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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_final

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ag3 Ga3 Se8 Si'
_chemical_formula_weight         1192.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I-42d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   5.9041(8)
_cell_length_b                   5.9041(8)
_cell_length_c                   10.499(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     365.99(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.1300
_exptl_crystal_size_mid          0.1300
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    5.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    29.310
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4718
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Rigaku AFC10 diffractometer'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2131
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.96
_diffrn_reflns_theta_max         32.57
_reflns_number_total             334
_reflns_number_gt                293
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  Diamond

_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)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       none
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_number_reflns         334
_refine_ls_number_parameters     10
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0558
_refine_ls_wR_factor_gt          0.0547
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_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
Ag Ag 0.0000 0.0000 0.0000 0.0236(3) Uani 0.75 4 d SP . .
Ga Ga 0.0000 0.0000 0.5000 0.0105(3) Uani 0.75 4 d SP . .
Si Si 0.0000 0.0000 0.5000 0.0105(3) Uani 0.25 4 d SP . .
Se Se 0.27802(10) 0.2500 0.1250 0.0211(2) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag 0.0216(3) 0.0216(3) 0.0276(6) 0.000 0.000 0.000
Ga 0.0089(3) 0.0089(3) 0.0136(6) 0.000 0.000 0.000
Si 0.0089(3) 0.0089(3) 0.0136(6) 0.000 0.000 0.000
Se 0.0091(2) 0.0179(3) 0.0364(5) 0.0135(3) 0.000 0.000

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag Se 2.5682(5) . ?
Ag Se 2.5682(5) 2 ?
Ag Se 2.5682(5) 3 ?
Ag Se 2.5682(5) 4 ?
Ga Se 2.3704(4) 10 ?
Ga Se 2.3704(4) 11_455 ?
Ga Se 2.3704(4) 9_445 ?
Ga Se 2.3704(4) 12_545 ?
Se Si 2.3704(4) 9_554 ?
Se Ga 2.3704(4) 9_554 ?
Se Si 2.3704(4) 5 ?
Se Ga 2.3704(4) 5 ?
Se Ag 2.5682(5) 13_454 ?

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
Se Ag Se 118.535(16) . 2 ?
Se Ag Se 105.139(7) . 3 ?
Se Ag Se 105.139(7) 2 3 ?
Se Ag Se 105.139(7) . 4 ?
Se Ag Se 105.139(7) 2 4 ?
Se Ag Se 118.535(16) 3 4 ?
Se Ga Se 107.851(8) 10 11_455 ?
Se Ga Se 112.762(17) 10 9_445 ?
Se Ga Se 107.851(8) 11_455 9_445 ?
Se Ga Se 107.851(8) 10 12_545 ?
Se Ga Se 112.762(17) 11_455 12_545 ?
Se Ga Se 107.851(8) 9_445 12_545 ?
Si Se Ga 0.0 9_554 9_554 ?
Si Se Si 112.87(2) 9_554 5 ?
Ga Se Si 112.87(2) 9_554 5 ?
Si Se Ga 112.87(2) 9_554 5 ?
Ga Se Ga 112.87(2) 9_554 5 ?
Si Se Ga 0.0 5 5 ?
Si Se Ag 115.362(13) 9_554 . ?
Ga Se Ag 115.362(13) 9_554 . ?
Si Se Ag 106.168(6) 5 . ?
Ga Se Ag 106.168(6) 5 . ?
Si Se Ag 106.168(6) 9_554 13_454 ?
Ga Se Ag 106.168(6) 9_554 13_454 ?
Si Se Ag 115.362(13) 5 13_454 ?
Ga Se Ag 115.362(13) 5 13_454 ?
Ag Se Ag 100.54(2) . 13_454 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        32.57
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.186
_database_code_depnum_ccdc_archive 'CCDC 890411'
