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_7062298
_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         'C25 H21 N5 O10 V2, H2 O, 2(H4 N)'
_chemical_formula_sum            'C25 H31 N7 O11 V2'
_chemical_formula_weight         707.45
_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   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
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_cell_angle_gamma                90
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_cell_length_c                   25.8864(12)
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_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.6790
_cell_volume                     2824.8(2)
_computing_cell_refinement       'Oxford Diffraction CrysAlis'
_computing_data_collection       'Oxford Diffraction CrysAlis'
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_computing_molecular_graphics    'Diamond software'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2017 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       7
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12900
_diffrn_reflns_point_group_measured_fraction_full 0.947
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_diffrn_reflns_theta_full        67.684
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_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44996
_exptl_absorpt_correction_type   multi-scan
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'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            orange
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_exptl_crystal_description       block
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_refine_diff_density_max         0.632
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5348
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0641
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+16.6690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5138
_reflns_number_total             5348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06279h2.cif
_cod_data_source_block           ft161-1a_a
_cod_depositor_comments
'Adding full bibliography for 7062297--7062298.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7062298
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.304
_shelx_estimated_absorpt_t_max   0.486
_shelx_res_checksum              34952