The first pentagonal-bipyramidal vanadium(III) complexes with a Schiff-base N<sub>3</sub>O<sub>2</sub> pentadentate ligand: synthesis, structure and magnetic properties.
Bazhenova, Tamara A.; Zorina, Leokadiya V.; Simonov, Sergey V.; Mironov, Vladimir S.; Maximova, Olga V.; Spillecke, Lena; Koo, Changhyun; Klingeler, Rüdiger; Manakin, Yuriy V.; Vasiliev, Alexander N.; Yagubskii, Eduard B.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15287–15298; doi:10.1039/d0dt03092a

data_7705589
_publ_section_title
;
 The first pentagonal-bipyramidal vanadium(III) complexes with a
 Schiff-base N<sub>3</sub>O<sub>2</sub> pentadentate ligand: synthesis,
 structure and magnetic properties.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15287
_journal_page_last               15298
_journal_paper_doi               10.1039/d0dt03092a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C25 H20 N7 O2 S2 V, 0.5(C2 H3 N), 0.5(C H4 O)'
_chemical_formula_sum            'C26.5 H23.5 N7.5 O2.5 S2 V'
_chemical_formula_weight         602.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-07-10 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9738(2)
_cell_length_b                   14.3549(2)
_cell_length_c                   27.3124(4)
_cell_measurement_reflns_used    13229
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      30.8830
_cell_measurement_theta_min      1.5970
_cell_volume                     5478.66(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            30256
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        29.500
_diffrn_reflns_theta_max         31.267
_diffrn_reflns_theta_min         1.603
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       stick
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 5144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         15367
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0407P)^2^+1.5708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                13382
_reflns_number_total             15367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03092a2.cif
_cod_data_source_block           2_150K
_cod_depositor_comments
'Adding full bibliography for 7705587--7705589.cif.'
_cod_original_formula_sum        'C26.50 H23.50 N7.50 O2.50 S2 V'
_cod_database_code               7705589
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.967
_oxdiff_exptl_absorpt_empirical_full_min 0.950
_oxdiff_exptl_absorpt_empirical_full_max 1.079
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              62204