#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/00/2200003.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_2200003
loop_
_publ_author_name
'Buqin Jing'
'Lianzhi Li'
'Daqi Wang'
'Tao Xu'
'Xinglin Guo'
_publ_section_title
;Aqua[N,N'-ethylenebis(o-vanillylideniminato-κ²N,O)]oxovanadium(IV)
 monohydrate
;
_journal_coeditor_code           AC6209
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2244
_journal_page_last               m2246
_journal_paper_doi               10.1107/S1600536805031843
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V (C18 H18 N2 O4) O (H2 O)], H2 O'
_chemical_formula_moiety         'C18 H20 N2 O6 V, H2 O'
_chemical_formula_sum            'C18 H22 N2 O7 V'
_chemical_formula_weight         429.32
_chemical_melting_point          295
_chemical_name_systematic
;
aqua{6,6'-dimethoxy-2,2'-[1,2-ethanediylbis(nitrilomethylidyne)]diphenolato-
κ²N,O}oxovanadium(IV) monohydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.086(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.613(7)
_cell_length_b                   6.701(4)
_cell_length_c                   22.383(12)
_cell_measurement_reflns_used    1765
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.5625
_cell_measurement_theta_min      3.174
_cell_volume                     1887.0(18)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9439
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.8084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0499P)²+0.8719P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                1977
_reflns_number_total             3311
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ac6209.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.

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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1886.9(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200003
_cod_database_fobs_code          2200003
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_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_type_symbol
V1 -0.03501(5) 0.42570(9) 0.19492(3) 0.0346(2) Uani d . 1 V
N1 -0.1061(2) 0.1957(5) 0.23651(16) 0.0442(9) Uani d . 1 N
N2 -0.0225(3) 0.2047(5) 0.13180(16) 0.0450(9) Uani d . 1 N
O1 -0.01517(19) 0.5668(4) 0.27119(11) 0.0419(7) Uani d . 1 O
O2 0.0226(2) 0.8223(5) 0.35532(13) 0.0593(9) Uani d . 1 O
O3 0.07910(19) 0.5695(4) 0.15981(11) 0.0395(6) Uani d . 1 O
O4 0.1938(2) 0.8578(5) 0.12422(13) 0.0564(8) Uani d . 1 O
O5 -0.1394(2) 0.5289(4) 0.16521(13) 0.0508(8) Uani d . 1 O
O6 0.1164(2) 0.2521(4) 0.23909(16) 0.0576(9) Uani d D 1 O
O7 0.1573(2) 0.8450(4) 0.25201(13) 0.0473(7) Uani d D 1 O
C1 -0.1282(3) 0.1872(6) 0.2912(2) 0.0485(11) Uani d . 1 C
H1 -0.1617 0.0725 0.3037 0.058 Uiso calc R 1 H
C2 -0.1053(3) 0.3418(7) 0.33511(18) 0.0420(10) Uani d . 1 C
C3 -0.0506(3) 0.5195(6) 0.32307(17) 0.0355(10) Uani d . 1 C
C4 -0.0320(3) 0.6558(7) 0.37104(19) 0.0462(11) Uani d . 1 C
C5 -0.0658(4) 0.6171(9) 0.4268(2) 0.0640(14) Uani d . 1 C
H5 -0.0527 0.7087 0.4576 0.077 Uiso calc R 1 H
C6 -0.1198(4) 0.4408(9) 0.4372(2) 0.0712(16) Uani d . 1 C
H6 -0.1425 0.4143 0.4750 0.085 Uiso calc R 1 H
C7 -0.1391(3) 0.3081(8) 0.3924(2) 0.0572(13) Uani d . 1 C
H7 -0.1758 0.1913 0.3998 0.069 Uiso calc R 1 H
C8 0.0688(4) 0.9471(7) 0.4015(2) 0.0789(17) Uani d . 1 C
H8A 0.1037 1.0577 0.3840 0.118 Uiso calc R 1 H
H8B 0.1196 0.8719 0.4263 0.118 Uiso calc R 1 H
H8C 0.0141 0.9959 0.4255 0.118 Uiso calc R 1 H
C9 -0.1374(5) 0.0328(8) 0.1951(3) 0.0898(19) Uani d . 1 C
H9A -0.1335 -0.0923 0.2169 0.108 Uiso calc R 1 H
H9B -0.2108 0.0526 0.1802 0.108 Uiso calc R 1 H
C10 -0.0742(5) 0.0186(8) 0.1463(3) 0.0844(17) Uani d . 1 C
H10A -0.1182 -0.0256 0.1115 0.101 Uiso calc R 1 H
H10B -0.0201 -0.0822 0.1550 0.101 Uiso calc R 1 H
C11 0.0273(3) 0.2209(7) 0.08406(19) 0.0506(12) Uani d . 1 C
H11 0.0240 0.1123 0.0581 0.061 Uiso calc R 1 H
C12 0.0875(3) 0.3899(6) 0.06681(18) 0.0425(10) Uani d . 1 C
C13 0.1106(3) 0.5531(6) 0.10500(17) 0.0362(9) Uani d . 1 C
C14 0.1738(3) 0.7079(6) 0.08344(18) 0.0414(10) Uani d . 1 C
C15 0.2084(3) 0.7045(8) 0.0271(2) 0.0550(12) Uani d . 1 C
H15 0.2481 0.8104 0.0138 0.066 Uiso calc R 1 H
C16 0.1845(4) 0.5437(9) -0.0102(2) 0.0647(15) Uani d . 1 C
H16 0.2082 0.5413 -0.0486 0.078 Uiso calc R 1 H
C17 0.1269(4) 0.3902(8) 0.0093(2) 0.0594(13) Uani d . 1 C
H17 0.1127 0.2815 -0.0159 0.071 Uiso calc R 1 H
C18 0.2774(3) 0.9908(7) 0.1150(2) 0.0684(15) Uani d . 1 C
H18A 0.2823 1.0883 0.1465 0.103 Uiso calc R 1 H
H18B 0.2639 1.0567 0.0771 0.103 Uiso calc R 1 H
H18C 0.3430 0.9181 0.1151 0.103 Uiso calc R 1 H
H19 0.1804(17) 0.303(5) 0.232(2) 0.080 Uiso d D 1 H
H20 0.124(3) 0.1198(19) 0.245(2) 0.080 Uiso d D 1 H
H21 0.151(3) 0.788(6) 0.2159(9) 0.080 Uiso d D 1 H
H22 0.104(2) 0.809(7) 0.2737(14) 0.080 Uiso d D 1 H
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
_geom_angle_publ_flag
O5 V1 O3 103.30(14) y
O5 V1 O1 101.88(13) y
O3 V1 O1 93.49(11) y
O5 V1 N1 98.14(14) y
O3 V1 N1 157.05(12) y
O1 V1 N1 90.00(13) y
O5 V1 N2 97.31(14) y
O3 V1 N2 89.08(13) y
O1 V1 N2 159.48(12) y
N1 V1 N2 80.08(15) y
O5 V1 O6 176.60(13) y
O3 V1 O6 79.38(11) y
O1 V1 O6 79.93(11) y
N1 V1 O6 78.92(12) y
N2 V1 O6 80.55(12) y
C1 N1 C9 120.4(4) ?
C1 N1 V1 127.2(3) ?
C9 N1 V1 112.4(3) ?
C11 N2 C10 120.8(4) ?
C11 N2 V1 125.2(3) ?
C10 N2 V1 113.9(3) ?
C3 O1 V1 128.8(2) ?
C4 O2 C8 118.6(4) ?
C13 O3 V1 127.9(2) ?
C14 O4 C18 118.1(3) ?
V1 O6 H19 117(3) ?
V1 O6 H20 128(3) ?
H19 O6 H20 108(2) ?
H21 O7 H22 111(2) ?
N1 C1 C2 125.1(4) ?
N1 C1 H1 117.5 ?
C2 C1 H1 117.5 ?
C7 C2 C3 119.8(4) ?
C7 C2 C1 116.7(4) ?
C3 C2 C1 123.5(4) ?
O1 C3 C2 125.1(4) ?
O1 C3 C4 117.8(4) ?
C2 C3 C4 117.1(4) ?
O2 C4 C5 125.6(4) ?
O2 C4 C3 112.9(4) ?
C5 C4 C3 121.5(5) ?
C4 C5 C6 120.0(5) ?
C4 C5 H5 120.0 ?
C6 C5 H5 120.0 ?
C7 C6 C5 120.0(5) ?
C7 C6 H6 120.0 ?
C5 C6 H6 120.0 ?
C6 C7 C2 121.6(5) ?
C6 C7 H7 119.2 ?
C2 C7 H7 119.2 ?
O2 C8 H8A 109.5 ?
O2 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
O2 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
C10 C9 N1 113.6(4) ?
C10 C9 H9A 108.8 ?
N1 C9 H9A 108.8 ?
C10 C9 H9B 108.8 ?
N1 C9 H9B 108.8 ?
H9A C9 H9B 107.7 ?
C9 C10 N2 113.9(4) ?
C9 C10 H10A 108.8 ?
N2 C10 H10A 108.8 ?
C9 C10 H10B 108.8 ?
N2 C10 H10B 108.8 ?
H10A C10 H10B 107.7 ?
N2 C11 C12 126.3(4) ?
N2 C11 H11 116.8 ?
C12 C11 H11 116.8 ?
C13 C12 C17 118.8(4) ?
C13 C12 C11 122.8(4) ?
C17 C12 C11 118.3(4) ?
O3 C13 C12 124.5(4) ?
O3 C13 C14 118.1(4) ?
C12 C13 C14 117.4(4) ?
C15 C14 O4 125.0(4) ?
C15 C14 C13 121.9(4) ?
O4 C14 C13 113.1(3) ?
C14 C15 C16 120.1(5) ?
C14 C15 H15 119.9 ?
C16 C15 H15 119.9 ?
C17 C16 C15 119.8(4) ?
C17 C16 H16 120.1 ?
C15 C16 H16 120.1 ?
C16 C17 C12 121.9(5) ?
C16 C17 H17 119.0 ?
C12 C17 H17 119.0 ?
O4 C18 H18A 109.5 ?
O4 C18 H18B 109.5 ?
H18A C18 H18B 109.5 ?
O4 C18 H18C 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O5 1.590(3) y
V1 O3 1.944(3) y
V1 O1 1.952(3) y
V1 N1 2.041(3) y
V1 N2 2.060(3) y
V1 O6 2.389(3) y
N1 C1 1.275(5) ?
N1 C9 1.468(5) ?
N2 C11 1.282(5) ?
N2 C10 1.455(6) ?
O1 C3 1.312(4) ?
O2 C4 1.370(5) ?
O2 C8 1.422(5) ?
O3 C13 1.321(4) ?
O4 C14 1.368(5) ?
O4 C18 1.407(5) ?
O6 H19 0.899(10) ?
O6 H20 0.900(10) ?
O7 H21 0.893(10) ?
O7 H22 0.896(10) ?
C1 C2 1.444(6) ?
C1 H1 0.9300 ?
C2 C7 1.398(6) ?
C2 C3 1.412(5) ?
C3 C4 1.416(5) ?
C4 C5 1.372(6) ?
C5 C6 1.391(7) ?
C5 H5 0.9300 ?
C6 C7 1.350(7) ?
C6 H6 0.9300 ?
C7 H7 0.9300 ?
C8 H8A 0.9600 ?
C8 H8B 0.9600 ?
C8 H8C 0.9600 ?
C9 C10 1.400(7) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
C11 C12 1.431(6) ?
C11 H11 0.9300 ?
C12 C13 1.406(5) ?
C12 C17 1.413(6) ?
C13 C14 1.414(5) ?
C14 C15 1.363(5) ?
C15 C16 1.384(6) ?
C15 H15 0.9300 ?
C16 C17 1.350(6) ?
C16 H16 0.9300 ?
C17 H17 0.9300 ?
C18 H18A 0.9600 ?
C18 H18B 0.9600 ?
C18 H18C 0.9600 ?
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
O6 H19 O7 2_545 0.899(10) 2.07(2) 2.915(4) 156(4)
O6 H20 O7 1_545 0.900(10) 1.892(12) 2.788(4) 173(4)
O7 H21 O3 . 0.893(10) 2.09(2) 2.889(4) 148(3)
O7 H21 O4 . 0.893(10) 2.21(3) 2.931(4) 138(4)
O7 H22 O2 . 0.896(10) 2.16(2) 2.969(4) 151(3)
O7 H22 O1 . 0.896(10) 2.20(3) 2.919(4) 136(3)
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
C2 C3 C4 C5 -0.1(6)
C3 C4 C5 C6 0.0(6)
C4 C5 C6 C7 -0.2(7)
