#------------------------------------------------------------------------------ #$Date: 2008-02-04 17:24:24 +0000 (Mon, 04 Feb 2008) $ #$Revision: 87 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203703.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_2203703 loop_ _publ_author_name 'Falah, Chiraz' 'Boughzala, Habib' 'Jouini, Tahar' _publ_section_title ; Tripotassium dibismuth(III) tris[arsenate(V)], K~3~Bi~2~(AsO~4~)~3~ ; _journal_issue 6 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i74 _journal_page_last i76 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'K3 Bi2 (As O4)3' _chemical_formula_structural 'K3 Bi2 (As O4)3' _chemical_formula_sum 'As3 Bi2 K3 O12' _chemical_formula_weight 952.02 _chemical_name_systematic ; Tripotassium dibismuth (III) arsenate (V) ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 114.71(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.030(2) _cell_length_b 13.773(2) _cell_length_c 7.009(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.93 _cell_measurement_theta_min 9.59 _cell_volume 1230.4(3) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf--Nonius, 1994)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w--2\q _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 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1387 _diffrn_reflns_theta_full 25.96 _diffrn_reflns_theta_max 25.96 _diffrn_reflns_theta_min 2.18 _diffrn_standards_decay_% 2 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 37.648 _exptl_absorpt_correction_T_max 0.2545 _exptl_absorpt_correction_T_min 0.1638 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 5.140 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1672 _exptl_crystal_size_max 0.108 _exptl_crystal_size_mid 0.036 _exptl_crystal_size_min 0.036 _refine_diff_density_max 1.087 _refine_diff_density_min -1.218 _refine_ls_extinction_coef 0.00050(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_matrix_type full _refine_ls_number_parameters 95 _refine_ls_number_reflns 1203 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0261 _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^)+(0.01P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0512 _reflns_number_gt 1006 _reflns_number_total 1203 _reflns_threshold_expression I>2\s(I) _[local]_cod_original_file br6141.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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_refinement_flags _atom_site_occupancy _atom_site_type_symbol Bi 0.26492(2) 0.35529(3) 0.33414(6) 0.00740(10) Uani d . 1 Bi As2 0.74345(6) 0.39168(7) 0.64105(14) 0.0059(2) Uani d . 1 As As1 0.5000 0.25740(10) 0.7500 0.0064(3) Uani d S 1 As K1 0.5000 0.4809(2) 0.2500 0.0146(7) Uani d S 1 K K2 0.5000 0.2230(2) 0.2500 0.0166(7) Uani d S 1 K K3 0.5000 0.0000 0.5000 0.0223(7) Uani d S 1 K O1 0.4261(5) 0.1874(5) 0.8290(10) 0.017(2) Uani d . 1 O O2 0.5689(4) 0.3355(5) 0.9520(10) 0.012(2) Uani d . 1 O O3 0.8531(5) 0.4344(5) 0.6360(10) 0.017(2) Uani d . 1 O O4 0.6725(5) 0.3346(5) 0.4080(10) 0.012(2) Uani d . 1 O O5 0.6681(4) 0.4806(5) 0.6740(10) 0.0110(10) Uani d . 1 O O6 0.7713(5) 0.3113(5) 0.8450(10) 0.0120(10) Uani d . 1 O 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 Bi 0.0066(2) 0.0060(2) 0.0089(2) -0.00010(10) 0.00260(10) 0.0008(2) As2 0.0062(4) 0.0035(5) 0.0072(4) -0.0002(4) 0.0022(3) -0.0001(4) As1 0.0049(6) 0.0067(7) 0.0059(6) 0.000 0.0005(5) 0.000 K1 0.0120(10) 0.012(2) 0.018(2) 0.000 0.0050(10) 0.000 K2 0.0120(10) 0.015(2) 0.020(2) 0.000 0.0040(10) 0.000 K3 0.0170(10) 0.027(2) 0.019(2) -0.005(2) 0.0040(10) 0.008(2) O1 0.012(3) 0.018(4) 0.017(4) -0.008(3) 0.004(3) -0.001(3) O2 0.010(3) 0.012(4) 0.013(3) -0.002(3) 0.002(3) -0.008(3) O3 0.012(3) 0.018(4) 0.019(4) -0.003(3) 0.005(3) 0.003(3) O4 0.021(3) 0.007(4) 0.011(3) -0.004(3) 0.009(3) -0.001(3) O5 0.010(3) 0.006(4) 0.020(4) 0.004(3) 0.008(3) -0.003(3) O6 0.017(3) 0.006(3) 0.008(3) 0.001(3) 0.002(3) 0.006(3) 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 Bi O2 2_656 2.199(6) Y Bi O4 2_655 2.231(6) Y Bi O6 8_455 2.296(7) Y Bi O5 5_666 2.457(7) Y Bi O1 7_556 2.505(6) Y Bi O6 2_656 2.579(7) Y Bi K1 . 3.9809(14) N Bi K3 4 3.9993(3) N Bi K2 . 4.0217(15) N Bi K1 5_666 4.0526(18) N Bi K2 7 4.3607(9) N As2 O3 . 1.663(6) Y As2 O5 . 1.694(6) Y As2 O4 . 1.709(6) Y As2 O6 . 1.717(6) Y As2 K1 . 3.5865(14) N As2 K2 7_656 3.7060(16) N As2 K3 4_656 3.7336(8) N As1 O1 2_656 1.668(7) n As1 O1 . 1.668(7) Y As1 O2 . 1.716(6) Y As1 O2 2_656 1.716(6) n As1 K2 . 3.5364(5) N As1 K2 1_556 3.5364(5) N As1 K1 5_666 3.604(3) N As1 K3 . 3.9545(12) N As1 K3 2_656 3.9545(12) N K1 O5 6_565 2.681(6) Y K1 O5 5_666 2.681(6) n K1 O2 6_565 2.860(7) Y K1 O2 5_666 2.860(7) n K1 O5 . 2.919(6) Y K1 O5 2_655 2.919(6) n K1 O4 2_655 2.984(7) n K1 O4 . 2.984(7) Y K1 O2 1_554 3.319(6) Y K1 O2 2_656 3.319(7) n K1 K1 5_665 3.5435(9) N K1 K1 5_666 3.5435(9) N K2 O4 . 2.684(6) Y K2 O4 2_655 2.684(6) n K2 O1 1_554 2.735(7) Y K2 O1 2_656 2.735(7) n K2 O3 8_455 2.865(7) Y K2 O3 7_656 2.865(7) n K2 O2 1_554 3.067(7) Y K2 O2 2_656 3.067(7) n K2 K3 2_655 3.536(3) N K2 K3 . 3.536(3) N K2 As1 1_554 3.5364(5) N K3 O3 4_646 2.681(7) Y K3 O3 8_455 2.681(7) Y K3 O3 7_656 2.757(7) Y K3 O3 3_445 2.757(7) n K3 O1 6 2.854(7) Y K3 O1 2_656 2.854(7) n K3 K3 2_655 3.5044 N K3 K3 2_656 3.5044 n K3 K2 5_656 3.536(3) N K3 As2 4_646 3.7336(9) N K3 As2 8_455 3.7336(8) N O1 Bi 7_556 2.505(6) N O1 K2 1_556 2.735(7) N O1 K3 2_656 2.854(7) N O2 Bi 2_656 2.199(6) N O2 K1 5_666 2.860(7) N O2 K2 1_556 3.067(7) N O2 K1 1_556 3.319(6) N O3 K3 4_656 2.681(7) N O3 K3 3 2.757(7) N O3 K2 7_656 2.865(7) N O4 Bi 2_655 2.231(6) N O5 Bi 5_666 2.457(6) N O5 K1 5_666 2.681(6) N O6 Bi 8_556 2.296(7) N O6 Bi 2_656 2.579(7) N 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 O2 Bi O4 2_656 2_655 82.1(2) Y O2 Bi O6 2_656 8_455 80.7(2) Y O4 Bi O6 2_655 8_455 82.8(2) Y O2 Bi O5 2_656 5_666 79.8(2) Y O4 Bi O5 2_655 5_666 79.9(2) Y O6 Bi O5 8_455 5_666 155.5(2) Y O2 Bi O1 2_656 7_556 155.3(2) Y O4 Bi O1 2_655 7_556 108.1(2) Y O6 Bi O1 8_455 7_556 78.5(2) Y O5 Bi O1 5_666 7_556 123.5(2) Y O2 Bi O6 2_656 2_656 85.1(2) Y O4 Bi O6 2_655 2_656 156.6(2) Y O6 Bi O6 8_455 2_656 75.9(2) Y O5 Bi O6 5_666 2_656 116.9(2) Y O1 Bi O6 7_556 2_656 77.2(2) Y O3 As2 O5 . . 112.5(3) Y O3 As2 O4 . . 108.4(3) Y O5 As2 O4 . . 108.3(3) Y O3 As2 O6 . . 110.9(3) Y O5 As2 O6 . . 107.0(3) Y O4 As2 O6 . . 109.7(3) Y O1 As1 O1 2_656 . 109.5(5) Y O1 As1 O2 2_656 . 114.8(3) Y O1 As1 O2 . . 107.7(3) Y O1 As1 O2 2_656 2_656 107.7(3) Y O1 As1 O2 . 2_656 114.8(3) Y O2 As1 O2 . 2_656 102.3(4) Y O5 K1 O5 6_565 5_666 157.2(3) N O5 K1 O2 6_565 6_565 77.30(19) N O5 K1 O2 5_666 6_565 82.58(19) N O5 K1 O2 6_565 5_666 82.58(19) N O5 K1 O2 5_666 5_666 77.30(19) N O2 K1 O2 6_565 5_666 55.8(2) N O5 K1 O5 6_565 . 78.41(15) N O5 K1 O5 5_666 . 101.62(14) N O2 K1 O5 6_565 . 62.38(18) N O2 K1 O5 5_666 . 117.8(2) N O5 K1 O5 6_565 2_655 101.62(14) N O5 K1 O5 5_666 2_655 78.41(15) N O2 K1 O5 6_565 2_655 117.8(2) N O2 K1 O5 5_666 2_655 62.38(18) N O5 K1 O5 . 2_655 179.8(3) N O5 K1 O4 6_565 2_655 134.7(2) N O5 K1 O4 5_666 2_655 64.08(18) N O2 K1 O4 6_565 2_655 146.59(18) N O2 K1 O4 5_666 2_655 111.08(17) N O5 K1 O4 . 2_655 124.15(19) N O5 K1 O4 2_655 2_655 55.70(18) N O5 K1 O4 6_565 . 64.08(18) N O5 K1 O4 5_666 . 134.7(2) N O2 K1 O4 6_565 . 111.08(17) N O2 K1 O4 5_666 . 146.59(18) N O5 K1 O4 . . 55.70(18) N O5 K1 O4 2_655 . 124.15(19) N O4 K1 O4 2_655 . 95.0(3) N O5 K1 O2 6_565 1_554 58.71(18) N O5 K1 O2 5_666 1_554 139.26(18) N O2 K1 O2 6_565 1_554 135.8(2) N O2 K1 O2 5_666 1_554 110.46(14) N O5 K1 O2 . 1_554 108.39(16) N O5 K1 O2 2_655 1_554 71.50(16) N O4 K1 O2 2_655 1_554 76.31(17) N O4 K1 O2 . 1_554 54.65(17) N O5 K1 O2 6_565 2_656 139.26(18) N O5 K1 O2 5_666 2_656 58.71(18) N O2 K1 O2 6_565 2_656 110.46(14) N O2 K1 O2 5_666 2_656 135.8(2) N O5 K1 O2 . 2_656 71.50(16) N O5 K1 O2 2_655 2_656 108.39(16) N O4 K1 O2 2_655 2_656 54.65(17) N O4 K1 O2 . 2_656 76.31(17) N O2 K1 O2 1_554 2_656 105.8(2) N O4 K2 O4 . 2_655 110.1(3) N O4 K2 O1 . 1_554 114.7(2) N O4 K2 O1 2_655 1_554 77.7(2) N O4 K2 O1 . 2_656 77.7(2) N O4 K2 O1 2_655 2_656 114.66(19) N O1 K2 O1 1_554 2_656 159.4(3) N O4 K2 O3 . 8_455 165.4(2) N O4 K2 O3 2_655 8_455 84.20(18) N O1 K2 O3 1_554 8_455 70.0(2) N O1 K2 O3 2_656 8_455 94.1(2) N O4 K2 O3 . 7_656 84.20(18) N O4 K2 O3 2_655 7_656 165.4(2) N O1 K2 O3 1_554 7_656 94.1(2) N O1 K2 O3 2_656 7_656 70.0(2) N O3 K2 O3 8_455 7_656 81.7(3) N O4 K2 O2 . 1_554 60.32(18) N O4 K2 O2 2_655 1_554 85.18(19) N O1 K2 O2 1_554 1_554 55.87(18) N O1 K2 O2 2_656 1_554 137.89(19) N O3 K2 O2 8_455 1_554 125.91(18) N O3 K2 O2 7_656 1_554 100.28(18) N O4 K2 O2 . 2_656 85.18(19) N O4 K2 O2 2_655 2_656 60.32(18) N O1 K2 O2 1_554 2_656 137.89(19) N O1 K2 O2 2_656 2_656 55.87(18) N O3 K2 O2 8_455 2_656 100.28(18) N O3 K2 O2 7_656 2_656 125.91(18) N O2 K2 O2 1_554 2_656 119.3(3) N O3 K3 O3 4_646 8_455 180.0 N O3 K3 O3 4_646 7_656 92.9(2) N O3 K3 O3 8_455 7_656 87.1(2) N O3 K3 O3 4_646 3_445 87.1(2) N O3 K3 O3 8_455 3_445 92.9(2) N O3 K3 O3 7_656 3_445 180.00(13) N O3 K3 O1 4_646 6 95.5(2) N O3 K3 O1 8_455 6 84.5(2) N O3 K3 O1 7_656 6 110.1(2) N O3 K3 O1 3_445 6 69.9(2) N O3 K3 O1 4_646 2_656 84.5(2) N O3 K3 O1 8_455 2_656 95.5(2) N O3 K3 O1 7_656 2_656 69.9(2) N O3 K3 O1 3_445 2_656 110.1(2) N O1 K3 O1 6 2_656 180.0(3) N As1 O1 Bi . 7_556 132.8(3) N As1 O1 K2 . 1_556 104.2(3) N Bi O1 K2 7_556 1_556 112.6(2) N As1 O1 K3 . 2_656 119.7(3) N Bi O1 K3 7_556 2_656 96.3(2) N K2 O1 K3 1_556 2_656 78.46(19) N As1 O2 Bi . 2_656 135.3(3) N As1 O2 K1 . 5_666 101.0(3) N Bi O2 K1 2_656 5_666 105.7(2) N As1 O2 K2 . 1_556 90.8(3) N Bi O2 K2 2_656 1_556 98.2(2) N K1 O2 K2 5_666 1_556 130.2(2) N As1 O2 K1 . 1_556 133.2(3) N Bi O2 K1 2_656 1_556 89.99(19) N K1 O2 K1 5_666 1_556 69.54(14) N K2 O2 K1 1_556 1_556 67.49(14) N As2 O3 K3 . 4_656 116.6(3) N As2 O3 K3 . 3 163.0(4) N K3 O3 K3 4_656 3 80.22(17) N As2 O3 K2 . 7_656 106.8(3) N K3 O3 K2 4_656 7_656 79.13(17) N K3 O3 K2 3 7_656 77.90(17) N As2 O4 Bi . 2_655 114.3(3) N As2 O4 K2 . . 136.3(3) N Bi O4 K2 2_655 . 109.5(2) N As2 O4 K1 . . 95.8(3) N Bi O4 K1 2_655 . 98.5(2) N K2 O4 K1 . . 77.44(17) N As2 O5 Bi . 5_666 113.4(3) N As2 O5 K1 . 5_666 145.1(3) N Bi O5 K1 5_666 5_666 101.5(2) N As2 O5 K1 . . 98.6(3) N Bi O5 K1 5_666 . 97.5(2) N K1 O5 K1 5_666 . 78.38(14) N As2 O6 Bi . 8_556 128.7(3) N As2 O6 Bi . 2_656 120.9(3) N Bi O6 Bi 8_556 2_656 104.1(2) N