$2594_DORSAMDEPOSITkentrolite.cif.txtTEXTR*chS[B\ data_doersam41 _audit_creation_method SHELXL-97 _chemical_name_systematic 'Lead Mangane Silicon Oxide' _chemical_name_common Pb2Mn2Si2O9 _chemical_melting_point ? _chemical_formula_moiety 'Mn2 O9 Pb2 Si2' _chemical_formula_sum 'Mn2 O9 Pb2 Si2' _chemical_formula_weight 724.44 _publ_contact_author_name 'Guido Doersam' _publ_contact_author_address ; Fachgebiet Mineralogie und Petrologie Technische Universitaet Berlin Ackerstr. 76 D-13355 Berlin ; _publ_contact_author_email 'guido.doersam@web.de' _publ_contact_author_phone '(+41) 3031472222' _publ_section_title ; Crystal structure of synthetic melanotekite (Pb2Fe2Si2O9), kentrolite (Pb2Mn2Si2O9) and the aluminium analogue (Pb2Al2Si2O9) ; _publ_requested_journal 'American Mineralogist' loop_ _publ_author_name _publ_author_address 'Guido Doersam' ; Fachgebiet Mineralogie und Petrologie Technische Universitaet Berlin Ackerstr. 76 D-13355 Berlin ; 'Axel Liebscher' ; Fachgebiet Mineralogie und Petrologie Technische Universitaet Berlin Ackerstr. 76 D-13355 Berlin ; 'Gerhard Franz' ; Fachgebiet Mineralogie und Petrologie Technische Universitaet Berlin Ackerstr. 76 D-13355 Berlin ; 'Bernd Wunder' ; GeoForschungszentrum Potsdam Telegraphenberg, D-14473 Potsdam, Germany ; 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 Orthorhombic _symmetry_space_group_name_H-M P21221 _symmetry_space_group_name_Hall 'P 2ac 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, -z+1/2' '-x, y, -z' _cell_length_a 7.0079(4) _cell_length_b 11.0665(5) _cell_length_c 9.9634(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 772.69(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6066 _cell_measurement_theta_min 3.4348 _cell_measurement_theta_max 32.3289 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.2145 _exptl_crystal_size_mid 0.1195 _exptl_crystal_size_min 0.0589 _exptl_absorpt_correction_T_min 0.030 _exptl_absorpt_correction_T_max 0.135 _exptl_absorpt_correction_type 'analytical' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 46.980 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Derived from synthesis experiments at 850 Degrees C ; _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 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.3031 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11777 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 32.33 _reflns_number_total 2592 _reflns_number_gt 2256 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0404P)^2^+3.0500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00255(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.411(11) _refine_ls_number_reflns 2592 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5486(3) 0.55249(16) 0.2001(3) 0.0086(3) Uani 0.72 1 d P . . Pb2 Pb 0.5348(9) 0.5476(5) 0.1989(10) 0.0267(16) Uani 0.28 1 d P . . Pb3 Pb 0.5479(2) -0.0598(2) 0.2974(3) 0.0095(2) Uani 0.65 1 d P . . Pb4 Pb 0.4986(4) -0.0557(5) 0.2985(7) 0.0245(8) Uani 0.35 1 d P . . Mn1 Mn 0.5000 0.10481(16) 0.0000 0.0068(4) Uani 1 2 d S . . Mn2 Mn 0.0000 0.60542(15) 0.0000 0.0063(4) Uani 1 2 d S . . Mn3 Mn 0.5016(2) 0.24901(10) 0.24963(12) 0.0069(2) Uani 1 1 d . . . Si1 Si 0.7876(4) 0.1571(2) 0.4971(2) 0.0087(5) Uani 1 1 d . . . Si2 Si 0.7867(4) 0.3436(2) -0.0037(2) 0.0069(5) Uani 1 1 d . . . O1 O 0.8887(10) 0.6091(5) 0.1731(5) 0.0099(12) Uani 1 1 d . . . O2 O 0.0000 0.2222(8) 0.5000 0.021(3) Uani 1 2 d S . . O3 O 0.7009(11) 0.3679(5) 0.1433(6) 0.0115(13) Uani 1 1 d . . . O4 O 0.8122(11) 0.4729(6) -0.0808(6) 0.0134(13) Uani 1 1 d . . . O5 O 0.7901(13) -0.1351(6) 0.1474(6) 0.0193(17) Uani 1 1 d . . . O6 O 0.6634(10) 0.2454(5) -0.0882(6) 0.0102(12) Uani 1 1 d . . . O7 O 0.8116(10) 0.0266(5) 0.4218(6) 0.0112(12) Uani 1 1 d . . . O8 O 0.6566(11) 0.2511(5) 0.4152(6) 0.0106(12) Uani 1 1 d . . . O9 O 0.6148(10) 0.1106(5) 0.1720(5) 0.0093(12) Uani 1 1 d . . . O10 O 0.0000 0.2811(8) 0.0000 0.015(2) Uani 1 2 d S . . 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 0.0091(4) 0.0077(5) 0.0090(5) 0.0011(5) -0.0015(4) 0.0040(4) Pb2 0.044(3) 0.0192(17) 0.017(2) 0.0012(15) -0.003(2) -0.0212(13) Pb3 0.0083(5) 0.0107(3) 0.0095(3) 0.0011(3) 0.0009(5) -0.0012(4) Pb4 0.044(2) 0.0163(9) 0.0127(7) 0.0004(8) -0.001(2) -0.0098(17) Mn1 0.0070(9) 0.0075(7) 0.0059(7) 0.000 -0.0004(6) 0.000 Mn2 0.0055(9) 0.0073(7) 0.0062(7) 0.000 0.0016(6) 0.000 Mn3 0.0075(6) 0.0068(5) 0.0064(5) -0.0008(4) -0.0006(4) -0.0001(4) Si1 0.0083(13) 0.0094(10) 0.0084(10) -0.0003(9) -0.0016(8) 0.0016(11) Si2 0.0058(12) 0.0072(9) 0.0077(10) -0.0003(9) 0.0005(8) 0.0012(11) O1 0.010(3) 0.014(3) 0.006(3) 0.0001(19) -0.002(2) 0.000(3) O2 0.003(5) 0.006(4) 0.054(7) 0.000 -0.012(5) 0.000 O3 0.016(4) 0.009(3) 0.010(3) -0.007(2) 0.006(3) -0.005(3) O4 0.016(3) 0.011(3) 0.013(3) 0.004(2) 0.007(3) -0.002(3) O5 0.037(5) 0.012(3) 0.009(3) -0.004(2) -0.004(3) 0.009(3) O6 0.009(3) 0.011(3) 0.011(3) 0.000(2) -0.001(2) -0.005(3) O7 0.007(3) 0.009(3) 0.017(3) -0.005(2) -0.001(3) 0.000(3) O8 0.010(3) 0.014(3) 0.008(3) 0.000(2) 0.000(2) 0.003(3) O9 0.009(3) 0.012(3) 0.007(3) 0.0002(19) -0.002(2) -0.002(2) O10 0.007(5) 0.007(4) 0.029(5) 0.000 0.002(4) 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 O3 2.373(6) . ? Pb1 O4 2.407(7) 2_665 ? Pb1 O1 2.460(6) 3_465 ? Pb1 O1 2.479(7) . ? Pb1 Mn3 3.410(2) . ? Pb2 O3 2.370(8) . ? Pb2 O1 2.384(10) 3_465 ? Pb2 O4 2.454(11) 2_665 ? Pb2 O1 2.585(10) . ? Pb2 Mn3 3.351(6) . ? Pb2 Mn2 3.454(9) 2_665 ? Pb3 O9 2.311(6) . ? Pb3 O5 2.409(8) . ? Pb3 O7 2.422(7) . ? Pb3 Mn3 3.466(3) . ? Pb3 Pb4 3.539(4) 3 ? Pb4 O9 2.375(8) . ? Pb4 O7 2.576(9) 3_455 ? Pb4 O5 2.624(9) 3_455 ? Pb4 O7 2.675(8) . ? Pb4 O5 2.684(9) . ? Pb4 Mn3 3.408(6) . ? Pb4 Mn1 3.464(6) . ? Pb4 Pb3 3.539(4) 3_455 ? Mn1 O9 1.894(6) . ? Mn1 O9 1.894(6) 4_655 ? Mn1 O7 2.113(7) 3_455 ? Mn1 O7 2.113(7) 2_654 ? Mn1 O6 2.122(6) 4_655 ? Mn1 O6 2.122(6) . ? Mn1 Mn3 2.9551(15) . ? Mn1 Mn3 2.9551(15) 4_655 ? Mn1 Pb4 3.464(6) 4_655 ? Mn2 O1 1.894(6) 4_755 ? Mn2 O1 1.894(6) . ? Mn2 O8 2.107(6) 3_565 ? Mn2 O8 2.107(6) 2_664 ? Mn2 O4 2.129(7) . ? Mn2 O4 2.129(7) 4_755 ? Mn2 Mn3 2.9695(15) 3_565 ? Mn2 Mn3 2.9695(15) 2_664 ? Mn2 Pb2 3.454(9) 2_664 ? Mn2 Pb2 3.454(9) 3_565 ? Mn3 O9 1.890(6) . ? Mn3 O1 1.919(6) 3_465 ? Mn3 O8 1.975(6) . ? Mn3 O6 1.981(7) 4_655 ? Mn3 O3 2.192(7) . ? Mn3 O5 2.200(8) 3_455 ? Mn3 Mn2 2.9695(15) 2_665 ? Si1 O8 1.610(7) . ? Si1 O5 1.612(7) 2_655 ? Si1 O7 1.636(6) . ? Si1 O2 1.654(5) 1_655 ? Si2 O3 1.606(6) . ? Si2 O6 1.624(7) . ? Si2 O4 1.634(7) . ? Si2 O10 1.647(5) 1_655 ? O1 Mn3 1.919(6) 3_565 ? O1 Pb2 2.384(10) 3_565 ? O1 Pb1 2.460(6) 3_565 ? O2 Si1 1.654(5) 1_455 ? O2 Si1 1.654(5) 4_656 ? O4 Pb1 2.407(7) 2_664 ? O4 Pb2 2.454(11) 2_664 ? O5 Si1 1.612(7) 2_654 ? O5 Mn3 2.200(8) 3 ? O5 Pb4 2.624(9) 3 ? O6 Mn3 1.981(7) 4_655 ? O7 Mn1 2.113(7) 2_655 ? O7 Pb4 2.576(9) 3 ? O8 Mn2 2.107(6) 2_665 ? O10 Si2 1.647(5) 4_655 ? O10 Si2 1.647(5) 1_455 ? 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 O3 Pb1 O4 86.2(2) . 2_665 ? O3 Pb1 O1 72.6(2) . 3_465 ? O4 Pb1 O1 68.6(2) 2_665 3_465 ? O3 Pb1 O1 76.1(2) . . ? O4 Pb1 O1 74.8(2) 2_665 . ? O1 Pb1 O1 132.7(2) 3_465 . ? O3 Pb1 Mn3 39.67(16) . . ? O4 Pb1 Mn3 78.07(16) 2_665 . ? O1 Pb1 Mn3 33.45(14) 3_465 . ? O1 Pb1 Mn3 110.96(14) . . ? O3 Pb2 O1 74.0(3) . 3_465 ? O3 Pb2 O4 85.2(3) . 2_665 ? O1 Pb2 O4 69.0(3) 3_465 2_665 ? O3 Pb2 O1 74.1(3) . . ? O1 Pb2 O1 131.1(3) 3_465 . ? O4 Pb2 O1 72.2(3) 2_665 . ? O3 Pb2 Mn3 40.69(19) . . ? O1 Pb2 Mn3 34.10(16) 3_465 . ? O4 Pb2 Mn3 78.7(2) 2_665 . ? O1 Pb2 Mn3 110.0(2) . . ? O3 Pb2 Mn2 80.0(2) . 2_665 ? O1 Pb2 Mn2 31.60(18) 3_465 2_665 ? O4 Pb2 Mn2 37.7(2) 2_665 2_665 ? O1 Pb2 Mn2 106.4(3) . 2_665 ? Mn3 Pb2 Mn2 51.72(11) . 2_665 ? O9 Pb3 O5 78.7(2) . . ? O9 Pb3 O7 78.4(2) . . ? O5 Pb3 O7 85.2(2) . . ? O9 Pb3 Mn3 30.65(15) . . ? O5 Pb3 Mn3 108.76(18) . . ? O7 Pb3 Mn3 75.65(17) . . ? O9 Pb3 Pb4 51.54(18) . 3 ? O5 Pb3 Pb4 47.9(2) . 3 ? O7 Pb3 Pb4 46.71(19) . 3 ? Mn3 Pb3 Pb4 71.95(5) . 3 ? O9 Pb4 O7 68.0(3) . 3_455 ? O9 Pb4 O5 71.1(3) . 3_455 ? O7 Pb4 O5 77.9(2) 3_455 3_455 ? O9 Pb4 O7 72.4(2) . . ? O7 Pb4 O7 140.0(3) 3_455 . ? O5 Pb4 O7 95.1(3) 3_455 . ? O9 Pb4 O5 72.3(2) . . ? O7 Pb4 O5 87.2(3) 3_455 . ? O5 Pb4 O5 143.3(3) 3_455 . ? O7 Pb4 O5 75.2(2) . . ? O9 Pb4 Mn3 32.31(16) . . ? O7 Pb4 Mn3 76.0(2) 3_455 . ? O5 Pb4 Mn3 40.20(19) 3_455 . ? O7 Pb4 Mn3 73.93(18) . . ? O5 Pb4 Mn3 103.8(2) . . ? O9 Pb4 Mn1 31.34(17) . . ? O7 Pb4 Mn1 37.44(17) 3_455 . ? O5 Pb4 Mn1 76.4(2) 3_455 . ? O7 Pb4 Mn1 102.5(2) . . ? O5 Pb4 Mn1 71.6(2) . . ? Mn3 Pb4 Mn1 50.93(9) . . ? O9 Pb4 Pb3 83.25(19) . 3_455 ? O7 Pb4 Pb3 43.19(15) 3_455 3_455 ? O5 Pb4 Pb3 42.90(19) 3_455 3_455 ? O7 Pb4 Pb3 137.1(2) . 3_455 ? O5 Pb4 Pb3 130.2(2) . 3_455 ? Mn3 Pb4 Pb3 66.99(7) . 3_455 ? Mn1 Pb4 Pb3 65.51(6) . 3_455 ? O9 Mn1 O9 176.1(4) . 4_655 ? O9 Mn1 O7 87.4(3) . 3_455 ? O9 Mn1 O7 95.3(3) 4_655 3_455 ? O9 Mn1 O7 95.3(3) . 2_654 ? O9 Mn1 O7 87.4(3) 4_655 2_654 ? O7 Mn1 O7 93.0(3) 3_455 2_654 ? O9 Mn1 O6 80.2(3) . 4_655 ? O9 Mn1 O6 96.9(3) 4_655 4_655 ? O7 Mn1 O6 90.8(2) 3_455 4_655 ? O7 Mn1 O6 173.9(3) 2_654 4_655 ? O9 Mn1 O6 96.9(3) . . ? O9 Mn1 O6 80.2(3) 4_655 . ? O7 Mn1 O6 173.9(3) 3_455 . ? O7 Mn1 O6 90.8(2) 2_654 . ? O6 Mn1 O6 85.7(4) 4_655 . ? O9 Mn1 Mn3 38.61(19) . . ? O9 Mn1 Mn3 138.12(19) 4_655 . ? O7 Mn1 Mn3 93.64(16) 3_455 . ? O7 Mn1 Mn3 132.83(17) 2_654 . ? O6 Mn1 Mn3 42.06(18) 4_655 . ? O6 Mn1 Mn3 87.18(17) . . ? O9 Mn1 Mn3 138.12(19) . 4_655 ? O9 Mn1 Mn3 38.61(19) 4_655 4_655 ? O7 Mn1 Mn3 132.83(17) 3_455 4_655 ? O7 Mn1 Mn3 93.64(16) 2_654 4_655 ? O6 Mn1 Mn3 87.18(17) 4_655 4_655 ? O6 Mn1 Mn3 42.06(18) . 4_655 ? Mn3 Mn1 Mn3 114.63(7) . 4_655 ? O9 Mn1 Pb4 142.5(2) . 4_655 ? O9 Mn1 Pb4 40.7(2) 4_655 4_655 ? O7 Mn1 Pb4 88.01(19) 3_455 4_655 ? O7 Mn1 Pb4 47.82(18) 2_654 4_655 ? O6 Mn1 Pb4 137.14(19) 4_655 4_655 ? O6 Mn1 Pb4 91.08(18) . 4_655 ? Mn3 Mn1 Pb4 178.14(11) . 4_655 ? Mn3 Mn1 Pb4 63.55(10) 4_655 4_655 ? O9 Mn1 Pb4 40.7(2) . . ? O9 Mn1 Pb4 142.5(2) 4_655 . ? O7 Mn1 Pb4 47.82(18) 3_455 . ? O7 Mn1 Pb4 88.01(19) 2_654 . ? O6 Mn1 Pb4 91.08(18) 4_655 . ? O6 Mn1 Pb4 137.14(19) . . ? Mn3 Mn1 Pb4 63.55(10) . . ? Mn3 Mn1 Pb4 178.14(11) 4_655 . ? Pb4 Mn1 Pb4 118.3(2) 4_655 . ? O1 Mn2 O1 177.5(4) 4_755 . ? O1 Mn2 O8 97.7(3) 4_755 3_565 ? O1 Mn2 O8 80.4(3) . 3_565 ? O1 Mn2 O8 80.4(3) 4_755 2_664 ? O1 Mn2 O8 97.7(3) . 2_664 ? O8 Mn2 O8 82.2(4) 3_565 2_664 ? O1 Mn2 O4 85.7(3) 4_755 . ? O1 Mn2 O4 96.0(3) . . ? O8 Mn2 O4 173.2(3) 3_565 . ? O8 Mn2 O4 92.6(3) 2_664 . ? O1 Mn2 O4 96.0(3) 4_755 4_755 ? O1 Mn2 O4 85.7(3) . 4_755 ? O8 Mn2 O4 92.6(3) 3_565 4_755 ? O8 Mn2 O4 173.2(3) 2_664 4_755 ? O4 Mn2 O4 92.9(4) . 4_755 ? O1 Mn2 Mn3 138.75(19) 4_755 3_565 ? O1 Mn2 Mn3 39.15(18) . 3_565 ? O8 Mn2 Mn3 41.61(18) 3_565 3_565 ? O8 Mn2 Mn3 85.99(17) 2_664 3_565 ? O4 Mn2 Mn3 133.93(18) . 3_565 ? O4 Mn2 Mn3 93.09(17) 4_755 3_565 ? O1 Mn2 Mn3 39.15(18) 4_755 2_664 ? O1 Mn2 Mn3 138.75(19) . 2_664 ? O8 Mn2 Mn3 85.99(17) 3_565 2_664 ? O8 Mn2 Mn3 41.61(18) 2_664 2_664 ? O4 Mn2 Mn3 93.09(17) . 2_664 ? O4 Mn2 Mn3 133.93(18) 4_755 2_664 ? Mn3 Mn2 Mn3 114.29(7) 3_565 2_664 ? O1 Mn2 Pb2 41.3(2) 4_755 2_664 ? O1 Mn2 Pb2 140.6(2) . 2_664 ? O8 Mn2 Pb2 139.0(2) 3_565 2_664 ? O8 Mn2 Pb2 89.11(19) 2_664 2_664 ? O4 Mn2 Pb2 44.8(2) . 2_664 ? O4 Mn2 Pb2 92.0(2) 4_755 2_664 ? Mn3 Mn2 Pb2 174.87(11) 3_565 2_664 ? Mn3 Mn2 Pb2 62.36(12) 2_664 2_664 ? O1 Mn2 Pb2 140.6(2) 4_755 3_565 ? O1 Mn2 Pb2 41.3(2) . 3_565 ? O8 Mn2 Pb2 89.11(19) 3_565 3_565 ? O8 Mn2 Pb2 139.0(2) 2_664 3_565 ? O4 Mn2 Pb2 92.0(2) . 3_565 ? O4 Mn2 Pb2 44.8(2) 4_755 3_565 ? Mn3 Mn2 Pb2 62.36(12) 3_565 3_565 ? Mn3 Mn2 Pb2 174.87(11) 2_664 3_565 ? Pb2 Mn2 Pb2 121.3(2) 2_664 3_565 ? O9 Mn3 O1 179.2(3) . 3_465 ? O9 Mn3 O8 96.9(3) . . ? O1 Mn3 O8 83.2(3) 3_465 . ? O9 Mn3 O6 84.0(3) . 4_655 ? O1 Mn3 O6 95.8(3) 3_465 4_655 ? O8 Mn3 O6 177.6(3) . 4_655 ? O9 Mn3 O3 91.2(3) . . ? O1 Mn3 O3 88.0(3) 3_465 . ? O8 Mn3 O3 92.6(3) . . ? O6 Mn3 O3 89.5(3) 4_655 . ? O9 Mn3 O5 90.5(3) . 3_455 ? O1 Mn3 O5 90.2(3) 3_465 3_455 ? O8 Mn3 O5 89.3(3) . 3_455 ? O6 Mn3 O5 88.5(3) 4_655 3_455 ? O3 Mn3 O5 177.2(3) . 3_455 ? O9 Mn3 Mn1 38.70(18) . . ? O1 Mn3 Mn1 141.06(18) 3_465 . ? O8 Mn3 Mn1 135.34(19) . . ? O6 Mn3 Mn1 45.87(18) 4_655 . ? O3 Mn3 Mn1 85.40(15) . . ? O5 Mn3 Mn1 94.61(16) 3_455 . ? O9 Mn3 Mn2 141.71(19) . 2_665 ? O1 Mn3 Mn2 38.53(18) 3_465 2_665 ? O8 Mn3 Mn2 45.10(18) . 2_665 ? O6 Mn3 Mn2 133.69(19) 4_655 2_665 ? O3 Mn3 Mn2 94.74(15) . 2_665 ? O5 Mn3 Mn2 85.23(16) 3_455 2_665 ? Mn1 Mn3 Mn2 179.55(6) . 2_665 ? O9 Mn3 Pb2 135.1(2) . . ? O1 Mn3 Pb2 44.2(2) 3_465 . ? O8 Mn3 Pb2 94.4(2) . . ? O6 Mn3 Pb2 86.5(2) 4_655 . ? O3 Mn3 Pb2 44.8(2) . . ? O5 Mn3 Pb2 133.0(2) 3_455 . ? Mn1 Mn3 Pb2 113.94(17) . . ? Mn2 Mn3 Pb2 65.92(17) 2_665 . ? O9 Mn3 Pb4 42.2(2) . . ? O1 Mn3 Pb4 138.6(2) 3_465 . ? O8 Mn3 Pb4 84.0(2) . . ? O6 Mn3 Pb4 95.3(2) 4_655 . ? O3 Mn3 Pb4 131.84(19) . . ? O5 Mn3 Pb4 50.4(2) 3_455 . ? Mn1 Mn3 Pb4 65.52(12) . . ? Mn2 Mn3 Pb4 114.64(12) 2_665 . ? Pb2 Mn3 Pb4 176.33(14) . . ? O9 Mn3 Pb1 134.3(2) . . ? O1 Mn3 Pb1 44.95(19) 3_465 . ? O8 Mn3 Pb1 93.21(19) . . ? O6 Mn3 Pb1 87.65(18) 4_655 . ? O3 Mn3 Pb1 43.73(17) . . ? O5 Mn3 Pb1 134.2(2) 3_455 . ? Mn1 Mn3 Pb1 114.23(7) . . ? Mn2 Mn3 Pb1 65.65(6) 2_665 . ? Pb2 Mn3 Pb1 1.60(14) . . ? Pb4 Mn3 Pb1 174.80(8) . . ? O9 Mn3 Pb3 38.56(18) . . ? O1 Mn3 Pb3 142.20(19) 3_465 . ? O8 Mn3 Pb3 81.11(19) . . ? O6 Mn3 Pb3 98.40(18) 4_655 . ? O3 Mn3 Pb3 126.77(18) . . ? O5 Mn3 Pb3 55.5(2) 3_455 . ? Mn1 Mn3 Pb3 65.38(7) . . ? Mn2 Mn3 Pb3 114.83(7) 2_665 . ? Pb2 Mn3 Pb3 170.61(13) . . ? Pb4 Mn3 Pb3 5.73(7) . . ? Pb1 Mn3 Pb3 169.07(7) . . ? O8 Si1 O5 112.1(4) . 2_655 ? O8 Si1 O7 113.4(3) . . ? O5 Si1 O7 109.1(3) 2_655 . ? O8 Si1 O2 103.9(4) . 1_655 ? O5 Si1 O2 110.7(3) 2_655 1_655 ? O7 Si1 O2 107.5(4) . 1_655 ? O3 Si2 O6 112.7(4) . . ? O3 Si2 O4 108.9(3) . . ? O6 Si2 O4 113.6(3) . . ? O3 Si2 O10 112.9(3) . 1_655 ? O6 Si2 O10 102.3(4) . 1_655 ? O4 Si2 O10 106.2(4) . 1_655 ? Mn2 O1 Mn3 102.3(3) . 3_565 ? Mn2 O1 Pb2 107.1(3) . 3_565 ? Mn3 O1 Pb2 101.7(3) 3_565 3_565 ? Mn2 O1 Pb1 105.3(3) . 3_565 ? Mn3 O1 Pb1 101.6(3) 3_565 3_565 ? Pb2 O1 Pb1 1.9(2) 3_565 3_565 ? Mn2 O1 Pb1 119.3(3) . . ? Mn3 O1 Pb1 124.0(3) 3_565 . ? Pb2 O1 Pb1 99.8(3) 3_565 . ? Pb1 O1 Pb1 101.4(2) 3_565 . ? Mn2 O1 Pb2 118.7(3) . . ? Mn3 O1 Pb2 124.8(3) 3_565 . ? Pb2 O1 Pb2 99.6(2) 3_565 . ? Pb1 O1 Pb2 101.2(3) 3_565 . ? Pb1 O1 Pb2 0.8(2) . . ? Si1 O2 Si1 128.3(6) 1_455 4_656 ? Si2 O3 Mn3 125.4(3) . . ? Si2 O3 Pb2 122.5(4) . . ? Mn3 O3 Pb2 94.5(3) . . ? Si2 O3 Pb1 122.0(3) . . ? Mn3 O3 Pb1 96.6(3) . . ? Pb2 O3 Pb1 2.7(2) . . ? Si2 O4 Mn2 119.5(4) . . ? Si2 O4 Pb1 111.6(3) . 2_664 ? Mn2 O4 Pb1 99.9(3) . 2_664 ? Si2 O4 Pb2 112.8(4) . 2_664 ? Mn2 O4 Pb2 97.6(3) . 2_664 ? Pb1 O4 Pb2 2.4(2) 2_664 2_664 ? Si1 O5 Mn3 125.0(4) 2_654 3 ? Si1 O5 Pb3 113.0(5) 2_654 . ? Mn3 O5 Pb3 112.6(3) 3 . ? Si1 O5 Pb4 120.0(4) 2_654 3 ? Mn3 O5 Pb4 89.4(3) 3 3 ? Pb3 O5 Pb4 89.2(2) . 3 ? Si1 O5 Pb4 108.3(4) 2_654 . ? Mn3 O5 Pb4 116.0(3) 3 . ? Pb3 O5 Pb4 4.83(18) . . ? Pb4 O5 Pb4 92.6(2) 3 . ? Si2 O6 Mn3 135.9(4) . 4_655 ? Si2 O6 Mn1 124.2(3) . . ? Mn3 O6 Mn1 92.1(3) 4_655 . ? Si1 O7 Mn1 120.2(4) . 2_655 ? Si1 O7 Pb3 120.3(4) . . ? Mn1 O7 Pb3 113.2(3) 2_655 . ? Si1 O7 Pb4 109.4(3) . 3 ? Mn1 O7 Pb4 94.7(3) 2_655 3 ? Pb3 O7 Pb4 90.1(3) . 3 ? Si1 O7 Pb4 115.3(4) . . ? Mn1 O7 Pb4 116.6(3) 2_655 . ? Pb3 O7 Pb4 5.42(17) . . ? Pb4 O7 Pb4 93.9(2) 3 . ? Si1 O8 Mn3 136.8(4) . . ? Si1 O8 Mn2 125.5(3) . 2_665 ? Mn3 O8 Mn2 93.3(3) . 2_665 ? Mn3 O9 Mn1 102.7(3) . . ? Mn3 O9 Pb3 110.8(3) . . ? Mn1 O9 Pb3 112.0(3) . . ? Mn3 O9 Pb4 105.5(3) . . ? Mn1 O9 Pb4 107.9(3) . . ? Pb3 O9 Pb4 8.39(11) . . ? Si2 O10 Si2 130.3(6) 4_655 1_455 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.500 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.435