#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:54:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179905 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/01/7020155.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_7020155
loop_
_publ_author_name
'Sartzi, Harikleia'
'Stoumpos, Constantinos C.'
'Giouli, Maria'
'Verginadis, Ioannis I.'
'Karkabounas, Spyridon Ch'
'Cunha-Silva, Luís'
'Escuer, Albert'
'Perlepes, Spyros P.'
_publ_section_title
;
 The "periodic table" of di-2-pyridyl ketone: vanadium
 complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11984
_journal_page_last               11988
_journal_paper_doi               10.1039/c2dt30710c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C24 H24 N4 O14 S2 V2, 2(C H4 O)'
_chemical_formula_sum            'C26 H32 N4 O16 S2 V2'
_chemical_formula_weight         822.56
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '23 May 2012'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                114.327(2)
_cell_angle_beta                 103.206(3)
_cell_angle_gamma                95.776(3)
_cell_formula_units_Z            1
_cell_length_a                   8.5309(8)
_cell_length_b                   9.6061(4)
_cell_length_c                   11.6078(5)
_cell_measurement_reflns_used    3397
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.06
_cell_volume                     823.27(9)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_molecular_graphics    'SHELXTL '
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXTL '
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi scans'
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_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            10352
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.9127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2762
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0458
_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)+(0.0363P)²+1.4254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                2148
_reflns_number_total             2762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30710c.txt
_cod_data_source_block           CS769E
_cod_database_code               7020155
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
V1 V 0.12661(8) 0.15972(7) 0.40956(6) 0.01437(19) Uani 1 1 d .
S1 S 0.18470(12) 0.11911(10) 0.67690(9) 0.0157(2) Uani 1 1 d .
O1 O -0.0965(3) 0.0204(3) 0.3169(3) 0.0196(6) Uani 1 1 d .
O2 O 0.0864(3) 0.3242(3) 0.4892(3) 0.0206(6) Uani 1 1 d .
O3 O 0.1790(3) 0.0687(3) 0.5348(3) 0.0179(6) Uani 1 1 d .
O4 O 0.1022(3) 0.2472(3) 0.7212(3) 0.0217(6) Uani 1 1 d .
O5 O 0.3547(3) 0.1581(3) 0.7575(3) 0.0222(6) Uani 1 1 d .
O6 O 0.2287(3) -0.0314(3) 0.2730(3) 0.0178(6) Uani 1 1 d .
O7 O 0.4145(3) -0.0336(3) 0.1490(3) 0.0218(6) Uani 1 1 d D
H5 H 0.502(3) -0.062(5) 0.185(4) 0.033 Uiso 1 1 d D
N1 N 0.3835(4) 0.2503(3) 0.4595(3) 0.0155(7) Uani 1 1 d .
N2 N 0.1136(4) 0.1849(3) 0.2341(3) 0.0154(7) Uani 1 1 d .
C1 C 0.4727(5) 0.3692(4) 0.5768(4) 0.0180(8) Uani 1 1 d .
H1 H 0.4201 0.4151 0.6429 0.022 Uiso 1 1 calc R
C2 C 0.6380(5) 0.4258(4) 0.6035(4) 0.0216(9) Uani 1 1 d .
H2 H 0.6993 0.5086 0.6877 0.026 Uiso 1 1 calc R
C3 C 0.7143(5) 0.3614(4) 0.5069(4) 0.0245(10) Uani 1 1 d .
H3 H 0.8283 0.3998 0.5235 0.029 Uiso 1 1 calc R
C4 C 0.6230(5) 0.2405(5) 0.3861(4) 0.0219(9) Uani 1 1 d .
H4 H 0.6727 0.1951 0.3179 0.026 Uiso 1 1 calc R
C5 C 0.4590(5) 0.1866(4) 0.3659(4) 0.0181(9) Uani 1 1 d .
C6 C 0.3411(5) 0.0569(4) 0.2362(4) 0.0181(9) Uani 1 1 d .
C7 C 0.2234(5) 0.1298(4) 0.1703(4) 0.0172(9) Uani 1 1 d .
C8 C 0.2276(5) 0.1426(5) 0.0568(4) 0.0244(10) Uani 1 1 d .
H8 H 0.3066 0.1034 0.0131 0.029 Uiso 1 1 calc R
C9 C 0.1155(6) 0.2131(5) 0.0081(4) 0.0285(10) Uani 1 1 d .
H9 H 0.1160 0.2228 -0.0701 0.034 Uiso 1 1 calc R
C10 C 0.0025(5) 0.2697(5) 0.0732(4) 0.0267(10) Uani 1 1 d .
H10 H -0.0753 0.3191 0.0409 0.032 Uiso 1 1 calc R
C11 C 0.0041(5) 0.2535(4) 0.1862(4) 0.0212(9) Uani 1 1 d .
H11 H -0.0741 0.2917 0.2312 0.025 Uiso 1 1 calc R
C12 C 0.2943(5) -0.1445(5) 0.3101(4) 0.0270(10) Uani 1 1 d .
H12A H 0.3171 -0.2251 0.2342 0.041 Uiso 1 1 calc R
H12B H 0.2136 -0.1935 0.3379 0.041 Uiso 1 1 calc R
H12C H 0.3967 -0.0920 0.3835 0.041 Uiso 1 1 calc R
C13 C 0.3849(7) 0.5789(6) 0.9063(5) 0.0546(15) Uani 1 1 d .
H13A H 0.4366 0.6908 0.9555 0.082 Uiso 1 1 calc R
H13B H 0.4695 0.5187 0.8860 0.082 Uiso 1 1 calc R
H13C H 0.3303 0.5471 0.9600 0.082 Uiso 1 1 calc R
O8 O 0.2672(4) 0.5502(4) 0.7874(4) 0.0423(9) Uani 1 1 d D
H6 H 0.201(6) 0.457(3) 0.764(5) 0.064 Uiso 1 1 d D
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'
S S 0.1246 0.1234 '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
O2 V1 O3 106.40(13) . .
O2 V1 O1 102.34(13) . .
O3 V1 O1 92.83(11) . .
O2 V1 N1 94.83(13) . .
O3 V1 N1 88.44(11) . .
O1 V1 N1 161.64(11) . .
O2 V1 N2 95.75(13) . .
O3 V1 N2 157.19(11) . .
O1 V1 N2 87.57(11) . .
N1 V1 N2 84.28(12) . .
O2 V1 O6 162.12(11) . .
O3 V1 O6 86.84(10) . .
O1 V1 O6 88.64(10) . .
N1 V1 O6 73.14(10) . .
N2 V1 O6 70.37(10) . .
O4 S1 O5 112.59(16) . .
O4 S1 O3 110.46(15) . .
O5 S1 O3 109.43(15) . .
O4 S1 O1 109.75(15) . 2_556
O5 S1 O1 107.60(15) . 2_556
O3 S1 O1 106.80(15) . 2_556
S1 O1 V1 134.21(17) 2_556 .
S1 O3 V1 134.95(16) . .
C12 O6 C6 115.0(3) . .
C12 O6 V1 121.8(2) . .
C6 O6 V1 102.49(19) . .
C6 O7 H5 115(3) . .
C1 N1 C5 118.7(3) . .
C1 N1 V1 123.8(2) . .
C5 N1 V1 117.5(3) . .
C7 N2 C11 119.3(3) . .
C7 N2 V1 117.0(3) . .
C11 N2 V1 123.7(3) . .
N1 C1 C2 121.7(4) . .
N1 C1 H1 119.2 . .
C2 C1 H1 119.2 . .
C1 C2 C3 119.4(4) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C4 C3 C2 119.2(4) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C5 C4 C3 118.9(4) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 122.2(4) . .
N1 C5 C6 112.9(3) . .
C4 C5 C6 124.8(3) . .
O7 C6 O6 114.0(3) . .
O7 C6 C7 109.8(3) . .
O6 C6 C7 101.3(3) . .
O7 C6 C5 115.4(3) . .
O6 C6 C5 106.5(3) . .
C7 C6 C5 108.9(3) . .
N2 C7 C8 121.7(4) . .
N2 C7 C6 113.7(3) . .
C8 C7 C6 124.5(3) . .
C9 C8 C7 118.8(4) . .
C9 C8 H8 120.6 . .
C7 C8 H8 120.6 . .
C8 C9 C10 119.6(4) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C9 C10 C11 118.9(4) . .
C9 C10 H10 120.5 . .
C11 C10 H10 120.5 . .
N2 C11 C10 121.5(4) . .
N2 C11 H11 119.2 . .
C10 C11 H11 119.2 . .
O6 C12 H12A 109.5 . .
O6 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
O6 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O8 C13 H13A 109.5 . .
O8 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
O8 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C13 O8 H6 104(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.587(3) .
V1 O3 1.977(2) .
V1 O1 1.984(3) .
V1 N1 2.125(3) .
V1 N2 2.128(3) .
V1 O6 2.280(3) .
S1 O4 1.446(3) .
S1 O5 1.450(3) .
S1 O3 1.502(3) .
S1 O1 1.506(2) 2_556
O1 S1 1.506(2) 2_556
O6 C12 1.442(4) .
O6 C6 1.463(4) .
O7 C6 1.359(4) .
O7 H5 0.895(10) .
N1 C1 1.344(5) .
N1 C5 1.349(5) .
N2 C7 1.342(5) .
N2 C11 1.343(5) .
C1 C2 1.374(5) .
C1 H1 0.9500 .
C2 C3 1.381(6) .
C2 H2 0.9500 .
C3 C4 1.378(6) .
C3 H3 0.9500 .
C4 C5 1.373(5) .
C4 H4 0.9500 .
C5 C6 1.530(6) .
C6 C7 1.523(5) .
C7 C8 1.380(5) .
C8 C9 1.376(6) .
C8 H8 0.9500 .
C9 C10 1.377(6) .
C9 H9 0.9500 .
C10 C11 1.381(6) .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 O8 1.410(6) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
O8 H6 0.906(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H5 O5 0.895(10) 1.774(14) 2.655(4) 168(4) 2_656
O8 H6 O4 0.906(10) 1.916(16) 2.808(4) 168(5) .
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_4
O2 V1 O1 S1 -116.1(2) . 2_556
O3 V1 O1 S1 -8.6(2) . 2_556
N1 V1 O1 S1 85.0(4) . 2_556
N2 V1 O1 S1 148.6(2) . 2_556
O6 V1 O1 S1 78.2(2) . 2_556
O4 S1 O3 V1 14.5(3) . .
O5 S1 O3 V1 -110.0(2) . .
O1 S1 O3 V1 133.8(2) 2_556 .
O2 V1 O3 S1 1.2(3) . .
O1 V1 O3 S1 -102.6(2) . .
N1 V1 O3 S1 95.8(2) . .
N2 V1 O3 S1 167.0(2) . .
O6 V1 O3 S1 169.0(2) . .
O2 V1 O6 C12 137.7(4) . .
O3 V1 O6 C12 -0.9(3) . .
O1 V1 O6 C12 -93.8(3) . .
N1 V1 O6 C12 88.4(3) . .
N2 V1 O6 C12 178.3(3) . .
O2 V1 O6 C6 7.4(5) . .
O3 V1 O6 C6 -131.2(2) . .
O1 V1 O6 C6 135.9(2) . .
N1 V1 O6 C6 -41.9(2) . .
N2 V1 O6 C6 48.0(2) . .
O2 V1 N1 C1 35.1(3) . .
O3 V1 N1 C1 -71.2(3) . .
O1 V1 N1 C1 -165.5(3) . .
N2 V1 N1 C1 130.5(3) . .
O6 V1 N1 C1 -158.4(3) . .
O2 V1 N1 C5 -143.0(3) . .
O3 V1 N1 C5 110.6(3) . .
O1 V1 N1 C5 16.4(5) . .
N2 V1 N1 C5 -47.7(3) . .
O6 V1 N1 C5 23.5(2) . .
O2 V1 N2 C7 141.8(3) . .
O3 V1 N2 C7 -24.5(5) . .
O1 V1 N2 C7 -116.0(3) . .
N1 V1 N2 C7 47.5(3) . .
O6 V1 N2 C7 -26.6(2) . .
O2 V1 N2 C11 -37.4(3) . .
O3 V1 N2 C11 156.2(3) . .
O1 V1 N2 C11 64.7(3) . .
N1 V1 N2 C11 -131.7(3) . .
O6 V1 N2 C11 154.1(3) . .
C5 N1 C1 C2 -0.5(5) . .
V1 N1 C1 C2 -178.7(3) . .
N1 C1 C2 C3 1.2(6) . .
C1 C2 C3 C4 -0.6(6) . .
C2 C3 C4 C5 -0.7(6) . .
C1 N1 C5 C4 -0.8(5) . .
V1 N1 C5 C4 177.4(3) . .
C1 N1 C5 C6 -177.9(3) . .
V1 N1 C5 C6 0.3(4) . .
C3 C4 C5 N1 1.4(6) . .
C3 C4 C5 C6 178.2(3) . .
C12 O6 C6 O7 48.1(4) . .
V1 O6 C6 O7 -177.6(3) . .
C12 O6 C6 C7 165.9(3) . .
V1 O6 C6 C7 -59.8(3) . .
C12 O6 C6 C5 -80.3(4) . .
V1 O6 C6 C5 54.0(3) . .
N1 C5 C6 O7 -166.5(3) . .
C4 C5 C6 O7 16.4(5) . .
N1 C5 C6 O6 -38.9(4) . .
C4 C5 C6 O6 144.0(3) . .
N1 C5 C6 C7 69.5(4) . .
C4 C5 C6 C7 -107.5(4) . .
C11 N2 C7 C8 0.4(5) . .
V1 N2 C7 C8 -178.9(3) . .
C11 N2 C7 C6 179.3(3) . .
V1 N2 C7 C6 0.0(4) . .
O7 C6 C7 N2 162.8(3) . .
O6 C6 C7 N2 42.0(4) . .
C5 C6 C7 N2 -70.0(4) . .
O7 C6 C7 C8 -18.4(5) . .
O6 C6 C7 C8 -139.2(4) . .
C5 C6 C7 C8 108.9(4) . .
N2 C7 C8 C9 -0.3(6) . .
C6 C7 C8 C9 -179.1(4) . .
C7 C8 C9 C10 0.3(6) . .
C8 C9 C10 C11 -0.3(6) . .
C7 N2 C11 C10 -0.5(6) . .
V1 N2 C11 C10 178.8(3) . .
C9 C10 C11 N2 0.4(6) . .
