data_plumbophyllite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 O44 Pb8 Si16' _chemical_formula_weight 2819.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 13.2083(4) _cell_length_b 9.7832(3) _cell_length_c 8.6545(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1118.32(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 16.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4960 _exptl_absorpt_coefficient_mu 122.181 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0123 _exptl_absorpt_correction_T_max 0.1937 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13812 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1268 _reflns_number_gt 1183 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0196P)^2^+9.4378P] 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 1268 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Pb Pb 0.531312(14) 0.18997(2) 0.46446(2) 0.01220(8) Uani 1 1 d . . . Si1 Si 0.27492(10) 0.18248(13) 0.31842(17) 0.0071(3) Uani 1 1 d . . . Si2 Si 0.30435(10) 0.07550(14) 0.63975(16) 0.0072(3) Uani 1 1 d . . . O1 O 0.3926(3) 0.2162(4) 0.3017(5) 0.0134(8) Uani 1 1 d . . . O2 O 0.2433(3) -0.0594(4) 0.6989(4) 0.0118(7) Uani 1 1 d . . . O3 O 0.2996(3) 0.1899(4) 0.7771(5) 0.0135(8) Uani 1 1 d . . . O4 O 0.2416(3) 0.1370(4) 0.4927(4) 0.0108(7) Uani 1 1 d . . . O5 O 0.4179(3) 0.0378(4) 0.5937(5) 0.0140(8) Uani 1 1 d . . . OW O 0.4610(7) 0.4439(13) 0.617(2) 0.071(5) Uani 0.50 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 Pb 0.00956(12) 0.01353(12) 0.01351(13) -0.00134(7) 0.00015(7) 0.00025(7) Si1 0.0071(6) 0.0067(6) 0.0075(7) 0.0005(5) 0.0004(5) 0.0009(5) Si2 0.0070(6) 0.0070(6) 0.0075(7) 0.0002(5) 0.0012(5) 0.0015(5) O1 0.0112(18) 0.0168(18) 0.0123(19) 0.0021(14) 0.0002(14) -0.0013(15) O2 0.0115(17) 0.0109(17) 0.013(2) 0.0034(14) 0.0008(14) -0.0011(15) O3 0.0149(19) 0.0128(18) 0.013(2) -0.0027(14) -0.0049(15) 0.0058(15) O4 0.0119(19) 0.0141(18) 0.0063(17) 0.0043(14) 0.0017(14) 0.0011(15) O5 0.0107(18) 0.0120(18) 0.019(2) 0.0025(15) 0.0049(15) 0.0037(14) OW 0.012(5) 0.043(7) 0.159(15) -0.026(8) 0.043(7) 0.007(5) _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 Pb O1 2.325(4) . ? Pb O5 2.381(4) 5_656 ? Pb O5 2.390(4) . ? Pb O1 2.526(4) 7_656 ? Pb OW 2.963(11) . ? Si1 O1 1.595(4) . ? Si1 O3 1.629(4) 4_554 ? Si1 O4 1.633(4) . ? Si1 O2 1.642(4) 3_554 ? Si2 O5 1.595(4) . ? Si2 O2 1.629(4) . ? Si2 O4 1.634(4) . ? Si2 O3 1.634(4) . ? O1 Pb 2.526(4) 7_656 ? O2 Si1 1.642(4) 3 ? O3 Si1 1.629(4) 4 ? O5 Pb 2.381(4) 5_656 ? OW OW 2.52(4) 7_657 ? OW OW 2.53(3) 5_666 ? OW O2 2.789(9) 2 ? 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 O1 Pb O5 101.38(13) . 5_656 ? O1 Pb O5 81.85(13) . . ? O5 Pb O5 72.11(14) 5_656 . ? O1 Pb O1 75.52(14) . 7_656 ? O5 Pb O1 77.89(13) 5_656 7_656 ? O5 Pb O1 137.68(13) . 7_656 ? O1 Pb OW 86.0(3) . . ? O5 Pb OW 165.3(4) 5_656 . ? O5 Pb OW 96.7(3) . . ? O1 Pb OW 116.5(3) 7_656 . ? O1 Si1 O3 114.2(2) . 4_554 ? O1 Si1 O4 113.8(2) . . ? O3 Si1 O4 104.4(2) 4_554 . ? O1 Si1 O2 110.0(2) . 3_554 ? O3 Si1 O2 105.6(2) 4_554 3_554 ? O4 Si1 O2 108.3(2) . 3_554 ? O5 Si2 O2 110.9(2) . . ? O5 Si2 O4 111.6(2) . . ? O2 Si2 O4 106.9(2) . . ? O5 Si2 O3 112.1(2) . . ? O2 Si2 O3 107.9(2) . . ? O4 Si2 O3 107.2(2) . . ? Si1 O1 Pb 133.6(2) . . ? Si1 O1 Pb 116.7(2) . 7_656 ? Pb O1 Pb 103.16(14) . 7_656 ? Si2 O2 Si1 131.8(2) . 3 ? Si1 O3 Si2 135.1(2) 4 . ? Si1 O4 Si2 133.1(2) . . ? Si2 O5 Pb 122.3(2) . 5_656 ? Si2 O5 Pb 124.2(2) . . ? Pb O5 Pb 107.90(14) 5_656 . ? OW OW OW 124.5(8) 7_657 5_666 ? OW OW O2 99.5(7) 7_657 2 ? OW OW O2 127.1(9) 5_666 2 ? OW OW Pb 106.2(4) 7_657 . ? OW OW Pb 83.0(6) 5_666 . ? O2 OW Pb 114.0(4) 2 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.900 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.201