# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_yr_nzsse_1a
_database_code_depnum_ccdc_archive 'CCDC 1955642'
loop_
_audit_author_name
_audit_author_address
'Run Ye'
;FJIRSM
China
;
_audit_update_record             
;
2019-09-24 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;
_audit_creation_date             2019-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Na2ZnSn2Se6
_chemical_name_systematic        Na2ZnSn2Se6
_chemical_formula_moiety         '0.13(Na16 Se48 Sn16 Zn8)'
_chemical_formula_sum            'Na2 Se6 Sn2 Zn'
_chemical_formula_weight         822.49
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   24.6051(7)
_cell_length_b                   13.5164(4)
_cell_length_c                   7.6031(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2528.58(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14014
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6660
_cell_measurement_theta_min      3.9920
_shelx_estimated_absorpt_T_max   0.444
_shelx_estimated_absorpt_T_min   0.391
_exptl_absorpt_coefficient_mu    23.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19055
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.251
_diffrn_reflns_theta_min         3.953
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00 -64.00   0.50    4.50    --   -0.40  45.00 150.00   50
  2  ω    -41.00  48.00   0.50    4.50    --   -0.40  45.00 150.00  178
  3  ω     61.00  89.00   0.50    4.50    --   -0.40  45.00 150.00   56
  4  ω    -89.00  89.00   0.50    4.50    --   -0.40  45.00  60.00  356
  5  ω    -89.00 -62.00   0.50    4.50    --   -0.40  45.00 120.00   54
  6  ω    -47.00  35.00   0.50    4.50    --   -0.40  45.00 120.00  164
  7  ω     43.00  88.00   0.50    4.50    --   -0.40  45.00 120.00   90
  8  ω    -89.00  89.00   0.50    4.50    --   -0.40  45.00   0.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000720000
_diffrn_orient_matrix_UB_12      0.0127651000
_diffrn_orient_matrix_UB_13      -0.0904970000
_diffrn_orient_matrix_UB_21      0.0136120000
_diffrn_orient_matrix_UB_22      -0.0448578000
_diffrn_orient_matrix_UB_23      -0.0198963000
_diffrn_orient_matrix_UB_31      -0.0254160000
_diffrn_orient_matrix_UB_32      -0.0240580000
_diffrn_orient_matrix_UB_33      -0.0108064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                1930
_reflns_number_total             1960
_reflns_odcompleteness_completeness 99.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 
;
 Flack x determined using 857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1960
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0156
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²+5.3602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0358
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sn1 Sn 0.63909(2) 0.37536(2) 0.52340(4) 0.01417(7) Uani 1 1 d . . . . .
Se1 Se 0.51402(2) 0.64896(3) 0.68562(6) 0.02061(10) Uani 1 1 d . . . . .
Se2 Se 0.57961(2) 0.46785(3) 0.31422(6) 0.01902(9) Uani 1 1 d . . . . .
Se3 Se 0.61301(2) 0.19641(3) 0.58771(6) 0.01768(9) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.5000 0.50311(10) 0.01760(14) Uani 1 2 d S T P . .
Na1 Na 0.54754(13) 0.8323(2) 0.5159(4) 0.0526(7) Uani 1 1 d . . . . .

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
Sn1 0.01446(11) 0.01195(11) 0.01609(13) -0.00196(9) 0.00110(9) 0.00060(8)
Se1 0.01370(17) 0.02184(19) 0.0263(2) -0.00700(18) -0.00202(16) -0.00026(14)
Se2 0.01860(19) 0.0234(2) 0.01506(19) 0.00434(15) 0.00336(15) 0.00341(15)
Se3 0.0258(2) 0.01302(18) 0.01423(19) -0.00135(14) 0.00246(15) -0.00174(14)
Zn1 0.0144(3) 0.0209(3) 0.0175(3) 0.000 0.000 -0.0003(2)
Na1 0.0744(19) 0.0463(15) 0.0370(14) 0.0134(13) -0.0151(15) -0.0197(14)

_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
Sn1 Se1 2.4960(5) 8_644 ?
Sn1 Se2 2.4969(5) . ?
Sn1 Se3 2.5498(5) . ?
Sn1 Se3 2.5760(5) 4_655 ?
Sn1 Na1 3.753(3) 8_644 ?
Se1 Sn1 2.4960(5) 4_655 ?
Se1 Zn1 2.4695(6) . ?
Se1 Na1 2.913(3) . ?
Se1 Na1 2.944(3) 6_665 ?
Se2 Zn1 2.4674(6) . ?
Se2 Na1 3.020(3) 5_544 ?
Se2 Na1 3.415(3) 8_644 ?
Se3 Sn1 2.5760(5) 8_644 ?
Se3 Na1 3.010(3) 4_645 ?
Zn1 Se1 2.4694(6) 2_665 ?
Zn1 Se2 2.4674(6) 2_665 ?
Na1 Sn1 3.753(3) 4_655 ?
Na1 Se1 2.944(3) 6_664 ?
Na1 Se2 3.415(3) 4_655 ?
Na1 Se2 3.020(3) 5 ?
Na1 Se3 3.010(3) 8_654 ?

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
Se1 Sn1 Se2 109.003(18) 8_644 . ?
Se1 Sn1 Se3 114.382(17) 8_644 . ?
Se1 Sn1 Se3 102.685(17) 8_644 4_655 ?
Se1 Sn1 Na1 50.85(5) 8_644 8_644 ?
Se2 Sn1 Se3 116.716(18) . . ?
Se2 Sn1 Se3 113.108(17) . 4_655 ?
Se2 Sn1 Na1 62.49(5) . 8_644 ?
Se3 Sn1 Se3 99.828(17) . 4_655 ?
Se3 Sn1 Na1 102.38(5) 4_655 8_644 ?
Se3 Sn1 Na1 155.72(5) . 8_644 ?
Sn1 Se1 Na1 105.92(7) 4_655 6_665 ?
Sn1 Se1 Na1 87.52(6) 4_655 . ?
Zn1 Se1 Sn1 100.338(17) . 4_655 ?
Zn1 Se1 Na1 118.53(6) . 6_665 ?
Zn1 Se1 Na1 118.96(6) . . ?
Na1 Se1 Na1 116.77(6) . 6_665 ?
Sn1 Se2 Na1 109.13(6) . 5_544 ?
Sn1 Se2 Na1 77.08(5) . 8_644 ?
Zn1 Se2 Sn1 100.53(2) . . ?
Zn1 Se2 Na1 109.67(7) . 5_544 ?
Zn1 Se2 Na1 133.27(5) . 8_644 ?
Na1 Se2 Na1 115.16(9) 5_544 8_644 ?
Sn1 Se3 Sn1 100.417(18) . 8_644 ?
Sn1 Se3 Na1 112.86(6) . 4_645 ?
Sn1 Se3 Na1 103.97(6) 8_644 4_645 ?
Se1 Zn1 Se1 111.62(4) 2_665 . ?
Se2 Zn1 Se1 111.085(15) 2_665 2_665 ?
Se2 Zn1 Se1 107.121(15) . 2_665 ?
Se2 Zn1 Se1 111.087(15) . . ?
Se2 Zn1 Se1 107.119(15) 2_665 . ?
Se2 Zn1 Se2 108.81(4) . 2_665 ?
Se1 Na1 Sn1 136.29(9) 6_664 4_655 ?
Se1 Na1 Sn1 41.64(4) . 4_655 ?
Se1 Na1 Se1 107.78(9) . 6_664 ?
Se1 Na1 Se2 136.29(11) 6_664 5 ?
Se1 Na1 Se2 125.88(11) 6_664 4_655 ?
Se1 Na1 Se2 79.50(7) . 4_655 ?
Se1 Na1 Se2 104.92(9) . 5 ?
Se1 Na1 Se3 87.02(8) 6_664 8_654 ?
Se1 Na1 Se3 147.39(13) . 8_654 ?
Se2 Na1 Sn1 87.24(7) 5 4_655 ?
Se2 Na1 Sn1 40.42(3) 4_655 4_655 ?
Se2 Na1 Se2 87.87(7) 5 4_655 ?
Se3 Na1 Sn1 108.24(9) 8_654 4_655 ?
Se3 Na1 Se2 68.49(7) 8_654 4_655 ?
Se3 Na1 Se2 80.57(7) 8_654 5 ?

_iucr_refine_instructions_details 
;
    yr_nzsse_1a.res created by SHELXL-2014/7

TITL yr_nzsse_1a_a.res in Fdd2
REM Old TITL yr_nzsse_1a_a.res in Fdd2
REM SHELXT solution in Fdd2
REM R1 0.043, Rweak 0.023, Alpha 0.002, Orientation as input
REM Flack x = 0.043 ( 0.007 ) from Parsons' quotients
REM Formula found by SHELXT: Na2 Sn2 Se7
CELL 0.71073 24.6051 13.5164 7.6031 90 90 90
ZERR 8 0.0007 0.0004 0.0002 0 0 0
LATT -4
SYMM -X,-Y,+Z
SYMM 0.25+X,0.25-Y,0.25+Z
SYMM 0.25-X,0.25+Y,0.25+Z
SFAC Na Se Sn Zn
UNIT 16 48 16 8
 
L.S. 20
PLAN  20
SIZE 0.05 0.045 0.042
TEMP 19.85
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\yr_nzsse_1a.hkl">
REM </olex2.extras>
 
WGHT    0.021400    5.360200
FVAR       0.09428
SN1   3    0.639093    0.375362    0.523397    11.00000    0.01446    0.01195 =
         0.01609   -0.00196    0.00110    0.00060
SE1   2    0.514018    0.648958    0.685624    11.00000    0.01370    0.02184 =
         0.02631   -0.00700   -0.00202   -0.00026
SE2   2    0.579606    0.467852    0.314224    11.00000    0.01860    0.02341 =
         0.01506    0.00434    0.00336    0.00341
SE3   2    0.613014    0.196408    0.587707    11.00000    0.02579    0.01302 =
         0.01423   -0.00135    0.00246   -0.00174
ZN1   4    0.500000    0.500000    0.503115    10.50000    0.01436    0.02093 =
         0.01751    0.00000    0.00000   -0.00031
NA1   1    0.547545    0.832303    0.515929    11.00000    0.07440    0.04626 =
         0.03704    0.01341   -0.01506   -0.01966
HKLF 4
 
REM  yr_nzsse_1a_a.res in Fdd2
REM R1 =  0.0156 for    1930 Fo > 4sig(Fo)  and  0.0161 for all    1960 data
REM     51 parameters refined using      1 restraints
 
END  
     
WGHT      0.0214      5.3600 

REM Highest difference peak  0.683,  deepest hole -0.865,  1-sigma level  0.145
Q1    1   0.6405  0.3742  0.4195  11.00000  0.05    0.68
Q2    1   0.6400  0.3784  0.6265  11.00000  0.05    0.49
Q3    1   0.6108  0.1884  0.6894  11.00000  0.05    0.46
Q4    1   0.5795  0.4722  0.4197  11.00000  0.05    0.44
Q5    1   0.6791  0.3771  0.3904  11.00000  0.05    0.42
Q6    1   0.6782  0.3928  0.5147  11.00000  0.05    0.41
Q7    1   0.6803  0.2686  0.5181  11.00000  0.05    0.41
Q8    1   0.6199  0.1647  0.4625  11.00000  0.05    0.41
Q9    1   0.5913  0.4518  0.5134  11.00000  0.05    0.39
Q10   1   0.6059  0.3881  0.5221  11.00000  0.05    0.38
Q11   1   0.5814  0.4362  0.2010  11.00000  0.05    0.38
Q12   1   0.5465  0.6631  0.6856  11.00000  0.05    0.37
Q13   1   0.6771  0.3585  0.5254  11.00000  0.05    0.37
Q14   1   0.6842  0.3353  0.4346  11.00000  0.05    0.36
Q15   1   0.5236  0.6665  0.7950  11.00000  0.05    0.36
Q16   1   0.6809  0.3609  0.6628  11.00000  0.05    0.34
Q17   1   0.5978  0.3827  0.1771  11.00000  0.05    0.34
Q18   1   0.6881  0.3695  0.6938  11.00000  0.05    0.34
Q19   1   0.4383  0.4968  0.5278  11.00000  0.05    0.34
Q20   1   0.5659  0.6308  0.5248  11.00000  0.05    0.34

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0156 for 1930 Fo > 4sig(Fo) and 0.0161 for all 19639 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.68, deepest hole -0.87
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0161
  REM R1_gt = 0.0156
  REM wR_ref = 0.0358
  REM GOOF = 1.089
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 19639
  REM Reflections_gt = 1930
  REM Parameters = n/a
  REM Hole = -0.87
  REM Peak = 0.68
  REM Flack = 0.012(4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.134
_oxdiff_exptl_absorpt_empirical_full_min 0.614
####################################################################### 
# 
# 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_yr_600_1_53_rt_a
_database_code_depnum_ccdc_archive 'CCDC 1955644'
loop_
_audit_author_name
_audit_author_address
'Run Ye'
;FJIRSM
China
;
_audit_update_record             
;
2019-09-24 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;
_audit_creation_date             2019-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Na2CdSn2Se6
_chemical_name_systematic        Na2CdSn2Se6_FDD2
_chemical_formula_moiety         '0.13(Cd8 Na16 Se48 Sn16)'
_chemical_formula_sum            'Cd Na2 Se6 Sn2'
_chemical_formula_weight         869.52
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   25.1984(14)
_cell_length_b                   13.4933(9)
_cell_length_c                   7.6733(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2609.0(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6995
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7760
_cell_measurement_theta_min      3.8750
_shelx_estimated_absorpt_T_max   0.502
_shelx_estimated_absorpt_T_min   0.375
_exptl_absorpt_coefficient_mu    22.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.036
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8550
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         3.901
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00 -20.00   0.50    6.00    --    5.00  45.00 150.00   52
  2  ω     18.00  78.00   0.50    6.00    --  -11.10  45.00 150.00  120
  3  ω     27.00  52.00   0.50    6.00    --  -11.10  45.00 120.00   50
  4  ω     39.00  77.00   0.50    6.00    --  -11.10  45.00  30.00   76
  5  ω    -98.00 -15.00   0.50    6.00    --  -11.10  45.00 120.00  166
  6  ω    -12.00  15.00   0.50    6.00    --  -11.10  45.00 120.00   54
  7  ω    -99.00  35.00   0.50    6.00    --  -11.10  45.00  30.00  268
  8  ω    -83.00 -55.00   0.50    6.00    --  -11.10  45.00  90.00   56
  9  ω    -24.00   2.00   0.50    6.00    --  -11.10  45.00  90.00   52
 10  ω    -95.00 -52.00   0.50    6.00    --  -11.10  45.00 150.00   86
 11  ω    -88.00  70.00   0.50    6.00    --  -11.10  45.00   0.00  316
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002284000
_diffrn_orient_matrix_UB_12      0.0330315000
_diffrn_orient_matrix_UB_13      0.0717741000
_diffrn_orient_matrix_UB_21      -0.0281123000
_diffrn_orient_matrix_UB_22      0.0017502000
_diffrn_orient_matrix_UB_23      -0.0033755000
_diffrn_orient_matrix_UB_31      -0.0013611000
_diffrn_orient_matrix_UB_32      -0.0409309000
_diffrn_orient_matrix_UB_33      0.0580235000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                1372
_reflns_number_total             1406
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 
;
 Flack x determined using 607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_coef       0.00017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1406
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0229
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0550
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Sn1 Sn 0.64126(2) 0.38390(4) 0.60025(7) 0.01655(18) Uani 1 1 d . . . . .
Cd1 Cd 0.5000 0.5000 0.57816(13) 0.0232(2) Uani 1 2 d S T P . .
Se1 Se 0.58462(3) 0.47121(7) 0.38306(10) 0.0216(2) Uani 1 1 d . . . . .
Se2 Se 0.73641(3) 0.40958(7) 0.52250(13) 0.0238(3) Uani 1 1 d . . . . .
Se3 Se 0.61559(4) 0.20449(6) 0.66034(12) 0.0202(2) Uani 1 1 d . . . . .
Na1 Na 0.69888(19) 0.5844(4) 0.3393(6) 0.0495(12) Uani 1 1 d . . . . .

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
Sn1 0.0152(3) 0.0165(3) 0.0180(3) -0.0018(2) 0.0007(2) 0.0009(2)
Cd1 0.0158(4) 0.0301(5) 0.0237(5) 0.000 0.000 -0.0003(4)
Se1 0.0183(4) 0.0289(5) 0.0177(5) 0.0039(4) 0.0020(3) 0.0024(3)
Se2 0.0142(4) 0.0287(5) 0.0285(6) -0.0054(4) 0.0009(4) 0.0007(3)
Se3 0.0270(4) 0.0170(5) 0.0165(4) -0.0007(3) 0.0018(3) -0.0013(3)
Na1 0.056(3) 0.049(3) 0.043(3) 0.013(2) 0.015(2) 0.011(2)

_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
Sn1 Se1 2.4904(10) . ?
Sn1 Se2 2.4951(10) . ?
Sn1 Se3 2.5479(10) . ?
Sn1 Se3 2.5687(11) 4_655 ?
Sn1 Na1 3.666(5) . ?
Cd1 Se1 2.6341(10) 2_665 ?
Cd1 Se1 2.6341(10) . ?
Cd1 Se2 2.6414(11) 15_455 ?
Cd1 Se2 2.6414(11) 4_655 ?
Se1 Na1 3.276(5) . ?
Se1 Na1 3.034(5) 8_644 ?
Se2 Cd1 2.6414(11) 7_554 ?
Se2 Na1 2.928(5) 10_665 ?
Se2 Na1 2.904(5) . ?
Se3 Sn1 2.5687(11) 8_644 ?
Se3 Na1 2.986(5) 5_545 ?
Na1 Se1 3.034(5) 4_655 ?
Na1 Se2 2.928(5) 10_664 ?
Na1 Se3 2.986(5) 5_554 ?

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
Se1 Sn1 Se2 108.97(4) . . ?
Se1 Sn1 Se3 113.95(3) . 4_655 ?
Se1 Sn1 Se3 115.16(4) . . ?
Se1 Sn1 Na1 60.81(8) . . ?
Se2 Sn1 Se3 114.78(4) . . ?
Se2 Sn1 Se3 103.57(3) . 4_655 ?
Se2 Sn1 Na1 52.14(8) . . ?
Se3 Sn1 Se3 99.65(3) . 4_655 ?
Se3 Sn1 Na1 105.01(9) 4_655 . ?
Se3 Sn1 Na1 154.24(8) . . ?
Se1 Cd1 Se1 110.73(5) 2_665 . ?
Se1 Cd1 Se2 107.79(3) 2_665 4_655 ?
Se1 Cd1 Se2 107.79(3) . 15_455 ?
Se1 Cd1 Se2 109.64(3) . 4_655 ?
Se1 Cd1 Se2 109.64(3) 2_665 15_455 ?
Se2 Cd1 Se2 111.26(6) 4_655 15_455 ?
Sn1 Se1 Cd1 98.82(4) . . ?
Sn1 Se1 Na1 111.65(9) . 8_644 ?
Sn1 Se1 Na1 77.62(9) . . ?
Cd1 Se1 Na1 106.67(10) . 8_644 ?
Cd1 Se1 Na1 134.50(9) . . ?
Na1 Se1 Na1 116.87(15) 8_644 . ?
Sn1 Se2 Cd1 98.42(3) . 7_554 ?
Sn1 Se2 Na1 85.16(10) . . ?
Sn1 Se2 Na1 109.91(11) . 10_665 ?
Cd1 Se2 Na1 115.53(11) 7_554 . ?
Cd1 Se2 Na1 114.78(10) 7_554 10_665 ?
Na1 Se2 Na1 124.10(9) . 10_665 ?
Sn1 Se3 Sn1 101.64(4) . 8_644 ?
Sn1 Se3 Na1 114.86(11) . 5_545 ?
Sn1 Se3 Na1 105.78(10) 8_644 5_545 ?
Se1 Na1 Sn1 41.57(6) . . ?
Se1 Na1 Sn1 86.15(11) 4_655 . ?
Se1 Na1 Se1 87.87(12) 4_655 . ?
Se2 Na1 Sn1 42.70(7) . . ?
Se2 Na1 Sn1 134.00(16) 10_664 . ?
Se2 Na1 Se1 139.02(18) 10_664 4_655 ?
Se2 Na1 Se1 81.83(12) . . ?
Se2 Na1 Se1 125.98(18) 10_664 . ?
Se2 Na1 Se1 103.01(15) . 4_655 ?
Se2 Na1 Se2 104.07(14) . 10_664 ?
Se2 Na1 Se3 153.15(19) . 5_554 ?
Se2 Na1 Se3 89.69(13) 10_664 5_554 ?
Se3 Na1 Sn1 111.92(14) 5_554 . ?
Se3 Na1 Se1 71.48(11) 5_554 . ?
Se3 Na1 Se1 79.39(11) 5_554 4_655 ?

_iucr_refine_instructions_details 
;
    yr_600_1_53_rt_a.res created by SHELXL-2014/7

TITL yr_600_1_53_rt_a_a.res in Fdd2
REM Old TITL yr_600_1_53_rt_a in Fdd2
REM SHELXT solution in Fdd2
REM R1 0.048, Rweak 0.022, Alpha 0.001, Orientation as input
REM Flack x = -0.001 ( 0.013 ) from Parsons' quotients
REM Formula found by SHELXT: Na2 Sn3 Se6
CELL 0.71073 25.1984 13.4933 7.6733 90 90 90
ZERR 8 0.0014 0.0009 0.0005 0 0 0
LATT -4
SYMM -X,-Y,+Z
SYMM 0.25+X,0.25-Y,0.25+Z
SYMM 0.25-X,0.25+Y,0.25+Z
SFAC Cd Na Se Sn
UNIT 8 16 48 16
 
L.S. 20 0 0
PLAN  20
SIZE 0.055 0.052 0.036
TEMP 19.85
list 4
fmap 2 53
acta
OMIT -2 54
REM <olex2.extras>
REM <HklSrc "%.\\yr_600_1_53_rt_a.hkl">
REM </olex2.extras>
 
WGHT    0.030600
EXTI    0.000169
FVAR       0.08225
SN1   4    0.641257    0.383904    0.600252    11.00000    0.01517    0.01651 =
         0.01796   -0.00182    0.00068    0.00093
CD1   1    0.500000    0.500000    0.578159    10.50000    0.01578    0.03013 =
         0.02370    0.00000    0.00000   -0.00031
SE1   3    0.584620    0.471212    0.383060    11.00000    0.01829    0.02891 =
         0.01772    0.00391    0.00202    0.00239
SE2   3    0.736414    0.409577    0.522497    11.00000    0.01420    0.02866 =
         0.02854   -0.00535    0.00089    0.00074
SE3   3    0.615587    0.204488    0.660338    11.00000    0.02703    0.01704 =
         0.01647   -0.00068    0.00182   -0.00127
NA1   2    0.698883    0.584392    0.339256    11.00000    0.05628    0.04888 =
         0.04321    0.01300    0.01506    0.01096
HKLF 4
 
REM  yr_600_1_53_rt_a_a.res in Fdd2
REM R1 =  0.0229 for    1372 Fo > 4sig(Fo)  and  0.0236 for all    1406 data
REM     52 parameters refined using      1 restraints
 
END  
     
WGHT      0.0306      0.0000 

REM Highest difference peak  0.800,  deepest hole -0.654,  1-sigma level  0.165
Q1    1   0.7468  0.3338  0.4248  11.00000  0.05    0.80
Q2    1   0.6112  0.2917  0.7359  11.00000  0.05    0.79
Q3    1   0.6413  0.3129  0.6045  11.00000  0.05    0.72
Q4    1   0.6394  0.3028  0.6549  11.00000  0.05    0.67
Q5    1   0.6413  0.4571  0.5907  11.00000  0.05    0.66
Q6    1   0.6397  0.2997  0.5481  11.00000  0.05    0.65
Q7    1   0.6232  0.4363  0.5684  11.00000  0.05    0.63
Q8    1   0.5006  0.5763  0.5636  11.00000  0.05    0.61
Q9    1   0.7425  0.4797  0.5180  11.00000  0.05    0.59
Q10   1   0.5912  0.5429  0.3913  11.00000  0.05    0.56
Q11   1   0.6076  0.3739  0.2646  11.00000  0.05    0.55
Q12   1   0.5977  0.3798  0.2751  11.00000  0.05    0.54
Q13   1   0.7374  0.3350  0.5451  11.00000  0.05    0.53
Q14   1   0.4999  0.5777  0.4655  11.00000  0.05    0.53
Q15   1   0.7496  0.3339  0.5864  11.00000  0.05    0.49
Q16   1   0.5988  0.5444  0.2864  11.00000  0.05    0.48
Q17   1   0.6264  0.1325  0.6936  11.00000  0.05    0.46
Q18   1   0.5000  0.5000  0.4735  10.50000  0.05    0.46
Q19   1   0.6173  0.3637  0.4743  11.00000  0.05    0.45
Q20   1   0.6105  0.5507  0.2573  11.00000  0.05    0.45

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0229 for 1372 Fo > 4sig(Fo) and 0.0236 for all 9110 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.80, deepest hole -0.65
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0236
  REM R1_gt = 0.0229
  REM wR_ref = 0.0550
  REM GOOF = 1.100
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 9110
  REM Reflections_gt = 1372
  REM Parameters = n/a
  REM Hole = -0.65
  REM Peak = 0.80
  REM Flack = 0.003(10)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.257
_oxdiff_exptl_absorpt_empirical_full_min 0.599
