data_new21sua _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lead Antimony sulfide (5.08/3.93/11) ; _chemical_name_common boulangerite _chemical_melting_point ? _chemical_formula_moiety 'Pb5.08 Sb3.93 S11' _chemical_formula_sum 'Pb5 S11 Sb4' _chemical_formula_weight 1875.61 _chemical_special_details ; The non-integer number of atoms in the unit-cell is due to the occurrence of partially occupied sites and substitutional disorder. ; 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' '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 'P21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 21.554(4) _cell_length_b 23.454(4) _cell_length_c 8.079(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.76(1) _cell_angle_gamma 90.00 _cell_volume 4012.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour silver _exptl_crystal_size_max 1.2 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 6.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6320 _exptl_absorpt_coefficient_mu 48.217 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2986 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'program SADABS (Sheldrick 2008)' _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 'Bruker AXS X8 APEX2 CCD' _diffrn_measurement_method 'integration of the spots (Apex suite)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 118995 _diffrn_reflns_av_R_equivalents 0.1564 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 30.58 _reflns_number_total 12443 _reflns_number_gt 8495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex program suite (Bruker 2003)' _computing_cell_refinement 'Apex program suite (Bruker 2003' _computing_data_reduction 'SAINT (Bruker 2003)' _computing_structure_solution 'none' _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^)+(0.0537P)^2^+334.9155P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12443 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 A1 Pb 0.12228(5) 0.49872(4) 0.94540(18) 0.0228(2) Uani 1 1 d . . . A2 Pb 0.30804(4) 0.15950(4) 0.02589(18) 0.01893(19) Uani 1 1 d . . . A3 Pb 0.20558(4) 0.32436(3) 0.97843(18) 0.0205(2) Uani 1 1 d . . . A4 Sb 0.46610(8) 0.43755(7) 0.3338(3) 0.0215(4) Uani 1 1 d . . . A5A Pb 0.13286(13) 0.09657(11) 0.2035(5) 0.0225(5) Uiso 0.695(13) 1 d P . . A5B Sb 0.1285(5) 0.1030(5) 0.200(2) 0.0225(5) Uiso 0.305(13) 1 d P . . A6 Sb 0.37145(7) 0.30864(6) 0.3090(3) 0.0164(3) Uani 1 1 d . . . A7 Sb 0.05948(8) 0.23021(7) 0.8996(4) 0.0263(4) Uani 1 1 d . . . A8 Sb 0.48592(7) 0.12122(6) 0.3615(3) 0.0148(3) Uani 1 1 d . . . A9 Sb 0.29219(7) 0.45695(6) 0.2789(3) 0.0220(4) Uani 1 1 d . . . A1' Pb 0.11178(5) 0.49911(4) 0.42704(19) 0.0245(2) Uani 1 1 d . . . A2' Pb 0.30543(4) 0.15990(4) 0.52952(18) 0.01987(19) Uani 1 1 d . . . A3' Pb 0.20703(4) 0.32108(4) 0.4782(2) 0.0239(2) Uani 1 1 d . . . A4' Pb 0.45191(5) 0.42983(4) 0.84862(19) 0.0248(2) Uani 1 1 d . . . A5A' Pb 0.13455(16) 0.09449(16) 0.6919(6) 0.0239(6) Uiso 0.464(13) 1 d P . . A5B' Sb 0.1262(3) 0.1049(3) 0.6779(9) 0.0239(6) Uiso 0.536(13) 1 d P . . A6' Sb 0.38703(7) 0.28390(6) 0.8181(3) 0.0158(3) Uani 1 1 d . . . A7' Pb 0.03872(5) 0.23296(4) 0.3978(2) 0.0268(2) Uani 1 1 d . . . A8' Pb 0.48697(4) 0.13465(4) 0.86647(18) 0.01921(19) Uani 1 1 d . . . A9' Sb 0.28390(7) 0.46674(6) 0.7692(3) 0.0174(3) Uani 1 1 d . . . S1 S 0.0656(3) 0.0142(2) 0.8986(12) 0.0189(12) Uani 1 1 d . . . S2 S 0.1866(3) 0.4165(2) 0.2198(11) 0.0159(11) Uani 1 1 d . . . S3 S 0.2481(3) 0.0287(2) 0.0143(12) 0.0193(13) Uani 1 1 d . . . S4 S 0.0968(3) 0.2940(3) 0.1548(13) 0.0241(15) Uani 1 1 d . . . S5 S 0.1569(3) 0.1729(2) 0.9512(14) 0.0253(14) Uani 1 1 d . . . S6 S 0.3338(3) 0.3747(2) 0.0649(10) 0.0195(14) Uani 1 1 d . . . S7 S 0.4180(3) 0.2218(2) 0.0690(10) 0.0155(12) Uani 1 1 d . . . S8 S 0.0149(3) 0.4450(2) 0.1533(11) 0.0192(14) Uani 1 1 d . . . S9 S 0.3744(2) 0.0923(2) 0.3099(11) 0.0153(10) Uani 1 1 d . . . S10 S 0.2766(3) 0.2494(2) 0.2666(11) 0.0144(11) Uani 1 1 d . . . S11 S 0.0118(3) 0.1348(2) 0.1411(11) 0.0166(11) Uani 1 1 d . . . S1' S 0.0712(3) 0.0182(2) 0.4172(11) 0.0163(11) Uani 1 1 d . . . S2' S 0.1866(3) 0.4120(2) 0.7164(11) 0.0166(11) Uani 1 1 d . . . S3' S 0.2448(3) 0.0285(2) 0.4793(11) 0.0184(13) Uani 1 1 d . . . S4' S 0.0951(3) 0.2938(2) 0.6960(11) 0.0215(15) Uani 1 1 d . . . S5' S 0.1549(3) 0.1759(2) 0.4548(14) 0.0235(14) Uani 1 1 d . . . S6' S 0.3287(3) 0.3740(2) 0.5159(9) 0.0153(13) Uani 1 1 d . . . S7' S 0.4198(3) 0.2192(3) 0.6047(10) 0.0172(13) Uani 1 1 d . . . S8' S 0.0125(3) 0.4385(2) 0.6096(9) 0.0146(12) Uani 1 1 d . . . S9' S 0.3676(3) 0.0847(2) 0.8122(11) 0.0161(11) Uani 1 1 d . . . S10' S 0.2769(3) 0.2510(2) 0.7614(11) 0.0155(11) Uani 1 1 d . . . S11' S 0.0172(3) 0.1389(2) 0.6306(12) 0.0197(12) 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 A1 0.0302(5) 0.0160(4) 0.0233(6) -0.0030(5) 0.0081(5) -0.0029(3) A2 0.0192(4) 0.0181(3) 0.0202(5) 0.0011(5) 0.0057(5) -0.0013(3) A3 0.0206(4) 0.0185(4) 0.0231(6) 0.0006(5) 0.0062(5) 0.0018(3) A4 0.0200(8) 0.0153(6) 0.0291(12) -0.0018(7) 0.0042(8) -0.0024(5) A6 0.0172(6) 0.0124(6) 0.0195(9) 0.0016(7) 0.0032(8) 0.0001(5) A7 0.0187(7) 0.0188(7) 0.0435(12) 0.0135(9) 0.0110(10) 0.0025(6) A8 0.0200(7) 0.0084(5) 0.0173(9) -0.0009(7) 0.0071(8) -0.0010(5) A9 0.0155(7) 0.0181(7) 0.0320(11) -0.0006(9) 0.0033(9) 0.0001(5) A1' 0.0372(5) 0.0151(3) 0.0228(6) 0.0000(5) 0.0092(6) -0.0020(3) A2' 0.0218(4) 0.0176(3) 0.0211(5) -0.0001(5) 0.0062(5) -0.0015(3) A3' 0.0212(4) 0.0260(4) 0.0256(6) 0.0001(5) 0.0077(6) 0.0018(3) A4' 0.0267(5) 0.0183(4) 0.0295(6) 0.0020(5) 0.0053(5) 0.0018(3) A6' 0.0194(7) 0.0102(5) 0.0184(8) 0.0004(7) 0.0049(8) -0.0026(5) A7' 0.0276(5) 0.0159(4) 0.0359(6) -0.0011(5) 0.0032(6) -0.0023(3) A8' 0.0231(4) 0.0122(3) 0.0231(5) -0.0004(4) 0.0061(5) 0.0007(3) A9' 0.0155(7) 0.0171(6) 0.0206(9) -0.0002(8) 0.0061(8) 0.0012(5) S1 0.014(3) 0.020(2) 0.024(4) 0.001(3) 0.005(3) 0.0007(18) S2 0.015(2) 0.013(2) 0.020(3) -0.002(3) 0.005(3) -0.0022(17) S3 0.022(3) 0.013(2) 0.025(4) 0.005(3) 0.008(3) -0.001(2) S4 0.017(3) 0.024(3) 0.033(5) -0.003(3) 0.007(3) -0.009(2) S5 0.022(3) 0.010(2) 0.045(5) -0.001(3) 0.010(4) 0.0034(19) S6 0.022(3) 0.015(2) 0.022(4) 0.005(3) 0.006(3) 0.000(2) S7 0.018(3) 0.013(2) 0.016(3) 0.003(3) 0.004(3) -0.0028(18) S8 0.018(3) 0.013(2) 0.029(4) -0.001(3) 0.010(3) -0.0044(19) S9 0.012(2) 0.018(2) 0.015(3) 0.000(3) 0.002(3) 0.0025(18) S10 0.019(3) 0.011(2) 0.016(3) -0.002(3) 0.009(3) -0.0012(17) S11 0.021(3) 0.0107(19) 0.021(4) 0.003(3) 0.011(3) 0.0036(19) S1' 0.017(2) 0.016(2) 0.016(3) 0.005(3) 0.003(3) 0.0042(18) S2' 0.020(3) 0.015(2) 0.017(3) 0.001(3) 0.007(3) 0.0002(18) S3' 0.016(3) 0.018(2) 0.021(4) -0.004(3) 0.003(3) 0.000(2) S4' 0.026(3) 0.015(3) 0.024(5) 0.006(3) 0.006(3) -0.009(2) S5' 0.012(2) 0.019(2) 0.041(4) -0.008(4) 0.009(4) 0.0046(19) S6' 0.020(3) 0.013(2) 0.015(4) -0.003(2) 0.008(3) 0.0009(18) S7' 0.017(3) 0.020(2) 0.017(4) -0.002(3) 0.007(3) -0.001(2) S8' 0.019(3) 0.015(2) 0.011(3) 0.000(2) 0.004(3) -0.0018(19) S9' 0.020(3) 0.009(2) 0.020(3) 0.001(3) 0.008(3) 0.0045(17) S10' 0.020(3) 0.014(2) 0.015(3) 0.001(3) 0.008(3) 0.0017(18) S11' 0.018(3) 0.018(2) 0.025(4) 0.004(3) 0.008(3) 0.004(2) _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 A1 S9' 2.790(7) 2_557 ? A1 S3 2.840(6) 2_556 ? A1 S9 3.022(7) 2_556 ? A1 S2 3.067(7) 1_556 ? A2 S7 2.751(6) . ? A2 S9' 2.922(7) 1_554 ? A2 S9 2.927(7) . ? A2 S10' 3.014(7) 1_554 ? A2 S10 3.029(7) . ? A3 S2' 2.924(7) . ? A3 S6 2.967(6) 1_556 ? A3 S2 2.990(7) 1_556 ? A3 S4 3.046(8) 1_556 ? A3 S4' 3.060(8) . ? A3 S10' 3.067(7) . ? A3 S10 3.087(7) 1_556 ? A4 S1' 2.468(6) 4_665 ? A4 S1 2.598(8) 2_556 ? A4 S11 2.616(7) 4_665 ? A5A S11 2.716(6) . ? A5A S5' 2.730(9) . ? A5A S5 2.833(10) 1_554 ? A5A S1' 2.998(8) . ? A5B S11 2.580(13) . ? A5B S5' 2.653(17) . ? A5B S5 2.752(18) 1_554 ? A6 S10 2.443(5) . ? A6 S6 2.520(7) . ? A6 S6' 2.562(7) . ? A7 S4' 2.447(7) . ? A7 S5 2.461(6) . ? A7 S4 2.553(9) 1_556 ? A8 S8' 2.425(7) 4_665 ? A8 S8 2.453(7) 4_665 ? A8 S9 2.457(5) . ? A9 S2 2.430(6) . ? A9 S6' 2.741(7) . ? A9 S3' 2.802(8) 2_556 ? A9 S6 2.846(7) . ? A9 S3 2.904(8) 2 ? A1' S9' 2.877(7) 2_556 ? A1' S8' 3.019(6) 3_566 ? A1' S8 3.023(7) . ? A1' S9 3.025(7) 2_556 ? A1' S3' 3.120(6) 2_556 ? A2' S7' 2.796(6) . ? A2' S10 2.968(7) . ? A2' S9 2.976(7) . ? A2' S10' 2.980(7) . ? A2' S9' 2.997(7) . ? A3' S6' 2.866(6) . ? A3' S2' 2.960(7) . ? A3' S10' 2.987(7) . ? A3' S10 2.994(7) . ? A3' S2 3.037(7) . ? A4' S1 2.743(6) 4_665 ? A4' S11 2.899(8) 4_666 ? A4' S1 2.919(8) 2_557 ? A4' S11' 2.935(8) 4_665 ? A4' S1' 2.959(8) 2_556 ? A5A' S11' 2.694(7) . ? A5A' S5 2.762(10) . ? A5A' S5' 2.797(10) . ? A5A' S1' 2.978(8) . ? A5A' S1 3.077(8) . ? A5B' S11' 2.441(8) . ? A5B' S5' 2.612(11) . ? A5B' S5 2.705(11) . ? A6' S10' 2.457(6) . ? A6' S7 2.484(7) 1_556 ? A6' S7' 2.495(7) . ? A7' S5' 2.800(6) . ? A7' S4' 2.867(8) . ? A7' S4 2.896(9) . ? A7' S11' 2.990(7) . ? A7' S11 3.081(7) . ? A8' S9' 2.787(6) . ? A8' S8' 2.825(7) 4_665 ? A8' S8 2.949(8) 4_666 ? A8' S7' 3.060(7) . ? A9' S2' 2.428(6) . ? A9' S3' 2.459(8) 2_556 ? A9' S3 2.470(8) 2_556 ? S1 A4 2.598(8) 2_546 ? S1 A4' 2.743(6) 4_565 ? S1 A4' 2.919(8) 2_547 ? S2 A3 2.990(7) 1_554 ? S2 A1 3.067(7) 1_554 ? S3 A9' 2.470(8) 2_546 ? S3 A1 2.840(6) 2_546 ? S3 A9 2.904(8) 2_545 ? S4 A7 2.553(9) 1_554 ? S4 A3 3.046(8) 1_554 ? S5 A5B 2.752(18) 1_556 ? S5 A5A 2.833(10) 1_556 ? S6 A3 2.967(6) 1_554 ? S7 A6' 2.484(7) 1_554 ? S8 A8 2.453(7) 4_565 ? S8 A8' 2.949(8) 4_564 ? S9 A1 3.022(7) 2_546 ? S9 A1' 3.025(7) 2_546 ? S10 A3 3.087(7) 1_554 ? S11 A4 2.616(7) 4_565 ? S11 A4' 2.899(8) 4_564 ? S1' A4 2.468(6) 4_565 ? S1' A4' 2.959(8) 2_546 ? S3' A9' 2.459(8) 2_546 ? S3' A9 2.802(8) 2_546 ? S3' A1' 3.120(6) 2_546 ? S8' A8 2.425(7) 4_565 ? S8' A8' 2.825(7) 4_565 ? S8' A1' 3.019(6) 3_566 ? S9' A1 2.790(7) 2_547 ? S9' A1' 2.877(7) 2_546 ? S9' A2 2.922(7) 1_556 ? S10' A2 3.014(7) 1_556 ? S11' A4' 2.935(8) 4_565 ? 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 S9' A1 S3 78.12(19) 2_557 2_556 ? S9' A1 S9 86.89(17) 2_557 2_556 ? S3 A1 S9 75.52(19) 2_556 2_556 ? S9' A1 S2 88.9(2) 2_557 1_556 ? S3 A1 S2 76.75(19) 2_556 1_556 ? S9 A1 S2 152.23(15) 2_556 1_556 ? S7 A2 S9' 86.02(19) . 1_554 ? S7 A2 S9 84.46(18) . . ? S9' A2 S9 86.30(17) 1_554 . ? S7 A2 S10' 77.55(18) . 1_554 ? S9' A2 S10' 94.2(2) 1_554 1_554 ? S9 A2 S10' 161.91(16) . 1_554 ? S7 A2 S10 80.78(18) . . ? S9' A2 S10 166.64(16) 1_554 . ? S9 A2 S10 90.4(2) . . ? S10' A2 S10 85.02(16) 1_554 . ? S2' A3 S6 83.64(18) . 1_556 ? S2' A3 S2 86.92(16) . 1_556 ? S6 A3 S2 78.11(17) 1_556 1_556 ? S2' A3 S4 119.16(19) . 1_556 ? S6 A3 S4 138.4(2) 1_556 1_556 ? S2 A3 S4 69.70(18) 1_556 1_556 ? S2' A3 S4' 68.94(17) . . ? S6 A3 S4' 146.1(2) 1_556 . ? S2 A3 S4' 118.25(18) 1_556 . ? S4 A3 S4' 74.59(18) 1_556 . ? S2' A3 S10' 89.9(2) . . ? S6 A3 S10' 79.26(18) 1_556 . ? S2 A3 S10' 157.35(15) 1_556 . ? S4 A3 S10' 130.36(16) 1_556 . ? S4' A3 S10' 81.1(2) . . ? S2' A3 S10 158.33(15) . 1_556 ? S6 A3 S10 74.92(17) 1_556 1_556 ? S2 A3 S10 91.67(19) 1_556 1_556 ? S4 A3 S10 80.24(19) 1_556 1_556 ? S4' A3 S10 129.52(15) . 1_556 ? S10' A3 S10 83.13(15) . 1_556 ? S1' A4 S1 90.6(2) 4_665 2_556 ? S1' A4 S11 90.4(2) 4_665 4_665 ? S1 A4 S11 95.5(3) 2_556 4_665 ? S11 A5A S5' 86.6(2) . . ? S11 A5A S5 87.5(2) . 1_554 ? S5' A5A S5 94.3(2) . 1_554 ? S11 A5A S1' 78.2(2) . . ? S5' A5A S1' 91.4(3) . . ? S5 A5A S1' 164.2(2) 1_554 . ? S11 A5B S5' 91.0(5) . . ? S11 A5B S5 92.0(5) . 1_554 ? S5' A5B S5 97.9(4) . 1_554 ? S10 A6 S6 95.8(2) . . ? S10 A6 S6' 92.2(2) . . ? S6 A6 S6' 92.34(19) . . ? S4' A7 S5 94.7(3) . . ? S4' A7 S4 95.4(2) . 1_556 ? S5 A7 S4 93.0(3) . 1_556 ? S8' A8 S8 98.6(2) 4_665 4_665 ? S8' A8 S9 93.1(2) 4_665 . ? S8 A8 S9 94.3(2) 4_665 . ? S2 A9 S6' 89.8(2) . . ? S2 A9 S3' 89.6(2) . 2_556 ? S6' A9 S3' 91.2(2) . 2_556 ? S2 A9 S6 90.4(2) . . ? S6' A9 S6 82.00(16) . . ? S3' A9 S6 173.2(2) 2_556 . ? S2 A9 S3 86.5(2) . 2 ? S6' A9 S3 170.0(2) . 2 ? S3' A9 S3 98.09(17) 2_556 2 ? S6 A9 S3 88.7(2) . 2 ? S9' A1' S8' 80.89(17) 2_556 3_566 ? S9' A1' S8 88.50(19) 2_556 . ? S8' A1' S8 69.68(17) 3_566 . ? S9' A1' S9 87.75(17) 2_556 2_556 ? S8' A1' S9 71.80(16) 3_566 2_556 ? S8 A1' S9 141.41(16) . 2_556 ? S9' A1' S3' 74.83(18) 2_556 2_556 ? S8' A1' S3' 137.55(15) 3_566 2_556 ? S8 A1' S3' 142.0(2) . 2_556 ? S9 A1' S3' 72.94(17) 2_556 2_556 ? S7' A2' S10 82.06(18) . . ? S7' A2' S9 82.91(18) . . ? S10 A2' S9 90.62(19) . . ? S7' A2' S10' 77.52(18) . . ? S10 A2' S10' 84.45(16) . . ? S9 A2' S10' 160.29(15) . . ? S7' A2' S9' 82.93(18) . . ? S10 A2' S9' 164.95(15) . . ? S9 A2' S9' 86.48(16) . . ? S10' A2' S9' 93.3(2) . . ? S6' A3' S2' 82.17(17) . . ? S6' A3' S10' 80.58(17) . . ? S2' A3' S10' 90.8(2) . . ? S6' A3' S10 75.97(16) . . ? S2' A3' S10 158.05(15) . . ? S10' A3' S10 83.88(16) . . ? S6' A3' S2 76.51(17) . . ? S2' A3' S2 84.03(16) . . ? S10' A3' S2 156.98(15) . . ? S10 A3' S2 92.6(2) . . ? S1 A4' S11 83.1(2) 4_665 4_666 ? S1 A4' S1 78.5(2) 4_665 2_557 ? S11 A4' S1 83.1(2) 4_666 2_557 ? S1 A4' S11' 80.5(2) 4_665 4_665 ? S11 A4' S11' 90.66(18) 4_666 4_665 ? S1 A4' S11' 158.74(17) 2_557 4_665 ? S1 A4' S1' 78.2(2) 4_665 2_556 ? S11 A4' S1' 161.16(16) 4_666 2_556 ? S1 A4' S1' 90.38(17) 2_557 2_556 ? S11' A4' S1' 89.1(2) 4_665 2_556 ? S11' A5A' S5 84.6(2) . . ? S11' A5A' S5' 82.6(2) . . ? S5 A5A' S5' 92.1(2) . . ? S11' A5A' S1' 79.1(2) . . ? S5 A5A' S1' 163.0(2) . . ? S5' A5A' S1' 90.5(3) . . ? S11' A5A' S1 78.8(2) . . ? S5 A5A' S1 91.7(3) . . ? S5' A5A' S1 160.5(2) . . ? S1' A5A' S1 80.56(18) . . ? S11' A5B' S5' 91.6(3) . . ? S11' A5B' S5 90.9(3) . . ? S5' A5B' S5 97.7(3) . . ? S10' A6' S7 94.1(2) . 1_556 ? S10' A6' S7' 93.9(2) . . ? S7 A6' S7' 98.0(2) 1_556 . ? S5' A7' S4' 82.8(2) . . ? S5' A7' S4 82.0(2) . . ? S4' A7' S4 98.90(17) . . ? S5' A7' S11' 77.5(2) . . ? S4' A7' S11' 86.0(2) . . ? S4 A7' S11' 158.14(18) . . ? S5' A7' S11 78.7(2) . . ? S4' A7' S11 159.15(18) . . ? S4 A7' S11 87.9(2) . . ? S11' A7' S11 80.82(17) . . ? S9' A8' S8' 85.98(19) . 4_665 ? S9' A8' S8 84.5(2) . 4_666 ? S8' A8' S8 98.85(16) 4_665 4_666 ? S9' A8' S7' 81.95(18) . . ? S8' A8' S7' 91.03(19) 4_665 . ? S8 A8' S7' 162.62(17) 4_666 . ? S2' A9' S3' 95.2(2) . 2_556 ? S2' A9' S3 95.1(2) . 2_556 ? S3' A9' S3 99.8(2) 2_556 2_556 ? A4 S1 A4' 96.7(2) 2_546 4_565 ? A4 S1 A4' 89.16(17) 2_546 2_547 ? A4' S1 A4' 101.5(2) 4_565 2_547 ? A4 S1 A5A' 96.9(3) 2_546 . ? A4' S1 A5A' 97.8(2) 4_565 . ? A4' S1 A5A' 159.0(2) 2_547 . ? A9 S2 A3 100.0(2) . 1_554 ? A9 S2 A3' 98.2(2) . . ? A3 S2 A3' 84.00(13) 1_554 . ? A9 S2 A1 100.2(2) . 1_554 ? A3 S2 A1 94.7(2) 1_554 1_554 ? A3' S2 A1 161.5(2) . 1_554 ? A9' S3 A1 99.9(2) 2_546 2_546 ? A9' S3 A9 98.96(19) 2_546 2_545 ? A1 S3 A9 95.1(2) 2_546 2_545 ? A7 S4 A7' 98.45(19) 1_554 . ? A7 S4 A3 85.0(3) 1_554 1_554 ? A7' S4 A3 154.2(3) . 1_554 ? A7 S5 A5B' 96.5(3) . . ? A7 S5 A5B 98.6(4) . 1_556 ? A5B' S5 A5B 101.0(3) . 1_556 ? A7 S5 A5A' 102.3(3) . . ? A5B' S5 A5A' 6.42(14) . . ? A5B S5 A5A' 97.3(4) 1_556 . ? A7 S5 A5A 101.7(3) . 1_556 ? A5B' S5 A5A 99.5(2) . 1_556 ? A5B S5 A5A 3.2(3) 1_556 1_556 ? A5A' S5 A5A 95.47(19) . 1_556 ? A6 S6 A9 91.9(3) . . ? A6 S6 A3 95.1(2) . 1_554 ? A9 S6 A3 91.6(2) . 1_554 ? A6' S7 A2 96.5(2) 1_554 . ? A8 S8 A8' 95.60(18) 4_565 4_564 ? A8 S8 A1' 89.6(3) 4_565 . ? A8' S8 A1' 148.5(2) 4_564 . ? A8 S9 A2 107.7(2) . . ? A8 S9 A2' 109.5(2) . . ? A2 S9 A2' 87.44(14) . . ? A8 S9 A1 99.7(2) . 2_546 ? A2 S9 A1 85.8(2) . 2_546 ? A2' S9 A1 150.7(2) . 2_546 ? A8 S9 A1' 96.6(2) . 2_546 ? A2 S9 A1' 155.5(2) . 2_546 ? A2' S9 A1' 87.7(2) . 2_546 ? A1 S9 A1' 86.73(14) 2_546 2_546 ? A6 S10 A2' 104.1(2) . . ? A6 S10 A3' 95.5(2) . . ? A2' S10 A3' 92.8(2) . . ? A6 S10 A2 101.8(2) . . ? A2' S10 A2 85.74(13) . . ? A3' S10 A2 162.5(2) . . ? A6 S10 A3 93.8(2) . 1_554 ? A2' S10 A3 161.9(2) . 1_554 ? A3' S10 A3 83.09(13) . 1_554 ? A2 S10 A3 92.9(2) . 1_554 ? A5B S11 A4 99.5(4) . 4_565 ? A5B S11 A5A 2.5(3) . . ? A4 S11 A5A 97.5(2) 4_565 . ? A5B S11 A4' 105.7(4) . 4_564 ? A4 S11 A4' 89.23(18) 4_565 4_564 ? A5A S11 A4' 104.2(2) . 4_564 ? A5B S11 A7' 92.1(4) . . ? A4 S11 A7' 97.4(3) 4_565 . ? A5A S11 A7' 93.9(2) . . ? A4' S11 A7' 159.8(2) 4_564 . ? A4 S1' A4' 94.3(2) 4_565 2_546 ? A4 S1' A5A' 102.7(2) 4_565 . ? A4' S1' A5A' 162.5(2) 2_546 . ? A4 S1' A5A 93.9(2) 4_565 . ? A4' S1' A5A 92.5(3) 2_546 . ? A5A' S1' A5A 82.50(16) . . ? A9' S2' A3 104.2(3) . . ? A9' S2' A3' 105.4(2) . . ? A3 S2' A3' 86.94(14) . . ? A9' S3' A9 98.9(2) 2_546 2_546 ? A9' S3' A1' 98.9(2) 2_546 2_546 ? A9 S3' A1' 95.5(2) 2_546 2_546 ? A7 S4' A7' 97.2(2) . . ? A7 S4' A3 86.5(2) . . ? A7' S4' A3 153.1(3) . . ? A5B' S5' A5B 94.6(3) . . ? A5B' S5' A5A 92.7(2) . . ? A5B S5' A5A 3.4(3) . . ? A5B' S5' A5A' 5.33(14) . . ? A5B S5' A5A' 93.0(4) . . ? A5A S5' A5A' 90.93(19) . . ? A5B' S5' A7' 95.7(3) . . ? A5B S5' A7' 97.2(4) . . ? A5A S5' A7' 100.2(3) . . ? A5A' S5' A7' 100.9(3) . . ? A6 S6' A9 93.4(2) . . ? A6 S6' A3' 96.04(19) . . ? A9 S6' A3' 95.5(2) . . ? A6' S7' A2' 95.8(2) . . ? A6' S7' A8' 94.3(3) . . ? A2' S7' A8' 96.42(19) . . ? A8 S8' A8' 102.01(19) 4_565 4_565 ? A8 S8' A1' 97.5(2) 4_565 3_566 ? A8' S8' A1' 94.30(18) 4_565 3_566 ? A8' S9' A1 104.2(2) . 2_547 ? A8' S9' A1' 98.4(2) . 2_546 ? A1 S9' A1' 88.06(14) 2_547 2_546 ? A8' S9' A2 98.6(2) . 1_556 ? A1 S9' A2 90.3(2) 2_547 1_556 ? A1' S9' A2 162.9(2) 2_546 1_556 ? A8' S9' A2' 98.08(19) . . ? A1 S9' A2' 157.7(2) 2_547 . ? A1' S9' A2' 90.1(2) 2_546 . ? A2 S9' A2' 85.02(13) 1_556 . ? A6' S10' A2' 92.1(2) . . ? A6' S10' A3' 107.5(2) . . ? A2' S10' A3' 92.7(2) . . ? A6' S10' A2 90.7(2) . 1_556 ? A2' S10' A2 83.74(13) . 1_556 ? A3' S10' A2 161.6(2) . 1_556 ? A6' S10' A3 106.7(2) . . ? A2' S10' A3 161.1(2) . . ? A3' S10' A3 83.91(13) . . ? A2 S10' A3 93.6(2) 1_556 . ? A5B' S11' A5A' 4.08(16) . . ? A5B' S11' A4' 106.3(3) . 4_565 ? A5A' S11' A4' 102.5(2) . 4_565 ? A5B' S11' A7' 94.7(3) . . ? A5A' S11' A7' 98.7(2) . . ? A4' S11' A7' 158.6(2) 4_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.098 _refine_diff_density_min -6.044 _refine_diff_density_rms 1.016