#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:50:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114850.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_4114850
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 Na2 O21'
_chemical_formula_weight         629.56
_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                 103.212(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1447(15)
_cell_length_b                   4.5530(5)
_cell_length_c                   19.4408(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      14.09
_cell_measurement_theta_min      9.41
_cell_volume                     1477.4(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-UNIX
_computing_publication_material  SHELXTL-UNIX
_computing_structure_refinement  SHELXTL-UNIX
_computing_structure_solution    SHELXTL-UNIX
_diffrn_ambient_temperature      295(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            3355
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        +/-1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Face-indexed analytical '
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    2.830
_exptl_crystal_description       'prism fragment '
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00162(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                2526
_reflns_number_total             3261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020106p_1.cif
_cod_data_source_block           co915B12Co2Na2O21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Integration' changed to
'integration' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4114850
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 0.557353(11) -0.00380(5) 0.451351(10) 0.00957(5) Uani 1 1 d .
O1 O 0.2500 1.1239(3) 0.0000 0.0069(2) Uani 1 2 d S
O2 O 0.21577(6) 0.7570(2) 0.07712(5) 0.00877(18) Uani 1 1 d .
O3 O 0.34342(5) 0.7334(2) 0.04872(5) 0.00808(18) Uani 1 1 d .
O4 O 0.31043(6) 0.4457(2) 0.14338(5) 0.0103(2) Uani 1 1 d .
O5 O 0.43453(6) 0.2305(2) 0.13272(5) 0.00785(17) Uani 1 1 d .
O6 O 0.36588(6) 0.0705(2) 0.22047(5) 0.00968(19) Uani 1 1 d .
O7 O 0.48450(6) -0.1812(2) 0.20829(5) 0.00800(17) Uani 1 1 d .
O8 O 0.42600(6) -0.2818(2) 0.30491(5) 0.00829(18) Uani 1 1 d .
O9 O 0.46947(6) -0.6358(2) 0.39542(5) 0.00697(17) Uani 1 1 d .
O10 O 0.45659(6) -0.2046(2) 0.46039(5) 0.00798(18) Uani 1 1 d .
O11 O 0.37880(5) -0.6276(2) 0.47174(5) 0.00717(17) Uani 1 1 d .
B1 B 0.18756(8) 0.9496(3) 0.01499(7) 0.0065(3) Uani 1 1 d .
B2 B 0.29052(9) 0.6440(3) 0.08783(8) 0.0080(3) Uani 1 1 d .
B3 B 0.37158(9) 0.2501(3) 0.16492(8) 0.0077(2) Uani 1 1 d .
B4 B 0.42783(9) -0.1298(3) 0.24527(8) 0.0074(2) Uani 1 1 d .
B5 B 0.49385(8) -0.4686(3) 0.33859(7) 0.0068(2) Uani 1 1 d .
B6 B 0.43586(8) -0.4825(4) 0.44332(7) 0.0059(2) Uani 1 1 d .
Na1 Na 0.34748(4) 0.05327(14) 0.35692(3) 0.01970(15) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Na Na 0.0362 0.0249 '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 O3 172.98(4) . 4_545
O10 Co1 O10 82.40(4) . 5_656
O3 Co1 O10 90.72(4) 4_545 5_656
O10 Co1 O5 91.01(4) . 4_545
O3 Co1 O5 95.96(4) 4_545 4_545
O10 Co1 O5 171.73(4) 5_656 4_545
O10 Co1 O11 84.46(4) . 5_646
O3 Co1 O11 96.48(4) 4_545 5_646
O10 Co1 O11 85.60(4) 5_656 5_646
O5 Co1 O11 88.82(4) 4_545 5_646
O10 Co1 O9 83.74(4) . 1_565
O3 Co1 O9 94.00(4) 4_545 1_565
O10 Co1 O9 82.55(4) 5_656 1_565
O5 Co1 O9 101.76(4) 4_545 1_565
O11 Co1 O9 164.26(3) 5_646 1_565
B1 O1 B1 111.80(15) 2 .
B2 O2 B1 118.16(11) . .
B2 O2 Na1 103.19(8) . 7
B1 O2 Na1 134.42(8) . 7
B2 O3 B1 118.31(10) . 2
B2 O3 Co1 120.42(9) . 4
B1 O3 Co1 117.84(7) 2 4
B3 O4 B2 134.18(11) . .
B3 O4 Na1 134.35(9) . 7
B2 O4 Na1 85.94(8) . 7
B3 O5 B5 121.63(10) . 4
B3 O5 Co1 121.80(9) . 4
B5 O5 Co1 116.33(7) 4 4
B3 O6 B4 118.25(11) . .
B3 O6 Na1 145.14(9) . .
B4 O6 Na1 83.93(7) . .
B4 O7 B5 122.76(11) . 4
B4 O8 B5 120.37(11) . .
B4 O8 Na1 99.21(8) . .
B5 O8 Na1 129.96(8) . .
B6 O9 B5 118.24(11) . .
B6 O9 Co1 111.63(8) . 1_545
B5 O9 Co1 116.90(7) . 1_545
B6 O9 Na1 92.21(8) . 1_545
B5 O9 Na1 115.40(7) . 1_545
Co1 O9 Na1 98.01(4) 1_545 1_545
B6 O10 Co1 126.74(9) . .
B6 O10 Co1 125.39(8) . 5_656
Co1 O10 Co1 97.60(4) . 5_656
B6 O10 Na1 97.34(7) . .
Co1 O10 Na1 101.68(4) . .
Co1 O10 Na1 103.49(4) 5_656 .
B6 O11 B1 116.74(11) . 7
B6 O11 Co1 108.91(8) . 5_646
B1 O11 Co1 123.44(8) 7 5_646
B6 O11 Na1 87.19(7) . 1_545
B1 O11 Na1 116.17(7) 7 1_545
Co1 O11 Na1 96.98(4) 5_646 1_545
O1 B1 O11 112.32(11) . 7
O1 B1 O2 112.23(10) . .
O11 B1 O2 107.79(10) 7 .
O1 B1 O3 108.85(10) . 2
O11 B1 O3 110.35(10) 7 2
O2 B1 O3 105.06(10) . 2
O2 B2 O3 121.68(12) . .
O2 B2 O4 115.01(12) . .
O3 B2 O4 123.22(12) . .
O4 B3 O5 122.17(12) . .
O4 B3 O6 116.15(12) . .
O5 B3 O6 121.67(12) . .
O7 B4 O8 121.66(12) . .
O7 B4 O6 120.65(12) . .
O8 B4 O6 117.57(12) . .
O7 B5 O8 113.63(10) 4_545 .
O7 B5 O9 106.57(11) 4_545 .
O8 B5 O9 107.51(10) . .
O7 B5 O5 109.25(10) 4_545 4_545
O8 B5 O5 107.97(11) . 4_545
O9 B5 O5 111.98(10) . 4_545
O10 B6 O9 121.00(12) . .
O10 B6 O11 121.42(12) . .
O9 B6 O11 117.57(13) . .
O2 Na1 O8 102.83(4) 7 .
O2 Na1 O9 129.89(4) 7 1_565
O8 Na1 O9 88.55(4) . 1_565
O2 Na1 O11 84.13(4) 7 1_565
O8 Na1 O11 133.32(4) . 1_565
O9 Na1 O11 55.52(3) 1_565 1_565
O2 Na1 O10 69.84(3) 7 .
O8 Na1 O10 71.12(3) . .
O9 Na1 O10 68.31(3) 1_565 .
O11 Na1 O10 68.36(3) 1_565 .
O2 Na1 O4 54.00(3) 7 7
O8 Na1 O4 131.00(4) . 7
O9 Na1 O4 140.30(4) 1_565 7
O11 Na1 O4 90.63(3) 1_565 7
O10 Na1 O4 121.87(4) . 7
O2 Na1 O6 135.96(4) 7 .
O8 Na1 O6 54.02(3) . .
O9 Na1 O6 90.00(4) 1_565 .
O11 Na1 O6 139.75(4) 1_565 .
O10 Na1 O6 121.51(4) . .
O4 Na1 O6 109.51(4) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O10 1.9975(10) .
Co1 O3 2.0155(9) 4_545
Co1 O10 2.0221(10) 5_656
Co1 O5 2.0636(9) 4_545
Co1 O11 2.3455(10) 5_646
Co1 O9 2.3475(10) 1_565
O1 B1 1.4154(16) 2
O1 B1 1.4154(16) .
O2 B2 1.3523(17) .
O2 B1 1.4815(17) .
O2 Na1 2.3347(11) 7
O3 B2 1.3717(17) .
O3 B1 1.5760(17) 2
O3 Co1 2.0155(9) 4
O4 B3 1.3663(18) .
O4 B2 1.3891(18) .
O4 Na1 2.7060(12) 7
O5 B3 1.3687(17) .
O5 B5 1.5254(17) 4
O5 Co1 2.0636(9) 4
O6 B3 1.3758(17) .
O6 B4 1.3993(17) .
O6 Na1 2.7432(12) .
O7 B4 1.3546(17) .
O7 B5 1.4353(17) 4
O8 B4 1.3569(17) .
O8 B5 1.4685(17) .
O8 Na1 2.4052(12) .
O9 B6 1.3899(17) .
O9 B5 1.4787(16) .
O9 Co1 2.3475(10) 1_545
O9 Na1 2.4945(12) 1_545
O10 B6 1.3352(18) .
O10 Co1 2.0221(10) 5_656
O10 Na1 2.6841(12) .
O11 B6 1.3952(17) .
O11 B1 1.4670(17) 7
O11 Co1 2.3456(10) 5_646
O11 Na1 2.6142(11) 1_545
B1 O11 1.4670(17) 7
B1 O3 1.5760(17) 2
B5 O7 1.4354(17) 4_545
B5 O5 1.5254(17) 4_545
Na1 O2 2.3347(11) 7
Na1 O9 2.4945(12) 1_565
Na1 O11 2.6142(11) 1_565
Na1 O4 2.7060(12) 7
