#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:53:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180101 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/47/7054744.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_7054744
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, C7 H11 N2, H2 O'
_chemical_formula_sum            'C14 H16 N3 O7 V'
_chemical_formula_weight         389.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.17150(10)
_cell_length_b                   29.4539(5)
_cell_length_c                   6.63980(10)
_cell_measurement_reflns_used    2137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_volume                     1598.08(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Reference Manual (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_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      293(2)
_diffrn_detector_area_resol_mean 0.055
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Nonius KappaCCD area-detector diffractometer
;
_diffrn_measurement_method       'φ scans + ω 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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3499
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.8514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0323
_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)+(0.0420P)²+0.6208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                1620
_reflns_number_total             1987
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5nj00164a3.cif
_cod_data_source_block           4.H2O
_cod_depositor_comments
'Adding full bibliography for 7054735--7054745.cif.'
_cod_database_code               7054744
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, 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 0.52673(4) 0.863150(12) 0.7500 0.03261(14) Uani 1 2 d S . .
N1 N 0.2810(2) 0.84335(6) 0.7500 0.0294(4) Uani 1 2 d S . .
N2 N 0.9769(3) 0.63767(7) 0.7500 0.0443(5) Uani 1 2 d S . .
H2 H 0.9089 0.6600 0.7500 0.066 Uiso 1 2 calc SR . .
N3 N 1.3014(2) 0.53105(6) 0.7500 0.0356(4) Uani 1 2 d S . .
O1 O 0.52984(19) 0.79521(5) 0.7500 0.0478(5) Uani 1 2 d S . .
O2 O 0.3921(2) 0.72961(6) 0.7500 0.0635(6) Uani 1 2 d S . .
O3 O 0.39967(19) 0.92067(5) 0.7500 0.0401(4) Uani 1 2 d S . .
O4 O 0.1586(2) 0.95647(5) 0.7500 0.0461(5) Uani 1 2 d S . .
O5 O 0.63638(15) 0.87152(4) 0.5514(2) 0.0507(3) Uani 1 1 d . . .
O6 O 0.7596(3) 0.71090(10) 0.6878(6) 0.0709(16) Uani 0.50 1 d PD A -1
H6A H 0.696(5) 0.6900(11) 0.668(8) 0.106 Uiso 0.50 1 d PD B -1
H6B H 0.697(5) 0.7327(10) 0.686(9) 0.106 Uiso 0.50 1 d PD C -1
C1 C 0.3983(3) 0.77075(8) 0.7500 0.0434(6) Uani 1 2 d S . .
C2 C 0.2446(3) 0.79946(7) 0.7500 0.0342(5) Uani 1 2 d S . .
C3 C 0.0841(3) 0.78515(8) 0.7500 0.0474(7) Uani 1 2 d S . .
H3 H 0.0580 0.7544 0.7500 0.057 Uiso 1 2 calc SR . .
C4 C -0.0377(3) 0.81809(9) 0.7500 0.0476(7) Uani 1 2 d S . .
H4 H -0.1470 0.8093 0.7500 0.057 Uiso 1 2 calc SR . .
C5 C 0.0016(3) 0.86381(8) 0.7500 0.0370(5) Uani 1 2 d S . .
H5 H -0.0795 0.8859 0.7500 0.044 Uiso 1 2 calc SR . .
C6 C 0.1654(3) 0.87551(7) 0.7500 0.0295(5) Uani 1 2 d S . .
C7 C 0.2402(3) 0.92216(7) 0.7500 0.0313(5) Uani 1 2 d S . .
C8 C 1.1385(4) 0.64586(8) 0.7500 0.0427(6) Uani 1 2 d S . .
H8 H 1.1753 0.6757 0.7500 0.051 Uiso 1 2 calc SR . .
C9 C 1.2492(3) 0.61162(7) 0.7500 0.0351(5) Uani 1 2 d S . .
H9 H 1.3605 0.6182 0.7500 0.042 Uiso 1 2 calc SR . .
C10 C 1.1961(3) 0.56567(8) 0.7500 0.0309(5) Uani 1 2 d S . .
C11 C 1.0238(3) 0.55863(8) 0.7500 0.0367(5) Uani 1 2 d S . .
H11 H 0.9820 0.5293 0.7500 0.044 Uiso 1 2 calc SR . .
C12 C 0.9206(3) 0.59460(9) 0.7500 0.0422(6) Uani 1 2 d S . .
H12 H 0.8083 0.5895 0.7500 0.051 Uiso 1 2 calc SR . .
C13 C 1.4784(3) 0.53876(9) 0.7500 0.0439(6) Uani 1 2 d S . .
H13A H 1.5338 0.5110 0.7824 0.066 Uiso 0.50 1 calc PR D -1
H13B H 1.5053 0.5614 0.8484 0.066 Uiso 0.50 1 calc PR D -1
H13C H 1.5123 0.5489 0.6191 0.066 Uiso 0.50 1 calc PR D -1
C14 C 1.2437(3) 0.48417(9) 0.7500 0.0545(8) Uani 1 2 d S . .
H14A H 1.1551 0.4811 0.8439 0.082 Uiso 0.50 1 calc PR E -1
H14B H 1.3316 0.4644 0.7886 0.082 Uiso 0.50 1 calc PR E -1
H14C H 1.2065 0.4762 0.6175 0.082 Uiso 0.50 1 calc PR E -1
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'
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 109.66(10) 6_557
O5 V1 O3 99.20(5) 6_557
O5 V1 O3 99.20(5) .
O5 V1 O1 98.39(5) 6_557
O5 V1 O1 98.39(5) .
O3 V1 O1 149.22(7) .
O5 V1 N1 125.17(5) 6_557
O5 V1 N1 125.17(5) .
O3 V1 N1 74.69(7) .
O1 V1 N1 74.53(7) .
C2 N1 C6 122.13(19) .
C2 N1 V1 119.13(14) .
C6 N1 V1 118.74(14) .
C8 N2 C12 120.3(2) .
C8 N2 H2 119.9 .
C12 N2 H2 119.9 .
C10 N3 C14 121.0(2) .
C10 N3 C13 121.2(2) .
C14 N3 C13 117.8(2) .
C1 O1 V1 123.10(15) .
C7 O3 V1 123.44(14) .
H6A O6 H6B 101(4) .
O2 C1 O1 126.2(2) .
O2 C1 C2 121.6(2) .
O1 C1 C2 112.2(2) .
N1 C2 C3 120.8(2) .
N1 C2 C1 111.02(19) .
C3 C2 C1 128.2(2) .
C2 C3 C4 117.9(2) .
C2 C3 H3 121.0 .
C4 C3 H3 121.0 .
C5 C4 C3 120.9(2) .
C5 C4 H4 119.6 .
C3 C4 H4 119.6 .
C6 C5 C4 117.9(2) .
C6 C5 H5 121.1 .
C4 C5 H5 121.1 .
N1 C6 C5 120.5(2) .
N1 C6 C7 111.09(18) .
C5 C6 C7 128.42(19) .
O4 C7 O3 125.3(2) .
O4 C7 C6 122.6(2) .
O3 C7 C6 112.05(18) .
N2 C8 C9 121.6(2) .
N2 C8 H8 119.2 .
C9 C8 H8 119.2 .
C8 C9 C10 120.3(2) .
C8 C9 H9 119.9 .
C10 C9 H9 119.9 .
N3 C10 C9 122.0(2) .
N3 C10 C11 121.8(2) .
C9 C10 C11 116.2(2) .
C12 C11 C10 120.1(2) .
C12 C11 H11 119.9 .
C10 C11 H11 119.9 .
N2 C12 C11 121.6(2) .
N2 C12 H12 119.2 .
C11 C12 H12 119.2 .
N3 C13 H13A 109.5 .
N3 C13 H13B 109.5 .
N3 C13 H13C 109.5 .
N3 C14 H14A 109.5 .
N3 C14 H14B 109.5 .
N3 C14 H14C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.6133(13) 6_557
V1 O5 1.6133(13) .
V1 O3 1.9869(16) .
V1 O1 2.0013(17) .
V1 N1 2.0912(18) .
N1 C2 1.327(3) .
N1 C6 1.338(3) .
N2 C8 1.343(4) .
N2 C12 1.349(3) .
N2 H2 0.8600 .
N3 C10 1.334(3) .
N3 C14 1.459(3) .
N3 C13 1.465(3) .
O1 C1 1.294(3) .
O2 C1 1.213(3) .
O3 C7 1.304(3) .
O4 C7 1.211(3) .
O6 H6A 0.815(10) .
O6 H6B 0.818(10) .
C1 C2 1.514(3) .
C2 C3 1.378(3) .
C3 C4 1.390(4) .
C3 H3 0.9300 .
C4 C5 1.384(3) .
C4 H4 0.9300 .
C5 C6 1.381(3) .
C5 H5 0.9300 .
C6 C7 1.504(3) .
C8 C9 1.355(3) .
C8 H8 0.9300 .
C9 C10 1.421(3) .
C9 H9 0.9300 .
C10 C11 1.423(3) .
C11 C12 1.354(3) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
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 O6 0.86 1.98 2.824(3) 167.9 6_557
N2 H2 O6 0.86 1.98 2.824(3) 167.9 .
O6 H6A O5 0.815(10) 2.38(3) 3.071(3) 144(5) 3_566
O6 H6B O1 0.818(10) 2.334(15) 3.140(3) 169(5) .
O6 H6B O2 0.818(10) 2.53(4) 3.080(3) 126(4) .
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 C2 -89.44(7) 6_557
O5 V1 N1 C2 89.44(7) .
O3 V1 N1 C2 180.0 .
O1 V1 N1 C2 0.0 .
O5 V1 N1 C6 90.56(7) 6_557
O5 V1 N1 C6 -90.56(7) .
O3 V1 N1 C6 0.0 .
O1 V1 N1 C6 180.0 .
O5 V1 O1 C1 124.28(5) 6_557
O5 V1 O1 C1 -124.28(5) .
O3 V1 O1 C1 0.0 .
N1 V1 O1 C1 0.0 .
O5 V1 O3 C7 -124.10(5) 6_557
O5 V1 O3 C7 124.10(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 .
C14 N3 C10 C9 180.0 .
C13 N3 C10 C9 0.0 .
C14 N3 C10 C11 0.0 .
C13 N3 C10 C11 180.0 .
C8 C9 C10 N3 180.0 .
C8 C9 C10 C11 0.0 .
N3 C10 C11 C12 180.0 .
C9 C10 C11 C12 0.0 .
C8 N2 C12 C11 0.0 .
C10 C11 C12 N2 0.0 .
