#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:49:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179025 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/23/4122318.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_4122318
loop_
_publ_author_name
'Fang, Lei'
'Iyer, Ratnasabapathy G.'
'Tan, Gangjian'
'West, Damien J.'
'Zhang, Shengbai'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 The New Phase [Tl4Sb6Se10][Sn5Sb2Se14]: A Naturally Formed Semiconducting
 Heterostructure with Two-Dimensional Conductance.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11079
_journal_page_last               11084
_journal_paper_doi               10.1021/ja505301y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'Sb8 Se24 Sn5 Tl4'
_chemical_formula_weight         4280.150
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.813(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   42.95(3)
_cell_length_b                   3.967(2)
_cell_length_c                   13.369(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2251(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5347
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    40.921
_exptl_crystal_density_diffrn    6.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3588
_refine_diff_density_max         3.608
_refine_diff_density_min         -2.871
_refine_diff_density_rms         0.621
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0809P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                1613
_reflns_number_total             2768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja505301y_si_002.cif
_cod_data_source_block           absx
_cod_depositor_comments          'Adding full bibliography for 4122318.cif.'
_cod_database_code               4122318
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
Tl1 Tl 0.29230(3) -0.5000 0.40838(11) 0.0362(4) Uani 1 2 d S
Tl2 Tl -0.00241(3) -2.5000 0.14636(10) 0.0359(4) Uani 1 2 d S
Sn1 Sn 0.35914(5) 0.0000 0.19543(15) 0.0195(5) Uani 1 2 d S
Sn2 Sn 0.5000 -1.0000 0.5000 0.0213(7) Uani 1 4 d S
Sn3 Sn 0.28761(5) -0.5000 0.05668(15) 0.0203(5) Uani 1 2 d S
Sb1 Sb 0.18948(5) -1.5000 0.29346(15) 0.0233(5) Uani 1 2 d SP
Sb2 Sb 0.08847(5) -2.5000 0.08791(15) 0.0233(5) Uani 1 2 d SP
Sb3 Sb 0.11086(5) -2.0000 0.36353(16) 0.0270(5) Uani 1 2 d SP
Sb4 Sb 0.43073(5) -0.5000 0.33800(15) 0.0191(5) Uani 1 2 d S
Se1 Se 0.36702(7) -0.5000 0.3401(2) 0.0206(7) Uani 1 2 d S
Se2 Se 0.13716(8) -2.0000 0.2009(2) 0.0225(7) Uani 1 2 d S
Se3 Se 0.43410(8) -1.0000 0.4822(2) 0.0243(7) Uani 1 2 d S
Se4 Se 0.06969(7) -2.5000 0.2648(2) 0.0211(7) Uani 1 2 d S
Se5 Se 0.29687(7) 0.0000 0.2046(2) 0.0225(7) Uani 1 2 d S
Se6 Se 0.22920(8) -1.0000 0.3720(3) 0.0281(7) Uani 1 2 d S
Se7 Se 0.35173(8) -0.5000 0.0496(2) 0.0257(7) Uani 1 2 d S
Se8 Se 0.50484(8) -1.5000 0.6526(2) 0.0252(7) Uani 1 2 d S
Se9 Se 0.34217(7) -1.0000 0.5534(2) 0.0222(7) Uani 1 2 d S
Se10 Se 0.04577(7) -3.0000 0.0285(2) 0.0249(7) Uani 1 2 d S
Se11 Se 0.42289(7) 0.0000 0.1917(2) 0.0244(7) Uani 1 2 d S
Se12 Se 0.27530(8) -1.0000 -0.0858(2) 0.0273(8) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se5 Sn1 Se11 . . 178.46(12) ?
Se5 Sn1 Se1 . 1_565 89.1(1) ?
Se11 Sn1 Se1 . 1_565 89.84(10) ?
Se5 Sn1 Se1 . . 89.1(1) ?
Se11 Sn1 Se1 . . 89.84(10) ?
Se1 Sn1 Se1 1_565 . 92.12(12) ?
Se5 Sn1 Se7 . . 91.39(10) ?
Se11 Sn1 Se7 . . 89.68(10) ?
Se1 Sn1 Se7 1_565 . 179.46(14) ?
Se1 Sn1 Se7 . . 88.12(8) ?
Se5 Sn1 Se7 . 1_565 91.39(10) ?
Se11 Sn1 Se7 . 1_565 89.68(10) ?
Se1 Sn1 Se7 1_565 1_565 88.12(8) ?
Se1 Sn1 Se7 . 1_565 179.46(14) ?
Se7 Sn1 Se7 . 1_565 91.64(12) ?
Se3 Sn2 Se3 . 3_636 180.00(13) ?
Se3 Sn2 Se8 . 1_565 91.31(8) ?
Se3 Sn2 Se8 3_636 1_565 88.69(8) ?
Se3 Sn2 Se8 . 3_626 88.69(8) ?
Se3 Sn2 Se8 3_636 3_626 91.31(8) ?
Se8 Sn2 Se8 1_565 3_626 180.0() ?
Se3 Sn2 Se8 . 3_636 88.69(8) ?
Se3 Sn2 Se8 3_636 3_636 91.31(8) ?
Se8 Sn2 Se8 1_565 3_636 91.0(1) ?
Se8 Sn2 Se8 3_626 3_636 89.0(1) ?
Se3 Sn2 Se8 . . 91.31(8) ?
Se3 Sn2 Se8 3_636 . 88.69(8) ?
Se8 Sn2 Se8 1_565 . 89.0(1) ?
Se8 Sn2 Se8 3_626 . 91.0(1) ?
Se8 Sn2 Se8 3_636 . 180.0() ?
Se12 Sn3 Se12 . 1_565 92.52(12) ?
Se12 Sn3 Se7 . . 93.61(11) ?
Se12 Sn3 Se7 1_565 . 93.61(11) ?
Se12 Sn3 Se5 . . 176.82(14) ?
Se12 Sn3 Se5 1_565 . 88.26(8) ?
Se7 Sn3 Se5 . . 89.42(9) ?
Se12 Sn3 Se5 . 1_545 88.26(8) ?
Se12 Sn3 Se5 1_565 1_545 176.82(14) ?
Se7 Sn3 Se5 . 1_545 89.42(9) ?
Se5 Sn3 Se5 . 1_545 90.81(12) ?
Se12 Sn3 Se12 . 7_535 90.53(10) ?
Se12 Sn3 Se12 1_565 7_535 90.53(10) ?
Se7 Sn3 Se12 . 7_535 174.00(12) ?
Se5 Sn3 Se12 . 7_535 86.38(10) ?
Se5 Sn3 Se12 1_545 7_535 86.38(10) ?
Se9 Sb1 Se6 7_526 . 93.90(11) ?
Se9 Sb1 Se6 7_526 1_545 93.90(11) ?
Se6 Sb1 Se6 . 1_545 93.67(13) ?
Se4 Sb2 Se10 . . 88.69(11) ?
Se4 Sb2 Se10 . 1_565 88.69(11) ?
Se10 Sb2 Se10 . 1_565 92.99(13) ?
Se2 Sb3 Se4 . . 86.04(10) ?
Se2 Sb3 Se4 . 1_565 86.04(10) ?
Se4 Sb3 Se4 . 1_565 88.46(11) ?
Se2 Sb3 Se9 . 7_526 87.43(11) ?
Se4 Sb3 Se9 . 7_526 173.28(13) ?
Se4 Sb3 Se9 1_565 7_526 92.67(7) ?
Se2 Sb3 Se9 . 7_516 87.43(11) ?
Se4 Sb3 Se9 . 7_516 92.67(7) ?
Se4 Sb3 Se9 1_565 7_516 173.28(13) ?
Se9 Sb3 Se9 7_526 7_516 85.46(11) ?
Se1 Sb4 Se8 . 3_636 176.83(12) ?
Se1 Sb4 Se3 . 1_565 86.44(10) ?
Se8 Sb4 Se3 3_636 1_565 91.36(10) ?
Se1 Sb4 Se3 . . 86.44(10) ?
Se8 Sb4 Se3 3_636 . 91.36(10) ?
Se3 Sb4 Se3 1_565 . 92.13(12) ?
Se1 Sb4 Se11 . 1_545 89.62(10) ?
Se8 Sb4 Se11 3_636 1_545 92.6(1) ?
Se3 Sb4 Se11 1_565 1_545 176.03(13) ?
Se3 Sb4 Se11 . 1_545 88.06(8) ?
Se1 Sb4 Se11 . . 89.62(10) ?
Se8 Sb4 Se11 3_636 . 92.6(1) ?
Se3 Sb4 Se11 1_565 . 88.06(8) ?
Se3 Sb4 Se11 . . 176.03(13) ?
Se11 Sb4 Se11 1_545 . 91.48(12) ?
Sb4 Se1 Sn1 . 1_545 90.48(10) ?
Sb4 Se1 Sn1 . . 90.48(10) ?
Sn1 Se1 Sn1 1_545 . 92.12(12) ?
Sb4 Se3 Sb4 1_545 . 92.13(12) ?
Sb4 Se3 Sn2 1_545 . 90.18(10) ?
Sb4 Se3 Sn2 . . 90.18(10) ?
Sb2 Se4 Sb3 . . 99.43(11) ?
Sb2 Se4 Sb3 . 1_545 99.43(11) ?
Sb3 Se4 Sb3 . 1_545 88.46(11) ?
Sb2 Se4 Tl2 . . 87.81(10) no
Sb3 Se4 Tl2 . . 134.70(7) no
Sb3 Se4 Tl2 1_545 . 134.70(7) ?
Sn1 Se5 Sn3 . . 90.16(10) no
Sn1 Se5 Sn3 . 1_565 90.16(10) ?
Sn3 Se5 Sn3 . 1_565 90.81(12) ?
Sb1 Se6 Sb1 . 1_565 93.67(13) ?
Sb1 Se6 Tl1 . 7_536 95.86(11) ?
Sb1 Se6 Tl1 1_565 7_536 95.86(11) ?
Sn1 Se7 Sn1 . 1_545 91.64(12) ?
Sn1 Se7 Sn3 . . 89.03(11) ?
Sn1 Se7 Sn3 1_545 . 89.03(11) ?
Sb4 Se8 Sn2 3_636 1_545 89.73(9) ?
Sb4 Se8 Sn2 3_636 . 89.73(9) ?
Sn2 Se8 Sn2 1_545 . 89.0(1) ?
Sb1 Se9 Sb3 7_526 7_526 96.49(10) ?
Sb1 Se9 Sb3 7_526 7_516 96.49(10) ?
Sb3 Se9 Sb3 7_526 7_516 85.46(11) ?
Sb2 Se10 Sb2 . 1_545 92.99(13) ?
Sn1 Se11 Sb4 . 1_565 90.07(10) ?
Sn1 Se11 Sb4 . . 90.07(10) ?
Sb4 Se11 Sb4 1_565 . 91.48(12) ?
Sn3 Se12 Sn3 . 1_545 92.52(12) ?
Sn3 Se12 Sn3 . 7_535 89.47(10) ?
Sn3 Se12 Sn3 1_545 7_535 89.47(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 Se6 3.210(4) 7_536
Tl2 Se4 3.255(4) .
Sn1 Se5 2.695(4) .
Sn1 Se11 2.746(4) .
Sn1 Se1 2.755(3) 1_565
Sn1 Se1 2.755(3) .
Sn1 Se7 2.766(3) .
Sn1 Se7 2.766(3) 1_565
Sn2 Se3 2.804(4) .
Sn2 Se3 2.804(4) 3_636
Sn2 Se8 2.830(2) .
Sn2 Se8 2.830(2) 1_565
Sn2 Se8 2.830(2) 3_626
Sn2 Se8 2.830(2) 3_636
Sn3 Se12 2.745(3) 1_565
Sn3 Se12 2.745(3) .
Sn3 Se7 2.770(4) .
Sn3 Se12 2.788(4) 7_535
Sn3 Se5 2.786(3) .
Sn3 Se5 2.786(3) 1_545
Sb1 Se9 2.626(4) 7_526
Sb1 Se6 2.720(3) .
Sb1 Se6 2.720(3) 1_545
Sb2 Se4 2.613(4) .
Sb2 Se10 2.735(3) 1_565
Sb2 Se10 2.736(3) .
Sb3 Se2 2.599(4) .
Sb3 Se4 2.844(3) .
Sb3 Se4 2.844(3) 1_565
Sb3 Se9 2.924(3) 7_526
Sb3 Se9 2.924(3) 7_516
Sb4 Se1 2.741(4) .
Sb4 Se8 2.751(4) 3_636
Sb4 Se3 2.755(3) 1_565
Sb4 Se3 2.755(3) .
Sb4 Se11 2.770(3) .
Sb4 Se11 2.770(3) 1_545
Se1 Sn1 2.755(3) 1_545
Se3 Sn4 2.755(3) 1_545
Se4 Sb3 2.844(3) 1_545
Se5 Sn3 2.786(3) 1_565
Se6 Sb1 2.720(3) 1_565
Se6 Tl1 3.210(4) 7_536
Se7 Sn1 2.766(3) 1_545
Se8 Sb4 2.750(4) 5_636
Se8 Sn2 2.830(2) 1_545
Se9 Sb1 2.626(4) 7_526
Se9 Sb3 2.924(3) 7_526
Se9 Sb3 2.924(3) 7_516
Se10 Sb2 2.736(3) 1_545
Se11 Sb4 2.769(3) 1_565
Se12 Sn3 2.745(3) 1_545
Se12 Sn3 2.788(4) 7_535
