#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000273.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_4000273 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'H5 B8 O16 Pr' _chemical_formula_weight 488.42 _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.860(2) _cell_length_b 14.131(3) _cell_length_c 7.940(2) _cell_angle_alpha 90.00 _cell_angle_beta 89.79(3) _cell_angle_gamma 90.00 _cell_volume 1106.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2454 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.93 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 4.511 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.269 _exptl_absorpt_correction_T_max 0.637 _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 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method 'Oscillation' _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2454 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2454 _reflns_number_gt 2062 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.2688P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2454 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1A Pr 0.88737(4) 0.32271(11) 0.16016(6) 0.0210(2) Uani 0.930(5) d P . . Pr1B Pr 0.8914(6) 0.2859(12) 0.1438(9) 0.0210(2) Uani 0.070(5) d P . . O1 O 0.6287(4) 0.3024(3) 0.1466(5) 0.0207(8) Uani 1 d . . . O2 O 1.1433(4) 0.2862(3) 0.1465(4) 0.0216(8) Uani 1 d . . . O3 O 0.3858(3) 0.2796(3) 0.1781(4) 0.0196(8) Uani 1 d . . . O4 O 0.7407(4) 0.2499(3) -0.0847(4) 0.0203(8) Uani 1 d . . . O5 O 0.7718(4) 0.3000(3) 0.4454(5) 0.0204(8) Uani 1 d . . . O6 O 1.2588(4) 0.4062(3) 0.2989(5) 0.0249(8) Uani 1 d . . . O7 O 1.0310(4) 0.2238(3) -0.0775(4) 0.0220(8) Uani 1 d . . . O8 O 0.4959(4) 0.4209(3) 0.2691(5) 0.0243(8) Uani 1 d . . . O9 O 1.3656(4) 0.5561(3) 0.3017(6) 0.0376(11) Uani 1 d . . . O10 O 1.0057(4) 0.2882(3) 0.4437(4) 0.0216(8) Uani 1 d . . . O11 O 0.9941(4) 0.4653(3) 0.2817(5) 0.0328(10) Uani 1 d . . . O12 O 0.9408(5) 0.4256(3) -0.0645(5) 0.0298(9) Uani 1 d . . . O13 O 0.8933(4) 0.3907(3) 0.6429(5) 0.0260(9) Uani 1 d . . . O14 O 0.8617(4) 0.1333(3) 0.2152(6) 0.0342(10) Uani 1 d . . . O15 O 0.8745(4) 0.6126(4) 0.2588(6) 0.0368(10) Uani 1 d . . . O16 O 0.7323(5) 0.4839(4) 0.1900(7) 0.0478(13) Uani 1 d . . . B1 B 1.1517(6) 0.2347(4) 0.0015(7) 0.0179(11) Uani 1 d . . . B2 B 0.5134(6) 0.3206(5) 0.2588(8) 0.0224(13) Uani 1 d . . . B3 B 1.2563(6) 0.3077(5) 0.2622(8) 0.0197(13) Uani 1 d . . . B4 B 1.3710(6) 0.4610(5) 0.2933(8) 0.0250(13) Uani 1 d . . . B5 B 0.7522(7) 0.5747(6) 0.2460(9) 0.0335(16) Uani 1 d . . . B6 B 0.8913(6) 0.3050(5) 0.5600(7) 0.0192(12) Uani 1 d . . . B7 B 1.1212(6) 0.2470(5) 0.4993(8) 0.0208(12) Uani 1 d . . . B8 B 1.0078(7) 0.5665(5) 0.2462(8) 0.0298(15) Uani 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 Pr1A 0.0144(2) 0.0320(6) 0.0167(2) 0.0032(2) 0.00279(13) -0.00179(18) Pr1B 0.0144(2) 0.0320(6) 0.0167(2) 0.0032(2) 0.00279(13) -0.00179(18) O1 0.0140(18) 0.031(2) 0.0177(18) -0.0023(15) 0.0028(14) -0.0018(15) O2 0.0162(18) 0.034(2) 0.0144(17) 0.0000(16) 0.0031(14) 0.0018(17) O3 0.0114(17) 0.031(2) 0.0158(17) -0.0006(15) 0.0041(14) 0.0010(15) O4 0.0128(16) 0.037(2) 0.0107(15) -0.0029(15) 0.0016(12) -0.0022(15) O5 0.0123(17) 0.029(2) 0.0200(18) 0.0014(15) 0.0003(14) -0.0010(15) O6 0.0160(18) 0.027(2) 0.031(2) -0.0006(17) 0.0056(15) 0.0002(16) O7 0.0143(17) 0.033(2) 0.0182(17) 0.0013(16) 0.0024(14) -0.0016(16) O8 0.0145(18) 0.029(2) 0.0290(19) -0.0056(16) 0.0044(15) 0.0017(16) O9 0.021(2) 0.031(3) 0.061(3) -0.008(2) 0.005(2) -0.0018(18) O10 0.0177(18) 0.032(2) 0.0148(16) 0.0029(16) 0.0058(14) 0.0033(17) O11 0.036(2) 0.029(2) 0.033(2) 0.0021(18) 0.0120(18) 0.0014(19) O12 0.039(2) 0.031(2) 0.0196(18) -0.0001(16) 0.0059(17) -0.0053(19) O13 0.019(2) 0.027(2) 0.032(2) -0.0061(17) 0.0009(16) 0.0005(16) O14 0.030(2) 0.037(3) 0.035(2) 0.005(2) 0.0021(18) 0.001(2) O15 0.030(2) 0.036(3) 0.044(2) -0.005(2) -0.0002(19) -0.001(2) O16 0.026(2) 0.044(3) 0.074(3) -0.009(3) 0.006(2) -0.005(2) B1 0.015(2) 0.023(3) 0.016(2) 0.003(2) 0.004(2) -0.002(2) B2 0.011(3) 0.037(4) 0.019(3) 0.001(3) 0.000(2) 0.000(2) B3 0.009(3) 0.030(4) 0.020(3) -0.002(2) 0.006(2) 0.004(2) B4 0.014(3) 0.038(4) 0.024(3) -0.002(3) 0.004(2) -0.001(3) B5 0.028(4) 0.041(4) 0.032(4) -0.001(3) 0.009(3) 0.002(3) B6 0.019(3) 0.028(4) 0.010(2) 0.003(2) 0.000(2) -0.002(2) B7 0.015(3) 0.025(3) 0.023(3) -0.002(2) 0.003(2) 0.000(2) B8 0.027(3) 0.036(4) 0.027(3) 0.001(3) 0.003(3) -0.002(3)