#------------------------------------------------------------------------------
#$Date: 2023-04-27 18:28:39 +0300 (Thu, 27 Apr 2023) $
#$Revision: 282882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/16/7051675.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_7051675
loop_
_publ_author_name
'Gyepes, Róbert'
'Pacigová, Silvia'
'Sivák, Michal'
'Tatiersky, Jozef'
_publ_section_title
;
 Experimental and computational evidence of solid-state anion--π and
 π--π interactions in [VO(O2)(L)(pa)]·xH2O complexes (L =
 picolinate, pyrazinate or quinolinate; pa = picolinamide)
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1515
_journal_paper_doi               10.1039/b819875f
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C12 H10 N3 O6 V, H2 O'
_chemical_formula_sum            'C12 H12 N3 O7 V'
_chemical_formula_weight         361.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.255(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6180(4)
_cell_length_b                   12.4218(8)
_cell_length_c                   13.6060(7)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1411.69(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'ω and π scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11336
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.9349
_exptl_absorpt_correction_T_min  0.8902
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0404
_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/[σ²(Fo²)+(0.0320P)²+1.0604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                2389
_reflns_number_total             3244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B819875F.txt
_cod_data_source_block           voo2picpa1a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7051675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.27279(4) 0.21803(4) 0.63290(3) 0.02924(13) Uani 1 1 d . . .
O1 O 0.15237(19) 0.18761(16) 0.70080(12) 0.0394(5) Uani 1 1 d . . .
O2 O 0.47071(19) 0.17426(16) 0.71554(12) 0.0396(4) Uani 1 1 d . . .
O3 O 0.44019(19) 0.28424(16) 0.73081(12) 0.0388(4) Uani 1 1 d . . .
C1 C 0.1866(3) 0.0421(2) 0.48197(17) 0.0304(5) Uani 1 1 d . . .
N2 N 0.2945(2) 0.06382(16) 0.56974(14) 0.0293(5) Uani 1 1 d . . .
C3 C 0.4021(3) -0.0127(2) 0.60881(19) 0.0373(6) Uani 1 1 d . . .
H3 H 0.4773 0.0008 0.6714 0.045 Uiso 1 1 calc R . .
C4 C 0.4070(3) -0.1097(2) 0.5613(2) 0.0416(7) Uani 1 1 d . . .
H4 H 0.4864 -0.1614 0.5902 0.050 Uiso 1 1 calc R . .
C5 C 0.2961(3) -0.1319(2) 0.4715(2) 0.0414(6) Uani 1 1 d . . .
H5 H 0.2976 -0.1987 0.4377 0.050 Uiso 1 1 calc R . .
C6 C 0.1825(3) -0.0542(2) 0.43181(19) 0.0376(6) Uani 1 1 d . . .
H6 H 0.1031 -0.0673 0.3709 0.045 Uiso 1 1 calc R . .
C7 C 0.0733(3) 0.1331(2) 0.44439(17) 0.0306(6) Uani 1 1 d . . .
O8 O 0.09580(18) 0.21546(14) 0.50296(12) 0.0325(4) Uani 1 1 d . . .
O9 O -0.02976(19) 0.12501(16) 0.36427(12) 0.0388(4) Uani 1 1 d . . .
C11 C 0.2566(3) 0.4419(2) 0.54573(16) 0.0294(5) Uani 1 1 d . . .
N12 N 0.2064(2) 0.38346(17) 0.61592(14) 0.0308(5) Uani 1 1 d . . .
C13 C 0.1208(3) 0.4327(2) 0.67300(18) 0.0397(7) Uani 1 1 d . . .
H13 H 0.0825 0.3919 0.7212 0.048 Uiso 1 1 calc R . .
C14 C 0.0870(3) 0.5420(3) 0.66299(19) 0.0452(7) Uani 1 1 d . . .
H14 H 0.0247 0.5751 0.7032 0.054 Uiso 1 1 calc R . .
C15 C 0.1442(3) 0.6021(2) 0.59456(19) 0.0429(7) Uani 1 1 d . . .
H15 H 0.1262 0.6776 0.5893 0.052 Uiso 1 1 calc R . .
C16 C 0.2289(3) 0.5508(2) 0.53316(18) 0.0348(6) Uani 1 1 d . . .
H16 H 0.2666 0.5899 0.4837 0.042 Uiso 1 1 calc R . .
C17 C 0.3446(3) 0.3752(2) 0.48543(17) 0.0282(5) Uani 1 1 d . . .
O18 O 0.39157(18) 0.28402(14) 0.51859(12) 0.0306(4) Uani 1 1 d . . .
N19 N 0.3692(2) 0.41530(18) 0.40026(14) 0.0310(5) Uani 1 1 d . . .
H19A H 0.4179 0.3691 0.3629 0.057(9) Uiso 1 1 d R . .
H19B H 0.3369 0.4835 0.3731 0.052(9) Uiso 1 1 d R . .
O20 O 0.7161(3) 0.12262(17) 0.18833(14) 0.0399(5) Uani 1 1 d . . .
H20A H 0.785(4) 0.128(3) 0.241(2) 0.054(10) Uiso 1 1 d . . .
H20B H 0.643(4) 0.157(3) 0.198(2) 0.056(10) Uiso 1 1 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'
O O 0.0106 0.0060 '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'
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
O1 V1 O2 102.07(8) . . ?
O1 V1 O3 100.78(8) . . ?
O2 V1 O3 44.11(8) . . ?
O1 V1 O8 92.53(8) . . ?
O2 V1 O8 153.33(8) . . ?
O3 V1 O8 153.89(8) . . ?
O1 V1 N2 98.93(9) . . ?
O2 V1 N2 79.85(8) . . ?
O3 V1 N2 123.22(8) . . ?
O8 V1 N2 75.88(7) . . ?
O1 V1 N12 95.48(9) . . ?
O2 V1 N12 121.64(8) . . ?
O3 V1 N12 78.18(8) . . ?
O8 V1 N12 78.27(7) . . ?
N2 V1 N12 150.82(7) . . ?
O1 V1 O18 166.31(8) . . ?
O2 V1 O18 91.08(7) . . ?
O3 V1 O18 85.96(7) . . ?
O8 V1 O18 76.87(6) . . ?
N2 V1 O18 87.01(7) . . ?
N12 V1 O18 74.08(7) . . ?
O3 O2 V1 68.55(10) . . ?
O2 O3 V1 67.34(10) . . ?
N2 C1 C6 122.8(2) . . ?
N2 C1 C7 113.6(2) . . ?
C6 C1 C7 123.5(2) . . ?
C3 N2 C1 117.9(2) . . ?
C3 N2 V1 126.76(17) . . ?
C1 N2 V1 115.34(16) . . ?
N2 C3 C4 122.2(2) . . ?
N2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 118.3(3) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C1 C6 C5 118.9(2) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
O9 C7 O8 125.6(2) . . ?
O9 C7 C1 120.6(2) . . ?
O8 C7 C1 113.81(19) . . ?
C7 O8 V1 121.32(15) . . ?
N12 C11 C16 122.6(2) . . ?
N12 C11 C17 112.6(2) . . ?
C16 C11 C17 124.8(2) . . ?
C13 N12 C11 118.7(2) . . ?
C13 N12 V1 123.21(18) . . ?
C11 N12 V1 118.04(16) . . ?
N12 C13 C14 121.3(3) . . ?
N12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 119.0(3) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C11 C16 C15 118.4(3) . . ?
C11 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
O18 C17 N19 123.3(2) . . ?
O18 C17 C11 117.8(2) . . ?
N19 C17 C11 118.9(2) . . ?
C17 O18 V1 115.06(14) . . ?
C17 N19 H19A 115.8 . . ?
C17 N19 H19B 126.0 . . ?
H19A N19 H19B 118.1 . . ?
H20A O20 H20B 105(3) . . ?
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 O1 1.5955(16) . ?
V1 O2 1.8775(16) . ?
V1 O3 1.8937(17) . ?
V1 O8 2.0310(16) . ?
V1 N2 2.127(2) . ?
V1 N12 2.130(2) . ?
V1 O18 2.2188(16) . ?
O2 O3 1.416(3) . ?
C1 N2 1.348(3) . ?
C1 C6 1.373(4) . ?
C1 C7 1.499(3) . ?
N2 C3 1.342(3) . ?
C3 C4 1.373(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O9 1.229(3) . ?
C7 O8 1.282(3) . ?
C11 N12 1.353(3) . ?
C11 C16 1.377(4) . ?
C11 C17 1.497(3) . ?
N12 C13 1.343(3) . ?
C13 C14 1.388(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 O18 1.249(3) . ?
C17 N19 1.325(3) . ?
N19 H19A 0.9318 . ?
N19 H19B 0.9387 . ?
O20 H20A 0.82(3) . ?
O20 H20B 0.80(3) . ?
