#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114851.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4114851
loop_
_publ_author_name
'Jesse L. C. Rowsell'
'Nicholas J. Taylor'
'Linda F. Nazar'
_publ_section_title
;
 Structure and Ion Exchange Properties of a New Cobalt Borate with a
 Tunnel Structure "Templated" by Na+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6522
_journal_page_last               6523
_journal_paper_doi               10.1021/ja020106p
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'B12 Co2 H4 Li2 O23'
_chemical_formula_weight         633.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.9100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4296(7)
_cell_length_b                   4.5518(2)
_cell_length_c                   19.5893(8)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      34.98
_cell_measurement_theta_min      2.42
_cell_volume                     1508.56(11)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      295(1)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX '
_diffrn_measurement_method       Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11583
_diffrn_reflns_theta_full        34.98
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.6494
_exptl_absorpt_correction_T_min  0.5532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Bronze
_exptl_crystal_density_diffrn    2.789
_exptl_crystal_description       'prism fragment '
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.904
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.904
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                2814
_reflns_number_total             3264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020106p_2.cif
_cod_data_source_block           co974m_H4B12Co2Li2O23
_cod_original_formula_sum        'H4 B12 Co2 Li2 O23'
_cod_database_code               4114851
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.5496 0.0173 0.4462 0.00980(9) Uani 0.5590(7) 1 d P
Co2 Co 0.5637 -0.0275 0.4594 0.00980(9) Uani 0.4410(7) 1 d P
O1 O 0.2500 1.1194(4) 0.0000 0.0109(3) Uani 1 2 d S
O2 O 0.21972(7) 0.7534(3) 0.07861(6) 0.0145(2) Uani 1 1 d .
O3 O 0.34298(7) 0.7288(3) 0.04566(6) 0.0118(2) Uani 1 1 d .
O4 O 0.31823(8) 0.4471(3) 0.14125(7) 0.0148(2) Uani 1 1 d .
O5 O 0.43997(7) 0.2296(3) 0.13078(6) 0.0116(2) Uani 1 1 d .
O6 O 0.36943(7) 0.0605(3) 0.21348(7) 0.0144(2) Uani 1 1 d .
O7 O 0.48753(7) -0.1844(3) 0.20784(6) 0.0117(2) Uani 1 1 d .
O8 O 0.42500(7) -0.2829(3) 0.30132(6) 0.0124(2) Uani 1 1 d .
O9 O 0.46661(7) -0.6316(3) 0.39533(6) 0.0112(2) Uani 1 1 d .
O10 O 0.45548(7) -0.2024(3) 0.46033(6) 0.0128(2) Uani 1 1 d .
O11 O 0.37702(7) -0.6205(3) 0.47060(6) 0.0106(2) Uani 1 1 d .
B1 B 0.18877(11) 0.9454(4) 0.01623(10) 0.0104(3) Uani 1 1 d .
B2 B 0.29321(11) 0.6407(4) 0.08633(10) 0.0115(3) Uani 1 1 d .
B3 B 0.37715(11) 0.2468(4) 0.16068(10) 0.0115(3) Uani 1 1 d .
B4 B 0.43047(11) -0.1329(4) 0.24255(10) 0.0114(3) Uani 1 1 d .
B5 B 0.49039(11) -0.4720(4) 0.33857(10) 0.0109(3) Uani 1 1 d .
B6 B 0.43358(11) -0.4794(4) 0.44254(10) 0.0092(3) Uani 1 1 d .
O12 O 0.3048 0.2936 0.3150 0.0390(7) Uani 0.67 1 d P
O13 O 0.2391 -0.1407 0.2405 0.0312(11) Uani 0.33 1 d P
Li1 Li 0.3646 0.0421 0.3882 0.060(2) Uiso 0.67 1 d P
Li2 Li 0.1890 0.8076 0.1759 0.060(2) Uiso 0.33 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O10 Co1 O10 82.39(5) . 5_656
O10 Co1 O5 90.18(5) . 4_545
O10 Co1 O5 164.11(5) 5_656 4_545
O10 Co1 O3 167.69(5) . 4_545
O10 Co1 O3 88.41(5) 5_656 4_545
O5 Co1 O3 96.65(5) 4_545 4_545
O10 Co1 O9 87.39(5) . 1_565
O10 Co1 O9 86.63(5) 5_656 1_565
O5 Co1 O9 107.13(4) 4_545 1_565
O3 Co1 O9 100.29(4) 4_545 1_565
O10 Co2 O3 91.48(5) 5_656 4_545
O10 Co2 O10 82.36(5) 5_656 .
O3 Co2 O10 167.37(5) 4_545 .
O10 Co2 O5 168.82(5) 5_656 4_545
O3 Co2 O5 97.26(5) 4_545 4_545
O10 Co2 O5 87.70(5) . 4_545
O10 Co2 O11 91.95(5) 5_656 5_646
O3 Co2 O11 100.87(5) 4_545 5_646
O10 Co2 O11 90.39(5) . 5_646
O5 Co2 O11 93.23(4) 4_545 5_646
B1 O1 B1 112.48(19) 2 .
B2 O2 B1 117.33(13) . .
B2 O2 Li2 112.40(11) . .
B1 O2 Li2 123.32(10) . .
B2 O2 Li1 114.57(11) . 7
B1 O2 Li1 117.61(10) . 7
B2 O3 B1 118.78(13) . 2
B2 O3 Co2 119.22(11) . 4
B1 O3 Co2 117.77(9) 2 4
B2 O3 Co1 120.27(11) . 4
B1 O3 Co1 119.89(9) 2 4
B3 O4 B2 136.43(15) . .
B3 O5 B5 120.75(13) . 4
B3 O5 Co1 120.31(11) . 4
B5 O5 Co1 118.29(9) 4 4
B3 O5 Co2 118.17(11) . 4
B5 O5 Co2 121.04(10) 4 4
B3 O6 B4 119.75(14) . .
B4 O7 B5 122.73(14) . 4
B4 O8 B5 120.58(13) . .
B4 O8 Li2 117.36(10) . 7
B5 O8 Li2 120.79(10) . 7
B4 O8 Li1 112.43(10) . .
B5 O8 Li1 112.73(9) . .
Li2 O8 Li1 50.60(2) 7 .
B6 O9 B5 119.72(13) . .
B6 O9 Co1 112.95(10) . 1_545
B5 O9 Co1 115.02(10) . 1_545
B6 O9 Li1 85.65(9) . 1_545
B5 O9 Li1 129.00(10) . 1_545
Co1 O9 Li1 88.47(4) 1_545 1_545
B6 O10 Co2 127.69(11) . 5_656
B6 O10 Co1 128.88(11) . .
B6 O10 Co1 123.52(11) . 5_656
Co1 O10 Co1 97.61(5) . 5_656
B6 O10 Co2 124.63(11) . .
Co2 O10 Co2 97.64(5) 5_656 .
B6 O10 Li1 101.34(10) . .
Co2 O10 Li1 90.55(5) 5_656 .
Co1 O10 Li1 98.56(5) . .
Co1 O10 Li1 101.04(5) 5_656 .
Co2 O10 Li1 109.00(5) . .
B6 O11 B1 118.34(13) . 7
B6 O11 Co2 108.09(10) . 5_646
B1 O11 Co2 123.73(10) 7 5_646
B6 O11 Li1 89.21(9) . 1_545
B1 O11 Li1 124.34(10) 7 1_545
Co2 O11 Li1 84.11(4) 5_646 1_545
O1 B1 O11 113.31(14) . 7
O1 B1 O2 111.41(13) . .
O11 B1 O2 108.51(13) 7 .
O1 B1 O3 108.84(13) . 2
O11 B1 O3 109.50(13) 7 2
O2 B1 O3 104.92(13) . 2
O2 B2 O3 122.53(16) . .
O2 B2 O4 116.29(15) . .
O3 B2 O4 121.00(15) . .
O4 B3 O5 123.38(16) . .
O4 B3 O6 115.00(15) . .
O5 B3 O6 121.61(16) . .
O7 B4 O8 123.18(16) . .
O7 B4 O6 119.04(15) . .
O8 B4 O6 117.44(15) . .
O7 B5 O9 108.21(13) 4_545 .
O7 B5 O8 111.79(14) 4_545 .
O9 B5 O8 109.78(14) . .
O7 B5 O5 110.12(14) 4_545 4_545
O9 B5 O5 110.02(14) . 4_545
O8 B5 O5 106.91(13) . 4_545
O10 B6 O9 120.40(15) . .
O10 B6 O11 120.99(15) . .
O9 B6 O11 118.61(15) . .
Li2 O12 Li1 120.583(2) 7_565 .
O12 Li1 O10 166.02(3) . .
O12 Li1 O11 94.07(3) . 1_565
O10 Li1 O11 87.27(4) . 1_565
O12 Li1 O2 107.55(3) . 7
O10 Li1 O2 85.90(4) . 7
O11 Li1 O2 99.47(4) 1_565 7
O12 Li1 O9 86.21(3) . 1_565
O10 Li1 O9 81.84(4) . 1_565
O11 Li1 O9 64.26(4) 1_565 1_565
O2 Li1 O9 159.94(4) 7 1_565
O12 Li1 O8 94.65(3) . .
O10 Li1 O8 77.93(4) . .
O11 Li1 O8 150.98(4) 1_565 .
O2 Li1 O8 104.14(4) 7 .
O9 Li1 O8 88.79(4) 1_565 .
O12 Li2 O13 107.066(1) 7_565 7
O13 Li2 O2 127.41(3) 1_565 .
O12 Li2 O2 100.46(3) 7_565 .
O13 Li2 O2 117.30(3) 7 .
O13 Li2 O8 103.50(3) 1_565 7
O12 Li2 O8 93.90(3) 7_565 7
O13 Li2 O8 104.14(3) 7 7
O2 Li2 O8 129.07(5) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O10 1.9966(12) .
Co1 O10 2.0371(12) 5_656
Co1 O5 2.0379(12) 4_545
Co1 O3 2.0771(11) 4_545
Co1 O9 2.2238(12) 1_565
Co2 O10 1.9826(12) 5_656
Co2 O3 2.0229(12) 4_545
Co2 O10 2.0521(12) .
Co2 O5 2.0725(12) 4_545
Co2 O11 2.1982(12) 5_646
O1 B1 1.425(2) 2
O1 B1 1.425(2) .
O2 B2 1.354(2) .
O2 B1 1.494(2) .
O2 Li2 2.1145(12) .
O2 Li1 2.2029(12) 7
O3 B2 1.371(2) .
O3 B1 1.557(2) 2
O3 Co2 2.0229(11) 4
O3 Co1 2.0771(11) 4
O4 B3 1.357(2) .
O4 B2 1.378(2) .
O5 B3 1.362(2) .
O5 B5 1.525(2) 4
O5 Co1 2.0379(12) 4
O5 Co2 2.0725(11) 4
O6 B3 1.369(2) .
O6 B4 1.393(2) .
O7 B4 1.353(2) .
O7 B5 1.441(2) 4
O8 B4 1.361(2) .
O8 B5 1.474(2) .
O8 Li2 2.1417(12) 7
O8 Li1 2.6560(12) .
O9 B6 1.386(2) .
O9 B5 1.469(2) .
O9 Co1 2.2238(12) 1_545
O9 Li1 2.2947(12) 1_545
O10 B6 1.339(2) .
O10 Co2 1.9826(12) 5_656
O10 Co1 2.0371(12) 5_656
O10 Li1 2.1607(12) .
O11 B6 1.395(2) .
O11 B1 1.469(2) 7
O11 Co2 2.1982(12) 5_646
O11 Li1 2.2006(12) 1_545
B1 O11 1.469(2) 7
B1 O3 1.557(2) 2
B5 O7 1.441(2) 4_545
B5 O5 1.525(2) 4_545
O12 Li2 1.8248 7_565
O12 Li1 1.9316 .
O13 Li2 1.9602 7
Li1 O11 2.2006(12) 1_565
Li1 O2 2.2029(12) 7
Li1 O9 2.2947(12) 1_565
Li2 O12 1.8248 7_565
Li2 O13 1.9602 7
Li2 O8 2.1417(12) 7
