#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/62/2016274.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2016274
loop_
_publ_author_name
'Zhao-Xun Lian'
'Ping Liu'
'Jia-Min Zhang'
'Tian-Xi Wang'
'Tian-Jun Lou'
_publ_section_title
catena-Poly[[(2,2'-bipyridyl)oxidovanadium]-di-μ₂-oxido-[(2,2'-bipyridyl)oxidovanadium]-μ₃-selenito-bis[(2,2'-bipyridyl)dioxidovanadium]-μ₃-selenito]
_journal_coeditor_code           LN3059
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m525
_journal_page_last               m527
_journal_paper_doi               10.1107/S0108270107047683
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[V4 O8 (Se O3)2 (C10 H8 N2)4]'
_chemical_formula_moiety         'C20 H16 N4 O7 Se V2'
_chemical_formula_sum            'C20 H16 N4 O7 Se V2'
_chemical_formula_weight         605.21
_chemical_name_common
;
Poly[tetrakis(2,2'-bipyridyl)di-μ₂-oxido-hexaoxido-di-μ₃-selenito-
tetravanadium]
;
_chemical_name_systematic
;
catena-Poly[[(2,2'-bipyridyl)oxidovanadium]-di-μ₂-oxido-[(2,2'-
bipyridyl)oxidovanadium]-μ₃-selenito-bis[(2,2'-bipyridyl)dioxidovanadium]-
μ₃-selenito]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                87.53(3)
_cell_angle_beta                 75.49(2)
_cell_angle_gamma                76.41(3)
_cell_formula_units_Z            2
_cell_length_a                   9.816(2)
_cell_length_b                   10.026(3)
_cell_length_c                   11.090(2)
_cell_measurement_reflns_used    3588
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1026.9(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2001)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2001)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'RAXISCS3 scanner'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotor target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3588
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.737
_exptl_absorpt_correction_T_max  0.361
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(TEXSAN; Molecular Structure Corporation, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.572
_refine_ls_extinction_coef       0.064(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0264
_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)+(0.0666P)²+0.4497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                3458
_reflns_number_total             3588
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ln3059.cif
_cod_data_source_block           I
_cod_original_cell_volume        1027.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2016274
_cod_database_fobs_code          2016274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Se Se1 0.34836(2) 0.48783(2) 0.639577(19) 0.01603(13) Uani d . 1
V V1 0.59671(4) 0.22075(4) 0.52822(4) 0.01738(14) Uani d . 1
V V2 0.12052(4) 0.52532(4) 0.91059(3) 0.01637(14) Uani d . 1
O O1 0.6138(2) 0.11717(18) 0.64349(17) 0.0288(4) Uani d . 1
O O2 0.45288(18) 0.20010(18) 0.49037(16) 0.0260(4) Uani d . 1
O O3 0.52610(17) 0.39875(17) 0.61313(15) 0.0201(3) Uani d . 1
O O4 0.36319(18) 0.64661(16) 0.65168(15) 0.0219(4) Uani d . 1
O O5 0.29475(17) 0.43883(17) 0.79379(15) 0.0219(4) Uani d . 1
O O6 0.01439(17) 0.40655(16) 0.92701(15) 0.0197(3) Uani d . 1
O O7 0.06057(18) 0.64205(19) 0.82039(16) 0.0265(4) Uani d . 1
N N1 0.8212(2) 0.2563(2) 0.5106(2) 0.0216(4) Uani d . 1
N N2 0.7443(2) 0.0766(2) 0.39155(18) 0.0209(4) Uani d . 1
N N3 0.2467(2) 0.3988(2) 1.04116(18) 0.0197(4) Uani d . 1
N N4 0.2426(2) 0.6546(2) 0.97566(18) 0.0197(4) Uani d . 1
C C1 0.8514(3) 0.3473(3) 0.5790(3) 0.0279(5) Uani d . 1
H H1 0.7750 0.4078 0.6313 0.033 Uiso calc R 1
C C2 0.9910(3) 0.3552(3) 0.5751(3) 0.0349(7) Uani d . 1
H H2 1.0083 0.4205 0.6230 0.042 Uiso calc R 1
C C3 1.1040(3) 0.2645(3) 0.4990(3) 0.0378(7) Uani d . 1
H H3 1.1991 0.2670 0.4953 0.045 Uiso calc R 1
C C4 1.0746(3) 0.1695(3) 0.4281(3) 0.0327(6) Uani d . 1
H H4 1.1497 0.1069 0.3767 0.039 Uiso calc R 1
C C5 0.9314(3) 0.1688(2) 0.4347(2) 0.0226(5) Uani d . 1
C C6 0.8878(3) 0.0716(2) 0.3638(2) 0.0225(5) Uani d . 1
C C7 0.9847(3) -0.0211(3) 0.2757(3) 0.0359(7) Uani d . 1
H H7 1.0826 -0.0216 0.2553 0.043 Uiso calc R 1
C C8 0.9346(4) -0.1130(3) 0.2183(3) 0.0403(7) Uani d . 1
H H8 0.9985 -0.1762 0.1594 0.048 Uiso calc R 1
C C9 0.7897(3) -0.1097(3) 0.2494(3) 0.0346(6) Uani d . 1
H H9 0.7543 -0.1719 0.2131 0.042 Uiso calc R 1
C C10 0.6965(3) -0.0125(2) 0.3355(2) 0.0260(5) Uani d . 1
H H10 0.5979 -0.0091 0.3550 0.031 Uiso calc R 1
C C11 0.2456(3) 0.2680(3) 1.0684(2) 0.0248(5) Uani d . 1
H H11 0.1960 0.2233 1.0283 0.030 Uiso calc R 1
C C12 0.3147(3) 0.1965(3) 1.1531(3) 0.0310(6) Uani d . 1
H H12 0.3124 0.1052 1.1693 0.037 Uiso calc R 1
C C13 0.3876(3) 0.2626(3) 1.2139(3) 0.0323(6) Uani d . 1
H H13 0.4339 0.2170 1.2727 0.039 Uiso calc R 1
C C14 0.3906(3) 0.3976(3) 1.1859(2) 0.0280(6) Uani d . 1
H H14 0.4401 0.4440 1.2246 0.034 Uiso calc R 1
C C15 0.3186(2) 0.4630(2) 1.0992(2) 0.0204(5) Uani d . 1
C C16 0.3146(2) 0.6075(2) 1.0632(2) 0.0207(5) Uani d . 1
C C17 0.3818(3) 0.6896(3) 1.1156(2) 0.0269(5) Uani d . 1
H H17 0.4318 0.6549 1.1754 0.032 Uiso calc R 1
C C18 0.3728(3) 0.8238(3) 1.0769(3) 0.0315(6) Uani d . 1
H H18 0.4154 0.8811 1.1115 0.038 Uiso calc R 1
C C19 0.2998(3) 0.8718(3) 0.9864(3) 0.0325(6) Uani d . 1
H H19 0.2931 0.9615 0.9588 0.039 Uiso calc R 1
C C20 0.2369(3) 0.7840(3) 0.9376(2) 0.0265(5) Uani d . 1
H H20 0.1888 0.8160 0.8760 0.032 Uiso calc R 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'
Se Se -0.0929 2.2259 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O4 Se1 O3 . . 101.45(8) y
O4 Se1 O5 . . 103.77(9) y
O3 Se1 O5 . . 96.61(8) y
O1 V1 O2 . . 104.96(10) y
O1 V1 O3 . . 101.88(8) y
O2 V1 O3 . . 101.74(8) y
O1 V1 N2 . . 93.55(9) y
O2 V1 N2 . . 94.56(9) y
O3 V1 N2 . . 153.69(8) y
O1 V1 N1 . . 90.74(9) y
O2 V1 N1 . . 160.71(9) y
O3 V1 N1 . . 85.54(8) y
N2 V1 N1 . . 72.96(8) ?
O1 V1 O4 . 2_666 165.34(8) y
O2 V1 O4 . 2_666 86.95(8) y
O3 V1 O4 . 2_666 83.60(7) y
N2 V1 O4 . 2_666 76.74(7) y
N1 V1 O4 . 2_666 76.03(7) y
O7 V2 O6 . . 106.45(9) y
O7 V2 O5 . . 97.50(9) y
O6 V2 O5 . . 103.55(8) y
O7 V2 O6 . 2_567 99.98(9) y
O6 V2 O6 . 2_567 81.99(8) y
O5 V2 O6 . 2_567 159.32(7) y
O7 V2 N4 . . 93.00(9) y
O6 V2 N4 . . 155.09(8) y
O5 V2 N4 . . 88.80(8) y
O6 V2 N4 2_567 . 79.37(7) y
O7 V2 N3 . . 164.14(8) y
O6 V2 N3 . . 89.38(8) y
O5 V2 N3 . . 79.25(7) y
O6 V2 N3 2_567 . 80.93(7) y
N4 V2 N3 . . 71.51(7) ?
O7 V2 V2 . 2_567 107.27(7) ?
O6 V2 V2 . 2_567 44.39(6) ?
O5 V2 V2 . 2_567 143.64(6) ?
O6 V2 V2 2_567 2_567 37.60(5) ?
N4 V2 V2 . 2_567 115.38(6) ?
N3 V2 V2 . 2_567 83.22(6) ?
Se1 O3 V1 . . 122.48(9) ?
Se1 O4 V1 . 2_666 119.57(9) ?
Se1 O5 V2 . . 125.06(10) ?
V2 O6 V2 . 2_567 98.01(8) ?
C1 N1 C5 . . 118.8(2) ?
C1 N1 V1 . . 124.72(17) ?
C5 N1 V1 . . 116.13(16) ?
C10 N2 C6 . . 119.2(2) ?
C10 N2 V1 . . 120.53(17) ?
C6 N2 V1 . . 120.24(16) ?
C11 N3 C15 . . 118.3(2) ?
C11 N3 V2 . . 123.87(16) ?
C15 N3 V2 . . 117.67(16) ?
C20 N4 C16 . . 118.7(2) ?
C20 N4 V2 . . 121.31(16) ?
C16 N4 V2 . . 119.75(16) ?
N1 C1 C2 . . 122.8(3) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C3 C2 C1 . . 118.5(3) ?
C3 C2 H2 . . 120.7 ?
C1 C2 H2 . . 120.7 ?
C2 C3 C4 . . 119.3(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.2(3) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N1 C5 C4 . . 121.3(2) ?
N1 C5 C6 . . 114.9(2) ?
C4 C5 C6 . . 123.7(2) ?
N2 C6 C7 . . 120.9(2) ?
N2 C6 C5 . . 115.4(2) ?
C7 C6 C5 . . 123.6(2) ?
C8 C7 C6 . . 119.5(3) ?
C8 C7 H7 . . 120.2 ?
C6 C7 H7 . . 120.2 ?
C9 C8 C7 . . 119.2(3) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 119.2(3) ?
C8 C9 H9 . . 120.4 ?
C10 C9 H9 . . 120.4 ?
N2 C10 C9 . . 122.0(3) ?
N2 C10 H10 . . 119.0 ?
C9 C10 H10 . . 119.0 ?
N3 C11 C12 . . 122.9(2) ?
N3 C11 H11 . . 118.5 ?
C12 C11 H11 . . 118.5 ?
C11 C12 C13 . . 118.9(3) ?
C11 C12 H12 . . 120.6 ?
C13 C12 H12 . . 120.6 ?
C14 C13 C12 . . 118.8(2) ?
C14 C13 H13 . . 120.6 ?
C12 C13 H13 . . 120.6 ?
C13 C14 C15 . . 119.0(2) ?
C13 C14 H14 . . 120.5 ?
C15 C14 H14 . . 120.5 ?
N3 C15 C14 . . 122.0(2) ?
N3 C15 C16 . . 114.8(2) ?
C14 C15 C16 . . 123.2(2) ?
N4 C16 C17 . . 121.9(2) ?
N4 C16 C15 . . 115.8(2) ?
C17 C16 C15 . . 122.3(2) ?
C18 C17 C16 . . 118.7(2) ?
C18 C17 H17 . . 120.6 ?
C16 C17 H17 . . 120.6 ?
C19 C18 C17 . . 119.3(2) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
C18 C19 C20 . . 118.8(2) ?
C18 C19 H19 . . 120.6 ?
C20 C19 H19 . . 120.6 ?
N4 C20 C19 . . 122.6(2) ?
N4 C20 H20 . . 118.7 ?
C19 C20 H20 . . 118.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1 O4 . 1.6464(16) y
Se1 O3 . 1.7210(17) y
Se1 O5 . 1.7439(17) y
V1 O1 . 1.6285(19) y
V1 O2 . 1.6292(17) y
V1 O3 . 1.9466(18) y
V1 N2 . 2.142(2) y
V1 N1 . 2.274(2) y
V1 O4 2_666 2.3511(18) y
V2 O7 . 1.6084(18) y
V2 O6 . 1.7337(16) y
V2 O5 . 1.9093(18) y
V2 O6 2_567 1.9876(18) y
V2 N4 . 2.210(2) y
V2 N3 . 2.289(2) y
V2 V2 2_567 2.8135(12) ?
O4 V1 2_666 2.3511(18) ?
O6 V2 2_567 1.9876(18) ?
N1 C1 . 1.339(3) ?
N1 C5 . 1.345(3) ?
N2 C10 . 1.341(3) ?
N2 C6 . 1.354(3) ?
N3 C11 . 1.334(3) ?
N3 C15 . 1.344(3) ?
N4 C20 . 1.339(3) ?
N4 C16 . 1.346(3) ?
C1 C2 . 1.382(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.376(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.384(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.391(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.477(4) ?
C6 C7 . 1.386(4) ?
C7 C8 . 1.384(4) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.370(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.387(4) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.374(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.382(4) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.381(4) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.386(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.481(3) ?
C16 C17 . 1.392(3) ?
C17 C18 . 1.384(4) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.382(4) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.383(4) ?
C19 H19 . 0.9300 ?
C20 H20 . 0.9300 ?
