# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_0912 _database_code_depnum_ccdc_archive 'CCDC 924305' #TrackingRef 'LaBeB3O7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B3 Be La O7' _chemical_formula_weight 292.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 '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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P m n 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 10.669(2) _cell_length_b 4.4434(9) _cell_length_c 4.2996(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 203.84(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153.15 _cell_measurement_reflns_used 1040 _cell_measurement_theta_min 3.8196 _cell_measurement_theta_max 33.6638 _exptl_crystal_description Chip _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 10.451 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.117 _exptl_absorpt_correction_T_max 0.352 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153.15 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2120 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 33.70 _reflns_number_total 778 _reflns_number_gt 771 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.430(16) _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 0.05(4) _refine_ls_number_reflns 778 _refine_ls_number_parameters 59 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.083 _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 La1 La 0.5000 0.21470(7) 0.2516 0.00468(16) Uani 1 2 d S . . O2 O 0.3687(3) 0.3629(9) -0.2866(11) 0.0042(9) Uani 1 1 d . . . Be1 Be 0.2502(4) 0.1829(10) -0.228(3) 0.0026(11) Uani 0.50 1 d PU . . B2 B 0.2502(4) 0.1829(10) -0.228(3) 0.0026(11) Uani 0.50 1 d PU . . B1 B 0.3793(5) 0.6822(10) -0.2152(18) 0.0038(10) Uani 1 1 d U . . O1 O 0.2744(4) 0.8571(9) -0.3671(9) 0.0064(6) Uani 1 1 d . . . O3 O 0.3713(5) 0.7208(8) 0.1235(12) 0.0056(8) Uani 1 1 d . . . O4 O 0.5000 0.8050(10) -0.3254(14) 0.0042(11) Uani 1 2 d S . . 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 La1 0.0036(2) 0.0062(2) 0.0042(2) 0.0000(4) 0.000 0.000 O2 0.0009(11) 0.0056(12) 0.006(3) -0.0027(14) 0.0003(12) 0.0003(10) Be1 0.0023(12) 0.0028(12) 0.0026(13) 0.0001(7) -0.0003(7) -0.0004(6) B2 0.0023(12) 0.0028(12) 0.0026(13) 0.0001(7) -0.0003(7) -0.0004(6) B1 0.0039(12) 0.0037(12) 0.0037(15) 0.0003(9) 0.0007(9) -0.0002(8) O1 0.0050(15) 0.0061(15) 0.0082(14) 0.0047(14) -0.0008(12) 0.0000(15) O3 0.008(2) 0.0051(17) 0.0034(19) 0.0000(12) 0.0015(17) -0.0011(12) O4 0.002(2) 0.003(2) 0.008(3) 0.0019(14) 0.000 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 La1 O2 2.517(5) 4_656 ? La1 O2 2.517(5) 1_556 ? La1 O4 2.573(5) 1_546 ? La1 O3 2.647(4) 1_545 ? La1 O3 2.647(4) 4_645 ? La1 O3 2.692(4) 4_655 ? La1 O3 2.692(4) . ? La1 O2 2.784(4) . ? La1 O2 2.784(4) 4_655 ? La1 O1 2.989(4) 2_565 ? La1 O1 2.989(4) 3_565 ? La1 B1 3.162(6) . ? O2 B1 1.456(6) . ? O2 Be1 1.518(6) . ? O2 La1 2.517(5) 1_554 ? Be1 O3 1.507(8) 2_564 ? Be1 O1 1.585(12) 2_565 ? Be1 O1 1.587(7) 1_545 ? Be1 Be1 2.695(5) 2_554 ? Be1 Be1 2.695(5) 2 ? Be1 La1 3.202(5) 2_554 ? B1 O3 1.469(10) . ? B1 O4 1.477(6) . ? B1 O1 1.511(7) . ? O1 B2 1.585(12) 2_564 ? O1 Be1 1.585(12) 2_564 ? O1 B2 1.587(7) 1_565 ? O1 Be1 1.587(7) 1_565 ? O1 La1 2.989(4) 2_564 ? O3 B2 1.507(8) 2_565 ? O3 Be1 1.507(8) 2_565 ? O3 La1 2.647(4) 1_565 ? O4 B1 1.477(6) 4_655 ? O4 La1 2.573(5) 1_564 ? 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 O2 La1 O2 67.61(17) 4_656 1_556 ? O2 La1 O4 68.14(13) 4_656 1_546 ? O2 La1 O4 68.14(13) 1_556 1_546 ? O2 La1 O3 132.04(14) 4_656 1_545 ? O2 La1 O3 95.31(14) 1_556 1_545 ? O4 La1 O3 63.92(14) 1_546 1_545 ? O2 La1 O3 95.31(14) 4_656 4_645 ? O2 La1 O3 132.04(14) 1_556 4_645 ? O4 La1 O3 63.92(14) 1_546 4_645 ? O3 La1 O3 62.5(2) 1_545 4_645 ? O2 La1 O3 70.07(14) 4_656 4_655 ? O2 La1 O3 103.10(14) 1_556 4_655 ? O4 La1 O3 137.37(14) 1_546 4_655 ? O3 La1 O3 156.2(2) 1_545 4_655 ? O3 La1 O3 112.7(2) 4_645 4_655 ? O2 La1 O3 103.10(14) 4_656 . ? O2 La1 O3 70.07(14) 1_556 . ? O4 La1 O3 137.37(14) 1_546 . ? O3 La1 O3 112.7(2) 1_545 . ? O3 La1 O3 156.2(2) 4_645 . ? O3 La1 O3 61.3(2) 4_655 . ? O2 La1 O2 150.88(16) 4_656 . ? O2 La1 O2 108.29(12) 1_556 . ? O4 La1 O2 139.01(11) 1_546 . ? O3 La1 O2 76.24(13) 1_545 . ? O3 La1 O2 106.50(14) 4_645 . ? O3 La1 O2 83.62(13) 4_655 . ? O3 La1 O2 51.37(13) . . ? O2 La1 O2 108.29(12) 4_656 4_655 ? O2 La1 O2 150.88(16) 1_556 4_655 ? O4 La1 O2 139.01(11) 1_546 4_655 ? O3 La1 O2 106.50(14) 1_545 4_655 ? O3 La1 O2 76.24(13) 4_645 4_655 ? O3 La1 O2 51.37(13) 4_655 4_655 ? O3 La1 O2 83.62(13) . 4_655 ? O2 La1 O2 60.41(16) . 4_655 ? O2 La1 O1 135.03(11) 4_656 2_565 ? O2 La1 O1 67.51(11) 1_556 2_565 ? O4 La1 O1 92.59(8) 1_546 2_565 ? O3 La1 O1 50.80(13) 1_545 2_565 ? O3 La1 O1 112.59(14) 4_645 2_565 ? O3 La1 O1 123.63(13) 4_655 2_565 ? O3 La1 O1 63.55(13) . 2_565 ? O2 La1 O1 52.45(11) . 2_565 ? O2 La1 O1 112.10(11) 4_655 2_565 ? O2 La1 O1 67.51(11) 4_656 3_565 ? O2 La1 O1 135.03(11) 1_556 3_565 ? O4 La1 O1 92.59(8) 1_546 3_565 ? O3 La1 O1 112.59(13) 1_545 3_565 ? O3 La1 O1 50.80(13) 4_645 3_565 ? O3 La1 O1 63.55(13) 4_655 3_565 ? O3 La1 O1 123.63(13) . 3_565 ? O2 La1 O1 112.10(11) . 3_565 ? O2 La1 O1 52.45(11) 4_655 3_565 ? O1 La1 O1 156.78(14) 2_565 3_565 ? O2 La1 B1 123.73(14) 4_656 . ? O2 La1 B1 95.87(15) 1_556 . ? O4 La1 B1 155.95(10) 1_546 . ? O3 La1 B1 101.62(14) 1_545 . ? O3 La1 B1 128.59(16) 4_645 . ? O3 La1 B1 61.90(14) 4_655 . ? O3 La1 B1 27.58(17) . . ? O2 La1 B1 27.41(13) . . ? O2 La1 B1 61.44(14) 4_655 . ? O1 La1 B1 64.08(12) 2_565 . ? O1 La1 B1 111.14(13) 3_565 . ? B1 O2 Be1 122.9(4) . . ? B1 O2 La1 112.2(3) . 1_554 ? Be1 O2 La1 117.2(4) . 1_554 ? B1 O2 La1 90.9(3) . . ? Be1 O2 La1 99.0(4) . . ? La1 O2 La1 108.29(12) 1_554 . ? O3 Be1 O2 119.8(5) 2_564 . ? O3 Be1 O1 107.7(5) 2_564 2_565 ? O2 Be1 O1 111.0(6) . 2_565 ? O3 Be1 O1 103.9(5) 2_564 1_545 ? O2 Be1 O1 106.4(4) . 1_545 ? O1 Be1 O1 107.0(4) 2_565 1_545 ? O3 Be1 Be1 80.4(4) 2_564 2_554 ? O2 Be1 Be1 100.8(4) . 2_554 ? O1 Be1 Be1 135.5(4) 2_565 2_554 ? O1 Be1 Be1 31.8(4) 1_545 2_554 ? O3 Be1 Be1 120.5(5) 2_564 2 ? O2 Be1 Be1 116.8(4) . 2 ? O1 Be1 Be1 31.86(15) 2_565 2 ? O1 Be1 Be1 75.5(4) 1_545 2 ? Be1 Be1 Be1 105.8(3) 2_554 2 ? O3 Be1 La1 55.1(2) 2_564 2_554 ? O2 Be1 La1 168.9(6) . 2_554 ? O1 Be1 La1 80.0(2) 2_565 2_554 ? O1 Be1 La1 67.8(2) 1_545 2_554 ? Be1 Be1 La1 69.2(3) 2_554 2_554 ? Be1 Be1 La1 71.8(2) 2 2_554 ? O3 Be1 La1 157.9(4) 2_564 . ? O2 Be1 La1 54.6(3) . . ? O1 Be1 La1 62.4(3) 2_565 . ? O1 Be1 La1 98.0(3) 1_545 . ? Be1 Be1 La1 120.9(3) 2_554 . ? Be1 Be1 La1 62.51(18) 2 . ? La1 Be1 La1 134.3(3) 2_554 . ? O2 B1 O3 108.6(4) . . ? O2 B1 O4 111.1(4) . . ? O3 B1 O4 109.0(5) . . ? O2 B1 O1 110.7(4) . . ? O3 B1 O1 109.0(5) . . ? O4 B1 O1 108.5(4) . . ? O2 B1 La1 61.7(3) . . ? O3 B1 La1 58.1(3) . . ? O4 B1 La1 95.2(3) . . ? O1 B1 La1 156.0(4) . . ? B1 O1 B2 119.2(4) . 2_564 ? B1 O1 Be1 119.2(4) . 2_564 ? B2 O1 Be1 0.0(4) 2_564 2_564 ? B1 O1 B2 115.3(4) . 1_565 ? B2 O1 B2 116.3(5) 2_564 1_565 ? Be1 O1 B2 116.3(5) 2_564 1_565 ? B1 O1 Be1 115.3(4) . 1_565 ? B2 O1 Be1 116.3(5) 2_564 1_565 ? Be1 O1 Be1 116.3(5) 2_564 1_565 ? B2 O1 Be1 0.0(3) 1_565 1_565 ? B1 O1 La1 126.6(3) . 2_564 ? B2 O1 La1 89.6(2) 2_564 2_564 ? Be1 O1 La1 89.6(2) 2_564 2_564 ? B2 O1 La1 82.7(2) 1_565 2_564 ? Be1 O1 La1 82.7(2) 1_565 2_564 ? B1 O3 B2 120.2(6) . 2_565 ? B1 O3 Be1 120.2(6) . 2_565 ? B2 O3 Be1 0.00(18) 2_565 2_565 ? B1 O3 La1 105.8(3) . 1_565 ? B2 O3 La1 97.0(3) 2_565 1_565 ? Be1 O3 La1 97.0(3) 2_565 1_565 ? B1 O3 La1 94.3(3) . . ? B2 O3 La1 126.1(4) 2_565 . ? Be1 O3 La1 126.1(4) 2_565 . ? La1 O3 La1 112.7(2) 1_565 . ? B1 O4 B1 121.4(6) . 4_655 ? B1 O4 La1 119.2(3) . 1_564 ? B1 O4 La1 119.2(3) 4_655 1_564 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.178 _refine_diff_density_min -2.679 _refine_diff_density_rms 0.302