#------------------------------------------------------------------------------ #$Date: 2012-01-04 11:21:40 +0000 (Wed, 04 Jan 2012) $ #$Revision: 31986 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/42/2204242.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204242 loop_ _publ_author_name 'Yao, Jiyong' 'Ibers, James A.' _publ_section_title ; RbPbPS~4~ ; _journal_issue 9 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i108 _journal_page_last i110 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'Rb Pb P S4' _chemical_formula_moiety 'P Pb Rb S4' _chemical_formula_structural 'Rb Pb P S4' _chemical_formula_sum 'P Pb Rb S4' _chemical_formula_weight 451.87 _chemical_name_systematic ; Rubidium lead phosphorus tetrasulfide ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P21 21 21' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.3987(7) _cell_length_b 6.6899(7) _cell_length_c 17.2975(19) _cell_measurement_reflns_used 7200 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 28.82 _cell_measurement_theta_min 2.35 _cell_volume 740.45(14) _computing_cell_refinement 'SAINT-Plus (Bruker, 2003)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_data_reduction SAINT-Plus _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2003)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.957 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 8784 _diffrn_reflns_theta_full 28.82 _diffrn_reflns_theta_max 28.82 _diffrn_reflns_theta_min 2.35 _diffrn_standards_decay_% <1 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 30.543 _exptl_absorpt_correction_T_max 0.60284 _exptl_absorpt_correction_T_min 0.04738 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; face indexed (SHELXTL; Sheldrick, 2003) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 4.053 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.016 _refine_diff_density_max 2.114 _refine_diff_density_min -1.568 _refine_ls_abs_structure_details 'Flack (1983): 704 Friedel pairs' _refine_ls_abs_structure_Flack 0.550(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.388 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 65 _refine_ls_number_reflns 1807 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.388 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0200 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.02P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0491 _reflns_number_gt 1759 _reflns_number_total 1807 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm6026.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 '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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol Rb 0.02119(9) 0.00342(8) 0.04319(3) 0.02110(13) Uani d 1 Rb Pb 0.28891(3) 0.47494(3) 0.230842(12) 0.01418(7) Uani d 1 Pb P 0.2189(2) 0.01031(19) 0.34791(8) 0.0100(3) Uani d 1 P S1 0.1533(2) 0.0316(2) 0.23134(8) 0.0131(3) Uani d 1 S S2 0.3990(2) 0.25142(19) 0.37520(10) 0.0142(3) Uani d 1 S S3 0.6101(3) 0.25876(19) 0.13163(10) 0.0134(3) Uani d 1 S S4 0.0472(2) 0.5039(2) 0.08806(8) 0.0135(3) Uani d 1 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rb 0.0374(3) 0.0118(3) 0.0142(3) -0.0009(2) 0.0062(2) -0.0007(2) Pb 0.01344(10) 0.01498(11) 0.01413(11) 0.00007(8) -0.00011(8) 0.00066(9) P 0.0121(6) 0.0077(6) 0.0103(6) -0.0002(6) 0.0001(5) 0.0003(5) S1 0.0152(6) 0.0152(6) 0.0089(6) -0.0015(5) 0.0010(5) 0.0003(7) S2 0.0181(8) 0.0069(6) 0.0178(8) -0.0015(5) -0.0035(7) 0.0000(5) S3 0.0176(7) 0.0070(6) 0.0155(8) -0.0013(5) 0.0000(6) 0.0004(5) S4 0.0158(6) 0.0130(7) 0.0116(6) 0.0004(6) 0.0045(5) 0.0004(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rb S1 . 3.3680(15) y Rb S2 2_554 3.4075(17) y Rb S4 1_545 3.4345(16) y Rb S4 . 3.4412(16) y Rb S3 4_455 3.4639(17) y Rb S2 3_545 3.4734(17) y Rb S3 1_455 3.4898(17) y Rb P 2_554 3.7660(15) ? Rb S4 4_455 3.7887(14) y Rb Pb 3_545 4.3877(7) ? Rb Rb 4 4.8324(9) ? Rb Rb 4_455 4.8324(9) ? Pb S4 . 2.9204(14) y Pb S1 3 2.9290(14) y Pb S2 . 2.9945(16) y Pb S3 . 3.0430(16) y Pb S1 . 3.0900(14) y Pb S3 3_655 3.1116(16) y Pb S2 3_655 3.2823(16) y Pb P 3_655 3.4392(14) ? Pb P 3 3.5315(14) ? Pb Pb 3_655 4.3504(4) ? Pb Pb 3_645 4.3504(4) ? Pb Rb 3 4.3877(7) ? P S4 3_545 2.0320(18) y P S2 . 2.038(2) y P S3 3_645 2.0381(19) y P S1 . 2.0644(19) y P Pb 3_645 3.4392(14) ? P Pb 3_545 3.5315(14) ? P Rb 2 3.7660(15) ? S1 Pb 3_545 2.9290(13) ? S2 Pb 3_645 3.2823(16) ? S2 Rb 2 3.4075(17) ? S2 Rb 3 3.4733(17) ? S3 P 3_655 2.0381(19) ? S3 Pb 3_645 3.1116(16) ? S3 Rb 4 3.4640(17) ? S3 Rb 1_655 3.4898(17) ? S4 P 3 2.0320(18) ? S4 Rb 1_565 3.4345(16) ? S4 Rb 4 3.7888(14) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Rb S2 . 2_554 144.54(4) ? S1 Rb S4 . 1_545 79.86(4) ? S2 Rb S4 2_554 1_545 72.46(3) ? S1 Rb S4 . . 73.46(3) ? S2 Rb S4 2_554 . 132.22(4) ? S4 Rb S4 1_545 . 153.30(5) ? S1 Rb S3 . 4_455 140.96(4) ? S2 Rb S3 2_554 4_455 57.37(3) ? S4 Rb S3 1_545 4_455 129.51(4) ? S4 Rb S3 . 4_455 75.05(3) ? S1 Rb S2 . 3_545 80.14(4) ? S2 Rb S2 2_554 3_545 102.70(4) ? S4 Rb S2 1_545 3_545 58.23(3) ? S4 Rb S2 . 3_545 114.71(3) ? S3 Rb S2 4_455 3_545 134.82(4) ? S1 Rb S3 . 1_455 74.82(4) ? S2 Rb S3 2_554 1_455 137.03(4) ? S4 Rb S3 1_545 1_455 114.44(3) ? S4 Rb S3 . 1_455 57.41(3) ? S3 Rb S3 4_455 1_455 106.36(4) ? S2 Rb S3 3_545 1_455 58.39(3) ? S1 Rb P . 2_554 139.22(4) ? S2 Rb P 2_554 2_554 32.52(3) ? S4 Rb P 1_545 2_554 99.07(3) ? S4 Rb P . 2_554 101.81(3) ? S3 Rb P 4_455 2_554 32.40(3) ? S2 Rb P 3_545 2_554 133.99(4) ? S3 Rb P 1_455 2_554 137.56(4) ? S1 Rb S4 . 4_455 141.33(3) ? S2 Rb S4 2_554 4_455 66.58(4) ? S4 Rb S4 1_545 4_455 99.30(3) ? S4 Rb S4 . 4_455 100.75(3) ? S3 Rb S4 4_455 4_455 67.31(4) ? S2 Rb S4 3_545 4_455 67.52(4) ? S3 Rb S4 1_455 4_455 70.47(4) ? P Rb S4 2_554 4_455 79.38(3) ? S1 Rb Pb . 3_545 41.85(2) ? S2 Rb Pb 2_554 3_545 143.68(3) ? S4 Rb Pb 1_545 3_545 77.19(2) ? S4 Rb Pb . 3_545 82.14(2) ? S3 Rb Pb 4_455 3_545 150.68(3) ? S2 Rb Pb 3_545 3_545 42.84(3) ? S3 Rb Pb 1_455 3_545 44.75(3) ? P Rb Pb 2_554 3_545 176.05(3) ? S4 Rb Pb 4_455 3_545 99.86(3) ? S1 Rb Rb . 4 95.41(3) ? S2 Rb Rb 2_554 4 88.78(3) ? S4 Rb Rb 1_545 4 134.59(3) ? S4 Rb Rb . 4 51.20(3) ? S3 Rb Rb 4_455 4 46.20(3) ? S2 Rb Rb 3_545 4 165.82(3) ? S3 Rb Rb 1_455 4 107.48(3) ? P Rb Rb 2_554 4 56.43(2) ? S4 Rb Rb 4_455 4 110.71(3) ? Pb Rb Rb 3_545 4 127.191(19) ? S1 Rb Rb . 4_455 115.26(3) ? S2 Rb Rb 2_554 4_455 100.20(3) ? S4 Rb Rb 1_545 4_455 140.01(3) ? S4 Rb Rb . 4_455 55.77(3) ? S3 Rb Rb 4_455 4_455 61.66(3) ? S2 Rb Rb 3_545 4_455 86.82(3) ? S3 Rb Rb 1_455 4_455 45.76(3) ? P Rb Rb 2_554 4_455 91.82(3) ? S4 Rb Rb 4_455 4_455 45.06(2) ? Pb Rb Rb 3_545 4_455 90.325(13) ? Rb Rb Rb 4 4_455 82.914(19) ? S4 Pb S1 . 3 70.65(4) ? S4 Pb S2 . . 149.64(4) ? S1 Pb S2 3 . 96.07(4) ? S4 Pb S3 . . 84.97(4) ? S1 Pb S3 3 . 147.13(4) ? S2 Pb S3 . . 94.25(4) ? S4 Pb S1 . . 85.27(4) ? S1 Pb S1 3 . 81.51(3) ? S2 Pb S1 . . 65.45(4) ? S3 Pb S1 . . 74.64(4) ? S4 Pb S3 . 3_655 135.72(4) ? S1 Pb S3 3 3_655 87.19(4) ? S2 Pb S3 . 3_655 67.56(4) ? S3 Pb S3 . 3_655 125.51(2) ? S1 Pb S3 . 3_655 129.93(4) ? S4 Pb S2 . 3_655 79.17(4) ? S1 Pb S2 3 3_655 129.76(4) ? S2 Pb S2 . 3_655 127.17(2) ? S3 Pb S2 . 3_655 62.73(3) ? S1 Pb S2 . 3_655 135.50(4) ? S3 Pb S2 3_655 3_655 87.53(4) ? S4 Pb P . 3_655 98.36(3) ? S1 Pb P 3 3_655 164.61(4) ? S2 Pb P . 3_655 98.58(4) ? S3 Pb P . 3_655 36.00(4) ? S1 Pb P . 3_655 108.92(3) ? S3 Pb P 3_655 3_655 94.05(4) ? S2 Pb P 3_655 3_655 35.20(3) ? S4 Pb P . 3 35.12(3) ? S1 Pb P 3 3 35.75(4) ? S2 Pb P . 3 124.86(4) ? S3 Pb P . 3 115.83(4) ? S1 Pb P . 3 78.87(3) ? S3 Pb P 3_655 3 116.43(4) ? S2 Pb P 3_655 3 107.85(4) ? P Pb P 3_655 3 133.25(4) ? S4 Pb Pb . 3_655 113.99(3) ? S1 Pb Pb 3 3_655 117.80(3) ? S2 Pb Pb . 3_655 96.36(3) ? S3 Pb Pb . 3_655 91.83(3) ? S1 Pb Pb . 3_655 155.77(3) ? S3 Pb Pb 3_655 3_655 44.38(3) ? S2 Pb Pb 3_655 3_655 43.45(3) ? P Pb Pb 3_655 3_655 55.87(2) ? P Pb Pb 3 3_655 125.36(2) ? S4 Pb Pb . 3_645 120.58(3) ? S1 Pb Pb 3 3_645 131.72(3) ? S2 Pb Pb . 3_645 48.92(3) ? S3 Pb Pb . 3_645 45.66(3) ? S1 Pb Pb . 3_645 55.66(3) ? S3 Pb Pb 3_655 3_645 102.93(3) ? S2 Pb Pb 3_655 3_645 98.08(3) ? P Pb Pb 3_655 3_645 62.91(2) ? P Pb Pb 3 3_645 132.98(2) ? Pb Pb Pb 3_655 3_645 100.508(12) ? S4 Pb Rb . 3 120.73(3) ? S1 Pb Rb 3 3 50.10(3) ? S2 Pb Rb . 3 52.07(3) ? S3 Pb Rb . 3 145.94(3) ? S1 Pb Rb . 3 84.96(3) ? S3 Pb Rb 3_655 3 52.15(3) ? S2 Pb Rb 3_655 3 138.46(3) ? P Pb Rb 3_655 3 139.81(2) ? P Pb Rb 3 3 85.67(2) ? Pb Pb Rb 3_655 3 96.413(11) ? Pb Pb Rb 3_645 3 100.282(11) ? S4 P S2 3_545 . 111.36(9) y S4 P S3 3_545 3_645 109.75(8) y S2 P S3 . 3_645 108.05(8) y S4 P S1 3_545 . 111.30(8) y S2 P S1 . . 106.65(8) y S3 P S1 3_645 . 109.62(8) y S4 P Pb 3_545 3_645 169.07(7) ? S2 P Pb . 3_645 68.19(6) ? S3 P Pb 3_645 3_645 61.34(6) ? S1 P Pb . 3_645 78.71(5) ? S4 P Pb 3_545 3_545 55.78(5) ? S2 P Pb . 3_545 131.50(7) ? S3 P Pb 3_645 3_545 120.37(7) ? S1 P Pb . 3_545 56.00(5) ? Pb P Pb 3_645 3_545 133.25(4) ? S4 P Rb 3_545 2 83.15(6) ? S2 P Rb . 2 64.02(6) ? S3 P Rb 3_645 2 65.62(6) ? S1 P Rb . 2 165.34(7) ? Pb P Rb 3_645 2 87.09(3) ? Pb P Rb 3_545 2 138.64(4) ? P S1 Pb . 3_545 88.25(6) ? P S1 Pb . . 90.69(6) ? Pb S1 Pb 3_545 . 113.34(4) ? P S1 Rb . . 172.30(7) ? Pb S1 Rb 3_545 . 88.05(4) ? Pb S1 Rb . . 96.98(4) ? P S2 Pb . . 93.96(7) ? P S2 Pb . 3_645 76.61(6) ? Pb S2 Pb . 3_645 87.63(4) ? P S2 Rb . 2 83.47(6) ? Pb S2 Rb . 2 174.99(6) ? Pb S2 Rb 3_645 2 95.93(4) ? P S2 Rb . 3 92.33(7) ? Pb S2 Rb . 3 85.09(4) ? Pb S2 Rb 3_645 3 166.32(5) ? Rb S2 Rb 2 3 90.70(4) ? P S3 Pb 3_655 . 82.66(6) ? P S3 Pb 3_655 3_645 105.04(7) ? Pb S3 Pb . 3_645 89.95(4) ? P S3 Rb 3_655 4 81.98(6) ? Pb S3 Rb . 4 99.39(4) ? Pb S3 Rb 3_645 4 169.05(5) ? P S3 Rb 3_655 1_655 94.34(7) ? Pb S3 Rb . 1_655 171.47(6) ? Pb S3 Rb 3_645 1_655 83.10(4) ? Rb S3 Rb 4 1_655 88.04(4) ? P S4 Pb 3 . 89.10(6) ? P S4 Rb 3 1_565 93.56(6) ? Pb S4 Rb . 1_565 106.35(4) ? P S4 Rb 3 . 95.90(6) ? Pb S4 Rb . . 98.73(4) ? Rb S4 Rb 1_565 . 153.29(5) ? P S4 Rb 3 4 176.19(7) ? Pb S4 Rb . 4 94.70(4) ? Rb S4 Rb 1_565 4 85.18(3) ? Rb S4 Rb . 4 83.74(3) ? _cod_database_code 2204242