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_7720202
_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         'C16 H16 N3 O5 V'
_chemical_formula_sum            'C16 H16 N3 O5 V'
_chemical_formula_weight         381.26
_chemical_name_systematic
'oxo-ethoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 93.011(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8838(3)
_cell_length_b                   10.7455(3)
_cell_length_c                   26.4644(7)
_cell_measurement_reflns_used    17778
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      77.4980
_cell_measurement_theta_min      3.3460
_cell_volume                     3374.77(16)
_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 1.000
_diffrn_measured_fraction_theta_max 0.963
_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     94.00 120.00   0.50    1.43    --  107.75  61.00  90.00   52
  2  \w    134.00 160.00   0.50    1.43    --  107.75  61.00  90.00   52
  3  \w    145.00 172.00   0.50    1.43    --  107.75  45.00  60.00   54
  4  \w    113.00 138.00   0.50    1.43    --  107.75  45.00  60.00   50
  5  \w    147.00 173.00   0.50    1.43    --  107.75  61.00-150.00   52
  6  \w    103.00 162.00   0.50    1.43    --  107.75  45.00-180.00  118
  7  \w     92.00 123.00   0.50    1.43    --  107.75  61.00-150.00   62
  8  \w    133.00 175.00   0.50    1.43    --  107.75  44.00-166.00   84
  9  \w     42.00 119.00   0.50    0.36    --   47.03  44.00-166.00  154
 10  \w     95.00 131.00   0.50    1.43    --  107.75  30.00 -30.00   72
 11  \w    135.00 161.00   0.50    1.43    --  107.75  30.00 -30.00   52
 12  \w     99.00 170.00   0.50    1.43    --  107.75  15.00 120.00  142
 13  \w    -22.00  28.00   0.50    0.36    --  -47.03  19.00   0.00  100
 14  \w    -49.00 -17.00   0.50    1.43    --  -86.25  45.00   0.00   64
 15  \w    -85.00 -60.00   0.50    0.36    --  -47.03 125.00  30.00   50
 16  \w    -49.00 -24.00   0.50    1.43    --  -86.25  44.00-166.00   50
 17  \w    -36.00  20.00   0.50    0.36    --  -47.03  44.00-166.00  112
 18  \w      5.00  31.00   0.50    0.36    --   47.03 -44.00  42.00   52
 19  \w    144.00 170.00   0.50    1.43    --  107.75 125.00  60.00   52
 20  \w    100.00 126.00   0.50    1.43    --  107.75 125.00  60.00   52
 21  \w     40.00  66.00   0.50    1.43    --  107.75 -77.00  30.00   52
 22  \w     36.00  71.00   0.50    1.43    --  107.75 -77.00 120.00   70
 23  \w     76.00 104.00   0.50    1.43    --  107.75 -77.00 120.00   56
 24  \w     39.00 101.00   0.50    1.43    --  107.75 -77.00 150.00  124
 25  \w     80.00 105.00   0.50    1.43    --  107.75 -77.00  30.00   50
 26  \w     36.00  67.00   0.50    1.43    --  107.75 -61.00 120.00   62
 27  \w     36.00  67.00   0.50    1.43    --  107.75 -61.00 -90.00   62
 28  \w     79.00 105.00   0.50    1.43    --  107.75 -77.00-180.00   52
 29  \w     44.00  70.00   0.50    1.43    --  107.75 -77.00-180.00   52
 30  \w     36.00  66.00   0.50    1.43    --  107.75 -61.00-180.00   60
 31  \w     36.00  67.00   0.50    1.43    --  107.75 -61.00-150.00   62
 32  \w     41.00  66.00   0.50    1.43    --  107.75 -61.00-120.00   50
 33  \w     39.00  67.00   0.50    1.43    --  107.75 -61.00  90.00   56
 34  \w     56.00 103.00   0.50    1.43    --  107.75-125.00   0.00   94
 35  \w     35.00  94.00   0.50    1.43    --  107.75 -95.00  30.00  118
 36  \w     37.00  63.00   0.50    1.43    --  107.75 -95.00   0.00   52
 37  \w     64.00 105.00   0.50    1.43    --  107.75 -95.00   0.00   82
 38  \w   -100.00 -34.00   0.50    0.36    --  -47.03 -44.00  42.00  132
 39  \w   -140.00-115.00   0.50    1.43    --  -86.25 -44.00  42.00   50
 40  \w   -119.00 -73.00   0.50    0.36    --  -47.03-125.00   0.00   92
;
_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      -0.0175672000
_diffrn_orient_matrix_UB_12      0.0358364000
_diffrn_orient_matrix_UB_13      0.0554347000
_diffrn_orient_matrix_UB_21      0.1086500000
_diffrn_orient_matrix_UB_22      -0.0698552000
_diffrn_orient_matrix_UB_23      0.0167801000
_diffrn_orient_matrix_UB_31      0.0687243000
_diffrn_orient_matrix_UB_32      0.1199646000
_diffrn_orient_matrix_UB_33      -0.0067770000
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31106
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.528
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.212
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_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_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0716P)^2^+3.4969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6333
_reflns_number_total             7066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720202
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V2 O10 N6 C32'
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.368
_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:
 C15(H15A,H15B), C15A(H15C,H15D)
2.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C10(H10), C12A(H12A), C2(H2), C13(H13), C11(H11), C12(H12),
 C2A(H2A), C13A(H13A), C7(H7), C11A(H11A), C8(H8), C7A(H7A), C8A(H8A), C6(H6),
 C6A(H6A)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C16A(H16D,H16E,H16F), C14A(H14D,
 H14E,H14F)
;
_shelx_res_checksum              26943
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.627