 
data_new-gonf3_3060
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'As3.20 Hg0.80 I1.60 S3.20'
_chemical_formula_weight          705.85
 
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                    9.532(2)
_cell_length_b                    15.094(2)
_cell_length_c                    9.5580(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.18(2)
_cell_angle_gamma                 90.00
_cell_volume                      1338.9(4)
_cell_formula_units_Z             5
_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     4.377
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1528
_exptl_absorpt_coefficient_mu     26.489
_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             7408
_diffrn_reflns_av_R_equivalents   0.0842
_diffrn_reflns_av_sigmaI/netI     0.1971
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          4.37
_diffrn_reflns_theta_max          32.22
_reflns_number_total              3711
_reflns_number_gt                 1229
_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^)+(0.1112P)^2^+0.0000P] 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        0.0007(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3711
_refine_ls_number_parameters      129
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2387
_refine_ls_R_factor_gt            0.0806
_refine_ls_wR_factor_ref          0.2432
_refine_ls_wR_factor_gt           0.2071
_refine_ls_goodness_of_fit_ref    0.888
_refine_ls_restrained_S_all       0.888
_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 0.50407(15) 0.05577(8) 0.69531(14) 0.0906(6) Uani 1 1 d . . .
I1 I 0.4584(2) 0.11369(12) 0.33923(17) 0.0705(6) Uani 1 1 d . . .
I2 I 0.5506(2) 0.21807(13) 0.7852(2) 0.0837(7) Uani 1 1 d . . .
As1 As 0.8725(15) 0.0363(7) 0.2662(13) 0.051(3) Uani 0.409(11) 1 d P . .
As1B As 0.8156(10) 0.0576(6) 0.2315(10) 0.060(2) Uani 0.591(11) 1 d P . .
As2 As 0.9029(8) 0.0452(5) 0.7738(8) 0.068(3) Uani 0.409(11) 1 d P . .
As2B As 0.9272(5) 0.1024(4) 0.8580(5) 0.068(2) Uani 0.591(11) 1 d P . .
As3 As 0.1418(3) 0.1852(2) 0.6598(3) 0.0794(10) Uani 1 1 d . . .
As4 As 0.1952(3) 0.15795(19) 0.9264(3) 0.0735(9) Uani 1 1 d . . .
S1 S 0.7020(7) -0.0262(5) 0.0619(6) 0.0675(18) Uani 1 1 d . . .
S2 S -0.007(2) 0.1243(11) -0.0322(18) 0.069(5) Uani 0.409(11) 1 d P . .
S2B S 0.0407(12) 0.0392(9) 0.1956(10) 0.070(4) Uani 0.591(11) 1 d P . .
S3 S 0.9016(8) 0.1658(6) 0.6329(8) 0.089(2) Uani 1 1 d . . .
S4 S 0.1883(8) 0.0476(5) 0.5836(6) 0.072(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 0.1035(11) 0.0634(8) 0.1085(10) -0.0268(7) 0.0319(7) -0.0117(7)
I1 0.0920(14) 0.0580(12) 0.0614(10) 0.0014(8) 0.0173(8) 0.0020(9)
I2 0.0982(15) 0.0603(12) 0.0943(14) -0.0254(10) 0.0251(11) -0.0139(11)
As1 0.072(9) 0.033(5) 0.053(6) -0.003(3) 0.029(5) -0.007(5)
As1B 0.060(6) 0.058(5) 0.059(4) -0.005(3) 0.008(3) -0.007(3)
As2 0.083(6) 0.062(6) 0.061(4) -0.006(4) 0.024(3) -0.013(4)
As2B 0.059(3) 0.079(4) 0.061(4) 0.004(3) 0.004(2) 0.010(3)
As3 0.087(2) 0.083(2) 0.0604(16) 0.0231(15) -0.0001(14) -0.0113(17)
As4 0.096(2) 0.0672(19) 0.0548(14) -0.0082(13) 0.0124(13) -0.0027(16)
S1 0.073(5) 0.074(5) 0.050(3) 0.010(3) 0.002(3) 0.006(4)
S2 0.096(14) 0.060(11) 0.058(11) -0.014(8) 0.029(10) -0.027(9)
S2B 0.058(8) 0.099(12) 0.048(6) -0.015(6) 0.004(5) -0.007(7)
S3 0.080(5) 0.105(7) 0.071(4) 0.019(4) -0.003(4) 0.010(5)
S4 0.083(5) 0.100(6) 0.034(3) -0.011(3) 0.013(3) -0.017(4)
 
_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 2.600(2) . ?
Hg I1 2.614(2) 3_656 ?
Hg S4 2.958(7) . ?
I1 Hg 2.614(2) 3_656 ?
As1 As1B 0.652(10) . ?
As1 S2B 1.877(18) 1_655 ?
As1 S4 2.093(13) 3_656 ?
As1 S1 2.429(14) . ?
As1 As2 2.573(15) 3_756 ?
As1B S1 2.145(11) . ?
As1B S2B 2.266(15) 1_655 ?
As1B S4 2.382(12) 3_656 ?
As2 As2B 1.166(8) . ?
As2 S2B 1.389(14) 3_656 ?
As2 S2 2.21(2) 1_656 ?
As2 S3 2.262(10) . ?
As2 As1 2.573(15) 3_756 ?
As2B S2 1.143(18) 1_656 ?
As2B S2B 2.235(15) 3_656 ?
As2B S3 2.316(9) . ?
As2B As4 2.626(6) 1_655 ?
As3 S3 2.264(8) 1_455 ?
As3 S4 2.278(8) . ?
As3 As4 2.516(4) . ?
As4 S2 2.114(17) 1_556 ?
As4 S1 2.208(8) 3_656 ?
As4 As2B 2.626(6) 1_455 ?
S1 As4 2.208(8) 3_656 ?
S2 As2B 1.143(17) 1_454 ?
S2 As4 2.114(17) 1_554 ?
S2 As2 2.21(2) 1_454 ?
S2 S2B 2.48(2) . ?
S2B As2 1.389(14) 3_656 ?
S2B As1 1.877(18) 1_455 ?
S2B As2B 2.235(15) 3_656 ?
S2B As1B 2.266(15) 1_455 ?
S3 As3 2.264(8) 1_655 ?
S4 As1 2.093(13) 3_656 ?
S4 As1B 2.382(12) 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 161.00(9) . 3_656 ?
I2 Hg S4 103.97(16) . . ?
I1 Hg S4 94.07(16) 3_656 . ?
As1B As1 S2B 119(2) . 1_655 ?
As1B As1 S4 109(2) . 3_656 ?
S2B As1 S4 130.8(8) 1_655 3_656 ?
As1B As1 S1 57.0(16) . . ?
S2B As1 S1 100.9(6) 1_655 . ?
S4 As1 S1 94.4(5) 3_656 . ?
As1B As1 As2 142(2) . 3_756 ?
S2B As1 As2 31.7(5) 1_655 3_756 ?
S4 As1 As2 100.5(5) 3_656 3_756 ?
S1 As1 As2 97.0(5) . 3_756 ?
As1 As1B S1 108.2(19) . . ?
As1 As1B S2B 46.4(18) . 1_655 ?
S1 As1B S2B 98.4(5) . 1_655 ?
As1 As1B S4 56.4(18) . 3_656 ?
S1 As1B S4 94.4(4) . 3_656 ?
S2B As1B S4 101.9(5) 1_655 3_656 ?
As2B As2 S2B 121.8(8) . 3_656 ?
As2B As2 S2 16.8(5) . 1_656 ?
S2B As2 S2 105.2(8) 3_656 1_656 ?
As2B As2 S3 77.8(5) . . ?
S2B As2 S3 144.4(7) 3_656 . ?
S2 As2 S3 90.7(5) 1_656 . ?
As2B As2 As1 114.5(6) . 3_756 ?
S2B As2 As1 45.3(6) 3_656 3_756 ?
S2 As2 As1 101.8(6) 1_656 3_756 ?
S3 As2 As1 100.8(4) . 3_756 ?
S2 As2B As2 146.0(11) 1_656 . ?
S2 As2B S2B 114.3(10) 1_656 3_656 ?
As2 As2B S2B 31.9(5) . 3_656 ?
S2 As2B S3 130.7(9) 1_656 . ?
As2 As2B S3 72.7(5) . . ?
S2B As2B S3 100.0(4) 3_656 . ?
S2 As2B As4 51.5(8) 1_656 1_655 ?
As2 As2B As4 115.9(5) . 1_655 ?
S2B As2B As4 100.7(3) 3_656 1_655 ?
S3 As2B As4 89.4(3) . 1_655 ?
S3 As3 S4 96.4(3) 1_455 . ?
S3 As3 As4 93.4(2) 1_455 . ?
S4 As3 As4 99.51(19) . . ?
S2 As4 S1 100.8(5) 1_556 3_656 ?
S2 As4 As3 104.3(5) 1_556 . ?
S1 As4 As3 100.58(19) 3_656 . ?
S2 As4 As2B 25.1(5) 1_556 1_455 ?
S1 As4 As2B 96.9(2) 3_656 1_455 ?
As3 As4 As2B 80.75(15) . 1_455 ?
As1B S1 As4 110.6(4) . 3_656 ?
As1B S1 As1 14.8(3) . . ?
As4 S1 As1 95.8(4) 3_656 . ?
As2B S2 As4 103.4(10) 1_454 1_554 ?
As2B S2 As2 17.2(6) 1_454 1_454 ?
As4 S2 As2 99.8(7) 1_554 1_454 ?
As2B S2 S2B 127.5(11) 1_454 . ?
As4 S2 S2B 107.3(9) 1_554 . ?
As2 S2 S2B 114.5(7) 1_454 . ?
As2 S2B As1 103.0(8) 3_656 1_455 ?
As2 S2B As2B 26.3(4) 3_656 3_656 ?
As1 S2B As2B 103.5(7) 1_455 3_656 ?
As2 S2B As1B 114.5(8) 3_656 1_455 ?
As1 S2B As1B 14.6(4) 1_455 1_455 ?
As2B S2B As1B 109.6(6) 3_656 1_455 ?
As2 S2B S2 130.2(8) 3_656 . ?
As1 S2B S2 109.2(7) 1_455 . ?
As2B S2B S2 107.5(5) 3_656 . ?
As1B S2B S2 94.6(6) 1_455 . ?
As2 S3 As3 99.7(3) . 1_655 ?
As2 S3 As2B 29.5(2) . . ?
As3 S3 As2B 93.4(3) 1_655 . ?
As1 S4 As3 103.2(4) 3_656 . ?
As1 S4 As1B 15.0(4) 3_656 3_656 ?
As3 S4 As1B 109.5(3) . 3_656 ?
As1 S4 Hg 101.3(4) 3_656 . ?
As3 S4 Hg 95.9(2) . . ?
As1B S4 Hg 86.9(3) 3_656 . ?
 
_diffrn_measured_fraction_theta_max    0.784
_diffrn_reflns_theta_full              32.22
_diffrn_measured_fraction_theta_full   0.784
_refine_diff_density_max    1.720
_refine_diff_density_min   -1.182
_refine_diff_density_rms    0.298
