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_7705587
_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         'C23 H21 Cl2 N5 O2 V, C2 H6 O, Cl'
_chemical_formula_sum            'C25 H27 Cl3 N5 O3 V'
_chemical_formula_weight         602.80
_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-2013
_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            4
_cell_length_a                   7.29023(8)
_cell_length_b                   15.38948(19)
_cell_length_c                   22.8617(3)
_cell_measurement_reflns_used    11477
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      32.7400
_cell_measurement_theta_min      2.2180
_cell_volume                     2564.92(5)
_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-2013 (Sheldrick, 2013)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.926
_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  0.0170
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21049
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        31.000
_diffrn_reflns_theta_max         32.885
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87604
_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            brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.715
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 3451 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.9687P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                8290
_reflns_number_total             8631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03092a2.cif
_cod_data_source_block           1_150K
_cod_depositor_comments
'Adding full bibliography for 7705587--7705589.cif.'
_cod_database_code               7705587
_shelx_estimated_absorpt_t_min   0.620
_shelx_estimated_absorpt_t_max   0.915
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.128
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-2
_shelx_res_checksum              46720