#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/70/2227029.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_2227029
loop_
_publ_author_name
'Wong, Hon Wee'
'Lo, Kong Mun'
'Ng, Seik Weng'
_publ_section_title
;
 (Acetylacetone
 isonicotinoylhydrazonato-κ³O,N',O')dioxidovanadate(V)
 monohydrate
;
_journal_coeditor_code           NK2049
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1020
_journal_paper_doi               10.1107/S1600536810028886
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[V (C11 H12 N3 O2) O2], H2 O'
_chemical_formula_moiety         'C11 H12 N3 O4 V, H2 O'
_chemical_formula_sum            'C11 H14 N3 O5 V'
_chemical_formula_weight         319.19
_chemical_name_systematic
;
(Acetylacetone isonicotinoylhydrazonato-
κ³O,N',O')dioxidovanadate(V) monohydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9848(10)
_cell_length_b                   6.6630(4)
_cell_length_c                   13.8904(10)
_cell_measurement_reflns_used    3731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.9
_cell_volume                     1294.32(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11995
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.8580
_exptl_absorpt_correction_T_min  0.7695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.724
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1610
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0616P)²+2.2562P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                1416
_reflns_number_total             1610
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            nk2049.cif
_cod_data_source_block           I
_cod_database_code               2227029
_cod_database_fobs_code          2227029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.41194(4) 0.2500 0.31526(4) 0.01205(19) Uani d S 1 . .
O O1 0.41890(11) 0.0504(3) 0.24747(12) 0.0191(4) Uani d . 1 . .
O O2 0.27403(16) 0.2500 0.32874(16) 0.0204(5) Uani d S 1 . .
O O3 0.54634(16) 0.2500 0.35590(16) 0.0189(5) Uani d S 1 . .
O O1W 0.47876(17) -0.2500 0.12798(18) 0.0194(5) Uani d SD 1 . .
H H1W 0.467(2) -0.148(3) 0.161(2) 0.040(10) Uiso d D 1 . .
N N1 0.40746(18) 0.2500 0.46744(19) 0.0138(5) Uani d S 1 . .
N N2 0.49679(19) 0.2500 0.51358(19) 0.0139(5) Uani d S 1 . .
N N3 0.84943(19) 0.2500 0.5420(2) 0.0155(5) Uani d SD 1 . .
H H3 0.9099(11) 0.2500 0.554(4) 0.059(18) Uiso d SD 1 . .
C C1 0.1102(2) 0.2500 0.3685(3) 0.0218(7) Uani d S 1 . .
H H1A 0.1065 0.2500 0.2981 0.033 Uiso calc SR 1 . .
H H1B 0.0784 0.3701 0.3937 0.033 Uiso calc PR 0.50 . .
H H1C 0.0784 0.1299 0.3937 0.033 Uiso calc PR 0.50 . .
C C2 0.2135(2) 0.2500 0.3993(2) 0.0163(6) Uani d S 1 . .
C C3 0.2387(2) 0.2500 0.4946(2) 0.0165(6) Uani d S 1 . .
H H3A 0.1889 0.2500 0.5412 0.020 Uiso calc SR 1 . .
C C4 0.3340(2) 0.2500 0.5277(2) 0.0137(6) Uani d S 1 . .
C C5 0.3508(2) 0.2500 0.6351(2) 0.0198(7) Uani d S 1 . .
H H5A 0.4197 0.2500 0.6480 0.030 Uiso calc SR 1 . .
H H5B 0.3218 0.1299 0.6635 0.030 Uiso calc PR 0.50 . .
H H5C 0.3218 0.3701 0.6635 0.030 Uiso calc PR 0.50 . .
C C6 0.5624(2) 0.2500 0.4488(2) 0.0140(6) Uani d S 1 . .
C C7 0.6634(2) 0.2500 0.4810(2) 0.0133(6) Uani d S 1 . .
C C8 0.7378(2) 0.2500 0.4146(2) 0.0156(6) Uani d S 1 . .
H H8 0.7246 0.2500 0.3475 0.019 Uiso calc SR 1 . .
C C9 0.8314(2) 0.2500 0.4473(2) 0.0165(6) Uani d S 1 . .
H H9 0.8828 0.2500 0.4025 0.020 Uiso calc SR 1 . .
C C10 0.7787(2) 0.2500 0.6080(2) 0.0166(6) Uani d S 1 . .
H H10 0.7941 0.2500 0.6746 0.020 Uiso calc SR 1 . .
C C11 0.6845(2) 0.2500 0.5800(2) 0.0153(6) Uani d S 1 . .
H H11 0.6347 0.2500 0.6265 0.018 Uiso calc SR 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 O1 . 7_565 109.11(13) ?
O1 V1 O2 . . 96.61(7) ?
O1 V1 O2 7_565 . 96.61(7) ?
O1 V1 O3 . . 96.25(7) ?
O1 V1 O3 7_565 . 96.25(7) ?
O2 V1 O3 . . 157.73(10) ?
O1 V1 N1 . . 125.34(6) ?
O1 V1 N1 7_565 . 125.34(6) ?
O2 V1 N1 . . 82.75(10) ?
O3 V1 N1 . . 74.98(10) ?
C2 O2 V1 . . 136.3(2) ?
C6 O3 V1 . . 116.6(2) ?
C4 N1 N2 . . 113.6(3) ?
C4 N1 V1 . . 130.9(2) ?
N2 N1 V1 . . 115.46(19) ?
C6 N2 N1 . . 108.4(3) ?
C9 N3 C10 . . 122.0(3) ?
C9 N3 H3 . . 112(4) ?
C10 N3 H3 . . 126(4) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O2 C2 C3 . . 124.3(3) ?
O2 C2 C1 . . 114.3(3) ?
C3 C2 C1 . . 121.4(3) ?
C2 C3 C4 . . 123.9(3) ?
C2 C3 H3A . . 118.1 ?
C4 C3 H3A . . 118.1 ?
N1 C4 C3 . . 121.8(3) ?
N1 C4 C5 . . 120.3(3) ?
C3 C4 C5 . . 117.9(3) ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
N2 C6 O3 . . 124.5(3) ?
N2 C6 C7 . . 118.0(3) ?
O3 C6 C7 . . 117.5(3) ?
C8 C7 C11 . . 119.4(3) ?
C8 C7 C6 . . 120.9(3) ?
C11 C7 C6 . . 119.7(3) ?
C9 C8 C7 . . 119.3(3) ?
C9 C8 H8 . . 120.3 ?
C7 C8 H8 . . 120.3 ?
N3 C9 C8 . . 120.0(3) ?
N3 C9 H9 . . 120.0 ?
C8 C9 H9 . . 120.0 ?
N3 C10 C11 . . 120.7(3) ?
N3 C10 H10 . . 119.7 ?
C11 C10 H10 . . 119.7 ?
C10 C11 C7 . . 118.6(3) ?
C10 C11 H11 . . 120.7 ?
C7 C11 H11 . . 120.7 ?
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 . 1.6323(17) ?
V1 O1 7_565 1.6323(17) ?
V1 O2 . 1.938(2) ?
V1 O3 . 1.962(2) ?
V1 N1 . 2.115(3) ?
O2 C2 . 1.295(4) ?
O3 C6 . 1.310(4) ?
O1W H1W . 0.838(10) ?
N1 C4 . 1.325(4) ?
N1 N2 . 1.404(4) ?
N2 C6 . 1.286(4) ?
N3 C9 . 1.340(4) ?
N3 C10 . 1.349(4) ?
N3 H3 . 0.861(10) ?
C1 C2 . 1.507(4) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 C3 . 1.369(5) ?
C3 C4 . 1.411(4) ?
C3 H3A . 0.9500 ?
C4 C5 . 1.510(4) ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
C6 C7 . 1.481(4) ?
C7 C8 . 1.391(4) ?
C7 C11 . 1.407(4) ?
C8 C9 . 1.385(4) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C11 . 1.373(5) ?
C10 H10 . 0.9500 ?
C11 H11 . 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
_geom_hbond_publ_flag
O1W H1w O1 . 0.840(10) 1.910(10) 2.732(2) 168(3) yes
N3 H3 O1w 2_655 0.860(10) 1.87(3) 2.683(4) 158(6) yes
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
O1 V1 O2 C2 . . . . 124.90(6) ?
O1 V1 O2 C2 7_565 . . . -124.90(6) ?
O3 V1 O2 C2 . . . . 0.0 ?
N1 V1 O2 C2 . . . . 0.0 ?
O1 V1 O3 C6 . . . . -124.96(6) ?
O1 V1 O3 C6 7_565 . . . 124.96(6) ?
O2 V1 O3 C6 . . . . 0.0 ?
N1 V1 O3 C6 . . . . 0.0 ?
O1 V1 N1 C4 . . . . -92.98(9) ?
O1 V1 N1 C4 7_565 . . . 92.98(9) ?
O2 V1 N1 C4 . . . . 0.0 ?
O3 V1 N1 C4 . . . . 180.0 ?
O1 V1 N1 N2 . . . . 87.02(9) ?
O1 V1 N1 N2 7_565 . . . -87.02(9) ?
O2 V1 N1 N2 . . . . 180.0 ?
O3 V1 N1 N2 . . . . 0.0 ?
C4 N1 N2 C6 . . . . 180.0 ?
V1 N1 N2 C6 . . . . 0.0 ?
V1 O2 C2 C3 . . . . 0.0 ?
V1 O2 C2 C1 . . . . 180.0 ?
O2 C2 C3 C4 . . . . 0.0 ?
C1 C2 C3 C4 . . . . 180.0 ?
N2 N1 C4 C3 . . . . 180.0 ?
V1 N1 C4 C3 . . . . 0.0 ?
N2 N1 C4 C5 . . . . 0.0 ?
V1 N1 C4 C5 . . . . 180.0 ?
C2 C3 C4 N1 . . . . 0.0 ?
C2 C3 C4 C5 . . . . 180.0 ?
N1 N2 C6 O3 . . . . 0.0 ?
N1 N2 C6 C7 . . . . 180.0 ?
V1 O3 C6 N2 . . . . 0.0 ?
V1 O3 C6 C7 . . . . 180.0 ?
N2 C6 C7 C8 . . . . 180.0 ?
O3 C6 C7 C8 . . . . 0.0 ?
N2 C6 C7 C11 . . . . 0.0 ?
O3 C6 C7 C11 . . . . 180.0 ?
C11 C7 C8 C9 . . . . 0.0 ?
C6 C7 C8 C9 . . . . 180.0 ?
C10 N3 C9 C8 . . . . 0.0 ?
C7 C8 C9 N3 . . . . 0.0 ?
C9 N3 C10 C11 . . . . 0.0 ?
N3 C10 C11 C7 . . . . 0.0 ?
C8 C7 C11 C10 . . . . 0.0 ?
C6 C7 C11 C10 . . . . 180.0 ?
