Nicotinoyl hydrazone-directed vanadium assemblies: metallosupramolecular isomerism, polymorphism, and catalytic oxidation performance.
Topić, Edi; Sarjanović, Josipa; Kuzman, Dino; Cocut, Andrea; Hrenar, Tomica; Pisk, Jana; Vrdoljak, Višnja; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4237–4249; doi:10.1039/d5dt03088a

data_7720198
_publ_section_title
;
 Nicotinoyl hydrazone-directed vanadium assemblies: metallosupramolecular
 isomerism, polymorphism, and catalytic oxidation performance.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4237
_journal_page_last               4249
_journal_paper_doi               10.1039/d5dt03088a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C18 H19 N3 O5 V'
_chemical_formula_sum            'C18 H19 N3 O5 V'
_chemical_formula_weight         408.30
_chemical_name_systematic
'oxo-n-butoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer form beta'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-22 deposited with the CCDC.	2026-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   25.3304(8)
_cell_length_b                   25.3304(8)
_cell_length_c                   15.9617(6)
_cell_measurement_reflns_used    6783
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.6810
_cell_measurement_theta_min      3.4010
_cell_volume                     8869.4(5)
_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_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_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    -25.00  24.00   0.50    1.00    --  -47.03  15.00 145.00   98
  2  \w    -50.00 -25.00   0.50    5.00    --  -86.25 126.00  45.00   50
  3  \w    -42.00 -15.00   0.50    5.00    --  -86.25  47.00-113.00   54
  4  \w    103.00 172.00   0.50    5.00    --  107.75 115.00 -39.00  138
  5  \w     79.00 110.00   0.50    5.00    --  107.75-126.00 -31.00   62
  6  \w     47.00  72.00   0.50    5.00    --  107.75-126.00 -31.00   50
  7  \w    -24.00  23.00   0.50    1.00    --   47.03 -19.00 120.00   94
  8  \w     68.00 120.00   0.50    1.00    --   47.03 172.00 102.00  104
  9  \w     35.00  62.00   0.50    5.00    --  107.75 -61.00 120.00   54
 10  \w     76.00 102.00   0.50    5.00    --  107.75 -95.00-120.00   52
 11  \w     88.00 114.00   0.50    5.00    --  107.75  77.00-150.00   52
 12  \w    144.00 170.00   0.50    5.00    --  107.75  77.00-150.00   52
 13  \w     38.00 103.00   0.50    5.00    --  107.75 -95.00 120.00  130
 14  \w    122.00 156.00   0.50    5.00    --  107.75 125.00 150.00   68
 15  \w     45.00  70.00   0.50    5.00    --  107.75 -61.00-180.00   50
 16  \w     37.00  89.00   0.50    5.00    --  107.75 -77.00  60.00  104
 17  \w    101.00 135.00   0.50    5.00    --  107.75  45.00 -30.00   68
 18  \w    140.00 165.00   0.50    5.00    --  107.75  45.00 -30.00   50
 19  \w     36.00  61.00   0.50    5.00    --  107.75 -77.00  90.00   50
 20  \w     38.00  64.00   0.50    5.00    --  107.75 -95.00 -90.00   52
 21  \w    143.00 178.00   0.50    5.00    --  107.75 125.00  60.00   70
 22  \w    103.00 129.00   0.50    5.00    --  107.75  30.00-120.00   52
 23  \w    152.00 177.00   0.50    5.00    --  107.75  15.00 145.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0696874000
_diffrn_orient_matrix_UB_12      0.0292060000
_diffrn_orient_matrix_UB_13      -0.0085606000
_diffrn_orient_matrix_UB_21      0.0070594000
_diffrn_orient_matrix_UB_22      0.0128107000
_diffrn_orient_matrix_UB_23      0.0949456000
_diffrn_orient_matrix_UB_31      -0.0054163000
_diffrn_orient_matrix_UB_32      -0.0624907000
_diffrn_orient_matrix_UB_33      0.0154330000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16040
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.742
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44242
_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_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             3798
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4107
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0712
_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/[\s^2^(Fo^2^)+(0.1224P)^2^+21.1636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3410
_reflns_number_total             4107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           4beta
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_original_cell_volume        8869.4(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7720198
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V C20 N3 O6'
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.744
_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. Restrained distances
 C17-C18
 1.5 with sigma of 0.02
 H18C-O4
 4.12 with sigma of 0.02
3. Rigid bond restraints
 O4, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C15, C16, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: H16A(0.5) H16(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C17(0.5) H17A(0.5)
 H17B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C19(H19A,H19B), C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C2(H2), C6(H6), C8(H8), C7(H7),
 C16(H16A), C16(H16)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              26392
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.076
_oxdiff_exptl_absorpt_empirical_full_min 0.636