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_1571562
_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         'C70 H48 N8 O19 V3'
_chemical_formula_sum            'C70 H48 N8 O19 V3'
_chemical_formula_weight         1458.02
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                87.11(2)
_cell_angle_beta                 69.06(2)
_cell_angle_gamma                79.74(3)
_cell_formula_units_Z            2
_cell_length_a                   15.307(5)
_cell_length_b                   15.582(5)
_cell_length_c                   18.458(5)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    292
_cell_measurement_theta_max      11.85
_cell_measurement_theta_min      10.19
_cell_volume                     4046(2)
_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      292
_diffrn_measured_fraction_theta_full 0.766
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.2692
_diffrn_reflns_Laue_measured_fraction_full 0.766
_diffrn_reflns_Laue_measured_fraction_max 0.766
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11453
_diffrn_reflns_point_group_measured_fraction_full 0.766
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         2.657
_diffrn_standards_decay_%        0.362
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1490.00
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     863
_refine_ls_number_reflns         10895
_refine_ls_number_restraints     942
_refine_ls_R_factor_all          0.2692
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1722P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2336
_refine_ls_wR_factor_ref         0.3156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3661
_reflns_number_total             10895
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            Complex2.cif
_cod_data_source_block           VO_L5-Me_
_cod_original_cell_volume        4045(2)
_cod_database_code               1571562
_shelx_res_checksum              70897
_shelx_hkl_checksum              95885
_shelx_fab_checksum              81234