#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004736.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7004736
loop_
_publ_author_name
'Davis, Martin F.'
'Jura, Marek'
'Leung, Alethea'
'Levason, William'
'Littlefield, Benjamin'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Synthesis, chemistry and structures of complexes of the
 dioxovanadium(v) halides VO2F and VO2Cl
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6265
_journal_page_last               6273
_journal_paper_doi               10.1039/b811422f
_journal_year                    2008
_chemical_formula_moiety         'C10 H10 Cl N2 O2 V'
_chemical_formula_sum            'C10 H10 Cl N2 O2 V'
_chemical_formula_weight         276.59
_chemical_name_common            chlorodioxobis(pyridine)vanadium(V)
_chemical_name_systematic
;
chlorodioxobis(pyridine)vanadium(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2008-04-19
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.454(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9806(10)
_cell_length_b                   7.3517(10)
_cell_length_c                   25.960(4)
_cell_measurement_reflns_used    11795
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1139.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_sigmaI/netI    0.0908
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15379
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0250P)²+1.1901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                1770
_reflns_number_total             2615
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b811422f.txt
_cod_data_source_block           08mj21
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7004736
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_type_symbol
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.77180(10) 0.15702(8) 0.12554(2) 0.02104(18) Uani 1 1 d . . .
Cl1 Cl 0.94730(16) 0.43757(11) 0.11880(3) 0.0279(2) Uani 1 1 d . . .
O1 O 0.8957(4) -0.0302(3) 0.11065(9) 0.0294(6) Uani 1 1 d . . .
O2 O 0.5253(4) 0.1145(4) 0.14492(9) 0.0328(6) Uani 1 1 d . . .
N1 N 0.6377(5) 0.2112(4) 0.04899(10) 0.0217(6) Uani 1 1 d . . .
N2 N 0.9130(4) 0.1556(4) 0.20335(10) 0.0205(6) Uani 1 1 d . . .
C1 C 0.4290(6) 0.2753(5) 0.03980(13) 0.0251(8) Uani 1 1 d . . .
H1 H 0.3394 0.2983 0.0681 0.030 Uiso 1 1 calc R . .
C2 C 0.3410(6) 0.3089(5) -0.00975(13) 0.0274(8) Uani 1 1 d . . .
H2 H 0.1935 0.3558 -0.0153 0.033 Uiso 1 1 calc R . .
C3 C 0.4688(6) 0.2737(5) -0.05110(14) 0.0290(9) Uani 1 1 d . . .
H3 H 0.4098 0.2942 -0.0854 0.035 Uiso 1 1 calc R . .
C4 C 0.6829(7) 0.2086(5) -0.04189(13) 0.0309(9) Uani 1 1 d . . .
H4 H 0.7747 0.1844 -0.0697 0.037 Uiso 1 1 calc R . .
C5 C 0.7620(6) 0.1791(5) 0.00843(12) 0.0258(8) Uani 1 1 d . . .
H5 H 0.9102 0.1343 0.0147 0.031 Uiso 1 1 calc R . .
C6 C 0.7972(6) 0.2217(5) 0.24199(12) 0.0237(8) Uani 1 1 d . . .
H6 H 0.6542 0.2742 0.2340 0.028 Uiso 1 1 calc R . .
C7 C 0.8787(6) 0.2162(5) 0.29297(13) 0.0260(8) Uani 1 1 d . . .
H7 H 0.7932 0.2644 0.3195 0.031 Uiso 1 1 calc R . .
C8 C 1.0869(6) 0.1394(5) 0.30477(13) 0.0280(8) Uani 1 1 d . . .
H8 H 1.1462 0.1335 0.3395 0.034 Uiso 1 1 calc R . .
C9 C 1.2068(6) 0.0716(5) 0.26525(13) 0.0266(8) Uani 1 1 d . . .
H9 H 1.3499 0.0182 0.2724 0.032 Uiso 1 1 calc R . .
C10 C 1.1155(6) 0.0827(5) 0.21506(13) 0.0244(8) Uani 1 1 d . . .
H10 H 1.1992 0.0369 0.1879 0.029 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O1 110.40(14) . . ?
O2 V1 N1 91.56(12) . . ?
O1 V1 N1 95.06(11) . . ?
O2 V1 N2 91.18(11) . . ?
O1 V1 N2 93.48(11) . . ?
N1 V1 N2 169.50(11) . . ?
O2 V1 Cl1 128.26(11) . . ?
O1 V1 Cl1 121.34(10) . . ?
N1 V1 Cl1 84.86(8) . . ?
N2 V1 Cl1 85.48(8) . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 V1 121.6(2) . . ?
C5 N1 V1 120.0(2) . . ?
C10 N2 C6 118.3(3) . . ?
C10 N2 V1 121.0(2) . . ?
C6 N2 V1 120.7(2) . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
N2 C6 C7 122.4(3) . . ?
N2 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C6 C7 C8 118.9(3) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C9 C8 C7 118.9(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 122.4(3) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.617(2) . ?
V1 O1 1.621(2) . ?
V1 N1 2.135(3) . ?
V1 N2 2.142(3) . ?
V1 Cl1 2.3256(10) . ?
N1 C1 1.342(4) . ?
N1 C5 1.346(4) . ?
N2 C10 1.342(4) . ?
N2 C6 1.344(4) . ?
C1 C2 1.382(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.383(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 N1 C1 28.7(3) . . . . ?
O1 V1 N1 C1 139.3(3) . . . . ?
N2 V1 N1 C1 -76.4(7) . . . . ?
Cl1 V1 N1 C1 -99.6(3) . . . . ?
O2 V1 N1 C5 -150.5(3) . . . . ?
O1 V1 N1 C5 -39.9(3) . . . . ?
N2 V1 N1 C5 104.4(6) . . . . ?
Cl1 V1 N1 C5 81.2(2) . . . . ?
O2 V1 N2 C10 141.3(3) . . . . ?
O1 V1 N2 C10 30.7(3) . . . . ?
N1 V1 N2 C10 -113.6(6) . . . . ?
Cl1 V1 N2 C10 -90.5(2) . . . . ?
O2 V1 N2 C6 -36.2(3) . . . . ?
O1 V1 N2 C6 -146.8(3) . . . . ?
N1 V1 N2 C6 68.9(7) . . . . ?
Cl1 V1 N2 C6 92.0(3) . . . . ?
C5 N1 C1 C2 -0.2(5) . . . . ?
V1 N1 C1 C2 -179.4(3) . . . . ?
N1 C1 C2 C3 0.8(5) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
C1 N1 C5 C4 -0.3(5) . . . . ?
V1 N1 C5 C4 178.9(3) . . . . ?
C3 C4 C5 N1 0.1(5) . . . . ?
C10 N2 C6 C7 -0.4(5) . . . . ?
V1 N2 C6 C7 177.2(3) . . . . ?
N2 C6 C7 C8 -0.2(5) . . . . ?
C6 C7 C8 C9 0.3(5) . . . . ?
C7 C8 C9 C10 0.1(5) . . . . ?
C6 N2 C10 C9 0.8(5) . . . . ?
V1 N2 C10 C9 -176.8(3) . . . . ?
C8 C9 C10 N2 -0.6(5) . . . . ?
