#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000385.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_4000385 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_name_common 'Ammonium Lithium Pyrofluoroberyllate' _chemical_formula_sum 'Be2 F7 H4 Li2 N' _[local]_cod_chemical_formula_sum_orig 'H4 Be2 F7 Li2 N' _chemical_formula_weight 182.94 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 9.842(2) _cell_length_b 12.221(2) _cell_length_c 10.025(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1205.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1546 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_absorpt_correction_T_min 0.8595 _exptl_absorpt_correction_T_max 0.92905 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.091088 _diffrn_orient_matrix_ub_12 0.0434777 _diffrn_orient_matrix_ub_13 0.0065273 _diffrn_orient_matrix_ub_21 -0.012715 _diffrn_orient_matrix_ub_22 0.0420686 _diffrn_orient_matrix_ub_23 -0.0734822 _diffrn_orient_matrix_ub_31 -0.0431899 _diffrn_orient_matrix_ub_32 0.0793102 _diffrn_orient_matrix_ub_33 0.0353991 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_unetI/netI 0.0666 _diffrn_reflns_number 8096 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 2702 _reflns_number_gt 1892 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SCALEPACK (Otwinoski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0307P)^2^+0.2463P] 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_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0070(11) _refine_ls_number_reflns 2702 _refine_ls_number_parameters 242 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -2(2) _refine_diff_density_max 0.389 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.071 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 N 0.2567(6) -0.0002(2) 0.7411(8) 0.0193(15) Uani 1 1 d D . . H1 H 0.306(3) 0.0580(19) 0.757(3) 0.029 Uiso 1 1 d D . . H2 H 0.174(2) 0.002(3) 0.768(3) 0.029 Uiso 1 1 d D . . H3 H 0.307(3) -0.0581(19) 0.758(3) 0.029 Uiso 1 1 d D . . H4 H 0.242(3) -0.003(2) 0.6518(19) 0.029 Uiso 1 1 d D . . N2 N 0.0087(7) 0.4996(2) 0.5147(8) 0.0211(16) Uani 1 1 d D . . H5 H -0.019(3) 0.542(3) 0.584(2) 0.032 Uiso 1 1 d D . . H6 H -0.057(3) 0.449(2) 0.500(3) 0.032 Uiso 1 1 d D . . H7 H 0.007(3) 0.545(2) 0.444(2) 0.032 Uiso 1 1 d D . . H8 H 0.088(2) 0.466(3) 0.533(3) 0.032 Uiso 1 1 d D . . Li1 Li 0.0216(9) 0.2513(8) 0.7296(11) 0.0166(18) Uani 1 1 d . . . Li2 Li -0.0238(9) 0.2496(8) 0.2224(11) 0.0145(19) Uani 1 1 d . . . Li3 Li -0.2208(9) 0.2452(9) 0.5336(12) 0.020(2) Uani 1 1 d . . . Li4 Li 0.2734(10) 0.2518(9) 0.5349(12) 0.020(2) Uani 1 1 d . . . Be1 Be -0.2354(7) 0.3778(7) 0.7868(7) 0.0154(15) Uani 1 1 d . . . Be2 Be 0.2785(7) 0.3855(7) 0.7778(7) 0.0153(15) Uani 1 1 d . . . Be3 Be -0.0204(7) 0.1160(7) 0.9717(8) 0.0159(15) Uani 1 1 d . . . Be4 Be 0.0239(7) 0.1167(8) 0.4773(8) 0.0166(15) Uani 1 1 d . . . F1 F 0.0264(3) 0.1275(3) 0.8281(3) 0.0262(7) Uani 1 1 d . . . F2 F 0.1986(3) 0.3015(3) 0.6956(3) 0.0171(8) Uani 1 1 d . . . F3 F 0.4306(2) 0.3774(2) 0.7466(3) 0.0126(5) Uani 1 1 d . . . F4 F 0.2486(2) 0.3737(2) 0.4281(2) 0.0155(5) Uani 1 1 d . . . F5 F -0.2691(4) 0.49548(13) 0.7312(5) 0.0142(9) Uani 1 1 d . . . F6 F -0.2953(3) 0.2935(3) 0.6923(3) 0.0150(8) Uani 1 1 d . . . F7 F -0.0796(2) 0.3650(2) 0.7964(3) 0.0140(5) Uani 1 1 d . . . F8 F -0.2029(2) 0.3676(2) 0.4274(3) 0.0143(5) Uani 1 1 d . . . F9 F -0.0205(3) 0.1327(3) 0.3325(3) 0.0289(7) Uani 1 1 d . . . F10 F -0.0477(3) 0.2020(3) 0.5681(3) 0.0177(8) Uani 1 1 d . . . F11 F 0.1777(3) 0.1281(3) 0.4911(4) 0.0289(7) Uani 1 1 d . . . F12 F 0.0200(5) -0.00016(13) 1.0264(5) 0.0178(10) Uani 1 1 d . . . F13 F -0.3254(3) 0.1291(3) 0.4844(3) 0.0288(7) Uani 1 1 d . . . F14 F 0.4493(3) 0.2036(3) 0.5603(3) 0.0175(8) Uani 1 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 N1 0.019(3) 0.022(4) 0.017(3) 0.0023(14) 0.005(2) 0.0007(11) N2 0.018(3) 0.019(4) 0.027(4) -0.0014(14) 0.006(2) -0.0008(11) Li1 0.023(4) 0.012(5) 0.015(4) 0.001(4) -0.010(4) 0.001(4) Li2 0.020(4) 0.008(5) 0.016(4) -0.001(4) 0.007(4) 0.004(4) Li3 0.016(4) 0.020(6) 0.024(4) 0.001(4) -0.008(3) 0.000(4) Li4 0.020(4) 0.020(6) 0.022(4) 0.000(4) -0.009(4) -0.002(4) Be1 0.017(3) 0.016(4) 0.014(3) 0.000(3) 0.000(2) -0.001(3) Be2 0.020(3) 0.018(4) 0.008(3) 0.000(3) 0.000(2) 0.000(3) Be3 0.011(3) 0.011(4) 0.026(3) -0.002(3) -0.001(2) 0.001(3) Be4 0.010(3) 0.019(4) 0.021(3) -0.002(3) 0.002(3) -0.001(3) F1 0.0457(14) 0.0180(13) 0.0150(11) 0.0027(12) 0.0018(10) 0.0045(12) F2 0.0155(14) 0.019(2) 0.0171(15) -0.0041(13) 0.0014(12) -0.0008(12) F3 0.0123(10) 0.0164(11) 0.0092(9) 0.0021(11) 0.0017(9) 0.0004(9) F4 0.0139(10) 0.0195(12) 0.0132(10) 0.0001(12) -0.0037(10) 0.0025(10) F5 0.0131(16) 0.015(2) 0.0141(17) 0.0004(9) 0.0012(16) -0.0007(7) F6 0.0117(14) 0.018(2) 0.0152(14) -0.0045(12) -0.0005(11) 0.0000(11) F7 0.0111(9) 0.0178(12) 0.0131(10) -0.0009(10) 0.0008(8) 0.0004(10) F8 0.0097(9) 0.0183(12) 0.0149(9) -0.0002(13) -0.0023(10) -0.0012(9) F9 0.0546(15) 0.0151(13) 0.0169(11) 0.0015(13) -0.0032(12) -0.0039(12) F10 0.0158(15) 0.019(2) 0.0183(15) -0.0026(12) -0.0034(12) 0.0046(12) F11 0.0178(12) 0.0174(13) 0.0517(13) -0.0108(13) 0.0046(11) -0.0017(11) F12 0.0216(19) 0.015(2) 0.0172(19) -0.0013(8) -0.0014(17) -0.0006(7) F13 0.0174(12) 0.0210(13) 0.0479(13) -0.0120(12) 0.0029(10) -0.0008(11) F14 0.0184(15) 0.014(2) 0.0199(16) -0.0015(12) -0.0020(12) 0.0046(12)