#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:50:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179734 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/30/7003078.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_7003078
loop_
_publ_author_name
'Pacigová, Silvia'
'Gyepes, Róbert'
'Tatiersky, Jozef'
'Sivák, Michal'
_publ_section_title
;
 Interpretation of the multiple vanadium-oxygen bonds in the central
 VO(η2-O2)+ group. Synthesis, structure, supramolecular interactions
 and DFT studies for complexes with 2,2′-bipyridine,
 1,10-phenanthroline, pyrazinato(1--) and pyrazinamide ligands
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              121
_journal_paper_doi               10.1039/b711347a
_journal_year                    2008
_chemical_formula_moiety         'C15 H11 N4 O5 V'
_chemical_formula_sum            'C15 H11 N4 O5 V'
_chemical_formula_weight         378.22
_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                 101.281(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5040(3)
_cell_length_b                   8.4130(5)
_cell_length_c                   23.3830(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1447.68(12)
_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(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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    0.0529
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9622
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0438
_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)+(0.0316P)²+1.4660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                2729
_reflns_number_total             3813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711347a.txt
_cod_data_source_block           voo2pcabpy
_cod_original_cell_volume        1447.67(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7003078
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
V V 0.39920(5) 0.81889(5) 0.149024(17) 0.02208(12) Uani 1 1 d . . .
N1 N 0.4802(2) 1.0572(2) 0.11709(8) 0.0209(4) Uani 1 1 d . . .
C2 C 0.5845(3) 1.1673(3) 0.14909(10) 0.0269(5) Uani 1 1 d . . .
H2 H 0.6477 1.1388 0.1859 0.032 Uiso 1 1 calc R . .
C3 C 0.6024(3) 1.3197(3) 0.13009(11) 0.0282(5) Uani 1 1 d . . .
H3 H 0.6768 1.3923 0.1535 0.034 Uiso 1 1 calc R . .
C4 C 0.5076(3) 1.3637(3) 0.07540(11) 0.0278(5) Uani 1 1 d . . .
H4 H 0.5164 1.4666 0.0617 0.033 Uiso 1 1 calc R . .
C5 C 0.4001(3) 1.2521(3) 0.04168(10) 0.0254(5) Uani 1 1 d . . .
H5 H 0.3359 1.2788 0.0048 0.030 Uiso 1 1 calc R . .
C6 C 0.3889(3) 1.0999(3) 0.06335(10) 0.0212(5) Uani 1 1 d . . .
C7 C 0.2784(3) 0.9720(3) 0.03078(10) 0.0205(5) Uani 1 1 d . . .
C8 C 0.1986(3) 0.9853(3) -0.02819(10) 0.0250(5) Uani 1 1 d . . .
H8 H 0.2106 1.0787 -0.0484 0.030 Uiso 1 1 calc R . .
C9 C 0.1017(3) 0.8589(3) -0.05633(11) 0.0282(5) Uani 1 1 d . . .
H9 H 0.0477 0.8663 -0.0956 0.034 Uiso 1 1 calc R . .
C10 C 0.0859(3) 0.7213(3) -0.02546(11) 0.0309(6) Uani 1 1 d . . .
H10 H 0.0236 0.6338 -0.0438 0.037 Uiso 1 1 calc R . .
C11 C 0.1647(3) 0.7160(3) 0.03322(11) 0.0275(5) Uani 1 1 d . . .
H11 H 0.1516 0.6243 0.0542 0.033 Uiso 1 1 calc R . .
N12 N 0.2592(2) 0.8380(2) 0.06088(8) 0.0213(4) Uani 1 1 d . . .
C13 C 0.7927(3) 0.7424(3) 0.19051(10) 0.0239(5) Uani 1 1 d . . .
C14 C 0.9619(3) 0.7230(3) 0.22607(11) 0.0326(6) Uani 1 1 d . . .
H14 H 1.0563 0.6803 0.2105 0.039 Uiso 1 1 calc R . .
N15 N 0.9924(3) 0.7646(3) 0.28246(10) 0.0387(6) Uani 1 1 d . . .
C16 C 0.8535(4) 0.8281(3) 0.30183(11) 0.0360(6) Uani 1 1 d . . .
H16 H 0.8710 0.8597 0.3406 0.043 Uiso 1 1 calc R . .
C17 C 0.6828(4) 0.8493(3) 0.26664(10) 0.0306(6) Uani 1 1 d . . .
H17 H 0.5894 0.8938 0.2822 0.037 Uiso 1 1 calc R . .
N18 N 0.6526(3) 0.8062(2) 0.21076(8) 0.0232(4) Uani 1 1 d . . .
C19 C 0.7497(3) 0.7025(3) 0.12674(10) 0.0242(5) Uani 1 1 d . . .
O20 O 0.8612(2) 0.6375(2) 0.10268(7) 0.0315(4) Uani 1 1 d . . .
O21 O 0.5888(2) 0.7466(2) 0.10159(7) 0.0231(3) Uani 1 1 d . . .
O22 O 0.3348(2) 0.6400(2) 0.15756(8) 0.0305(4) Uani 1 1 d . . .
O23 O 0.3357(2) 0.9302(2) 0.21091(7) 0.0332(4) Uani 1 1 d . . .
O24 O 0.1964(2) 0.9383(2) 0.16017(7) 0.0316(4) Uani 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'
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O22 V O23 104.23(9) . . ?
O22 V O24 102.22(9) . . ?
O23 V O24 44.58(7) . . ?
O22 V O21 92.67(8) . . ?
O23 V O21 151.14(7) . . ?
O24 V O21 153.37(7) . . ?
O22 V N12 95.03(8) . . ?
O23 V N12 124.17(8) . . ?
O24 V N12 80.48(7) . . ?
O21 V N12 76.28(7) . . ?
O22 V N18 96.78(8) . . ?
O23 V N18 80.25(8) . . ?
O24 V N18 124.40(8) . . ?
O21 V N18 74.57(7) . . ?
N12 V N18 148.95(8) . . ?
O22 V N1 168.05(8) . . ?
O23 V N1 86.38(8) . . ?
O24 V N1 81.34(8) . . ?
O21 V N1 79.97(7) . . ?
N12 V N1 74.17(7) . . ?
N18 V N1 90.36(7) . . ?
C2 N1 C6 117.9(2) . . ?
C2 N1 V 126.31(15) . . ?
C6 N1 V 114.86(15) . . ?
N1 C2 C3 123.2(2) . . ?
N1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
C2 C3 C4 118.9(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
N1 C6 C5 121.8(2) . . ?
N1 C6 C7 114.6(2) . . ?
C5 C6 C7 123.6(2) . . ?
N12 C7 C8 120.8(2) . . ?
N12 C7 C6 116.46(19) . . ?
C8 C7 C6 122.7(2) . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C10 C11 118.7(2) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N12 C11 C10 122.5(2) . . ?
N12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C11 N12 C7 119.2(2) . . ?
C11 N12 V 121.59(16) . . ?
C7 N12 V 118.99(15) . . ?
N18 C13 C14 121.5(2) . . ?
N18 C13 C19 114.1(2) . . ?
C14 C13 C19 124.3(2) . . ?
N15 C14 C13 121.4(2) . . ?
N15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C16 N15 C14 116.5(2) . . ?
N15 C16 C17 122.9(2) . . ?
N15 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
N18 C17 C16 120.4(2) . . ?
N18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 N18 C13 117.3(2) . . ?
C17 N18 V 127.07(17) . . ?
C13 N18 V 115.60(15) . . ?
O20 C19 O21 125.6(2) . . ?
O20 C19 C13 121.5(2) . . ?
O21 C19 C13 112.9(2) . . ?
C19 O21 V 121.55(15) . . ?
O24 O23 V 68.52(10) . . ?
O23 O24 V 66.90(10) . . ?
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
V O22 1.6048(18) . ?
V O23 1.8621(18) . ?
V O24 1.8838(17) . ?
V O21 2.0596(16) . ?
V N12 2.1284(19) . ?
V N18 2.1533(18) . ?
V N1 2.264(2) . ?
N1 C2 1.342(3) . ?
N1 C6 1.356(3) . ?
C2 C3 1.373(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.476(3) . ?
C7 N12 1.352(3) . ?
C7 C8 1.396(3) . ?
C8 C9 1.380(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(3) . ?
C10 H10 0.9300 . ?
C11 N12 1.340(3) . ?
C11 H11 0.9300 . ?
C13 N18 1.346(3) . ?
C13 C14 1.384(3) . ?
C13 C19 1.501(3) . ?
C14 N15 1.340(3) . ?
C14 H14 0.9300 . ?
N15 C16 1.327(4) . ?
C16 C17 1.392(3) . ?
C16 H16 0.9300 . ?
C17 N18 1.332(3) . ?
C17 H17 0.9300 . ?
C19 O20 1.225(3) . ?
C19 O21 1.290(3) . ?
O23 O24 1.421(2) . ?
