#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/09/2010953.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_2010953
loop_
_publ_author_name
'Uemura, Ryushi'
'Tsuchimoto, Masanobu'
'Ohba, Shigeru'
_publ_section_title
;[N,N'-Bis(3-carboxysalicylidene)-1,2-diphenyl-(RR,SS)-1,2-ethanediyldiaminato-O,N,N',O'](methanol-O)oxovanadium(IV)
 and
 [N,N'-bis(3-carboxysalicylidene)-2,3-dimethyl-2,3-butanediyldiaminato-O,N,N',O']oxovanadium(IV)
 monohydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e199
_journal_page_last               e200
_journal_paper_doi               10.1107/S0108270100005679
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[V1 O1 (C22 H22 N2 O6)], H2 O'
_chemical_formula_moiety         'C22 H22 N2 O7 V, H2 O1'
_chemical_formula_sum            'C22 H24 N2 O8 V'
_chemical_formula_weight         495.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                107.66(2)
_cell_angle_beta                 96.21(2)
_cell_angle_gamma                100.45(2)
_cell_formula_units_Z            2
_cell_length_a                   10.508(3)
_cell_length_b                   11.728(2)
_cell_length_c                   9.726(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     1106.0(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .085
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6772
_diffrn_reflns_theta_max         30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .500
_exptl_absorpt_correction_T_max  .915
_exptl_absorpt_correction_T_min  .860
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         .70
_refine_diff_density_min         -.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6445
_refine_ls_R_factor_gt           .039
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0742P)² + 0.2356P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .116
_reflns_number_gt                5528
_reflns_number_total             6445
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0271.cif
_cod_data_source_block           II
_cod_original_cell_volume        1106.1(5)
_cod_database_code               2010953
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
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_occupancy
_atom_site_type_symbol
V1 .93844(2) .23532(2) .43953(2) .02608(8) Uani 1.00 V
O2 1.00360(10) .31260(10) .34620(10) .0416(3) Uani 1.00 O
O3 1.06780(10) .24980(10) .60740(10) .0326(2) Uani 1.00 O
O4 .96380(10) .06960(10) .35300(10) .0355(2) Uani 1.00 O
O5 1.43430(10) .29040(10) .8360(2) .0545(4) Uani 1.00 O
O6 1.2818(2) .17820(10) .6463(2) .0536(4) Uani 1.00 O
O7 1.1604(2) -.17820(10) .1322(2) .0585(4) Uani 1.00 O
O8 1.1578(2) -.0317(2) .3342(2) .0669(5) Uani 1.00 O
O33 .5718(2) .1209(2) .9139(3) .0841(7) Uani 1.00 O
N9 .85100(10) .35520(10) .57930(10) .0267(2) Uani 1.00 N
N10 .74390(10) .16860(10) .34780(10) .0299(2) Uani 1.00 N
C11 1.11520(10) .34850(10) .7264(2) .0264(2) Uani 1.00 C
C12 1.24100(10) .36410(10) .8077(2) .0295(3) Uani 1.00 C
C13 1.3267(2) .2754(2) .7658(2) .0373(3) Uani 1.00 C
C14 1.2919(2) .4686(2) .9299(2) .0367(3) Uani 1.00 C
C15 1.2216(2) .5585(2) .9752(2) .0383(3) Uani 1.00 C
C16 1.0979(2) .54220(10) .8990(2) .0337(3) Uani 1.00 C
C17 1.04250(10) .43900(10) .7751(2) .0275(2) Uani 1.00 C
C18 .91160(10) .43230(10) .7037(2) .0294(3) Uani 1.00 C
C19 .71700(10) .36160(10) .5147(2) .0290(3) Uani 1.00 C
C20 .7378(2) .4369(2) .4117(2) .0439(4) Uani 1.00 C
C21 .6416(2) .4238(2) .6310(2) .0421(4) Uani 1.00 C
C22 .64540(10) .22530(10) .4301(2) .0314(3) Uani 1.00 C
C23 .5195(2) .2162(2) .3277(2) .0510(5) Uani 1.00 C
C24 .6139(2) .1548(2) .5361(3) .0486(4) Uani 1.00 C
C25 .70500(10) .0797(2) .2253(2) .0350(3) Uani 1.00 C
C26 .78700(10) .00430(10) .1483(2) .0326(3) Uani 1.00 C
C27 .7338(2) -.0738(2) .0052(2) .0414(4) Uani 1.00 C
C28 .8010(2) -.1537(2) -.0740(2) .0452(4) Uani 1.00 C
C29 .9215(2) -.1611(2) -.0074(2) .0389(3) Uani 1.00 C
C30 .9760(2) -.08800(10) .1365(2) .0324(3) Uani 1.00 C
C31 1.1044(2) -.1032(2) .1997(2) .0416(4) Uani 1.00 C
C32 .91040(10) -.00160(10) .2160(2) .0294(3) Uani 1.00 C
H6 1.209(3) .175(3) .623(4) .09000(10) Uiso 1.00 H
H8 1.100(4) .015(3) .369(4) .09850(10) Uiso 1.00 H
H14 1.374(2) .481(2) .981(2) .04735(7) Uiso 1.00 H
H15 1.260(2) .630(2) 1.060(3) .05258(8) Uiso 1.00 H
H16 1.047(2) .599(2) .924(3) .05054(8) Uiso 1.00 H
H18 .872(2) .489(2) .753(2) .03272(6) Uiso 1.00 H
H20A .795(3) .520(2) .464(3) .05827(9) Uiso 1.00 H
H20B .774(2) .401(2) .337(3) .05209(8) Uiso 1.00 H
H20C .657(3) .448(2) .366(3) .06366(9) Uiso 1.00 H
H21A .641(2) .396(2) .710(3) .05008(8) Uiso 1.00 H
H21B .685(3) .515(3) .667(3) .06448(9) Uiso 1.00 H
H21C .551(3) .411(2) .581(3) .06145(9) Uiso 1.00 H
H23A .470(3) .268(2) .377(3) .06091(9) Uiso 1.00 H
H23B .473(3) .142(2) .297(3) .05343(8) Uiso 1.00 H
H23C .537(3) .242(2) .244(3) .06223(9) Uiso 1.00 H
H24A .541(2) .179(2) .583(3) .05292(8) Uiso 1.00 H
H24B .682(3) .173(3) .610(3) .06670(10) Uiso 1.00 H
H24C .587(3) .061(3) .482(3) .06793(10) Uiso 1.00 H
H25 .615(2) .052(2) .185(3) .05270(8) Uiso 1.00 H
H27 .661(3) -.069(3) -.032(3) .06791(10) Uiso 1.00 H
H28 .768(3) -.206(3) -.173(3) .06824(10) Uiso 1.00 H
H29 .969(2) -.206(2) -.055(3) .05341(8) Uiso 1.00 H
H33A .532(4) .157(3) .881(4) .09040(10) Uiso 1.00 H
H33B .645(3) .138(3) .897(3) .07480(10) Uiso 1.00 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C)
;
V V .300 .529
;International Tables for Crystallography
(1992, Vol. C)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 V1 O3 1_555 1_555 109.44(6) no
O2 V1 O4 1_555 1_555 105.60(6) no
O2 V1 N9 1_555 1_555 103.98(6) no
O2 V1 N10 1_555 1_555 107.38(6) no
O3 V1 O4 1_555 1_555 86.82(5) no
O3 V1 N9 1_555 1_555 88.75(5) no
O3 V1 N10 1_555 1_555 142.90(6) no
O4 V1 N9 1_555 1_555 149.87(5) no
O4 V1 N10 1_555 1_555 87.72(5) no
N9 V1 N10 1_555 1_555 78.08(5) no
V1 O3 C11 1_555 1_555 127.10(10) no
V1 O4 C32 1_555 1_555 123.20(10) no
C13 O6 H6 1_555 1_555 108(2) no
C31 O8 H8 1_555 1_555 108(2) no
H33A O33 H33B 1_555 1_555 106(4) no
V1 N9 C18 1_555 1_555 123.40(10) no
V1 N9 C19 1_555 1_555 114.75(8) no
C18 N9 C19 1_555 1_555 121.10(10) no
V1 N10 C22 1_555 1_555 117.64(8) no
V1 N10 C25 1_555 1_555 122.10(10) no
C22 N10 C25 1_555 1_555 120.20(10) no
O3 C11 C12 1_555 1_555 119.90(10) no
O3 C11 C17 1_555 1_555 121.70(10) no
C12 C11 C17 1_555 1_555 118.40(10) no
C11 C12 C13 1_555 1_555 123.00(10) no
C11 C12 C14 1_555 1_555 119.90(10) no
C13 C12 C14 1_555 1_555 117.00(10) no
O5 C13 O6 1_555 1_555 120.1(2) no
O5 C13 C12 1_555 1_555 122.20(10) no
O6 C13 C12 1_555 1_555 117.70(10) no
C12 C14 C15 1_555 1_555 121.50(10) no
C12 C14 H14 1_555 1_555 121.0(10) no
C15 C14 H14 1_555 1_555 118.0(10) no
C14 C15 C16 1_555 1_555 118.90(10) no
C14 C15 H15 1_555 1_555 119(2) no
C16 C15 H15 1_555 1_555 122(2) no
C15 C16 C17 1_555 1_555 121.9(2) no
C15 C16 H16 1_555 1_555 122.0(10) no
C17 C16 H16 1_555 1_555 116.0(10) no
C11 C17 C16 1_555 1_555 119.50(10) no
C11 C17 C18 1_555 1_555 123.80(10) no
C16 C17 C18 1_555 1_555 116.80(10) no
N9 C18 C17 1_555 1_555 126.40(10) no
N9 C18 H18 1_555 1_555 119.0(10) no
C17 C18 H18 1_555 1_555 115.0(10) no
N9 C19 C20 1_555 1_555 106.70(10) no
N9 C19 C21 1_555 1_555 112.70(10) no
N9 C19 C22 1_555 1_555 104.80(10) no
C20 C19 C21 1_555 1_555 108.9(2) no
C20 C19 C22 1_555 1_555 112.00(10) no
C21 C19 C22 1_555 1_555 111.60(10) no
C19 C20 H20A 1_555 1_555 112(2) no
C19 C20 H20B 1_555 1_555 113(2) no
C19 C20 H20C 1_555 1_555 113(2) no
H20A C20 H20B 1_555 1_555 108(2) no
H20A C20 H20C 1_555 1_555 107(2) no
H20B C20 H20C 1_555 1_555 104(2) no
C19 C21 H21A 1_555 1_555 115(2) no
C19 C21 H21B 1_555 1_555 106(2) no
C19 C21 H21C 1_555 1_555 107(2) no
H21A C21 H21B 1_555 1_555 109(2) no
H21A C21 H21C 1_555 1_555 110(2) no
H21B C21 H21C 1_555 1_555 110(2) no
N10 C22 C19 1_555 1_555 105.50(10) no
N10 C22 C23 1_555 1_555 112.20(10) no
N10 C22 C24 1_555 1_555 106.10(10) no
C19 C22 C23 1_555 1_555 111.6(2) no
C19 C22 C24 1_555 1_555 111.10(10) no
C23 C22 C24 1_555 1_555 110.2(2) no
C22 C23 H23A 1_555 1_555 110(2) no
C22 C23 H23B 1_555 1_555 110(2) no
C22 C23 H23C 1_555 1_555 113(2) no
H23A C23 H23B 1_555 1_555 109(2) no
H23A C23 H23C 1_555 1_555 106(3) no
H23B C23 H23C 1_555 1_555 109(2) no
C22 C24 H24A 1_555 1_555 111(2) no
C22 C24 H24B 1_555 1_555 111(2) no
C22 C24 H24C 1_555 1_555 111(2) no
H24A C24 H24B 1_555 1_555 106(2) no
H24A C24 H24C 1_555 1_555 107(2) no
H24B C24 H24C 1_555 1_555 111(3) no
N10 C25 C26 1_555 1_555 125.40(10) no
N10 C25 H25 1_555 1_555 120.0(10) no
C26 C25 H25 1_555 1_555 113.0(10) no
C25 C26 C27 1_555 1_555 117.20(10) no
C25 C26 C32 1_555 1_555 122.80(10) no
C27 C26 C32 1_555 1_555 119.80(10) no
C26 C27 C28 1_555 1_555 121.6(2) no
C26 C27 H27 1_555 1_555 118(2) no
C28 C27 H27 1_555 1_555 120(2) no
C27 C28 C29 1_555 1_555 118.90(10) no
C27 C28 H28 1_555 1_555 123(2) no
C29 C28 H28 1_555 1_555 118(2) no
C28 C29 C30 1_555 1_555 121.3(2) no
C28 C29 H29 1_555 1_555 121(2) no
C30 C29 H29 1_555 1_555 117(2) no
C29 C30 C31 1_555 1_555 117.7(2) no
C29 C30 C32 1_555 1_555 120.0(2) no
C31 C30 C32 1_555 1_555 122.30(10) no
O7 C31 O8 1_555 1_555 119.8(2) no
O7 C31 C30 1_555 1_555 122.40(10) no
O8 C31 C30 1_555 1_555 117.8(2) no
O4 C32 C26 1_555 1_555 121.80(10) no
O4 C32 C30 1_555 1_555 119.90(10) no
C26 C32 C30 1_555 1_555 118.30(10) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O2 . . 1.588(2) yes
V1 O3 . . 1.9520(10) yes
V1 O4 . . 1.9500(10) yes
V1 N9 . . 2.0610(10) yes
V1 N10 . . 2.0470(10) yes
O3 C11 . . 1.335(2) no
O4 C32 . . 1.334(2) no
O5 C13 . . 1.210(2) no
O6 C13 . . 1.324(2) no
O6 H6 . . .77(4) no
O7 C31 . . 1.213(3) no
O8 C31 . . 1.317(2) no
O8 H8 . . .91(4) no
O33 H33A . . .76(4) no
O33 H33B . . .81(4) no
N9 C18 . . 1.284(2) no
N9 C19 . . 1.503(2) no
N10 C22 . . 1.504(2) no
N10 C25 . . 1.289(2) no
C11 C12 . . 1.416(2) no
C11 C17 . . 1.415(2) no
C12 C13 . . 1.490(2) no
C12 C14 . . 1.393(2) no
C14 C15 . . 1.387(3) no
C14 H14 . . .91(2) no
C15 C16 . . 1.375(2) no
C15 H15 . . .96(2) no
C16 C17 . . 1.402(2) no
C16 H16 . . .92(3) no
C17 C18 . . 1.449(2) no
C18 H18 . . .89(2) no
C19 C20 . . 1.532(3) no
C19 C21 . . 1.531(2) no
C19 C22 . . 1.558(2) no
C20 H20A . . 1.00(2) no
C20 H20B . . .88(3) no
C20 H20C . . .96(3) no
C21 H21A . . .92(3) no
C21 H21B . . 1.02(3) no
C21 H21C . . .99(3) no
C22 C23 . . 1.534(3) no
C22 C24 . . 1.532(3) no
C23 H23A . . .93(3) no
C23 H23B . . .86(2) no
C23 H23C . . .97(3) no
C24 H24A . . .97(3) no
C24 H24B . . .90(3) no
C24 H24C . . 1.04(3) no
C25 C26 . . 1.449(2) no
C25 H25 . . .94(2) no
C26 C27 . . 1.401(2) no
C26 C32 . . 1.412(2) no
C27 C28 . . 1.375(3) no
C27 H27 . . .83(3) no
C28 C29 . . 1.388(3) no
C28 H28 . . .96(2) no
C29 C30 . . 1.393(2) no
C29 H29 . . .86(3) no
C30 C31 . . 1.485(3) no
C30 C32 . . 1.412(2) no
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 H6 O3 . .77(4) 1.87(4) 2.569(2) 152(3)
O8 H8 O4 1_555 .91(4) 1.68(4) 2.535(2) 154(3)
O33 H33A O5 1_455 .76(4) 2.11(4) 2.886(3) 167(3)
O33 H33B O7 2_756 .81(4) 2.08(4) 2.888(3) 175(4)
