New V<sup>V</sup>O<sub>2</sub>, V<sup>V</sup>O, V<sup>V</sup>OV<sup>V</sup>O and electrogenerated V<sup>IV</sup>OV<sup>V</sup>O systems of valproic acid hydrazones: a study of catalytic activity.
Patra, Roumi; Sinha, Debopam; Mondal, Sandip; Rajak, Kajal Krishna; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5471–5485; doi:10.1039/d4dt02030h

data_7717824
_publ_section_title
;
 New V<sup>V</sup>O<sub>2</sub>, V<sup>V</sup>O,
 V<sup>V</sup>OV<sup>V</sup>O and electrogenerated
 V<sup>IV</sup>OV<sup>V</sup>O systems of valproic acid hydrazones: a
 study of catalytic activity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5471
_journal_page_last               5485
_journal_paper_doi               10.1039/d4dt02030h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H22 N2 O2'
_chemical_formula_sum            'C15 H22 N2 O2'
_chemical_formula_weight         262.34
_chemical_name_common            'hydrazone ligand'
_chemical_name_systematic        'hydrazone ligand'
_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_block_doi                 10.5517/ccdc.csd.cc2cjzqm
_audit_creation_date             2025-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-08 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.716(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0199(16)
_cell_length_b                   19.834(3)
_cell_length_c                   9.7259(15)
_cell_measurement_reflns_used    3564
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      17.5
_cell_volume                     1567.6(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23217
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.258
_diffrn_reflns_theta_min         3.102
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.2969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.116
_refine_diff_density_min         -0.119
_refine_diff_density_rms         0.023
_refine_ls_extinction_coef       0.029(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0546P)^2^+0.2663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2321
_reflns_number_total             3490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02030h2.cif
_cod_data_source_block           L1
_cod_depositor_comments
'Adding full bibliography for 7717823--7717828.cif.'
_cod_original_cell_volume        1567.7(4)
_cod_database_code               7717824
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.985
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C6-C5 = C6A-C5 = C7-C6 = C7A-C6A = C8A-C7A = C8-C7
 1.51 with sigma of 0.01
 C9-C10A = C9-C10 = C11A-C10A = C11-C10
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8 \\sim C7A \\sim C8A \\sim C6A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C9 \\sim C10 \\sim C11 \\sim C10A \\sim C11A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C11A) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H5B)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(H5A)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(H9BC)=Sof(H9BD)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(H9AA)=Sof(H9AB)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C5(H5A), C5(H5B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C9(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B),
 C7A(H7AA,H7AB), C6A(H6AA,H6AB), C10A(H10C,H10D)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C14(H14), C15(H15), C13(H13), C12(H12)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C8A(H8AA,H8AB,H8AC), C11A(H11D,H11E,H11F)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              7886
_olex2_submission_special_instructions 'No special instructions were received'