#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100692.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_1100692 _publ_requested_journal 'Analytical Sciences' loop_ _publ_author_name 'Falah, Chiraz' 'Boughzala, Habib' 'Jouini, Tahar' _chemical_name_systematic ; hexapotassium dibismuth diphosphate ; _chemical_formula_moiety 'Bi2 K6 O21 P6' _chemical_formula_sum 'Bi2 K6 O21 P6' _chemical_formula_weight 1174.38 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' 'P' 'P' 0.1023 0.0942 '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' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.985(2) _cell_length_b 9.045(2) _cell_length_c 10.256(3) _cell_angle_alpha 111.87(2) _cell_angle_beta 104.25(2) _cell_angle_gamma 102.00(2) _cell_volume 549.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description parallelipipedic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 3.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 17.659 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.1871 _exptl_absorpt_correction_T_max 0.2866 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'diffractometer CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 2754 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.98 _reflns_number_total 2754 _reflns_number_gt 2651 _reflns_threshold_expression >2sigma(I) _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^)+(0.0475P)^2^+71.2920P] 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 SHELXL _refine_ls_extinction_coef 0.0087(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2754 _refine_ls_number_parameters 158 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.006 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 Bi1 Bi 0.67687(13) 0.66883(12) 0.85113(12) 0.0042(4) Uiso 1 1 d . . . Bi2 Bi 0.3217(3) 0.3305(2) 0.1483(2) 0.0271(6) Uiso 1 1 d . . . P1 P 0.8382(17) 0.0825(14) 0.8579(12) 0.016(2) Uiso 1 1 d . . . P2 P 0.574(2) 0.3016(19) 0.8679(17) 0.027(3) Uiso 1 1 d . . . P3 P 0.434(2) 0.7029(16) 0.1198(16) 0.025(3) Uiso 1 1 d . . . P4 P 0.170(2) 0.9106(16) 0.1153(15) 0.028(3) Uiso 1 1 d . . . P5 P 0.2671(16) 0.4239(13) 0.4921(11) 0.0228(19) Uiso 1 1 d . . . P6 P 0.6830(15) 0.3908(12) 0.4949(11) 0.0204(18) Uiso 1 1 d . . . K1 K 0.943(2) 0.5979(18) 0.2386(18) 0.044(3) Uiso 1 1 d . . . K2 K 0.2609(19) 0.8894(14) 0.8138(14) 0.035(2) Uiso 1 1 d . . . K3 K 0.070(2) 0.4206(15) 0.7785(15) 0.035(3) Uiso 1 1 d . . . K4 K 0.768(2) 0.1270(16) 0.2183(15) 0.040(3) Uiso 1 1 d . . . K5 K 0.628(2) 0.7536(17) 0.5102(16) 0.054(3) Uiso 1 1 d . . . K6' K 0.251(7) 0.040(3) 0.498(3) 0.045(10) Uiso 0.47(9) 1 d P . . K6'' K 0.163(7) 0.031(3) 0.501(3) 0.051(9) Uiso 0.53(9) 1 d P . . O1 O 0.932(7) 0.018(6) 0.745(6) 0.060(11) Uiso 1 1 d . . . O2 O 0.969(5) 0.214(4) 0.009(4) 0.031(7) Uiso 1 1 d . . . O3 O 0.686(4) 0.928(4) 0.844(3) 0.020(6) Uiso 1 1 d . . . O4 O 0.698(5) 0.180(4) 0.794(3) 0.025(6) Uiso 1 1 d . . . O5 O 0.754(5) 0.479(4) 0.950(3) 0.026(6) Uiso 1 1 d . . . O6 O 0.551(5) 0.288(4) 0.015(4) 0.032(7) Uiso 1 1 d . . . O7 O 0.395(4) 0.295(3) 0.759(3) 0.024(5) Uiso 1 1 d . . . O8 O 0.652(6) 0.764(5) 0.210(4) 0.044(8) Uiso 1 1 d . . . O9 O 0.484(5) 0.761(4) 0.016(4) 0.025(6) Uiso 1 1 d . . . O10 O 0.316(7) 0.551(6) 0.109(5) 0.057(11) Uiso 1 1 d . . . O11 O 0.348(4) 0.852(4) 0.203(3) 0.026(7) Uiso 1 1 d . . . O12 O 0.295(6) 0.059(5) 0.116(4) 0.040(9) Uiso 1 1 d . . . O13 O 0.005(6) 0.928(5) 0.200(5) 0.043(9) Uiso 1 1 d . . . O14 O 0.038(5) 0.777(4) 0.953(4) 0.030(7) Uiso 1 1 d . . . O15 O 0.209(6) 0.442(4) 0.361(4) 0.033(8) Uiso 1 1 d . . . O16 O 0.448(4) 0.335(4) 0.491(3) 0.026(6) Uiso 1 1 d . . . O17 O 0.336(5) 0.584(4) 0.648(3) 0.019(6) Uiso 1 1 d . . . O18 O 0.084(7) 0.313(6) 0.486(5) 0.060(11) Uiso 1 1 d . . . O19 O 0.634(5) 0.413(4) 0.364(4) 0.024(7) Uiso 1 1 d . . . O20 O 0.762(4) 0.538(3) 0.645(3) 0.015(5) Uiso 1 1 d . . . O21 O 0.779(4) 0.253(3) 0.494(3) 0.025(5) Uiso 1 1 d . . . _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 Bi1 O14 2.31(3) 1_655 Y Bi1 O20 2.30(3) . Y Bi1 O5 2.38(3) . Y Bi1 O3 2.36(3) . Y Bi1 O9 2.43(3) 1_556 Y Bi1 O17 2.49(3) . Y Bi1 K5 3.801(14) . ? Bi1 K2 3.873(11) . ? Bi1 K3 3.933(12) 1_655 ? Bi1 K3 4.099(14) . ? Bi1 K4 4.226(13) 1_566 ? Bi1 K1 4.293(16) 1_556 ? Bi2 O10 2.18(4) . Y Bi2 O2 2.30(3) 1_455 Y Bi2 O12 2.32(4) . Y Bi2 O6 2.35(3) . Y Bi2 O15 2.44(4) . Y Bi2 O19 2.43(3) . Y Bi2 K5 3.885(14) . ? Bi2 K1 3.986(15) 1_455 ? Bi2 K4 3.983(13) . ? Bi2 K2 4.031(12) 1_544 ? Bi2 K1 4.188(16) . ? Bi2 K3 4.216(13) 1_554 ? P1 O2 1.46(4) 1_556 Y P1 O1 1.47(5) . Y P1 O3 1.50(3) 1_545 Y P1 O4 1.62(3) . Y P1 K5 3.381(18) 1_545 ? P1 K3 3.618(17) 1_655 ? P1 K4 3.733(17) 1_556 ? P1 K2 3.767(15) 1_645 ? P2 O7 1.43(3) . Y P2 O5 1.58(3) . Y P2 O6 1.60(4) 1_556 Y P2 O4 1.63(3) . Y P2 K6' 3.46(3) . ? P2 K1 3.61(2) 1_556 ? P2 K2 3.67(2) 1_545 ? P2 K6'' 3.65(3) . ? P2 K3 3.84(2) 1_655 ? P3 O10 1.40(5) . Y P3 O8 1.43(4) . Y P3 O9 1.43(3) . Y P3 O11 1.63(3) . Y P3 K3 3.39(2) 1_554 ? P3 K4 3.661(18) 1_565 ? P3 K5 3.71(2) . ? P4 O12 1.44(4) 1_565 Y P4 O14 1.53(4) 1_554 Y P4 O13 1.60(4) . Y P4 O11 1.64(3) . Y P4 K2 3.252(18) 1_554 ? P4 K6' 3.50(3) 1_565 ? P4 K1 3.728(19) 1_455 ? P4 K6'' 3.71(3) 1_565 ? P5 O15 1.39(4) . Y P5 O18 1.42(5) . Y P5 O17 1.57(3) . Y P5 O16 1.64(3) . Y P5 K5 3.394(17) . ? P5 K6' 3.47(3) . ? P5 K3 3.543(17) . ? P5 K6'' 3.51(3) . ? P5 K4 3.596(17) 1_455 ? P6 O19 1.41(3) . Y P6 O20 1.48(3) . Y P6 O21 1.53(3) . Y P6 O16 1.60(3) . Y P6 K4 3.234(16) . ? P6 K3 3.330(16) 1_655 ? P6 K5 3.333(17) . ? K1 O5 2.60(3) 1_554 Y K1 O8 2.79(4) . Y K1 O15 2.87(4) 1_655 Y K1 O13 3.12(4) 1_655 Y K1 O6 3.09(4) . Y K1 O10 3.24(5) 1_655 Y K1 O19 3.25(4) . Y K1 O11 3.44(3) 1_655 Y K1 K6'' 3.55(3) 1_665 ? K1 P2 3.61(2) 1_554 ? K1 K6' 3.66(3) 1_665 ? K1 P4 3.728(19) 1_655 ? K2 O14 2.65(4) . Y K2 O3 2.84(3) . Y K2 O1 2.84(5) 1_465 Y K2 O12 2.82(4) 1_566 Y K2 O17 2.89(3) . Y K2 O9 3.01(3) 1_556 Y K2 O6 3.28(4) 1_566 Y K2 P4 3.252(18) 1_556 ? K2 P2 3.67(2) 1_565 ? K2 P1 3.767(15) 1_465 ? K2 K6'' 3.84(3) 1_565 ? K3 O21 2.73(3) 1_455 Y K3 O7 2.76(3) . Y K3 O18 2.82(5) . Y K3 O20 2.87(3) 1_455 Y K3 O17 3.00(3) . Y K3 O10 3.02(5) 1_556 Y K3 O4 3.10(3) 1_455 Y K3 O14 3.14(3) . Y K3 O5 3.16(3) 1_455 Y K3 P6 3.330(16) 1_455 ? K3 O9 3.32(3) 1_556 Y K3 P3 3.39(2) 1_556 ? K4 O21 2.60(3) . Y K4 O18 2.69(5) 1_655 Y K4 O13 2.68(4) 1_645 Y K4 O19 2.94(3) . Y K4 O9 3.05(3) 1_545 Y K4 O12 3.06(4) . Y K4 O2 3.08(4) . Y K4 O8 3.18(4) 1_545 Y K4 O6 3.22(4) . Y K4 O15 3.28(4) 1_655 Y K4 O11 3.36(3) 1_545 Y K5 O1 2.67(5) 1_565 Y K5 O19 2.89(3) . Y K5 O20 2.95(3) . Y K5 O3 3.07(3) . Y K5 O17 3.20(3) . Y _cod_database_code 1100692