data_publication_text
_publ_requested_journal          'to be submitted'
_publ_contact_author_name        'Bettina V. Lotsch'
_publ_contact_author_address     
;Max-Planck-Institut für Festkörperforschung
Heisenbergstraße 1
70569 Stuttgart
Germany
;
_publ_contact_author_email       b.lotsch@fkf.mpg.de
_publ_contact_author_phone       '+49(0)711 6891610'
_publ_contact_author_fax         '+49(0)711 6891612'
loop_
_publ_author_name
_publ_author_address
'Kuhn, Alexander'
;Max-Planck-Institut für Festkörperforschung
Heisenbergstraße 1
70569 Stuttgart
Germany
;
'Holzmann, Tanja'
;Max-Planck-Institut für Festkörperforschung
Heisenbergstraße 1
70569 Stuttgart
Germany
;
'Nuss, Jürgen'
;Max-Planck-Institut für Festkörperforschung
Heisenbergstraße 1
70569 Stuttgart
Germany
;
'Lotsch, Bettina V.'
;Max-Planck-Institut für Festkörperforschung
Heisenbergstraße 1
70569 Stuttgart
Germany
;  
  
data_ak46hs
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Li2 S3 Sn' 
_chemical_formula_weight          228.75

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Li'  'Li'  -0.0003   0.0001
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            15
_space_group_name_H-M_alt         'C 2/c'
_space_group_name_Hall            '-C 2yc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    6.3961(7)
_cell_length_b                    11.0893(13)
_cell_length_c                    12.4157(14)
_cell_angle_alpha                 90
_cell_angle_beta                  99.860(2)
_cell_angle_gamma                 90
_cell_volume                      867.62(17)
_cell_formula_units_Z             8
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     3.502          
_exptl_crystal_F_000              832
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.300
_exptl_crystal_size_mid           0.250
_exptl_crystal_size_min           0.060
_exptl_absorpt_coefficient_mu     7.110
_shelx_estimated_absorpt_T_min    0.224
_shelx_estimated_absorpt_T_max    0.675
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.224 
_exptl_absorpt_correction_T_max   0.675 
_exptl_absorpt_process_details    
; 
semi empirical absorption correction with SADABS,
G.M. Sheldrick, SADABS, Version 2007/4, University of Göttingen. Germany. 
; 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       298(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'SMART APEX II, Bruker AXS' 
_diffrn_measurement_method        \wscan 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             6216
_diffrn_reflns_av_unetI/netI      0.0246
_diffrn_reflns_av_R_equivalents   0.0282
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.331
_diffrn_reflns_theta_max          34.707
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.940
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.940
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.940
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              1754
_reflns_number_gt                 1620
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker Suite (Bruker AXS)'
_computing_cell_refinement        'Bruker Suite (Bruker AXS)'
_computing_data_reduction         'Bruker Suite (Bruker AXS)'
_computing_structure_solution     'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0433P)²+23.2323P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1754
_refine_ls_number_parameters      51
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0540
_refine_ls_R_factor_gt            0.0503
_refine_ls_wR_factor_ref          0.1619
_refine_ls_wR_factor_gt           0.1594
_refine_ls_goodness_of_fit_ref    1.542
_refine_ls_restrained_S_all       1.542
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
S1 S 0.1127(3) 0.08521(13) 0.63106(14) 0.0147(3) Uani 1 1 d . . . . .
S2 S 0.1349(2) 0.24069(13) 0.13088(13) 0.0136(3) Uani 1 1 d . . . . .
S3 S 0.3658(3) 0.08948(15) 0.37062(14) 0.0162(3) Uani 1 1 d . . . . .
Li1 Li 0.248(2) 0.0840(13) -0.0002(12) 0.028(3) Uiso 1 1 d . . . . .
Li3 Li 0.2500 0.2500 0.5000 0.030(5) Uiso 1 2 d S . P . .
Li2 Li 0.0000 0.4151(6) 0.2500 0.023(2) Uani 0.920(6) 2 d S T P . .
Sn3 Sn 0.0000 0.4151(6) 0.2500 0.023(2) Uani 0.080(6) 2 d S T P . .
Sn1 Sn 0.0000 0.08315(5) 0.2500 0.0132(2) Uani 0.953(4) 2 d S T P . .
Li4 Li 0.0000 0.08315(5) 0.2500 0.0132(2) Uani 0.047(4) 2 d S T P . .
Sn2 Sn 0.0000 0.74977(5) 0.2500 0.01274(19) Uani 0.966(4) 2 d S T P . .
Li5 Li 0.0000 0.74977(5) 0.2500 0.01274(19) Uani 0.034(4) 2 d S T P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 Li5 2.5324(16) 5_566 ?
S1 Sn2 2.5324(16) 5_566 ?
S1 Li4 2.5594(16) 5_556 ?
S1 Sn1 2.5594(16) 5_556 ?
S1 Li1 2.583(16) 2 ?
S1 Sn3 2.6580(17) 7_556 ?
S1 Li2 2.6580(17) 7_556 ?
S1 Li3 2.6922(16) . ?
S1 Li1 2.721(15) 6_556 ?
S2 Sn1 2.5338(16) . ?
S2 Li5 2.5434(16) 3_545 ?
S2 Sn2 2.5434(16) 3_545 ?
S2 Li1 2.567(15) . ?
S2 Li2 2.666(5) . ?
S2 Li3 2.7094(16) 2 ?
S2 Li1 2.719(15) 7 ?
S3 Sn1 2.5540(17) . ?
S3 Li5 2.5650(17) 3_545 ?
S3 Sn2 2.5650(17) 3_545 ?
S3 Li3 2.5895(17) . ?
S3 Sn3 2.676(5) 3_545 ?
S3 Li2 2.676(5) 3_545 ?
S3 Li1 2.694(15) 6_556 ?
S3 Li1 2.709(16) 2_655 ?
Li1 S1 2.583(15) 2 ?
Li1 S3 2.694(15) 6 ?
Li1 S3 2.709(16) 2_655 ?
Li1 S2 2.719(15) 7 ?
Li1 S1 2.721(15) 6 ?
Li3 S3 2.5895(17) 7_556 ?
Li3 S1 2.6922(16) 7_556 ?
Li3 S2 2.7094(16) 2 ?
Li3 S2 2.7094(16) 8_556 ?
Li2 S1 2.6579(17) 8_455 ?
Li2 S1 2.6579(17) 7_556 ?
Li2 S2 2.666(5) 2 ?
Li2 S3 2.676(5) 3_455 ?
Li2 S3 2.676(5) 4 ?
Sn1 S2 2.5338(16) 2 ?
Sn1 S3 2.5539(17) 2 ?
Sn1 S1 2.5594(16) 6 ?
Sn1 S1 2.5594(16) 5_556 ?
Sn2 S1 2.5324(16) 5_566 ?
Sn2 S1 2.5324(16) 6_565 ?
Sn2 S2 2.5434(16) 3_455 ?
Sn2 S2 2.5434(16) 4 ?
Sn2 S3 2.5650(17) 4 ?
Sn2 S3 2.5650(17) 3_455 ?
 
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
 _geom_angle_publ_flag
Li5 S1 Sn2 0.0 5_566 5_566 ?
Li5 S1 Li4 93.11(6) 5_566 5_556 ?
Sn2 S1 Li4 93.11(6) 5_566 5_556 ?
Li5 S1 Sn1 93.11(6) 5_566 5_556 ?
Sn2 S1 Sn1 93.11(6) 5_566 5_556 ?
Li4 S1 Sn1 0.000(18) 5_556 5_556 ?
Li5 S1 Li1 93.3(3) 5_566 2 ?
Sn2 S1 Li1 93.3(3) 5_566 2 ?
Li4 S1 Li1 92.9(3) 5_556 2 ?
Sn1 S1 Li1 92.9(3) 5_556 2 ?
Li5 S1 Sn3 90.47(11) 5_566 7_556 ?
Sn2 S1 Sn3 90.47(11) 5_566 7_556 ?
Li4 S1 Sn3 90.36(12) 5_556 7_556 ?
Sn1 S1 Sn3 90.36(12) 5_556 7_556 ?
Li1 S1 Sn3 174.9(3) 2 7_556 ?
Li5 S1 Li2 90.47(11) 5_566 7_556 ?
Sn2 S1 Li2 90.47(11) 5_566 7_556 ?
Li4 S1 Li2 90.36(12) 5_556 7_556 ?
Sn1 S1 Li2 90.36(12) 5_556 7_556 ?
Li1 S1 Li2 174.9(3) 2 7_556 ?
Sn3 S1 Li2 0.0(3) 7_556 7_556 ?
Li5 S1 Li3 90.97(5) 5_566 . ?
Sn2 S1 Li3 90.97(5) 5_566 . ?
Li4 S1 Li3 175.66(7) 5_556 . ?
Sn1 S1 Li3 175.66(7) 5_556 . ?
Li1 S1 Li3 88.4(3) 2 . ?
Sn3 S1 Li3 88.12(11) 7_556 . ?
Li2 S1 Li3 88.12(11) 7_556 . ?
Li5 S1 Li1 177.1(3) 5_566 6_556 ?
Sn2 S1 Li1 177.1(3) 5_566 6_556 ?
Li4 S1 Li1 89.6(3) 5_556 6_556 ?
Sn1 S1 Li1 89.6(3) 5_556 6_556 ?
Li1 S1 Li1 87.7(5) 2 6_556 ?
Sn3 S1 Li1 88.3(3) 7_556 6_556 ?
Li2 S1 Li1 88.3(3) 7_556 6_556 ?
Li3 S1 Li1 86.3(3) . 6_556 ?
Sn1 S2 Li5 93.35(5) . 3_545 ?
Sn1 S2 Sn2 93.35(5) . 3_545 ?
Li5 S2 Sn2 0.00(3) 3_545 3_545 ?
Sn1 S2 Li1 93.7(3) . . ?
Li5 S2 Li1 93.8(3) 3_545 . ?
Sn2 S2 Li1 93.8(3) 3_545 . ?
Sn1 S2 Li2 90.08(11) . . ?
Li5 S2 Li2 90.05(5) 3_545 . ?
Sn2 S2 Li2 90.05(5) 3_545 . ?
Li1 S2 Li2 174.5(3) . . ?
Sn1 S2 Li3 90.64(5) . 2 ?
Li5 S2 Li3 175.37(7) 3_545 2 ?
Sn2 S2 Li3 175.37(7) 3_545 2 ?
Li1 S2 Li3 88.3(3) . 2 ?
Li2 S2 Li3 87.59(5) . 2 ?
Sn1 S2 Li1 176.1(3) . 7 ?
Li5 S2 Li1 89.9(3) 3_545 7 ?
Sn2 S2 Li1 89.9(3) 3_545 7 ?
Li1 S2 Li1 88.3(4) . 7 ?
Li2 S2 Li1 87.8(3) . 7 ?
Li3 S2 Li1 86.0(3) 2 7 ?
Sn1 S3 Li5 92.36(6) . 3_545 ?
Sn1 S3 Sn2 92.36(6) . 3_545 ?
Li5 S3 Sn2 0.000(19) 3_545 3_545 ?
Sn1 S3 Li3 92.97(6) . . ?
Li5 S3 Li3 92.62(5) 3_545 . ?
Sn2 S3 Li3 92.62(5) 3_545 . ?
Sn1 S3 Sn3 90.08(5) . 3_545 ?
Li5 S3 Sn3 90.15(11) 3_545 3_545 ?
Sn2 S3 Sn3 90.15(11) 3_545 3_545 ?
Li3 S3 Sn3 175.79(10) . 3_545 ?
Sn1 S3 Li2 90.08(5) . 3_545 ?
Li5 S3 Li2 90.15(11) 3_545 3_545 ?
Sn2 S3 Li2 90.15(11) 3_545 3_545 ?
Li3 S3 Li2 175.79(10) . 3_545 ?
Sn3 S3 Li2 0.00(19) 3_545 3_545 ?
Sn1 S3 Li1 90.4(3) . 6_556 ?
Li5 S3 Li1 176.7(3) 3_545 6_556 ?
Sn2 S3 Li1 176.7(3) 3_545 6_556 ?
Li3 S3 Li1 89.0(3) . 6_556 ?
Sn3 S3 Li1 88.1(3) 3_545 6_556 ?
Li2 S3 Li1 88.1(3) 3_545 6_556 ?
Sn1 S3 Li1 177.1(3) . 2_655 ?
Li5 S3 Li1 90.0(3) 3_545 2_655 ?
Sn2 S3 Li1 90.0(3) 3_545 2_655 ?
Li3 S3 Li1 88.6(3) . 2_655 ?
Sn3 S3 Li1 88.2(3) 3_545 2_655 ?
Li2 S3 Li1 88.2(3) 3_545 2_655 ?
Li1 S3 Li1 87.2(5) 6_556 2_655 ?
S2 Li1 S1 94.5(5) . 2 ?
S2 Li1 S3 176.9(6) . 6 ?
S1 Li1 S3 86.6(4) 2 6 ?
S2 Li1 S3 86.3(4) . 2_655 ?
S1 Li1 S3 177.1(7) 2 2_655 ?
S3 Li1 S3 92.8(5) 6 2_655 ?
S2 Li1 S2 91.7(4) . 7 ?
S1 Li1 S2 85.9(4) 2 7 ?
S3 Li1 S2 91.2(5) 6 7 ?
S3 Li1 S2 91.2(5) 2_655 7 ?
S2 Li1 S1 86.2(5) . 6 ?
S1 Li1 S1 92.3(5) 2 6 ?
S3 Li1 S1 90.8(4) 6 6 ?
S3 Li1 S1 90.6(5) 2_655 6 ?
S2 Li1 S1 177.2(6) 7 6 ?
S3 Li3 S3 180.0 7_556 . ?
S3 Li3 S1 86.22(5) 7_556 . ?
S3 Li3 S1 93.78(5) . . ?
S3 Li3 S1 93.78(5) 7_556 7_556 ?
S3 Li3 S1 86.22(5) . 7_556 ?
S1 Li3 S1 180.0 . 7_556 ?
S3 Li3 S2 94.08(5) 7_556 2 ?
S3 Li3 S2 85.92(5) . 2 ?
S1 Li3 S2 88.84(5) . 2 ?
S1 Li3 S2 91.16(5) 7_556 2 ?
S3 Li3 S2 85.92(5) 7_556 8_556 ?
S3 Li3 S2 94.08(5) . 8_556 ?
S1 Li3 S2 91.16(5) . 8_556 ?
S1 Li3 S2 88.84(5) 7_556 8_556 ?
S2 Li3 S2 180.0 2 8_556 ?
S1 Li2 S1 179.9(3) 8_455 7_556 ?
S1 Li2 S2 92.88(12) 8_455 . ?
S1 Li2 S2 87.02(11) 7_556 . ?
S1 Li2 S2 87.02(11) 8_455 2 ?
S1 Li2 S2 92.88(12) 7_556 2 ?
S2 Li2 S2 87.0(2) . 2 ?
S1 Li2 S3 87.37(11) 8_455 3_455 ?
S1 Li2 S3 92.73(12) 7_556 3_455 ?
S2 Li2 S3 179.67(14) . 3_455 ?
S2 Li2 S3 92.78(5) 2 3_455 ?
S1 Li2 S3 92.73(12) 8_455 4 ?
S1 Li2 S3 87.37(11) 7_556 4 ?
S2 Li2 S3 92.78(5) . 4 ?
S2 Li2 S3 179.67(14) 2 4 ?
S3 Li2 S3 87.4(2) 3_455 4 ?
S2 Sn1 S2 92.83(7) . 2 ?
S2 Sn1 S3 90.46(5) . 2 ?
S2 Sn1 S3 87.37(5) 2 2 ?
S2 Sn1 S3 87.37(5) . . ?
S2 Sn1 S3 90.46(5) 2 . ?
S3 Sn1 S3 176.85(8) 2 . ?
S2 Sn1 S1 90.49(5) . 6 ?
S2 Sn1 S1 175.85(5) 2 6 ?
S3 Sn1 S1 90.11(5) 2 6 ?
S3 Sn1 S1 92.18(6) . 6 ?
S2 Sn1 S1 175.85(5) . 5_556 ?
S2 Sn1 S1 90.49(5) 2 5_556 ?
S3 Sn1 S1 92.18(6) 2 5_556 ?
S3 Sn1 S1 90.11(5) . 5_556 ?
S1 Sn1 S1 86.31(7) 6 5_556 ?
S1 Sn2 S1 87.46(8) 5_566 6_565 ?
S1 Sn2 S2 92.47(5) 5_566 3_455 ?
S1 Sn2 S2 90.82(5) 6_565 3_455 ?
S1 Sn2 S2 90.82(5) 5_566 4 ?
S1 Sn2 S2 92.47(5) 6_565 4 ?
S2 Sn2 S2 175.46(7) 3_455 4 ?
S1 Sn2 S3 176.67(5) 5_566 4 ?
S1 Sn2 S3 90.19(5) 6_565 4 ?
S2 Sn2 S3 89.93(5) 3_455 4 ?
S2 Sn2 S3 86.93(5) 4 4 ?
S1 Sn2 S3 90.19(5) 5_566 3_455 ?
S1 Sn2 S3 176.67(5) 6_565 3_455 ?
S2 Sn2 S3 86.93(5) 3_455 3_455 ?
S2 Sn2 S3 89.93(5) 4 3_455 ?
S3 Sn2 S3 92.26(8) 4 3_455 ?
 
_refine_diff_density_max    5.976
_refine_diff_density_min   -2.244
_refine_diff_density_rms    0.353

_shelxl_version_number 2013-2



