Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_address ; State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; _publ_contact_author_email ygy@ms.fjirsm.ac.cn _publ_contact_author_fax '86 591 3710051' _publ_contact_author_phone '86 591 3710051' _publ_requested_coeditor_name ? #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Open-Framework Aluminoborates Synergistically Templated by Two Types of Primary Amines ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name #_publ_author_footnote _publ_author_address 'Gao-juan Cao' ; Current address: State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Jian Lin' ; Xiamen University, Xiamen, Fujian 361005, P. R. China ; 'Wei-Hui Fang' ; State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; 'Guo-Yu Yang' ; State Key Laboratory of The Structural Chemistry Fujian Institute of Research on the structure of matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; # Attachment '2.cif' #SUBMISSION DETAILS _publ_contact_author_name 'Professor Guo-Yu Yang' # Attachment '- 1-4 cif.txt' data_1 _database_code_depnum_ccdc_archive 'CCDC 763048' #TrackingRef '- 1-4 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H18 Al B5 N2 O10' _chemical_formula_weight 347.24 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.0982(11) _cell_length_b 13.2447(8) _cell_length_c 17.8453(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3095.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3115 _cell_measurement_theta_min 2.2824 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Cubic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8019 _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 'SCXmini 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 22455 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3501 _reflns_number_gt 3204 _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^)+(0.0554P)^2^+0.6041P] 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_number_reflns 3501 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Al Al 0.49302(3) 0.23750(3) 0.627629(19) 0.01843(12) Uani 1 1 d . . . B1 B 0.63357(11) 0.27894(11) 0.50647(8) 0.0226(3) Uani 1 1 d . . . B2 B 0.78430(11) 0.31527(11) 0.42926(8) 0.0245(3) Uani 1 1 d . . . B3 B 0.61879(12) 0.38855(11) 0.39241(8) 0.0256(3) Uani 1 1 d . . . B4 B 0.54420(12) 0.54441(11) 0.33600(8) 0.0249(3) Uani 1 1 d . . . B5 B 0.53772(12) 0.38721(11) 0.26505(8) 0.0241(3) Uani 1 1 d . . . O1 O 0.59574(7) 0.23258(8) 0.56635(5) 0.0308(2) Uani 1 1 d . . . O2 O 0.73594(7) 0.26364(8) 0.48810(6) 0.0337(3) Uani 1 1 d . . . O3 O 0.57803(7) 0.34039(8) 0.46049(5) 0.0322(2) Uani 1 1 d . . . O4 O 0.88297(7) 0.29511(9) 0.41912(6) 0.0366(3) Uani 1 1 d . . . O5 O 0.72946(8) 0.38092(8) 0.38821(5) 0.0348(3) Uani 1 1 d . . . O6 O 0.58874(8) 0.49572(7) 0.39432(5) 0.0299(2) Uani 1 1 d . . . O7 O 0.57256(8) 0.33774(7) 0.32694(5) 0.0316(2) Uani 1 1 d . . . O8 O 0.51758(9) 0.64145(8) 0.33701(7) 0.0405(3) Uani 1 1 d . . . O9 O 0.52294(9) 0.49144(7) 0.27085(5) 0.0348(3) Uani 1 1 d . . . O10 O 0.51609(9) 0.34242(8) 0.20099(6) 0.0380(3) Uani 1 1 d . . . C1 C 0.68008(16) 0.54996(19) 0.58341(12) 0.0632(6) Uani 1 1 d . . . H1A H 0.7457 0.5279 0.5659 0.095 Uiso 1 1 calc R . . H1B H 0.6397 0.4923 0.5970 0.095 Uiso 1 1 calc R . . H1C H 0.6888 0.5928 0.6264 0.095 Uiso 1 1 calc R . . C3 C 0.74016(18) 0.1750(2) 0.23520(14) 0.0808(8) Uani 1 1 d . . . H3A H 0.6974 0.1604 0.1928 0.121 Uiso 1 1 calc R . . H3B H 0.8098 0.1594 0.2231 0.121 Uiso 1 1 calc R . . H3C H 0.7346 0.2453 0.2477 0.121 Uiso 1 1 calc R . . C2 C 0.70707(15) 0.11290(16) 0.30024(13) 0.0617(6) Uani 1 1 d . . . H2A H 0.7185 0.0422 0.2889 0.074 Uiso 1 1 calc R . . H2B H 0.7486 0.1301 0.3434 0.074 Uiso 1 1 calc R . . C4 C 0.56615(19) 0.07461(14) 0.38939(11) 0.0593(6) Uani 1 1 d . . . H4A H 0.5789 0.0029 0.3837 0.071 Uiso 1 1 calc R . . H4B H 0.6073 0.0988 0.4309 0.071 Uiso 1 1 calc R . . C5 C 0.4576(2) 0.0905(2) 0.40683(13) 0.0738(7) Uani 1 1 d . . . H5A H 0.4437 0.1616 0.4092 0.111 Uiso 1 1 calc R . . H5B H 0.4419 0.0600 0.4542 0.111 Uiso 1 1 calc R . . H5C H 0.4163 0.0603 0.3684 0.111 Uiso 1 1 calc R . . N1 N 0.62829(9) 0.60628(9) 0.52385(6) 0.0291(3) Uani 1 1 d . . . H1D H 0.5668 0.6253 0.5397 0.044 Uiso 1 1 calc R . . H1E H 0.6217 0.5671 0.4836 0.044 Uiso 1 1 calc R . . H1F H 0.6649 0.6606 0.5121 0.044 Uiso 1 1 calc R . . N2 N 0.59757(11) 0.12798(10) 0.31935(8) 0.0433(4) Uani 1 1 d . . . H2C H 0.5589 0.1057 0.2811 0.052 Uiso 1 1 calc R . . H2D H 0.5856 0.1945 0.3248 0.052 Uiso 1 1 calc 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 Al 0.0192(2) 0.0174(2) 0.0186(2) 0.00182(13) -0.00169(13) 0.00029(13) B1 0.0198(7) 0.0259(7) 0.0220(6) -0.0001(5) 0.0009(5) 0.0022(5) B2 0.0219(7) 0.0270(7) 0.0247(7) -0.0023(5) 0.0020(5) 0.0006(6) B3 0.0264(7) 0.0271(7) 0.0234(7) 0.0030(5) -0.0024(6) 0.0046(6) B4 0.0274(7) 0.0205(7) 0.0269(7) -0.0023(5) -0.0007(6) 0.0015(6) B5 0.0277(7) 0.0219(7) 0.0229(7) -0.0043(5) 0.0005(6) 0.0000(6) O1 0.0254(5) 0.0397(6) 0.0273(5) 0.0085(4) 0.0038(4) 0.0018(4) O2 0.0221(5) 0.0427(6) 0.0362(5) 0.0154(4) 0.0067(4) 0.0101(4) O3 0.0209(5) 0.0455(6) 0.0302(5) 0.0123(4) 0.0018(4) 0.0085(4) O4 0.0227(5) 0.0501(7) 0.0370(6) 0.0008(5) 0.0068(4) 0.0061(5) O5 0.0255(5) 0.0444(6) 0.0345(5) 0.0152(4) 0.0041(4) 0.0034(5) O6 0.0389(6) 0.0257(5) 0.0251(5) -0.0052(4) -0.0084(4) 0.0049(4) O7 0.0449(6) 0.0196(5) 0.0303(5) -0.0016(4) -0.0081(4) 0.0058(4) O8 0.0495(7) 0.0204(5) 0.0516(7) -0.0042(5) -0.0014(5) 0.0060(5) O9 0.0571(7) 0.0222(5) 0.0251(5) -0.0011(4) -0.0131(5) 0.0069(4) O10 0.0486(6) 0.0361(6) 0.0293(5) -0.0135(4) -0.0024(4) -0.0030(5) C1 0.0513(11) 0.0825(16) 0.0559(11) 0.0259(10) -0.0107(9) 0.0036(10) C3 0.0558(13) 0.117(2) 0.0695(14) -0.0158(14) -0.0011(11) 0.0299(14) C2 0.0512(11) 0.0543(12) 0.0795(14) -0.0135(10) -0.0221(10) 0.0208(9) C4 0.0838(16) 0.0358(9) 0.0583(11) 0.0009(8) -0.0288(11) -0.0036(10) C5 0.0877(18) 0.0789(16) 0.0548(12) -0.0042(11) -0.0030(12) -0.0066(14) N1 0.0272(6) 0.0308(6) 0.0295(6) 0.0003(4) 0.0010(5) -0.0035(5) N2 0.0534(9) 0.0313(7) 0.0453(7) -0.0119(6) -0.0227(6) 0.0088(6) _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 O10 1.7106(10) 7_566 ? Al O4 1.7205(10) 4_456 ? Al O8 1.7285(11) 5_666 ? Al O1 1.7351(10) . ? B1 O1 1.3282(17) . ? B1 O3 1.3656(17) . ? B1 O2 1.3951(16) . ? B2 O4 1.3321(17) . ? B2 O5 1.3448(18) . ? B2 O2 1.4041(17) . ? B3 O5 1.4551(18) . ? B3 O3 1.4724(17) . ? B3 O6 1.4735(17) . ? B3 O7 1.4779(18) . ? B4 O8 1.3318(17) . ? B4 O6 1.3562(17) . ? B4 O9 1.3863(17) . ? B5 O10 1.3187(17) . ? B5 O7 1.3629(17) . ? B5 O9 1.3979(17) . ? O4 Al 1.7205(10) 4_556 ? O8 Al 1.7285(11) 5_666 ? O10 Al 1.7106(10) 7_565 ? C1 N1 1.465(2) . ? C3 C2 1.487(4) . ? C2 N2 1.488(2) . ? C4 C5 1.471(3) . ? C4 N2 1.494(3) . ? 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 O10 Al O4 111.33(6) 7_566 4_456 ? O10 Al O8 107.99(6) 7_566 5_666 ? O4 Al O8 110.04(6) 4_456 5_666 ? O10 Al O1 108.79(5) 7_566 . ? O4 Al O1 109.55(5) 4_456 . ? O8 Al O1 109.10(6) 5_666 . ? O1 B1 O3 124.06(12) . . ? O1 B1 O2 118.71(12) . . ? O3 B1 O2 117.22(12) . . ? O4 B2 O5 125.01(13) . . ? O4 B2 O2 116.21(12) . . ? O5 B2 O2 118.77(12) . . ? O5 B3 O3 111.94(11) . . ? O5 B3 O6 109.52(12) . . ? O3 B3 O6 107.54(11) . . ? O5 B3 O7 109.62(12) . . ? O3 B3 O7 107.85(12) . . ? O6 B3 O7 110.34(11) . . ? O8 B4 O6 124.14(12) . . ? O8 B4 O9 116.56(12) . . ? O6 B4 O9 119.30(12) . . ? O10 B5 O7 123.93(13) . . ? O10 B5 O9 118.60(12) . . ? O7 B5 O9 117.46(11) . . ? B1 O1 Al 141.16(9) . . ? B1 O2 B2 122.58(11) . . ? B1 O3 B3 124.11(11) . . ? B2 O4 Al 158.29(10) . 4_556 ? B2 O5 B3 123.29(11) . . ? B4 O6 B3 123.73(11) . . ? B5 O7 B3 123.98(10) . . ? B4 O8 Al 157.07(11) . 5_666 ? B4 O9 B5 122.28(11) . . ? B5 O10 Al 168.47(11) . 7_565 ? N2 C2 C3 112.68(16) . . ? C5 C4 N2 112.07(17) . . ? C2 N2 C4 113.20(15) . . ? 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 H1D O3 0.89 1.95 2.8071(15) 161.0 5_666 N1 H1E O6 0.89 1.90 2.7849(15) 170.9 . N1 H1F O2 0.89 1.93 2.8131(15) 170.3 8_765 N1 H1F O4 0.89 2.51 3.1258(16) 126.5 8_765 N2 H2D O7 0.90 1.91 2.8007(16) 172.9 . N2 H2C O9 0.90 2.07 2.8902(16) 150.4 3_645 N2 H2C O8 0.90 2.38 3.1769(18) 147.5 3_645 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.256 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.068 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 763049' #TrackingRef '- 1-4 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 Al B5 N2 O10' _chemical_formula_weight 361.27 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.1331(13) _cell_length_b 13.3590(9) _cell_length_c 17.9234(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3144.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2791 _cell_measurement_theta_min 2.4530 _cell_measurement_theta_max 27.4487 _exptl_crystal_description Cubic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7861 _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 'SCXmini 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 23189 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3584 _reflns_number_gt 3093 _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^)+(0.1137P)^2^+2.0947P] 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_number_reflns 3584 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.49080(5) 0.25719(5) 0.62831(3) 0.0188(2) Uani 1 1 d . . . B1 B 0.62964(19) 0.2162(2) 0.50363(14) 0.0237(5) Uani 1 1 d . . . B2 B 0.78227(19) 0.1878(2) 0.42768(14) 0.0252(5) Uani 1 1 d . . . B3 B 0.6204(2) 0.1109(2) 0.38809(14) 0.0261(5) Uani 1 1 d . . . B4 B 0.5482(2) -0.04399(19) 0.33025(14) 0.0247(5) Uani 1 1 d . . . B5 B 0.5417(2) 0.11243(19) 0.26054(14) 0.0240(5) Uani 1 1 d . . . O1 O 0.59017(13) 0.25639(14) 0.56491(10) 0.0333(4) Uani 1 1 d . . . O2 O 0.73131(13) 0.23737(14) 0.48580(10) 0.0326(4) Uani 1 1 d . . . O3 O 0.57659(12) 0.15583(14) 0.45587(9) 0.0318(4) Uani 1 1 d . . . O4 O 0.87998(13) 0.21236(15) 0.41779(10) 0.0368(4) Uani 1 1 d . . . O5 O 0.73110(14) 0.11986(14) 0.38664(10) 0.0339(4) Uani 1 1 d . . . O6 O 0.59220(15) 0.00375(13) 0.38871(9) 0.0320(4) Uani 1 1 d . . . O7 O 0.57670(15) 0.16146(12) 0.32257(9) 0.0331(4) Uani 1 1 d . . . O8 O 0.52111(16) -0.14016(13) 0.33104(11) 0.0392(5) Uani 1 1 d . . . O9 O 0.52834(15) 0.00926(12) 0.26518(9) 0.0328(4) Uani 1 1 d . . . O10 O 0.51808(15) 0.15793(13) 0.19725(10) 0.0349(4) Uani 1 1 d . . . C2 C 0.2918(3) 0.1008(3) 0.35591(18) 0.0639(10) Uani 1 1 d . . . H2A H 0.2470 0.1544 0.3701 0.096 Uiso 1 1 calc R . . H2B H 0.2583 0.0588 0.3200 0.096 Uiso 1 1 calc R . . H2C H 0.3526 0.1281 0.3343 0.096 Uiso 1 1 calc R . . C1 C 0.3191(2) 0.0396(2) 0.42413(16) 0.0440(7) Uani 1 1 d . . . H1A H 0.2577 0.0113 0.4456 0.053 Uiso 1 1 calc R . . H1B H 0.3634 -0.0152 0.4097 0.053 Uiso 1 1 calc R . . C4 C 0.4459(4) 0.1003(4) 0.9093(3) 0.0903(15) Uani 1 1 d . . . H4A H 0.4369 0.1715 0.9111 0.136 Uiso 1 1 calc R . . H4B H 0.4248 0.0715 0.9559 0.136 Uiso 1 1 calc R . . H4C H 0.4055 0.0729 0.8696 0.136 Uiso 1 1 calc R . . C3 C 0.5553(3) 0.0768(3) 0.8960(2) 0.0631(10) Uani 1 1 d . . . H3A H 0.5645 0.0049 0.8920 0.076 Uiso 1 1 calc R . . H3B H 0.5962 0.1008 0.9373 0.076 Uiso 1 1 calc R . . C5 C 0.6973(3) 0.1061(3) 0.8084(2) 0.0639(10) Uani 1 1 d . . . H5A H 0.7379 0.1218 0.8521 0.077 Uiso 1 1 calc R . . H5B H 0.7057 0.0355 0.7976 0.077 Uiso 1 1 calc R . . C6 C 0.7340(3) 0.1658(4) 0.7443(2) 0.0747(12) Uani 1 1 d . . . H6A H 0.6913 0.1535 0.7018 0.112 Uiso 1 1 calc R . . H6B H 0.8028 0.1469 0.7327 0.112 Uiso 1 1 calc R . . H6C H 0.7319 0.2356 0.7568 0.112 Uiso 1 1 calc R . . N1 N 0.37114(15) 0.10286(15) 0.48041(11) 0.0293(4) Uani 1 1 d . . . H1C H 0.4305 0.1238 0.4622 0.044 Uiso 1 1 calc R . . H1D H 0.3819 0.0673 0.5216 0.044 Uiso 1 1 calc R . . H1E H 0.3323 0.1555 0.4912 0.044 Uiso 1 1 calc R . . N2 N 0.5883(2) 0.1268(2) 0.82473(14) 0.0485(6) Uani 1 1 d . . . H2D H 0.5497 0.1044 0.7867 0.058 Uiso 1 1 calc R . . H2E H 0.5789 0.1933 0.8287 0.058 Uiso 1 1 calc 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 Al 0.0180(4) 0.0190(4) 0.0192(4) -0.0021(2) -0.0013(2) -0.0001(2) B1 0.0189(11) 0.0284(12) 0.0237(11) -0.0001(9) -0.0006(9) -0.0025(10) B2 0.0214(11) 0.0297(12) 0.0246(11) -0.0004(9) 0.0024(9) -0.0017(10) B3 0.0262(13) 0.0271(12) 0.0251(12) -0.0021(9) -0.0029(10) -0.0061(10) B4 0.0270(12) 0.0219(11) 0.0253(12) 0.0039(9) -0.0013(9) -0.0018(10) B5 0.0260(12) 0.0231(11) 0.0230(11) 0.0034(9) 0.0004(9) -0.0006(9) O1 0.0247(8) 0.0457(11) 0.0295(9) -0.0090(7) 0.0052(7) -0.0015(7) O2 0.0220(8) 0.0413(10) 0.0346(9) -0.0156(7) 0.0074(7) -0.0099(7) O3 0.0213(8) 0.0444(10) 0.0297(9) -0.0096(7) 0.0011(7) -0.0076(7) O4 0.0231(8) 0.0491(11) 0.0382(10) -0.0036(8) 0.0074(7) -0.0070(8) O5 0.0277(9) 0.0398(10) 0.0342(9) -0.0137(7) 0.0061(7) -0.0041(8) O6 0.0426(10) 0.0263(8) 0.0273(8) 0.0063(6) -0.0105(7) -0.0085(7) O7 0.0479(11) 0.0208(8) 0.0306(9) 0.0030(6) -0.0079(8) -0.0076(7) O8 0.0491(11) 0.0234(8) 0.0451(11) 0.0042(7) -0.0060(9) -0.0087(8) O9 0.0531(11) 0.0216(8) 0.0237(8) 0.0008(6) -0.0116(8) -0.0048(7) O10 0.0455(11) 0.0317(9) 0.0274(9) 0.0102(7) -0.0029(7) 0.0020(8) C2 0.056(2) 0.098(3) 0.0380(17) -0.0092(17) -0.0100(15) 0.021(2) C1 0.0419(15) 0.0457(16) 0.0444(15) -0.0075(12) -0.0095(12) -0.0021(13) C4 0.096(4) 0.110(4) 0.064(3) -0.022(3) 0.010(3) -0.020(3) C3 0.085(3) 0.0497(19) 0.055(2) -0.0087(15) -0.0030(19) -0.0115(19) C5 0.063(2) 0.056(2) 0.072(2) -0.0104(17) -0.0198(19) 0.0212(18) C6 0.053(2) 0.090(3) 0.081(3) 0.013(2) 0.003(2) 0.015(2) N1 0.0265(10) 0.0303(10) 0.0310(10) 0.0002(8) -0.0003(8) 0.0021(8) N2 0.0576(16) 0.0416(13) 0.0465(14) -0.0108(11) -0.0133(12) 0.0003(12) _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 O10 1.7150(18) 7_566 ? Al O4 1.7224(18) 4_456 ? Al O1 1.7304(18) . ? Al O8 1.7319(19) 5_656 ? B1 O1 1.328(3) . ? B1 O3 1.367(3) . ? B1 O2 1.402(3) . ? B2 O4 1.337(3) . ? B2 O5 1.347(3) . ? B2 O2 1.404(3) . ? B3 O5 1.458(3) . ? B3 O7 1.472(3) . ? B3 O3 1.472(3) . ? B3 O6 1.479(3) . ? B4 O8 1.333(3) . ? B4 O6 1.356(3) . ? B4 O9 1.391(3) . ? B5 O10 1.324(3) . ? B5 O7 1.370(3) . ? B5 O9 1.392(3) . ? O4 Al 1.7224(18) 4_556 ? O8 Al 1.7319(19) 5_656 ? O10 Al 1.7150(18) 7_565 ? C2 C1 1.515(5) . ? C1 N1 1.483(3) . ? C4 C3 1.490(6) . ? C3 N2 1.505(4) . ? C5 C6 1.480(6) . ? C5 N2 1.486(5) . ? 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 O10 Al O4 111.47(10) 7_566 4_456 ? O10 Al O1 108.65(9) 7_566 . ? O4 Al O1 108.89(9) 4_456 . ? O10 Al O8 108.21(9) 7_566 5_656 ? O4 Al O8 109.80(10) 4_456 5_656 ? O1 Al O8 109.81(10) . 5_656 ? O1 B1 O3 123.9(2) . . ? O1 B1 O2 118.6(2) . . ? O3 B1 O2 117.5(2) . . ? O4 B2 O5 124.9(2) . . ? O4 B2 O2 116.1(2) . . ? O5 B2 O2 119.0(2) . . ? O5 B3 O7 109.7(2) . . ? O5 B3 O3 111.78(19) . . ? O7 B3 O3 108.6(2) . . ? O5 B3 O6 109.2(2) . . ? O7 B3 O6 110.63(18) . . ? O3 B3 O6 106.88(19) . . ? O8 B4 O6 124.0(2) . . ? O8 B4 O9 116.9(2) . . ? O6 B4 O9 119.2(2) . . ? O10 B5 O7 123.7(2) . . ? O10 B5 O9 118.4(2) . . ? O7 B5 O9 117.9(2) . . ? B1 O1 Al 147.17(17) . . ? B1 O2 B2 121.87(19) . . ? B1 O3 B3 123.91(19) . . ? B2 O4 Al 158.92(18) . 4_556 ? B2 O5 B3 122.9(2) . . ? B4 O6 B3 123.81(18) . . ? B5 O7 B3 124.00(19) . . ? B4 O8 Al 153.96(18) . 5_656 ? B4 O9 B5 122.20(19) . . ? B5 O10 Al 165.92(19) . 7_565 ? N1 C1 C2 110.5(3) . . ? C4 C3 N2 108.7(4) . . ? C6 C5 N2 111.5(3) . . ? C5 N2 C3 111.2(3) . . ? 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 H1C O3 0.89 1.97 2.824(3) 160.5 . N1 H1D O6 0.89 1.90 2.786(3) 177.5 5_656 N1 H1E O2 0.89 1.99 2.880(3) 173.3 4_456 N1 H1E O4 0.89 2.48 3.072(3) 124.0 4_456 N2 H2D O9 0.90 2.06 2.872(3) 150.3 5_656 N2 H2D O8 0.90 2.36 3.145(3) 146.4 5_656 N2 H2E O7 0.90 1.94 2.833(3) 169.5 7_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.231 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.075 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 763050' #TrackingRef '- 1-4 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H17 Al B5 N2 O10.50' _chemical_formula_weight 342.23 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.0751(9) _cell_length_b 13.3143(8) _cell_length_c 17.3722(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3024.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6310 _cell_measurement_theta_min 2.1845 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Cubic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.4000 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8542 _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 'SCXmini 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 21484 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3456 _reflns_number_gt 2881 _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^)+(0.1290P)^2^+2.3028P] 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_number_reflns 3456 _refine_ls_number_parameters 207 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.2016 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.00821(5) 0.24094(5) 0.63037(4) 0.0242(2) Uani 1 1 d . . . B1 B -0.0528(2) 0.1072(2) 0.76168(16) 0.0308(6) Uani 1 1 d . . . B2 B -0.0712(2) -0.0522(2) 0.82782(16) 0.0311(6) Uani 1 1 d . . . B3 B -0.1354(2) 0.1029(2) 0.89143(17) 0.0336(6) Uani 1 1 d . . . B4 B -0.2975(2) 0.1775(2) 0.93665(16) 0.0312(6) Uani 1 1 d . . . B5 B -0.1436(2) 0.2013(2) 1.01389(16) 0.0298(6) Uani 1 1 d . . . O1 O -0.0203(2) 0.15490(17) 0.69946(13) 0.0523(6) Uani 1 1 d . . . O2 O -0.05020(17) 0.00301(12) 0.76161(10) 0.0389(5) Uani 1 1 d . . . O3 O -0.08611(17) 0.15453(13) 0.82617(12) 0.0413(5) Uani 1 1 d . . . O4 O -0.0468(2) -0.14961(14) 0.82518(13) 0.0504(6) Uani 1 1 d . . . O5 O -0.11129(16) -0.00540(14) 0.88989(10) 0.0376(5) Uani 1 1 d . . . O6 O -0.24498(15) 0.11756(18) 0.88823(12) 0.0452(5) Uani 1 1 d . . . O7 O -0.09052(14) 0.14432(16) 0.96292(12) 0.0425(5) Uani 1 1 d . . . O8 O -0.39678(14) 0.19864(18) 0.93075(12) 0.0441(5) Uani 1 1 d . . . O9 O -0.24621(13) 0.22087(16) 0.99936(11) 0.0379(5) Uani 1 1 d . . . O10 O -0.10254(15) 0.23831(17) 1.07819(12) 0.0433(5) Uani 1 1 d . . . C1 C -0.1607(3) -0.0477(3) 1.0965(2) 0.0586(9) Uani 1 1 d . . . H1A H -0.1508 -0.0845 1.1441 0.070 Uiso 1 1 calc R . . H1B H -0.1210 0.0138 1.0997 0.070 Uiso 1 1 calc R . . C2 C -0.2676(4) -0.0221(5) 1.0890(4) 0.0970(16) Uani 1 1 d . . . H2A H -0.2776 0.0165 1.0430 0.146 Uiso 1 1 calc R . . H2B H -0.2886 0.0166 1.1329 0.146 Uiso 1 1 calc R . . H2C H -0.3075 -0.0825 1.0863 0.146 Uiso 1 1 calc R . . C4 C -0.1589(5) 0.3988(5) 0.8162(6) 0.145(3) Uani 1 1 d . . . H4A H -0.2078 0.3648 0.8481 0.218 Uiso 1 1 calc R . . H4B H -0.1753 0.3877 0.7630 0.218 Uiso 1 1 calc R . . H4C H -0.1607 0.4695 0.8270 0.218 Uiso 1 1 calc R . . N1 N -0.12168(18) -0.10894(17) 1.03160(13) 0.0366(5) Uani 1 1 d . . . H1C H -0.1584 -0.1650 1.0277 0.055 Uiso 1 1 calc R . . H1D H -0.0565 -0.1246 1.0401 0.055 Uiso 1 1 calc R . . H1E H -0.1267 -0.0740 0.9881 0.055 Uiso 1 1 calc R . . N2 N -0.0593(3) 0.3609(2) 0.83175(17) 0.0581(8) Uani 1 1 d . . . H2D H -0.0165 0.3797 0.7938 0.070 Uiso 1 1 calc R . . H2E H -0.0613 0.2934 0.8328 0.070 Uiso 1 1 calc R . . C3 C -0.0215(10) 0.3983(5) 0.9049(4) 0.181(5) Uani 1 1 d . . . H3A H -0.0217 0.4704 0.9044 0.271 Uiso 1 1 calc R . . H3B H 0.0470 0.3745 0.9130 0.271 Uiso 1 1 calc R . . H3C H -0.0647 0.3746 0.9457 0.271 Uiso 1 1 calc R . . OW O -0.2054(12) -0.2495(13) 1.1888(8) 0.209(6) Uiso 0.50 1 d PD . . H1W H -0.2570 -0.2527 1.1592 0.313 Uiso 0.50 1 d PRD . . H2W H -0.1600 -0.2824 1.1645 0.313 Uiso 0.50 1 d PRD . . 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 0.0267(4) 0.0235(4) 0.0224(4) 0.0026(2) 0.0016(2) -0.0002(2) B1 0.0335(14) 0.0287(13) 0.0302(13) 0.0074(10) 0.0002(11) -0.0001(10) B2 0.0370(14) 0.0260(12) 0.0302(13) 0.0023(10) 0.0000(11) 0.0028(11) B3 0.0313(14) 0.0349(14) 0.0345(14) -0.0069(11) 0.0043(11) 0.0032(11) B4 0.0293(13) 0.0347(13) 0.0295(13) 0.0025(10) -0.0022(11) 0.0014(11) B5 0.0258(13) 0.0326(13) 0.0309(13) -0.0021(10) 0.0001(10) 0.0006(10) O1 0.0662(15) 0.0513(13) 0.0395(11) 0.0229(10) 0.0008(10) -0.0092(10) O2 0.0617(13) 0.0274(9) 0.0277(9) 0.0004(7) 0.0093(9) 0.0042(8) O3 0.0545(12) 0.0245(9) 0.0448(11) 0.0005(7) 0.0123(9) 0.0037(8) O4 0.0709(15) 0.0270(10) 0.0532(13) 0.0046(8) -0.0051(11) 0.0103(9) O5 0.0499(12) 0.0337(9) 0.0292(9) 0.0040(7) 0.0099(8) -0.0009(8) O6 0.0319(10) 0.0615(13) 0.0421(11) -0.0207(10) -0.0040(8) 0.0034(9) O7 0.0249(9) 0.0592(13) 0.0435(11) -0.0203(9) -0.0016(8) 0.0078(8) O8 0.0290(10) 0.0640(14) 0.0392(10) 0.0020(9) -0.0059(8) 0.0082(9) O9 0.0299(9) 0.0453(10) 0.0385(10) -0.0126(8) -0.0038(8) 0.0093(7) O10 0.0303(10) 0.0591(13) 0.0404(11) -0.0164(9) -0.0037(8) -0.0022(9) C1 0.065(2) 0.057(2) 0.0540(19) -0.0127(16) 0.0108(17) 0.0048(17) C2 0.089(4) 0.082(3) 0.120(4) -0.012(3) 0.016(3) 0.000(3) C4 0.098(4) 0.085(4) 0.252(9) 0.055(5) 0.078(6) 0.039(3) N1 0.0347(12) 0.0371(11) 0.0379(11) -0.0005(9) -0.0010(9) -0.0028(9) N2 0.084(2) 0.0410(14) 0.0496(15) 0.0059(11) 0.0264(15) -0.0036(14) C3 0.383(15) 0.092(4) 0.067(3) 0.021(3) -0.041(6) -0.108(7) _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 1.701(2) . ? Al1 O4 1.725(2) 3_556 ? Al1 O8 1.729(2) 6_657 ? Al1 O10 1.731(2) 7_565 ? B1 O1 1.324(3) . ? B1 O3 1.357(3) . ? B1 O2 1.387(3) . ? B2 O4 1.336(3) . ? B2 O5 1.351(3) . ? B2 O2 1.392(3) . ? B3 O6 1.447(4) . ? B3 O3 1.474(4) . ? B3 O5 1.476(3) . ? B3 O7 1.480(3) . ? B4 O8 1.333(3) . ? B4 O6 1.347(4) . ? B4 O9 1.404(3) . ? B5 O10 1.334(3) . ? B5 O7 1.357(3) . ? B5 O9 1.390(3) . ? O4 Al1 1.725(2) 3_546 ? O8 Al1 1.729(2) 6_557 ? O10 Al1 1.731(2) 7_566 ? C1 C2 1.444(7) . ? C1 N1 1.482(4) . ? C4 N2 1.421(7) . ? N2 C3 1.452(7) . ? 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 O4 108.50(12) . 3_556 ? O1 Al1 O8 111.80(12) . 6_657 ? O4 Al1 O8 109.86(12) 3_556 6_657 ? O1 Al1 O10 107.10(12) . 7_565 ? O4 Al1 O10 110.17(12) 3_556 7_565 ? O8 Al1 O10 109.37(11) 6_657 7_565 ? O1 B1 O3 123.6(2) . . ? O1 B1 O2 118.1(3) . . ? O3 B1 O2 118.2(2) . . ? O4 B2 O5 124.6(2) . . ? O4 B2 O2 115.9(2) . . ? O5 B2 O2 119.5(2) . . ? O6 B3 O3 109.9(2) . . ? O6 B3 O5 110.0(2) . . ? O3 B3 O5 110.4(2) . . ? O6 B3 O7 112.0(2) . . ? O3 B3 O7 107.4(2) . . ? O5 B3 O7 107.1(2) . . ? O8 B4 O6 125.0(3) . . ? O8 B4 O9 116.0(2) . . ? O6 B4 O9 119.0(2) . . ? O10 B5 O7 123.2(2) . . ? O10 B5 O9 118.1(2) . . ? O7 B5 O9 118.7(2) . . ? B1 O1 Al1 165.9(2) . . ? B1 O2 B2 121.5(2) . . ? B1 O3 B3 124.0(2) . . ? B2 O4 Al1 151.0(2) . 3_546 ? B2 O5 B3 123.2(2) . . ? B4 O6 B3 124.1(2) . . ? B5 O7 B3 123.6(2) . . ? B4 O8 Al1 144.7(2) . 6_557 ? B5 O9 B4 121.7(2) . . ? B5 O10 Al1 146.57(19) . 7_566 ? C2 C1 N1 113.3(4) . . ? C4 N2 C3 110.9(7) . . ? 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 H1C O9 0.89 2.03 2.904(3) 168.3 8 N1 H1C O8 0.89 2.58 3.113(3) 119.2 8 N1 H1D O7 0.89 1.94 2.816(3) 167.5 5_557 N1 H1E O5 0.89 1.95 2.825(3) 169.3 . N2 H2D O2 0.90 2.09 2.874(3) 144.4 3_556 N2 H2D O4 0.90 2.26 3.063(4) 148.1 3_556 N2 H2E O3 0.90 1.88 2.772(3) 170.4 . OW H1W O10 0.85 2.32 3.166(16) 179.8 8 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.662 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.088 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 782936' #TrackingRef '- 1-4 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H18 Al B5 N2 O12' _chemical_formula_weight 355.22 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 13.458(11) _cell_length_b 15.599(14) _cell_length_c 7.326(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1538(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3816 _cell_measurement_theta_min 2.0006 _cell_measurement_theta_max 27.4256 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7483 _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 'SCXmini 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 11214 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.40 _reflns_number_total 3460 _reflns_number_gt 2494 _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^)+(0.1000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(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 0.3(3) _refine_ls_number_reflns 3460 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 -0.09889(8) 0.27778(7) 0.73913(17) 0.0324(3) Uani 1 1 d . . . B1 B 0.1048(3) 0.3445(3) 0.7634(7) 0.0331(9) Uani 1 1 d . . . B2 B 0.2840(3) 0.3661(3) 0.7782(7) 0.0324(10) Uani 1 1 d . . . B3 B 0.1741(3) 0.4942(3) 0.7659(7) 0.0331(9) Uani 1 1 d . . . B4 B 0.1492(3) 0.6435(3) 0.8838(7) 0.0341(10) Uani 1 1 d . . . B5 B 0.1605(3) 0.6207(3) 0.5557(6) 0.0312(9) Uani 1 1 d . . . O1 O 0.03019(17) 0.28757(17) 0.7597(6) 0.0423(7) Uani 1 1 d . . . O2 O 0.20166(17) 0.31208(17) 0.7564(5) 0.0418(7) Uani 1 1 d . . . O3 O 0.09095(17) 0.43096(17) 0.7735(5) 0.0396(7) Uani 1 1 d . . . O4 O 0.37548(19) 0.32943(17) 0.7887(4) 0.0396(7) Uani 1 1 d . . . O5 O 0.27006(17) 0.45194(16) 0.7901(4) 0.0381(7) Uani 1 1 d . . . O6 O 0.1581(2) 0.55632(18) 0.9111(4) 0.0386(7) Uani 1 1 d . . . O7 O 0.1704(2) 0.53513(19) 0.5839(4) 0.0399(7) Uani 1 1 d . . . O8 O 0.1348(2) 0.69934(19) 1.0190(4) 0.0456(8) Uani 1 1 d . . . O9 O 0.1509(2) 0.67526(19) 0.7042(4) 0.0399(7) Uani 1 1 d . . . O10 O 0.1601(2) 0.65140(19) 0.3828(4) 0.0410(7) Uani 1 1 d . . . C1 C 0.0911(3) 0.3821(3) 0.2498(8) 0.0471(10) Uani 1 1 d . . . H1A H 0.0556 0.3605 0.1442 0.057 Uiso 1 1 calc R . . H1B H 0.0560 0.3635 0.3584 0.057 Uiso 1 1 calc R . . C2 C 0.1939(4) 0.3460(4) 0.2514(11) 0.0784(18) Uani 1 1 d . . . H2A H 0.2308 0.3687 0.1502 0.118 Uiso 1 1 calc R . . H2B H 0.1907 0.2847 0.2418 0.118 Uiso 1 1 calc R . . H2C H 0.2263 0.3614 0.3634 0.118 Uiso 1 1 calc R . . C3 C 0.0991(5) 0.0499(5) 0.8119(16) 0.117(4) Uani 1 1 d . . . H3A H 0.1150 0.0526 0.9395 0.176 Uiso 1 1 calc R . . H3B H 0.1293 0.0000 0.7591 0.176 Uiso 1 1 calc R . . H3C H 0.0284 0.0468 0.7969 0.176 Uiso 1 1 calc R . . N1 N 0.0931(2) 0.4776(2) 0.2437(6) 0.0388(7) Uani 1 1 d . . . H1C H 0.1308 0.4974 0.3342 0.058 Uiso 1 1 calc R . . H1D H 0.0316 0.4978 0.2559 0.058 Uiso 1 1 calc R . . H1E H 0.1181 0.4948 0.1373 0.058 Uiso 1 1 calc R . . N2 N 0.1378(3) 0.1285(2) 0.7182(8) 0.0594(12) Uani 1 1 d . . . H2D H 0.1041 0.1742 0.7567 0.089 Uiso 1 1 calc R . . H2E H 0.1303 0.1230 0.5981 0.089 Uiso 1 1 calc R . . H2F H 0.2019 0.1352 0.7443 0.089 Uiso 1 1 calc R . . O1W O 0.4499(4) 0.3392(3) 0.1677(7) 0.0909(15) Uani 1 1 d . . . H1W H 0.5009 0.3573 0.2242 0.136 Uiso 1 1 d R . . H2W H 0.4281 0.3362 0.0590 0.136 Uiso 1 1 d R . . O2W O 0.1146(4) 0.1006(4) 0.3473(9) 0.113(2) Uani 1 1 d . . . H3W H 0.1273 0.0473 0.3402 0.169 Uiso 1 1 d R . . H4W H 0.1647 0.1323 0.3676 0.169 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 Al 0.0314(5) 0.0276(5) 0.0380(6) 0.0009(6) -0.0021(6) -0.0009(4) B1 0.0286(18) 0.033(2) 0.038(2) 0.004(2) -0.002(2) -0.0018(15) B2 0.0244(18) 0.030(2) 0.043(3) 0.000(2) -0.0009(19) 0.0009(15) B3 0.0318(19) 0.031(2) 0.037(3) 0.002(2) -0.001(2) 0.0011(15) B4 0.032(2) 0.038(3) 0.032(2) -0.004(2) -0.0006(19) -0.0032(19) B5 0.032(2) 0.032(2) 0.030(2) -0.0028(19) -0.0029(18) -0.0021(17) O1 0.0324(13) 0.0335(14) 0.0611(19) 0.0016(16) 0.0008(16) -0.0024(10) O2 0.0322(13) 0.0308(14) 0.062(2) -0.0034(16) -0.0034(16) 0.0025(10) O3 0.0302(12) 0.0307(14) 0.058(2) 0.0025(15) 0.0022(15) 0.0006(10) O4 0.0320(13) 0.0309(15) 0.0558(19) -0.0026(13) -0.0078(14) 0.0022(10) O5 0.0273(12) 0.0294(13) 0.058(2) -0.0002(14) -0.0031(14) 0.0018(10) O6 0.0451(17) 0.0311(16) 0.0394(16) 0.0041(13) 0.0046(13) 0.0034(12) O7 0.0532(18) 0.0319(16) 0.0345(17) -0.0009(13) -0.0010(14) 0.0002(13) O8 0.061(2) 0.0401(18) 0.0356(17) -0.0050(15) 0.0061(15) 0.0020(15) O9 0.0552(17) 0.0264(14) 0.0380(16) 0.0036(12) 0.0006(13) 0.0040(12) O10 0.0430(16) 0.0395(17) 0.0405(17) 0.0038(14) -0.0027(13) 0.0022(13) C1 0.054(2) 0.039(2) 0.048(2) -0.004(2) 0.004(2) -0.0016(18) C2 0.076(3) 0.072(4) 0.087(5) 0.001(4) 0.007(4) 0.033(3) C3 0.072(4) 0.067(5) 0.212(13) 0.020(6) -0.008(6) -0.008(3) N1 0.0377(15) 0.0365(18) 0.0423(18) -0.004(2) 0.0021(17) 0.0039(12) N2 0.053(2) 0.036(2) 0.089(4) -0.008(2) -0.013(2) 0.0000(17) O1W 0.100(3) 0.083(3) 0.089(3) -0.001(3) -0.030(3) -0.031(3) O2W 0.093(4) 0.109(4) 0.137(5) -0.053(4) -0.044(4) 0.043(3) _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 O8 1.721(4) 2_564 ? Al O10 1.734(3) 2_565 ? Al O4 1.746(3) 4_455 ? Al O1 1.750(3) . ? B1 O1 1.341(5) . ? B1 O3 1.364(5) . ? B1 O2 1.399(5) . ? B2 O5 1.355(5) . ? B2 O4 1.360(5) . ? B2 O2 1.401(5) . ? B3 O6 1.455(6) . ? B3 O5 1.461(5) . ? B3 O7 1.479(6) . ? B3 O3 1.492(5) . ? B4 O8 1.333(6) . ? B4 O6 1.380(6) . ? B4 O9 1.406(6) . ? B5 O10 1.354(6) . ? B5 O7 1.357(6) . ? B5 O9 1.387(6) . ? O4 Al 1.746(3) 4 ? O8 Al 1.721(4) 2_565 ? O10 Al 1.734(3) 2_564 ? C1 N1 1.492(5) . ? C1 C2 1.493(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N2 1.499(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N2 H2D 0.8900 . ? N2 H2E 0.8900 . ? N2 H2F 0.8900 . ? O1W H1W 0.8499 . ? O1W H2W 0.8500 . ? O2W H3W 0.8499 . ? O2W H4W 0.8500 . ? 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 O8 Al O10 107.66(17) 2_564 2_565 ? O8 Al O4 109.75(16) 2_564 4_455 ? O10 Al O4 112.96(17) 2_565 4_455 ? O8 Al O1 109.95(18) 2_564 . ? O10 Al O1 111.33(16) 2_565 . ? O4 Al O1 105.18(13) 4_455 . ? O1 B1 O3 123.6(3) . . ? O1 B1 O2 117.3(4) . . ? O3 B1 O2 119.1(3) . . ? O5 B2 O4 122.5(3) . . ? O5 B2 O2 119.5(3) . . ? O4 B2 O2 118.0(3) . . ? O6 B3 O5 110.0(3) . . ? O6 B3 O7 111.5(3) . . ? O5 B3 O7 109.5(3) . . ? O6 B3 O3 107.6(3) . . ? O5 B3 O3 111.1(3) . . ? O7 B3 O3 107.1(3) . . ? O8 B4 O6 123.3(4) . . ? O8 B4 O9 117.9(4) . . ? O6 B4 O9 118.8(4) . . ? O10 B5 O7 119.4(4) . . ? O10 B5 O9 121.1(4) . . ? O7 B5 O9 119.6(4) . . ? B1 O1 Al 143.4(3) . . ? B1 O2 B2 121.0(3) . . ? B1 O3 B3 123.3(3) . . ? B2 O4 Al 124.8(2) . 4 ? B2 O5 B3 124.1(3) . . ? B4 O6 B3 124.3(4) . . ? B5 O7 B3 124.4(3) . . ? B4 O8 Al 150.7(3) . 2_565 ? B5 O9 B4 121.3(3) . . ? B5 O10 Al 142.7(3) . 2_564 ? N1 C1 C2 111.1(4) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N2 H2D 109.5 . . ? C3 N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? C3 N2 H2F 109.5 . . ? H2D N2 H2F 109.5 . . ? H2E N2 H2F 109.5 . . ? H1W O1W H2W 138.9 . . ? H3W O2W H4W 114.7 . . ? 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 H1C O7 0.89 1.99 2.846(5) 159.8 . N1 H1C O10 0.89 2.46 3.033(5) 122.5 . N1 H1D O3 0.89 1.99 2.866(4) 166.7 2_564 N1 H1E O6 0.89 1.99 2.865(6) 167.7 1_554 N2 H2D O1 0.89 2.03 2.888(5) 161.9 . N2 H2D O2 0.89 2.52 3.002(5) 114.7 . N2 H2E O2W 0.89 1.88 2.770(8) 174.9 . N2 H2F O10 0.89 2.13 2.996(5) 163.9 3_545 O1W H1W O2W 0.85 1.89 2.743(7) 179.0 4 O1W H2W O4 0.85 2.11 2.956(6) 179.4 1_554 O2W H3W O5 0.85 2.06 2.822(5) 148.4 3_544 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.539 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.079