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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, 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/  #
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#                                                                            #
#            Copyright International Union of Crystallography                #
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##############################################################################
                                             
data_I
_audit_creation_method     SHELXTL-Plus
_chemical_name_systematic
;
tetracobalt diniobium nonaoxide
;
_chemical_name_common     ?
_chemical_formula_moiety     'Co4 Nb2 O9'
_chemical_formula_sum     'Co4 Nb2 O9'
_chemical_formula_iupac     'Co4 Nb2 O9'
_chemical_formula_weight     565.54
_chemical_melting_point     ?
_symmetry_cell_setting     trigonal
_symmetry_space_group_name_H-M     'P -3 c 1'
_symmetry_space_group_name_Hall     '-P 3 2"c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+y, -x, z'
    'y, x, -z+1/2'
    'x-y, -y, -z+1/2'
    '-x, -x+y, -z+1/2'
    '-x, -y, -z'
    'y, -x+y, -z'
    'x-y, x, -z'
    '-y, -x, z-1/2'
    '-x+y, y, z-1/2'
    'x, x-y, z-1/2'
_cell_length_a     5.1736(3)
_cell_length_b     5.1736(3)
_cell_length_c     14.1457(11)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     327.90(4)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     34
_cell_measurement_theta_min     4.54
_cell_measurement_theta_max     29.96
_cell_measurement_temperature     297.0(10)
_exptl_crystal_description     block
_exptl_crystal_colour     violet
_exptl_crystal_size_max     0.12
_exptl_crystal_size_mid     0.07
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     5.728
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     524
_exptl_absorpt_coefficient_mu     13.292
_exptl_absorpt_correction_type     psi-scan
_exptl_absorpt_process_details     '(XSCANS; Siemens, 1996)'
_exptl_absorpt_correction_T_min     0.272
_exptl_absorpt_correction_T_max     0.510
_exptl_special_details     ?
_diffrn_ambient_temperature     297.0(10)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker P4'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     1234
_diffrn_reflns_av_R_equivalents     0.0764
_diffrn_reflns_av_sigmaI/netI     0.0418
_diffrn_reflns_theta_min     2.88
_diffrn_reflns_theta_max     29.95
_diffrn_reflns_theta_full     29.95
_diffrn_measured_fraction_theta_max     0.994
_diffrn_measured_fraction_theta_full     0.994
_diffrn_reflns_limit_h_min     -7
_diffrn_reflns_limit_h_max     7
_diffrn_reflns_limit_k_min     -7
_diffrn_reflns_limit_k_max     7
_diffrn_reflns_limit_l_min     -19
_diffrn_reflns_limit_l_max     19
_diffrn_standards_number     2
_diffrn_standards_interval_count     48
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     1.5
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    -1 0 4
    -1 1 -4
_refine_special_details     ?
_reflns_number_total     328
_reflns_number_gt     262
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0374
_refine_ls_R_factor_gt     0.0309
_refine_ls_wR_factor_gt     0.0762
_refine_ls_wR_factor_ref     0.0794
_refine_ls_goodness_of_fit_ref     1.284
_refine_ls_restrained_S_all     1.284
_refine_ls_number_reflns     328
_refine_ls_number_parameters     25
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     .
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0148P)²+2.3726P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.945
_refine_diff_density_min     -0.798
_refine_ls_extinction_method     SHELXTL-Plus
_refine_ls_extinction_coef     0.0107(11)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Co' 'Co' 0.3494 0.9721
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Nb' 'Nb' -2.0727 0.6215
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'XSCANS (Siemens, 1996)'
_computing_cell_refinement     'XSCANS'
_computing_data_reduction     'XSCANS'
_computing_structure_solution     'SHELXTL-Plus (Sheldrick, 1998)'
_computing_structure_refinement     'SHELXTL-Plus'
_computing_molecular_graphics
                              'CaRIne Crystallography (Boudias & Monceau, 1998)'
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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Nb Nb1 0.0000 0.0000 0.14215(4) 0.0081(3) Uani d S 1 . .
    Co Co1 0.3333 0.6667 0.19304(7) 0.0103(3) Uani d S 1 . .
    Co Co2 0.3333 0.6667 -0.01377(8) 0.0101(3) Uani d S 1 . .
    O O1 0.0000 0.2876(9) 0.2500 0.0091(9) Uani d S 1 . .
    O O2 0.0235(7) 0.6821(7) 0.0847(2) 0.0116(7) Uani d . 1 . .
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
    Nb1 0.0087(3) 0.0087(3) 0.0068(3) 0.00437(15) 0.000 0.000
    Co1 0.0097(4) 0.0097(4) 0.0116(5) 0.0048(2) 0.000 0.000
    Co2 0.0102(4) 0.0102(4) 0.0098(5) 0.0051(2) 0.000 0.000
    O1 0.009(2) 0.0087(14) 0.0095(19) 0.0045(10) 0.0012(15) 0.0006(8)
    O2 0.0103(15) 0.0104(15) 0.0135(15) 0.0049(13) -0.0005(11) -0.0024(12)
_geom_special_details     ?
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
    Nb1 O2 3_455 1.892(3) ?
    Nb1 O2 1_545 1.892(3) yes
    Nb1 O2 2_665 1.892(3) ?
    Nb1 O1 . 2.131(3) yes
    Nb1 O1 3 2.131(3) ?
    Nb1 O1 2 2.131(3) ?
    Co1 O1 3_565 2.022(2) ?
    Co1 O1 . 2.022(2) yes
    Co1 O1 2_665 2.022(2) ?
    Co1 O2 . 2.247(3) yes
    Co1 O2 3_565 2.247(3) ?
    Co1 O2 2_665 2.247(3) ?
    Co2 O2 7_565 2.083(3) ?
    Co2 O2 9_665 2.083(3) ?
    Co2 O2 8 2.083(3) yes
    Co2 O2 3_565 2.155(3) ?
    Co2 O2 . 2.155(3) yes
    Co2 O2 2_665 2.155(3) ?
    O1 Co1 4_455 2.022(2) ?
    O1 Nb1 4 2.131(3) ?
    O2 Nb1 1_565 1.892(3) ?
    O2 Co2 7_565 2.083(3) ?
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
    O2 Nb1 O2 3_455 1_545 102.93(11) ?
    O2 Nb1 O2 3_455 2_665 102.93(11) ?
    O2 Nb1 O2 1_545 2_665 102.93(11) ?
    O2 Nb1 O1 3_455 . 91.50(11) ?
    O2 Nb1 O1 1_545 . 159.50(13) ?
    O2 Nb1 O1 2_665 . 87.65(11) ?
    O2 Nb1 O1 3_455 3 159.50(13) ?
    O2 Nb1 O1 1_545 3 87.65(11) ?
    O2 Nb1 O1 2_665 3 91.50(11) ?
    O1 Nb1 O1 . 3 74.41(13) ?
    O2 Nb1 O1 3_455 2 87.65(11) ?
    O2 Nb1 O1 1_545 2 91.50(11) ?
    O2 Nb1 O1 2_665 2 159.50(13) ?
    O1 Nb1 O1 . 2 74.41(13) ?
    O1 Nb1 O1 3 2 74.41(13) ?
    O1 Co1 O1 3_565 . 105.17(5) ?
    O1 Co1 O1 3_565 2_665 105.17(5) ?
    O1 Co1 O1 . 2_665 105.17(5) ?
    O1 Co1 O2 3_565 . 81.47(11) ?
    O1 Co1 O2 . . 91.63(10) ?
    O1 Co1 O2 2_665 . 159.21(11) ?
    O1 Co1 O2 3_565 3_565 91.63(10) ?
    O1 Co1 O2 . 3_565 159.21(11) ?
    O1 Co1 O2 2_665 3_565 81.47(11) ?
    O2 Co1 O2 . 3_565 78.64(13) ?
    O1 Co1 O2 3_565 2_665 159.21(11) ?
    O1 Co1 O2 . 2_665 81.47(11) ?
    O1 Co1 O2 2_665 2_665 91.63(9) ?
    O2 Co1 O2 . 2_665 78.64(13) ?
    O2 Co1 O2 3_565 2_665 78.64(13) ?
    O2 Co2 O2 7_565 9_665 98.72(12) ?
    O2 Co2 O2 7_565 8 98.72(12) ?
    O2 Co2 O2 9_665 8 98.72(12) ?
    O2 Co2 O2 7_565 3_565 168.48(10) ?
    O2 Co2 O2 9_665 3_565 89.44(12) ?
    O2 Co2 O2 8 3_565 87.97(17) ?
    O2 Co2 O2 7_565 . 89.44(12) ?
    O2 Co2 O2 9_665 . 87.97(16) ?
    O2 Co2 O2 8 . 168.48(10) ?
    O2 Co2 O2 3_565 . 82.70(13) ?
    O2 Co2 O2 7_565 2_665 87.97(16) ?
    O2 Co2 O2 9_665 2_665 168.48(10) ?
    O2 Co2 O2 8 2_665 89.44(12) ?
    O2 Co2 O2 3_565 2_665 82.70(13) ?
    O2 Co2 O2 . 2_665 82.70(13) ?
    Co1 O1 Co1 4_455 . 114.1(2) ?
    Co1 O1 Nb1 4_455 . 131.67(5) ?
    Co1 O1 Nb1 . . 95.40(3) ?
    Co1 O1 Nb1 4_455 4 95.40(3) ?
    Co1 O1 Nb1 . 4 131.67(5) ?
    Nb1 O1 Nb1 . 4 91.44(17) ?
    Nb1 O2 Co2 1_565 7_565 123.06(16) ?
    Nb1 O2 Co2 1_565 . 132.99(17) ?
    Co2 O2 Co2 7_565 . 90.56(12) ?
    Nb1 O2 Co1 1_565 . 95.47(13) ?
    Co2 O2 Co1 7_565 . 129.54(15) ?
    Co2 O2 Co1 . . 83.25(12) ?
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O1 Co1 O1 Co1 3_565 . . 4_455 18.27(8) ?
    O2 Co1 O1 Co1 . . . 4_455 -63.33(8) ?
    O2 Co1 O1 Co1 3_565 . . 4_455 -124.6(3) ?
    O2 Co1 O1 Co1 2_665 . . 4_455 -141.58(9) ?
    O1 Co1 O1 Nb1 3_565 . . . 159.01(15) ?
    O1 Co1 O1 Nb1 2_665 . . . -90.22(9) ?
    O2 Co1 O1 Nb1 . . . . 77.41(11) ?
    O2 Co1 O1 Nb1 3_565 . . . 16.1(3) ?
    O2 Co1 O1 Nb1 2_665 . . . -0.85(10) ?
    O1 Co1 O1 Nb1 3_565 . . 4 -104.22(12) ?
    O1 Co1 O1 Nb1 2_665 . . 4 6.55(19) ?
    O2 Co1 O1 Nb1 . . . 4 174.2(2) ?
    O2 Co1 O1 Nb1 3_565 . . 4 112.9(2) ?
    O2 Co1 O1 Nb1 2_665 . . 4 95.9(2) ?
    O2 Nb1 O1 Co1 3_455 . . 4_455 27.5(2) ?
    O2 Nb1 O1 Co1 1_545 . . 4_455 -107.7(3) ?
    O2 Nb1 O1 Co1 2_665 . . 4_455 130.4(2) ?
    O1 Nb1 O1 Co1 3 . . 4_455 -137.42(16) ?
    O1 Nb1 O1 Co1 2 . . 4_455 -59.7(2) ?
    O2 Nb1 O1 Co1 3_455 . . . -101.88(12) ?
    O2 Nb1 O1 Co1 1_545 . . . 123.0(3) ?
    O2 Nb1 O1 Co1 2_665 . . . 1.00(12) ?
    O1 Nb1 O1 Co1 3 . . . 93.21(11) ?
    O2 Nb1 O1 Nb1 3_455 . . 4 126.02(10) ?
    O2 Nb1 O1 Nb1 1_545 . . 4 -9.1(3) ?
    O2 Nb1 O1 Nb1 2_665 . . 4 -131.10(10) ?
    O2 Co2 O2 Nb1 7_565 . . 1_565 -139.0(3) ?
    O2 Co2 O2 Nb1 9_665 . . 1_565 -40.3(2) ?
    O2 Co2 O2 Nb1 8 . . 1_565 85.6(8) ?
    O2 Co2 O2 Nb1 3_565 . . 1_565 49.4(3) ?
    O2 Co2 O2 Nb1 2_665 . . 1_565 132.96(18) ?
    O2 Co2 O2 Co2 7_565 . . 7_565 0.0 ?
    O2 Co2 O2 Co2 9_665 . . 7_565 98.75(12) ?
    O2 Co2 O2 Co2 8 . . 7_565 -135.4(6) ?
    O2 Co2 O2 Co2 3_565 . . 7_565 -171.55(13) ?
    O2 Co2 O2 Co2 2_665 . . 7_565 -88.03(17) ?
    O2 Co2 O2 Co1 7_565 . . . 129.79(14) ?
    O2 Co2 O2 Co1 9_665 . . . -131.46(11) ?
    O2 Co2 O2 Co1 8 . . . -5.6(7) ?
    O1 Co1 O2 Nb1 3_565 . . 1_565 0.95(12) ?
    O1 Co1 O2 Nb1 . . . 1_565 106.05(14) ?
    O1 Co1 O2 Nb1 2_665 . . 1_565 -109.6(3) ?
    O2 Co1 O2 Nb1 3_565 . . 1_565 -92.46(19) ?
    O2 Co1 O2 Nb1 2_665 . . 1_565 -172.99(15) ?
    O1 Co1 O2 Co2 3_565 . . 7_565 -141.2(2) ?
    O1 Co1 O2 Co2 . . . 7_565 -36.1(2) ?
    O1 Co1 O2 Co2 2_665 . . 7_565 108.3(3) ?
    O2 Co1 O2 Co2 3_565 . . 7_565 125.39(15) ?
    O2 Co1 O2 Co2 2_665 . . 7_565 44.9(2) ?
    O1 Co1 O2 Co2 3_565 . . . 133.68(10) ?
    O1 Co1 O2 Co2 . . . . -121.22(12) ?
    O1 Co1 O2 Co2 2_665 . . . 23.2(3) ?
data_global
_journal_date_recd_electronic     2006-03-21
_journal_date_accepted     2006-04-03
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2006
_journal_volume     62
_journal_issue      5
_journal_page_first     i117
_journal_page_last     i119
_journal_paper_category     EI
_journal_coeditor_code     HB2026
_publ_contact_author_name     'Sylvain Bernès'
_publ_contact_author_address
;
DEP, Facultad de Ciencias Químicas
Universidad Autónoma de Nuevo León
Guerrero y Progreso, S/N, Col. Treviño
Monterrey 64570
Mexico
;
_publ_contact_author_email     sylvain_bernes@hotmail.com
_publ_contact_author_fax     (+52)(81)82204918
_publ_contact_author_phone     (+52)(81)82204900*3460
_publ_section_title
;
Redetermination of Co₄Nb₂O₉ by single-crystal X-ray methods
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    "Castellanos R., María A." .
;
Facultad de Química
Universidad Nacional Autónoma de México
AP 70-197
México DF 04510
Mexico
;
    "Bernès, Sylvain" .
;
DEP, Facultad de Ciencias Químicas
Universidad Autónoma de Nuevo León
Guerrero y Progreso, S/N, Col. Treviño
Monterrey 64570
Mexico
;
    "Vega-González, Marina" .
;
Universidad Nacional Autónoma de México
Facultad de Química
AP 70-197
México DF 04510
Mexico
;
