data_pbbep200-2a _audit_creation_date 2013-06-24 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _publ_contact_author_name ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Be2 O8 P2 Pb' _chemical_formula_sum 'Be2 O8 P2 Pb' _chemical_formula_weight 415.15 _chemical_melting_point ? _chemical_oxdiff_formula 'Pb Be2 P2 O8' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Be' 'Be' 0.0005 0.0002 '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' 'P' 'P' 0.1023 0.0942 '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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 8.08884(14) _cell_length_b 9.01969(12) _cell_length_c 8.39135(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.1221(14) _cell_angle_gamma 90.00 _cell_volume 612.222(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13334 _cell_measurement_temperature 293.0 _cell_measurement_theta_max 28.9693 _cell_measurement_theta_min 3.3093 _exptl_absorpt_coefficient_mu 28.086 _exptl_absorpt_correction_T_max 0.262 _exptl_absorpt_correction_T_min 0.138 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) 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_crystal_colour block _exptl_crystal_colour_lustre ? _exptl_crystal_colour_modifier ? _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 4.504 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.1106 _exptl_crystal_size_mid 0.0941 _exptl_crystal_size_min 0.0646 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0170 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 26291 _diffrn_reflns_theta_full 29.03 _diffrn_reflns_theta_max 29.03 _diffrn_reflns_theta_min 3.32 _diffrn_ambient_temperature 293.0 _diffrn_detector_area_resol_mean 16.0087 _diffrn_measured_fraction_theta_full 0.9978 _diffrn_measured_fraction_theta_max 0.9776 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -87.00 13.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -77.0000 -60.0000 100 #__ type_ start__ end____ width___ exp.time_ 2 omega -68.00 -8.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -57.0000 -180.0000 60 #__ type_ start__ end____ width___ exp.time_ 3 omega 2.00 80.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 57.0000 150.0000 78 #__ type_ start__ end____ width___ exp.time_ 4 omega 11.00 88.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 57.0000 60.0000 77 #__ type_ start__ end____ width___ exp.time_ 5 omega -23.00 62.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -101.0000 -87.0000 85 #__ type_ start__ end____ width___ exp.time_ 6 omega -46.00 32.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -57.0000 60.0000 78 #__ type_ start__ end____ width___ exp.time_ 7 omega -50.00 48.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -77.0000 0.0000 98 #__ type_ start__ end____ width___ exp.time_ 8 omega -44.00 32.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -57.0000 150.0000 76 #__ type_ start__ end____ width___ exp.time_ 9 omega 47.00 81.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -131.0000 165.1146 34 #__ type_ start__ end____ width___ exp.time_ 10 omega -93.00 -35.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -178.0000 60.0000 58 #__ type_ start__ end____ width___ exp.time_ 11 omega -90.00 9.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -37.0000 30.0000 99 #__ type_ start__ end____ width___ exp.time_ 12 omega -86.00 4.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -57.0000 150.0000 90 #__ type_ start__ end____ width___ exp.time_ 13 omega -94.00 -32.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 178.0000 -150.0000 62 #__ type_ start__ end____ width___ exp.time_ 14 omega -25.00 61.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -99.0000 90.0000 86 #__ type_ start__ end____ width___ exp.time_ 15 omega -51.00 49.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -77.0000 -180.0000 100 #__ type_ start__ end____ width___ exp.time_ 16 omega 35.00 95.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 178.0000 120.0000 60 #__ type_ start__ end____ width___ exp.time_ 17 omega -82.00 -5.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 137.0000 -2.2783 77 #__ type_ start__ end____ width___ exp.time_ 18 omega -22.00 25.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - -17.0725 -101.0000 162.0000 47 #__ type_ start__ end____ width___ exp.time_ 19 omega -49.00 41.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -57.0000 30.0000 90 #__ type_ start__ end____ width___ exp.time_ 20 omega -2.00 88.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 57.0000 30.0000 90 #__ type_ start__ end____ width___ exp.time_ 21 omega 1.00 81.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -131.0000 165.1146 80 #__ type_ start__ end____ width___ exp.time_ 22 omega -2.00 88.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 57.0000 -180.0000 90 #__ type_ start__ end____ width___ exp.time_ 23 omega -25.00 61.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 -99.0000 -60.0000 86 #__ type_ start__ end____ width___ exp.time_ 24 omega -54.00 92.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 0.0000 -150.0000 146 #__ type_ start__ end____ width___ exp.time_ 25 omega -54.00 92.00 1.0000 12.4900 omega____ theta____ kappa____ phi______ frames - 19.4162 0.0000 -180.0000 146 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0070848000 _diffrn_orient_matrix_UB_12 0.0614272000 _diffrn_orient_matrix_UB_13 0.0523004000 _diffrn_orient_matrix_UB_21 0.0500351000 _diffrn_orient_matrix_UB_22 0.0429110000 _diffrn_orient_matrix_UB_23 -0.0517731000 _diffrn_orient_matrix_UB_31 -0.0716702000 _diffrn_orient_matrix_UB_32 0.0238656000 _diffrn_orient_matrix_UB_33 -0.0415706000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1507 _reflns_number_total 1589 _reflns_odcompleteness_completeness 99.78 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.722 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.161 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0154 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+1.2384P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0303 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.756214(15) 0.592730(13) 0.106101(14) 0.01170(5) Uani 1 1 d . . . P1 P 0.56368(10) 0.91347(8) 0.23133(9) 0.00633(15) Uani 1 1 d . . . P2 P 0.93382(10) 0.19688(8) 0.06753(9) 0.00615(15) Uani 1 1 d . . . Be1 Be 0.5761(5) 0.1935(4) 0.0641(5) 0.0087(8) Uani 1 1 d . . . Be2 Be 1.0725(5) 0.4184(5) 0.2730(5) 0.0089(8) Uani 1 1 d . . . O1 O 0.5175(3) 1.0730(2) 0.1966(3) 0.0099(5) Uani 1 1 d . . . O2 O 0.5554(3) 0.8154(2) 0.0834(2) 0.0088(4) Uani 1 1 d . . . O3 O 0.7412(3) 0.8980(2) 0.2997(3) 0.0111(5) Uani 1 1 d . . . O4 O 0.5538(3) 0.3612(2) 0.1369(3) 0.0094(4) Uani 1 1 d . . . O5 O 0.9533(3) 0.3570(2) 0.1299(3) 0.0095(4) Uani 1 1 d . . . O6 O 0.9375(3) 0.8204(2) 0.0666(3) 0.0093(4) Uani 1 1 d . . . O7 O 1.0203(3) 0.5885(2) 0.2978(3) 0.0107(5) Uani 1 1 d . . . O8 O 0.7621(3) 0.1689(2) 0.0045(3) 0.0106(5) 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 0.01130(7) 0.01026(7) 0.01354(7) 0.00020(5) 0.00041(4) -0.00065(5) P1 0.0063(4) 0.0056(4) 0.0071(4) 0.0001(3) 0.0005(3) 0.0002(3) P2 0.0068(4) 0.0040(3) 0.0077(3) -0.0001(3) 0.0002(3) -0.0004(3) Be1 0.008(2) 0.0091(19) 0.0094(18) -0.0017(15) -0.0002(15) 0.0009(15) Be2 0.0046(19) 0.0113(19) 0.0109(19) 0.0012(15) 0.0014(15) 0.0014(15) O1 0.0139(12) 0.0044(10) 0.0115(11) 0.0015(8) 0.0040(9) 0.0021(9) O2 0.0091(11) 0.0093(10) 0.0080(10) -0.0019(8) 0.0004(8) 0.0017(9) O3 0.0063(12) 0.0181(12) 0.0088(11) -0.0004(9) 0.0004(9) -0.0010(9) O4 0.0107(12) 0.0070(10) 0.0104(11) -0.0023(8) 0.0038(9) 0.0000(9) O5 0.0096(12) 0.0060(10) 0.0129(11) -0.0003(9) -0.0012(9) 0.0020(9) O6 0.0087(11) 0.0083(10) 0.0109(10) -0.0015(9) 0.0018(9) -0.0025(8) O7 0.0144(12) 0.0078(11) 0.0100(11) -0.0023(9) -0.0017(9) 0.0005(9) O8 0.0076(11) 0.0118(11) 0.0125(11) -0.0050(9) 0.0000(9) -0.0008(9) _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 O4 2.666(2) . ? Pb1 O7 2.672(2) . ? Pb1 O5 2.665(2) . ? Pb1 O2 2.590(2) . ? Pb1 O6 2.545(2) . ? Pb1 O3 2.575(2) 4_575 ? P1 O4 1.534(2) 2_655 ? P1 O2 1.525(2) . ? P1 O1 1.515(2) . ? P1 O3 1.551(2) . ? P2 O7 1.539(2) 2_745 ? P2 O5 1.544(2) . ? P2 O6 1.543(2) 3_765 ? P2 O8 1.507(2) . ? O4 Be1 1.642(4) . ? O2 Be1 1.632(4) 3_665 ? O1 Be1 1.626(5) 1_565 ? O8 Be1 1.602(5) . ? O7 Be2 1.605(4) . ? O5 Be2 1.635(5) . ? O6 Be2 1.612(5) 2_755 ? O3 Be2 1.637(5) 2_755 ? 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 O4 Pb1 O7 114.88(7) . . ? O5 Pb1 O4 74.64(7) . . ? O5 Pb1 O7 57.72(7) . . ? O2 Pb1 O4 103.26(7) . . ? O2 Pb1 O7 123.78(7) . . ? O2 Pb1 O5 177.89(7) . . ? O6 Pb1 O4 176.82(7) . . ? O6 Pb1 O7 68.27(7) . . ? O6 Pb1 O5 107.98(7) . . ? O6 Pb1 O2 74.12(7) . . ? O6 Pb1 O3 82.52(7) . 4_575 ? O3 Pb1 O4 95.43(7) 4_575 . ? O3 Pb1 O7 129.62(7) 4_575 . ? O3 Pb1 O5 97.34(7) 4_575 . ? O3 Pb1 O2 82.71(7) 4_575 . ? O4 P1 O3 106.28(13) 2_655 . ? O2 P1 O4 112.47(13) . 2_655 ? O2 P1 O3 106.71(13) . . ? O1 P1 O4 106.11(13) . 2_655 ? O1 P1 O2 112.58(13) . . ? O1 P1 O3 112.60(13) . . ? O7 P2 O5 108.73(12) 2_745 . ? O7 P2 O6 108.04(13) 2_745 3_765 ? O6 P2 O5 105.86(12) 3_765 . ? O8 P2 O7 111.84(13) . 2_745 ? O8 P2 O5 111.67(13) . . ? O8 P2 O6 110.47(12) . 3_765 ? P1 O4 Pb1 102.17(10) 2_645 . ? P1 O4 Be1 128.3(2) 2_645 . ? Be1 O4 Pb1 128.15(18) . . ? P2 O7 Pb1 128.62(12) 2_755 . ? P2 O7 Be2 129.7(2) 2_755 . ? Be2 O7 Pb1 98.40(18) . . ? P2 O5 Pb1 131.32(12) . . ? P2 O5 Be2 128.7(2) . . ? Be2 O5 Pb1 97.84(17) . . ? P1 O2 Pb1 111.31(11) . . ? P1 O2 Be1 132.3(2) . 3_665 ? Be1 O2 Pb1 115.18(18) 3_665 . ? P1 O1 Be1 133.9(2) . 1_565 ? P2 O6 Pb1 113.79(11) 3_765 . ? P2 O6 Be2 134.4(2) 3_765 2_755 ? Be2 O6 Pb1 107.68(18) 2_755 . ? P1 O3 Pb1 114.07(12) . 4_576 ? P1 O3 Be2 134.8(2) . 2_755 ? Be2 O3 Pb1 109.08(18) 2_755 4_576 ? P2 O8 Be1 137.1(2) . . ? O2 Be1 O4 104.8(3) 3_665 . ? O1 Be1 O4 109.2(3) 1_545 . ? O1 Be1 O2 107.2(3) 1_545 3_665 ? O8 Be1 O4 110.3(3) . . ? O8 Be1 O2 111.6(3) . 3_665 ? O8 Be1 O1 113.4(3) . 1_545 ? O7 Be2 O5 105.3(3) . . ? O7 Be2 O6 113.7(3) . 2_745 ? O7 Be2 O3 113.5(3) . 2_745 ? O5 Be2 O3 103.3(3) . 2_745 ? O6 Be2 O5 113.4(3) 2_745 . ? O6 Be2 O3 107.3(3) 2_745 2_745 ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 11 1 1 0.0341 11.0000 1.0000 1.0000 0.0358 0.5415 -0.8061 -5 7 -9 0.0337 -5.0000 7.0000 -9.0000 -0.0053 0.5162 0.8995 9 -4 6 0.0345 9.0000 -4.0000 6.0000 0.0043 -0.0320 -0.9899 6 11 -2 0.0426 6.0000 11.0000 -2.0000 0.5286 0.8758 -0.0844 9 -1 7 0.0306 9.0000 -1.0000 7.0000 0.2409 0.0450 -0.9599 -3 11 4 0.0435 -3.0000 11.0000 4.0000 0.9062 0.1148 0.3112 6 -2 10 0.0301 6.0000 -2.0000 10.0000 0.3576 -0.3033 -0.8935 -6 -3 10 0.0443 -6.0000 -3.0000 10.0000 0.3812 -0.9467 -0.0573 -8 4 -8 0.0302 -8.0000 4.0000 -8.0000 -0.1160 0.1855 1.0014 6 -7 8 0.0366 6.0000 -7.0000 8.0000 -0.0541 -0.4144 -0.9296 -4 -12 2 0.0427 -4.0000 -12.0000 2.0000 -0.6042 -0.8186 -0.0828 1 -9 -9 0.0445 1.0000 -9.0000 -9.0000 -1.0306 0.1298 0.0877 6 1 -10 0.0410 6.0000 1.0000 -10.0000 -0.5041 0.8609 0.0096