# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yang, Guo-Yu' _publ_contact_author_email ygy@fjirsm.ac.cn _publ_section_title ; Two additive-induced isomeric aluminoborates templated by methylamine ; _publ_author_name 'Guo-Yu Yang' # Attachment '- 763046-763047.cif' data_1 #TrackingRef '- 763046-763047.cif' _database_code_depnum_ccdc_archive 'CCDC 763046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H16 Al B5 N2 O12' _chemical_formula_weight 341.20 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 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 10.9744(18) _cell_length_b 10.9744(18) _cell_length_c 23.216(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2796.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4396 _cell_measurement_theta_min 3.1569 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Octahedral _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8816 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SCXimini CCD' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11402 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1594 _reflns_number_gt 1491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0675P)^2^+0.8026P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(3) _refine_ls_number_reflns 1594 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _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 Al1 Al 1.0000 0.0000 0.0000 0.0151(2) Uani 1 4 d S . . Al2 Al 1.5000 0.5000 0.0000 0.0144(2) Uani 1 4 d S . . B1 B 1.07304(18) 0.1805(2) 0.08458(9) 0.0211(4) Uani 1 1 d . . . B2 B 1.2728(3) 0.2500 0.1250 0.0224(7) Uani 1 2 d S . . B3 B 1.47164(18) 0.31976(18) 0.08508(8) 0.0177(4) Uani 1 1 d . . . O1 O 1.00707(14) 0.12743(13) 0.04363(6) 0.0309(4) Uani 1 1 d . . . O2 O 1.19725(13) 0.17237(14) 0.08755(6) 0.0269(3) Uani 1 1 d . . . O3 O 1.01229(18) 0.2500 0.1250 0.0303(5) Uani 1 2 d S . . O4 O 1.34855(13) 0.32632(15) 0.08702(6) 0.0287(4) Uani 1 1 d . . . O5 O 1.53881(12) 0.37839(12) 0.04492(6) 0.0226(3) Uani 1 1 d . . . O6 O 1.53422(17) 0.2500 0.1250 0.0317(5) Uani 1 2 d S . . C C 0.8584(3) 0.4117(3) 0.03622(16) 0.0658(9) Uani 1 1 d . . . H0A H 0.8093 0.4762 0.0207 0.099 Uiso 1 1 calc R . . H0B H 0.9337 0.4070 0.0153 0.099 Uiso 1 1 calc R . . H0C H 0.8750 0.4277 0.0761 0.099 Uiso 1 1 calc R . . N N 0.79332(19) 0.29663(19) 0.03094(8) 0.0378(5) Uani 1 1 d . . . H0D H 0.8301 0.2403 0.0523 0.057 Uiso 1 1 calc R . . H0E H 0.7932 0.2731 -0.0057 0.057 Uiso 1 1 calc R . . H0F H 0.7169 0.3062 0.0430 0.057 Uiso 1 1 calc R . . OW O 0.7013(4) 0.0680(3) 0.07591(19) 0.1412(18) Uani 1 1 d . . . H1W H 0.6532 0.1209 0.0901 0.212 Uiso 1 1 d R . . H2W H 0.7325 0.0063 0.0924 0.212 Uiso 1 1 d R . . 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 Al1 0.0177(3) 0.0177(3) 0.0099(4) 0.000 0.000 0.000 Al2 0.0159(3) 0.0159(3) 0.0114(4) 0.000 0.000 0.000 B1 0.0182(10) 0.0242(10) 0.0207(10) -0.0070(8) -0.0003(7) 0.0002(8) B2 0.0159(13) 0.0347(17) 0.0167(15) 0.0030(11) 0.000 0.000 B3 0.0193(10) 0.0206(9) 0.0132(9) 0.0034(7) -0.0021(7) -0.0015(8) O1 0.0261(7) 0.0398(8) 0.0268(7) -0.0209(6) -0.0054(6) 0.0055(7) O2 0.0181(6) 0.0381(8) 0.0244(7) -0.0133(6) 0.0004(5) 0.0065(6) O3 0.0153(9) 0.0469(13) 0.0286(10) -0.0253(9) 0.000 0.000 O4 0.0182(7) 0.0408(8) 0.0272(7) 0.0136(7) 0.0013(6) 0.0063(6) O5 0.0211(6) 0.0264(7) 0.0202(6) 0.0090(5) 0.0002(5) 0.0001(6) O6 0.0159(9) 0.0474(13) 0.0316(11) 0.0230(10) 0.000 0.000 C 0.062(2) 0.0542(18) 0.081(2) -0.0079(17) -0.0290(18) 0.0017(17) N 0.0366(10) 0.0416(11) 0.0352(11) -0.0009(9) -0.0023(9) 0.0070(9) OW 0.139(3) 0.0639(18) 0.221(4) 0.043(2) 0.106(3) 0.047(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 Al1 O1 1.7285(13) . ? Al1 O1 1.7285(13) 4_645 ? Al1 O1 1.7285(13) 2_755 ? Al1 O1 1.7285(13) 3_665 ? Al2 O5 1.7464(12) 3_675 ? Al2 O5 1.7464(12) 2_865 ? Al2 O5 1.7464(13) . ? Al2 O5 1.7464(13) 4_745 ? B1 O1 1.329(2) . ? B1 O2 1.368(2) . ? B1 O3 1.381(2) . ? B2 O4 1.473(2) 14_454 ? B2 O4 1.473(2) . ? B2 O2 1.473(2) . ? B2 O2 1.473(2) 14_454 ? B3 O5 1.352(2) . ? B3 O4 1.353(2) . ? B3 O6 1.385(2) . ? O3 B1 1.381(2) 14_454 ? O6 B3 1.385(2) 14_454 ? C N 1.456(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 O1 Al1 O1 110.08(5) . 4_645 ? O1 Al1 O1 108.25(11) . 2_755 ? O1 Al1 O1 110.08(5) 4_645 2_755 ? O1 Al1 O1 110.08(5) . 3_665 ? O1 Al1 O1 108.26(11) 4_645 3_665 ? O1 Al1 O1 110.08(5) 2_755 3_665 ? O5 Al2 O5 110.89(5) 3_675 2_865 ? O5 Al2 O5 110.89(5) 3_675 . ? O5 Al2 O5 106.67(9) 2_865 . ? O5 Al2 O5 106.67(9) 3_675 4_745 ? O5 Al2 O5 110.89(5) 2_865 4_745 ? O5 Al2 O5 110.89(5) . 4_745 ? O1 B1 O2 123.40(18) . . ? O1 B1 O3 117.71(17) . . ? O2 B1 O3 118.87(17) . . ? O4 B2 O4 111.3(2) 14_454 . ? O4 B2 O2 110.01(9) 14_454 . ? O4 B2 O2 107.06(9) . . ? O4 B2 O2 107.06(9) 14_454 14_454 ? O4 B2 O2 110.01(9) . 14_454 ? O2 B2 O2 111.4(2) . 14_454 ? O5 B3 O4 122.82(16) . . ? O5 B3 O6 117.03(16) . . ? O4 B3 O6 120.14(17) . . ? B1 O1 Al1 142.93(14) . . ? B1 O2 B2 123.60(17) . . ? B1 O3 B1 122.3(2) 14_454 . ? B3 O4 B2 123.56(16) . . ? B3 O5 Al2 129.99(12) . . ? B3 O6 B3 120.5(2) . 14_454 ? 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 N H0D O1 0.89 2.31 3.006(2) 134.8 . N H0D OW 0.89 2.42 2.899(4) 113.8 . N H0D O3 0.89 2.62 3.287(2) 132.7 . N H0E O2 0.89 2.11 2.983(3) 167.6 4_645 N H0E O4 0.89 2.44 3.090(3) 129.9 4_645 N H0F O5 0.89 2.11 2.952(2) 157.5 1_455 OW H1W O6 0.85 2.09 2.941(3) 179.6 1_455 OW H2W O2 0.85 2.11 2.877(3) 149.8 2_755 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.217 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.054 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 763047' #TrackingRef '- 763046-763047.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H14 Al B5 N2 O11' _chemical_formula_weight 323.18 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 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 9.7449(17) _cell_length_b 10.5879(12) _cell_length_c 8.5134(14) _cell_angle_alpha 90.00 _cell_angle_beta 120.862(7) _cell_angle_gamma 90.00 _cell_volume 754.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1066 _cell_measurement_theta_min 2.7871 _cell_measurement_theta_max 27.4487 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7934 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SCXimini CCD' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2848 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1694 _reflns_number_gt 1553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0950P)^2^+0.5544P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.025(7) _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 -0.1(4) _refine_ls_number_reflns 1694 _refine_ls_number_parameters 104 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Al Al 0.0000 0.88711(11) 1.0000 0.0242(3) Uani 1 2 d S . . B1 B 0.2933(4) 0.7349(3) 1.1782(4) 0.0284(7) Uani 1 1 d . . . B2 B 0.4928(4) 0.5727(3) 1.2442(5) 0.0291(7) Uani 1 1 d . . . B3 B 0.5000 0.6903(4) 1.5000 0.0263(10) Uani 1 2 d S . . O1 O 0.1616(3) 0.7919(3) 1.0476(3) 0.0431(7) Uani 1 1 d . . . O2 O 0.3504(3) 0.6337(2) 1.1242(3) 0.0385(6) Uani 1 1 d . . . O3 O 0.3757(3) 0.7714(2) 1.3583(3) 0.0298(5) Uani 1 1 d . . . O4 O 0.5519(3) 0.4798(3) 1.1902(3) 0.0405(6) Uani 1 1 d . . . O5 O 0.5735(3) 0.6107(3) 1.4233(3) 0.0362(6) Uani 1 1 d . . . C C 0.8121(11) 0.3778(13) 1.7284(12) 0.121(3) Uani 1 1 d U . . H0A H 0.9037 0.3250 1.7994 0.181 Uiso 1 1 calc R . . H0B H 0.7171 0.3270 1.6732 0.181 Uiso 1 1 calc R . . H0C H 0.8056 0.4400 1.8065 0.181 Uiso 1 1 calc R . . N N 0.8270(6) 0.4406(5) 1.5865(6) 0.0848(17) Uani 1 1 d . . . H0D H 0.7502 0.4983 1.5319 0.127 Uiso 1 1 calc R . . H0E H 0.8180 0.3840 1.5045 0.127 Uiso 1 1 calc R . . H0F H 0.9220 0.4781 1.6362 0.127 Uiso 1 1 calc R . . OW O 0.1185(7) 0.5884(9) 0.7520(8) 0.079(3) Uani 0.50 1 d P . . H1W H 0.2060 0.5598 0.7672 0.118 Uiso 0.50 1 d PR . . H2W H 0.1299 0.6429 0.8312 0.118 Uiso 0.50 1 d PR . . 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 Al 0.0207(5) 0.0245(6) 0.0197(6) 0.000 0.0047(4) 0.000 B1 0.0304(17) 0.0292(16) 0.0223(15) -0.0017(13) 0.0112(13) 0.0031(13) B2 0.0269(16) 0.0277(16) 0.0254(16) -0.0020(13) 0.0081(13) -0.0004(14) B3 0.028(2) 0.027(2) 0.0162(19) 0.000 0.0058(17) 0.000 O1 0.0374(13) 0.0552(17) 0.0262(11) -0.0004(11) 0.0087(10) 0.0179(12) O2 0.0323(12) 0.0438(14) 0.0230(11) -0.0083(9) 0.0024(9) 0.0102(10) O3 0.0318(11) 0.0301(11) 0.0214(10) 0.0020(8) 0.0093(8) 0.0083(9) O4 0.0355(13) 0.0429(14) 0.0316(12) -0.0103(11) 0.0089(10) 0.0086(11) O5 0.0322(12) 0.0417(13) 0.0238(11) -0.0027(9) 0.0065(9) 0.0126(10) C 0.122(3) 0.121(3) 0.120(3) 0.0000(10) 0.0623(16) 0.0024(10) N 0.088(3) 0.099(3) 0.041(2) -0.001(2) 0.014(2) 0.063(3) OW 0.036(3) 0.121(7) 0.030(3) -0.033(4) -0.017(2) 0.011(4) _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 Al O1 1.734(3) 2_557 ? Al O1 1.734(3) . ? Al O4 1.732(2) 3_455 ? Al O4 1.732(2) 4_557 ? B1 O1 1.336(4) . ? B1 O3 1.372(4) . ? B1 O2 1.391(4) . ? B2 O4 1.335(4) . ? B2 O5 1.370(4) . ? B2 O2 1.390(4) . ? B3 O5 1.459(4) . ? B3 O5 1.459(4) 2_658 ? B3 O3 1.470(3) 2_658 ? B3 O3 1.470(3) . ? O4 Al 1.732(2) 3_545 ? C N 1.450(10) . ? 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 Al O1 108.9(2) 2_557 . ? O1 Al O4 110.06(12) 2_557 3_455 ? O1 Al O4 108.44(11) . 3_455 ? O1 Al O4 108.44(11) 2_557 4_557 ? O1 Al O4 110.06(12) . 4_557 ? O4 Al O4 111.0(2) 3_455 4_557 ? O1 B1 O3 124.4(3) . . ? O1 B1 O2 116.7(3) . . ? O3 B1 O2 118.9(3) . . ? O4 B2 O5 119.8(3) . . ? O4 B2 O2 122.2(3) . . ? O5 B2 O2 117.9(3) . . ? O5 B3 O5 109.5(4) . 2_658 ? O5 B3 O3 108.49(13) . 2_658 ? O5 B3 O3 110.94(13) 2_658 2_658 ? O5 B3 O3 110.94(12) . . ? O5 B3 O3 108.49(13) 2_658 . ? O3 B3 O3 108.5(4) 2_658 . ? B1 O1 Al 145.8(2) . . ? B2 O2 B1 122.2(3) . . ? B1 O3 B3 121.1(3) . . ? B2 O4 Al 140.2(2) . 3_545 ? B2 O5 B3 122.3(2) . . ? 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 N H0D O5 0.89 1.90 2.785(4) 173.8 . N H0D O4 0.89 2.54 3.077(5) 119.2 . N H0E O3 0.89 2.00 2.856(5) 160.6 3_545 N H0F OW 0.89 2.02 2.898(10) 170.5 1_656 OW H1W O4 0.85 2.35 3.203(8) 179.7 2_657 OW H2W O2 0.85 2.31 2.834(5) 119.9 . OW H2W O1 0.85 2.32 3.172(8) 179.8 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.528 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.082