#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:53:55 +0100 (vie 25 de mar de 2016) $
#$Revision: 180101 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/47/7054741.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_7054741
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, C5 H6 N O, H2 O'
_chemical_formula_sum            'C12 H11 N2 O8 V'
_chemical_formula_weight         362.17
_chemical_name_systematic
;
 ?
;
_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                 95.055(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8481(2)
_cell_length_b                   6.42100(10)
_cell_length_c                   13.8887(3)
_cell_measurement_reflns_used    2917
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.4760
_cell_measurement_theta_min      5.6380
_cell_volume                     697.17(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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4933
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    0.0257
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3489
_diffrn_reflns_theta_full        74.65
_diffrn_reflns_theta_max         74.65
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    6.416
_exptl_absorpt_correction_T_max  0.7397
_exptl_absorpt_correction_T_min  0.1834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0144(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1552
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0333
_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)+(0.0610P)²+0.2173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                1535
_reflns_number_total             1552
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5nj00164a3.cif
_cod_data_source_block           2.H2O
_cod_depositor_comments
'Adding full bibliography for 7054735--7054745.cif.'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7054741
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
V1 V 0.42268(5) 0.2500 0.19920(2) 0.01619(18) Uani 1 2 d S
N1 N 0.6246(2) 0.2500 0.11119(13) 0.0162(4) Uani 1 2 d S
N2 N 1.1675(3) 0.2500 0.61724(14) 0.0207(4) Uani 1 2 d S
H2 H 1.0860 0.2500 0.6569 0.031 Uiso 1 2 calc SR
O1 O 0.3137(2) 0.2500 0.06522(12) 0.0209(4) Uani 1 2 d S
O2 O 0.3379(2) 0.2500 -0.09465(12) 0.0258(4) Uani 1 2 d S
O3 O 0.6368(2) 0.2500 0.29011(11) 0.0228(4) Uani 1 2 d S
O4 O 0.9225(2) 0.2500 0.31096(13) 0.0320(5) Uani 1 2 d S
O5 O 0.33255(15) 0.4560(2) 0.23918(8) 0.0252(3) Uani 1 1 d .
O6 O 0.9574(2) 0.2500 0.49721(13) 0.0268(4) Uani 1 2 d S
H6O H 0.9393 0.2500 0.4367 0.040 Uiso 1 2 calc SR
O7 O 0.9279(2) 0.2500 0.74299(13) 0.0265(4) Uani 1 2 d SD
H7O H 0.862(3) 0.350(3) 0.7441(17) 0.040 Uiso 1 1 d D
C1 C 0.3996(3) 0.2500 -0.01109(16) 0.0172(4) Uani 1 2 d S
C2 C 0.5901(3) 0.2500 0.01551(15) 0.0159(4) Uani 1 2 d S
C3 C 0.7200(3) 0.2500 -0.04574(17) 0.0206(5) Uani 1 2 d S
H3 H 0.6952 0.2500 -0.1139 0.025 Uiso 1 2 calc SR
C4 C 0.8885(3) 0.2500 -0.00431(18) 0.0245(5) Uani 1 2 d S
H4 H 0.9805 0.2500 -0.0444 0.029 Uiso 1 2 calc SR
C5 C 0.9215(3) 0.2500 0.09584(19) 0.0252(5) Uani 1 2 d S
H5 H 1.0357 0.2500 0.1250 0.030 Uiso 1 2 calc SR
C6 C 0.7846(3) 0.2500 0.15158(16) 0.0191(5) Uani 1 2 d S
C7 C 0.7861(3) 0.2500 0.25944(16) 0.0207(5) Uani 1 2 d S
C8 C 1.3335(3) 0.2500 0.65491(17) 0.0232(5) Uani 1 2 d S
H8 H 1.3598 0.2500 0.7230 0.028 Uiso 1 2 calc SR
C9 C 1.4618(3) 0.2500 0.59538(18) 0.0245(5) Uani 1 2 d S
H9 H 1.5780 0.2500 0.6211 0.029 Uiso 1 2 calc SR
C10 C 1.4193(3) 0.2500 0.49476(18) 0.0233(5) Uani 1 2 d S
H10 H 1.5076 0.2500 0.4521 0.028 Uiso 1 2 calc SR
C11 C 1.2509(3) 0.2500 0.45785(16) 0.0219(5) Uani 1 2 d S
H11 H 1.2219 0.2500 0.3900 0.026 Uiso 1 2 calc SR
C12 C 1.1236(3) 0.2500 0.52155(17) 0.0199(5) Uani 1 2 d S
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
O5 V1 O5 109.39(9) 4_565
O5 V1 O1 99.01(5) 4_565
O5 V1 O1 99.01(5) .
O5 V1 O3 98.66(5) 4_565
O5 V1 O3 98.66(5) .
O1 V1 O3 149.16(7) .
O5 V1 N1 125.30(5) 4_565
O5 V1 N1 125.30(5) .
O1 V1 N1 74.71(7) .
O3 V1 N1 74.45(7) .
C6 N1 C2 121.5(2) .
C6 N1 V1 119.41(15) .
C2 N1 V1 119.12(16) .
C12 N2 C8 122.3(2) .
C12 N2 H2 118.9 .
C8 N2 H2 118.9 .
C1 O1 V1 123.55(15) .
C7 O3 V1 121.95(15) .
C12 O6 H6O 109.5 .
O2 C1 O1 125.7(2) .
O2 C1 C2 122.4(2) .
O1 C1 C2 111.88(18) .
N1 C2 C3 121.1(2) .
N1 C2 C1 110.74(19) .
C3 C2 C1 128.1(2) .
C2 C3 C4 118.0(2) .
C2 C3 H3 121.0 .
C4 C3 H3 121.0 .
C5 C4 C3 119.9(2) .
C5 C4 H4 120.0 .
C3 C4 H4 120.0 .
C6 C5 C4 118.4(2) .
C6 C5 H5 120.8 .
C4 C5 H5 120.8 .
N1 C6 C5 121.1(2) .
N1 C6 C7 110.2(2) .
C5 C6 C7 128.7(2) .
O4 C7 O3 125.4(2) .
O4 C7 C6 120.6(2) .
O3 C7 C6 114.0(2) .
C9 C8 N2 120.1(2) .
C9 C8 H8 119.9 .
N2 C8 H8 119.9 .
C8 C9 C10 118.8(2) .
C8 C9 H9 120.6 .
C10 C9 H9 120.6 .
C11 C10 C9 120.4(2) .
C11 C10 H10 119.8 .
C9 C10 H10 119.8 .
C10 C11 C12 118.9(2) .
C10 C11 H11 120.5 .
C12 C11 H11 120.5 .
O6 C12 N2 114.6(2) .
O6 C12 C11 125.9(2) .
N2 C12 C11 119.5(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.6212(13) 4_565
V1 O5 1.6212(13) .
V1 O1 1.9783(17) .
V1 O3 2.0109(17) .
V1 N1 2.0848(19) .
N1 C6 1.330(3) .
N1 C2 1.332(3) .
N2 C12 1.343(3) .
N2 C8 1.361(3) .
N2 H2 0.8800 .
O1 C1 1.305(3) .
O2 C1 1.217(3) .
O3 C7 1.281(3) .
O4 C7 1.234(3) .
O6 C12 1.318(3) .
O6 H6O 0.8400 .
O7 H7O 0.828(10) .
C1 C2 1.508(3) .
C2 C3 1.384(3) .
C3 C4 1.395(3) .
C3 H3 0.9500 .
C4 C5 1.392(4) .
C4 H4 0.9500 .
C5 C6 1.378(3) .
C5 H5 0.9500 .
C6 C7 1.497(3) .
C8 C9 1.358(4) .
C8 H8 0.9500 .
C9 C10 1.408(3) .
C9 H9 0.9500 .
C10 C11 1.375(3) .
C10 H10 0.9500 .
C11 C12 1.392(3) .
C11 H11 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
N2 H2 O7 0.88 1.80 2.677(3) 177.1 .
O6 H6O O4 0.84 1.74 2.577(2) 174.6 .
O7 H7O O5 0.828(10) 1.997(11) 2.8090(18) 166(2) 3_666
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 -89.69(7) 4_565
O5 V1 N1 C6 89.69(7) .
O1 V1 N1 C6 180.0 .
O3 V1 N1 C6 0.0 .
O5 V1 N1 C2 90.31(7) 4_565
O5 V1 N1 C2 -90.31(7) .
O1 V1 N1 C2 0.0 .
O3 V1 N1 C2 180.0 .
O5 V1 O1 C1 -124.28(5) 4_565
O5 V1 O1 C1 124.28(5) .
O3 V1 O1 C1 0.0 .
N1 V1 O1 C1 0.0 .
O5 V1 O3 C7 124.36(5) 4_565
O5 V1 O3 C7 -124.36(5) .
O1 V1 O3 C7 0.0 .
N1 V1 O3 C7 0.0 .
V1 O1 C1 O2 180.0 .
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 180.0 .
O1 C1 C2 N1 0.0 .
O2 C1 C2 C3 0.0 .
O1 C1 C2 C3 180.0 .
N1 C2 C3 C4 0.0 .
C1 C2 C3 C4 180.0 .
C2 C3 C4 C5 0.0 .
C3 C4 C5 C6 0.0 .
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 .
C12 N2 C8 C9 0.0 .
N2 C8 C9 C10 0.0 .
C8 C9 C10 C11 0.0 .
C9 C10 C11 C12 0.0 .
C8 N2 C12 O6 180.0 .
C8 N2 C12 C11 0.0 .
C10 C11 C12 O6 180.0 .
C10 C11 C12 N2 0.0 .
