani 1 1 d . . . . .
C17 C 1.0617(5) 0.1702(2) 0.3590(4) 0.0217(8) Uani 1 1 d . . . . .
H17A H 0.972069 0.194315 0.310558 0.026 Uiso 1 1 calc R U . . .
H17B H 1.142679 0.207589 0.390726 0.026 Uiso 1 1 calc R U . . .
C18 C 1.1727(7) 0.1195(3) 0.3008(5) 0.0370(12) Uani 1 1 d . . . . .
H18A H 1.278292 0.103296 0.344696 0.055 Uiso 1 1 calc R U . . .
H18B H 1.212714 0.144373 0.242092 0.055 Uiso 1 1 calc R U . . .
H18C H 1.098988 0.077963 0.278140 0.055 Uiso 1 1 calc R U . . .
C19 C 0.8580(6) 0.1948(2) 0.4862(3) 0.0193(7) Uani 1 1 d . . . . .
H19A H 0.944898 0.231431 0.514414 0.023 Uiso 1 1 calc R U . . .
H19B H 0.778417 0.217772 0.431590 0.023 Uiso 1 1 calc R U . . .
C20 C 0.7441(8) 0.1713(3) 0.5682(4) 0.0334(11) Uani 1 1 d . . . . .
H20A H 0.650632 0.138031 0.539924 0.050 Uiso 1 1 calc R U . . .
H20B H 0.687088 0.213258 0.595954 0.050 Uiso 1 1 calc R U . . .
H20C H 0.820756 0.147257 0.622078 0.050 Uiso 1 1 calc R U . . .
C21 C 0.8371(6) 0.0763(2) 0.3973(4) 0.0262(9) Uani 1 1 d . . . . .
H21A H 0.775406 0.054716 0.452632 0.031 Uiso 1 1 calc R U . . .
H21B H 0.910378 0.038280 0.369116 0.031 Uiso 1 1 calc R U . . .
C22 C 0.6946(7) 0.1018(3) 0.3148(4) 0.0314(10) Uani 1 1 d . . . . .
H22A H 0.627311 0.141988 0.340261 0.047 Uiso 1 1 calc R U . . .
H22B H 0.611287 0.062424 0.295408 0.047 Uiso 1 1 calc R U . . .
H22C H 0.753712 0.117398 0.255869 0.047 Uiso 1 1 calc R U . . .
C23 C 1.0946(7) 0.1006(3) 0.5191(4) 0.0311(10) Uani 1 1 d . . . . .
H23A H 1.161299 0.062910 0.485876 0.037 Uiso 1 1 calc R U . . .
H23B H 1.026033 0.076881 0.569889 0.037 Uiso 1 1 calc R U . . .
C24 C 1.2296(7) 0.1510(3) 0.5732(4) 0.0363(12) Uani 1 1 d . . . . .
H24A H 1.293641 0.177057 0.523675 0.054 Uiso 1 1 calc R U . . .
H24B H 1.316341 0.123443 0.617916 0.054 Uiso 1 1 calc R U . . .
H24C H 1.166459 0.185140 0.613347 0.054 Uiso 1 1 calc R U . . .
N2 N 0.3531(5) 0.68113(19) 0.0614(3) 0.0179(6) Uani 1 1 d . . . . .
C25 C 0.2293(10) 0.6613(4) 0.1394(5) 0.0483(16) Uani 1 1 d . . . . .
H25A H 0.301220 0.643496 0.200760 0.058 Uiso 1 1 calc R U . . .
H25B H 0.147700 0.622278 0.113012 0.058 Uiso 1 1 calc R U . . .
C26 C 0.1143(10) 0.7277(7) 0.1672(7) 0.083(4) Uani 1 1 d . . . . .
H26A H 0.044097 0.745620 0.106212 0.124 Uiso 1 1 calc R U . . .
H26B H 0.194855 0.765562 0.195817 0.124 Uiso 1 1 calc R U . . .
H26C H 0.032046 0.713364 0.216798 0.124 Uiso 1 1 calc R U . . .
C27 C 0.4570(9) 0.6134(3) 0.0371(5) 0.0420(13) Uani 1 1 d . . . . .
H27A H 0.521864 0.595631 0.100671 0.050 Uiso 1 1 calc R U . . .
H27B H 0.368095 0.576269 0.013038 0.050 Uiso 1 1 calc R U . . .
C28 C 0.5869(8) 0.6204(3) -0.0373(5) 0.0413(13) Uani 1 1 d . . . . .
H28A H 0.522541 0.625709 -0.104728 0.062 Uiso 1 1 calc R U . . .
H28B H 0.663171 0.577549 -0.035722 0.062 Uiso 1 1 calc R U . . .
H28C H 0.662502 0.662718 -0.021687 0.062 Uiso 1 1 calc R U . . .
C29 C 0.2384(10) 0.7075(4) -0.0356(5) 0.0496(16) Uani 1 1 d . . . . .
H29A H 0.178525 0.753180 -0.020821 0.060 Uiso 1 1 calc R U . . .
H29B H 0.319115 0.716834 -0.089051 0.060 Uiso 1 1 calc R U . . .
C30 C 0.0949(13) 0.6526(9) -0.0740(10) 0.111(5) Uani 1 1 d . U . . .
H30A H 0.139861 0.604093 -0.058159 0.167 Uiso 1 1 calc R U . . .
H30B H 0.068679 0.657577 -0.147257 0.167 Uiso 1 1 calc R U . . .
H30C H -0.015528 0.660835 -0.041148 0.167 Uiso 1 1 calc R U . . .
C31 C 0.4758(10) 0.7411(4) 0.0929(6) 0.0511(16) Uani 1 1 d . . . . .
H31A H 0.551204 0.750756 0.037097 0.061 Uiso 1 1 calc R U . . .
H31B H 0.400791 0.784216 0.100447 0.061 Uiso 1 1 calc R U . . .
C32 C 0.5963(11) 0.7332(6) 0.1853(7) 0.073(3) Uani 1 1 d . . . . .
H32A H 0.525219 0.732673 0.243575 0.109 Uiso 1 1 calc R U . . .
H32B H 0.681107 0.773486 0.191555 0.109 Uiso 1 1 calc R U . . .
H32C H 0.663460 0.688191 0.182873 0.109 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.617(3) . ?
V1 O1 1.636(3) . ?
V1 O9 1.957(3) . ?
V1 O5 1.980(3) . ?
V1 O8 2.033(3) . ?
V2 O2 1.622(3) . ?
V2 O4 1.628(3) . ?
V2 O8 1.954(3) . ?
V2 O6 1.965(3) . ?
V2 O5 2.032(3) . ?
O5 C9 1.414(4) . ?
O6 C10 1.300(5) . ?
O7 C10 1.217(5) . ?
O8 C1 1.415(5) . ?
O9 C2 1.320(7) . ?
O10 C2 1.220(6) . ?
C1 C3 1.540(10) . ?
C1 C2 1.544(8) . ?
C1 H1 1.0000 . ?
C3 C4 1.333(11) . ?
C3 C8 1.408(8) . ?
C4 C5 1.435(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.356(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(13) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C11 1.513(5) . ?
C9 C10 1.531(5) . ?
C9 H9 1.0000 . ?
C11 C12 1.393(6) . ?
C11 C16 1.397(5) . ?
C12 C13 1.405(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N1 C23 1.506(6) . ?
N1 C21 1.515(6) . ?
N1 C19 1.518(5) . ?
N1 C17 1.524(5) . ?
C17 C18 1.517(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.510(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.527(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.507(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N2 C31 1.480(8) . ?
N2 C25 1.499(7) . ?
N2 C27 1.532(7) . ?
N2 C29 1.557(7) . ?
C25 C26 1.571(12) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.455(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.533(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.457(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 V1 O1 108.26(16) . . ?
O3 V1 O9 103.75(16) . . ?
O1 V1 O9 98.07(16) . . ?
O3 V1 O5 104.52(15) . . ?
O1 V1 O5 94.61(14) . . ?
O9 V1 O5 143.45(14) . . ?
O3 V1 O8 114.37(16) . . ?
O1 V1 O8 137.05(16) . . ?
O9 V1 O8 77.16(14) . . ?
O5 V1 O8 70.31(11) . . ?
O2 V2 O4 108.33(19) . . ?
O2 V2 O8 103.16(18) . . ?
O4 V2 O8 96.08(17) . . ?
O2 V2 O6 102.31(16) . . ?
O4 V2 O6 97.28(16) . . ?
O8 V2 O6 145.73(13) . . ?
O2 V2 O5 116.65(16) . . ?
O4 V2 O5 134.85(17) . . ?
O8 V2 O5 70.84(12) . . ?
O6 V2 O5 77.40(12) . . ?
C9 O5 V1 126.3(2) . . ?
C9 O5 V2 118.6(2) . . ?
V1 O5 V2 108.01(12) . . ?
C10 O6 V2 121.7(2) . . ?
C1 O8 V2 129.5(3) . . ?
C1 O8 V1 119.0(3) . . ?
V2 O8 V1 109.03(14) . . ?
C2 O9 V1 122.0(3) . . ?
O8 C1 C3 112.2(5) . . ?
O8 C1 C2 106.3(4) . . ?
C3 C1 C2 109.3(4) . . ?
O8 C1 H1 109.6 . . ?
C3 C1 H1 109.6 . . ?
C2 C1 H1 109.6 . . ?
O10 C2 O9 125.3(5) . . ?
O10 C2 C1 120.9(5) . . ?
O9 C2 C1 113.7(4) . . ?
C4 C3 C8 119.6(7) . . ?
C4 C3 C1 121.3(5) . . ?
C8 C3 C1 119.0(7) . . ?
C3 C4 C5 122.2(7) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C6 C5 C4 116.9(10) . . ?
C6 C5 H5 121.6 . . ?
C4 C5 H5 121.6 . . ?
C7 C6 C5 121.4(7) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 120.5(7) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C3 119.3(9) . . ?
C7 C8 H8 120.4 . . ?
C3 C8 H8 120.4 . . ?
O5 C9 C11 113.5(3) . . ?
O5 C9 C10 107.6(3) . . ?
C11 C9 C10 109.9(3) . . ?
O5 C9 H9 108.6 . . ?
C11 C9 H9 108.6 . . ?
C10 C9 H9 108.6 . . ?
O7 C10 O6 124.7(4) . . ?
O7 C10 C9 121.0(3) . . ?
O6 C10 C9 114.3(3) . . ?
C12 C11 C16 119.6(3) . . ?
C12 C11 C9 121.6(3) . . ?
C16 C11 C9 118.8(3) . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 120.2(4) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.2(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 119.8(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C11 120.5(4) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C23 N1 C21 107.1(4) . . ?
C23 N1 C19 111.3(4) . . ?
C21 N1 C19 111.4(3) . . ?
C23 N1 C17 110.3(3) . . ?
C21 N1 C17 111.2(4) . . ?
C19 N1 C17 105.6(3) . . ?
C18 C17 N1 114.9(4) . . ?
C18 C17 H17A 108.5 . . ?
N1 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
N1 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N1 114.7(3) . . ?
C20 C19 H19A 108.6 . . ?
N1 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
N1 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 C22 114.1(4) . . ?
N1 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
N1 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 C24 115.3(4) . . ?
N1 C23 H23A 108.4 . . ?
C24 C23 H23A 108.4 . . ?
N1 C23 H23B 108.4 . . ?
C24 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C31 N2 C25 113.3(5) . . ?
C31 N2 C27 111.9(5) . . ?
C25 N2 C27 107.4(4) . . ?
C31 N2 C29 105.7(5) . . ?
C25 N2 C29 109.1(5) . . ?
C27 N2 C29 109.5(4) . . ?
N2 C25 C26 110.7(7) . . ?
N2 C25 H25A 109.5 . . ?
C26 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 N2 116.9(5) . . ?
C28 C27 H27A 108.1 . . ?
N2 C27 H27A 108.1 . . ?
C28 C27 H27B 108.1 . . ?
N2 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N2 111.9(8) . . ?
C30 C29 H29A 109.2 . . ?
N2 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
N2 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 N2 118.4(7) . . ?
C32 C31 H31A 107.7 . . ?
N2 C31 H31A 107.7 . . ?
C32 C31 H31B 107.7 . . ?
N2 C31 H31B 107.7 . . ?
H31A C31 H31B 107.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 O8 C1 C3 95.2(5) . . . . ?
V1 O8 C1 C3 -104.5(4) . . . . ?
V2 O8 C1 C2 -145.3(4) . . . . ?
V1 O8 C1 C2 14.9(6) . . . . ?
V1 O9 C2 O10 -179.3(4) . . . . ?
V1 O9 C2 C1 2.2(6) . . . . ?
O8 C1 C2 O10 170.8(5) . . . . ?
C3 C1 C2 O10 -67.9(7) . . . . ?
O8 C1 C2 O9 -10.6(7) . . . . ?
C3 C1 C2 O9 110.7(5) . . . . ?
O8 C1 C3 C4 15.2(7) . . . . ?
C2 C1 C3 C4 -102.5(6) . . . . ?
O8 C1 C3 C8 -167.1(5) . . . . ?
C2 C1 C3 C8 75.2(6) . . . . ?
C8 C3 C4 C5 -2.1(9) . . . . ?
C1 C3 C4 C5 175.6(6) . . . . ?
C3 C4 C5 C6 2.2(11) . . . . ?
C4 C5 C6 C7 -1.8(12) . . . . ?
C5 C6 C7 C8 1.3(12) . . . . ?
C6 C7 C8 C3 -1.2(11) . . . . ?
C4 C3 C8 C7 1.6(9) . . . . ?
C1 C3 C8 C7 -176.3(6) . . . . ?
V1 O5 C9 C11 89.3(4) . . . . ?
V2 O5 C9 C11 -123.9(3) . . . . ?
V1 O5 C9 C10 -148.8(2) . . . . ?
V2 O5 C9 C10 -2.0(4) . . . . ?
V2 O6 C10 O7 -173.5(3) . . . . ?
V2 O6 C10 C9 6.5(4) . . . . ?
O5 C9 C10 O7 177.3(3) . . . . ?
C11 C9 C10 O7 -58.6(5) . . . . ?
O5 C9 C10 O6 -2.6(4) . . . . ?
C11 C9 C10 O6 121.5(4) . . . . ?
O5 C9 C11 C12 11.0(5) . . . . ?
C10 C9 C11 C12 -109.6(4) . . . . ?
O5 C9 C11 C16 -169.5(3) . . . . ?
C10 C9 C11 C16 69.9(4) . . . . ?
C16 C11 C12 C13 -0.4(6) . . . . ?
C9 C11 C12 C13 179.1(4) . . . . ?
C11 C12 C13 C14 -0.3(7) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 0.3(8) . . . . ?
C14 C15 C16 C11 -1.0(7) . . . . ?
C12 C11 C16 C15 1.1(6) . . . . ?
C9 C11 C16 C15 -178.5(4) . . . . ?
C23 N1 C17 C18 61.1(5) . . . . ?
C21 N1 C17 C18 -57.6(5) . . . . ?
C19 N1 C17 C18 -178.6(4) . . . . ?
C23 N1 C19 C20 -61.9(5) . . . . ?
C21 N1 C19 C20 57.6(5) . . . . ?
C17 N1 C19 C20 178.5(4) . . . . ?
C23 N1 C21 C22 -179.2(4) . . . . ?
C19 N1 C21 C22 59.0(5) . . . . ?
C17 N1 C21 C22 -58.6(5) . . . . ?
C21 N1 C23 C24 -178.8(4) . . . . ?
C19 N1 C23 C24 -56.8(5) . . . . ?
C17 N1 C23 C24 60.0(6) . . . . ?
C31 N2 C25 C26 57.0(7) . . . . ?
C27 N2 C25 C26 -178.9(5) . . . . ?
C29 N2 C25 C26 -60.3(7) . . . . ?
C31 N2 C27 C28 -54.9(7) . . . . ?
C25 N2 C27 C28 -179.8(5) . . . . ?
C29 N2 C27 C28 61.9(7) . . . . ?
C31 N2 C29 C30 -176.3(7) . . . . ?
C25 N2 C29 C30 -54.3(8) . . . . ?
C27 N2 C29 C30 63.0(7) . . . . ?
C25 N2 C31 C32 58.1(8) . . . . ?
C27 N2 C31 C32 -63.5(8) . . . . ?
C29 N2 C31 C32 177.5(7) . . . . ?

_refine_diff_density_max         2.067
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.115



