Dinuclear oxidovanadium complexes with dihydrazone ligands derived from diethyl 2,6-dimethylpyridine-3,5-dicarboxylate obtained from Hantzsch reaction; crystal structure and catalytic activity
Soltani, Fatemeh; Bikas, Rahman; Heydari, Neda; Kozakiewicz-Piekarz, Anna; New Journal of Chemistry 47 (2023) 6102–6113; doi:10.1039/D2NJ06279H

data_7062297
_publ_section_title
;
 Dinuclear oxidovanadium complexes with dihydrazone ligands derived from
 diethyl 2,6-dimethylpyridine-3,5-dicarboxylate obtained from Hantzsch
 reaction; crystal structure and catalytic activity
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6102
_journal_page_last               6113
_journal_paper_doi               10.1039/D2NJ06279H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C29 H25 N5 O8 V2, 2(C H4O), H0.64 O0.32, 2(H4 N)'
_chemical_formula_sum            'C31 H41.64 N7 O10.32 V2'
_chemical_formula_weight         779.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-02-13 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_c                   7.4106(2)
_cell_measurement_reflns_used    6595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5350
_cell_measurement_theta_min      4.4680
_cell_volume                     3710.13(14)
_computing_cell_refinement       'Oxford Diffraction CrysAlis'
_computing_data_collection       'Oxford Diffraction CrysAlis'
_computing_data_reduction        'Oxford Diffraction CrysAlis'
_computing_molecular_graphics    'Diamond software'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13121
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.915
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1621
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+14.6306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3330
_reflns_number_total             3635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06279h2.cif
_cod_data_source_block           fs31_3_a
_cod_depositor_comments
'Adding full bibliography for 7062297--7062298.cif.'
_cod_database_code               7062297
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.620
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              18427