#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000270.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_4000270 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'B5 Ce H7 N O15' _[local]_cod_chemical_formula_sum_orig 'H7 B5 Ce N O15' _chemical_formula_weight 455.22 _symmetry_cell_setting 'monoclinic' _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_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 6.4650(10) _cell_length_b 15.571(3) _cell_length_c 10.656(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(3) _cell_angle_gamma 90.00 _cell_volume 1072.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4182 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 4.205 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.714 _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 4182 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2295 _reflns_number_gt 2011 _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^)+(0.0217P)^2^+42.3557P] 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 0.0019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2295 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 Ce1 Ce 0.15053(9) 0.79901(3) 0.35004(6) 0.0152(2) Uani 1 d . . . O1 O-1 0.4441(10) 0.7020(4) 0.2516(6) 0.0130(13) Uani 1 d . . . O2 O-1 -0.1341(9) 0.7999(4) 0.5272(6) 0.0119(13) Uani 1 d . . . O3 O-1 0.0519(10) 0.7176(4) 0.1432(6) 0.0157(14) Uani 1 d . . . O4 O-1 0.5319(10) 0.7866(4) 0.4211(6) 0.0142(14) Uani 1 d . . . O5 O-1 -0.0603(10) 0.9318(4) 0.6390(6) 0.0140(13) Uani 1 d . . . O6 O-1 0.2787(10) 0.9495(4) 0.4032(7) 0.0168(14) Uani 1 d . . . O7 O-1 0.6166(10) 0.9132(4) 0.5316(6) 0.0155(14) Uani 1 d . . . O8 O-1 0.2030(9) 0.8270(4) 0.5923(6) 0.0141(13) Uani 1 d . . . O9 O-1 -0.1990(10) 0.7339(4) 0.2891(7) 0.0177(14) Uani 1 d . . . O10 O 0.3422(15) 0.8681(5) 0.1686(9) 0.038(2) Uani 1 d . . . O11 O -0.0944(13) 0.9155(5) 0.2649(9) 0.035(2) Uani 1 d . . . O12 O 0.1571(15) 0.6576(5) 0.4640(10) 0.044(2) Uani 1 d . . . O13A O 0.277(4) 0.5330(14) 0.498(2) 0.052(5) Uani 0.50 d P . . O13B O 0.295(4) 0.5320(14) 0.421(2) 0.052(5) Uani 0.50 d P . . O14A O 0.097(4) 0.5614(19) 0.338(3) 0.055(5) Uani 0.50 d P . . O14B O -0.018(4) 0.5521(18) 0.356(3) 0.055(5) Uani 0.50 d P . . O15 O 0.631(3) 0.6334(11) 0.4261(18) 0.124(7) Uani 1 d . . . N1 N 0.158(2) 0.5820(7) 0.4242(13) 0.048(3) Uani 1 d . . . B1 B -0.1498(17) 0.7046(7) 0.1706(10) 0.016(2) Uani 1 d . . . B2 B -0.3546(15) 0.8201(7) 0.5283(9) 0.0110(19) Uani 1 d . . . B3 B 0.2405(18) 1.0371(7) 0.4088(10) 0.016(2) Uani 1 d . . . B4 B -0.0175(15) 0.8387(6) 0.6319(10) 0.0113(19) Uani 1 d . . . B5 B 0.598(2) 0.7318(9) 0.3274(11) 0.026(3) 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 Ce1 0.0155(3) 0.0125(3) 0.0175(3) -0.0017(2) -0.0022(2) -0.0001(2) O1 0.016(3) 0.014(3) 0.009(3) -0.003(2) 0.006(3) 0.003(3) O2 0.010(3) 0.013(3) 0.012(3) -0.005(2) 0.000(2) 0.004(2) O3 0.009(3) 0.021(3) 0.017(3) -0.001(3) -0.002(3) -0.003(3) O4 0.012(3) 0.017(3) 0.014(3) -0.005(3) -0.004(3) 0.004(3) O5 0.017(3) 0.011(3) 0.015(3) -0.002(2) 0.000(3) 0.003(2) O6 0.015(3) 0.012(3) 0.024(4) -0.002(3) 0.000(3) 0.001(3) O7 0.017(3) 0.012(3) 0.017(4) 0.000(3) -0.002(3) 0.002(3) O8 0.006(3) 0.019(3) 0.017(3) 0.003(3) 0.004(3) 0.002(2) O9 0.013(3) 0.022(3) 0.018(4) -0.004(3) 0.000(3) -0.005(3) O10 0.050(6) 0.021(4) 0.044(6) 0.004(4) 0.015(5) -0.003(4) O11 0.027(4) 0.023(4) 0.053(6) 0.005(4) -0.010(4) -0.001(3) O12 0.053(6) 0.018(4) 0.061(7) 0.008(4) 0.026(5) 0.010(4) O13A 0.068(10) 0.029(6) 0.060(12) 0.003(11) -0.012(13) 0.021(6) O13B 0.068(10) 0.029(6) 0.060(12) 0.003(11) -0.012(13) 0.021(6) O14A 0.060(15) 0.061(10) 0.043(10) -0.014(8) 0.006(12) 0.007(13) O14B 0.060(15) 0.061(10) 0.043(10) -0.014(8) 0.006(12) 0.007(13) O15 0.18(2) 0.094(12) 0.103(14) 0.000(11) -0.012(13) 0.017(12) N1 0.072(9) 0.025(5) 0.048(8) 0.011(5) 0.031(7) 0.017(6) B1 0.020(5) 0.015(5) 0.012(5) -0.006(4) 0.003(4) 0.000(4) B2 0.006(4) 0.018(5) 0.009(5) 0.001(4) -0.002(4) 0.003(4) B3 0.023(6) 0.015(5) 0.008(5) 0.000(4) 0.003(4) -0.004(4) B4 0.008(4) 0.013(5) 0.013(5) 0.000(4) 0.000(4) 0.002(4) B5 0.019(6) 0.044(7) 0.015(6) -0.016(5) -0.010(5) -0.003(5) _cod_database_code 4000270