Influence of ancillary ligands on the formation and functionality of oxovanadium(V) metallosupramolecular assemblies: advanced computational and catalytic analyses.
Topić, Edi; Sarjanović, Josipa; Musija, Danijela; Mandarić, Mirna; Cocut, Andrea; Hrenar, Tomica; Agustin, Dominique; Pisk, Jana; Vrdoljak, Višnja; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5532–5545; doi:10.1039/d5dt00105f

data_7718146
_publ_section_title
;
 Influence of ancillary ligands on the formation and functionality of
 oxovanadium(V) metallosupramolecular assemblies: advanced computational
 and catalytic analyses.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5532
_journal_page_last               5545
_journal_paper_doi               10.1039/d5dt00105f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H20 N3 O5 V'
_chemical_formula_sum            'C18 H20 N3 O5 V'
_chemical_formula_weight         409.31
_chemical_name_systematic
butoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-19 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7033(9)
_cell_length_b                   15.0094(10)
_cell_length_c                   10.7908(8)
_cell_measurement_reflns_used    3542
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.7710
_cell_measurement_theta_min      2.9270
_cell_volume                     1895.5(2)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -32.00  21.00   0.50    1.50    --  -47.03  78.00 105.00  106
  2  \w     -7.00  35.00   0.50    1.50    --   47.03 -78.00 -19.00   84
  3  \w    -71.00 -45.00   0.50    4.00    --  -86.25  78.00 105.00   52
  4  \w     39.00  79.00   0.50    4.00    --  106.40 -78.00 -19.00   80
  5  \w    115.00 141.00   0.50    4.00    --  106.40  78.00 105.00   52
  6  \w   -102.00 -77.00   0.50    1.50    --  -47.03-125.00-120.00   50
  7  \w   -116.00 -74.00   0.50    1.50    --  -47.03-125.00 120.00   84
  8  \w    -43.00 -13.00   0.50    4.00    --  -86.25  38.00 120.00   60
  9  \w    -42.00 -15.00   0.50    4.00    --  -86.25  38.00  60.00   54
 10  \w     38.00 103.00   0.50    4.00    --  106.40 -77.00  90.00  130
 11  \w     34.00  66.00   0.50    4.00    --  106.40 -57.00   0.00   64
 12  \w     43.00 101.00   0.50    4.00    --  106.40 -99.00 -90.00  116
 13  \w     45.00  72.00   0.50    4.00    --  106.40 -77.00 150.00   54
 14  \w     36.00  66.00   0.50    4.00    --  106.40 -57.00 150.00   60
 15  \w     38.00  64.00   0.50    4.00    --  106.40 -57.00 -90.00   52
 16  \w     35.00  60.00   0.50    4.00    --  106.40 -57.00 120.00   50
 17  \w     52.00 104.00   0.50    4.00    --  106.40 -77.00-180.00  104
 18  \w     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       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_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
_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_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.434
_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
_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_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_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0499
_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/[\s^2^(Fo^2^)+(0.0756P)^2^+1.5163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1424
_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_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_2271
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_database_code               7718146
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.627
_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)
;
_shelx_res_checksum              35678
_shelx_hkl_checksum              26078
_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
;