# Supplementary Information (SI) for Dalton Transactions.
# 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_2271
_database_code_depnum_ccdc_archive 'CCDC 2367618'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-19 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
butoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v)
_chemical_formula_moiety         'C18 H20 N3 O5 V'
_chemical_formula_sum            'C18 H20 N3 O5 V'
_chemical_formula_weight         409.31
_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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   11.7033(9)
_cell_length_b                   15.0094(10)
_cell_length_c                   10.7908(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1895.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3542
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.7710
_cell_measurement_theta_min      2.9270
_shelx_estimated_absorpt_T_max   0.800
_shelx_estimated_absorpt_T_min   0.627
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_T_max  0.42270
_exptl_absorpt_correction_T_min  0.35840
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.123
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7936
_diffrn_reflns_point_group_measured_fraction_full 0.732
_diffrn_reflns_point_group_measured_fraction_max 0.692
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.471
_diffrn_reflns_theta_min         2.944
_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 0.962
_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  21.00   0.50    1.50    --  -47.03  78.00 105.00  106
  2  ω     -7.00  35.00   0.50    1.50    --   47.03 -78.00 -19.00   84
  3  ω    -71.00 -45.00   0.50    4.00    --  -86.25  78.00 105.00   52
  4  ω     39.00  79.00   0.50    4.00    --  106.40 -78.00 -19.00   80
  5  ω    115.00 141.00   0.50    4.00    --  106.40  78.00 105.00   52
  6  ω   -102.00 -77.00   0.50    1.50    --  -47.03-125.00-120.00   50
  7  ω   -116.00 -74.00   0.50    1.50    --  -47.03-125.00 120.00   84
  8  ω    -43.00 -13.00   0.50    4.00    --  -86.25  38.00 120.00   60
  9  ω    -42.00 -15.00   0.50    4.00    --  -86.25  38.00  60.00   54
 10  ω     38.00 103.00   0.50    4.00    --  106.40 -77.00  90.00  130
 11  ω     34.00  66.00   0.50    4.00    --  106.40 -57.00   0.00   64
 12  ω     43.00 101.00   0.50    4.00    --  106.40 -99.00 -90.00  116
 13  ω     45.00  72.00   0.50    4.00    --  106.40 -77.00 150.00   54
 14  ω     36.00  66.00   0.50    4.00    --  106.40 -57.00 150.00   60
 15  ω     38.00  64.00   0.50    4.00    --  106.40 -57.00 -90.00   52
 16  ω     35.00  60.00   0.50    4.00    --  106.40 -57.00 120.00   50
 17  ω     52.00 104.00   0.50    4.00    --  106.40 -77.00-180.00  104
 18  ω     83.00 109.00   0.50    4.00    --  106.40 -78.00 -19.00   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         0.361
_reflns_Friedel_fraction_full    0.432
_reflns_Friedel_fraction_max     0.390
_reflns_number_gt                2423
_reflns_number_total             2792
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 
;
 Flack x determined using 563 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(12)
_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     268
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.090
_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)+(0.0756P)²+1.5163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1424
_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) groups
2. Restrained distances
 C24-C25A
 1.52 with sigma of 0.02
 C24-C25
 1.52 with sigma of 0.012
 C25-C27
 2.54 with sigma of 0.04
 C25A-C27A
 2.54 with sigma of 0.04
 C25-C26 \\sim C26-C27
 with sigma of 0.02
 C25A-C26A \\sim C26A-C27A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C25A \\sim C26A \\sim C27A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C26A, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H24A(0.666667) H24B(0.666667) H24C(0.333333) H24D(0.333333)
 C25(0.666667) H25A(0.666667) H25B(0.666667) C26(0.666667) H26A(0.666667)
 H26B(0.666667) C27(0.666667) H27A(0.666667) H27B(0.666667) H27C(0.666667)
 C25A(0.333333) H25C(0.333333) H25D(0.333333) C26A(0.333333) H26C(0.333333)
 H26D(0.333333) C27A(0.333333) H27D(0.333333) H27E(0.333333) H27F(0.333333)
6.a Free rotating group:
 C25(C26,C27), C25A(C26A,C27A)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24(H24C,H24D), C25(H25A,H25B), C26(H26A,H26B), C25A(H25C,
 H25D), C26A(H26C,H26D)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C7(H7), C5(H5), C18(H18), C21(H21), C11(H11), C20(H20)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F)
;
_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 0.57741(7) 0.74049(5) 0.44456(12) 0.0247(2) Uani 1 1 d . . . . .
O2 O 0.4644(4) 0.7972(3) 0.3513(5) 0.0304(9) Uani 1 1 d . . . . .
O22 O 0.6611(4) 0.8228(2) 0.4658(5) 0.0331(10) Uani 1 1 d . . . . .
O15 O 0.6904(3) 0.6429(2) 0.4681(4) 0.0286(9) Uani 1 1 d . . . . .
O23 O 0.5142(4) 0.7294(3) 0.5933(4) 0.0315(10) Uani 1 1 d . . . . .
N12 N 0.6419(4) 0.7103(3) 0.2656(5) 0.0247(10) Uani 1 1 d . . . . .
O9 O 0.3202(4) 0.9302(3) 0.3282(5) 0.0368(10) Uani 1 1 d . . . . .
N13 N 0.7145(5) 0.6364(3) 0.2563(5) 0.0295(11) Uani 1 1 d . . . . .
N19 N 0.9626(4) 0.3876(3) 0.4089(5) 0.0296(11) Uani 1 1 d . . . . .
C14 C 0.7343(5) 0.6081(4) 0.3687(6) 0.0273(12) Uani 1 1 d . . . . .
C17 C 0.8626(6) 0.5135(4) 0.4954(6) 0.0317(14) Uani 1 1 d . . . . .
H17 H 0.845629 0.548880 0.565986 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4772(5) 0.8509(4) 0.2532(6) 0.0275(12) Uani 1 1 d . . . . .
C6 C 0.4981(7) 0.9654(4) 0.0508(8) 0.0416(16) Uani 1 1 d . . . . .
H6 H 0.507408 1.006260 -0.015601 0.050 Uiso 1 1 calc R U . . .
C16 C 0.8135(5) 0.5326(4) 0.3827(6) 0.0281(13) Uani 1 1 d . . . . .
C7 C 0.4119(6) 0.9784(4) 0.1360(8) 0.0370(15) Uani 1 1 d . . . . .
H7 H 0.359645 1.026201 0.124979 0.044 Uiso 1 1 calc R U . . .
C5 C 0.5702(6) 0.8942(4) 0.0612(7) 0.0350(14) Uani 1 1 d . . . . .
H5 H 0.627062 0.884307 -0.000094 0.042 Uiso 1 1 calc R U . . .
C10 C 0.2368(7) 0.9986(5) 0.3128(8) 0.0497(19) Uani 1 1 d . . . . .
H10A H 0.194635 0.988578 0.235561 0.074 Uiso 1 1 calc R U . . .
H10B H 0.274879 1.056676 0.309376 0.074 Uiso 1 1 calc R U . . .
H10C H 0.183512 0.997494 0.382854 0.074 Uiso 1 1 calc R U . . .
C18 C 0.9371(6) 0.4418(4) 0.5049(7) 0.0349(15) Uani 1 1 d . . . . .
H18 H 0.971927 0.430359 0.582770 0.042 Uiso 1 1 calc R U . . .
C21 C 0.8416(6) 0.4787(4) 0.2811(7) 0.0370(15) Uani 1 1 d . . . . .
H21 H 0.811001 0.491191 0.201468 0.044 Uiso 1 1 calc R U . . .
C11 C 0.6318(5) 0.7586(4) 0.1674(6) 0.0292(13) Uani 1 1 d . . . . .
H11 H 0.673725 0.742513 0.095401 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5603(5) 0.8353(4) 0.1629(7) 0.0319(14) Uani 1 1 d . . . . .
C8 C 0.4007(5) 0.9220(4) 0.2384(6) 0.0295(13) Uani 1 1 d . . . . .
C20 C 0.9140(6) 0.4075(4) 0.2981(7) 0.0345(15) Uani 1 1 d . . . . .
H20 H 0.930735 0.370441 0.229073 0.041 Uiso 1 1 calc R U . . .
C24 C 0.5368(7) 0.7768(6) 0.7038(8) 0.051(2) Uani 1 1 d D . . . .
H24A H 0.579031 0.832213 0.684574 0.061 Uiso 0.6667 1 calc R U P A 1
H24B H 0.584508 0.740075 0.759761 0.061 Uiso 0.6667 1 calc R U P A 1
H24C H 0.499924 0.835993 0.697648 0.061 Uiso 0.3333 1 calc R U P B 2
H24D H 0.620215 0.786693 0.709697 0.061 Uiso 0.3333 1 calc R U P B 2
C25 C 0.4264(11) 0.7989(9) 0.7658(15) 0.078(5) Uani 0.6667 1 d DG U P C 1
H25A H 0.383700 0.838563 0.708954 0.094 Uiso 0.6667 1 calc R U P C 1
H25B H 0.445050 0.834581 0.840251 0.094 Uiso 0.6667 1 calc R U P C 1
C26 C 0.3441(12) 0.7254(10) 0.8067(16) 0.091(5) Uani 0.6667 1 d DG U P C 1
H26A H 0.265269 0.749357 0.807801 0.109 Uiso 0.6667 1 calc R U P C 1
H26B H 0.346610 0.676102 0.745837 0.109 Uiso 0.6667 1 calc R U P C 1
C27 C 0.374(3) 0.6891(15) 0.9353(19) 0.142(11) Uani 0.6667 1 d DG U P C 1
H27A H 0.455541 0.676267 0.939568 0.213 Uiso 0.6667 1 calc R U P C 1
H27B H 0.330269 0.634229 0.950332 0.213 Uiso 0.6667 1 calc R U P C 1
H27C H 0.353630 0.733463 0.998294 0.213 Uiso 0.6667 1 calc R U P C 1
C25A C 0.497(2) 0.7332(17) 0.822(2) 0.074(8) Uani 0.3333 1 d DG U P C 2
H25C H 0.487455 0.784929 0.877686 0.089 Uiso 0.3333 1 calc R U P C 2
H25D H 0.567840 0.703483 0.851080 0.089 Uiso 0.3333 1 calc R U P C 2
C26A C 0.404(2) 0.6696(15) 0.867(3) 0.091(9) Uani 0.3333 1 d DG U P C 2
H26C H 0.361066 0.646702 0.794404 0.109 Uiso 0.3333 1 calc R U P C 2
H26D H 0.439993 0.618165 0.908868 0.109 Uiso 0.3333 1 calc R U P C 2
C27A C 0.321(2) 0.715(2) 0.956(3) 0.071(10) Uani 0.3333 1 d DG U P C 2
H27D H 0.298711 0.773198 0.922760 0.107 Uiso 0.3333 1 calc R U P C 2
H27E H 0.357816 0.722982 1.036806 0.107 Uiso 0.3333 1 calc R U P C 2
H27F H 0.252597 0.677755 0.965994 0.107 Uiso 0.3333 1 calc R 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
V1 O2 1.867(4) . ?
V1 O22 1.593(4) . ?
V1 O15 1.989(4) . ?
V1 O23 1.776(5) . ?
V1 N12 2.122(5) . ?
V1 N19 2.377(5) 3_465 ?
O2 C3 1.339(8) . ?
O15 C14 1.299(7) . ?
O23 C24 1.413(9) . ?
N12 N13 1.401(6) . ?
N12 C11 1.289(8) . ?
O9 C10 1.426(8) . ?
O9 C8 1.357(8) . ?
N13 C14 1.305(8) . ?
N19 C18 1.350(9) . ?
N19 C20 1.357(9) . ?
C14 C16 1.473(8) . ?
C17 H17 0.9500 . ?
C17 C16 1.375(9) . ?
C17 C18 1.389(9) . ?
C3 C4 1.396(10) . ?
C3 C8 1.402(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(11) . ?
C6 C5 1.365(9) . ?
C16 C21 1.401(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.399(9) . ?
C5 H5 0.9500 . ?
C5 C4 1.415(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C18 H18 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.377(9) . ?
C11 H11 0.9500 . ?
C11 C4 1.424(8) . ?
C20 H20 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 H24C 0.9900 . ?
C24 H24D 0.9900 . ?
C24 C25 1.491(11) . ?
C24 C25A 1.503(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.5303 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.5300 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C25A C26A 1.5306 . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C27A 1.5300 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 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
O2 V1 O15 151.0(2) . . ?
O2 V1 N12 81.8(2) . . ?
O2 V1 N19 83.16(18) . 3_465 ?
O22 V1 O2 99.2(2) . . ?
O22 V1 O15 98.30(19) . . ?
O22 V1 O23 101.5(2) . . ?
O22 V1 N12 94.5(2) . . ?
O22 V1 N19 176.4(2) . 3_465 ?
O15 V1 N12 73.90(18) . . ?
O15 V1 N19 78.51(17) . 3_465 ?
O23 V1 O2 103.6(2) . . ?
O23 V1 O15 95.3(2) . . ?
O23 V1 N12 161.96(19) . . ?
O23 V1 N19 80.49(19) . 3_465 ?
N12 V1 N19 83.16(19) . 3_465 ?
C3 O2 V1 128.5(4) . . ?
C14 O15 V1 117.0(4) . . ?
C24 O23 V1 129.6(4) . . ?
N13 N12 V1 116.7(4) . . ?
C11 N12 V1 126.5(4) . . ?
C11 N12 N13 116.2(5) . . ?
C8 O9 C10 117.2(5) . . ?
C14 N13 N12 107.4(5) . . ?
C18 N19 V1 119.2(4) . 3_565 ?
C18 N19 C20 116.8(5) . . ?
C20 N19 V1 123.8(4) . 3_565 ?
O15 C14 N13 124.5(5) . . ?
O15 C14 C16 118.2(5) . . ?
N13 C14 C16 117.3(5) . . ?
C16 C17 H17 120.4 . . ?
C16 C17 C18 119.3(6) . . ?
C18 C17 H17 120.4 . . ?
O2 C3 C4 121.9(5) . . ?
O2 C3 C8 118.5(6) . . ?
C4 C3 C8 119.5(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(6) . . ?
C17 C16 C14 121.0(6) . . ?
C17 C16 C21 118.3(5) . . ?
C21 C16 C14 120.8(6) . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.1(7) . . ?
C4 C5 H5 119.9 . . ?
O9 C10 H10A 109.5 . . ?
O9 C10 H10B 109.5 . . ?
O9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N19 C18 C17 123.3(6) . . ?
N19 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C16 C21 H21 120.4 . . ?
C20 C21 C16 119.2(6) . . ?
C20 C21 H21 120.4 . . ?
N12 C11 H11 118.8 . . ?
N12 C11 C4 122.4(6) . . ?
C4 C11 H11 118.8 . . ?
C3 C4 C5 119.6(6) . . ?
C3 C4 C11 121.4(6) . . ?
C5 C4 C11 118.9(6) . . ?
O9 C8 C3 115.5(6) . . ?
O9 C8 C7 125.0(5) . . ?
C7 C8 C3 119.4(6) . . ?
N19 C20 C21 123.1(6) . . ?
N19 C20 H20 118.5 . . ?
C21 C20 H20 118.5 . . ?
O23 C24 H24A 109.8 . . ?
O23 C24 H24B 109.8 . . ?
O23 C24 H24C 108.3 . . ?
O23 C24 H24D 108.3 . . ?
O23 C24 C25 109.2(9) . . ?
O23 C24 C25A 116.0(12) . . ?
H24A C24 H24B 108.3 . . ?
H24C C24 H24D 107.4 . . ?
C25 C24 H24A 109.8 . . ?
C25 C24 H24B 109.8 . . ?
C25A C24 H24C 108.3 . . ?
C25A C24 H24D 108.3 . . ?
C24 C25 H25A 107.1 . . ?
C24 C25 H25B 107.1 . . ?
C24 C25 C26 120.9(11) . . ?
H25A C25 H25B 106.8 . . ?
C26 C25 H25A 107.1 . . ?
C26 C25 H25B 107.1 . . ?
C25 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 C25 112.1 . . ?
C27 C26 H26A 109.2 . . ?
C27 C26 H26B 109.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C25A H25C 102.2 . . ?
C24 C25A H25D 102.2 . . ?
C24 C25A C26A 139(3) . . ?
H25C C25A H25D 104.8 . . ?
C26A C25A H25C 102.2 . . ?
C26A C25A H25D 102.2 . . ?
C25A C26A H26C 109.2 . . ?
C25A C26A H26D 109.2 . . ?
H26C C26A H26D 107.9 . . ?
C27A C26A C25A 112.1 . . ?
C27A C26A H26C 109.2 . . ?
C27A C26A H26D 109.2 . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 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 O2 C3 C4 38.3(8) . . . . ?
V1 O2 C3 C8 -145.0(5) . . . . ?
V1 O15 C14 N13 4.3(7) . . . . ?
V1 O15 C14 C16 -176.8(4) . . . . ?
V1 O23 C24 C25 137.4(8) . . . . ?
V1 O23 C24 C25A -161.0(12) . . . . ?
V1 N12 N13 C14 -6.4(6) . . . . ?
V1 N12 C11 C4 -9.1(9) . . . . ?
V1 N19 C18 C17 -174.0(5) 3_565 . . . ?
V1 N19 C20 C21 175.5(5) 3_565 . . . ?
O2 V1 O23 C24 -106.1(6) . . . . ?
O2 C3 C4 C5 -179.9(6) . . . . ?
O2 C3 C4 C11 3.3(10) . . . . ?
O2 C3 C8 O9 0.9(8) . . . . ?
O2 C3 C8 C7 -179.4(6) . . . . ?
O22 V1 O2 C3 47.6(5) . . . . ?
O22 V1 O23 C24 -3.6(7) . . . . ?
O15 V1 O2 C3 -78.8(6) . . . . ?
O15 V1 O23 C24 96.0(6) . . . . ?
O15 C14 C16 C17 -16.3(9) . . . . ?
O15 C14 C16 C21 164.3(6) . . . . ?
O23 V1 O2 C3 151.9(5) . . . . ?
O23 C24 C25 C26 59.9(15) . . . . ?
O23 C24 C25A C26A -29(3) . . . . ?
N12 V1 O2 C3 -45.6(5) . . . . ?
N12 V1 O23 C24 148.1(7) . . . . ?
N12 N13 C14 O15 1.6(8) . . . . ?
N12 N13 C14 C16 -177.4(5) . . . . ?
N12 C11 C4 C3 -15.2(10) . . . . ?
N12 C11 C4 C5 168.0(6) . . . . ?
N13 N12 C11 C4 179.5(5) . . . . ?
N13 C14 C16 C17 162.7(6) . . . . ?
N13 C14 C16 C21 -16.7(9) . . . . ?
N19 V1 O2 C3 -129.7(5) 3_465 . . . ?
N19 V1 O23 C24 173.4(7) 3_465 . . . ?
C14 C16 C21 C20 -178.6(6) . . . . ?
C17 C16 C21 C20 1.9(10) . . . . ?
C6 C7 C8 O9 178.8(7) . . . . ?
C6 C7 C8 C3 -0.9(10) . . . . ?
C6 C5 C4 C3 -0.6(10) . . . . ?
C6 C5 C4 C11 176.2(7) . . . . ?
C16 C17 C18 N19 -1.6(10) . . . . ?
C16 C21 C20 N19 -1.7(11) . . . . ?
C7 C6 C5 C4 -2.9(12) . . . . ?
C5 C6 C7 C8 3.7(12) . . . . ?
C10 O9 C8 C3 -176.5(6) . . . . ?
C10 O9 C8 C7 3.8(9) . . . . ?
C18 N19 C20 C21 -0.2(10) . . . . ?
C18 C17 C16 C14 -179.8(6) . . . . ?
C18 C17 C16 C21 -0.3(10) . . . . ?
C11 N12 N13 C14 165.9(5) . . . . ?
C4 C3 C8 O9 177.7(5) . . . . ?
C4 C3 C8 C7 -2.6(9) . . . . ?
C8 C3 C4 C5 3.4(9) . . . . ?
C8 C3 C4 C11 -173.4(6) . . . . ?
C20 N19 C18 C17 1.9(10) . . . . ?
C24 C25 C26 C27 86(2) . . . . ?
C24 C25A C26A C27A -114(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_4948
_database_code_depnum_ccdc_archive 'CCDC 2367621'
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.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_vrf_PLAT430_exp_4948            
;
PROBLEM: Short Inter D...A Contact  O9       ..N19      .       2.76 Ang.  
RESPONSE: V-py coordination tetramer.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        
tetrakis(propoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v))
_chemical_formula_moiety         'C17 H18 N3 O5 V'
_chemical_formula_sum            'C17 H18 N3 O5 V'
_chemical_formula_weight         395.28
_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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.5584(2)
_cell_length_b                   17.5584(2)
_cell_length_c                   22.6538(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6984.1(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.0480
_cell_measurement_theta_min      3.1740
_shelx_estimated_absorpt_T_max   0.751
_shelx_estimated_absorpt_T_min   0.517
_exptl_absorpt_coefficient_mu    5.058
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (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    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 -2 0.0291
1 1 2 0.0399
1 -1 -2 0.0484
-1 1 2 0.0329
0 -1 2 0.0276
0 1 -2 0.0276

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14473
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.331
_diffrn_reflns_theta_min         3.184
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -46.00   0.50    5.43    --  -46.93 -45.00-134.00   74
  2  ω    -49.00  19.00   0.50    5.43    --  -46.93  45.00  15.00  136
  3  ω     76.00 101.00   0.50    5.43    --   46.93  45.00  15.00   50
  4  ω    -51.00 -26.00   0.50   21.73    --  -86.25  45.00  15.00   50
  5  ω    102.00 177.00   0.50   21.73    --  106.38  45.00  15.00  150
  6  ω   -119.00 -87.00   0.50    5.43    --  -46.93-125.00  30.00   64
  7  ω   -117.00 -85.00   0.50    5.43    --  -46.93-125.00 -30.00   64
  8  ω    -43.00 -13.00   0.50   21.73    --  -86.25  38.00  90.00   60
  9  ω    -59.00 -33.00   0.50   21.73    --  -86.25  57.00-120.00   52
 10  ω    -43.00 -18.00   0.50   21.73    --  -86.25  38.00-180.00   50
 11  ω    -40.00 -14.00   0.50   21.73    --  -86.25  38.00-150.00   52
 12  ω    105.00 177.00   0.50   21.73    --  106.38 125.00-150.00  144
 13  ω     39.00  98.00   0.50   21.73    --  106.38 -99.00  60.00  118
 14  ω    106.00 177.00   0.50   21.73    --  106.38  57.00 120.00  142
 15  ω     39.00  65.00   0.50   21.73    --  106.38 -77.00  30.00   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                2828
_reflns_number_total             3531
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 (Sheldrick, 2015)'
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.042
_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)+(0.0951P)²+4.6355P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1585
_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:
 C24(H24A,H24B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C18(H18), C17(H17), C11(H11), C21(H21), C13(H13), C12(H12), C20(H20)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C26(H26A,H26B,H26C)
;
_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 0.14210(3) 0.35651(3) 0.39708(2) 0.0497(2) Uani 1 1 d . . . . .
O2 O 0.20108(12) 0.26482(11) 0.37749(9) 0.0540(5) Uani 1 1 d . . . . .
O9 O 0.13249(12) 0.44890(11) 0.43544(9) 0.0561(5) Uani 1 1 d . . . . .
O23 O 0.12263(12) 0.37849(12) 0.32223(10) 0.0595(5) Uani 1 1 d . . . . .
O22 O 0.06539(13) 0.31518(13) 0.41574(12) 0.0696(6) Uani 1 1 d . . . . .
O14 O 0.06967(14) 0.58136(12) 0.45502(11) 0.0658(6) Uani 1 1 d . . . . .
N19 N 0.33343(14) 0.01323(13) 0.37765(11) 0.0508(5) Uani 1 1 d . . . . .
N5 N 0.19499(14) 0.32162(13) 0.47759(11) 0.0518(5) Uani 1 1 d . . . . .
N4 N 0.23208(15) 0.25090(13) 0.47551(11) 0.0561(6) Uani 1 1 d . . . . .
C8 C 0.12320(15) 0.46888(16) 0.49148(13) 0.0494(6) Uani 1 1 d . . . . .
C16 C 0.26522(16) 0.15229(16) 0.40729(13) 0.0506(6) Uani 1 1 d . . . . .
C6 C 0.18704(17) 0.35212(17) 0.52888(14) 0.0546(7) Uani 1 1 d . . . . .
H6 H 0.207559 0.326910 0.561291 0.065 Uiso 1 1 calc R U . . .
C3 C 0.23101(16) 0.22742(16) 0.42141(13) 0.0499(6) Uani 1 1 d . . . . .
C7 C 0.14796(16) 0.42340(17) 0.53887(14) 0.0525(7) Uani 1 1 d . . . . .
C18 C 0.28967(19) 0.05097(18) 0.33966(14) 0.0581(7) Uani 1 1 d . . . . .
H18 H 0.281581 0.029617 0.302615 0.070 Uiso 1 1 calc R U . . .
C10 C 0.08896(16) 0.54019(17) 0.50369(14) 0.0533(7) Uani 1 1 d . . . . .
C17 C 0.25550(18) 0.12014(18) 0.35209(14) 0.0574(7) Uani 1 1 d . . . . .
H17 H 0.226316 0.144740 0.323622 0.069 Uiso 1 1 calc R U . . .
C11 C 0.07748(19) 0.5624(2) 0.56143(15) 0.0634(8) Uani 1 1 d . . . . .
H11 H 0.054787 0.609063 0.569526 0.076 Uiso 1 1 calc R U . . .
C21 C 0.3081(2) 0.11189(19) 0.44779(15) 0.0670(9) Uani 1 1 d . . . . .
H21 H 0.314739 0.130105 0.485993 0.080 Uiso 1 1 calc R U . . .
C13 C 0.13638(19) 0.4478(2) 0.59687(15) 0.0628(8) Uani 1 1 d . . . . .
H13 H 0.153618 0.418263 0.628220 0.075 Uiso 1 1 calc R U . . .
C12 C 0.0997(2) 0.5151(2) 0.60757(16) 0.0692(9) Uani 1 1 d . . . . .
H12 H 0.089541 0.529463 0.646286 0.083 Uiso 1 1 calc R U . . .
C20 C 0.3410(2) 0.04390(19) 0.43043(15) 0.0642(8) Uani 1 1 d . . . . .
H20 H 0.370495 0.017978 0.457962 0.077 Uiso 1 1 calc R U . . .
C24 C 0.0556(2) 0.3567(2) 0.29057(18) 0.0778(10) Uani 1 1 d . . . . .
H24A H 0.021481 0.400016 0.287668 0.093 Uiso 1 1 calc R U . . .
H24B H 0.029450 0.316646 0.311943 0.093 Uiso 1 1 calc R U . . .
C15 C 0.0485(2) 0.6589(2) 0.46302(19) 0.0765(10) Uani 1 1 d . . . . .
H15A H 0.041717 0.682552 0.425190 0.115 Uiso 1 1 calc R U . . .
H15B H 0.087880 0.684963 0.484394 0.115 Uiso 1 1 calc R U . . .
H15C H 0.001763 0.661408 0.484866 0.115 Uiso 1 1 calc R U . . .
C25 C 0.0746(3) 0.3302(3) 0.2321(2) 0.0953(13) Uani 1 1 d . . . . .
H25A H 0.027844 0.318288 0.211230 0.114 Uiso 1 1 calc R U . . .
H25B H 0.099761 0.371045 0.210870 0.114 Uiso 1 1 calc R U . . .
C26 C 0.1229(3) 0.2644(3) 0.2315(2) 0.1042(15) Uani 1 1 d . . . . .
H26A H 0.124253 0.243325 0.192416 0.156 Uiso 1 1 calc R U . . .
H26B H 0.103318 0.226993 0.258486 0.156 Uiso 1 1 calc R U . . .
H26C H 0.173440 0.278653 0.243265 0.156 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 O2 1.965(2) . ?
V1 O9 1.848(2) . ?
V1 O23 1.772(2) . ?
V1 O22 1.587(2) . ?
V1 N19 2.439(2) 11_666 ?
V1 N5 2.136(2) . ?
O2 C3 1.303(4) . ?
O9 C8 1.327(4) . ?
O23 C24 1.430(4) . ?
O14 C10 1.361(4) . ?
O14 C15 1.422(4) . ?
N19 C18 1.330(4) . ?
N19 C20 1.318(4) . ?
N5 N4 1.403(3) . ?
N5 C6 1.287(4) . ?
N4 C3 1.293(4) . ?
C8 C7 1.407(4) . ?
C8 C10 1.416(4) . ?
C16 C3 1.484(4) . ?
C16 C17 1.383(4) . ?
C16 C21 1.383(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.445(4) . ?
C7 C13 1.397(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.384(4) . ?
C10 C11 1.380(5) . ?
C17 H17 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.391(5) . ?
C21 H21 0.9300 . ?
C21 C20 1.383(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.367(5) . ?
C12 H12 0.9300 . ?
C20 H20 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.443(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.434(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 N19 80.96(8) . 11_666 ?
O2 V1 N5 74.26(9) . . ?
O9 V1 O2 150.87(10) . . ?
O9 V1 N19 78.93(9) . 11_666 ?
O9 V1 N5 83.69(10) . . ?
O23 V1 O2 93.67(10) . . ?
O23 V1 O9 103.95(10) . . ?
O23 V1 N19 81.63(9) . 11_666 ?
O23 V1 N5 164.38(10) . . ?
O22 V1 O2 97.63(10) . . ?
O22 V1 O9 101.45(11) . . ?
O22 V1 O23 100.99(12) . . ?
O22 V1 N19 177.13(12) . 11_666 ?
O22 V1 N5 90.60(12) . . ?
N5 V1 N19 86.62(9) . 11_666 ?
C3 O2 V1 116.94(18) . . ?
C8 O9 V1 133.87(18) . . ?
C24 O23 V1 125.5(2) . . ?
C10 O14 C15 118.0(3) . . ?
C18 N19 V1 122.4(2) . 16_656 ?
C20 N19 V1 121.4(2) . 16_656 ?
C20 N19 C18 116.2(3) . . ?
N4 N5 V1 115.27(18) . . ?
C6 N5 V1 127.2(2) . . ?
C6 N5 N4 116.7(2) . . ?
C3 N4 N5 107.9(2) . . ?
O9 C8 C7 122.8(3) . . ?
O9 C8 C10 118.2(3) . . ?
C7 C8 C10 119.0(3) . . ?
C17 C16 C3 120.5(3) . . ?
C17 C16 C21 117.3(3) . . ?
C21 C16 C3 122.2(3) . . ?
N5 C6 H6 118.2 . . ?
N5 C6 C7 123.6(3) . . ?
C7 C6 H6 118.2 . . ?
O2 C3 C16 116.5(3) . . ?
N4 C3 O2 124.7(3) . . ?
N4 C3 C16 118.8(3) . . ?
C8 C7 C6 121.3(3) . . ?
C13 C7 C8 119.9(3) . . ?
C13 C7 C6 118.8(3) . . ?
N19 C18 H18 118.1 . . ?
N19 C18 C17 123.8(3) . . ?
C17 C18 H18 118.1 . . ?
O14 C10 C8 114.6(3) . . ?
O14 C10 C11 125.6(3) . . ?
C11 C10 C8 119.8(3) . . ?
C16 C17 C18 119.3(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C16 C21 H21 120.6 . . ?
C16 C21 C20 118.8(3) . . ?
C20 C21 H21 120.6 . . ?
C7 C13 H13 120.0 . . ?
C12 C13 C7 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
N19 C20 C21 124.7(3) . . ?
N19 C20 H20 117.7 . . ?
C21 C20 H20 117.7 . . ?
O23 C24 H24A 109.5 . . ?
O23 C24 H24B 109.5 . . ?
O23 C24 C25 110.9(4) . . ?
H24A C24 H24B 108.1 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
O14 C15 H15A 109.5 . . ?
O14 C15 H15B 109.5 . . ?
O14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C24 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 C24 113.9(5) . . ?
C26 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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 O2 C3 N4 -8.4(4) . . . . ?
V1 O2 C3 C16 170.95(18) . . . . ?
V1 O9 C8 C7 26.3(4) . . . . ?
V1 O9 C8 C10 -155.7(2) . . . . ?
V1 O23 C24 C25 -137.0(3) . . . . ?
V1 N19 C18 C17 -179.3(2) 16_656 . . . ?
V1 N19 C20 C21 -179.4(3) 16_656 . . . ?
V1 N5 N4 C3 6.4(3) . . . . ?
V1 N5 C6 C7 -9.1(4) . . . . ?
O2 V1 O9 C8 -72.1(3) . . . . ?
O2 V1 O23 C24 94.6(3) . . . . ?
O9 V1 O23 C24 -108.8(3) . . . . ?
O9 C8 C7 C6 1.5(4) . . . . ?
O9 C8 C7 C13 -180.0(3) . . . . ?
O9 C8 C10 O14 -0.6(4) . . . . ?
O9 C8 C10 C11 179.1(3) . . . . ?
O23 V1 O9 C8 162.4(3) . . . . ?
O23 C24 C25 C26 61.2(5) . . . . ?
O22 V1 O9 C8 57.9(3) . . . . ?
O22 V1 O23 C24 -4.0(3) . . . . ?
O14 C10 C11 C12 180.0(3) . . . . ?
N19 V1 O9 C8 -119.2(3) 11_666 . . . ?
N19 V1 O23 C24 174.8(3) 11_666 . . . ?
N19 C18 C17 C16 -1.4(5) . . . . ?
N5 V1 O9 C8 -31.5(3) . . . . ?
N5 V1 O23 C24 133.3(4) . . . . ?
N5 N4 C3 O2 0.8(4) . . . . ?
N5 N4 C3 C16 -178.5(2) . . . . ?
N5 C6 C7 C8 -7.4(5) . . . . ?
N5 C6 C7 C13 174.1(3) . . . . ?
N4 N5 C6 C7 -177.8(3) . . . . ?
C8 C7 C13 C12 1.3(5) . . . . ?
C8 C10 C11 C12 0.3(5) . . . . ?
C16 C21 C20 N19 -1.3(6) . . . . ?
C6 N5 N4 C3 176.5(3) . . . . ?
C6 C7 C13 C12 179.9(3) . . . . ?
C3 C16 C17 C18 178.3(3) . . . . ?
C3 C16 C21 C20 -177.1(3) . . . . ?
C7 C8 C10 O14 177.5(2) . . . . ?
C7 C8 C10 C11 -2.8(4) . . . . ?
C7 C13 C12 C11 -3.8(6) . . . . ?
C18 N19 C20 C21 -1.2(5) . . . . ?
C10 C8 C7 C6 -176.5(3) . . . . ?
C10 C8 C7 C13 2.0(4) . . . . ?
C10 C11 C12 C13 3.1(6) . . . . ?
C17 C16 C3 O2 -8.9(4) . . . . ?
C17 C16 C3 N4 170.5(3) . . . . ?
C17 C16 C21 C20 2.4(5) . . . . ?
C21 C16 C3 O2 170.6(3) . . . . ?
C21 C16 C3 N4 -10.0(4) . . . . ?
C21 C16 C17 C18 -1.2(5) . . . . ?
C20 N19 C18 C17 2.6(5) . . . . ?
C15 O14 C10 C8 -168.3(3) . . . . ?
C15 O14 C10 C11 12.0(5) . . . . ?

_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_2480_auto
_database_code_depnum_ccdc_archive 'CCDC 2367623'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-19 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
pentoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v)
_chemical_formula_moiety         'C19 H22 N3 O5 V'
_chemical_formula_sum            'C19 H22 N3 O5 V'
_chemical_formula_weight         423.33
_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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   11.8119(5)
_cell_length_b                   14.9558(6)
_cell_length_c                   10.9912(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1941.67(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5410
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.9810
_cell_measurement_theta_min      4.7540
_shelx_estimated_absorpt_T_max   0.875
_shelx_estimated_absorpt_T_min   0.509
_exptl_absorpt_coefficient_mu    4.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8648
_diffrn_reflns_point_group_measured_fraction_full 0.815
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.158
_diffrn_reflns_theta_min         2.955
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     50.00  75.00   0.50    0.30    --   47.03  66.00  25.00   50
  2  ω    106.00 132.00   0.50    1.20    --  107.75  80.00 140.00   52
  3  ω    133.00 175.00   0.50    1.20    --  107.75  80.00 140.00   84
  4  ω    105.00 178.00   0.50    1.20    --  107.75  66.00  25.00  146
  5  ω    104.00 134.00   0.50    1.20    --  107.75  45.00 -60.00   60
  6  ω    144.00 172.00   0.50    1.20    --  107.75  45.00 -60.00   56
  7  ω     99.00 175.00   0.50    1.20    --  107.75  76.00-104.00  152
  8  ω    -79.00 -42.00   0.50    0.30    --  -47.03 -38.00   0.00   74
  9  ω   -115.00 -82.00   0.50    0.30    --  -47.03 -38.00   0.00   66
 10  ω    -42.00 -16.00   0.50    1.20    --  -86.25  45.00-150.00   52
 11  ω   -113.00 -74.00   0.50    0.30    --  -47.03-125.00-180.00   78
 12  ω   -120.00 -86.00   0.50    0.30    --  -47.03-125.00 -30.00   68
 13  ω     35.00  81.00   0.50    1.20    --  107.75 -95.00 120.00   92
 14  ω     47.00  75.00   0.50    1.20    --  107.75 -77.00 -60.00   56
 15  ω     38.00  63.00   0.50    1.20    --  107.75 -61.00 -60.00   50
 16  ω     35.00  88.00   0.50    1.20    --  107.75 -77.00  30.00  106
 17  ω     42.00  67.00   0.50    1.20    --  107.75 -61.00  30.00   50
 18  ω    -26.00   6.00   0.50    0.30    --   47.03 -19.00-120.00   64
 19  ω     35.00  60.00   0.50    1.20    --  107.75 -61.00-180.00   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         0.502
_reflns_Friedel_fraction_full    0.609
_reflns_Friedel_fraction_max     0.551
_reflns_number_gt                2778
_reflns_number_total             3226
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.033(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0541
_refine_ls_restrained_S_all      1.149
_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)+(0.0905P)²+1.5530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1793
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.967(16)
 0.033(16)
2. 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) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C27A-C28
 1.52 with sigma of 0.02
 C26-C27
 1.52 with sigma of 0.02
 C24-C25
 1.52 with sigma of 0.01
 C25-C26
 1.52 with sigma of 0.01
 C27-C28
 1.52 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C25A, C26A, C27A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H24A(0.333333) H24B(0.333333) H24C(0.666667) H24D(0.666667)
 C25A(0.333333) H25A(0.333333) H25B(0.333333) C26A(0.333333) H26A(0.333333)
 H26B(0.333333) C27A(0.333333) H27A(0.333333) H27B(0.333333) C25(0.666667)
 H25C(0.666667) H25D(0.666667) C27(0.666667) H27C(0.666667) H27D(0.666667)
 H28A(0.333333) H28B(0.333333) H28C(0.333333) H28D(0.666667) H28E(0.666667)
 H28F(0.666667) C26(0.666667) H26C(0.666667) H26D(0.666667)
6.a Free rotating group:
 C24(C25A,C26A,C27A)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24(H24C,H24D), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,
 H27B), C25(H25C,H25D), C27(H27C,H27D), C26(H26C,H26D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C11(H11), C12(H12), C16(H16), C15(H15), C18(H18), C14(H14)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C28(H28D,H28E,H28F)
;
_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 0.41665(8) 0.25949(6) 0.40518(15) 0.0237(3) Uani 1 1 d . . . . .
O2 O 0.5307(4) 0.2047(3) 0.3143(5) 0.0301(11) Uani 1 1 d . . . . .
O9 O 0.3031(4) 0.3556(3) 0.4283(5) 0.0278(10) Uani 1 1 d . . . . .
N6 N 0.3521(5) 0.2887(3) 0.2298(6) 0.0243(11) Uani 1 1 d . . . . .
O20 O 0.6766(4) 0.0732(3) 0.2933(6) 0.0388(12) Uani 1 1 d . . . . .
O22 O 0.3360(4) 0.1754(3) 0.4255(6) 0.0351(12) Uani 1 1 d . . . . .
N7 N 0.2788(5) 0.3612(4) 0.2203(6) 0.0298(12) Uani 1 1 d . . . . .
O23 O 0.4795(4) 0.2707(3) 0.5511(5) 0.0310(11) Uani 1 1 d . . . . .
N13 N 0.0297(5) 0.6095(4) 0.3714(6) 0.0288(13) Uani 1 1 d . . . . .
C8 C 0.2588(5) 0.3894(4) 0.3303(7) 0.0270(14) Uani 1 1 d . . . . .
C10 C 0.1773(5) 0.4647(4) 0.3445(7) 0.0243(13) Uani 1 1 d . . . . .
C5 C 0.3625(6) 0.2408(4) 0.1339(8) 0.0290(14) Uani 1 1 d . . . . .
H5 H 0.320119 0.256306 0.063537 0.035 Uiso 1 1 calc R U . . .
C17 C 0.5043(7) 0.0347(5) 0.0186(9) 0.0386(18) Uani 1 1 d . . . . .
H17 H 0.497393 -0.006063 -0.047246 0.046 Uiso 1 1 calc R U . . .
C11 C 0.1350(6) 0.4868(4) 0.4568(8) 0.0318(15) Uani 1 1 d . . . . .
H11 H 0.156218 0.453667 0.526858 0.038 Uiso 1 1 calc R U . . .
C4 C 0.4367(6) 0.1638(4) 0.1294(7) 0.0285(14) Uani 1 1 d . . . . .
C3 C 0.5193(5) 0.1502(4) 0.2176(7) 0.0263(13) Uani 1 1 d . . . . .
C12 C 0.0601(7) 0.5589(4) 0.4666(8) 0.0336(16) Uani 1 1 d . . . . .
H12 H 0.029434 0.572649 0.544276 0.040 Uiso 1 1 calc R U . . .
C16 C 0.4297(6) 0.1053(5) 0.0280(8) 0.0348(16) Uani 1 1 d . . . . .
H16 H 0.374043 0.114717 -0.032993 0.042 Uiso 1 1 calc R U . . .
C19 C 0.5968(6) 0.0796(4) 0.2041(7) 0.0278(14) Uani 1 1 d . . . . .
C15 C 0.1429(7) 0.5147(5) 0.2435(8) 0.0392(18) Uani 1 1 d . . . . .
H15 H 0.168130 0.499693 0.164047 0.047 Uiso 1 1 calc R U . . .
C18 C 0.5884(6) 0.0227(4) 0.1034(8) 0.0341(16) Uani 1 1 d . . . . .
H18 H 0.641306 -0.024567 0.093533 0.041 Uiso 1 1 calc R U . . .
C14 C 0.0709(6) 0.5868(5) 0.2624(8) 0.0377(18) Uani 1 1 d . . . . .
H14 H 0.049785 0.621972 0.194121 0.045 Uiso 1 1 calc R U . . .
C21 C 0.7591(8) 0.0050(6) 0.2802(10) 0.049(2) Uani 1 1 d . . . . .
H21A H 0.798264 0.012327 0.202223 0.073 Uiso 1 1 calc R U . . .
H21B H 0.721993 -0.053576 0.282471 0.073 Uiso 1 1 calc R U . . .
H21C H 0.814019 0.009148 0.346772 0.073 Uiso 1 1 calc R U . . .
C24 C 0.4651(10) 0.2206(7) 0.6588(10) 0.064(3) Uani 1 1 d DG . . . .
H24A H 0.499192 0.161496 0.641182 0.077 Uiso 0.3333 1 calc R U P A 1
H24B H 0.382550 0.210172 0.665082 0.077 Uiso 0.3333 1 calc R U P A 1
H24C H 0.427928 0.162975 0.639470 0.077 Uiso 0.6667 1 calc R U P B 2
H24D H 0.415740 0.253797 0.715840 0.077 Uiso 0.6667 1 calc R U P B 2
C25A C 0.503(2) 0.2432(14) 0.7871(10) 0.071(9) Uani 0.3333 1 d G . P C 1
H25A H 0.531101 0.188110 0.826898 0.085 Uiso 0.3333 1 calc R U P C 1
H25B H 0.436873 0.264707 0.834037 0.085 Uiso 0.3333 1 calc R U P C 1
C26A C 0.595(2) 0.3138(14) 0.7914(19) 0.060(8) Uani 0.3333 1 d G . P C 1
H26A H 0.567844 0.368235 0.749593 0.072 Uiso 0.3333 1 calc R U P C 1
H26B H 0.662052 0.291531 0.746196 0.072 Uiso 0.3333 1 calc R U P C 1
C27A C 0.632(3) 0.3386(14) 0.920(2) 0.070(9) Uani 0.3333 1 d DG . P C 1
H27A H 0.683291 0.390663 0.916994 0.084 Uiso 0.3333 1 calc R U P C 1
H27B H 0.564535 0.354986 0.968703 0.084 Uiso 0.3333 1 calc R U P C 1
C25 C 0.5771(12) 0.2034(12) 0.7173(16) 0.068(5) Uani 0.6667 1 d D . P C 2
H25C H 0.621001 0.165198 0.660838 0.082 Uiso 0.6667 1 calc R U P C 2
H25D H 0.562560 0.167118 0.791051 0.082 Uiso 0.6667 1 calc R U P C 2
C27 C 0.638(3) 0.3179(17) 0.880(2) 0.111(10) Uani 0.6667 1 d D . P C 2
H27C H 0.556655 0.324974 0.897394 0.133 Uiso 0.6667 1 calc R U P C 2
H27D H 0.673642 0.377951 0.882766 0.133 Uiso 0.6667 1 calc R U P C 2
C28 C 0.6913(10) 0.2595(9) 0.9768(15) 0.077(3) Uani 1 1 d D . . . .
H28A H 0.765790 0.251883 0.939005 0.115 Uiso 0.3333 1 calc R U P C 1
H28B H 0.646044 0.205387 0.964235 0.115 Uiso 0.3333 1 calc R U P C 1
H28C H 0.700609 0.270158 1.064203 0.115 Uiso 0.3333 1 calc R U P C 1
H28D H 0.725167 0.206722 0.938616 0.115 Uiso 0.6667 1 calc R U P C 2
H28E H 0.632927 0.240660 1.034745 0.115 Uiso 0.6667 1 calc R U P C 2
H28F H 0.750004 0.293374 1.019765 0.115 Uiso 0.6667 1 calc R U P C 2
C26 C 0.6530(18) 0.2791(14) 0.755(2) 0.087(6) Uani 0.6667 1 d D . P C 2
H26C H 0.642828 0.328076 0.695099 0.105 Uiso 0.6667 1 calc R U P C 2
H26D H 0.732300 0.258203 0.747239 0.105 Uiso 0.6667 1 calc R 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
V1 O2 1.866(5) . ?
V1 O9 1.982(4) . ?
V1 N6 2.118(6) . ?
V1 O22 1.594(4) . ?
V1 O23 1.775(6) . ?
V1 N13 2.400(5) 3_565 ?
O2 C3 1.347(9) . ?
O9 C8 1.300(8) . ?
N6 N7 1.392(7) . ?
N6 C5 1.280(10) . ?
O20 C19 1.364(9) . ?
O20 C21 1.418(9) . ?
N7 C8 1.301(10) . ?
O23 C24 1.411(11) . ?
N13 C12 1.341(10) . ?
N13 C14 1.336(10) . ?
C8 C10 1.490(9) . ?
C10 C11 1.372(11) . ?
C10 C15 1.398(10) . ?
C5 H5 0.9500 . ?
C5 C4 1.449(9) . ?
C17 H17 0.9500 . ?
C17 C16 1.378(11) . ?
C17 C18 1.374(13) . ?
C11 H11 0.9500 . ?
C11 C12 1.398(10) . ?
C4 C3 1.390(10) . ?
C4 C16 1.419(11) . ?
C3 C19 1.405(9) . ?
C12 H12 0.9500 . ?
C16 H16 0.9500 . ?
C19 C18 1.399(11) . ?
C15 H15 0.9500 . ?
C15 C14 1.389(10) . ?
C18 H18 0.9500 . ?
C14 H14 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 H24C 0.9900 . ?
C24 H24D 0.9900 . ?
C24 C25A 1.5175 . ?
C24 C25 1.493(11) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C25A C26A 1.5180 . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26A C27A 1.5185 . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
C27A C28 1.51(2) . ?
C25 H25C 0.9900 . ?
C25 H25D 0.9900 . ?
C25 C26 1.501(12) . ?
C27 H27C 0.9900 . ?
C27 H27D 0.9900 . ?
C27 C28 1.51(2) . ?
C27 C26 1.51(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 H28D 0.9800 . ?
C28 H28E 0.9800 . ?
C28 H28F 0.9800 . ?
C26 H26C 0.9900 . ?
C26 H26D 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
O2 V1 O9 151.1(2) . . ?
O2 V1 N6 82.1(2) . . ?
O2 V1 N13 82.8(2) . 3_565 ?
O9 V1 N6 74.0(2) . . ?
O9 V1 N13 78.73(19) . 3_565 ?
N6 V1 N13 83.7(2) . 3_565 ?
O22 V1 O2 99.2(2) . . ?
O22 V1 O9 98.6(2) . . ?
O22 V1 N6 94.3(3) . . ?
O22 V1 O23 101.4(3) . . ?
O22 V1 N13 177.0(2) . 3_565 ?
O23 V1 O2 102.9(2) . . ?
O23 V1 O9 95.7(2) . . ?
O23 V1 N6 162.4(2) . . ?
O23 V1 N13 80.2(2) . 3_565 ?
C3 O2 V1 128.0(4) . . ?
C8 O9 V1 116.6(4) . . ?
N7 N6 V1 116.9(4) . . ?
C5 N6 V1 126.9(5) . . ?
C5 N6 N7 115.7(6) . . ?
C19 O20 C21 116.8(7) . . ?
C8 N7 N6 107.2(6) . . ?
C24 O23 V1 131.1(5) . . ?
C12 N13 V1 119.3(5) . 3_465 ?
C14 N13 V1 123.3(5) . 3_465 ?
C14 N13 C12 117.3(6) . . ?
O9 C8 N7 124.8(6) . . ?
O9 C8 C10 117.9(6) . . ?
N7 C8 C10 117.4(6) . . ?
C11 C10 C8 120.8(6) . . ?
C11 C10 C15 118.6(6) . . ?
C15 C10 C8 120.6(6) . . ?
N6 C5 H5 119.0 . . ?
N6 C5 C4 122.0(7) . . ?
C4 C5 H5 119.0 . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C18 C17 C16 120.7(7) . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.1(7) . . ?
C12 C11 H11 120.5 . . ?
C3 C4 C5 121.2(7) . . ?
C3 C4 C16 119.8(6) . . ?
C16 C4 C5 118.8(7) . . ?
O2 C3 C4 122.1(6) . . ?
O2 C3 C19 118.3(6) . . ?
C4 C3 C19 119.6(7) . . ?
N13 C12 C11 123.0(8) . . ?
N13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C17 C16 C4 119.6(7) . . ?
C17 C16 H16 120.2 . . ?
C4 C16 H16 120.2 . . ?
O20 C19 C3 115.2(6) . . ?
O20 C19 C18 125.2(6) . . ?
C18 C19 C3 119.6(7) . . ?
C10 C15 H15 120.8 . . ?
C14 C15 C10 118.3(7) . . ?
C14 C15 H15 120.8 . . ?
C17 C18 C19 120.6(6) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
N13 C14 C15 123.6(8) . . ?
N13 C14 H14 118.2 . . ?
C15 C14 H14 118.2 . . ?
O20 C21 H21A 109.5 . . ?
O20 C21 H21B 109.5 . . ?
O20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O23 C24 H24A 105.1 . . ?
O23 C24 H24B 105.1 . . ?
O23 C24 H24C 109.6 . . ?
O23 C24 H24D 109.6 . . ?
O23 C24 C25A 128.7(8) . . ?
O23 C24 C25 110.2(10) . . ?
H24A C24 H24B 105.9 . . ?
H24C C24 H24D 108.1 . . ?
C25A C24 H24A 105.1 . . ?
C25A C24 H24B 105.1 . . ?
C25 C24 H24C 109.6 . . ?
C25 C24 H24D 109.6 . . ?
C24 C25A H25A 108.9 . . ?
C24 C25A H25B 108.9 . . ?
C24 C25A C26A 113.3 . . ?
H25A C25A H25B 107.7 . . ?
C26A C25A H25A 108.9 . . ?
C26A C25A H25B 108.9 . . ?
C25A C26A H26A 108.8 . . ?
C25A C26A H26B 108.8 . . ?
C25A C26A C27A 113.7 . . ?
H26A C26A H26B 107.7 . . ?
C27A C26A H26A 108.8 . . ?
C27A C26A H26B 108.8 . . ?
C26A C27A H27A 109.9 . . ?
C26A C27A H27B 109.9 . . ?
H27A C27A H27B 108.3 . . ?
C28 C27A C26A 109.1(14) . . ?
C28 C27A H27A 109.9 . . ?
C28 C27A H27B 109.9 . . ?
C24 C25 H25C 107.0 . . ?
C24 C25 H25D 107.0 . . ?
C24 C25 C26 121.1(14) . . ?
H25C C25 H25D 106.8 . . ?
C26 C25 H25C 107.0 . . ?
C26 C25 H25D 107.0 . . ?
H27C C27 H27D 107.9 . . ?
C28 C27 H27C 109.2 . . ?
C28 C27 H27D 109.2 . . ?
C26 C27 H27C 109.2 . . ?
C26 C27 H27D 109.2 . . ?
C26 C27 C28 112(2) . . ?
C27A C28 H28A 109.5 . . ?
C27A C28 H28B 109.5 . . ?
C27A C28 H28C 109.5 . . ?
C27 C28 H28D 109.5 . . ?
C27 C28 H28E 109.5 . . ?
C27 C28 H28F 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H28D C28 H28E 109.5 . . ?
H28D C28 H28F 109.5 . . ?
H28E C28 H28F 109.5 . . ?
C25 C26 C27 118(2) . . ?
C25 C26 H26C 107.8 . . ?
C25 C26 H26D 107.8 . . ?
C27 C26 H26C 107.8 . . ?
C27 C26 H26D 107.8 . . ?
H26C C26 H26D 107.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O2 C3 C4 38.0(9) . . . . ?
V1 O2 C3 C19 -144.5(5) . . . . ?
V1 O9 C8 N7 4.1(9) . . . . ?
V1 O9 C8 C10 -177.1(4) . . . . ?
V1 N6 N7 C8 -6.3(6) . . . . ?
V1 N6 C5 C4 -9.5(10) . . . . ?
V1 O23 C24 C25A -166.9(14) . . . . ?
V1 O23 C24 C25 136.9(10) . . . . ?
V1 N13 C12 C11 -173.4(5) 3_465 . . . ?
V1 N13 C14 C15 175.3(6) 3_465 . . . ?
O2 V1 O23 C24 -102.3(8) . . . . ?
O2 C3 C19 O20 0.6(9) . . . . ?
O2 C3 C19 C18 -178.9(6) . . . . ?
O9 V1 O2 C3 -79.9(7) . . . . ?
O9 V1 O23 C24 100.0(8) . . . . ?
O9 C8 C10 C11 -11.5(9) . . . . ?
O9 C8 C10 C15 168.1(7) . . . . ?
N6 V1 O2 C3 -45.7(6) . . . . ?
N6 V1 O23 C24 152.9(9) . . . . ?
N6 N7 C8 O9 1.6(9) . . . . ?
N6 N7 C8 C10 -177.1(5) . . . . ?
N6 C5 C4 C3 -15.2(11) . . . . ?
N6 C5 C4 C16 169.5(7) . . . . ?
O20 C19 C18 C17 179.7(7) . . . . ?
O22 V1 O2 C3 47.5(6) . . . . ?
O22 V1 O23 C24 0.1(9) . . . . ?
N7 N6 C5 C4 179.2(6) . . . . ?
N7 C8 C10 C11 167.3(7) . . . . ?
N7 C8 C10 C15 -13.1(10) . . . . ?
O23 V1 O2 C3 151.5(5) . . . . ?
O23 C24 C25A C26A -19(3) . . . . ?
O23 C24 C25 C26 58(2) . . . . ?
N13 V1 O2 C3 -130.3(6) 3_565 . . . ?
N13 V1 O23 C24 177.5(9) 3_565 . . . ?
C8 C10 C11 C12 178.9(6) . . . . ?
C8 C10 C15 C14 -177.0(7) . . . . ?
C10 C11 C12 N13 -1.9(11) . . . . ?
C10 C15 C14 N13 -2.2(13) . . . . ?
C5 N6 N7 C8 165.8(6) . . . . ?
C5 C4 C3 O2 3.5(11) . . . . ?
C5 C4 C3 C19 -173.9(6) . . . . ?
C5 C4 C16 C17 176.1(7) . . . . ?
C11 C10 C15 C14 2.6(11) . . . . ?
C4 C3 C19 O20 178.2(6) . . . . ?
C4 C3 C19 C18 -1.4(10) . . . . ?
C3 C4 C16 C17 0.8(11) . . . . ?
C3 C19 C18 C17 -0.8(11) . . . . ?
C12 N13 C14 C15 -0.3(12) . . . . ?
C16 C17 C18 C19 3.0(12) . . . . ?
C16 C4 C3 O2 178.8(7) . . . . ?
C16 C4 C3 C19 1.4(10) . . . . ?
C15 C10 C11 C12 -0.7(11) . . . . ?
C18 C17 C16 C4 -2.9(12) . . . . ?
C14 N13 C12 C11 2.3(11) . . . . ?
C21 O20 C19 C3 -177.5(7) . . . . ?
C21 O20 C19 C18 2.0(10) . . . . ?
C24 C25A C26A C27A 178.5 . . . . ?
C24 C25 C26 C27 89(3) . . . . ?
C25A C26A C27A C28 68(3) . . . . ?
C28 C27 C26 C25 78(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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.967(16)
2 0.033(16)

####################################################################### 
# 
# 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_4139
_database_code_depnum_ccdc_archive 'CCDC 2367619'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-13 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
"dioxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v) dihydrate"
_chemical_formula_moiety         'C14 H11 N3 O5 V, 2(H2 O)'
_chemical_formula_sum            'C14 H15 N3 O7 V'
_chemical_formula_weight         388.23
_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2890(3)
_cell_length_b                   10.4109(5)
_cell_length_c                   10.5800(4)
_cell_angle_alpha                107.183(4)
_cell_angle_beta                 97.280(3)
_cell_angle_gamma                91.817(4)
_cell_volume                     758.82(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6378
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.9630
_cell_measurement_theta_min      4.4200
_shelx_estimated_absorpt_T_max   0.838
_shelx_estimated_absorpt_T_min   0.509
_exptl_absorpt_coefficient_mu    5.908
_exptl_absorpt_correction_T_max  0.15308
_exptl_absorpt_correction_T_min  0.05224
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.031
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11559
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.755
_diffrn_reflns_theta_min         4.419
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_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   -111.00 -31.00   0.50    0.34    --  -47.16 -59.00 -38.00  160
  2  ω     32.00 118.00   0.50    0.34    --   47.16  59.00 101.00  172
  3  ω    -23.00  16.00   0.50    0.34    --   47.16 -59.00 -38.00   78
  4  ω     25.00  53.00   0.50    0.34    --   47.16 -59.00 -38.00   56
  5  ω    -47.00 -20.00   0.50    1.36    --  -86.25  59.00 101.00   54
  6  ω   -139.00-114.00   0.50    1.36    --  -86.25 -59.00 -38.00   50
  7  ω    119.00 162.00   0.50    1.36    --  107.75  59.00 101.00   86
  8  ω     36.00  65.00   0.50    1.36    --  107.75 -59.00 -38.00   58
  9  ω   -114.00 -89.00   0.50    0.34    --  -47.16 -77.00-150.00   50
 10  ω    -10.00  17.00   0.50    0.34    --  -47.16  59.00 101.00   54
 11  ω    -61.00 -18.00   0.50    0.34    --  -47.16  59.00 101.00   86
 12  ω     57.00  95.00   0.50    0.34    --   47.16-125.00 150.00   76
 13  ω     37.00  88.00   0.50    0.34    --   47.16-125.00  30.00  102
 14  ω    -50.00 -14.00   0.50    1.36    --  -86.25  45.00 -90.00   72
 15  ω    -49.00 -16.00   0.50    1.36    --  -86.25  45.00 -60.00   66
 16  ω     96.00 175.00   0.50    1.36    --  107.75 125.00 150.00  158
 17  ω     41.00  88.00   0.50    1.36    --  107.75 -95.00 -90.00   94
 18  ω     35.00  71.00   0.50    1.36    --  107.75 -61.00 150.00   72
 19  ω    118.00 144.00   0.50    1.36    --  107.75 125.00-180.00   52
 20  ω    147.00 174.00   0.50    1.36    --  107.75 125.00-180.00   54
 21  ω    110.00 178.00   0.50    1.36    --  107.75  45.00-120.00  136
 22  ω     41.00  66.00   0.50    1.36    --  107.75 -61.00-180.00   50
 23  ω     71.00 110.00   0.50    1.36    --  107.75-125.00 -90.00   78
 24  ω     39.00  67.00   0.50    1.36    --  107.75-125.00 120.00   56
 25  ω     36.00  61.00   0.50    1.36    --  107.75-125.00 -90.00   50
 26  ω     42.00  67.00   0.50    1.36    --  107.75 -77.00-150.00   50
 27  ω     79.00 104.00   0.50    1.36    --  107.75 -77.00-120.00   50
 28  ω     78.00 108.00   0.50    1.36    --  107.75-125.00 120.00   60
 29  ω     94.00 120.00   0.50    1.36    --  107.75  77.00 -90.00   52
 30  ω    132.00 158.00   0.50    1.36    --  107.75  77.00 -90.00   52
 31  ω    102.00 128.00   0.50    1.36    --  107.75  77.00-180.00   52
 32  ω    136.00 178.00   0.50    1.36    --  107.75  77.00-180.00   84
 33  ω     73.00 102.00   0.50    1.36    --  107.75-125.00-120.00   58
 34  ω     89.00 150.00   0.50    1.36    --  107.75  77.00 120.00  122
 35  ω     78.00 103.00   0.50    1.36    --  107.75 -95.00  90.00   50
 36  ω     37.00  62.00   0.50    1.36    --  107.75-125.00 -60.00   50
 37  ω     79.00 111.00   0.50    1.36    --  107.75-125.00 -60.00   64
 38  ω     41.00  72.00   0.50    1.36    --  107.75-125.00  90.00   62
 39  ω    135.00 164.00   0.50    1.36    --  107.75 125.00 120.00   58
 40  ω    106.00 178.00   0.50    1.36    --  107.75  45.00 -30.00  144
 41  ω     39.00  64.00   0.50    1.36    --  107.75-125.00 -30.00   50
 42  ω    127.00 153.00   0.50    1.36    --  107.75 125.00 -90.00   52
 43  ω     77.00 112.00   0.50    1.36    --  107.75-125.00 -30.00   70
 44  ω     99.00 155.00   0.50    1.36    --  107.75  15.00  30.00  112
 45  ω     84.00 109.00   0.50    1.36    --  107.75-125.00-150.00   50
 46  ω     80.00 112.00   0.50    1.36    --  107.75-125.00  90.00   64
 47  ω     38.00  63.00   0.50    1.36    --  107.75-125.00-150.00   50
 48  ω     39.00  64.00   0.50    1.36    --  107.75 -61.00  60.00   50
 49  ω     58.00 112.00   0.50    1.36    --  107.75-125.00  30.00  108
 50  ω    127.00 169.00   0.50    1.36    --  107.75  45.00  60.00   84
 51  ω     58.00  84.00   0.50    1.36    --  107.75 -77.00   0.00   52
 52  ω     37.00  62.00   0.50    1.36    --  107.75 -77.00 120.00   50
 53  ω     67.00  96.00   0.50    1.36    --  107.75 -77.00 120.00   58
 54  ω     44.00  69.00   0.50    1.36    --  107.75 -95.00-180.00   50
 55  ω     38.00  99.00   0.50    1.36    --  107.75 -95.00 -30.00  122
 56  ω     52.00  98.00   0.50    1.36    --  107.75 -95.00  30.00   92
 57  ω    120.00 161.00   0.50    1.36    --  107.75 125.00   0.00   82
 58  ω     99.00 124.00   0.50    1.36    --  107.75 125.00  60.00   50
 59  ω    140.00 178.00   0.50    1.36    --  107.75 125.00  60.00   76
 60  ω    111.00 136.00   0.50    1.36    --  107.75  45.00 -60.00   50
 61  ω     97.00 149.00   0.50    1.36    --  107.75  15.00 -30.00  104
 62  ω     83.00 108.00   0.50    1.36    --  107.75 -82.00  18.99   50
 63  ω     39.00 105.00   0.50    1.36    --  107.75 -95.00 120.00  132
;
_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                2869
_reflns_number_total             3175
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.078
_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)+(0.1387P)²+0.0838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1820
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H24A,H24B} of O24
 At 1.5 times of:
  All C(H,H,H) groups, {H25A,H25B} of O25
2. Others
 Fixed X: H24A(0.64222) H24B(0.74325)
 Fixed Y: H24A(0.03517) H24B(0.0902)
 Fixed Z: H24A(0.96929) H24B(1.0949)
3.a Free rotating group:
 O25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C9(H9), C7(H7), C5(H5), C19(H19), C6(H6), C16(H16), C18(H18)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.34273(7) 0.70253(4) 0.67434(4) 0.0434(2) Uani 1 1 d . . . . .
O2 O 0.2772(3) 0.7746(2) 0.5296(2) 0.0472(5) Uani 1 1 d . . . . .
O13 O 0.4480(3) 0.5613(2) 0.7488(2) 0.0491(5) Uani 1 1 d . . . . .
O20 O 0.1650(3) 0.9594(2) 0.4151(2) 0.0507(5) Uani 1 1 d . . . . .
O23 O 0.1718(3) 0.7432(2) 0.7616(2) 0.0540(5) Uani 1 1 d . . . . .
O22 O 0.5224(3) 0.8079(2) 0.7470(2) 0.0551(6) Uani 1 1 d . . . . .
N10 N 0.2736(3) 0.5155(2) 0.5218(2) 0.0433(5) Uani 1 1 d . . . . .
N11 N 0.3208(4) 0.3996(2) 0.5561(3) 0.0469(5) Uani 1 1 d . . . . .
N17 N 0.5513(5) 0.1314(3) 0.8504(4) 0.0648(8) Uani 1 1 d . . . . .
C12 C 0.4083(4) 0.4361(3) 0.6763(3) 0.0457(6) Uani 1 1 d . . . . .
C4 C 0.1109(4) 0.8275(3) 0.3467(3) 0.0466(6) Uani 1 1 d . . . . .
C14 C 0.4644(4) 0.3289(3) 0.7365(3) 0.0472(6) Uani 1 1 d . . . . .
C3 C 0.1715(4) 0.7320(3) 0.4129(3) 0.0445(6) Uani 1 1 d . . . . .
C15 C 0.4215(5) 0.1933(3) 0.6639(4) 0.0540(7) Uani 1 1 d . . . . .
H15 H 0.361099 0.168932 0.574252 0.065 Uiso 1 1 calc R U . . .
O25 O 0.8540(5) -0.2162(4) 0.9058(3) 0.0809(9) Uani 1 1 d G . . . .
H25A H 0.826333 -0.145172 0.965942 0.121 Uiso 1 1 d G U . . .
H25B H 0.759477 -0.234100 0.842683 0.121 Uiso 1 1 d G U . . .
C8 C 0.1211(4) 0.5947(3) 0.3458(3) 0.0469(6) Uani 1 1 d . . . . .
C9 C 0.1811(4) 0.4920(3) 0.4035(3) 0.0468(6) Uani 1 1 d . . . . .
H9 H 0.150886 0.400680 0.351553 0.056 Uiso 1 1 calc R U . . .
C7 C 0.0150(5) 0.5540(3) 0.2168(3) 0.0526(7) Uani 1 1 d . . . . .
H7 H -0.018120 0.460969 0.172862 0.063 Uiso 1 1 calc R U . . .
C5 C 0.0073(5) 0.7851(4) 0.2211(3) 0.0532(7) Uani 1 1 d . . . . .
H5 H -0.032589 0.850001 0.178549 0.064 Uiso 1 1 calc R U . . .
C19 C 0.5557(5) 0.3610(4) 0.8657(3) 0.0550(7) Uani 1 1 d . . . . .
H19 H 0.589562 0.452514 0.915668 0.066 Uiso 1 1 calc R U . . .
C6 C -0.0400(5) 0.6476(4) 0.1554(3) 0.0544(7) Uani 1 1 d . . . . .
H6 H -0.109916 0.619820 0.068592 0.065 Uiso 1 1 calc R U . . .
O24 O 0.7162(7) 0.0133(4) 1.0299(4) 0.0964(11) Uani 1 1 d . . . . .
H24A H 0.642220 0.035170 0.969290 0.116 Uiso 1 1 d . U . . .
H24B H 0.743250 0.090200 1.094900 0.116 Uiso 1 1 d . U . . .
C16 C 0.4672(5) 0.0954(4) 0.7230(5) 0.0626(9) Uani 1 1 d . . . . .
H16 H 0.439576 0.002865 0.674319 0.075 Uiso 1 1 calc R U . . .
C18 C 0.5975(6) 0.2598(4) 0.9218(4) 0.0657(9) Uani 1 1 d . . . . .
H18 H 0.658941 0.281315 1.010915 0.079 Uiso 1 1 calc R U . . .
C21 C 0.0905(6) 1.0572(4) 0.3549(4) 0.0584(8) Uani 1 1 d . . . . .
H21A H 0.141492 1.048420 0.271577 0.088 Uiso 1 1 calc R U . . .
H21B H 0.124084 1.148094 0.416486 0.088 Uiso 1 1 calc R U . . .
H21C H -0.044874 1.041833 0.335464 0.088 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 O2 1.911(2) . ?
V1 O13 1.994(2) . ?
V1 O23 1.636(2) . ?
V1 O22 1.632(2) . ?
V1 N10 2.127(2) . ?
O2 C3 1.315(4) . ?
O13 C12 1.303(4) . ?
O20 C4 1.367(4) . ?
O20 C21 1.439(4) . ?
N10 N11 1.400(3) . ?
N10 C9 1.294(4) . ?
N11 C12 1.290(4) . ?
N17 C16 1.346(6) . ?
N17 C18 1.334(6) . ?
C12 C14 1.484(4) . ?
C4 C3 1.427(4) . ?
C4 C5 1.381(5) . ?
C14 C15 1.397(5) . ?
C14 C19 1.381(5) . ?
C3 C8 1.408(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.373(5) . ?
O25 H25A 0.8700 . ?
O25 H25B 0.8699 . ?
C8 C9 1.434(4) . ?
C8 C7 1.418(4) . ?
C9 H9 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.366(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(5) . ?
C19 H19 0.9500 . ?
C19 C18 1.378(5) . ?
C6 H6 0.9500 . ?
O24 H24A 0.871 . ?
O24 H24B 0.885 . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
O2 V1 O13 151.88(10) . . ?
O2 V1 N10 82.72(9) . . ?
O13 V1 N10 73.73(9) . . ?
O23 V1 O2 102.26(11) . . ?
O23 V1 O13 100.27(11) . . ?
O23 V1 N10 110.51(11) . . ?
O22 V1 O2 96.77(11) . . ?
O22 V1 O13 91.67(10) . . ?
O22 V1 O23 108.77(13) . . ?
O22 V1 N10 139.88(12) . . ?
C3 O2 V1 135.3(2) . . ?
C12 O13 V1 117.05(19) . . ?
C4 O20 C21 115.8(2) . . ?
N11 N10 V1 116.30(18) . . ?
C9 N10 V1 129.1(2) . . ?
C9 N10 N11 114.4(2) . . ?
C12 N11 N10 108.4(2) . . ?
C18 N17 C16 122.4(3) . . ?
O13 C12 C14 118.1(3) . . ?
N11 C12 O13 124.1(3) . . ?
N11 C12 C14 117.9(3) . . ?
O20 C4 C3 115.4(3) . . ?
O20 C4 C5 124.1(3) . . ?
C5 C4 C3 120.5(3) . . ?
C15 C14 C12 120.2(3) . . ?
C19 C14 C12 120.9(3) . . ?
C19 C14 C15 118.9(3) . . ?
O2 C3 C4 119.2(3) . . ?
O2 C3 C8 123.1(3) . . ?
C8 C3 C4 117.6(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.5(4) . . ?
C16 C15 H15 120.3 . . ?
H25A O25 H25B 104.5 . . ?
C3 C8 C9 121.1(3) . . ?
C3 C8 C7 120.7(3) . . ?
C7 C8 C9 118.1(3) . . ?
N10 C9 C8 124.3(3) . . ?
N10 C9 H9 117.8 . . ?
C8 C9 H9 117.8 . . ?
C8 C7 H7 119.8 . . ?
C6 C7 C8 120.4(3) . . ?
C6 C7 H7 119.8 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C14 C19 H19 120.1 . . ?
C18 C19 C14 119.7(4) . . ?
C18 C19 H19 120.1 . . ?
C7 C6 C5 119.8(3) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
H24A O24 H24B 103.9 . . ?
N17 C16 C15 119.6(4) . . ?
N17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
N17 C18 C19 119.8(4) . . ?
N17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
O20 C21 H21A 109.5 . . ?
O20 C21 H21B 109.5 . . ?
O20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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 O2 C3 C4 161.4(2) . . . . ?
V1 O2 C3 C8 -21.6(5) . . . . ?
V1 O13 C12 N11 6.7(4) . . . . ?
V1 O13 C12 C14 -172.3(2) . . . . ?
V1 N10 N11 C12 -3.5(3) . . . . ?
V1 N10 C9 C8 7.0(5) . . . . ?
O2 C3 C8 C9 1.0(5) . . . . ?
O2 C3 C8 C7 -176.6(3) . . . . ?
O13 C12 C14 C15 178.6(3) . . . . ?
O13 C12 C14 C19 0.1(5) . . . . ?
O20 C4 C3 O2 -2.1(4) . . . . ?
O20 C4 C3 C8 -179.3(3) . . . . ?
O20 C4 C5 C6 178.6(3) . . . . ?
N10 N11 C12 O13 -1.8(4) . . . . ?
N10 N11 C12 C14 177.1(3) . . . . ?
N11 N10 C9 C8 -178.7(3) . . . . ?
N11 C12 C14 C15 -0.4(5) . . . . ?
N11 C12 C14 C19 -178.9(3) . . . . ?
C12 C14 C15 C16 -177.2(3) . . . . ?
C12 C14 C19 C18 176.6(3) . . . . ?
C4 C3 C8 C9 178.1(3) . . . . ?
C4 C3 C8 C7 0.4(5) . . . . ?
C4 C5 C6 C7 0.8(5) . . . . ?
C14 C15 C16 N17 0.5(5) . . . . ?
C14 C19 C18 N17 0.7(6) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C3 C8 C9 N10 4.5(5) . . . . ?
C3 C8 C7 C6 0.0(5) . . . . ?
C15 C14 C19 C18 -2.0(5) . . . . ?
C8 C7 C6 C5 -0.7(5) . . . . ?
C9 N10 N11 C12 -178.6(3) . . . . ?
C9 C8 C7 C6 -177.7(3) . . . . ?
C7 C8 C9 N10 -177.8(3) . . . . ?
C5 C4 C3 O2 176.9(3) . . . . ?
C5 C4 C3 C8 -0.3(5) . . . . ?
C19 C14 C15 C16 1.4(5) . . . . ?
C16 N17 C18 C19 1.2(6) . . . . ?
C18 N17 C16 C15 -1.9(6) . . . . ?
C21 O20 C4 C3 -174.5(3) . . . . ?
C21 O20 C4 C5 6.5(5) . . . . ?

_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_2911
_database_code_depnum_ccdc_archive 'CCDC 2367622'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-13 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
tetrakis(ethoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v))
_chemical_formula_moiety         'C64 H64 N12 O20 V4'
_chemical_formula_sum            'C64 H64 N12 O20 V4'
_chemical_formula_weight         1525.03
_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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.6211(4)
_cell_length_b                   17.6211(4)
_cell_length_c                   21.2898(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6610.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6752
_cell_measurement_temperature    173.16(10)
_cell_measurement_theta_max      76.4740
_cell_measurement_theta_min      3.2480
_shelx_estimated_absorpt_T_max   0.523
_shelx_estimated_absorpt_T_min   0.431
_exptl_absorpt_coefficient_mu    5.322
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.400
_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            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 -2 0.0741
-2 -8 10 0.0693
8 3 9 0.0709
-8 -3 -9 0.0759
0 0 -14 0.0961
0 0 14 0.0851
-5 -5 -11 0.0790
5 5 11 0.0637
-6 1 12 0.0894
6 -1 -12 0.0894
9 0 -9 0.0787
-9 0 9 0.0589
-5 5 11 0.0600
5 -5 -11 0.1043
0 11 0 0.0672
0 -11 0 0.0782

_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12910
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.872
_diffrn_reflns_theta_min         3.256
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     47.00  72.00   0.50    0.60    --   46.91  52.00-124.00   50
  2  ω    119.00 174.00   0.50    1.00    --  107.75  52.00-124.00  110
  3  ω    134.00 159.00   0.50    1.00    --  107.75  15.00 -90.00   50
  4  ω     83.00 109.00   0.50    0.60    --   46.91  52.00-124.00   52
  5  ω    -25.00  27.00   0.50    0.60    --  -46.91  19.00  60.00  104
  6  ω    -59.00 -34.00   0.50    1.00    --  -86.25  52.00-124.00   50
  7  ω   -118.00 -76.00   0.50    0.60    --  -46.91-125.00  30.00   84
  8  ω     41.00  67.00   0.50    1.00    --  107.75 -77.00 -60.00   52
  9  ω     75.00 101.00   0.50    1.00    --  107.75 -77.00 -90.00   52
 10  ω     47.00  89.00   0.50    1.00    --  107.75 -77.00-120.00   84
 11  ω     39.00  71.00   0.50    1.00    --  107.75 -77.00 -90.00   64
 12  ω     39.00  64.00   0.50    1.00    --  107.75 -61.00-150.00   50
 13  ω     75.00 100.00   0.50    1.00    --  107.75 -77.00 -60.00   50
 14  ω     39.00  64.00   0.50    1.00    --  107.75 -61.00 -30.00   50
 15  ω     43.00  70.00   0.50    1.00    --  107.75 -61.00  90.00   54
 16  ω     36.00  67.00   0.50    1.00    --  107.75 -61.00 120.00   62
 17  ω     35.00  61.00   0.50    1.00    --  107.75 -61.00 -90.00   52
 18  ω     79.00 104.00   0.50    1.00    --  107.75 -95.00 -90.00   50
 19  ω     74.00 102.00   0.50    1.00    --  107.75 -92.00-131.00   56
 20  ω     42.00  67.00   0.50    1.00    --  107.75 -95.00 -90.00   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                2963
_reflns_number_total             3437
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      1.131
_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)+(0.0534P)²+15.2595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1352
_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:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C5(H5), C16(H16), C11(H11), C14(H14), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C)
;
_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 0.10728(3) 0.39458(3) 0.35849(2) 0.03131(17) Uani 1 1 d . . . . .
O2 O 0.20013(11) 0.38185(11) 0.31934(9) 0.0341(4) Uani 1 1 d . . . . .
O9 O 0.01461(11) 0.45295(11) 0.37624(10) 0.0340(4) Uani 1 1 d . . . . .
O20 O 0.33127(12) 0.31428(12) 0.30110(11) 0.0395(5) Uani 1 1 d . . . . .
O23 O 0.12660(12) 0.38378(12) 0.43990(11) 0.0389(5) Uani 1 1 d . . . . .
O22 O 0.06635(13) 0.31628(12) 0.34277(12) 0.0439(5) Uani 1 1 d . . . . .
N6 N 0.07488(13) 0.44429(13) 0.27126(11) 0.0311(5) Uani 1 1 d . . . . .
N7 N 0.00585(13) 0.48406(14) 0.27146(11) 0.0334(5) Uani 1 1 d . . . . .
N13 N -0.23213(14) 0.58909(14) 0.37249(12) 0.0329(5) Uani 1 1 d . . . . .
C3 C 0.22159(16) 0.37079(15) 0.25999(14) 0.0304(6) Uani 1 1 d . . . . .
C8 C -0.01979(16) 0.48378(16) 0.32867(14) 0.0311(6) Uani 1 1 d . . . . .
C4 C 0.17811(16) 0.39612(16) 0.20885(14) 0.0330(6) Uani 1 1 d . . . . .
C12 C -0.19783(18) 0.54179(19) 0.41214(15) 0.0410(7) Uani 1 1 d . . . . .
H12 H -0.221774 0.531271 0.451165 0.049 Uiso 1 1 calc R U . . .
C10 C -0.09366(16) 0.52070(16) 0.34245(14) 0.0321(6) Uani 1 1 d . . . . .
C19 C 0.29182(16) 0.33494(16) 0.24851(14) 0.0326(6) Uani 1 1 d . . . . .
C18 C 0.31583(17) 0.32228(18) 0.18777(16) 0.0393(7) Uani 1 1 d . . . . .
H18 H 0.363179 0.298135 0.180294 0.047 Uiso 1 1 calc R U . . .
C5 C 0.10747(16) 0.43633(17) 0.21710(14) 0.0339(6) Uani 1 1 d . . . . .
H5 H 0.083797 0.457939 0.181216 0.041 Uiso 1 1 calc R U . . .
C16 C 0.20384(18) 0.38274(19) 0.14715(15) 0.0414(7) Uani 1 1 d . . . . .
H16 H 0.174819 0.399974 0.112352 0.050 Uiso 1 1 calc R U . . .
C11 C -0.12918(18) 0.50727(19) 0.39937(15) 0.0404(7) Uani 1 1 d . . . . .
H11 H -0.106496 0.474527 0.429443 0.049 Uiso 1 1 calc R U . . .
C14 C -0.19714(18) 0.60272(19) 0.31812(15) 0.0419(7) Uani 1 1 d . . . . .
H14 H -0.220505 0.636798 0.289451 0.050 Uiso 1 1 calc R U . . .
C15 C -0.12916(19) 0.57027(19) 0.30114(15) 0.0422(7) Uani 1 1 d . . . . .
H15 H -0.106783 0.581637 0.261644 0.051 Uiso 1 1 calc R U . . .
C17 C 0.2708(2) 0.3448(2) 0.13734(16) 0.0466(8) Uani 1 1 d . . . . .
H17 H 0.286619 0.333858 0.095672 0.056 Uiso 1 1 calc R U . . .
C21 C 0.40897(18) 0.2932(2) 0.29280(18) 0.0479(8) Uani 1 1 d . . . . .
H21A H 0.411767 0.245984 0.268644 0.072 Uiso 1 1 calc R U . . .
H21B H 0.432715 0.285753 0.333961 0.072 Uiso 1 1 calc R U . . .
H21C H 0.435710 0.333573 0.270104 0.072 Uiso 1 1 calc R U . . .
C24 C 0.0951(2) 0.3290(2) 0.48218(18) 0.0497(8) Uani 1 1 d . . . . .
H24A H 0.130484 0.320720 0.517648 0.060 Uiso 1 1 calc R U . . .
H24B H 0.088285 0.280072 0.460051 0.060 Uiso 1 1 calc R U . . .
C25 C 0.0195(2) 0.3561(2) 0.5070(2) 0.0565(9) Uani 1 1 d . . . . .
H25A H -0.017674 0.356692 0.472811 0.085 Uiso 1 1 calc R U . . .
H25B H 0.025123 0.407427 0.524117 0.085 Uiso 1 1 calc R U . . .
H25C H 0.002138 0.321747 0.540227 0.085 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 O2 1.850(2) . ?
V1 O9 1.9666(19) . ?
V1 O23 1.776(2) . ?
V1 O22 1.592(2) . ?
V1 N6 2.131(2) . ?
V1 N13 2.403(2) 16_666 ?
O2 C3 1.333(3) . ?
O9 C8 1.299(3) . ?
O20 C19 1.367(4) . ?
O20 C21 1.429(4) . ?
O23 C24 1.432(4) . ?
N6 N7 1.404(3) . ?
N6 C5 1.296(4) . ?
N7 C8 1.299(4) . ?
N13 C12 1.331(4) . ?
N13 C14 1.333(4) . ?
C3 C4 1.404(4) . ?
C3 C19 1.411(4) . ?
C8 C10 1.484(4) . ?
C4 C5 1.443(4) . ?
C4 C16 1.410(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.381(4) . ?
C10 C11 1.384(4) . ?
C10 C15 1.388(4) . ?
C19 C18 1.379(4) . ?
C18 H18 0.9500 . ?
C18 C17 1.393(5) . ?
C5 H5 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.371(5) . ?
C11 H11 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.376(4) . ?
C15 H15 0.9500 . ?
C17 H17 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.510(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 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
O2 V1 O9 152.19(9) . . ?
O2 V1 N6 83.93(9) . . ?
O2 V1 N13 80.67(9) . 16_666 ?
O9 V1 N6 74.34(9) . . ?
O9 V1 N13 79.71(8) . 16_666 ?
O23 V1 O2 104.90(10) . . ?
O23 V1 O9 91.58(9) . . ?
O23 V1 N6 161.00(10) . . ?
O23 V1 N13 81.78(9) . 16_666 ?
O22 V1 O2 101.59(11) . . ?
O22 V1 O9 96.74(10) . . ?
O22 V1 O23 101.48(12) . . ?
O22 V1 N6 92.96(11) . . ?
O22 V1 N13 175.30(11) . 16_666 ?
N6 V1 N13 83.15(9) . 16_666 ?
C3 O2 V1 134.08(18) . . ?
C8 O9 V1 117.15(18) . . ?
C19 O20 C21 117.1(3) . . ?
C24 O23 V1 127.7(2) . . ?
N7 N6 V1 115.76(17) . . ?
C5 N6 V1 127.8(2) . . ?
C5 N6 N7 116.2(2) . . ?
C8 N7 N6 107.6(2) . . ?
C12 N13 V1 123.3(2) . 11_566 ?
C12 N13 C14 117.0(3) . . ?
C14 N13 V1 119.6(2) . 11_566 ?
O2 C3 C4 122.2(3) . . ?
O2 C3 C19 118.6(3) . . ?
C4 C3 C19 119.1(3) . . ?
O9 C8 C10 116.0(3) . . ?
N7 C8 O9 124.8(3) . . ?
N7 C8 C10 119.2(3) . . ?
C3 C4 C5 122.2(3) . . ?
C3 C4 C16 119.6(3) . . ?
C16 C4 C5 118.2(3) . . ?
N13 C12 H12 118.4 . . ?
N13 C12 C11 123.3(3) . . ?
C11 C12 H12 118.4 . . ?
C11 C10 C8 119.6(3) . . ?
C11 C10 C15 117.3(3) . . ?
C15 C10 C8 123.1(3) . . ?
O20 C19 C3 115.1(3) . . ?
O20 C19 C18 124.7(3) . . ?
C18 C19 C3 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C19 C18 C17 120.1(3) . . ?
C17 C18 H18 119.9 . . ?
N6 C5 C4 122.9(3) . . ?
N6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C4 C16 H16 120.0 . . ?
C17 C16 C4 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C12 C11 C10 119.5(3) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
N13 C14 H14 118.1 . . ?
N13 C14 C15 123.8(3) . . ?
C15 C14 H14 118.1 . . ?
C10 C15 H15 120.4 . . ?
C14 C15 C10 119.2(3) . . ?
C14 C15 H15 120.4 . . ?
C18 C17 H17 119.6 . . ?
C16 C17 C18 120.8(3) . . ?
C16 C17 H17 119.6 . . ?
O20 C21 H21A 109.5 . . ?
O20 C21 H21B 109.5 . . ?
O20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O23 C24 H24A 109.6 . . ?
O23 C24 H24B 109.6 . . ?
O23 C24 C25 110.4(3) . . ?
H24A C24 H24B 108.1 . . ?
C25 C24 H24A 109.6 . . ?
C25 C24 H24B 109.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 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 O2 C3 C4 26.7(4) . . . . ?
V1 O2 C3 C19 -155.8(2) . . . . ?
V1 O9 C8 N7 -5.9(4) . . . . ?
V1 O9 C8 C10 173.93(18) . . . . ?
V1 O23 C24 C25 -84.2(4) . . . . ?
V1 N6 N7 C8 3.6(3) . . . . ?
V1 N6 C5 C4 -6.2(4) . . . . ?
V1 N13 C12 C11 175.8(3) 11_566 . . . ?
V1 N13 C14 C15 -175.2(3) 11_566 . . . ?
O2 V1 O23 C24 -120.4(2) . . . . ?
O2 C3 C4 C5 0.4(4) . . . . ?
O2 C3 C4 C16 180.0(3) . . . . ?
O2 C3 C19 O20 0.5(4) . . . . ?
O2 C3 C19 C18 179.8(3) . . . . ?
O9 V1 O2 C3 -68.8(3) . . . . ?
O9 V1 O23 C24 82.2(3) . . . . ?
O9 C8 C10 C11 -13.5(4) . . . . ?
O9 C8 C10 C15 165.1(3) . . . . ?
O20 C19 C18 C17 179.2(3) . . . . ?
O23 V1 O2 C3 166.7(2) . . . . ?
O22 V1 O2 C3 61.4(3) . . . . ?
O22 V1 O23 C24 -15.0(3) . . . . ?
N6 V1 O2 C3 -30.4(2) . . . . ?
N6 V1 O23 C24 123.7(3) . . . . ?
N6 N7 C8 O9 1.2(4) . . . . ?
N6 N7 C8 C10 -178.6(2) . . . . ?
N7 N6 C5 C4 -179.2(2) . . . . ?
N7 C8 C10 C11 166.4(3) . . . . ?
N7 C8 C10 C15 -15.1(4) . . . . ?
N13 V1 O2 C3 -114.4(3) 16_666 . . . ?
N13 V1 O23 C24 161.6(3) 16_666 . . . ?
N13 C12 C11 C10 -1.0(5) . . . . ?
N13 C14 C15 C10 -0.5(6) . . . . ?
C3 C4 C5 N6 -8.2(5) . . . . ?
C3 C4 C16 C17 0.3(5) . . . . ?
C3 C19 C18 C17 0.0(5) . . . . ?
C8 C10 C11 C12 179.9(3) . . . . ?
C8 C10 C15 C14 -179.1(3) . . . . ?
C4 C3 C19 O20 178.1(2) . . . . ?
C4 C3 C19 C18 -2.6(4) . . . . ?
C4 C16 C17 C18 -3.0(5) . . . . ?
C12 N13 C14 C15 0.7(5) . . . . ?
C19 C3 C4 C5 -177.1(3) . . . . ?
C19 C3 C4 C16 2.4(4) . . . . ?
C19 C18 C17 C16 2.9(5) . . . . ?
C5 N6 N7 C8 177.5(3) . . . . ?
C5 C4 C16 C17 179.9(3) . . . . ?
C16 C4 C5 N6 172.3(3) . . . . ?
C11 C10 C15 C14 -0.5(5) . . . . ?
C14 N13 C12 C11 0.0(5) . . . . ?
C15 C10 C11 C12 1.2(5) . . . . ?
C21 O20 C19 C3 -166.7(3) . . . . ?
C21 O20 C19 C18 14.0(4) . . . . ?

_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_4442
_database_code_depnum_ccdc_archive 'CCDC 2367620'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-19 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
# start Validation Reply Form
_vrf_PLAT430_exp_4442            
;
PROBLEM: Short Inter D...A Contact  O2       ..N13      .       2.79 Ang.  
RESPONSE: V-py coordination tetramer.
;
_vrf_PLAT910_exp_4442            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: Some of the low-angle reflections obscured by beam stop.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        
tetrakis(methoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v))
_chemical_formula_moiety         'C60 H56 N12 O20 V4'
_chemical_formula_sum            'C60 H56 N12 O20 V4'
_chemical_formula_weight         1468.92
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.5925(4)
_cell_length_b                   17.5925(4)
_cell_length_c                   21.6260(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6693.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.493
_cell_measurement_theta_min      4.282
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34740
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         4.282
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1285
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00 -78.00   1.00   40.00    --  -28.78-178.00 -30.00   29
  2  ω     12.00  99.00   1.00   40.00    --   30.34  37.00  90.00   87
  3  ω    -38.00  62.00   1.00   40.00    --   30.34 -37.00 -90.00  100
  4  ω     30.00  75.00   1.00   40.00    --   30.34 -99.00-150.00   45
  5  ω    -40.00  54.00   1.00   40.00    --   30.34 -57.00 150.00   94
  6  ω      7.00 101.00   1.00   40.00    --   30.34  57.00-180.00   94
  7  ω     35.00 110.00   1.00   40.00    --   30.34 178.00 150.00   75
  8  ω     -3.00  86.00   1.00   40.00    --   30.34  77.00 -30.00   89
  9  ω     -2.00 104.00   1.00   40.00    --   30.34  37.00 -60.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2870
_reflns_number_total             3830
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.024
_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)+(0.0623P)²+6.9113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1321
_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:
 C9(H9), C7(H7), C5(H5), C15(H15), C16(H16), C6(H6), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C)
;
_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 0.64320(2) 0.35509(2) 0.60638(2) 0.04015(16) Uani 1 1 d . . . . .
O2 O 0.63217(10) 0.44856(10) 0.56885(8) 0.0451(4) Uani 1 1 d . . . . .
O13 O 0.70088(10) 0.26239(10) 0.62459(8) 0.0445(4) Uani 1 1 d . . . . .
O23 O 0.62973(11) 0.37303(11) 0.68659(9) 0.0496(5) Uani 1 1 d . . . . .
O20 O 0.56583(12) 0.58064(10) 0.55117(9) 0.0524(5) Uani 1 1 d . . . . .
O22 O 0.56566(11) 0.31459(12) 0.58860(10) 0.0587(5) Uani 1 1 d . . . . .
N10 N 0.69572(12) 0.32391(11) 0.52127(10) 0.0399(5) Uani 1 1 d . . . . .
N17 N 0.84245(12) 0.01771(12) 0.62264(10) 0.0418(5) Uani 1 1 d . . . . .
N11 N 0.73663(13) 0.25548(12) 0.52214(10) 0.0457(5) Uani 1 1 d . . . . .
C3 C 0.62238(13) 0.47087(14) 0.51024(11) 0.0376(5) Uani 1 1 d . . . . .
C9 C 0.68891(15) 0.35715(14) 0.46854(12) 0.0426(6) Uani 1 1 d . . . . .
H9 H 0.711005 0.334365 0.434153 0.051 Uiso 1 1 calc R U . . .
C4 C 0.64878(14) 0.42792(14) 0.45999(12) 0.0415(6) Uani 1 1 d . . . . .
C12 C 0.73472(14) 0.22912(14) 0.57840(12) 0.0419(6) Uani 1 1 d . . . . .
C8 C 0.58746(14) 0.54171(14) 0.49936(12) 0.0410(6) Uani 1 1 d . . . . .
C14 C 0.77361(15) 0.15604(14) 0.59254(12) 0.0423(6) Uani 1 1 d . . . . .
C7 C 0.57655(17) 0.56675(17) 0.43964(13) 0.0531(7) Uani 1 1 d . . . . .
H7 H 0.552543 0.613030 0.432552 0.064 Uiso 1 1 calc R U . . .
C5 C 0.63812(18) 0.45509(17) 0.39950(13) 0.0542(7) Uani 1 1 d . . . . .
H5 H 0.655873 0.427223 0.365934 0.065 Uiso 1 1 calc R U . . .
C15 C 0.76649(19) 0.12475(18) 0.65021(14) 0.0606(8) Uani 1 1 d . . . . .
H15 H 0.738341 0.149493 0.680538 0.073 Uiso 1 1 calc R U . . .
C16 C 0.8013(2) 0.05638(17) 0.66303(14) 0.0620(9) Uani 1 1 d . . . . .
H16 H 0.795452 0.036182 0.702487 0.074 Uiso 1 1 calc R U . . .
C6 C 0.6011(2) 0.52337(19) 0.39017(14) 0.0635(9) Uani 1 1 d . . . . .
H6 H 0.592647 0.540441 0.350062 0.076 Uiso 1 1 calc R U . . .
C21 C 0.5448(2) 0.65816(17) 0.54397(16) 0.0663(9) Uani 1 1 d . . . . .
H21A H 0.499479 0.661378 0.519385 0.099 Uiso 1 1 calc R U . . .
H21B H 0.585164 0.685242 0.523785 0.099 Uiso 1 1 calc R U . . .
H21C H 0.535564 0.680220 0.583869 0.099 Uiso 1 1 calc R U . . .
C18 C 0.8509(2) 0.04996(18) 0.56744(14) 0.0690(10) Uani 1 1 d . . . . .
H18 H 0.881356 0.025406 0.538496 0.083 Uiso 1 1 calc R U . . .
C19 C 0.8175(2) 0.11719(19) 0.55072(14) 0.0730(11) Uani 1 1 d . . . . .
H19 H 0.824593 0.136479 0.511099 0.088 Uiso 1 1 calc R U . . .
C24 C 0.5749(2) 0.3386(2) 0.72531(18) 0.0856(12) Uani 1 1 d . . . . .
H24A H 0.528927 0.330294 0.702326 0.128 Uiso 1 1 calc R U . . .
H24B H 0.564470 0.371350 0.759801 0.128 Uiso 1 1 calc R U . . .
H24C H 0.593954 0.290827 0.740085 0.128 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 O2 1.8439(18) . ?
V1 O13 1.9608(17) . ?
V1 O23 1.7789(19) . ?
V1 O22 1.586(2) . ?
V1 N10 2.131(2) . ?
V1 N17 2.420(2) 15_666 ?
O2 C3 1.338(3) . ?
O13 C12 1.302(3) . ?
O23 C24 1.414(4) . ?
O20 C8 1.367(3) . ?
O20 C21 1.422(3) . ?
N10 N11 1.403(3) . ?
N10 C9 1.287(3) . ?
N17 C16 1.323(3) . ?
N17 C18 1.330(4) . ?
N11 C12 1.303(3) . ?
C3 C4 1.403(4) . ?
C3 C8 1.409(3) . ?
C9 H9 0.9300 . ?
C9 C4 1.443(3) . ?
C4 C5 1.405(4) . ?
C12 C14 1.488(3) . ?
C8 C7 1.378(4) . ?
C14 C15 1.369(4) . ?
C14 C19 1.372(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(4) . ?
C16 H16 0.9300 . ?
C6 H6 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C18 H18 0.9300 . ?
C18 C19 1.369(4) . ?
C19 H19 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O13 152.20(8) . . ?
O2 V1 N10 83.97(8) . . ?
O2 V1 N17 80.66(8) . 15_666 ?
O13 V1 N10 74.63(8) . . ?
O13 V1 N17 79.11(7) . 15_666 ?
O23 V1 O2 104.89(9) . . ?
O23 V1 O13 91.18(8) . . ?
O23 V1 N10 160.99(8) . . ?
O23 V1 N17 82.54(8) . 15_666 ?
O22 V1 O2 101.73(10) . . ?
O22 V1 O13 96.90(9) . . ?
O22 V1 O23 101.62(11) . . ?
O22 V1 N10 92.74(10) . . ?
O22 V1 N17 174.37(10) . 15_666 ?
N10 V1 N17 82.39(8) . 15_666 ?
C3 O2 V1 133.80(16) . . ?
C12 O13 V1 117.16(16) . . ?
C24 O23 V1 126.3(2) . . ?
C8 O20 C21 117.6(2) . . ?
N11 N10 V1 115.58(15) . . ?
C9 N10 V1 127.43(17) . . ?
C9 N10 N11 116.7(2) . . ?
C16 N17 V1 123.40(18) . 12_757 ?
C16 N17 C18 115.8(2) . . ?
C18 N17 V1 120.77(18) . 12_757 ?
C12 N11 N10 107.8(2) . . ?
O2 C3 C4 122.2(2) . . ?
O2 C3 C8 118.3(2) . . ?
C4 C3 C8 119.4(2) . . ?
N10 C9 H9 118.3 . . ?
N10 C9 C4 123.4(2) . . ?
C4 C9 H9 118.3 . . ?
C3 C4 C9 121.8(2) . . ?
C3 C4 C5 119.6(2) . . ?
C5 C4 C9 118.6(2) . . ?
O13 C12 N11 124.6(2) . . ?
O13 C12 C14 116.2(2) . . ?
N11 C12 C14 119.2(2) . . ?
O20 C8 C3 115.3(2) . . ?
O20 C8 C7 124.7(2) . . ?
C7 C8 C3 120.0(2) . . ?
C15 C14 C12 119.5(2) . . ?
C15 C14 C19 116.9(3) . . ?
C19 C14 C12 123.6(2) . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.3(3) . . ?
C6 C7 H7 119.8 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.6(3) . . ?
C16 C15 H15 120.2 . . ?
N17 C16 C15 124.0(3) . . ?
N17 C16 H16 118.0 . . ?
C15 C16 H16 118.0 . . ?
C7 C6 H6 119.5 . . ?
C5 C6 C7 120.9(3) . . ?
C5 C6 H6 119.5 . . ?
O20 C21 H21A 109.5 . . ?
O20 C21 H21B 109.5 . . ?
O20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N17 C18 H18 118.1 . . ?
N17 C18 C19 123.9(3) . . ?
C19 C18 H18 118.1 . . ?
C14 C19 H19 120.1 . . ?
C18 C19 C14 119.9(3) . . ?
C18 C19 H19 120.1 . . ?
O23 C24 H24A 109.5 . . ?
O23 C24 H24B 109.5 . . ?
O23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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 O2 C3 C4 -27.2(4) . . . . ?
V1 O2 C3 C8 155.87(18) . . . . ?
V1 O13 C12 N11 4.3(3) . . . . ?
V1 O13 C12 C14 -175.90(16) . . . . ?
V1 N10 N11 C12 -3.0(3) . . . . ?
V1 N10 C9 C4 6.5(4) . . . . ?
V1 N17 C16 C15 -175.1(3) 12_757 . . . ?
V1 N17 C18 C19 174.3(3) 12_757 . . . ?
O2 V1 O23 C24 122.5(3) . . . . ?
O2 C3 C4 C9 -0.6(4) . . . . ?
O2 C3 C4 C5 -178.7(2) . . . . ?
O2 C3 C8 O20 -0.9(3) . . . . ?
O2 C3 C8 C7 179.8(2) . . . . ?
O13 V1 O2 C3 70.7(3) . . . . ?
O13 V1 O23 C24 -80.4(3) . . . . ?
O13 C12 C14 C15 5.7(4) . . . . ?
O13 C12 C14 C19 -174.0(3) . . . . ?
O23 V1 O2 C3 -165.9(2) . . . . ?
O20 C8 C7 C6 179.4(3) . . . . ?
O22 V1 O2 C3 -60.4(2) . . . . ?
O22 V1 O23 C24 16.9(3) . . . . ?
N10 V1 O2 C3 31.2(2) . . . . ?
N10 V1 O23 C24 -121.5(3) . . . . ?
N10 N11 C12 O13 -0.6(4) . . . . ?
N10 N11 C12 C14 179.6(2) . . . . ?
N10 C9 C4 C3 8.4(4) . . . . ?
N10 C9 C4 C5 -173.5(3) . . . . ?
N17 V1 O2 C3 114.4(2) 15_666 . . . ?
N17 V1 O23 C24 -159.3(3) 15_666 . . . ?
N17 C18 C19 C14 1.4(6) . . . . ?
N11 N10 C9 C4 -179.8(2) . . . . ?
N11 C12 C14 C15 -174.5(3) . . . . ?
N11 C12 C14 C19 5.9(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C3 C8 C7 C6 -1.3(4) . . . . ?
C9 N10 N11 C12 -177.5(2) . . . . ?
C9 C4 C5 C6 -178.8(3) . . . . ?
C4 C3 C8 O20 -177.9(2) . . . . ?
C4 C3 C8 C7 2.8(4) . . . . ?
C4 C5 C6 C7 2.1(5) . . . . ?
C12 C14 C15 C16 178.8(3) . . . . ?
C12 C14 C19 C18 -179.6(3) . . . . ?
C8 C3 C4 C9 176.3(2) . . . . ?
C8 C3 C4 C5 -1.8(4) . . . . ?
C8 C7 C6 C5 -1.1(5) . . . . ?
C14 C15 C16 N17 0.2(6) . . . . ?
C15 C14 C19 C18 0.8(5) . . . . ?
C16 N17 C18 C19 -2.7(6) . . . . ?
C21 O20 C8 C3 167.5(2) . . . . ?
C21 O20 C8 C7 -13.3(4) . . . . ?
C18 N17 C16 C15 1.9(5) . . . . ?
C19 C14 C15 C16 -1.6(5) . . . . ?

_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_6176_auto
_database_code_depnum_ccdc_archive 'CCDC 2400624'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-13 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_audit_creation_date             2025-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
(ethanol)-cis-(2-oxido-3-methoxybenzaldehydeisonicotinylhydrazonato)-dioxomolybdenum(vi)
_chemical_formula_moiety         'C16 H17 Mo N3 O6'
_chemical_formula_sum            'C16 H17 Mo N3 O6'
_chemical_formula_weight         443.26
_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'
Mo Mo -0.0483 2.7339 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.28057(4)
_cell_length_b                   10.45368(5)
_cell_length_c                   12.64056(6)
_cell_angle_alpha                113.2670(4)
_cell_angle_beta                 96.4325(4)
_cell_angle_gamma                97.8303(4)
_cell_volume                     860.915(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      79.7270
_cell_measurement_theta_min      3.8590
_shelx_estimated_absorpt_T_max   0.446
_shelx_estimated_absorpt_T_min   0.275
_exptl_absorpt_coefficient_mu    6.596
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             448
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1020
0 -2 1 0.0981
0 2 -1 0.1152
1 -2 1 0.0941
2 1 -1 0.1030
-1 0 0 0.0978
0 0 -1 0.0438

_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.146
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.888
_diffrn_reflns_theta_min         3.871
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  14.00   0.50    0.05    --   18.00  96.00-152.97   52
  2  ω    -15.00  11.00   0.50    0.05    --   18.00 100.00 -59.87   52
  3  ω     11.00  36.00   0.50    0.05    --   34.00  77.00 -30.82   50
  4  ω     14.00  40.00   0.50    0.05    --   34.00  73.00 -87.03   52
  5  ω     17.00  44.00   0.50    0.05    --   38.00  73.00-172.10   54
  6  ω     17.00  42.00   0.50    0.05    --   38.00  73.00  -7.59   50
  7  ω     11.00  36.00   0.50    0.05    --   34.00  77.00  10.11   50
  8  ω    -12.00  13.00   0.50    0.05    --   18.00 100.00  59.33   50
  9  ω     11.00  36.00   0.50    0.05    --   34.00  77.00 138.51   50
 10  ω     18.00  43.00   0.50    0.05    --   38.00  71.00 129.21   50
 11  ω     17.00  42.00   0.50    0.05    --   38.00  72.00  77.12   50
 12  ω     29.00  55.00   0.50    0.05    --   46.00  65.00 134.51   52
 13  ω     93.00 118.00   0.50    0.05    --   46.00  65.00 134.51   50
 14  ω     68.00 121.00   0.50    0.05    --   48.10  19.00  60.00  106
 15  ω     60.00  88.00   0.50    0.05    --   42.00  67.00  30.78   56
 16  ω     27.00  53.00   0.50    0.05    --   42.00  67.00  30.78   52
 17  ω     38.00  65.00   0.50    0.05    --   48.10  19.00  60.00   54
 18  ω     17.00  42.00   0.50    0.05    --   38.00  72.00-129.06   50
 19  ω     36.00  66.00   0.50    0.05    --   48.10  57.00-150.00   60
 20  ω     67.00  92.00   0.50    0.05    --  113.25   0.00-150.00   50
 21  ω     91.00 125.00   0.50    0.05    --  113.25  77.00-180.00   68
 22  ω    137.00 177.00   0.50    0.05    --  113.25  77.00-180.00   80
 23  ω     92.00 148.00   0.50    0.05    --  113.25  77.00 -30.00  112
 24  ω    135.00 178.00   0.50    0.05    --  113.25  77.00   0.00   86
 25  ω     91.00 128.00   0.50    0.05    --  113.25  77.00   0.00   74
 26  ω     92.00 156.00   0.50    0.05    --  113.25  77.00  30.00  128
 27  ω     91.00 140.00   0.50    0.05    --  113.25  77.00  90.00   98
 28  ω     93.00 173.00   0.50    0.05    --  113.25  77.00 120.00  160
 29  ω    141.00 167.00   0.50    0.05    --  113.25  77.00 150.00   52
 30  ω     91.00 129.00   0.50    0.05    --  113.25  77.00 150.00   76
 31  ω     96.00 122.00   0.50    0.05    --  113.25  77.00 -60.00   52
 32  ω    135.00 160.00   0.50    0.05    --  113.25  77.00 -60.00   50
 33  ω    128.00 177.00   0.50    0.05    --  113.25  77.00-120.00   98
 34  ω     94.00 120.00   0.50    0.05    --  113.25  77.00-120.00   52
 35  ω     93.00 119.00   0.50    0.05    --  113.25  77.00-150.00   52
 36  ω    124.00 149.00   0.50    0.05    --  113.25  77.00-150.00   50
 37  ω     91.00 157.00   0.50    0.05    --  113.25  75.00-133.81  132
 38  ω     95.00 142.00   0.50    0.05    --  113.25  77.00 -90.00   94
 39  ω    100.00 125.00   0.50    0.05    --  113.25  61.00-150.00   50
 40  ω     91.00 178.00   0.50    0.05    --  113.25  77.00  60.00  174
 41  ω    100.00 147.00   0.50    0.05    --  113.25  61.00  60.00   94
 42  ω     99.00 132.00   0.50    0.05    --  113.25  61.00  30.00   66
 43  ω     98.00 143.00   0.50    0.05    --  113.25  61.00  90.00   90
 44  ω     97.00 150.00   0.50    0.05    --  113.25  62.00 177.26  106
 45  ω     97.00 136.00   0.50    0.05    --  113.25  61.00 120.00   78
 46  ω    153.00 178.00   0.50    0.05    --  113.25  61.00  30.00   50
 47  ω    148.00 178.00   0.50    0.05    --  113.25  61.00-150.00   60
 48  ω    148.00 174.00   0.50    0.05    --  113.25  61.00 -90.00   52
 49  ω     98.00 144.00   0.50    0.05    --  113.25  61.00 -90.00   92
 50  ω     99.00 161.00   0.50    0.05    --  113.25  61.00 -60.00  124
 51  ω    102.00 134.00   0.50    0.05    --  113.25  61.00 -30.00   64
 52  ω    103.00 150.00   0.50    0.05    --  113.25  61.00   0.00   94
 53  ω    113.00 138.00   0.50    0.05    --  113.25  45.00  60.00   50
 54  ω    100.00 127.00   0.50    0.05    --  113.25  61.00 150.00   54
 55  ω    141.00 169.00   0.50    0.05    --  113.25  45.00 150.00   56
 56  ω    149.00 174.00   0.50    0.05    --  113.25  61.00  90.00   50
 57  ω    108.00 133.00   0.50    0.05    --  113.25  30.00 120.00   50
 58  ω    142.00 168.00   0.50    0.05    --  113.25  30.00  30.00   52
 59  ω    111.00 137.00   0.50    0.05    --  113.25  45.00 -90.00   52
 60  ω    122.00 148.00   0.50    0.05    --  113.25  45.00-120.00   52
 61  ω    107.00 166.00   0.50    0.05    --  113.25  45.00-150.00  118
 62  ω    117.00 143.00   0.50    0.05    --  113.25  30.00-120.00   52
 63  ω    118.00 178.00   0.50    0.05    --  113.25   0.00-150.00  120
 64  ω    139.00 165.00   0.50    0.05    --  113.25  30.00 -90.00   52
 65  ω    114.00 139.00   0.50    0.05    --  113.25  30.00 -30.00   50
 66  ω    153.00 178.00   0.50    0.05    --  113.25  30.00 -30.00   50
 67  ω    104.00 160.00   0.50    0.05    --  113.25  17.00  13.05  112
 68  ω    131.00 178.00   0.50    0.05    --  113.25 125.00 -30.00   94
 69  ω    124.00 177.00   0.50    0.05    --  113.25 125.00 -60.00  106
 70  ω    112.00 137.00   0.50    0.05    --  113.25 127.00 -28.00   50
 71  ω    115.00 145.00   0.50    0.05    --  113.25 125.00  30.00   60
 72  ω    151.00 178.00   0.50    0.05    --  113.25 125.00  30.00   54
 73  ω    153.00 178.00   0.50    0.05    --  113.25 125.00  90.00   50
 74  ω    104.00 140.00   0.50    0.05    --  113.25 145.00 139.00   72
 75  ω    116.00 159.00   0.50    0.05    --  113.25 125.00 150.00   86
 76  ω    119.00 151.00   0.50    0.05    --  113.25 125.00 120.00   64
 77  ω    111.00 138.00   0.50    0.05    --  113.25 125.00  90.00   54
 78  ω    117.00 163.00   0.50    0.05    --  113.25 125.00 -90.00   92
 79  ω    131.00 157.00   0.50    0.05    --  113.25 125.00-120.00   52
 80  ω     42.00  67.00   0.50    0.05    --  113.25 -61.00-120.00   50
 81  ω     61.00  90.00   0.50    0.05    --  113.25 -77.00-150.00   58
 82  ω     80.00 105.00   0.50    0.05    --  113.25 -77.00-120.00   50
 83  ω     42.00  77.00   0.50    0.05    --  113.25 -77.00-120.00   70
 84  ω     60.00  98.00   0.50    0.05    --  113.25 -77.00 -60.00   76
 85  ω     73.00  98.00   0.50    0.05    --  113.25 -77.00 120.00   50
 86  ω     43.00  85.00   0.50    0.05    --  113.25 -77.00  90.00   84
 87  ω     42.00  70.00   0.50    0.05    --  113.25 -77.00 -30.00   56
 88  ω     42.00  68.00   0.50    0.05    --  113.25 -61.00 -90.00   52
 89  ω     42.00  67.00   0.50    0.05    --  113.25 -61.00-180.00   50
 90  ω     91.00 140.00   0.50    0.05    --  113.25 -86.00-105.18   98
 91  ω     46.00  71.00   0.50    0.05    --  113.25-127.00-104.00   50
 92  ω     45.00  78.00   0.50    0.05    --  113.25-125.00-180.00   66
 93  ω     38.00  93.00   0.50    0.05    --   48.10-127.00-104.00  110
 94  ω     45.00  79.00   0.50    0.05    --  113.25-125.00 -30.00   68
 95  ω     87.00 125.00   0.50    0.05    --  113.25-145.00  87.00   76
 96  ω     48.00  91.00   0.50    0.05    --  113.25-125.00 120.00   86
 97  ω     46.00 107.00   0.50    0.05    --   48.10-145.00  87.00  122
 98  ω     48.00  76.00   0.50    0.05    --  113.25-125.00   0.00   56
 99  ω     76.00 105.00   0.50    0.05    --  113.25 -95.00  90.00   58
100  ω     57.00 111.00   0.50    0.05    --  113.25-125.00  90.00  108
101  ω     78.00 104.00   0.50    0.05    --  113.25 -95.00 150.00   52
102  ω     69.00 102.00   0.50    0.05    --  113.25 -95.00   0.00   66
103  ω     66.00  93.00   0.50    0.05    --  113.25 -95.00  60.00   54
104  ω     44.00  80.00   0.50    0.05    --  113.25-125.00-120.00   72
105  ω     45.00  80.00   0.50    0.05    --  113.25-125.00-150.00   70
106  ω     86.00 111.00   0.50    0.05    --  113.25-125.00-150.00   50
107  ω     81.00 106.00   0.50    0.05    --  113.25 -95.00-120.00   50
108  ω     43.00  73.00   0.50    0.05    --  113.25 -87.00  76.41   60
109  ω     92.00 118.00   0.50    0.05    --  113.25 -87.00  76.41   52
110  ω    -73.00 -31.00   0.50    0.05    --  -48.10 -62.00  70.63   84
111  ω    -58.00 -33.00   0.50    0.05    --  -48.10 -57.00 -60.00   50
112  ω    -75.00 -37.00   0.50    0.05    --  -48.10 -57.00-120.00   76
113  ω   -119.00 -86.00   0.50    0.05    --  -48.10 -57.00-120.00   66
114  ω   -117.00 -91.00   0.50    0.05    --  -48.10 -57.00 -60.00   52
115  ω   -114.00 -82.00   0.50    0.05    --  -48.10-127.00-104.00   64
116  ω   -141.00-116.00   0.50    0.05    --  -91.75-127.00-104.00   50
117  ω   -115.00 -88.00   0.50    0.05    --  -48.10-145.00  87.00   54
118  ω   -130.00-105.00   0.50    0.05    --  -91.75-145.00  87.00   50
119  ω    -94.00 -68.00   0.50    0.05    --  -82.00 -53.00 -31.89   52
120  ω    -76.00 -51.00   0.50    0.05    --  -70.00 -67.00 -54.45   50
121  ω   -104.00 -78.00   0.50    0.05    --  -91.75 -68.00-142.47   52
122  ω    -78.00 -52.00   0.50    0.05    --  -70.00 -67.00-149.25   52
123  ω   -101.00 -73.00   0.50    0.05    --  -91.75 -67.00 -93.39   56
124  ω   -101.00 -73.00   0.50    0.05    --  -91.75 -67.00 -39.36   56
125  ω    -85.00 -53.00   0.50    0.05    --  -70.00 -67.00 -40.47   64
126  ω    -91.00 -64.00   0.50    0.05    --  -82.00 -66.00 -77.73   54
127  ω   -141.00-114.00   0.50    0.05    --  -70.00 -67.00 -54.45   54
128  ω   -108.00 -73.00   0.50    0.05    --  -91.75 -67.00  51.97   70
129  ω    -80.00 -53.00   0.50    0.05    --  -70.00 -67.00 145.77   54
130  ω    -94.00 -68.00   0.50    0.05    --  -86.00 -66.00 140.47   52
131  ω   -108.00 -73.00   0.50    0.05    --  -91.75 -67.00 127.52   70
132  ω    -90.00 -48.00   0.50    0.05    --  -66.00 -66.00 177.72   84
133  ω   -154.00-128.00   0.50    0.05    --  -86.00 -66.00 140.47   52
134  ω    -72.00 -42.00   0.50    0.05    --  -58.00 -65.00  40.45   60
135  ω    -95.00 -68.00   0.50    0.05    --  -86.00 -65.00 -28.71   54
136  ω    -85.00 -37.00   0.50    0.05    --  -54.00 -65.00   9.38   96
137  ω    -82.00 -56.00   0.50    0.05    --  -74.00 -65.00 -72.36   52
138  ω    -78.00 -52.00   0.50    0.05    --  -70.00 -65.00-110.55   52
139  ω    -80.00 -52.00   0.50    0.05    --  -70.00 -65.00-124.84   56
140  ω    -79.00 -53.00   0.50    0.05    --  -70.00 -63.00-137.97   52
141  ω    -99.00 -74.00   0.50    0.05    --  -91.75 -66.00-123.37   50
142  ω   -100.00 -75.00   0.50    0.05    --  -91.75 -62.00-157.89   50
143  ω    -83.00 -58.00   0.50    0.05    --  -74.00 -63.00-165.94   50
144  ω   -140.00-114.00   0.50    0.05    --  -70.00 -65.00-124.84   52
145  ω   -101.00 -75.00   0.50    0.05    --  -91.75 -62.00 -65.88   52
146  ω    -85.00 -57.00   0.50    0.05    --  -74.00 -62.00-105.79   56
147  ω   -140.00-113.00   0.50    0.05    --  -74.00 -62.00-105.79   54
148  ω   -102.00 -75.00   0.50    0.05    --  -91.75 -61.00-109.01   54
149  ω   -101.00 -75.00   0.50    0.05    --  -91.75 -61.00 -90.00   52
150  ω   -101.00 -75.00   0.50    0.05    --  -91.75 -61.00-120.00   52
151  ω   -101.00 -76.00   0.50    0.05    --  -91.75 -60.00-139.16   50
152  ω   -107.00 -75.00   0.50    0.05    --  -91.75 -62.00  17.79   64
153  ω    -78.00 -51.00   0.50    0.05    --  -66.00 -59.00  60.71   54
154  ω    -85.00 -59.00   0.50    0.05    --  -74.00 -58.00  42.50   52
155  ω   -111.00 -77.00   0.50    0.05    --  -91.75 -58.00  76.19   68
156  ω   -106.00 -76.00   0.50    0.05    --  -91.75 -58.00  94.53   60
157  ω   -126.00 -99.00   0.50    0.05    --  -66.00 -58.00  99.37   54
158  ω    -99.00 -64.00   0.50    0.05    --  -78.00 -57.00  36.05   70
159  ω    -85.00 -59.00   0.50    0.05    --  -74.00 -57.00  81.75   52
160  ω   -100.00 -69.00   0.50    0.05    --  -82.00 -56.00  19.18   62
161  ω    -84.00 -59.00   0.50    0.05    --  -74.00 -56.00   1.03   50
162  ω    -87.00 -60.00   0.50    0.05    --  -74.00 -55.00 -19.01   54
163  ω    -98.00 -63.00   0.50    0.05    --  -78.00 -56.00  95.20   70
164  ω    -78.00 -53.00   0.50    0.05    --  -66.00 -58.00  99.37   50
165  ω    -96.00 -64.00   0.50    0.05    --  -82.00 -64.00 163.18   64
166  ω    -89.00 -57.00   0.50    0.05    --  -74.00 -64.00 174.24   64
167  ω    -78.00 -53.00   0.50    0.05    --  -91.75 127.00 -28.00   50
168  ω    -63.00 -37.00   0.50    0.05    --  -48.10 127.00 -28.00   52
169  ω    -85.00 -58.00   0.50    0.05    --  -48.10 145.00 139.00   54
;
_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                3675
_reflns_number_total             3703
_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 1.171.42.81a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0137(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0197
_refine_ls_restrained_S_all      1.070
_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)+(0.0268P)²+0.3936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0516
_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:
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C11(H11), C13(H13), C12(H12), C18(H18), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_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
Mo1 Mo 0.56332(2) 0.47265(2) 0.75392(2) 0.02944(7) Uani 1 1 d . . . . .
O2 O 0.62651(18) 0.68659(12) 0.83417(11) 0.0361(3) Uani 1 1 d . . . . .
O9 O 0.37953(18) 0.30062(12) 0.66053(10) 0.0345(3) Uani 1 1 d . . . . .
O14 O 0.29877(19) 0.02371(13) 0.54614(12) 0.0402(3) Uani 1 1 d . . . . .
O24 O 0.3147(2) 0.52190(15) 0.85379(13) 0.0434(3) Uani 1 1 d . . . . .
O22 O 0.6618(2) 0.44349(14) 0.86842(12) 0.0438(3) Uani 1 1 d . . . . .
O23 O 0.7254(2) 0.44969(15) 0.66462(13) 0.0443(3) Uani 1 1 d . . . . .
N5 N 0.3840(2) 0.55760(15) 0.65099(13) 0.0331(3) Uani 1 1 d . . . . .
N4 N 0.4119(2) 0.70578(15) 0.69445(14) 0.0368(3) Uani 1 1 d . . . . .
C8 C 0.2809(2) 0.24810(17) 0.55087(14) 0.0315(3) Uani 1 1 d . . . . .
N19 N 0.6785(3) 1.21129(16) 0.97839(16) 0.0472(4) Uani 1 1 d . . . . .
C3 C 0.5411(3) 0.76043(17) 0.78777(15) 0.0332(3) Uani 1 1 d . . . . .
C7 C 0.2188(3) 0.33398(18) 0.49833(15) 0.0341(4) Uani 1 1 d . . . . .
C16 C 0.5947(3) 0.91742(17) 0.85071(15) 0.0339(4) Uani 1 1 d . . . . .
C17 C 0.5082(3) 1.0051(2) 0.81203(18) 0.0431(4) Uani 1 1 d . . . . .
H17 H 0.420501 0.966818 0.742610 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2644(3) 0.48756(19) 0.55519(15) 0.0348(4) Uani 1 1 d . . . . .
H6 H 0.204041 0.538092 0.520656 0.042 Uiso 1 1 calc R U . . .
C11 C 0.1248(3) 0.0396(2) 0.37748(17) 0.0430(4) Uani 1 1 d . . . . .
H11 H 0.094597 -0.058595 0.336011 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1060(3) 0.2703(2) 0.38532(16) 0.0410(4) Uani 1 1 d . . . . .
H13 H 0.062340 0.326784 0.350696 0.049 Uiso 1 1 calc R U . . .
C12 C 0.0608(3) 0.1251(2) 0.32670(17) 0.0465(5) Uani 1 1 d . . . . .
H12 H -0.013332 0.083522 0.252264 0.056 Uiso 1 1 calc R U . . .
C10 C 0.2331(2) 0.09848(18) 0.48914(16) 0.0342(4) Uani 1 1 d . . . . .
C18 C 0.5538(3) 1.1496(2) 0.8778(2) 0.0481(5) Uani 1 1 d . . . . .
H18 H 0.494864 1.207470 0.850940 0.058 Uiso 1 1 calc R U . . .
C21 C 0.7282(3) 0.98016(19) 0.95294(17) 0.0404(4) Uani 1 1 d . . . . .
H21 H 0.792016 0.925135 0.980669 0.049 Uiso 1 1 calc R U . . .
C15 C 0.2711(3) -0.12707(19) 0.48077(19) 0.0449(5) Uani 1 1 d . . . . .
H15A H 0.321780 -0.147271 0.410230 0.067 Uiso 1 1 calc R U . . .
H15B H 0.138765 -0.167470 0.461169 0.067 Uiso 1 1 calc R U . . .
H15C H 0.334401 -0.167449 0.527130 0.067 Uiso 1 1 calc R U . . .
C25 C 0.1238(3) 0.4496(3) 0.8291(2) 0.0553(6) Uani 1 1 d . . . . .
H25A H 0.074338 0.416383 0.746311 0.066 Uiso 1 1 calc R U . . .
H25B H 0.048964 0.515405 0.872401 0.066 Uiso 1 1 calc R U . . .
C20 C 0.7646(3) 1.1267(2) 1.01289(19) 0.0477(5) Uani 1 1 d . . . . .
H20 H 0.854585 1.168263 1.081321 0.057 Uiso 1 1 calc R U . . .
C26 C 0.1058(4) 0.3263(3) 0.8612(2) 0.0744(9) Uani 1 1 d . . . . .
H26A H 0.169594 0.256598 0.813131 0.112 Uiso 1 1 calc R U . . .
H26B H -0.025114 0.284975 0.849170 0.112 Uiso 1 1 calc R U . . .
H26C H 0.161379 0.357873 0.942098 0.112 Uiso 1 1 calc R U . . .
H24 H 0.329(4) 0.594(3) 0.906(2) 0.055(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 2.0163(12) . ?
Mo1 O9 1.9317(12) . ?
Mo1 O24 2.3208(14) . ?
Mo1 O22 1.6962(13) . ?
Mo1 O23 1.6989(14) . ?
Mo1 N5 2.2436(14) . ?
O2 C3 1.317(2) . ?
O9 C8 1.344(2) . ?
O14 C10 1.352(2) . ?
O14 C15 1.434(2) . ?
O24 C25 1.425(3) . ?
O24 H24 0.76(3) . ?
N5 N4 1.3998(19) . ?
N5 C6 1.285(2) . ?
N4 C3 1.294(2) . ?
C8 C7 1.402(3) . ?
C8 C10 1.415(2) . ?
N19 C18 1.339(3) . ?
N19 C20 1.326(3) . ?
C3 C16 1.484(2) . ?
C7 C6 1.447(2) . ?
C7 C13 1.413(2) . ?
C16 C17 1.385(3) . ?
C16 C21 1.386(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.376(3) . ?
C6 H6 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.388(3) . ?
C11 C10 1.388(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.372(3) . ?
C12 H12 0.9300 . ?
C18 H18 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.385(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.491(4) . ?
C20 H20 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O24 78.44(5) . . ?
O2 Mo1 N5 71.75(5) . . ?
O9 Mo1 O2 149.00(5) . . ?
O9 Mo1 O24 80.47(5) . . ?
O9 Mo1 N5 81.38(5) . . ?
O22 Mo1 O2 96.64(6) . . ?
O22 Mo1 O9 104.16(6) . . ?
O22 Mo1 O24 85.67(7) . . ?
O22 Mo1 O23 104.91(7) . . ?
O22 Mo1 N5 160.11(6) . . ?
O23 Mo1 O2 97.82(6) . . ?
O23 Mo1 O9 98.70(6) . . ?
O23 Mo1 O24 169.19(6) . . ?
O23 Mo1 N5 92.87(6) . . ?
N5 Mo1 O24 76.33(6) . . ?
C3 O2 Mo1 119.23(11) . . ?
C8 O9 Mo1 132.82(11) . . ?
C10 O14 C15 116.86(15) . . ?
Mo1 O24 H24 117(2) . . ?
C25 O24 Mo1 132.11(12) . . ?
C25 O24 H24 110(2) . . ?
N4 N5 Mo1 115.66(10) . . ?
C6 N5 Mo1 128.19(12) . . ?
C6 N5 N4 116.10(15) . . ?
C3 N4 N5 108.65(14) . . ?
O9 C8 C7 123.14(15) . . ?
O9 C8 C10 117.16(16) . . ?
C7 C8 C10 119.65(16) . . ?
C20 N19 C18 117.06(17) . . ?
O2 C3 C16 116.58(16) . . ?
N4 C3 O2 124.68(15) . . ?
N4 C3 C16 118.71(16) . . ?
C8 C7 C6 122.83(16) . . ?
C8 C7 C13 119.68(16) . . ?
C13 C7 C6 117.49(17) . . ?
C17 C16 C3 121.29(17) . . ?
C17 C16 C21 118.14(17) . . ?
C21 C16 C3 120.52(16) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 C16 119.0(2) . . ?
C18 C17 H17 120.5 . . ?
N5 C6 C7 123.27(16) . . ?
N5 C6 H6 118.4 . . ?
C7 C6 H6 118.4 . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.02(18) . . ?
C7 C13 H13 120.0 . . ?
C12 C13 C7 119.92(19) . . ?
C12 C13 H13 120.0 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.61(18) . . ?
C13 C12 H12 119.7 . . ?
O14 C10 C8 115.81(16) . . ?
O14 C10 C11 125.09(16) . . ?
C11 C10 C8 119.10(18) . . ?
N19 C18 C17 123.4(2) . . ?
N19 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C16 C21 H21 120.8 . . ?
C20 C21 C16 118.48(19) . . ?
C20 C21 H21 120.8 . . ?
O14 C15 H15A 109.5 . . ?
O14 C15 H15B 109.5 . . ?
O14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O24 C25 H25A 109.2 . . ?
O24 C25 H25B 109.2 . . ?
O24 C25 C26 111.9(2) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
N19 C20 C21 123.8(2) . . ?
N19 C20 H20 118.1 . . ?
C21 C20 H20 118.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
Mo1 O2 C3 N4 2.4(2) . . . . ?
Mo1 O2 C3 C16 -179.66(11) . . . . ?
Mo1 O9 C8 C7 -33.2(2) . . . . ?
Mo1 O9 C8 C10 149.30(13) . . . . ?
Mo1 O24 C25 C26 79.6(3) . . . . ?
Mo1 N5 N4 C3 0.22(18) . . . . ?
Mo1 N5 C6 C7 2.8(3) . . . . ?
O2 C3 C16 C17 -177.44(17) . . . . ?
O2 C3 C16 C21 0.0(3) . . . . ?
O9 C8 C7 C6 3.5(3) . . . . ?
O9 C8 C7 C13 -176.14(17) . . . . ?
O9 C8 C10 O14 -2.4(2) . . . . ?
O9 C8 C10 C11 177.40(16) . . . . ?
N5 N4 C3 O2 -1.6(2) . . . . ?
N5 N4 C3 C16 -179.50(15) . . . . ?
N4 N5 C6 C7 179.98(16) . . . . ?
N4 C3 C16 C17 0.6(3) . . . . ?
N4 C3 C16 C21 178.03(17) . . . . ?
C8 C7 C6 N5 9.2(3) . . . . ?
C8 C7 C13 C12 -1.3(3) . . . . ?
C3 C16 C17 C18 175.66(18) . . . . ?
C3 C16 C21 C20 -175.74(18) . . . . ?
C7 C8 C10 O14 179.94(15) . . . . ?
C7 C8 C10 C11 -0.2(3) . . . . ?
C7 C13 C12 C11 0.1(3) . . . . ?
C16 C17 C18 N19 0.0(3) . . . . ?
C16 C21 C20 N19 0.2(3) . . . . ?
C17 C16 C21 C20 1.8(3) . . . . ?
C6 N5 N4 C3 -177.33(16) . . . . ?
C6 C7 C13 C12 179.05(18) . . . . ?
C13 C7 C6 N5 -171.11(18) . . . . ?
C12 C11 C10 O14 178.85(18) . . . . ?
C12 C11 C10 C8 -1.0(3) . . . . ?
C10 C8 C7 C6 -179.02(16) . . . . ?
C10 C8 C7 C13 1.3(3) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C18 N19 C20 C21 -2.0(3) . . . . ?
C21 C16 C17 C18 -1.8(3) . . . . ?
C15 O14 C10 C8 -173.01(15) . . . . ?
C15 O14 C10 C11 7.2(3) . . . . ?
C20 N19 C18 C17 1.9(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
;
####################################################################### 
# 
# 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_4571
_database_code_depnum_ccdc_archive 'CCDC 2367624'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2025-02-13 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_4571            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         29 Note
RESPONSE: Some of the low-angle reflections were obvious outliers and were omitted from refinement.
;
# Added during the CSD deposition process: Thursday 13 February 2025 12:20 AM
# end Validation Reply Form

_audit_creation_date             2025-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C14 H11 N3 O5 V), 2(C14 H12 N3 O5 V), 1[H2O], 1[C2H10O3]'
_chemical_formula_sum            'C29 H29 N6 O12 V2'
_chemical_formula_weight         755.46
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   15.4904(9)
_cell_length_b                   30.9857(12)
_cell_length_c                   14.0729(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.513(7)
_cell_angle_gamma                90
_cell_volume                     6441.6(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3249
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.3580
_cell_measurement_theta_min      4.3870
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.644
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.558
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14553
_diffrn_reflns_point_group_measured_fraction_full 0.819
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         4.188
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 102.00   1.00   10.00    --   28.50 179.00  30.00   68
  2  ω     19.00  90.00   1.00   10.00    --   28.50  57.00  30.00   71
  3  ω    -98.00  30.00   1.00   10.00    --  -31.31  19.00-150.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.602
_reflns_Friedel_fraction_full    0.643
_reflns_Friedel_fraction_max     0.601
_reflns_number_gt                8208
_reflns_number_total             10650
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         10650
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      0.970
_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)+(0.0265P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0911
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.72(2)
 0.28(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 H19-N19
 0.86 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N42(H42), C44(H44), C17(H17), C40(H40), C74(H74), C51(H51), C6(H6), C52(H52),
 C21(H21), C57(H57), C20(H20), C84(H84), C75(H75), C29(H29), C53(H53), C18(H18),
  C83(H83), C78(H78), C41(H41), C76(H76), C43(H43), C62(H62), C10(H10),
 C86(H86), C87(H87), C63(H63), C12(H12), C66(H66), C65(H65), C36(H36), C11(H11),
  C34(H34), C35(H35)
4.b Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C56(H56A,H56B,H56C), C14(H14A,H14B,H14C), C38(H38A,H38B,
 H38C)
;
_atom_sites_solution_hydrogens   mixed
_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
V47 V 0.60359(7) 0.08917(3) 0.88108(8) 0.0374(2) Uani 1 1 d . . . . .
V70 V 0.39307(6) 0.12099(3) 0.28182(8) 0.0378(2) Uani 1 1 d . . . . .
V24 V 0.60694(7) 0.61203(3) 0.88906(10) 0.0482(3) Uani 1 1 d . . . . .
V1 V 0.38932(7) 0.64279(3) 0.21298(9) 0.0498(3) Uani 1 1 d . . . . .
O48 O 0.6548(2) 0.03264(12) 0.9091(3) 0.0443(10) Uani 1 1 d . . . . .
O55 O 0.6593(3) -0.05187(12) 0.9036(3) 0.0477(11) Uani 1 1 d . . . . .
O2 O 0.3837(3) 0.58084(12) 0.1817(3) 0.0524(12) Uani 1 1 d . . . . .
O68 O 0.5245(2) 0.08084(13) 0.9309(3) 0.0449(10) Uani 1 1 d . . . . .
N58 N 0.7422(3) 0.10817(14) 0.9227(3) 0.0355(11) Uani 1 1 d . . . . .
O15 O 0.3412(3) 0.69897(12) 0.1786(3) 0.0476(11) Uani 1 1 d . . . . .
O25 O 0.6125(3) 0.54911(12) 0.8980(4) 0.0510(11) Uani 1 1 d . . . . .
O71 O 0.3418(2) 0.06371(12) 0.2654(3) 0.0450(11) Uani 1 1 d . . . . .
O67 O 0.6057(3) 0.15186(12) 0.9027(4) 0.0493(12) Uani 1 1 d . . . . .
N59 N 0.7593(3) 0.15272(14) 0.9339(4) 0.0396(12) Uani 1 1 d . . . . .
O88 O 0.3891(3) 0.18466(13) 0.2831(4) 0.0554(11) Uani 1 1 d . . . . .
O69 O 0.5605(3) 0.08749(13) 0.7593(3) 0.0531(11) Uani 1 1 d . . . . .
O89 O 0.3377(3) -0.02159(13) 0.2619(3) 0.0498(11) Uani 1 1 d . . . . .
N4 N 0.2297(3) 0.58126(15) 0.1546(4) 0.0430(12) Uani 1 1 d . . . . .
N28 N 0.7465(3) 0.59572(15) 0.9597(4) 0.0413(12) Uani 1 1 d . . . . .
N27 N 0.7653(3) 0.55145(15) 0.9681(4) 0.0439(13) Uani 1 1 d . . . . .
O92 O 0.4626(3) 0.11683(13) 0.2180(3) 0.0569(12) Uani 1 1 d . . . . .
O91 O 0.4478(3) 0.11583(13) 0.3989(3) 0.0588(12) Uani 1 1 d . . . . .
N79 N 0.2551(3) 0.13839(15) 0.2127(4) 0.0396(12) Uani 1 1 d . . . . .
O32 O 0.6470(3) 0.66615(13) 0.9518(4) 0.0588(13) Uani 1 1 d . . . . .
O37 O 0.6325(4) 0.74943(15) 0.9411(4) 0.0680(14) Uani 1 1 d . . . . .
N19 N 0.3097(4) 0.42518(15) 0.1818(4) 0.0483(13) Uani 1 1 d D . . . .
C50 C 0.8123(3) 0.03906(16) 0.9264(4) 0.0332(13) Uani 1 1 d . . . . .
O13 O 0.3500(3) 0.78223(14) 0.2118(4) 0.0697(15) Uani 1 1 d . . . . .
O23 O 0.4787(3) 0.64934(14) 0.1775(5) 0.0816(18) Uani 1 1 d . . . . .
N5 N 0.2491(3) 0.62586(15) 0.1670(4) 0.0403(12) Uani 1 1 d . . . . .
O45 O 0.5089(3) 0.61471(14) 0.9075(4) 0.0727(16) Uani 1 1 d . . . . .
N64 N 0.6807(4) 0.30902(17) 0.9219(4) 0.0522(14) Uani 1 1 d . . . . .
N42 N 0.6907(4) 0.39465(15) 0.9249(4) 0.0490(13) Uani 1 1 d . . . . .
H42 H 0.690120 0.366896 0.923945 0.059 Uiso 1 1 calc R U . . .
C49 C 0.7342(3) 0.01475(17) 0.9148(4) 0.0306(12) Uani 1 1 d . . . . .
N80 N 0.2372(3) 0.18285(15) 0.2013(4) 0.0410(12) Uani 1 1 d . . . . .
N85 N 0.3125(4) 0.33943(16) 0.2116(4) 0.0503(14) Uani 1 1 d . . . . .
C16 C 0.3056(4) 0.51371(17) 0.1688(4) 0.0334(13) Uani 1 1 d . . . . .
C54 C 0.7398(4) -0.03022(18) 0.9126(4) 0.0357(13) Uani 1 1 d . . . . .
C44 C 0.6145(4) 0.46101(17) 0.8827(5) 0.0405(14) Uani 1 1 d . . . . .
H44 H 0.561287 0.475853 0.851850 0.049 Uiso 1 1 calc R U . . .
C72 C 0.2636(3) 0.04512(17) 0.2216(4) 0.0327(13) Uani 1 1 d . . . . .
C39 C 0.6924(4) 0.48340(17) 0.9298(5) 0.0377(14) Uani 1 1 d . . . . .
C3 C 0.3069(4) 0.56106(18) 0.1675(5) 0.0420(15) Uani 1 1 d . . . . .
C26 C 0.6916(4) 0.53146(17) 0.9326(5) 0.0373(14) Uani 1 1 d . . . . .
O22 O 0.4189(4) 0.64238(16) 0.3311(4) 0.0768(16) Uani 1 1 d . . . . .
C73 C 0.2591(4) -0.00056(18) 0.2194(4) 0.0375(14) Uani 1 1 d . . . . .
C17 C 0.3867(4) 0.49092(18) 0.1860(5) 0.0459(16) Uani 1 1 d . . . . .
H17 H 0.440432 0.505720 0.192907 0.055 Uiso 1 1 calc R U . . .
C40 C 0.7704(4) 0.46004(19) 0.9744(5) 0.0452(15) Uani 1 1 d . . . . .
H40 H 0.824295 0.474127 1.006727 0.054 Uiso 1 1 calc R U . . .
C74 C 0.1774(4) -0.02117(19) 0.1775(5) 0.0444(15) Uani 1 1 d . . . . .
H74 H 0.174629 -0.051146 0.178395 0.053 Uiso 1 1 calc R U . . .
O46 O 0.5952(4) 0.62133(15) 0.7724(4) 0.0822(16) Uani 1 1 d . . . . .
C51 C 0.8947(4) 0.01785(19) 0.9329(5) 0.0448(15) Uani 1 1 d . . . . .
H51 H 0.946839 0.033871 0.938841 0.054 Uiso 1 1 calc R U . . .
C6 C 0.1787(4) 0.6498(2) 0.1591(4) 0.0435(16) Uani 1 1 d . . . . .
H6 H 0.122087 0.636822 0.144416 0.052 Uiso 1 1 calc R U . . .
C52 C 0.8978(4) -0.0266(2) 0.9306(5) 0.0508(17) Uani 1 1 d . . . . .
H52 H 0.952080 -0.040748 0.936281 0.061 Uiso 1 1 calc R U . . .
C21 C 0.2285(4) 0.49020(19) 0.1572(5) 0.0458(16) Uani 1 1 d . . . . .
H21 H 0.173196 0.504316 0.144071 0.055 Uiso 1 1 calc R U . . .
C57 C 0.8121(4) 0.08470(17) 0.9316(4) 0.0392(14) Uani 1 1 d . . . . .
H57 H 0.867272 0.098739 0.942428 0.047 Uiso 1 1 calc R U . . .
C20 C 0.2316(4) 0.4463(2) 0.1645(5) 0.0478(16) Uani 1 1 d . . . . .
H20 H 0.178500 0.430886 0.157362 0.057 Uiso 1 1 calc R U . . .
C84 C 0.2345(4) 0.3178(2) 0.1911(5) 0.0502(17) Uani 1 1 d . . . . .
H84 H 0.180494 0.333190 0.170568 0.060 Uiso 1 1 calc R U . . .
C75 C 0.0987(4) 0.0028(2) 0.1335(5) 0.0504(16) Uani 1 1 d . . . . .
H75 H 0.044386 -0.011190 0.102525 0.061 Uiso 1 1 calc R U . . .
C77 C 0.1843(3) 0.06838(17) 0.1802(4) 0.0351(13) Uani 1 1 d . . . . .
C82 C 0.3114(4) 0.25103(18) 0.2323(5) 0.0397(14) Uani 1 1 d . . . . .
C60 C 0.6818(4) 0.17176(18) 0.9199(4) 0.0370(13) Uani 1 1 d . . . . .
C29 C 0.8142(4) 0.62091(19) 0.9839(5) 0.0458(16) Uani 1 1 d . . . . .
H29 H 0.871879 0.608948 1.006035 0.055 Uiso 1 1 calc R U . . .
C53 C 0.8182(4) -0.05030(18) 0.9195(4) 0.0429(15) Uani 1 1 d . . . . .
H53 H 0.819806 -0.080269 0.916851 0.051 Uiso 1 1 calc R U . . .
C30 C 0.8056(4) 0.66756(19) 0.9787(5) 0.0481(17) Uani 1 1 d . . . . .
C18 C 0.3871(4) 0.4472(2) 0.1927(5) 0.0524(17) Uani 1 1 d . . . . .
H18 H 0.441461 0.432331 0.205058 0.063 Uiso 1 1 calc R U . . .
C61 C 0.6807(4) 0.21983(18) 0.9222(4) 0.0369(14) Uani 1 1 d . . . . .
C81 C 0.3121(4) 0.20346(19) 0.2405(5) 0.0396(14) Uani 1 1 d . . . . .
C83 C 0.2311(4) 0.27389(19) 0.1992(5) 0.0443(16) Uani 1 1 d . . . . .
H83 H 0.175735 0.259618 0.182731 0.053 Uiso 1 1 calc R U . . .
C78 C 0.1835(4) 0.11394(19) 0.1786(5) 0.0421(15) Uani 1 1 d . . . . .
H78 H 0.128057 0.127577 0.151432 0.051 Uiso 1 1 calc R U . . .
C41 C 0.7669(4) 0.41561(19) 0.9700(5) 0.0479(16) Uani 1 1 d . . . . .
H41 H 0.819303 0.399870 0.999296 0.057 Uiso 1 1 calc R U . . .
C76 C 0.1023(4) 0.0467(2) 0.1365(5) 0.0476(17) Uani 1 1 d . . . . .
H76 H 0.049649 0.062584 0.109281 0.057 Uiso 1 1 calc R U . . .
C8 C 0.2661(5) 0.71746(19) 0.1848(5) 0.0454(16) Uani 1 1 d . . . . .
C90 C 0.3357(4) -0.06785(18) 0.2549(5) 0.0535(18) Uani 1 1 d . . . . .
H90A H 0.313789 -0.076264 0.186199 0.080 Uiso 1 1 calc R U . . .
H90B H 0.296298 -0.079146 0.290095 0.080 Uiso 1 1 calc R U . . .
H90C H 0.395670 -0.079044 0.283919 0.080 Uiso 1 1 calc R U . . .
C43 C 0.6157(5) 0.41653(19) 0.8815(6) 0.0526(17) Uani 1 1 d . . . . .
H43 H 0.562788 0.401600 0.849591 0.063 Uiso 1 1 calc R U . . .
C62 C 0.7604(4) 0.2429(2) 0.9537(5) 0.0505(17) Uani 1 1 d . . . . .
H62 H 0.815650 0.228609 0.975491 0.061 Uiso 1 1 calc R U . . .
C10 C 0.1888(5) 0.7850(2) 0.1978(5) 0.065(2) Uani 1 1 d . . . . .
H10 H 0.189162 0.814814 0.204810 0.079 Uiso 1 1 calc R U . . .
C86 C 0.3891(5) 0.3180(2) 0.2433(5) 0.057(2) Uani 1 1 d . . . . .
H86 H 0.443312 0.333208 0.258584 0.069 Uiso 1 1 calc R U . . .
C87 C 0.3919(4) 0.27284(19) 0.2547(5) 0.0510(18) Uani 1 1 d . . . . .
H87 H 0.446819 0.258251 0.276899 0.061 Uiso 1 1 calc R U . . .
C63 C 0.7573(5) 0.28746(19) 0.9526(5) 0.0507(17) Uani 1 1 d . . . . .
H63 H 0.811265 0.302783 0.974378 0.061 Uiso 1 1 calc R U . . .
C12 C 0.1053(5) 0.7189(2) 0.1708(5) 0.0580(19) Uani 1 1 d . . . . .
H12 H 0.050386 0.704623 0.159719 0.070 Uiso 1 1 calc R U . . .
C7 C 0.1852(4) 0.6959(2) 0.1723(5) 0.0449(16) Uani 1 1 d . . . . .
C33 C 0.7178(5) 0.7334(2) 0.9570(5) 0.0547(18) Uani 1 1 d . . . . .
C66 C 0.6025(5) 0.2432(2) 0.8904(6) 0.0592(18) Uani 1 1 d . . . . .
H66 H 0.547142 0.229036 0.868757 0.071 Uiso 1 1 calc R U . . .
C56 C 0.6617(5) -0.09758(19) 0.8984(7) 0.067(2) Uani 1 1 d . . . . .
H56A H 0.680865 -0.105995 0.842272 0.101 Uiso 1 1 calc R U . . .
H56B H 0.602340 -0.108971 0.890906 0.101 Uiso 1 1 calc R U . . .
H56C H 0.703380 -0.108695 0.958428 0.101 Uiso 1 1 calc R U . . .
C31 C 0.7228(4) 0.6879(2) 0.9627(5) 0.0488(16) Uani 1 1 d . . . . .
C14 C 0.3566(6) 0.8282(2) 0.2301(6) 0.080(2) Uani 1 1 d . . . . .
H14A H 0.314437 0.842991 0.175760 0.121 Uiso 1 1 calc R U . . .
H14B H 0.416967 0.837729 0.236017 0.121 Uiso 1 1 calc R U . . .
H14C H 0.342827 0.834414 0.290826 0.121 Uiso 1 1 calc R U . . .
C9 C 0.2673(5) 0.7631(2) 0.1994(5) 0.0516(17) Uani 1 1 d . . . . .
C65 C 0.6050(6) 0.2866(2) 0.8903(7) 0.067(2) Uani 1 1 d . . . . .
H65 H 0.550613 0.301555 0.866709 0.081 Uiso 1 1 calc R U . . .
C36 C 0.8841(5) 0.6931(2) 0.9883(6) 0.064(2) Uani 1 1 d . . . . .
H36 H 0.939907 0.679862 0.997866 0.077 Uiso 1 1 calc R U . . .
C11 C 0.1109(5) 0.7620(2) 0.1857(6) 0.070(2) Uani 1 1 d . . . . .
H11 H 0.059235 0.776729 0.187964 0.084 Uiso 1 1 calc R U . . .
C34 C 0.7953(6) 0.7563(2) 0.9666(6) 0.071(2) Uani 1 1 d . . . . .
H34 H 0.792302 0.786230 0.961358 0.085 Uiso 1 1 calc R U . . .
C38 C 0.6198(6) 0.7954(2) 0.9257(6) 0.077(2) Uani 1 1 d . . . . .
H38A H 0.640037 0.804022 0.870482 0.116 Uiso 1 1 calc R U . . .
H38B H 0.654093 0.810394 0.984658 0.116 Uiso 1 1 calc R U . . .
H38C H 0.556756 0.802245 0.911828 0.116 Uiso 1 1 calc R U . . .
C35 C 0.8780(5) 0.7359(2) 0.9838(7) 0.074(2) Uani 1 1 d . . . . .
H35 H 0.930000 0.752359 0.992241 0.089 Uiso 1 1 calc R U . . .
H19 H 0.314(5) 0.3967(9) 0.191(5) 0.089 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V47 O48 1.914(4) . ?
V47 O68 1.605(4) . ?
V47 N58 2.131(4) . ?
V47 O67 1.965(4) . ?
V47 O69 1.642(4) . ?
V70 O71 1.930(4) . ?
V70 O88 1.974(4) . ?
V70 O92 1.601(4) . ?
V70 O91 1.618(4) . ?
V70 N79 2.134(5) . ?
V24 O25 1.954(4) . ?
V24 N28 2.151(5) . ?
V24 O32 1.910(4) . ?
V24 O45 1.617(4) . ?
V24 O46 1.622(5) . ?
V1 O2 1.965(4) . ?
V1 O15 1.898(4) . ?
V1 O23 1.620(4) . ?
V1 N5 2.137(5) . ?
V1 O22 1.585(5) . ?
O48 C49 1.329(6) . ?
O55 C54 1.389(6) . ?
O55 C56 1.419(7) . ?
O2 C3 1.299(7) . ?
N58 N59 1.406(6) . ?
N58 C57 1.279(7) . ?
O15 C8 1.324(7) . ?
O25 C26 1.297(7) . ?
O71 C72 1.315(6) . ?
O67 C60 1.287(7) . ?
N59 C60 1.298(7) . ?
O88 C81 1.299(7) . ?
O89 C73 1.352(6) . ?
O89 C90 1.436(6) . ?
N4 N5 1.414(6) . ?
N4 C3 1.314(7) . ?
N28 N27 1.400(6) . ?
N28 C29 1.269(7) . ?
N27 C26 1.262(7) . ?
N79 N80 1.405(6) . ?
N79 C78 1.309(7) . ?
O32 C31 1.322(7) . ?
O37 C33 1.366(8) . ?
O37 C38 1.445(7) . ?
N19 C20 1.332(7) . ?
N19 C18 1.348(8) . ?
N19 H19 0.89(3) . ?
C50 C49 1.392(7) . ?
C50 C51 1.415(7) . ?
C50 C57 1.416(7) . ?
O13 C14 1.446(7) . ?
O13 C9 1.374(8) . ?
N5 C6 1.297(7) . ?
N64 C63 1.316(7) . ?
N64 C65 1.320(9) . ?
N42 H42 0.8600 . ?
N42 C41 1.329(7) . ?
N42 C43 1.326(8) . ?
C49 C54 1.397(7) . ?
N80 C81 1.294(7) . ?
N85 C84 1.335(7) . ?
N85 C86 1.315(8) . ?
C16 C3 1.467(7) . ?
C16 C17 1.396(8) . ?
C16 C21 1.366(7) . ?
C54 C53 1.342(7) . ?
C44 H44 0.9300 . ?
C44 C39 1.376(8) . ?
C44 C43 1.379(7) . ?
C72 C73 1.417(7) . ?
C72 C77 1.391(7) . ?
C39 C26 1.490(7) . ?
C39 C40 1.387(8) . ?
C73 C74 1.381(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.357(8) . ?
C40 H40 0.9300 . ?
C40 C41 1.379(8) . ?
C74 H74 0.9300 . ?
C74 C75 1.403(8) . ?
C51 H51 0.9300 . ?
C51 C52 1.379(8) . ?
C6 H6 0.9300 . ?
C6 C7 1.440(8) . ?
C52 H52 0.9300 . ?
C52 C53 1.402(8) . ?
C21 H21 0.9300 . ?
C21 C20 1.365(8) . ?
C57 H57 0.9300 . ?
C20 H20 0.9300 . ?
C84 H84 0.9300 . ?
C84 C83 1.368(8) . ?
C75 H75 0.9300 . ?
C75 C76 1.362(8) . ?
C77 C78 1.412(7) . ?
C77 C76 1.405(7) . ?
C82 C81 1.478(8) . ?
C82 C83 1.384(8) . ?
C82 C87 1.370(8) . ?
C60 C61 1.490(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.451(8) . ?
C53 H53 0.9300 . ?
C30 C31 1.386(8) . ?
C30 C36 1.423(8) . ?
C18 H18 0.9300 . ?
C61 C62 1.379(8) . ?
C61 C66 1.366(8) . ?
C83 H83 0.9300 . ?
C78 H78 0.9300 . ?
C41 H41 0.9300 . ?
C76 H76 0.9300 . ?
C8 C7 1.384(8) . ?
C8 C9 1.428(8) . ?
C90 H90A 0.9600 . ?
C90 H90B 0.9600 . ?
C90 H90C 0.9600 . ?
C43 H43 0.9300 . ?
C62 H62 0.9300 . ?
C62 C63 1.381(8) . ?
C10 H10 0.9300 . ?
C10 C9 1.387(9) . ?
C10 C11 1.368(10) . ?
C86 H86 0.9300 . ?
C86 C87 1.408(8) . ?
C87 H87 0.9300 . ?
C63 H63 0.9300 . ?
C12 H12 0.9300 . ?
C12 C7 1.423(8) . ?
C12 C11 1.348(9) . ?
C33 C31 1.411(8) . ?
C33 C34 1.366(10) . ?
C66 H66 0.9300 . ?
C66 C65 1.345(8) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C65 H65 0.9300 . ?
C36 H36 0.9300 . ?
C36 C35 1.329(9) . ?
C11 H11 0.9300 . ?
C34 H34 0.9300 . ?
C34 C35 1.383(10) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C35 H35 0.9300 . ?

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
O48 V47 N58 82.83(17) . . ?
O48 V47 O67 152.38(19) . . ?
O68 V47 O48 94.96(19) . . ?
O68 V47 N58 139.7(2) . . ?
O68 V47 O67 94.1(2) . . ?
O68 V47 O69 109.1(2) . . ?
O67 V47 N58 73.49(18) . . ?
O69 V47 O48 101.5(2) . . ?
O69 V47 N58 110.8(2) . . ?
O69 V47 O67 100.1(2) . . ?
O71 V70 O88 155.13(17) . . ?
O71 V70 N79 81.84(17) . . ?
O88 V70 N79 73.84(18) . . ?
O92 V70 O71 100.40(19) . . ?
O92 V70 O88 96.5(2) . . ?
O92 V70 O91 109.2(2) . . ?
O92 V70 N79 121.0(2) . . ?
O91 V70 O71 95.84(19) . . ?
O91 V70 O88 95.6(2) . . ?
O91 V70 N79 129.4(2) . . ?
O25 V24 N28 73.58(18) . . ?
O32 V24 O25 147.6(2) . . ?
O32 V24 N28 81.42(19) . . ?
O45 V24 O25 93.8(2) . . ?
O45 V24 N28 143.1(2) . . ?
O45 V24 O32 94.1(2) . . ?
O45 V24 O46 109.2(3) . . ?
O46 V24 O25 103.4(2) . . ?
O46 V24 N28 107.5(2) . . ?
O46 V24 O32 103.5(2) . . ?
O2 V1 N5 73.76(17) . . ?
O15 V1 O2 148.34(19) . . ?
O15 V1 N5 82.12(17) . . ?
O23 V1 O2 92.1(2) . . ?
O23 V1 O15 96.5(2) . . ?
O23 V1 N5 145.4(3) . . ?
O22 V1 O2 101.9(2) . . ?
O22 V1 O15 104.0(2) . . ?
O22 V1 O23 108.6(3) . . ?
O22 V1 N5 105.2(3) . . ?
C49 O48 V47 135.5(3) . . ?
C54 O55 C56 116.7(5) . . ?
C3 O2 V1 118.1(3) . . ?
N59 N58 V47 116.3(3) . . ?
C57 N58 V47 128.5(4) . . ?
C57 N58 N59 114.9(4) . . ?
C8 O15 V1 131.7(4) . . ?
C26 O25 V24 117.6(3) . . ?
C72 O71 V70 138.3(3) . . ?
C60 O67 V47 118.3(4) . . ?
C60 N59 N58 107.1(4) . . ?
C81 O88 V70 118.1(4) . . ?
C73 O89 C90 116.9(4) . . ?
C3 N4 N5 107.3(4) . . ?
N27 N28 V24 115.1(3) . . ?
C29 N28 V24 127.9(4) . . ?
C29 N28 N27 116.5(5) . . ?
C26 N27 N28 107.9(5) . . ?
N80 N79 V70 115.8(3) . . ?
C78 N79 V70 130.0(4) . . ?
C78 N79 N80 114.2(4) . . ?
C31 O32 V24 130.9(4) . . ?
C33 O37 C38 117.7(6) . . ?
C20 N19 C18 120.0(5) . . ?
C20 N19 H19 122(5) . . ?
C18 N19 H19 117(5) . . ?
C49 C50 C51 119.4(5) . . ?
C49 C50 C57 122.1(5) . . ?
C51 C50 C57 118.5(5) . . ?
C9 O13 C14 117.5(5) . . ?
N4 N5 V1 115.9(3) . . ?
C6 N5 V1 129.6(4) . . ?
C6 N5 N4 114.0(5) . . ?
C63 N64 C65 117.7(6) . . ?
C41 N42 H42 120.0 . . ?
C43 N42 H42 120.0 . . ?
C43 N42 C41 120.0(5) . . ?
O48 C49 C50 122.4(5) . . ?
O48 C49 C54 118.5(5) . . ?
C50 C49 C54 119.0(5) . . ?
C81 N80 N79 108.3(4) . . ?
C86 N85 C84 119.0(6) . . ?
C17 C16 C3 119.5(5) . . ?
C21 C16 C3 123.1(5) . . ?
C21 C16 C17 117.3(5) . . ?
O55 C54 C49 115.1(5) . . ?
C53 C54 O55 123.5(5) . . ?
C53 C54 C49 121.5(5) . . ?
C39 C44 H44 120.1 . . ?
C39 C44 C43 119.8(6) . . ?
C43 C44 H44 120.1 . . ?
O71 C72 C73 118.7(5) . . ?
O71 C72 C77 122.8(5) . . ?
C77 C72 C73 118.5(5) . . ?
C44 C39 C26 120.3(5) . . ?
C44 C39 C40 118.3(5) . . ?
C40 C39 C26 121.5(5) . . ?
O2 C3 N4 123.4(5) . . ?
O2 C3 C16 119.0(5) . . ?
N4 C3 C16 117.5(5) . . ?
O25 C26 C39 115.2(5) . . ?
N27 C26 O25 125.6(5) . . ?
N27 C26 C39 119.2(5) . . ?
O89 C73 C72 116.1(5) . . ?
O89 C73 C74 123.6(5) . . ?
C74 C73 C72 120.3(5) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.1(6) . . ?
C18 C17 H17 119.9 . . ?
C39 C40 H40 120.5 . . ?
C41 C40 C39 118.9(6) . . ?
C41 C40 H40 120.5 . . ?
C73 C74 H74 119.8 . . ?
C73 C74 C75 120.4(6) . . ?
C75 C74 H74 119.8 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 C50 120.0(5) . . ?
C52 C51 H51 120.0 . . ?
N5 C6 H6 118.9 . . ?
N5 C6 C7 122.2(5) . . ?
C7 C6 H6 118.9 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.3(5) . . ?
C53 C52 H52 120.3 . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.9(6) . . ?
C20 C21 H21 119.6 . . ?
N58 C57 C50 125.3(5) . . ?
N58 C57 H57 117.4 . . ?
C50 C57 H57 117.4 . . ?
N19 C20 C21 120.8(5) . . ?
N19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
N85 C84 H84 118.8 . . ?
N85 C84 C83 122.4(6) . . ?
C83 C84 H84 118.8 . . ?
C74 C75 H75 120.2 . . ?
C76 C75 C74 119.6(6) . . ?
C76 C75 H75 120.2 . . ?
C72 C77 C78 121.8(5) . . ?
C72 C77 C76 120.3(5) . . ?
C76 C77 C78 117.9(5) . . ?
C83 C82 C81 121.5(5) . . ?
C87 C82 C81 119.2(5) . . ?
C87 C82 C83 119.3(6) . . ?
O67 C60 N59 124.3(5) . . ?
O67 C60 C61 117.8(5) . . ?
N59 C60 C61 117.8(5) . . ?
N28 C29 H29 118.5 . . ?
N28 C29 C30 122.9(6) . . ?
C30 C29 H29 118.5 . . ?
C54 C53 C52 120.8(5) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C31 C30 C29 121.8(6) . . ?
C31 C30 C36 119.0(6) . . ?
C36 C30 C29 119.2(6) . . ?
N19 C18 C17 120.8(6) . . ?
N19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C62 C61 C60 120.7(5) . . ?
C66 C61 C60 122.6(5) . . ?
C66 C61 C62 116.7(6) . . ?
O88 C81 C82 117.9(5) . . ?
N80 C81 O88 123.8(5) . . ?
N80 C81 C82 118.3(5) . . ?
C84 C83 C82 118.9(6) . . ?
C84 C83 H83 120.5 . . ?
C82 C83 H83 120.5 . . ?
N79 C78 C77 124.8(5) . . ?
N79 C78 H78 117.6 . . ?
C77 C78 H78 117.6 . . ?
N42 C41 C40 121.8(6) . . ?
N42 C41 H41 119.1 . . ?
C40 C41 H41 119.1 . . ?
C75 C76 C77 120.9(5) . . ?
C75 C76 H76 119.5 . . ?
C77 C76 H76 119.5 . . ?
O15 C8 C7 124.3(5) . . ?
O15 C8 C9 117.7(6) . . ?
C7 C8 C9 117.9(6) . . ?
O89 C90 H90A 109.5 . . ?
O89 C90 H90B 109.5 . . ?
O89 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
N42 C43 C44 121.2(6) . . ?
N42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C61 C62 H62 120.4 . . ?
C61 C62 C63 119.3(6) . . ?
C63 C62 H62 120.4 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C11 C10 C9 119.0(7) . . ?
N85 C86 H86 118.8 . . ?
N85 C86 C87 122.3(6) . . ?
C87 C86 H86 118.8 . . ?
C82 C87 C86 118.0(6) . . ?
C82 C87 H87 121.0 . . ?
C86 C87 H87 121.0 . . ?
N64 C63 C62 122.4(6) . . ?
N64 C63 H63 118.8 . . ?
C62 C63 H63 118.8 . . ?
C7 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C7 118.6(7) . . ?
C8 C7 C6 121.3(5) . . ?
C8 C7 C12 120.7(6) . . ?
C12 C7 C6 118.0(6) . . ?
O37 C33 C31 114.0(6) . . ?
O37 C33 C34 127.2(6) . . ?
C34 C33 C31 118.8(7) . . ?
C61 C66 H66 119.7 . . ?
C65 C66 C61 120.6(7) . . ?
C65 C66 H66 119.7 . . ?
O55 C56 H56A 109.5 . . ?
O55 C56 H56B 109.5 . . ?
O55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O32 C31 C30 122.2(6) . . ?
O32 C31 C33 118.0(6) . . ?
C30 C31 C33 119.7(6) . . ?
O13 C14 H14A 109.5 . . ?
O13 C14 H14B 109.5 . . ?
O13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O13 C9 C8 114.7(6) . . ?
O13 C9 C10 124.8(6) . . ?
C10 C9 C8 120.5(7) . . ?
N64 C65 C66 123.2(7) . . ?
N64 C65 H65 118.4 . . ?
C66 C65 H65 118.4 . . ?
C30 C36 H36 119.8 . . ?
C35 C36 C30 120.3(7) . . ?
C35 C36 H36 119.8 . . ?
C10 C11 H11 118.4 . . ?
C12 C11 C10 123.2(7) . . ?
C12 C11 H11 118.4 . . ?
C33 C34 H34 119.4 . . ?
C33 C34 C35 121.3(6) . . ?
C35 C34 H34 119.4 . . ?
O37 C38 H38A 109.5 . . ?
O37 C38 H38B 109.5 . . ?
O37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C35 C34 120.8(7) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?

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
V47 O48 C49 C50 18.3(8) . . . . ?
V47 O48 C49 C54 -164.0(4) . . . . ?
V47 N58 N59 C60 3.3(6) . . . . ?
V47 N58 C57 C50 -7.9(9) . . . . ?
V47 O67 C60 N59 -7.3(8) . . . . ?
V47 O67 C60 C61 171.7(4) . . . . ?
V70 O71 C72 C73 172.6(4) . . . . ?
V70 O71 C72 C77 -9.5(9) . . . . ?
V70 O88 C81 N80 3.3(9) . . . . ?
V70 O88 C81 C82 -173.7(4) . . . . ?
V70 N79 N80 C81 -2.2(6) . . . . ?
V70 N79 C78 C77 -0.9(10) . . . . ?
V24 O25 C26 N27 5.5(8) . . . . ?
V24 O25 C26 C39 -175.1(4) . . . . ?
V24 N28 N27 C26 -1.8(6) . . . . ?
V24 N28 C29 C30 8.5(9) . . . . ?
V24 O32 C31 C30 -35.9(10) . . . . ?
V24 O32 C31 C33 143.7(5) . . . . ?
V1 O2 C3 N4 13.1(8) . . . . ?
V1 O2 C3 C16 -165.0(4) . . . . ?
V1 O15 C8 C7 -33.5(9) . . . . ?
V1 O15 C8 C9 150.5(5) . . . . ?
V1 N5 C6 C7 6.6(9) . . . . ?
O48 C49 C54 O55 0.6(8) . . . . ?
O48 C49 C54 C53 -179.1(5) . . . . ?
O55 C54 C53 C52 -178.6(6) . . . . ?
O2 V1 O15 C8 73.9(7) . . . . ?
N58 N59 C60 O67 2.2(8) . . . . ?
N58 N59 C60 C61 -176.7(5) . . . . ?
O15 C8 C7 C6 5.2(10) . . . . ?
O15 C8 C7 C12 -174.0(6) . . . . ?
O15 C8 C9 O13 -4.1(9) . . . . ?
O15 C8 C9 C10 174.3(6) . . . . ?
O71 C72 C73 O89 -1.2(8) . . . . ?
O71 C72 C73 C74 177.5(5) . . . . ?
O71 C72 C77 C78 2.8(9) . . . . ?
O71 C72 C77 C76 -178.4(5) . . . . ?
O67 C60 C61 C62 170.9(6) . . . . ?
O67 C60 C61 C66 -11.5(9) . . . . ?
N59 N58 C57 C50 178.0(5) . . . . ?
N59 C60 C61 C62 -10.1(9) . . . . ?
N59 C60 C61 C66 167.5(6) . . . . ?
O89 C73 C74 C75 -179.2(6) . . . . ?
N4 N5 C6 C7 178.1(5) . . . . ?
N28 N27 C26 O25 -2.2(8) . . . . ?
N28 N27 C26 C39 178.5(5) . . . . ?
N28 C29 C30 C31 10.9(10) . . . . ?
N28 C29 C30 C36 -167.9(6) . . . . ?
N27 N28 C29 C30 179.6(6) . . . . ?
N79 N80 C81 O88 -0.5(8) . . . . ?
N79 N80 C81 C82 176.5(5) . . . . ?
O37 C33 C31 O32 0.4(9) . . . . ?
O37 C33 C31 C30 -180.0(6) . . . . ?
O37 C33 C34 C35 179.3(7) . . . . ?
C50 C49 C54 O55 178.3(5) . . . . ?
C50 C49 C54 C53 -1.3(9) . . . . ?
C50 C51 C52 C53 1.4(10) . . . . ?
O23 V1 O15 C8 178.7(6) . . . . ?
N5 V1 O15 C8 33.5(6) . . . . ?
N5 N4 C3 O2 -4.4(8) . . . . ?
N5 N4 C3 C16 173.7(5) . . . . ?
N5 C6 C7 C8 6.2(10) . . . . ?
N5 C6 C7 C12 -174.6(6) . . . . ?
C49 C50 C51 C52 -1.8(9) . . . . ?
C49 C50 C57 N58 -2.8(10) . . . . ?
C49 C54 C53 C52 1.0(9) . . . . ?
N80 N79 C78 C77 179.0(5) . . . . ?
N85 C84 C83 C82 1.7(10) . . . . ?
N85 C86 C87 C82 -0.3(10) . . . . ?
C16 C17 C18 N19 0.8(10) . . . . ?
C16 C21 C20 N19 -1.0(11) . . . . ?
C44 C39 C26 O25 7.1(9) . . . . ?
C44 C39 C26 N27 -173.6(6) . . . . ?
C44 C39 C40 C41 -0.1(9) . . . . ?
C72 C73 C74 C75 2.3(9) . . . . ?
C72 C77 C78 N79 1.7(10) . . . . ?
C72 C77 C76 C75 -0.3(10) . . . . ?
C39 C44 C43 N42 -0.1(11) . . . . ?
C39 C40 C41 N42 -0.5(10) . . . . ?
C3 N4 N5 V1 -5.3(6) . . . . ?
C3 N4 N5 C6 -178.1(5) . . . . ?
C3 C16 C17 C18 176.4(6) . . . . ?
C3 C16 C21 C20 -176.2(6) . . . . ?
C26 C39 C40 C41 179.6(6) . . . . ?
O22 V1 O15 C8 -70.3(6) . . . . ?
C73 C72 C77 C78 -179.4(5) . . . . ?
C73 C72 C77 C76 -0.6(9) . . . . ?
C73 C74 C75 C76 -3.1(10) . . . . ?
C17 C16 C3 O2 0.6(9) . . . . ?
C17 C16 C3 N4 -177.6(5) . . . . ?
C17 C16 C21 C20 1.4(10) . . . . ?
C40 C39 C26 O25 -172.7(5) . . . . ?
C40 C39 C26 N27 6.7(9) . . . . ?
C74 C75 C76 C77 2.1(11) . . . . ?
C51 C50 C49 O48 179.4(5) . . . . ?
C51 C50 C49 C54 1.7(8) . . . . ?
C51 C50 C57 N58 177.0(6) . . . . ?
C51 C52 C53 C54 -1.0(10) . . . . ?
C21 C16 C3 O2 178.3(6) . . . . ?
C21 C16 C3 N4 0.0(9) . . . . ?
C21 C16 C17 C18 -1.4(9) . . . . ?
C57 N58 N59 C60 178.1(5) . . . . ?
C57 C50 C49 O48 -0.8(9) . . . . ?
C57 C50 C49 C54 -178.4(5) . . . . ?
C57 C50 C51 C52 178.4(6) . . . . ?
C20 N19 C18 C17 -0.3(10) . . . . ?
C84 N85 C86 C87 1.1(10) . . . . ?
C77 C72 C73 O89 -179.1(5) . . . . ?
C77 C72 C73 C74 -0.4(9) . . . . ?
C60 C61 C62 C63 178.4(6) . . . . ?
C60 C61 C66 C65 -177.4(7) . . . . ?
C29 N28 N27 C26 -174.0(6) . . . . ?
C29 C30 C31 O32 0.3(10) . . . . ?
C29 C30 C31 C33 -179.3(6) . . . . ?
C29 C30 C36 C35 180.0(7) . . . . ?
C30 C36 C35 C34 -2.0(13) . . . . ?
C18 N19 C20 C21 0.3(10) . . . . ?
C61 C62 C63 N64 -0.4(10) . . . . ?
C61 C66 C65 N64 -1.5(14) . . . . ?
C81 C82 C83 C84 -178.7(6) . . . . ?
C81 C82 C87 C86 178.1(6) . . . . ?
C83 C82 C81 O88 -172.0(6) . . . . ?
C83 C82 C81 N80 10.9(9) . . . . ?
C83 C82 C87 C86 0.2(10) . . . . ?
C78 N79 N80 C81 177.9(5) . . . . ?
C78 C77 C76 C75 178.6(6) . . . . ?
C41 N42 C43 C44 -0.6(10) . . . . ?
C76 C77 C78 N79 -177.1(6) . . . . ?
C90 O89 C73 C72 -176.3(5) . . . . ?
C90 O89 C73 C74 5.1(9) . . . . ?
C43 N42 C41 C40 0.9(10) . . . . ?
C43 C44 C39 C26 -179.3(6) . . . . ?
C43 C44 C39 C40 0.4(9) . . . . ?
C62 C61 C66 C65 0.2(11) . . . . ?
C86 N85 C84 C83 -1.8(10) . . . . ?
C87 C82 C81 O88 10.2(9) . . . . ?
C87 C82 C81 N80 -166.9(6) . . . . ?
C87 C82 C83 C84 -0.8(9) . . . . ?
C63 N64 C65 C66 1.7(12) . . . . ?
C7 C8 C9 O13 179.7(6) . . . . ?
C7 C8 C9 C10 -1.9(10) . . . . ?
C7 C12 C11 C10 3.1(12) . . . . ?
C33 C34 C35 C36 2.2(13) . . . . ?
C66 C61 C62 C63 0.6(10) . . . . ?
C56 O55 C54 C49 178.3(6) . . . . ?
C56 O55 C54 C53 -2.1(9) . . . . ?
C31 C30 C36 C35 1.2(11) . . . . ?
C31 C33 C34 C35 -1.5(11) . . . . ?
C14 O13 C9 C8 -178.0(6) . . . . ?
C14 O13 C9 C10 3.6(10) . . . . ?
C9 C8 C7 C6 -178.8(6) . . . . ?
C9 C8 C7 C12 2.0(9) . . . . ?
C9 C10 C11 C12 -3.0(12) . . . . ?
C65 N64 C63 C62 -0.7(11) . . . . ?
C36 C30 C31 O32 179.1(6) . . . . ?
C36 C30 C31 C33 -0.5(10) . . . . ?
C11 C10 C9 O13 -179.4(7) . . . . ?
C11 C10 C9 C8 2.4(11) . . . . ?
C11 C12 C7 C6 178.2(6) . . . . ?
C11 C12 C7 C8 -2.6(10) . . . . ?
C34 C33 C31 O32 -178.9(6) . . . . ?
C34 C33 C31 C30 0.7(10) . . . . ?
C38 O37 C33 C31 -174.8(6) . . . . ?
C38 O37 C33 C34 4.5(11) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 218 electrons were 
found in a volume of 928Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
2[H2O], 2[CH4O] per Asymmetric Unit 
which account for 224 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 -0.001 0.135 0.555 63.8 10.1 '1 H2O'
2 -0.006 0.500 -0.983 336.0 89.2 '2 C2H10O3'
3 -0.001 0.865 0.055 63.8 10.2 '1 H2O'
4 0.499 0.365 0.055 63.8 10.2 '1 H2O'
5 0.499 0.635 0.555 63.8 10.1 '1 H2O'
6 0.494 0.000 -0.340 336.0 89.2 '2 C2H10O3'

_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.72(2)
2 0.28(2)

