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_7720203
_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         '0.5(C34 H36 N6 O10 V2)'
_chemical_formula_sum            'C17 H18 N3 O5 V'
_chemical_formula_weight         395.28
_chemical_name_systematic
'oxo-n-propoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer form alpha'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_formula_units_Z            16
_cell_length_a                   15.7460(2)
_cell_length_b                   13.50300(10)
_cell_length_c                   34.1126(4)
_cell_measurement_reflns_used    12497
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.8820
_cell_measurement_theta_min      3.8190
_cell_volume                     7252.96(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_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   -117.00 -45.00   0.50    2.50    --  -46.93 -51.00   4.00  144
  2  \w    -58.00 -33.00   0.50    9.00    --  -86.25  51.00 150.00   50
  3  \w   -145.00-120.00   0.50    9.00    --  -86.25-101.00 138.00   50
  4  \w     89.00 174.00   0.50    9.00    --  106.38  77.00  -4.00  170
  5  \w   -118.00 -92.00   0.50    2.50    --  -46.93-125.00-180.00   52
  6  \w     -4.00  26.00   0.50    2.50    --  -46.93  19.00 150.00   60
  7  \w    -22.00  21.00   0.50    2.50    --   46.93 -19.00-150.00   86
  8  \w    -40.00 -14.00   0.50    9.00    --  -86.25  38.00  90.00   52
  9  \w     89.00 162.00   0.50    9.00    --  106.38  77.00-120.00  146
 10  \w     34.00  68.00   0.50    9.00    --  106.38 -77.00-180.00   68
 11  \w     34.00  59.00   0.50    9.00    --  106.38 -57.00  30.00   50
 12  \w     34.00  72.00   0.50    9.00    --  106.38 -77.00 150.00   76
 13  \w     79.00 104.00   0.50    9.00    --  106.38 -77.00-180.00   50
 14  \w     34.00 105.00   0.50    9.00    --  106.38 -77.00  30.00  142
 15  \w     39.00  64.00   0.50    9.00    --  106.38 -57.00 -90.00   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      0.0118563000
_diffrn_orient_matrix_UB_12      0.0388396000
_diffrn_orient_matrix_UB_13      -0.0421107000
_diffrn_orient_matrix_UB_21      0.0619050000
_diffrn_orient_matrix_UB_22      -0.0856104000
_diffrn_orient_matrix_UB_23      -0.0086523000
_diffrn_orient_matrix_UB_31      -0.0748225000
_diffrn_orient_matrix_UB_32      -0.0646416000
_diffrn_orient_matrix_UB_33      -0.0138447000
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            29109
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.337
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7363
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0452
_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/[\s^2^(Fo^2^)+(0.0819P)^2^+2.4504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6071
_reflns_number_total             7363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           3alpha
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720203
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V C N O'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.793
_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
 O4-C15
 1.5 with sigma of 0.02
 O4-C18
 1.5 with sigma of 0.02
 C19-O4
 2.3 with sigma of 0.02
 H17A-O4
 2.85 with sigma of 0.02
 C15-C17
 2.54 with sigma of 0.04
 C17A-C15A
 2.54 with sigma of 0.04
 C18-C20
 2.54 with sigma of 0.04
 C15-C16 \\sim C16-C17
 with sigma of 0.02
 C17A-C16A \\sim C16A-C15A
 with sigma of 0.02
 C18-C19 \\sim C19-C20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C17A \\sim C16A \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C18 \\sim C19 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17A, C16A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
6.a Free rotating group:
 C15(C16,C17), C17A(C16A,C15A), C18(C19,C20)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C16A(H16C,H16D), C15A(H15C,H15D), C18(H18A,
 H18B), C19(H19A,H19B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C10A(H10A), C10(H10), C11(H11), C8(H8), C12(H12),
 C13A(H13A), C11A(H11A), C6(H6), C7(H7), C2A(H2A), C12A(H12A), C8A(H8A),
 C7A(H7A), C6A(H6A)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C17(H17A,H17B,H17C), C17A(H17D,
 H17E,H17F), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              52117
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.772