Crystal structures of a series of bis(acetylacetonato)oxovanadium(IV) complexes containing N-donor pyridyl ligands
Rood, Jeffrey A.; Reehl, Steven R.; Jacoby, Kaitlyn A.; Oliver, Allen; Acta Crystallographica Section E 76 (2020) 826–830; doi:10.1107/S2056989020006246

data_2243389
_publ_section_title
;
 Crystal structures of a series of bis(acetylacetonato)oxovanadium(IV)
 complexes containing N-donor pyridyl ligands
;
_journal_coeditor_code           ZL2781
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              826
_journal_page_last               830
_journal_paper_doi               10.1107/S2056989020006246
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[V (C5 H7 O2)2 O(C6 H4 N2)]'
_chemical_formula_moiety         'C16 H18 N2 O5 V'
_chemical_formula_sum            'C16 H18 N2 O5 V'
_chemical_formula_weight         369.26
_chemical_name_systematic
Bis(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')oxido(pyridine-4-carbonitrile-\k<i>N</i>)vanadium(IV)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 99.030(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1930(9)
_cell_length_b                   13.5080(9)
_cell_length_c                   13.3651(9)
_cell_measurement_reflns_used    7973
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.70
_cell_volume                     1639.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
XP (Bruker, 2015) and Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21763
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.314
_diffrn_reflns_theta_min         2.703
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9266
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0324P)^2^+1.6979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                1832
_reflns_number_total             2038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2781sup1.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243389
_cod_database_fobs_code          2243389
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.958
_shelx_hkl_checksum              43382
_shelx_res_checksum              82750