Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Gerrard, Lee' 'Weller, M.' _publ_contact_author_name 'Dr Lee Gerrard' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton Hampshire So17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'LAG4@SOTON.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; 2-Dimensional Sheet Structures from Linked Metal FluorideTetrahedra ; data_1 _database_code_CSD 189068 _audit_creation_date 2002-06-25T14:03:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Ethylenediammonium Dilithiumtetrafluoroberyllate' _chemical_formula_sum 'C H5 Be F4 Li N' _chemical_formula_weight 123.01 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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' _cell_length_a 19.467(4) _cell_length_b 4.7968(10) _cell_length_c 9.867(2) _cell_angle_alpha 90 _cell_angle_beta 106.98(3) _cell_angle_gamma 90 _cell_volume 881.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14029 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_absorpt_correction_T_min 0.96133 _exptl_absorpt_correction_T_max 1.05191 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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 0.194194 _diffrn_orient_matrix_ub_12 -0.85879E-2 _diffrn_orient_matrix_ub_13 -0.603538E-1 _diffrn_orient_matrix_ub_21 0.871795E-1 _diffrn_orient_matrix_ub_22 -0.9115E-3 _diffrn_orient_matrix_ub_23 0.813862E-1 _diffrn_orient_matrix_ub_31 -0.322518E-1 _diffrn_orient_matrix_ub_32 -0.105621 _diffrn_orient_matrix_ub_33 0.356905E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_number 7349 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 1004 _reflns_number_gt 799 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0621P)^2^+0.0000P] 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 0.001(2) _refine_ls_number_reflns 1004 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.312 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Li Li -0.0003 0.0001 '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 Li1 Li 0.24656(14) -0.0652(5) 0.1447(3) 0.0198(5) Uani 1 1 d . . . Be1 Be 0.16201(11) -0.0575(4) 0.35280(19) 0.0179(4) Uani 1 1 d . . . F1 F 0.22635(5) 0.06894(16) 0.30738(9) 0.0197(3) Uani 1 1 d . . . F2 F 0.16309(5) -0.05860(17) -0.00198(9) 0.0193(3) Uani 1 1 d . . . F3 F 0.32628(5) 0.12130(17) 0.13196(9) 0.0206(3) Uani 1 1 d . . . F4 F 0.09198(5) -0.00434(16) 0.23442(9) 0.0229(3) Uani 1 1 d . . . N1 N 0.09985(7) 0.4649(3) 0.07532(14) 0.0189(3) Uani 1 1 d . . . C1 C 0.02970(8) 0.4895(3) -0.03476(16) 0.0195(4) Uani 1 1 d . . . H1 H 0.1089(10) 0.624(4) 0.133(2) 0.031(5) Uiso 1 1 d . . . H2 H 0.1372(10) 0.473(3) 0.037(2) 0.027(5) Uiso 1 1 d . . . H3 H 0.1030(11) 0.309(4) 0.125(2) 0.039(5) Uiso 1 1 d . . . H4 H 0.0221(9) 0.331(4) -0.0948(18) 0.023(4) Uiso 1 1 d . . . H5 H 0.0292(8) 0.650(4) -0.0918(18) 0.023(4) Uiso 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 Li1 0.0232(14) 0.0190(12) 0.0181(13) -0.0005(9) 0.0077(10) 0.0011(10) Be1 0.0219(10) 0.0185(10) 0.0138(9) -0.0003(6) 0.0062(8) -0.0006(7) F1 0.0245(5) 0.0182(5) 0.0191(5) -0.0018(3) 0.0106(4) -0.0029(3) F2 0.0223(5) 0.0207(5) 0.0157(5) 0.0017(3) 0.0069(4) 0.0000(3) F3 0.0252(5) 0.0160(5) 0.0232(5) -0.0002(3) 0.0112(4) -0.0001(3) F4 0.0216(5) 0.0275(5) 0.0179(5) 0.0033(3) 0.0032(4) -0.0003(3) N1 0.0182(7) 0.0208(7) 0.0171(7) 0.0011(5) 0.0046(6) 0.0000(5) C1 0.0201(9) 0.0232(9) 0.0151(8) 0.0002(6) 0.0046(6) 0.0008(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Li1 F3 1.827(3) . ? Li1 F2 1.833(3) . ? Li1 F1 1.854(3) 4_545 ? Li1 F1 1.875(3) . ? Li1 Be1 2.929(3) 6 ? Li1 Be1 2.953(3) 4_545 ? Li1 Be1 2.984(3) . ? Li1 Be1 3.012(3) 4 ? Li1 Li1 3.151(3) 4 ? Li1 Li1 3.151(3) 4_545 ? Li1 Li1 3.396(5) 7_545 ? Be1 F2 1.532(2) 6_556 ? Be1 F4 1.535(2) . ? Be1 F3 1.558(2) 4_545 ? Be1 F1 1.570(2) . ? Be1 Li1 2.929(3) 6_556 ? Be1 Li1 2.953(3) 4 ? Be1 Li1 3.012(3) 4_545 ? F1 Li1 1.854(3) 4 ? F2 Be1 1.532(2) 6 ? F3 Be1 1.558(2) 4 ? N1 C1 1.480(2) . ? C1 C1 1.510(3) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Li1 F2 120.82(14) . . ? F3 Li1 F1 107.28(13) . 4_545 ? F2 Li1 F1 109.76(13) . 4_545 ? F3 Li1 F1 106.60(13) . . ? F2 Li1 F1 108.09(13) . . ? F1 Li1 F1 102.79(12) 4_545 . ? F3 Li1 Be1 94.52(11) . 6 ? F2 Li1 Be1 26.71(6) . 6 ? F1 Li1 Be1 118.52(12) 4_545 6 ? F1 Li1 Be1 125.08(12) . 6 ? F3 Li1 Be1 82.54(10) . 4_545 ? F2 Li1 Be1 114.42(11) . 4_545 ? F1 Li1 Be1 27.73(6) 4_545 4_545 ? F1 Li1 Be1 122.95(13) . 4_545 ? Be1 Li1 Be1 109.47(9) 6 4_545 ? F3 Li1 Be1 133.76(12) . . ? F2 Li1 Be1 90.17(10) . . ? F1 Li1 Be1 90.51(9) 4_545 . ? F1 Li1 Be1 27.19(6) . . ? Be1 Li1 Be1 114.18(10) 6 . ? Be1 Li1 Be1 117.15(10) 4_545 . ? F3 Li1 Be1 24.91(6) . 4 ? F2 Li1 Be1 112.21(11) . 4 ? F1 Li1 Be1 129.79(13) 4_545 4 ? F1 Li1 Be1 89.24(10) . 4 ? Be1 Li1 Be1 90.39(9) 6 4 ? Be1 Li1 Be1 107.06(10) 4_545 4 ? Be1 Li1 Be1 115.33(9) . 4 ? F3 Li1 Li1 78.43(9) . 4 ? F2 Li1 Li1 111.38(12) . 4 ? F1 Li1 Li1 126.74(15) 4_545 4 ? F1 Li1 Li1 32.12(8) . 4 ? Be1 Li1 Li1 113.52(10) 6 4 ? Be1 Li1 Li1 133.93(15) 4_545 4 ? Be1 Li1 Li1 57.47(9) . 4 ? Be1 Li1 Li1 57.86(6) 4 4 ? F3 Li1 Li1 123.00(16) . 4_545 ? F2 Li1 Li1 113.00(13) . 4_545 ? F1 Li1 Li1 32.53(3) 4_545 4_545 ? F1 Li1 Li1 71.05(12) . 4_545 ? Be1 Li1 Li1 134.82(12) 6 4_545 ? Be1 Li1 Li1 58.42(6) 4_545 4_545 ? Be1 Li1 Li1 58.73(9) . 4_545 ? Be1 Li1 Li1 134.33(15) 4 4_545 ? Li1 Li1 Li1 99.13(14) 4 4_545 ? F3 Li1 Li1 87.43(11) . 7_545 ? F2 Li1 Li1 65.74(10) . 7_545 ? F1 Li1 Li1 69.03(9) 4_545 7_545 ? F1 Li1 Li1 165.59(16) . 7_545 ? Be1 Li1 Li1 55.06(8) 6 7_545 ? Be1 Li1 Li1 54.40(7) 4_545 7_545 ? Be1 Li1 Li1 138.59(13) . 7_545 ? Be1 Li1 Li1 105.12(11) 4 7_545 ? Li1 Li1 Li1 161.34(13) 4 7_545 ? Li1 Li1 Li1 98.78(7) 4_545 7_545 ? F2 Be1 F4 114.69(13) 6_556 . ? F2 Be1 F3 107.92(12) 6_556 4_545 ? F4 Be1 F3 108.06(12) . 4_545 ? F2 Be1 F1 109.41(13) 6_556 . ? F4 Be1 F1 108.89(12) . . ? F3 Be1 F1 107.64(12) 4_545 . ? F2 Be1 Li1 32.54(7) 6_556 6_556 ? F4 Be1 Li1 146.47(12) . 6_556 ? F3 Be1 Li1 94.55(10) 4_545 6_556 ? F1 Be1 Li1 86.38(10) . 6_556 ? F2 Be1 Li1 81.82(10) 6_556 4 ? F4 Be1 Li1 105.82(11) . 4 ? F3 Be1 Li1 135.98(12) 4_545 4 ? F1 Be1 Li1 33.32(7) . 4 ? Li1 Be1 Li1 70.53(9) 6_556 4 ? F2 Be1 Li1 142.07(12) 6_556 . ? F4 Be1 Li1 91.39(9) . . ? F3 Be1 Li1 87.69(9) 4_545 . ? F1 Be1 Li1 33.06(7) . . ? Li1 Be1 Li1 114.49(10) 6_556 . ? Li1 Be1 Li1 64.11(7) 4 . ? F2 Be1 Li1 116.08(12) 6_556 4_545 ? F4 Be1 Li1 122.13(11) . 4_545 ? F3 Be1 Li1 29.59(7) 4_545 4_545 ? F1 Be1 Li1 78.23(9) . 4_545 ? Li1 Be1 Li1 89.61(9) 6_556 4_545 ? Li1 Be1 Li1 107.06(10) 4 4_545 ? Li1 Be1 Li1 63.41(7) . 4_545 ? Be1 F1 Li1 118.94(11) . 4 ? Be1 F1 Li1 119.75(12) . . ? Li1 F1 Li1 115.36(10) 4 . ? Be1 F2 Li1 120.75(12) 6 . ? Be1 F3 Li1 125.50(11) 4 . ? N1 C1 C1 109.67(16) . 5_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F4 0.939(18) 2.116(18) 3.0183(16) 160.8(16) 1_565 N1 H1 F3 0.939(18) 2.291(19) 2.9233(18) 124.2(14) 4 N1 H2 F3 0.92(2) 2.04(2) 2.8530(17) 147.0(16) 7 N1 H3 F4 0.88(2) 1.90(2) 2.7739(16) 169(2) . #===========================================================END data_2 _database_code_CSD 189069 _audit_creation_date 2002-06-25T14:00:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Methylammonium Lithiumtetrafluoroberyllate hydrate' _chemical_formula_sum 'C H8 Be F4 Li N O' _chemical_formula_weight 142.03 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.567(3) _cell_length_b 4.8493(10) _cell_length_c 9.974(2) _cell_angle_alpha 90 _cell_angle_beta 100.63(3) _cell_angle_gamma 90 _cell_volume 597.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2565 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_absorpt_correction_T_min 0.97772 _exptl_absorpt_correction_T_max 1.03278 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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 -0.144526 _diffrn_orient_matrix_ub_12 -0.727698E-1 _diffrn_orient_matrix_ub_13 -0.103301E-1 _diffrn_orient_matrix_ub_21 0.42897E-2 _diffrn_orient_matrix_ub_22 -0.26741E-2 _diffrn_orient_matrix_ub_23 -0.799208E-1 _diffrn_orient_matrix_ub_31 0.147021 _diffrn_orient_matrix_ub_32 -0.714424E-1 _diffrn_orient_matrix_ub_33 -0.78091E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_unetI/netI 0.0506 _diffrn_reflns_number 3779 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 1047 _reflns_number_gt 745 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0546P)^2^+0.0000P] 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_number_reflns 1047 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.216 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Li Li -0.0003 0.0001 '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' O O 0.0106 0.006 '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 Li1 Li 0.5040(3) 0.1843(8) 0.3524(4) 0.0251(9) Uani 1 1 d . . . Be1 Be 0.6299(3) 0.3083(6) 0.6268(3) 0.0228(7) Uani 1 1 d . . . F1 F 0.46566(10) -0.1814(3) 0.31322(12) 0.0246(4) Uani 1 1 d . . . F2 F 0.62774(11) 0.1982(3) 0.48290(13) 0.0260(4) Uani 1 1 d . . . F3 F 0.38438(11) 0.3743(3) 0.38024(13) 0.0287(4) Uani 1 1 d . . . F4 F 0.73628(11) 0.2445(3) 0.72664(13) 0.0305(4) Uani 1 1 d . . . N1 N 0.2720(2) 0.2216(5) 0.1047(2) 0.0263(5) Uani 1 1 d . . . H1 H 0.281(3) 0.075(8) 0.152(3) 0.069(12) Uiso 1 1 d . . . H2 H 0.284(2) 0.363(6) 0.160(3) 0.054(10) Uiso 1 1 d . . . H3 H 0.324(3) 0.232(6) 0.057(3) 0.049(10) Uiso 1 1 d . . . C1 C 0.1621(3) 0.2404(7) 0.0199(3) 0.0388(7) Uani 1 1 d . . . H4 H 0.150(3) 0.098(7) -0.050(3) 0.069(11) Uiso 1 1 d . . . H5 H 0.106(3) 0.237(7) 0.066(4) 0.078(13) Uiso 1 1 d . . . H6 H 0.161(2) 0.396(7) -0.043(3) 0.067(10) Uiso 1 1 d . . . O1 O 0.9535(2) 0.2242(5) 0.2542(3) 0.0595(8) Uani 1 1 d . . . H7 H 0.892(4) 0.241(9) 0.232(5) 0.096(17) Uiso 1 1 d . . . H8 H 0.983(3) 0.384(9) 0.256(4) 0.084(13) Uiso 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 Li1 0.029(2) 0.024(2) 0.024(2) 0.0023(15) 0.0082(17) -0.0013(17) Be1 0.0242(17) 0.0222(16) 0.0217(16) -0.0005(12) 0.0040(13) 0.0023(13) F1 0.0279(8) 0.0228(8) 0.0241(7) -0.0011(5) 0.0072(6) -0.0024(6) F2 0.0279(8) 0.0282(8) 0.0224(7) -0.0023(5) 0.0060(6) -0.0002(6) F3 0.0320(8) 0.0202(8) 0.0372(8) -0.0012(6) 0.0152(6) 0.0009(6) F4 0.0251(8) 0.0389(9) 0.0262(8) 0.0066(6) 0.0014(6) 0.0003(6) N1 0.0285(13) 0.0258(14) 0.0241(12) -0.0002(10) 0.0035(10) -0.0041(10) C1 0.0274(16) 0.046(2) 0.0418(17) 0.0046(14) 0.0023(13) -0.0004(13) O1 0.0288(14) 0.0365(14) 0.114(2) -0.0032(13) 0.0142(14) -0.0008(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Li1 F3 1.828(4) . ? Li1 F2 1.836(4) . ? Li1 F1 1.860(4) . ? Li1 F1 1.878(4) 2_655 ? Li1 Be1 2.952(5) 3_656 ? Li1 Be1 2.960(5) . ? Li1 Be1 2.979(5) 4_565 ? Li1 Be1 3.010(5) 3_666 ? Li1 Li1 3.159(5) 2_645 ? Li1 Li1 3.159(5) 2_655 ? Li1 Li1 3.463(7) 3_656 ? Be1 F2 1.527(3) . ? Be1 F4 1.543(3) . ? Be1 F3 1.550(3) 3_666 ? Be1 F1 1.564(4) 3_656 ? Be1 Li1 2.952(5) 3_656 ? Be1 Li1 2.979(5) 4_566 ? Be1 Li1 3.010(5) 3_666 ? F1 Be1 1.564(4) 3_656 ? F1 Li1 1.878(4) 2_645 ? F3 Be1 1.550(3) 3_666 ? N1 C1 1.483(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Li1 F2 119.1(2) . . ? F3 Li1 F1 108.9(2) . . ? F2 Li1 F1 109.7(2) . . ? F3 Li1 F1 105.4(2) . 2_655 ? F2 Li1 F1 109.2(2) . 2_655 ? F1 Li1 F1 103.46(18) . 2_655 ? F3 Li1 Be1 84.33(16) . 3_656 ? F2 Li1 Be1 113.52(17) . 3_656 ? F1 Li1 Be1 27.64(10) . 3_656 ? F1 Li1 Be1 123.58(18) 2_655 3_656 ? F3 Li1 Be1 94.09(16) . . ? F2 Li1 Be1 25.61(10) . . ? F1 Li1 Be1 117.48(18) . . ? F1 Li1 Be1 125.61(19) 2_655 . ? Be1 Li1 Be1 108.29(14) 3_656 . ? F3 Li1 Be1 132.46(19) . 4_565 ? F2 Li1 Be1 92.12(17) . 4_565 ? F1 Li1 Be1 90.36(15) . 4_565 ? F1 Li1 Be1 27.14(10) 2_655 4_565 ? Be1 Li1 Be1 116.88(16) 3_656 4_565 ? Be1 Li1 Be1 115.35(16) . 4_565 ? F3 Li1 Be1 24.67(10) . 3_666 ? F2 Li1 Be1 109.42(17) . 3_666 ? F1 Li1 Be1 131.8(2) . 3_666 ? F1 Li1 Be1 89.08(15) 2_655 3_666 ? Be1 Li1 Be1 108.84(17) 3_656 3_666 ? Be1 Li1 Be1 88.89(13) . 3_666 ? Be1 Li1 Be1 115.08(15) 4_565 3_666 ? F3 Li1 Li1 123.8(2) . 2_645 ? F2 Li1 Li1 114.1(2) . 2_645 ? F1 Li1 Li1 32.50(5) . 2_645 ? F1 Li1 Li1 71.67(18) 2_655 2_645 ? Be1 Li1 Li1 58.24(10) 3_656 2_645 ? Be1 Li1 Li1 134.55(17) . 2_645 ? Be1 Li1 Li1 58.64(15) 4_565 2_645 ? Be1 Li1 Li1 136.1(2) 3_666 2_645 ? F3 Li1 Li1 77.42(14) . 2_655 ? F2 Li1 Li1 110.64(19) . 2_655 ? F1 Li1 Li1 128.3(2) . 2_655 ? F1 Li1 Li1 32.15(13) 2_655 2_655 ? Be1 Li1 Li1 135.7(2) 3_656 2_655 ? Be1 Li1 Li1 112.94(15) . 2_655 ? Be1 Li1 Li1 57.40(14) 4_565 2_655 ? Be1 Li1 Li1 57.69(10) 3_666 2_655 ? Li1 Li1 Li1 100.3(2) 2_645 2_655 ? F3 Li1 Li1 88.67(18) . 3_656 ? F2 Li1 Li1 64.50(14) . 3_656 ? F1 Li1 Li1 68.85(14) . 3_656 ? F1 Li1 Li1 165.8(3) 2_655 3_656 ? Be1 Li1 Li1 54.25(12) 3_656 3_656 ? Be1 Li1 Li1 54.04(12) . 3_656 ? Be1 Li1 Li1 138.7(2) 4_565 3_656 ? Be1 Li1 Li1 104.99(18) 3_666 3_656 ? Li1 Li1 Li1 98.68(12) 2_645 3_656 ? Li1 Li1 Li1 160.6(2) 2_655 3_656 ? F2 Be1 F4 113.6(2) . . ? F2 Be1 F3 108.84(19) . 3_666 ? F4 Be1 F3 107.94(19) . 3_666 ? F2 Be1 F1 109.9(2) . 3_656 ? F4 Be1 F1 108.02(19) . 3_656 ? F3 Be1 F1 108.5(2) 3_666 3_656 ? F2 Be1 Li1 82.61(15) . 3_656 ? F4 Be1 Li1 103.28(16) . 3_656 ? F3 Be1 Li1 138.1(2) 3_666 3_656 ? F1 Be1 Li1 33.50(11) 3_656 3_656 ? F2 Be1 Li1 31.31(12) . . ? F4 Be1 Li1 143.85(19) . . ? F3 Be1 Li1 97.00(16) 3_666 . ? F1 Be1 Li1 87.50(15) 3_656 . ? Li1 Be1 Li1 71.71(14) 3_656 . ? F2 Be1 Li1 142.54(19) . 4_566 ? F4 Be1 Li1 91.87(15) . 4_566 ? F3 Be1 Li1 87.07(16) 3_666 4_566 ? F1 Be1 Li1 33.23(11) 3_656 4_566 ? Li1 Be1 Li1 64.37(11) 3_656 4_566 ? Li1 Be1 Li1 115.66(16) . 4_566 ? F2 Be1 Li1 115.93(17) . 3_666 ? F4 Be1 Li1 123.24(18) . 3_666 ? F3 Be1 Li1 29.49(11) 3_666 3_666 ? F1 Be1 Li1 79.41(15) 3_656 3_666 ? Li1 Be1 Li1 108.84(17) 3_656 3_666 ? Li1 Be1 Li1 91.11(13) . 3_666 ? Li1 Be1 Li1 63.66(11) 4_566 3_666 ? Be1 F1 Li1 118.86(18) 3_656 . ? Be1 F1 Li1 119.64(18) 3_656 2_645 ? Li1 F1 Li1 115.35(15) . 2_645 ? Be1 F2 Li1 123.08(19) . . ? Be1 F3 Li1 125.84(19) 3_666 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F4 0.85(4) 2.00(4) 2.831(3) 164(3) 3_656 N1 H2 F4 0.88(3) 2.25(3) 3.099(3) 163(3) 3_666 N1 H2 F3 0.88(3) 2.32(3) 2.943(3) 128(2) . N1 H3 F3 0.88(4) 2.10(4) 2.897(3) 149(3) 4_565 N1 H3 F1 0.88(4) 2.75(3) 3.281(3) 120(2) 2_655 O1 H7 F4 0.77(5) 1.95(5) 2.697(3) 164(5) 4_565 O1 H8 O1 0.86(4) 1.84(4) 2.699(2) 176(4) 2_755