 
data_biagioniite
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'Tl2SbS2'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'S2 Sb Tl2'
_chemical_formula_weight          594.61
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Tl'  'Tl'  -2.8358   9.6688
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb'  'Sb'  -0.5866   1.5461
 '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'
 
_symmetry_cell_setting            'monoclinic'
_symmetry_space_group_name_H-M    Pc
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, z+1/2'
 
_cell_length_a                    11.0895(9)
_cell_length_b                    14.3124(11)
_cell_length_c                    7.9352(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.230(8)
_cell_angle_gamma                 90.00
_cell_volume                      1252.02(17)
_cell_formula_units_Z             8
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     508
_cell_measurement_theta_min       7.8
_cell_measurement_theta_max       13.8
 
_exptl_crystal_description        block
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.065
_exptl_crystal_size_mid           0.050
_exptl_crystal_size_min           0.040
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     6.309
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1960
_exptl_absorpt_coefficient_mu     56.155
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.121
_exptl_absorpt_correction_T_max   0.155
_exptl_absorpt_process_details    
'(ABSPACK; Oxford Diffraction, 2006)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       298(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   'Bruker D8 Venture'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  .
_diffrn_standards_interval_time   .
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             20833
_diffrn_reflns_av_R_equivalents   0.0321
_diffrn_reflns_av_sigmaI/netI     0.0424
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.33
_diffrn_reflns_theta_max          37.49
_reflns_number_total              4520
_reflns_number_gt                 2655
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'APEX3 (Bruker Inc., 2016)'
_computing_cell_refinement        'APEX3 (Bruker Inc., 2016)'
_computing_data_reduction         'APEX3 (Bruker Inc., 2016)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 2001)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 2008)'
 
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     .
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.000085(15)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.003(10)
_refine_ls_number_reflns          4520
_refine_ls_number_parameters      182
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0315
_refine_ls_R_factor_gt            0.0243
_refine_ls_wR_factor_ref          0.0717
_refine_ls_wR_factor_gt           0.0713
_refine_ls_goodness_of_fit_ref    0.939
_refine_ls_restrained_S_all       0.939
_refine_ls_shift/su_max           0.001
_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
Tl1 Tl 0.23733(13) 0.59615(8) 0.42312(14) 0.0344(3) Uani 1 1 d . . .
Tl2 Tl 0.04141(14) 0.91367(9) 0.72629(15) 0.0437(4) Uani 1 1 d . . .
Tl3 Tl 0.69297(12) 0.90702(8) 0.12240(13) 0.0299(3) Uani 1 1 d . . .
Tl4 Tl 0.35736(13) 0.89299(8) 0.62921(17) 0.0356(3) Uani 1 1 d . . .
Tl5 Tl 0.56511(13) 0.60615(8) 0.89568(17) 0.0355(3) Uani 1 1 d . . .
Tl6 Tl 0.96143(15) 0.79027(10) 0.30728(18) 0.0526(4) Uani 1 1 d . . .
Tl7 Tl 0.8383(2) 0.49262(12) 0.6517(2) 0.0838(7) Uani 1 1 d . . .
Tl8 Tl 0.96092(16) 0.68618(11) 0.8476(2) 0.0713(5) Uani 1 1 d . . .
Sb1 Sb 0.31287(16) 0.68477(11) 0.9379(2) 0.0143(4) Uani 1 1 d . . .
Sb2 Sb 0.61774(17) 0.68126(12) 0.3516(2) 0.0167(4) Uani 1 1 d . . .
Sb3 Sb 0.30962(17) 0.83097(11) 0.1799(2) 0.0155(4) Uani 1 1 d . . .
Sb4 Sb 0.62590(17) 0.82160(12) 0.6039(2) 0.0157(4) Uani 1 1 d . . .
S1 S 0.1528(7) 0.5806(4) 0.0502(9) 0.0188(15) Uani 1 1 d . . .
S2 S 0.7909(7) 0.9183(5) 0.5002(8) 0.0177(14) Uani 1 1 d . . .
S3 S 0.1927(7) 0.7465(4) 0.6551(8) 0.0162(14) Uani 1 1 d . . .
S4 S 0.7352(8) 0.7510(5) 0.8912(8) 0.0229(17) Uani 1 1 d . . .
S5 S 0.8479(7) 0.6293(4) 0.4144(9) 0.0191(15) Uani 1 1 d . . .
S6 S 0.5150(7) 0.5673(5) 0.5200(9) 0.0237(17) Uani 1 1 d . . .
S7 S 0.0903(7) 0.8956(5) 0.1036(8) 0.0202(15) Uani 1 1 d . . .
S8 S 0.4270(7) 0.9350(4) 0.0130(9) 0.0179(14) Uani 1 1 d . . .
 
 
_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
Tl1 S3 2.909(6) . ?
Tl1 S1 2.916(7) 2_565 ?
Tl1 S1 3.014(7) . ?
Tl1 S6 3.119(8) . ?
Tl2 S7 2.967(7) 2_575 ?
Tl2 S7 2.995(6) 1_556 ?
Tl2 S3 3.011(6) . ?
Tl2 S2 3.140(7) 1_455 ?
Tl2 Tl8 3.537(2) 1_455 ?
Tl2 Tl4 3.680(2) . ?
Tl3 S2 2.932(7) 2_574 ?
Tl3 S4 2.960(7) 1_554 ?
Tl3 S8 3.010(7) . ?
Tl3 S2 3.080(6) . ?
Tl3 Tl6 3.586(2) . ?
Tl4 S8 2.768(7) 2_575 ?
Tl4 S3 2.802(7) . ?
Tl4 S8 3.118(7) 1_556 ?
Tl4 Sb4 3.175(2) . ?
Tl5 S6 2.750(7) 2_565 ?
Tl5 S4 2.805(8) . ?
Tl5 S6 3.024(7) . ?
Tl5 Sb1 3.067(2) . ?
Tl5 Tl7 3.737(3) 2_565 ?
Tl6 S7 2.726(7) 1_655 ?
Tl6 S5 2.802(7) . ?
Tl6 S2 3.148(7) . ?
Tl7 S5 2.712(7) 2_565 ?
Tl7 S5 2.725(7) . ?
Tl7 Tl8 3.388(3) . ?
Tl7 Tl5 3.737(3) 2_564 ?
Tl8 S4 2.726(9) . ?
Tl8 S1 2.942(7) 1_656 ?
Tl8 Tl2 3.537(2) 1_655 ?
Sb1 S1 2.552(8) 1_556 ?
Sb1 S3 2.635(6) . ?
Sb1 Sb3 2.843(2) 1_556 ?
Sb2 S6 2.465(8) . ?
Sb2 S5 2.653(8) . ?
Sb2 Sb4 2.830(3) . ?
Sb3 S8 2.458(7) . ?
Sb3 S7 2.612(7) . ?
Sb3 Sb1 2.843(2) 1_554 ?
Sb4 S2 2.504(8) . ?
Sb4 S4 2.663(7) . ?
S1 Sb1 2.552(8) 1_554 ?
S1 Tl1 2.916(7) 2_564 ?
S1 Tl8 2.942(7) 1_454 ?
S2 Tl3 2.932(7) 2_575 ?
S2 Tl2 3.140(7) 1_655 ?
S4 Tl3 2.960(7) 1_556 ?
S5 Tl7 2.712(7) 2_564 ?
S6 Tl5 2.750(7) 2_564 ?
S7 Tl6 2.726(7) 1_455 ?
S7 Tl2 2.967(7) 2_574 ?
S7 Tl2 2.995(6) 1_554 ?
S8 Tl4 2.768(7) 2_574 ?
S8 Tl4 3.118(7) 1_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
S3 Tl1 S1 109.9(2) . 2_565 ?
S3 Tl1 S1 128.30(18) . . ?
S1 Tl1 S1 101.43(16) 2_565 . ?
S3 Tl1 S6 100.0(2) . . ?
S1 Tl1 S6 98.4(2) 2_565 . ?
S1 Tl1 S6 115.2(2) . . ?
S7 Tl2 S7 112.80(18) 2_575 1_556 ?
S7 Tl2 S3 123.0(2) 2_575 . ?
S7 Tl2 S3 94.30(19) 1_556 . ?
S7 Tl2 S2 88.55(18) 2_575 1_455 ?
S7 Tl2 S2 128.7(2) 1_556 1_455 ?
S3 Tl2 S2 112.72(18) . 1_455 ?
S7 Tl2 Tl8 175.15(14) 2_575 1_455 ?
S7 Tl2 Tl8 70.87(14) 1_556 1_455 ?
S3 Tl2 Tl8 58.79(14) . 1_455 ?
S2 Tl2 Tl8 86.63(13) 1_455 1_455 ?
S7 Tl2 Tl4 78.08(15) 2_575 . ?
S7 Tl2 Tl4 97.43(15) 1_556 . ?
S3 Tl2 Tl4 48.25(14) . . ?
S2 Tl2 Tl4 133.28(14) 1_455 . ?
Tl8 Tl2 Tl4 104.89(5) 1_455 . ?
S2 Tl3 S4 110.44(19) 2_574 1_554 ?
S2 Tl3 S8 100.24(19) 2_574 . ?
S4 Tl3 S8 97.9(2) 1_554 . ?
S2 Tl3 S2 99.96(17) 2_574 . ?
S4 Tl3 S2 125.46(19) 1_554 . ?
S8 Tl3 S2 120.3(2) . . ?
S2 Tl3 Tl6 102.22(15) 2_574 . ?
S4 Tl3 Tl6 73.84(15) 1_554 . ?
S8 Tl3 Tl6 157.54(12) . . ?
S2 Tl3 Tl6 55.73(14) . . ?
S8 Tl4 S3 153.8(2) 2_575 . ?
S8 Tl4 S8 96.05(14) 2_575 1_556 ?
S3 Tl4 S8 99.61(18) . 1_556 ?
S8 Tl4 Sb4 88.15(16) 2_575 . ?
S3 Tl4 Sb4 112.76(15) . . ?
S8 Tl4 Sb4 89.39(15) 1_556 . ?
S8 Tl4 Tl2 107.73(16) 2_575 . ?
S3 Tl4 Tl2 53.29(14) . . ?
S8 Tl4 Tl2 85.44(14) 1_556 . ?
Sb4 Tl4 Tl2 163.72(5) . . ?
S6 Tl5 S4 146.5(2) 2_565 . ?
S6 Tl5 S6 99.49(14) 2_565 . ?
S4 Tl5 S6 100.10(19) . . ?
S6 Tl5 Sb1 94.00(17) 2_565 . ?
S4 Tl5 Sb1 110.66(17) . . ?
S6 Tl5 Sb1 95.92(16) . . ?
S6 Tl5 Tl7 69.32(16) 2_565 2_565 ?
S4 Tl5 Tl7 77.28(16) . 2_565 ?
S6 Tl5 Tl7 121.17(15) . 2_565 ?
Sb1 Tl5 Tl7 140.75(6) . 2_565 ?
S7 Tl6 S5 156.5(2) 1_655 . ?
S7 Tl6 S2 110.3(2) 1_655 . ?
S5 Tl6 S2 91.0(2) . . ?
S7 Tl6 Tl3 87.99(15) 1_655 . ?
S5 Tl6 Tl3 97.28(15) . . ?
S2 Tl6 Tl3 53.97(12) . . ?
S5 Tl7 S5 172.7(2) 2_565 . ?
S5 Tl7 Tl8 101.14(15) 2_565 . ?
S5 Tl7 Tl8 71.71(15) . . ?
S5 Tl7 Tl5 97.84(15) 2_565 2_564 ?
S5 Tl7 Tl5 89.20(15) . 2_564 ?
Tl8 Tl7 Tl5 145.09(7) . 2_564 ?
S4 Tl8 S1 136.5(2) . 1_656 ?
S4 Tl8 Tl7 90.45(16) . . ?
S1 Tl8 Tl7 93.52(14) 1_656 . ?
S4 Tl8 Tl2 89.07(15) . 1_655 ?
S1 Tl8 Tl2 115.64(15) 1_656 1_655 ?
Tl7 Tl8 Tl2 136.75(7) . 1_655 ?
S1 Sb1 S3 100.8(2) 1_556 . ?
S1 Sb1 Sb3 97.69(17) 1_556 1_556 ?
S3 Sb1 Sb3 106.63(15) . 1_556 ?
S1 Sb1 Tl5 120.08(17) 1_556 . ?
S3 Sb1 Tl5 114.38(17) . . ?
Sb3 Sb1 Tl5 114.99(7) 1_556 . ?
S6 Sb2 S5 101.8(2) . . ?
S6 Sb2 Sb4 93.87(18) . . ?
S5 Sb2 Sb4 96.30(16) . . ?
S8 Sb3 S7 101.2(2) . . ?
S8 Sb3 Sb1 92.04(17) . 1_554 ?
S7 Sb3 Sb1 100.60(17) . 1_554 ?
S2 Sb4 S4 102.1(2) . . ?
S2 Sb4 Sb2 97.38(16) . . ?
S4 Sb4 Sb2 108.22(16) . . ?
S2 Sb4 Tl4 124.53(17) . . ?
S4 Sb4 Tl4 114.27(19) . . ?
Sb2 Sb4 Tl4 108.35(7) . . ?
Sb1 S1 Tl1 97.1(3) 1_554 2_564 ?
Sb1 S1 Tl8 89.9(2) 1_554 1_454 ?
Tl1 S1 Tl8 119.8(2) 2_564 1_454 ?
Sb1 S1 Tl1 98.4(2) 1_554 . ?
Tl1 S1 Tl1 109.0(2) 2_564 . ?
Tl8 S1 Tl1 128.9(3) 1_454 . ?
Sb4 S2 Tl3 93.0(2) . 2_575 ?
Sb4 S2 Tl3 95.6(2) . . ?
Tl3 S2 Tl3 105.2(2) 2_575 . ?
Sb4 S2 Tl2 115.7(2) . 1_655 ?
Tl3 S2 Tl2 99.54(19) 2_575 1_655 ?
Tl3 S2 Tl2 138.7(3) . 1_655 ?
Sb4 S2 Tl6 109.7(2) . . ?
Tl3 S2 Tl6 157.1(3) 2_575 . ?
Tl3 S2 Tl6 70.30(14) . . ?
Tl2 S2 Tl6 74.01(17) 1_655 . ?
Sb1 S3 Tl4 92.3(2) . . ?
Sb1 S3 Tl1 100.7(2) . . ?
Tl4 S3 Tl1 110.5(2) . . ?
Sb1 S3 Tl2 110.3(2) . . ?
Tl4 S3 Tl2 78.46(15) . . ?
Tl1 S3 Tl2 147.5(2) . . ?
Sb4 S4 Tl8 111.1(2) . . ?
Sb4 S4 Tl5 92.7(2) . . ?
Tl8 S4 Tl5 112.2(2) . . ?
Sb4 S4 Tl3 99.0(2) . 1_556 ?
Tl8 S4 Tl3 123.0(3) . 1_556 ?
Tl5 S4 Tl3 113.4(3) . 1_556 ?
Sb2 S5 Tl7 94.5(2) . 2_564 ?
Sb2 S5 Tl7 102.8(3) . . ?
Tl7 S5 Tl7 93.90(19) 2_564 . ?
Sb2 S5 Tl6 99.6(2) . . ?
Tl7 S5 Tl6 106.1(3) 2_564 . ?
Tl7 S5 Tl6 148.5(3) . . ?
Sb2 S6 Tl5 106.2(3) . 2_564 ?
Sb2 S6 Tl5 111.5(2) . . ?
Tl5 S6 Tl5 119.8(3) 2_564 . ?
Sb2 S6 Tl1 106.3(3) . . ?
Tl5 S6 Tl1 105.3(2) 2_564 . ?
Tl5 S6 Tl1 106.8(2) . . ?
Sb3 S7 Tl6 101.6(2) . 1_455 ?
Sb3 S7 Tl2 116.6(3) . 2_574 ?
Tl6 S7 Tl2 100.9(2) 1_455 2_574 ?
Sb3 S7 Tl2 109.0(3) . 1_554 ?
Tl6 S7 Tl2 126.2(3) 1_455 1_554 ?
Tl2 S7 Tl2 103.2(2) 2_574 1_554 ?
Sb3 S8 Tl4 100.1(3) . 2_574 ?
Sb3 S8 Tl3 108.9(2) . . ?
Tl4 S8 Tl3 108.8(2) 2_574 . ?
Sb3 S8 Tl4 108.7(2) . 1_554 ?
Tl4 S8 Tl4 116.6(2) 2_574 1_554 ?
Tl3 S8 Tl4 112.8(2) . 1_554 ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              37.49
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    1.717
_refine_diff_density_min   -1.569
_refine_diff_density_rms    0.401

#
# h,k,l, Fc-squared, Fo-squared, sigma(Fo-squared) and status flag
#
data_shelx
_shelx_title ' weird phase in Pc'
_shelx_refln_list_code          4
_shelx_F_calc_maximum      677.78
_exptl_crystal_F_000      1960.00
_reflns_d_resolution_high  0.5839
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, z+1/2'
 
_cell_length_a    11.0895
_cell_length_b    14.3124
_cell_length_c     7.9352
_cell_angle_alpha  90.000
_cell_angle_beta   96.230
_cell_angle_gamma  90.000
 
_shelx_F_squared_multiplier     1.000
 
