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_7720200
_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 beta'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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            8
_cell_length_a                   16.1589(5)
_cell_length_b                   7.4570(2)
_cell_length_c                   30.2326(7)
_cell_measurement_reflns_used    4533
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      75.5430
_cell_measurement_theta_min      2.9250
_cell_volume                     3642.94(17)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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   -106.00 -79.00   0.50    8.00    --  -46.93-156.00  -2.00   54
  2  \w    -71.00 -12.00   0.50    8.00    --  -46.93 121.00-122.00  118
  3  \w     57.00  82.00   0.50    8.00    --   46.93-156.00  -2.00   50
  4  \w   -123.00 -98.00   0.50   32.00    --  -86.25-156.00  -2.00   50
  5  \w    -73.00 -48.00   0.50   32.00    --  -86.25 121.00-122.00   50
  6  \w     51.00 125.00   0.50   32.00    --  106.38-156.00  -2.00  148
  7  \w    103.00 128.00   0.50   32.00    --  106.38 121.00-122.00   50
  8  \w   -119.00 -94.00   0.50    8.00    --  -46.93 -77.00 -90.00   50
  9  \w   -115.00 -89.00   0.50    8.00    --  -46.93 -77.00 -30.00   52
 10  \w   -119.00 -92.00   0.50    8.00    --  -46.93 -77.00 -60.00   54
 11  \w   -119.00 -90.00   0.50    8.00    --  -46.93 -77.00   0.00   58
 12  \w   -117.00 -92.00   0.50    8.00    --  -46.93 -77.00-120.00   50
 13  \w   -126.00 -90.00   0.50   32.00    --  -86.25 -99.00-120.00   72
 14  \w    -43.00 -18.00   0.50   32.00    --  -86.25  38.00  60.00   50
 15  \w    -43.00 -13.00   0.50   32.00    --  -86.25  38.00 -90.00   60
 16  \w    104.00 141.00   0.50   32.00    --  106.38 125.00 -60.00   74
 17  \w     34.00  59.00   0.50   32.00    --  106.38 -57.00  30.00   50
 18  \w     35.00  66.00   0.50   32.00    --  106.38 -57.00-150.00   62
 19  \w     34.00  59.00   0.50   32.00    --  106.38 -57.00 120.00   50
 20  \w     41.00  85.00   0.50   32.00    --  106.38 -77.00-150.00   88
 21  \w    100.00 178.00   0.50   32.00    --  106.38  19.00  60.00  156
 22  \w    146.00 177.00   0.50   32.00    --  106.38 125.00 -60.00   62
 23  \w     34.00  59.00   0.50   32.00    --  106.38 -57.00-180.00   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      0.0284198000
_diffrn_orient_matrix_UB_12      -0.0146134000
_diffrn_orient_matrix_UB_13      -0.0485182000
_diffrn_orient_matrix_UB_21      -0.0900189000
_diffrn_orient_matrix_UB_22      -0.0346008000
_diffrn_orient_matrix_UB_23      -0.0144351000
_diffrn_orient_matrix_UB_31      -0.0132496000
_diffrn_orient_matrix_UB_32      0.2031257000
_diffrn_orient_matrix_UB_33      -0.0059672000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            17864
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.291
_diffrn_reflns_theta_min         5.475
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.849
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.384(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6342
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1182P)^2^+1.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.766
_reflns_Friedel_fraction_max     0.675
_reflns_number_gt                4636
_reflns_number_total             6342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           3beta
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720200
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V2 C32 N6 O12'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.615(15)
 0.385(15)
2. 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
3. Restrained distances
 O4A-C15A
 1.5 with sigma of 0.02
 C15A-O4A
 1.5 with sigma of 0.02
 C15-O4
 1.5 with sigma of 0.02
 H17A-O4A
 2.97 with sigma of 0.02
 C17A-C15A
 2.54 with sigma of 0.04
 C17A-C16A \\sim C16A-C15A
 with sigma of 0.02
4. Rigid bond restraints
 O4, C15, C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C17A \\sim C16A \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O4 \\sim C15 \\sim C16 \\sim C17: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
6. Rigid body (RIGU) restrains
 C17A, C16A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Free rotating group:
 C17A(C16A,C15A), C17(C16,C15)
7.b Secondary CH2 refined with riding coordinates:
 C16A(H16A,H16B), C15A(H15A,H15B), C16(H16C,H16D), C15(H15C,H15D)
7.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C10A(H10A), C2(H2), C11(H11), C12A(H12A), C10(H10), C11A(H11A),
 C8A(H8A), C6(H6), C13(H13), C12(H12), C7(H7), C2A(H2A), C7A(H7A), C8(H8),
 C6A(H6A)
7.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C17A(H17A,H17B,H17C), C17(H17D,
 H17E,H17F)
;
_shelx_res_checksum              64820
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.773