# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_WSe2_4
_database_code_depnum_ccdc_archive 'CCDC 1899867'
loop_
_audit_author_name
_audit_author_address
'Dong Wang'
;Shanghai Institute of Ceramics
China
;
_audit_update_record             
;
2019-02-27 deposited with the CCDC.	2019-07-02 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Se8 W4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1367.08

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.838(3)
_cell_length_b                   3.2911(7)
_cell_length_c                   5.9117(13)
_cell_angle_alpha                90
_cell_angle_beta                 111.468(6)
_cell_angle_gamma                90
_cell_volume                     250.55(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1148
_cell_measurement_theta_min      3.1638
_cell_measurement_theta_max      30.0713
_cell_measurement_temperature    273.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    9.061
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             568

_exptl_absorpt_coefficient_mu    74.748
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_T_max  0.106

_exptl_special_details           
;
;

_diffrn_ambient_temperature      273.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 10.4167

_diffrn_reflns_number            1270
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7

_refine_special_details          
;
;

_reflns_number_total             252
_reflns_number_gt                237
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0946
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_restrained_S_all      0.850
_refine_ls_number_reflns         252
_refine_ls_number_parameters     19
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.139
_refine_diff_density_min         -1.090
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 786)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W001 0.25685(5) 0.5 0.19725(10) 0.0296(4) Uani d T P S 1 . .
Se Se02 0.14190(13) 0 0.3296(3) 0.0305(6) Uani d T P S 1 . .
Se Se03 0.39518(13) 0 0.2055(3) 0.0317(5) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W001 0.0379(6) 0.0319(6) 0.0204(6) 0 0.0124(4) 0
Se02 0.0359(10) 0.0342(10) 0.0227(10) 0 0.0124(7) 0
Se03 0.0386(10) 0.0335(11) 0.0245(10) 0 0.0134(7) 0

_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W001 Se03 . 2.5112(13) ?
W001 Se03 1_565 2.5112(13) ?
W001 Se03 7 2.5353(18) ?
W001 Se02 . 2.6003(13) ?
W001 Se02 1_565 2.6003(13) ?
W001 Se02 7_556 2.6301(17) ?
W001 W001 7 2.8034(10) ?
W001 W001 7_565 2.8034(10) ?
Se02 W001 1_545 2.6002(13) ?
Se02 W001 7_556 2.6301(17) ?
Se03 W001 1_545 2.5113(13) ?
Se03 W001 7 2.5353(18) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se03 W001 Se03 . 1_565 81.88(5) ?
Se03 W001 Se03 . 7 112.51(5) ?
Se03 W001 Se03 1_565 7 112.51(5) ?
Se03 W001 Se02 . . 97.20(4) ?
Se03 W001 Se02 1_565 . 162.70(7) ?
Se03 W001 Se02 7 . 83.91(6) ?
Se03 W001 Se02 . 1_565 162.70(7) ?
Se03 W001 Se02 1_565 1_565 97.20(4) ?
Se03 W001 Se02 7 1_565 83.91(6) ?
Se02 W001 Se02 . 1_565 78.52(5) ?
Se03 W001 Se02 . 7_556 82.75(6) ?
Se03 W001 Se02 1_565 7_556 82.75(6) ?
Se03 W001 Se02 7 7_556 159.17(6) ?
Se02 W001 Se02 . 7_556 80.00(5) ?
Se02 W001 Se02 1_565 7_556 80.00(5) ?
Se03 W001 W001 . 7 56.66(4) ?
Se03 W001 W001 1_565 7 102.69(4) ?
Se03 W001 W001 7 7 55.85(3) ?
Se02 W001 W001 . 7 90.94(4) ?
Se02 W001 W001 1_565 7 139.40(6) ?
Se02 W001 W001 7_556 7 137.07(3) ?
Se03 W001 W001 . 7_565 102.69(4) ?
Se03 W001 W001 1_565 7_565 56.66(4) ?
Se03 W001 W001 7 7_565 55.85(3) ?
Se02 W001 W001 . 7_565 139.40(6) ?
Se02 W001 W001 1_565 7_565 90.94(4) ?
Se02 W001 W001 7_556 7_565 137.07(3) ?
W001 W001 W001 7 7_565 71.89(3) ?
W001 Se02 W001 1_545 . 78.52(5) ?
W001 Se02 W001 1_545 7_556 100.00(5) ?
W001 Se02 W001 . 7_556 100.00(5) ?
W001 Se03 W001 . 1_545 81.88(5) ?
W001 Se03 W001 . 7 67.49(5) ?
W001 Se03 W001 1_545 7 67.49(5) ?

_shelx_res_file                  
;


    C2-8_a.res created by SHELXL-2014/7


TITL C2-8_a.res in C2/m
REM Old TITL C2-8 in C2

REM SHELXT solution in C2/m
REM R1 0.087,  Rweak 0.007,  Alpha 0.011,  Orientation as input
REM Formula found by SHELXT:  Se2 W

CELL  0.71073  13.8377   3.2911   5.9117   90.000  111.468   90.000
ZERR    1.000   0.0030   0.0007   0.0013    0.000    0.006    0.000
LATT  7
SYMM -X, Y, -Z
SFAC SE W
UNIT 8 4
TEMP 0
L.S. 10
BOND
OMIT -2 50.0
LIST 4
OMIT -16 0 2
OMIT 0 0 2
OMIT -14 0 4
OMIT 2 0 2
OMIT 5 1 1
OMIT -2 0 3
omit -4 0 3
omit -1 1 2
omit -3 1 1
FMAP 2
PLAN 20
ACTA
WGHT    0.100000
FVAR       0.23504
W001  2    0.256845    0.500000    0.197245    10.50000    0.03786    0.03188 =
         0.02045    0.00000    0.01238    0.00000
SE02  1    0.141903    0.000000    0.329632    10.50000    0.03589    0.03420 =
         0.02273    0.00000    0.01244    0.00000
SE03  1    0.395181    0.000000    0.205482    10.50000    0.03859    0.03348 =
         0.02454    0.00000    0.01338    0.00000
HKLF 4

REM  C2-8_a.res in C2/m
REM R1 =  0.0296 for     237 Fo > 4sig(Fo)  and  0.0319 for all     252 data
REM     19 parameters refined using      0 restraints

END

WGHT      0.0543      1.7529

REM Highest difference peak  2.139,  deepest hole -1.090,  1-sigma level  0.358
Q1    1   0.1887  0.5000  0.1406  10.50000  0.05    2.14
Q2    1   0.3232  0.5000  0.2742  10.50000  0.05    1.73
Q3    1   0.2703  0.3089  0.1054  11.00000  0.05    1.27
Q4    1   0.0412  0.0000  0.4910  10.50000  0.05    1.02
Q5    1   0.3395  0.0000  0.1763  10.50000  0.05    1.01
Q6    1   0.3224  0.0000  0.0618  10.50000  0.05    0.92
Q7    1   0.2366  0.5000  0.4556  10.50000  0.05    0.90
Q8    1   0.4499  0.0000  0.2193  10.50000  0.05    0.89
Q9    1   0.0814  0.0000  0.2440  10.50000  0.05    0.88
Q10   1   0.2099  0.0000  0.3510  10.50000  0.05    0.87
Q11   1   0.2523  0.5000 -0.0392  10.50000  0.05    0.85
Q12   1   0.3918  0.0000  0.0121  10.50000  0.05    0.81
Q13   1   0.4071  0.0000  0.5055  10.50000  0.05    0.74
Q14   1   0.0924 -0.5000  0.1615  10.50000  0.05    0.55
Q15   1   0.3925  0.2044  0.3973  11.00000  0.05    0.52
Q16   1   0.0309  0.3424  0.1339  11.00000  0.05    0.50
Q17   1   0.0000  0.0000  0.0000  10.25000  0.05    0.48
Q18   1   0.3704  0.3272  0.0735  11.00000  0.05    0.45
Q19   1   0.0723  0.0000  0.0345  10.50000  0.05    0.45
Q20   1   0.1179  0.3517  0.3235  11.00000  0.05    0.43
;
_shelx_res_checksum              42845
