#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/30/8103050.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8103050 loop_ _publ_author_name 'Wilhelm Klein' 'Martin Jansen' _publ_section_title ; Refinement of the crystal structure of dilead(II) oxide chromate(VI), Pb2O(CrO4) ; _journal_issue 2 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 219 _journal_volume 225 _journal_year 2010 _chemical_formula_moiety 'Cr O5 Pb2' _chemical_formula_structural 'Pb2 O Cr O4' _chemical_formula_sum 'Cr O5 Pb2' _chemical_formula_weight 546.38 _chemical_name_common 'Lead Chromate Oxide' _chemical_name_systematic ' Dilead(II) Chromate(VI) Oxide' _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 115.189(17) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.063(3) _cell_length_b 5.7035(9) _cell_length_c 7.1719(17) _cell_measurement_reflns_used 6180 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.62 _cell_measurement_theta_min 3.10 _cell_volume 520.5(2) _computing_cell_refinement 'STOE X-AREA (Stoe & Cie, 2002)' _computing_data_collection 'STOE X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'STOE X-RED (Stoe & Cie, 2002)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'omega scan' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2723 _diffrn_reflns_theta_full 29.65 _diffrn_reflns_theta_max 29.65 _diffrn_reflns_theta_min 3.14 _exptl_absorpt_coefficient_mu 66.501 _exptl_absorpt_correction_T_max 0.001 _exptl_absorpt_correction_T_min 0.001 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-SHAPE (Stoe & Cie, 2002)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 6.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 2.356 _refine_diff_density_min -3.563 _refine_diff_density_rms 0.535 _refine_ls_extinction_coef 0.0051(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_matrix_type full _refine_ls_number_parameters 46 _refine_ls_number_reflns 796 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0301 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.0780 _reflns_number_gt 729 _reflns_number_total 796 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file 710043.cff _[local]_cod_data_source_block pb2ocro4 _cod_original_cell_volume 520.55(19) _cod_database_code 8103050 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 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 0.02039(3) 0.0000 0.26693(5) 0.01297(18) Uani 1 2 d S . . Pb2 Pb 0.35691(3) 0.0000 0.88721(5) 0.01470(18) Uani 1 2 d S . . Cr Cr 0.32999(12) 0.0000 0.3405(2) 0.0109(3) Uani 1 2 d S . . O1 O 0.4074(7) 0.0000 0.5928(13) 0.0271(19) Uani 1 2 d S . . O2 O 0.2043(8) 0.0000 0.2958(15) 0.033(2) Uani 1 2 d S . . O3 O 0.3517(5) 0.2325(12) 0.2272(9) 0.0231(12) Uani 1 1 d . . . O4 O 0.0000 0.2474(14) 0.0000 0.0134(13) 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 0.0126(2) 0.0178(3) 0.0096(2) 0.000 0.00575(16) 0.000 Pb2 0.0098(2) 0.0173(3) 0.0166(2) 0.000 0.00518(16) 0.000 Cr 0.0071(6) 0.0140(8) 0.0114(6) 0.000 0.0039(6) 0.000 O1 0.024(4) 0.035(5) 0.018(3) 0.000 0.005(3) 0.000 O2 0.024(4) 0.043(6) 0.036(5) 0.000 0.016(4) 0.000 O3 0.020(2) 0.021(3) 0.029(3) 0.007(3) 0.011(2) -0.002(2) O4 0.011(3) 0.015(4) 0.014(3) 0.000 0.005(2) 0.000 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' Cr Cr 0.3209 0.6236 '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' 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 O4 75.8(3) 5 . ? O4 Pb1 O2 80.05(18) 5 . ? O4 Pb1 O2 80.05(18) . . ? O4 Pb1 O3 76.99(15) 5 3_445 ? O4 Pb1 O3 117.48(14) . 3_445 ? O2 Pb1 O3 145.98(14) . 3_445 ? O4 Pb1 O3 117.48(14) 5 4_455 ? O4 Pb1 O3 76.99(15) . 4_455 ? O2 Pb1 O3 145.98(14) . 4_455 ? O3 Pb1 O3 67.9(3) 3_445 4_455 ? O4 Pb1 Pb1 37.92(16) 5 5 ? O4 Pb1 Pb1 37.92(16) . 5 ? O2 Pb1 Pb1 77.3(2) . 5 ? O3 Pb1 Pb1 98.62(13) 3_445 5 ? O3 Pb1 Pb1 98.62(13) 4_455 5 ? O4 Pb1 Pb1 139.15(14) 5 5_556 ? O4 Pb1 Pb1 139.15(14) . 5_556 ? O2 Pb1 Pb1 119.1(2) . 5_556 ? O3 Pb1 Pb1 67.97(13) 3_445 5_556 ? O3 Pb1 Pb1 67.97(13) 4_455 5_556 ? Pb1 Pb1 Pb1 163.53(2) 5 5_556 ? O4 Pb2 O4 76.7(3) 7_556 3_546 ? O4 Pb2 O1 77.20(16) 7_556 . ? O4 Pb2 O1 77.20(16) 3_546 . ? O4 Pb2 Pb2 38.34(15) 7_556 5_657 ? O4 Pb2 Pb2 38.34(16) 3_546 5_657 ? O1 Pb2 Pb2 73.6(2) . 5_657 ? O3 Cr O3 106.9(5) 2 . ? O3 Cr O2 108.1(3) 2 . ? O3 Cr O2 108.1(3) . . ? O3 Cr O1 111.2(3) 2 . ? O3 Cr O1 111.2(3) . . ? O2 Cr O1 111.1(5) . . ? Cr O1 Pb2 128.9(5) . . ? Cr O2 Pb1 174.2(6) . . ? Cr O3 Pb1 137.0(3) . 3 ? Pb1 O4 Pb1 104.2(3) . 5 ? Pb1 O4 Pb2 107.98(2) . 7_556 ? Pb1 O4 Pb2 116.995(17) 5 7_556 ? Pb1 O4 Pb2 116.994(17) . 3_454 ? Pb1 O4 Pb2 107.98(2) 5 3_454 ? Pb2 O4 Pb2 103.3(3) 7_556 3_454 ? 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 2.296(5) 5 ? Pb1 O4 2.296(5) . ? Pb1 O2 2.505(10) . ? Pb1 O3 2.731(6) 3_445 ? Pb1 O3 2.731(6) 4_455 ? Pb1 Pb1 3.6221(11) 5 ? Pb1 Pb1 3.6245(10) 5_556 ? Pb2 O4 2.322(5) 7_556 ? Pb2 O4 2.322(5) 3_546 ? Pb2 O1 2.498(9) . ? Pb2 Pb2 3.6431(12) 5_657 ? Cr O3 1.650(6) 2 ? Cr O3 1.650(6) . ? Cr O2 1.657(10) . ? Cr O1 1.668(9) . ? O3 Pb1 2.731(6) 3 ? O4 Pb1 2.296(5) 5 ? O4 Pb2 2.322(5) 7_556 ? O4 Pb2 2.322(5) 3_454 ?