#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:50:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179734 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/30/7003079.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_7003079
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         'C17 H11 N4 O5 V'
_chemical_formula_sum            'C17 H11 N4 O5 V'
_chemical_formula_weight         402.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   14.2730(7)
_cell_length_b                   11.1150(7)
_cell_length_c                   10.1940(11)
_cell_measurement_reflns_used    2138
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1617.2(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    0.1357
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22161
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3560
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0635
_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)+(0.0194P)²+1.8152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                2035
_reflns_number_total             3560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711347a.txt
_cod_data_source_block           voo2pcaphen
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7003079
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, 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
V V 0.41723(6) 0.18896(6) 0.68382(10) 0.0272(2) Uani 1 1 d . . .
C2 C 0.4253(4) 0.3137(5) 0.4184(5) 0.0345(13) Uani 1 1 d . . .
H2 H 0.4368 0.2364 0.3875 0.041 Uiso 1 1 calc R . .
C3 C 0.4221(4) 0.4085(5) 0.3285(6) 0.0425(15) Uani 1 1 d . . .
H3 H 0.4291 0.3935 0.2392 0.051 Uiso 1 1 calc R . .
C4 C 0.4087(4) 0.5225(5) 0.3721(6) 0.0402(15) Uani 1 1 d . . .
H4 H 0.4103 0.5866 0.3135 0.048 Uiso 1 1 calc R . .
C5 C 0.3922(4) 0.5436(5) 0.5071(6) 0.0374(16) Uani 1 1 d . . .
C6 C 0.3752(4) 0.6595(5) 0.5605(7) 0.0441(16) Uani 1 1 d . . .
H6 H 0.3777 0.7263 0.5056 0.053 Uiso 1 1 calc R . .
C7 C 0.3558(3) 0.6750(4) 0.6878(9) 0.0442(14) Uani 1 1 d . . .
H7 H 0.3424 0.7516 0.7193 0.053 Uiso 1 1 calc R . .
C8 C 0.3553(4) 0.5724(5) 0.7779(6) 0.0354(15) Uani 1 1 d . . .
C9 C 0.3368(4) 0.5811(5) 0.9131(7) 0.0429(16) Uani 1 1 d . . .
H9 H 0.3229 0.6552 0.9505 0.051 Uiso 1 1 calc R . .
C10 C 0.3395(4) 0.4807(5) 0.9886(6) 0.0366(15) Uani 1 1 d . . .
H10 H 0.3278 0.4859 1.0781 0.044 Uiso 1 1 calc R . .
C11 C 0.3600(4) 0.3684(5) 0.9311(6) 0.0339(14) Uani 1 1 d . . .
H11 H 0.3606 0.3002 0.9840 0.041 Uiso 1 1 calc R . .
C13 C 0.3752(4) 0.4574(5) 0.7298(6) 0.0301(16) Uani 1 1 d . . .
C14 C 0.3944(4) 0.4431(5) 0.5896(6) 0.0331(15) Uani 1 1 d . . .
C15 C 0.2605(4) 0.0608(4) 0.8089(6) 0.0270(12) Uani 1 1 d . . .
C17 C 0.3939(4) 0.0096(5) 0.9185(6) 0.0364(15) Uani 1 1 d . . .
H17 H 0.4575 0.0195 0.9347 0.044 Uiso 1 1 calc R . .
C18 C 0.3440(4) -0.0733(5) 0.9911(5) 0.0337(15) Uani 1 1 d . . .
H18 H 0.3750 -0.1170 1.0556 0.040 Uiso 1 1 calc R . .
C20 C 0.2112(4) -0.0245(5) 0.8809(6) 0.0360(15) Uani 1 1 d . . .
H20 H 0.1474 -0.0344 0.8653 0.043 Uiso 1 1 calc R . .
C21 C 0.2164(4) 0.1418(4) 0.7067(6) 0.0297(14) Uani 1 1 d . . .
N1 N 0.4126(3) 0.3298(4) 0.5464(4) 0.0286(12) Uani 1 1 d . . .
N12 N 0.3786(3) 0.3565(4) 0.8038(5) 0.0258(11) Uani 1 1 d . . .
N16 N 0.3530(3) 0.0760(3) 0.8253(4) 0.0264(10) Uani 1 1 d . . .
N19 N 0.2527(4) -0.0930(4) 0.9721(4) 0.0395(13) Uani 1 1 d . . .
O22 O 0.1320(2) 0.1433(3) 0.6885(5) 0.0352(8) Uani 1 1 d . . .
O23 O 0.2781(2) 0.2072(3) 0.6481(3) 0.0311(10) Uani 1 1 d . . .
O24 O 0.5167(2) 0.1691(3) 0.8001(4) 0.0336(9) Uani 1 1 d . . .
O25 O 0.5395(2) 0.2527(3) 0.6973(4) 0.0321(8) Uani 1 1 d . . .
O26 O 0.4317(3) 0.0852(3) 0.5769(4) 0.0340(9) 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'
V V 0.3005 0.5294 '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'
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
O26 V O24 104.46(18) . . ?
O26 V O25 101.60(17) . . ?
O24 V O25 45.07(15) . . ?
O26 V O23 94.34(16) . . ?
O24 V O23 150.70(15) . . ?
O25 V O23 151.64(14) . . ?
O26 V N1 95.00(18) . . ?
O24 V N1 122.45(17) . . ?
O25 V N1 78.37(17) . . ?
O23 V N1 76.99(16) . . ?
O26 V N16 95.29(17) . . ?
O24 V N16 80.01(16) . . ?
O25 V N16 124.89(18) . . ?
O23 V N16 76.00(15) . . ?
N1 V N16 151.71(18) . . ?
O26 V N12 168.16(18) . . ?
O24 V N12 86.58(15) . . ?
O25 V N12 83.05(15) . . ?
O23 V N12 77.25(14) . . ?
N1 V N12 75.13(16) . . ?
N16 V N12 90.78(16) . . ?
N1 C2 C3 122.6(6) . . ?
N1 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.8(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C14 C5 C4 116.7(5) . . ?
C14 C5 C6 119.9(6) . . ?
C4 C5 C6 123.4(5) . . ?
C7 C6 C5 121.6(5) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C6 C7 C8 120.6(5) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C13 C8 C9 116.4(5) . . ?
C13 C8 C7 119.4(6) . . ?
C9 C8 C7 124.2(6) . . ?
C10 C9 C8 119.6(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 119.9(6) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
N12 C11 C10 122.3(5) . . ?
N12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
N12 C13 C8 124.7(5) . . ?
N12 C13 C14 116.6(6) . . ?
C8 C13 C14 118.7(5) . . ?
N1 C14 C5 123.3(6) . . ?
N1 C14 C13 116.9(6) . . ?
C5 C14 C13 119.8(6) . . ?
N16 C15 C20 121.2(5) . . ?
N16 C15 C21 114.8(5) . . ?
C20 C15 C21 124.0(5) . . ?
N16 C17 C18 121.6(5) . . ?
N16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
N19 C18 C17 122.4(5) . . ?
N19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
N19 C20 C15 121.9(6) . . ?
N19 C20 H20 119.0 . . ?
C15 C20 H20 119.0 . . ?
O22 C21 O23 126.6(5) . . ?
O22 C21 C15 121.6(5) . . ?
O23 C21 C15 111.8(5) . . ?
C2 N1 C14 117.9(5) . . ?
C2 N1 V 123.4(4) . . ?
C14 N1 V 118.7(4) . . ?
C11 N12 C13 117.0(5) . . ?
C11 N12 V 130.4(4) . . ?
C13 N12 V 112.6(4) . . ?
C17 N16 C15 116.6(5) . . ?
C17 N16 V 128.4(4) . . ?
C15 N16 V 114.6(3) . . ?
C18 N19 C20 116.1(5) . . ?
C21 O23 V 121.9(3) . . ?
O25 O24 V 68.40(19) . . ?
O24 O25 V 66.53(18) . . ?
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 O26 1.600(4) . ?
V O24 1.863(3) . ?
V O25 1.889(3) . ?
V O23 2.029(3) . ?
V N1 2.101(4) . ?
V N16 2.121(4) . ?
V N12 2.295(5) . ?
C2 N1 1.330(7) . ?
C2 C3 1.397(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.357(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.416(8) . ?
C4 H4 0.9300 . ?
C5 C14 1.399(7) . ?
C5 C6 1.420(8) . ?
C6 C7 1.339(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.464(8) . ?
C7 H7 0.9300 . ?
C8 C13 1.399(8) . ?
C8 C9 1.406(9) . ?
C9 C10 1.356(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.409(7) . ?
C10 H10 0.9300 . ?
C11 N12 1.331(7) . ?
C11 H11 0.9300 . ?
C13 N12 1.352(7) . ?
C13 C14 1.463(8) . ?
C14 N1 1.359(7) . ?
C15 N16 1.342(6) . ?
C15 C20 1.390(7) . ?
C15 C21 1.515(7) . ?
C17 N16 1.337(7) . ?
C17 C18 1.380(8) . ?
C17 H17 0.9300 . ?
C18 N19 1.334(7) . ?
C18 H18 0.9300 . ?
C20 N19 1.340(7) . ?
C20 H20 0.9300 . ?
C21 O22 1.219(6) . ?
C21 O23 1.289(6) . ?
O24 O25 1.438(5) . ?
