# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm #TrackingRef '- ccdc_861193_cif.txt' _journal_coden_Cambridge 1350 _publ_contact_author_name 'Pan, Shi-Lie' _publ_contact_author_email slpan@ms.xjb.ac.cn _publ_section_title ; Li5Rb2B7O14: A new congruently melting Compound with two kinds of B-O one-dimensional chains and Short UV Absorption Edge ; loop_ _publ_author_name 'Yun Yang' 'Shi-Lie Pan' 'Xueling Hou' 'Xiaoyu Dong' 'Xin Su' ; Zhihua Yang ; 'Wenwu Zhao' 'Min Zhang' 'Zhaohui Chen' # Attachment 'XCray crystallographic file.cif' data_4 #TrackingRef '- ccdc_861193_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 861193' #TrackingRef 'XCray crystallographic file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B7 Li5 O14 Rb2' _chemical_formula_weight 505.31 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ama2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.376(2) _cell_length_b 13.5114(13) _cell_length_c 4.3900(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1208.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 24.99 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 8.179 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1769 _exptl_absorpt_correction_T_max 0.5607 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2864 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1024 _reflns_number_gt 983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0104(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(13) _refine_ls_number_reflns 1024 _refine_ls_number_parameters 134 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 0.346185(15) 0.31283(2) 1.03281(18) 0.02044(17) Uani 1 1 d . . . O1 O 0.2500 0.3134(2) 0.5255(18) 0.0189(8) Uani 1 2 d S . . O2 O 0.30879(11) 0.46429(17) 0.5319(9) 0.0157(5) Uani 1 1 d . . . O3 O 0.49189(14) 0.2816(2) 0.8560(7) 0.0148(6) Uani 1 1 d . . . O4 O 0.2500 0.6187(3) 0.4408(8) 0.0096(8) Uani 1 2 d S . . O5 O 0.32541(13) 0.60877(19) 0.8525(6) 0.0110(6) Uani 1 1 d . . . O6 O 0.36764(13) 0.60309(19) 0.3494(6) 0.0113(6) Uani 1 1 d . . . O7 O 0.42679(11) 0.52316(18) 0.9557(5) 0.0120(6) Uani 1 1 d . . . O8 O 0.52495(14) 0.1132(2) 0.9425(5) 0.0195(7) Uani 1 1 d . . . B1 B 0.2500 0.4120(4) 0.533(2) 0.0144(11) Uani 1 2 d S . . B2 B 0.31087(18) 0.5740(3) 0.5403(16) 0.0096(7) Uani 1 1 d . . . B3 B 0.50873(18) 0.2004(3) 1.0386(19) 0.0121(8) Uani 1 1 d . . . B4 B 0.37414(18) 0.5758(3) 1.0446(16) 0.0092(8) Uani 1 1 d . . . Li1 Li 0.2500 0.1748(6) 0.527(4) 0.0148(17) Uani 1 2 d S . . Li2 Li 0.4315(4) 0.5097(5) 0.518(2) 0.0313(16) Uani 1 1 d . . . Li3 Li 0.5120(3) 0.0850(4) 0.519(2) 0.0153(12) 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 Rb1 0.0178(2) 0.0197(2) 0.0238(2) -0.0013(3) 0.0010(3) 0.00073(13) O1 0.0261(18) 0.0095(18) 0.0209(19) 0.000(2) 0.000 0.000 O2 0.0162(12) 0.0103(12) 0.0207(12) 0.0022(19) -0.0014(19) 0.0020(9) O3 0.0266(15) 0.0070(13) 0.0106(14) -0.0014(12) 0.0001(12) 0.0013(12) O4 0.0104(16) 0.0098(18) 0.0085(19) 0.0009(14) 0.000 0.000 O5 0.0105(12) 0.0141(15) 0.0084(13) -0.0019(12) -0.0010(12) 0.0033(11) O6 0.0073(13) 0.0172(16) 0.0093(13) -0.0013(12) -0.0011(11) -0.0003(11) O7 0.0099(11) 0.0138(13) 0.0123(15) -0.0008(11) -0.0003(11) 0.0030(10) O8 0.0285(15) 0.0171(15) 0.0129(17) -0.0037(11) -0.0031(12) 0.0111(12) B1 0.023(3) 0.012(3) 0.008(2) -0.003(4) 0.000 0.000 B2 0.0096(17) 0.0133(19) 0.0060(16) -0.002(2) 0.004(3) -0.0001(13) B3 0.0113(17) 0.015(2) 0.0097(18) -0.005(3) 0.001(3) 0.0012(14) B4 0.0107(17) 0.0077(18) 0.0092(17) -0.001(3) 0.001(3) -0.0032(14) Li1 0.016(4) 0.011(4) 0.017(4) -0.006(6) 0.000 0.000 Li2 0.040(4) 0.035(4) 0.019(3) -0.005(5) 0.002(5) 0.023(3) Li3 0.018(3) 0.011(3) 0.017(3) 0.001(4) 0.001(4) 0.004(2) _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 Rb1 O1 2.919(6) 1_556 ? Rb1 O1 2.967(6) . ? Rb1 O6 2.978(3) 5_545 ? Rb1 O2 3.093(3) 1_556 ? Rb1 O3 3.097(3) . ? Rb1 O2 3.099(3) . ? Rb1 O5 3.123(3) 5_545 ? Rb1 O4 3.299(3) 5_545 ? Rb1 O7 3.300(2) . ? O1 B1 1.333(6) . ? O1 Li1 1.874(8) . ? O1 Rb1 2.919(6) 4_554 ? O1 Rb1 2.919(6) 1_554 ? O1 Rb1 2.967(6) 4 ? O2 B1 1.390(4) . ? O2 B2 1.483(4) . ? O2 Li2 2.574(8) . ? O2 Rb1 3.093(3) 1_554 ? O3 B3 1.402(6) . ? O3 B3 1.415(9) 6_654 ? O3 Li3 1.941(7) 6_655 ? O4 B2 1.447(4) . ? O4 B2 1.447(4) 4 ? O4 Li1 1.967(18) 5_554 ? O4 Rb1 3.299(3) 5_554 ? O4 Rb1 3.299(3) 8_554 ? O5 B4 1.377(6) . ? O5 B2 1.479(7) . ? O5 Li1 1.935(8) 5 ? O5 Rb1 3.123(3) 5_554 ? O6 B4 1.394(7) 1_554 ? O6 B2 1.481(6) . ? O6 Li2 1.958(8) . ? O6 Rb1 2.978(3) 5_554 ? O7 B4 1.345(5) . ? O7 Li2 1.930(10) . ? O7 Li3 1.942(6) 6_655 ? O7 Li3 1.947(6) 5 ? O7 Li2 2.479(10) 1_556 ? O8 B3 1.294(5) . ? O8 Li2 1.912(7) 6_655 ? O8 Li3 1.915(11) . ? O8 Li2 2.387(8) 5_545 ? O8 Li3 2.574(11) 1_556 ? O8 Rb1 3.336(3) 6_654 ? B1 O2 1.390(4) 4 ? B3 O3 1.415(9) 6_655 ? B4 O6 1.394(7) 1_556 ? Li1 O5 1.935(8) 8_544 ? Li1 O5 1.935(8) 5_544 ? Li1 O4 1.967(18) 5_545 ? Li2 O8 1.912(7) 6_654 ? Li2 O8 2.387(8) 5_554 ? Li2 O7 2.479(10) 1_554 ? Li3 O3 1.941(7) 6_654 ? Li3 O7 1.942(6) 6_654 ? Li3 O7 1.947(6) 5_544 ? Li3 O8 2.574(11) 1_554 ? 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 O1 Rb1 O1 96.471(12) 1_556 . ? O1 Rb1 O6 107.55(8) 1_556 5_545 ? O1 Rb1 O6 84.07(8) . 5_545 ? O1 Rb1 O2 46.20(8) 1_556 1_556 ? O1 Rb1 O2 111.54(10) . 1_556 ? O6 Rb1 O2 148.99(8) 5_545 1_556 ? O1 Rb1 O3 146.06(12) 1_556 . ? O1 Rb1 O3 116.45(12) . . ? O6 Rb1 O3 70.24(7) 5_545 . ? O2 Rb1 O3 120.25(7) 1_556 . ? O1 Rb1 O2 111.03(10) 1_556 . ? O1 Rb1 O2 45.82(8) . . ? O6 Rb1 O2 118.20(8) 5_545 . ? O2 Rb1 O2 90.30(6) 1_556 . ? O3 Rb1 O2 98.50(7) . . ? O1 Rb1 O5 65.06(8) 1_556 5_545 ? O1 Rb1 O5 104.49(9) . 5_545 ? O6 Rb1 O5 45.67(6) 5_545 5_545 ? O2 Rb1 O5 103.44(8) 1_556 5_545 ? O3 Rb1 O5 97.02(7) . 5_545 ? O2 Rb1 O5 150.30(7) . 5_545 ? O1 Rb1 Li3 128.2(2) 1_556 6_655 ? O1 Rb1 Li3 125.5(2) . 6_655 ? O6 Rb1 Li3 105.81(12) 5_545 6_655 ? O2 Rb1 Li3 87.16(16) 1_556 6_655 ? O3 Rb1 Li3 35.83(13) . 6_655 ? O2 Rb1 Li3 85.66(16) . 6_655 ? O5 Rb1 Li3 120.73(15) 5_545 6_655 ? O1 Rb1 B1 24.34(12) 1_556 1_556 ? O1 Rb1 B1 96.19(17) . 1_556 ? O6 Rb1 B1 131.83(11) 5_545 1_556 ? O2 Rb1 B1 25.27(9) 1_556 1_556 ? O3 Rb1 B1 143.86(11) . 1_556 ? O2 Rb1 B1 93.37(16) . 1_556 ? O5 Rb1 B1 88.79(13) 5_545 1_556 ? Li3 Rb1 B1 112.39(17) 6_655 1_556 ? O1 Rb1 O4 72.18(9) 1_556 5_545 ? O1 Rb1 O4 61.17(9) . 5_545 ? O6 Rb1 O4 45.38(6) 5_545 5_545 ? O2 Rb1 O4 117.80(7) 1_556 5_545 ? O3 Rb1 O4 115.49(6) . 5_545 ? O2 Rb1 O4 106.98(7) . 5_545 ? O5 Rb1 O4 43.32(7) 5_545 5_545 ? Li3 Rb1 O4 151.19(12) 6_655 5_545 ? B1 Rb1 O4 93.02(9) 1_556 5_545 ? O1 Rb1 O7 114.07(8) 1_556 . ? O1 Rb1 O7 104.45(8) . . ? O6 Rb1 O7 135.95(7) 5_545 . ? O2 Rb1 O7 68.01(6) 1_556 . ? O3 Rb1 O7 67.33(7) . . ? O2 Rb1 O7 58.73(6) . . ? O5 Rb1 O7 150.93(7) 5_545 . ? Li3 Rb1 O7 34.71(11) 6_655 . ? B1 Rb1 O7 90.82(10) 1_556 . ? O4 Rb1 O7 165.44(7) 5_545 . ? O1 Rb1 B2 81.33(11) 1_556 5_545 ? O1 Rb1 B2 82.32(12) . 5_545 ? O6 Rb1 B2 26.61(10) 5_545 5_545 ? O2 Rb1 B2 125.81(12) 1_556 5_545 ? O3 Rb1 B2 94.48(8) . 5_545 ? O2 Rb1 B2 126.73(12) . 5_545 ? O5 Rb1 B2 26.40(14) 5_545 5_545 ? Li3 Rb1 B2 128.09(12) 6_655 5_545 ? B1 Rb1 B2 105.43(14) 1_556 5_545 ? O4 Rb1 B2 25.31(8) 5_545 5_545 ? O7 Rb1 B2 161.78(8) . 5_545 ? B1 O1 Li1 178.4(10) . . ? B1 O1 Rb1 91.1(5) . 4_554 ? Li1 O1 Rb1 90.0(5) . 4_554 ? B1 O1 Rb1 91.1(5) . 1_554 ? Li1 O1 Rb1 90.0(5) . 1_554 ? Rb1 O1 Rb1 84.4(2) 4_554 1_554 ? B1 O1 Rb1 89.2(5) . . ? Li1 O1 Rb1 89.7(5) . . ? Rb1 O1 Rb1 179.1(2) 4_554 . ? Rb1 O1 Rb1 96.471(12) 1_554 . ? B1 O1 Rb1 89.2(5) . 4 ? Li1 O1 Rb1 89.7(5) . 4 ? Rb1 O1 Rb1 96.471(12) 4_554 4 ? Rb1 O1 Rb1 179.1(2) 1_554 4 ? Rb1 O1 Rb1 82.7(2) . 4 ? B1 O2 B2 122.1(3) . . ? B1 O2 Li2 163.2(3) . . ? B2 O2 Li2 74.6(2) . . ? B1 O2 Rb1 83.0(4) . 1_554 ? B2 O2 Rb1 132.2(4) . 1_554 ? Li2 O2 Rb1 84.39(19) . 1_554 ? B1 O2 Rb1 82.8(4) . . ? B2 O2 Rb1 129.4(4) . . ? Li2 O2 Rb1 86.3(2) . . ? Rb1 O2 Rb1 90.30(6) 1_554 . ? B3 O3 B3 134.5(4) . 6_654 ? B3 O3 Li3 121.7(5) . 6_655 ? B3 O3 Li3 101.7(4) 6_654 6_655 ? B3 O3 Rb1 101.4(2) . . ? B3 O3 Rb1 102.4(2) 6_654 . ? Li3 O3 Rb1 75.1(2) 6_655 . ? B2 O4 B2 118.0(4) . 4 ? B2 O4 Li1 116.1(3) . 5_554 ? B2 O4 Li1 116.1(3) 4 5_554 ? B2 O4 Rb1 77.64(18) . 5_554 ? B2 O4 Rb1 143.5(3) 4 5_554 ? Li1 O4 Rb1 78.9(2) 5_554 5_554 ? B2 O4 Rb1 143.5(3) . 8_554 ? B2 O4 Rb1 77.64(18) 4 8_554 ? Li1 O4 Rb1 78.9(2) 5_554 8_554 ? Rb1 O4 Rb1 72.88(7) 5_554 8_554 ? B4 O5 B2 127.5(3) . . ? B4 O5 Li1 118.6(6) . 5 ? B2 O5 Li1 110.8(5) . 5 ? B4 O5 Rb1 117.6(2) . 5_554 ? B2 O5 Rb1 83.8(2) . 5_554 ? Li1 O5 Rb1 83.1(4) 5 5_554 ? B4 O6 B2 123.1(3) 1_554 . ? B4 O6 Li2 97.5(3) 1_554 . ? B2 O6 Li2 97.6(3) . . ? B4 O6 Rb1 121.7(2) 1_554 5_554 ? B2 O6 Rb1 89.16(19) . 5_554 ? Li2 O6 Rb1 127.5(3) . 5_554 ? B4 O7 Li2 112.2(4) . . ? B4 O7 Li3 150.3(4) . 6_655 ? Li2 O7 Li3 92.3(4) . 6_655 ? B4 O7 Li3 116.3(3) . 5 ? Li2 O7 Li3 98.0(4) . 5 ? Li3 O7 Li3 74.3(3) 6_655 5 ? B4 O7 Li2 77.3(3) . 1_556 ? Li2 O7 Li2 169.1(4) . 1_556 ? Li3 O7 Li2 77.1(3) 6_655 1_556 ? Li3 O7 Li2 81.6(4) 5 1_556 ? B4 O7 Rb1 91.62(19) . . ? Li2 O7 Rb1 92.6(2) . . ? Li3 O7 Rb1 69.93(19) 6_655 . ? Li3 O7 Rb1 143.0(2) 5 . ? Li2 O7 Rb1 81.6(2) 1_556 . ? B3 O8 Li2 148.4(5) . 6_655 ? B3 O8 Li3 117.5(4) . . ? Li2 O8 Li3 93.5(4) 6_655 . ? B3 O8 Li2 106.5(3) . 5_545 ? Li2 O8 Li2 80.7(3) 6_655 5_545 ? Li3 O8 Li2 84.8(3) . 5_545 ? B3 O8 Li3 77.7(4) . 1_556 ? Li2 O8 Li3 75.4(3) 6_655 1_556 ? Li3 O8 Li3 155.6(3) . 1_556 ? Li2 O8 Li3 72.2(3) 5_545 1_556 ? B3 O8 Rb1 96.0(3) . 6_654 ? Li2 O8 Rb1 89.3(3) 6_655 6_654 ? Li3 O8 Rb1 69.2(2) . 6_654 ? Li2 O8 Rb1 151.5(2) 5_545 6_654 ? Li3 O8 Rb1 130.96(17) 1_556 6_654 ? O1 B1 O2 120.5(2) . 4 ? O1 B1 O2 120.5(2) . . ? O2 B1 O2 119.0(4) 4 . ? O1 B1 Rb1 64.5(4) . 4_554 ? O2 B1 Rb1 71.7(3) 4 4_554 ? O2 B1 Rb1 137.0(6) . 4_554 ? O1 B1 Rb1 64.5(4) . 1_554 ? O2 B1 Rb1 137.0(6) 4 1_554 ? O2 B1 Rb1 71.7(3) . 1_554 ? Rb1 B1 Rb1 74.6(2) 4_554 1_554 ? O1 B1 Rb1 66.5(4) . 4 ? O2 B1 Rb1 71.9(3) 4 4 ? O2 B1 Rb1 137.2(6) . 4 ? Rb1 B1 Rb1 85.50(8) 4_554 4 ? Rb1 B1 Rb1 131.02(18) 1_554 4 ? O4 B2 O5 108.6(3) . . ? O4 B2 O6 112.8(4) . . ? O5 B2 O6 106.4(3) . . ? O4 B2 O2 112.7(3) . . ? O5 B2 O2 110.3(5) . . ? O6 B2 O2 105.9(3) . . ? O4 B2 Li1 69.5(3) . 5 ? O5 B2 Li1 39.9(3) . 5 ? O6 B2 Li1 130.0(3) . 5 ? O2 B2 Li1 119.2(4) . 5 ? O4 B2 Rb1 77.06(19) . 5_554 ? O5 B2 Rb1 69.83(17) . 5_554 ? O6 B2 Rb1 64.23(17) . 5_554 ? O2 B2 Rb1 168.9(2) . 5_554 ? Li1 B2 Rb1 68.4(2) 5 5_554 ? O8 B3 O3 126.1(7) . . ? O8 B3 O3 118.7(5) . 6_655 ? O3 B3 O3 115.2(3) . 6_655 ? O8 B3 Li3 73.5(4) . 1_556 ? O3 B3 Li3 158.6(4) . 1_556 ? O3 B3 Li3 46.4(3) 6_655 1_556 ? O8 B3 Li3 37.9(3) . . ? O3 B3 Li3 88.6(4) . . ? O3 B3 Li3 155.6(3) 6_655 . ? Li3 B3 Li3 109.2(2) 1_556 . ? O8 B3 Rb1 127.5(3) . . ? O3 B3 Rb1 56.43(17) . . ? O3 B3 Rb1 85.8(2) 6_655 . ? Li3 B3 Rb1 106.0(2) 1_556 . ? Li3 B3 Rb1 104.5(2) . . ? O8 B3 Rb1 86.7(3) . 6_655 ? O3 B3 Rb1 125.0(2) . 6_655 ? O3 B3 Rb1 55.5(2) 6_655 6_655 ? Li3 B3 Rb1 58.37(17) 1_556 6_655 ? Li3 B3 Rb1 116.17(18) . 6_655 ? Rb1 B3 Rb1 139.1(2) . 6_655 ? O8 B3 Rb1 63.7(3) . 6_654 ? O3 B3 Rb1 83.7(3) . 6_654 ? O3 B3 Rb1 127.3(2) 6_655 6_654 ? Li3 B3 Rb1 115.70(19) 1_556 6_654 ? Li3 B3 Rb1 57.22(17) . 6_654 ? Rb1 B3 Rb1 137.9(2) . 6_654 ? Rb1 B3 Rb1 73.09(7) 6_655 6_654 ? O7 B4 O5 124.6(5) . . ? O7 B4 O6 119.6(4) . 1_556 ? O5 B4 O6 115.7(3) . 1_556 ? O7 B4 Li2 71.7(3) . 1_556 ? O5 B4 Li2 160.8(4) . 1_556 ? O6 B4 Li2 49.7(3) 1_556 1_556 ? O7 B4 Li2 40.8(3) . . ? O5 B4 Li2 84.0(4) . . ? O6 B4 Li2 159.5(3) 1_556 . ? Li2 B4 Li2 112.3(3) 1_556 . ? O7 B4 Li3 38.3(2) . 5 ? O5 B4 Li3 132.9(5) . 5 ? O6 B4 Li3 96.9(4) 1_556 5 ? Li2 B4 Li3 65.8(3) 1_556 5 ? Li2 B4 Li3 63.6(3) . 5 ? O7 B4 Rb1 66.45(17) . . ? O5 B4 Rb1 101.4(2) . . ? O6 B4 Rb1 105.1(3) 1_556 . ? Li2 B4 Rb1 74.8(2) 1_556 . ? Li2 B4 Rb1 74.54(19) . . ? Li3 B4 Rb1 101.63(15) 5 . ? O1 Li1 O5 117.3(5) . 8_544 ? O1 Li1 O5 117.3(5) . 5_544 ? O5 Li1 O5 105.1(6) 8_544 5_544 ? O1 Li1 O4 112.9(8) . 5_545 ? O5 Li1 O4 100.9(5) 8_544 5_545 ? O5 Li1 O4 100.9(5) 5_544 5_545 ? O1 Li1 B2 118.7(7) . 8_544 ? O5 Li1 B2 29.3(3) 8_544 8_544 ? O5 Li1 B2 80.0(5) 5_544 8_544 ? O4 Li1 B2 120.9(3) 5_545 8_544 ? O1 Li1 B2 118.7(7) . 5_544 ? O5 Li1 B2 80.0(5) 8_544 5_544 ? O5 Li1 B2 29.3(3) 5_544 5_544 ? O4 Li1 B2 120.9(3) 5_545 5_544 ? B2 Li1 B2 52.1(3) 8_544 5_544 ? O1 Li1 Rb1 57.3(4) . 4_554 ? O5 Li1 Rb1 63.3(3) 8_544 4_554 ? O5 Li1 Rb1 116.6(7) 5_544 4_554 ? O4 Li1 Rb1 141.7(3) 5_545 4_554 ? B2 Li1 Rb1 62.4(3) 8_544 4_554 ? B2 Li1 Rb1 91.9(5) 5_544 4_554 ? O1 Li1 Rb1 57.3(4) . 1_554 ? O5 Li1 Rb1 116.6(7) 8_544 1_554 ? O5 Li1 Rb1 63.3(3) 5_544 1_554 ? O4 Li1 Rb1 141.7(3) 5_545 1_554 ? B2 Li1 Rb1 91.9(5) 8_544 1_554 ? B2 Li1 Rb1 62.4(3) 5_544 1_554 ? Rb1 Li1 Rb1 68.8(3) 4_554 1_554 ? O1 Li1 Rb1 58.0(4) . 4 ? O5 Li1 Rb1 93.0(2) 8_544 4 ? O5 Li1 Rb1 160.4(6) 5_544 4 ? O4 Li1 Rb1 67.7(4) 5_545 4 ? B2 Li1 Rb1 119.44(10) 8_544 4 ? B2 Li1 Rb1 169.7(5) 5_544 4 ? Rb1 Li1 Rb1 78.10(11) 4_554 4 ? Rb1 Li1 Rb1 115.2(2) 1_554 4 ? O8 Li2 O7 106.2(4) 6_654 . ? O8 Li2 O6 143.3(5) 6_654 . ? O7 Li2 O6 106.5(4) . . ? O8 Li2 O8 96.5(3) 6_654 5_554 ? O7 Li2 O8 97.1(4) . 5_554 ? O6 Li2 O8 95.7(3) . 5_554 ? O8 Li2 O7 84.7(3) 6_654 1_554 ? O7 Li2 O7 169.1(4) . 1_554 ? O6 Li2 O7 63.2(3) . 1_554 ? O8 Li2 O7 81.3(3) 5_554 1_554 ? O8 Li2 B4 112.0(4) 6_654 1_554 ? O7 Li2 B4 139.1(3) . 1_554 ? O6 Li2 B4 32.9(2) . 1_554 ? O8 Li2 B4 92.7(3) 5_554 1_554 ? O7 Li2 B4 31.00(16) 1_554 1_554 ? O8 Li2 O2 104.4(3) 6_654 . ? O7 Li2 O2 87.2(3) . . ? O6 Li2 O2 61.1(2) . . ? O8 Li2 O2 156.6(3) 5_554 . ? O7 Li2 O2 90.2(3) 1_554 . ? B4 Li2 O2 69.9(2) 1_554 . ? O8 Li2 B4 128.9(4) 6_654 . ? O7 Li2 B4 27.05(17) . . ? O6 Li2 B4 80.0(3) . . ? O8 Li2 B4 105.5(3) 5_554 . ? O7 Li2 B4 143.2(3) 1_554 . ? B4 Li2 B4 112.3(3) 1_554 . ? O2 Li2 B4 69.2(2) . . ? O8 Li2 Li3 43.3(2) 6_654 6_654 ? O7 Li2 Li3 147.7(4) . 6_654 ? O6 Li2 Li3 105.8(4) . 6_654 ? O8 Li2 Li3 80.2(3) 5_554 6_654 ? O7 Li2 Li3 42.8(2) 1_554 6_654 ? B4 Li2 Li3 73.1(3) 1_554 6_654 ? O2 Li2 Li3 108.1(3) . 6_654 ? B4 Li2 Li3 171.6(4) . 6_654 ? O8 Li2 Li3 63.1(3) 6_654 6_655 ? O7 Li2 Li3 44.0(3) . 6_655 ? O6 Li2 Li3 150.2(4) . 6_655 ? O8 Li2 Li3 92.8(3) 5_554 6_655 ? O7 Li2 Li3 146.5(3) 1_554 6_655 ? B4 Li2 Li3 173.1(4) 1_554 6_655 ? O2 Li2 Li3 105.9(3) . 6_655 ? B4 Li2 Li3 70.2(3) . 6_655 ? Li3 Li2 Li3 103.8(3) 6_654 6_655 ? O8 Li2 Li2 57.1(2) 6_654 2_665 ? O7 Li2 Li2 93.3(3) . 2_665 ? O6 Li2 Li2 136.2(4) . 2_665 ? O8 Li2 Li2 42.3(2) 5_554 2_665 ? O7 Li2 Li2 92.6(2) 1_554 2_665 ? B4 Li2 Li2 119.3(3) 1_554 2_665 ? O2 Li2 Li2 160.8(4) . 2_665 ? B4 Li2 Li2 117.1(2) . 2_665 ? Li3 Li2 Li2 63.0(2) 6_654 2_665 ? Li3 Li2 Li2 63.0(2) 6_655 2_665 ? O8 Li2 Li3 84.9(3) 6_654 5_554 ? O7 Li2 Li3 137.8(4) . 5_554 ? O6 Li2 Li3 82.2(3) . 5_554 ? O8 Li2 Li3 40.8(2) 5_554 5_554 ? O7 Li2 Li3 41.3(2) 1_554 5_554 ? B4 Li2 Li3 61.5(3) 1_554 5_554 ? O2 Li2 Li3 130.2(4) . 5_554 ? B4 Li2 Li3 139.4(3) . 5_554 ? Li3 Li2 Li3 48.5(3) 6_654 5_554 ? Li3 Li2 Li3 121.2(3) 6_655 5_554 ? Li2 Li2 Li3 58.2(2) 2_665 5_554 ? O8 Li3 O3 100.3(3) . 6_654 ? O8 Li3 O7 101.6(4) . 6_654 ? O3 Li3 O7 132.2(5) 6_654 6_654 ? O8 Li3 O7 110.3(4) . 5_544 ? O3 Li3 O7 108.0(3) 6_654 5_544 ? O7 Li3 O7 103.2(3) 6_654 5_544 ? O8 Li3 Li3 102.9(2) . 2_655 ? O3 Li3 Li3 154.1(4) 6_654 2_655 ? O7 Li3 Li3 52.9(2) 6_654 2_655 ? O7 Li3 Li3 52.7(2) 5_544 2_655 ? O8 Li3 O8 155.6(3) . 1_554 ? O3 Li3 O8 60.2(3) 6_654 1_554 ? O7 Li3 O8 84.5(3) 6_654 1_554 ? O7 Li3 O8 90.8(4) 5_544 1_554 ? Li3 Li3 O8 99.55(15) 2_655 1_554 ? O8 Li3 B3 131.7(3) . 1_554 ? O3 Li3 B3 31.9(2) 6_654 1_554 ? O7 Li3 B3 110.3(4) 6_654 1_554 ? O7 Li3 B3 96.7(3) 5_544 1_554 ? Li3 Li3 B3 125.1(2) 2_655 1_554 ? O8 Li3 B3 28.81(16) 1_554 1_554 ? O8 Li3 B3 24.55(16) . . ? O3 Li3 B3 77.3(3) 6_654 . ? O7 Li3 B3 124.0(4) 6_654 . ? O7 Li3 B3 109.8(4) 5_544 . ? Li3 Li3 B3 123.2(2) 2_655 . ? O8 Li3 B3 137.0(3) 1_554 . ? B3 Li3 B3 109.2(2) 1_554 . ? O8 Li3 Li2 43.2(3) . 6_655 ? O3 Li3 Li2 137.2(4) 6_654 6_655 ? O7 Li3 Li2 60.1(3) 6_654 6_655 ? O7 Li3 Li2 106.5(4) 5_544 6_655 ? Li3 Li3 Li2 68.7(2) 2_655 6_655 ? O8 Li3 Li2 143.0(3) 1_554 6_655 ? B3 Li3 Li2 156.3(3) 1_554 6_655 ? B3 Li3 Li2 67.7(3) . 6_655 ? O8 Li3 Li2 142.9(3) . 6_654 ? O3 Li3 Li2 98.7(4) 6_654 6_654 ? O7 Li3 Li2 43.7(2) 6_654 6_654 ? O7 Li3 Li2 93.3(4) 5_544 6_654 ? Li3 Li3 Li2 68.7(2) 2_655 6_654 ? O8 Li3 Li2 41.5(2) 1_554 6_654 ? B3 Li3 Li2 69.5(3) 1_554 6_654 ? B3 Li3 Li2 156.6(3) . 6_654 ? Li2 Li3 Li2 103.8(3) 6_655 6_654 ? O8 Li3 B4 96.2(4) . 5_544 ? O3 Li3 B4 90.9(2) 6_654 5_544 ? O7 Li3 B4 127.8(3) 6_654 5_544 ? O7 Li3 B4 25.38(14) 5_544 5_544 ? Li3 Li3 B4 75.5(3) 2_655 5_544 ? O8 Li3 B4 98.5(3) 1_554 5_544 ? B3 Li3 B4 91.9(3) 1_554 5_544 ? B3 Li3 B4 88.2(3) . 5_544 ? Li2 Li3 B4 111.2(4) 6_655 5_544 ? Li2 Li3 B4 115.0(4) 6_654 5_544 ? O8 Li3 Li2 54.5(3) . 5_545 ? O3 Li3 Li2 125.3(3) 6_654 5_545 ? O7 Li3 Li2 101.9(3) 6_654 5_545 ? O7 Li3 Li2 57.1(3) 5_544 5_545 ? Li3 Li3 Li2 62.8(2) 2_655 5_545 ? O8 Li3 Li2 147.9(3) 1_554 5_545 ? B3 Li3 Li2 142.8(3) 1_554 5_545 ? B3 Li3 Li2 64.2(3) . 5_545 ? Li2 Li3 Li2 58.8(4) 6_655 5_545 ? Li2 Li3 Li2 131.5(2) 6_654 5_545 ? B4 Li3 Li2 52.7(2) 5_544 5_545 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.394 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.089