'2594_DORSAMDEPOSITKentrolite-Al-cif.txtTEXTR*ch4èÃôB\Ãôˆ¬<Ç data_doersam2 _audit_creation_method SHELXL-97 _chemical_name_systematic 'Lead Aluminium Silicon Oxide' _chemical_name_common Pb2Al2Si2O9 _chemical_melting_point ? _chemical_formula_moiety 'Al2 O9 Pb2 Si2' _chemical_formula_sum 'Al2 O9 Pb2 Si2' _chemical_formula_weight 668.52 _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' 'Al' 'Al' 0.0645 0.0514 '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' '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 Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 6.8981(7) _cell_length_b 10.6906(15) _cell_length_c 9.7413(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 718.37(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2386 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 28.0 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.0847 _exptl_crystal_size_mid 0.0760 _exptl_crystal_size_min 0.0572 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_correction_T_min 0.006 _exptl_absorpt_correction_T_max 0.050 _exptl_absorpt_coefficient_mu 47.424 _exptl_absorpt_correction_type 'analytical' _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 hydrothermal synthesis experiments at 2GPa 600 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_% 'none' _diffrn_reflns_number 3317 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.499 _diffrn_reflns_theta_max 28.5872 _reflns_number_total 786 _reflns_number_gt 674 _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_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^)+(0.0391P)^2^+0.0000P] 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 0.0043(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 786 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.45060(4) 0.30435(3) 0.54954(3) 0.01228(15) Uani 1 1 d . . . Al1 Al 0.5000 0.0000 0.0000 0.0058(6) Uani 1 2 d S . . Al2 Al 0.5000 0.1467(3) 0.2500 0.0067(6) Uani 1 2 d S . . Si1 Si 0.2171(2) -0.08831(19) 0.24876(17) 0.0073(4) Uani 1 1 d . . . O1 O 0.3477(6) 0.0082(4) 0.3372(5) 0.0084(9) Uani 1 1 d . . . O2 O 0.3080(7) -0.1068(5) 0.0965(5) 0.0108(10) Uani 1 1 d . . . O3 O 0.1854(6) -0.2260(5) 0.3169(5) 0.0093(10) Uani 1 1 d . . . O4 O 0.0000 -0.0227(7) 0.2500 0.0102(14) Uani 1 2 d S . . O5 O 0.6096(7) 0.1410(5) 0.4230(5) 0.0076(10) 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 0.0136(2) 0.0153(2) 0.0079(2) -0.00104(10) -0.00055(9) -0.00010(10) Al1 0.0050(12) 0.0104(17) 0.0021(13) -0.0001(11) -0.0003(10) 0.0014(12) Al2 0.0065(12) 0.0108(17) 0.0027(12) 0.000 -0.0012(11) 0.000 Si1 0.0053(8) 0.0129(10) 0.0036(8) 0.0005(7) 0.0001(7) -0.0009(7) O1 0.008(2) 0.014(3) 0.003(2) 0.0005(19) 0.0009(19) -0.001(2) O2 0.015(2) 0.014(3) 0.004(2) -0.0021(19) 0.0031(19) -0.004(2) O3 0.008(2) 0.010(3) 0.010(2) 0.0007(18) 0.0013(19) -0.0036(19) O4 0.005(3) 0.008(4) 0.018(4) 0.000 -0.001(3) 0.000 O5 0.007(2) 0.012(3) 0.004(2) 0.0007(18) -0.0018(18) -0.001(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 Pb1 O2 2.375(5) 8_556 ? Pb1 O5 2.402(5) . ? Pb1 O5 2.439(5) 3_456 ? Pb1 O3 2.474(5) 7_665 ? Pb1 Al1 3.3069(5) 4_655 ? Al1 O5 1.846(5) 8 ? Al1 O5 1.846(5) 4_655 ? Al1 O1 1.905(4) 8 ? Al1 O1 1.905(4) 4_655 ? Al1 O2 1.985(5) . ? Al1 O2 1.985(5) 5_655 ? Al1 Al2 2.8969(17) 5_655 ? Al1 Al2 2.8969(17) . ? Al1 Pb1 3.3069(5) 8 ? Al1 Pb1 3.3069(5) 4_655 ? Al2 O5 1.848(4) . ? Al2 O5 1.848(4) 4_655 ? Al2 O3 1.977(5) 7_665 ? Al2 O3 1.977(5) 6_666 ? Al2 O1 2.004(5) 4_655 ? Al2 O1 2.004(5) . ? Al2 Al1 2.8969(17) 4_655 ? Si1 O1 1.618(5) . ? Si1 O2 1.622(5) . ? Si1 O3 1.630(5) . ? Si1 O4 1.654(3) . ? O1 Al1 1.905(4) 4_655 ? O2 Pb1 2.375(5) 8 ? O3 Al2 1.977(5) 6_556 ? O3 Pb1 2.474(5) 7_655 ? O4 Si1 1.654(3) 4 ? O5 Al1 1.846(5) 4_655 ? O5 Pb1 2.439(5) 3_556 ? 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 68.99(16) 8_556 . ? O2 Pb1 O5 78.01(17) 8_556 3_456 ? O5 Pb1 O5 132.12(14) . 3_456 ? O2 Pb1 O3 84.42(16) 8_556 7_665 ? O5 Pb1 O3 66.90(15) . 7_665 ? O5 Pb1 O3 76.47(14) 3_456 7_665 ? O2 Pb1 Al1 36.45(11) 8_556 4_655 ? O5 Pb1 Al1 33.17(12) . 4_655 ? O5 Pb1 Al1 110.55(13) 3_456 4_655 ? O3 Pb1 Al1 77.08(11) 7_665 4_655 ? O5 Al1 O5 180.0(4) 8 4_655 ? O5 Al1 O1 81.35(19) 8 8 ? O5 Al1 O1 98.65(19) 4_655 8 ? O5 Al1 O1 98.65(19) 8 4_655 ? O5 Al1 O1 81.35(19) 4_655 4_655 ? O1 Al1 O1 180.00(15) 8 4_655 ? O5 Al1 O2 89.8(2) 8 . ? O5 Al1 O2 90.2(2) 4_655 . ? O1 Al1 O2 89.99(19) 8 . ? O1 Al1 O2 90.01(19) 4_655 . ? O5 Al1 O2 90.2(2) 8 5_655 ? O5 Al1 O2 89.8(2) 4_655 5_655 ? O1 Al1 O2 90.01(19) 8 5_655 ? O1 Al1 O2 89.99(19) 4_655 5_655 ? O2 Al1 O2 180.0(3) . 5_655 ? O5 Al1 Al2 38.38(14) 8 5_655 ? O5 Al1 Al2 141.62(14) 4_655 5_655 ? O1 Al1 Al2 43.51(14) 8 5_655 ? O1 Al1 Al2 136.49(14) 4_655 5_655 ? O2 Al1 Al2 94.98(14) . 5_655 ? O2 Al1 Al2 85.02(14) 5_655 5_655 ? O5 Al1 Al2 141.62(14) 8 . ? O5 Al1 Al2 38.38(14) 4_655 . ? O1 Al1 Al2 136.49(14) 8 . ? O1 Al1 Al2 43.51(14) 4_655 . ? O2 Al1 Al2 85.02(14) . . ? O2 Al1 Al2 94.98(14) 5_655 . ? Al2 Al1 Al2 180.0 5_655 . ? O5 Al1 Pb1 45.40(16) 8 8 ? O5 Al1 Pb1 134.60(16) 4_655 8 ? O1 Al1 Pb1 91.10(14) 8 8 ? O1 Al1 Pb1 88.90(14) 4_655 8 ? O2 Al1 Pb1 45.29(15) . 8 ? O2 Al1 Pb1 134.71(15) 5_655 8 ? Al2 Al1 Pb1 65.79(5) 5_655 8 ? Al2 Al1 Pb1 114.21(5) . 8 ? O5 Al1 Pb1 134.60(16) 8 4_655 ? O5 Al1 Pb1 45.40(16) 4_655 4_655 ? O1 Al1 Pb1 88.90(14) 8 4_655 ? O1 Al1 Pb1 91.10(14) 4_655 4_655 ? O2 Al1 Pb1 134.71(15) . 4_655 ? O2 Al1 Pb1 45.29(15) 5_655 4_655 ? Al2 Al1 Pb1 114.21(5) 5_655 4_655 ? Al2 Al1 Pb1 65.79(5) . 4_655 ? Pb1 Al1 Pb1 180.000(13) 8 4_655 ? O5 Al2 O5 176.2(4) . 4_655 ? O5 Al2 O3 89.2(2) . 7_665 ? O5 Al2 O3 93.4(2) 4_655 7_665 ? O5 Al2 O3 93.4(2) . 6_666 ? O5 Al2 O3 89.2(2) 4_655 6_666 ? O3 Al2 O3 93.1(3) 7_665 6_666 ? O5 Al2 O1 98.5(2) . 4_655 ? O5 Al2 O1 78.7(2) 4_655 4_655 ? O3 Al2 O1 170.67(19) 7_665 4_655 ? O3 Al2 O1 91.71(19) 6_666 4_655 ? O5 Al2 O1 78.7(2) . . ? O5 Al2 O1 98.5(2) 4_655 . ? O3 Al2 O1 91.71(19) 7_665 . ? O3 Al2 O1 170.67(19) 6_666 . ? O1 Al2 O1 84.7(3) 4_655 . ? O5 Al2 Al1 138.5(2) . . ? O5 Al2 Al1 38.32(17) 4_655 . ? O3 Al2 Al1 130.51(13) 7_665 . ? O3 Al2 Al1 95.48(14) 6_666 . ? O1 Al2 Al1 40.87(13) 4_655 . ? O1 Al2 Al1 87.48(16) . . ? O5 Al2 Al1 38.32(17) . 4_655 ? O5 Al2 Al1 138.5(2) 4_655 4_655 ? O3 Al2 Al1 95.48(14) 7_665 4_655 ? O3 Al2 Al1 130.51(13) 6_666 4_655 ? O1 Al2 Al1 87.48(16) 4_655 4_655 ? O1 Al2 Al1 40.87(13) . 4_655 ? Al1 Al2 Al1 114.42(11) . 4_655 ? O1 Si1 O2 110.4(3) . . ? O1 Si1 O3 115.7(2) . . ? O2 Si1 O3 108.3(3) . . ? O1 Si1 O4 103.3(3) . . ? O2 Si1 O4 114.1(2) . . ? O3 Si1 O4 105.0(3) . . ? Si1 O1 Al1 136.1(3) . 4_655 ? Si1 O1 Al2 122.5(3) . . ? Al1 O1 Al2 95.6(2) 4_655 . ? Si1 O2 Al1 128.4(3) . . ? Si1 O2 Pb1 116.4(3) . 8 ? Al1 O2 Pb1 98.27(19) . 8 ? Si1 O3 Al2 125.0(3) . 6_556 ? Si1 O3 Pb1 107.8(2) . 7_655 ? Al2 O3 Pb1 98.45(18) 6_556 7_655 ? Si1 O4 Si1 129.8(5) 4 . ? Al1 O5 Al2 103.3(3) 4_655 . ? Al1 O5 Pb1 101.4(2) 4_655 . ? Al2 O5 Pb1 104.9(2) . . ? Al1 O5 Pb1 123.1(2) 4_655 3_556 ? Al2 O5 Pb1 119.1(2) . 3_556 ? Pb1 O5 Pb1 102.12(19) . 3_556 ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.411 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.296