 
data_theta25
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'As4 Hg I2 S4'
_chemical_formula_weight          882.31
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'As'  'As'   0.0499   2.0058
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Hg'  'Hg'  -2.3894   9.2266
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    9.5000(10)
_cell_length_b                    15.024(2)
_cell_length_c                    9.5180(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.61(2)
_cell_angle_gamma                 90.00
_cell_volume                      1320.3(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     4.439
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1528
_exptl_absorpt_coefficient_mu     26.862
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_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   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4830
_diffrn_reflns_av_R_equivalents   0.1050
_diffrn_reflns_av_sigmaI/netI     0.1172
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -5
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          2.59
_diffrn_reflns_theta_max          25.00
_reflns_number_total              2320
_reflns_number_gt                 1270
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0534P)^2^+55.4123P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00042(15)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          2320
_refine_ls_number_parameters      120
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1537
_refine_ls_R_factor_gt            0.0821
_refine_ls_wR_factor_ref          0.1981
_refine_ls_wR_factor_gt           0.1715
_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
Hg Hg 0.5079(2) 0.05157(9) 0.7057(2) 0.0816(6) Uani 1 1 d . . .
I1 I 0.4647(3) 0.11735(14) 0.3426(2) 0.0637(7) Uani 1 1 d . . .
I2 I 0.5557(3) 0.21466(15) 0.7925(3) 0.0772(8) Uani 1 1 d . . .
As1 As 0.8630(5) 0.0417(2) 0.2584(4) 0.0781(13) Uani 1 1 d . . .
As2 As 0.9040(5) 0.0450(4) 0.7730(6) 0.048(2) Uani 0.674(16) 1 d P . .
As2B As 0.9295(13) 0.1022(10) 0.8578(16) 0.072(7) Uani 0.326(16) 1 d P . .
As3 As 0.1411(5) 0.1885(2) 0.6638(4) 0.0702(11) Uani 1 1 d . . .
As4 As 0.2087(4) 0.1576(2) 0.9345(4) 0.0644(10) Uani 1 1 d . . .
S1 S 0.7054(9) -0.0183(5) 0.0671(9) 0.056(2) Uani 1 1 d . . .
S2 S -0.0009(16) 0.1264(7) -0.0301(15) 0.052(4) Uani 0.674(16) 1 d P . .
S2B S 0.042(3) 0.035(2) 0.201(3) 0.067(9) Uani 0.326(16) 1 d P . .
S3 S 0.9045(11) 0.1621(6) 0.6268(11) 0.077(3) Uani 1 1 d . . .
S4 S 0.1880(11) 0.0531(6) 0.5795(9) 0.066(2) 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
Hg 0.0852(12) 0.0611(9) 0.1015(13) -0.0230(8) 0.0279(9) -0.0057(8)
I1 0.0753(17) 0.0544(12) 0.0628(15) 0.0007(11) 0.0188(12) -0.0007(11)
I2 0.093(2) 0.0579(13) 0.0814(18) -0.0204(12) 0.0210(15) -0.0078(12)
As1 0.117(3) 0.063(2) 0.068(3) -0.0232(18) 0.048(2) -0.041(2)
As2 0.048(3) 0.050(4) 0.045(3) -0.008(3) 0.008(2) -0.006(2)
As2B 0.048(8) 0.091(11) 0.074(14) 0.017(11) 0.008(8) 0.019(7)
As3 0.088(3) 0.063(2) 0.058(2) 0.0163(17) 0.012(2) -0.0052(19)
As4 0.090(3) 0.0493(18) 0.053(2) -0.0066(16) 0.016(2) -0.0099(18)
S1 0.056(5) 0.064(5) 0.045(5) 0.014(4) 0.011(4) 0.009(4)
S2 0.065(9) 0.052(6) 0.039(8) -0.004(5) 0.013(7) 0.002(6)
S2B 0.053(18) 0.10(2) 0.041(16) 0.000(14) -0.007(13) -0.010(16)
S3 0.078(7) 0.072(6) 0.074(6) 0.015(5) 0.004(5) 0.009(5)
S4 0.074(6) 0.085(6) 0.038(5) -0.004(4) 0.013(4) -0.015(5)
 
_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
Hg I2 2.592(3) . ?
Hg I1 2.603(3) 3_656 ?
Hg S4 2.994(10) . ?
I1 Hg 2.603(3) 3_656 ?
As1 S2B 1.91(3) 1_655 ?
As1 S4 2.235(9) 3_656 ?
As1 S1 2.255(9) . ?
As1 As2 2.646(7) 3_756 ?
As2 As2B 1.165(16) . ?
As2 S2B 1.31(3) 3_656 ?
As2 S2 2.242(16) 1_656 ?
As2 S3 2.243(10) . ?
As2 As1 2.646(7) 3_756 ?
As2B S2 1.173(19) 1_656 ?
As2B S2B 2.17(3) 3_656 ?
As2B S3 2.335(17) . ?
As2B As4 2.711(14) 1_655 ?
As3 S3 2.228(11) 1_455 ?
As3 S4 2.269(10) . ?
As3 As4 2.547(5) . ?
As4 S2 2.148(14) 1_556 ?
As4 S1 2.248(9) 3_656 ?
As4 As2B 2.711(14) 1_455 ?
S1 As4 2.248(9) 3_656 ?
S2 As2B 1.173(19) 1_454 ?
S2 As4 2.148(14) 1_554 ?
S2 As2 2.242(16) 1_454 ?
S2 S2B 2.54(3) . ?
S2B As2 1.31(3) 3_656 ?
S2B As1 1.91(3) 1_455 ?
S2B As2B 2.17(3) 3_656 ?
S3 As3 2.228(11) 1_655 ?
S4 As1 2.235(9) 3_656 ?
 
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
I2 Hg I1 163.92(11) . 3_656 ?
I2 Hg S4 101.87(19) . . ?
I1 Hg S4 94.06(19) 3_656 . ?
S2B As1 S4 121.2(10) 1_655 3_656 ?
S2B As1 S1 102.3(8) 1_655 . ?
S4 As1 S1 95.3(3) 3_656 . ?
S2B As1 As2 27.8(10) 1_655 3_756 ?
S4 As1 As2 95.0(3) 3_656 3_756 ?
S1 As1 As2 97.3(3) . 3_756 ?
As2B As2 S2B 122.4(13) . 3_656 ?
As2B As2 S2 16.5(6) . 1_656 ?
S2B As2 S2 106.1(12) 3_656 1_656 ?
As2B As2 S3 79.7(7) . . ?
S2B As2 S3 141.5(13) 3_656 . ?
S2 As2 S3 91.8(4) 1_656 . ?
As2B As2 As1 113.4(6) . 3_756 ?
S2B As2 As1 43.0(13) 3_656 3_756 ?
S2 As2 As1 100.3(4) 1_656 3_756 ?
S3 As2 As1 101.1(3) . 3_756 ?
As2 As2B S2 147.2(12) . 1_656 ?
As2 As2B S2B 30.6(8) . 3_656 ?
S2 As2B S2B 116.8(11) 1_656 3_656 ?
As2 As2B S3 70.9(7) . . ?
S2 As2B S3 130.4(11) 1_656 . ?
S2B As2B S3 96.7(10) 3_656 . ?
As2 As2B As4 116.4(8) . 1_655 ?
S2 As2B As4 49.7(8) 1_656 1_655 ?
S2B As2B As4 100.9(9) 3_656 1_655 ?
S3 As2B As4 90.7(5) . 1_655 ?
S3 As3 S4 93.4(4) 1_455 . ?
S3 As3 As4 97.6(3) 1_455 . ?
S4 As3 As4 99.8(3) . . ?
S2 As4 S1 98.6(4) 1_556 3_656 ?
S2 As4 As3 100.1(4) 1_556 . ?
S1 As4 As3 99.7(3) 3_656 . ?
S2 As4 As2B 24.6(4) 1_556 1_455 ?
S1 As4 As2B 92.6(4) 3_656 1_455 ?
As3 As4 As2B 77.6(3) . 1_455 ?
As4 S1 As1 101.8(4) 3_656 . ?
As2B S2 As4 105.7(10) 1_454 1_554 ?
As2B S2 As2 16.3(7) 1_454 1_454 ?
As4 S2 As2 101.2(5) 1_554 1_454 ?
As2B S2 S2B 124.1(12) 1_454 . ?
As4 S2 S2B 106.6(9) 1_554 . ?
As2 S2 S2B 112.3(8) 1_454 . ?
As2 S2B As1 109.1(18) 3_656 1_455 ?
As2 S2B As2B 27.0(8) 3_656 3_656 ?
As1 S2B As2B 107.2(14) 1_455 3_656 ?
As2 S2B S2 129.8(17) 3_656 . ?
As1 S2B S2 104.3(12) 1_455 . ?
As2B S2B S2 107.3(11) 3_656 . ?
As3 S3 As2 101.0(4) 1_655 . ?
As3 S3 As2B 92.5(5) 1_655 . ?
As2 S3 As2B 29.4(4) . . ?
As1 S4 As3 103.6(4) 3_656 . ?
As1 S4 Hg 94.7(3) 3_656 . ?
As3 S4 Hg 97.5(3) . . ?
 
_diffrn_measured_fraction_theta_max    1.000
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   1.000
_refine_diff_density_max    1.916
_refine_diff_density_min   -1.288
_refine_diff_density_rms    0.294
