#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:53:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180101 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/47/7054742.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_7054742
loop_
_publ_author_name
'Koleša-Dobravc, Tanja'
'Meden, Anton'
'Perdih, Franc'
_publ_section_title
;
 Influence of noncovalent interactions on the structures of metal--organic
 hybrids based on a [VO2(2,6-pydc)]−tecton with cations of
 imidazole, pyridine and its derivatives
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              4265
_journal_paper_doi               10.1039/C5NJ00164A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C7 H3 N O6 V, 1.0(C5 H7 N2), H2 O'
_chemical_formula_sum            'C12 H12 N3 O7 V'
_chemical_formula_weight         361.19
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 97.755(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1855(2)
_cell_length_b                   6.5443(2)
_cell_length_c                   13.8669(3)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.5110
_cell_measurement_theta_min      5.9520
_cell_volume                     736.03(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics
'ORTEP-3 for Windows version 2.02 (Farrugia, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4933
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3693
_diffrn_reflns_theta_full        74.69
_diffrn_reflns_theta_max         74.69
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    6.041
_exptl_absorpt_correction_T_max  0.6771
_exptl_absorpt_correction_T_min  0.1961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0362
_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)+(0.0746P)²+0.1147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                1586
_reflns_number_total             1627
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5nj00164a3.cif
_cod_data_source_block           3.H2O
_cod_depositor_comments
'Adding full bibliography for 7054735--7054745.cif.'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7054742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.39860(4) 0.7500 0.68170(3) 0.02372(19) Uani 1 2 d S . .
N1 N 0.6260(2) 0.7500 0.62831(12) 0.0173(4) Uani 1 2 d S . .
O1 O 0.5697(2) 0.7500 0.79782(12) 0.0325(4) Uani 1 2 d S . .
O2 O 0.8350(3) 0.7500 0.86367(12) 0.0376(5) Uani 1 2 d S . .
O3 O 0.3430(2) 0.7500 0.53864(12) 0.0299(4) Uani 1 2 d S . .
O4 O 0.4264(3) 0.7500 0.39120(13) 0.0394(5) Uani 1 2 d S . .
O5 O 0.29676(16) 0.5498(2) 0.70751(10) 0.0365(3) Uani 1 1 d . . .
O6 O 0.1420(2) 0.2500 0.80229(14) 0.0335(4) Uani 1 2 d S . .
H6O H 0.1815 0.3532 0.7777 0.050 Uiso 1 1 d R . .
C1 C 0.7278(3) 0.7500 0.79409(16) 0.0249(5) Uani 1 2 d S . .
C2 C 0.7647(3) 0.7500 0.69057(15) 0.0205(4) Uani 1 2 d S . .
C3 C 0.9165(3) 0.7500 0.65766(19) 0.0280(5) Uani 1 2 d S . .
H3 H 1.0157 0.7500 0.7020 0.034 Uiso 1 2 calc SR . .
C4 C 0.9197(3) 0.7500 0.5576(2) 0.0336(6) Uani 1 2 d S . .
H4 H 1.0225 0.7500 0.5329 0.040 Uiso 1 2 calc SR . .
C5 C 0.7734(3) 0.7500 0.49319(17) 0.0291(5) Uani 1 2 d S . .
H5 H 0.7741 0.7500 0.4247 0.035 Uiso 1 2 calc SR . .
C6 C 0.6275(3) 0.7500 0.53277(15) 0.0207(5) Uani 1 2 d S . .
C7 C 0.4535(3) 0.7500 0.47957(17) 0.0249(5) Uani 1 2 d S . .
N2A N 0.4078(5) 0.7500 -0.0396(2) 0.0286(8) Uani 0.661(6) 2 d SP A 1
H2A H 0.4514 0.7500 -0.0943 0.043 Uiso 0.661(6) 2 calc SPR A 1
N3A N 0.2050(4) 0.7500 0.2145(2) 0.0232(8) Uani 0.661(6) 2 d SP A 1
H3A H 0.2695 0.7500 0.2707 0.035 Uiso 0.661(6) 2 calc SPR A 1
H3B H 0.0972 0.7500 0.2130 0.035 Uiso 0.661(6) 2 calc SPR A 1
C8A C 0.4446(9) 0.7500 0.1329(6) 0.0214(14) Uani 0.661(6) 2 d SP A 1
H8A H 0.5159 0.7500 0.1930 0.026 Uiso 0.661(6) 2 calc SPR A 1
C9A C 0.5072(7) 0.7500 0.0462(3) 0.0259(9) Uani 0.661(6) 2 d SP A 1
H9A H 0.6233 0.7500 0.0465 0.031 Uiso 0.661(6) 2 calc SPR A 1
C10A C 0.2419(7) 0.7500 -0.0427(3) 0.0309(10) Uani 0.661(6) 2 d SP A 1
H10A H 0.1747 0.7500 -0.1042 0.037 Uiso 0.661(6) 2 calc SPR A 1
C11A C 0.1682(6) 0.7500 0.0399(4) 0.0270(11) Uani 0.661(6) 2 d SP A 1
H11A H 0.0515 0.7500 0.0365 0.032 Uiso 0.661(6) 2 calc SPR A 1
C12A C 0.2711(4) 0.7500 0.1312(4) 0.0184(9) Uani 0.661(6) 2 d SP A 1
N2B N 0.1319(8) 0.7500 0.1002(5) 0.0274(16) Uiso 0.339(6) 2 d SP A 2
H2B H 0.0302 0.7500 0.1142 0.041 Uiso 0.339(6) 2 calc SPR A 2
C9B C 0.1585(17) 0.7500 0.0064(10) 0.034(3) Uiso 0.339(6) 2 d SP A 2
H9B H 0.0642 0.7500 -0.0417 0.041 Uiso 0.339(6) 2 calc SPR A 2
C10B C 0.2581(12) 0.7500 0.1722(9) 0.022(2) Uiso 0.339(6) 2 d SP A 2
H10B H 0.2413 0.7500 0.2387 0.027 Uiso 0.339(6) 2 calc SPR A 2
N3B N 0.5983(9) 0.7500 0.0252(5) 0.0267(15) Uiso 0.339(6) 2 d SP A 2
H3C H 0.6845 0.7500 0.0706 0.040 Uiso 0.339(6) 2 calc SPR A 2
H3D H 0.6124 0.7500 -0.0366 0.040 Uiso 0.339(6) 2 calc SPR A 2
C12B C 0.4472(13) 0.7500 0.0499(6) 0.022(2) Uiso 0.339(6) 2 d SP A 2
C11B C 0.415(2) 0.7500 0.1449(14) 0.027(4) Uiso 0.339(6) 2 d SP A 2
H11B H 0.5061 0.7500 0.1951 0.033 Uiso 0.339(6) 2 calc SPR A 2
C8B C 0.3068(16) 0.7500 -0.0249(8) 0.031(3) Uiso 0.339(6) 2 d SP A 2
H8B H 0.3184 0.7500 -0.0922 0.037 Uiso 0.339(6) 2 calc SPR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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
O5 V1 O5 108.07(10) . 4_575
O5 V1 O3 99.59(6) . .
O5 V1 O3 99.59(6) 4_575 .
O5 V1 O1 98.55(6) . .
O5 V1 O1 98.55(6) 4_575 .
O3 V1 O1 148.86(7) . .
O5 V1 N1 125.95(5) . .
O5 V1 N1 125.95(5) 4_575 .
O3 V1 N1 74.93(7) . .
O1 V1 N1 73.94(7) . .
C6 N1 C2 121.73(19) . .
C6 N1 V1 118.79(14) . .
C2 N1 V1 119.47(14) . .
C1 O1 V1 124.31(14) . .
C7 O3 V1 123.22(15) . .
O2 C1 O1 125.8(2) . .
O2 C1 C2 122.8(2) . .
O1 C1 C2 111.46(19) . .
N1 C2 C3 120.8(2) . .
N1 C2 C1 110.82(19) . .
C3 C2 C1 128.3(2) . .
C2 C3 C4 118.0(2) . .
C2 C3 H3 121.0 . .
C4 C3 H3 121.0 . .
C3 C4 C5 120.6(2) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C6 C5 C4 117.4(2) . .
C6 C5 H5 121.3 . .
C4 C5 H5 121.3 . .
N1 C6 C5 121.5(2) . .
N1 C6 C7 110.60(19) . .
C5 C6 C7 127.9(2) . .
O4 C7 O3 126.0(2) . .
O4 C7 C6 121.6(2) . .
O3 C7 C6 112.46(19) . .
C9A N2A C10A 120.8(4) . .
C9A N2A H2A 119.6 . .
C10A N2A H2A 119.6 . .
C12A N3A H3A 120.0 . .
C12A N3A H3B 120.0 . .
H3A N3A H3B 120.0 . .
C9A C8A C12A 118.6(6) . .
C9A C8A H8A 120.7 . .
C12A C8A H8A 120.7 . .
N2A C9A C8A 121.5(5) . .
N2A C9A H9A 119.3 . .
C8A C9A H9A 119.3 . .
N2A C10A C11A 121.9(5) . .
N2A C10A H10A 119.0 . .
C11A C10A H10A 119.0 . .
C10A C11A C12A 118.1(5) . .
C10A C11A H11A 120.9 . .
C12A C11A H11A 120.9 . .
N3A C12A C8A 120.4(5) . .
N3A C12A C11A 120.5(3) . .
C8A C12A C11A 119.1(5) . .
C10B N2B C9B 120.8(10) . .
C10B N2B H2B 119.6 . .
C9B N2B H2B 119.6 . .
C8B C9B N2B 125.7(11) . .
C8B C9B H9B 117.2 . .
N2B C9B H9B 117.2 . .
N2B C10B C11B 116.5(14) . .
N2B C10B H10B 121.7 . .
C11B C10B H10B 121.7 . .
C12B N3B H3C 120.0 . .
C12B N3B H3D 120.0 . .
H3C N3B H3D 120.0 . .
N3B C12B C11B 123.6(10) . .
N3B C12B C8B 119.7(9) . .
C11B C12B C8B 116.7(12) . .
C12B C11B C10B 124.5(16) . .
C12B C11B H11B 117.8 . .
C10B C11B H11B 117.8 . .
C9B C8B C12B 115.8(11) . .
C9B C8B H8B 122.1 . .
C12B C8B H8B 122.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.6186(13) .
V1 O5 1.6186(13) 4_575
V1 O3 1.9746(17) .
V1 O1 1.9865(19) .
V1 N1 2.0941(18) .
N1 C6 1.327(3) .
N1 C2 1.330(3) .
O1 C1 1.302(3) .
O2 C1 1.213(3) .
O3 C7 1.299(3) .
O4 C7 1.215(3) .
O6 H6O 0.8404 .
C1 C2 1.506(3) .
C2 C3 1.380(3) .
C3 C4 1.392(4) .
C3 H3 0.9500 .
C4 C5 1.394(4) .
C4 H4 0.9500 .
C5 C6 1.380(3) .
C5 H5 0.9500 .
C6 C7 1.513(3) .
N2A C9A 1.347(6) .
N2A C10A 1.353(6) .
N2A H2A 0.8800 .
N3A C12A 1.340(5) .
N3A H3A 0.8800 .
N3A H3B 0.8800 .
C8A C9A 1.370(10) .
C8A C12A 1.417(8) .
C8A H8A 0.9500 .
C9A H9A 0.9500 .
C10A C11A 1.365(7) .
C10A H10A 0.9500 .
C11A C12A 1.423(7) .
C11A H11A 0.9500 .
N2B C10B 1.337(10) .
N2B C9B 1.347(13) .
N2B H2B 0.8800 .
C9B C8B 1.344(19) .
C9B H9B 0.9500 .
C10B C11B 1.38(2) .
C10B H10B 0.9500 .
N3B C12B 1.327(12) .
N3B H3C 0.8800 .
N3B H3D 0.8800 .
C12B C11B 1.379(19) .
C12B C8B 1.440(15) .
C11B H11B 0.9500 .
C8B H8B 0.9500 .
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
O6 H6O O5 0.84 1.93 2.7624(18) 168.2 .
N2A H2A O1 0.88 1.89 2.765(4) 173.1 1_554
N3A H3A O4 0.88 1.97 2.844(3) 176.1 .
N3A H3B O6 0.88 1.94 2.819(4) 175.1 3_566
N2B H2B O6 0.88 1.94 2.770(8) 156.4 3_566
N3B H3C O6 0.88 2.11 2.978(7) 169.3 3_666
N3B H3D O1 0.88 2.28 3.130(7) 163.8 1_554
N3B H3D O2 0.88 2.43 3.153(8) 139.5 1_554
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
O5 V1 N1 C6 91.02(7) .
O5 V1 N1 C6 -91.02(7) 4_575
O3 V1 N1 C6 0.0 .
O1 V1 N1 C6 180.0 .
O5 V1 N1 C2 -88.98(7) .
O5 V1 N1 C2 88.98(7) 4_575
O3 V1 N1 C2 180.0 .
O1 V1 N1 C2 0.0 .
O5 V1 O1 C1 125.07(5) .
O5 V1 O1 C1 -125.07(5) 4_575
O3 V1 O1 C1 0.000(1) .
N1 V1 O1 C1 0.0 .
O5 V1 O3 C7 -124.83(5) .
O5 V1 O3 C7 124.83(5) 4_575
O1 V1 O3 C7 0.0 .
N1 V1 O3 C7 0.0 .
V1 O1 C1 O2 180.000(1) .
V1 O1 C1 C2 0.0 .
C6 N1 C2 C3 0.0 .
V1 N1 C2 C3 180.0 .
C6 N1 C2 C1 180.0 .
V1 N1 C2 C1 0.0 .
O2 C1 C2 N1 180.000(1) .
O1 C1 C2 N1 0.0 .
O2 C1 C2 C3 0.000(1) .
O1 C1 C2 C3 180.0 .
N1 C2 C3 C4 0.000(1) .
C1 C2 C3 C4 180.0 .
C2 C3 C4 C5 0.000(1) .
C3 C4 C5 C6 0.000(1) .
C2 N1 C6 C5 0.0 .
V1 N1 C6 C5 180.0 .
C2 N1 C6 C7 180.0 .
V1 N1 C6 C7 0.0 .
C4 C5 C6 N1 0.0 .
C4 C5 C6 C7 180.0 .
V1 O3 C7 O4 180.0 .
V1 O3 C7 C6 0.0 .
N1 C6 C7 O4 180.0 .
C5 C6 C7 O4 0.0 .
N1 C6 C7 O3 0.0 .
C5 C6 C7 O3 180.0 .
C10A N2A C9A C8A 0.0 .
C12A C8A C9A N2A 0.0 .
C9A N2A C10A C11A 0.0 .
N2A C10A C11A C12A 0.0 .
C9A C8A C12A N3A 180.0 .
C9A C8A C12A C11A 0.0 .
C10A C11A C12A N3A 180.0 .
C10A C11A C12A C8A 0.0 .
C10B N2B C9B C8B 0.000(1) .
C9B N2B C10B C11B 0.000(1) .
N3B C12B C11B C10B 180.0 .
C8B C12B C11B C10B 0.000(1) .
N2B C10B C11B C12B 0.000(2) .
N2B C9B C8B C12B 0.000(1) .
N3B C12B C8B C9B 180.0 .
C11B C12B C8B C9B 0.000(1) .
