data_athene _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As Hg0 Pd2 Sb0' _chemical_formula_weight 287.72 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' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y, -z' 'y, x, z' 'y, x, -z' 'x-y, -y, -z' 'x-y, -y, z' '-x, -x+y, z' '-x, -x+y, -z' '-y, x-y, z' '-y, x-y, -z' '-x+y, -x, -z' '-x+y, -x, z' _cell_length_a 6.8130(10) _cell_length_b 6.8130(10) _cell_length_c 3.4892(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 140.26(4) _cell_formula_units_Z 2 _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 6.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 250 _exptl_absorpt_coefficient_mu 24.155 _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 2419 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 34.95 _reflns_number_total 261 _reflns_number_gt 261 _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^)+(0.0182P)^2^+3.2229P] 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 0.070(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_number_reflns 261 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 2.178 _refine_ls_restrained_S_all 2.178 _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 Pd1 Pd 0.7424(4) 0.0000 0.0000 0.0203(8) Uani 1 4 d S . . Pd2 Pd 0.3984(5) 0.0000 0.5000 0.0279(11) Uani 1 4 d S . . As1 As 0.0000 0.0000 0.5000 0.0182(12) Uani 1 12 d S . . As2 As 0.3333 0.6667 0.0000 0.0287(11) Uani 0.60(2) 6 d SP . . Hg2 Hg 0.3333 0.6667 0.0000 0.0287(11) Uani 0.40(2) 6 d SP . . 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 Pd1 0.0126(9) 0.0198(12) 0.0310(14) 0.000 0.000 0.0099(6) Pd2 0.0221(11) 0.058(2) 0.0159(11) 0.000 0.000 0.0288(12) As1 0.0217(16) 0.0217(16) 0.011(2) 0.000 0.000 0.0108(8) As2 0.0066(7) 0.0066(7) 0.073(3) 0.000 0.000 0.0033(4) Hg2 0.0066(7) 0.0066(7) 0.073(3) 0.000 0.000 0.0033(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 Pd1 As1 2.4746(18) 1_655 ? Pd1 As1 2.4746(18) 1_654 ? Pd1 Hg2 2.5682(17) 3 ? Pd1 As2 2.5682(17) 3 ? Pd1 Hg2 2.5682(17) 1_545 ? Pd1 As2 2.5682(17) 1_545 ? Pd1 Pd2 2.922(3) 1_554 ? Pd1 Pd2 2.922(3) . ? Pd1 Pd2 2.954(2) 3_655 ? Pd1 Pd2 2.954(2) 7_654 ? Pd1 Pd2 2.954(2) 3_654 ? Pd1 Pd2 2.954(2) 7_655 ? Pd2 As1 2.714(3) . ? Pd2 Hg2 2.7186(9) 1_545 ? Pd2 As2 2.7186(9) 1_545 ? Pd2 Hg2 2.7186(9) 3_556 ? Pd2 As2 2.7186(9) 3_556 ? Pd2 Hg2 2.7186(9) 1_546 ? Pd2 As2 2.7186(9) 1_546 ? Pd2 Hg2 2.7186(9) 3 ? Pd2 As2 2.7186(9) 3 ? Pd2 Pd1 2.922(3) 1_556 ? Pd2 Pd1 2.954(2) 3_545 ? As1 Pd1 2.4746(19) 7_666 ? As1 Pd1 2.4746(18) 3_545 ? As1 Pd1 2.4746(18) 1_455 ? As1 Pd1 2.4746(19) 7_665 ? As1 Pd1 2.4746(18) 1_456 ? As1 Pd1 2.4746(18) 3_546 ? As1 Pd2 2.714(3) 7 ? As1 Pd2 2.714(3) 3 ? As2 Pd1 2.5682(17) 3 ? As2 Pd1 2.5682(17) 1_565 ? As2 Pd1 2.5682(17) 7_665 ? As2 Pd2 2.7186(9) 1_565 ? As2 Pd2 2.7186(9) 3_554 ? As2 Pd2 2.7186(9) 1_564 ? As2 Pd2 2.7186(9) 3 ? As2 Pd2 2.7186(9) 7_665 ? As2 Pd2 2.7186(9) 7_664 ? 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 As1 Pd1 As1 89.66(9) 1_655 1_654 ? As1 Pd1 Hg2 117.133(6) 1_655 3 ? As1 Pd1 Hg2 117.134(6) 1_654 3 ? As1 Pd1 As2 117.133(6) 1_655 3 ? As1 Pd1 As2 117.134(6) 1_654 3 ? Hg2 Pd1 As2 0.0 3 3 ? As1 Pd1 Hg2 117.134(6) 1_655 1_545 ? As1 Pd1 Hg2 117.133(6) 1_654 1_545 ? Hg2 Pd1 Hg2 99.96(9) 3 1_545 ? As2 Pd1 Hg2 99.96(9) 3 1_545 ? As1 Pd1 As2 117.134(6) 1_655 1_545 ? As1 Pd1 As2 117.133(6) 1_654 1_545 ? Hg2 Pd1 As2 99.96(9) 3 1_545 ? As2 Pd1 As2 99.96(9) 3 1_545 ? Hg2 Pd1 As2 0.0 1_545 1_545 ? As1 Pd1 Pd2 171.83(8) 1_655 1_554 ? As1 Pd1 Pd2 98.50(4) 1_654 1_554 ? Hg2 Pd1 Pd2 58.95(5) 3 1_554 ? As2 Pd1 Pd2 58.95(5) 3 1_554 ? Hg2 Pd1 Pd2 58.95(5) 1_545 1_554 ? As2 Pd1 Pd2 58.95(5) 1_545 1_554 ? As1 Pd1 Pd2 98.50(4) 1_655 . ? As1 Pd1 Pd2 171.83(8) 1_654 . ? Hg2 Pd1 Pd2 58.95(5) 3 . ? As2 Pd1 Pd2 58.95(5) 3 . ? Hg2 Pd1 Pd2 58.95(5) 1_545 . ? As2 Pd1 Pd2 58.95(5) 1_545 . ? Pd2 Pd1 Pd2 73.33(9) 1_554 . ? As1 Pd1 Pd2 59.22(6) 1_655 3_655 ? As1 Pd1 Pd2 108.71(7) 1_654 3_655 ? Hg2 Pd1 Pd2 58.48(5) 3 3_655 ? As2 Pd1 Pd2 58.48(5) 3 3_655 ? Hg2 Pd1 Pd2 134.10(6) 1_545 3_655 ? As2 Pd1 Pd2 134.10(6) 1_545 3_655 ? Pd2 Pd1 Pd2 117.43(7) 1_554 3_655 ? Pd2 Pd1 Pd2 75.84(5) . 3_655 ? As1 Pd1 Pd2 108.71(7) 1_655 7_654 ? As1 Pd1 Pd2 59.22(6) 1_654 7_654 ? Hg2 Pd1 Pd2 134.10(6) 3 7_654 ? As2 Pd1 Pd2 134.10(6) 3 7_654 ? Hg2 Pd1 Pd2 58.48(5) 1_545 7_654 ? As2 Pd1 Pd2 58.48(5) 1_545 7_654 ? Pd2 Pd1 Pd2 75.84(5) 1_554 7_654 ? Pd2 Pd1 Pd2 117.43(7) . 7_654 ? Pd2 Pd1 Pd2 164.53(13) 3_655 7_654 ? As1 Pd1 Pd2 108.71(7) 1_655 3_654 ? As1 Pd1 Pd2 59.22(6) 1_654 3_654 ? Hg2 Pd1 Pd2 58.48(5) 3 3_654 ? As2 Pd1 Pd2 58.48(5) 3 3_654 ? Hg2 Pd1 Pd2 134.10(6) 1_545 3_654 ? As2 Pd1 Pd2 134.10(6) 1_545 3_654 ? Pd2 Pd1 Pd2 75.84(5) 1_554 3_654 ? Pd2 Pd1 Pd2 117.43(7) . 3_654 ? Pd2 Pd1 Pd2 72.39(6) 3_655 3_654 ? Pd2 Pd1 Pd2 105.45(8) 7_654 3_654 ? As1 Pd1 Pd2 59.22(6) 1_655 7_655 ? As1 Pd1 Pd2 108.71(7) 1_654 7_655 ? Hg2 Pd1 Pd2 134.10(6) 3 7_655 ? As2 Pd1 Pd2 134.10(6) 3 7_655 ? Hg2 Pd1 Pd2 58.48(5) 1_545 7_655 ? As2 Pd1 Pd2 58.48(5) 1_545 7_655 ? Pd2 Pd1 Pd2 117.43(7) 1_554 7_655 ? Pd2 Pd1 Pd2 75.84(5) . 7_655 ? Pd2 Pd1 Pd2 105.45(8) 3_655 7_655 ? Pd2 Pd1 Pd2 72.39(6) 7_654 7_655 ? Pd2 Pd1 Pd2 164.53(13) 3_654 7_655 ? As1 Pd2 Hg2 104.75(7) . 1_545 ? As1 Pd2 As2 104.75(7) . 1_545 ? Hg2 Pd2 As2 0.0 1_545 1_545 ? As1 Pd2 Hg2 104.75(7) . 3_556 ? Hg2 Pd2 Hg2 150.50(13) 1_545 3_556 ? As2 Pd2 Hg2 150.50(13) 1_545 3_556 ? As1 Pd2 As2 104.75(7) . 3_556 ? Hg2 Pd2 As2 150.50(13) 1_545 3_556 ? As2 Pd2 As2 150.50(13) 1_545 3_556 ? Hg2 Pd2 As2 0.0 3_556 3_556 ? As1 Pd2 Hg2 104.75(7) . 1_546 ? Hg2 Pd2 Hg2 79.84(3) 1_545 1_546 ? As2 Pd2 Hg2 79.84(3) 1_545 1_546 ? Hg2 Pd2 Hg2 92.68(4) 3_556 1_546 ? As2 Pd2 Hg2 92.68(4) 3_556 1_546 ? As1 Pd2 As2 104.75(7) . 1_546 ? Hg2 Pd2 As2 79.84(3) 1_545 1_546 ? As2 Pd2 As2 79.84(3) 1_545 1_546 ? Hg2 Pd2 As2 92.68(4) 3_556 1_546 ? As2 Pd2 As2 92.68(4) 3_556 1_546 ? Hg2 Pd2 As2 0.0 1_546 1_546 ? As1 Pd2 Hg2 104.75(7) . 3 ? Hg2 Pd2 Hg2 92.68(4) 1_545 3 ? As2 Pd2 Hg2 92.68(4) 1_545 3 ? Hg2 Pd2 Hg2 79.84(3) 3_556 3 ? As2 Pd2 Hg2 79.84(3) 3_556 3 ? Hg2 Pd2 Hg2 150.50(13) 1_546 3 ? As2 Pd2 Hg2 150.50(13) 1_546 3 ? As1 Pd2 As2 104.75(7) . 3 ? Hg2 Pd2 As2 92.68(4) 1_545 3 ? As2 Pd2 As2 92.68(4) 1_545 3 ? Hg2 Pd2 As2 79.84(3) 3_556 3 ? As2 Pd2 As2 79.84(3) 3_556 3 ? Hg2 Pd2 As2 150.50(13) 1_546 3 ? As2 Pd2 As2 150.50(13) 1_546 3 ? Hg2 Pd2 As2 0.0 3 3 ? As1 Pd2 Pd1 143.34(5) . 1_556 ? Hg2 Pd2 Pd1 100.31(8) 1_545 1_556 ? As2 Pd2 Pd1 100.31(8) 1_545 1_556 ? Hg2 Pd2 Pd1 54.03(4) 3_556 1_556 ? As2 Pd2 Pd1 54.03(4) 3_556 1_556 ? Hg2 Pd2 Pd1 54.03(4) 1_546 1_556 ? As2 Pd2 Pd1 54.03(4) 1_546 1_556 ? Hg2 Pd2 Pd1 100.31(8) 3 1_556 ? As2 Pd2 Pd1 100.31(8) 3 1_556 ? As1 Pd2 Pd1 143.34(5) . . ? Hg2 Pd2 Pd1 54.03(4) 1_545 . ? As2 Pd2 Pd1 54.03(4) 1_545 . ? Hg2 Pd2 Pd1 100.31(8) 3_556 . ? As2 Pd2 Pd1 100.31(8) 3_556 . ? Hg2 Pd2 Pd1 100.31(8) 1_546 . ? As2 Pd2 Pd1 100.31(8) 1_546 . ? Hg2 Pd2 Pd1 54.03(4) 3 . ? As2 Pd2 Pd1 54.03(4) 3 . ? Pd1 Pd2 Pd1 73.33(9) 1_556 . ? As1 Pd2 Pd1 51.55(7) . 3_545 ? Hg2 Pd2 Pd1 53.64(4) 1_545 3_545 ? As2 Pd2 Pd1 53.64(4) 1_545 3_545 ? Hg2 Pd2 Pd1 155.42(12) 3_556 3_545 ? As2 Pd2 Pd1 155.42(12) 3_556 3_545 ? Hg2 Pd2 Pd1 99.50(5) 1_546 3_545 ? As2 Pd2 Pd1 99.50(5) 1_546 3_545 ? Hg2 Pd2 Pd1 98.71(4) 3 3_545 ? As2 Pd2 Pd1 98.71(4) 3 3_545 ? Pd1 Pd2 Pd1 148.36(6) 1_556 3_545 ? Pd1 Pd2 Pd1 98.40(5) . 3_545 ? Pd1 As1 Pd1 138.46(3) 7_666 3_545 ? Pd1 As1 Pd1 138.46(3) 7_666 1_455 ? Pd1 As1 Pd1 75.78(7) 3_545 1_455 ? Pd1 As1 Pd1 89.66(9) 7_666 7_665 ? Pd1 As1 Pd1 75.78(7) 3_545 7_665 ? Pd1 As1 Pd1 75.78(7) 1_455 7_665 ? Pd1 As1 Pd1 75.78(7) 7_666 1_456 ? Pd1 As1 Pd1 138.46(3) 3_545 1_456 ? Pd1 As1 Pd1 89.66(9) 1_455 1_456 ? Pd1 As1 Pd1 138.46(3) 7_665 1_456 ? Pd1 As1 Pd1 75.78(7) 7_666 3_546 ? Pd1 As1 Pd1 89.66(9) 3_545 3_546 ? Pd1 As1 Pd1 138.46(3) 1_455 3_546 ? Pd1 As1 Pd1 138.46(3) 7_665 3_546 ? Pd1 As1 Pd1 75.78(7) 1_456 3_546 ? Pd1 As1 Pd2 135.17(4) 7_666 7 ? Pd1 As1 Pd2 69.231(16) 3_545 7 ? Pd1 As1 Pd2 69.231(16) 1_455 7 ? Pd1 As1 Pd2 135.17(4) 7_665 7 ? Pd1 As1 Pd2 69.231(16) 1_456 7 ? Pd1 As1 Pd2 69.231(16) 3_546 7 ? Pd1 As1 Pd2 69.231(16) 7_666 3 ? Pd1 As1 Pd2 135.17(4) 3_545 3 ? Pd1 As1 Pd2 69.231(16) 1_455 3 ? Pd1 As1 Pd2 69.231(16) 7_665 3 ? Pd1 As1 Pd2 69.231(16) 1_456 3 ? Pd1 As1 Pd2 135.17(4) 3_546 3 ? Pd2 As1 Pd2 120.0 7 3 ? Pd1 As1 Pd2 69.231(16) 7_666 . ? Pd1 As1 Pd2 69.231(16) 3_545 . ? Pd1 As1 Pd2 135.17(4) 1_455 . ? Pd1 As1 Pd2 69.231(16) 7_665 . ? Pd1 As1 Pd2 135.17(4) 1_456 . ? Pd1 As1 Pd2 69.231(16) 3_546 . ? Pd2 As1 Pd2 120.0 7 . ? Pd2 As1 Pd2 120.0 3 . ? Pd1 As2 Pd1 120.0 3 1_565 ? Pd1 As2 Pd1 120.0 3 7_665 ? Pd1 As2 Pd1 120.0 1_565 7_665 ? Pd1 As2 Pd2 67.88(7) 3 1_565 ? Pd1 As2 Pd2 67.03(6) 1_565 1_565 ? Pd1 As2 Pd2 140.075(16) 7_665 1_565 ? Pd1 As2 Pd2 67.03(6) 3 3_554 ? Pd1 As2 Pd2 140.075(17) 1_565 3_554 ? Pd1 As2 Pd2 67.88(7) 7_665 3_554 ? Pd2 As2 Pd2 134.903(11) 1_565 3_554 ? Pd1 As2 Pd2 67.88(7) 3 1_564 ? Pd1 As2 Pd2 67.03(6) 1_565 1_564 ? Pd1 As2 Pd2 140.075(16) 7_665 1_564 ? Pd2 As2 Pd2 79.84(3) 1_565 1_564 ? Pd2 As2 Pd2 83.24(2) 3_554 1_564 ? Pd1 As2 Pd2 67.03(6) 3 3 ? Pd1 As2 Pd2 140.075(17) 1_565 3 ? Pd1 As2 Pd2 67.88(7) 7_665 3 ? Pd2 As2 Pd2 83.24(2) 1_565 3 ? Pd2 As2 Pd2 79.84(3) 3_554 3 ? Pd2 As2 Pd2 134.903(11) 1_564 3 ? Pd1 As2 Pd2 140.075(16) 3 7_665 ? Pd1 As2 Pd2 67.88(7) 1_565 7_665 ? Pd1 As2 Pd2 67.03(6) 7_665 7_665 ? Pd2 As2 Pd2 83.24(2) 1_565 7_665 ? Pd2 As2 Pd2 134.903(11) 3_554 7_665 ? Pd2 As2 Pd2 134.903(11) 1_564 7_665 ? Pd2 As2 Pd2 83.24(2) 3 7_665 ? Pd1 As2 Pd2 140.075(16) 3 7_664 ? Pd1 As2 Pd2 67.88(7) 1_565 7_664 ? Pd1 As2 Pd2 67.03(6) 7_665 7_664 ? Pd2 As2 Pd2 134.903(11) 1_565 7_664 ? Pd2 As2 Pd2 83.24(2) 3_554 7_664 ? Pd2 As2 Pd2 83.24(2) 1_564 7_664 ? Pd2 As2 Pd2 134.903(11) 3 7_664 ? Pd2 As2 Pd2 79.84(3) 7_665 7_664 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 34.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.360 _refine_diff_density_min -1.249 _refine_diff_density_rms 1.110