&2594_DORSAMDEPOSITmelanotekite.cif.txtTEXTR*ch4|B]W data_doersam15 _audit_creation_method SHELXL-97 _chemical_name_systematic 'Lead Iron Silicon Oxide' _chemical_name_common Pb2Fe2Si2O9 _chemical_melting_point ? _chemical_formula_moiety 'Fe2 O9 Pb2 Si2' _chemical_formula_sum 'Fe2 O9 Pb2 Si2' _chemical_formula_weight 726.269 _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' 'Fe' 'Fe' 0.3463 0.8444 '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 6.9788(6) _cell_length_b 11.0164(11) _cell_length_c 10.0881(9) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 775.59(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1298 _cell_measurement_theta_min 2.9127 _cell_measurement_theta_max 28.7128 _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.0875 _exptl_crystal_size_mid 0.0422 _exptl_crystal_size_min 0.0293 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 47.289 _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.389 _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 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 4577 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 28.72 _reflns_number_total 911 _reflns_number_gt 621 _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^)+(0.0376P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 911 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Pb1 Pb 0.44818(17) 0.3016(2) 0.5494(3) 0.0104(3) Uani 0.70 1 d P . . Pb2 Pb 0.5121(6) 0.3088(5) 0.5499(6) 0.0300(11) Uani 0.30 1 d P . . Fe1 Fe 0.5000 0.0000 0.0000 0.0070(6) Uani 1 2 d S . . Fe2 Fe 0.5000 0.1521(3) 0.2500 0.0073(6) Uani 1 2 d S . . Si1 Si 0.2151(4) -0.0864(3) 0.2503(3) 0.0062(8) Uani 1 1 d . . . O1 O 0.3414(10) 0.0109(8) 0.3347(7) 0.0073(19) Uani 1 1 d . . . O2 O 0.3039(12) -0.1082(9) 0.1019(8) 0.013(2) Uani 1 1 d . . . O3 O 0.1914(10) -0.2201(9) 0.3227(8) 0.012(2) Uani 1 1 d . . . O4 O 0.0000 -0.0244(12) 0.2500 0.020(3) Uani 1 2 d S . . O5 O 0.6146(11) 0.1481(9) 0.4259(8) 0.011(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0078(5) 0.0114(5) 0.0120(4) -0.0018(5) -0.0011(6) -0.0012(5) Pb2 0.065(3) 0.0140(17) 0.0108(12) 0.0020(14) 0.000(3) 0.014(3) Fe1 0.0090(11) 0.0052(14) 0.0069(11) -0.0005(12) -0.0012(9) 0.0010(9) Fe2 0.0080(12) 0.0081(13) 0.0059(12) 0.000 0.0006(9) 0.000 Si1 0.0033(15) 0.0072(19) 0.0081(16) 0.0032(18) -0.0016(12) -0.0012(14) O1 0.010(4) 0.004(5) 0.007(5) 0.004(5) -0.001(3) -0.001(4) O2 0.016(5) 0.013(6) 0.010(5) -0.002(5) 0.005(3) -0.003(4) O3 0.008(4) 0.016(6) 0.012(5) -0.001(5) 0.001(3) -0.004(3) O4 0.005(6) 0.015(8) 0.040(8) 0.000 -0.005(5) 0.000 O5 0.011(4) 0.015(5) 0.008(5) 0.003(4) 0.000(3) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.401(9) . ? Pb1 O5 2.406(8) 3_456 ? Pb1 O2 2.415(10) 8_556 ? Pb1 O3 2.498(9) 7_665 ? Pb1 Pb2 3.427(4) 3_456 ? Pb2 O5 2.283(11) . ? Pb2 O3 2.625(10) 5_656 ? Pb2 O2 2.696(11) 8_556 ? Pb2 O2 2.707(10) 6_666 ? Pb2 O3 2.715(10) 7_665 ? Pb2 Pb1 3.427(4) 3_556 ? Fe1 O5 1.964(9) 4_655 ? Fe1 O5 1.964(9) 8 ? Fe1 O1 2.005(7) 4_655 ? Fe1 O1 2.005(7) 8 ? Fe1 O2 2.086(9) 5_655 ? Fe1 O2 2.086(9) . ? Fe2 O5 1.947(8) 4_655 ? Fe2 O5 1.947(8) . ? Fe2 O3 2.075(9) 6_666 ? Fe2 O3 2.075(8) 7_665 ? Fe2 O1 2.091(8) . ? Fe2 O1 2.091(8) 4_655 ? Si1 O1 1.628(8) . ? Si1 O2 1.638(9) . ? Si1 O4 1.649(7) . ? Si1 O3 1.652(10) . ? O1 Fe1 2.005(7) 4_655 ? O2 Pb1 2.415(10) 8 ? O2 Pb2 2.696(11) 8 ? O2 Pb2 2.707(10) 6_556 ? O3 Fe2 2.075(8) 6_556 ? O3 Pb1 2.498(9) 7_655 ? O3 Pb2 2.625(10) 5_656 ? O3 Pb2 2.715(10) 7_655 ? O4 Si1 1.649(7) 4 ? O5 Fe1 1.964(9) 4_655 ? O5 Pb1 2.406(8) 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 O5 Pb1 O5 133.2(3) . 3_456 ? O5 Pb1 O2 72.2(3) . 8_556 ? O5 Pb1 O2 77.1(3) 3_456 8_556 ? O5 Pb1 O3 69.3(3) . 7_665 ? O5 Pb1 O3 74.9(3) 3_456 7_665 ? O2 Pb1 O3 87.3(3) 8_556 7_665 ? O5 Pb1 Pb2 91.6(2) . 3_456 ? O5 Pb1 Pb2 41.6(2) 3_456 3_456 ? O2 Pb1 Pb2 51.7(2) 8_556 3_456 ? O3 Pb1 Pb2 49.6(2) 7_665 3_456 ? O5 Pb2 O3 74.5(3) . 5_656 ? O5 Pb2 O2 68.9(3) . 8_556 ? O3 Pb2 O2 91.4(3) 5_656 8_556 ? O5 Pb2 O2 73.5(3) . 6_666 ? O3 Pb2 O2 79.0(3) 5_656 6_666 ? O2 Pb2 O2 142.4(3) 8_556 6_666 ? O5 Pb2 O3 67.1(3) . 7_665 ? O3 Pb2 O3 141.5(3) 5_656 7_665 ? O2 Pb2 O3 77.7(3) 8_556 7_665 ? O2 Pb2 O3 87.5(3) 6_666 7_665 ? O5 Pb2 Pb1 44.4(2) . 3_556 ? O3 Pb2 Pb1 46.4(2) 5_656 3_556 ? O2 Pb2 Pb1 104.2(2) 8_556 3_556 ? O2 Pb2 Pb1 44.5(2) 6_666 3_556 ? O3 Pb2 Pb1 100.2(2) 7_665 3_556 ? O5 Fe1 O5 180.0(4) 4_655 8 ? O5 Fe1 O1 81.9(3) 4_655 4_655 ? O5 Fe1 O1 98.1(3) 8 4_655 ? O5 Fe1 O1 98.1(3) 4_655 8 ? O5 Fe1 O1 81.9(3) 8 8 ? O1 Fe1 O1 180.0(2) 4_655 8 ? O5 Fe1 O2 88.8(4) 4_655 5_655 ? O5 Fe1 O2 91.2(4) 8 5_655 ? O1 Fe1 O2 90.8(3) 4_655 5_655 ? O1 Fe1 O2 89.2(3) 8 5_655 ? O5 Fe1 O2 91.2(4) 4_655 . ? O5 Fe1 O2 88.8(4) 8 . ? O1 Fe1 O2 89.2(3) 4_655 . ? O1 Fe1 O2 90.8(3) 8 . ? O2 Fe1 O2 180.0(6) 5_655 . ? O5 Fe2 O5 177.4(6) 4_655 . ? O5 Fe2 O3 87.6(3) 4_655 6_666 ? O5 Fe2 O3 94.2(3) . 6_666 ? O5 Fe2 O3 94.2(3) 4_655 7_665 ? O5 Fe2 O3 87.6(3) . 7_665 ? O3 Fe2 O3 94.5(5) 6_666 7_665 ? O5 Fe2 O1 97.9(3) 4_655 . ? O5 Fe2 O1 80.1(3) . . ? O3 Fe2 O1 171.8(3) 6_666 . ? O3 Fe2 O1 91.1(3) 7_665 . ? O5 Fe2 O1 80.1(3) 4_655 4_655 ? O5 Fe2 O1 97.9(3) . 4_655 ? O3 Fe2 O1 91.1(3) 6_666 4_655 ? O3 Fe2 O1 171.8(3) 7_665 4_655 ? O1 Fe2 O1 83.9(4) . 4_655 ? O1 Si1 O2 111.7(4) . . ? O1 Si1 O4 102.8(5) . . ? O2 Si1 O4 113.8(4) . . ? O1 Si1 O3 114.2(4) . . ? O2 Si1 O3 108.1(5) . . ? O4 Si1 O3 106.2(5) . . ? Si1 O1 Fe1 134.0(5) . 4_655 ? Si1 O1 Fe2 124.2(4) . . ? Fe1 O1 Fe2 95.3(3) 4_655 . ? Si1 O2 Fe1 127.9(5) . . ? Si1 O2 Pb1 119.2(5) . 8 ? Fe1 O2 Pb1 97.1(3) . 8 ? Si1 O2 Pb2 120.1(5) . 8 ? Fe1 O2 Pb2 91.1(3) . 8 ? Pb1 O2 Pb2 7.98(14) 8 8 ? Si1 O2 Pb2 106.4(4) . 6_556 ? Fe1 O2 Pb2 114.1(4) . 6_556 ? Pb1 O2 Pb2 83.8(3) 8 6_556 ? Pb2 O2 Pb2 91.1(3) 8 6_556 ? Si1 O3 Fe2 120.9(4) . 6_556 ? Si1 O3 Pb1 111.0(5) . 7_655 ? Fe2 O3 Pb1 97.9(3) 6_556 7_655 ? Si1 O3 Pb2 118.0(4) . 5_656 ? Fe2 O3 Pb2 115.3(4) 6_556 5_656 ? Pb1 O3 Pb2 84.0(3) 7_655 5_656 ? Si1 O3 Pb2 108.7(5) . 7_655 ? Fe2 O3 Pb2 92.3(3) 6_556 7_655 ? Pb1 O3 Pb2 8.75(13) 7_655 7_655 ? Pb2 O3 Pb2 92.4(3) 5_656 7_655 ? Si1 O4 Si1 131.1(9) 4 . ? Fe2 O5 Fe1 101.4(4) . 4_655 ? Fe2 O5 Pb2 110.7(4) . . ? Fe1 O5 Pb2 107.9(4) 4_655 . ? Fe2 O5 Pb1 105.0(4) . . ? Fe1 O5 Pb1 101.0(3) 4_655 . ? Pb2 O5 Pb1 10.71(13) . . ? Fe2 O5 Pb1 119.1(4) . 3_556 ? Fe1 O5 Pb1 123.1(4) 4_655 3_556 ? Pb2 O5 Pb1 93.9(3) . 3_556 ? Pb1 O5 Pb1 104.6(3) . 3_556 ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.960 _refine_diff_density_min -3.036 _refine_diff_density_rms 0.549