# 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 2023

####################################################################### 
# 
# 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_fs31_3_a
_database_code_depnum_ccdc_archive 'CCDC 2206036'
loop_
_audit_author_name
_audit_author_address
'Anna Kozakiewicz-Piekarz'
;Faculty of Chemistry, Nicolaus Copernicus University in Torun
Poland
;
_audit_update_record             
;
2023-02-13 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C29 H25 N5 O8 V2, 2(C H4O), H0.64 O0.32, 2(H4 N)'
_chemical_formula_sum            'C31 H41.64 N7 O10.32 V2'
_chemical_formula_weight         779.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 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+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   39.6854(8)
_cell_length_b                   12.6155(2)
_cell_length_c                   7.4106(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3710.13(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6595
_cell_measurement_theta_min      4.4680
_cell_measurement_theta_max      75.5350

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             1621
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.761
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            13121
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.227
_diffrn_reflns_theta_max         77.915
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             3635
_reflns_number_gt                3330
_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       'Oxford Diffraction CrysAlis'
_computing_cell_refinement       'Oxford Diffraction CrysAlis'
_computing_data_reduction        'Oxford Diffraction CrysAlis'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Diamond software'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_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)+(0.0555P)²+14.6306P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3635
_refine_ls_number_parameters     246
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.1822
_refine_ls_wR_factor_gt          0.1805
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_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 0.40048(2) 0.77544(5) 0.72666(10) 0.0227(2) Uani 1 1 d . . . . .
C1 C 0.29546(12) 0.9091(4) 0.7864(7) 0.0405(11) Uani 1 1 d . . . . .
H1A H 0.316500 0.935751 0.827272 0.049 Uiso 1 1 calc R U . . .
C2 C 0.26615(12) 0.9687(4) 0.8139(7) 0.0413(12) Uani 1 1 d . . . . .
H2A H 0.267182 1.034035 0.877390 0.050 Uiso 1 1 calc R U . . .
C3 C 0.23578(12) 0.9321(4) 0.7483(7) 0.0376(11) Uani 1 1 d . . . . .
H3A H 0.215888 0.972916 0.764607 0.045 Uiso 1 1 calc R U . . .
C4 C 0.23431(12) 0.8365(4) 0.6591(8) 0.0447(13) Uani 1 1 d . . . . .
H4A H 0.213355 0.811647 0.613947 0.054 Uiso 1 1 calc R U . . .
C5 C 0.26327(11) 0.7760(4) 0.6346(8) 0.0390(11) Uani 1 1 d . . . . .
H5A H 0.262066 0.710178 0.572801 0.047 Uiso 1 1 calc R U . . .
C6 C 0.29419(11) 0.8125(4) 0.7012(6) 0.0308(9) Uani 1 1 d . . . . .
C7 C 0.32603(10) 0.7493(3) 0.6807(6) 0.0278(9) Uani 1 1 d . . . . .
O8 O 0.35279(7) 0.7962(3) 0.7444(5) 0.0423(9) Uani 1 1 d . . . . .
C9 C 0.32661(10) 0.6499(4) 0.6126(6) 0.0291(9) Uani 1 1 d . . . . .
H9A H 0.306365 0.622864 0.561955 0.035 Uiso 1 1 calc R U . . .
C10 C 0.35533(10) 0.5833(3) 0.6115(6) 0.0235(8) Uani 1 1 d . . . . .
N11 N 0.38522(8) 0.6203(3) 0.6596(5) 0.0228(7) Uani 1 1 d . . . . .
N12 N 0.41042(8) 0.5421(3) 0.6665(5) 0.0247(7) Uani 1 1 d . . . . .
C13 C 0.43831(10) 0.5853(3) 0.7191(5) 0.0218(8) Uani 1 1 d . . . . .
O14 O 0.44044(7) 0.6869(2) 0.7589(4) 0.0298(7) Uani 1 1 d . . . . .
C15 C 0.35131(10) 0.4682(3) 0.5668(7) 0.0300(9) Uani 1 1 d . . . . .
H15A H 0.329214 0.456574 0.511130 0.045 Uiso 1 1 calc R U . . .
H15B H 0.353023 0.426055 0.677498 0.045 Uiso 1 1 calc R U . . .
H15C H 0.369057 0.446637 0.482474 0.045 Uiso 1 1 calc R U . . .
C16 C 0.46962(9) 0.5215(3) 0.7370(5) 0.0217(8) Uani 1 1 d . . . . .
C17 C 0.47044(10) 0.4107(3) 0.7436(5) 0.0227(8) Uani 1 1 d . . . . .
C18 C 0.43977(10) 0.3408(3) 0.7462(6) 0.0289(9) Uani 1 1 d . . . . .
H18A H 0.421865 0.375268 0.815829 0.043 Uiso 1 1 calc R U . . .
H18B H 0.445443 0.272679 0.801981 0.043 Uiso 1 1 calc R U . . .
H18C H 0.431991 0.328885 0.622284 0.043 Uiso 1 1 calc R U . . .
N19 N 0.500000 0.3584(4) 0.750000 0.0238(10) Uani 1 2 d S T P . .
C20 C 0.500000 0.5765(4) 0.750000 0.0231(11) Uani 1 2 d S T P . .
H20A H 0.499999 0.651780 0.749999 0.028 Uiso 1 2 calc R U P . .
O21 O 0.40963(9) 0.8483(3) 0.9028(5) 0.0535(11) Uani 1 1 d . . . . .
O22 O 0.41071(9) 0.8456(3) 0.5524(5) 0.0460(9) Uani 1 1 d . . . . .
C23 C 0.3453(2) 0.8539(8) 0.2376(14) 0.098(3) Uani 1 1 d . . . . .
H23A H 0.323220 0.831566 0.191910 0.148 Uiso 0.52 1 d R U P A 1
H23C H 0.342875 0.880043 0.361456 0.148 Uiso 0.52 1 d R U P A 1
H23B H 0.360790 0.793479 0.236100 0.148 Uiso 0.52 1 d R U P A 1
H23F H 0.337285 0.877495 0.119073 0.148 Uiso 0.48 1 d R U P B 2
H23E H 0.326040 0.831096 0.310829 0.148 Uiso 0.48 1 d R U P B 2
H23D H 0.360930 0.794510 0.222246 0.148 Uiso 0.48 1 d R U P B 2
O24A O 0.3586(3) 0.9385(17) 0.1231(18) 0.143(7) Uani 0.52 1 d . . P C 1
H24A H 0.375824 0.916800 0.068927 0.215 Uiso 0.52 1 calc R U P C 1
O24B O 0.3623(3) 0.9408(11) 0.327(3) 0.143(8) Uani 0.48 1 d . . P C 2
H24B H 0.348082 0.979183 0.379225 0.215 Uiso 0.48 1 calc R U P C 2
N25 N 0.43084(10) 0.9411(3) 1.2236(5) 0.0339(9) Uani 1 1 d . . . . .
H25A H 0.424498 1.006973 1.233253 0.051 Uiso 1 1 d R U . . .
H25B H 0.451898 0.917994 1.225641 0.051 Uiso 1 1 d R U . . .
H25C H 0.422458 0.913495 1.124759 0.051 Uiso 1 1 d R U . . .
H25D H 0.421088 0.914014 1.318281 0.051 Uiso 1 1 d R U . . .
O1W O 0.500000 0.8573(11) 1.250000 0.031(3) Uani 0.32 2 d S T P . .
H1WA H 0.500000 0.782577 1.250000 0.047 Uiso 0.32 2 d R U P . .
H1WB H 0.494440 0.870227 1.119080 0.047 Uiso 0.16 1 d R U P . .


_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 O22 1.618(3) . ?
V1 O21 1.637(4) . ?
V1 O8 1.915(3) . ?
V1 O14 1.954(3) . ?
V1 N11 2.108(3) . ?
C1 C6 1.373(7) . ?
C1 C2 1.400(7) . ?
C1 H1A 0.9500 . ?
C2 C3 1.379(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.391(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.400(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.501(6) . ?
C7 O8 1.304(5) . ?
C7 C9 1.352(6) . ?
C9 C10 1.416(6) . ?
C9 H9A 0.9500 . ?
C10 N11 1.324(5) . ?
C10 C15 1.498(6) . ?
N11 N12 1.406(5) . ?
N12 C13 1.294(5) . ?
C13 O14 1.318(5) . ?
C13 C16 1.487(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C20 1.394(5) . ?
C16 C17 1.399(6) . ?
C17 N19 1.347(5) . ?
C17 C18 1.503(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9500 . ?
C23 O24B 1.447(15) . ?
C23 O24A 1.462(18) . ?
C23 H23A 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23F 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23D 0.9800 . ?
O24A H24A 0.8400 . ?
O24B H24B 0.8400 . ?
N25 H25A 0.8711 . ?
N25 H25B 0.8853 . ?
N25 H25C 0.8769 . ?
N25 H25D 0.8709 . ?
O1W H1WA 0.9423 . ?
O1W H1WB 1.0083 . ?

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
O22 V1 O21 105.9(2) . . ?
O22 V1 O8 103.16(18) . . ?
O21 V1 O8 95.02(17) . . ?
O22 V1 O14 101.94(15) . . ?
O21 V1 O14 92.47(15) . . ?
O8 V1 O14 150.67(14) . . ?
O22 V1 N11 113.08(17) . . ?
O21 V1 N11 140.6(2) . . ?
O8 V1 N11 81.92(13) . . ?
O14 V1 N11 74.43(12) . . ?
C6 C1 C2 120.9(5) . . ?
C6 C1 H1A 119.6 . . ?
C2 C1 H1A 119.6 . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 119.9(5) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
C1 C6 C5 119.0(4) . . ?
C1 C6 C7 119.1(4) . . ?
C5 C6 C7 121.9(4) . . ?
O8 C7 C9 122.8(4) . . ?
O8 C7 C6 114.1(4) . . ?
C9 C7 C6 123.0(4) . . ?
C7 O8 V1 135.9(3) . . ?
C7 C9 C10 124.5(4) . . ?
C7 C9 H9A 117.8 . . ?
C10 C9 H9A 117.8 . . ?
N11 C10 C9 120.7(4) . . ?
N11 C10 C15 119.8(4) . . ?
C9 C10 C15 119.4(4) . . ?
C10 N11 N12 113.6(3) . . ?
C10 N11 V1 130.4(3) . . ?
N12 N11 V1 116.0(2) . . ?
C13 N12 N11 108.9(3) . . ?
N12 C13 O14 122.1(4) . . ?
N12 C13 C16 120.9(3) . . ?
O14 C13 C16 117.0(3) . . ?
C13 O14 V1 118.4(2) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C16 C17 118.3(4) . . ?
C20 C16 C13 117.3(4) . . ?
C17 C16 C13 124.3(3) . . ?
N19 C17 C16 120.8(4) . . ?
N19 C17 C18 114.7(4) . . ?
C16 C17 C18 124.6(4) . . ?
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 . . ?
C17 N19 C17 121.3(5) . 3_656 ?
C16 C20 C16 120.3(5) . 3_656 ?
C16 C20 H20A 119.8 . . ?
C16 C20 H20A 119.8 3_656 . ?
O24A C23 H23A 109.4 . . ?
O24A C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
O24A C23 H23B 109.6 . . ?
H23A C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
O24B C23 H23F 109.3 . . ?
O24B C23 H23E 109.5 . . ?
H23F C23 H23E 109.5 . . ?
O24B C23 H23D 109.6 . . ?
H23F C23 H23D 109.5 . . ?
H23E C23 H23D 109.5 . . ?
C23 O24A H24A 109.5 . . ?
C23 O24B H24B 109.5 . . ?
H25A N25 H25B 125.8 . . ?
H25A N25 H25C 109.7 . . ?
H25B N25 H25C 104.0 . . ?
H25A N25 H25D 100.4 . . ?
H25B N25 H25D 106.1 . . ?
H25C N25 H25D 110.4 . . ?
H1WA O1W H1WB 99.3 . . ?

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
C6 C1 C2 C3 -2.6(8) . . . . ?
C1 C2 C3 C4 1.1(8) . . . . ?
C2 C3 C4 C5 0.1(8) . . . . ?
C3 C4 C5 C6 0.1(8) . . . . ?
C2 C1 C6 C5 2.7(8) . . . . ?
C2 C1 C6 C7 -177.7(5) . . . . ?
C4 C5 C6 C1 -1.5(8) . . . . ?
C4 C5 C6 C7 179.0(5) . . . . ?
C1 C6 C7 O8 -1.9(6) . . . . ?
C5 C6 C7 O8 177.6(4) . . . . ?
C1 C6 C7 C9 174.2(5) . . . . ?
C5 C6 C7 C9 -6.3(7) . . . . ?
C9 C7 O8 V1 17.3(7) . . . . ?
C6 C7 O8 V1 -166.6(3) . . . . ?
O8 C7 C9 C10 3.8(7) . . . . ?
C6 C7 C9 C10 -171.9(4) . . . . ?
C7 C9 C10 N11 -8.2(7) . . . . ?
C7 C9 C10 C15 167.8(4) . . . . ?
C9 C10 N11 N12 174.7(4) . . . . ?
C15 C10 N11 N12 -1.4(5) . . . . ?
C9 C10 N11 V1 -5.2(6) . . . . ?
C15 C10 N11 V1 178.8(3) . . . . ?
C10 N11 N12 C13 -178.3(3) . . . . ?
V1 N11 N12 C13 1.5(4) . . . . ?
N11 N12 C13 O14 0.7(5) . . . . ?
N11 N12 C13 C16 -179.3(3) . . . . ?
N12 C13 O14 V1 -2.8(5) . . . . ?
C16 C13 O14 V1 177.2(3) . . . . ?
N12 C13 C16 C20 164.4(3) . . . . ?
O14 C13 C16 C20 -15.5(5) . . . . ?
N12 C13 C16 C17 -16.3(6) . . . . ?
O14 C13 C16 C17 163.7(4) . . . . ?
C20 C16 C17 N19 -4.4(5) . . . . ?
C13 C16 C17 N19 176.3(3) . . . . ?
C20 C16 C17 C18 174.9(3) . . . . ?
C13 C16 C17 C18 -4.3(7) . . . . ?
C16 C17 N19 C17 2.3(3) . . . 3_656 ?
C18 C17 N19 C17 -177.2(4) . . . 3_656 ?
C17 C16 C20 C16 2.2(3) . . . 3_656 ?
C13 C16 C20 C16 -178.5(4) . . . 3_656 ?

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
C15 H15C N11 0.98 2.62 3.488(6) 148.0 7_565 yes
O24A^a H24A^a O21 0.84 2.02 2.840(14) 167.0 1_554 yes
O24A^a H24A^a N25 0.84 2.49 2.964(12) 117.1 1_554 yes
N25 H25A O21 0.87 2.29 3.088(6) 151.5 7_576 yes
N25 H25A O22 0.87 2.36 3.080(5) 140.6 7_576 yes
N25 H25B O1W 0.89 2.06 2.948(7) 175.2 . yes
N25 H25C O21 0.88 1.91 2.781(5) 173.1 . yes
N25 H25D O22 0.87 1.98 2.833(5) 165.6 1_556 yes
N25 H25D O24B^b 0.87 2.36 2.824(15) 113.9 1_556 yes
O1W H1WA N19 0.94 1.78 2.720(15) 180.0 5_667 yes

_refine_diff_density_max         0.551
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.089

####################################################################### 
# 
# 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_ft161-1a_a
_database_code_depnum_ccdc_archive 'CCDC 2206037'
loop_
_audit_author_name
_audit_author_address
'Anna Kozakiewicz-Piekarz'
;Faculty of Chemistry, Nicolaus Copernicus University in Torun
Poland
;
_audit_update_record             
;
2023-02-13 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H21 N5 O10 V2, H2 O, 2(H4 N)'
_chemical_formula_sum            'C25 H31 N7 O11 V2'
_chemical_formula_weight         707.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.1522(4)
_cell_length_b                   15.2574(7)
_cell_length_c                   25.8864(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.0557(2)
_cell_angle_gamma                90
_cell_volume                     2824.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1253
_cell_measurement_theta_min      2.6790
_cell_measurement_theta_max      21.9390

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    6.205
_shelx_estimated_absorpt_T_min   0.304
_shelx_estimated_absorpt_T_max   0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            12900
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.362
_diffrn_reflns_theta_max         78.338
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measured_fraction_theta_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_point_group_measured_fraction_full 0.947
_reflns_number_total             5348
_reflns_number_gt                5138
_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       'Oxford Diffraction CrysAlis'
_computing_cell_refinement       'Oxford Diffraction CrysAlis'
_computing_data_reduction        'Oxford Diffraction CrysAlis'
_computing_structure_solution    'SHELXT-2017 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Diamond software'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_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)+(0.0276P)²+16.6690P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5348
_refine_ls_number_parameters     431
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.008
_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
V1A V 0.57699(10) 0.25450(4) 0.65231(3) 0.01294(18) Uani 1 1 d . . . . .
V1B V 0.88303(10) 0.75905(4) 0.65303(3) 0.01279(17) Uani 1 1 d . . . . .
C1A C 0.3963(6) -0.0130(3) 0.56265(18) 0.0199(9) Uani 1 1 d . . . . .
H1A H 0.366270 -0.012040 0.526891 0.024 Uiso 1 1 calc R U . . .
C2A C 0.3731(6) -0.0885(3) 0.59024(18) 0.0208(9) Uani 1 1 d . . . . .
H2A H 0.327185 -0.139679 0.573640 0.025 Uiso 1 1 calc R U . . .
C3A C 0.4168(6) -0.0905(3) 0.64294(18) 0.0196(9) Uani 1 1 d . . . . .
H3A H 0.400198 -0.143033 0.662104 0.024 Uiso 1 1 calc R U . . .
C4A C 0.4836(6) -0.0168(3) 0.66692(17) 0.0172(9) Uani 1 1 d . . . . .
O5A O 0.5288(5) -0.0113(2) 0.71787(12) 0.0221(7) Uani 1 1 d . . . . .
C6A C 0.4674(8) -0.0815(3) 0.74988(19) 0.0275(11) Uani 1 1 d . . . . .
H6A H 0.507357 -0.070859 0.785554 0.041 Uiso 1 1 calc R U . . .
H6B H 0.330710 -0.085449 0.748549 0.041 Uiso 1 1 calc R U . . .
H6C H 0.521887 -0.136637 0.737572 0.041 Uiso 1 1 calc R U . . .
C7A C 0.5083(6) 0.0622(3) 0.63916(16) 0.0151(8) Uani 1 1 d . . . . .
O8A O 0.5756(4) 0.13089(19) 0.66464(11) 0.0170(6) Uani 1 1 d . . . . .
C9A C 0.4643(6) 0.0636(3) 0.58667(17) 0.0168(8) Uani 1 1 d . . . . .
C10A C 0.4982(6) 0.1400(3) 0.55601(16) 0.0170(8) Uani 1 1 d . . . . .
H10A H 0.476064 0.136306 0.519888 0.020 Uiso 1 1 calc R U . . .
N11A N 0.5574(5) 0.2144(2) 0.57457(13) 0.0149(7) Uani 1 1 d . . . . .
N12A N 0.5956(5) 0.2772(2) 0.53698(13) 0.0162(7) Uani 1 1 d . . . . .
C13A C 0.6439(6) 0.3496(3) 0.56041(16) 0.0143(8) Uani 1 1 d . . . . .
O14A O 0.6525(4) 0.35656(19) 0.61046(11) 0.0183(6) Uani 1 1 d . . . . .
C15A C 0.6953(6) 0.4281(3) 0.52949(16) 0.0142(8) Uani 1 1 d . . . . .
C16A C 0.7142(6) 0.4284(3) 0.47540(16) 0.0145(8) Uani 1 1 d . . . . .
C17A C 0.6824(7) 0.3496(3) 0.44109(17) 0.0232(10) Uani 1 1 d . . . . .
H17A H 0.777224 0.312253 0.447599 0.035 Uiso 1 1 d R U . . .
H17B H 0.696874 0.360713 0.408649 0.035 Uiso 1 1 d R U . . .
H17C H 0.565404 0.337193 0.446599 0.035 Uiso 1 1 d R U . . .
N18A N 0.7689(5) 0.5013(2) 0.45051(13) 0.0148(7) Uani 1 1 d . . . . .
C16B C 0.8053(6) 0.5766(3) 0.47583(16) 0.0146(8) Uani 1 1 d . . . . .
C17B C 0.8712(6) 0.6509(3) 0.44254(16) 0.0176(9) Uani 1 1 d . . . . .
H17D H 0.974384 0.681408 0.459822 0.026 Uiso 1 1 calc R U . . .
H17E H 0.767889 0.691988 0.436789 0.026 Uiso 1 1 calc R U . . .
H17F H 0.914341 0.627927 0.409278 0.026 Uiso 1 1 calc R U . . .
C15B C 0.7857(6) 0.5811(3) 0.52984(16) 0.0145(8) Uani 1 1 d . . . . .
C18B C 0.7324(6) 0.5057(3) 0.55587(16) 0.0144(8) Uani 1 1 d . . . . .
H18B H 0.721113 0.506964 0.592422 0.017 Uiso 1 1 calc R U . . .
C13B C 0.8193(6) 0.6613(3) 0.56104(15) 0.0139(8) Uani 1 1 d . . . . .
O14B O 0.8436(4) 0.65200(19) 0.61074(11) 0.0179(6) Uani 1 1 d . . . . .
N12B N 0.8203(5) 0.7384(2) 0.53898(13) 0.0163(7) Uani 1 1 d . . . . .
N11B N 0.8518(5) 0.8032(2) 0.57632(13) 0.0134(7) Uani 1 1 d . . . . .
C10B C 0.8536(6) 0.8825(3) 0.55784(16) 0.0169(8) Uani 1 1 d . . . . .
H10B H 0.823849 0.889809 0.522330 0.020 Uiso 1 1 calc R U . . .
C9B C 0.8968(6) 0.9592(3) 0.58681(17) 0.0167(8) Uani 1 1 d . . . . .
C1B C 0.9144(6) 1.0401(3) 0.56004(18) 0.0196(9) Uani 1 1 d . . . . .
H1B H 0.883202 1.043414 0.524413 0.023 Uiso 1 1 calc R U . . .
C2B C 0.9763(6) 1.1134(3) 0.58549(18) 0.0216(9) Uani 1 1 d . . . . .
H2B H 0.987799 1.167363 0.567448 0.026 Uiso 1 1 calc R U . . .
C3B C 1.0225(6) 1.1090(3) 0.63794(18) 0.0196(9) Uani 1 1 d . . . . .
H3B H 1.069208 1.159491 0.655108 0.024 Uiso 1 1 calc R U . . .
C4B C 1.0005(6) 1.0316(3) 0.66486(16) 0.0172(9) Uani 1 1 d . . . . .
O5B O 1.0412(5) 1.0208(2) 0.71573(12) 0.0215(7) Uani 1 1 d . . . . .
C6B C 1.1286(7) 1.0936(3) 0.74128(18) 0.0231(10) Uani 1 1 d . . . . .
H6D H 1.151404 1.078675 0.777558 0.035 Uiso 1 1 calc R U . . .
H6E H 1.247680 1.107033 0.724340 0.035 Uiso 1 1 calc R U . . .
H6F H 1.046292 1.144894 0.739383 0.035 Uiso 1 1 calc R U . . .
C7B C 0.9347(6) 0.9542(3) 0.63992(16) 0.0160(8) Uani 1 1 d . . . . .
O8B O 0.9142(4) 0.88267(19) 0.66710(11) 0.0180(6) Uani 1 1 d . . . . .
O22A O 0.7336(4) 0.2749(2) 0.69751(12) 0.0196(6) Uani 1 1 d . . . . .
O21A O 0.3691(4) 0.2819(2) 0.67181(12) 0.0193(6) Uani 1 1 d . . . . .
O21B O 1.0813(5) 0.7268(2) 0.67746(13) 0.0237(7) Uani 1 1 d . . . . .
O22B O 0.7128(4) 0.7385(2) 0.69337(12) 0.0212(7) Uani 1 1 d . . . . .
O1W O 0.8640(5) 0.4769(2) 0.34494(12) 0.0248(7) Uani 1 1 d . . . . .
H1WA H 0.956458 0.441705 0.348393 0.037 Uiso 1 1 d R U . . .
H1WB H 0.833028 0.496755 0.374683 0.037 Uiso 1 1 d R U . . .
N24 N 0.0651(5) 0.3695(2) 0.71868(14) 0.0179(7) Uani 1 1 d D . . . .
H24A H 0.179(2) 0.3357(15) 0.7091(11) 0.027 Uiso 1 1 d D U . . .
H24B H 0.059(4) 0.4245(10) 0.6979(9) 0.027 Uiso 1 1 d D U . . .
H24C H -0.048(2) 0.3333(15) 0.7116(11) 0.027 Uiso 1 1 d D U . . .
H24D H 0.070(4) 0.3844(18) 0.7561(3) 0.027 Uiso 1 1 d D U . . .
N23 N 1.3834(5) 0.6439(3) 0.72294(14) 0.0212(8) Uani 1 1 d D . . . .
H23A H 1.5077(19) 0.6678(17) 0.7127(11) 0.032 Uiso 1 1 d D U . . .
H23B H 1.339(4) 0.6022(14) 0.6960(8) 0.032 Uiso 1 1 d D U . . .
H23C H 1.292(3) 0.6930(12) 0.7264(11) 0.032 Uiso 1 1 d D U . . .
H23D H 1.395(4) 0.6128(16) 0.7566(5) 0.032 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
V1A O21A 1.625(3) . ?
V1A O22A 1.649(3) . ?
V1A O8A 1.913(3) . ?
V1A O14A 1.973(3) . ?
V1A N11A 2.108(3) . ?
V1B O21B 1.628(3) . ?
V1B O22B 1.635(3) . ?
V1B O8B 1.934(3) . ?
V1B O14B 1.986(3) . ?
V1B N11B 2.109(3) . ?
C1A C2A 1.366(6) . ?
C1A C9A 1.410(6) . ?
C1A H1A 0.9500 . ?
C2A C3A 1.400(7) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.370(6) . ?
C3A H3A 0.9500 . ?
C4A O5A 1.360(5) . ?
C4A C7A 1.414(6) . ?
O5A C6A 1.424(5) . ?
C6A H6A 0.9800 . ?
C6A H6B 0.9800 . ?
C6A H6C 0.9800 . ?
C7A O8A 1.328(5) . ?
C7A C9A 1.395(6) . ?
C9A C10A 1.431(6) . ?
C10A N11A 1.303(5) . ?
C10A H10A 0.9500 . ?
N11A N12A 1.392(5) . ?
N12A C13A 1.307(5) . ?
C13A O14A 1.301(5) . ?
C13A C15A 1.487(6) . ?
C15A C18B 1.391(6) . ?
C15A C16A 1.407(6) . ?
C16A N18A 1.344(5) . ?
C16A C17A 1.512(6) . ?
C17A H17A 0.9011 . ?
C17A H17B 0.8631 . ?
C17A H17C 0.8700 . ?
N18A C16B 1.348(5) . ?
C16B C15B 1.407(6) . ?
C16B C17B 1.501(6) . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
C15B C18B 1.387(6) . ?
C15B C13B 1.486(6) . ?
C18B H18B 0.9500 . ?
C13B O14B 1.306(5) . ?
C13B N12B 1.308(5) . ?
N12B N11B 1.401(5) . ?
N11B C10B 1.301(5) . ?
C10B C9B 1.423(6) . ?
C10B H10B 0.9500 . ?
C9B C7B 1.403(6) . ?
C9B C1B 1.422(6) . ?
C1B C2B 1.371(6) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.399(7) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.380(6) . ?
C3B H3B 0.9500 . ?
C4B O5B 1.358(5) . ?
C4B C7B 1.427(6) . ?
O5B C6B 1.436(5) . ?
C6B H6D 0.9800 . ?
C6B H6E 0.9800 . ?
C6B H6F 0.9800 . ?
C7B O8B 1.306(5) . ?
O1W H1WA 0.8565 . ?
O1W H1WB 0.8566 . ?
N24 H24A 0.9969(19) . ?
N24 H24B 0.9971(19) . ?
N24 H24C 0.9970(19) . ?
N24 H24D 0.9969(19) . ?
N23 H23A 0.9970(19) . ?
N23 H23B 0.9970(19) . ?
N23 H23C 0.9969(19) . ?
N23 H23D 0.9970(19) . ?

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
O21A V1A O22A 110.60(16) . . ?
O21A V1A O8A 101.34(14) . . ?
O22A V1A O8A 94.12(14) . . ?
O21A V1A O14A 102.62(14) . . ?
O22A V1A O14A 93.12(14) . . ?
O8A V1A O14A 150.64(13) . . ?
O21A V1A N11A 108.13(15) . . ?
O22A V1A N11A 140.99(15) . . ?
O8A V1A N11A 82.70(13) . . ?
O14A V1A N11A 73.89(13) . . ?
O21B V1B O22B 110.04(17) . . ?
O21B V1B O8B 96.96(15) . . ?
O22B V1B O8B 98.80(14) . . ?
O21B V1B O14B 95.09(15) . . ?
O22B V1B O14B 95.09(14) . . ?
O8B V1B O14B 157.24(13) . . ?
O21B V1B N11B 123.62(16) . . ?
O22B V1B N11B 125.77(16) . . ?
O8B V1B N11B 82.98(13) . . ?
O14B V1B N11B 74.27(12) . . ?
C2A C1A C9A 120.7(4) . . ?
C2A C1A H1A 119.7 . . ?
C9A C1A H1A 119.7 . . ?
C1A C2A C3A 120.1(4) . . ?
C1A C2A H2A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C4A C3A C2A 120.1(4) . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
O5A C4A C3A 124.9(4) . . ?
O5A C4A C7A 114.2(4) . . ?
C3A C4A C7A 120.9(4) . . ?
C4A O5A C6A 116.4(4) . . ?
O5A C6A H6A 109.5 . . ?
O5A C6A H6B 109.5 . . ?
H6A C6A H6B 109.5 . . ?
O5A C6A H6C 109.5 . . ?
H6A C6A H6C 109.5 . . ?
H6B C6A H6C 109.5 . . ?
O8A C7A C9A 123.5(4) . . ?
O8A C7A C4A 117.7(4) . . ?
C9A C7A C4A 118.7(4) . . ?
C7A O8A V1A 134.2(3) . . ?
C7A C9A C1A 119.6(4) . . ?
C7A C9A C10A 121.0(4) . . ?
C1A C9A C10A 119.3(4) . . ?
N11A C10A C9A 124.1(4) . . ?
N11A C10A H10A 118.0 . . ?
C9A C10A H10A 118.0 . . ?
C10A N11A N12A 113.9(3) . . ?
C10A N11A V1A 128.7(3) . . ?
N12A N11A V1A 117.1(3) . . ?
C13A N12A N11A 108.0(3) . . ?
O14A C13A N12A 122.9(4) . . ?
O14A C13A C15A 117.3(4) . . ?
N12A C13A C15A 119.8(4) . . ?
C13A O14A V1A 118.0(3) . . ?
C18B C15A C16A 117.8(4) . . ?
C18B C15A C13A 117.9(4) . . ?
C16A C15A C13A 124.2(4) . . ?
N18A C16A C15A 120.5(4) . . ?
N18A C16A C17A 114.9(4) . . ?
C15A C16A C17A 124.6(4) . . ?
C16A C17A H17A 106.3 . . ?
C16A C17A H17B 113.4 . . ?
H17A C17A H17B 102.5 . . ?
C16A C17A H17C 102.7 . . ?
H17A C17A H17C 123.8 . . ?
H17B C17A H17C 108.6 . . ?
C16A N18A C16B 121.9(4) . . ?
N18A C16B C15B 120.4(4) . . ?
N18A C16B C17B 115.2(4) . . ?
C15B C16B C17B 124.4(4) . . ?
C16B C17B H17D 109.5 . . ?
C16B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
C16B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C18B C15B C16B 118.0(4) . . ?
C18B C15B C13B 117.6(4) . . ?
C16B C15B C13B 124.4(4) . . ?
C15B C18B C15A 121.3(4) . . ?
C15B C18B H18B 119.3 . . ?
C15A C18B H18B 119.3 . . ?
O14B C13B N12B 121.8(4) . . ?
O14B C13B C15B 117.9(4) . . ?
N12B C13B C15B 120.3(4) . . ?
C13B O14B V1B 118.2(3) . . ?
C13B N12B N11B 109.5(3) . . ?
C10B N11B N12B 113.9(3) . . ?
C10B N11B V1B 130.0(3) . . ?
N12B N11B V1B 116.2(2) . . ?
N11B C10B C9B 124.9(4) . . ?
N11B C10B H10B 117.5 . . ?
C9B C10B H10B 117.5 . . ?
C7B C9B C1B 120.5(4) . . ?
C7B C9B C10B 120.9(4) . . ?
C1B C9B C10B 118.4(4) . . ?
C2B C1B C9B 120.2(4) . . ?
C2B C1B H1B 119.9 . . ?
C9B C1B H1B 119.9 . . ?
C1B C2B C3B 120.2(4) . . ?
C1B C2B H2B 119.9 . . ?
C3B C2B H2B 119.9 . . ?
C4B C3B C2B 120.3(4) . . ?
C4B C3B H3B 119.8 . . ?
C2B C3B H3B 119.8 . . ?
O5B C4B C3B 124.7(4) . . ?
O5B C4B C7B 114.1(4) . . ?
C3B C4B C7B 121.2(4) . . ?
C4B O5B C6B 116.5(3) . . ?
O5B C6B H6D 109.5 . . ?
O5B C6B H6E 109.5 . . ?
H6D C6B H6E 109.5 . . ?
O5B C6B H6F 109.5 . . ?
H6D C6B H6F 109.5 . . ?
H6E C6B H6F 109.5 . . ?
O8B C7B C9B 123.5(4) . . ?
O8B C7B C4B 119.0(4) . . ?
C9B C7B C4B 117.5(4) . . ?
C7B O8B V1B 136.5(3) . . ?
H1WA O1W H1WB 109.2 . . ?
H24A N24 H24B 109.5(3) . . ?
H24A N24 H24C 109.5(3) . . ?
H24B N24 H24C 109.4(3) . . ?
H24A N24 H24D 109.5(3) . . ?
H24B N24 H24D 109.5(3) . . ?
H24C N24 H24D 109.5(3) . . ?
H23A N23 H23B 109.5(3) . . ?
H23A N23 H23C 109.5(3) . . ?
H23B N23 H23C 109.5(3) . . ?
H23A N23 H23D 109.5(3) . . ?
H23B N23 H23D 109.5(3) . . ?
H23C N23 H23D 109.5(3) . . ?

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
C9A C1A C2A C3A 0.0(7) . . . . ?
C1A C2A C3A C4A -0.2(7) . . . . ?
C2A C3A C4A O5A 179.4(4) . . . . ?
C2A C3A C4A C7A 0.4(7) . . . . ?
C3A C4A O5A C6A -12.9(6) . . . . ?
C7A C4A O5A C6A 166.2(4) . . . . ?
O5A C4A C7A O8A 1.6(6) . . . . ?
C3A C4A C7A O8A -179.3(4) . . . . ?
O5A C4A C7A C9A -179.4(4) . . . . ?
C3A C4A C7A C9A -0.3(6) . . . . ?
C9A C7A O8A V1A 19.8(6) . . . . ?
C4A C7A O8A V1A -161.3(3) . . . . ?
O8A C7A C9A C1A 179.0(4) . . . . ?
C4A C7A C9A C1A 0.1(6) . . . . ?
O8A C7A C9A C10A 3.0(6) . . . . ?
C4A C7A C9A C10A -175.9(4) . . . . ?
C2A C1A C9A C7A 0.0(7) . . . . ?
C2A C1A C9A C10A 176.1(4) . . . . ?
C7A C9A C10A N11A -5.3(7) . . . . ?
C1A C9A C10A N11A 178.6(4) . . . . ?
C9A C10A N11A N12A 174.8(4) . . . . ?
C9A C10A N11A V1A -11.7(6) . . . . ?
C10A N11A N12A C13A 176.7(4) . . . . ?
V1A N11A N12A C13A 2.4(4) . . . . ?
N11A N12A C13A O14A 0.3(5) . . . . ?
N11A N12A C13A C15A 179.2(3) . . . . ?
N12A C13A O14A V1A -3.0(5) . . . . ?
C15A C13A O14A V1A 178.0(3) . . . . ?
O14A C13A C15A C18B -5.6(6) . . . . ?
N12A C13A C15A C18B 175.4(4) . . . . ?
O14A C13A C15A C16A 172.3(4) . . . . ?
N12A C13A C15A C16A -6.7(6) . . . . ?
C18B C15A C16A N18A 0.9(6) . . . . ?
C13A C15A C16A N18A -177.1(4) . . . . ?
C18B C15A C16A C17A 178.9(4) . . . . ?
C13A C15A C16A C17A 0.9(7) . . . . ?
C15A C16A N18A C16B -0.8(6) . . . . ?
C17A C16A N18A C16B -179.0(4) . . . . ?
C16A N18A C16B C15B -0.4(6) . . . . ?
C16A N18A C16B C17B 178.0(4) . . . . ?
N18A C16B C15B C18B 1.5(6) . . . . ?
C17B C16B C15B C18B -176.7(4) . . . . ?
N18A C16B C15B C13B -178.9(4) . . . . ?
C17B C16B C15B C13B 2.9(7) . . . . ?
C16B C15B C18B C15A -1.4(6) . . . . ?
C13B C15B C18B C15A 178.9(4) . . . . ?
C16A C15A C18B C15B 0.3(6) . . . . ?
C13A C15A C18B C15B 178.4(4) . . . . ?
C18B C15B C13B O14B 17.0(6) . . . . ?
C16B C15B C13B O14B -162.7(4) . . . . ?
C18B C15B C13B N12B -161.7(4) . . . . ?
C16B C15B C13B N12B 18.6(6) . . . . ?
N12B C13B O14B V1B 0.0(5) . . . . ?
C15B C13B O14B V1B -178.7(3) . . . . ?
O14B C13B N12B N11B 0.5(6) . . . . ?
C15B C13B N12B N11B 179.1(4) . . . . ?
C13B N12B N11B C10B -179.5(4) . . . . ?
C13B N12B N11B V1B -0.7(4) . . . . ?
N12B N11B C10B C9B -174.9(4) . . . . ?
V1B N11B C10B C9B 6.5(7) . . . . ?
N11B C10B C9B C7B -2.6(7) . . . . ?
N11B C10B C9B C1B 172.8(4) . . . . ?
C7B C9B C1B C2B 2.8(7) . . . . ?
C10B C9B C1B C2B -172.7(4) . . . . ?
C9B C1B C2B C3B 0.0(7) . . . . ?
C1B C2B C3B C4B -2.1(7) . . . . ?
C2B C3B C4B O5B -179.9(4) . . . . ?
C2B C3B C4B C7B 1.4(7) . . . . ?
C3B C4B O5B C6B -5.8(6) . . . . ?
C7B C4B O5B C6B 172.9(4) . . . . ?
C1B C9B C7B O8B 177.3(4) . . . . ?
C10B C9B C7B O8B -7.4(7) . . . . ?
C1B C9B C7B C4B -3.3(6) . . . . ?
C10B C9B C7B C4B 172.0(4) . . . . ?
O5B C4B C7B O8B 1.9(6) . . . . ?
C3B C4B C7B O8B -179.3(4) . . . . ?
O5B C4B C7B C9B -177.5(4) . . . . ?
C3B C4B C7B C9B 1.3(6) . . . . ?
C9B C7B O8B V1B 15.0(7) . . . . ?
C4B C7B O8B V1B -164.4(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
C6A H6A O21A 0.98 2.65 3.133(6) 110.3 2_646 yes
C6A H6C O22B 0.98 2.61 3.573(6) 167.8 1_545 yes
C6B H6F O21B 0.98 2.65 3.288(6) 122.9 2_756 yes
O1W H1WA O14B 0.86 2.28 3.091(5) 157.6 3_766 yes
O1W H1WB N18A 0.86 2.02 2.841(5) 161.1 . yes
N24 H24A O21A 0.9969(19) 1.858(10) 2.827(5) 163(3) . yes
N24 H24B O1W 0.9971(19) 1.948(11) 2.909(5) 161(2) 3_666 yes
N24 H24C O22A 0.9970(19) 1.834(5) 2.829(5) 175(2) 1_455 yes
N24 H24D O5B 0.9969(19) 2.34(2) 2.966(5) 119.6(19) 2_646 yes
N24 H24D O8B 0.9969(19) 1.990(8) 2.967(5) 166(2) 2_646 yes
N23 H23A O22B 0.9970(19) 1.888(8) 2.867(5) 166(2) 1_655 yes
N23 H23B O1W 0.9970(19) 2.163(13) 3.100(5) 156(2) 3_766 yes
N23 H23C O22A 0.9969(19) 2.34(3) 2.990(5) 122(2) 2_756 yes
N23 H23C O21B 0.9969(19) 2.04(2) 2.765(5) 128(2) . yes
N23 H23D O5A 0.9970(19) 2.08(2) 2.890(5) 137(2) 2_756 yes
N23 H23D O8A 0.9970(19) 2.067(17) 2.931(5) 144(2) 2_756 yes

_refine_diff_density_max         0.632
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.101

