#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/40/2014094.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_2014094
loop_
_publ_author_name
'Höwing, Jonas'
'Gustafsson, Torbjörn'
'Thomas, John O.'
_publ_section_title
;
 Lithium vanadate Li₃₊ₓV₆O₁₃ at low temperature
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i66
_journal_page_last               i68
_journal_paper_doi               10.1107/S0108270104012508
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'Li3.24 V6 O13'
_chemical_formula_moiety         'Li3.24 V6 O13'
_chemical_formula_sum            'Li3.24 O13 V6'
_chemical_formula_weight         536.3
_chemical_name_common            'lithium hexavanadate'
_chemical_name_systematic        ' ?'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 111.913(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.487(5)
_cell_length_b                   3.9200(10)
_cell_length_c                   11.738(5)
_cell_measurement_reflns_used    1332
_cell_measurement_temperature    95
_cell_measurement_theta_max      100.737
_cell_measurement_theta_min      5.015
_cell_volume                     917.2(5)
_computing_cell_refinement       'SAINT-Plus (Bruker 2003)'
_computing_data_collection       'SMART (Bruker 2003)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'Diamond  (Berghoff, 1996)'
_computing_publication_material  Jana2000
_computing_structure_refinement  'Jana2000 (Petricek and Dusek, 2000)'
_computing_structure_solution    'program (reference)'
_diffrn_ambient_temperature      95
_diffrn_detector_area_resol_mean 512*512
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.872
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6862
_diffrn_reflns_theta_full        50.13
_diffrn_reflns_theta_max         50.52
_diffrn_reflns_theta_min         2.51
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.337
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.882(2)
_exptl_crystal_description       shard
_exptl_crystal_F_000             1007
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.17
_refine_diff_density_min         -3.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.15
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2499
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.0094
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/σ²(I)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                2499
_reflns_number_total             2500
_reflns_threshold_expression     I>-15σ(I)
_cod_data_source_file            bc1040.cif
_cod_data_source_block           I
_cod_original_cell_volume        917.3(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014094
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
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
V1 0.25074(2) 0.2505(3) 0.15895(4) 0.00891(9) Uani d . 1 . . V
V2 0.43362(2) 0.2602(2) 0.28384(3) 0.00776(10) Uani d . 1 . . V
V3 0.06766(2) 0.2437(3) 0.04010(3) 0.00708(10) Uani d . 1 . . V
O1 0.24970(10) 0.2513(12) 0.32840(15) 0.0100(4) Uani d . 1 . . O
O2 0.05420(10) 0.2553(10) 0.19755(15) 0.0083(4) Uani d . 1 . . O
O3 0.45260(10) 0.2484(10) 0.46420(14) 0.0081(4) Uani d . 1 . . O
O4 0.25 0.25 0 0.0103(6) Uani d . 1 . . O
O5 0.35033(9) 0.2527(10) 0.22231(14) 0.0090(4) Uani d . 1 . . O
O6 0.14983(9) 0.2503(10) 0.08635(14) 0.0090(4) Uani d . 1 . . O
O7 0.45761(10) 0.2556(9) 0.13822(14) 0.0085(4) Uani d . 1 . . O
Li1 0.0450(3) 0.259(2) 0.3629(4) 0.0127(8) Uiso d . 1 . . Li
Li2 0.25 0.25 0.5 0.061(8) Uani d . 1 . . Li
Li3 0.155(2) 0.26(2) 0.270(3) 0.0127(8) Uiso d . 0.12(2) . . Li
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li 0.000 0.000 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
O 0.018 0.010 'International Tables Vol C Tables  4.2.6.8 and 6.1.1.4'
V 0.356 0.783 '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
O1 V1 O1 . 6_545 85.62(14) no
O1 V1 O1 . 6_555 85.51(14) no
O1 V1 O4 . . 178.95(6) no
O1 V1 O5 . . 92.18(7) no
O1 V1 O6 . . 90.65(7) no
O1 V1 O1 6_545 . 85.62(14) no
O1 V1 O1 6_545 6_555 171.12(11) no
O1 V1 O4 6_545 . 94.38(8) no
O1 V1 O5 6_545 . 90.66(13) no
O1 V1 O6 6_545 . 89.78(13) no
O1 V1 O1 6_555 . 85.51(14) no
O1 V1 O1 6_555 6_545 171.12(11) no
O1 V1 O4 6_555 . 94.49(8) no
O1 V1 O5 6_555 . 90.10(13) no
O1 V1 O6 6_555 . 89.90(13) no
O4 V1 O5 . . 88.87(4) no
O4 V1 O6 . . 88.31(4) no
O5 V1 O6 . . 177.16(6) no
O2 V2 O2 6_545 6_555 164.23(7) no
O2 V2 O3 6_545 . 83.90(12) no
O2 V2 O5 6_545 . 96.12(15) no
O2 V2 O7 6_545 . 91.15(12) no
O2 V2 O7 6_545 2_655 82.48(11) no
O2 V2 O2 6_555 6_545 164.23(7) no
O2 V2 O3 6_555 . 86.53(12) no
O2 V2 O5 6_555 . 98.21(15) no
O2 V2 O7 6_555 . 92.23(12) no
O2 V2 O7 6_555 2_655 83.29(11) no
O3 V2 O5 . . 102.75(8) no
O3 V2 O7 . . 154.92(8) no
O3 V2 O7 . 2_655 77.96(7) no
O5 V2 O7 . . 102.22(7) no
O5 V2 O7 . 2_655 178.37(16) no
O7 V2 O7 . 2_655 77.02(7) no
O7 V2 O7 2_655 . 77.02(7) no
O2 V3 O3 . 6_545 86.48(13) no
O2 V3 O3 . 6_555 84.03(13) no
O2 V3 O3 . 8_454 81.38(7) no
O2 V3 O6 . . 101.86(7) no
O2 V3 O7 . 7_555 157.23(9) no
O3 V3 O3 6_545 6_555 155.86(9) no
O3 V3 O3 6_545 8_454 79.05(12) no
O3 V3 O6 6_545 . 102.79(16) no
O3 V3 O7 6_545 7_555 90.20(11) no
O3 V3 O3 6_555 6_545 155.86(9) no
O3 V3 O3 6_555 8_454 77.62(12) no
O3 V3 O6 6_555 . 100.87(16) no
O3 V3 O7 6_555 7_555 90.04(11) no
O3 V3 O3 8_454 6_545 79.05(12) no
O3 V3 O3 8_454 6_555 77.62(12) no
O3 V3 O6 8_454 . 176.32(10) no
O3 V3 O7 8_454 7_555 75.88(7) no
O6 V3 O7 . 7_555 100.84(8) no
O2 Li1 O2 . 2_555 97.70(19) no
O2 Li1 O3 . 7_556 173.3(3) no
O2 Li1 O7 . 6_545 89.9(3) no
O2 Li1 O7 . 6_555 90.8(3) no
O2 Li1 O2 2_555 . 97.70(19) no
O2 Li1 O3 2_555 7_556 88.9(3) no
O2 Li1 O7 2_555 6_545 88.0(3) no
O2 Li1 O7 2_555 6_555 88.9(3) no
O3 Li1 O7 7_556 6_545 89.0(3) no
O3 Li1 O7 7_556 6_555 90.6(3) no
O7 Li1 O7 6_545 6_555 176.9(4) no
O7 Li1 O7 6_555 6_545 176.9(4) no
O1 Li2 O1 . 7_556 180 no
O1 Li2 O4 . 6_545 90.11(11) no
O1 Li2 O4 . 6_555 89.89(11) no
O1 Li2 O1 7_556 . 180 no
O1 Li2 O4 7_556 6_545 89.89(11) no
O1 Li2 O4 7_556 6_555 90.11(11) no
O4 Li2 O4 6_545 6_555 180 no
O4 Li2 O4 6_555 6_545 180 no
O1 Li3 O2 . . 176(3) no
O1 Li3 O5 . 6_545 92(3) no
O1 Li3 O5 . 6_555 94(3) no
O1 Li3 O6 . . 90.5(19) no
O2 Li3 O5 . 6_545 86(2) no
O2 Li3 O5 . 6_555 88(2) no
O2 Li3 O6 . . 86.0(11) no
O5 Li3 O5 6_545 6_555 170(3) no
O5 Li3 O6 6_545 . 93(2) no
O5 Li3 O5 6_555 6_545 170(3) no
O5 Li3 O6 6_555 . 95(3) no
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
V1 O1 . . 1.997(3) no
V1 O1 . 6_545 1.964(4) yes
V1 O1 . 6_555 1.968(4) yes
V1 O4 . . 1.8598(5) yes
V1 O5 . . 1.986(2) yes
V1 O6 . . 2.012(2) yes
V2 O2 . 6_545 1.999(4) yes
V2 O2 . 6_555 1.959(4) yes
V2 O3 . . 2.0010(10) yes
V2 O5 . . 1.661(2) yes
V2 O7 . . 1.961(2) yes
V2 O7 . 2_655 2.169(2) yes
V3 O2 . . 1.9743(16) yes
V3 O3 . 6_545 1.988(4) yes
V3 O3 . 6_555 2.021(4) yes
V3 O3 . 8_454 2.294(2) yes
V3 O6 . . 1.642(2) yes
V3 O7 . 7_555 1.9560(10) yes
Li1 O2 . . 2.024(6) yes
Li1 O2 . 2_555 1.979(6) yes
Li1 O3 . 7_556 2.011(5) yes
Li1 O7 . 6_545 1.974(9) yes
Li1 O7 . 6_555 1.948(9) yes
Li2 O1 . . 2.012(3) yes
Li2 O1 . 7_556 2.012(3) yes
Li2 O4 . 6_545 1.9600(10) yes
Li2 O4 . 6_555 1.9600(10) yes
Li3 O1 . . 1.89(4) yes
Li3 O2 . . 2.01(4) yes
Li3 O5 . 6_545 2.00(8) yes
Li3 O5 . 6_555 1.94(8) yes
Li3 O6 . . 2.12(4) yes
