Syntheses, Structures, and Electrochemical Properties of Metallacyclic Oxidovanadium(V) Complexes with Asymmetric Multidentate Linking Ligands.
Hasegawa, Kyoko; Muto, Masahiro; Hamada, Masanobu; Yamada, Yasunori; Tokii, Tadashi; Koikawa, Masayuki; Molecules (Basel, Switzerland) 29 (2024) 1700–; doi:10.3390/molecules29081700

data_1571560
_publ_section_title
;
 Syntheses, Structures, and Electrochemical Properties of Metallacyclic
 Oxidovanadium(V) Complexes with Asymmetric Multidentate Linking Ligands.
;
_journal_issue                   8
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              1700
_journal_paper_doi               10.3390/molecules29081700
_journal_volume                  29
_journal_year                    2024
_chemical_formula_moiety         'C26 H28 N3 O6 V'
_chemical_formula_sum            'C26 H28 N3 O6 V'
_chemical_formula_weight         529.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.705(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.978(3)
_cell_length_b                   7.5880(14)
_cell_length_c                   28.042(5)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    301
_cell_measurement_theta_max      12.22
_cell_measurement_theta_min      10.19
_cell_volume                     2495.7(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control (Rigaku, 1998)'
_computing_data_reduction        'MSC/AFC Diffractometer Control'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      301
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.2359
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            5577
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.530
_diffrn_standards_decay_%        -0.977
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1104.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.2748
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.3181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1828
_reflns_number_total             5478
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            Complex4.cif
_cod_data_source_block           (HNEt3)[VO2(L5-H)]
_cod_original_cell_volume        2495.7(8)
_cod_database_code               1571560
_shelx_res_checksum              76607
_shelx_hkl_checksum              47099