#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/15/2221529.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_2221529
loop_
_publ_author_name
'Wong, Hon Wee'
'Lo, Kong Mun'
'Ng, Seik Weng'
_publ_section_title
(Benzohydrazidato-κ²N',O)[2-(benzoylhydrazono-κ²N,O)propionato-κO]oxidovanadium(V)
_journal_coeditor_code           TK2396
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m422
_journal_paper_doi               10.1107/S1600536809009520
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[V (C7 H7 N2 O) (C10 H8 N2 O3)O]'
_chemical_formula_moiety         'C17 H15 N4 O5 V'
_chemical_formula_sum            'C17 H15 N4 O5 V'
_chemical_formula_weight         406.27
_chemical_name_systematic
;
(Benzohydrazidato-κ²N',O)[2-(benzoylhydrazono-
κ²N,O)propionato-κO]oxidovanadium(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 96.6030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9424(2)
_cell_length_b                   6.23840(10)
_cell_length_c                   25.7215(5)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.9
_cell_volume                     1744.18(5)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_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  0.027
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11614
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4010
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.00
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0443P)²+0.9013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.091
_reflns_number_gt                3330
_reflns_number_total             4010
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk2396.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2221529
_cod_database_fobs_code          2221529
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.63939(3) 0.51362(5) 0.667678(11) 0.02025(10) Uani d . 1 . .
O O1 0.71456(13) 0.3013(2) 0.65899(5) 0.0310(3) Uani d . 1 . .
O O2 0.47660(11) 0.4125(2) 0.63552(5) 0.0252(3) Uani d . 1 . .
O O3 0.77761(11) 0.7223(2) 0.66978(4) 0.0227(3) Uani d . 1 . .
O O4 0.87206(11) 0.9694(2) 0.62563(5) 0.0250(3) Uani d . 1 . .
O O5 0.53800(11) 0.7850(2) 0.69541(4) 0.0229(3) Uani d . 1 . .
N N1 0.49712(13) 0.6388(3) 0.56603(5) 0.0230(3) Uani d . 1 . .
N N2 0.60460(13) 0.6815(2) 0.59808(5) 0.0200(3) Uani d . 1 . .
N N3 0.57784(13) 0.6090(2) 0.76970(5) 0.0204(3) Uani d D 1 . .
H H3 0.582(2) 0.584(4) 0.8033(4) 0.039(6) Uiso d D 1 . .
N N4 0.63345(14) 0.4678(2) 0.73974(6) 0.0213(3) Uani d D 1 . .
H H4 0.6650(17) 0.363(3) 0.7597(7) 0.029(6) Uiso d D 1 . .
C C1 0.32064(16) 0.4069(3) 0.56296(7) 0.0235(4) Uani d . 1 . .
C C2 0.26918(17) 0.4956(3) 0.51595(7) 0.0271(4) Uani d . 1 . .
H H2 0.3101 0.6096 0.5006 0.033 Uiso calc R 1 . .
C C3 0.15882(18) 0.4191(3) 0.49134(8) 0.0316(4) Uani d . 1 . .
H H3A 0.1242 0.4805 0.4592 0.038 Uiso calc R 1 . .
C C4 0.09839(18) 0.2527(3) 0.51358(8) 0.0346(5) Uani d . 1 . .
H H4A 0.0221 0.2011 0.4968 0.041 Uiso calc R 1 . .
C C5 0.14961(19) 0.1621(4) 0.56019(8) 0.0366(5) Uani d . 1 . .
H H5 0.1086 0.0477 0.5754 0.044 Uiso calc R 1 . .
C C6 0.26067(19) 0.2380(3) 0.58478(8) 0.0330(5) Uani d . 1 . .
H H6 0.2959 0.1747 0.6166 0.040 Uiso calc R 1 . .
C C7 0.43810(16) 0.4902(3) 0.58978(7) 0.0221(4) Uani d . 1 . .
C C8 0.67646(16) 0.8356(3) 0.58852(7) 0.0217(4) Uani d . 1 . .
C C9 0.78589(16) 0.8481(3) 0.62982(6) 0.0212(4) Uani d . 1 . .
C C10 0.65613(17) 0.9934(3) 0.54563(7) 0.0273(4) Uani d . 1 . .
H H10A 0.6174 0.9223 0.5139 0.041 Uiso calc R 1 . .
H H10B 0.7352 1.0546 0.5388 0.041 Uiso calc R 1 . .
H H10C 0.6022 1.1080 0.5557 0.041 Uiso calc R 1 . .
C C11 0.52823(15) 0.7794(3) 0.74341(6) 0.0191(3) Uani d . 1 . .
C C12 0.46480(15) 0.9478(3) 0.77016(7) 0.0207(4) Uani d . 1 . .
C C13 0.41422(15) 1.1174(3) 0.73968(7) 0.0235(4) Uani d . 1 . .
H H13 0.4241 1.1237 0.7035 0.028 Uiso calc R 1 . .
C C14 0.34966(17) 1.2765(3) 0.76211(8) 0.0297(4) Uani d . 1 . .
H H14 0.3142 1.3913 0.7413 0.036 Uiso calc R 1 . .
C C15 0.33666(18) 1.2683(3) 0.81518(8) 0.0341(5) Uani d . 1 . .
H H15 0.2914 1.3766 0.8305 0.041 Uiso calc R 1 . .
C C16 0.38955(18) 1.1029(4) 0.84576(8) 0.0335(5) Uani d . 1 . .
H H16 0.3821 1.1002 0.8822 0.040 Uiso calc R 1 . .
C C17 0.45334(17) 0.9412(3) 0.82367(7) 0.0275(4) Uani d . 1 . .
H H17 0.4889 0.8270 0.8447 0.033 Uiso calc R 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 N4 . . 95.10(7) ?
O1 V1 O2 . . 97.53(7) ?
N4 V1 O2 . . 103.39(6) ?
O1 V1 O3 . . 98.34(7) ?
N4 V1 O3 . . 100.63(6) ?
O2 V1 O3 . . 149.76(5) ?
O1 V1 N2 . . 110.29(6) ?
N4 V1 N2 . . 154.60(6) ?
O2 V1 N2 . . 74.50(5) ?
O3 V1 N2 . . 75.90(5) ?
O1 V1 O5 . . 168.87(6) ?
N4 V1 O5 . . 73.77(5) ?
O2 V1 O5 . . 85.25(5) ?
O3 V1 O5 . . 84.11(5) ?
N2 V1 O5 . . 80.84(5) ?
C7 O2 V1 . . 116.27(11) ?
C9 O3 V1 . . 119.54(11) ?
C11 O5 V1 . . 113.82(11) ?
C7 N1 N2 . . 106.71(14) ?
C8 N2 N1 . . 121.87(15) ?
C8 N2 V1 . . 119.25(12) ?
N1 N2 V1 . . 118.51(11) ?
C11 N3 N4 . . 114.16(14) ?
C11 N3 H3 . . 127.7(16) ?
N4 N3 H3 . . 118.0(16) ?
N3 N4 V1 . . 121.87(11) ?
N3 N4 H4 . . 108.9(13) ?
V1 N4 H4 . . 129.3(13) ?
C2 C1 C6 . . 119.31(17) ?
C2 C1 C7 . . 120.58(16) ?
C6 C1 C7 . . 120.11(17) ?
C3 C2 C1 . . 120.43(18) ?
C3 C2 H2 . . 119.8 ?
C1 C2 H2 . . 119.8 ?
C2 C3 C4 . . 120.11(19) ?
C2 C3 H3A . . 119.9 ?
C4 C3 H3A . . 119.9 ?
C5 C4 C3 . . 119.82(19) ?
C5 C4 H4A . . 120.1 ?
C3 C4 H4A . . 120.1 ?
C4 C5 C6 . . 120.10(19) ?
C4 C5 H5 . . 120.0 ?
C6 C5 H5 . . 120.0 ?
C5 C6 C1 . . 120.22(19) ?
C5 C6 H6 . . 119.9 ?
C1 C6 H6 . . 119.9 ?
O2 C7 N1 . . 123.88(16) ?
O2 C7 C1 . . 117.71(16) ?
N1 C7 C1 . . 118.41(15) ?
N2 C8 C10 . . 126.85(16) ?
N2 C8 C9 . . 110.97(15) ?
C10 C8 C9 . . 122.07(16) ?
O4 C9 O3 . . 124.44(16) ?
O4 C9 C8 . . 121.82(16) ?
O3 C9 C8 . . 113.73(15) ?
C8 C10 H10A . . 109.5 ?
C8 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C8 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
O5 C11 N3 . . 116.36(15) ?
O5 C11 C12 . . 122.63(15) ?
N3 C11 C12 . . 121.00(15) ?
C13 C12 C17 . . 120.13(16) ?
C13 C12 C11 . . 117.19(15) ?
C17 C12 C11 . . 122.68(16) ?
C14 C13 C12 . . 119.97(17) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C13 C14 C15 . . 119.90(19) ?
C13 C14 H14 . . 120.0 ?
C15 C14 H14 . . 120.0 ?
C16 C15 C14 . . 120.17(18) ?
C16 C15 H15 . . 119.9 ?
C14 C15 H15 . . 119.9 ?
C15 C16 C17 . . 120.52(18) ?
C15 C16 H16 . . 119.7 ?
C17 C16 H16 . . 119.7 ?
C16 C17 C12 . . 119.28(18) ?
C16 C17 H17 . . 120.4 ?
C12 C17 H17 . . 120.4 ?
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 . 1.5890(10) ?
V1 O2 . 1.9790(10) ?
V1 O3 . 1.9920(10) ?
V1 O5 . 2.1880(10) ?
V1 N2 . 2.0710(10) ?
V1 N4 . 1.884(2) ?
O2 C7 . 1.297(2) ?
O3 C9 . 1.304(2) ?
O4 C9 . 1.223(2) ?
O5 C11 . 1.252(2) ?
N1 C7 . 1.319(2) ?
N1 N2 . 1.382(2) ?
N2 C8 . 1.283(2) ?
N3 C11 . 1.341(2) ?
N3 N4 . 1.359(2) ?
N3 H3 . 0.874(9) ?
N4 H4 . 0.879(9) ?
C1 C2 . 1.389(3) ?
C1 C6 . 1.393(3) ?
C1 C7 . 1.481(2) ?
C2 C3 . 1.382(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.389(3) ?
C3 H3A . 0.9500 ?
C4 C5 . 1.384(3) ?
C4 H4A . 0.9500 ?
C5 C6 . 1.387(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C8 C10 . 1.476(3) ?
C8 C9 . 1.509(2) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 C12 . 1.473(2) ?
C12 C13 . 1.393(3) ?
C12 C17 . 1.397(2) ?
C13 C14 . 1.382(3) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.389(3) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.383(3) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.385(3) ?
C16 H16 . 0.9500 ?
C17 H17 . 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
N3 H3 O4 2_646 0.870(10) 1.970(10) 2.823(2) 164(2) yes
N4 H4 O3 2_646 0.880(10) 2.050(10) 2.861(2) 154(2) yes
