#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2012180.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_2012180
loop_
_publ_author_name
'Ishizawa, Nobuo'
'Yamashita, Reiko'
'Oishi, Shuji'
'Hester, James R.'
'Kishimoto, Shunji'
_publ_section_title
;
 A synchrotron X-ray study of triclinic LiCa~2~Nb~3~O~10~ with
 perovskite-type slabs
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1006
_journal_page_last               1009
_journal_volume                  57
_journal_year                    2001
_chemical_formula_structural     'Li Ca2 Nb3 O10'
_chemical_formula_sum            'Ca2 Li Nb3 O10'
_chemical_formula_weight         525.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                89.999(4)
_cell_angle_beta                 90.245(4)
_cell_angle_gamma                89.999(5)
_cell_formula_units_Z            4
_cell_length_a                   5.4809(3)
_cell_length_b                   5.4804(3)
_cell_length_c                   26.5533(16)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.74
_cell_measurement_theta_min      32.463
_cell_volume                     797.59(8)
_computing_cell_refinement       'Xtal3.4 (Hall et al., 1995)'
_computing_data_collection       'DIFF14A (Vaalsta & Hester, 1997)'
_computing_data_reduction        Xtal3.4
_computing_molecular_graphics
'ORTEP (Johnson, 1970) and ATOMS (Dowty, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'KEK BL14A four-circle'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     .75008(2)
_diffrn_reflns_av_R_equivalents  .021
_diffrn_reflns_av_sigmaI/netI    .009
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            5607
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         .81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         8
_exptl_absorpt_coefficient_mu    5.565
_exptl_absorpt_correction_T_max  .885
_exptl_absorpt_correction_T_min  .598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             984
_exptl_crystal_size_max          .08
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .03
_refine_diff_density_max         2.13
_refine_diff_density_min         -4.03
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .941
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      .941
_refine_ls_R_factor_all          .059
_refine_ls_R_factor_gt           .051
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.101P)^2^+5.14P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .169
_reflns_number_gt                3750
_reflns_number_total             4904
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    br1337.cif
_[local]_cod_data_source_block   I
_cod_database_code               2012180
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_type_symbol
Nb1 0 0 0 .01101(14) Uani d S 1 Nb
Nb2 0 .5 .5 .01100(14) Uani d S 1 Nb
Nb3 .99467(6) .99965(6) .154237(13) .01070(13) Uani d . 1 Nb
Nb4 .99469(6) .50045(6) .654254(13) .01071(13) Uani d . 1 Nb
Nb5 .5 .5 0 .01103(14) Uani d S 1 Nb
Nb6 .5 0 .5 .01107(14) Uani d S 1 Nb
Nb7 .50344(6) .50842(6) .154250(13) .01073(13) Uani d . 1 Nb
Nb8 .50337(6) .99167(6) .654242(13) .01078(13) Uani d . 1 Nb
Ca1 .00721(19) .49439(18) .08093(4) .0262(3) Uani d . 1 Ca
Ca2 .00730(19) .00563(18) .58089(4) .0261(3) Uani d . 1 Ca
Ca3 .49521(19) .00654(18) .07870(4) .0266(3) Uani d . 1 Ca
Ca4 .49512(19) .49343(18) .57871(4) .0264(3) Uani d . 1 Ca
Li1 .747(2) .760(2) .2606(5) .019(3) Uiso d P .64(3) Li
Li2 .247(2) .259(2) .2403(5) .027(4) Uiso d P .70(4) Li
Li3 .252(4) .752(4) .2487(9) .019(6) Uiso d P .35(3) Li
Li4 .755(4) .252(4) .2485(9) .014(6) Uiso d P .31(3) Li
O1 .2455(7) .7526(6) .14114(19) .0341(9) Uani d . 1 O
O2 .7545(6) .2539(6) .35880(19) .0331(9) Uani d . 1 O
O3 .7453(5) .7570(5) .13183(11) .0129(5) Uani d . 1 O
O4 .2547(5) .2568(5) .36811(11) .0135(5) Uani d . 1 O
O5 .7485(7) .2570(6) .14111(19) .0332(9) Uani d . 1 O
O6 .7494(6) .2433(6) .64121(19) .0329(9) Uani d . 1 O
O7 .2490(6) .2536(5) .15727(12) .0187(6) Uani d . 1 O
O8 .7512(6) .7544(5) .34269(12) .0181(6) Uani d . 1 O
O9 .7998(5) .7000(5) .01381(12) .0162(6) Uani d . 1 O
O10 .1993(5) .1999(5) .48638(11) .0154(5) Uani d . 1 O
O11 .6950(6) .1952(6) .0001(2) .0401(11) Uani d . 1 O
O12 .6961(6) .3045(6) .5001(2) .0399(11) Uani d . 1 O
O13 .5335(7) .5408(7) .22112(12) .0274(8) Uani d . 1 O
O14 .4669(7) .0399(7) .27870(12) .0279(8) Uani d . 1 O
O15 .9636(7) .9703(7) .22111(12) .0269(8) Uani d . 1 O
O16 .9649(7) .5295(7) .72114(12) .0265(8) Uani d . 1 O
O17 .4467(8) .4599(8) .07152(13) .0361(10) Uani d . 1 O
O18 .5525(8) .9605(8) .42844(13) .0364(10) Uani d . 1 O
O19 .0428(8) .0541(8) .07147(13) .0373(10) Uani d . 1 O
O20 .0415(8) .4460(8) .57145(13) .0371(10) Uani d . 1 O
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 .0109(3) .0117(3) .0105(3) .00033(17) .00056(18) .00010(18)
Nb2 .0110(3) .0114(3) .0106(3) -.00187(17) .00051(18) .00087(18)
Nb3 .0093(2) .00845(19) .0144(2) -.00092(13) .00060(14) .00083(14)
Nb4 .0092(2) .00857(19) .0144(2) -.00065(13) .00061(14) .00017(14)
Nb5 .0123(3) .0102(2) .0106(3) .00033(17) .00090(18) .00070(18)
Nb6 .0124(3) .0101(2) .0108(3) -.00175(17) .00097(18) .00029(18)
Nb7 .0097(2) .00812(19) .0143(2) -.00105(13) .00014(14) .00047(13)
Nb8 .0096(2) .00816(19) .0146(2) -.00060(13) .00016(14) .00065(13)
Ca1 .0250(5) .0237(5) .0299(6) -.0038(4) -.0043(4) .0051(4)
Ca2 .0248(5) .0236(5) .0299(6) .0028(4) -.0047(4) -.0046(4)
Ca3 .0272(6) .0251(5) .0276(6) -.0075(4) -.0061(4) .0074(4)
Ca4 .0263(6) .0254(5) .0273(6) .0065(4) -.0066(4) -.0070(4)
O1 .0169(16) .0153(15) .070(3) .0044(12) -.0020(16) -.0006(16)
O2 .0135(15) .0129(14) .073(3) -.0071(11) .0008(16) .0010(15)
O3 .0136(12) .0111(11) .0140(13) -.0063(9) .0001(10) .0002(9)
O4 .0135(12) .0125(12) .0146(13) .0039(9) -.0011(10) -.0003(9)
O5 .0175(16) .0144(15) .068(3) .0040(12) .0024(16) .0019(15)
O6 .0145(15) .0114(14) .073(3) -.0066(11) .0030(16) -.0017(15)
O7 .0195(15) .0161(13) .0205(15) -.0127(11) -.0009(11) .0016(11)
O8 .0195(14) .0162(13) .0185(15) .0071(10) .0011(11) .0001(10)
O9 .0145(13) .0132(12) .0208(14) -.0074(10) -.0043(10) .0067(10)
O10 .0149(13) .0133(12) .0180(14) .0032(9) -.0041(10) -.0040(10)
O11 .0105(14) .0112(13) .099(4) .0019(11) .0010(17) .0007(17)
O12 .0107(14) .0106(13) .099(4) -.0050(11) .0013(17) .0013(16)
O13 .038(2) .0354(18) .0087(13) -.0204(15) .0007(12) .0017(12)
O14 .039(2) .0357(18) .0093(13) .0190(15) .0006(13) .0006(12)
O15 .038(2) .0348(18) .0082(13) -.0201(15) .0004(12) .0003(12)
O16 .0353(19) .0362(18) .0080(13) .0175(14) -.0003(12) .0001(12)
O17 .050(2) .051(2) .0076(14) -.0335(19) .0018(14) -.0010(13)
O18 .049(2) .052(2) .0077(14) .0296(19) .0051(14) .0010(14)
O19 .055(3) .048(2) .0084(14) -.034(2) .0006(15) -.0016(14)
O20 .054(3) .049(2) .0082(14) .031(2) .0008(15) .0029(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -.0010 .0000 'Sasaki (1989)'
Ca Ca .2190 .3410 'Sasaki (1989)'
Nb Nb -1.7990 .6860 'Sasaki (1989)'
O O .0090 .0070 'Sasaki (1989)'
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
O15 Li1 O13 . . 115.6(7) no
O15 Li1 O8 . . 122.6(6) no
O15 Li1 O14 . '1 565' 97.5(5) no
O15 Li1 O16 . '2 766' 95.9(5) no
O13 Li1 O8 . . 121.7(6) no
O13 Li1 O14 . '1 565' 97.3(5) no
O13 Li1 O16 . '2 766' 95.6(5) no
O8 Li1 O14 . '1 565' 78.3(4) no
O8 Li1 O16 . '2 766' 76.9(4) no
O8 Li1 Li4 . '1 565' 97.6(7) no
O8 Li1 Li3 . . 97.0(7) no
O8 Li1 Li3 . '1 655' 96.1(6) no
O8 Li1 Li4 . . 95.8(6) no
O14 Li1 O16 '1 565' '2 766' 155.3(7) no
O16 Li2 O14 '2 666' . 117.1(7) no
O16 Li2 O7 '2 666' . 122.8(6) no
O16 Li2 O13 '2 666' . 97.4(5) no
O16 Li2 O15 '2 666' '1 445' 97.1(5) no
O14 Li2 O7 . . 120.1(6) no
O14 Li2 O13 . . 96.2(5) no
O14 Li2 O15 . '1 445' 96.2(5) no
O7 Li2 O13 . . 77.2(4) no
O7 Li2 O15 . '1 445' 76.9(4) no
O13 Li2 O15 . '1 445' 154.0(7) no
O13 Li3 O16 . '2 666' 98.5(9) no
O13 Li3 O15 . '1 455' 138.9(12) no
O13 Li3 O14 . '1 565' 97.8(9) no
O13 Li3 O1 . . 69.6(7) no
O16 Li3 O15 '2 666' '1 455' 97.1(9) no
O16 Li3 O14 '2 666' '1 565' 135.6(12) no
O16 Li3 O1 '2 666' . 112.1(9) no
O15 Li3 O14 '1 455' '1 565' 97.0(9) no
O15 Li3 O1 '1 455' . 69.3(7) no
O14 Li3 O1 '1 565' . 112.3(9) no
O15 Li4 O16 '1 545' '2 766' 99.0(9) no
O15 Li4 O14 '1 545' . 97.9(9) no
O15 Li4 O13 '1 545' . 139.2(12) no
O15 Li4 O5 '1 545' . 70.0(7) no
O16 Li4 O14 '2 766' . 135.2(12) no
O16 Li4 O13 '2 766' . 97.0(9) no
O16 Li4 O5 '2 766' . 112.6(9) no
O14 Li4 O13 . . 96.5(9) no
O14 Li4 O5 . . 112.2(9) no
O13 Li4 O5 . . 69.2(7) no
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 O19 2 1.934(3) no
Nb1 O19 . 1.934(3) yes
Nb1 O11 '2 655' 1.985(3) no
Nb1 O11 '1 455' 1.985(3) yes
Nb1 O9 '2 665' 2.011(3) no
Nb1 O9 '1 445' 2.011(3) yes
Nb2 O20 '2 566' 1.933(3) no
Nb2 O20 . 1.933(3) yes
Nb2 O12 '2 666' 1.981(3) no
Nb2 O12 '1 455' 1.981(3) yes
Nb2 O10 '2 566' 2.008(3) no
Nb2 O10 . 2.008(3) yes
Nb3 O15 . 1.792(3) yes
Nb3 O1 '1 655' 1.962(4) yes
Nb3 O7 '1 665' 1.971(3) yes
Nb3 O5 '1 565' 1.982(4) yes
Nb3 O3 . 1.996(3) yes
Nb3 O19 '1 665' 2.235(4) yes
Nb4 O16 . 1.791(3) yes
Nb4 O2 '2 766' 1.956(3) yes
Nb4 O8 '2 766' 1.974(3) yes
Nb4 O6 . 1.977(3) yes
Nb4 O4 '2 666' 1.996(3) yes
Nb4 O20 '1 655' 2.235(4) yes
Nb5 O17 '2 665' 1.935(3) no
Nb5 O17 . 1.935(3) yes
Nb5 O11 . 1.983(3) yes
Nb5 O11 '2 665' 1.983(3) no
Nb5 O9 '2 665' 2.008(3) no
Nb5 O9 . 2.008(3) yes
Nb6 O18 '1 545' 1.935(3) yes
Nb6 O18 '2 666' 1.935(3) no
Nb6 O12 '2 656' 1.985(3) no
Nb6 O12 . 1.985(3) yes
Nb6 O10 . 2.010(3) yes
Nb6 O10 '2 656' 2.010(3) no
Nb7 O13 . 1.791(3) yes
Nb7 O5 . 1.957(4) yes
Nb7 O7 . 1.975(3) yes
Nb7 O1 . 1.976(4) yes
Nb7 O3 . 1.994(3) yes
Nb7 O17 . 2.233(4) yes
Nb8 O14 '2 666' 1.796(3) yes
Nb8 O6 '1 565' 1.961(3) yes
Nb8 O8 '2 676' 1.973(3) yes
Nb8 O2 '2 666' 1.981(3) yes
Nb8 O4 '2 666' 1.993(3) yes
Nb8 O18 '2 676' 2.231(4) yes
Ca1 O9 '1 455' 2.392(3) yes
Ca1 O17 . 2.430(5) yes
Ca1 O19 . 2.434(4) yes
Ca1 O3 '1 455' 2.444(3) yes
Ca1 O1 . 2.499(4) yes
Ca1 O5 '1 455' 2.505(4) yes
Ca1 O7 . 2.754(3) yes
Ca1 O9 '2 665' 2.933(3) yes
Ca1 O19 '1 565' 3.084(4) yes
Ca1 O17 '1 455' 3.087(5) yes
Ca1 O11 '1 455' 3.193(4) yes
Ca1 O11 '2 665' 3.196(4) yes
Ca2 O10 '2 556' 2.393(3) yes
Ca2 O18 '2 666' 2.434(5) yes
Ca2 O20 . 2.434(4) yes
Ca2 O4 '2 556' 2.446(3) yes
Ca2 O2 '2 656' 2.505(4) yes
Ca2 O6 '1 455' 2.506(4) yes
Ca2 O8 '2 666' 2.753(3) yes
Ca2 O10 . 2.926(3) yes
Ca2 O18 '2 566' 3.083(5) yes
Ca2 O20 '1 545' 3.083(4) yes
Ca2 O12 '1 455' 3.188(4) yes
Ca2 O12 '2 656' 3.192(4) yes
Ca3 O3 '1 545' 2.392(3) yes
Ca3 O19 . 2.500(5) yes
Ca3 O17 . 2.506(4) yes
Ca3 O5 . 2.557(4) yes
Ca3 O1 '1 545' 2.565(4) yes
Ca3 O11 . 2.578(5) yes
Ca3 O11 '2 655' 2.582(5) yes
Ca3 O7 . 2.834(3) yes
Ca3 O9 '1 545' 2.933(3) yes
Ca3 O17 '1 545' 3.014(4) yes
Ca3 O19 '1 655' 3.020(5) yes
Ca3 O9 '2 665' 3.347(3) yes
Ca4 O4 '2 666' 2.394(3) yes
Ca4 O20 . 2.506(5) yes
Ca4 O18 '2 666' 2.508(4) yes
Ca4 O6 . 2.560(4) yes
Ca4 O2 '2 666' 2.562(4) yes
Ca4 O12 . 2.581(5) yes
Ca4 O12 '2 666' 2.586(5) yes
Ca4 O8 '2 666' 2.837(3) yes
Ca4 O10 '2 666' 2.940(3) yes
Ca4 O18 '2 676' 3.010(4) yes
Ca4 O20 '1 655' 3.013(5) yes
Ca4 O10 . 3.346(3) yes
Li1 O15 . 1.962(12) yes
Li1 O13 . 1.975(12) yes
Li1 O8 . 2.180(14) yes
Li1 O14 '1 565' 2.224(12) yes
Li1 O16 '2 766' 2.289(12) yes
Li2 O16 '2 666' 1.937(12) yes
Li2 O14 . 1.981(12) yes
Li2 O7 . 2.205(14) yes
Li2 O13 . 2.262(12) yes
Li2 O15 '1 445' 2.274(12) yes
Li3 O13 . 2.07(2) yes
Li3 O16 '2 666' 2.11(2) yes
Li3 O15 '1 455' 2.11(2) yes
Li3 O14 '1 565' 2.12(2) yes
Li4 O15 '1 545' 2.06(2) yes
Li4 O16 '2 766' 2.10(2) yes
Li4 O14 . 2.12(2) yes
Li4 O13 . 2.12(2) yes