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_1571561
_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         'C60 H33 N6 O15 V3, [+ solvents]'
_chemical_formula_sum            'C60 H33 N6 O15 V3'
_chemical_formula_weight         1230.74
_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     dual
_audit_creation_date             2023-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                102.99(3)
_cell_angle_beta                 98.16(3)
_cell_angle_gamma                108.59(3)
_cell_formula_units_Z            2
_cell_length_a                   12.465(5)
_cell_length_b                   16.244(6)
_cell_length_c                   18.285(8)
_cell_measurement_reflns_used    8270
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3327(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26785
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.419
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   REQAB
_exptl_crystal_colour            'dull greenish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0074(10)
_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   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         14423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0919P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8693
_reflns_number_total             14423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Complex1.cif
_cod_data_source_block           (VO)3(L5-H)3
_cod_original_cell_volume        3327(2)
_cod_database_code               1571561
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C9(H9), C49(H49), C7(H7), C36(H36), C12(H12), C56(H56), C29(H29),
 C47(H47), C32(H32), C5(H5), C58(H58), C16(H16), C27(H27), C59(H59), C19(H19),
 C17(H17), C4(H4), C23(H23), C3(H3), C57(H57), C37(H37), C38(H38), C39(H39),
 C2(H2), C18(H18), C22(H22), C44(H44), C45(H45), C24(H24), C42(H42), C43(H43),
 C25(H25)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 252 electrons were 
found in a volume of 1107\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[C3H7NO], 0.5[H2O] per Asymmetric Unit 
which account for 250 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77668
_shelx_hkl_checksum              9021
_shelx_fab_checksum              63005
_olex2_submission_original_sample_id (VO)3(L5-H)3
_olex2_submission_special_instructions 'No special instructions were received'