#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/16/4001667.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_4001667
loop_
_publ_author_name
'Kaib, Thomas'
'Haddadpour, Sima'
'Kapitein, Manuel'
'Bron, Philipp'
'Schröder, Cornelia'
'Eckert, Hellmut'
'Roling, Bernhard'
'Dehnen, Stefanie'
_publ_section_title
;
 New Lithium Chalcogenidotetrelates, LiChT: Synthesis and Characterization
 of the Li+-Conducting Tetralithiumortho-Sulfidostannate Li4SnS4
;
_journal_issue                   11
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2211
_journal_paper_doi               10.1021/cm3011315
_journal_volume                  24
_journal_year                    2012
_chemical_formula_sum            'C13 H52 Li4 O13 S4 Sn'
_chemical_formula_weight         691.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.849(2)
_cell_length_b                   23.029(5)
_cell_length_c                   14.610(3)
_cell_measurement_temperature    193(2)
_cell_volume                     3610.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1316
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49422
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.319
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 XPREP by Bruker 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0294
_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)+(0.0147P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                4808
_reflns_number_total             7081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm3011315_si_002.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 2(1) / c'
_cod_database_code               4001667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.171143(15) 0.388852(8) 0.689994(13) 0.02950(6) Uani 1 1 d . . .
S1 S 0.27774(6) 0.45872(3) 0.61144(5) 0.03534(17) Uani 1 1 d . . .
O1 O 0.5389(2) 0.39892(11) 0.59665(18) 0.0520(7) Uani 1 1 d . . .
Li1 Li -0.1119(4) 0.4789(2) 0.4571(4) 0.0400(11) Uani 1 1 d . . .
H1O H 0.486(3) 0.4114(17) 0.605(3) 0.061(14) Uiso 1 1 d . . .
S2 S 0.31536(6) 0.34017(3) 0.80281(5) 0.03300(16) Uani 1 1 d . . .
O2 O -0.05667(17) 0.50485(9) 0.58684(15) 0.0405(5) Uani 1 1 d . . .
C2 C -0.1266(3) 0.55217(16) 0.6211(3) 0.0522(9) Uani 1 1 d . . .
Li2 Li 0.1690(4) 0.2278(2) 0.3552(4) 0.0485(13) Uani 1 1 d . . .
H2A H -0.088(3) 0.5627(17) 0.688(3) 0.090(13) Uiso 1 1 d . . .
H2B H -0.130(3) 0.5863(16) 0.579(2) 0.064(11) Uiso 1 1 d . . .
H2C H -0.225(3) 0.5367(15) 0.623(2) 0.071(11) Uiso 1 1 d . . .
H2O H -0.029(3) 0.4811(18) 0.638(3) 0.088(13) Uiso 1 1 d . . .
S3 S 0.02224(6) 0.43778(3) 0.76972(5) 0.03439(16) Uani 1 1 d . . .
O3 O -0.2234(2) 0.31279(10) 0.63221(17) 0.0517(6) Uani 1 1 d . . .
Li3 Li -0.3501(4) 0.3548(2) 0.6841(4) 0.0486(13) Uani 1 1 d . . .
H3OO H -0.158(3) 0.3195(14) 0.631(2) 0.046(10) Uiso 1 1 d . . .
S4 S 0.05466(6) 0.32079(3) 0.58810(5) 0.03470(17) Uani 1 1 d . . .
O4 O 0.5824(2) 0.42796(9) 0.01532(18) 0.0543(7) Uani 1 1 d . . .
C4 C 0.6087(3) 0.36870(16) -0.0015(3) 0.0866(15) Uani 1 1 d . . .
H4A H 0.6938 0.3604 0.0232 0.130 Uiso 1 1 calc R . .
H4B H 0.5955 0.3615 -0.0669 0.130 Uiso 1 1 calc R . .
H4C H 0.5546 0.3443 0.0279 0.130 Uiso 1 1 calc R . .
Li4 Li 0.6721(5) 0.4767(2) 0.1060(4) 0.0535(14) Uani 1 1 d . . .
H4O H 0.514(3) 0.4360(14) -0.005(2) 0.051(11) Uiso 1 1 d . . .
O5 O -0.12457(19) 0.39661(9) 0.44758(17) 0.0507(6) Uani 1 1 d . . .
C5 C -0.1437(5) 0.36619(19) 0.3607(3) 0.0789(14) Uani 1 1 d . . .
H5A H -0.169(3) 0.3948(17) 0.310(3) 0.079(12) Uiso 1 1 d . . .
H5B H -0.221(4) 0.336(2) 0.360(3) 0.113(15) Uiso 1 1 d . . .
H5C H -0.065(4) 0.344(2) 0.354(3) 0.103(15) Uiso 1 1 d . . .
H5O H -0.067(3) 0.3722(17) 0.487(3) 0.090(13) Uiso 1 1 d . . .
O6 O 0.5491(2) 0.29599(12) 0.72735(19) 0.0542(7) Uani 1 1 d . . .
C6 C 0.5852(3) 0.24882(16) 0.7835(3) 0.0656(11) Uani 1 1 d . . .
H6A H 0.6594 0.2321 0.7662 0.098 Uiso 1 1 calc R . .
H6B H 0.5198 0.2204 0.7766 0.098 Uiso 1 1 calc R . .
H6C H 0.6014 0.2613 0.8469 0.098 Uiso 1 1 calc R . .
H6O H 0.502(3) 0.3077(14) 0.739(2) 0.038(12) Uiso 1 1 d . . .
O7 O 0.34166(18) 0.44214(10) -0.06261(16) 0.0439(5) Uani 1 1 d . . .
C7 C 0.2633(3) 0.42302(16) 0.0031(2) 0.0573(9) Uani 1 1 d . . .
H7A H 0.2871 0.4427 0.0609 0.086 Uiso 1 1 calc R . .
H7B H 0.2728 0.3819 0.0123 0.086 Uiso 1 1 calc R . .
H7C H 0.1779 0.4317 -0.0202 0.086 Uiso 1 1 calc R . .
H7O H 0.330(2) 0.4182(13) -0.102(2) 0.029(8) Uiso 1 1 d . . .
O8 O 0.1033(2) 0.22412(11) 0.7456(2) 0.0543(7) Uani 1 1 d . . .
C8 C 0.1932(3) 0.18620(15) 0.7143(3) 0.0726(12) Uani 1 1 d . . .
H8A H 0.2635 0.2085 0.7015 0.109 Uiso 1 1 calc R . .
H8B H 0.1562 0.1667 0.6589 0.109 Uiso 1 1 calc R . .
H8C H 0.2202 0.1580 0.7614 0.109 Uiso 1 1 calc R . .
H8O H 0.088(3) 0.2415(14) 0.703(2) 0.036(10) Uiso 1 1 d . . .
O9 O -0.2578(2) 0.40457(12) 0.7716(2) 0.0655(8) Uani 1 1 d . . .
C9 C -0.3011(4) 0.45560(19) 0.8074(3) 0.0889(14) Uani 1 1 d . B .
H9A H -0.2975 0.4867 0.7642 0.133 Uiso 1 1 calc R . .
H9B H -0.2500 0.4649 0.8649 0.133 Uiso 1 1 calc R . .
H9C H -0.3857 0.4502 0.8178 0.133 Uiso 1 1 calc R . .
H9O H -0.198(4) 0.410(2) 0.759(3) 0.099(19) Uiso 1 1 d . . .
O10 O 0.2358(2) 0.27827(12) 0.45259(19) 0.0632(8) Uani 1 1 d . . .
H10O H 0.195(3) 0.2926(13) 0.477(2) 0.031(10) Uiso 1 1 d . . .
O11 O 0.03615(19) 0.32036(10) 0.88733(17) 0.0535(6) Uani 1 1 d . . .
C11 C -0.0809(4) 0.29734(18) 0.8935(4) 0.0676(13) Uani 1 1 d . . .
H11A H -0.137(4) 0.3234(19) 0.919(3) 0.094(14) Uiso 1 1 d . . .
H11B H -0.129(6) 0.286(3) 0.833(5) 0.18(3) Uiso 1 1 d . . .
H11C H -0.067(3) 0.2631(18) 0.935(3) 0.081(12) Uiso 1 1 d . . .
H11O H 0.021(3) 0.3536(15) 0.848(2) 0.058(10) Uiso 1 1 d . . .
O12 O 0.5960(2) 0.47364(11) 0.21494(19) 0.0598(7) Uani 1 1 d . . .
C12 C 0.5333(4) 0.42640(17) 0.2487(3) 0.0779(12) Uani 1 1 d . . .
H12A H 0.5003 0.4016 0.1982 0.117 Uiso 1 1 calc R . .
H12B H 0.4664 0.4406 0.2788 0.117 Uiso 1 1 calc R . .
H12C H 0.5906 0.4048 0.2923 0.117 Uiso 1 1 calc R . .
H12O H 0.623(3) 0.4900(16) 0.260(3) 0.061(13) Uiso 1 1 d . . .
O13 O 0.1551(2) 0.54352(13) -0.1281(2) 0.0724(9) Uani 1 1 d . . .
H13O H 0.124(3) 0.5210(14) -0.151(2) 0.035(10) Uiso 1 1 d . . .
C1A C 0.5874(19) 0.4345(10) 0.535(2) 0.074(5) Uani 0.55(6) 1 d P A 1
H1AA H 0.6617 0.4173 0.5188 0.111 Uiso 0.55(6) 1 calc PR A 1
H1AB H 0.6070 0.4717 0.5634 0.111 Uiso 0.55(6) 1 calc PR A 1
H1AC H 0.5272 0.4393 0.4806 0.111 Uiso 0.55(6) 1 calc PR A 1
C1B C 0.556(3) 0.412(2) 0.500(3) 0.088(9) Uani 0.45(6) 1 d P A 2
H1BA H 0.4801 0.4047 0.4597 0.133 Uiso 0.45(6) 1 calc PR A 2
H1BB H 0.6216 0.3886 0.4831 0.133 Uiso 0.45(6) 1 calc PR A 2
H1BC H 0.5780 0.4526 0.4960 0.133 Uiso 0.45(6) 1 calc PR A 2
C3A C -0.2446(8) 0.2555(5) 0.5934(8) 0.054(3) Uiso 0.494(19) 1 d P B 3
H3AA H -0.3284 0.2437 0.5975 0.081 Uiso 0.494(19) 1 calc PR B 3
H3AB H -0.1873 0.2287 0.6272 0.081 Uiso 0.494(19) 1 calc PR B 3
H3AC H -0.2322 0.2560 0.5297 0.081 Uiso 0.494(19) 1 calc PR B 3
C3B C -0.2664(7) 0.2757(4) 0.5572(7) 0.045(3) Uiso 0.506(19) 1 d P B 4
H3BA H -0.2582 0.2950 0.5001 0.068 Uiso 0.506(19) 1 calc PR B 4
H3BB H -0.3524 0.2664 0.5583 0.068 Uiso 0.506(19) 1 calc PR B 4
H3BC H -0.2179 0.2407 0.5622 0.068 Uiso 0.506(19) 1 calc PR B 4
C10A C 0.3541(17) 0.2940(15) 0.489(2) 0.096(7) Uani 0.63(5) 1 d P C 5
H10A H 0.4110 0.2810 0.4485 0.145 Uiso 0.63(5) 1 calc PR C 5
H10B H 0.3759 0.2767 0.5486 0.145 Uiso 0.63(5) 1 calc PR C 5
H10C H 0.3588 0.3356 0.4942 0.145 Uiso 0.63(5) 1 calc PR C 5
C10B C 0.358(3) 0.2704(12) 0.5066(17) 0.050(5) Uani 0.37(5) 1 d P C 6
H10D H 0.4182 0.2631 0.4658 0.075 Uiso 0.37(5) 1 calc PR C 6
H10E H 0.3561 0.2379 0.5477 0.075 Uiso 0.37(5) 1 calc PR C 6
H10F H 0.3811 0.3048 0.5421 0.075 Uiso 0.37(5) 1 calc PR C 6
C13A C 0.064(2) 0.5612(13) -0.068(2) 0.080(7) Uani 0.46(5) 1 d P D 7
H13A H -0.0150 0.5692 -0.1051 0.119 Uiso 0.46(5) 1 calc PR D 7
H13B H 0.0928 0.5955 -0.0340 0.119 Uiso 0.46(5) 1 calc PR D 7
H13C H 0.0535 0.5304 -0.0252 0.119 Uiso 0.46(5) 1 calc PR D 7
C13B C 0.073(2) 0.5794(12) -0.099(2) 0.079(6) Uani 0.54(5) 1 d P D 8
H13D H 0.0920 0.6186 -0.1137 0.118 Uiso 0.54(5) 1 calc PR D 8
H13E H 0.0766 0.5756 -0.0330 0.118 Uiso 0.54(5) 1 calc PR D 8
H13F H -0.0094 0.5697 -0.1287 0.118 Uiso 0.54(5) 1 calc PR D 8
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Li Li -0.0003 0.0001 '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'
S S 0.1246 0.1234 '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'
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
S1 Sn1 S2 109.68(3) . .
S1 Sn1 S4 113.20(3) . .
S2 Sn1 S4 110.84(3) . .
S1 Sn1 S3 109.04(3) . .
S2 Sn1 S3 107.77(3) . .
S4 Sn1 S3 106.10(3) . .
Sn1 S1 Li1 102.63(12) . 3_566
C1A O1 C1B 30.7(11) . .
C1A O1 Li3 119.2(9) . 1_655
C1B O1 Li3 126.2(9) . 1_655
O5 Li1 O2 112.1(3) . .
O5 Li1 O2 102.5(2) . 3_566
O2 Li1 O2 94.9(2) . 3_566
O5 Li1 S1 121.6(2) . 3_566
O2 Li1 S1 108.6(2) . 3_566
O2 Li1 S1 114.0(2) 3_566 3_566
O5 Li1 Li1 115.9(3) . 3_566
O2 Li1 Li1 48.45(17) . 3_566
O2 Li1 Li1 46.43(15) 3_566 3_566
S1 Li1 Li1 122.4(3) 3_566 3_566
Sn1 S2 Li2 97.36(12) . 4_566
C2 O2 Li1 116.9(2) . .
C2 O2 Li1 120.1(2) . 3_566
Li1 O2 Li1 85.1(2) . 3_566
O10 Li2 O11 112.7(3) . 4_565
O10 Li2 O8 108.4(3) . 4_565
O11 Li2 O8 108.9(3) 4_565 4_565
O10 Li2 S2 115.8(2) . 4_565
O11 Li2 S2 104.6(2) 4_565 4_565
O8 Li2 S2 106.1(2) 4_565 4_565
C3B O3 C3A 29.1(4) . .
C3B O3 Li3 115.8(4) . .
C3A O3 Li3 122.2(4) . .
O9 Li3 O6 118.6(3) . 1_455
O9 Li3 O1 110.4(3) . 1_455
O6 Li3 O1 105.3(2) 1_455 1_455
O9 Li3 O3 103.5(2) . .
O6 Li3 O3 104.5(3) 1_455 .
O1 Li3 O3 114.8(3) 1_455 .
C4 O4 Li4 126.5(3) . .
O4 Li4 O12 108.8(3) . .
O4 Li4 O13 111.3(3) . 3_665
O12 Li4 O13 112.7(3) . 3_665
O4 Li4 O7 109.3(3) . 3_665
O12 Li4 O7 106.5(3) . 3_665
O13 Li4 O7 108.1(3) 3_665 3_665
C5 O5 Li1 123.3(3) . .
C6 O6 Li3 129.0(3) . 1_655
C7 O7 Li4 118.6(3) . 3_665
C8 O8 Li2 114.5(3) . 4_566
C9 O9 Li3 126.1(3) . .
C10A O10 C10B 24.5(15) . .
C10A O10 Li2 133.4(8) . .
C10B O10 Li2 123.3(12) . .
C11 O11 Li2 121.2(3) . 4_566
C12 O12 Li4 127.9(3) . .
C13B O13 C13A 25.5(13) . .
C13B O13 Li4 141.6(9) . 3_665
C13A O13 Li4 134.0(13) . 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3736(8) .
Sn1 S2 2.3797(9) .
Sn1 S4 2.3909(9) .
Sn1 S3 2.4061(9) .
S1 Li1 2.403(5) 3_566
O1 C1A 1.375(18) .
O1 C1B 1.48(3) .
O1 Li3 1.914(6) 1_655
Li1 O5 1.903(5) .
Li1 O2 1.994(6) .
Li1 O2 2.060(5) 3_566
Li1 S1 2.403(5) 3_566
Li1 Li1 2.742(9) 3_566
S2 Li2 2.432(5) 4_566
O2 C2 1.458(4) .
O2 Li1 2.060(5) 3_566
Li2 O10 1.896(6) .
Li2 O11 1.931(6) 4_565
Li2 O8 1.990(6) 4_565
Li2 S2 2.432(5) 4_565
O3 C3B 1.413(7) .
O3 C3A 1.441(8) .
O3 Li3 1.925(6) .
Li3 O9 1.890(6) .
Li3 O6 1.906(6) 1_455
Li3 O1 1.914(6) 1_455
O4 C4 1.423(4) .
O4 Li4 1.893(6) .
Li4 O12 1.899(7) .
Li4 O13 1.913(5) 3_665
Li4 O7 1.971(6) 3_665
O5 C5 1.438(5) .
O6 C6 1.383(4) .
O6 Li3 1.906(6) 1_655
O7 C7 1.442(4) .
O7 Li4 1.972(6) 3_665
O8 C8 1.433(4) .
O8 Li2 1.990(6) 4_566
O9 C9 1.396(4) .
O10 C10A 1.363(17) .
O10 C10B 1.45(2) .
O11 C11 1.391(4) .
O11 Li2 1.931(6) 4_566
O12 C12 1.410(4) .
O13 C13B 1.33(2) .
O13 C13A 1.48(2) .
O13 Li4 1.913(5) 3_665
