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#$Date: 2020-12-21 19:40:07 +0200 (Mon, 21 Dec 2020) $
#$Revision: 260053 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/98/1559836.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_1559836
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            'O13 Si3 Tb4.66'
_chemical_formula_weight         1053.59
_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                   9.493(4)
_cell_length_b                   9.493(4)
_cell_length_c                   6.852(5)
_cell_measurement_temperature    571(2)
_cell_volume                     534.8(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      571(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1840
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.425
_diffrn_reflns_theta_min         3.871
_exptl_absorpt_coefficient_mu    32.920
_exptl_crystal_density_diffrn    6.544
_exptl_crystal_F_000             908
_refine_diff_density_max         2.621
_refine_diff_density_min         -2.168
_refine_diff_density_rms         0.377
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0319
_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)+2.4391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                405
_reflns_number_total             442
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tso6m.cif
_cod_data_source_block           tsbo6m
_cod_original_cell_volume        534.7(6)
_cod_database_code               1559836
_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 -0.00417(7) 0.75862(6) 0.2500 0.0109(3) Uani 1 2 d S T P . .
Tb2 Tb 0.3333 0.6667 -0.00172(16) 0.0116(3) Uani 0.828(4) 3 d S T . . .
Si3 Si 0.3731(4) 0.9713(4) 0.2500 0.0097(7) Uani 1 2 d S T P . .
O1 O -0.1658(9) 0.3268(11) 0.2500 0.018(2) Uani 1 2 d S T P . .
O2 O 0.0000 1.0000 0.2500 0.047(7) Uani 1 6 d S T P . .
O3 O 0.4730(9) 0.8726(9) 0.2500 0.019(2) Uani 1 2 d S T P . .
O4 O 0.2538(7) 0.9086(7) 0.0605(11) 0.0220(16) 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
O2 Tb1 O4 104.55(15) . 8_455
O2 Tb1 O4 104.55(15) . 5_455
O4 Tb1 O4 133.4(3) 8_455 5_455
O2 Tb1 O3 152.17(18) . 2_665
O4 Tb1 O3 85.44(15) 8_455 2_665
O4 Tb1 O3 85.44(15) 5_455 2_665
O2 Tb1 O4 84.67(14) . .
O4 Tb1 O4 78.74(13) 8_455 .
O4 Tb1 O4 139.5(2) 5_455 .
O3 Tb1 O4 71.7(2) 2_665 .
O2 Tb1 O4 84.68(14) . 10_556
O4 Tb1 O4 139.5(2) 8_455 10_556
O4 Tb1 O4 78.74(13) 5_455 10_556
O3 Tb1 O4 71.7(2) 2_665 10_556
O4 Tb1 O4 62.7(3) . 10_556
O2 Tb1 O1 108.71(16) . 2_565
O4 Tb1 O1 68.28(16) 8_455 2_565
O4 Tb1 O1 68.28(16) 5_455 2_565
O3 Tb1 O1 99.1(2) 2_665 2_565
O4 Tb1 O1 146.48(16) . 2_565
O4 Tb1 O1 146.48(16) 10_556 2_565
O2 Tb1 Si3 84.94(6) . .
O4 Tb1 Si3 109.07(15) 8_455 .
O4 Tb1 Si3 109.07(15) 5_455 .
O3 Tb1 Si3 67.24(19) 2_665 .
O4 Tb1 Si3 31.38(16) . .
O4 Tb1 Si3 31.38(16) 10_556 .
O1 Tb1 Si3 166.36(17) 2_565 .
O2 Tb1 Si3 79.84(6) . 3_465
O4 Tb1 Si3 75.13(14) 8_455 3_465
O4 Tb1 Si3 75.13(14) 5_455 3_465
O3 Tb1 Si3 127.99(19) 2_665 3_465
O4 Tb1 Si3 145.00(16) . 3_465
O4 Tb1 Si3 145.00(16) 10_556 3_465
O1 Tb1 Si3 28.87(16) 2_565 3_465
Si3 Tb1 Si3 164.77(7) . 3_465
O2 Tb1 Tb1 30.0 . 3_465
O4 Tb1 Tb1 93.71(14) 8_455 3_465
O4 Tb1 Tb1 93.71(14) 5_455 3_465
O3 Tb1 Tb1 177.83(18) 2_665 3_465
O4 Tb1 Tb1 110.12(14) . 3_465
O4 Tb1 Tb1 110.12(14) 10_556 3_465
O1 Tb1 Tb1 78.70(16) 2_565 3_465
Si3 Tb1 Tb1 114.94(6) . 3_465
Si3 Tb1 Tb1 49.84(6) 3_465 3_465
O2 Tb1 Tb1 30.0 . 2_675
O4 Tb1 Tb1 111.74(17) 8_455 2_675
O4 Tb1 Tb1 111.74(17) 5_455 2_675
O3 Tb1 Tb1 122.17(18) 2_665 2_675
O4 Tb1 Tb1 59.68(15) . 2_675
O4 Tb1 Tb1 59.68(15) 10_556 2_675
O1 Tb1 Tb1 138.71(16) 2_565 2_675
Si3 Tb1 Tb1 54.94(6) . 2_675
Si3 Tb1 Tb1 109.84(6) 3_465 2_675
Tb1 Tb1 Tb1 60.0 3_465 2_675
O1 Tb2 O1 73.4(2) 7_565 9_665
O1 Tb2 O1 73.4(2) 7_565 8
O1 Tb2 O1 73.4(2) 9_665 8
O1 Tb2 O3 126.4(3) 7_565 .
O1 Tb2 O3 93.04(19) 9_665 .
O1 Tb2 O3 152.5(3) 8 .
O1 Tb2 O3 93.04(19) 7_565 2_665
O1 Tb2 O3 152.5(3) 9_665 2_665
O1 Tb2 O3 126.4(3) 8 2_665
O3 Tb2 O3 75.6(2) . 2_665
O1 Tb2 O3 152.5(3) 7_565 3_565
O1 Tb2 O3 126.4(3) 9_665 3_565
O1 Tb2 O3 93.04(19) 8 3_565
O3 Tb2 O3 75.6(2) . 3_565
O3 Tb2 O3 75.6(2) 2_665 3_565
O1 Tb2 O4 67.9(2) 7_565 .
O1 Tb2 O4 86.6(2) 9_665 .
O1 Tb2 O4 140.1(2) 8 .
O3 Tb2 O4 59.6(2) . .
O3 Tb2 O4 65.9(2) 2_665 .
O3 Tb2 O4 126.1(2) 3_565 .
O1 Tb2 O4 86.6(2) 7_565 2_665
O1 Tb2 O4 140.1(2) 9_665 2_665
O1 Tb2 O4 67.9(2) 8 2_665
O3 Tb2 O4 126.1(2) . 2_665
O3 Tb2 O4 59.6(2) 2_665 2_665
O3 Tb2 O4 65.9(2) 3_565 2_665
O4 Tb2 O4 117.70(8) . 2_665
O1 Tb2 O4 140.1(2) 7_565 3_565
O1 Tb2 O4 67.9(2) 9_665 3_565
O1 Tb2 O4 86.6(2) 8 3_565
O3 Tb2 O4 65.9(2) . 3_565
O3 Tb2 O4 126.1(2) 2_665 3_565
O3 Tb2 O4 59.6(2) 3_565 3_565
O4 Tb2 O4 117.70(8) . 3_565
O4 Tb2 O4 117.70(8) 2_665 3_565
O1 Tb2 Si3 93.04(17) 7_565 2_665
O1 Tb2 Si3 165.48(17) 9_665 2_665
O1 Tb2 Si3 98.1(2) 8 2_665
O3 Tb2 Si3 99.36(15) . 2_665
O3 Tb2 Si3 29.60(18) 2_665 2_665
O3 Tb2 Si3 64.70(18) 3_565 2_665
O4 Tb2 Si3 93.09(13) . 2_665
O4 Tb2 Si3 30.33(14) 2_665 2_665
O4 Tb2 Si3 124.30(14) 3_565 2_665
O1 Tb2 Si3 165.48(17) 7_565 3_565
O1 Tb2 Si3 98.1(2) 9_665 3_565
O1 Tb2 Si3 93.04(17) 8 3_565
O3 Tb2 Si3 64.70(18) . 3_565
O3 Tb2 Si3 99.36(15) 2_665 3_565
O3 Tb2 Si3 29.60(18) 3_565 3_565
O4 Tb2 Si3 124.30(14) . 3_565
O4 Tb2 Si3 93.09(13) 2_665 3_565
O4 Tb2 Si3 30.33(14) 3_565 3_565
Si3 Tb2 Si3 94.03(5) 2_665 3_565
O1 Tb2 Si3 98.1(2) 7_565 .
O1 Tb2 Si3 93.04(17) 9_665 .
O1 Tb2 Si3 165.48(17) 8 .
O3 Tb2 Si3 29.60(18) . .
O3 Tb2 Si3 64.70(18) 2_665 .
O3 Tb2 Si3 99.36(15) 3_565 .
O4 Tb2 Si3 30.33(14) . .
O4 Tb2 Si3 124.30(14) 2_665 .
O4 Tb2 Si3 93.09(13) 3_565 .
Si3 Tb2 Si3 94.03(5) 2_665 .
Si3 Tb2 Si3 94.03(5) 3_565 .
O1 Si3 O4 112.4(3) 3_565 .
O1 Si3 O4 112.4(3) 3_565 10_556
O4 Si3 O4 105.8(5) . 10_556
O1 Si3 O3 112.3(5) 3_565 .
O4 Si3 O3 106.7(3) . .
O4 Si3 O3 106.7(3) 10_556 .
O1 Si3 Tb1 131.7(4) 3_565 .
O4 Si3 Tb1 53.0(2) . .
O4 Si3 Tb1 53.0(2) 10_556 .
O3 Si3 Tb1 116.0(3) . .
O1 Si3 Tb2 136.6(2) 3_565 .
O4 Si3 Tb2 59.8(2) . .
O4 Si3 Tb2 110.6(2) 10_556 .
O3 Si3 Tb2 47.6(2) . .
Tb1 Si3 Tb2 80.64(7) . .
O1 Si3 Tb2 136.6(2) 3_565 10_556
O4 Si3 Tb2 110.6(2) . 10_556
O4 Si3 Tb2 59.8(2) 10_556 10_556
O3 Si3 Tb2 47.6(2) . 10_556
Tb1 Si3 Tb2 80.64(7) . 10_556
Tb2 Si3 Tb2 64.72(8) . 10_556
O1 Si3 Tb1 56.5(3) 3_565 2_675
O4 Si3 Tb1 79.7(3) . 2_675
O4 Si3 Tb1 79.7(3) 10_556 2_675
O3 Si3 Tb1 168.8(3) . 2_675
Tb1 Si3 Tb1 75.23(7) . 2_675
Tb2 Si3 Tb1 139.47(7) . 2_675
Tb2 Si3 Tb1 139.47(7) 10_556 2_675
Si3 O1 Tb2 128.9(2) 2_665 7_565
Si3 O1 Tb2 128.9(2) 2_665 4_565
Tb2 O1 Tb2 92.7(3) 7_565 4_565
Si3 O1 Tb1 94.6(4) 2_665 3_455
Tb2 O1 Tb1 103.5(2) 7_565 3_455
Tb2 O1 Tb1 103.5(2) 4_565 3_455
Tb1 O2 Tb1 120.0 . 2_675
Tb1 O2 Tb1 120.0 . 3_465
Tb1 O2 Tb1 120.0 2_675 3_465
Si3 O3 Tb1 123.2(4) . 3_565
Si3 O3 Tb2 102.8(3) . .
Tb1 O3 Tb2 116.2(2) 3_565 .
Si3 O3 Tb2 102.8(3) . 10_556
Tb1 O3 Tb2 116.2(2) 3_565 10_556
Tb2 O3 Tb2 89.9(3) . 10_556
Si3 O4 Tb1 139.6(3) . 9_665
Si3 O4 Tb1 95.6(3) . .
Tb1 O4 Tb1 117.3(2) 9_665 .
Si3 O4 Tb2 89.8(3) . .
Tb1 O4 Tb2 104.4(3) 9_665 .
Tb1 O4 Tb2 101.67(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.2718(11) .
Tb1 O4 2.317(7) 8_455
Tb1 O4 2.317(7) 5_455
Tb1 O3 2.386(8) 2_665
Tb1 O4 2.495(6) .
Tb1 O4 2.495(6) 10_556
Tb1 O1 2.786(9) 2_565
Tb1 Si3 3.110(3) .
Tb1 Si3 3.331(3) 3_465
Tb1 Tb1 3.9349(19) 3_465
Tb1 Tb1 3.9349(19) 2_675
Tb2 O1 2.351(6) 7_565
Tb2 O1 2.351(6) 9_665
Tb2 O1 2.351(6) 8
Tb2 O3 2.442(5) .
Tb2 O3 2.442(5) 2_665
Tb2 O3 2.442(5) 3_565
Tb2 O4 2.786(7) .
Tb2 O4 2.786(7) 2_665
Tb2 O4 2.786(7) 3_565
Tb2 Si3 3.223(3) 2_665
Tb2 Si3 3.223(3) 3_565
Tb2 Si3 3.223(3) .
Si3 O1 1.613(8) 3_565
Si3 O4 1.628(7) .
Si3 O4 1.627(7) 10_556
Si3 O3 1.632(8) .
Si3 Tb2 3.223(3) 10_556
Si3 Tb1 3.331(3) 2_675
O1 Si3 1.613(8) 2_665
O1 Tb2 2.351(6) 7_565
O1 Tb2 2.351(6) 4_565
O1 Tb1 2.786(9) 3_455
O2 Tb1 2.2718(11) 2_675
O2 Tb1 2.2718(11) 3_465
O3 Tb1 2.386(8) 3_565
O3 Tb2 2.442(5) 10_556
O4 Tb1 2.317(7) 9_665
