#------------------------------------------------------------------------------
#$Date: 2020-05-16 08:28:11 +0300 (Sat, 16 May 2020) $
#$Revision: 252093 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243389.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_2243389
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(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-κ²O,O')oxido(pyridine-4-carbonitrile-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                 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 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  0.0318
_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 et al., 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/[σ²(Fo²)+(0.0324P)²+1.6979P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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   0.909
_shelx_estimated_absorpt_t_max   0.958
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 0.89112(2) 0.750000 0.01271(10) Uani d 1 . .
O O1 0.500000 1.00987(10) 0.750000 0.0210(3) Uani d 1 . .
O O2 0.60596(10) 0.86813(7) 0.63185(7) 0.0166(2) Uani d 1 . .
O O3 0.31046(10) 0.86962(7) 0.65896(7) 0.0151(2) Uani d 1 . .
N N1 0.500000 0.71328(11) 0.750000 0.0130(3) Uani d 1 . .
N N2 0.500000 0.31564(14) 0.750000 0.0318(4) Uani d 1 . .
C C1 0.54997(15) 0.87153(9) 0.53874(10) 0.0157(3) Uani d 1 . .
C C2 0.39870(16) 0.87878(10) 0.50203(10) 0.0195(3) Uani d 1 . .
H H2 0.369478 0.886023 0.431015 0.023 Uiso calc 1 . .
C C3 0.28850(15) 0.87607(9) 0.56257(10) 0.0155(3) Uani d 1 . .
C C4 0.65451(16) 0.86478(11) 0.46315(11) 0.0214(3) Uani d 1 . .
H H4A 0.653674 0.797228 0.436328 0.032 Uiso calc 1 . .
H H4B 0.754227 0.881506 0.496340 0.032 Uiso calc 1 . .
H H4C 0.623837 0.911208 0.407492 0.032 Uiso calc 1 . .
C C5 0.12947(16) 0.88186(11) 0.51467(11) 0.0223(3) Uani d 1 . .
H H5A 0.121409 0.870964 0.441516 0.033 Uiso calc 1 . .
H H5B 0.090305 0.947415 0.527156 0.033 Uiso calc 1 . .
H H5C 0.073029 0.830993 0.544114 0.033 Uiso calc 1 . .
C C6 0.37746(14) 0.66216(10) 0.75924(9) 0.0148(3) Uani d 1 . .
H H6 0.290548 0.697948 0.765924 0.018 Uiso calc 1 . .
C C7 0.37194(14) 0.55958(10) 0.75947(10) 0.0164(3) Uani d 1 . .
H H7 0.283303 0.525726 0.765917 0.020 Uiso calc 1 . .
C C8 0.500000 0.50744(14) 0.750000 0.0161(4) Uani d 1 . .
C C9 0.500000 0.40014(15) 0.750000 0.0222(4) Uani d 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 O3 . 2_656 98.42(3) ?
O1 V1 O3 . . 98.42(3) ?
O3 V1 O3 2_656 . 163.17(6) ?
O1 V1 O2 . 2_656 98.91(3) ?
O3 V1 O2 2_656 2_656 89.01(4) ?
O3 V1 O2 . 2_656 88.39(4) ?
O1 V1 O2 . . 98.91(3) ?
O3 V1 O2 2_656 . 88.39(4) ?
O3 V1 O2 . . 89.01(4) ?
O2 V1 O2 2_656 . 162.19(6) ?
O1 V1 N1 . . 180.0 ?
O3 V1 N1 2_656 . 81.58(3) ?
O3 V1 N1 . . 81.58(3) ?
O2 V1 N1 2_656 . 81.09(3) ?
O2 V1 N1 . . 81.09(3) ?
C1 O2 V1 . . 126.40(9) ?
C3 O3 V1 . . 126.45(9) ?
C6 N1 C6 . 2_656 118.13(15) ?
C6 N1 V1 . . 120.93(8) ?
C6 N1 V1 2_656 . 120.93(8) ?
O2 C1 C2 . . 124.87(12) ?
O2 C1 C4 . . 116.92(12) ?
C2 C1 C4 . . 118.19(12) ?
C3 C2 C1 . . 124.49(13) ?
C3 C2 H2 . . 117.8 ?
C1 C2 H2 . . 117.8 ?
O3 C3 C2 . . 125.06(13) ?
O3 C3 C5 . . 115.03(12) ?
C2 C3 C5 . . 119.91(12) ?
C1 C4 H4A . . 109.5 ?
C1 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C1 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C3 C5 H5A . . 109.5 ?
C3 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C3 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
N1 C6 C7 . . 123.05(12) ?
N1 C6 H6 . . 118.5 ?
C7 C6 H6 . . 118.5 ?
C6 C7 C8 . . 118.22(12) ?
C6 C7 H7 . . 120.9 ?
C8 C7 H7 . . 120.9 ?
C7 C8 C7 2_656 . 119.33(17) ?
C7 C8 C9 2_656 . 120.33(8) ?
C7 C8 C9 . . 120.33(8) ?
N2 C9 C8 . . 180.0 ?
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 . 1.6040(14) ?
V1 O3 2_656 1.9838(9) ?
V1 O3 . 1.9838(9) ?
V1 O2 2_656 2.0055(9) ?
V1 O2 . 2.0055(9) ?
V1 N1 . 2.4022(15) ?
O2 C1 . 1.2706(17) ?
O3 C3 . 1.2752(17) ?
N1 C6 . 1.3435(15) ?
N1 C6 2_656 1.3435(15) ?
N2 C9 . 1.141(3) ?
C1 C2 . 1.4035(19) ?
C1 C4 . 1.5024(18) ?
C2 C3 . 1.3928(19) ?
C2 H2 . 0.9500 ?
C3 C5 . 1.5031(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 . 1.3866(19) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3946(16) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.449(3) ?
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
C4 H4C O1 5_676 0.98 2.47 3.4249(16) 164
C7 H7 O1 3_445 0.95 2.59 3.4673(14) 154
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 . . . . -9.23(18) ?
V1 O2 C1 C4 . . . . 172.30(9) ?
O2 C1 C2 C3 . . . . -4.8(2) ?
C4 C1 C2 C3 . . . . 173.61(13) ?
V1 O3 C3 C2 . . . . 14.38(18) ?
V1 O3 C3 C5 . . . . -165.06(9) ?
C1 C2 C3 O3 . . . . 2.2(2) ?
C1 C2 C3 C5 . . . . -178.42(13) ?
C6 N1 C6 C7 2_656 . . . -0.12(9) ?
V1 N1 C6 C7 . . . . 179.88(9) ?
N1 C6 C7 C8 . . . . 0.22(17) ?
C6 C7 C8 C7 . . . 2_656 -0.11(8) ?
C6 C7 C8 C9 . . . . 179.89(8) ?

_cod_database_fobs_code 2243389
