# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_exp_3698_auto
_database_code_depnum_ccdc_archive 'CCDC 2367532'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](methoxo)oxovanadium(v) methanol solvate"
_chemical_formula_moiety         'C14 H12 N3 O4 V, 1[CH4O]'
_chemical_formula_sum            'C15 H16 N3 O5 V'
_chemical_formula_weight         369.25
_chemical_absolute_configuration .
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   18.1755(4)
_cell_length_b                   18.1755(4)
_cell_length_c                   10.3739(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3427.0(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    17514
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      77.547
_cell_measurement_theta_min      4.909
_shelx_estimated_absorpt_T_max   0.784
_shelx_estimated_absorpt_T_min   0.656
_exptl_absorpt_coefficient_mu    5.112
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4845
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17514
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.547
_diffrn_reflns_theta_min         4.909
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                3308
_reflns_number_total             3558
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 
;
 Flack x determined using 1407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0506P)²+1.9758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1028
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C6(H6), C12(H12), C13(H13), C11(H11)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.33785(4) 0.19726(3) 0.13677(6) 0.03979(18) Uani 1 1 d . . . . .
O1 O 0.30711(14) 0.29010(14) 0.0564(2) 0.0405(6) Uani 1 1 d . . . . .
O4 O 0.34454(17) 0.14479(16) -0.0070(3) 0.0493(6) Uani 1 1 d . . . . .
O2 O 0.39847(17) 0.14303(16) 0.2468(3) 0.0506(7) Uani 1 1 d . . . . .
N2 N 0.35335(19) 0.27956(18) 0.2798(3) 0.0431(7) Uani 1 1 d . . . . .
N3 N 0.24576(19) 0.54969(18) -0.0556(3) 0.0433(7) Uani 1 1 d . . . . .
O3 O 0.25937(18) 0.17286(19) 0.1880(3) 0.0562(8) Uani 1 1 d . . . . .
N1 N 0.3379(2) 0.35184(19) 0.2424(3) 0.0483(8) Uani 1 1 d . . . . .
C1 C 0.3141(2) 0.3499(2) 0.1232(4) 0.0400(7) Uani 1 1 d . . . . .
C3 C 0.2752(2) 0.4217(2) -0.0679(4) 0.0439(8) Uani 1 1 d . . . . .
H3 H 0.279530 0.378606 -0.119244 0.053 Uiso 1 1 calc R U . . .
C4 C 0.2521(2) 0.4875(2) -0.1220(4) 0.0454(8) Uani 1 1 d . . . . .
H4 H 0.240221 0.488191 -0.211148 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3995(2) 0.1378(2) 0.3752(4) 0.0462(9) Uani 1 1 d . . . . .
C5 C 0.2641(3) 0.5481(2) 0.0696(4) 0.0493(9) Uani 1 1 d . . . . .
H5 H 0.260951 0.592413 0.117999 0.059 Uiso 1 1 calc R U . . .
C8 C 0.3844(2) 0.1987(3) 0.4542(4) 0.0489(9) Uani 1 1 d . . . . .
C2 C 0.2918(2) 0.4199(2) 0.0622(4) 0.0404(8) Uani 1 1 d . . . . .
C7 C 0.3676(2) 0.2699(3) 0.4002(4) 0.0496(9) Uani 1 1 d . . . . .
H7 H 0.367009 0.311359 0.455838 0.060 Uiso 1 1 calc R U . . .
C10 C 0.4173(3) 0.0706(3) 0.4318(5) 0.0597(11) Uani 1 1 d . . . . .
H10 H 0.428698 0.029190 0.379543 0.072 Uiso 1 1 calc R U . . .
C6 C 0.2872(3) 0.4849(2) 0.1310(4) 0.0489(9) Uani 1 1 d . . . . .
H6 H 0.299836 0.486069 0.219822 0.059 Uiso 1 1 calc R U . . .
C12 C 0.4033(3) 0.1240(4) 0.6428(5) 0.0707(14) Uani 1 1 d . . . . .
H12 H 0.404512 0.118985 0.733909 0.085 Uiso 1 1 calc R U . . .
C13 C 0.3868(3) 0.1907(3) 0.5888(4) 0.0588(11) Uani 1 1 d . . . . .
H13 H 0.376993 0.231858 0.642612 0.071 Uiso 1 1 calc R U . . .
C11 C 0.4182(3) 0.0646(3) 0.5661(6) 0.0683(15) Uani 1 1 d . . . . .
H11 H 0.429269 0.018551 0.604783 0.082 Uiso 1 1 calc R U . . .
C14 C 0.2979(4) 0.0873(3) -0.0494(6) 0.0728(15) Uani 1 1 d . . . . .
H14A H 0.286420 0.094261 -0.140926 0.109 Uiso 1 1 calc R U . . .
H14B H 0.252257 0.087912 0.000817 0.109 Uiso 1 1 calc R U . . .
H14C H 0.322764 0.039939 -0.037560 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 O1 1.963(3) . ?
V1 O4 1.775(3) . ?
V1 O2 1.868(3) . ?
V1 N2 2.125(3) . ?
V1 N3 2.380(3) 4_655 ?
V1 O3 1.585(3) . ?
O1 C1 1.296(5) . ?
O4 C14 1.415(6) . ?
O2 C9 1.336(5) . ?
N2 N1 1.398(5) . ?
N2 C7 1.288(5) . ?
N3 C4 1.328(5) . ?
N3 C5 1.341(5) . ?
N1 C1 1.310(5) . ?
C1 C2 1.477(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(6) . ?
C3 C2 1.383(5) . ?
C4 H4 0.9500 . ?
C9 C8 1.403(6) . ?
C9 C10 1.394(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(6) . ?
C8 C7 1.442(6) . ?
C8 C13 1.405(6) . ?
C2 C6 1.384(5) . ?
C7 H7 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.398(8) . ?
C6 H6 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.369(7) . ?
C12 C11 1.368(9) . ?
C13 H13 0.9500 . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
O1 V1 N2 74.28(11) . . ?
O1 V1 N3 77.05(11) . 4_655 ?
O4 V1 O1 97.15(12) . . ?
O4 V1 O2 100.93(14) . . ?
O4 V1 N2 162.89(14) . . ?
O4 V1 N3 80.96(13) . 4_655 ?
O2 V1 O1 151.76(13) . . ?
O2 V1 N2 82.34(13) . . ?
O2 V1 N3 84.55(13) . 4_655 ?
N2 V1 N3 82.66(13) . 4_655 ?
O3 V1 O1 97.27(15) . . ?
O3 V1 O4 101.13(17) . . ?
O3 V1 O2 100.28(16) . . ?
O3 V1 N2 94.72(16) . . ?
O3 V1 N3 174.20(15) . 4_655 ?
C1 O1 V1 117.8(2) . . ?
C14 O4 V1 128.1(3) . . ?
C9 O2 V1 130.9(3) . . ?
N1 N2 V1 116.2(2) . . ?
C7 N2 V1 127.4(3) . . ?
C7 N2 N1 116.0(3) . . ?
C4 N3 V1 125.4(3) . 3_565 ?
C4 N3 C5 117.6(3) . . ?
C5 N3 V1 116.9(3) . 3_565 ?
C1 N1 N2 107.6(3) . . ?
O1 C1 N1 124.0(3) . . ?
O1 C1 C2 117.8(3) . . ?
N1 C1 C2 118.2(3) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(4) . . ?
N3 C4 C3 123.4(4) . . ?
N3 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
O2 C9 C8 121.6(3) . . ?
O2 C9 C10 119.0(4) . . ?
C10 C9 C8 119.4(4) . . ?
N3 C5 H5 118.6 . . ?
N3 C5 C6 122.7(4) . . ?
C6 C5 H5 118.6 . . ?
C9 C8 C7 121.5(4) . . ?
C9 C8 C13 119.5(4) . . ?
C13 C8 C7 119.0(4) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C6 118.0(4) . . ?
C6 C2 C1 122.1(3) . . ?
N2 C7 C8 122.8(4) . . ?
N2 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.4(5) . . ?
C11 C10 H10 120.3 . . ?
C5 C6 C2 119.5(4) . . ?
C5 C6 H6 120.3 . . ?
C2 C6 H6 120.3 . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.3(5) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 C8 120.3(5) . . ?
C12 C13 H13 119.8 . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.1(5) . . ?
C12 C11 H11 119.5 . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
V1 O1 C1 N1 -2.6(5) . . . . ?
V1 O1 C1 C2 179.3(3) . . . . ?
V1 O2 C9 C8 -36.4(6) . . . . ?
V1 O2 C9 C10 144.7(3) . . . . ?
V1 N2 N1 C1 2.2(4) . . . . ?
V1 N2 C7 C8 7.9(6) . . . . ?
V1 N3 C4 C3 -174.6(3) 3_565 . . . ?
V1 N3 C5 C6 174.7(4) 3_565 . . . ?
O1 V1 O4 C14 -109.1(4) . . . . ?
O1 V1 O2 C9 75.6(5) . . . . ?
O1 C1 C2 C3 -9.9(5) . . . . ?
O1 C1 C2 C6 170.6(4) . . . . ?
O4 V1 O2 C9 -155.6(4) . . . . ?
O2 V1 O4 C14 92.7(4) . . . . ?
O2 C9 C8 C7 -0.6(6) . . . . ?
O2 C9 C8 C13 -179.4(4) . . . . ?
O2 C9 C10 C11 -179.7(4) . . . . ?
N2 V1 O4 C14 -167.7(5) . . . . ?
N2 V1 O2 C9 41.5(4) . . . . ?
N2 N1 C1 O1 0.1(5) . . . . ?
N2 N1 C1 C2 178.2(3) . . . . ?
N3 V1 O4 C14 175.3(4) 4_655 . . . ?
N3 V1 O2 C9 124.8(4) 4_655 . . . ?
N3 C5 C6 C2 -0.2(7) . . . . ?
O3 V1 O4 C14 -10.2(5) . . . . ?
O3 V1 O2 C9 -52.0(4) . . . . ?
N1 N2 C7 C8 179.8(4) . . . . ?
N1 C1 C2 C3 171.9(4) . . . . ?
N1 C1 C2 C6 -7.6(6) . . . . ?
C1 C2 C6 C5 -178.3(4) . . . . ?
C3 C2 C6 C5 2.2(7) . . . . ?
C4 N3 C5 C6 -1.5(7) . . . . ?
C4 C3 C2 C1 178.0(4) . . . . ?
C4 C3 C2 C6 -2.5(6) . . . . ?
C9 C8 C7 N2 11.9(7) . . . . ?
C9 C8 C13 C12 -0.5(7) . . . . ?
C9 C10 C11 C12 -1.3(8) . . . . ?
C5 N3 C4 C3 1.2(6) . . . . ?
C8 C9 C10 C11 1.3(7) . . . . ?
C2 C3 C4 N3 0.8(6) . . . . ?
C7 N2 N1 C1 -170.6(4) . . . . ?
C7 C8 C13 C12 -179.4(4) . . . . ?
C10 C9 C8 C7 178.4(4) . . . . ?
C10 C9 C8 C13 -0.4(6) . . . . ?
C13 C8 C7 N2 -169.2(4) . . . . ?
C13 C12 C11 C10 0.4(8) . . . . ?
C11 C12 C13 C8 0.5(8) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 144 electrons were 
found in a volume of 714Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH4O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.895 356.7 71.5 '4 CH4O'
2 0.500 0.500 -0.538 356.7 71.5 '4 CH4O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_2635
_database_code_depnum_ccdc_archive 'CCDC 2367535'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](propoxo)oxovanadium(v)"
_chemical_formula_moiety         'C16 H16 N3 O4 V'
_chemical_formula_sum            'C16 H16 N3 O4 V'
_chemical_formula_weight         365.26
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

# start Validation Reply Form
_vrf_PLAT430_exp_2635            
;
PROBLEM: Short Inter D...A Contact  O1       ..N3       .       2.80 Ang.  
RESPONSE: Polymer with V-py coordination bond.
;
# end Validation Reply Form

_cell_length_a                   12.9499(3)
_cell_length_b                   11.4867(3)
_cell_length_c                   21.6234(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3216.52(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.7810
_cell_measurement_theta_min      4.0540
_shelx_estimated_absorpt_T_max   0.900
_shelx_estimated_absorpt_T_min   0.335
_exptl_absorpt_coefficient_mu    5.393
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -1 0.0332
1 0 1 0.0175
0 -2 -1 0.1010
0 2 1 0.1350
1 0 -2 0.0097
-1 0 2 0.0097

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16891
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.678
_diffrn_reflns_theta_min         4.089
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  26.00   0.50    1.10    --  -46.91  87.00 -60.00   80
  2  ω    -61.00 -17.00   0.50    1.10    --  -46.91  87.00 -60.00   88
  3  ω    -58.00 -28.00   0.50    4.30    --  -86.25 113.00  22.00   60
  4  ω    101.00 163.00   0.50    4.30    --  107.75  38.00 164.00  124
  5  ω    105.00 165.00   0.50    4.30    --  107.75 113.00  22.00  120
  6  ω   -111.00 -73.00   0.50    1.10    --  -46.91-125.00   0.00   76
  7  ω    -22.00  28.00   0.50    1.10    --  -46.91  19.00-120.00  100
  8  ω   -111.00 -77.00   0.50    1.10    --  -46.91-125.00 -30.00   68
  9  ω     38.00  64.00   0.50    4.30    --  107.75 -61.00 -30.00   52
 10  ω     40.00  66.00   0.50    4.30    --  107.75 -61.00-180.00   52
 11  ω     37.00  66.00   0.50    4.30    --  107.75 -95.00  90.00   58
 12  ω     37.00  63.00   0.50    4.30    --  107.75 -61.00   0.00   52
 13  ω     36.00  70.00   0.50    4.30    --  107.75 -61.00 -90.00   68
 14  ω     77.00 102.00   0.50    4.30    --  107.75 -77.00-180.00   50
 15  ω     36.00  61.00   0.50    4.30    --  107.75 -61.00 -60.00   50
 16  ω     36.00  61.00   0.50    4.30    --  107.75 -61.00-150.00   50
 17  ω    102.00 167.00   0.50    4.30    --  107.75  30.00  30.00  130
 18  ω     67.00  92.00   0.50    4.30    --  107.75 -95.00  90.00   50
 19  ω     35.00  63.00   0.50    4.30    --  107.75 -77.00-180.00   56
 20  ω     86.00 133.00   0.50    4.30    --  107.75 -87.00-177.00   94
 21  ω     97.00 148.00   0.50    4.30    --  107.75 125.00   0.00  102
 22  ω     38.00  64.00   0.50    4.30    --  107.75 -77.00   0.00   52
 23  ω     37.00  63.00   0.50    4.30    --  107.75 -87.00-177.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3040
_reflns_number_total             3389
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0479P)²+2.2125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1024
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C5(H5), C6(H6), C10(H10), C13(H13), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.53172(2) 0.65908(3) 0.70060(2) 0.02376(12) Uani 1 1 d . . . . .
O1 O 0.41485(10) 0.55113(13) 0.70734(6) 0.0257(3) Uani 1 1 d . . . . .
O2 O 0.60255(11) 0.77958(13) 0.66147(6) 0.0296(3) Uani 1 1 d . . . . .
O4 O 0.51155(11) 0.71395(14) 0.77569(6) 0.0314(3) Uani 1 1 d . . . . .
O3 O 0.62221(12) 0.56704(16) 0.70908(8) 0.0393(4) Uani 1 1 d . . . . .
N1 N 0.41173(12) 0.53188(14) 0.60135(7) 0.0232(3) Uani 1 1 d . . . . .
N2 N 0.49511(12) 0.60832(14) 0.60820(7) 0.0222(3) Uani 1 1 d . . . . .
N3 N 0.11474(12) 0.28700(14) 0.67962(7) 0.0251(3) Uani 1 1 d . . . . .
C2 C 0.28544(14) 0.43219(16) 0.66332(8) 0.0227(4) Uani 1 1 d . . . . .
C1 C 0.37632(14) 0.50953(16) 0.65671(9) 0.0229(4) Uani 1 1 d . . . . .
C3 C 0.20970(15) 0.42307(18) 0.61773(9) 0.0260(4) Uani 1 1 d . . . . .
H3 H 0.215465 0.465501 0.580180 0.031 Uiso 1 1 calc R U . . .
C4 C 0.12605(15) 0.35100(18) 0.62834(9) 0.0268(4) Uani 1 1 d . . . . .
H4 H 0.073805 0.346656 0.597577 0.032 Uiso 1 1 calc R U . . .
C7 C 0.54209(14) 0.63870(17) 0.55797(9) 0.0238(4) Uani 1 1 d . . . . .
H7 H 0.519292 0.606186 0.519946 0.029 Uiso 1 1 calc R U . . .
C8 C 0.62707(14) 0.71918(18) 0.55674(9) 0.0255(4) Uani 1 1 d . . . . .
C9 C 0.65537(14) 0.78608(18) 0.60860(9) 0.0270(4) Uani 1 1 d . . . . .
C5 C 0.18842(16) 0.29619(19) 0.72286(9) 0.0295(4) Uani 1 1 d . . . . .
H5 H 0.182084 0.250412 0.759247 0.035 Uiso 1 1 calc R U . . .
C6 C 0.27297(15) 0.36852(19) 0.71740(9) 0.0281(4) Uani 1 1 d . . . . .
H6 H 0.321776 0.374649 0.750038 0.034 Uiso 1 1 calc R U . . .
C10 C 0.73674(17) 0.8656(2) 0.60391(11) 0.0355(5) Uani 1 1 d . . . . .
H10 H 0.756878 0.910562 0.638745 0.043 Uiso 1 1 calc R U . . .
C13 C 0.68034(17) 0.7355(2) 0.50069(10) 0.0327(4) Uani 1 1 d . . . . .
H13 H 0.660890 0.691581 0.465323 0.039 Uiso 1 1 calc R U . . .
C11 C 0.78773(19) 0.8781(2) 0.54800(12) 0.0422(6) Uani 1 1 d . . . . .
H11 H 0.843066 0.932111 0.545034 0.051 Uiso 1 1 calc R U . . .
C12 C 0.76029(19) 0.8142(2) 0.49638(11) 0.0399(5) Uani 1 1 d . . . . .
H12 H 0.796115 0.824342 0.458426 0.048 Uiso 1 1 calc R U . . .
C14 C 0.53383(19) 0.6790(3) 0.83703(11) 0.0446(6) Uani 1 1 d . . . . .
H14A H 0.546820 0.748918 0.862686 0.054 Uiso 1 1 calc R U . . .
H14B H 0.597353 0.631090 0.837188 0.054 Uiso 1 1 calc R U . . .
C16 C 0.4611(2) 0.5918(3) 0.93366(12) 0.0491(6) Uani 1 1 d . . . . .
H16A H 0.529516 0.558509 0.941517 0.074 Uiso 1 1 calc R U . . .
H16B H 0.407845 0.538286 0.948759 0.074 Uiso 1 1 calc R U . . .
H16C H 0.454906 0.666532 0.955227 0.074 Uiso 1 1 calc R U . . .
C15 C 0.4472(2) 0.6107(3) 0.86463(12) 0.0517(7) Uani 1 1 d . . . . .
H15A H 0.442781 0.534098 0.843763 0.062 Uiso 1 1 calc R U . . .
H15B H 0.381386 0.652320 0.857302 0.062 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 O1 1.9619(14) . ?
V1 O2 1.8636(15) . ?
V1 O4 1.7612(15) . ?
V1 O3 1.5889(16) . ?
V1 N2 2.1345(16) . ?
V1 N3 2.4417(16) 8_665 ?
O1 C1 1.294(2) . ?
O2 C9 1.334(2) . ?
O4 C14 1.416(3) . ?
N1 N2 1.400(2) . ?
N1 C1 1.307(2) . ?
N2 C7 1.293(2) . ?
N3 C4 1.339(3) . ?
N3 C5 1.340(3) . ?
C2 C1 1.482(3) . ?
C2 C3 1.395(3) . ?
C2 C6 1.389(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(3) . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.438(3) . ?
C8 C9 1.408(3) . ?
C8 C13 1.407(3) . ?
C9 C10 1.398(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(3) . ?
C6 H6 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.385(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.378(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(4) . ?
C12 H12 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.494(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 C15 1.519(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?

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 N2 74.07(6) . . ?
O1 V1 N3 78.17(6) . 8_665 ?
O2 V1 O1 151.98(6) . . ?
O2 V1 N2 83.53(6) . . ?
O2 V1 N3 81.43(6) . 8_665 ?
O4 V1 O1 92.48(6) . . ?
O4 V1 O2 103.04(7) . . ?
O4 V1 N2 158.08(7) . . ?
O4 V1 N3 80.83(6) . 8_665 ?
O3 V1 O1 98.04(8) . . ?
O3 V1 O2 100.58(8) . . ?
O3 V1 O4 103.94(8) . . ?
O3 V1 N2 95.17(7) . . ?
O3 V1 N3 174.12(7) . 8_665 ?
N2 V1 N3 79.51(6) . 8_665 ?
C1 O1 V1 117.89(12) . . ?
C9 O2 V1 133.07(13) . . ?
C14 O4 V1 137.09(17) . . ?
C1 N1 N2 107.27(15) . . ?
N1 N2 V1 116.22(11) . . ?
C7 N2 V1 127.46(13) . . ?
C7 N2 N1 116.32(16) . . ?
C4 N3 V1 124.71(13) . 8_655 ?
C4 N3 C5 117.18(17) . . ?
C5 N3 V1 118.10(13) . 8_655 ?
C3 C2 C1 122.38(17) . . ?
C6 C2 C1 119.31(16) . . ?
C6 C2 C3 118.29(18) . . ?
O1 C1 N1 124.52(17) . . ?
O1 C1 C2 116.49(16) . . ?
N1 C1 C2 118.99(16) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.61(18) . . ?
C4 C3 H3 120.7 . . ?
N3 C4 C3 123.50(18) . . ?
N3 C4 H4 118.2 . . ?
C3 C4 H4 118.2 . . ?
N2 C7 H7 118.3 . . ?
N2 C7 C8 123.32(18) . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 122.38(17) . . ?
C13 C8 C7 118.48(18) . . ?
C13 C8 C9 119.07(19) . . ?
O2 C9 C8 121.23(17) . . ?
O2 C9 C10 119.02(19) . . ?
C10 C9 C8 119.66(19) . . ?
N3 C5 H5 118.2 . . ?
N3 C5 C6 123.57(18) . . ?
C6 C5 H5 118.2 . . ?
C2 C6 H6 120.6 . . ?
C5 C6 C2 118.78(18) . . ?
C5 C6 H6 120.6 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(2) . . ?
C11 C10 H10 120.3 . . ?
C8 C13 H13 119.5 . . ?
C12 C13 C8 120.9(2) . . ?
C12 C13 H13 119.5 . . ?
C10 C11 H11 119.1 . . ?
C12 C11 C10 121.8(2) . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
O4 C14 H14A 109.3 . . ?
O4 C14 H14B 109.3 . . ?
O4 C14 C15 111.72(19) . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
C14 C15 C16 112.2(2) . . ?
C14 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?

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 O1 C1 N1 2.0(2) . . . . ?
V1 O1 C1 C2 -177.54(12) . . . . ?
V1 O2 C9 C8 32.7(3) . . . . ?
V1 O2 C9 C10 -150.82(16) . . . . ?
V1 O4 C14 C15 -91.8(3) . . . . ?
V1 N2 C7 C8 -3.1(3) . . . . ?
V1 N3 C4 C3 179.78(15) 8_655 . . . ?
V1 N3 C5 C6 -177.68(17) 8_655 . . . ?
O1 V1 O2 C9 -71.6(2) . . . . ?
O1 V1 O4 C14 79.6(2) . . . . ?
O2 V1 O4 C14 -123.9(2) . . . . ?
O2 C9 C10 C11 -175.9(2) . . . . ?
O4 V1 O2 C9 166.39(17) . . . . ?
O4 C14 C15 C16 -169.4(2) . . . . ?
O3 V1 O2 C9 59.24(18) . . . . ?
O3 V1 O4 C14 -19.3(2) . . . . ?
N1 N2 C7 C8 178.08(17) . . . . ?
N2 V1 O2 C9 -34.84(17) . . . . ?
N2 V1 O4 C14 130.7(2) . . . . ?
N2 N1 C1 O1 -0.9(2) . . . . ?
N2 N1 C1 C2 178.60(15) . . . . ?
N2 C7 C8 C9 -10.7(3) . . . . ?
N2 C7 C8 C13 172.54(19) . . . . ?
N3 V1 O2 C9 -115.16(18) 8_665 . . . ?
N3 V1 O4 C14 157.2(2) 8_665 . . . ?
N3 C5 C6 C2 -2.7(3) . . . . ?
C2 C3 C4 N3 -1.6(3) . . . . ?
C1 N1 N2 V1 -0.45(18) . . . . ?
C1 N1 N2 C7 178.54(17) . . . . ?
C1 C2 C3 C4 -178.38(18) . . . . ?
C1 C2 C6 C5 -179.57(19) . . . . ?
C3 C2 C1 O1 150.49(18) . . . . ?
C3 C2 C1 N1 -29.1(3) . . . . ?
C3 C2 C6 C5 2.2(3) . . . . ?
C4 N3 C5 C6 1.0(3) . . . . ?
C7 C8 C9 O2 -1.5(3) . . . . ?
C7 C8 C9 C10 -177.98(19) . . . . ?
C7 C8 C13 C12 178.0(2) . . . . ?
C8 C9 C10 C11 0.6(3) . . . . ?
C8 C13 C12 C11 -0.3(4) . . . . ?
C9 C8 C13 C12 1.1(3) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C5 N3 C4 C3 1.2(3) . . . . ?
C6 C2 C1 O1 -27.7(3) . . . . ?
C6 C2 C1 N1 152.73(18) . . . . ?
C6 C2 C3 C4 -0.2(3) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C13 C8 C9 O2 175.29(19) . . . . ?
C13 C8 C9 C10 -1.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_exp_2986_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2367533'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](1-pentoxo)oxovanadium(v)"
_chemical_formula_moiety         'C35.667 H28.5 N6 O8 V2'
_chemical_formula_sum            'C35.67 H28.50 N6 O8 V2'
_chemical_formula_weight         771.03
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_H-M_alt        'I b c a'
_space_group_name_Hall           '-I 2b 2c'
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'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'

# start Validation Reply Form
_vrf_PLAT213_exp_2986_twin1_hklf4 
;
PROBLEM: Atom C21             has ADP max/min Ratio .....        4.3 prolat
RESPONSE: The pentoxy chain is in severe disorder.
;
_vrf_PLAT241_exp_2986_twin1_hklf4 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C19A Check 
RESPONSE: The pentoxy chain is in severe disorder.
;
_vrf_PLAT430_exp_2986_twin1_hklf4 
;
PROBLEM: Short Inter D...A Contact  O1       ..N3A      .       2.86 Ang.  
RESPONSE: Polymeric chain with V-py coordination bond.
;
# end Validation Reply Form

_cell_length_a                   21.2703(3)
_cell_length_b                   29.7362(4)
_cell_length_c                   22.5536(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14265.1(4)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    33047
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      77.758
_cell_measurement_theta_min      4.123
_shelx_estimated_absorpt_T_max   0.908
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    4.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33047
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.758
_diffrn_reflns_theta_min         4.123
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5571
_reflns_number_total             7431
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1305P)²+16.8622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2074
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Restrained distances
 C17A-C16A
 1.5 with sigma of 0.02
 C19A-C17A
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 C20-C21
 1.5 with sigma of 0.02
 C17-C18
 1.5 with sigma of 0.02
 C14-C19
 1.5 with sigma of 0.02
 C18-C17 \\sim C16-C15 \\sim C14-C19 \\sim C20-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C20 \\sim C21: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C18A) = Uanis(C17A)
Uanis(C19) = Uanis(C14)
4. Others
 Fixed Sof: H16C(0.5) H16D(0.5) H16A(0.5) H16B(0.5) C15(0.6666) H19D(0.5)
 H19E(0.5) H19F(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C16(0.6666) C17(0.6666)
 C18A(0.5) H18A(0.5) H18B(0.5) C18(0.6666) C17A(0.5) H17A(0.5) C21(0.3334)
 C20(0.3334) C19(0.3334)
5.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C15A(H15A,H15B), C16A(H16C,H16D), C16A(H16A,H16B), C18A(H18A,
 H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C6A(H6A), C3A(H3A), C5A(H5A), C6(H6), C4(H4), C5(H5), C4A(H4A),
 C3(H3), C13A(H13A), C7(H7), C11A(H11A), C10A(H10A), C12A(H12A), C10(H10),
 C13(H13), C11(H11), C12(H12), C17A(H17A)
5.c Idealised Me refined as rotating group:
 C19A(H19D,H19E,H19F), C19A(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.34108(3) 0.78653(2) 0.15127(3) 0.03399(19) Uani 1 1 d . . . . .
V1 V 0.56259(4) 0.56931(2) 0.36518(3) 0.0486(2) Uani 1 1 d . . . . .
O1A O 0.39611(12) 0.74840(8) 0.20052(11) 0.0351(5) Uani 1 1 d . . . . .
O4A O 0.40236(12) 0.82132(9) 0.12429(11) 0.0387(6) Uani 1 1 d . . . . .
O2A O 0.27926(12) 0.79347(9) 0.09350(12) 0.0408(6) Uani 1 1 d . . . . .
O1 O 0.58509(14) 0.62330(10) 0.41104(12) 0.0483(7) Uani 1 1 d . . . . .
O3A O 0.31359(15) 0.81716(9) 0.20280(13) 0.0476(7) Uani 1 1 d . . . . .
N2A N 0.28437(14) 0.73067(10) 0.17659(13) 0.0353(6) Uani 1 1 d . . . . .
N3 N 0.62058(14) 0.73200(10) 0.57868(13) 0.0352(6) Uani 1 1 d . . . . .
N1A N 0.31453(15) 0.69778(10) 0.21121(14) 0.0380(7) Uani 1 1 d . . . . .
O2 O 0.50435(18) 0.53069(10) 0.33106(14) 0.0609(9) Uani 1 1 d . . . . .
N3A N 0.49251(16) 0.62293(10) 0.31909(13) 0.0408(7) Uani 1 1 d . . . . .
O4 O 0.61153(18) 0.58474(13) 0.30513(15) 0.0681(10) Uani 1 1 d . . . . .
O3 O 0.60280(18) 0.53275(12) 0.39994(16) 0.0672(10) Uani 1 1 d . . . . .
N2 N 0.49631(17) 0.57256(10) 0.43507(14) 0.0433(8) Uani 1 1 d . . . . .
N1 N 0.50338(17) 0.60844(11) 0.47436(14) 0.0422(7) Uani 1 1 d . . . . .
C1A C 0.37198(18) 0.71091(11) 0.22063(15) 0.0349(7) Uani 1 1 d . . . . .
C2A C 0.41391(18) 0.68103(11) 0.25545(16) 0.0357(7) Uani 1 1 d . . . . .
C7A C 0.22548(18) 0.72569(12) 0.16833(17) 0.0380(8) Uani 1 1 d . . . . .
H7A H 0.205014 0.700969 0.186742 0.046 Uiso 1 1 calc R U . . .
C2 C 0.57400(18) 0.66806(12) 0.49801(16) 0.0377(8) Uani 1 1 d . . . . .
C6A C 0.47830(19) 0.68668(12) 0.25548(17) 0.0391(8) Uani 1 1 d . . . . .
H6A H 0.496907 0.710492 0.233549 0.047 Uiso 1 1 calc R U . . .
C3A C 0.38888(19) 0.64548(12) 0.28872(16) 0.0395(8) Uani 1 1 d . . . . .
H3A H 0.344822 0.640363 0.290283 0.047 Uiso 1 1 calc R U . . .
C8A C 0.18807(18) 0.75611(13) 0.13199(17) 0.0388(8) Uani 1 1 d . . . . .
C1 C 0.55166(19) 0.63125(13) 0.45807(17) 0.0403(8) Uani 1 1 d . . . . .
C5A C 0.51556(19) 0.65740(13) 0.28771(17) 0.0414(8) Uani 1 1 d . . . . .
H5A H 0.559762 0.661988 0.287554 0.050 Uiso 1 1 calc R U . . .
C9A C 0.21700(17) 0.78882(12) 0.09592(16) 0.0364(8) Uani 1 1 d . . . . .
C6 C 0.6329(2) 0.68584(13) 0.49178(16) 0.0411(8) Uani 1 1 d . . . . .
H6 H 0.658997 0.676606 0.459806 0.049 Uiso 1 1 calc R U . . .
C4 C 0.56284(19) 0.71484(13) 0.58346(18) 0.0414(8) Uani 1 1 d . . . . .
H4 H 0.537373 0.724726 0.615511 0.050 Uiso 1 1 calc R U . . .
C5 C 0.65488(19) 0.71778(13) 0.53272(17) 0.0419(8) Uani 1 1 d . . . . .
H5 H 0.695898 0.729790 0.527511 0.050 Uiso 1 1 calc R U . . .
C4A C 0.4303(2) 0.61803(13) 0.31922(17) 0.0426(9) Uani 1 1 d . . . . .
H4A H 0.413175 0.594029 0.341834 0.051 Uiso 1 1 calc R U . . .
C3 C 0.53771(19) 0.68361(14) 0.54476(18) 0.0427(8) Uani 1 1 d . . . . .
H3 H 0.496016 0.672906 0.550148 0.051 Uiso 1 1 calc R U . . .
C13A C 0.12258(19) 0.75127(14) 0.13028(18) 0.0442(9) Uani 1 1 d . . . . .
H13A H 0.103094 0.728693 0.153736 0.053 Uiso 1 1 calc R U . . .
C7 C 0.4578(2) 0.54167(14) 0.44918(18) 0.0490(10) Uani 1 1 d . . . . .
H7 H 0.434204 0.545077 0.484681 0.059 Uiso 1 1 calc R U . . .
C11A C 0.1151(2) 0.81020(15) 0.0589(2) 0.0498(10) Uani 1 1 d . . . . .
H11A H 0.090279 0.828547 0.033574 0.060 Uiso 1 1 calc R U . . .
C10A C 0.1793(2) 0.81518(14) 0.05913(19) 0.0469(9) Uani 1 1 d . . . . .
H10A H 0.198238 0.836865 0.033906 0.056 Uiso 1 1 calc R U . . .
C12A C 0.0859(2) 0.77868(15) 0.0952(2) 0.0490(10) Uani 1 1 d . . . . .
H12A H 0.041390 0.776088 0.095760 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4723(2) 0.49722(14) 0.3568(2) 0.0561(12) Uani 1 1 d . . . . .
C8 C 0.4479(2) 0.50149(15) 0.4139(2) 0.0555(11) Uani 1 1 d . . . . .
C10 C 0.4620(3) 0.45765(16) 0.3240(3) 0.0693(15) Uani 1 1 d . . . . .
H10 H 0.479172 0.454470 0.285304 0.083 Uiso 1 1 calc R U . . .
C13 C 0.4126(3) 0.46624(16) 0.4369(2) 0.0661(14) Uani 1 1 d . . . . .
H13 H 0.395489 0.469007 0.475623 0.079 Uiso 1 1 calc R U . . .
C11 C 0.4270(3) 0.42388(17) 0.3483(3) 0.080(2) Uani 1 1 d . . . . .
H11 H 0.419623 0.397315 0.325950 0.096 Uiso 1 1 calc R U . . .
C12 C 0.4019(3) 0.42752(16) 0.4053(3) 0.0766(18) Uani 1 1 d . . . . .
H12 H 0.377824 0.403705 0.421832 0.092 Uiso 1 1 calc R U . . .
C14A C 0.4194(2) 0.86563(14) 0.1439(2) 0.0464(9) Uani 1 1 d . . . . .
H14A H 0.465631 0.867472 0.148155 0.056 Uiso 1 1 calc R U . . .
H14B H 0.400426 0.871327 0.183303 0.056 Uiso 1 1 calc R U . . .
C15A C 0.3975(3) 0.90101(16) 0.1011(3) 0.0653(13) Uani 1 1 d . . . . .
H15A H 0.414378 0.930445 0.114012 0.078 Uiso 1 1 calc R U . . .
H15B H 0.415627 0.894341 0.061613 0.078 Uiso 1 1 calc R U . . .
C16A C 0.3284(4) 0.9050(2) 0.0948(5) 0.121(4) Uani 1 1 d D . . . .
H16C H 0.315859 0.879914 0.068500 0.145 Uiso 0.5 1 calc R U P A 1
H16D H 0.311166 0.897629 0.134448 0.145 Uiso 0.5 1 calc R U P A 1
H16A H 0.321848 0.916929 0.054330 0.145 Uiso 0.5 1 calc R U P B -1
H16B H 0.312956 0.873592 0.093903 0.145 Uiso 0.5 1 calc R U P B -1
C15 C 0.7191(5) 0.5929(3) 0.3038(4) 0.079(3) Uani 0.6666 1 d D . P C 1
C14 C 0.6665(5) 0.5621(3) 0.2890(4) 0.117(3) Uani 1 1 d D . . . .
C19A C 0.2249(4) 0.9413(3) 0.0893(6) 0.165(6) Uani 1 1 d D . . . .
H19D H 0.210321 0.910009 0.088885 0.247 Uiso 0.5 1 calc R U P D 1
H19E H 0.201406 0.958667 0.059755 0.247 Uiso 0.5 1 calc R U P D 1
H19F H 0.217871 0.954206 0.128742 0.247 Uiso 0.5 1 calc R U P D 1
H19A H 0.217577 0.918762 0.058342 0.247 Uiso 0.5 1 calc R U P E -1
H19B H 0.231977 0.970712 0.070951 0.247 Uiso 0.5 1 calc R U P E -1
H19C H 0.188001 0.942878 0.115314 0.247 Uiso 0.5 1 calc R U P E -1
C16 C 0.7332(4) 0.6073(3) 0.3692(4) 0.080(2) Uani 0.6666 1 d D . P . .
C17 C 0.7472(5) 0.5675(3) 0.4120(5) 0.092(3) Uani 0.6666 1 d D . P C .
C18A C 0.2932(7) 0.9427(4) 0.0750(8) 0.092(3) Uani 0.5 1 d . . P F 1
H18A H 0.297935 0.945249 0.031441 0.111 Uiso 0.5 1 calc R U P F 1
H18B H 0.311370 0.970236 0.092824 0.111 Uiso 0.5 1 calc R U P F 1
C18 C 0.7574(7) 0.5819(5) 0.4759(5) 0.115(4) Uani 0.6666 1 d D . P . .
C17A C 0.2869(6) 0.9270(4) 0.1285(7) 0.092(3) Uani 0.5 1 d D . P F -1
H17A H 0.292494 0.933535 0.169370 0.111 Uiso 0.5 1 calc R U P F -1
C21 C 0.8251(8) 0.5135(5) 0.2355(11) 0.092(7) Uani 0.3334 1 d D U P C 2
C20 C 0.7865(6) 0.5550(5) 0.2560(9) 0.101(7) Uani 0.3334 1 d D U P C 2
C19 C 0.7272(8) 0.5437(8) 0.2775(12) 0.117(3) Uani 0.3334 1 d D U P C 2


_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 O1A 1.972(3) . ?
V1A O4A 1.772(3) . ?
V1A O2A 1.863(3) . ?
V1A O3A 1.588(3) . ?
V1A N2A 2.131(3) . ?
V1A N3 2.444(3) 16_654 ?
V1 O1 1.969(3) . ?
V1 O2 1.856(4) . ?
V1 N3A 2.418(3) . ?
V1 O4 1.769(4) . ?
V1 O3 1.590(3) . ?
V1 N2 2.117(4) . ?
O1A C1A 1.308(4) . ?
O4A C14A 1.436(5) . ?
O2A C9A 1.333(5) . ?
O1 C1 1.299(5) . ?
N2A N1A 1.406(4) . ?
N2A C7A 1.275(5) . ?
N3 C4 1.334(5) . ?
N3 C5 1.337(5) . ?
N1A C1A 1.301(5) . ?
O2 C9 1.338(6) . ?
N3A C5A 1.339(5) . ?
N3A C4A 1.331(5) . ?
O4 C14 1.397(8) . ?
N2 N1 1.395(4) . ?
N2 C7 1.271(6) . ?
N1 C1 1.284(5) . ?
C1A C2A 1.484(5) . ?
C2A C6A 1.380(6) . ?
C2A C3A 1.401(5) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.457(5) . ?
C2 C1 1.495(5) . ?
C2 C6 1.368(6) . ?
C2 C3 1.386(5) . ?
C6A H6A 0.9500 . ?
C6A C5A 1.384(5) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.384(5) . ?
C8A C9A 1.409(5) . ?
C8A C13A 1.401(6) . ?
C5A H5A 0.9500 . ?
C9A C10A 1.395(5) . ?
C6 H6 0.9500 . ?
C6 C5 1.404(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.382(5) . ?
C5 H5 0.9500 . ?
C4A H4A 0.9500 . ?
C3 H3 0.9500 . ?
C13A H13A 0.9500 . ?
C13A C12A 1.378(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.451(6) . ?
C11A H11A 0.9500 . ?
C11A C10A 1.373(6) . ?
C11A C12A 1.390(7) . ?
C10A H10A 0.9500 . ?
C12A H12A 0.9500 . ?
C9 C8 1.394(7) . ?
C9 C10 1.407(6) . ?
C8 C13 1.390(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.365(9) . ?
C13 H13 0.9500 . ?
C13 C12 1.374(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(10) . ?
C12 H12 0.9500 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C14A C15A 1.503(6) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15A C16A 1.481(9) . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C16A C18A 1.422(13) . ?
C16A C17A 1.335(14) . ?
C15 C14 1.483(14) . ?
C15 C16 1.564(11) . ?
C14 C19 1.428(12) . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C19A C18A 1.489(18) . ?
C19A C17A 1.644(13) . ?
C16 C17 1.556(14) . ?
C17 C18 1.520(11) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C18A C17A 1.30(2) . ?
C18 C18 1.13(2) 7_645 ?
C17A H17A 0.9500 . ?
C21 C21 1.04(5) 8_455 ?
C21 C20 1.553(12) . ?
C20 C19 1.391(16) . ?

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
O1A V1A N2A 74.75(11) . . ?
O1A V1A N3 78.34(10) . 16_654 ?
O4A V1A O1A 95.30(11) . . ?
O4A V1A O2A 102.38(12) . . ?
O4A V1A N2A 164.51(12) . . ?
O4A V1A N3 84.94(11) . 16_654 ?
O2A V1A O1A 151.25(11) . . ?
O2A V1A N2A 82.77(12) . . ?
O2A V1A N3 80.83(11) . 16_654 ?
O3A V1A O1A 97.82(13) . . ?
O3A V1A O4A 100.79(14) . . ?
O3A V1A O2A 100.86(14) . . ?
O3A V1A N2A 92.44(13) . . ?
O3A V1A N3 173.44(12) . 16_654 ?
N2A V1A N3 81.45(11) . 16_654 ?
O1 V1 N3A 80.67(11) . . ?
O1 V1 N2 74.54(13) . . ?
O2 V1 O1 152.19(14) . . ?
O2 V1 N3A 79.53(13) . . ?
O2 V1 N2 83.83(15) . . ?
O4 V1 O1 92.73(16) . . ?
O4 V1 O2 103.64(18) . . ?
O4 V1 N3A 82.10(14) . . ?
O4 V1 N2 161.85(15) . . ?
O3 V1 O1 99.66(17) . . ?
O3 V1 O2 98.07(18) . . ?
O3 V1 N3A 174.05(17) . . ?
O3 V1 O4 103.79(19) . . ?
O3 V1 N2 91.28(16) . . ?
N2 V1 N3A 83.08(12) . . ?
C1A O1A V1A 116.9(2) . . ?
C14A O4A V1A 128.0(3) . . ?
C9A O2A V1A 131.4(2) . . ?
C1 O1 V1 116.4(3) . . ?
N1A N2A V1A 115.6(2) . . ?
C7A N2A V1A 127.4(3) . . ?
C7A N2A N1A 116.6(3) . . ?
C4 N3 V1A 120.5(2) . 16_655 ?
C4 N3 C5 116.4(3) . . ?
C5 N3 V1A 123.2(3) . 16_655 ?
C1A N1A N2A 108.1(3) . . ?
C9 O2 V1 128.3(3) . . ?
C5A N3A V1 120.4(3) . . ?
C4A N3A V1 122.7(3) . . ?
C4A N3A C5A 116.7(3) . . ?
C14 O4 V1 124.5(4) . . ?
N1 N2 V1 115.9(3) . . ?
C7 N2 V1 125.6(3) . . ?
C7 N2 N1 117.6(4) . . ?
C1 N1 N2 108.0(3) . . ?
O1A C1A C2A 117.3(3) . . ?
N1A C1A O1A 124.6(3) . . ?
N1A C1A C2A 118.1(3) . . ?
C6A C2A C1A 121.6(3) . . ?
C6A C2A C3A 117.9(3) . . ?
C3A C2A C1A 120.5(3) . . ?
N2A C7A H7A 118.4 . . ?
N2A C7A C8A 123.1(3) . . ?
C8A C7A H7A 118.4 . . ?
C6 C2 C1 120.8(3) . . ?
C6 C2 C3 117.4(4) . . ?
C3 C2 C1 121.7(4) . . ?
C2A C6A H6A 120.3 . . ?
C2A C6A C5A 119.5(4) . . ?
C5A C6A H6A 120.3 . . ?
C2A C3A H3A 121.0 . . ?
C4A C3A C2A 118.0(4) . . ?
C4A C3A H3A 121.0 . . ?
C9A C8A C7A 121.0(3) . . ?
C13A C8A C7A 119.7(4) . . ?
C13A C8A C9A 119.3(4) . . ?
O1 C1 C2 116.8(4) . . ?
N1 C1 O1 125.1(4) . . ?
N1 C1 C2 117.9(3) . . ?
N3A C5A C6A 123.3(4) . . ?
N3A C5A H5A 118.3 . . ?
C6A C5A H5A 118.3 . . ?
O2A C9A C8A 121.9(3) . . ?
O2A C9A C10A 119.3(3) . . ?
C10A C9A C8A 118.7(4) . . ?
C2 C6 H6 120.1 . . ?
C2 C6 C5 119.9(4) . . ?
C5 C6 H6 120.1 . . ?
N3 C4 H4 117.9 . . ?
N3 C4 C3 124.2(4) . . ?
C3 C4 H4 117.9 . . ?
N3 C5 C6 122.9(4) . . ?
N3 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
N3A C4A C3A 124.6(4) . . ?
N3A C4A H4A 117.7 . . ?
C3A C4A H4A 117.7 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.4 . . ?
C8A C13A H13A 119.4 . . ?
C12A C13A C8A 121.2(4) . . ?
C12A C13A H13A 119.4 . . ?
N2 C7 H7 118.3 . . ?
N2 C7 C8 123.4(4) . . ?
C8 C7 H7 118.3 . . ?
C10A C11A H11A 119.5 . . ?
C10A C11A C12A 121.0(4) . . ?
C12A C11A H11A 119.5 . . ?
C9A C10A H10A 119.5 . . ?
C11A C10A C9A 120.9(4) . . ?
C11A C10A H10A 119.5 . . ?
C13A C12A C11A 118.9(4) . . ?
C13A C12A H12A 120.5 . . ?
C11A C12A H12A 120.5 . . ?
O2 C9 C8 121.5(4) . . ?
O2 C9 C10 118.3(5) . . ?
C8 C9 C10 120.2(5) . . ?
C9 C8 C7 121.9(5) . . ?
C13 C8 C7 119.6(5) . . ?
C13 C8 C9 118.5(4) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.3(6) . . ?
C11 C10 H10 120.4 . . ?
C8 C13 H13 119.1 . . ?
C12 C13 C8 121.9(6) . . ?
C12 C13 H13 119.1 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.5(5) . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 118.6(6) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
O4A C14A H14A 109.3 . . ?
O4A C14A H14B 109.3 . . ?
O4A C14A C15A 111.5(4) . . ?
H14A C14A H14B 108.0 . . ?
C15A C14A H14A 109.3 . . ?
C15A C14A H14B 109.3 . . ?
C14A C15A H15A 108.5 . . ?
C14A C15A H15B 108.5 . . ?
H15A C15A H15B 107.5 . . ?
C16A C15A C14A 115.1(5) . . ?
C16A C15A H15A 108.5 . . ?
C16A C15A H15B 108.5 . . ?
C15A C16A H16C 105.3 . . ?
C15A C16A H16D 105.3 . . ?
C15A C16A H16A 104.8 . . ?
C15A C16A H16B 104.8 . . ?
H16C C16A H16D 106.0 . . ?
H16C C16A H16A 71.2 . . ?
H16C C16A H16B 35.7 . . ?
H16D C16A H16A 149.3 . . ?
H16D C16A H16B 71.8 . . ?
H16A C16A H16B 105.8 . . ?
C18A C16A C15A 128.0(9) . . ?
C18A C16A H16C 105.3 . . ?
C18A C16A H16D 105.3 . . ?
C18A C16A H16A 49.6 . . ?
C18A C16A H16B 124.3 . . ?
C17A C16A C15A 129.9(8) . . ?
C17A C16A H16C 122.2 . . ?
C17A C16A H16D 49.6 . . ?
C17A C16A H16A 104.8 . . ?
C17A C16A H16B 104.8 . . ?
C17A C16A C18A 56.2(9) . . ?
C14 C15 C16 121.7(7) . . ?
O4 C14 C15 106.0(7) . . ?
O4 C14 C19 171.9(14) . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19D C19A H19A 45.1 . . ?
H19D C19A H19B 153.1 . . ?
H19D C19A H19C 78.4 . . ?
H19E C19A H19F 109.5 . . ?
H19E C19A H19A 78.2 . . ?
H19E C19A H19B 47.2 . . ?
H19E C19A H19C 88.5 . . ?
H19F C19A H19A 153.0 . . ?
H19F C19A H19B 93.3 . . ?
H19F C19A H19C 46.9 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
C18A C19A H19A 91.1 . . ?
C18A C19A H19B 74.4 . . ?
C18A C19A H19C 155.3 . . ?
C18A C19A C17A 48.8(8) . . ?
C17A C19A H19D 90.8 . . ?
C17A C19A H19E 155.5 . . ?
C17A C19A H19F 74.7 . . ?
C17A C19A H19A 109.5 . . ?
C17A C19A H19B 109.5 . . ?
C17A C19A H19C 109.5 . . ?
C17 C16 C15 114.4(8) . . ?
C18 C17 C16 113.7(9) . . ?
C16A C18A C19A 115.0(12) . . ?
C16A C18A H18A 108.5 . . ?
C16A C18A H18B 108.5 . . ?
C19A C18A H18A 108.5 . . ?
C19A C18A H18B 108.5 . . ?
H18A C18A H18B 107.5 . . ?
C17A C18A C16A 58.5(8) . . ?
C17A C18A C19A 71.8(11) . . ?
C17A C18A H18A 163.2 . . ?
C17A C18A H18B 87.7 . . ?
C18 C18 C17 150.7(18) 7_645 . ?
C16A C17A C19A 110.6(10) . . ?
C16A C17A H17A 124.7 . . ?
C19A C17A H17A 124.7 . . ?
C18A C17A C16A 65.3(10) . . ?
C18A C17A C19A 59.4(9) . . ?
C18A C17A H17A 144.5 . . ?
C21 C21 C20 115(2) 8_455 . ?
C19 C20 C21 112.9(14) . . ?
C20 C19 C14 142.1(19) . . ?

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
V1A O1A C1A N1A -1.2(5) . . . . ?
V1A O1A C1A C2A 177.3(2) . . . . ?
V1A O4A C14A C15A -103.9(4) . . . . ?
V1A O2A C9A C8A -34.9(5) . . . . ?
V1A O2A C9A C10A 149.0(3) . . . . ?
V1A N2A N1A C1A 1.5(4) . . . . ?
V1A N2A C7A C8A 8.6(5) . . . . ?
V1A N3 C4 C3 -179.4(3) 16_655 . . . ?
V1A N3 C5 C6 178.8(3) 16_655 . . . ?
V1 O1 C1 N1 -4.6(5) . . . . ?
V1 O1 C1 C2 171.3(2) . . . . ?
V1 O2 C9 C8 39.8(6) . . . . ?
V1 O2 C9 C10 -142.2(4) . . . . ?
V1 N3A C5A C6A 173.5(3) . . . . ?
V1 N3A C4A C3A -173.6(3) . . . . ?
V1 O4 C14 C15 -110.4(6) . . . . ?
V1 N2 N1 C1 -1.3(4) . . . . ?
V1 N2 C7 C8 -8.6(6) . . . . ?
O1A V1A O4A C14A -100.8(3) . . . . ?
O1A V1A O2A C9A 78.4(4) . . . . ?
O1A C1A C2A C6A -14.6(5) . . . . ?
O1A C1A C2A C3A 166.5(3) . . . . ?
O4A V1A O2A C9A -155.0(3) . . . . ?
O4A C14A C15A C16A 64.6(6) . . . . ?
O2A V1A O4A C14A 102.0(3) . . . . ?
O2A C9A C10A C11A 177.7(4) . . . . ?
O1 V1 O2 C9 -82.8(5) . . . . ?
O1 V1 O4 C14 111.3(6) . . . . ?
O3A V1A O4A C14A -1.8(3) . . . . ?
O3A V1A O2A C9A -51.3(3) . . . . ?
N2A V1A O4A C14A -150.0(4) . . . . ?
N2A V1A O2A C9A 39.8(3) . . . . ?
N2A N1A C1A O1A -0.2(5) . . . . ?
N2A N1A C1A C2A -178.8(3) . . . . ?
N2A C7A C8A C9A 10.5(6) . . . . ?
N2A C7A C8A C13A -173.0(4) . . . . ?
N3 V1A O4A C14A -178.6(3) 16_654 . . . ?
N3 V1A O2A C9A 122.3(3) 16_654 . . . ?
N3 C4 C3 C2 0.9(6) . . . . ?
N1A N2A C7A C8A -178.0(3) . . . . ?
N1A C1A C2A C6A 164.1(3) . . . . ?
N1A C1A C2A C3A -14.8(5) . . . . ?
O2 V1 O4 C14 -91.4(6) . . . . ?
O2 C9 C8 C7 -2.3(7) . . . . ?
O2 C9 C8 C13 177.1(4) . . . . ?
O2 C9 C10 C11 -177.0(4) . . . . ?
N3A V1 O2 C9 -128.1(4) . . . . ?
N3A V1 O4 C14 -168.5(6) . . . . ?
O4 V1 O2 C9 152.8(4) . . . . ?
O3 V1 O2 C9 46.4(4) . . . . ?
O3 V1 O4 C14 10.6(7) . . . . ?
N2 V1 O2 C9 -44.0(4) . . . . ?
N2 V1 O4 C14 155.9(6) . . . . ?
N2 N1 C1 O1 3.8(5) . . . . ?
N2 N1 C1 C2 -172.1(3) . . . . ?
N2 C7 C8 C9 -10.9(7) . . . . ?
N2 C7 C8 C13 169.8(4) . . . . ?
N1 N2 C7 C8 -177.1(4) . . . . ?
C1A C2A C6A C5A -178.7(3) . . . . ?
C1A C2A C3A C4A 178.5(3) . . . . ?
C2A C6A C5A N3A 0.7(6) . . . . ?
C2A C3A C4A N3A -0.2(6) . . . . ?
C7A N2A N1A C1A -172.7(3) . . . . ?
C7A C8A C9A O2A -0.2(6) . . . . ?
C7A C8A C9A C10A 176.0(4) . . . . ?
C7A C8A C13A C12A -178.3(4) . . . . ?
C2 C6 C5 N3 0.2(6) . . . . ?
C6A C2A C3A C4A -0.4(5) . . . . ?
C3A C2A C6A C5A 0.2(5) . . . . ?
C8A C9A C10A C11A 1.5(6) . . . . ?
C8A C13A C12A C11A 3.0(6) . . . . ?
C1 C2 C6 C5 -174.8(3) . . . . ?
C1 C2 C3 C4 174.3(4) . . . . ?
C5A N3A C4A C3A 1.0(6) . . . . ?
C9A C8A C13A C12A -1.7(6) . . . . ?
C6 C2 C1 O1 -13.0(5) . . . . ?
C6 C2 C1 N1 163.2(4) . . . . ?
C6 C2 C3 C4 -1.9(6) . . . . ?
C4 N3 C5 C6 -1.3(6) . . . . ?
C5 N3 C4 C3 0.8(6) . . . . ?
C4A N3A C5A C6A -1.3(5) . . . . ?
C3 C2 C1 O1 170.9(3) . . . . ?
C3 C2 C1 N1 -12.8(5) . . . . ?
C3 C2 C6 C5 1.4(6) . . . . ?
C13A C8A C9A O2A -176.7(3) . . . . ?
C13A C8A C9A C10A -0.5(5) . . . . ?
C7 N2 N1 C1 168.3(4) . . . . ?
C7 C8 C13 C12 179.9(5) . . . . ?
C10A C11A C12A C13A -2.1(6) . . . . ?
C12A C11A C10A C9A -0.2(7) . . . . ?
C9 C8 C13 C12 0.6(7) . . . . ?
C9 C10 C11 C12 -0.7(8) . . . . ?
C8 C9 C10 C11 1.0(7) . . . . ?
C8 C13 C12 C11 -0.3(8) . . . . ?
C10 C9 C8 C7 179.7(4) . . . . ?
C10 C9 C8 C13 -0.9(7) . . . . ?
C10 C11 C12 C13 0.4(9) . . . . ?
C14A C15A C16A C18A 157.1(12) . . . . ?
C14A C15A C16A C17A 82.6(11) . . . . ?
C15A C16A C18A C19A -163.6(10) . . . . ?
C15A C16A C18A C17A -117.1(13) . . . . ?
C15A C16A C17A C19A 153.5(9) . . . . ?
C15A C16A C17A C18A 114.0(12) . . . . ?
C16A C18A C17A C19A -136.2(9) . . . . ?
C15 C16 C17 C18 -176.9(10) . . . . ?
C14 C15 C16 C17 58.6(12) . . . . ?
C19A C18A C17A C16A 136.2(9) . . . . ?
C16 C15 C14 O4 63.9(10) . . . . ?
C16 C17 C18 C18 115(2) . . . 7_645 ?
C18A C16A C17A C19A 39.5(9) . . . . ?
C18A C19A C17A C16A -42.2(10) . . . . ?
C17A C16A C18A C19A -46.5(12) . . . . ?
C17A C19A C18A C16A 40.6(10) . . . . ?
C21 C21 C20 C19 -46(3) 8_455 . . . ?
C21 C20 C19 C14 -160(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_4327
_database_code_depnum_ccdc_archive 'CCDC 2367536'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](methoxo)oxovanadium(v) methanol solvate"
_chemical_formula_moiety         'C28 H24 N6 O8 V2, 0.5[CH4O]'
_chemical_formula_sum            'C28.50 H26 N6 O8.50 V2'
_chemical_formula_weight         690.43
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_H-M_alt        'I b c a'
_space_group_name_Hall           '-I 2b 2c'
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'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
# start Validation Reply Form
_vrf_PLAT430_exp_4327            
;
PROBLEM: Short Inter D...A Contact  O1       ..N3A      .       2.82 Ang.  
RESPONSE: Polymer with V-py coordination bond.
;
# end Validation Reply Form
_cell_length_a                   22.0687(2)
_cell_length_b                   20.5886(2)
_cell_length_c                   26.8420(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12196.0(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    18194
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.9860
_cell_measurement_theta_min      3.2950
_shelx_estimated_absorpt_T_max   0.761
_shelx_estimated_absorpt_T_min   0.359
_exptl_absorpt_coefficient_mu    5.668
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 2 -1 0.0909
-2 -2 1 0.0780
1 -2 0 0.0994
-1 2 0 0.0955
0 0 -1 0.0270
0 0 1 0.0240
1 -1 0 0.0818

_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.051
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34430
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.725
_diffrn_reflns_theta_min         4.006
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -101.00 -34.00   0.50    1.00    --  -47.29 -63.00  -7.00  134
  2  ω    -74.00 -49.00   0.50    5.50    --  -86.25  64.00 -83.00   50
  3  ω     45.00  71.00   0.50    5.50    --  107.75-102.00 -96.00   52
  4  ω     36.00  70.00   0.50    5.50    --  107.75 -63.00  -7.00   68
  5  ω     92.00 175.00   0.50    5.50    --  107.75  63.00 129.00  166
  6  ω    126.00 151.00   0.50    5.50    --  107.75  64.00 -83.00   50
  7  ω     35.00  60.00   0.50    5.50    --  107.75 -64.00 140.00   50
  8  ω    -25.00  20.00   0.50    1.00    --  -47.29  19.00 -90.00   90
  9  ω   -115.00 -90.00   0.50    1.00    --  -47.29 -77.00 -60.00   50
 10  ω     89.00 119.00   0.50    1.00    --   47.29  77.00  60.00   60
 11  ω     80.00 111.00   0.50    5.50    --  107.75-125.00   0.00   62
 12  ω     37.00  63.00   0.50    5.50    --  107.75 -95.00  60.00   52
 13  ω     44.00  70.00   0.50    5.50    --  107.75 -61.00  30.00   52
 14  ω     54.00 111.00   0.50    5.50    --  107.75-125.00 -30.00  114
 15  ω     68.00 106.00   0.50    5.50    --  107.75-125.00-180.00   76
 16  ω    107.00 137.00   0.50    5.50    --  107.75 125.00 150.00   60
 17  ω     38.00 107.00   0.50    5.50    --  107.75-125.00-150.00  138
 18  ω     36.00  67.00   0.50    5.50    --  107.75 -61.00  60.00   62
 19  ω    133.00 167.00   0.50    5.50    --  107.75  30.00  60.00   68
 20  ω     39.00  67.00   0.50    5.50    --  107.75-125.00 -60.00   56
 21  ω     75.00 107.00   0.50    5.50    --  107.75-125.00 -60.00   64
 22  ω     97.00 122.00   0.50    5.50    --  107.75 125.00  30.00   50
 23  ω    142.00 176.00   0.50    5.50    --  107.75 125.00  30.00   68
 24  ω     35.00  60.00   0.50    5.50    --  107.75 -61.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5950
_reflns_number_total             6412
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+11.9058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C14A(0.75) H14D(0.75) H14E(0.75) H14F(0.75) C15A(0.25) H15A(0.25)
 H15B(0.25) H15C(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C6(H6), C3A(H3A), C4(H4), C3(H3), C4A(H4A), C5A(H5A),
 C13(H13), C7A(H7A), C6A(H6A), C10(H10), C12(H12), C11(H11), C13A(H13A),
 C11A(H11A), C10A(H10A), C12A(H12A)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15A(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.84490(2) 0.66087(2) 0.79792(2) 0.02415(9) Uani 1 1 d . . . . .
V1A V 0.62901(2) 0.44455(2) 0.54894(2) 0.03047(10) Uani 1 1 d . . . . .
O1 O 0.79325(5) 0.60748(6) 0.75435(5) 0.0265(2) Uani 1 1 d . . . . .
O2 O 0.90484(6) 0.72265(6) 0.80887(5) 0.0309(3) Uani 1 1 d . . . . .
O4 O 0.87308(6) 0.59401(6) 0.83276(5) 0.0302(3) Uani 1 1 d . . . . .
O1A O 0.58381(6) 0.41220(6) 0.60794(5) 0.0308(3) Uani 1 1 d . . . . .
O3 O 0.79348(6) 0.68796(7) 0.83393(5) 0.0344(3) Uani 1 1 d . . . . .
N2 N 0.82274(6) 0.72149(7) 0.73623(5) 0.0247(3) Uani 1 1 d . . . . .
O2A O 0.65920(6) 0.50921(8) 0.50818(6) 0.0405(3) Uani 1 1 d . . . . .
O4A O 0.69250(6) 0.39590(8) 0.56535(6) 0.0408(3) Uani 1 1 d . . . . .
O3A O 0.59539(7) 0.39968(8) 0.50922(6) 0.0417(3) Uani 1 1 d . . . . .
N1 N 0.78817(7) 0.69260(7) 0.69869(5) 0.0263(3) Uani 1 1 d . . . . .
N3A N 0.41741(7) 0.37338(7) 0.73464(6) 0.0268(3) Uani 1 1 d . . . . .
N2A N 0.55544(7) 0.50961(8) 0.55767(6) 0.0286(3) Uani 1 1 d . . . . .
N1A N 0.51420(6) 0.49396(7) 0.59514(6) 0.0286(3) Uani 1 1 d . . . . .
N3 N 0.67380(7) 0.51470(8) 0.61172(6) 0.0299(3) Uani 1 1 d . . . . .
C7 C 0.83691(8) 0.78163(8) 0.72953(7) 0.0269(3) Uani 1 1 d . . . . .
H7 H 0.821078 0.803334 0.701138 0.032 Uiso 1 1 calc R U . . .
C8 C 0.87544(8) 0.81751(9) 0.76283(7) 0.0273(4) Uani 1 1 d . . . . .
C2A C 0.49487(8) 0.41796(8) 0.65941(7) 0.0264(3) Uani 1 1 d . . . . .
C1 C 0.77561(7) 0.63357(9) 0.71238(6) 0.0251(3) Uani 1 1 d . . . . .
C9 C 0.90819(8) 0.78664(8) 0.80138(7) 0.0271(3) Uani 1 1 d . . . . .
C2 C 0.74003(8) 0.59252(8) 0.67776(7) 0.0260(3) Uani 1 1 d . . . . .
C1A C 0.53370(8) 0.44251(8) 0.61841(7) 0.0273(4) Uani 1 1 d . . . . .
C5 C 0.67353(8) 0.57970(9) 0.60807(7) 0.0308(4) Uani 1 1 d . . . . .
H5 H 0.650024 0.599002 0.582378 0.037 Uiso 1 1 calc R U . . .
C6 C 0.70562(8) 0.62013(9) 0.63968(7) 0.0276(3) Uani 1 1 d . . . . .
H6 H 0.704228 0.665925 0.635505 0.033 Uiso 1 1 calc R U . . .
C3A C 0.50192(8) 0.35640(9) 0.67970(7) 0.0297(4) Uani 1 1 d . . . . .
H3A H 0.533180 0.328410 0.668253 0.036 Uiso 1 1 calc R U . . .
C4 C 0.70673(8) 0.48859(9) 0.64851(7) 0.0310(4) Uani 1 1 d . . . . .
H4 H 0.707218 0.442660 0.651844 0.037 Uiso 1 1 calc R U . . .
C3 C 0.74016(8) 0.52530(9) 0.68202(7) 0.0299(4) Uani 1 1 d . . . . .
H3 H 0.762883 0.504694 0.707589 0.036 Uiso 1 1 calc R U . . .
C4A C 0.46259(8) 0.33647(9) 0.71695(7) 0.0297(4) Uani 1 1 d . . . . .
H4A H 0.467948 0.294338 0.730691 0.036 Uiso 1 1 calc R U . . .
C5A C 0.41138(9) 0.43250(9) 0.71461(8) 0.0333(4) Uani 1 1 d . . . . .
H5A H 0.379326 0.459304 0.726246 0.040 Uiso 1 1 calc R U . . .
C13 C 0.88304(9) 0.88489(9) 0.75601(8) 0.0326(4) Uani 1 1 d . . . . .
H13 H 0.861651 0.906318 0.730071 0.039 Uiso 1 1 calc R U . . .
C7A C 0.54124(9) 0.55975(10) 0.53133(7) 0.0319(4) Uani 1 1 d . . . . .
H7A H 0.503921 0.580999 0.538074 0.038 Uiso 1 1 calc R U . . .
C6A C 0.44888(9) 0.45677(9) 0.67813(8) 0.0336(4) Uani 1 1 d . . . . .
H6A H 0.443304 0.499657 0.665909 0.040 Uiso 1 1 calc R U . . .
C10 C 0.94772(9) 0.82273(10) 0.83114(8) 0.0337(4) Uani 1 1 d . . . . .
H10 H 0.970468 0.801803 0.856536 0.040 Uiso 1 1 calc R U . . .
C8A C 0.57917(9) 0.58518(10) 0.49214(7) 0.0358(4) Uani 1 1 d . . . . .
C12 C 0.92120(10) 0.92021(10) 0.78656(8) 0.0375(4) Uani 1 1 d . . . . .
H12 H 0.925130 0.965808 0.782182 0.045 Uiso 1 1 calc R U . . .
C9A C 0.63691(10) 0.55896(10) 0.48226(8) 0.0367(4) Uani 1 1 d . . . . .
C11 C 0.95378(9) 0.88875(10) 0.82370(8) 0.0376(4) Uani 1 1 d . . . . .
H11 H 0.980575 0.912984 0.844235 0.045 Uiso 1 1 calc R U . . .
C14 C 0.85800(11) 0.57453(12) 0.88208(8) 0.0434(5) Uani 1 1 d . . . . .
H14A H 0.850746 0.527579 0.882748 0.065 Uiso 1 1 calc R U . . .
H14B H 0.821326 0.597384 0.892885 0.065 Uiso 1 1 calc R U . . .
H14C H 0.891523 0.585214 0.904572 0.065 Uiso 1 1 calc R U . . .
C13A C 0.55877(11) 0.63940(12) 0.46514(8) 0.0430(5) Uani 1 1 d . . . . .
H13A H 0.519826 0.657020 0.471815 0.052 Uiso 1 1 calc R U . . .
C11A C 0.65192(13) 0.64132(13) 0.41971(9) 0.0516(6) Uani 1 1 d . . . . .
H11A H 0.676943 0.660682 0.395042 0.062 Uiso 1 1 calc R U . . .
C10A C 0.67301(12) 0.58783(12) 0.44569(9) 0.0483(6) Uani 1 1 d . . . . .
H10A H 0.712066 0.570740 0.438652 0.058 Uiso 1 1 calc R U . . .
C12A C 0.59487(12) 0.66729(12) 0.42897(9) 0.0500(6) Uani 1 1 d . . . . .
H12A H 0.580890 0.703792 0.410628 0.060 Uiso 1 1 calc R U . . .
C14A C 0.6964(2) 0.3252(2) 0.56454(19) 0.0587(10) Uani 0.75 1 d . . P A 1
H14D H 0.676466 0.307412 0.594178 0.088 Uiso 0.75 1 calc R U P A 1
H14E H 0.739102 0.311989 0.564340 0.088 Uiso 0.75 1 calc R U P A 1
H14F H 0.676358 0.308561 0.534565 0.088 Uiso 0.75 1 calc R U P A 1
C15A C 0.7151(6) 0.3422(7) 0.5439(5) 0.054(3) Uani 0.25 1 d . . P A -1
H15A H 0.681710 0.313942 0.533401 0.081 Uiso 0.25 1 calc R U P A -1
H15B H 0.740705 0.319055 0.567847 0.081 Uiso 0.25 1 calc R U P A -1
H15C H 0.739314 0.354431 0.514772 0.081 Uiso 0.25 1 calc R U P A -1


_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 1.9684(12) . ?
V1 O2 1.8586(13) . ?
V1 O4 1.7765(13) . ?
V1 O3 1.5914(13) . ?
V1 N2 2.1306(14) . ?
V1 N3A 2.4379(15) 15_565 ?
V1A O1A 1.9865(13) . ?
V1A O2A 1.8475(15) . ?
V1A O4A 1.7777(15) . ?
V1A O3A 1.5941(15) . ?
V1A N2A 2.1178(16) . ?
V1A N3 2.4296(16) . ?
O1 C1 1.307(2) . ?
O2 C9 1.335(2) . ?
O4 C14 1.423(2) . ?
O1A C1A 1.301(2) . ?
N2 N1 1.397(2) . ?
N2 C7 1.290(2) . ?
O2A C9A 1.332(3) . ?
O4A C14A 1.459(4) . ?
O4A C15A 1.342(12) . ?
N1 C1 1.300(2) . ?
N3A C4A 1.341(2) . ?
N3A C5A 1.337(2) . ?
N2A N1A 1.394(2) . ?
N2A C7A 1.290(3) . ?
N1A C1A 1.303(2) . ?
N3 C5 1.342(2) . ?
N3 C4 1.339(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.438(3) . ?
C8 C9 1.413(3) . ?
C8 C13 1.409(3) . ?
C2A C1A 1.484(2) . ?
C2A C3A 1.388(3) . ?
C2A C6A 1.386(3) . ?
C1 C2 1.481(2) . ?
C9 C10 1.397(3) . ?
C2 C6 1.395(3) . ?
C2 C3 1.389(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(3) . ?
C6 H6 0.9500 . ?
C3A H3A 0.9500 . ?
C3A C4A 1.386(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.387(3) . ?
C3 H3 0.9500 . ?
C4A H4A 0.9500 . ?
C5A H5A 0.9500 . ?
C5A C6A 1.376(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.382(3) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.443(3) . ?
C6A H6A 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.380(3) . ?
C8A C9A 1.409(3) . ?
C8A C13A 1.405(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.389(3) . ?
C9A C10A 1.397(3) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13A H13A 0.9500 . ?
C13A C12A 1.381(3) . ?
C11A H11A 0.9500 . ?
C11A C10A 1.384(4) . ?
C11A C12A 1.390(4) . ?
C10A H10A 0.9500 . ?
C12A H12A 0.9500 . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C14A C15A 0.774(13) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 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
O1 V1 N2 74.48(5) . . ?
O1 V1 N3A 78.73(5) . 15_565 ?
O2 V1 O1 152.64(6) . . ?
O2 V1 N2 83.41(6) . . ?
O2 V1 N3A 80.85(6) . 15_565 ?
O4 V1 O1 94.75(6) . . ?
O4 V1 O2 101.42(6) . . ?
O4 V1 N2 160.63(6) . . ?
O4 V1 N3A 85.00(6) . 15_565 ?
O3 V1 O1 98.26(7) . . ?
O3 V1 O2 99.88(7) . . ?
O3 V1 O4 101.63(7) . . ?
O3 V1 N2 95.92(6) . . ?
O3 V1 N3A 172.99(6) . 15_565 ?
N2 V1 N3A 77.20(5) . 15_565 ?
O1A V1A N2A 74.87(6) . . ?
O1A V1A N3 81.41(5) . . ?
O2A V1A O1A 153.48(6) . . ?
O2A V1A N2A 83.47(6) . . ?
O2A V1A N3 80.54(6) . . ?
O4A V1A O1A 90.54(7) . . ?
O4A V1A O2A 105.57(7) . . ?
O4A V1A N2A 158.93(7) . . ?
O4A V1A N3 80.93(6) . . ?
O3A V1A O1A 96.05(7) . . ?
O3A V1A O2A 100.91(8) . . ?
O3A V1A O4A 101.89(8) . . ?
O3A V1A N2A 94.80(7) . . ?
O3A V1A N3 176.26(7) . . ?
N2A V1A N3 81.91(6) . . ?
C1 O1 V1 117.06(11) . . ?
C9 O2 V1 133.73(12) . . ?
C14 O4 V1 128.77(13) . . ?
C1A O1A V1A 116.00(12) . . ?
N1 N2 V1 115.88(10) . . ?
C7 N2 V1 127.97(12) . . ?
C7 N2 N1 116.15(15) . . ?
C9A O2A V1A 136.90(13) . . ?
C14A O4A V1A 127.3(2) . . ?
C15A O4A V1A 130.6(6) . . ?
C15A O4A C14A 31.7(6) . . ?
C1 N1 N2 108.11(14) . . ?
C4A N3A V1 124.82(12) . 15_465 ?
C5A N3A V1 118.56(12) . 15_465 ?
C5A N3A C4A 116.59(16) . . ?
N1A N2A V1A 115.73(11) . . ?
C7A N2A V1A 129.18(13) . . ?
C7A N2A N1A 114.95(16) . . ?
C1A N1A N2A 108.55(15) . . ?
C5 N3 V1A 122.71(12) . . ?
C4 N3 V1A 119.60(12) . . ?
C4 N3 C5 117.18(16) . . ?
N2 C7 H7 118.3 . . ?
N2 C7 C8 123.36(17) . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 121.77(16) . . ?
C13 C8 C7 119.69(17) . . ?
C13 C8 C9 118.49(17) . . ?
C3A C2A C1A 122.50(16) . . ?
C6A C2A C1A 119.70(16) . . ?
C6A C2A C3A 117.79(17) . . ?
O1 C1 C2 117.65(15) . . ?
N1 C1 O1 124.35(16) . . ?
N1 C1 C2 117.99(16) . . ?
O2 C9 C8 121.73(16) . . ?
O2 C9 C10 118.26(17) . . ?
C10 C9 C8 119.92(17) . . ?
C6 C2 C1 121.06(16) . . ?
C3 C2 C1 121.05(16) . . ?
C3 C2 C6 117.88(16) . . ?
O1A C1A N1A 124.57(17) . . ?
O1A C1A C2A 119.21(16) . . ?
N1A C1A C2A 116.22(16) . . ?
N3 C5 H5 118.2 . . ?
N3 C5 C6 123.57(17) . . ?
C6 C5 H5 118.2 . . ?
C2 C6 H6 120.6 . . ?
C5 C6 C2 118.88(17) . . ?
C5 C6 H6 120.6 . . ?
C2A C3A H3A 120.6 . . ?
C4A C3A C2A 118.89(17) . . ?
C4A C3A H3A 120.6 . . ?
N3 C4 H4 118.4 . . ?
N3 C4 C3 123.25(17) . . ?
C3 C4 H4 118.4 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.24(17) . . ?
C4 C3 H3 120.4 . . ?
N3A C4A C3A 123.60(16) . . ?
N3A C4A H4A 118.2 . . ?
C3A C4A H4A 118.2 . . ?
N3A C5A H5A 118.1 . . ?
N3A C5A C6A 123.83(17) . . ?
C6A C5A H5A 118.1 . . ?
C8 C13 H13 119.6 . . ?
C12 C13 C8 120.90(19) . . ?
C12 C13 H13 119.6 . . ?
N2A C7A H7A 118.3 . . ?
N2A C7A C8A 123.31(19) . . ?
C8A C7A H7A 118.3 . . ?
C2A C6A H6A 120.4 . . ?
C5A C6A C2A 119.27(17) . . ?
C5A C6A H6A 120.4 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.11(19) . . ?
C11 C10 H10 119.9 . . ?
C9A C8A C7A 121.52(19) . . ?
C13A C8A C7A 118.6(2) . . ?
C13A C8A C9A 119.81(19) . . ?
C13 C12 H12 120.1 . . ?
C13 C12 C11 119.71(18) . . ?
C11 C12 H12 120.1 . . ?
O2A C9A C8A 122.01(18) . . ?
O2A C9A C10A 118.9(2) . . ?
C10A C9A C8A 119.0(2) . . ?
C10 C11 C12 120.85(19) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8A C13A H13A 119.7 . . ?
C12A C13A C8A 120.5(2) . . ?
C12A C13A H13A 119.7 . . ?
C10A C11A H11A 119.3 . . ?
C10A C11A C12A 121.4(2) . . ?
C12A C11A H11A 119.3 . . ?
C9A C10A H10A 120.0 . . ?
C11A C10A C9A 120.1(2) . . ?
C11A C10A H10A 120.0 . . ?
C13A C12A C11A 119.2(2) . . ?
C13A C12A H12A 120.4 . . ?
C11A C12A H12A 120.4 . . ?
O4A C14A H14D 109.5 . . ?
O4A C14A H14E 109.5 . . ?
O4A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C15A C14A O4A 65.8(11) . . ?
C15A C14A H14D 171.4 . . ?
C15A C14A H14E 67.1 . . ?
C15A C14A H14F 79.1 . . ?
O4A C15A H15A 109.5 . . ?
O4A C15A H15B 109.5 . . ?
O4A C15A H15C 109.5 . . ?
C14A C15A O4A 82.5(11) . . ?
C14A C15A H15A 62.4 . . ?
C14A C15A H15B 67.5 . . ?
C14A C15A H15C 167.7 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 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
V1 O1 C1 N1 -2.5(2) . . . . ?
V1 O1 C1 C2 176.16(11) . . . . ?
V1 O2 C9 C8 -29.4(3) . . . . ?
V1 O2 C9 C10 153.91(14) . . . . ?
V1 N2 N1 C1 2.44(17) . . . . ?
V1 N2 C7 C8 4.7(2) . . . . ?
V1 N3A C4A C3A 177.70(14) 15_465 . . . ?
V1 N3A C5A C6A -178.97(16) 15_465 . . . ?
V1A O1A C1A N1A -4.7(2) . . . . ?
V1A O1A C1A C2A 175.13(12) . . . . ?
V1A O2A C9A C8A 18.8(3) . . . . ?
V1A O2A C9A C10A -164.14(16) . . . . ?
V1A O4A C14A C15A 108.9(13) . . . . ?
V1A O4A C15A C14A -97.5(13) . . . . ?
V1A N2A N1A C1A 3.44(17) . . . . ?
V1A N2A C7A C8A -7.1(3) . . . . ?
V1A N3 C5 C6 -170.99(14) . . . . ?
V1A N3 C4 C3 171.47(14) . . . . ?
O1 V1 O2 C9 68.8(2) . . . . ?
O1 V1 O4 C14 -105.53(17) . . . . ?
O1 C1 C2 C6 162.04(16) . . . . ?
O1 C1 C2 C3 -18.3(2) . . . . ?
O2 V1 O4 C14 96.65(17) . . . . ?
O2 C9 C10 C11 178.23(18) . . . . ?
O4 V1 O2 C9 -166.18(17) . . . . ?
O1A V1A O2A C9A -57.4(3) . . . . ?
O1A V1A O4A C14A 68.0(3) . . . . ?
O1A V1A O4A C15A 108.9(8) . . . . ?
O3 V1 O2 C9 -62.06(18) . . . . ?
O3 V1 O4 C14 -6.07(18) . . . . ?
N2 V1 O2 C9 32.83(17) . . . . ?
N2 V1 O4 C14 -160.57(19) . . . . ?
N2 N1 C1 O1 -0.1(2) . . . . ?
N2 N1 C1 C2 -178.78(14) . . . . ?
N2 C7 C8 C9 9.9(3) . . . . ?
N2 C7 C8 C13 -172.68(17) . . . . ?
O2A V1A O4A C14A -133.4(3) . . . . ?
O2A V1A O4A C15A -92.4(8) . . . . ?
O2A C9A C10A C11A -177.2(2) . . . . ?
O4A V1A O2A C9A 177.17(19) . . . . ?
O3A V1A O2A C9A 71.4(2) . . . . ?
O3A V1A O4A C14A -28.3(3) . . . . ?
O3A V1A O4A C15A 12.6(8) . . . . ?
N1 N2 C7 C8 -175.88(15) . . . . ?
N1 C1 C2 C6 -19.2(2) . . . . ?
N1 C1 C2 C3 160.44(17) . . . . ?
N3A V1 O2 C9 110.87(17) 15_565 . . . ?
N3A V1 O4 C14 176.25(17) 15_565 . . . ?
N3A C5A C6A C2A 1.9(3) . . . . ?
N2A V1A O2A C9A -22.24(19) . . . . ?
N2A V1A O4A C14A 113.4(3) . . . . ?
N2A V1A O4A C15A 154.3(8) . . . . ?
N2A N1A C1A O1A 0.6(2) . . . . ?
N2A N1A C1A C2A -179.18(14) . . . . ?
N2A C7A C8A C9A -4.3(3) . . . . ?
N2A C7A C8A C13A 178.84(19) . . . . ?
N1A N2A C7A C8A 177.50(17) . . . . ?
N3 V1A O2A C9A -105.1(2) . . . . ?
N3 V1A O4A C14A 149.2(3) . . . . ?
N3 V1A O4A C15A -169.9(8) . . . . ?
N3 C5 C6 C2 -0.4(3) . . . . ?
N3 C4 C3 C2 0.0(3) . . . . ?
C7 N2 N1 C1 -177.01(15) . . . . ?
C7 C8 C9 O2 -0.2(3) . . . . ?
C7 C8 C9 C10 176.42(17) . . . . ?
C7 C8 C13 C12 -178.07(17) . . . . ?
C8 C9 C10 C11 1.5(3) . . . . ?
C8 C13 C12 C11 1.7(3) . . . . ?
C2A C3A C4A N3A 0.3(3) . . . . ?
C1 C2 C6 C5 179.51(16) . . . . ?
C1 C2 C3 C4 -179.32(16) . . . . ?
C9 C8 C13 C12 -0.6(3) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C1A C2A C3A C4A -178.12(17) . . . . ?
C1A C2A C6A C5A 177.11(18) . . . . ?
C5 N3 C4 C3 -0.5(3) . . . . ?
C6 C2 C3 C4 0.3(3) . . . . ?
C3A C2A C1A O1A -15.1(3) . . . . ?
C3A C2A C1A N1A 164.77(17) . . . . ?
C3A C2A C6A C5A -1.8(3) . . . . ?
C4 N3 C5 C6 0.7(3) . . . . ?
C3 C2 C6 C5 -0.1(3) . . . . ?
C4A N3A C5A C6A -0.8(3) . . . . ?
C5A N3A C4A C3A -0.3(3) . . . . ?
C13 C8 C9 O2 -177.62(16) . . . . ?
C13 C8 C9 C10 -1.0(3) . . . . ?
C13 C12 C11 C10 -1.2(3) . . . . ?
C7A N2A N1A C1A 179.52(16) . . . . ?
C7A C8A C9A O2A 0.6(3) . . . . ?
C7A C8A C9A C10A -176.50(19) . . . . ?
C7A C8A C13A C12A 176.8(2) . . . . ?
C6A C2A C1A O1A 166.06(17) . . . . ?
C6A C2A C1A N1A -14.1(2) . . . . ?
C6A C2A C3A C4A 0.8(3) . . . . ?
C8A C9A C10A C11A -0.1(3) . . . . ?
C8A C13A C12A C11A -0.4(4) . . . . ?
C9A C8A C13A C12A 0.0(3) . . . . ?
C13A C8A C9A O2A 177.33(19) . . . . ?
C13A C8A C9A C10A 0.3(3) . . . . ?
C10A C11A C12A C13A 0.5(4) . . . . ?
C12A C11A C10A C9A -0.3(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 176 electrons were 
found in a volume of 1296Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH4O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.123 0.250 0.000 323.9 43.6 '2 CH4O'
2 0.390 0.250 0.500 323.9 45.4 '2 CH4O'
3 -0.560 0.750 0.500 323.9 43.6 '2 CH4O'
4 -0.155 0.750 0.000 323.9 45.4 '2 CH4O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
####################################################################### 
# 
# 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_exp_3517
_database_code_depnum_ccdc_archive 'CCDC 2367534'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](n-butoxo)oxovanadium(v)"
_chemical_formula_moiety         'C17 H18 N3 O4 V'
_chemical_formula_sum            'C17 H18 N3 O4 V'
_chemical_formula_weight         379.28
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

# start Validation Reply Form
_vrf_PLAT430_exp_3517            
;
PROBLEM: Short Inter D...A Contact  O1       ..N3       .       2.84 Ang.  
RESPONSE: Polymer with V-py coordination bond.
;
# end Validation Reply Form

_cell_length_a                   12.5068(2)
_cell_length_b                   11.70940(10)
_cell_length_c                   23.1275(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3386.96(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    11889
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.5380
_cell_measurement_theta_min      3.8310
_shelx_estimated_absorpt_T_max   0.813
_shelx_estimated_absorpt_T_min   0.434
_exptl_absorpt_coefficient_mu    5.143
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1568
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0192
0 0 1 0.0232
-1 0 0 0.0392
1 0 0 0.0392
1 2 -1 0.0731
-4 6 -3 0.0477
-5 -5 3 0.0734
3 -7 4 0.0995

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24059
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.813
_diffrn_reflns_theta_min         3.823
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  18.00   0.50    1.27    --  -46.91  50.00 -95.00  100
  2  ω    -42.00 -13.00   0.50    5.00    --  -86.25 113.00 133.00   58
  3  ω   -136.00-110.00   0.50    5.00    --  -86.25 -73.00 -74.00   52
  4  ω    -56.00 -31.00   0.50    5.00    --  -86.25  50.00 -95.00   50
  5  ω     97.00 133.00   0.50    5.00    --  107.75  50.00 -95.00   72
  6  ω    130.00 156.00   0.50    5.00    --  107.75 113.00 133.00   52
  7  ω     40.00  65.00   0.50    5.00    --  107.75 -73.00 -74.00   50
  8  ω   -119.00 -93.00   0.50    1.27    --  -46.91-125.00-120.00   52
  9  ω    -24.00  26.00   0.50    1.27    --  -46.91  19.00  60.00  100
 10  ω   -111.00 -84.00   0.50    1.27    --  -46.91-125.00-150.00   54
 11  ω   -106.00 -73.00   0.50    1.27    --  -46.91-125.00-180.00   66
 12  ω    111.00 137.00   0.50    5.00    --  107.75 125.00   0.00   52
 13  ω     37.00  63.00   0.50    5.00    --  107.75 -61.00-180.00   52
 14  ω     98.00 124.00   0.50    5.00    --  107.75  77.00 -90.00   52
 15  ω     36.00  88.00   0.50    5.00    --  107.75 -95.00  90.00  104
 16  ω     95.00 177.00   0.50    5.00    --  107.75  30.00-150.00  164
 17  ω     41.00  74.00   0.50    5.00    --  107.75-125.00  60.00   66
 18  ω    148.00 174.00   0.50    5.00    --  107.75 125.00  60.00   52
 19  ω    148.00 174.00   0.50    5.00    --  107.75  77.00 -90.00   52
 20  ω    106.00 134.00   0.50    5.00    --  107.75  45.00 -30.00   56
 21  ω    137.00 177.00   0.50    5.00    --  107.75  45.00 -30.00   80
 22  ω    153.00 178.00   0.50    5.00    --  107.75  30.00 120.00   50
 23  ω    145.00 174.00   0.50    5.00    --  107.75  45.00 -60.00   58
 24  ω    108.00 146.00   0.50    5.00    --  107.75  30.00 120.00   76
 25  ω     38.00  64.00   0.50    5.00    --  107.75 -95.00 -60.00   52
 26  ω     35.00  66.00   0.50    5.00    --  107.75 -61.00 -30.00   62
 27  ω     99.00 124.00   0.50    5.00    --  107.75  45.00 -60.00   50
 28  ω     67.00 105.00   0.50    5.00    --  107.75 -77.00 -60.00   76
 29  ω     38.00  85.00   0.50    5.00    --  107.75 -95.00  60.00   94
 30  ω     53.00  79.00   0.50    5.00    --  107.75 -77.00  30.00   52
 31  ω     35.00  71.00   0.50    5.00    --  107.75 -61.00 120.00   72
 32  ω    105.00 146.00   0.50    5.00    --  107.75  45.00  30.00   82
 33  ω     42.00  68.00   0.50    5.00    --  107.75 -61.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3295
_reflns_number_total             3604
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0476
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0704P)²+3.7488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1330
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C5(H5), C3(H3), C4(H4), C13(H13), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.45708(3) 0.35438(3) 0.69152(2) 0.02428(15) Uani 1 1 d . . . . .
O1 O 0.57735(14) 0.46146(14) 0.70099(7) 0.0263(3) Uani 1 1 d . . . . .
O2 O 0.38773(14) 0.23441(15) 0.65526(7) 0.0302(4) Uani 1 1 d . . . . .
O4 O 0.47119(14) 0.30924(15) 0.76393(7) 0.0311(4) Uani 1 1 d . . . . .
N2 N 0.50445(15) 0.40043(15) 0.60613(8) 0.0221(4) Uani 1 1 d . . . . .
N1 N 0.58813(15) 0.47912(16) 0.60193(8) 0.0234(4) Uani 1 1 d . . . . .
O3 O 0.36371(16) 0.44622(17) 0.69458(9) 0.0398(5) Uani 1 1 d . . . . .
N3 N 0.88767(15) 0.72605(16) 0.67791(8) 0.0244(4) Uani 1 1 d . . . . .
C2 C 0.71112(17) 0.58248(18) 0.66236(10) 0.0221(4) Uani 1 1 d . . . . .
C1 C 0.61922(17) 0.50352(18) 0.65454(10) 0.0230(4) Uani 1 1 d . . . . .
C6 C 0.78187(19) 0.60435(19) 0.61697(10) 0.0248(5) Uani 1 1 d . . . . .
H6 H 0.770688 0.571380 0.579932 0.030 Uiso 1 1 calc R U . . .
C7 C 0.46310(17) 0.36545(19) 0.55825(10) 0.0232(5) Uani 1 1 d . . . . .
H7 H 0.488917 0.397904 0.523285 0.028 Uiso 1 1 calc R U . . .
C8 C 0.38017(17) 0.28021(19) 0.55434(10) 0.0249(5) Uani 1 1 d . . . . .
C5 C 0.86821(19) 0.6747(2) 0.62699(10) 0.0258(5) Uani 1 1 d . . . . .
H5 H 0.916819 0.687716 0.596123 0.031 Uiso 1 1 calc R U . . .
C9 C 0.34453(18) 0.21877(19) 0.60321(11) 0.0269(5) Uani 1 1 d . . . . .
C3 C 0.7314(2) 0.6328(2) 0.71566(11) 0.0286(5) Uani 1 1 d . . . . .
H3 H 0.686058 0.618238 0.747777 0.034 Uiso 1 1 calc R U . . .
C4 C 0.8191(2) 0.7046(2) 0.72115(10) 0.0291(5) Uani 1 1 d . . . . .
H4 H 0.831271 0.740324 0.757437 0.035 Uiso 1 1 calc R U . . .
C13 C 0.33782(19) 0.2537(2) 0.49963(11) 0.0303(5) Uani 1 1 d . . . . .
H13 H 0.362508 0.293982 0.466572 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2656(2) 0.1348(2) 0.59631(13) 0.0343(6) Uani 1 1 d . . . . .
H10 H 0.239523 0.094049 0.628913 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2259(2) 0.1118(2) 0.54174(14) 0.0388(6) Uani 1 1 d . . . . .
H11 H 0.172890 0.054337 0.537392 0.047 Uiso 1 1 calc R U . . .
C12 C 0.2611(2) 0.1701(2) 0.49318(12) 0.0363(6) Uani 1 1 d . . . . .
H12 H 0.232744 0.152848 0.456085 0.044 Uiso 1 1 calc R U . . .
C14 C 0.4457(3) 0.3705(4) 0.81498(14) 0.0526(9) Uani 1 1 d . . . . .
H14A H 0.373801 0.347852 0.828767 0.063 Uiso 1 1 calc R U . . .
H14B H 0.444469 0.453423 0.806615 0.063 Uiso 1 1 calc R U . . .
C16 C 0.5153(3) 0.4254(3) 0.91290(14) 0.0479(7) Uani 1 1 d . . . . .
H16A H 0.536177 0.504133 0.902200 0.057 Uiso 1 1 calc R U . . .
H16B H 0.440091 0.426348 0.926246 0.057 Uiso 1 1 calc R U . . .
C17 C 0.5858(3) 0.3816(3) 0.95906(18) 0.0562(9) Uani 1 1 d . . . . .
H17A H 0.660545 0.387460 0.946626 0.084 Uiso 1 1 calc R U . . .
H17B H 0.568404 0.301523 0.966928 0.084 Uiso 1 1 calc R U . . .
H17C H 0.575376 0.426860 0.994259 0.084 Uiso 1 1 calc R U . . .
C15 C 0.5274(4) 0.3459(4) 0.86111(18) 0.0636(10) Uani 1 1 d . . . . .
H15A H 0.599967 0.354733 0.844632 0.076 Uiso 1 1 calc R U . . .
H15B H 0.519496 0.265782 0.874137 0.076 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 O1 1.9704(17) . ?
V1 O2 1.8519(18) . ?
V1 O4 1.7648(18) . ?
V1 N2 2.1311(19) . ?
V1 O3 1.589(2) . ?
V1 N3 2.4753(19) 8_755 ?
O1 C1 1.293(3) . ?
O2 C9 1.332(3) . ?
O4 C14 1.418(3) . ?
N2 N1 1.398(3) . ?
N2 C7 1.289(3) . ?
N1 C1 1.309(3) . ?
N3 C5 1.344(3) . ?
N3 C4 1.341(3) . ?
C2 C1 1.486(3) . ?
C2 C6 1.397(3) . ?
C2 C3 1.389(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.378(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.442(3) . ?
C8 C9 1.412(3) . ?
C8 C13 1.406(3) . ?
C5 H5 0.9500 . ?
C9 C10 1.402(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(3) . ?
C4 H4 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.379(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(4) . ?
C12 H12 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.505(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.477(5) . ?
C16 C15 1.524(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?

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 N2 74.32(7) . . ?
O1 V1 N3 78.56(7) . 8_755 ?
O2 V1 O1 152.95(7) . . ?
O2 V1 N2 84.40(7) . . ?
O2 V1 N3 81.33(7) . 8_755 ?
O4 V1 O1 90.51(8) . . ?
O4 V1 O2 104.44(8) . . ?
O4 V1 N2 158.01(8) . . ?
O4 V1 N3 81.98(8) . 8_755 ?
N2 V1 N3 79.50(7) . 8_755 ?
O3 V1 O1 97.21(9) . . ?
O3 V1 O2 100.91(10) . . ?
O3 V1 O4 103.53(10) . . ?
O3 V1 N2 94.26(9) . . ?
O3 V1 N3 173.18(9) . 8_755 ?
C1 O1 V1 117.35(15) . . ?
C9 O2 V1 134.71(15) . . ?
C14 O4 V1 128.0(2) . . ?
N1 N2 V1 116.06(14) . . ?
C7 N2 V1 127.17(16) . . ?
C7 N2 N1 116.75(19) . . ?
C1 N1 N2 107.56(18) . . ?
C5 N3 V1 121.66(15) . 8_765 ?
C4 N3 V1 121.36(15) . 8_765 ?
C4 N3 C5 117.0(2) . . ?
C6 C2 C1 120.8(2) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 C6 118.3(2) . . ?
O1 C1 N1 124.7(2) . . ?
O1 C1 C2 116.7(2) . . ?
N1 C1 C2 118.60(19) . . ?
C2 C6 H6 120.7 . . ?
C5 C6 C2 118.7(2) . . ?
C5 C6 H6 120.7 . . ?
N2 C7 H7 117.9 . . ?
N2 C7 C8 124.2(2) . . ?
C8 C7 H7 117.9 . . ?
C9 C8 C7 122.0(2) . . ?
C13 C8 C7 118.7(2) . . ?
C13 C8 C9 119.3(2) . . ?
N3 C5 C6 123.8(2) . . ?
N3 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
O2 C9 C8 121.7(2) . . ?
O2 C9 C10 119.0(2) . . ?
C10 C9 C8 119.2(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(2) . . ?
C4 C3 H3 120.6 . . ?
N3 C4 C3 123.4(2) . . ?
N3 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
C8 C13 H13 119.5 . . ?
C12 C13 C8 121.1(2) . . ?
C12 C13 H13 119.5 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.5(3) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.0 . . ?
C10 C11 C12 122.0(2) . . ?
C12 C11 H11 119.0 . . ?
C13 C12 C11 118.9(2) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
O4 C14 H14A 109.7 . . ?
O4 C14 H14B 109.7 . . ?
O4 C14 C15 109.9(3) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H16A C16 H16B 108.5 . . ?
C17 C16 H16A 110.3 . . ?
C17 C16 H16B 110.3 . . ?
C17 C16 C15 107.3(3) . . ?
C15 C16 H16A 110.3 . . ?
C15 C16 H16B 110.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C15 C16 111.9(3) . . ?
C14 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?

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 O1 C1 N1 -0.7(3) . . . . ?
V1 O1 C1 C2 -178.92(14) . . . . ?
V1 O2 C9 C8 26.5(3) . . . . ?
V1 O2 C9 C10 -156.96(19) . . . . ?
V1 O4 C14 C15 -142.6(3) . . . . ?
V1 N2 N1 C1 1.6(2) . . . . ?
V1 N2 C7 C8 -4.8(3) . . . . ?
V1 N3 C5 C6 -178.74(17) 8_765 . . . ?
V1 N3 C4 C3 -179.61(19) 8_765 . . . ?
O1 V1 O2 C9 -66.5(3) . . . . ?
O1 V1 O4 C14 71.6(2) . . . . ?
O2 V1 O4 C14 -131.2(2) . . . . ?
O2 C9 C10 C11 -175.2(2) . . . . ?
O4 V1 O2 C9 171.9(2) . . . . ?
O4 C14 C15 C16 169.8(3) . . . . ?
N2 V1 O2 C9 -28.6(2) . . . . ?
N2 V1 O4 C14 117.2(3) . . . . ?
N2 N1 C1 O1 -0.6(3) . . . . ?
N2 N1 C1 C2 177.55(17) . . . . ?
N2 C7 C8 C9 -6.7(3) . . . . ?
N2 C7 C8 C13 176.7(2) . . . . ?
N1 N2 C7 C8 176.66(19) . . . . ?
O3 V1 O2 C9 64.7(2) . . . . ?
O3 V1 O4 C14 -25.9(3) . . . . ?
N3 V1 O2 C9 -108.7(2) 8_755 . . . ?
N3 V1 O4 C14 150.0(2) 8_755 . . . ?
C2 C6 C5 N3 -1.4(4) . . . . ?
C2 C3 C4 N3 -1.8(4) . . . . ?
C1 C2 C6 C5 -177.5(2) . . . . ?
C1 C2 C3 C4 179.0(2) . . . . ?
C6 C2 C1 O1 160.0(2) . . . . ?
C6 C2 C1 N1 -18.3(3) . . . . ?
C6 C2 C3 C4 1.6(3) . . . . ?
C7 N2 N1 C1 -179.75(19) . . . . ?
C7 C8 C9 O2 -1.8(3) . . . . ?
C7 C8 C9 C10 -178.3(2) . . . . ?
C7 C8 C13 C12 177.8(2) . . . . ?
C8 C9 C10 C11 1.5(4) . . . . ?
C8 C13 C12 C11 -0.1(4) . . . . ?
C5 N3 C4 C3 0.3(4) . . . . ?
C9 C8 C13 C12 1.1(4) . . . . ?
C9 C10 C11 C12 -0.6(4) . . . . ?
C3 C2 C1 O1 -17.3(3) . . . . ?
C3 C2 C1 N1 164.4(2) . . . . ?
C3 C2 C6 C5 -0.1(3) . . . . ?
C4 N3 C5 C6 1.3(4) . . . . ?
C13 C8 C9 O2 174.8(2) . . . . ?
C13 C8 C9 C10 -1.7(3) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C17 C16 C15 C14 170.5(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_exp_5521
_database_code_depnum_ccdc_archive 'CCDC 2367538'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](ethoxo)oxovanadium(v) ethanol solvate"
_chemical_formula_moiety         'C28.84 H23 N6 O8 V2, 1.507(C), 0.5[C2H6O]'
_chemical_formula_sum            'C31.34 H26 N6 O8.50 V2'
_chemical_formula_weight         724.60
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_H-M_alt        'I b c a'
_space_group_name_Hall           '-I 2b 2c'
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'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'

# start Validation Reply Form
_vrf_PLAT430_exp_5521            
;
PROBLEM: Short Inter D...A Contact  O003     ..N3A      .       2.84 Ang.  
RESPONSE: Polymer with V-py coordination bond.
;
# end Validation Reply Form

_cell_length_a                   20.6605(9)
_cell_length_b                   22.3137(8)
_cell_length_c                   29.1125(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13421.2(10)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    12733
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.4210
_cell_measurement_theta_min      3.0480
_shelx_estimated_absorpt_T_max   0.903
_shelx_estimated_absorpt_T_min   0.288
_exptl_absorpt_coefficient_mu    5.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5921
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            86108
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.432
_diffrn_reflns_theta_min         3.962
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -68.00   0.50    5.02    --  -47.97-133.00-118.00   74
  2  ω    -87.00 -35.00   0.50    5.02    --  -47.97 133.00 -50.00  104
  3  ω   -118.00 -69.00   0.50    5.02    --  -47.97-137.00  63.00   98
  4  ω    -93.00 -56.00   0.50    5.02    --  -47.97 137.00 126.00   74
  5  ω     47.00  73.00   0.50    5.02    --   47.97-137.00  63.00   52
  6  ω     40.00  72.00   0.50    5.02    --   47.97-133.00-118.00   64
  7  ω   -112.00 -87.00   0.50   20.07    --  -91.75-137.00  63.00   50
  8  ω    -88.00 -55.00   0.50   20.07    --  -91.75 137.00 126.00   66
  9  ω    -93.00 -68.00   0.50   20.07    --  -91.75-133.00-118.00   50
 10  ω   -146.00-111.00   0.50   20.07    --  -91.75-133.00-118.00   70
 11  ω     88.00 145.00   0.50   20.07    --  107.59 137.00 126.00  114
 12  ω     91.00 154.00   0.50   20.07    --  107.59 133.00 -50.00  126
 13  ω     86.00 118.00   0.50   20.07    --  107.59-137.00  63.00   64
 14  ω     84.00 117.00   0.50   20.07    --  107.59-133.00-118.00   66
 15  ω   -120.00 -88.00   0.50    5.02    --  -47.97 -77.00-180.00   64
 16  ω   -121.00 -96.00   0.50    5.02    --  -47.97 -77.00  30.00   50
 17  ω   -119.00 -89.00   0.50    5.02    --  -47.97 -77.00 120.00   60
 18  ω   -116.00 -87.00   0.50    5.02    --  -47.97-125.00  90.00   58
 19  ω    -24.00  15.00   0.50    5.02    --  -47.97  19.00  60.00   78
 20  ω   -121.00 -96.00   0.50    5.02    --  -47.97 -77.00 -90.00   50
 21  ω     89.00 121.00   0.50    5.02    --   47.97  77.00-150.00   64
 22  ω     89.00 115.00   0.50    5.02    --   47.97  77.00 120.00   52
 23  ω     90.00 116.00   0.50    5.02    --   47.97  77.00 150.00   52
 24  ω     88.00 113.00   0.50    5.02    --   47.97  77.00-180.00   50
 25  ω    -53.00 -26.00   0.50   20.07    --  -91.75  57.00 120.00   54
 26  ω   -151.00 -93.00   0.50   20.07    --  -91.75 -99.00-150.00  116
 27  ω   -140.00 -92.00   0.50   20.07    --  -91.75 -99.00  90.00   96
 28  ω    -85.00 -36.00   0.50   20.07    --  -91.75 125.00   0.00   98
 29  ω   -157.00 -98.00   0.50   20.07    --  -91.75 -57.00 -30.00  118
 30  ω   -133.00-102.00   0.50   20.07    --  -91.75 -99.00 120.00   62
 31  ω    -59.00 -33.00   0.50   20.07    --  -91.75  57.00 150.00   52
 32  ω   -159.00 -81.00   0.50   20.07    --  -91.75 -57.00 -60.00  156
 33  ω    -63.00 -20.00   0.50   20.07    --  -91.75  57.00 -90.00   86
 34  ω    -81.00 -56.00   0.50   20.07    --  -91.75 133.00 -50.00   50
 35  ω    -47.00 -21.00   0.50   20.07    --  -91.75  57.00 -30.00   52
 36  ω   -127.00 -86.00   0.50   20.07    --  -91.75-125.00 -60.00   82
 37  ω     82.00 111.00   0.50   20.07    --  107.59-125.00   0.00   58
 38  ω     43.00  99.00   0.50   20.07    --  107.59-125.00 -60.00  112
 39  ω     39.00 100.00   0.50   20.07    --  107.59 -99.00  90.00  122
 40  ω     36.00  62.00   0.50   20.07    --  107.59 -57.00-150.00   52
 41  ω     69.00 111.00   0.50   20.07    --  107.59-125.00  90.00   84
 42  ω     39.00  66.00   0.50   20.07    --  107.59 -57.00  90.00   54
 43  ω     39.00  64.00   0.50   20.07    --  107.59-125.00  90.00   50
 44  ω     95.00 165.00   0.50   20.07    --  107.59 125.00 -30.00  140
 45  ω     97.00 166.00   0.50   20.07    --  107.59  38.00 120.00  138
 46  ω     37.00  99.00   0.50   20.07    --  107.59 -99.00 -60.00  124
 47  ω     77.00 110.00   0.50   20.07    --  107.59-125.00 -90.00   66
 48  ω     56.00 109.00   0.50   20.07    --  107.59-112.00   0.73  106
 49  ω     40.00  65.00   0.50   20.07    --  107.59 -57.00 -60.00   50
 50  ω     35.00  60.00   0.50   20.07    --  107.59 -57.00 -90.00   50
 51  ω     51.00 108.00   0.50   20.07    --  107.59-125.00-180.00  114
 52  ω     35.00  66.00   0.50   20.07    --  107.59 -57.00 120.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4346
_reflns_number_total             6996
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0577
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0868P)²+7.4950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1696
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4A(H4A), C4(H4), C3A(H3A), C6(H6), C5A(H5A), C6A(H6A),
 C13(H13), C10(H10), C5(H5), C7A(H7A), C12(H12), C11(H11), C13A(H13A),
 C10A(H10A), C12A(H12A), C11A(H11A)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.40728(3) 0.59600(3) 0.46115(2) 0.05924(19) Uani 1 1 d . . . . .
V1A V 0.18433(4) 0.38352(3) 0.68796(3) 0.0813(3) Uani 1 1 d . . . . .
O003 O 0.35359(11) 0.54648(10) 0.50166(8) 0.0604(6) Uani 1 1 d . . . . .
O004 O 0.34193(12) 0.62285(11) 0.42774(9) 0.0664(6) Uani 1 1 d . . . . .
O1A O 0.15917(14) 0.33766(11) 0.63303(10) 0.0775(7) Uani 1 1 d . . . . .
O006 O 0.46974(12) 0.65415(11) 0.45097(9) 0.0699(7) Uani 1 1 d . . . . .
O007 O 0.43450(14) 0.54397(12) 0.42903(9) 0.0752(7) Uani 1 1 d . . . . .
N2 N 0.46750(14) 0.57340(11) 0.51788(10) 0.0573(7) Uani 1 1 d . . . . .
N3A N 0.12755(14) 0.17052(12) 0.51830(10) 0.0596(7) Uani 1 1 d . . . . .
N1 N 0.43839(15) 0.53905(12) 0.55245(10) 0.0614(7) Uani 1 1 d . . . . .
O2A O 0.24587(19) 0.41615(12) 0.72659(11) 0.0959(10) Uani 1 1 d . . . . .
N1A N 0.24223(17) 0.27196(13) 0.64719(11) 0.0696(8) Uani 1 1 d . . . . .
O3A O 0.14053(18) 0.34916(14) 0.72417(11) 0.1012(10) Uani 1 1 d . . . . .
O4A O 0.1357(2) 0.44519(14) 0.67205(12) 0.1085(12) Uani 1 1 d . . . . .
N2A N 0.25198(18) 0.31201(13) 0.68342(11) 0.0708(8) Uani 1 1 d . . . . .
N3 N 0.25845(18) 0.42823(13) 0.63157(11) 0.0701(8) Uani 1 1 d . . . . .
C1 C 0.37942(19) 0.52762(14) 0.54002(12) 0.0588(8) Uani 1 1 d . . . . .
C8 C 0.56463(17) 0.62140(15) 0.49111(12) 0.0602(8) Uani 1 1 d . . . . .
C2 C 0.33758(18) 0.49228(15) 0.57134(12) 0.0601(8) Uani 1 1 d . . . . .
C7 C 0.52871(19) 0.58500(15) 0.52281(13) 0.0633(9) Uani 1 1 d . . . . .
H7 H 0.550270 0.569004 0.548026 0.076 Uiso 1 1 calc R U . . .
C1A C 0.1924(2) 0.28929(16) 0.62413(14) 0.0669(10) Uani 1 1 d . . . . .
C9 C 0.53418(17) 0.65431(15) 0.45623(13) 0.0610(8) Uani 1 1 d . . . . .
C2A C 0.16996(18) 0.24995(15) 0.58593(12) 0.0619(9) Uani 1 1 d . . . . .
C3 C 0.27133(19) 0.49110(16) 0.56546(13) 0.0659(9) Uani 1 1 d . . . . .
H3 H 0.251987 0.511604 0.541267 0.079 Uiso 1 1 calc R U . . .
C4A C 0.0904(2) 0.21495(17) 0.53307(14) 0.0714(10) Uani 1 1 d . . . . .
H4A H 0.049499 0.219392 0.520160 0.086 Uiso 1 1 calc R U . . .
C4 C 0.2342(2) 0.45870(17) 0.59636(14) 0.0711(10) Uani 1 1 d . . . . .
H4 H 0.189622 0.458256 0.592179 0.085 Uiso 1 1 calc R U . . .
C3A C 0.1094(2) 0.25505(16) 0.56670(14) 0.0705(10) Uani 1 1 d . . . . .
H3A H 0.081402 0.285235 0.576247 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3635(2) 0.45997(16) 0.60777(13) 0.0674(9) Uani 1 1 d . . . . .
H6 H 0.407921 0.459332 0.612835 0.081 Uiso 1 1 calc R U . . .
C5A C 0.18604(18) 0.16638(18) 0.53708(14) 0.0696(10) Uani 1 1 d . . . . .
H5A H 0.212864 0.135401 0.527371 0.083 Uiso 1 1 calc R U . . .
C6A C 0.20926(19) 0.20475(17) 0.56975(15) 0.0725(10) Uani 1 1 d . . . . .
H6A H 0.251153 0.200391 0.580944 0.087 Uiso 1 1 calc R U . . .
C13 C 0.63220(19) 0.62630(18) 0.49557(15) 0.0728(10) Uani 1 1 d . . . . .
H13 H 0.653249 0.604941 0.518578 0.087 Uiso 1 1 calc R U . . .
C10 C 0.57112(19) 0.69114(17) 0.42765(15) 0.0731(10) Uani 1 1 d . . . . .
H10 H 0.550910 0.713443 0.404785 0.088 Uiso 1 1 calc R U . . .
C5 C 0.3223(2) 0.42900(17) 0.63617(14) 0.0716(10) Uani 1 1 d . . . . .
H5 H 0.340289 0.407161 0.660184 0.086 Uiso 1 1 calc R U . . .
C8A C 0.3118(3) 0.33440(19) 0.75229(14) 0.0860(13) Uani 1 1 d . . . . .
C9A C 0.2866(3) 0.39238(19) 0.75791(16) 0.0856(13) Uani 1 1 d . . . . .
C7A C 0.2950(2) 0.29738(18) 0.71293(15) 0.0795(12) Uani 1 1 d . . . . .
H7A H 0.316723 0.261221 0.709020 0.095 Uiso 1 1 calc R U . . .
C12 C 0.6675(2) 0.6619(2) 0.46667(16) 0.0838(12) Uani 1 1 d . . . . .
H12 H 0.712276 0.664058 0.469743 0.101 Uiso 1 1 calc R U . . .
C14 C 0.3275(3) 0.6073(2) 0.38136(16) 0.0934(14) Uani 1 1 d . . . . .
H14A H 0.281212 0.610116 0.376295 0.112 Uiso 1 1 calc R U . . .
H14B H 0.340690 0.566304 0.375593 0.112 Uiso 1 1 calc R U . . .
C11 C 0.6367(2) 0.6947(2) 0.43299(17) 0.0816(12) Uani 1 1 d . . . . .
H11 H 0.660776 0.719405 0.413748 0.098 Uiso 1 1 calc R U . . .
C13A C 0.3553(3) 0.3127(2) 0.78439(17) 0.1088(18) Uani 1 1 d . . . . .
H13A H 0.372282 0.274329 0.781119 0.131 Uiso 1 1 calc R U . . .
C10A C 0.3053(3) 0.4268(2) 0.79458(18) 0.1088(19) Uani 1 1 d . . . . .
H10A H 0.288987 0.465354 0.798349 0.131 Uiso 1 1 calc R U . . .
C12A C 0.3735(4) 0.3475(3) 0.82092(17) 0.121(2) Uani 1 1 d . . . . .
H12A H 0.402760 0.333017 0.842525 0.145 Uiso 1 1 calc R U . . .
C11A C 0.3480(4) 0.4040(3) 0.8252(2) 0.129(3) Uani 1 1 d . . . . .
H11A H 0.360411 0.427416 0.850095 0.155 Uiso 1 1 calc R U . . .
C15 C 0.3616(4) 0.6479(3) 0.34923(19) 0.137(2) Uani 1 1 d . . . . .
H15A H 0.350127 0.637783 0.318226 0.206 Uiso 1 1 calc R U . . .
H15B H 0.407494 0.643605 0.353188 0.206 Uiso 1 1 calc R U . . .
H15C H 0.349282 0.688574 0.355426 0.206 Uiso 1 1 calc R U . . .
C14A C 0.0778(15) 0.4620(10) 0.6885(10) 0.212(16) Uani 0.84(6) 1 d . . . A -1
C15A C 0.0339(13) 0.4425(11) 0.6647(8) 0.251(12) Uani 0.97(6) 1 d . . . A 1
C16A C 0.0340(14) 0.5028(11) 0.6828(6) 0.209(14) Uani 0.53(4) 1 d . . . B 2


_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 O003 1.960(2) . ?
V1 O004 1.769(2) . ?
V1 O006 1.854(3) . ?
V1 O007 1.593(3) . ?
V1 N2 2.129(3) . ?
V1 N3A 2.460(3) 12_665 ?
V1A O1A 1.968(3) . ?
V1A O2A 1.847(4) . ?
V1A O3A 1.587(3) . ?
V1A O4A 1.765(4) . ?
V1A N2A 2.125(4) . ?
V1A N3 2.457(3) . ?
O003 C1 1.308(4) . ?
O004 C14 1.425(5) . ?
O1A C1A 1.306(5) . ?
O006 C9 1.340(4) . ?
N2 N1 1.401(4) . ?
N2 C7 1.299(5) . ?
N3A C4A 1.326(5) . ?
N3A C5A 1.330(5) . ?
N1 C1 1.296(5) . ?
O2A C9A 1.349(6) . ?
N1A N2A 1.397(4) . ?
N1A C1A 1.288(5) . ?
O4A C14A 1.342(15) . ?
N2A C7A 1.279(5) . ?
N3 C4 1.328(5) . ?
N3 C5 1.325(5) . ?
C1 C2 1.483(5) . ?
C8 C7 1.436(5) . ?
C8 C9 1.402(5) . ?
C8 C13 1.406(5) . ?
C2 C3 1.380(5) . ?
C2 C6 1.390(5) . ?
C7 H7 0.9300 . ?
C1A C2A 1.491(5) . ?
C9 C10 1.397(5) . ?
C2A C3A 1.376(6) . ?
C2A C6A 1.378(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(5) . ?
C4A H4A 0.9300 . ?
C4A C3A 1.383(5) . ?
C4 H4 0.9300 . ?
C3A H3A 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.373(5) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.366(5) . ?
C6A H6A 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.369(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.366(6) . ?
C5 H5 0.9300 . ?
C8A C9A 1.404(7) . ?
C8A C7A 1.454(6) . ?
C8A C13A 1.385(7) . ?
C9A C10A 1.372(6) . ?
C7A H7A 0.9300 . ?
C12 H12 0.9300 . ?
C12 C11 1.379(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.479(8) . ?
C11 H11 0.9300 . ?
C13A H13A 0.9300 . ?
C13A C12A 1.369(7) . ?
C10A H10A 0.9300 . ?
C10A C11A 1.353(9) . ?
C12A H12A 0.9300 . ?
C12A C11A 1.372(10) . ?
C11A H11A 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14A C15A 1.22(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 V1 N2 74.36(10) . . ?
O003 V1 N3A 78.96(10) . 12_665 ?
O004 V1 O003 95.16(11) . . ?
O004 V1 O006 101.91(11) . . ?
O004 V1 N2 162.42(12) . . ?
O004 V1 N3A 85.40(11) . 12_665 ?
O006 V1 O003 152.21(11) . . ?
O006 V1 N2 83.28(11) . . ?
O006 V1 N3A 80.72(11) . 12_665 ?
O007 V1 O003 98.17(12) . . ?
O007 V1 O004 101.16(13) . . ?
O007 V1 O006 99.81(14) . . ?
O007 V1 N2 94.38(12) . . ?
O007 V1 N3A 173.11(12) . 12_665 ?
N2 V1 N3A 78.83(10) . 12_665 ?
O1A V1A N2A 74.50(12) . . ?
O1A V1A N3 80.37(11) . . ?
O2A V1A O1A 151.80(14) . . ?
O2A V1A N2A 83.17(14) . . ?
O2A V1A N3 79.49(13) . . ?
O3A V1A O1A 97.93(15) . . ?
O3A V1A O2A 100.28(17) . . ?
O3A V1A O4A 103.11(18) . . ?
O3A V1A N2A 93.07(15) . . ?
O3A V1A N3 174.63(15) . . ?
O4A V1A O1A 92.41(15) . . ?
O4A V1A O2A 104.11(17) . . ?
O4A V1A N2A 160.55(14) . . ?
O4A V1A N3 82.10(14) . . ?
N2A V1A N3 81.57(12) . . ?
C1 O003 V1 117.7(2) . . ?
C14 O004 V1 126.7(3) . . ?
C1A O1A V1A 116.9(3) . . ?
C9 O006 V1 132.5(2) . . ?
N1 N2 V1 115.9(2) . . ?
C7 N2 V1 127.4(2) . . ?
C7 N2 N1 116.6(3) . . ?
C4A N3A V1 123.8(3) . 12_655 ?
C4A N3A C5A 116.4(3) . . ?
C5A N3A V1 119.8(2) . 12_655 ?
C1 N1 N2 108.1(3) . . ?
C9A O2A V1A 133.3(3) . . ?
C1A N1A N2A 108.5(3) . . ?
C14A O4A V1A 129.2(6) . . ?
N1A N2A V1A 115.6(3) . . ?
C7A N2A V1A 127.4(3) . . ?
C7A N2A N1A 116.4(3) . . ?
C4 N3 V1A 119.3(3) . . ?
C5 N3 V1A 123.9(3) . . ?
C5 N3 C4 116.5(3) . . ?
O003 C1 C2 117.3(3) . . ?
N1 C1 O003 124.0(3) . . ?
N1 C1 C2 118.7(3) . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 C13 118.1(3) . . ?
C13 C8 C7 119.8(3) . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 C6 117.8(3) . . ?
C6 C2 C1 121.4(3) . . ?
N2 C7 C8 123.0(3) . . ?
N2 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
O1A C1A C2A 118.1(4) . . ?
N1A C1A O1A 124.4(4) . . ?
N1A C1A C2A 117.4(3) . . ?
O006 C9 C8 121.8(3) . . ?
O006 C9 C10 118.5(3) . . ?
C10 C9 C8 119.6(3) . . ?
C3A C2A C1A 122.6(3) . . ?
C3A C2A C6A 117.2(3) . . ?
C6A C2A C1A 120.2(4) . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(4) . . ?
C4 C3 H3 120.7 . . ?
N3A C4A H4A 118.3 . . ?
N3A C4A C3A 123.3(4) . . ?
C3A C4A H4A 118.3 . . ?
N3 C4 C3 124.1(4) . . ?
N3 C4 H4 118.0 . . ?
C3 C4 H4 118.0 . . ?
C2A C3A C4A 119.5(3) . . ?
C2A C3A H3A 120.2 . . ?
C4A C3A H3A 120.2 . . ?
C2 C6 H6 120.6 . . ?
C5 C6 C2 118.8(4) . . ?
C5 C6 H6 120.6 . . ?
N3A C5A H5A 117.9 . . ?
N3A C5A C6A 124.2(3) . . ?
C6A C5A H5A 117.9 . . ?
C2A C6A H6A 120.3 . . ?
C5A C6A C2A 119.3(4) . . ?
C5A C6A H6A 120.3 . . ?
C8 C13 H13 119.4 . . ?
C12 C13 C8 121.2(4) . . ?
C12 C13 H13 119.4 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 H10 119.7 . . ?
N3 C5 C6 124.2(4) . . ?
N3 C5 H5 117.9 . . ?
C6 C5 H5 117.9 . . ?
C9A C8A C7A 121.8(5) . . ?
C13A C8A C9A 119.0(4) . . ?
C13A C8A C7A 119.2(5) . . ?
O2A C9A C8A 121.0(4) . . ?
O2A C9A C10A 118.8(5) . . ?
C10A C9A C8A 120.2(5) . . ?
N2A C7A C8A 123.3(4) . . ?
N2A C7A H7A 118.3 . . ?
C8A C7A H7A 118.3 . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 119.9(4) . . ?
C11 C12 H12 120.0 . . ?
O004 C14 H14A 109.5 . . ?
O004 C14 H14B 109.5 . . ?
O004 C14 C15 110.6(5) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C10 C11 C12 120.5(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C8A C13A H13A 119.9 . . ?
C12A C13A C8A 120.3(6) . . ?
C12A C13A H13A 119.9 . . ?
C9A C10A H10A 120.5 . . ?
C11A C10A C9A 119.0(6) . . ?
C11A C10A H10A 120.5 . . ?
C13A C12A H12A 120.5 . . ?
C13A C12A C11A 119.1(6) . . ?
C11A C12A H12A 120.5 . . ?
C10A C11A C12A 122.5(5) . . ?
C10A C11A H11A 118.8 . . ?
C12A C11A H11A 118.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C15A C14A O4A 111(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
V1 O003 C1 N1 -0.9(4) . . . . ?
V1 O003 C1 C2 177.5(2) . . . . ?
V1 O004 C14 C15 -88.6(5) . . . . ?
V1 O006 C9 C8 -33.0(5) . . . . ?
V1 O006 C9 C10 150.8(3) . . . . ?
V1 N2 N1 C1 1.8(3) . . . . ?
V1 N2 C7 C8 6.4(5) . . . . ?
V1 N3A C4A C3A 177.0(3) 12_655 . . . ?
V1 N3A C5A C6A -178.6(3) 12_655 . . . ?
V1A O1A C1A N1A -4.1(5) . . . . ?
V1A O1A C1A C2A 173.2(2) . . . . ?
V1A O2A C9A C8A 31.5(6) . . . . ?
V1A O2A C9A C10A -151.2(4) . . . . ?
V1A O4A C14A C15A -95(2) . . . . ?
V1A N2A C7A C8A -10.4(6) . . . . ?
V1A N3 C4 C3 172.7(3) . . . . ?
V1A N3 C5 C6 -171.9(3) . . . . ?
O003 V1 O004 C14 -109.1(3) . . . . ?
O003 V1 O006 C9 72.7(4) . . . . ?
O003 C1 C2 C3 -14.4(5) . . . . ?
O003 C1 C2 C6 166.4(3) . . . . ?
O004 V1 O006 C9 -160.7(3) . . . . ?
O1A V1A O2A C9A -73.9(5) . . . . ?
O1A V1A O4A C14A 103(2) . . . . ?
O1A C1A C2A C3A -14.5(5) . . . . ?
O1A C1A C2A C6A 168.2(3) . . . . ?
O006 V1 O004 C14 92.9(4) . . . . ?
O006 C9 C10 C11 177.3(4) . . . . ?
O007 V1 O004 C14 -9.7(4) . . . . ?
O007 V1 O006 C9 -56.9(3) . . . . ?
N2 V1 O004 C14 -161.4(4) . . . . ?
N2 V1 O006 C9 36.4(3) . . . . ?
N2 N1 C1 O003 -0.6(4) . . . . ?
N2 N1 C1 C2 -179.1(3) . . . . ?
N3A V1 O004 C14 172.4(3) 12_665 . . . ?
N3A V1 O006 C9 116.1(3) 12_665 . . . ?
N3A C4A C3A C2A 0.8(6) . . . . ?
N3A C5A C6A C2A 2.1(6) . . . . ?
N1 N2 C7 C8 -177.7(3) . . . . ?
N1 C1 C2 C3 164.2(3) . . . . ?
N1 C1 C2 C6 -15.0(5) . . . . ?
O2A V1A O4A C14A -100(2) . . . . ?
O2A C9A C10A C11A -177.7(5) . . . . ?
N1A N2A C7A C8A 179.1(3) . . . . ?
N1A C1A C2A C3A 163.1(4) . . . . ?
N1A C1A C2A C6A -14.2(5) . . . . ?
O3A V1A O2A C9A 55.5(4) . . . . ?
O3A V1A O4A C14A 4(2) . . . . ?
O4A V1A O2A C9A 162.0(4) . . . . ?
N2A V1A O2A C9A -36.4(4) . . . . ?
N2A V1A O4A C14A 150(2) . . . . ?
N2A N1A C1A O1A 2.3(5) . . . . ?
N2A N1A C1A C2A -175.1(3) . . . . ?
N3 V1A O2A C9A -119.0(4) . . . . ?
N3 V1A O4A C14A -177(2) . . . . ?
C1 C2 C3 C4 -178.3(3) . . . . ?
C1 C2 C6 C5 178.8(3) . . . . ?
C8 C9 C10 C11 0.9(6) . . . . ?
C8 C13 C12 C11 1.2(6) . . . . ?
C2 C3 C4 N3 -0.2(6) . . . . ?
C2 C6 C5 N3 -0.8(6) . . . . ?
C7 N2 N1 C1 -174.6(3) . . . . ?
C7 C8 C9 O006 0.9(5) . . . . ?
C7 C8 C9 C10 177.1(3) . . . . ?
C7 C8 C13 C12 -178.2(4) . . . . ?
C1A N1A N2A V1A 0.5(4) . . . . ?
C1A N1A N2A C7A 172.1(3) . . . . ?
C1A C2A C3A C4A -176.5(3) . . . . ?
C1A C2A C6A C5A 175.2(4) . . . . ?
C9 C8 C7 N2 9.6(5) . . . . ?
C9 C8 C13 C12 -0.3(6) . . . . ?
C9 C10 C11 C12 0.0(7) . . . . ?
C3 C2 C6 C5 -0.5(5) . . . . ?
C4A N3A C5A C6A -0.4(6) . . . . ?
C4 N3 C5 C6 1.5(6) . . . . ?
C3A C2A C6A C5A -2.2(6) . . . . ?
C6 C2 C3 C4 0.9(5) . . . . ?
C5A N3A C4A C3A -1.1(6) . . . . ?
C6A C2A C3A C4A 0.9(6) . . . . ?
C13 C8 C7 N2 -172.5(3) . . . . ?
C13 C8 C9 O006 -177.0(3) . . . . ?
C13 C8 C9 C10 -0.8(5) . . . . ?
C13 C12 C11 C10 -1.1(7) . . . . ?
C5 N3 C4 C3 -1.0(5) . . . . ?
C8A C9A C10A C11A -0.4(8) . . . . ?
C8A C13A C12A C11A 0.0(9) . . . . ?
C9A C8A C7A N2A -7.2(7) . . . . ?
C9A C8A C13A C12A -0.1(8) . . . . ?
C9A C10A C11A C12A 0.2(9) . . . . ?
C7A C8A C9A O2A -0.3(7) . . . . ?
C7A C8A C9A C10A -177.6(4) . . . . ?
C7A C8A C13A C12A 177.8(5) . . . . ?
C13A C8A C9A O2A 177.6(4) . . . . ?
C13A C8A C9A C10A 0.3(7) . . . . ?
C13A C8A C7A N2A 174.9(4) . . . . ?
C13A C12A C11A C10A -0.1(10) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 228 electrons were 
found in a volume of 1888Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C2H6O] per Asymmetric Unit 
which account for 208 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.860 0.250 472.1 57.2 '2 C2H6O'
2 0.000 -0.842 0.750 472.1 50.4 '2 C2H6O'
3 0.500 -0.966 0.250 472.1 50.4 '2 C2H6O'
4 0.500 -0.870 0.750 472.1 57.2 '2 C2H6O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
####################################################################### 
# 
# 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_exp_3983
_database_code_depnum_ccdc_archive 'CCDC 2367537'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](ethoxo)oxovanadium(v)"
_chemical_formula_moiety         'C15 H14 N3 O4 V'
_chemical_formula_sum            'C15 H14 N3 O4 V'
_chemical_formula_weight         351.23
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

# start Validation Reply Form
_vrf_PLAT430_exp_3983            
;
PROBLEM: Short Inter D...A Contact  O1       ..N3       .       2.79 Ang.  
RESPONSE: Polymer with V-py coordination bond.
;
# end Validation Reply Form

_cell_length_a                   13.05222(6)
_cell_length_b                   11.39032(5)
_cell_length_c                   21.55450(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3204.49(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    84126
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.5470
_cell_measurement_theta_min      3.8620
_shelx_estimated_absorpt_T_max   0.589
_shelx_estimated_absorpt_T_min   0.124
_exptl_absorpt_coefficient_mu    5.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1440
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 2 -1 0.0935
-1 0 2 0.0633
2 -1 2 0.1620
-2 1 -2 0.0838
1 0 1 0.0493
-1 0 -2 0.0571
-1 0 -1 0.0608
2 1 -2 0.1076
5 0 -11 0.0743

_exptl_crystal_size_max          0.665
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            127302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.765
_diffrn_reflns_theta_min         4.102
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     30.00  61.00   0.50    0.06    --   47.29  65.00-169.89   62
  2  ω     84.00 119.00   0.50    0.06    --   47.29  65.00-169.89   70
  3  ω     29.00  60.00   0.50    0.06    --   47.29  66.00   6.94   62
  4  ω     32.00  95.00   0.50    0.06    --   47.29  63.00  36.30  126
  5  ω     30.00  59.00   0.50    0.06    --   47.29  63.00  96.83   58
  6  ω     65.00  91.00   0.50    0.06    --   47.29  63.00  96.83   52
  7  ω     84.00 119.00   0.50    0.06    --   47.29  63.00 120.18   70
  8  ω     81.00 117.00   0.50    0.06    --   47.29  63.00 161.01   72
  9  ω     30.00  63.00   0.50    0.06    --   47.29  63.00 161.01   66
 10  ω     30.00  68.00   0.50    0.06    --   47.29  63.00 120.18   76
 11  ω     32.00  58.00   0.50    0.06    --   47.29  57.00  90.00   52
 12  ω     31.00  57.00   0.50    0.06    --   47.29  62.00 -24.29   52
 13  ω     32.00  60.00   0.50    0.06    --   47.29  57.00 -30.00   56
 14  ω     94.00 120.00   0.50    0.06    --   47.29  57.00 -30.00   52
 15  ω     95.00 120.00   0.50    0.06    --   47.29  61.00 -82.86   50
 16  ω     33.00  76.00   0.50    0.06    --   47.29  61.00 -82.86   86
 17  ω     32.00  58.00   0.50    0.06    --   47.29  57.00 -90.00   52
 18  ω     33.00  58.00   0.50    0.06    --   47.29  57.00-120.00   50
 19  ω     35.00  63.00   0.50    0.06    --   47.29  38.00-120.00   56
 20  ω     35.00  80.00   0.50    0.06    --   47.29  18.00 -57.00   90
 21  ω     98.00 123.00   0.50    0.06    --   47.29  18.00 -57.00   50
 22  ω     88.00 174.00   0.50    0.24    --  107.75  77.00 -90.00  172
 23  ω    143.00 169.00   0.50    0.24    --  107.75  77.00-180.00   52
 24  ω     88.00 136.00   0.50    0.24    --  107.75  77.00-180.00   96
 25  ω     88.00 123.00   0.50    0.24    --  107.75  77.00-120.00   70
 26  ω    135.00 177.00   0.50    0.24    --  107.75  77.00-120.00   84
 27  ω     88.00 178.00   0.50    0.24    --  107.75  77.00-150.00  180
 28  ω     88.00 177.00   0.50    0.24    --  107.75  77.00  30.00  178
 29  ω    121.00 172.00   0.50    0.24    --  107.75  77.00 -30.00  102
 30  ω     88.00 169.00   0.50    0.24    --  107.75  77.00  60.00  162
 31  ω     88.00 128.00   0.50    0.24    --  107.75  77.00 120.00   80
 32  ω     88.00 113.00   0.50    0.24    --  107.75  77.00 150.00   50
 33  ω    123.00 177.00   0.50    0.24    --  107.75  77.00 150.00  108
 34  ω    153.00 178.00   0.50    0.24    --  107.75  77.00  90.00   50
 35  ω     89.00 137.00   0.50    0.24    --  107.75  77.00  90.00   96
 36  ω    132.00 157.00   0.50    0.24    --  107.75  77.00   0.00   50
 37  ω    133.00 174.00   0.50    0.24    --  107.75  77.00 -60.00   82
 38  ω     88.00 124.00   0.50    0.24    --  107.75  77.00 -60.00   72
 39  ω     88.00 113.00   0.50    0.24    --  107.75  77.00 -30.00   50
 40  ω     88.00 114.00   0.50    0.24    --  107.75  77.00   0.00   52
 41  ω     86.00 126.00   0.50    0.24    --  107.75  74.00  55.15   80
 42  ω    130.00 163.00   0.50    0.24    --  107.75  74.00  55.15   66
 43  ω    150.00 178.00   0.50    0.24    --  107.75  65.00  93.07   56
 44  ω     91.00 124.00   0.50    0.24    --  107.75  65.00  93.07   66
 45  ω     91.00 117.00   0.50    0.24    --  107.75  61.00  90.00   52
 46  ω     91.00 162.00   0.50    0.24    --  107.75  61.00 150.00  142
 47  ω    133.00 168.00   0.50    0.24    --  107.75  61.00  90.00   70
 48  ω    127.00 153.00   0.50    0.24    --  107.75  61.00 -30.00   52
 49  ω     91.00 133.00   0.50    0.24    --  107.75  61.00  30.00   84
 50  ω     92.00 117.00   0.50    0.24    --  107.75  61.00 -30.00   50
 51  ω     94.00 131.00   0.50    0.24    --  107.75  61.00 -90.00   74
 52  ω     91.00 123.00   0.50    0.24    --  107.75  61.00-120.00   64
 53  ω     91.00 148.00   0.50    0.24    --  107.75  61.00-150.00  114
 54  ω    143.00 169.00   0.50    0.24    --  107.75  61.00-120.00   52
 55  ω    153.00 178.00   0.50    0.24    --  107.75  61.00 -90.00   50
 56  ω     92.00 152.00   0.50    0.24    --  107.75  61.00 -60.00  120
 57  ω     91.00 117.00   0.50    0.24    --  107.75  61.00-180.00   52
 58  ω     91.00 166.00   0.50    0.24    --  107.75  61.00   0.00  150
 59  ω    142.00 175.00   0.50    0.24    --  107.75  55.00 138.65   66
 60  ω     95.00 132.00   0.50    0.24    --  107.75  55.00 138.65   74
 61  ω     91.00 129.00   0.50    0.24    --  107.75  61.00 120.00   76
 62  ω     91.00 124.00   0.50    0.24    --  107.75  61.00  60.00   66
 63  ω    130.00 176.00   0.50    0.24    --  107.75  45.00 120.00   92
 64  ω     97.00 155.00   0.50    0.24    --  107.75  45.00  30.00  116
 65  ω     97.00 122.00   0.50    0.24    --  107.75  45.00 120.00   50
 66  ω     99.00 154.00   0.50    0.24    --  107.75  45.00   0.00  110
 67  ω    142.00 167.00   0.50    0.24    --  107.75  30.00   0.00   50
 68  ω    101.00 126.00   0.50    0.24    --  107.75  30.00   0.00   50
 69  ω    112.00 164.00   0.50    0.24    --  107.75  30.00 -30.00  104
 70  ω    135.00 178.00   0.50    0.24    --  107.75  18.00 -57.00   86
 71  ω     99.00 125.00   0.50    0.24    --  107.75  18.00 -57.00   52
 72  ω     98.00 147.00   0.50    0.24    --  107.75  45.00-120.00   98
 73  ω     95.00 149.00   0.50    0.24    --  107.75  15.00-150.00  108
 74  ω     95.00 161.00   0.50    0.24    --  107.75  45.00-150.00  132
 75  ω    151.00 178.00   0.50    0.24    --  107.75 125.00-180.00   54
 76  ω    144.00 174.00   0.50    0.24    --  107.75 125.00-120.00   60
 77  ω    108.00 146.00   0.50    0.24    --  107.75 125.00-180.00   76
 78  ω    103.00 128.00   0.50    0.24    --  107.75 123.00-135.65   50
 79  ω    153.00 178.00   0.50    0.24    --  107.75 123.00-135.65   50
 80  ω    105.00 155.00   0.50    0.24    --  107.75 125.00   0.00  100
 81  ω    122.00 177.00   0.50    0.24    --  107.75 125.00  90.00  110
 82  ω    109.00 163.00   0.50    0.24    --  107.75 125.00 150.00  108
 83  ω    -27.00  26.00   0.50    0.06    --   47.29 -18.00 134.00  106
 84  ω     35.00  93.00   0.50    0.24    --  107.75 -80.00 -13.54  116
 85  ω     98.00 128.00   0.50    0.24    --  107.75 -80.00 -13.54   60
 86  ω     36.00  83.00   0.50    0.24    --  107.75 -77.00  99.24   94
 87  ω     38.00  68.00   0.50    0.24    --  107.75 -77.00 -60.00   60
 88  ω     40.00  92.00   0.50    0.24    --  107.75 -77.00 -90.00  104
 89  ω     38.00  90.00   0.50    0.24    --  107.75 -72.00-152.41  104
 90  ω     45.00  85.00   0.50    0.24    --  107.75 -79.00-167.21   80
 91  ω     98.00 123.00   0.50    0.24    --  107.75 -79.00-167.21   50
 92  ω     44.00  71.00   0.50    0.24    --  107.75 -61.00 -90.00   54
 93  ω     38.00  81.00   0.50    0.24    --  107.75 -73.00  67.04   86
 94  ω     35.00  67.00   0.50    0.24    --  107.75 -61.00 120.00   64
 95  ω     34.00  94.00   0.50    0.06    --   47.29-125.00  90.00  120
 96  ω     35.00  60.00   0.50    0.24    --  107.75-125.00 120.00   50
 97  ω     53.00  95.00   0.50    0.06    --   47.29-125.00   0.00   84
 98  ω     36.00  75.00   0.50    0.24    --  107.75-125.00 -60.00   78
 99  ω     87.00 112.00   0.50    0.24    --  107.75-125.00 -60.00   50
100  ω     68.00 112.00   0.50    0.24    --  107.75-125.00-150.00   88
101  ω     71.00 112.00   0.50    0.24    --  107.75-125.00-180.00   82
102  ω     41.00  66.00   0.50    0.24    --  107.75-125.00-150.00   50
103  ω     49.00 112.00   0.50    0.24    --  107.75-125.00   0.00  126
104  ω     81.00 112.00   0.50    0.24    --  107.75-125.00 -30.00   62
105  ω     68.00 112.00   0.50    0.24    --  107.75-125.00  90.00   88
106  ω     68.00 112.00   0.50    0.24    --  107.75-125.00 120.00   88
107  ω     87.00 112.00   0.50    0.24    --  107.75-125.00 150.00   50
108  ω     35.00  71.00   0.50    0.24    --  107.75-102.00 174.47   72
109  ω     36.00  67.00   0.50    0.24    --  107.75-125.00 150.00   62
110  ω     78.00 107.00   0.50    0.24    --  107.75-102.00 174.47   58
111  ω     53.00 111.00   0.50    0.24    --  107.75-125.00  30.00  116
112  ω     35.00 107.00   0.50    0.24    --  107.75-105.00  31.11  144
113  ω     36.00  69.00   0.50    0.24    --  107.75 -95.00  60.00   66
114  ω     40.00  75.00   0.50    0.24    --  107.75 -86.00 131.32   70
115  ω     81.00 117.00   0.50    0.24    --  107.75 -86.00 131.32   72
116  ω     43.00  78.00   0.50    0.24    --  107.75 -82.00-107.66   70
117  ω     80.00 107.00   0.50    0.24    --  107.75 -82.00-107.66   54
118  ω     37.00  99.00   0.50    0.24    --  107.75 -93.00-120.59  124
119  ω     35.00 107.00   0.50    0.24    --  107.75-105.00-147.91  144
120  ω    -62.00  24.00   0.50    0.06    --  -47.29  57.00-180.00  172
121  ω    -26.00  24.00   0.50    0.06    --  -47.29  18.00 -57.00  100
122  ω    -84.00 -37.00   0.50    0.06    --  -47.29 -19.00  30.00   94
123  ω   -114.00 -86.00   0.50    0.06    --  -47.29 -19.00  30.00   56
124  ω    -86.00 -35.00   0.50    0.06    --  -47.29 -18.00 134.00  102
125  ω   -122.00 -90.00   0.50    0.06    --  -47.29 -18.00 134.00   64
126  ω   -139.00-114.00   0.50    0.24    --  -86.25 -18.00 134.00   50
127  ω   -101.00 -68.00   0.50    0.24    --  -86.25 -66.00 -11.09   66
128  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00 -50.76   52
129  ω    -93.00 -68.00   0.50    0.24    --  -86.25 -66.00 -62.13   50
130  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00-136.65   52
131  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00-104.70   52
132  ω   -158.00-132.00   0.50    0.24    --  -86.25 -66.00-104.70   52
133  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00 -74.47   52
134  ω    -93.00 -68.00   0.50    0.24    --  -86.25 -66.00 -96.59   50
135  ω    -93.00 -68.00   0.50    0.24    --  -86.25 -66.00 -25.96   50
136  ω    -93.00 -68.00   0.50    0.24    --  -86.25 -66.00  -3.80   50
137  ω    -99.00 -68.00   0.50    0.24    --  -86.25 -65.00   7.59   62
138  ω    -93.00 -68.00   0.50    0.24    --  -86.25 -65.00  97.97   50
139  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00 108.82   52
140  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -66.00 140.72   52
141  ω    -94.00 -68.00   0.50    0.24    --  -86.25 -65.00 169.47   52
142  ω    -96.00 -69.00   0.50    0.24    --  -86.25 -64.00 158.32   54
143  ω   -104.00 -69.00   0.50    0.24    --  -86.25 -64.00  44.02   70
144  ω   -103.00 -68.00   0.50    0.24    --  -86.25 -65.00  51.34   70
145  ω   -155.00-129.00   0.50    0.24    --  -86.25 -63.00 150.78   52
146  ω   -103.00 -69.00   0.50    0.24    --  -86.25 -64.00  12.70   68
147  ω    -95.00 -69.00   0.50    0.24    --  -86.25 -63.00 -38.08   52
148  ω    -94.00 -69.00   0.50    0.24    --  -86.25 -64.00 -82.86   50
149  ω    -95.00 -69.00   0.50    0.24    --  -86.25 -63.00-164.54   52
150  ω   -109.00 -69.00   0.50    0.24    --  -86.25 -64.00-147.21   80
151  ω    -94.00 -69.00   0.50    0.24    --  -86.25 -62.00-133.27   50
152  ω    -98.00 -69.00   0.50    0.24    --  -86.25 -62.00 -96.32   58
153  ω    -96.00 -70.00   0.50    0.24    --  -86.25 -61.00-180.00   52
154  ω   -148.00-122.00   0.50    0.24    --  -86.25 -63.00 -38.08   52
155  ω   -104.00 -71.00   0.50    0.24    --  -86.25 -61.00-120.00   66
156  ω   -115.00 -69.00   0.50    0.24    --  -86.25 -63.00  28.50   92
157  ω    -94.00 -69.00   0.50    0.24    --  -86.25 -62.00  65.48   50
158  ω    -95.00 -70.00   0.50    0.24    --  -86.25 -60.00  72.11   50
159  ω    -96.00 -70.00   0.50    0.24    --  -86.25 -61.00  82.59   52
160  ω    -96.00 -70.00   0.50    0.24    --  -86.25 -61.00 120.00   52
161  ω    -95.00 -69.00   0.50    0.24    --  -86.25 -63.00 150.78   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3373
_reflns_number_total             3412
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00051(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²+1.5078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0820
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C7(H7), C4(H4), C13(H13), C10(H10), C12(H12), C11(H11)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.46889(2) 0.66207(2) 0.29970(2) 0.02049(10) Uani 1 1 d . . . . .
O1 O 0.58435(7) 0.55257(9) 0.29108(4) 0.0231(2) Uani 1 1 d . . . . .
O2 O 0.40107(8) 0.78406(9) 0.34031(4) 0.0257(2) Uani 1 1 d . . . . .
O4 O 0.48404(8) 0.71560(9) 0.22336(5) 0.0266(2) Uani 1 1 d . . . . .
O3 O 0.37830(9) 0.56969(10) 0.29307(5) 0.0339(3) Uani 1 1 d . . . . .
N1 N 0.59119(9) 0.53285(10) 0.39744(5) 0.0217(2) Uani 1 1 d . . . . .
N2 N 0.50830(9) 0.60995(10) 0.39184(5) 0.0201(2) Uani 1 1 d . . . . .
N3 N 0.88637(9) 0.29026(10) 0.31760(5) 0.0224(2) Uani 1 1 d . . . . .
C1 C 0.62457(10) 0.51078(11) 0.34141(6) 0.0206(3) Uani 1 1 d . . . . .
C2 C 0.71561(10) 0.43389(11) 0.33412(6) 0.0203(3) Uani 1 1 d . . . . .
C8 C 0.37926(11) 0.72129(12) 0.44541(6) 0.0238(3) Uani 1 1 d . . . . .
C6 C 0.78896(10) 0.42295(12) 0.38059(6) 0.0232(3) Uani 1 1 d . . . . .
H6 H 0.781555 0.463581 0.418817 0.028 Uiso 1 1 calc R U . . .
C5 C 0.87282(11) 0.35171(12) 0.36994(6) 0.0234(3) Uani 1 1 d . . . . .
H5 H 0.923545 0.346009 0.401408 0.028 Uiso 1 1 calc R U . . .
C9 C 0.35050(11) 0.79029(12) 0.39391(7) 0.0238(3) Uani 1 1 d . . . . .
C3 C 0.72998(11) 0.37287(12) 0.27909(7) 0.0244(3) Uani 1 1 d . . . . .
H3 H 0.682313 0.380146 0.245999 0.029 Uiso 1 1 calc R U . . .
C7 C 0.46314(10) 0.63919(12) 0.44268(7) 0.0224(3) Uani 1 1 d . . . . .
H7 H 0.486332 0.604860 0.480313 0.027 Uiso 1 1 calc R U . . .
C4 C 0.81500(11) 0.30125(13) 0.27332(7) 0.0258(3) Uani 1 1 d . . . . .
H4 H 0.823202 0.257641 0.236076 0.031 Uiso 1 1 calc R U . . .
C13 C 0.32746(12) 0.73583(13) 0.50201(7) 0.0315(3) Uani 1 1 d . . . . .
H13 H 0.346814 0.689654 0.536785 0.038 Uiso 1 1 calc R U . . .
C10 C 0.27095(12) 0.87187(14) 0.40033(8) 0.0327(3) Uani 1 1 d . . . . .
H10 H 0.250852 0.918881 0.366022 0.039 Uiso 1 1 calc R U . . .
C12 C 0.24917(15) 0.81585(15) 0.50787(8) 0.0390(4) Uani 1 1 d . . . . .
H12 H 0.214257 0.824646 0.546265 0.047 Uiso 1 1 calc R U . . .
C11 C 0.22173(13) 0.88379(15) 0.45684(9) 0.0393(4) Uani 1 1 d . . . . .
H11 H 0.168034 0.939562 0.460885 0.047 Uiso 1 1 calc R U . . .
C14 C 0.45054(15) 0.67285(18) 0.16497(8) 0.0412(4) Uani 1 1 d . . . . .
H14A H 0.425451 0.739260 0.139533 0.049 Uiso 1 1 calc R U . . .
H14B H 0.392833 0.617715 0.171247 0.049 Uiso 1 1 calc R U . . .
C15 C 0.53410(18) 0.6122(2) 0.13153(11) 0.0607(6) Uani 1 1 d . . . . .
H15A H 0.508634 0.583831 0.091461 0.091 Uiso 1 1 calc R U . . .
H15B H 0.558171 0.545469 0.156282 0.091 Uiso 1 1 calc R U . . .
H15C H 0.590872 0.666954 0.124675 0.091 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 O1 1.9650(10) . ?
V1 O2 1.8657(10) . ?
V1 O4 1.7659(11) . ?
V1 O3 1.5893(11) . ?
V1 N2 2.1357(11) . ?
V1 N3 2.4187(12) 8_765 ?
O1 C1 1.2957(16) . ?
O2 C9 1.3323(17) . ?
O4 C14 1.4185(19) . ?
N1 N2 1.3986(15) . ?
N1 C1 1.3083(18) . ?
N2 C7 1.2881(18) . ?
N3 C5 1.3395(18) . ?
N3 C4 1.3396(18) . ?
C1 C2 1.4844(18) . ?
C2 C6 1.3913(19) . ?
C2 C3 1.3875(19) . ?
C8 C9 1.411(2) . ?
C8 C7 1.4411(19) . ?
C8 C13 1.404(2) . ?
C6 H6 0.9500 . ?
C6 C5 1.3817(19) . ?
C5 H5 0.9500 . ?
C9 C10 1.400(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(2) . ?
C7 H7 0.9500 . ?
C4 H4 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.375(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.384(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.392(3) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.479(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
O1 V1 N2 74.14(4) . . ?
O1 V1 N3 78.42(4) . 8_765 ?
O2 V1 O1 151.76(4) . . ?
O2 V1 N2 83.40(4) . . ?
O2 V1 N3 81.15(4) . 8_765 ?
O4 V1 O1 92.59(4) . . ?
O4 V1 O2 103.48(5) . . ?
O4 V1 N2 159.31(5) . . ?
O4 V1 N3 81.53(4) . 8_765 ?
O3 V1 O1 98.15(5) . . ?
O3 V1 O2 100.50(5) . . ?
O3 V1 O4 103.19(5) . . ?
O3 V1 N2 94.52(5) . . ?
O3 V1 N3 174.38(5) . 8_765 ?
N2 V1 N3 80.29(4) . 8_765 ?
C1 O1 V1 117.70(8) . . ?
C9 O2 V1 132.96(9) . . ?
C14 O4 V1 132.35(11) . . ?
C1 N1 N2 107.38(10) . . ?
N1 N2 V1 116.17(8) . . ?
C7 N2 V1 127.52(9) . . ?
C7 N2 N1 116.29(11) . . ?
C5 N3 V1 123.57(9) . 8_755 ?
C5 N3 C4 117.36(12) . . ?
C4 N3 V1 119.07(9) . 8_755 ?
O1 C1 N1 124.56(12) . . ?
O1 C1 C2 116.90(11) . . ?
N1 C1 C2 118.54(12) . . ?
C6 C2 C1 121.83(12) . . ?
C3 C2 C1 119.62(12) . . ?
C3 C2 C6 118.53(12) . . ?
C9 C8 C7 122.10(12) . . ?
C13 C8 C9 119.32(13) . . ?
C13 C8 C7 118.54(13) . . ?
C2 C6 H6 120.7 . . ?
C5 C6 C2 118.57(12) . . ?
C5 C6 H6 120.7 . . ?
N3 C5 C6 123.46(13) . . ?
N3 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
O2 C9 C8 121.38(12) . . ?
O2 C9 C10 119.24(13) . . ?
C10 C9 C8 119.28(13) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.74(13) . . ?
C4 C3 H3 120.6 . . ?
N2 C7 C8 123.38(13) . . ?
N2 C7 H7 118.3 . . ?
C8 C7 H7 118.3 . . ?
N3 C4 C3 123.30(13) . . ?
N3 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
C8 C13 H13 119.5 . . ?
C12 C13 C8 121.05(15) . . ?
C12 C13 H13 119.5 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.77(15) . . ?
C11 C10 H10 120.1 . . ?
C13 C12 H12 120.4 . . ?
C13 C12 C11 119.14(15) . . ?
C11 C12 H12 120.4 . . ?
C10 C11 C12 121.45(15) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
O4 C14 H14A 109.3 . . ?
O4 C14 H14B 109.3 . . ?
O4 C14 C15 111.45(16) . . ?
H14A C14 H14B 108.0 . . ?
C15 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
V1 O1 C1 N1 2.76(17) . . . . ?
V1 O1 C1 C2 -176.43(8) . . . . ?
V1 O2 C9 C8 32.5(2) . . . . ?
V1 O2 C9 C10 -151.21(11) . . . . ?
V1 O4 C14 C15 -100.8(2) . . . . ?
V1 N2 C7 C8 -4.3(2) . . . . ?
V1 N3 C5 C6 -178.57(10) 8_755 . . . ?
V1 N3 C4 C3 -179.58(11) 8_755 . . . ?
O1 V1 O2 C9 -72.39(16) . . . . ?
O1 V1 O4 C14 82.54(14) . . . . ?
O1 C1 C2 C6 153.13(13) . . . . ?
O1 C1 C2 C3 -25.37(18) . . . . ?
O2 V1 O4 C14 -120.86(14) . . . . ?
O2 C9 C10 C11 -176.35(15) . . . . ?
O4 V1 O2 C9 164.60(12) . . . . ?
O3 V1 O2 C9 58.16(13) . . . . ?
O3 V1 O4 C14 -16.46(15) . . . . ?
N1 N2 C7 C8 177.44(12) . . . . ?
N1 C1 C2 C6 -26.11(19) . . . . ?
N1 C1 C2 C3 155.38(13) . . . . ?
N2 V1 O2 C9 -35.23(12) . . . . ?
N2 V1 O4 C14 131.68(16) . . . . ?
N2 N1 C1 O1 -1.41(18) . . . . ?
N2 N1 C1 C2 177.77(11) . . . . ?
N3 V1 O2 C9 -116.39(13) 8_765 . . . ?
N3 V1 O4 C14 160.43(14) 8_765 . . . ?
C1 N1 N2 V1 -0.45(13) . . . . ?
C1 N1 N2 C7 178.04(12) . . . . ?
C1 C2 C6 C5 -178.60(12) . . . . ?
C1 C2 C3 C4 -179.69(12) . . . . ?
C2 C6 C5 N3 -1.5(2) . . . . ?
C2 C3 C4 N3 -2.1(2) . . . . ?
C8 C9 C10 C11 0.0(2) . . . . ?
C8 C13 C12 C11 -0.5(3) . . . . ?
C6 C2 C3 C4 1.8(2) . . . . ?
C5 N3 C4 C3 0.6(2) . . . . ?
C9 C8 C7 N2 -10.3(2) . . . . ?
C9 C8 C13 C12 0.2(2) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C3 C2 C6 C5 -0.1(2) . . . . ?
C7 C8 C9 O2 -1.2(2) . . . . ?
C7 C8 C9 C10 -177.42(14) . . . . ?
C7 C8 C13 C12 177.75(15) . . . . ?
C4 N3 C5 C6 1.3(2) . . . . ?
C13 C8 C9 O2 176.31(13) . . . . ?
C13 C8 C9 C10 0.0(2) . . . . ?
C13 C8 C7 N2 172.22(14) . . . . ?
C13 C12 C11 C10 0.5(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
