#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2009009.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_2009009
loop_
_publ_author_name
'Lutz, M.'
'Hagen, H.'
'Schreurs, A. M. M.'
'Spek, A. L.'
'van Koten, G.'
_publ_section_title
;
 The twinned structure of the
 \m-isopropoxidodiisopropoxido(<i>p</i>-tolylimido)vanadium(V) dimer,
 twin refinement against CCD area-detector data
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1636
_journal_page_last               1639
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[V2 (C7 H7 N)2 (C3 H7 O)6]'
_chemical_formula_moiety         'C32 H56 N2 O6 V2'
_chemical_formula_sum            'C32 H56 N2 O6 V2'
_chemical_formula_weight         666.67
_chemical_melting_point          316
_chemical_name_systematic
;
bis((\m^2^-Isopropoxo)-di-isopropoxy-4-Methylphenylimido-vanadium(v))
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.297(4)
_cell_angle_beta                 71.869(4)
_cell_angle_gamma                61.3013(18)
_cell_formula_units_Z            1
_cell_length_a                   9.7491(6)
_cell_length_b                   10.0291(6)
_cell_length_c                   11.1681(5)
_cell_measurement_temperature    150(2)
_cell_volume                     907.28(9)
_computing_cell_refinement       'see above'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'see above'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.015
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18748
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         18748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.070
_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/[\s^2^(Fo^2^)+(0.0378P)^2^+3.2555P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.174
_reflns_number_gt                16570
_reflns_number_total             18748
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    fg1541.cif
_[local]_cod_data_source_block   s2004a
_cod_database_code               2009009
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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
V 0.09634(4) 0.40966(4) 0.35830(3) 0.01771(11) Uani d . 1 V
O1 0.11886(17) 0.56053(16) 0.26980(13) 0.0233(3) Uani d . 1 O
O2 0.12243(15) 0.39492(15) 0.51737(12) 0.0188(3) Uani d . 1 O
O3 -0.06219(16) 0.37786(16) 0.33799(13) 0.0237(3) Uani d . 1 O
N1 0.2636(2) 0.25189(19) 0.27968(15) 0.0213(4) Uani d . 1 N
C1 0.3978(2) 0.1152(2) 0.21911(18) 0.0204(4) Uani d . 1 C
C2 0.5397(3) 0.1119(3) 0.1341(2) 0.0289(5) Uani d . 1 C
H2 0.5437 0.2044 0.1157 0.035 Uiso calc R 1 H
C3 0.6746(3) -0.0258(3) 0.0768(2) 0.0314(5) Uani d . 1 C
H3 0.7699 -0.0257 0.0197 0.038 Uiso calc R 1 H
C4 0.6744(3) -0.1627(2) 0.10027(19) 0.0264(5) Uani d . 1 C
C5 0.5327(3) -0.1592(3) 0.1835(2) 0.0294(5) Uani d . 1 C
H5 0.5294 -0.2521 0.2007 0.035 Uiso calc R 1 H
C6 0.3964(3) -0.0236(2) 0.2420(2) 0.0257(5) Uani d . 1 C
H6 0.3010 -0.0246 0.2981 0.031 Uiso calc R 1 H
C7 0.8214(3) -0.3134(3) 0.0396(2) 0.0378(6) Uani d . 1 C
H7A 0.9108 -0.2958 -0.0147 0.057 Uiso calc R 1 H
H7B 0.7907 -0.3633 -0.0114 0.057 Uiso calc R 1 H
H7C 0.8581 -0.3789 0.1055 0.057 Uiso calc R 1 H
C8 0.2469(3) 0.5673(3) 0.1709(2) 0.0267(5) Uani d . 1 C
H8 0.2864 0.4885 0.1013 0.032 Uiso calc R 1 H
C9 0.3888(3) 0.5357(3) 0.2173(2) 0.0379(6) Uani d . 1 C
H9A 0.4320 0.4333 0.2471 0.057 Uiso calc R 1 H
H9B 0.3506 0.6112 0.2868 0.057 Uiso calc R 1 H
H9C 0.4759 0.5423 0.1479 0.057 Uiso calc R 1 H
C10 0.1786(3) 0.7236(3) 0.1213(3) 0.0490(7) Uani d . 1 C
H10A 0.0872 0.7407 0.0915 0.073 Uiso calc R 1 H
H10B 0.2652 0.7295 0.0511 0.073 Uiso calc R 1 H
H10C 0.1389 0.8016 0.1891 0.073 Uiso calc R 1 H
C11 0.2491(2) 0.2926(2) 0.57076(19) 0.0211(5) Uani d . 1 C
H11 0.2156 0.3349 0.6593 0.025 Uiso calc R 1 H
C12 0.4109(3) 0.2897(3) 0.5006(2) 0.0292(5) Uani d . 1 C
H12A 0.3950 0.3939 0.4992 0.044 Uiso calc R 1 H
H12B 0.4499 0.2456 0.4137 0.044 Uiso calc R 1 H
H12C 0.4924 0.2277 0.5434 0.044 Uiso calc R 1 H
C13 0.2592(3) 0.1368(3) 0.5789(2) 0.0297(5) Uani d . 1 C
H13A 0.1505 0.1476 0.6252 0.044 Uiso calc R 1 H
H13B 0.3378 0.0723 0.6234 0.044 Uiso calc R 1 H
H13C 0.2959 0.0898 0.4935 0.044 Uiso calc R 1 H
C14 -0.0588(3) 0.2464(3) 0.2957(2) 0.0275(5) Uani d . 1 C
H14 0.0495 0.1835 0.2305 0.033 Uiso calc R 1 H
C15 -0.1956(3) 0.2983(3) 0.2372(3) 0.0435(7) Uani d . 1 C
H15A -0.1782 0.3581 0.1658 0.065 Uiso calc R 1 H
H15B -0.3017 0.3613 0.3006 0.065 Uiso calc R 1 H
H15C -0.1955 0.2090 0.2074 0.065 Uiso calc R 1 H
C16 -0.0804(4) 0.1542(3) 0.4066(3) 0.0470(7) Uani d . 1 C
H16A 0.0095 0.1231 0.4424 0.070 Uiso calc R 1 H
H16B -0.0789 0.0634 0.3784 0.070 Uiso calc R 1 H
H16C -0.1858 0.2162 0.4711 0.070 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
V 0.01317(19) 0.0163(2) 0.02222(19) -0.00647(14) -0.00504(14) 0.00303(13)
O1 0.0194(8) 0.0219(8) 0.0266(8) -0.0113(7) -0.0035(6) 0.0056(6)
O2 0.0133(7) 0.0167(8) 0.0208(7) -0.0024(6) -0.0070(6) 0.0036(5)
O3 0.0177(8) 0.0199(8) 0.0347(8) -0.0100(7) -0.0077(6) 0.0020(6)
N1 0.0171(9) 0.0208(10) 0.0232(9) -0.0080(8) -0.0046(7) 0.0020(7)
C1 0.0170(11) 0.0178(11) 0.0220(11) -0.0048(9) -0.0059(9) -0.0009(8)
C2 0.0231(12) 0.0217(13) 0.0347(13) -0.0100(10) -0.0010(10) 0.0025(10)
C3 0.0208(12) 0.0276(14) 0.0310(13) -0.0072(11) 0.0041(10) -0.0014(10)
C4 0.0242(12) 0.0230(13) 0.0249(11) -0.0058(10) -0.0061(9) -0.0049(9)
C5 0.0307(13) 0.0193(12) 0.0383(13) -0.0127(11) -0.0088(11) -0.0016(10)
C6 0.0217(12) 0.0222(13) 0.0298(12) -0.0110(10) -0.0027(9) 0.0000(9)
C7 0.0301(14) 0.0285(15) 0.0379(14) -0.0051(11) -0.0003(11) -0.0118(11)
C8 0.0271(12) 0.0309(13) 0.0246(12) -0.0199(11) -0.0011(10) 0.0026(9)
C9 0.0276(13) 0.0401(16) 0.0492(16) -0.0220(12) -0.0071(11) 0.0059(12)
C10 0.0472(17) 0.0563(19) 0.0531(17) -0.0346(15) -0.0185(14) 0.0326(14)
C11 0.0171(11) 0.0171(11) 0.0245(11) -0.0028(9) -0.0101(9) 0.0030(8)
C12 0.0190(12) 0.0273(13) 0.0397(14) -0.0070(10) -0.0153(10) 0.0081(10)
C13 0.0280(13) 0.0211(13) 0.0348(13) -0.0061(10) -0.0138(10) 0.0063(10)
C14 0.0240(12) 0.0261(13) 0.0366(13) -0.0143(10) -0.0109(10) 0.0019(10)
C15 0.0385(15) 0.0515(18) 0.0536(17) -0.0265(14) -0.0228(13) 0.0050(13)
C16 0.0605(19) 0.0440(17) 0.0584(17) -0.0381(15) -0.0288(15) 0.0212(13)
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_3
_geom_angle
_geom_angle_publ_flag
N1 V O3 . 100.17(7) yes
N1 V O1 . 103.29(7) yes
O3 V O1 . 113.52(7) yes
N1 V O2 . 101.31(7) yes
O3 V O2 . 118.48(6) yes
O1 V O2 . 116.22(6) yes
N1 V O2 2_566 173.38(7) yes
O3 V O2 2_566 80.79(6) yes
O1 V O2 2_566 82.14(6) yes
O2 V O2 2_566 72.67(6) yes
C8 O1 V . 134.38(13) no
C11 O2 V . 134.84(12) no
C11 O2 V 2_566 117.79(11) no
V O2 V 2_566 107.33(6) yes
C14 O3 V . 132.05(13) no
C1 N1 V . 176.18(16) no
N1 C1 C2 . 120.84(19) no
N1 C1 C6 . 121.20(19) no
C2 C1 C6 . 117.96(19) no
C3 C2 C1 . 120.3(2) no
C3 C2 H2 . 119.9 no
C1 C2 H2 . 119.9 no
C4 C3 C2 . 122.0(2) no
C4 C3 H3 . 119.0 no
C2 C3 H3 . 119.0 no
C3 C4 C5 . 117.71(19) no
C3 C4 C7 . 122.3(2) no
C5 C4 C7 . 120.0(2) no
C6 C5 C4 . 121.6(2) no
C6 C5 H5 . 119.2 no
C4 C5 H5 . 119.2 no
C5 C6 C1 . 120.5(2) no
C5 C6 H6 . 119.8 no
C1 C6 H6 . 119.8 no
C4 C7 H7A . 109.5 no
C4 C7 H7B . 109.5 no
H7A C7 H7B . 109.5 no
C4 C7 H7C . 109.5 no
H7A C7 H7C . 109.5 no
H7B C7 H7C . 109.5 no
O1 C8 C9 . 110.48(18) no
O1 C8 C10 . 108.36(19) no
C9 C8 C10 . 111.26(19) no
O1 C8 H8 . 108.9 no
C9 C8 H8 . 108.9 no
C10 C8 H8 . 108.9 no
C8 C9 H9A . 109.5 no
C8 C9 H9B . 109.5 no
H9A C9 H9B . 109.5 no
C8 C9 H9C . 109.5 no
H9A C9 H9C . 109.5 no
H9B C9 H9C . 109.5 no
C8 C10 H10A . 109.5 no
C8 C10 H10B . 109.5 no
H10A C10 H10B . 109.5 no
C8 C10 H10C . 109.5 no
H10A C10 H10C . 109.5 no
H10B C10 H10C . 109.5 no
O2 C11 C13 . 110.78(16) no
O2 C11 C12 . 110.71(16) no
C13 C11 C12 . 114.05(18) no
O2 C11 H11 . 107.0 no
C13 C11 H11 . 107.0 no
C12 C11 H11 . 107.0 no
C11 C12 H12A . 109.5 no
C11 C12 H12B . 109.5 no
H12A C12 H12B . 109.5 no
C11 C12 H12C . 109.5 no
H12A C12 H12C . 109.5 no
H12B C12 H12C . 109.5 no
C11 C13 H13A . 109.5 no
C11 C13 H13B . 109.5 no
H13A C13 H13B . 109.5 no
C11 C13 H13C . 109.5 no
H13A C13 H13C . 109.5 no
H13B C13 H13C . 109.5 no
O3 C14 C16 . 108.86(19) no
O3 C14 C15 . 108.18(19) no
C16 C14 C15 . 111.6(2) no
O3 C14 H14 . 109.4 no
C16 C14 H14 . 109.4 no
C15 C14 H14 . 109.4 no
C14 C15 H15A . 109.5 no
C14 C15 H15B . 109.5 no
H15A C15 H15B . 109.5 no
C14 C15 H15C . 109.5 no
H15A C15 H15C . 109.5 no
H15B C15 H15C . 109.5 no
C14 C16 H16A . 109.5 no
C14 C16 H16B . 109.5 no
H16A C16 H16B . 109.5 no
C14 C16 H16C . 109.5 no
H16A C16 H16C . 109.5 no
H16B C16 H16C . 109.5 no
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
V N1 . 1.6709(16) yes
V O3 . 1.8014(14) yes
V O1 . 1.8037(14) yes
V O2 . 1.8560(13) yes
V O2 2_566 2.2151(13) yes
O1 C8 . 1.412(2) no
O2 C11 . 1.440(2) no
O2 V 2_566 2.2151(13) no
O3 C14 . 1.419(2) no
N1 C1 . 1.389(2) yes
C1 C2 . 1.400(3) no
C1 C6 . 1.401(3) no
C2 C3 . 1.386(3) no
C2 H2 . 0.9500 no
C3 C4 . 1.378(3) no
C3 H3 . 0.9500 no
C4 C5 . 1.391(3) no
C4 C7 . 1.510(3) no
C5 C6 . 1.382(3) no
C5 H5 . 0.9500 no
C6 H6 . 0.9500 no
C7 H7A . 0.9800 no
C7 H7B . 0.9800 no
C7 H7C . 0.9800 no
C8 C9 . 1.510(3) no
C8 C10 . 1.513(3) no
C8 H8 . 1.0000 no
C9 H9A . 0.9800 no
C9 H9B . 0.9800 no
C9 H9C . 0.9800 no
C10 H10A . 0.9800 no
C10 H10B . 0.9800 no
C10 H10C . 0.9800 no
C11 C13 . 1.514(3) no
C11 C12 . 1.514(3) no
C11 H11 . 1.0000 no
C12 H12A . 0.9800 no
C12 H12B . 0.9800 no
C12 H12C . 0.9800 no
C13 H13A . 0.9800 no
C13 H13B . 0.9800 no
C13 H13C . 0.9800 no
C14 C16 . 1.507(3) no
C14 C15 . 1.516(3) no
C14 H14 . 1.0000 no
C15 H15A . 0.9800 no
C15 H15B . 0.9800 no
C15 H15C . 0.9800 no
C16 H16A . 0.9800 no
C16 H16B . 0.9800 no
C16 H16C . 0.9800 no
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_4
_geom_torsion
_geom_torsion_publ_flag
N1 V O1 C8 . . -9.7(2) no
O3 V O1 C8 . . -117.19(18) no
O2 V O1 C8 . . 100.25(18) no
O2 V O1 C8 2_566 . 166.48(19) no
N1 V O2 C11 . . 5.11(19) no
O3 V O2 C11 . . 113.38(17) no
O1 V O2 C11 . . -105.98(17) no
O2 V O2 C11 2_566 . -177.7(2) no
N1 V O2 V . 2_566 -177.16(8) no
O3 V O2 V . 2_566 -68.90(8) no
O1 V O2 V . 2_566 71.74(8) no
O2 V O2 V 2_566 2_566 0.0 no
N1 V O3 C14 . . 13.44(19) no
O1 V O3 C14 . . 122.88(17) no
O2 V O3 C14 . . -95.47(18) no
O2 V O3 C14 2_566 . -159.92(18) no
O3 V N1 C1 . . -52(2) no
O1 V N1 C1 . . -169(2) no
O2 V N1 C1 . . 70(2) no
O2 V N1 C1 2_566 . 46(3) no
V N1 C1 C2 . . -173(2) no
V N1 C1 C6 . . 6(2) no
N1 C1 C2 C3 . . 178.3(2) no
C6 C1 C2 C3 . . -1.0(3) no
C1 C2 C3 C4 . . 0.2(3) no
C2 C3 C4 C5 . . 0.5(3) no
C2 C3 C4 C7 . . -179.2(2) no
C3 C4 C5 C6 . . -0.4(3) no
C7 C4 C5 C6 . . 179.3(2) no
C4 C5 C6 C1 . . -0.4(3) no
N1 C1 C6 C5 . . -178.23(19) no
C2 C1 C6 C5 . . 1.1(3) no
V O1 C8 C9 . . -68.0(2) no
V O1 C8 C10 . . 169.85(16) no
V O2 C11 C13 . . -69.6(2) no
V O2 C11 C13 2_566 . 112.89(15) no
V O2 C11 C12 . . 58.0(2) no
V O2 C11 C12 2_566 . -119.56(15) no
V O3 C14 C16 . . 86.2(2) no
V O3 C14 C15 . . -152.40(16) no