data_dinilawiite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'dinilawiite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'Al2 H0 O29 Pb8 S5' _chemical_formula_weight 2335.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'I 2/a' _space_group_name_Hall '-I 2ya' _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' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.4100(5) _cell_length_b 9.2191(2) _cell_length_c 21.6980(15) _cell_angle_alpha 90 _cell_angle_beta 107.276(8) _cell_angle_gamma 90 _cell_volume 3325.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15974 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description blade _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 4.665 _exptl_crystal_F_000 3976 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 40.807 _shelx_estimated_absorpt_T_min 0.106 _shelx_estimated_absorpt_T_max 0.374 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 20577 _diffrn_reflns_av_unetI/netI 0.0510 _diffrn_reflns_av_R_equivalents 0.0969 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.229 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 3776 _reflns_number_gt 3190 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _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^)+(0.0138P)^2^+162.5000P] 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_number_reflns 3776 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.38846(2) 0.04138(5) 0.21318(2) 0.02356(11) Uani 1 1 d . . . . . Pb2 Pb 0.53271(2) 0.86153(5) 0.36788(2) 0.02428(11) Uani 1 1 d . . . . . Pb3 Pb 0.44757(2) 0.24663(5) 0.36527(2) 0.02559(12) Uani 1 1 d . . . . . Pb4 Pb 0.17866(3) 0.54986(5) 0.14015(2) 0.02957(12) Uani 1 1 d . . . . . Al1 Al 0.250000 0.250000 0.250000 0.0173(9) Uani 1 2 d S . P . . Al2 Al 0.500000 0.000000 0.500000 0.0225(10) Uani 1 2 d S . P . . S1 S 0.60556(15) 0.1689(3) 0.26977(15) 0.0229(6) Uani 1 1 d . . . . . S2 S 0.5982(2) 0.1238(4) 0.17857(18) 0.0433(9) Uani 1 1 d . . . . . O1 O 0.6725(5) 0.2698(9) 0.2956(5) 0.043(2) Uani 1 1 d . . . . . O2 O 0.6196(5) 0.0349(9) 0.3081(5) 0.035(2) Uani 1 1 d . . . . . O3 O 0.5296(5) 0.2385(10) 0.2702(5) 0.033(2) Uani 1 1 d . . . . . O4 O 0.4270(4) 0.0162(8) 0.3217(4) 0.0187(15) Uani 1 1 d . . . . . OH5 O 0.3563(4) 0.2729(8) 0.2462(4) 0.0199(16) Uani 1 1 d . . . . . OH6 O 0.2671(4) 0.0491(8) 0.2362(4) 0.0197(16) Uani 1 1 d . . . . . OH7 O 0.2024(4) 0.2885(8) 0.1600(3) 0.0201(16) Uani 1 1 d . . . . . OH8 O 0.4463(4) 0.9393(9) 0.5611(4) 0.0265(18) Uani 1 1 d . . . . . OH9 O 0.4605(5) 0.8417(9) 0.4425(4) 0.0258(17) Uani 1 1 d . . . . . OH10 O 0.4100(5) 0.1044(9) 0.4483(4) 0.0282(18) Uani 1 1 d . . . . . OW11 O 0.317(2) 0.689(4) 0.5654(14) 0.273(19) Uani 1 1 d . . . . . OW12 O 0.426(2) 0.566(2) 0.4875(13) 0.216(14) Uani 1 1 d . . . . . OW13 O 0.2262(15) 0.921(4) 0.484(3) 0.153(19) Uani 0.5 1 d . . P . . S S 0.250000 0.3128(11) 0.500000 0.209(10) Uani 1 2 d S T P . . O14 O 0.2481(15) 0.406(3) 0.4353(13) 0.169(9) Uiso 1 1 d . . . . . O15 O 0.298(3) 0.197(5) 0.534(2) 0.144(16) Uiso 0.5 1 d . . P . . O16 O 0.340(3) 0.294(5) 0.522(2) 0.141(15) Uiso 0.5 1 d . . P . . 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 0.0238(2) 0.0246(2) 0.0233(2) 0.00192(18) 0.00854(17) 0.00489(16) Pb2 0.02252(19) 0.0241(2) 0.0261(2) 0.00117(18) 0.00709(17) 0.00514(16) Pb3 0.0246(2) 0.0222(2) 0.0277(2) -0.00178(19) 0.00437(18) -0.00207(16) Pb4 0.0233(2) 0.0311(2) 0.0343(3) 0.0068(2) 0.00864(19) -0.00236(17) Al1 0.0123(18) 0.018(2) 0.019(2) 0.0054(19) 0.0010(17) 0.0025(16) Al2 0.020(2) 0.027(2) 0.018(2) 0.003(2) 0.0001(18) 0.0027(18) S1 0.0209(12) 0.0176(12) 0.0314(15) 0.0006(12) 0.0094(11) 0.0004(10) S2 0.050(2) 0.045(2) 0.0368(19) 0.0097(17) 0.0161(16) 0.0218(16) O1 0.029(4) 0.026(5) 0.068(7) 0.001(5) 0.007(5) -0.009(4) O2 0.050(5) 0.018(4) 0.041(5) 0.012(4) 0.019(4) 0.004(4) O3 0.022(4) 0.035(5) 0.048(6) -0.004(4) 0.018(4) 0.005(3) O4 0.015(3) 0.020(4) 0.019(4) 0.004(3) 0.002(3) 0.000(3) OH5 0.017(3) 0.017(3) 0.023(4) -0.001(3) 0.002(3) 0.002(3) OH6 0.012(3) 0.018(4) 0.026(4) 0.002(3) 0.002(3) 0.002(3) OH7 0.026(4) 0.020(4) 0.012(4) -0.003(3) 0.003(3) 0.006(3) OH8 0.022(4) 0.027(4) 0.030(5) 0.002(4) 0.007(3) 0.001(3) OH9 0.029(4) 0.024(4) 0.023(4) -0.002(4) 0.007(3) 0.000(3) OH10 0.025(4) 0.030(4) 0.027(4) 0.003(4) 0.005(3) 0.005(3) OW11 0.39(5) 0.30(4) 0.14(2) -0.08(3) 0.09(3) -0.12(4) OW12 0.39(4) 0.115(18) 0.16(2) 0.058(17) 0.11(3) -0.06(2) OW13 0.045(18) 0.10(2) 0.26(6) -0.04(3) -0.04(2) 0.008(15) S 0.292(18) 0.055(5) 0.43(3) 0.000 0.33(2) 0.000 _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 O4 2.260(7) . ? Pb1 OH6 2.312(7) . ? Pb1 OH5 2.371(7) . ? Pb1 O1 2.704(9) 4_545 ? Pb1 O3 3.011(8) . ? Pb1 O3 3.107(9) 4_545 ? Pb1 Al1 3.3603(4) . ? Pb1 O14 3.42(3) 7 ? Pb1 S1 3.452(3) 4_545 ? Pb1 Pb3 3.6760(7) . ? Pb1 OW11 3.74(4) 8_554 ? Pb1 Pb4 3.7959(7) 7 ? Pb2 O4 2.308(7) 1_565 ? Pb2 OH9 2.334(8) . ? Pb2 OH8 2.356(8) 5_676 ? Pb2 O2 2.773(9) 1_565 ? Pb2 O3 3.084(10) 4 ? Pb2 O16 3.09(5) 5_666 ? Pb2 S2 3.106(3) 4 ? Pb2 O15 3.13(4) 5_666 ? Pb2 Al2 3.3379(5) 1_565 ? Pb2 OH5 3.656(8) 4 ? Pb2 S1 3.688(3) 4 ? Pb2 Pb4 3.7227(6) 7_565 ? Pb3 O4 2.310(7) . ? Pb3 OH10 2.468(8) . ? Pb3 OH7 2.525(7) 7 ? Pb3 OH5 2.611(7) . ? Pb3 OH8 2.674(8) 5_666 ? Pb3 O3 2.836(9) . ? Pb3 Pb4 3.4872(6) 7 ? Pb3 Al2 3.6005(5) . ? Pb3 Al1 3.6025(5) . ? Pb3 S2 3.631(4) 4 ? Pb3 OW12 3.72(3) 5_666 ? Pb4 O4 2.313(7) 7 ? Pb4 OH7 2.461(7) . ? Pb4 OH10 2.516(8) 7 ? Pb4 OH6 2.724(8) 7 ? Pb4 OH9 2.740(8) 7_565 ? Pb4 O1 3.259(9) 4 ? Pb4 O2 3.358(9) 4 ? Pb4 S2 3.521(4) 6_565 ? Pb4 OW13 3.57(6) 7_565 ? Pb4 Al1 3.6204(5) . ? Pb4 Al2 3.6764(6) 3_454 ? Al1 OH5 1.889(7) 7 ? Al1 OH5 1.889(7) . ? Al1 OH6 1.914(7) 7 ? Al1 OH6 1.914(7) . ? Al1 OH7 1.915(7) . ? Al1 OH7 1.915(7) 7 ? Al2 OH10 1.896(8) 5_656 ? Al2 OH10 1.896(7) . ? Al2 OH9 1.910(8) 5_666 ? Al2 OH9 1.910(8) 1_545 ? Al2 OH8 1.918(8) 5_666 ? Al2 OH8 1.918(8) 1_545 ? S1 O1 1.466(9) . ? S1 O2 1.468(8) . ? S1 O3 1.473(8) . ? S1 S2 1.989(5) . ? OW13 OW13 0.90(6) 2_556 ? S O15 1.42(5) 2_556 ? S O15 1.42(5) . ? S O16 1.50(4) . ? S O16 1.50(4) 2_556 ? S O14 1.64(3) 2_556 ? S O14 1.64(3) . ? O15 O16 1.23(6) . ? 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 O4 Pb1 OH6 77.7(2) . . ? O4 Pb1 OH5 78.6(3) . . ? OH6 Pb1 OH5 66.1(2) . . ? O4 Pb1 O1 88.1(3) . 4_545 ? OH6 Pb1 O1 71.3(3) . 4_545 ? OH5 Pb1 O1 137.1(3) . 4_545 ? O4 Pb1 O3 71.3(3) . . ? OH6 Pb1 O3 125.4(2) . . ? OH5 Pb1 O3 64.5(2) . . ? O1 Pb1 O3 147.5(3) 4_545 . ? O4 Pb1 O3 78.6(3) . 4_545 ? OH6 Pb1 O3 114.9(2) . 4_545 ? OH5 Pb1 O3 156.3(2) . 4_545 ? O1 Pb1 O3 48.2(2) 4_545 4_545 ? O3 Pb1 O3 101.78(8) . 4_545 ? O4 Pb1 Al1 79.84(18) . . ? OH6 Pb1 Al1 33.39(18) . . ? OH5 Pb1 Al1 33.12(17) . . ? O1 Pb1 Al1 104.64(19) 4_545 . ? O3 Pb1 Al1 96.43(15) . . ? O3 Pb1 Al1 145.48(16) 4_545 . ? O4 Pb1 O14 154.6(5) . 7 ? OH6 Pb1 O14 77.0(5) . 7 ? OH5 Pb1 O14 89.8(5) . 7 ? O1 Pb1 O14 85.3(5) 4_545 7 ? O3 Pb1 O14 123.7(5) . 7 ? O3 Pb1 O14 113.8(5) 4_545 7 ? Al1 Pb1 O14 78.2(4) . 7 ? O4 Pb1 S1 78.22(19) . 4_545 ? OH6 Pb1 S1 90.45(18) . 4_545 ? OH5 Pb1 S1 149.95(19) . 4_545 ? O1 Pb1 S1 23.82(18) 4_545 4_545 ? O3 Pb1 S1 124.16(17) . 4_545 ? O3 Pb1 S1 25.26(15) 4_545 4_545 ? Al1 Pb1 S1 123.01(5) . 4_545 ? O14 Pb1 S1 103.5(4) 7 4_545 ? O4 Pb1 Pb3 36.92(19) . . ? OH6 Pb1 Pb3 79.68(18) . . ? OH5 Pb1 Pb3 45.05(17) . . ? O1 Pb1 Pb3 122.7(2) 4_545 . ? O3 Pb1 Pb3 48.96(17) . . ? O3 Pb1 Pb3 111.22(17) 4_545 . ? Al1 Pb1 Pb3 61.398(11) . . ? O14 Pb1 Pb3 134.6(4) 7 . ? S1 Pb1 Pb3 115.11(5) 4_545 . ? O4 Pb1 OW11 139.0(5) . 8_554 ? OH6 Pb1 OW11 96.3(6) . 8_554 ? OH5 Pb1 OW11 136.3(5) . 8_554 ? O1 Pb1 OW11 52.3(6) 4_545 8_554 ? O3 Pb1 OW11 136.0(6) . 8_554 ? O3 Pb1 OW11 67.2(5) 4_545 8_554 ? Al1 Pb1 OW11 116.7(6) . 8_554 ? O14 Pb1 OW11 46.6(7) 7 8_554 ? S1 Pb1 OW11 61.2(5) 4_545 8_554 ? Pb3 Pb1 OW11 174.7(6) . 8_554 ? O4 Pb1 Pb4 34.34(17) . 7 ? OH6 Pb1 Pb4 45.36(18) . 7 ? OH5 Pb1 Pb4 77.71(19) . 7 ? O1 Pb1 Pb4 69.0(2) 4_545 7 ? O3 Pb1 Pb4 101.88(18) . 7 ? O3 Pb1 Pb4 87.08(17) 4_545 7 ? Al1 Pb1 Pb4 60.420(10) . 7 ? O14 Pb1 Pb4 121.3(4) 7 7 ? S1 Pb1 Pb4 72.35(5) 4_545 7 ? Pb3 Pb1 Pb4 55.614(12) . 7 ? OW11 Pb1 Pb4 119.1(6) 8_554 7 ? O4 Pb2 OH9 80.0(3) 1_565 . ? O4 Pb2 OH8 75.6(3) 1_565 5_676 ? OH9 Pb2 OH8 67.5(3) . 5_676 ? O4 Pb2 O2 85.2(3) 1_565 1_565 ? OH9 Pb2 O2 148.3(3) . 1_565 ? OH8 Pb2 O2 81.8(3) 5_676 1_565 ? O4 Pb2 O3 78.5(2) 1_565 4 ? OH9 Pb2 O3 122.6(2) . 4 ? OH8 Pb2 O3 149.8(3) 5_676 4 ? O2 Pb2 O3 80.8(2) 1_565 4 ? O4 Pb2 O16 157.0(9) 1_565 5_666 ? OH9 Pb2 O16 80.7(9) . 5_666 ? OH8 Pb2 O16 85.4(9) 5_676 5_666 ? O2 Pb2 O16 105.2(9) 1_565 5_666 ? O3 Pb2 O16 123.0(9) 4 5_666 ? O4 Pb2 S2 83.18(19) 1_565 4 ? OH9 Pb2 S2 71.1(2) . 4 ? OH8 Pb2 S2 135.9(2) 5_676 4 ? O2 Pb2 S2 134.8(2) 1_565 4 ? O3 Pb2 S2 54.06(17) 4 4 ? O16 Pb2 S2 102.3(9) 5_666 4 ? O4 Pb2 O15 150.5(9) 1_565 5_666 ? OH9 Pb2 O15 96.1(9) . 5_666 ? OH8 Pb2 O15 75.9(9) 5_676 5_666 ? O2 Pb2 O15 83.4(10) 1_565 5_666 ? O3 Pb2 O15 125.9(9) 4 5_666 ? O16 Pb2 O15 22.7(10) 5_666 5_666 ? S2 Pb2 O15 123.4(9) 4 5_666 ? O4 Pb2 Al2 79.60(19) 1_565 1_565 ? OH9 Pb2 Al2 33.84(19) . 1_565 ? OH8 Pb2 Al2 34.2(2) 5_676 1_565 ? O2 Pb2 Al2 115.93(19) 1_565 1_565 ? O3 Pb2 Al2 151.01(14) 4 1_565 ? O16 Pb2 Al2 77.4(9) 5_666 1_565 ? S2 Pb2 Al2 104.63(7) 4 1_565 ? O15 Pb2 Al2 81.2(9) 5_666 1_565 ? O4 Pb2 OH5 110.9(2) 1_565 4 ? OH9 Pb2 OH5 162.6(2) . 4 ? OH8 Pb2 OH5 127.4(2) 5_676 4 ? O2 Pb2 OH5 48.8(2) 1_565 4 ? O3 Pb2 OH5 50.50(18) 4 4 ? O16 Pb2 OH5 90.9(9) 5_666 4 ? S2 Pb2 OH5 96.15(13) 4 4 ? O15 Pb2 OH5 81.0(9) 5_666 4 ? Al2 Pb2 OH5 157.84(11) 1_565 4 ? O4 Pb2 S1 72.62(19) 1_565 4 ? OH9 Pb2 S1 99.66(19) . 4 ? OH8 Pb2 S1 147.42(18) 5_676 4 ? O2 Pb2 S1 102.4(2) 1_565 4 ? O3 Pb2 S1 22.99(15) 4 4 ? O16 Pb2 S1 123.3(9) 5_666 4 ? S2 Pb2 S1 32.63(8) 4 4 ? O15 Pb2 S1 136.5(9) 5_666 4 ? Al2 Pb2 S1 130.01(5) 1_565 4 ? OH5 Pb2 S1 72.13(12) 4 4 ? O4 Pb2 Pb4 36.37(18) 1_565 7_565 ? OH9 Pb2 Pb4 47.23(19) . 7_565 ? OH8 Pb2 Pb4 79.54(18) 5_676 7_565 ? O2 Pb2 Pb4 121.35(18) 1_565 7_565 ? O3 Pb2 Pb4 88.73(15) 4 7_565 ? O16 Pb2 Pb4 127.7(9) 5_666 7_565 ? S2 Pb2 Pb4 61.29(8) 4 7_565 ? O15 Pb2 Pb4 142.0(9) 5_666 7_565 ? Al2 Pb2 Pb4 62.477(12) 1_565 7_565 ? OH5 Pb2 Pb4 136.97(11) 4 7_565 ? S1 Pb2 Pb4 70.69(4) 4 7_565 ? O4 Pb3 OH10 76.6(3) . . ? O4 Pb3 OH7 76.7(2) . 7 ? OH10 Pb3 OH7 67.0(2) . 7 ? O4 Pb3 OH5 72.9(2) . . ? OH10 Pb3 OH5 123.8(2) . . ? OH7 Pb3 OH5 60.7(2) 7 . ? O4 Pb3 OH8 69.6(2) . 5_666 ? OH10 Pb3 OH8 60.6(2) . 5_666 ? OH7 Pb3 OH8 122.3(2) 7 5_666 ? OH5 Pb3 OH8 139.5(2) . 5_666 ? O4 Pb3 O3 74.2(3) . . ? OH10 Pb3 O3 144.7(3) . . ? OH7 Pb3 O3 123.4(2) 7 . ? OH5 Pb3 O3 64.7(2) . . ? OH8 Pb3 O3 90.6(2) 5_666 . ? O4 Pb3 Pb4 41.06(18) . 7 ? OH10 Pb3 Pb4 46.16(19) . 7 ? OH7 Pb3 Pb4 44.88(17) 7 7 ? OH5 Pb3 Pb4 81.21(16) . 7 ? OH8 Pb3 Pb4 80.47(17) 5_666 7 ? O3 Pb3 Pb4 113.77(18) . 7 ? O4 Pb3 Al2 73.90(18) . . ? OH10 Pb3 Al2 29.55(17) . . ? OH7 Pb3 Al2 95.26(17) 7 . ? OH5 Pb3 Al2 142.65(16) . . ? OH8 Pb3 Al2 31.39(17) 5_666 . ? O3 Pb3 Al2 120.84(17) . . ? Pb4 Pb3 Al2 62.466(12) 7 . ? O4 Pb3 Al1 73.98(16) . . ? OH10 Pb3 Al1 96.09(18) . . ? OH7 Pb3 Al1 30.44(16) 7 . ? OH5 Pb3 Al1 30.40(16) . . ? OH8 Pb3 Al1 140.19(17) 5_666 . ? O3 Pb3 Al1 94.49(17) . . ? Pb4 Pb3 Al1 61.390(10) 7 . ? Al2 Pb3 Al1 121.920(13) . . ? O4 Pb3 S2 141.12(18) . 4 ? OH10 Pb3 S2 128.0(2) . 4 ? OH7 Pb3 S2 86.18(18) 7 4 ? OH5 Pb3 S2 68.30(17) . 4 ? OH8 Pb3 S2 146.03(18) 5_666 4 ? O3 Pb3 S2 87.33(19) . 4 ? Pb4 Pb3 S2 130.90(6) 7 4 ? Al2 Pb3 S2 143.18(6) . 4 ? Al1 Pb3 S2 73.73(6) . 4 ? O4 Pb3 Pb1 35.99(18) . . ? OH10 Pb3 Pb1 108.5(2) . . ? OH7 Pb3 Pb1 75.15(16) 7 . ? OH5 Pb3 Pb1 39.98(16) . . ? OH8 Pb3 Pb1 99.57(18) 5_666 . ? O3 Pb3 Pb1 53.20(18) . . ? Pb4 Pb3 Pb1 63.935(14) 7 . ? Al2 Pb3 Pb1 109.858(14) . . ? Al1 Pb3 Pb1 54.979(10) . . ? S2 Pb3 Pb1 106.06(6) 4 . ? O4 Pb3 OW12 139.3(4) . 5_666 ? OH10 Pb3 OW12 80.6(4) . 5_666 ? OH7 Pb3 OW12 123.7(5) 7 5_666 ? OH5 Pb3 OW12 146.8(4) . 5_666 ? OH8 Pb3 OW12 70.0(4) 5_666 5_666 ? O3 Pb3 OW12 109.9(5) . 5_666 ? Pb4 Pb3 OW12 126.7(3) 7 5_666 ? Al2 Pb3 OW12 69.7(3) . 5_666 ? Al1 Pb3 OW12 142.2(5) . 5_666 ? S2 Pb3 OW12 78.9(4) 4 5_666 ? Pb1 Pb3 OW12 161.1(5) . 5_666 ? O4 Pb4 OH7 77.9(2) 7 . ? O4 Pb4 OH10 75.6(3) 7 7 ? OH7 Pb4 OH10 67.2(2) . 7 ? O4 Pb4 OH6 68.8(2) 7 7 ? OH7 Pb4 OH6 60.6(2) . 7 ? OH10 Pb4 OH6 121.1(2) 7 7 ? O4 Pb4 OH9 71.8(2) 7 7_565 ? OH7 Pb4 OH9 122.8(2) . 7_565 ? OH10 Pb4 OH9 58.9(2) 7 7_565 ? OH6 Pb4 OH9 138.4(2) 7 7_565 ? O4 Pb4 O1 128.8(3) 7 4 ? OH7 Pb4 O1 117.6(2) . 4 ? OH10 Pb4 O1 155.2(3) 7 4 ? OH6 Pb4 O1 77.8(2) 7 4 ? OH9 Pb4 O1 119.3(2) 7_565 4 ? O4 Pb4 O2 137.2(2) 7 4 ? OH7 Pb4 O2 78.3(2) . 4 ? OH10 Pb4 O2 125.2(2) 7 4 ? OH6 Pb4 O2 68.6(2) 7 4 ? OH9 Pb4 O2 150.2(2) 7_565 4 ? O1 Pb4 O2 42.5(2) 4 4 ? O4 Pb4 Pb3 41.00(18) 7 7 ? OH7 Pb4 Pb3 46.38(17) . 7 ? OH10 Pb4 Pb3 45.04(19) 7 7 ? OH6 Pb4 Pb3 78.55(15) 7 7 ? OH9 Pb4 Pb3 80.67(17) 7_565 7 ? O1 Pb4 Pb3 156.22(19) 4 7 ? O2 Pb4 Pb3 124.42(14) 4 7 ? O4 Pb4 S2 74.06(19) 7 6_565 ? OH7 Pb4 S2 148.57(18) . 6_565 ? OH10 Pb4 S2 117.79(19) 7 6_565 ? OH6 Pb4 S2 95.67(17) 7 6_565 ? OH9 Pb4 S2 60.45(17) 7_565 6_565 ? O1 Pb4 S2 71.88(16) 4 6_565 ? O2 Pb4 S2 113.95(15) 4 6_565 ? Pb3 Pb4 S2 112.75(6) 7 6_565 ? O4 Pb4 OW13 152.5(5) 7 7_565 ? OH7 Pb4 OW13 96.5(6) . 7_565 ? OH10 Pb4 OW13 77.4(5) 7 7_565 ? OH6 Pb4 OW13 131.8(5) 7 7_565 ? OH9 Pb4 OW13 89.8(5) 7_565 7_565 ? O1 Pb4 OW13 77.8(5) 4 7_565 ? O2 Pb4 OW13 65.3(5) 4 7_565 ? Pb3 Pb4 OW13 117.5(5) 7 7_565 ? S2 Pb4 OW13 114.9(5) 6_565 7_565 ? O4 Pb4 Al1 73.57(17) 7 . ? OH7 Pb4 Al1 29.59(16) . . ? OH10 Pb4 Al1 94.79(18) 7 . ? OH6 Pb4 Al1 31.24(15) 7 . ? OH9 Pb4 Al1 140.66(17) 7_565 . ? O1 Pb4 Al1 96.88(17) 4 . ? O2 Pb4 Al1 68.17(15) 4 . ? Pb3 Pb4 Al1 60.875(11) 7 . ? S2 Pb4 Al1 125.40(6) 6_565 . ? OW13 Pb4 Al1 114.2(5) 7_565 . ? O4 Pb4 Al2 72.27(17) 7 3_454 ? OH7 Pb4 Al2 94.53(16) . 3_454 ? OH10 Pb4 Al2 28.54(18) 7 3_454 ? OH6 Pb4 Al2 137.20(14) 7 3_454 ? OH9 Pb4 Al2 30.40(16) 7_565 3_454 ? O1 Pb4 Al2 143.26(18) 4 3_454 ? O2 Pb4 Al2 144.65(16) 4 3_454 ? Pb3 Pb4 Al2 60.276(10) 7 3_454 ? S2 Pb4 Al2 90.25(6) 6_565 3_454 ? OW13 Pb4 Al2 81.5(4) 7_565 3_454 ? Al1 Pb4 Al2 119.318(13) . 3_454 ? OH5 Al1 OH5 180.0 7 . ? OH5 Al1 OH6 84.3(3) 7 7 ? OH5 Al1 OH6 95.7(3) . 7 ? OH5 Al1 OH6 95.7(3) 7 . ? OH5 Al1 OH6 84.3(3) . . ? OH6 Al1 OH6 180.0 7 . ? OH5 Al1 OH7 86.1(3) 7 . ? OH5 Al1 OH7 93.9(3) . . ? OH6 Al1 OH7 86.6(3) 7 . ? OH6 Al1 OH7 93.4(3) . . ? OH5 Al1 OH7 93.9(3) 7 7 ? OH5 Al1 OH7 86.1(3) . 7 ? OH6 Al1 OH7 93.4(3) 7 7 ? OH6 Al1 OH7 86.6(3) . 7 ? OH7 Al1 OH7 180.0 . 7 ? OH5 Al1 Pb1 136.7(2) 7 . ? OH5 Al1 Pb1 43.3(2) . . ? OH6 Al1 Pb1 138.3(2) 7 . ? OH6 Al1 Pb1 41.7(2) . . ? OH7 Al1 Pb1 89.2(2) . . ? OH7 Al1 Pb1 90.8(2) 7 . ? OH5 Al1 Pb1 43.3(2) 7 7 ? OH5 Al1 Pb1 136.7(2) . 7 ? OH6 Al1 Pb1 41.7(2) 7 7 ? OH6 Al1 Pb1 138.3(2) . 7 ? OH7 Al1 Pb1 90.8(2) . 7 ? OH7 Al1 Pb1 89.2(2) 7 7 ? Pb1 Al1 Pb1 180.000(19) . 7 ? OH5 Al1 Pb3 135.6(2) 7 . ? OH5 Al1 Pb3 44.4(2) . . ? OH6 Al1 Pb3 93.5(2) 7 . ? OH6 Al1 Pb3 86.5(2) . . ? OH7 Al1 Pb3 138.1(2) . . ? OH7 Al1 Pb3 41.9(2) 7 . ? Pb1 Al1 Pb3 63.622(11) . . ? Pb1 Al1 Pb3 116.378(11) 7 . ? OH5 Al1 Pb3 44.4(2) 7 7 ? OH5 Al1 Pb3 135.6(2) . 7 ? OH6 Al1 Pb3 86.5(2) 7 7 ? OH6 Al1 Pb3 93.5(2) . 7 ? OH7 Al1 Pb3 41.9(2) . 7 ? OH7 Al1 Pb3 138.1(2) 7 7 ? Pb1 Al1 Pb3 116.379(11) . 7 ? Pb1 Al1 Pb3 63.621(11) 7 7 ? Pb3 Al1 Pb3 180.0 . 7 ? OH5 Al1 Pb4 88.0(2) 7 . ? OH5 Al1 Pb4 92.0(2) . . ? OH6 Al1 Pb4 47.6(2) 7 . ? OH6 Al1 Pb4 132.4(2) . . ? OH7 Al1 Pb4 39.4(2) . . ? OH7 Al1 Pb4 140.6(2) 7 . ? Pb1 Al1 Pb4 114.242(12) . . ? Pb1 Al1 Pb4 65.758(11) 7 . ? Pb3 Al1 Pb4 122.263(11) . . ? Pb3 Al1 Pb4 57.737(10) 7 . ? OH5 Al1 Pb4 92.0(2) 7 7 ? OH5 Al1 Pb4 88.0(2) . 7 ? OH6 Al1 Pb4 132.4(2) 7 7 ? OH6 Al1 Pb4 47.6(2) . 7 ? OH7 Al1 Pb4 140.6(2) . 7 ? OH7 Al1 Pb4 39.4(2) 7 7 ? Pb1 Al1 Pb4 65.758(11) . 7 ? Pb1 Al1 Pb4 114.242(11) 7 7 ? Pb3 Al1 Pb4 57.736(10) . 7 ? Pb3 Al1 Pb4 122.264(10) 7 7 ? Pb4 Al1 Pb4 180.0 . 7 ? OH10 Al2 OH10 180.0 5_656 . ? OH10 Al2 OH9 85.8(3) 5_656 5_666 ? OH10 Al2 OH9 94.2(3) . 5_666 ? OH10 Al2 OH9 94.2(3) 5_656 1_545 ? OH10 Al2 OH9 85.8(3) . 1_545 ? OH9 Al2 OH9 180.0 5_666 1_545 ? OH10 Al2 OH8 94.0(3) 5_656 5_666 ? OH10 Al2 OH8 86.0(3) . 5_666 ? OH9 Al2 OH8 94.2(3) 5_666 5_666 ? OH9 Al2 OH8 85.8(3) 1_545 5_666 ? OH10 Al2 OH8 86.0(3) 5_656 1_545 ? OH10 Al2 OH8 94.0(3) . 1_545 ? OH9 Al2 OH8 85.8(3) 5_666 1_545 ? OH9 Al2 OH8 94.2(3) 1_545 1_545 ? OH8 Al2 OH8 180.0 5_666 1_545 ? OH10 Al2 Pb2 89.6(3) 5_656 1_545 ? OH10 Al2 Pb2 90.4(3) . 1_545 ? OH9 Al2 Pb2 137.1(2) 5_666 1_545 ? OH9 Al2 Pb2 42.9(2) 1_545 1_545 ? OH8 Al2 Pb2 43.6(2) 5_666 1_545 ? OH8 Al2 Pb2 136.4(2) 1_545 1_545 ? OH10 Al2 Pb2 90.4(3) 5_656 5_666 ? OH10 Al2 Pb2 89.6(3) . 5_666 ? OH9 Al2 Pb2 42.9(2) 5_666 5_666 ? OH9 Al2 Pb2 137.1(2) 1_545 5_666 ? OH8 Al2 Pb2 136.4(2) 5_666 5_666 ? OH8 Al2 Pb2 43.6(2) 1_545 5_666 ? Pb2 Al2 Pb2 180.0 1_545 5_666 ? OH10 Al2 Pb3 140.1(3) 5_656 . ? OH10 Al2 Pb3 39.9(3) . . ? OH9 Al2 Pb3 90.2(2) 5_666 . ? OH9 Al2 Pb3 89.8(2) 1_545 . ? OH8 Al2 Pb3 46.6(2) 5_666 . ? OH8 Al2 Pb3 133.4(2) 1_545 . ? Pb2 Al2 Pb3 67.109(11) 1_545 . ? Pb2 Al2 Pb3 112.891(11) 5_666 . ? OH10 Al2 Pb3 39.9(3) 5_656 5_656 ? OH10 Al2 Pb3 140.1(3) . 5_656 ? OH9 Al2 Pb3 89.8(2) 5_666 5_656 ? OH9 Al2 Pb3 90.2(2) 1_545 5_656 ? OH8 Al2 Pb3 133.4(2) 5_666 5_656 ? OH8 Al2 Pb3 46.6(2) 1_545 5_656 ? Pb2 Al2 Pb3 112.892(11) 1_545 5_656 ? Pb2 Al2 Pb3 67.108(11) 5_666 5_656 ? Pb3 Al2 Pb3 180.0 . 5_656 ? OH10 Al2 Pb4 39.3(3) 5_656 3_545 ? OH10 Al2 Pb4 140.7(3) . 3_545 ? OH9 Al2 Pb4 46.5(2) 5_666 3_545 ? OH9 Al2 Pb4 133.5(2) 1_545 3_545 ? OH8 Al2 Pb4 93.9(2) 5_666 3_545 ? OH8 Al2 Pb4 86.1(2) 1_545 3_545 ? Pb2 Al2 Pb4 116.103(11) 1_545 3_545 ? Pb2 Al2 Pb4 63.897(11) 5_666 3_545 ? Pb3 Al2 Pb4 122.743(11) . 3_545 ? Pb3 Al2 Pb4 57.258(11) 5_656 3_545 ? OH10 Al2 Pb4 140.7(3) 5_656 7 ? OH10 Al2 Pb4 39.3(3) . 7 ? OH9 Al2 Pb4 133.5(2) 5_666 7 ? OH9 Al2 Pb4 46.5(2) 1_545 7 ? OH8 Al2 Pb4 86.1(2) 5_666 7 ? OH8 Al2 Pb4 93.9(2) 1_545 7 ? Pb2 Al2 Pb4 63.897(11) 1_545 7 ? Pb2 Al2 Pb4 116.103(11) 5_666 7 ? Pb3 Al2 Pb4 57.257(11) . 7 ? Pb3 Al2 Pb4 122.742(11) 5_656 7 ? Pb4 Al2 Pb4 180.0 3_545 7 ? O1 S1 O2 109.7(6) . . ? O1 S1 O3 109.5(5) . . ? O2 S1 O3 111.2(5) . . ? O1 S1 S2 108.8(5) . . ? O2 S1 S2 109.8(4) . . ? O3 S1 S2 107.8(4) . . ? O1 S1 Pb1 48.1(4) . 4 ? O2 S1 Pb1 141.4(4) . 4 ? O3 S1 Pb1 64.2(4) . 4 ? S2 S1 Pb1 107.78(15) . 4 ? O1 S1 Pb2 105.0(4) . 4_545 ? O2 S1 Pb2 145.3(4) . 4_545 ? O3 S1 Pb2 54.8(4) . 4_545 ? S2 S1 Pb2 57.39(12) . 4_545 ? Pb1 S1 Pb2 66.38(5) 4 4_545 ? O1 S1 Pb1 157.2(4) . . ? O2 S1 Pb1 84.5(4) . . ? O3 S1 Pb1 47.7(4) . . ? S2 S1 Pb1 81.37(14) . . ? Pb1 S1 Pb1 109.76(7) 4 . ? Pb2 S1 Pb1 62.58(4) 4_545 . ? O1 S1 Pb4 56.0(4) . 4_545 ? O2 S1 Pb4 59.9(4) . 4_545 ? O3 S1 Pb4 149.9(4) . 4_545 ? S2 S1 Pb4 102.16(14) . 4_545 ? Pb1 S1 Pb4 103.63(7) 4 4_545 ? Pb2 S1 Pb4 148.61(8) 4_545 4_545 ? Pb1 S1 Pb4 143.58(8) . 4_545 ? O1 S1 Pb3 106.3(4) . . ? O2 S1 Pb3 83.2(4) . . ? O3 S1 Pb3 32.3(4) . . ? S2 S1 Pb3 135.03(15) . . ? Pb1 S1 Pb3 76.59(5) 4 . ? Pb2 S1 Pb3 87.08(5) 4_545 . ? Pb1 S1 Pb3 56.44(4) . . ? Pb4 S1 Pb3 120.68(8) 4_545 . ? O1 S1 Pb2 126.3(5) . 1_545 ? O2 S1 Pb2 28.6(4) . 1_545 ? O3 S1 Pb2 82.9(4) . 1_545 ? S2 S1 Pb2 116.62(16) . 1_545 ? Pb1 S1 Pb2 131.04(8) 4 1_545 ? Pb2 S1 Pb2 122.83(7) 4_545 1_545 ? Pb1 S1 Pb2 60.45(4) . 1_545 ? Pb4 S1 Pb2 86.75(6) 4_545 1_545 ? Pb3 S1 Pb2 57.86(4) . 1_545 ? O1 S1 Pb4 60.7(4) . 6_665 ? O2 S1 Pb4 148.0(4) . 6_665 ? O3 S1 Pb4 100.5(4) . 6_665 ? S2 S1 Pb4 54.36(14) . 6_665 ? Pb1 S1 Pb4 57.54(4) 4 6_665 ? Pb2 S1 Pb4 55.04(4) 4_545 6_665 ? Pb1 S1 Pb4 115.85(7) . 6_665 ? Pb4 S1 Pb4 94.04(6) 4_545 6_665 ? Pb3 S1 Pb4 128.31(7) . 6_665 ? Pb2 S1 Pb4 170.91(8) 1_545 6_665 ? S1 S2 Pb2 89.98(14) . 4_545 ? S1 S2 Pb4 98.32(17) . 6_665 ? Pb2 S2 Pb4 68.02(7) 4_545 6_665 ? S1 S2 Pb3 113.89(17) . 4_545 ? Pb2 S2 Pb3 120.51(12) 4_545 4_545 ? Pb4 S2 Pb3 145.90(11) 6_665 4_545 ? S1 S2 Pb1 69.29(13) . . ? Pb2 S2 Pb1 64.75(7) 4_545 . ? Pb4 S2 Pb1 130.85(9) 6_665 . ? Pb3 S2 Pb1 74.12(8) 4_545 . ? S1 S2 Pb1 47.21(12) . 4 ? Pb2 S2 Pb1 58.85(6) 4_545 4 ? Pb4 S2 Pb1 55.09(6) 6_665 4 ? Pb3 S2 Pb1 159.00(11) 4_545 4 ? Pb1 S2 Pb1 88.45(7) . 4 ? S1 O1 Pb1 108.0(4) . 4 ? S1 O1 Pb4 102.1(4) . 4_545 ? Pb1 O1 Pb4 148.4(3) 4 4_545 ? S1 O1 Pb4 99.6(5) . 6_665 ? Pb1 O1 Pb4 69.2(2) 4 6_665 ? Pb4 O1 Pb4 115.1(3) 4_545 6_665 ? S1 O2 Pb2 136.7(5) . 1_545 ? S1 O2 Pb4 97.8(4) . 4_545 ? Pb2 O2 Pb4 121.9(3) 1_545 4_545 ? S1 O2 Pb1 73.7(4) . . ? Pb2 O2 Pb1 68.84(19) 1_545 . ? Pb4 O2 Pb1 168.3(3) 4_545 . ? S1 O2 Pb3 75.8(3) . . ? Pb2 O2 Pb3 65.19(18) 1_545 . ? Pb4 O2 Pb3 132.1(3) 4_545 . ? Pb1 O2 Pb3 54.66(12) . . ? S1 O3 Pb3 131.6(5) . . ? S1 O3 Pb1 111.0(4) . . ? Pb3 O3 Pb1 77.8(2) . . ? S1 O3 Pb2 102.2(5) . 4_545 ? Pb3 O3 Pb2 126.1(3) . 4_545 ? Pb1 O3 Pb2 79.3(2) . 4_545 ? S1 O3 Pb1 90.6(4) . 4 ? Pb3 O3 Pb1 101.8(3) . 4 ? Pb1 O3 Pb1 151.7(3) . 4 ? Pb2 O3 Pb1 78.4(2) 4_545 4 ? S1 O3 Pb2 76.0(4) . 1_545 ? Pb3 O3 Pb2 64.85(18) . 1_545 ? Pb1 O3 Pb2 65.22(16) . 1_545 ? Pb2 O3 Pb2 140.1(3) 4_545 1_545 ? Pb1 O3 Pb2 140.7(3) 4 1_545 ? Pb1 O4 Pb2 117.9(3) . 1_545 ? Pb1 O4 Pb3 107.1(3) . . ? Pb2 O4 Pb3 112.6(3) 1_545 . ? Pb1 O4 Pb4 112.2(3) . 7 ? Pb2 O4 Pb4 107.4(3) 1_545 7 ? Pb3 O4 Pb4 97.9(3) . 7 ? Al1 OH5 Pb1 103.6(3) . . ? Al1 OH5 Pb3 105.2(3) . . ? Pb1 OH5 Pb3 95.0(2) . . ? Al1 OH5 O2 112.9(3) . 4 ? Pb1 OH5 O2 125.2(4) . 4 ? Pb3 OH5 O2 112.1(3) . 4 ? Al1 OH5 Pb2 140.9(3) . 4_545 ? Pb1 OH5 Pb2 77.1(2) . 4_545 ? Pb3 OH5 Pb2 113.7(2) . 4_545 ? O2 OH5 Pb2 48.8(2) 4 4_545 ? Al1 OH5 Pb4 64.0(2) . 7 ? Pb1 OH5 Pb4 67.15(17) . 7 ? Pb3 OH5 Pb4 58.90(14) . 7 ? O2 OH5 Pb4 166.8(3) 4 7 ? Pb2 OH5 Pb4 141.9(2) 4_545 7 ? Al1 OH5 Pb4 60.88(18) . . ? Pb1 OH5 Pb4 126.3(2) . . ? Pb3 OH5 Pb4 137.8(2) . . ? O2 OH5 Pb4 53.8(2) 4 . ? Pb2 OH5 Pb4 86.77(15) 4_545 . ? Pb4 OH5 Pb4 124.91(18) 7 . ? Al1 OH6 Pb1 105.0(3) . . ? Al1 OH6 Pb4 101.2(3) . 7 ? Pb1 OH6 Pb4 97.5(2) . 7 ? Al1 OH6 O1 165.4(4) . 4_545 ? Pb1 OH6 O1 60.6(2) . 4_545 ? Pb4 OH6 O1 83.9(3) 7 4_545 ? Al1 OH6 Pb3 64.74(19) . . ? Pb1 OH6 Pb3 65.44(15) . . ? Pb4 OH6 Pb3 59.27(13) 7 . ? O1 OH6 Pb3 107.7(2) 4_545 . ? Al1 OH7 Pb4 111.0(3) . . ? Al1 OH7 Pb3 107.7(3) . 7 ? Pb4 OH7 Pb3 88.7(2) . 7 ? Al1 OH7 Pb1 60.89(18) . . ? Pb4 OH7 Pb1 135.7(3) . . ? Pb3 OH7 Pb1 135.5(3) 7 . ? Al1 OH7 Pb1 59.75(19) . 7 ? Pb4 OH7 Pb1 69.27(16) . 7 ? Pb3 OH7 Pb1 65.99(16) 7 7 ? Pb1 OH7 Pb1 120.64(18) . 7 ? Al2 OH8 Pb2 102.2(3) 1_565 5_676 ? Al2 OH8 Pb3 102.0(3) 1_565 5_666 ? Pb2 OH8 Pb3 99.4(3) 5_676 5_666 ? Al2 OH8 Pb4 65.6(2) 1_565 3 ? Pb2 OH8 Pb4 65.35(17) 5_676 3 ? Pb3 OH8 Pb4 58.63(14) 5_666 3 ? Al2 OH9 Pb2 103.3(3) 1_565 . ? Al2 OH9 Pb4 103.0(3) 1_565 7_565 ? Pb2 OH9 Pb4 94.1(3) . 7_565 ? Al2 OH9 Pb3 62.2(2) 1_565 1_565 ? Pb2 OH9 Pb3 67.53(19) . 1_565 ? Pb4 OH9 Pb3 57.71(14) 7_565 1_565 ? Al2 OH9 Pb3 61.9(2) 1_565 5_666 ? Pb2 OH9 Pb3 126.6(3) . 5_666 ? Pb4 OH9 Pb3 138.1(3) 7_565 5_666 ? Pb3 OH9 Pb3 124.11(19) 1_565 5_666 ? Al2 OH10 Pb3 110.5(3) . . ? Al2 OH10 Pb4 112.1(4) . 7 ? Pb3 OH10 Pb4 88.8(3) . 7 ? Al2 OH10 Pb2 60.7(2) . 5_666 ? Pb3 OH10 Pb2 132.4(3) . 5_666 ? Pb4 OH10 Pb2 138.8(3) 7 5_666 ? Al2 OH10 Pb2 60.1(2) . 1_545 ? Pb3 OH10 Pb2 71.07(19) . 1_545 ? Pb4 OH10 Pb2 67.86(19) 7 1_545 ? Pb2 OH10 Pb2 120.81(19) 5_666 1_545 ? Pb1 OW11 Pb3 73.5(7) 8 5_666 ? Pb1 OW11 Pb4 94.6(6) 8 8_565 ? Pb3 OW11 Pb4 115.3(7) 5_666 8_565 ? Pb3 OW12 Pb3 138.9(9) 5_666 . ? OW13 OW13 Pb4 92(7) 2_556 7_565 ? OW13 OW13 Pb4 74(8) 2_556 8_565 ? Pb4 OW13 Pb4 163.7(8) 7_565 8_565 ? OW13 OW13 Pb2 150.5(10) 2_556 6_575 ? Pb4 OW13 Pb2 88.7(11) 7_565 6_575 ? Pb4 OW13 Pb2 99.3(9) 8_565 6_575 ? O15 S O15 83(4) 2_556 . ? O15 S O16 119(3) 2_556 . ? O15 S O16 49(2) . . ? O15 S O16 49(2) 2_556 2_556 ? O15 S O16 119(3) . 2_556 ? O16 S O16 167(4) . 2_556 ? O15 S O14 134(2) 2_556 2_556 ? O15 S O14 95(2) . 2_556 ? O16 S O14 92(2) . 2_556 ? O16 S O14 95(2) 2_556 2_556 ? O15 S O14 95(2) 2_556 . ? O15 S O14 134(2) . . ? O16 S O14 95(2) . . ? O16 S O14 92(2) 2_556 . ? O14 S O14 117.0(19) 2_556 . ? O15 S Pb2 27.2(19) 2_556 6_565 ? O15 S Pb2 109.3(19) . 6_565 ? O16 S Pb2 142.4(19) . 6_565 ? O16 S Pb2 28.7(19) 2_556 6_565 ? O14 S Pb2 123.6(9) 2_556 6_565 ? O14 S Pb2 80.5(9) . 6_565 ? O15 S Pb2 109.3(19) 2_556 5_666 ? O15 S Pb2 27.2(19) . 5_666 ? O16 S Pb2 28.7(19) . 5_666 ? O16 S Pb2 142.4(19) 2_556 5_666 ? O14 S Pb2 80.5(9) 2_556 5_666 ? O14 S Pb2 123.6(9) . 5_666 ? Pb2 S Pb2 136.3(2) 6_565 5_666 ? S O14 Pb1 135.5(12) . 7 ? O16 O15 S 69(3) . . ? O16 O15 Pb2 77(3) . 5_666 ? S O15 Pb2 141(3) . 5_666 ? O15 O16 S 62(3) . . ? O15 O16 Pb2 80(3) . 5_666 ? S O16 Pb2 138(3) . 5_666 ? _refine_diff_density_max 3.991 _refine_diff_density_min -1.621 _refine_diff_density_rms 0.386 _shelx_res_file ; TITL dinilawiite R23.res created by SHELXL-2016/6 at 13:38:43 on 13-Jun-2023 CELL 0.71075 17.41000 9.21914 21.69800 90.00000 107.27600 90.00000 ZERR 4 0.00054 0.00023 0.00152 0.00000 0.00750 0.00000 LATT 2 SYMM .50-X, +Y, -Z SFAC AL H O PB S UNIT 8 0 116 32 20 L.S. 20 omit -2 0 10 omit -10 6 18 omit -3 5 22 CONN 12 3.0 PB1 CONN 12 3.0 PB2 CONN 12 3.0 PB3 CONN 12 3.0 PB4 EQIV $1 -x+1, y+1/2, -z+1/2 EQIV $2 -x+1, y-1/2, -z+1/2 BIND OH5 O2_$1 BIND OH6 O1_$2 FMAP 2 PLAN 20 ACTA SIZE 0.100 0.050 0.030 WGHT 0.013800 162.500000 FVAR 0.06595 PB1 4 0.388456 0.041376 0.213181 11.00000 0.02375 0.02463 = 0.02331 0.00192 0.00854 0.00489 PB2 4 0.532711 0.861528 0.367884 11.00000 0.02252 0.02413 = 0.02610 0.00117 0.00709 0.00514 PB3 4 0.447567 0.246629 0.365274 11.00000 0.02464 0.02224 = 0.02769 -0.00178 0.00437 -0.00207 PB4 4 0.178661 0.549858 0.140154 11.00000 0.02327 0.03115 = 0.03434 0.00678 0.00864 -0.00236 AL1 1 0.250000 0.250000 0.250000 10.50000 0.01230 0.01780 = 0.01929 0.00536 0.00102 0.00246 AL2 1 0.500000 0.000000 0.500000 10.50000 0.01958 0.02660 = 0.01791 0.00337 0.00013 0.00266 S1 5 0.605559 0.168893 0.269774 11.00000 0.02086 0.01761 = 0.03142 0.00063 0.00942 0.00044 S2 5 0.598224 0.123845 0.178566 11.00000 0.05041 0.04454 = 0.03683 0.00974 0.01607 0.02180 O1 3 0.672506 0.269769 0.295647 11.00000 0.02859 0.02634 = 0.06812 0.00094 0.00741 -0.00874 O2 3 0.619559 0.034915 0.308058 11.00000 0.04955 0.01750 = 0.04057 0.01193 0.01932 0.00397 O3 3 0.529564 0.238541 0.270234 11.00000 0.02230 0.03490 = 0.04775 -0.00368 0.01838 0.00477 O4 3 0.427047 0.016159 0.321676 11.00000 0.01511 0.02027 = 0.01904 0.00396 0.00247 0.00041 OH5 3 0.356326 0.272905 0.246207 11.00000 0.01746 0.01717 = 0.02281 -0.00074 0.00245 0.00239 OH6 3 0.267084 0.049069 0.236152 11.00000 0.01245 0.01771 = 0.02629 0.00188 0.00186 0.00188 OH7 3 0.202434 0.288459 0.159951 11.00000 0.02577 0.02029 = 0.01238 -0.00290 0.00299 0.00581 OH8 3 0.446321 0.939279 0.561054 11.00000 0.02194 0.02675 = 0.03027 0.00190 0.00708 0.00135 OH9 3 0.460511 0.841741 0.442525 11.00000 0.02911 0.02412 = 0.02337 -0.00220 0.00658 0.00032 OH10 3 0.410026 0.104379 0.448293 11.00000 0.02538 0.02984 = 0.02727 0.00306 0.00468 0.00496 OW11 3 0.316880 0.689347 0.565372 11.00000 0.38974 0.30132 = 0.13902 -0.07724 0.09479 -0.12086 OW12 3 0.426338 0.566044 0.487494 11.00000 0.39103 0.11537 = 0.16095 0.05800 0.10940 -0.05933 OW13 3 0.226208 0.921282 0.484417 10.50000 0.04474 0.09727 = 0.26076 -0.03504 -0.04164 0.00845 S 5 0.250000 0.312847 0.500000 10.50000 0.29186 0.05524 = 0.42575 0.00000 0.33164 0.00000 O14 3 0.248145 0.405606 0.435316 11.00000 0.16898 O15 3 0.298190 0.197044 0.533909 10.50000 0.14441 O16 3 0.339735 0.294196 0.522121 10.50000 0.14101 HKLF 4 REM dinilawiite REM R1 = 0.0363 for 3190 Fo > 4sig(Fo) and 0.0474 for all 3776 data REM 201 parameters refined using 0 restraints END WGHT 0.0138 162.4388 REM Highest difference peak 3.991, deepest hole -1.621, 1-sigma level 0.386 Q1 1 0.1990 0.5792 0.1788 11.00000 0.05 3.99 Q2 1 0.2087 0.3742 0.4787 11.00000 0.05 2.05 Q3 1 0.4234 0.2383 0.3868 11.00000 0.05 1.89 Q4 1 0.3995 0.0411 0.1803 11.00000 0.05 1.67 Q5 1 0.3032 0.2807 0.5602 11.00000 0.05 1.50 Q6 1 0.3728 -0.0444 0.2033 11.00000 0.05 1.50 Q7 1 0.4840 0.2460 0.3515 11.00000 0.05 1.45 Q8 1 0.4598 0.7128 0.4482 11.00000 0.05 1.45 Q9 1 0.3646 0.1603 0.1969 11.00000 0.05 1.40 Q10 1 0.3645 0.0651 0.2327 11.00000 0.05 1.38 Q11 1 0.5417 0.7805 0.4262 11.00000 0.05 1.37 Q12 1 0.5267 0.7701 0.3108 11.00000 0.05 1.34 Q13 1 0.1879 0.4543 0.0922 11.00000 0.05 1.33 Q14 1 0.6042 0.1487 0.2276 11.00000 0.05 1.33 Q15 1 0.3156 0.7415 0.5559 11.00000 0.05 1.32 Q16 1 0.5648 0.8995 0.3418 11.00000 0.05 1.31 Q17 1 0.2252 -0.0323 0.2067 11.00000 0.05 1.31 Q18 1 0.3419 0.1037 0.2299 11.00000 0.05 1.30 Q19 1 0.3897 0.1552 0.2720 11.00000 0.05 1.29 Q20 1 0.4272 0.3238 0.4064 11.00000 0.05 1.29 ; _shelx_res_checksum 37517 _shelx_hkl_file ; -2 1 1 3747.29 97.55 -2 -1 1 2906.93 85.40 -2 -1 1 3145.36 86.24 2 -1 -1 3461.74 90.64 2 1 -1 2866.35 83.58 2 1 -1 3366.12 94.28 -1 1 -2 7.02 1.37 1 1 2 11.07 1.36 -1 -1 -2 14.99 2.15 1 -1 2 6.90 1.43 -3 0 1 5.31 1.40 -3 0 1 2.10 1.36 3 0 -1 1.56 2.05 1 0 3 7.90 0.91 -1 0 -3 5.70 0.91 -1 0 -3 8.96 1.17 1 0 3 5.60 1.12 2 0 2 879.86 15.63 -2 0 -2 877.65 16.47 -2 0 -2 836.61 15.26 2 0 2 876.06 15.18 2 1 1 1273.18 24.02 -2 1 -1 1229.05 23.31 2 -1 1 1202.42 23.51 -2 -1 -1 1314.58 28.94 2 1 1 1319.23 26.67 -2 1 -1 1301.47 26.37 2 -1 1 1280.84 26.12 -2 -1 -1 1229.38 24.14 0 1 3 945.69 13.80 0 1 -3 864.67 21.27 0 1 -3 847.21 20.62 0 -1 -3 888.00 12.78 0 -1 -3 891.50 21.28 0 1 3 861.21 18.19 -2 1 3 31.04 1.14 2 -1 -3 29.47 1.04 2 1 -3 35.15 2.17 -2 -1 3 29.86 1.25 2 1 -3 35.32 1.33 0 0 4 2809.75 78.73 0 0 -4 2826.28 81.73 0 0 4 2779.36 80.76 0 0 -4 2859.39 79.71 2 0 -4 647.27 12.70 -2 0 4 659.15 14.59 -3 0 3 8.34 1.65 3 0 -3 4.55 2.47 -3 0 3 3.62 2.46 -3 0 -1 2.89 1.43 -3 0 -1 1.81 2.08 3 0 1 5.68 1.40 3 0 1 0.51 1.45 3 1 -2 150.87 3.63 3 -1 -2 144.53 3.09 3 1 -2 138.71 4.15 -3 -1 2 146.21 3.37 -3 1 2 151.87 3.29 -3 -1 2 141.60 6.12 3 1 0 1428.83 31.57 3 -1 0 1371.76 31.10 3 1 0 1440.27 34.84 3 -1 0 1435.01 31.33 -3 -1 0 1388.03 31.23 -3 1 0 1508.34 35.14 -3 -1 0 1438.39 31.63 -3 1 0 1373.13 33.50 1 -1 -4 6.07 0.91 -1 -1 4 6.60 0.80 -1 -1 4 1.11 1.71 1 1 -4 5.81 2.82 -1 1 4 4.95 0.88 0 2 0 140.14 4.27 0 -2 0 141.05 3.52 0 -2 0 150.30 3.16 0 2 0 147.63 3.56 1 2 -1 27.03 2.26 1 2 -1 24.19 2.77 1 -2 -1 22.23 1.20 -1 -2 1 22.43 2.94 -1 -2 1 22.74 1.50 -1 2 1 25.29 1.79 -1 0 5 2.62 1.44 1 0 -5 7.37 1.54 4 0 -2 442.44 9.29 4 0 -2 466.62 10.20 -4 0 2 446.26 9.72 -4 0 2 435.80 9.40 1 2 1 334.95 8.85 1 2 1 329.10 5.34 -1 2 -1 314.75 6.31 -1 -2 -1 325.20 7.05 1 -2 1 316.19 6.77 -1 -2 -1 312.14 5.38 0 2 -2 317.51 5.31 0 2 -2 284.08 6.87 0 2 -2 294.81 7.03 0 -2 -2 290.14 4.40 0 -2 -2 299.09 7.30 0 2 2 294.45 7.15 2 -1 3 491.89 8.79 -2 1 -3 503.92 10.76 2 1 3 519.96 10.04 2 1 3 499.75 10.32 -2 -1 -3 521.41 8.85 -2 -1 -3 543.33 13.11 2 -1 3 523.55 13.60 -2 1 -3 547.36 9.10 -4 0 0 124.82 3.79 -4 0 0 124.02 3.70 4 0 0 113.51 3.75 4 0 0 112.96 3.66 -1 -1 -4 4.66 1.82 1 -1 4 6.18 0.57 1 -1 4 9.70 1.95 -1 1 -4 9.52 0.57 -1 1 -4 7.68 2.91 1 1 4 8.12 1.46 -1 -1 -4 6.77 1.43 1 1 4 6.95 1.73 3 1 -4 2187.90 54.17 3 1 -4 2078.70 58.02 -3 -1 4 1945.70 54.88 -3 -1 4 1971.66 49.26 3 -1 -4 1929.89 47.27 2 2 0 1370.88 31.56 2 -2 0 1332.66 30.30 2 2 0 1476.36 33.61 -2 -2 0 1341.82 34.84 -2 2 0 1459.87 33.99 -2 -2 0 1404.79 32.36 -2 2 2 3.57 1.35 2 -2 -2 1.56 1.41 2 2 -2 5.06 2.01 -2 -2 2 6.76 1.17 -2 -2 2 5.77 1.94 2 2 -2 4.21 1.24 -3 1 -2 2.04 1.22 3 1 2 5.36 1.46 -3 1 -2 3.69 1.86 3 -1 2 4.38 2.06 -3 -1 -2 6.66 1.50 -3 -1 -2 6.49 1.79 3 -1 2 2.34 1.86 3 1 2 3.51 1.75 3 0 -5 -1.84 1.65 -3 0 5 2.15 1.66 -4 1 1 254.89 6.40 -4 -1 1 273.75 6.88 -4 1 1 275.43 6.15 4 1 -1 286.69 8.71 4 -1 -1 260.22 6.01 4 1 -1 255.55 8.60 2 0 4 2870.61 83.89 -2 0 -4 3099.64 85.28 2 0 4 3058.27 87.52 -2 0 -4 2853.60 82.89 -1 -2 3 2968.75 77.52 -1 -2 3 2681.02 87.66 1 2 -3 2664.32 86.90 1 2 -3 3520.29 89.74 2 1 -5 213.66 6.13 -2 -1 5 194.33 7.96 2 -1 -5 204.63 4.79 -2 1 5 203.95 3.63 4 0 -4 401.51 9.53 -4 0 4 424.99 10.10 -4 0 4 415.73 9.63 3 0 3 0.66 2.17 -3 0 -3 -0.21 1.40 -3 0 -3 2.46 2.62 3 0 3 -0.80 2.46 -4 -1 3 3196.38 98.23 4 1 -3 3040.36 107.70 -4 -1 3 3114.34 103.58 -4 1 3 3607.81 112.11 4 1 -3 3480.34 106.34 0 1 -5 2742.46 96.51 0 -1 -5 2902.21 93.41 0 1 -5 2768.50 91.72 0 -1 -5 2727.83 76.08 0 1 5 2856.95 80.06 0 -1 5 3334.49 83.92 1 0 5 0.91 1.17 -1 0 -5 -0.46 1.23 1 0 5 -0.42 1.47 -1 0 -5 8.91 2.28 3 2 -1 1428.60 36.42 -3 2 1 1554.98 34.43 -3 -2 1 1356.53 35.23 -3 -2 1 1478.33 35.00 3 2 -1 1574.28 39.73 3 -2 -1 1475.34 33.26 -1 2 -3 646.52 18.56 1 2 3 646.44 14.94 -1 -2 -3 699.29 15.96 -1 -2 -3 571.29 10.22 1 2 3 704.93 10.20 -2 0 6 4312.34 158.25 2 0 -6 4154.78 152.41 -2 -2 -2 318.29 6.35 2 2 2 369.44 8.41 2 -2 2 352.11 8.38 -2 -2 -2 395.28 8.86 2 2 2 368.66 6.28 -2 2 -2 351.87 8.35 4 -1 1 2283.77 67.26 4 -1 1 2115.84 58.29 -4 -1 -1 2314.48 62.54 4 1 1 2317.73 61.74 -4 -1 -1 2234.86 60.98 -4 1 -1 2313.16 64.79 4 1 1 2289.65 63.13 -4 1 -1 2273.33 66.74 4 0 2 4546.53 162.10 -4 0 -2 4850.06 168.39 4 0 2 4632.34 164.10 -4 0 -2 4658.31 166.57 0 0 -6 1116.91 26.89 0 0 -6 1162.72 27.89 5 0 -1 16.31 2.34 -5 0 1 5.89 2.24 -5 0 1 4.93 2.41 5 0 -1 7.93 2.25 0 -2 -4 736.15 18.70 0 2 4 709.32 18.57 0 2 4 817.05 9.93 0 2 -4 689.40 21.88 0 2 -4 687.59 21.40 0 2 -4 877.04 10.67 2 2 -4 5678.73 280.33 2 -2 -4 7881.13 294.57 -2 -2 4 6446.78 263.78 -2 2 4 8671.29 324.93 -2 -2 4 5390.12 271.00 2 2 -4 8323.94 327.98 3 2 -3 102.96 2.94 3 2 -3 85.73 6.48 -3 -2 3 83.30 5.96 -3 -2 3 87.98 2.68 3 -2 -3 86.73 3.06 -5 0 3 3.89 2.14 -5 0 3 1.97 3.54 5 0 -3 3.32 2.27 5 0 -3 0.02 3.30 -3 -2 -1 21.14 2.36 3 2 1 17.22 2.30 -3 2 -1 17.35 2.10 3 2 1 10.19 1.84 -3 -2 -1 25.01 2.06 3 -2 1 15.03 2.18 -3 2 -1 15.86 1.83 1 -1 -6 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1148.97 53.13 5 2 -13 1203.69 56.11 -5 -2 13 994.14 33.91 11 0 -7 -1.65 4.82 11 0 -7 1.02 3.85 -11 0 7 -0.40 4.77 -11 0 7 -5.48 6.41 11 1 -6 112.98 13.11 -11 -1 6 143.61 10.45 11 1 -6 134.70 9.41 -11 1 6 149.93 13.28 -11 1 6 132.42 9.16 -11 -1 6 118.66 8.07 11 -1 -6 104.46 7.74 -1 0 -13 -2.66 3.33 1 0 13 1.04 3.83 -1 0 -13 0.45 2.99 8 4 0 242.57 14.93 -8 4 0 263.30 11.17 -8 4 0 247.29 14.97 8 -4 0 251.76 14.90 -8 -4 0 253.84 11.11 -8 -4 0 198.81 16.33 8 4 0 260.28 11.80 -10 -2 8 748.86 34.00 10 2 -8 780.22 30.25 10 2 -8 973.99 32.20 -10 -2 8 855.25 33.43 10 -2 -8 683.17 23.86 -10 2 8 819.22 41.35 -10 2 8 953.51 38.37 8 4 -6 2239.02 83.75 8 4 -6 1960.06 78.67 -8 -4 6 1790.35 73.62 -8 -4 6 1816.48 63.46 8 -4 -6 1775.44 58.11 -8 4 6 2277.38 70.25 11 1 -2 263.85 12.82 -11 1 2 295.17 13.98 -11 -1 2 291.46 14.14 -11 -1 2 295.82 12.99 11 -1 -2 273.78 14.07 11 -1 -2 252.52 12.62 11 1 -2 296.73 14.51 -11 1 2 303.65 12.91 11 0 -1 -5.35 4.09 11 0 -1 -7.43 4.48 -11 0 1 6.39 4.07 -11 0 1 -4.65 4.44 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729.11 29.97 -2 -6 2 686.24 22.44 -2 6 2 683.30 31.78 -3 -5 -6 1000.15 37.34 -3 -5 -6 807.71 23.32 -3 5 -6 928.01 33.65 3 5 6 1051.37 24.99 -3 5 -6 1005.47 24.41 3 5 6 866.07 33.44 -3 5 -6 947.44 34.78 -3 -1 -12 1416.09 55.26 3 1 12 1849.62 58.54 3 1 12 1415.19 58.36 -3 -1 -12 1913.41 62.69 -3 1 -12 1886.38 53.10 3 -1 12 1375.13 46.82 -3 1 -12 1455.25 64.29 3 -1 12 1793.38 63.61 -6 0 14 193.44 9.51 6 0 -14 157.10 14.22 1 6 -3 962.03 40.41 1 6 -3 1014.75 35.97 -1 6 3 1073.49 27.71 -1 6 3 1163.98 28.20 1 6 -3 1136.63 30.92 -1 6 3 955.72 35.52 4 -5 5 221.75 12.47 -4 -5 -5 217.20 7.22 -4 5 -5 268.45 12.16 -4 5 -5 262.01 7.08 4 5 5 302.26 9.64 4 5 5 258.25 12.48 -4 -5 -5 282.99 13.84 8 -2 6 188.24 9.76 -8 -2 -6 138.25 8.03 -8 2 -6 177.57 9.92 8 -2 6 134.64 10.49 8 2 6 164.08 11.08 -8 -2 -6 178.62 8.89 8 2 6 155.91 13.75 -8 2 -6 161.12 10.02 -7 4 9 203.46 6.36 7 4 -9 192.36 12.13 -7 -4 9 159.16 6.27 -7 -4 9 172.30 11.43 7 -4 -9 143.95 4.94 7 4 -9 208.07 7.73 -3 -4 11 461.78 21.25 3 4 -11 481.24 21.57 -3 -4 11 396.98 6.68 10 -1 3 1953.71 72.88 -10 1 -3 2182.84 75.23 10 -1 3 2083.97 75.23 -10 -1 -3 2180.11 87.14 10 1 3 1983.94 73.83 -10 1 -3 2088.55 77.16 -10 -1 -3 1934.98 83.95 10 1 3 2093.20 74.04 2 5 7 40.65 1.44 -2 -5 -7 42.26 10.34 -2 5 -7 43.63 5.78 -2 5 -7 39.51 2.05 -2 -5 -7 32.61 2.30 -2 5 -7 35.46 1.41 -2 5 -7 34.86 6.05 2 5 7 37.21 5.94 -11 -1 8 110.45 7.84 -11 -1 8 104.39 9.65 11 1 -8 109.67 8.38 11 1 -8 133.45 13.44 11 -1 -8 75.58 7.22 -11 1 8 106.39 12.93 -11 1 8 96.79 8.66 1 1 -14 9.13 4.00 -1 -1 14 -1.46 3.28 -1 1 14 9.11 3.35 1 -1 -14 3.03 2.97 1 1 -14 -0.79 4.43 1 -1 -14 2.54 2.73 -6 -4 10 2048.15 86.00 -6 4 10 2276.27 67.76 6 -4 -10 1734.86 48.97 6 4 -10 2171.75 90.81 -6 -4 10 1704.75 54.91 6 4 -10 2397.63 73.21 11 -2 -5 585.54 27.77 11 2 -5 667.71 32.50 -11 -2 5 642.75 27.41 -11 2 5 715.68 24.36 11 2 -5 605.97 23.86 -11 2 5 589.75 24.14 -11 -2 5 598.97 22.02 -8 -2 12 905.91 37.07 8 2 -12 1072.91 42.64 -8 -2 12 1074.75 42.77 -8 2 12 1131.11 41.05 8 -2 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-1 963.03 36.33 -3 -6 1 836.94 30.05 -3 -6 1 797.02 27.80 -3 6 1 854.25 32.22 3 6 -1 946.11 30.95 -3 6 1 804.70 28.75 -3 6 1 1004.78 27.48 -1 6 -3 608.07 21.35 1 6 3 680.46 20.80 -1 6 -3 668.23 22.36 -1 6 -3 649.69 23.57 1 6 3 664.67 19.76 1 6 3 597.47 23.08 -8 1 -7 65.25 6.58 8 1 7 52.69 9.04 8 -1 7 53.99 6.38 8 -1 7 43.13 4.86 8 1 7 58.83 5.71 -8 -1 -7 63.90 5.77 -8 1 -7 54.89 7.30 -8 -1 -7 57.08 5.65 9 -1 -12 336.17 19.24 -9 -1 12 367.28 20.30 -9 -1 12 415.36 17.90 9 1 -12 359.59 17.62 -9 1 12 383.61 17.77 -2 6 -2 513.85 22.01 2 6 2 475.75 18.34 -2 6 -2 446.91 22.49 -2 -6 -2 457.44 13.55 -2 -6 -2 475.97 19.47 2 6 2 518.60 14.60 -2 6 -2 503.17 14.92 -1 4 11 135.19 10.09 1 4 -11 158.08 11.27 1 4 -11 143.14 16.07 -9 4 3 11.68 3.92 9 -4 -3 8.89 5.83 -9 -4 3 17.71 5.23 -9 -4 3 7.85 4.38 9 4 -3 13.33 4.66 9 4 -3 18.15 7.22 -11 0 9 1.60 5.02 11 0 -9 0.44 4.04 -11 0 9 2.67 4.40 -3 4 -9 224.49 16.59 3 -4 9 171.38 12.34 -3 -4 -9 240.38 18.94 -3 -4 -9 170.46 5.20 3 4 9 249.85 6.80 3 4 9 199.66 15.94 5 -5 4 1063.78 48.01 5 5 4 1188.19 35.56 -5 -5 -4 907.07 29.37 5 5 4 1058.47 48.67 -5 -5 -4 1068.26 39.99 -5 5 -4 1100.26 37.79 -5 5 -4 1111.18 30.32 0 0 14 4625.84 216.31 0 0 -14 5758.89 288.38 0 0 -14 4787.07 247.10 7 -5 -2 2198.37 91.29 7 5 -2 2688.78 98.40 -7 -5 2 2088.47 87.93 7 5 -2 2512.52 108.57 -7 -5 2 2344.37 89.66 -7 5 2 2830.51 97.30 8 4 2 2013.37 75.04 -8 -4 -2 1680.51 66.45 8 -4 2 1971.42 83.47 -8 -4 -2 2029.24 73.86 -8 4 -2 2135.20 76.83 -8 4 -2 2016.13 76.04 8 4 2 2002.40 68.50 -8 1 13 136.66 7.75 8 1 -13 133.30 14.51 -8 -1 13 135.09 7.57 -8 -1 13 137.58 10.09 -8 -4 8 82.66 12.44 8 -4 -8 48.24 6.02 -8 -4 8 60.25 4.80 8 4 -8 95.68 8.63 8 4 -8 86.64 8.24 -8 4 8 76.01 6.77 -11 0 -1 0.92 4.16 -11 0 -1 -3.53 4.37 11 0 1 -3.51 4.57 11 0 1 -2.36 4.24 7 -5 -4 3.13 2.93 -7 5 4 7.83 2.90 -7 -5 4 5.15 3.43 7 5 -4 12.15 7.27 -7 -5 4 3.03 4.45 7 5 -4 4.59 5.77 1 5 8 331.45 16.95 -1 5 -8 343.09 16.57 -1 5 -8 365.71 24.00 0 6 4 335.15 14.53 0 6 -4 335.76 13.88 0 6 -4 381.14 9.87 0 6 -4 334.00 14.18 0 6 4 355.34 11.25 0 6 4 365.88 8.11 -7 2 13 18.83 5.63 -7 -2 13 18.96 3.47 7 -2 -13 14.00 3.37 7 2 -13 38.78 5.96 -7 -2 13 24.16 5.60 -10 3 7 278.96 15.30 10 -3 -7 273.77 10.75 10 3 -7 293.04 15.59 -10 -3 7 252.59 16.27 10 3 -7 327.93 19.21 -10 3 7 325.03 12.33 -10 -3 7 311.01 16.52 -2 6 4 248.78 7.59 -2 6 4 188.16 11.29 2 6 -4 202.73 10.84 -2 -6 4 190.82 7.76 2 6 -4 239.07 10.37 -2 -6 4 197.75 10.61 -2 6 4 212.95 5.98 -3 -6 3 90.98 5.88 -3 6 3 82.16 7.59 -3 6 3 106.56 4.23 -3 6 3 80.05 6.75 3 6 -3 108.55 5.62 -3 -6 3 103.91 10.26 3 6 -3 98.47 7.12 -9 4 5 157.42 10.27 -9 -4 5 127.99 7.87 -9 4 5 170.77 7.52 9 -4 -5 128.42 6.71 -9 -4 5 141.47 15.99 9 4 -5 157.43 8.68 9 4 -5 143.40 10.08 -3 6 -1 57.15 5.68 3 6 1 72.78 6.34 3 6 1 63.18 7.61 -3 -6 -1 71.37 4.86 -3 6 -1 78.34 5.39 -3 -6 -1 79.61 6.89 -3 6 -1 69.02 7.69 -6 -4 -6 1379.48 60.67 -6 4 -6 1225.01 45.45 6 4 6 1215.37 55.97 6 -4 6 1300.23 48.01 6 4 6 1423.64 38.78 -6 4 -6 1426.30 36.22 -8 3 -5 449.45 16.68 8 -3 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29.33 -1 5 -24 338.61 48.89 -1 5 -24 347.04 55.73 -12 -10 8 3.25 8.37 12 10 -8 1.07 16.75 -12 10 8 2.49 11.29 21 -2 1 8.88 11.12 -21 -2 -1 -17.37 10.55 21 2 1 4.21 9.80 11 -8 11 -2.24 11.71 11 8 11 -2.03 17.34 -11 8 -11 2.05 16.23 -11 -8 -11 -0.95 12.11 -16 -8 12 1.44 14.96 16 -8 -12 26.09 7.76 -16 -8 12 0.25 15.00 -11 9 16 8.68 13.08 -11 -9 16 4.29 12.76 22 -2 -4 -4.32 17.12 0 8 20 67.68 18.62 17 -5 -20 -1.23 9.03 -10 -2 -20 17.17 10.10 10 2 20 -2.51 8.92 10 -2 20 6.81 11.65 -11 2 -19 35.15 8.32 -11 -2 -19 18.80 12.85 11 2 19 27.97 11.50 11 -2 19 41.56 14.34 17 -4 9 108.49 21.24 -17 -4 -9 120.00 19.52 -7 11 -4 -0.48 9.01 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 3005