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_7717827
_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         'C38 H44 N4 O7 V2, [+ solvents]'
_chemical_formula_sum            'C38 H44 N4 O7 V2'
_chemical_formula_weight         770.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc252plk
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.983(5)
_cell_angle_beta                 89.588(5)
_cell_angle_gamma                75.312(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6752(14)
_cell_length_b                   13.712(2)
_cell_length_c                   17.313(3)
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      17.57
_cell_measurement_theta_min      2.22
_cell_volume                     1929.6(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1812
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20644
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        17.642
_diffrn_reflns_theta_max         17.642
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.948
_exptl_transmission_factor_min   0.880
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0056(17)
_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   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         2499
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1203P)^2^+7.0856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1673
_reflns_number_total             2499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02030h2.cif
_cod_data_source_block           complex6
_cod_depositor_comments
'Adding full bibliography for 7717823--7717828.cif.'
_cod_database_code               7717827
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.856
_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
 C13-C14 \\sim C14-C15
 with sigma of 0.02
 C37-C38 \\sim C38-C36
 with sigma of 0.02
3. Restrained planarity
 C5, C23, C22, C21, C20, C19, C18, C17, C16, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C23 \\sim C22 \\sim C21 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim C16 \\sim
C6 \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C38 \\sim C37: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C5) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C23) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C19) = Uanis(C18) =
Uanis(C17) = Uanis(C16) = Uanis(C6) = Uanis(C5)
Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) =
Uanis(C23) = Uanis(C5) = Uanis(C6) = Uanis(C16)
Uanis(C13) = Uanis(C14) = Uanis(C15)
Uanis(C25) = Uanis(C24) = Uanis(C29) = Uanis(C28) = Uanis(C27) = Uanis(C26)
Uanis(C10) = Uanis(C9) = Uanis(C13)
Uanis(C36) = Uanis(C32) = Uanis(C38) = Uanis(C37)
Uanis(C9) = Uanis(C8) = Uanis(C13)
Uanis(N2) = Uanis(C4)
Uanis(C30) = Uanis(C1) = Uanis(C31) = Uanis(C2) = Uanis(C24) = Uanis(C29) =
Uanis(C3) = Uanis(N2) = Uanis(N1)
5. Rigid body (RIGU) restrains
 C23, C22, C21, C20, C19, C18, C17, C16, C6, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C32(H32), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C33(H33A,H33B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,
 H14B), C13(H13A,H13B), C34(H34A,H34B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C31(H31), C23(H23), C7(H7), C17(H17), C27(H27), C28(H28), C18(H18),
 C3(H3), C20(H20), C25(H25), C30(H30), C26(H26), C19(H19)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'