data_guettardite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As Pb S4 Sb' _chemical_formula_weight 532.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.527(4) _cell_length_b 7.971(4) _cell_length_c 20.102(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.814(7) _cell_angle_gamma 90.00 _cell_volume 1337.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 300(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 5.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 35.215 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 5845 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 20.91 _reflns_number_total 1264 _reflns_number_gt 1101 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0364P)^2^+150.9698P] 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 0.00002(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1264 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Pb1 Pb 0.51738(17) 0.09255(19) 0.79750(7) 0.0363(6) Uani 1 1 d . . . Pb2 Pb 0.02426(19) 0.0854(2) 0.80266(8) 0.0496(6) Uani 1 1 d . . . Sb1 Sb 0.9116(3) 0.1951(3) 0.02558(11) 0.0248(10) Uani 0.977(10) 1 d P . . Sb2 Sb 0.6597(3) 0.0196(3) 0.61316(11) 0.0276(11) Uani 0.943(11) 1 d P . . As1 As 0.3586(4) 0.1708(4) 0.99402(17) 0.0224(14) Uani 0.984(15) 1 d P . . As2 As 0.8067(4) 0.0063(4) 0.36812(15) 0.0234(14) Uani 1.049(15) 1 d P . . S1 S 0.1403(9) 0.0094(10) 0.0764(4) 0.0201(19) Uani 1 1 d . . . S2 S 0.7043(10) 0.0416(10) 0.0840(4) 0.024(2) Uani 1 1 d . . . S3 S 0.5440(10) 0.1932(11) 0.4419(4) 0.032(2) Uani 1 1 d . . . S4 S 0.4148(9) 0.1675(10) 0.6574(4) 0.0193(18) Uani 1 1 d . . . S5 S 0.1506(10) 0.1584(11) 0.4531(5) 0.036(2) Uani 1 1 d . . . S6 S 0.2689(9) 0.1414(10) 0.2817(4) 0.0207(19) Uani 1 1 d . . . S7 S 0.9997(9) 0.1658(10) 0.6596(4) 0.0220(19) Uani 1 1 d . . . S8 S 0.7558(9) 0.1549(10) 0.2686(4) 0.024(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 Pb1 0.0364(9) 0.0364(10) 0.0336(9) 0.0056(7) 0.0015(6) -0.0097(7) Pb2 0.0486(11) 0.0658(12) 0.0390(10) 0.0202(8) 0.0200(7) 0.0279(9) Sb1 0.0290(15) 0.0175(15) 0.0281(15) -0.0009(10) 0.0059(10) 0.0015(11) Sb2 0.0383(18) 0.0166(16) 0.0267(16) 0.0004(11) 0.0040(11) -0.0024(11) As1 0.019(2) 0.016(2) 0.031(2) 0.0068(15) 0.0009(14) 0.0017(15) As2 0.021(2) 0.024(2) 0.023(2) -0.0016(15) -0.0005(13) 0.0028(14) S1 0.022(4) 0.015(4) 0.023(4) 0.009(4) 0.004(3) -0.007(3) S2 0.035(5) 0.017(5) 0.023(4) -0.006(4) 0.013(4) -0.003(4) S3 0.034(5) 0.020(5) 0.044(5) -0.012(4) 0.015(4) 0.002(4) S4 0.018(4) 0.018(4) 0.022(4) -0.007(4) 0.004(3) 0.009(4) S5 0.030(5) 0.015(5) 0.068(7) -0.016(4) 0.023(5) 0.002(4) S6 0.025(4) 0.019(5) 0.019(4) -0.006(3) 0.006(3) 0.005(4) S7 0.029(5) 0.019(5) 0.018(4) 0.012(4) 0.006(4) 0.000(4) S8 0.027(5) 0.017(5) 0.030(5) 0.001(4) 0.010(4) 0.005(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 Pb1 S4 2.837(8) . ? Pb1 S6 2.968(8) 4_566 ? Pb1 S8 3.001(8) 4_566 ? Pb2 S7 2.911(7) 1_455 ? Pb2 S8 3.058(8) 4_466 ? Pb2 S2 3.068(8) 3_656 ? Pb2 S6 3.104(8) 4_566 ? Sb1 S1 2.494(8) 1_655 ? Sb1 S1 2.586(8) 3_655 ? Sb1 S2 2.618(9) . ? Sb1 S7 2.868(8) 4_565 ? Sb2 S6 2.442(8) 3_656 ? Sb2 S3 2.517(9) 3_656 ? Sb2 S5 2.700(9) 3_656 ? Sb2 S4 2.702(8) . ? As1 S5 2.253(9) 4_566 ? As1 S2 2.295(9) 3_656 ? As1 S3 2.334(9) 4_566 ? As2 S8 2.289(9) . ? As2 S7 2.301(9) 3_756 ? As2 S4 2.313(9) 3_656 ? S1 Sb1 2.494(8) 1_455 ? S1 Sb1 2.586(8) 3_655 ? S2 As1 2.295(8) 3_656 ? S2 Pb2 3.068(8) 3_656 ? S3 As1 2.334(9) 4_565 ? S3 Sb2 2.517(9) 3_656 ? S4 As2 2.313(9) 3_656 ? S5 As1 2.253(9) 4_565 ? S5 Sb2 2.700(9) 3_656 ? S6 Sb2 2.442(8) 3_656 ? S6 Pb1 2.968(8) 4_565 ? S6 Pb2 3.104(8) 4_565 ? S7 As2 2.301(9) 3_756 ? S7 Sb1 2.868(8) 4_566 ? S7 Pb2 2.911(7) 1_655 ? S8 Pb1 3.001(8) 4_565 ? S8 Pb2 3.058(8) 4_665 ? 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 S4 Pb1 S6 71.0(2) . 4_566 ? S4 Pb1 S8 75.5(2) . 4_566 ? S6 Pb1 S8 89.8(2) 4_566 4_566 ? S7 Pb2 S8 74.4(2) 1_455 4_466 ? S7 Pb2 S2 134.2(2) 1_455 3_656 ? S8 Pb2 S2 143.7(2) 4_466 3_656 ? S7 Pb2 S6 68.0(2) 1_455 4_566 ? S8 Pb2 S6 89.3(2) 4_466 4_566 ? S2 Pb2 S6 84.6(2) 3_656 4_566 ? S1 Sb1 S1 86.7(3) 1_655 3_655 ? S1 Sb1 S2 94.7(3) 1_655 . ? S1 Sb1 S2 92.2(2) 3_655 . ? S1 Sb1 S7 79.2(2) 1_655 4_565 ? S1 Sb1 S7 163.3(2) 3_655 4_565 ? S2 Sb1 S7 80.2(2) . 4_565 ? S6 Sb2 S3 93.1(3) 3_656 3_656 ? S6 Sb2 S5 94.8(3) 3_656 3_656 ? S3 Sb2 S5 81.8(3) 3_656 3_656 ? S6 Sb2 S4 91.0(3) 3_656 . ? S3 Sb2 S4 85.9(3) 3_656 . ? S5 Sb2 S4 166.7(3) 3_656 . ? S5 As1 S2 98.0(4) 4_566 3_656 ? S5 As1 S3 96.3(3) 4_566 4_566 ? S2 As1 S3 96.9(3) 3_656 4_566 ? S8 As2 S7 96.5(3) . 3_756 ? S8 As2 S4 96.7(3) . 3_656 ? S7 As2 S4 100.6(3) 3_756 3_656 ? Sb1 S1 Sb1 93.3(3) 1_455 3_655 ? As1 S2 Sb1 97.1(3) 3_656 . ? As1 S2 Pb2 107.4(3) 3_656 3_656 ? Sb1 S2 Pb2 90.6(3) . 3_656 ? As1 S3 Sb2 92.3(3) 4_565 3_656 ? As2 S4 Sb2 108.5(3) 3_656 . ? As2 S4 Pb1 99.5(3) 3_656 . ? Sb2 S4 Pb1 97.6(2) . . ? As1 S5 Sb2 89.5(3) 4_565 3_656 ? Sb2 S6 Pb1 103.7(3) 3_656 4_565 ? Sb2 S6 Pb2 107.8(3) 3_656 4_565 ? Pb1 S6 Pb2 88.2(2) 4_565 4_565 ? As2 S7 Sb1 93.7(3) 3_756 4_566 ? As2 S7 Pb2 101.4(3) 3_756 1_655 ? Sb1 S7 Pb2 164.8(3) 4_566 1_655 ? As2 S8 Pb1 101.1(3) . 4_565 ? As2 S8 Pb2 98.9(3) . 4_665 ? Pb1 S8 Pb2 90.5(2) 4_565 4_665 ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 20.91 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.827 _refine_diff_density_min -1.750 _refine_diff_density_rms 0.357