#------------------------------------------------------------------------------
#$Date: 2020-12-21 19:45:39 +0200 (Mon, 21 Dec 2020) $
#$Revision: 260054 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/98/1559837.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_1559837
loop_
_publ_author_name
'Chen, Pengyun'
'Li, R.K.'
_publ_section_title
;
 Two high terbium content apatites: Tb5Si2BO13 and Tb4.66Si3O13
;
_journal_name_full               'Journal of Alloys and Compounds'
_journal_page_first              859
_journal_page_last               864
_journal_paper_doi               10.1016/j.jallcom.2014.10.159
_journal_volume                  622
_journal_year                    2015
_chemical_formula_sum            'B O13 Si2 Tb5'
_chemical_formula_weight         1069.59
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.2569(10)
_cell_length_b                   9.2569(10)
_cell_length_c                   6.8297(12)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.5
_cell_volume                     506.83(12)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5221
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         2.541
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    34.745
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    7.009
_exptl_crystal_description       Prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.565
_refine_diff_density_min         -2.002
_refine_diff_density_rms         0.388
_refine_ls_extinction_coef       0.0060(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0199P)²+8.7006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                396
_reflns_number_total             418
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tsbon1.cif
_cod_data_source_block           tsbon
_cod_original_cell_volume        506.83(14)
_cod_database_code               1559837
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.75848(10) 0.76602(10) 0.2500 0.0127(4) Uani 1 2 d S T P . .
Tb2 Tb 0.3333 0.6667 -0.00072(17) 0.0195(4) Uani 1 3 d S T P . .
Si1 Si 0.6294(7) 1.0298(7) 0.2500 0.0062(11) Uani 0.6667 2 d S T P . .
B1 B 0.6294(7) 1.0298(7) 0.2500 0.0062(11) Uani 0.3333 2 d S T P . .
O1 O 0.5139(16) 0.8376(14) 0.2500 0.013(2) Uani 1 2 d S T P . .
O2 O 0.5297(15) 1.1282(14) 0.2500 0.016(3) Uani 1 2 d S T P . .
O3 O 1.0000 1.0000 0.2500 0.019(5) Uani 1 6 d S T P . .
O4 O 0.9099(10) 0.6550(12) 0.0626(12) 0.0153(19) 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
O3 Tb1 O4 104.9(2) . 8_565
O3 Tb1 O4 104.9(2) . 5_565
O4 Tb1 O4 135.3(5) 8_565 5_565
O3 Tb1 O2 151.1(3) . 3_565
O4 Tb1 O2 84.8(2) 8_565 3_565
O4 Tb1 O2 84.8(2) 5_565 3_565
O3 Tb1 O4 84.3(2) . .
O4 Tb1 O4 77.52(17) 8_565 .
O4 Tb1 O4 137.9(3) 5_565 .
O2 Tb1 O4 71.1(3) 3_565 .
O3 Tb1 O4 84.3(2) . 10_556
O4 Tb1 O4 137.9(3) 8_565 10_556
O4 Tb1 O4 77.52(17) 5_565 10_556
O2 Tb1 O4 71.1(3) 3_565 10_556
O4 Tb1 O4 62.4(4) . 10_556
O3 Tb1 O1 109.1(3) . .
O4 Tb1 O1 69.6(2) 8_565 .
O4 Tb1 O1 69.6(2) 5_565 .
O2 Tb1 O1 99.8(4) 3_565 .
O4 Tb1 O1 146.6(2) . .
O4 Tb1 O1 146.6(2) 10_556 .
O3 Tb1 B1 84.47(11) . 2_765
O4 Tb1 B1 107.7(2) 8_565 2_765
O4 Tb1 B1 107.7(2) 5_565 2_765
O2 Tb1 B1 66.7(3) 3_565 2_765
O4 Tb1 B1 31.2(2) . 2_765
O4 Tb1 B1 31.2(2) 10_556 2_765
O1 Tb1 B1 166.4(3) . 2_765
O3 Tb1 Si1 84.47(11) . 2_765
O4 Tb1 Si1 107.7(2) 8_565 2_765
O4 Tb1 Si1 107.7(2) 5_565 2_765
O2 Tb1 Si1 66.7(3) 3_565 2_765
O4 Tb1 Si1 31.2(2) . 2_765
O4 Tb1 Si1 31.2(2) 10_556 2_765
O1 Tb1 Si1 166.4(3) . 2_765
B1 Tb1 Si1 0.00(13) 2_765 2_765
O3 Tb1 Si1 80.38(10) . .
O4 Tb1 Si1 76.5(2) 8_565 .
O4 Tb1 Si1 76.5(2) 5_565 .
O2 Tb1 Si1 128.5(3) 3_565 .
O4 Tb1 Si1 145.2(2) . .
O4 Tb1 Si1 145.2(2) 10_556 .
O1 Tb1 Si1 28.7(3) . .
B1 Tb1 Si1 164.85(13) 2_765 .
Si1 Tb1 Si1 164.85(13) 2_765 .
O3 Tb1 Tb1 30.0 . 3_675
O4 Tb1 Tb1 94.7(2) 8_565 3_675
O4 Tb1 Tb1 94.7(2) 5_565 3_675
O2 Tb1 Tb1 178.9(3) 3_565 3_675
O4 Tb1 Tb1 109.8(2) . 3_675
O4 Tb1 Tb1 109.8(2) 10_556 3_675
O1 Tb1 Tb1 79.1(3) . 3_675
B1 Tb1 Tb1 114.47(11) 2_765 3_675
Si1 Tb1 Tb1 114.47(11) 2_765 3_675
Si1 Tb1 Tb1 50.38(10) . 3_675
O3 Tb1 Tb1 30.0 . 2_765
O4 Tb1 Tb1 111.3(2) 8_565 2_765
O4 Tb1 Tb1 111.3(2) 5_565 2_765
O2 Tb1 Tb1 121.1(3) 3_565 2_765
O4 Tb1 Tb1 59.3(2) . 2_765
O4 Tb1 Tb1 59.3(2) 10_556 2_765
O1 Tb1 Tb1 139.1(3) . 2_765
B1 Tb1 Tb1 54.47(11) 2_765 2_765
Si1 Tb1 Tb1 54.47(11) 2_765 2_765
Si1 Tb1 Tb1 110.38(10) . 2_765
Tb1 Tb1 Tb1 60.0 3_675 2_765
O1 Tb2 O1 73.3(3) 2_665 3_565
O1 Tb2 O1 73.3(3) 2_665 .
O1 Tb2 O1 73.3(3) 3_565 .
O1 Tb2 O2 93.9(3) 2_665 8_455
O1 Tb2 O2 125.9(4) 3_565 8_455
O1 Tb2 O2 153.6(4) . 8_455
O1 Tb2 O2 125.9(4) 2_665 7_675
O1 Tb2 O2 153.6(4) 3_565 7_675
O1 Tb2 O2 93.9(3) . 7_675
O2 Tb2 O2 74.8(3) 8_455 7_675
O1 Tb2 O2 153.6(4) 2_665 9_655
O1 Tb2 O2 93.9(3) 3_565 9_655
O1 Tb2 O2 125.9(4) . 9_655
O2 Tb2 O2 74.8(3) 8_455 9_655
O2 Tb2 O2 74.8(3) 7_675 9_655
O1 Tb2 O4 67.7(3) 2_665 9
O1 Tb2 O4 140.0(3) 3_565 9
O1 Tb2 O4 87.2(3) . 9
O2 Tb2 O4 66.6(3) 8_455 9
O2 Tb2 O4 59.1(3) 7_675 9
O2 Tb2 O4 125.4(3) 9_655 9
O1 Tb2 O4 87.2(3) 2_665 7_665
O1 Tb2 O4 67.7(3) 3_565 7_665
O1 Tb2 O4 140.0(3) . 7_665
O2 Tb2 O4 59.1(3) 8_455 7_665
O2 Tb2 O4 125.4(3) 7_675 7_665
O2 Tb2 O4 66.6(4) 9_655 7_665
O4 Tb2 O4 117.63(9) 9 7_665
O1 Tb2 O4 140.0(3) 2_665 8_565
O1 Tb2 O4 87.2(3) 3_565 8_565
O1 Tb2 O4 67.7(3) . 8_565
O2 Tb2 O4 125.4(3) 8_455 8_565
O2 Tb2 O4 66.6(4) 7_675 8_565
O2 Tb2 O4 59.1(3) 9_655 8_565
O4 Tb2 O4 117.63(9) 9 8_565
O4 Tb2 O4 117.63(9) 7_665 8_565
O1 Tb2 Si1 94.0(2) 2_665 8_455
O1 Tb2 Si1 97.7(3) 3_565 8_455
O1 Tb2 Si1 165.9(2) . 8_455
O2 Tb2 Si1 29.4(3) 8_455 8_455
O2 Tb2 Si1 98.5(2) 7_675 8_455
O2 Tb2 Si1 64.5(3) 9_655 8_455
O4 Tb2 Si1 93.5(2) 9 8_455
O4 Tb2 Si1 30.09(19) 7_665 8_455
O4 Tb2 Si1 123.6(2) 8_565 8_455
O1 Tb2 Si1 97.7(3) 2_665 7_675
O1 Tb2 Si1 165.9(2) 3_565 7_675
O1 Tb2 Si1 94.0(2) . 7_675
O2 Tb2 Si1 64.5(3) 8_455 7_675
O2 Tb2 Si1 29.4(3) 7_675 7_675
O2 Tb2 Si1 98.5(2) 9_655 7_675
O4 Tb2 Si1 30.09(19) 9 7_675
O4 Tb2 Si1 123.6(2) 7_665 7_675
O4 Tb2 Si1 93.5(2) 8_565 7_675
Si1 Tb2 Si1 93.59(8) 8_455 7_675
O1 Tb2 Si1 165.9(2) 2_665 9_655
O1 Tb2 Si1 94.0(2) 3_565 9_655
O1 Tb2 Si1 97.7(3) . 9_655
O2 Tb2 Si1 98.5(2) 8_455 9_655
O2 Tb2 Si1 64.5(3) 7_675 9_655
O2 Tb2 Si1 29.4(3) 9_655 9_655
O4 Tb2 Si1 123.6(2) 9 9_655
O4 Tb2 Si1 93.5(2) 7_665 9_655
O4 Tb2 Si1 30.09(19) 8_565 9_655
Si1 Tb2 Si1 93.59(8) 8_455 9_655
Si1 Tb2 Si1 93.59(8) 7_675 9_655
O1 Si1 O4 111.2(4) . 12_676
O1 Si1 O4 111.2(4) . 3_675
O4 Si1 O4 108.1(7) 12_676 3_675
O1 Si1 O2 113.1(7) . .
O4 Si1 O2 106.4(5) 12_676 .
O4 Si1 O2 106.4(5) 3_675 .
O1 Si1 Tb1 130.6(5) . 3_675
O4 Si1 Tb1 54.1(3) 12_676 3_675
O4 Si1 Tb1 54.1(3) 3_675 3_675
O2 Si1 Tb1 116.3(5) . 3_675
O1 Si1 Tb2 136.7(3) . 4_675
O4 Si1 Tb2 59.7(4) 12_676 4_675
O4 Si1 Tb2 111.7(4) 3_675 4_675
O2 Si1 Tb2 47.6(3) . 4_675
Tb1 Si1 Tb2 81.24(13) 3_675 4_675
O1 Si1 Tb2 136.7(3) . 7_675
O4 Si1 Tb2 111.7(4) 12_676 7_675
O4 Si1 Tb2 59.7(4) 3_675 7_675
O2 Si1 Tb2 47.6(3) . 7_675
Tb1 Si1 Tb2 81.24(13) 3_675 7_675
Tb2 Si1 Tb2 65.36(12) 4_675 7_675
O1 Si1 Tb1 55.5(5) . .
O4 Si1 Tb1 79.9(4) 12_676 .
O4 Si1 Tb1 79.9(4) 3_675 .
O2 Si1 Tb1 168.6(5) . .
Tb1 Si1 Tb1 75.15(13) 3_675 .
Tb2 Si1 Tb1 139.57(12) 4_675 .
Tb2 Si1 Tb1 139.57(12) 7_675 .
Si1 O1 Tb2 128.3(3) . 10_556
Si1 O1 Tb2 128.3(3) . .
Tb2 O1 Tb2 92.9(4) 10_556 .
Si1 O1 Tb1 95.8(6) . .
Tb2 O1 Tb1 103.8(3) 10_556 .
Tb2 O1 Tb1 103.8(3) . .
Si1 O2 Tb1 122.9(6) . 2_665
Si1 O2 Tb2 103.1(5) . 4_675
Tb1 O2 Tb2 115.7(4) 2_665 4_675
Si1 O2 Tb2 103.1(5) . 7_675
Tb1 O2 Tb2 115.7(4) 2_665 7_675
Tb2 O2 Tb2 90.9(4) 4_675 7_675
Tb1 O3 Tb1 120.0 3_675 2_765
Tb1 O3 Tb1 120.0 3_675 .
Tb1 O3 Tb1 120.0 2_765 .
B1 O4 Si1 0.0(4) 2_765 2_765
B1 O4 Tb1 141.8(5) 2_765 9_655
Si1 O4 Tb1 141.8(5) 2_765 9_655
B1 O4 Tb1 94.7(4) 2_765 .
Si1 O4 Tb1 94.7(4) 2_765 .
Tb1 O4 Tb1 116.5(4) 9_655 .
B1 O4 Tb2 90.2(4) 2_765 7_665
Si1 O4 Tb2 90.2(4) 2_765 7_665
Tb1 O4 Tb2 103.4(3) 9_655 7_665
Tb1 O4 Tb2 101.8(3) . 7_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O3 2.2017(8) .
Tb1 O4 2.308(8) 8_565
Tb1 O4 2.308(8) 5_565
Tb1 O2 2.373(13) 3_565
Tb1 O4 2.469(8) .
Tb1 O4 2.469(8) 10_556
Tb1 O1 2.658(12) .
Tb1 B1 3.039(6) 2_765
Tb1 Si1 3.039(6) 2_765
Tb1 Si1 3.211(6) .
Tb1 Tb1 3.8134(14) 3_675
Tb1 Tb1 3.8134(14) 2_765
Tb2 O1 2.363(9) 2_665
Tb2 O1 2.363(9) 3_565
Tb2 O1 2.363(9) .
Tb2 O2 2.389(8) 8_455
Tb2 O2 2.389(8) 7_675
Tb2 O2 2.389(8) 9_655
Tb2 O4 2.722(9) 9
Tb2 O4 2.722(9) 7_665
Tb2 O4 2.722(9) 8_565
Tb2 Si1 3.153(5) 8_455
Tb2 Si1 3.153(5) 7_675
Tb2 Si1 3.153(5) 9_655
Si1 O1 1.551(13) .
Si1 O4 1.581(9) 12_676
Si1 O4 1.581(9) 3_675
Si1 O2 1.588(13) .
Si1 Tb1 3.039(6) 3_675
Si1 Tb2 3.153(5) 4_675
Si1 Tb2 3.153(5) 7_675
O1 Tb2 2.363(9) 10_556
O2 Tb1 2.373(12) 2_665
O2 Tb2 2.389(8) 4_675
O2 Tb2 2.389(8) 7_675
O3 Tb1 2.2017(8) 3_675
O3 Tb1 2.2017(8) 2_765
O4 B1 1.581(9) 2_765
O4 Si1 1.581(9) 2_765
O4 Tb1 2.308(8) 9_655
O4 Tb2 2.722(9) 7_665
