##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
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##############################################################################
data_global
_audit_creation_method     'by teXsan'
_journal_date_recd_electronic     2001-05-21
_journal_date_accepted     2001-09-10
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2001
_journal_volume     57
_journal_issue     12
_journal_page_first     1378
_journal_page_last     1380
_journal_paper_category     FM
_publ_contact_author_name     'Toshihiro Yamase'
_publ_contact_author_address
;
Research Laboratory of Resources Utilization
Tokyo Institute of Technology
4259 Nagatsuta
Midori-ku
Yokohama 226-8503
Japan
;
_publ_contact_author_email
                              'tyamase@res.titech.ac.jptyamase@res.titech.ac.jp'
_publ_contact_author_fax     '+81-(0)45-924-5276'
_publ_contact_author_phone     '+81-(0)45-924-5260'
_publ_section_title
;
A three-dimensional inorganic/organic hybrid vanadium oxide with a
pentacoordinate Co(II) complex, [Co(4,4'-bipy)V₂O₆]
;
loop_
    _publ_author_name
    _publ_author_address
    'Yang, Lan'
;
Chemical Resources Laboratory
Tokyo Institute of Technology
4259 Nagatsuta
Midori-ku
Yokohama 226-8503
Japan
;
    'Naruke, Haruo'
;
Chemical Resources Laboratory
Tokyo Institute of Technology
4259 Nagatsuta
Midori-ku
Yokohama 226-8503
Japan
;
    'Yamase, Toshihiro'
;
Chemical Resources Laboratory
Tokyo Institute of Technology
4259 Nagatsuta
Midori-ku
Yokohama 226-8503
Japan
;
data_I
_chemical_formula_moiety     'C10 H8 Co N2 O6 V2'
_chemical_formula_sum     'C10 H8 Co N2 O6 V2'
_chemical_formula_iupac     '[Co (C10 H8 N2) V2 O6]'
_chemical_formula_weight     412.99
_chemical_melting_point     ?
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'P-1'
loop_
    _symmetry_equiv_pos_as_xyz
    x,y,z
    -x,-y,-z
_cell_length_a     8.1634(9)
_cell_length_b     8.5720(10)
_cell_length_c     10.1710(10)
_cell_angle_alpha     87.079(5)
_cell_angle_beta     75.833(4)
_cell_angle_gamma     75.233(6)
_cell_volume     667.2(2)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     3503
_cell_measurement_theta_min     3.1
_cell_measurement_theta_max     27.5
_cell_measurement_temperature     296
_exptl_crystal_description     'plate'
_exptl_crystal_colour     'black'
_exptl_crystal_size_max      .2
_exptl_crystal_size_mid      .2
_exptl_crystal_size_min      .1
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     2.055
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     406
_exptl_absorpt_coefficient_mu     2.627
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(software?; Higashi, 1995)'
_exptl_absorpt_correction_T_min      .597
_exptl_absorpt_correction_T_max      .769
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .7107
_diffrn_measurement_device_type     'Rigaku RAXIS-RAPID imaging-plate'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     10.00
_diffrn_reflns_number     3920
_diffrn_reflns_av_R_equivalents      .032
_diffrn_reflns_theta_max     27.47
_diffrn_reflns_theta_full     27.47
_diffrn_measured_fraction_theta_max      .971
_diffrn_measured_fraction_theta_full      .971
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_h_max     10
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     10
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_number     0
_diffrn_standards_decay_%     0
_refine_special_details
;
Refinement using reflections with F² > 1.0 sigma(F²). The weighted
R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are
based on F. The threshold expression of F² > 2.0 sigma(F²) is used only
for calculating R-factor (gt).
;
_reflns_number_total     2961
_reflns_number_gt     2174
_reflns_threshold_expression     F²>2σ(F²)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_R_factor_gt      .044
_refine_ls_wR_factor_ref      .174
_refine_ls_goodness_of_fit_ref     1.924
_refine_ls_number_reflns     2340
_refine_ls_number_parameters     190
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                    'w = 1/[σ²(Fo²) + {0.085[Max(Fo²,0) + 2Fc²]/3}²]'
_refine_ls_shift/su_max      .002
_refine_diff_density_max      .93
_refine_diff_density_min      -.82
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details     ?
_refine_ls_abs_structure_Flack     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'Co' 'Co'  .349  .972
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
    'V' 'V'  .300  .529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
    'O' 'O'  .011  .006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
    'N' 'N'  .006  .003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
    'C' 'C'  .003  .002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
    'H' 'H'  .000  .000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
_computing_data_collection     'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement     'PROCESS-AUTO'
_computing_data_reduction     'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_structure_solution     'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement
                                'TEXSAN (Molecular Structure Corporation, 1985)'
_computing_molecular_graphics     'ORTEPII (Johnson, 1976)'
_computing_publication_material
                                'TEXSAN (Molecular Structure Corporation, 1999)'
loop_
    _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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Co  .15624(4)  -.33906(5)  -.94205(3)  .01490(10)
                                                    Uani d . 1.00 . . Co
    V1  .23138(5)  -.77366(6)  -.96987(4)  .01610(10)
                                                    Uani d . 1.00 . . V
    V2  .37325(5)  -.09006(6)  -.80229(4)  .01500(10)
                                                    Uani d . 1.00 . . V
    O1  .2178(2)  -.5793(3)  -.9527(2)  .0230(5) Uani d . 1.00 . . O
    O2  .2707(2)  -.1978(3)  -.8703(2)  .0219(5) Uani d . 1.00 . . O
    O3  .3483(3)  -.1289(3)  -.6422(2)  .0261(5) Uani d . 1.00 . . O
    O4  .2811(2)  -.8774(3)  -.8225(2)  .0219(5) Uani d . 1.00 . . O
    O5  -.0414(2)  -.2058(3) -1.0122(2)  .0241(5) Uani d . 1.00 . . O
    O6  .3953(2)  -.8565(3) -1.1148(2)  .0227(5) Uani d . 1.00 . . O
    N1  -.0205(3)  -.3466(3)  -.7485(2)  .0220(6) Uani d . 1.00 . . N
    N2  .3334(3)  -.3351(3) -1.1342(2)  .0170(5) Uani d . 1.00 . . N
    C1  -.0876(4)  -.4734(4)  -.7077(3)  .0285(8) Uani d . 1.00 . . C
    C2  -.2165(4)  -.4741(4)  -.5889(3)  .0244(7) Uani d . 1.00 . . C
    C3  -.2807(3)  -.3344(4)  -.5066(3)  .0206(7) Uani d . 1.00 . . C
    C4  -.2121(4)  -.2035(4)  -.5482(3)  .0254(7) Uani d . 1.00 . . C
    C5  -.0828(4)  -.2136(4)  -.6687(3)  .0231(7) Uani d . 1.00 . . C
    C6  .3272(4)  -.2039(4) -1.2104(3)  .0230(7) Uani d . 1.00 . . C
    C7  .4490(4)  -.1956(4) -1.3333(3)  .0238(7) Uani d . 1.00 . . C
    C8  .4621(3)  -.4661(4) -1.1791(3)  .0209(7) Uani d . 1.00 . . C
    C9  .5889(3)  -.4702(4) -1.3004(3)  .0235(7) Uani d . 1.00 . . C
    C10  -.4169(3)  -.3331(4)  -.3789(3)  .0198(7) Uani d . 1.00 . . C
    H1  -.2629  -.5802  -.5582  .0330 Uiso calc . 1.00 . . H
    H2  -.2516  -.1051  -.4763  .0330 Uiso calc . 1.00 . . H
    H3  -.0239  -.1138  -.6984  .0330 Uiso calc . 1.00 . . H
    H4  -.0547  -.5725  -.7778  .0330 Uiso calc . 1.00 . . H
    H5  .4602  -.5693 -1.1143  .0330 Uiso calc . 1.00 . . H
    H6  .6811  -.5872 -1.3214  .0330 Uiso calc . 1.00 . . H
    H7  .4386  -.0808 -1.3831  .0330 Uiso calc . 1.00 . . H
    H8  .2379  -.0889 -1.1787  .0330 Uiso calc . 1.00 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Co  .0141(2)  .0166(3)  .0124(2)  -.0029(2)  -.0006(2)  -.0019(2)
    V1  .0128(2)  .0169(3)  .0162(2)  -.0014(2)  -.0008(2)  -.0009(2)
    V2  .0148(2)  .0174(3)  .0114(2)  -.0019(2)  -.0020(2)  -.0023(2)
    O1  .0258(9)  .0143(8)  .0230(10)
                                     -.0009(8)  .0014(8)  -.0019(9)
    O2  .0197(10)  .0250(10)
                            .0240(10)
                                     -.0109(8)  -.0035(8)  -.0053(9)
    O3  .0390(10)
                 .0230(10)
                          .0127(8)  -.0044(9)  -.0040(8)  .0018(9)
    O4  .0249(10)  .0170(10)
                            .0222(9)  .0016(8)  -.0097(8)  -.0005(8)
    O5  .0164(9)  .0300(10)
                           .0230(10)
                                    -.0017(8)  -.0035(7)  .0026(9)
    O6  .0172(8)  .0240(10)
                           .0241(10)  -.0036(8)  -.0005(7)  -.0078(9)
    N1  .0178(10)  .0320(10)
                            .0139(10)  -.0067(9)  .0023(7)  -.0068(10)
    N2  .0144(9)  .0200(10)
                           .0157(10)  -.0087(8)  .0038(7)  -.0019(8)
    C1  .0270(10)
                 .031(2)  .0240(10)
                                   -.0130(10)
                                             .0100(10)
                                                      -.0140(10)
    C2  .0320(10)
                 .019(2)  .0210(10)
                                   -.0140(10)
                                             .0043(10)  .0010(10)
    C3  .0170(10)
                 .030(2)  .0120(10)
                                   -.0060(10)
                                             .0017(9)  -.0020(10)
    C4  .0220(10)
                 .026(2)  .0240(10)
                                   -.0070(10)
                                             .0046(9)  -.0060(10)
    C5  .0280(10)
                 .0110(10)
                          .0240(10)
                                   -.0060(10)
                                             .0051(10)  .0010(10)
    C6  .0240(10)
                 .0190(10)
                          .0210(10)
                                   .0010(10)
                                            -.0024(9)  -.0037(10)
    C7  .0270(10)
                 .021(2)  .0210(10)
                                   -.0050(10)
                                             -.0017(10)  -.0010(10)
    C8  .0180(10)
                 .022(2)  .0180(10)
                                   -.0050(10)  .0048(9)  .0040(10)
    C9  .0140(10)
                 .032(2)  .0200(10)
                                   -.0050(10)
                                             .0041(9)  .0000(10)
    C10  .0150(10)
                  .030(2)  .0130(10)
                                    -.0050(10)
                                              -.0001(8)  -.0070(10)
_geom_special_details
;
 ?
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Co O1 . . 1.994(3) yes
    Co O2 . . 1.968(3) yes
    Co O5 . . 1.990(3) yes
    Co N1 . . 2.145(3) yes
    Co N2 . . 2.132(3) yes
    V1 O1 . . 1.657(3) yes
    V1 O4 . . 1.783(3) yes
    V1 O5 . 2_543 1.658(3) yes
    V1 O6 . . 1.768(3) yes
    V2 O2 . . 1.666(3) yes
    V2 O3 . . 1.619(3) yes
    V2 O4 . 1_565 1.809(3) yes
    V2 O6 . 2_643 1.819(3) yes
    N1 C1 . . 1.342(6) no
    N1 C5 . . 1.347(5) no
    N2 C6 . . 1.330(6) no
    N2 C8 . . 1.338(5) no
    C1 C2 . . 1.396(5) no
    C1 H4 . . 1.074 no
    C2 C3 . . 1.406(6) no
    C2 H1 . . 1.075 no
    C3 C4 . . 1.382(6) no
    C3 C10 . . 1.487(5) no
    C4 C5 . . 1.398(5) no
    C4 H2 . . 1.076 no
    C5 H3 . . 1.080 no
    C6 C7 . . 1.405(6) no
    C6 H8 . . 1.076 no
    C7 C10 . 1_654 1.398(5) no
    C7 H7 . . 1.077 no
    C8 C9 . . 1.398(5) no
    C8 H5 . . 1.077 no
    C9 C10 . 1_654 1.384(6) no
    C9 H6 . . 1.084 no
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_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 Co O2 . . . 128.80(10)
                            no
    O1 Co O5 . . . 121.40(10)
                            no
    O1 Co N1 . . . 89.80(10)
                           no
    O1 Co N2 . . . 89.50(10)
                           no
    O2 Co O5 . . . 109.80(10)
                            no
    O2 Co N1 . . . 91.90(10)
                           no
    O2 Co N2 . . . 88.50(10)
                           no
    O5 Co N1 . . . 89.40(10)
                           no
    O5 Co N2 . . . 91.20(10)
                           no
    N1 Co N2 . . . 179.20(10)
                            no
    O1 V1 O4 . . . 109.20(10)
                            no
    O1 V1 O5 . . 2_543 108.80(10)
                                no
    O1 V1 O6 . . . 110.70(10)
                            no
    O4 V1 O5 . . 2_543 109.90(10)
                                no
    O4 V1 O6 . . . 109.50(10)
                            no
    O5 V1 O6 2_543 . . 108.70(10)
                                no
    O2 V2 O3 . . . 109.3(2) no
    O2 V2 O4 . . 1_565 109.60(10)
                                no
    O2 V2 O6 . . 2_643 109.50(10)
                                no
    O3 V2 O4 . . 1_565 109.00(10)
                                no
    O3 V2 O6 . . 2_643 109.30(10)
                                no
    O4 V2 O6 1_565 . 2_643 110.10(10)
                                    no
    Co O1 V1 . . . 168.6(2) no
    Co O2 V2 . . . 175.6(2) no
    V1 O4 V2 . . 1_545 128.9(2) no
    Co O5 V1 . . 2_543 136.5(2) no
    V1 O6 V2 . . 2_643 147.3(2) no
    Co N1 C1 . . . 122.9(3) no
    Co N1 C5 . . . 119.6(3) no
    C1 N1 C5 . . . 117.1(3) no
    Co N2 C6 . . . 122.7(3) no
    Co N2 C8 . . . 119.8(3) no
    C6 N2 C8 . . . 117.5(3) no
    N1 C1 C2 . . . 123.8(4) no
    N1 C1 H4 . . . 117.6 no
    C2 C1 H4 . . . 117.9 no
    C1 C2 C3 . . . 118.6(4) no
    C1 C2 H1 . . . 121.2 no
    C3 C2 H1 . . . 120.2 no
    C2 C3 C4 . . . 117.9(4) no
    C2 C3 C10 . . . 119.4(4) no
    C4 C3 C10 . . . 122.7(4) no
    C3 C4 C5 . . . 119.7(4) no
    C3 C4 H2 . . . 115.6 no
    C5 C4 H2 . . . 124.2 no
    N1 C5 C4 . . . 123.0(4) no
    N1 C5 H3 . . . 117.2 no
    C4 C5 H3 . . . 119.7 no
    N2 C6 C7 . . . 123.7(4) no
    N2 C6 H8 . . . 123.3 no
    C7 C6 H8 . . . 112.6 no
    C6 C7 C10 . . 1_654 118.3(4) no
    C6 C7 H7 . . . 117.8 no
    C10 C7 H7 1_654 . . 123.8 no
    N2 C8 C9 . . . 123.2(4) no
    N2 C8 H5 . . . 114.5 no
    C9 C8 H5 . . . 122.3 no
    C8 C9 C10 . . 1_654 119.2(4) no
    C8 C9 H6 . . . 112.9 no
    C10 C9 H6 1_654 . . 127.9 no
    C3 C10 C7 . . 1_456 122.0(4) no
    C3 C10 C9 . . 1_456 119.8(4) no
    C7 C10 C9 1_456 . 1_456 118.2(4) no
