#------------------------------------------------------------------------------
#$Date: 2020-05-16 08:28:11 +0300 (Sat, 16 May 2020) $
#$Revision: 252093 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243388.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243388
loop_
_publ_author_name
'Rood, Jeffrey A.'
'Reehl, Steven R.'
'Jacoby, Kaitlyn A.'
'Oliver, Allen'
_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 (C5 H5 N)]'
_chemical_formula_moiety         'C15 H19 N O5 V'
_chemical_formula_sum            'C15 H19 N O5 V'
_chemical_formula_weight         344.25
_chemical_name_systematic
Bis(acetylacetonato-κ²O,O')oxido(pyridine-κN)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                 103.367(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8820(5)
_cell_length_b                   15.2092(11)
_cell_length_c                   13.9871(9)
_cell_measurement_reflns_used    8119
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.68
_cell_volume                     1631.33(19)
_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 et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (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 ω and φ-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         2.678
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       tablet
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0362P)²+1.4639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                1882
_reflns_number_total             2037
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zl2781sup1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243388
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.937
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.500000 0.41643(2) 0.750000 0.01694(10) Uani d 1 . .
O O1 0.500000 0.52179(9) 0.750000 0.0239(3) Uani d 1 . .
O O2 0.54371(12) 0.39403(6) 0.61740(7) 0.0211(2) Uani d 1 . .
O O3 0.24437(11) 0.39799(6) 0.69551(7) 0.0212(2) Uani d 1 . .
N N1 0.500000 0.25955(10) 0.750000 0.0193(3) Uani d 1 . .
C C1 0.43127(17) 0.37920(9) 0.53797(9) 0.0209(3) Uani d 1 . .
C C2 0.25102(18) 0.37547(10) 0.52875(10) 0.0264(3) Uani d 1 . .
H H2 0.179805 0.365061 0.465064 0.032 Uiso calc 1 . .
C C3 0.16766(17) 0.38580(8) 0.60560(10) 0.0211(3) Uani d 1 . .
C C4 -0.02841(18) 0.38382(11) 0.58352(12) 0.0312(3) Uani d 1 . .
H H4A -0.066433 0.356674 0.638591 0.047 Uiso calc 1 . .
H H4B -0.072855 0.349511 0.523659 0.047 Uiso calc 1 . .
H H4C -0.073646 0.443987 0.573924 0.047 Uiso calc 1 . .
C C5 0.5033(2) 0.36549(12) 0.44857(11) 0.0322(3) Uani d 1 . .
H H5A 0.542558 0.421933 0.427631 0.048 Uiso calc 1 . .
H H5B 0.412268 0.340944 0.395398 0.048 Uiso calc 1 . .
H H5C 0.601990 0.324655 0.464361 0.048 Uiso calc 1 . .
C C6 0.37706(16) 0.21376(9) 0.78046(9) 0.0224(3) Uani d 1 . .
H H6 0.289206 0.245242 0.802491 0.027 Uiso calc 1 . .
C C7 0.37197(19) 0.12280(10) 0.78135(10) 0.0274(3) Uani d 1 . .
H H7 0.282169 0.092712 0.803098 0.033 Uiso calc 1 . .
C C8 0.500000 0.07661(13) 0.750000 0.0293(4) Uani d 1 . .
H H8 0.500002 0.014145 0.750000 0.035 Uiso calc 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 V1 O2 . . 99.84(3) ?
O1 V1 O2 . 2_656 99.85(3) ?
O2 V1 O2 . 2_656 160.31(6) ?
O1 V1 O3 . 2_656 98.05(3) ?
O2 V1 O3 . 2_656 87.43(4) ?
O2 V1 O3 2_656 2_656 89.83(4) ?
O1 V1 O3 . . 98.05(3) ?
O2 V1 O3 . . 89.83(4) ?
O2 V1 O3 2_656 . 87.42(4) ?
O3 V1 O3 2_656 . 163.90(6) ?
O1 V1 N1 . . 180.0 ?
O2 V1 N1 . . 80.16(3) ?
O2 V1 N1 2_656 . 80.15(3) ?
O3 V1 N1 2_656 . 81.95(3) ?
O3 V1 N1 . . 81.95(3) ?
C1 O2 V1 . . 127.47(9) ?
C3 O3 V1 . . 126.95(9) ?
C6 N1 C6 . 2_656 117.39(16) ?
C6 N1 V1 . . 121.31(8) ?
C6 N1 V1 2_656 . 121.30(8) ?
O2 C1 C2 . . 125.19(12) ?
O2 C1 C5 . . 115.52(12) ?
C2 C1 C5 . . 119.28(12) ?
C3 C2 C1 . . 125.12(13) ?
C3 C2 H2 . . 117.4 ?
C1 C2 H2 . . 117.4 ?
O3 C3 C2 . . 125.19(12) ?
O3 C3 C4 . . 115.80(12) ?
C2 C3 C4 . . 119.01(12) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C1 C5 H5A . . 109.5 ?
C1 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C1 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
N1 C6 C7 . . 123.15(13) ?
N1 C6 H6 . . 118.4 ?
C7 C6 H6 . . 118.4 ?
C8 C7 C6 . . 118.72(14) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
C7 C8 C7 . 2_656 118.87(19) ?
C7 C8 H8 . . 120.6 ?
C7 C8 H8 2_656 . 120.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O1 . 1.6024(14) ?
V1 O2 . 1.9925(9) ?
V1 O2 2_656 1.9925(9) ?
V1 O3 2_656 2.0023(9) ?
V1 O3 . 2.0023(9) ?
V1 N1 . 2.3861(16) ?
O2 C1 . 1.2710(16) ?
O3 C3 . 1.2766(16) ?
N1 C6 . 1.3402(15) ?
N1 C6 2_656 1.3402(15) ?
C1 C2 . 1.3977(19) ?
C1 C5 . 1.5025(19) ?
C2 C3 . 1.392(2) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.5047(18) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C6 C7 . 1.384(2) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3816(18) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C5 H5A O1 5_666 0.98 2.58 3.2589(18) 127
C7 H7 O1 3_445 0.95 2.43 3.2487(17) 144
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
V1 O2 C1 C2 . . . . -0.2(2) ?
V1 O2 C1 C5 . . . . 179.40(9) ?
O2 C1 C2 C3 . . . . -1.3(2) ?
C5 C1 C2 C3 . . . . 179.11(14) ?
V1 O3 C3 C2 . . . . 5.89(19) ?
V1 O3 C3 C4 . . . . -173.40(9) ?
C1 C2 C3 O3 . . . . -1.8(2) ?
C1 C2 C3 C4 . . . . 177.47(13) ?
C6 N1 C6 C7 2_656 . . . -0.21(9) ?
V1 N1 C6 C7 . . . . 179.79(9) ?
N1 C6 C7 C8 . . . . 0.41(18) ?
C6 C7 C8 C7 . . . 2_656 -0.19(9) ?

_cod_database_fobs_code 2243388
