data_northstarite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'northstarite' _chemical_compound_source 'North Star mine, Utah' _chemical_formula_sum 'O18 Pb6 S2 Te5' _chemical_formula_weight 2233.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 10.2495(5) _cell_length_b 10.2495(5) _cell_length_c 11.6677(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1061.50(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20072 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'Chip' _exptl_crystal_colour 'Colorless' _exptl_crystal_density_diffrn 6.987 _exptl_crystal_F_000 1856 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.015 _exptl_absorpt_coefficient_mu 54.423 _exptl_absorpt_correction_T_min 0.365 _exptl_absorpt_correction_T_max 1.000 _shelx_estimated_absorpt_T_min 0.172 _shelx_estimated_absorpt_T_max 0.496 _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 25512 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_av_R_equivalents 0.1601 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.492 _diffrn_reflns_theta_max 27.435 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 1621 _reflns_number_gt 1476 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.907 _reflns_Friedel_fraction_max 0.997 _reflns_Friedel_fraction_full 0.998 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+6.1470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 637 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 1621 _refine_ls_number_parameters 94 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.66140(10) 0.67516(14) 0.30337(5) 0.0208(3) Uani 1 1 d . . . . . Pb2 Pb 0.66736(8) 0.67976(11) 0.64246(5) 0.0207(3) Uani 1 1 d . . . . . Te1 Te 0.666667 0.333333 0.6632(2) 0.0143(5) Uani 1 3 d S T P . . Te2 Te 0.666667 0.333333 0.2805(3) 0.0157(6) Uani 1 3 d S T P . . Te3 Te 0.35729(10) 0.36016(11) 0.47308(18) 0.0166(2) Uani 1 1 d . . . . . S1 S 0.000000 0.000000 0.4269(6) 0.0182(14) Uani 1 3 d S T P . . S2 S 0.000000 0.000000 0.2528(7) 0.030(2) Uani 1 3 d S T P . . O1 O 0.6281(16) 0.4709(16) 0.7507(11) 0.017(3) Uani 1 1 d . . . . . O2 O 0.6266(14) 0.4668(17) 0.1952(12) 0.018(3) Uani 1 1 d . . . . . O3 O 0.3785(17) 0.2548(15) 0.3502(12) 0.018(3) Uani 1 1 d . . . . . O4 O 0.3774(18) 0.2524(17) 0.5948(12) 0.022(3) Uani 1 1 d . . . . . O5 O 0.5576(10) 0.5223(10) 0.4747(14) 0.023(2) Uani 1 1 d . . . . . O6 O 0.0471(11) 0.1518(10) 0.4660(15) 0.025(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 0.0257(6) 0.0179(6) 0.0182(5) -0.0009(4) 0.0010(3) 0.0105(5) Pb2 0.0265(5) 0.0162(6) 0.0194(5) 0.0009(4) -0.0015(4) 0.0108(4) Te1 0.0133(7) 0.0133(7) 0.0161(15) 0.000 0.000 0.0067(4) Te2 0.0135(8) 0.0135(8) 0.0202(16) 0.000 0.000 0.0067(4) Te3 0.0164(4) 0.0180(4) 0.0154(5) 0.0012(11) 0.0018(10) 0.0086(4) S1 0.019(2) 0.019(2) 0.017(3) 0.000 0.000 0.0093(10) S2 0.028(2) 0.028(2) 0.035(6) 0.000 0.000 0.0138(12) O1 0.034(9) 0.015(7) 0.008(6) -0.006(5) -0.006(6) 0.017(7) O2 0.008(7) 0.018(8) 0.024(7) -0.002(6) -0.005(6) 0.002(6) O3 0.021(8) 0.018(7) 0.020(8) -0.003(6) -0.003(6) 0.012(6) O4 0.026(8) 0.026(8) 0.013(8) 0.000(6) -0.004(6) 0.012(7) O5 0.014(4) 0.023(5) 0.025(5) -0.009(8) -0.010(8) 0.005(4) O6 0.030(5) 0.019(5) 0.028(6) 0.001(7) 0.002(8) 0.012(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 O2 2.349(15) . ? Pb1 O5 2.432(15) . ? Pb1 O3 2.582(13) 3_665 ? Pb1 O4 2.632(14) 4_664 ? Pb1 O1 2.642(15) 4_664 ? Pb1 O6 2.835(13) 2_665 ? Pb1 O1 3.240(15) 5_564 ? Pb1 S2 3.4529(18) 1_665 ? Pb1 Te2 3.5409(12) . ? Pb1 S1 3.695(3) 1_665 ? Pb1 Te1 3.7010(15) 4_664 ? Pb1 Te3 3.7412(15) . ? Pb2 O1 2.341(14) . ? Pb2 O5 2.426(14) . ? Pb2 O4 2.536(15) 3_665 ? Pb2 O3 2.619(14) 4_665 ? Pb2 O2 2.681(12) 4_665 ? Pb2 O6 2.909(14) 2_665 ? Pb2 O2 3.270(13) 5_565 ? Pb2 Te1 3.5554(11) . ? Pb2 S2 3.587(3) 4_665 ? Pb2 Te2 3.7247(16) 4_665 ? Pb2 Te3 3.7850(15) . ? Te1 O1 1.935(14) . ? Te1 O1 1.935(14) 2_655 ? Te1 O1 1.935(14) 3_665 ? Te1 O4 2.767(16) 2_655 ? Te1 O4 2.767(16) 3_665 ? Te1 O4 2.767(16) . ? Te1 O5 3.464(13) 2_655 ? Te1 O5 3.464(13) 3_665 ? Te1 O5 3.464(13) . ? Te2 O2 1.895(15) 3_665 ? Te2 O2 1.895(15) 2_655 ? Te2 O2 1.895(15) . ? Te2 O3 2.767(15) 2_655 ? Te2 O3 2.767(15) 3_665 ? Te2 O3 2.767(15) . ? Te2 O5 3.507(13) . ? Te2 O5 3.507(13) 3_665 ? Te2 O5 3.507(13) 2_655 ? Te3 O3 1.871(14) . ? Te3 O4 1.872(14) . ? Te3 O5 1.888(9) . ? Te3 O6 2.808(10) . ? Te3 O1 3.081(13) 4_664 ? Te3 O2 3.098(15) 4_665 ? Te3 O6 3.651(10) 3 ? Te3 S1 3.7161(16) . ? S1 O6 1.453(11) 3 ? S1 O6 1.453(11) . ? S1 O6 1.453(11) 2 ? S1 S2 2.031(9) . ? 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 O2 Pb1 O5 92.1(5) . . ? O2 Pb1 O3 71.2(5) . 3_665 ? O5 Pb1 O3 80.4(4) . 3_665 ? O2 Pb1 O4 77.5(5) . 4_664 ? O5 Pb1 O4 149.6(4) . 4_664 ? O3 Pb1 O4 121.4(5) 3_665 4_664 ? O2 Pb1 O1 75.1(4) . 4_664 ? O5 Pb1 O1 79.7(4) . 4_664 ? O3 Pb1 O1 139.9(5) 3_665 4_664 ? O4 Pb1 O1 70.1(4) 4_664 4_664 ? O2 Pb1 O6 144.9(4) . 2_665 ? O5 Pb1 O6 82.3(4) . 2_665 ? O3 Pb1 O6 73.7(4) 3_665 2_665 ? O4 Pb1 O6 122.1(4) 4_664 2_665 ? O1 Pb1 O6 136.6(4) 4_664 2_665 ? O2 Pb1 O1 121.5(5) . 5_564 ? O5 Pb1 O1 108.2(3) . 5_564 ? O3 Pb1 O1 163.3(4) 3_665 5_564 ? O4 Pb1 O1 57.2(4) 4_664 5_564 ? O1 Pb1 O1 56.8(6) 4_664 5_564 ? O6 Pb1 O1 92.9(3) 2_665 5_564 ? O2 Pb1 S2 114.1(3) . 1_665 ? O5 Pb1 S2 131.8(3) . 1_665 ? O3 Pb1 S2 71.8(3) 3_665 1_665 ? O4 Pb1 S2 77.9(4) 4_664 1_665 ? O1 Pb1 S2 144.0(3) 4_664 1_665 ? O6 Pb1 S2 52.7(3) 2_665 1_665 ? O1 Pb1 S2 92.2(3) 5_564 1_665 ? O2 Pb1 Te2 29.6(3) . . ? O5 Pb1 Te2 69.1(3) . . ? O3 Pb1 Te2 50.8(3) 3_665 . ? O4 Pb1 Te2 106.8(3) 4_664 . ? O1 Pb1 Te2 89.4(3) 4_664 . ? O6 Pb1 Te2 120.0(2) 2_665 . ? O1 Pb1 Te2 145.3(3) 5_564 . ? S2 Pb1 Te2 115.85(4) 1_665 . ? O2 Pb1 S1 132.5(3) . 1_665 ? O5 Pb1 S1 99.8(3) . 1_665 ? O3 Pb1 S1 65.9(3) 3_665 1_665 ? O4 Pb1 S1 108.2(3) 4_664 1_665 ? O1 Pb1 S1 152.1(3) 4_664 1_665 ? O6 Pb1 S1 20.8(3) 2_665 1_665 ? O1 Pb1 S1 98.0(3) 5_564 1_665 ? S2 Pb1 S1 32.80(15) 1_665 1_665 ? Te2 Pb1 S1 116.67(3) . 1_665 ? O2 Pb1 Te1 91.0(3) . 4_664 ? O5 Pb1 Te1 104.4(2) . 4_664 ? O3 Pb1 Te1 161.9(3) 3_665 4_664 ? O4 Pb1 Te1 48.3(3) 4_664 4_664 ? O1 Pb1 Te1 30.0(3) 4_664 4_664 ? O6 Pb1 Te1 124.0(2) 2_665 4_664 ? O1 Pb1 Te1 31.5(2) 5_564 4_664 ? S2 Pb1 Te1 114.24(8) 1_665 4_664 ? Te2 Pb1 Te1 113.99(4) . 4_664 ? S1 Pb1 Te1 128.80(4) 1_665 4_664 ? O2 Pb1 Te3 79.5(3) . . ? O5 Pb1 Te3 26.1(2) . . ? O3 Pb1 Te3 97.8(3) 3_665 . ? O4 Pb1 Te3 123.7(3) 4_664 . ? O1 Pb1 Te3 54.5(3) 4_664 . ? O6 Pb1 Te3 105.8(3) 2_665 . ? O1 Pb1 Te3 95.5(2) 5_564 . ? S2 Pb1 Te3 157.60(14) 1_665 . ? Te2 Pb1 Te3 66.69(4) . . ? S1 Pb1 Te3 124.96(11) 1_665 . ? Te1 Pb1 Te3 81.86(4) 4_664 . ? O1 Pb2 O5 90.9(5) . . ? O1 Pb2 O4 71.8(5) . 3_665 ? O5 Pb2 O4 80.4(4) . 3_665 ? O1 Pb2 O3 76.3(4) . 4_665 ? O5 Pb2 O3 146.5(4) . 4_665 ? O4 Pb2 O3 122.7(5) 3_665 4_665 ? O1 Pb2 O2 74.5(4) . 4_665 ? O5 Pb2 O2 78.2(4) . 4_665 ? O4 Pb2 O2 139.4(5) 3_665 4_665 ? O3 Pb2 O2 68.6(5) 4_665 4_665 ? O1 Pb2 O6 146.1(4) . 2_665 ? O5 Pb2 O6 80.9(4) . 2_665 ? O4 Pb2 O6 74.4(4) 3_665 2_665 ? O3 Pb2 O6 126.0(4) 4_665 2_665 ? O2 Pb2 O6 134.3(4) 4_665 2_665 ? O1 Pb2 O2 119.6(5) . 5_565 ? O5 Pb2 O2 106.7(3) . 5_565 ? O4 Pb2 O2 165.7(5) 3_665 5_565 ? O3 Pb2 O2 57.2(4) 4_665 5_565 ? O2 Pb2 O2 54.9(6) 4_665 5_565 ? O6 Pb2 O2 94.2(3) 2_665 5_565 ? O1 Pb2 Te1 30.3(3) . . ? O5 Pb2 Te1 67.8(3) . . ? O4 Pb2 Te1 50.7(4) 3_665 . ? O3 Pb2 Te1 106.4(3) 4_665 . ? O2 Pb2 Te1 89.1(3) 4_665 . ? O6 Pb2 Te1 119.3(2) 2_665 . ? O2 Pb2 Te1 143.3(3) 5_565 . ? O1 Pb2 S2 107.1(4) . 4_665 ? O5 Pb2 S2 144.2(3) . 4_665 ? O4 Pb2 S2 76.5(4) 3_665 4_665 ? O3 Pb2 S2 69.1(4) 4_665 4_665 ? O2 Pb2 S2 135.9(3) 4_665 4_665 ? O6 Pb2 S2 66.8(3) 2_665 4_665 ? O2 Pb2 S2 91.2(3) 5_565 4_665 ? Te1 Pb2 S2 114.57(5) . 4_665 ? O1 Pb2 Te2 89.9(4) . 4_665 ? O5 Pb2 Te2 102.3(2) . 4_665 ? O4 Pb2 Te2 161.6(3) 3_665 4_665 ? O3 Pb2 Te2 47.9(3) 4_665 4_665 ? O2 Pb2 Te2 29.0(3) 4_665 4_665 ? O6 Pb2 Te2 123.95(19) 2_665 4_665 ? O2 Pb2 Te2 30.6(3) 5_565 4_665 ? Te1 Pb2 Te2 113.06(4) . 4_665 ? S2 Pb2 Te2 108.28(9) 4_665 4_665 ? O1 Pb2 Te3 78.7(3) . . ? O5 Pb2 Te3 25.0(3) . . ? O4 Pb2 Te3 97.1(4) 3_665 . ? O3 Pb2 Te3 121.6(3) 4_665 . ? O2 Pb2 Te3 54.0(3) 4_665 . ? O6 Pb2 Te3 103.2(3) 2_665 . ? O2 Pb2 Te3 93.8(3) 5_565 . ? Te1 Pb2 Te3 65.77(4) . . ? S2 Pb2 Te3 169.13(12) 4_665 . ? Te2 Pb2 Te3 80.54(4) 4_665 . ? O1 Pb2 Pb1 57.0(4) . 6_655 ? O5 Pb2 Pb1 118.9(2) . 6_655 ? O4 Pb2 Pb1 42.7(3) 3_665 6_655 ? O3 Pb2 Pb1 80.0(3) 4_665 6_655 ? O2 Pb2 Pb1 127.1(3) 4_665 6_655 ? O6 Pb2 Pb1 98.5(2) 2_665 6_655 ? O2 Pb2 Pb1 134.0(2) 5_565 6_655 ? Te1 Pb2 Pb1 59.77(3) . 6_655 ? S2 Pb2 Pb1 55.15(5) 4_665 6_655 ? Te2 Pb2 Pb1 125.04(5) 4_665 6_655 ? Te3 Pb2 Pb1 125.28(4) . 6_655 ? O1 Te1 O1 94.7(5) . 2_655 ? O1 Te1 O1 94.7(5) . 3_665 ? O1 Te1 O1 94.7(5) 2_655 3_665 ? O1 Te1 O4 164.5(5) . 2_655 ? O1 Te1 O4 78.0(5) 2_655 2_655 ? O1 Te1 O4 72.6(5) 3_665 2_655 ? O1 Te1 O4 72.6(5) . 3_665 ? O1 Te1 O4 164.5(5) 2_655 3_665 ? O1 Te1 O4 78.0(5) 3_665 3_665 ? O4 Te1 O4 112.0(3) 2_655 3_665 ? O1 Te1 O4 78.0(5) . . ? O1 Te1 O4 72.6(5) 2_655 . ? O1 Te1 O4 164.5(5) 3_665 . ? O4 Te1 O4 112.0(3) 2_655 . ? O4 Te1 O4 112.0(3) 3_665 . ? O1 Te1 O5 138.5(5) . 2_655 ? O1 Te1 O5 71.8(5) 2_655 2_655 ? O1 Te1 O5 124.6(5) 3_665 2_655 ? O4 Te1 O5 52.2(3) 2_655 2_655 ? O4 Te1 O5 123.6(4) 3_665 2_655 ? O4 Te1 O5 60.6(3) . 2_655 ? O1 Te1 O5 124.6(5) . 3_665 ? O1 Te1 O5 138.5(4) 2_655 3_665 ? O1 Te1 O5 71.8(5) 3_665 3_665 ? O4 Te1 O5 60.6(3) 2_655 3_665 ? O4 Te1 O5 52.2(3) 3_665 3_665 ? O4 Te1 O5 123.6(4) . 3_665 ? O5 Te1 O5 84.0(3) 2_655 3_665 ? O1 Te1 O5 71.8(5) . . ? O1 Te1 O5 124.6(5) 2_655 . ? O1 Te1 O5 138.5(5) 3_665 . ? O4 Te1 O5 123.6(4) 2_655 . ? O4 Te1 O5 60.6(3) 3_665 . ? O4 Te1 O5 52.2(3) . . ? O5 Te1 O5 84.0(3) 2_655 . ? O5 Te1 O5 84.0(3) 3_665 . ? O1 Te1 Pb2 127.2(4) . 3_665 ? O1 Te1 Pb2 107.2(4) 2_655 3_665 ? O1 Te1 Pb2 37.6(4) 3_665 3_665 ? O4 Te1 Pb2 45.2(3) 2_655 3_665 ? O4 Te1 Pb2 75.3(3) 3_665 3_665 ? O4 Te1 Pb2 154.1(3) . 3_665 ? O5 Te1 Pb2 94.21(15) 2_655 3_665 ? O5 Te1 Pb2 40.4(2) 3_665 3_665 ? O5 Te1 Pb2 124.0(2) . 3_665 ? O2 Te2 O2 95.0(6) 3_665 2_655 ? O2 Te2 O2 95.0(6) 3_665 . ? O2 Te2 O2 95.0(6) 2_655 . ? O2 Te2 O3 73.6(5) 3_665 2_655 ? O2 Te2 O3 77.2(5) 2_655 2_655 ? O2 Te2 O3 165.2(5) . 2_655 ? O2 Te2 O3 77.2(5) 3_665 3_665 ? O2 Te2 O3 165.2(5) 2_655 3_665 ? O2 Te2 O3 73.6(5) . 3_665 ? O3 Te2 O3 111.7(3) 2_655 3_665 ? O2 Te2 O3 165.2(5) 3_665 . ? O2 Te2 O3 73.6(5) 2_655 . ? O2 Te2 O3 77.2(5) . . ? O3 Te2 O3 111.7(3) 2_655 . ? O3 Te2 O3 111.7(3) 3_665 . ? O2 Te2 O5 138.0(4) 3_665 . ? O2 Te2 O5 125.3(4) 2_655 . ? O2 Te2 O5 72.3(5) . . ? O3 Te2 O5 122.4(4) 2_655 . ? O3 Te2 O5 60.8(3) 3_665 . ? O3 Te2 O5 51.8(3) . . ? O2 Te2 O5 72.3(5) 3_665 3_665 ? O2 Te2 O5 138.0(4) 2_655 3_665 ? O2 Te2 O5 125.3(4) . 3_665 ? O3 Te2 O5 60.8(3) 2_655 3_665 ? O3 Te2 O5 51.8(3) 3_665 3_665 ? O3 Te2 O5 122.4(4) . 3_665 ? O5 Te2 O5 82.8(3) . 3_665 ? O2 Te2 O5 125.3(4) 3_665 2_655 ? O2 Te2 O5 72.3(5) 2_655 2_655 ? O2 Te2 O5 138.0(4) . 2_655 ? O3 Te2 O5 51.8(3) 2_655 2_655 ? O3 Te2 O5 122.4(4) 3_665 2_655 ? O3 Te2 O5 60.8(3) . 2_655 ? O5 Te2 O5 82.8(3) . 2_655 ? O5 Te2 O5 82.8(3) 3_665 2_655 ? O2 Te2 Pb1 37.8(4) 3_665 3_665 ? O2 Te2 Pb1 107.6(4) 2_655 3_665 ? O2 Te2 Pb1 127.4(4) . 3_665 ? O3 Te2 Pb1 46.3(3) 2_655 3_665 ? O3 Te2 Pb1 73.9(3) 3_665 3_665 ? O3 Te2 Pb1 154.2(3) . 3_665 ? O5 Te2 Pb1 122.55(18) . 3_665 ? O5 Te2 Pb1 40.4(2) 3_665 3_665 ? O5 Te2 Pb1 94.46(15) 2_655 3_665 ? O3 Te3 O4 99.3(4) . . ? O3 Te3 O5 97.3(7) . . ? O4 Te3 O5 96.9(7) . . ? O3 Te3 O6 87.3(6) . . ? O4 Te3 O6 89.4(6) . . ? O5 Te3 O6 171.5(4) . . ? O3 Te3 O1 72.1(5) . 4_664 ? O4 Te3 O1 168.9(6) . 4_664 ? O5 Te3 O1 77.7(5) . 4_664 ? O6 Te3 O1 97.0(4) . 4_664 ? O3 Te3 O2 169.4(5) . 4_665 ? O4 Te3 O2 73.3(6) . 4_665 ? O5 Te3 O2 76.4(5) . 4_665 ? O6 Te3 O2 100.1(4) . 4_665 ? O1 Te3 O2 114.1(2) 4_664 4_665 ? O3 Te3 O6 62.8(5) . 3 ? O4 Te3 O6 64.3(5) . 3 ? O5 Te3 O6 147.6(3) . 3 ? O6 Te3 O6 40.9(3) . 3 ? O1 Te3 O6 115.5(4) 4_664 3 ? O2 Te3 O6 118.5(4) 4_665 3 ? O3 Te3 S1 69.9(5) . . ? O4 Te3 S1 82.4(5) . . ? O5 Te3 S1 166.8(4) . . ? O6 Te3 S1 20.2(2) . . ? O1 Te3 S1 100.6(3) 4_664 . ? O2 Te3 S1 115.7(3) 4_665 . ? O6 Te3 S1 22.73(17) 3 . ? O3 Te3 Pb1 78.8(5) . . ? O4 Te3 Pb1 128.4(5) . . ? O5 Te3 Pb1 34.5(5) . . ? O6 Te3 Pb1 141.1(3) . . ? O1 Te3 Pb1 44.3(3) 4_664 . ? O2 Te3 Pb1 99.5(2) 4_665 . ? O6 Te3 Pb1 141.6(3) 3 . ? S1 Te3 Pb1 139.69(13) . . ? O3 Te3 Pb2 127.6(5) . . ? O4 Te3 Pb2 79.8(5) . . ? O5 Te3 Pb2 32.9(5) . . ? O6 Te3 Pb2 144.6(3) . . ? O1 Te3 Pb2 99.8(3) 4_664 . ? O2 Te3 Pb2 44.5(2) 4_665 . ? O6 Te3 Pb2 144.1(3) 3 . ? S1 Te3 Pb2 156.83(13) . . ? Pb1 Te3 Pb2 63.43(2) . . ? O6 S1 O6 110.6(7) 3 . ? O6 S1 O6 110.6(7) 3 2 ? O6 S1 O6 110.6(7) . 2 ? O6 S1 S2 108.3(7) 3 . ? O6 S1 S2 108.3(7) . . ? O6 S1 S2 108.3(7) 2 . ? O6 S1 Pb1 109.9(4) 3 1_445 ? O6 S1 Pb1 138.3(4) . 1_445 ? O6 S1 Pb1 44.0(7) 2 1_445 ? S2 S1 Pb1 67.04(11) . 1_445 ? O6 S1 Pb1 44.0(7) 3 2_655 ? O6 S1 Pb1 109.9(4) . 2_655 ? O6 S1 Pb1 138.3(4) 2 2_655 ? S2 S1 Pb1 67.04(11) . 2_655 ? Pb1 S1 Pb1 105.76(12) 1_445 2_655 ? O6 S1 Pb1 138.3(4) 3 3_565 ? O6 S1 Pb1 44.0(7) . 3_565 ? O6 S1 Pb1 109.9(4) 2 3_565 ? S2 S1 Pb1 67.04(11) . 3_565 ? Pb1 S1 Pb1 105.76(12) 1_445 3_565 ? Pb1 S1 Pb1 105.76(12) 2_655 3_565 ? O6 S1 Te3 76.1(4) 3 . ? O6 S1 Te3 41.9(4) . . ? O6 S1 Te3 148.0(7) 2 . ? S2 S1 Te3 98.33(12) . . ? Pb1 S1 Te3 165.2(2) 1_445 . ? Pb1 S1 Te3 68.61(3) 2_655 . ? Pb1 S1 Te3 64.38(3) 3_565 . ? O6 S1 Te3 41.9(4) 3 3 ? O6 S1 Te3 148.0(7) . 3 ? O6 S1 Te3 76.1(4) 2 3 ? S2 S1 Te3 98.33(12) . 3 ? Pb1 S1 Te3 68.61(3) 1_445 3 ? Pb1 S1 Te3 64.38(3) 2_655 3 ? Pb1 S1 Te3 165.2(2) 3_565 3 ? Te3 S1 Te3 117.94(6) . 3 ? O6 S1 Te3 148.0(7) 3 2 ? O6 S1 Te3 76.1(4) . 2 ? O6 S1 Te3 41.9(4) 2 2 ? S2 S1 Te3 98.33(12) . 2 ? Pb1 S1 Te3 64.38(3) 1_445 2 ? Pb1 S1 Te3 165.2(2) 2_655 2 ? Pb1 S1 Te3 68.61(3) 3_565 2 ? Te3 S1 Te3 117.94(6) . 2 ? Te3 S1 Te3 117.94(6) 3 2 ? O6 S1 Pb2 23.2(6) 3 2_655 ? O6 S1 Pb2 89.9(6) . 2_655 ? O6 S1 Pb2 110.8(7) 2 2_655 ? S2 S1 Pb2 126.91(8) . 2_655 ? Pb1 S1 Pb2 127.18(5) 1_445 2_655 ? Pb1 S1 Pb2 59.88(3) 2_655 2_655 ? Pb1 S1 Pb2 126.91(6) 3_565 2_655 ? Te3 S1 Pb2 62.94(6) . 2_655 ? Te3 S1 Pb2 59.37(6) 3 2_655 ? Te3 S1 Pb2 134.7(2) 2 2_655 ? O6 S1 Pb2 110.8(7) 3 3_565 ? O6 S1 Pb2 23.2(6) . 3_565 ? O6 S1 Pb2 89.9(6) 2 3_565 ? S2 S1 Pb2 126.91(8) . 3_565 ? Pb1 S1 Pb2 126.91(6) 1_445 3_565 ? Pb1 S1 Pb2 127.18(5) 2_655 3_565 ? Pb1 S1 Pb2 59.88(3) 3_565 3_565 ? Te3 S1 Pb2 59.37(6) . 3_565 ? Te3 S1 Pb2 134.7(2) 3 3_565 ? Te3 S1 Pb2 62.94(6) 2 3_565 ? Pb2 S1 Pb2 87.64(12) 2_655 3_565 ? S1 S2 Pb1 80.17(14) . 1_445 ? S1 S2 Pb1 80.17(14) . 3_565 ? Pb1 S2 Pb1 117.14(8) 1_445 3_565 ? S1 S2 Pb1 80.17(14) . 2_655 ? Pb1 S2 Pb1 117.14(8) 1_445 2_655 ? Pb1 S2 Pb1 117.14(8) 3_565 2_655 ? S1 S2 Pb2 111.04(12) . 6_544 ? Pb1 S2 Pb2 66.67(4) 1_445 6_544 ? Pb1 S2 Pb2 168.8(3) 3_565 6_544 ? Pb1 S2 Pb2 66.37(3) 2_655 6_544 ? S1 S2 Pb2 111.04(12) . 5_454 ? Pb1 S2 Pb2 66.37(3) 1_445 5_454 ? Pb1 S2 Pb2 66.67(4) 3_565 5_454 ? Pb1 S2 Pb2 168.8(3) 2_655 5_454 ? Pb2 S2 Pb2 107.86(13) 6_544 5_454 ? S1 S2 Pb2 111.04(12) . 4_664 ? Pb1 S2 Pb2 168.8(3) 1_445 4_664 ? Pb1 S2 Pb2 66.37(3) 3_565 4_664 ? Pb1 S2 Pb2 66.67(4) 2_655 4_664 ? Pb2 S2 Pb2 107.86(13) 6_544 4_664 ? Pb2 S2 Pb2 107.86(13) 5_454 4_664 ? S1 S2 Te3 55.05(9) . . ? Pb1 S2 Te3 135.2(2) 1_445 . ? Pb1 S2 Te3 57.91(7) 3_565 . ? Pb1 S2 Te3 61.88(7) 2_655 . ? Pb2 S2 Te3 127.90(6) 6_544 . ? Pb2 S2 Te3 124.16(6) 5_454 . ? Pb2 S2 Te3 56.03(4) 4_664 . ? S1 S2 Te3 55.05(9) . 3 ? Pb1 S2 Te3 61.88(7) 1_445 3 ? Pb1 S2 Te3 135.2(2) 3_565 3 ? Pb1 S2 Te3 57.91(7) 2_655 3 ? Pb2 S2 Te3 56.03(4) 6_544 3 ? Pb2 S2 Te3 127.90(6) 5_454 3 ? Pb2 S2 Te3 124.16(6) 4_664 3 ? Te3 S2 Te3 90.44(13) . 3 ? S1 S2 Te3 55.05(9) . 2 ? Pb1 S2 Te3 57.91(7) 1_445 2 ? Pb1 S2 Te3 61.88(7) 3_565 2 ? Pb1 S2 Te3 135.2(2) 2_655 2 ? Pb2 S2 Te3 124.16(6) 6_544 2 ? Pb2 S2 Te3 56.03(4) 5_454 2 ? Pb2 S2 Te3 127.90(6) 4_664 2 ? Te3 S2 Te3 90.44(13) . 2 ? Te3 S2 Te3 90.44(13) 3 2 ? Te1 O1 Pb2 112.2(6) . . ? Te1 O1 Pb1 106.9(6) . 4_665 ? Pb2 O1 Pb1 105.9(5) . 4_665 ? Te1 O1 Te3 152.1(6) . 4_665 ? Pb2 O1 Te3 90.1(4) . 4_665 ? Pb1 O1 Te3 81.3(4) 4_665 4_665 ? Te1 O1 Pb1 87.5(5) . 6_655 ? Pb2 O1 Pb1 85.8(4) . 6_655 ? Pb1 O1 Pb1 155.6(5) 4_665 6_655 ? Te3 O1 Pb1 77.3(3) 4_665 6_655 ? Te1 O1 Te3 74.6(4) . . ? Pb2 O1 Te3 66.7(3) . . ? Pb1 O1 Te3 66.9(3) 4_665 . ? Te3 O1 Te3 131.8(4) 4_665 . ? Pb1 O1 Te3 137.2(4) 6_655 . ? Te2 O2 Pb1 112.6(6) . . ? Te2 O2 Pb2 107.7(6) . 4_664 ? Pb1 O2 Pb2 104.5(5) . 4_664 ? Te2 O2 Te3 152.1(7) . 4_664 ? Pb1 O2 Te3 89.3(5) . 4_664 ? Pb2 O2 Te3 81.5(3) 4_664 4_664 ? Te2 O2 Pb2 88.1(4) . 6_654 ? Pb1 O2 Pb2 85.4(4) . 6_654 ? Pb2 O2 Pb2 155.6(5) 4_664 6_654 ? Te3 O2 Pb2 76.3(3) 4_664 6_654 ? Te2 O2 Te3 75.4(4) . . ? Pb1 O2 Te3 65.6(3) . . ? Pb2 O2 Te3 66.9(3) 4_664 . ? Te3 O2 Te3 131.3(4) 4_664 . ? Pb2 O2 Te3 136.6(4) 6_654 . ? Te3 O3 Pb1 138.8(7) . 2_655 ? Te3 O3 Pb2 118.3(6) . 4_664 ? Pb1 O3 Pb2 96.2(4) 2_655 4_664 ? Te3 O3 Te2 118.2(6) . . ? Pb1 O3 Te2 82.8(4) 2_655 . ? Pb2 O3 Te2 87.5(4) 4_664 . ? Te3 O3 Pb1 72.7(4) . . ? Pb1 O3 Pb1 143.5(5) 2_655 . ? Pb2 O3 Pb1 73.3(3) 4_664 . ? Te2 O3 Pb1 62.3(3) . . ? Te3 O4 Pb2 139.7(7) . 2_655 ? Te3 O4 Pb1 117.3(7) . 4_665 ? Pb2 O4 Pb1 96.4(5) 2_655 4_665 ? Te3 O4 Te1 117.3(7) . . ? Pb2 O4 Te1 84.1(5) 2_655 . ? Pb1 O4 Te1 86.5(4) 4_665 . ? Te3 O4 Pb2 72.2(4) . . ? Pb2 O4 Pb2 143.8(5) 2_655 . ? Pb1 O4 Pb2 71.9(3) 4_665 . ? Te1 O4 Pb2 61.5(3) . . ? Te3 O5 Pb2 122.1(7) . . ? Te3 O5 Pb1 119.4(7) . . ? Pb2 O5 Pb1 109.1(3) . . ? Te3 O5 Te1 91.6(4) . . ? Pb2 O5 Te1 71.8(4) . . ? Pb1 O5 Te1 136.3(4) . . ? Te3 O5 Te2 90.8(4) . . ? Pb2 O5 Te2 136.0(3) . . ? Pb1 O5 Te2 70.6(4) . . ? Te1 O5 Te2 79.6(2) . . ? Te3 O5 Te3 145.5(4) . 3_665 ? Pb2 O5 Te3 74.1(2) . 3_665 ? Pb1 O5 Te3 74.9(2) . 3_665 ? Te1 O5 Te3 63.14(16) . 3_665 ? Te2 O5 Te3 63.12(17) . 3_665 ? S1 O6 Te3 117.9(5) . . ? S1 O6 Pb1 115.2(9) . 3_565 ? Te3 O6 Pb1 88.8(3) . 3_565 ? S1 O6 Pb2 145.4(8) . 3_565 ? Te3 O6 Pb2 87.0(3) . 3_565 ? Pb1 O6 Pb2 87.1(3) 3_565 3_565 ? S1 O6 Te3 81.2(4) . 2 ? Te3 O6 Te3 160.7(4) . 2 ? Pb1 O6 Te3 79.1(3) 3_565 2 ? Pb2 O6 Te3 77.5(3) 3_565 2 ? _refine_diff_density_max 2.263 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.459 _shelx_res_file ; TITL northstarite ns17fc-P63.res created by SHELXL-2016/6 at 20:49:08 on 07-Jul-2019 CELL 0.71075 10.24950 10.24950 11.66770 90.00000 90.00000 120.00000 ZERR 2 0.00051 0.00051 0.00082 0.00000 0.00000 0.00000 LATT -1 SYMM -Y, +X-Y, +Z SYMM -X+Y, -X, +Z SYMM -X, -Y, .50+Z SYMM +Y, -X+Y, .50+Z SYMM +X-Y, +X, .50+Z SFAC O PB S TE UNIT 36 12 4 10 L.S. 20 CONN 12 3.0 PB1 CONN 12 3.0 PB2 CONN 10 3.0 Te1 CONN 10 3.0 Te2 CONN 10 3.0 Te3 FMAP 2 PLAN 8 ACTA SIZE 0.050 0.050 0.015 WGHT 0.035000 6.147000 FVAR 0.06806 PB1 2 0.661404 0.675161 0.303372 11.00000 0.02573 0.01795 = 0.01820 -0.00094 0.00101 0.01049 PB2 2 0.667364 0.679764 0.642461 11.00000 0.02653 0.01616 = 0.01943 0.00095 -0.00151 0.01077 TE1 4 0.666667 0.333333 0.663174 10.33333 0.01334 0.01334 = 0.01612 0.00000 0.00000 0.00667 TE2 4 0.666667 0.333333 0.280504 10.33333 0.01348 0.01348 = 0.02019 0.00000 0.00000 0.00674 TE3 4 0.357292 0.360160 0.473077 11.00000 0.01635 0.01799 = 0.01539 0.00120 0.00179 0.00863 S1 3 0.000000 0.000000 0.426933 10.33333 0.01861 0.01861 = 0.01725 0.00000 0.00000 0.00930 S2 3 0.000000 0.000000 0.252827 10.33333 0.02769 0.02769 = 0.03526 0.00000 0.00000 0.01385 O1 1 0.628063 0.470873 0.750709 11.00000 0.03427 0.01487 = 0.00762 -0.00593 -0.00557 0.01687 O2 1 0.626556 0.466799 0.195225 11.00000 0.00836 0.01754 = 0.02376 -0.00233 -0.00489 0.00213 O3 1 0.378470 0.254833 0.350205 11.00000 0.02149 0.01772 = 0.01955 -0.00259 -0.00304 0.01232 O4 1 0.377392 0.252400 0.594758 11.00000 0.02649 0.02597 = 0.01288 -0.00033 -0.00373 0.01158 O5 1 0.557618 0.522316 0.474705 11.00000 0.01397 0.02314 = 0.02513 -0.00913 -0.01048 0.00458 O6 1 0.047144 0.151823 0.466004 11.00000 0.03018 0.01858 = 0.02763 0.00112 0.00186 0.01217 HKLF 4 REM northstarite REM R1 = 0.0329 for 1476 Fo > 4sig(Fo) and 0.0363 for all 1621 data REM 94 parameters refined using 1 restraints END WGHT 0.0350 6.1467 REM Highest difference peak 2.263, deepest hole -1.100, 1-sigma level 0.459 Q1 1 0.0000 0.0000 0.0954 10.33333 0.05 2.26 Q2 1 0.0000 0.0000 0.3488 10.33333 0.05 2.24 Q3 1 0.2588 0.3553 0.4662 11.00000 0.05 1.92 Q4 1 0.5901 0.6469 0.3460 11.00000 0.05 1.79 Q5 1 0.6667 0.3333 0.0052 10.33333 0.05 1.73 Q6 1 0.2890 0.2730 0.4299 11.00000 0.05 1.67 Q7 1 0.6730 0.6143 0.5918 11.00000 0.05 1.64 Q8 1 0.5857 0.6486 0.2777 11.00000 0.05 1.63 ; _shelx_res_checksum 10197 _shelx_hkl_file ; 0 0 2 551.15 22.23 0 0 -2 392.03 16.61 0 0 2 604.74 24.21 0 0 2 372.43 15.99 0 0 -2 474.70 19.91 0 0 -2 500.36 19.77 1 -2 0 306.63 17.37 -2 1 0 508.21 21.59 -1 2 0 324.74 19.57 1 -2 0 347.54 20.40 1 1 0 490.42 21.64 -2 1 0 540.01 20.82 -1 -1 0 522.56 23.33 1 -2 0 508.50 21.84 2 -1 0 465.92 22.17 1 1 0 492.02 21.56 2 -1 0 488.95 20.04 -1 -1 0 593.61 25.75 -2 1 0 456.00 22.18 -1 -1 0 532.17 23.22 1 1 0 500.11 21.63 2 -1 0 581.38 22.17 -1 2 0 332.31 22.48 -1 2 0 591.87 26.72 0 -1 -2 34.15 0.91 1 -1 2 37.44 1.38 0 1 -2 19.77 2.34 0 1 2 35.22 0.67 -1 1 2 34.88 0.71 -1 0 -2 34.53 1.47 1 0 2 33.31 1.11 0 1 2 33.40 1.20 0 -1 -2 33.72 2.08 0 1 2 32.80 2.03 1 0 -2 27.41 0.92 -1 1 2 29.35 1.19 -1 0 -2 35.56 1.14 1 -1 2 37.40 1.54 1 0 2 33.29 1.40 1 -1 2 32.81 1.48 1 0 2 32.32 0.78 1 -1 -2 29.57 1.94 -1 1 -2 42.10 1.98 -1 1 2 32.52 0.81 -1 0 2 25.72 1.45 1 -1 -2 32.27 0.74 0 -1 2 36.31 1.60 -1 1 -2 36.71 1.32 0 -1 2 23.93 2.78 -1 0 2 35.09 1.34 -1 1 2 33.78 1.06 1 0 -2 23.57 2.12 0 1 -2 31.06 1.21 1 0 -2 34.80 1.27 0 1 -2 29.59 1.60 -1 1 -2 28.73 1.33 0 1 -2 36.81 2.14 -1 0 2 34.41 0.87 1 -2 -1 69.02 2.69 2 -1 -1 68.08 1.65 1 1 -1 60.06 2.62 -1 -1 -1 71.28 2.64 -1 2 -1 53.69 3.36 -1 2 -1 51.84 3.23 1 1 -1 60.00 2.73 1 1 1 64.34 3.22 -2 1 1 69.05 1.78 1 -2 1 73.12 3.70 -1 -1 -1 76.58 2.41 -1 -1 1 69.16 2.13 1 1 1 66.17 2.32 -1 2 -1 75.96 2.99 -1 2 -1 66.76 3.26 -1 2 -1 48.16 2.82 -1 -1 1 73.35 3.50 2 -1 -1 49.88 3.26 -1 2 1 52.04 2.92 -2 1 -1 64.25 2.19 1 -2 -1 61.12 3.60 2 -1 1 63.70 1.82 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18.64 1.01 2 -2 1 18.16 0.92 -2 2 -1 16.47 2.60 2 -2 -1 15.69 1.84 2 -2 -1 13.35 0.50 2 -2 1 13.03 2.32 -2 2 1 16.40 0.79 2 -2 -1 16.30 0.80 -2 2 1 12.06 2.75 2 0 1 15.57 0.80 0 0 3 7.17 0.61 0 0 -3 2.79 0.79 0 0 -3 7.08 0.58 0 0 -3 7.63 0.73 0 0 3 4.55 0.56 0 0 3 3.68 0.93 -2 1 2 11.42 1.61 1 1 2 14.99 0.55 1 1 2 15.59 0.79 1 1 -2 19.86 1.70 -1 -1 2 14.00 2.13 -1 2 2 17.37 2.03 -2 1 2 16.05 0.79 2 -1 2 15.48 1.32 -1 2 2 16.52 0.79 -1 2 2 15.22 0.66 -1 2 -2 19.98 1.94 1 -2 2 15.45 1.42 -1 -1 2 14.68 3.10 -2 1 2 16.39 1.24 1 1 2 17.00 1.23 1 -2 2 15.95 1.44 2 -1 2 15.54 0.89 1 0 -3 42.17 2.30 0 -1 -3 42.52 1.74 1 -1 -3 39.91 1.05 1 0 -3 41.48 2.21 1 0 -3 35.49 1.29 1 -1 -3 36.38 2.39 0 -1 -3 39.26 2.82 -1 1 -3 43.00 1.81 1 0 -3 39.90 1.69 -1 0 -3 42.92 2.78 0 1 -3 28.22 2.95 1 -1 3 44.95 2.73 -1 1 -3 46.88 2.13 -1 0 -3 40.32 1.55 1 -1 -3 41.18 1.11 -1 0 -3 44.81 1.44 -1 1 -3 36.71 1.79 1 0 3 42.71 1.94 1 -1 3 40.89 2.17 0 1 3 42.94 1.95 0 -1 3 46.03 1.89 1 0 3 42.39 1.63 0 1 -3 36.14 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9.72 5.67 3 5 -12 10.02 5.70 7 0 -12 0.30 1.98 7 -7 12 0.82 5.99 7 0 12 7.19 2.53 0 7 12 0.60 1.76 7 0 -12 0.11 2.04 7 0 -12 -1.22 1.98 0 7 -12 -3.06 4.82 -7 7 12 0.22 3.99 7 -7 12 -1.76 4.48 -7 7 -12 -0.44 4.04 2 3 -14 8.50 5.84 2 3 14 18.68 4.54 3 -5 14 45.43 7.01 -5 2 14 1.60 3.70 -3 5 -14 3.44 8.02 5 -2 14 22.05 6.07 -2 5 -14 0.78 4.53 3 2 -14 1.29 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 77886