# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsDy9Cd4Se18
_database_code_depnum_ccdc_archive 'CCDC 1444678'
_audit_update_record             
;
2015-12-29 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd4 Cs Dy9 Se18'
_chemical_formula_sum            'Cd4 Cs Dy9 Se18'
_chemical_formula_weight         3466.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.7025(16)
_cell_length_b                   17.7025(16)
_cell_length_c                   9.883(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2682.3(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1139
_cell_measurement_theta_min      2.3009
_cell_measurement_theta_max      27.4642

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.1300
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.0900
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4359
_exptl_absorpt_coefficient_mu    40.184
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Mercury2
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5756
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         24.97
_reflns_number_total             1050
_reflns_number_gt                1016
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0582P)²+89.4546P] 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     SHELXL
_refine_ls_extinction_coef       0.000039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1050
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Cs1 Cs 0.0000 0.0000 0.5000 0.0502(6) Uani 1 6 d S . .
Dy1 Dy 0.15416(3) 0.25976(3) 0.00284(6) 0.0137(2) Uani 0.33 1 d P . .
Cd1 Cd 0.15416(3) 0.25976(3) 0.00284(6) 0.0137(2) Uani 0.67 1 d P . .
Dy2 Dy 0.05719(3) 0.42568(3) 0.00219(4) 0.0111(2) Uani 1 1 d . . .
Dy3 Dy 0.0000 0.0000 0.0000 0.0087(3) Uani 1 6 d S . .
Se1 Se 0.17325(5) 0.39864(5) 0.16596(8) 0.0097(3) Uani 1 1 d . . .
Se2 Se 0.01299(6) 0.13793(6) 0.16441(8) 0.0117(3) Uani 1 1 d . . .
Se3 Se 0.28501(5) 0.25044(6) 0.16531(8) 0.0088(3) Uani 1 1 d . . .


_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
Cs1 Se2 4.0564(10) 2 ?
Cs1 Se2 4.0564(10) 11_556 ?
Cs1 Se2 4.0564(10) 12_556 ?
Cs1 Se2 4.0564(10) 10_556 ?
Cs1 Se2 4.0564(10) . ?
Cs1 Se2 4.0564(10) 3 ?
Cs1 Se1 4.1348(9) 5 ?
Cs1 Se1 4.1348(9) 17_445 ?
Cs1 Se1 4.1348(9) 16 ?
Cs1 Se1 4.1348(9) 4_445 ?
Cs1 Se1 4.1349(9) 18_545 ?
Cs1 Se1 4.1349(9) 6_455 ?
Dy1 Se2 2.7974(10) 11 ?
Dy1 Se1 2.8155(10) . ?
Dy1 Se2 2.8384(11) . ?
Dy1 Se3 2.8903(10) . ?
Dy1 Se3 2.8965(10) 12 ?
Dy1 Se3 2.9219(10) 9_554 ?
Dy1 Dy2 3.9930(9) 6_455 ?
Dy2 Se1 2.8097(9) 14_455 ?
Dy2 Se2 2.8355(9) 8_554 ?
Dy2 Se1 2.8379(9) . ?
Dy2 Se3 2.8469(10) 12 ?
Dy2 Se1 2.8611(9) 8_554 ?
Dy2 Se3 2.8831(9) 14_455 ?
Dy2 Dy1 3.9929(9) 8_554 ?
Dy2 Cs1 4.8871(6) 7_554 ?
Dy3 Se2 2.8450(8) 10 ?
Dy3 Se2 2.8450(8) . ?
Dy3 Se2 2.8450(8) 12 ?
Dy3 Se2 2.8450(8) 2 ?
Dy3 Se2 2.8450(8) 3 ?
Dy3 Se2 2.8450(8) 11 ?
Se1 Dy2 2.8096(9) 15 ?
Se1 Dy2 2.8612(9) 6_455 ?
Se1 Cs1 4.1348(9) 7_554 ?
Se2 Cd1 2.7974(10) 12 ?
Se2 Dy1 2.7974(10) 12 ?
Se2 Dy2 2.8355(9) 6_455 ?
Se3 Dy2 2.8469(10) 11 ?
Se3 Dy2 2.8832(9) 15 ?
Se3 Dy1 2.8965(10) 11 ?
Se3 Cd1 2.8965(10) 11 ?
Se3 Dy1 2.9218(10) 5 ?
Se3 Cd1 2.9218(10) 5 ?

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
Se2 Cs1 Se2 180.0 2 11_556 ?
Se2 Cs1 Se2 120.19(2) 2 12_556 ?
Se2 Cs1 Se2 59.81(2) 11_556 12_556 ?
Se2 Cs1 Se2 120.19(2) 2 10_556 ?
Se2 Cs1 Se2 59.81(2) 11_556 10_556 ?
Se2 Cs1 Se2 59.81(2) 12_556 10_556 ?
Se2 Cs1 Se2 59.81(2) 2 . ?
Se2 Cs1 Se2 120.19(2) 11_556 . ?
Se2 Cs1 Se2 120.19(2) 12_556 . ?
Se2 Cs1 Se2 180.0 10_556 . ?
Se2 Cs1 Se2 59.81(2) 2 3 ?
Se2 Cs1 Se2 120.19(2) 11_556 3 ?
Se2 Cs1 Se2 180.0 12_556 3 ?
Se2 Cs1 Se2 120.19(2) 10_556 3 ?
Se2 Cs1 Se2 59.81(2) . 3 ?
Se2 Cs1 Se1 119.302(17) 2 5 ?
Se2 Cs1 Se1 60.698(17) 11_556 5 ?
Se2 Cs1 Se1 120.490(17) 12_556 5 ?
Se2 Cs1 Se1 89.207(17) 10_556 5 ?
Se2 Cs1 Se1 90.793(17) . 5 ?
Se2 Cs1 Se1 59.510(17) 3 5 ?
Se2 Cs1 Se1 60.698(17) 2 17_445 ?
Se2 Cs1 Se1 119.302(17) 11_556 17_445 ?
Se2 Cs1 Se1 59.510(17) 12_556 17_445 ?
Se2 Cs1 Se1 90.793(17) 10_556 17_445 ?
Se2 Cs1 Se1 89.207(17) . 17_445 ?
Se2 Cs1 Se1 120.490(17) 3 17_445 ?
Se1 Cs1 Se1 180.0 5 17_445 ?
Se2 Cs1 Se1 120.491(17) 2 16 ?
Se2 Cs1 Se1 59.509(17) 11_556 16 ?
Se2 Cs1 Se1 90.794(17) 12_556 16 ?
Se2 Cs1 Se1 119.302(17) 10_556 16 ?
Se2 Cs1 Se1 60.698(17) . 16 ?
Se2 Cs1 Se1 89.206(17) 3 16 ?
Se1 Cs1 Se1 60.0 5 16 ?
Se1 Cs1 Se1 120.0 17_445 16 ?
Se2 Cs1 Se1 59.509(17) 2 4_445 ?
Se2 Cs1 Se1 120.491(17) 11_556 4_445 ?
Se2 Cs1 Se1 89.206(17) 12_556 4_445 ?
Se2 Cs1 Se1 60.698(17) 10_556 4_445 ?
Se2 Cs1 Se1 119.302(17) . 4_445 ?
Se2 Cs1 Se1 90.794(17) 3 4_445 ?
Se1 Cs1 Se1 120.0 5 4_445 ?
Se1 Cs1 Se1 60.0 17_445 4_445 ?
Se1 Cs1 Se1 180.0 16 4_445 ?
Se2 Cs1 Se1 89.206(17) 2 18_545 ?
Se2 Cs1 Se1 90.794(17) 11_556 18_545 ?
Se2 Cs1 Se1 119.302(17) 12_556 18_545 ?
Se2 Cs1 Se1 59.510(17) 10_556 18_545 ?
Se2 Cs1 Se1 120.490(17) . 18_545 ?
Se2 Cs1 Se1 60.698(17) 3 18_545 ?
Se1 Cs1 Se1 60.0 5 18_545 ?
Se1 Cs1 Se1 120.0 17_445 18_545 ?
Se1 Cs1 Se1 120.0 16 18_545 ?
Se1 Cs1 Se1 60.0 4_445 18_545 ?
Se2 Cs1 Se1 90.794(17) 2 6_455 ?
Se2 Cs1 Se1 89.206(17) 11_556 6_455 ?
Se2 Cs1 Se1 60.698(17) 12_556 6_455 ?
Se2 Cs1 Se1 120.490(17) 10_556 6_455 ?
Se2 Cs1 Se1 59.510(17) . 6_455 ?
Se2 Cs1 Se1 119.302(17) 3 6_455 ?
Se1 Cs1 Se1 120.0 5 6_455 ?
Se1 Cs1 Se1 60.0 17_445 6_455 ?
Se1 Cs1 Se1 60.0 16 6_455 ?
Se1 Cs1 Se1 120.0 4_445 6_455 ?
Se1 Cs1 Se1 180.0 18_545 6_455 ?
Se2 Dy1 Se1 178.49(3) 11 . ?
Se2 Dy1 Se2 90.48(4) 11 . ?
Se1 Dy1 Se2 90.98(3) . . ?
Se2 Dy1 Se3 91.31(3) 11 . ?
Se1 Dy1 Se3 88.97(3) . . ?
Se2 Dy1 Se3 94.04(3) . . ?
Se2 Dy1 Se3 91.23(3) 11 12 ?
Se1 Dy1 Se3 88.38(3) . 12 ?
Se2 Dy1 Se3 90.36(3) . 12 ?
Se3 Dy1 Se3 174.90(4) . 12 ?
Se2 Dy1 Se3 88.10(3) 11 9_554 ?
Se1 Dy1 Se3 90.44(3) . 9_554 ?
Se2 Dy1 Se3 178.58(3) . 9_554 ?
Se3 Dy1 Se3 86.10(3) . 9_554 ?
Se3 Dy1 Se3 89.57(3) 12 9_554 ?
Se2 Dy1 Dy2 135.70(3) 11 6_455 ?
Se1 Dy1 Dy2 45.767(19) . 6_455 ?
Se2 Dy1 Dy2 45.242(19) . 6_455 ?
Se3 Dy1 Dy2 90.78(3) . 6_455 ?
Se3 Dy1 Dy2 90.48(2) 12 6_455 ?
Se3 Dy1 Dy2 136.18(2) 9_554 6_455 ?
Se1 Dy2 Se2 94.32(3) 14_455 8_554 ?
Se1 Dy2 Se1 94.13(3) 14_455 . ?
Se2 Dy2 Se1 91.56(3) 8_554 . ?
Se1 Dy2 Se3 175.53(3) 14_455 12 ?
Se2 Dy2 Se3 88.85(3) 8_554 12 ?
Se1 Dy2 Se3 88.92(3) . 12 ?
Se1 Dy2 Se1 89.03(3) 14_455 8_554 ?
Se2 Dy2 Se1 90.10(3) 8_554 8_554 ?
Se1 Dy2 Se1 176.31(3) . 8_554 ?
Se3 Dy2 Se1 87.81(3) 12 8_554 ?
Se1 Dy2 Se3 89.23(3) 14_455 14_455 ?
Se2 Dy2 Se3 176.40(3) 8_554 14_455 ?
Se1 Dy2 Se3 87.56(3) . 14_455 ?
Se3 Dy2 Se3 87.646(15) 12 14_455 ?
Se1 Dy2 Se3 90.58(3) 8_554 14_455 ?
Se1 Dy2 Dy1 91.00(2) 14_455 8_554 ?
Se2 Dy2 Dy1 45.30(2) 8_554 8_554 ?
Se1 Dy2 Dy1 136.84(2) . 8_554 ?
Se3 Dy2 Dy1 88.99(2) 12 8_554 ?
Se1 Dy2 Dy1 44.84(2) 8_554 8_554 ?
Se3 Dy2 Dy1 135.39(2) 14_455 8_554 ?
Se1 Dy2 Cs1 57.686(19) 14_455 7_554 ?
Se2 Dy2 Cs1 56.07(2) 8_554 7_554 ?
Se1 Dy2 Cs1 57.655(19) . 7_554 ?
Se3 Dy2 Cs1 126.78(2) 12 7_554 ?
Se1 Dy2 Cs1 125.89(2) 8_554 7_554 ?
Se3 Dy2 Cs1 125.90(2) 14_455 7_554 ?
Dy1 Dy2 Cs1 90.527(13) 8_554 7_554 ?
Se2 Dy3 Se2 180.00(4) 10 . ?
Se2 Dy3 Se2 90.61(3) 10 12 ?
Se2 Dy3 Se2 89.39(3) . 12 ?
Se2 Dy3 Se2 89.39(3) 10 2 ?
Se2 Dy3 Se2 90.61(3) . 2 ?
Se2 Dy3 Se2 89.39(3) 12 2 ?
Se2 Dy3 Se2 89.39(3) 10 3 ?
Se2 Dy3 Se2 90.61(3) . 3 ?
Se2 Dy3 Se2 180.00(3) 12 3 ?
Se2 Dy3 Se2 90.61(3) 2 3 ?
Se2 Dy3 Se2 90.61(3) 10 11 ?
Se2 Dy3 Se2 89.39(3) . 11 ?
Se2 Dy3 Se2 90.61(3) 12 11 ?
Se2 Dy3 Se2 180.00(7) 2 11 ?
Se2 Dy3 Se2 89.39(3) 3 11 ?
Dy2 Se1 Dy1 92.41(3) 15 . ?
Dy2 Se1 Dy2 174.13(4) 15 . ?
Dy1 Se1 Dy2 92.28(3) . . ?
Dy2 Se1 Dy2 90.97(3) 15 6_455 ?
Dy1 Se1 Dy2 89.40(3) . 6_455 ?
Dy2 Se1 Dy2 92.61(3) . 6_455 ?
Dy2 Se1 Cs1 87.27(2) 15 7_554 ?
Dy1 Se1 Cs1 135.82(3) . 7_554 ?
Dy2 Se1 Cs1 86.91(2) . 7_554 ?
Dy2 Se1 Cs1 134.78(3) 6_455 7_554 ?
Cd1 Se2 Dy1 0.00(2) 12 12 ?
Cd1 Se2 Dy2 92.93(3) 12 6_455 ?
Dy1 Se2 Dy2 92.93(3) 12 6_455 ?
Cd1 Se2 Dy1 90.60(3) 12 . ?
Dy1 Se2 Dy1 90.60(3) 12 . ?
Dy2 Se2 Dy1 89.46(3) 6_455 . ?
Cd1 Se2 Dy3 90.45(3) 12 . ?
Dy1 Se2 Dy3 90.45(3) 12 . ?
Dy2 Se2 Dy3 176.51(4) 6_455 . ?
Dy1 Se2 Dy3 89.62(3) . . ?
Cd1 Se2 Cs1 136.50(3) 12 . ?
Dy1 Se2 Cs1 136.50(3) 12 . ?
Dy2 Se2 Cs1 88.48(2) 6_455 . ?
Dy1 Se2 Cs1 132.90(3) . . ?
Dy3 Se2 Cs1 89.68(2) . . ?
Dy2 Se3 Dy2 91.97(3) 11 15 ?
Dy2 Se3 Dy1 93.84(3) 11 . ?
Dy2 Se3 Dy1 89.38(3) 15 . ?
Dy2 Se3 Dy1 90.42(3) 11 11 ?
Dy2 Se3 Dy1 176.28(4) 15 11 ?
Dy1 Se3 Dy1 87.61(3) . 11 ?
Dy2 Se3 Cd1 90.42(3) 11 11 ?
Dy2 Se3 Cd1 176.28(4) 15 11 ?
Dy1 Se3 Cd1 87.61(3) . 11 ?
Dy1 Se3 Cd1 0.00(2) 11 11 ?
Dy2 Se3 Dy1 90.11(3) 11 5 ?
Dy2 Se3 Dy1 92.42(3) 15 5 ?
Dy1 Se3 Dy1 175.60(4) . 5 ?
Dy1 Se3 Dy1 90.43(3) 11 5 ?
Cd1 Se3 Dy1 90.43(3) 11 5 ?
Dy2 Se3 Cd1 90.11(3) 11 5 ?
Dy2 Se3 Cd1 92.42(3) 15 5 ?
Dy1 Se3 Cd1 175.60(4) . 5 ?
Dy1 Se3 Cd1 90.43(3) 11 5 ?
Cd1 Se3 Cd1 90.43(3) 11 5 ?
Dy1 Se3 Cd1 0.00(3) 5 5 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.535
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.447
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsEr9Cd4Se18
_database_code_depnum_ccdc_archive 'CCDC 1444679'
_audit_update_record             
;
2015-12-29 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd4 Cs Er9 Se18'
_chemical_formula_sum            'Cd4 Cs Er9 Se18'
_chemical_formula_weight         3509.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.584(5)
_cell_length_b                   17.584(5)
_cell_length_c                   9.825(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2630.8(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2732
_cell_measurement_theta_min      3.3850
_cell_measurement_theta_max      27.4797

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.1100
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.0900
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4413
_exptl_absorpt_coefficient_mu    43.330
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2460
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5518
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1002
_reflns_number_gt                964
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0662P)²+5.4442P] 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         1002
_refine_ls_number_parameters     50
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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
Cs1 Cs 0.0000 0.0000 0.5000 0.0457(5) Uani 1 6 d S . .
Er1 Er 0.15412(3) 0.25983(3) 0.00321(5) 0.0127(2) Uani 0.33 1 d P . .
Cd1 Cd 0.15412(3) 0.25983(3) 0.00321(5) 0.0127(2) Uani 0.67 1 d P . .
Er2 Er 0.05720(2) 0.42587(2) 0.00204(4) 0.0122(2) Uani 1 1 d . . .
Er3 Er 0.0000 0.0000 0.0000 0.0101(3) Uani 1 6 d S . .
Se1 Se 0.17324(5) 0.39903(5) 0.16644(8) 0.0105(3) Uani 1 1 d . . .
Se2 Se 0.01295(6) 0.13758(6) 0.16496(8) 0.0128(3) Uani 1 1 d . . .
Se3 Se 0.28524(5) 0.25058(6) 0.16546(8) 0.0095(3) Uani 1 1 d . . .


_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
Cs1 Se2 4.0234(15) 2 ?
Cs1 Se2 4.0234(15) 11_556 ?
Cs1 Se2 4.0234(15) 3 ?
Cs1 Se2 4.0234(15) . ?
Cs1 Se2 4.0234(15) 12_556 ?
Cs1 Se2 4.0234(15) 10_556 ?
Cs1 Se1 4.1017(15) 17_445 ?
Cs1 Se1 4.1017(15) 5 ?
Cs1 Se1 4.1018(15) 16 ?
Cs1 Se1 4.1018(15) 4_445 ?
Cs1 Se1 4.1019(15) 6_455 ?
Cs1 Se1 4.1019(15) 18_545 ?
Er1 Se2 2.7884(12) 11 ?
Er1 Se1 2.8023(11) . ?
Er1 Se2 2.8235(12) . ?
Er1 Se3 2.8738(12) . ?
Er1 Se3 2.8805(12) 12 ?
Er1 Se3 2.9023(12) 9_554 ?
Er2 Se1 2.7905(11) 14_455 ?
Er2 Se2 2.8169(11) 8_554 ?
Er2 Se1 2.8209(11) . ?
Er2 Se3 2.8284(11) 12 ?
Er2 Se1 2.8398(11) 8_554 ?
Er2 Se3 2.8652(11) 14_455 ?
Er2 Cs1 4.8540(14) 7_554 ?
Er3 Se2 2.8249(11) 10 ?
Er3 Se2 2.8249(11) 12 ?
Er3 Se2 2.8249(11) 3 ?
Er3 Se2 2.8249(11) . ?
Er3 Se2 2.8249(11) 2 ?
Er3 Se2 2.8249(11) 11 ?
Se1 Er2 2.7904(11) 15 ?
Se1 Er2 2.8399(11) 6_455 ?
Se1 Cs1 4.1018(15) 7_554 ?
Se2 Cd1 2.7884(12) 12 ?
Se2 Er1 2.7884(12) 12 ?
Se2 Er2 2.8169(11) 6_455 ?
Se3 Er2 2.8284(11) 11 ?
Se3 Er2 2.8652(11) 15 ?
Se3 Er1 2.8805(12) 11 ?
Se3 Cd1 2.8805(12) 11 ?
Se3 Er1 2.9023(12) 5 ?
Se3 Cd1 2.9023(12) 5 ?

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
Se2 Cs1 Se2 180.000(13) 2 11_556 ?
Se2 Cs1 Se2 59.74(3) 2 3 ?
Se2 Cs1 Se2 120.26(3) 11_556 3 ?
Se2 Cs1 Se2 59.74(3) 2 . ?
Se2 Cs1 Se2 120.26(3) 11_556 . ?
Se2 Cs1 Se2 59.74(3) 3 . ?
Se2 Cs1 Se2 120.26(3) 2 12_556 ?
Se2 Cs1 Se2 59.74(3) 11_556 12_556 ?
Se2 Cs1 Se2 180.00(2) 3 12_556 ?
Se2 Cs1 Se2 120.26(3) . 12_556 ?
Se2 Cs1 Se2 120.26(3) 2 10_556 ?
Se2 Cs1 Se2 59.74(3) 11_556 10_556 ?
Se2 Cs1 Se2 120.26(3) 3 10_556 ?
Se2 Cs1 Se2 180.00(2) . 10_556 ?
Se2 Cs1 Se2 59.74(3) 12_556 10_556 ?
Se2 Cs1 Se1 60.69(2) 2 17_445 ?
Se2 Cs1 Se1 119.31(2) 11_556 17_445 ?
Se2 Cs1 Se1 120.41(2) 3 17_445 ?
Se2 Cs1 Se1 89.118(17) . 17_445 ?
Se2 Cs1 Se1 59.59(2) 12_556 17_445 ?
Se2 Cs1 Se1 90.882(17) 10_556 17_445 ?
Se2 Cs1 Se1 119.31(2) 2 5 ?
Se2 Cs1 Se1 60.69(2) 11_556 5 ?
Se2 Cs1 Se1 59.59(2) 3 5 ?
Se2 Cs1 Se1 90.882(17) . 5 ?
Se2 Cs1 Se1 120.41(2) 12_556 5 ?
Se2 Cs1 Se1 89.118(17) 10_556 5 ?
Se1 Cs1 Se1 180.0 17_445 5 ?
Se2 Cs1 Se1 120.41(2) 2 16 ?
Se2 Cs1 Se1 59.59(2) 11_556 16 ?
Se2 Cs1 Se1 89.117(17) 3 16 ?
Se2 Cs1 Se1 60.70(2) . 16 ?
Se2 Cs1 Se1 90.883(17) 12_556 16 ?
Se2 Cs1 Se1 119.30(2) 10_556 16 ?
Se1 Cs1 Se1 120.0 17_445 16 ?
Se1 Cs1 Se1 60.0 5 16 ?
Se2 Cs1 Se1 59.59(2) 2 4_445 ?
Se2 Cs1 Se1 120.41(2) 11_556 4_445 ?
Se2 Cs1 Se1 90.883(17) 3 4_445 ?
Se2 Cs1 Se1 119.30(2) . 4_445 ?
Se2 Cs1 Se1 89.117(17) 12_556 4_445 ?
Se2 Cs1 Se1 60.70(2) 10_556 4_445 ?
Se1 Cs1 Se1 60.0 17_445 4_445 ?
Se1 Cs1 Se1 120.0 5 4_445 ?
Se1 Cs1 Se1 180.0 16 4_445 ?
Se2 Cs1 Se1 90.883(17) 2 6_455 ?
Se2 Cs1 Se1 89.118(17) 11_556 6_455 ?
Se2 Cs1 Se1 119.30(2) 3 6_455 ?
Se2 Cs1 Se1 59.59(2) . 6_455 ?
Se2 Cs1 Se1 60.70(2) 12_556 6_455 ?
Se2 Cs1 Se1 120.41(2) 10_556 6_455 ?
Se1 Cs1 Se1 60.0 17_445 6_455 ?
Se1 Cs1 Se1 120.0 5 6_455 ?
Se1 Cs1 Se1 60.0 16 6_455 ?
Se1 Cs1 Se1 120.0 4_445 6_455 ?
Se2 Cs1 Se1 89.117(17) 2 18_545 ?
Se2 Cs1 Se1 90.882(17) 11_556 18_545 ?
Se2 Cs1 Se1 60.70(2) 3 18_545 ?
Se2 Cs1 Se1 120.41(2) . 18_545 ?
Se2 Cs1 Se1 119.30(2) 12_556 18_545 ?
Se2 Cs1 Se1 59.59(2) 10_556 18_545 ?
Se1 Cs1 Se1 120.0 17_445 18_545 ?
Se1 Cs1 Se1 60.0 5 18_545 ?
Se1 Cs1 Se1 120.0 16 18_545 ?
Se1 Cs1 Se1 60.0 4_445 18_545 ?
Se1 Cs1 Se1 180.00(2) 6_455 18_545 ?
Se2 Er1 Se1 178.41(3) 11 . ?
Se2 Er1 Se2 90.41(4) 11 . ?
Se1 Er1 Se2 91.08(3) . . ?
Se2 Er1 Se3 91.44(3) 11 . ?
Se1 Er1 Se3 89.01(3) . . ?
Se2 Er1 Se3 93.99(4) . . ?
Se2 Er1 Se3 91.04(3) 11 12 ?
Se1 Er1 Se3 88.40(3) . 12 ?
Se2 Er1 Se3 90.58(3) . 12 ?
Se3 Er1 Se3 174.79(4) . 12 ?
Se2 Er1 Se3 87.97(3) 11 9_554 ?
Se1 Er1 Se3 90.55(3) . 9_554 ?
Se2 Er1 Se3 178.38(3) . 9_554 ?
Se3 Er1 Se3 86.04(4) . 9_554 ?
Se3 Er1 Se3 89.46(3) 12 9_554 ?
Se1 Er2 Se2 94.15(3) 14_455 8_554 ?
Se1 Er2 Se1 93.94(3) 14_455 . ?
Se2 Er2 Se1 91.49(3) 8_554 . ?
Se1 Er2 Se3 175.67(3) 14_455 12 ?
Se2 Er2 Se3 88.88(3) 8_554 12 ?
Se1 Er2 Se3 89.07(3) . 12 ?
Se1 Er2 Se1 89.14(3) 14_455 8_554 ?
Se2 Er2 Se1 90.44(3) 8_554 8_554 ?
Se1 Er2 Se1 176.24(2) . 8_554 ?
Se3 Er2 Se1 87.74(3) 12 8_554 ?
Se1 Er2 Se3 89.42(3) 14_455 14_455 ?
Se2 Er2 Se3 176.33(3) 8_554 14_455 ?
Se1 Er2 Se3 87.40(3) . 14_455 ?
Se3 Er2 Se3 87.60(2) 12 14_455 ?
Se1 Er2 Se3 90.48(3) 8_554 14_455 ?
Se1 Er2 Cs1 57.583(18) 14_455 7_554 ?
Se2 Er2 Cs1 55.96(3) 8_554 7_554 ?
Se1 Er2 Cs1 57.549(18) . 7_554 ?
Se3 Er2 Cs1 126.749(19) 12 7_554 ?
Se1 Er2 Cs1 126.12(2) 8_554 7_554 ?
Se3 Er2 Cs1 125.85(3) 14_455 7_554 ?
Se2 Er3 Se2 90.36(3) 10 12 ?
Se2 Er3 Se2 89.64(3) 10 3 ?
Se2 Er3 Se2 180.00(3) 12 3 ?
Se2 Er3 Se2 180.00(4) 10 . ?
Se2 Er3 Se2 89.64(3) 12 . ?
Se2 Er3 Se2 90.36(3) 3 . ?
Se2 Er3 Se2 89.64(3) 10 2 ?
Se2 Er3 Se2 89.64(3) 12 2 ?
Se2 Er3 Se2 90.36(3) 3 2 ?
Se2 Er3 Se2 90.36(3) . 2 ?
Se2 Er3 Se2 90.36(3) 10 11 ?
Se2 Er3 Se2 90.36(3) 12 11 ?
Se2 Er3 Se2 89.64(3) 3 11 ?
Se2 Er3 Se2 89.64(3) . 11 ?
Se2 Er3 Se2 180.00(6) 2 11 ?
Er2 Se1 Er1 92.27(3) 15 . ?
Er2 Se1 Er2 174.32(4) 15 . ?
Er1 Se1 Er2 92.15(3) . . ?
Er2 Se1 Er2 90.86(3) 15 6_455 ?
Er1 Se1 Er2 89.19(3) . 6_455 ?
Er2 Se1 Er2 92.76(3) . 6_455 ?
Er2 Se1 Cs1 87.37(2) 15 7_554 ?
Er1 Se1 Cs1 135.74(3) . 7_554 ?
Er2 Se1 Cs1 86.98(2) . 7_554 ?
Er2 Se1 Cs1 135.06(3) 6_455 7_554 ?
Cd1 Se2 Er1 0.000(18) 12 12 ?
Cd1 Se2 Er2 92.88(3) 12 6_455 ?
Er1 Se2 Er2 92.88(3) 12 6_455 ?
Cd1 Se2 Er1 90.34(3) 12 . ?
Er1 Se2 Er1 90.34(3) 12 . ?
Er2 Se2 Er1 89.23(3) 6_455 . ?
Cd1 Se2 Er3 90.30(3) 12 . ?
Er1 Se2 Er3 90.30(3) 12 . ?
Er2 Se2 Er3 176.62(4) 6_455 . ?
Er1 Se2 Er3 89.59(3) . . ?
Cd1 Se2 Cs1 136.65(3) 12 . ?
Er1 Se2 Cs1 136.65(3) 12 . ?
Er2 Se2 Cs1 88.58(4) 6_455 . ?
Er1 Se2 Cs1 133.01(3) . . ?
Er3 Se2 Cs1 89.91(4) . . ?
Er2 Se3 Er2 92.07(3) 11 15 ?
Er2 Se3 Er1 93.87(3) 11 . ?
Er2 Se3 Er1 89.27(3) 15 . ?
Er2 Se3 Er1 90.38(3) 11 11 ?
Er2 Se3 Er1 176.10(3) 15 11 ?
Er1 Se3 Er1 87.53(3) . 11 ?
Er2 Se3 Cd1 90.38(3) 11 11 ?
Er2 Se3 Cd1 176.10(3) 15 11 ?
Er1 Se3 Cd1 87.53(3) . 11 ?
Er1 Se3 Cd1 0.00(2) 11 11 ?
Er2 Se3 Er1 90.26(3) 11 5 ?
Er2 Se3 Er1 92.49(3) 15 5 ?
Er1 Se3 Er1 175.45(4) . 5 ?
Er1 Se3 Er1 90.54(3) 11 5 ?
Cd1 Se3 Er1 90.54(3) 11 5 ?
Er2 Se3 Cd1 90.26(3) 11 5 ?
Er2 Se3 Cd1 92.49(3) 15 5 ?
Er1 Se3 Cd1 175.45(4) . 5 ?
Er1 Se3 Cd1 90.54(3) 11 5 ?
Cd1 Se3 Cd1 90.54(3) 11 5 ?
Er1 Se3 Cd1 0.00(2) 5 5 ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         3.259
_refine_diff_density_min         -2.679
_refine_diff_density_rms         0.366
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsHo9Cd4Se18
_database_code_depnum_ccdc_archive 'CCDC 1444680'
_audit_update_record             
;
2015-12-29 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd4 Cs Ho9 Se18'
_chemical_formula_sum            'Cd4 Cs Ho9 Se18'
_chemical_formula_weight         3488.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.635(6)
_cell_length_b                   17.635(6)
_cell_length_c                   9.857(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2654.9(18)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2555
_cell_measurement_theta_min      3.3747
_cell_measurement_theta_max      27.3948

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.1300
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4386
_exptl_absorpt_coefficient_mu    41.717
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.0321
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5596
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.09
_diffrn_reflns_theta_max         24.98
_reflns_number_total             1025
_reflns_number_gt                930
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0528P)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     SHELXL
_refine_ls_extinction_coef       0.00051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1025
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Cs1 Cs 0.0000 0.0000 0.5000 0.0452(7) Uani 1 6 d S . .
Ho1 Ho 0.15417(4) 0.25976(4) 0.00280(7) 0.0101(3) Uani 0.33 1 d P . .
Cd1 Cd 0.15417(4) 0.25976(4) 0.00280(7) 0.0101(3) Uani 0.67 1 d P . .
Ho2 Ho 0.05730(3) 0.42590(4) 0.00218(5) 0.0089(3) Uani 1 1 d . . .
Ho3 Ho 0.0000 0.0000 0.0000 0.0070(4) Uani 1 6 d S . .
Se1 Se 0.17322(7) 0.39884(7) 0.16637(11) 0.0074(4) Uani 1 1 d . . .
Se2 Se 0.01316(8) 0.13787(8) 0.16472(11) 0.0098(4) Uani 1 1 d . . .
Se3 Se 0.28511(7) 0.25057(7) 0.16528(11) 0.0066(4) Uani 1 1 d . . .


_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
Cs1 Se2 4.0402(18) 11_556 ?
Cs1 Se2 4.0403(18) 2 ?
Cs1 Se2 4.0402(18) 3 ?
Cs1 Se2 4.0402(18) 12_556 ?
Cs1 Se2 4.0402(18) . ?
Cs1 Se2 4.0402(18) 10_556 ?
Cs1 Se1 4.1164(17) 17_445 ?
Cs1 Se1 4.1164(17) 5 ?
Cs1 Se1 4.1164(17) 16 ?
Cs1 Se1 4.1164(17) 4_445 ?
Cs1 Se1 4.1165(17) 6_455 ?
Cs1 Se1 4.1165(17) 18_545 ?
Ho1 Se2 2.7924(15) 11 ?
Ho1 Se1 2.8113(14) . ?
Ho1 Se2 2.8296(16) . ?
Ho1 Se3 2.8807(15) . ?
Ho1 Se3 2.8876(15) 12 ?
Ho1 Se3 2.9115(15) 9_554 ?
Ho1 Ho2 3.9796(17) 6_455 ?
Ho2 Se1 2.7975(14) 14_455 ?
Ho2 Se2 2.8237(14) 8_554 ?
Ho2 Se1 2.8287(14) . ?
Ho2 Se3 2.8379(14) 12 ?
Ho2 Se1 2.8496(14) 8_554 ?
Ho2 Se3 2.8744(14) 14_455 ?
Ho2 Ho1 3.9796(17) 8_554 ?
Ho2 Cs1 4.8666(16) 7_554 ?
Ho3 Se2 2.8350(13) 3 ?
Ho3 Se2 2.8351(13) . ?
Ho3 Se2 2.8351(13) 11 ?
Ho3 Se2 2.8351(13) 10 ?
Ho3 Se2 2.8351(13) 12 ?
Ho3 Se2 2.8351(13) 2 ?
Se1 Ho2 2.7974(14) 15 ?
Se1 Ho2 2.8497(14) 6_455 ?
Se1 Cs1 4.1164(17) 7_554 ?
Se2 Cd1 2.7924(15) 12 ?
Se2 Ho1 2.7924(15) 12 ?
Se2 Ho2 2.8237(14) 6_455 ?
Se3 Ho2 2.8379(14) 11 ?
Se3 Ho2 2.8745(14) 15 ?
Se3 Ho1 2.8876(15) 11 ?
Se3 Cd1 2.8876(15) 11 ?
Se3 Ho1 2.9115(15) 5 ?
Se3 Cd1 2.9115(15) 5 ?

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
Se2 Cs1 Se2 180.0 11_556 2 ?
Se2 Cs1 Se2 120.25(4) 11_556 3 ?
Se2 Cs1 Se2 59.75(4) 2 3 ?
Se2 Cs1 Se2 59.75(4) 11_556 12_556 ?
Se2 Cs1 Se2 120.25(4) 2 12_556 ?
Se2 Cs1 Se2 180.00(3) 3 12_556 ?
Se2 Cs1 Se2 120.25(4) 11_556 . ?
Se2 Cs1 Se2 59.75(4) 2 . ?
Se2 Cs1 Se2 59.75(4) 3 . ?
Se2 Cs1 Se2 120.25(4) 12_556 . ?
Se2 Cs1 Se2 59.75(4) 11_556 10_556 ?
Se2 Cs1 Se2 120.25(4) 2 10_556 ?
Se2 Cs1 Se2 120.25(4) 3 10_556 ?
Se2 Cs1 Se2 59.75(4) 12_556 10_556 ?
Se2 Cs1 Se2 180.00(3) . 10_556 ?
Se2 Cs1 Se1 119.34(2) 11_556 17_445 ?
Se2 Cs1 Se1 60.66(2) 2 17_445 ?
Se2 Cs1 Se1 120.40(3) 3 17_445 ?
Se2 Cs1 Se1 59.60(3) 12_556 17_445 ?
Se2 Cs1 Se1 89.18(2) . 17_445 ?
Se2 Cs1 Se1 90.82(2) 10_556 17_445 ?
Se2 Cs1 Se1 60.66(2) 11_556 5 ?
Se2 Cs1 Se1 119.34(2) 2 5 ?
Se2 Cs1 Se1 59.60(3) 3 5 ?
Se2 Cs1 Se1 120.40(3) 12_556 5 ?
Se2 Cs1 Se1 90.82(2) . 5 ?
Se2 Cs1 Se1 89.18(2) 10_556 5 ?
Se1 Cs1 Se1 180.0 17_445 5 ?
Se2 Cs1 Se1 59.60(3) 11_556 16 ?
Se2 Cs1 Se1 120.40(3) 2 16 ?
Se2 Cs1 Se1 89.18(2) 3 16 ?
Se2 Cs1 Se1 90.82(2) 12_556 16 ?
Se2 Cs1 Se1 60.66(2) . 16 ?
Se2 Cs1 Se1 119.34(2) 10_556 16 ?
Se1 Cs1 Se1 120.0 17_445 16 ?
Se1 Cs1 Se1 60.0 5 16 ?
Se2 Cs1 Se1 120.40(3) 11_556 4_445 ?
Se2 Cs1 Se1 59.60(3) 2 4_445 ?
Se2 Cs1 Se1 90.82(2) 3 4_445 ?
Se2 Cs1 Se1 89.18(2) 12_556 4_445 ?
Se2 Cs1 Se1 119.34(2) . 4_445 ?
Se2 Cs1 Se1 60.66(2) 10_556 4_445 ?
Se1 Cs1 Se1 60.0 17_445 4_445 ?
Se1 Cs1 Se1 120.0 5 4_445 ?
Se1 Cs1 Se1 180.0 16 4_445 ?
Se2 Cs1 Se1 89.18(2) 11_556 6_455 ?
Se2 Cs1 Se1 90.82(2) 2 6_455 ?
Se2 Cs1 Se1 119.34(2) 3 6_455 ?
Se2 Cs1 Se1 60.66(2) 12_556 6_455 ?
Se2 Cs1 Se1 59.60(3) . 6_455 ?
Se2 Cs1 Se1 120.40(3) 10_556 6_455 ?
Se1 Cs1 Se1 60.0 17_445 6_455 ?
Se1 Cs1 Se1 120.0 5 6_455 ?
Se1 Cs1 Se1 60.0 16 6_455 ?
Se1 Cs1 Se1 120.0 4_445 6_455 ?
Se2 Cs1 Se1 90.82(2) 11_556 18_545 ?
Se2 Cs1 Se1 89.18(2) 2 18_545 ?
Se2 Cs1 Se1 60.66(2) 3 18_545 ?
Se2 Cs1 Se1 119.34(2) 12_556 18_545 ?
Se2 Cs1 Se1 120.40(3) . 18_545 ?
Se2 Cs1 Se1 59.60(3) 10_556 18_545 ?
Se1 Cs1 Se1 120.0 17_445 18_545 ?
Se1 Cs1 Se1 60.0 5 18_545 ?
Se1 Cs1 Se1 120.0 16 18_545 ?
Se1 Cs1 Se1 60.0 4_445 18_545 ?
Se1 Cs1 Se1 180.0 6_455 18_545 ?
Se2 Ho1 Se1 178.54(4) 11 . ?
Se2 Ho1 Se2 90.52(5) 11 . ?
Se1 Ho1 Se2 90.89(4) . . ?
Se2 Ho1 Se3 91.39(4) 11 . ?
Se1 Ho1 Se3 88.89(4) . . ?
Se2 Ho1 Se3 93.92(5) . . ?
Se2 Ho1 Se3 91.21(4) 11 12 ?
Se1 Ho1 Se3 88.39(4) . 12 ?
Se2 Ho1 Se3 90.50(4) . 12 ?
Se3 Ho1 Se3 174.85(5) . 12 ?
Se2 Ho1 Se3 88.03(4) 11 9_554 ?
Se1 Ho1 Se3 90.56(4) . 9_554 ?
Se2 Ho1 Se3 178.55(4) . 9_554 ?
Se3 Ho1 Se3 86.09(5) . 9_554 ?
Se3 Ho1 Se3 89.56(4) 12 9_554 ?
Se2 Ho1 Ho2 135.69(3) 11 6_455 ?
Se1 Ho1 Ho2 45.73(3) . 6_455 ?
Se2 Ho1 Ho2 45.20(3) . 6_455 ?
Se3 Ho1 Ho2 90.69(4) . 6_455 ?
Se3 Ho1 Ho2 90.55(4) 12 6_455 ?
Se3 Ho1 Ho2 136.25(3) 9_554 6_455 ?
Se1 Ho2 Se2 94.26(4) 14_455 8_554 ?
Se1 Ho2 Se1 94.05(4) 14_455 . ?
Se2 Ho2 Se1 91.66(4) 8_554 . ?
Se1 Ho2 Se3 175.51(4) 14_455 12 ?
Se2 Ho2 Se3 88.89(4) 8_554 12 ?
Se1 Ho2 Se3 89.04(4) . 12 ?
Se1 Ho2 Se1 89.09(4) 14_455 8_554 ?
Se2 Ho2 Se1 90.23(4) 8_554 8_554 ?
Se1 Ho2 Se1 176.21(3) . 8_554 ?
Se3 Ho2 Se1 87.71(4) 12 8_554 ?
Se1 Ho2 Se3 89.29(4) 14_455 14_455 ?
Se2 Ho2 Se3 176.38(4) 8_554 14_455 ?
Se1 Ho2 Se3 87.40(4) . 14_455 ?
Se3 Ho2 Se3 87.60(3) 12 14_455 ?
Se1 Ho2 Se3 90.51(4) 8_554 14_455 ?
Se1 Ho2 Ho1 91.04(4) 14_455 8_554 ?
Se2 Ho2 Ho1 45.32(3) 8_554 8_554 ?
Se1 Ho2 Ho1 136.96(3) . 8_554 ?
Se3 Ho2 Ho1 88.91(4) 12 8_554 ?
Se1 Ho2 Ho1 44.94(3) 8_554 8_554 ?
Se3 Ho2 Ho1 135.43(3) 14_455 8_554 ?
Se1 Ho2 Cs1 57.66(3) 14_455 7_554 ?
Se2 Ho2 Cs1 56.09(4) 8_554 7_554 ?
Se1 Ho2 Cs1 57.63(3) . 7_554 ?
Se3 Ho2 Cs1 126.82(3) 12 7_554 ?
Se1 Ho2 Cs1 126.06(3) 8_554 7_554 ?
Se3 Ho2 Cs1 125.84(4) 14_455 7_554 ?
Ho1 Ho2 Cs1 90.62(2) 8_554 7_554 ?
Se2 Ho3 Se2 90.46(4) 3 . ?
Se2 Ho3 Se2 89.54(4) 3 11 ?
Se2 Ho3 Se2 89.54(4) . 11 ?
Se2 Ho3 Se2 89.54(4) 3 10 ?
Se2 Ho3 Se2 180.00(6) . 10 ?
Se2 Ho3 Se2 90.46(4) 11 10 ?
Se2 Ho3 Se2 180.00(5) 3 12 ?
Se2 Ho3 Se2 89.54(4) . 12 ?
Se2 Ho3 Se2 90.46(4) 11 12 ?
Se2 Ho3 Se2 90.46(4) 10 12 ?
Se2 Ho3 Se2 90.46(4) 3 2 ?
Se2 Ho3 Se2 90.46(4) . 2 ?
Se2 Ho3 Se2 180.00(8) 11 2 ?
Se2 Ho3 Se2 89.54(4) 10 2 ?
Se2 Ho3 Se2 89.54(4) 12 2 ?
Ho2 Se1 Ho1 92.40(4) 15 . ?
Ho2 Se1 Ho2 174.16(5) 15 . ?
Ho1 Se1 Ho2 92.17(4) . . ?
Ho2 Se1 Ho2 90.91(4) 15 6_455 ?
Ho1 Se1 Ho2 89.33(4) . 6_455 ?
Ho2 Se1 Ho2 92.78(4) . 6_455 ?
Ho2 Se1 Cs1 87.29(3) 15 7_554 ?
Ho1 Se1 Cs1 135.69(4) . 7_554 ?
Ho2 Se1 Cs1 86.89(3) . 7_554 ?
Ho2 Se1 Cs1 134.97(4) 6_455 7_554 ?
Cd1 Se2 Ho1 0.00(2) 12 12 ?
Cd1 Se2 Ho2 92.91(4) 12 6_455 ?
Ho1 Se2 Ho2 92.91(4) 12 6_455 ?
Cd1 Se2 Ho1 90.44(4) 12 . ?
Ho1 Se2 Ho1 90.44(4) 12 . ?
Ho2 Se2 Ho1 89.49(4) 6_455 . ?
Cd1 Se2 Ho3 90.32(4) 12 . ?
Ho1 Se2 Ho3 90.32(4) 12 . ?
Ho2 Se2 Ho3 176.64(5) 6_455 . ?
Ho1 Se2 Ho3 89.57(4) . . ?
Cd1 Se2 Cs1 136.50(4) 12 . ?
Ho1 Se2 Cs1 136.50(4) 12 . ?
Ho2 Se2 Cs1 88.46(4) 6_455 . ?
Ho1 Se2 Cs1 133.06(4) . . ?
Ho3 Se2 Cs1 89.83(4) . . ?
Ho2 Se3 Ho2 92.07(4) 11 15 ?
Ho2 Se3 Ho1 93.86(4) 11 . ?
Ho2 Se3 Ho1 89.40(4) 15 . ?
Ho2 Se3 Ho1 90.40(4) 11 11 ?
Ho2 Se3 Ho1 176.19(5) 15 11 ?
Ho1 Se3 Ho1 87.55(4) . 11 ?
Ho2 Se3 Cd1 90.40(4) 11 11 ?
Ho2 Se3 Cd1 176.19(5) 15 11 ?
Ho1 Se3 Cd1 87.55(4) . 11 ?
Ho1 Se3 Cd1 0.00(3) 11 11 ?
Ho2 Se3 Ho1 90.15(4) 11 5 ?
Ho2 Se3 Ho1 92.44(4) 15 5 ?
Ho1 Se3 Ho1 175.53(5) . 5 ?
Ho1 Se3 Ho1 90.45(4) 11 5 ?
Cd1 Se3 Ho1 90.45(4) 11 5 ?
Ho2 Se3 Cd1 90.15(4) 11 5 ?
Ho2 Se3 Cd1 92.44(4) 15 5 ?
Ho1 Se3 Cd1 175.53(5) . 5 ?
Ho1 Se3 Cd1 90.45(4) 11 5 ?
Cd1 Se3 Cd1 90.45(4) 11 5 ?
Ho1 Se3 Cd1 0.00(3) 5 5 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         4.853
_refine_diff_density_min         -4.011
_refine_diff_density_rms         0.878
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsTb9Cd4Se18
_database_code_depnum_ccdc_archive 'CCDC 1444681'
_audit_update_record             
;
2015-12-29 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd4 Cs Se18 Tb9'
_chemical_formula_sum            'Cd4 Cs Se18 Tb9'
_chemical_formula_weight         3434.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.7731(11)
_cell_length_b                   17.7731(11)
_cell_length_c                   9.9180(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2713.2(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1178
_cell_measurement_theta_min      2.2917
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.0900
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4332
_exptl_absorpt_coefficient_mu    38.731
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3571
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Mercury2
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5854
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1062
_reflns_number_gt                1025
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0613P)²+82.2931P] 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     SHELXL
_refine_ls_extinction_coef       0.00074(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1062
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_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
Cs1 Cs 0.0000 0.0000 0.5000 0.0515(6) Uani 1 6 d S . .
Tb1 Tb 0.15422(3) 0.25980(3) 0.00260(6) 0.0127(2) Uani 0.33 1 d P . .
Cd1 Cd 0.15422(3) 0.25980(3) 0.00260(6) 0.0127(2) Uani 0.67 1 d P . .
Tb2 Tb 0.05724(3) 0.42570(3) 0.00234(4) 0.0090(2) Uani 1 1 d . . .
Tb3 Tb 0.0000 0.0000 0.0000 0.0065(3) Uani 1 6 d S . .
Se1 Se 0.17319(5) 0.39839(5) 0.16572(8) 0.0081(3) Uani 1 1 d . . .
Se2 Se 0.01303(6) 0.13808(5) 0.16399(8) 0.0105(3) Uani 1 1 d . . .
Se3 Se 0.28484(5) 0.25040(5) 0.16523(8) 0.0065(3) Uani 1 1 d . . .


_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
Cs1 Se2 4.0759(9) 11_556 ?
Cs1 Se2 4.0759(9) 2 ?
Cs1 Se2 4.0759(9) 3 ?
Cs1 Se2 4.0759(9) . ?
Cs1 Se2 4.0759(9) 12_556 ?
Cs1 Se2 4.0759(9) 10_556 ?
Cs1 Se1 4.1551(8) 17_445 ?
Cs1 Se1 4.1551(8) 5 ?
Cs1 Se1 4.1551(8) 4_445 ?
Cs1 Se1 4.1551(8) 16 ?
Cs1 Se1 4.1552(8) 18_545 ?
Cs1 Se1 4.1552(8) 6_455 ?
Tb1 Se2 2.8038(10) 11 ?
Tb1 Se1 2.8228(10) . ?
Tb1 Se2 2.8479(10) . ?
Tb1 Se3 2.8994(10) . ?
Tb1 Se3 2.9067(10) 12 ?
Tb1 Se3 2.9334(10) 9_554 ?
Tb1 Tb2 4.0113(8) 6_455 ?
Tb2 Se1 2.8200(9) 14_455 ?
Tb2 Se2 2.8474(9) 8_554 ?
Tb2 Se1 2.8476(9) . ?
Tb2 Se3 2.8599(9) 12 ?
Tb2 Se1 2.8728(9) 8_554 ?
Tb2 Se3 2.8938(9) 14_455 ?
Tb2 Tb1 4.0112(8) 8_554 ?
Tb2 Cs1 4.9053(5) 7_554 ?
Tb3 Se2 2.8553(8) . ?
Tb3 Se2 2.8553(8) 3 ?
Tb3 Se2 2.8553(8) 11 ?
Tb3 Se2 2.8553(8) 10 ?
Tb3 Se2 2.8553(8) 12 ?
Tb3 Se2 2.8553(8) 2 ?
Se1 Tb2 2.8199(9) 15 ?
Se1 Tb2 2.8729(9) 6_455 ?
Se1 Cs1 4.1551(8) 7_554 ?
Se2 Cd1 2.8038(10) 12 ?
Se2 Tb1 2.8038(10) 12 ?
Se2 Tb2 2.8474(9) 6_455 ?
Se3 Tb2 2.8599(9) 11 ?
Se3 Tb2 2.8939(9) 15 ?
Se3 Tb1 2.9067(10) 11 ?
Se3 Cd1 2.9067(10) 11 ?
Se3 Tb1 2.9333(10) 5 ?
Se3 Cd1 2.9333(10) 5 ?

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
Se2 Cs1 Se2 180.0 11_556 2 ?
Se2 Cs1 Se2 120.181(19) 11_556 3 ?
Se2 Cs1 Se2 59.819(19) 2 3 ?
Se2 Cs1 Se2 120.181(19) 11_556 . ?
Se2 Cs1 Se2 59.819(19) 2 . ?
Se2 Cs1 Se2 59.819(19) 3 . ?
Se2 Cs1 Se2 59.819(19) 11_556 12_556 ?
Se2 Cs1 Se2 120.181(19) 2 12_556 ?
Se2 Cs1 Se2 180.00(2) 3 12_556 ?
Se2 Cs1 Se2 120.181(19) . 12_556 ?
Se2 Cs1 Se2 59.819(19) 11_556 10_556 ?
Se2 Cs1 Se2 120.181(19) 2 10_556 ?
Se2 Cs1 Se2 120.181(19) 3 10_556 ?
Se2 Cs1 Se2 180.00(2) . 10_556 ?
Se2 Cs1 Se2 59.819(19) 12_556 10_556 ?
Se2 Cs1 Se1 119.287(16) 11_556 17_445 ?
Se2 Cs1 Se1 60.713(16) 2 17_445 ?
Se2 Cs1 Se1 120.514(16) 3 17_445 ?
Se2 Cs1 Se1 89.252(17) . 17_445 ?
Se2 Cs1 Se1 59.486(16) 12_556 17_445 ?
Se2 Cs1 Se1 90.748(17) 10_556 17_445 ?
Se2 Cs1 Se1 60.713(16) 11_556 5 ?
Se2 Cs1 Se1 119.287(16) 2 5 ?
Se2 Cs1 Se1 59.486(16) 3 5 ?
Se2 Cs1 Se1 90.748(17) . 5 ?
Se2 Cs1 Se1 120.514(16) 12_556 5 ?
Se2 Cs1 Se1 89.252(17) 10_556 5 ?
Se1 Cs1 Se1 180.00(2) 17_445 5 ?
Se2 Cs1 Se1 120.515(16) 11_556 4_445 ?
Se2 Cs1 Se1 59.485(16) 2 4_445 ?
Se2 Cs1 Se1 90.749(17) 3 4_445 ?
Se2 Cs1 Se1 119.286(16) . 4_445 ?
Se2 Cs1 Se1 89.251(17) 12_556 4_445 ?
Se2 Cs1 Se1 60.714(16) 10_556 4_445 ?
Se1 Cs1 Se1 60.0 17_445 4_445 ?
Se1 Cs1 Se1 120.0 5 4_445 ?
Se2 Cs1 Se1 59.485(16) 11_556 16 ?
Se2 Cs1 Se1 120.515(16) 2 16 ?
Se2 Cs1 Se1 89.251(17) 3 16 ?
Se2 Cs1 Se1 60.714(16) . 16 ?
Se2 Cs1 Se1 90.749(17) 12_556 16 ?
Se2 Cs1 Se1 119.286(16) 10_556 16 ?
Se1 Cs1 Se1 120.0 17_445 16 ?
Se1 Cs1 Se1 60.0 5 16 ?
Se1 Cs1 Se1 180.00(3) 4_445 16 ?
Se2 Cs1 Se1 90.748(17) 11_556 18_545 ?
Se2 Cs1 Se1 89.252(17) 2 18_545 ?
Se2 Cs1 Se1 60.713(16) 3 18_545 ?
Se2 Cs1 Se1 120.514(16) . 18_545 ?
Se2 Cs1 Se1 119.287(16) 12_556 18_545 ?
Se2 Cs1 Se1 59.486(16) 10_556 18_545 ?
Se1 Cs1 Se1 120.0 17_445 18_545 ?
Se1 Cs1 Se1 60.0 5 18_545 ?
Se1 Cs1 Se1 60.0 4_445 18_545 ?
Se1 Cs1 Se1 120.0 16 18_545 ?
Se2 Cs1 Se1 89.252(17) 11_556 6_455 ?
Se2 Cs1 Se1 90.748(17) 2 6_455 ?
Se2 Cs1 Se1 119.287(16) 3 6_455 ?
Se2 Cs1 Se1 59.486(16) . 6_455 ?
Se2 Cs1 Se1 60.713(16) 12_556 6_455 ?
Se2 Cs1 Se1 120.514(16) 10_556 6_455 ?
Se1 Cs1 Se1 60.0 17_445 6_455 ?
Se1 Cs1 Se1 120.0 5 6_455 ?
Se1 Cs1 Se1 120.0 4_445 6_455 ?
Se1 Cs1 Se1 60.0 16 6_455 ?
Se1 Cs1 Se1 180.00(2) 18_545 6_455 ?
Se2 Tb1 Se1 178.62(3) 11 . ?
Se2 Tb1 Se2 90.42(4) 11 . ?
Se1 Tb1 Se2 90.93(3) . . ?
Se2 Tb1 Se3 91.24(3) 11 . ?
Se1 Tb1 Se3 88.95(3) . . ?
Se2 Tb1 Se3 94.03(3) . . ?
Se2 Tb1 Se3 91.34(3) 11 12 ?
Se1 Tb1 Se3 88.38(3) . 12 ?
Se2 Tb1 Se3 90.20(3) . 12 ?
Se3 Tb1 Se3 175.03(4) . 12 ?
Se2 Tb1 Se3 88.22(3) 11 9_554 ?
Se1 Tb1 Se3 90.43(3) . 9_554 ?
Se2 Tb1 Se3 178.63(3) . 9_554 ?
Se3 Tb1 Se3 86.13(3) . 9_554 ?
Se3 Tb1 Se3 89.69(3) 12 9_554 ?
Se2 Tb1 Tb2 135.62(2) 11 6_455 ?
Se1 Tb1 Tb2 45.740(19) . 6_455 ?
Se2 Tb1 Tb2 45.221(19) . 6_455 ?
Se3 Tb1 Tb2 90.72(2) . 6_455 ?
Se3 Tb1 Tb2 90.41(2) 12 6_455 ?
Se3 Tb1 Tb2 136.14(2) 9_554 6_455 ?
Se1 Tb2 Se2 94.47(3) 14_455 8_554 ?
Se1 Tb2 Se1 94.30(3) 14_455 . ?
Se2 Tb2 Se1 91.64(3) 8_554 . ?
Se1 Tb2 Se3 175.39(3) 14_455 12 ?
Se2 Tb2 Se3 88.83(3) 8_554 12 ?
Se1 Tb2 Se3 88.82(3) . 12 ?
Se1 Tb2 Se1 88.99(3) 14_455 8_554 ?
Se2 Tb2 Se1 89.92(3) 8_554 8_554 ?
Se1 Tb2 Se1 176.24(2) . 8_554 ?
Se3 Tb2 Se1 87.79(3) 12 8_554 ?
Se1 Tb2 Se3 89.12(3) 14_455 14_455 ?
Se2 Tb2 Se3 176.39(3) 8_554 14_455 ?
Se1 Tb2 Se3 87.62(3) . 14_455 ?
Se3 Tb2 Se3 87.617(13) 12 14_455 ?
Se1 Tb2 Se3 90.61(3) 8_554 14_455 ?
Se1 Tb2 Tb1 91.03(2) 14_455 8_554 ?
Se2 Tb2 Tb1 45.23(2) 8_554 8_554 ?
Se1 Tb2 Tb1 136.85(2) . 8_554 ?
Se3 Tb2 Tb1 89.01(2) 12 8_554 ?
Se1 Tb2 Tb1 44.724(19) 8_554 8_554 ?
Se3 Tb2 Tb1 135.31(2) 14_455 8_554 ?
Se1 Tb2 Cs1 57.785(18) 14_455 7_554 ?
Se2 Tb2 Cs1 56.160(19) 8_554 7_554 ?
Se1 Tb2 Cs1 57.754(18) . 7_554 ?
Se3 Tb2 Cs1 126.826(18) 12 7_554 ?
Se1 Tb2 Cs1 125.814(19) 8_554 7_554 ?
Se3 Tb2 Cs1 125.95(2) 14_455 7_554 ?
Tb1 Tb2 Cs1 90.528(11) 8_554 7_554 ?
Se2 Tb3 Se2 90.76(2) . 3 ?
Se2 Tb3 Se2 89.24(2) . 11 ?
Se2 Tb3 Se2 89.24(2) 3 11 ?
Se2 Tb3 Se2 180.00(4) . 10 ?
Se2 Tb3 Se2 89.24(2) 3 10 ?
Se2 Tb3 Se2 90.76(2) 11 10 ?
Se2 Tb3 Se2 89.24(2) . 12 ?
Se2 Tb3 Se2 180.00(4) 3 12 ?
Se2 Tb3 Se2 90.76(2) 11 12 ?
Se2 Tb3 Se2 90.76(2) 10 12 ?
Se2 Tb3 Se2 90.76(2) . 2 ?
Se2 Tb3 Se2 90.76(2) 3 2 ?
Se2 Tb3 Se2 180.00(6) 11 2 ?
Se2 Tb3 Se2 89.24(2) 10 2 ?
Se2 Tb3 Se2 89.24(2) 12 2 ?
Tb2 Se1 Tb1 92.49(3) 15 . ?
Tb2 Se1 Tb2 173.94(4) 15 . ?
Tb1 Se1 Tb2 92.39(3) . . ?
Tb2 Se1 Tb2 91.01(3) 15 6_455 ?
Tb1 Se1 Tb2 89.54(3) . 6_455 ?
Tb2 Se1 Tb2 92.62(3) . 6_455 ?
Tb2 Se1 Cs1 87.17(2) 15 7_554 ?
Tb1 Se1 Cs1 135.81(3) . 7_554 ?
Tb2 Se1 Cs1 86.82(2) . 7_554 ?
Tb2 Se1 Cs1 134.65(3) 6_455 7_554 ?
Cd1 Se2 Tb1 0.000(19) 12 12 ?
Cd1 Se2 Tb2 92.93(3) 12 6_455 ?
Tb1 Se2 Tb2 92.93(3) 12 6_455 ?
Cd1 Se2 Tb1 90.75(2) 12 . ?
Tb1 Se2 Tb1 90.75(2) 12 . ?
Tb2 Se2 Tb1 89.55(3) 6_455 . ?
Cd1 Se2 Tb3 90.59(3) 12 . ?
Tb1 Se2 Tb3 90.59(3) 12 . ?
Tb2 Se2 Tb3 176.41(4) 6_455 . ?
Tb1 Se2 Tb3 89.70(3) . . ?
Cd1 Se2 Cs1 136.40(3) 12 . ?
Tb1 Se2 Cs1 136.40(3) 12 . ?
Tb2 Se2 Cs1 88.37(2) 6_455 . ?
Tb1 Se2 Cs1 132.85(3) . . ?
Tb3 Se2 Cs1 89.57(2) . . ?
Tb2 Se3 Tb2 91.93(2) 11 15 ?
Tb2 Se3 Tb1 93.83(3) 11 . ?
Tb2 Se3 Tb1 89.42(2) 15 . ?
Tb2 Se3 Tb1 90.41(3) 11 11 ?
Tb2 Se3 Tb1 176.41(3) 15 11 ?
Tb1 Se3 Tb1 87.70(3) . 11 ?
Tb2 Se3 Cd1 90.41(3) 11 11 ?
Tb2 Se3 Cd1 176.41(3) 15 11 ?
Tb1 Se3 Cd1 87.70(3) . 11 ?
Tb1 Se3 Cd1 0.00(3) 11 11 ?
Tb2 Se3 Tb1 90.00(3) 11 5 ?
Tb2 Se3 Tb1 92.42(3) 15 5 ?
Tb1 Se3 Tb1 175.69(4) . 5 ?
Tb1 Se3 Tb1 90.31(3) 11 5 ?
Cd1 Se3 Tb1 90.31(3) 11 5 ?
Tb2 Se3 Cd1 90.00(3) 11 5 ?
Tb2 Se3 Cd1 92.42(3) 15 5 ?
Tb1 Se3 Cd1 175.69(4) . 5 ?
Tb1 Se3 Cd1 90.31(3) 11 5 ?
Cd1 Se3 Cd1 90.31(3) 11 5 ?
Tb1 Se3 Cd1 0.00(3) 5 5 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.986
_refine_diff_density_min         -3.138
_refine_diff_density_rms         0.602
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsTm9Cd4Se18
_database_code_depnum_ccdc_archive 'CCDC 1444682'
_audit_update_record             
;
2015-12-29 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd4 Cs Se18 Tm9'
_chemical_formula_sum            'Cd4 Cs Se18 Tm9'
_chemical_formula_weight         3524.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.489(6)
_cell_length_b                   17.489(6)
_cell_length_c                   9.765(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2586.5(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2814
_cell_measurement_theta_min      3.4043
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.1250
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.1100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4440
_exptl_absorpt_coefficient_mu    45.325
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2124
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5287
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         24.98
_reflns_number_total             975
_reflns_number_gt                931
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0711P)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     SHELXL
_refine_ls_extinction_coef       0.00097(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         975
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
Cs1 Cs 0.0000 0.0000 0.5000 0.0395(6) Uani 1 6 d S . .
Tm1 Tm 0.22764(3) 0.40696(4) 0.66317(6) 0.0078(3) Uani 0.33 1 d P . .
Cd1 Cd 0.22764(3) 0.40696(4) 0.66317(6) 0.0078(3) Uani 0.67 1 d P . .
Tm2 Tm 0.27621(3) 0.03540(3) 0.66480(4) 0.0084(3) Uani 1 1 d . . .
Tm3 Tm 0.0000 0.0000 0.0000 0.0065(3) Uani 1 6 d S . .
Se1 Se 0.10755(6) 0.26755(6) 0.50026(10) 0.0062(4) Uani 1 1 d . . .
Se2 Se 0.13745(7) 0.01283(7) 0.83488(9) 0.0084(4) Uani 1 1 d . . .
Se3 Se 0.08271(7) 0.38133(6) 0.83217(9) 0.0058(4) Uani 1 1 d . . .


_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
Cs1 Se2 3.9978(17) 2 ?
Cs1 Se2 3.9978(17) 10_556 ?
Cs1 Se2 3.9978(17) . ?
Cs1 Se2 3.9978(17) 11_556 ?
Cs1 Se2 3.9978(17) 3 ?
Cs1 Se2 3.9978(17) 12_556 ?
Cs1 Se1 4.0781(17) 11_556 ?
Cs1 Se1 4.0781(17) 2 ?
Cs1 Se1 4.0781(17) . ?
Cs1 Se1 4.0781(17) 10_556 ?
Cs1 Se1 4.0781(17) 3 ?
Cs1 Se1 4.0781(17) 12_556 ?
Tm1 Se2 2.7735(14) 17_556 ?
Tm1 Se1 2.7866(13) . ?
Tm1 Se2 2.8070(14) 9_554 ?
Tm1 Se3 2.8578(14) 15_556 ?
Tm1 Se3 2.8657(14) . ?
Tm1 Se3 2.8879(14) 16_556 ?
Tm1 Tm2 3.9340(16) 9_554 ?
Tm2 Se1 2.7748(13) 11_556 ?
Tm2 Se2 2.8011(13) . ?
Tm2 Se1 2.8073(13) 3 ?
Tm2 Se3 2.8109(13) 3 ?
Tm2 Se1 2.8233(13) 5 ?
Tm2 Se3 2.8491(13) 7_544 ?
Tm2 Tm1 3.9341(16) 5 ?
Tm3 Se2 2.8086(12) 12_556 ?
Tm3 Se2 2.8086(12) 3_554 ?
Tm3 Se2 2.8086(12) 10_556 ?
Tm3 Se2 2.8086(12) 11_556 ?
Tm3 Se2 2.8086(12) 1_554 ?
Tm3 Se2 2.8086(12) 2_554 ?
Se1 Tm2 2.7748(13) 12_556 ?
Se1 Tm2 2.8073(13) 2 ?
Se1 Tm2 2.8232(13) 9_554 ?
Se2 Cd1 2.7736(14) 18_546 ?
Se2 Tm1 2.7736(14) 18_546 ?
Se2 Cd1 2.8071(14) 5 ?
Se2 Tm1 2.8071(14) 5 ?
Se2 Tm3 2.8086(12) 1_556 ?
Se3 Tm2 2.8109(13) 2 ?
Se3 Tm2 2.8491(13) 4_455 ?
Se3 Cd1 2.8579(14) 14_456 ?
Se3 Tm1 2.8579(14) 14_456 ?
Se3 Cd1 2.8879(14) 16_556 ?
Se3 Tm1 2.8879(14) 16_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
Se2 Cs1 Se2 120.24(4) 2 10_556 ?
Se2 Cs1 Se2 59.76(4) 2 . ?
Se2 Cs1 Se2 180.0 10_556 . ?
Se2 Cs1 Se2 180.0 2 11_556 ?
Se2 Cs1 Se2 59.76(4) 10_556 11_556 ?
Se2 Cs1 Se2 120.24(4) . 11_556 ?
Se2 Cs1 Se2 59.76(4) 2 3 ?
Se2 Cs1 Se2 120.24(4) 10_556 3 ?
Se2 Cs1 Se2 59.76(4) . 3 ?
Se2 Cs1 Se2 120.24(4) 11_556 3 ?
Se2 Cs1 Se2 120.24(4) 2 12_556 ?
Se2 Cs1 Se2 59.76(4) 10_556 12_556 ?
Se2 Cs1 Se2 120.24(4) . 12_556 ?
Se2 Cs1 Se2 59.76(4) 11_556 12_556 ?
Se2 Cs1 Se2 180.0 3 12_556 ?
Se2 Cs1 Se1 89.104(19) 2 11_556 ?
Se2 Cs1 Se1 119.30(2) 10_556 11_556 ?
Se2 Cs1 Se1 60.70(2) . 11_556 ?
Se2 Cs1 Se1 90.896(19) 11_556 11_556 ?
Se2 Cs1 Se1 120.44(2) 3 11_556 ?
Se2 Cs1 Se1 59.56(2) 12_556 11_556 ?
Se2 Cs1 Se1 90.896(19) 2 2 ?
Se2 Cs1 Se1 60.70(2) 10_556 2 ?
Se2 Cs1 Se1 119.30(2) . 2 ?
Se2 Cs1 Se1 89.104(19) 11_556 2 ?
Se2 Cs1 Se1 59.56(2) 3 2 ?
Se2 Cs1 Se1 120.44(2) 12_556 2 ?
Se1 Cs1 Se1 180.0 11_556 2 ?
Se2 Cs1 Se1 59.56(2) 2 . ?
Se2 Cs1 Se1 89.104(19) 10_556 . ?
Se2 Cs1 Se1 90.896(19) . . ?
Se2 Cs1 Se1 120.44(2) 11_556 . ?
Se2 Cs1 Se1 119.30(2) 3 . ?
Se2 Cs1 Se1 60.70(2) 12_556 . ?
Se1 Cs1 Se1 60.0 11_556 . ?
Se1 Cs1 Se1 120.0 2 . ?
Se2 Cs1 Se1 120.44(2) 2 10_556 ?
Se2 Cs1 Se1 90.896(19) 10_556 10_556 ?
Se2 Cs1 Se1 89.104(19) . 10_556 ?
Se2 Cs1 Se1 59.56(2) 11_556 10_556 ?
Se2 Cs1 Se1 60.70(2) 3 10_556 ?
Se2 Cs1 Se1 119.30(2) 12_556 10_556 ?
Se1 Cs1 Se1 120.0 11_556 10_556 ?
Se1 Cs1 Se1 60.0 2 10_556 ?
Se1 Cs1 Se1 180.00(3) . 10_556 ?
Se2 Cs1 Se1 119.30(2) 2 3 ?
Se2 Cs1 Se1 120.44(2) 10_556 3 ?
Se2 Cs1 Se1 59.56(2) . 3 ?
Se2 Cs1 Se1 60.70(2) 11_556 3 ?
Se2 Cs1 Se1 90.896(19) 3 3 ?
Se2 Cs1 Se1 89.104(19) 12_556 3 ?
Se1 Cs1 Se1 60.0 11_556 3 ?
Se1 Cs1 Se1 120.0 2 3 ?
Se1 Cs1 Se1 120.0 . 3 ?
Se1 Cs1 Se1 60.0 10_556 3 ?
Se2 Cs1 Se1 60.70(2) 2 12_556 ?
Se2 Cs1 Se1 59.56(2) 10_556 12_556 ?
Se2 Cs1 Se1 120.44(2) . 12_556 ?
Se2 Cs1 Se1 119.30(2) 11_556 12_556 ?
Se2 Cs1 Se1 89.104(19) 3 12_556 ?
Se2 Cs1 Se1 90.896(19) 12_556 12_556 ?
Se1 Cs1 Se1 120.0 11_556 12_556 ?
Se1 Cs1 Se1 60.0 2 12_556 ?
Se1 Cs1 Se1 60.0 . 12_556 ?
Se1 Cs1 Se1 120.0 10_556 12_556 ?
Se1 Cs1 Se1 180.0 3 12_556 ?
Se2 Tm1 Se1 178.24(4) 17_556 . ?
Se2 Tm1 Se2 90.43(5) 17_556 9_554 ?
Se1 Tm1 Se2 91.21(4) . 9_554 ?
Se2 Tm1 Se3 91.48(4) 17_556 15_556 ?
Se1 Tm1 Se3 89.05(4) . 15_556 ?
Se2 Tm1 Se3 94.11(4) 9_554 15_556 ?
Se2 Tm1 Se3 90.99(4) 17_556 . ?
Se1 Tm1 Se3 88.35(4) . . ?
Se2 Tm1 Se3 90.63(4) 9_554 . ?
Se3 Tm1 Se3 174.64(4) 15_556 . ?
Se2 Tm1 Se3 87.91(4) 17_556 16_556 ?
Se1 Tm1 Se3 90.45(4) . 16_556 ?
Se2 Tm1 Se3 178.34(4) 9_554 16_556 ?
Se3 Tm1 Se3 85.96(4) 15_556 16_556 ?
Se3 Tm1 Se3 89.38(4) . 16_556 ?
Se2 Tm1 Tm2 135.80(3) 17_556 9_554 ?
Se1 Tm1 Tm2 45.85(2) . 9_554 ?
Se2 Tm1 Tm2 45.39(2) 9_554 9_554 ?
Se3 Tm1 Tm2 90.93(4) 15_556 9_554 ?
Se3 Tm1 Tm2 90.62(4) . 9_554 ?
Se3 Tm1 Tm2 136.27(3) 16_556 9_554 ?
Se1 Tm2 Se2 94.09(4) 11_556 . ?
Se1 Tm2 Se1 93.86(4) 11_556 3 ?
Se2 Tm2 Se1 91.34(4) . 3 ?
Se1 Tm2 Se3 175.77(3) 11_556 3 ?
Se2 Tm2 Se3 88.91(4) . 3 ?
Se1 Tm2 Se3 89.04(4) 3 3 ?
Se1 Tm2 Se1 89.16(4) 11_556 5 ?
Se2 Tm2 Se1 90.58(4) . 5 ?
Se1 Tm2 Se1 176.30(3) 3 5 ?
Se3 Tm2 Se1 87.83(4) 3 5 ?
Se1 Tm2 Se3 89.46(4) 11_556 7_544 ?
Se2 Tm2 Se3 176.30(3) . 7_544 ?
Se1 Tm2 Se3 87.39(4) 3 7_544 ?
Se3 Tm2 Se3 87.59(3) 3 7_544 ?
Se1 Tm2 Se3 90.50(4) 5 7_544 ?
Se1 Tm2 Tm1 90.97(4) 11_556 5 ?
Se2 Tm2 Tm1 45.52(3) . 5 ?
Se1 Tm2 Tm1 136.84(3) 3 5 ?
Se3 Tm2 Tm1 89.01(4) 3 5 ?
Se1 Tm2 Tm1 45.09(2) 5 5 ?
Se3 Tm2 Tm1 135.56(3) 7_544 5 ?
Se1 Tm2 Cs1 57.53(2) 11_556 . ?
Se2 Tm2 Cs1 55.86(3) . . ?
Se1 Tm2 Cs1 57.50(2) 3 . ?
Se3 Tm2 Cs1 126.70(2) 3 . ?
Se1 Tm2 Cs1 126.12(2) 5 . ?
Se3 Tm2 Cs1 125.83(4) 7_544 . ?
Tm1 Tm2 Cs1 90.55(2) 5 . ?
Se2 Tm3 Se2 180.00(5) 12_556 3_554 ?
Se2 Tm3 Se2 90.32(4) 12_556 10_556 ?
Se2 Tm3 Se2 89.68(4) 3_554 10_556 ?
Se2 Tm3 Se2 90.32(4) 12_556 11_556 ?
Se2 Tm3 Se2 89.68(4) 3_554 11_556 ?
Se2 Tm3 Se2 90.32(4) 10_556 11_556 ?
Se2 Tm3 Se2 89.68(4) 12_556 1_554 ?
Se2 Tm3 Se2 90.32(4) 3_554 1_554 ?
Se2 Tm3 Se2 180.00(4) 10_556 1_554 ?
Se2 Tm3 Se2 89.68(4) 11_556 1_554 ?
Se2 Tm3 Se2 89.68(4) 12_556 2_554 ?
Se2 Tm3 Se2 90.32(4) 3_554 2_554 ?
Se2 Tm3 Se2 89.68(4) 10_556 2_554 ?
Se2 Tm3 Se2 180.00(5) 11_556 2_554 ?
Se2 Tm3 Se2 90.32(4) 1_554 2_554 ?
Tm2 Se1 Tm1 92.22(4) 12_556 . ?
Tm2 Se1 Tm2 174.41(4) 12_556 2 ?
Tm1 Se1 Tm2 92.17(4) . 2 ?
Tm2 Se1 Tm2 90.84(4) 12_556 9_554 ?
Tm1 Se1 Tm2 89.06(4) . 9_554 ?
Tm2 Se1 Tm2 92.68(4) 2 9_554 ?
Tm2 Se1 Cs1 87.43(2) 12_556 . ?
Tm1 Se1 Cs1 135.86(3) . . ?
Tm2 Se1 Cs1 87.01(2) 2 . ?
Tm2 Se1 Cs1 135.08(3) 9_554 . ?
Cd1 Se2 Tm1 0.000(15) 18_546 18_546 ?
Cd1 Se2 Tm2 92.88(4) 18_546 . ?
Tm1 Se2 Tm2 92.88(4) 18_546 . ?
Cd1 Se2 Cd1 90.31(4) 18_546 5 ?
Tm1 Se2 Cd1 90.31(4) 18_546 5 ?
Tm2 Se2 Cd1 89.09(4) . 5 ?
Cd1 Se2 Tm1 90.31(4) 18_546 5 ?
Tm1 Se2 Tm1 90.31(4) 18_546 5 ?
Tm2 Se2 Tm1 89.09(4) . 5 ?
Cd1 Se2 Tm1 0.00(3) 5 5 ?
Cd1 Se2 Tm3 90.26(4) 18_546 1_556 ?
Tm1 Se2 Tm3 90.26(4) 18_546 1_556 ?
Tm2 Se2 Tm3 176.59(4) . 1_556 ?
Cd1 Se2 Tm3 89.58(4) 5 1_556 ?
Tm1 Se2 Tm3 89.58(4) 5 1_556 ?
Cd1 Se2 Cs1 136.74(4) 18_546 . ?
Tm1 Se2 Cs1 136.74(4) 18_546 . ?
Tm2 Se2 Cs1 88.69(4) . . ?
Cd1 Se2 Cs1 132.96(4) 5 . ?
Tm1 Se2 Cs1 132.96(4) 5 . ?
Tm3 Se2 Cs1 89.92(4) 1_556 . ?
Tm2 Se3 Tm2 92.06(4) 2 4_455 ?
Tm2 Se3 Cd1 93.95(4) 2 14_456 ?
Tm2 Se3 Cd1 89.23(4) 4_455 14_456 ?
Tm2 Se3 Tm1 93.95(4) 2 14_456 ?
Tm2 Se3 Tm1 89.23(4) 4_455 14_456 ?
Cd1 Se3 Tm1 0.00(3) 14_456 14_456 ?
Tm2 Se3 Tm1 90.44(4) 2 . ?
Tm2 Se3 Tm1 175.98(4) 4_455 . ?
Cd1 Se3 Tm1 87.47(4) 14_456 . ?
Tm1 Se3 Tm1 87.47(4) 14_456 . ?
Tm2 Se3 Cd1 90.28(4) 2 16_556 ?
Tm2 Se3 Cd1 92.51(4) 4_455 16_556 ?
Cd1 Se3 Cd1 175.37(4) 14_456 16_556 ?
Tm1 Se3 Cd1 175.37(4) 14_456 16_556 ?
Tm1 Se3 Cd1 90.62(4) . 16_556 ?
Tm2 Se3 Tm1 90.28(4) 2 16_556 ?
Tm2 Se3 Tm1 92.51(4) 4_455 16_556 ?
Cd1 Se3 Tm1 175.37(4) 14_456 16_556 ?
Tm1 Se3 Tm1 175.37(4) 14_456 16_556 ?
Tm1 Se3 Tm1 90.62(4) . 16_556 ?
Cd1 Se3 Tm1 0.000(15) 16_556 16_556 ?

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         3.169
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.444
