# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Lee Antony Gerrard' 'M. Weller' _publ_contact_author_name 'Dr Lee Antony 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 'Chemical Communications' _publ_section_title ; The first organically templated 1-D lithioberyllofluoride chain, [LiBe2F7][C4N2H12][H2O]1.5 ; data_s92 _database_code_CSD 197150 _audit_creation_date 2002-09-25T15:43:33-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Piperazinium Lithium Heptafluorodiberyllium sesquihydrate' _chemical_formula_sum 'C4 H15 Be2 F7 Li N2 O1.50' _chemical_formula_weight 273.14 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.318(5) _cell_length_b 8.138(5) _cell_length_c 10.007(5) _cell_angle_alpha 71.910(5) _cell_angle_beta 76.832(5) _cell_angle_gamma 81.816(5) _cell_volume 549.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2391 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 278 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.89178 _exptl_absorpt_correction_T_max 1.09616 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.768593E-1 _diffrn_orient_matrix_UB_12 0.965607E-1 _diffrn_orient_matrix_UB_13 -0.652477E-1 _diffrn_orient_matrix_UB_21 -0.443168E-1 _diffrn_orient_matrix_UB_22 -0.120083E-1 _diffrn_orient_matrix_UB_23 -0.837061E-1 _diffrn_orient_matrix_UB_31 -0.109291 _diffrn_orient_matrix_UB_32 0.85698E-1 _diffrn_orient_matrix_UB_33 0.149959E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_number 11909 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 2493 _reflns_number_gt 2163 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement ; SCALEPACK (Otwinoski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS (Dowty, 1999)' _computing_publication_material 'WINGX (Farrugia, 1998)' #----------------------------------------------------------------------------# # 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^)+(0.0540P)^2^+0.2874P] 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 0.007(6) _refine_ls_number_reflns 2493 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.613 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Be1 Be 0.6167(3) 0.7544(2) 0.3536(2) 0.0153(4) Uani 1 1 d . . . Be2 Be 0.9397(3) 0.5067(2) 0.28752(19) 0.0150(4) Uani 1 1 d . . . Li1 Li 0.7247(3) 0.4587(3) 0.5913(3) 0.0164(5) Uani 1 1 d . . . F1 F 0.87641(12) 0.38806(11) 0.44050(9) 0.0165(2) Uani 1 1 d . . . F2 F 0.93587(12) 0.40983(12) 0.17837(9) 0.0193(2) Uani 1 1 d . . . F3 F 0.80175(13) 0.67792(12) 0.26290(10) 0.0235(2) Uani 1 1 d . . . F4 F 0.85734(12) 0.44154(11) 0.73479(9) 0.0177(2) Uani 1 1 d . . . F5 F 0.61903(13) 0.67569(11) 0.51351(9) 0.0195(2) Uani 1 1 d . . . F6 F 0.44244(12) 0.70729(11) 0.31371(9) 0.0200(2) Uani 1 1 d . . . F7 F 0.61980(13) 0.95240(11) 0.30962(10) 0.0202(2) Uani 1 1 d . . . N1 N 0.83027(18) 0.05535(17) 0.44353(14) 0.0161(3) Uani 1 1 d . . . C1 C 1.0121(2) 0.0160(2) 0.35039(16) 0.0172(3) Uani 1 1 d . . . C2 C 0.8236(2) -0.0499(2) 0.59601(16) 0.0170(3) Uani 1 1 d . . . N2 N 0.69238(17) 0.44372(16) 0.01286(13) 0.0151(3) Uani 1 1 d . . . C3 C 0.5352(2) 0.3370(2) 0.10548(16) 0.0173(3) Uani 1 1 d . . . C4 C 0.6278(2) 0.6316(2) -0.02844(17) 0.0184(3) Uani 1 1 d . . . H1 H 0.736(3) 0.026(3) 0.413(2) 0.034(6) Uiso 1 1 d . . . H2 H 0.823(3) 0.169(3) 0.435(2) 0.023(5) Uiso 1 1 d . . . H3 H 1.016(3) -0.102(2) 0.3535(19) 0.016(4) Uiso 1 1 d . . . H4 H 1.012(3) 0.091(3) 0.253(2) 0.022(5) Uiso 1 1 d . . . H5 H 0.826(3) -0.168(3) 0.598(2) 0.022(5) Uiso 1 1 d . . . H6 H 0.703(3) -0.020(3) 0.651(2) 0.024(5) Uiso 1 1 d . . . H7 H 0.786(3) 0.425(3) 0.056(2) 0.025(5) Uiso 1 1 d . . . H8 H 0.739(3) 0.410(2) -0.066(2) 0.021(5) Uiso 1 1 d . . . H9 H 0.499(3) 0.376(2) 0.192(2) 0.019(4) Uiso 1 1 d . . . H10 H 0.580(3) 0.222(3) 0.1264(19) 0.019(4) Uiso 1 1 d . . . H11 H 0.734(3) 0.693(3) -0.093(2) 0.026(5) Uiso 1 1 d . . . H12 H 0.592(3) 0.667(2) 0.060(2) 0.021(5) Uiso 1 1 d . . . O1A O 1.0103(4) 0.9101(4) 0.0190(3) 0.0475(7) Uani 0.5 1 d P . . O2A O 1.3293(2) -0.0539(2) 0.08337(15) 0.0540(5) 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 Be1 0.0147(9) 0.0150(9) 0.0175(9) -0.0049(7) -0.0054(7) -0.0012(7) Be2 0.0147(9) 0.0172(9) 0.0136(8) -0.0047(7) -0.0032(6) -0.0013(7) Li1 0.0171(12) 0.0163(12) 0.0173(12) -0.0064(10) -0.0037(9) -0.0018(9) F1 0.0187(4) 0.0148(4) 0.0150(4) -0.0049(3) -0.0009(3) -0.0009(3) F2 0.0192(5) 0.0241(5) 0.0196(4) -0.0111(4) -0.0087(3) 0.0011(3) F3 0.0211(5) 0.0226(5) 0.0226(5) -0.0047(4) -0.0027(4) 0.0047(4) F4 0.0158(4) 0.0245(5) 0.0149(4) -0.0064(3) -0.0036(3) -0.0054(3) F5 0.0248(5) 0.0181(4) 0.0165(4) -0.0059(3) -0.0072(3) 0.0028(3) F6 0.0189(5) 0.0211(5) 0.0210(4) -0.0019(4) -0.0084(3) -0.0072(3) F7 0.0226(5) 0.0135(4) 0.0269(5) -0.0042(4) -0.0122(4) -0.0015(3) N1 0.0137(6) 0.0151(6) 0.0212(6) -0.0064(5) -0.0057(5) -0.0002(5) C1 0.0163(7) 0.0177(7) 0.0185(7) -0.0067(6) -0.0033(5) -0.0011(5) C2 0.0143(7) 0.0171(7) 0.0198(7) -0.0062(6) -0.0021(5) -0.0018(5) N2 0.0127(6) 0.0207(6) 0.0126(6) -0.0055(5) -0.0042(5) 0.0006(5) C3 0.0178(7) 0.0167(7) 0.0160(7) -0.0012(6) -0.0048(6) -0.0025(6) C4 0.0172(7) 0.0173(7) 0.0208(7) -0.0025(6) -0.0064(6) -0.0045(6) O1A 0.0415(17) 0.0656(19) 0.0349(15) -0.0114(15) -0.0071(12) -0.0097(15) O2A 0.0598(10) 0.0623(11) 0.0209(7) -0.0017(7) -0.0065(6) 0.0314(8) #----------------------------------------------------------------------------# # 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 Be1 F5 1.531(2) . ? Be1 F7 1.535(2) . ? Be1 F6 1.549(2) . ? Be1 F3 1.611(2) . ? Be1 Li1 2.972(3) . ? Be1 Li1 3.093(3) 2_666 ? Be2 F2 1.539(2) . ? Be2 F1 1.542(2) . ? Be2 F4 1.550(2) 2_766 ? Be2 F3 1.588(2) . ? Be2 Li1 3.022(3) . ? Be2 Li1 3.058(3) 2_766 ? Li1 F5 1.831(3) . ? Li1 F6 1.835(3) 2_666 ? Li1 F1 1.854(3) . ? Li1 F4 1.869(3) . ? Li1 Be2 3.058(3) 2_766 ? Li1 Be1 3.093(3) 2_666 ? F4 Be2 1.550(2) 2_766 ? F6 Li1 1.835(3) 2_666 ? N1 C2 1.494(2) . ? N1 C1 1.497(2) . ? C1 C2 1.513(2) 2_756 ? C2 C1 1.513(2) 2_756 ? N2 C4 1.491(2) . ? N2 C3 1.4949(19) . ? C3 C4 1.515(2) 2_665 ? C4 C3 1.515(2) 2_665 ? O1A O1A 1.388(7) 2_775 ? 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 F5 Be1 F7 110.95(12) . . ? F5 Be1 F6 111.71(12) . . ? F7 Be1 F6 109.32(12) . . ? F5 Be1 F3 108.78(12) . . ? F7 Be1 F3 108.23(12) . . ? F6 Be1 F3 107.74(13) . . ? F5 Be1 Li1 30.71(7) . . ? F7 Be1 Li1 135.99(11) . . ? F6 Be1 Li1 107.55(11) . . ? F3 Be1 Li1 82.04(10) . . ? F5 Be1 Li1 86.44(9) . 2_666 ? F7 Be1 Li1 127.76(11) . 2_666 ? F6 Be1 Li1 26.19(7) . 2_666 ? F3 Be1 Li1 111.75(11) . 2_666 ? Li1 Be1 Li1 82.35(9) . 2_666 ? F2 Be2 F1 109.29(13) . . ? F2 Be2 F4 108.42(12) . 2_766 ? F1 Be2 F4 111.07(12) . 2_766 ? F2 Be2 F3 110.43(12) . . ? F1 Be2 F3 109.04(12) . . ? F4 Be2 F3 108.58(13) 2_766 . ? F2 Be2 Li1 130.66(11) . . ? F1 Be2 Li1 29.98(7) . . ? F4 Be2 Li1 112.92(10) 2_766 . ? F3 Be2 Li1 80.72(9) . . ? F2 Be2 Li1 128.06(11) . 2_766 ? F1 Be2 Li1 82.81(10) . 2_766 ? F4 Be2 Li1 29.42(7) 2_766 2_766 ? F3 Be2 Li1 112.44(11) . 2_766 ? Li1 Be2 Li1 84.43(9) . 2_766 ? F5 Li1 F6 115.41(14) . 2_666 ? F5 Li1 F1 106.71(13) . . ? F6 Li1 F1 107.17(13) 2_666 . ? F5 Li1 F4 115.26(13) . . ? F6 Li1 F4 100.58(13) 2_666 . ? F1 Li1 F4 111.52(14) . . ? F5 Li1 Be1 25.27(6) . . ? F6 Li1 Be1 118.63(12) 2_666 . ? F1 Li1 Be1 82.27(10) . . ? F4 Li1 Be1 132.86(12) . . ? F5 Li1 Be2 82.86(10) . . ? F6 Li1 Be2 124.40(12) 2_666 . ? F1 Li1 Be2 24.55(6) . . ? F4 Li1 Be2 118.79(12) . . ? Be1 Li1 Be2 59.50(7) . . ? F5 Li1 Be2 108.89(11) . 2_766 ? F6 Li1 Be2 122.14(12) 2_666 2_766 ? F1 Li1 Be2 93.10(11) . 2_766 ? F4 Li1 Be2 24.04(6) . 2_766 ? Be1 Li1 Be2 117.45(10) . 2_766 ? Be2 Li1 Be2 95.57(9) . 2_766 ? F5 Li1 Be1 99.45(11) . 2_666 ? F6 Li1 Be1 21.87(6) 2_666 2_666 ? F1 Li1 Be1 99.68(11) . 2_666 ? F4 Li1 Be1 122.12(12) . 2_666 ? Be1 Li1 Be1 97.65(9) . 2_666 ? Be2 Li1 Be1 109.88(9) . 2_666 ? Be2 Li1 Be1 143.99(10) 2_766 2_666 ? Be2 F1 Li1 125.47(12) . . ? Be2 F3 Be1 136.81(11) . . ? Be2 F4 Li1 126.54(11) 2_766 . ? Be1 F5 Li1 124.02(11) . . ? Be1 F6 Li1 131.94(12) . 2_666 ? C2 N1 C1 111.07(12) . . ? N1 C1 C2 110.22(13) . 2_756 ? N1 C2 C1 110.03(12) . 2_756 ? C4 N2 C3 111.03(12) . . ? N2 C3 C4 109.97(12) . 2_665 ? N2 C4 C3 110.54(12) . 2_665 ?