# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2014

 
data_h 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 Dy4S4Te3  
; 
_chemical_name_common             Dy4S4Te3  
_chemical_melting_point           ? 
_chemical_formula_moiety          Dy4S4Te3  
_chemical_formula_sum 
 'Dy4 S4 Te3' 
_chemical_formula_weight          1161.04 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Te'  'Te'  -0.5308   1.6751 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Dy'  'Dy'  -0.1892   4.4098 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic  
_symmetry_space_group_name_H-M    C2/m        
 
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' 
 
_cell_length_a                    6.7198(9) 
_cell_length_b                    13.748(2) 
_cell_length_c                    6.7151(14) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.363(13) 
_cell_angle_gamma                 90.00 
_cell_volume                      603.59(18) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     582 
_cell_measurement_theta_min       2.96 
_cell_measurement_theta_max       25.47 
 
_exptl_crystal_description        block     
_exptl_crystal_colour             'dark red'
_exptl_crystal_size_max           0.10      
_exptl_crystal_size_mid           0.06      
_exptl_crystal_size_min           0.04      
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     6.388 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              968 
_exptl_absorpt_coefficient_mu     32.210 
_exptl_absorpt_correction_type    'Psi-scan'            
_exptl_absorpt_correction_T_min   0.4781                
_exptl_absorpt_correction_T_max   1.0000                
_exptl_absorpt_process_details    'Psi (Rigaku WinAFC)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'rotating-anode generator'  
_diffrn_radiation_monochromator   graphite                   
_diffrn_measurement_device_type   'Rigaku AFC7R'             
_diffrn_measurement_method        'ω-2θ'                   
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  200 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             639 
_diffrn_reflns_av_R_equivalents   0.0563 
_diffrn_reflns_av_sigmaI/netI     0.0400 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        2 
_diffrn_reflns_theta_min          2.96 
_diffrn_reflns_theta_max          25.47 
_reflns_number_total              582 
_reflns_number_gt                 504 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'WinAFC'                       
_computing_cell_refinement        'WinAFC'                       
_computing_data_reduction         'CrystalStructure Version 3.10'
_computing_structure_solution     'Siemens SHELXTLTM 5'        
_computing_structure_refinement   'Siemens SHELXTLTM 5'        
_computing_molecular_graphics     'Bruker SHELXTL'               
_computing_publication_material   'Siemens SHELXTLTM 5'        
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0853P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    ? 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          582 
_refine_ls_number_parameters      30 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0518 
_refine_ls_R_factor_gt            0.0481 
_refine_ls_wR_factor_ref          0.1186 
_refine_ls_wR_factor_gt           0.1166 
_refine_ls_goodness_of_fit_ref    0.996 
_refine_ls_restrained_S_all       0.996 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Dy1 Dy 0.24135(9) 0.33943(5) 0.24498(9) 0.0050(3) Uani 1 1 d . . . 
Te1 Te 0.1320(2) 0.5000 -0.1332(2) 0.0123(4) Uani 1 2 d S . . 
Te2 Te 0.5000 0.5000 0.5000 0.0329(7) Uani 1 4 d S . . 
S1 S 0.0000 0.2116(4) 0.0000 0.0071(11) Uani 1 2 d S . . 
S2 S 0.0000 0.2838(4) 0.5000 0.0069(11) Uani 1 2 d S . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Dy1 0.0050(5) 0.0035(5) 0.0082(5) -0.0006(3) 0.0047(3) -0.0004(2) 
Te1 0.0143(8) 0.0068(8) 0.0183(8) 0.000 0.0088(6) 0.000 
Te2 0.0376(15) 0.0040(12) 0.0407(16) 0.000 -0.0241(12) 0.000 
S1 0.009(2) 0.004(3) 0.010(3) 0.000 0.005(2) 0.000 
S2 0.008(2) 0.004(2) 0.011(3) 0.000 0.007(2) 0.000 
 
_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 
Dy1 S1 2.682(4) . ? 
Dy1 S2 2.7261(16) . ? 
Dy1 S2 2.729(3) 7_556 ? 
Dy1 S1 2.7460(15) 7 ? 
Dy1 Te2 3.0743(8) . ? 
Dy1 Te1 3.2957(13) 5_565 ? 
Dy1 Te1 3.3169(14) . ? 
Te1 Te1 2.796(3) 5_565 ? 
Te1 Dy1 3.2957(13) 2 ? 
Te1 Dy1 3.2957(13) 5_565 ? 
Te1 Dy1 3.3169(14) 6_565 ? 
Te2 Dy1 3.0743(8) 5_666 ? 
Te2 Dy1 3.0743(8) 6_565 ? 
Te2 Dy1 3.0743(8) 2_656 ? 
S1 Dy1 2.682(4) 2 ? 
S1 Dy1 2.7460(15) 7 ? 
S1 Dy1 2.7460(15) 8_455 ? 
S2 Dy1 2.7261(16) 2_556 ? 
S2 Dy1 2.729(3) 8_455 ? 
S2 Dy1 2.729(3) 7_556 ? 
 
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 
S1 Dy1 S2 80.69(7) . . ? 
S1 Dy1 S2 100.67(14) . 7_556 ? 
S2 Dy1 S2 79.44(5) . 7_556 ? 
S1 Dy1 S1 80.91(6) . 7 ? 
S2 Dy1 S1 148.82(17) . 7 ? 
S2 Dy1 S1 79.51(7) 7_556 7 ? 
S1 Dy1 Te2 175.00(9) . . ? 
S2 Dy1 Te2 101.15(8) . . ? 
S2 Dy1 Te2 84.27(9) 7_556 . ? 
S1 Dy1 Te2 99.35(8) 7 . ? 
S1 Dy1 Te1 88.78(8) . 5_565 ? 
S2 Dy1 Te1 78.39(9) . 5_565 ? 
S2 Dy1 Te1 154.11(5) 7_556 5_565 ? 
S1 Dy1 Te1 126.06(8) 7 5_565 ? 
Te2 Dy1 Te1 87.05(3) . 5_565 ? 
S1 Dy1 Te1 88.34(8) . . ? 
S2 Dy1 Te1 127.53(8) . . ? 
S2 Dy1 Te1 152.86(4) 7_556 . ? 
S1 Dy1 Te1 76.70(9) 7 . ? 
Te2 Dy1 Te1 86.86(3) . . ? 
Te1 Dy1 Te1 50.03(5) 5_565 . ? 
Te1 Te1 Dy1 65.38(4) 5_565 2 ? 
Te1 Te1 Dy1 65.38(4) 5_565 5_565 ? 
Dy1 Te1 Dy1 84.11(4) 2 5_565 ? 
Te1 Te1 Dy1 64.59(4) 5_565 6_565 ? 
Dy1 Te1 Dy1 129.97(5) 2 6_565 ? 
Dy1 Te1 Dy1 75.56(3) 5_565 6_565 ? 
Te1 Te1 Dy1 64.59(4) 5_565 . ? 
Dy1 Te1 Dy1 75.56(3) 2 . ? 
Dy1 Te1 Dy1 129.97(5) 5_565 . ? 
Dy1 Te1 Dy1 83.45(4) 6_565 . ? 
Dy1 Te2 Dy1 180.0 5_666 . ? 
Dy1 Te2 Dy1 88.21(3) 5_666 6_565 ? 
Dy1 Te2 Dy1 91.79(3) . 6_565 ? 
Dy1 Te2 Dy1 91.79(3) 5_666 2_656 ? 
Dy1 Te2 Dy1 88.21(3) . 2_656 ? 
Dy1 Te2 Dy1 180.0 6_565 2_656 ? 
Dy1 S1 Dy1 98.10(17) . 2 ? 
Dy1 S1 Dy1 99.09(6) . 7 ? 
Dy1 S1 Dy1 100.17(6) 2 7 ? 
Dy1 S1 Dy1 100.17(6) . 8_455 ? 
Dy1 S1 Dy1 99.09(6) 2 8_455 ? 
Dy1 S1 Dy1 150.4(2) 7 8_455 ? 
Dy1 S2 Dy1 147.4(2) . 2_556 ? 
Dy1 S2 Dy1 99.50(5) . 8_455 ? 
Dy1 S2 Dy1 100.56(5) 2_556 8_455 ? 
Dy1 S2 Dy1 100.56(5) . 7_556 ? 
Dy1 S2 Dy1 99.50(5) 2_556 7_556 ? 
Dy1 S2 Dy1 103.26(18) 8_455 7_556 ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              25.47 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    6.212 
_refine_diff_density_min   -5.755 
_refine_diff_density_rms    0.832 
