Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Norbert Mitzel' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Universitat Munster Corrensstr. 30 Munster D-48149 GERMANY ; _publ_contact_author_email MITZEL@UNI-MUENSTER.DE _publ_section_title ; Organoaluminium complexes with sterically demanding oximato ligands: Does a bulky and rigid ligand backbone change the aggregation motif? ; loop_ _publ_author_name 'Norbert Mitzel' 'Klaus Bergander' 'Roland Frohlich' 'Matthias Ullrich' data_hgh081 _database_code_depnum_ccdc_archive 'CCDC 275303' _audit_creation_method SHELXL-97 _chemical_name_systematic 'bis-({\m2-bicyclo[2.2.1]heptane-2-one oximato-N,O} dimethylaluminium)' _chemical_name_common ;bis-((mu2-bicyclo(2.2.1)heptane-2-one oximato-N,O) dimethylaluminium) ; _chemical_melting_point 108 _chemical_formula_moiety 'C9 H18 AL N O' _chemical_formula_sum 'C18 H32 Al2 N2 O2' _chemical_formula_weight 362.42 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' 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.235(4) _cell_length_b 8.3840(17) _cell_length_c 12.596(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.19(3) _cell_angle_gamma 90.00 _cell_volume 2031.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4408 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71093 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9940 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.14 _reflns_number_total 2466 _reflns_number_gt 2043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0739P)^2^+0.5724P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2466 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 0.47195(2) 1.18432(5) 0.45058(3) 0.02480(16) Uani 1 1 d . . . O1 O 0.48506(5) 1.12355(13) 0.58597(8) 0.0257(2) Uani 1 1 d . . . N1 N 0.45690(6) 0.97122(14) 0.38987(9) 0.0236(3) Uani 1 1 d . . . C1 C 0.40862(7) 0.90098(17) 0.33901(10) 0.0233(3) Uani 1 1 d . . . C2 C 0.34029(7) 0.97593(19) 0.30973(11) 0.0277(3) Uani 1 1 d . . . H2 H 0.3405 1.0918 0.2995 0.033 Uiso 1 1 calc R . . C3 C 0.31997(8) 0.8750(2) 0.21268(12) 0.0334(4) Uani 1 1 d . . . H3A H 0.2723 0.8923 0.1903 0.040 Uiso 1 1 calc R . . H3B H 0.3513 0.8897 0.1533 0.040 Uiso 1 1 calc R . . C4 C 0.33037(8) 0.7147(2) 0.26875(13) 0.0328(4) Uani 1 1 d . . . H4 H 0.3206 0.6211 0.2246 0.039 Uiso 1 1 calc R . . C5 C 0.28379(8) 0.7314(2) 0.36630(14) 0.0370(4) Uani 1 1 d . . . H5A H 0.3002 0.6648 0.4241 0.044 Uiso 1 1 calc R . . H5B H 0.2361 0.7029 0.3497 0.044 Uiso 1 1 calc R . . C6 C 0.28997(8) 0.9112(2) 0.39478(12) 0.0326(4) Uani 1 1 d . . . H6A H 0.2451 0.9638 0.3904 0.039 Uiso 1 1 calc R . . H6B H 0.3089 0.9256 0.4656 0.039 Uiso 1 1 calc R . . C7 C 0.40617(8) 0.72965(19) 0.30565(12) 0.0280(3) Uani 1 1 d . . . H7A H 0.4161 0.6587 0.3646 0.034 Uiso 1 1 calc R . . H7B H 0.4384 0.7082 0.2483 0.034 Uiso 1 1 calc R . . C8 C 0.55625(9) 1.2662(2) 0.38366(14) 0.0383(4) Uani 1 1 d . . . H8A H 0.5661 1.3710 0.4105 0.057 Uiso 1 1 calc R . . H8B H 0.5495 1.2714 0.3082 0.057 Uiso 1 1 calc R . . H8C H 0.5945 1.1965 0.3994 0.057 Uiso 1 1 calc R . . C9 C 0.38653(9) 1.31087(19) 0.45022(14) 0.0354(4) Uani 1 1 d . . . H9A H 0.3485 1.2460 0.4739 0.053 Uiso 1 1 calc R . . H9B H 0.3772 1.3483 0.3796 0.053 Uiso 1 1 calc R . . H9C H 0.3919 1.4004 0.4971 0.053 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 Al1 0.0259(3) 0.0232(3) 0.0253(2) -0.00104(16) -0.00280(17) -0.00090(16) O1 0.0224(5) 0.0299(5) 0.0248(5) -0.0028(4) -0.0036(4) 0.0040(4) N1 0.0225(6) 0.0263(6) 0.0220(5) 0.0009(5) -0.0019(4) 0.0011(5) C1 0.0240(7) 0.0257(7) 0.0200(6) 0.0021(5) 0.0003(5) -0.0023(5) C2 0.0257(7) 0.0301(8) 0.0273(7) 0.0025(6) -0.0055(6) -0.0012(6) C3 0.0298(8) 0.0440(9) 0.0264(7) 0.0001(7) -0.0077(6) -0.0045(7) C4 0.0289(8) 0.0350(8) 0.0344(8) -0.0046(7) -0.0047(6) -0.0099(6) C5 0.0276(8) 0.0403(9) 0.0432(9) 0.0043(7) 0.0016(7) -0.0093(7) C6 0.0242(7) 0.0433(9) 0.0304(7) 0.0025(7) -0.0005(6) 0.0011(6) C7 0.0279(7) 0.0273(8) 0.0289(7) -0.0026(6) -0.0022(6) -0.0038(6) C8 0.0413(9) 0.0386(9) 0.0351(9) -0.0007(7) 0.0015(7) -0.0125(7) C9 0.0398(9) 0.0286(8) 0.0379(9) -0.0009(6) -0.0065(7) 0.0067(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 Al1 O1 1.7968(11) . ? Al1 C8 1.9545(18) . ? Al1 C9 1.9559(17) . ? Al1 N1 1.9645(13) . ? O1 N1 1.4030(15) 5_676 ? N1 C1 1.2711(18) . ? N1 O1 1.4029(15) 5_676 ? C1 C7 1.497(2) . ? C1 C2 1.502(2) . ? C2 C3 1.536(2) . ? C2 C6 1.545(2) . ? C3 C4 1.531(2) . ? C4 C5 1.530(2) . ? C4 C7 1.534(2) . ? C5 C6 1.554(2) . ? 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 C8 113.26(7) . . ? O1 Al1 C9 105.73(7) . . ? C8 Al1 C9 120.44(8) . . ? O1 Al1 N1 97.56(5) . . ? C8 Al1 N1 105.85(7) . . ? C9 Al1 N1 111.70(7) . . ? N1 O1 Al1 118.40(8) 5_676 . ? C1 N1 O1 115.25(12) . 5_676 ? C1 N1 Al1 136.39(11) . . ? O1 N1 Al1 108.33(8) 5_676 . ? N1 C1 C7 127.45(13) . . ? N1 C1 C2 124.56(14) . . ? C7 C1 C2 107.81(12) . . ? C1 C2 C3 100.68(12) . . ? C1 C2 C6 103.46(12) . . ? C3 C2 C6 101.54(12) . . ? C4 C3 C2 94.81(12) . . ? C5 C4 C3 102.38(13) . . ? C5 C4 C7 107.94(13) . . ? C3 C4 C7 101.01(12) . . ? C4 C5 C6 103.26(12) . . ? C2 C6 C5 103.18(12) . . ? C1 C7 C4 101.08(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.361 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.055 data_mat2_NEW _database_code_depnum_ccdc_archive 'CCDC 275304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tris-((mu2-(1R,4R)-1,7,7-trimethylbicyclo(2.2.1)heptane-2-one oximato-O)dimethylaluminium) ; _chemical_melting_point 130 _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Al3 N3 O3' _chemical_formula_weight 669.86 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' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.7886(13) _cell_length_b 20.1732(19) _cell_length_c 14.6935(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.182(2) _cell_angle_gamma 90.00 _cell_volume 4055.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47369 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 30.03 _reflns_number_total 23078 _reflns_number_gt 16562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0728P)^2^+0.1089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(12) _refine_ls_number_reflns 23078 _refine_ls_number_parameters 913 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.003 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 Al1A Al 0.32022(8) 0.36908(6) 0.58043(7) 0.0280(2) Uani 1 1 d . A 1 Al2A Al 0.18368(7) 0.30467(5) 0.40011(6) 0.0215(2) Uani 1 1 d . A 1 Al3A Al 0.23194(7) 0.46544(5) 0.40734(7) 0.0234(2) Uani 1 1 d . A 1 N1A N 0.1190(2) 0.33562(14) 0.56725(18) 0.0257(6) Uani 1 1 d . A 1 N2A N 0.30873(19) 0.36808(14) 0.29426(17) 0.0238(6) Uani 1 1 d . A 1 N3A N 0.3917(2) 0.48774(14) 0.5496(2) 0.0308(7) Uani 1 1 d . A 1 O1A O 0.20965(16) 0.32587(11) 0.52399(14) 0.0246(5) Uani 1 1 d . A 1 O2A O 0.23520(16) 0.38152(11) 0.35730(14) 0.0220(5) Uani 1 1 d . A 1 O3A O 0.30000(15) 0.44964(10) 0.52143(14) 0.0234(5) Uani 1 1 d . A 1 C1A C 0.4315(3) 0.3254(2) 0.5372(3) 0.0498(11) Uani 1 1 d . A 1 H1AB H 0.4227 0.3245 0.4699 0.075 Uiso 1 1 calc R A 1 H1AC H 0.4366 0.2799 0.5607 0.075 Uiso 1 1 calc R A 1 H1AD H 0.4915 0.3497 0.5591 0.075 Uiso 1 1 calc R A 1 C2A C 0.3098(4) 0.3817(2) 0.7097(2) 0.0518(12) Uani 1 1 d . A 1 H2AB H 0.2487 0.4048 0.7166 0.078 Uiso 1 1 calc R A 1 H2AC H 0.3653 0.4082 0.7377 0.078 Uiso 1 1 calc R A 1 H2AD H 0.3103 0.3384 0.7402 0.078 Uiso 1 1 calc R A 1 C3A C 0.1044(2) 0.28648(15) 0.6162(2) 0.0214(6) Uani 1 1 d . A 1 C4A C 0.1626(3) 0.22293(16) 0.6382(2) 0.0308(8) Uani 1 1 d . A 1 H4AA H 0.2290 0.2324 0.6694 0.037 Uiso 1 1 calc R A 1 H4AB H 0.1676 0.1965 0.5823 0.037 Uiso 1 1 calc R A 1 C5A C 0.0998(3) 0.18796(16) 0.7023(2) 0.0329(8) Uani 1 1 d . A 1 H5AA H 0.1112 0.1391 0.7083 0.039 Uiso 1 1 calc R A 1 C6A C 0.1139(3) 0.22605(18) 0.7935(2) 0.0383(9) Uani 1 1 d . A 1 H6AA H 0.1840 0.2345 0.8137 0.046 Uiso 1 1 calc R A 1 H6AB H 0.0857 0.2014 0.8422 0.046 Uiso 1 1 calc R A 1 C7A C 0.0578(3) 0.29176(18) 0.7699(2) 0.0358(8) Uani 1 1 d . A 1 H7AA H 0.1024 0.3303 0.7783 0.043 Uiso 1 1 calc R A 1 H7AB H 0.0047 0.2977 0.8087 0.043 Uiso 1 1 calc R A 1 C8A C 0.0156(2) 0.28331(17) 0.6671(2) 0.0302(8) Uani 1 1 d . A 1 C9A C -0.0053(3) 0.20743(18) 0.6617(3) 0.0367(8) Uani 1 1 d . A 1 C10A C -0.0344(3) 0.1831(2) 0.5640(3) 0.0508(11) Uani 1 1 d . A 1 H10A H -0.0467 0.1353 0.5646 0.076 Uiso 1 1 calc R A 1 H10B H 0.0186 0.1923 0.5271 0.076 Uiso 1 1 calc R A 1 H10C H -0.0938 0.2061 0.5373 0.076 Uiso 1 1 calc R A 1 C11A C -0.0838(3) 0.1841(2) 0.7204(3) 0.0632(13) Uani 1 1 d . A 1 H11A H -0.0931 0.1361 0.7131 0.095 Uiso 1 1 calc R A 1 H11B H -0.1455 0.2069 0.7004 0.095 Uiso 1 1 calc R A 1 H11C H -0.0626 0.1944 0.7850 0.095 Uiso 1 1 calc R A 1 C12A C -0.0661(3) 0.3308(2) 0.6333(3) 0.0419(9) Uani 1 1 d . A 1 H12A H -0.0879 0.3222 0.5683 0.063 Uiso 1 1 calc R A 1 H12B H -0.0422 0.3765 0.6407 0.063 Uiso 1 1 calc R A 1 H12C H -0.1209 0.3244 0.6689 0.063 Uiso 1 1 calc R A 1 C13A C 0.0440(2) 0.30285(19) 0.3593(2) 0.0314(8) Uani 1 1 d . A 1 H13A H 0.0147 0.3449 0.3749 0.047 Uiso 1 1 calc R A 1 H13B H 0.0139 0.2664 0.3897 0.047 Uiso 1 1 calc R A 1 H13C H 0.0331 0.2964 0.2927 0.047 Uiso 1 1 calc R A 1 C14A C 0.2624(3) 0.22724(18) 0.3778(3) 0.0360(9) Uani 1 1 d . A 1 H14A H 0.3308 0.2355 0.4019 0.054 Uiso 1 1 calc R A 1 H14B H 0.2574 0.2188 0.3117 0.054 Uiso 1 1 calc R A 1 H14C H 0.2385 0.1885 0.4086 0.054 Uiso 1 1 calc R A 1 C15A C 0.2733(2) 0.38145(16) 0.2126(2) 0.0222(7) Uani 1 1 d . A 1 C16A C 0.1738(2) 0.40723(19) 0.1752(2) 0.0330(8) Uani 1 1 d . A 1 H16A H 0.1610 0.4511 0.2013 0.040 Uiso 1 1 calc R A 1 H16B H 0.1215 0.3760 0.1872 0.040 Uiso 1 1 calc R A 1 C17A C 0.1829(3) 0.4120(2) 0.0725(2) 0.0418(9) Uani 1 1 d . A 1 H17A H 0.1190 0.4134 0.0320 0.050 Uiso 1 1 calc R A 1 C18A C 0.2511(3) 0.4695(2) 0.0589(3) 0.0533(12) Uani 1 1 d . A 1 H18A H 0.2320 0.5100 0.0903 0.064 Uiso 1 1 calc R A 1 H18B H 0.2519 0.4793 -0.0071 0.064 Uiso 1 1 calc R A 1 C19A C 0.3524(3) 0.4430(2) 0.1036(3) 0.0464(10) Uani 1 1 d . A 1 H19A H 0.4005 0.4433 0.0590 0.056 Uiso 1 1 calc R A 1 H19B H 0.3780 0.4703 0.1574 0.056 Uiso 1 1 calc R A 1 C20A C 0.3312(3) 0.37233(19) 0.1326(2) 0.0338(8) Uani 1 1 d . A 1 C21A C 0.2464(3) 0.3514(2) 0.0574(2) 0.0402(9) Uani 1 1 d . A 1 C22A C 0.2780(4) 0.3472(3) -0.0391(3) 0.0733(16) Uani 1 1 d . A 1 H22A H 0.2234 0.3603 -0.0847 0.110 Uiso 1 1 calc R A 1 H22B H 0.2974 0.3016 -0.0511 0.110 Uiso 1 1 calc RD A 1 H22C H 0.3335 0.3770 -0.0430 0.110 Uiso 1 1 calc R A 1 C23A C 0.2014(4) 0.2844(2) 0.0761(3) 0.0593(13) Uani 1 1 d . A 1 H23A H 0.1489 0.2742 0.0268 0.089 Uiso 1 1 calc R A 1 H23B H 0.1746 0.2861 0.1348 0.089 Uiso 1 1 calc R A 1 H23C H 0.2517 0.2499 0.0787 0.089 Uiso 1 1 calc R A 1 C24A C 0.4196(3) 0.3273(3) 0.1507(3) 0.0550(12) Uani 1 1 d . A 1 H24A H 0.4663 0.3464 0.1994 0.082 Uiso 1 1 calc R A 1 H24B H 0.4508 0.3229 0.0946 0.082 Uiso 1 1 calc R A 1 H24C H 0.3989 0.2835 0.1698 0.082 Uiso 1 1 calc R A 1 C25A C 0.0969(2) 0.48094(18) 0.4265(3) 0.0353(9) Uani 1 1 d . A 1 H25A H 0.0736 0.4438 0.4611 0.053 Uiso 1 1 calc R A 1 H25B H 0.0563 0.4847 0.3671 0.053 Uiso 1 1 calc R A 1 H25C H 0.0926 0.5221 0.4612 0.053 Uiso 1 1 calc R A 1 C26A C 0.2998(3) 0.53040(17) 0.3402(2) 0.0313(8) Uani 1 1 d . A 1 H26A H 0.3668 0.5152 0.3366 0.047 Uiso 1 1 calc R A 1 H26B H 0.3016 0.5731 0.3722 0.047 Uiso 1 1 calc R A 1 H26C H 0.2653 0.5355 0.2782 0.047 Uiso 1 1 calc R A 1 C27A C 0.3718(2) 0.53915(17) 0.5937(2) 0.0252(7) Uani 1 1 d . A 1 C28A C 0.2774(3) 0.5643(2) 0.6181(4) 0.0576(13) Uani 1 1 d . A 1 H28A H 0.2446 0.5310 0.6532 0.069 Uiso 1 1 calc R A 1 H28B H 0.2329 0.5774 0.5629 0.069 Uiso 1 1 calc R A 1 C29A C 0.3111(3) 0.6248(2) 0.6776(4) 0.0613(14) Uani 1 1 d . A 1 H29A H 0.2588 0.6582 0.6843 0.074 Uiso 1 1 calc R A 1 C30A C 0.3610(5) 0.5972(3) 0.7667(4) 0.097(2) Uani 1 1 d . A 1 H30A H 0.3209 0.5620 0.7905 0.116 Uiso 1 1 calc R A 1 H30B H 0.3733 0.6325 0.8135 0.116 Uiso 1 1 calc R A 1 C31A C 0.4580(5) 0.5687(2) 0.7413(3) 0.0721(17) Uani 1 1 d . A 1 H31A H 0.4621 0.5203 0.7525 0.086 Uiso 1 1 calc R A 1 H31B H 0.5149 0.5906 0.7767 0.086 Uiso 1 1 calc R A 1 C32A C 0.4529(3) 0.58447(19) 0.6376(3) 0.0370(9) Uani 1 1 d . A 1 C33A C 0.3964(3) 0.65072(19) 0.6321(3) 0.0381(9) Uani 1 1 d . A 1 C34A C 0.3687(4) 0.6740(2) 0.5334(3) 0.0625(14) Uani 1 1 d . A 1 H34A H 0.3332 0.6387 0.4977 0.094 Uiso 1 1 calc R A 1 H34B H 0.4282 0.6849 0.5063 0.094 Uiso 1 1 calc R A 1 H34C H 0.3271 0.7134 0.5329 0.094 Uiso 1 1 calc R A 1 C35A C 0.4545(3) 0.7071(2) 0.6867(3) 0.0487(11) Uani 1 1 d . A 1 H35A H 0.4732 0.6928 0.7502 0.073 Uiso 1 1 calc R A 1 H35B H 0.4135 0.7468 0.6860 0.073 Uiso 1 1 calc R A 1 H35C H 0.5134 0.7171 0.6583 0.073 Uiso 1 1 calc R A 1 C36A C 0.5453(3) 0.5809(2) 0.5977(4) 0.0712(17) Uani 1 1 d . A 1 H36A H 0.5334 0.5920 0.5323 0.107 Uiso 1 1 calc R A 1 H36B H 0.5719 0.5359 0.6050 0.107 Uiso 1 1 calc R A 1 H36C H 0.5921 0.6124 0.6291 0.107 Uiso 1 1 calc R A 1 Al1B Al 0.81254(8) 0.52015(6) 0.08750(6) 0.0242(2) Uani 1 1 d . B 1 Al2B Al 0.68647(7) 0.44440(6) -0.08735(6) 0.0261(2) Uani 1 1 d . B 1 Al3B Al 0.78408(7) 0.35671(5) 0.09149(6) 0.0228(2) Uani 1 1 d . B 1 N3B N 0.69386(19) 0.45308(14) 0.19666(18) 0.0266(6) Uani 1 1 d . B 1 O1B O 0.79214(16) 0.49463(11) -0.03500(14) 0.0256(5) Uani 1 1 d D B 1 O2B O 0.71144(16) 0.36676(10) -0.02194(14) 0.0261(5) Uani 1 1 d D B 1 O3B O 0.77053(16) 0.44170(12) 0.13527(13) 0.0254(5) Uani 1 1 d . B 1 C1B C 0.9526(2) 0.53336(18) 0.1266(2) 0.0304(8) Uani 1 1 d . B 1 H1BA H 0.9885 0.4932 0.1137 0.046 Uiso 1 1 calc R B 1 H1BB H 0.9631 0.5426 0.1926 0.046 Uiso 1 1 calc R B 1 H1BC H 0.9762 0.5708 0.0931 0.046 Uiso 1 1 calc R B 1 C2B C 0.7248(3) 0.59307(19) 0.1057(3) 0.0373(9) Uani 1 1 d . B 1 H2BA H 0.6575 0.5802 0.0836 0.056 Uiso 1 1 calc R B 1 H2BB H 0.7429 0.6320 0.0715 0.056 Uiso 1 1 calc R B 1 H2BC H 0.7300 0.6039 0.1712 0.056 Uiso 1 1 calc R B 1 N1B N 0.8824(2) 0.48308(14) -0.07764(17) 0.0257(6) Uani 1 1 d . B 1 C3B C 0.9098(2) 0.53653(15) -0.1124(2) 0.0246(7) Uani 1 1 d D B 1 C4B C 0.8645(3) 0.60466(17) -0.1188(2) 0.0305(8) Uani 1 1 d . B 1 H4BA H 0.8622 0.6243 -0.0573 0.037 Uiso 1 1 calc R B 1 H4BB H 0.7978 0.6039 -0.1527 0.037 Uiso 1 1 calc R B 1 C5B C 0.9366(3) 0.64198(17) -0.1725(3) 0.0395(9) Uani 1 1 d . B 1 H5BA H 0.9098 0.6833 -0.2038 0.047 Uiso 1 1 calc R B 1 C6B C 1.0309(3) 0.65199(18) -0.1054(3) 0.0479(10) Uani 1 1 d D B 1 H6BA H 1.0766 0.6825 -0.1313 0.058 Uiso 1 1 calc R B 1 H6BB H 1.0160 0.6698 -0.0459 0.058 Uiso 1 1 calc R B 1 C7B C 1.0736(3) 0.58177(19) -0.0943(3) 0.0395(9) Uani 1 1 d . B 1 H7BA H 1.0764 0.5666 -0.0299 0.047 Uiso 1 1 calc R B 1 H7BB H 1.1402 0.5803 -0.1126 0.047 Uiso 1 1 calc R B 1 C8B C 1.0021(3) 0.53819(17) -0.1590(2) 0.0285(7) Uani 1 1 d . B 1 C9B C 0.9677(3) 0.58781(18) -0.2380(2) 0.0356(8) Uani 1 1 d . B 1 C10B C 0.8840(3) 0.5604(2) -0.3050(2) 0.0460(10) Uani 1 1 d . B 1 H10D H 0.8647 0.5932 -0.3529 0.069 Uiso 1 1 calc R B 1 H10E H 0.8281 0.5505 -0.2720 0.069 Uiso 1 1 calc R B 1 H10F H 0.9053 0.5197 -0.3330 0.069 Uiso 1 1 calc R B 1 C11B C 1.0503(3) 0.6096(2) -0.2925(3) 0.0552(12) Uani 1 1 d . B 1 H11D H 1.1046 0.6275 -0.2502 0.083 Uiso 1 1 calc R B 1 H11E H 1.0258 0.6438 -0.3369 0.083 Uiso 1 1 calc R B 1 H11F H 1.0731 0.5714 -0.3250 0.083 Uiso 1 1 calc R B 1 C12B C 1.0412(3) 0.47191(18) -0.1829(2) 0.0382(9) Uani 1 1 d . B 1 H12D H 1.0597 0.4464 -0.1266 0.057 Uiso 1 1 calc R B 1 H12E H 1.0986 0.4782 -0.2151 0.057 Uiso 1 1 calc R B 1 H12F H 0.9907 0.4478 -0.2227 0.057 Uiso 1 1 calc R B 1 C13B C 0.6953(3) 0.4282(2) -0.2173(2) 0.0441(10) Uani 1 1 d . B 1 H13D H 0.7584 0.4076 -0.2240 0.066 Uiso 1 1 calc R B 1 H13E H 0.6896 0.4703 -0.2507 0.066 Uiso 1 1 calc R B 1 H13F H 0.6423 0.3985 -0.2423 0.066 Uiso 1 1 calc R B 1 C14B C 0.5707(3) 0.48491(19) -0.0466(3) 0.0367(9) Uani 1 1 d . B 1 H14D H 0.5799 0.4888 0.0204 0.055 Uiso 1 1 calc R B 1 H14E H 0.5134 0.4572 -0.0658 0.055 Uiso 1 1 calc R B 1 H14F H 0.5607 0.5291 -0.0739 0.055 Uiso 1 1 calc R B 1 N2B N 0.7305(3) 0.30302(18) -0.0606(3) 0.0188(10) Uani 0.542(4) 1 d PD B 1 C15B C 0.6537(4) 0.2742(3) -0.0963(5) 0.022(2) Uani 0.542(4) 1 d PD B 1 C16B C 0.5482(3) 0.2951(2) -0.1055(4) 0.0333(15) Uani 0.542(4) 1 d PD B 1 H16C H 0.5373 0.3370 -0.1403 0.040 Uiso 0.542(4) 1 calc PR B 1 H16D H 0.5248 0.3001 -0.0449 0.040 Uiso 0.542(4) 1 calc PR B 1 C17B C 0.4992(3) 0.2360(2) -0.1593(4) 0.0343(16) Uani 0.542(4) 1 d PD B 1 H17B H 0.4277 0.2316 -0.1550 0.041 Uiso 0.542(4) 1 calc PR B 1 C18B C 0.5246(4) 0.2412(3) -0.2571(3) 0.0377(17) Uani 0.542(4) 1 d PD B 1 H18C H 0.5145 0.2868 -0.2812 0.045 Uiso 0.542(4) 1 calc PR B 1 H18D H 0.4850 0.2100 -0.2985 0.045 Uiso 0.542(4) 1 calc PR B 1 C19B C 0.6338(5) 0.2221(3) -0.2461(3) 0.034(2) Uani 0.542(4) 1 d PD B 1 H19C H 0.6743 0.2590 -0.2647 0.041 Uiso 0.542(4) 1 calc PR B 1 H19D H 0.6448 0.1824 -0.2832 0.041 Uiso 0.542(4) 1 calc PR B 1 C20B C 0.6580(3) 0.2072(2) -0.1418(3) 0.0223(12) Uani 0.542(4) 1 d PD B 1 C21B C 0.5602(3) 0.1772(2) -0.1205(3) 0.0263(14) Uani 0.542(4) 1 d PD B 1 C22B C 0.5341(5) 0.1111(2) -0.1696(4) 0.037(2) Uani 0.542(4) 1 d PD B 1 H22D H 0.4716 0.0950 -0.1530 0.055 Uiso 0.542(4) 1 calc PR B 1 H22E H 0.5854 0.0785 -0.1509 0.055 Uiso 0.542(4) 1 calc PR B 1 H22F H 0.5287 0.1178 -0.2361 0.055 Uiso 0.542(4) 1 calc PR B 1 C23B C 0.5584(5) 0.1654(3) -0.0178(4) 0.046(4) Uani 0.542(4) 1 d PD B 1 H23D H 0.4950 0.1467 -0.0077 0.069 Uiso 0.542(4) 1 calc PR B 1 H23E H 0.5685 0.2076 0.0152 0.069 Uiso 0.542(4) 1 calc PR B 1 H23F H 0.6105 0.1344 0.0050 0.069 Uiso 0.542(4) 1 calc PR B 1 C24B C 0.7512(3) 0.1686(3) -0.1163(4) 0.0384(17) Uani 0.542(4) 1 d PD B 1 H24D H 0.7610 0.1612 -0.0499 0.058 Uiso 0.542(4) 1 calc PR B 1 H24E H 0.8066 0.1938 -0.1344 0.058 Uiso 0.542(4) 1 calc PR B 1 H24F H 0.7466 0.1258 -0.1481 0.058 Uiso 0.542(4) 1 calc PR B 1 C25B C 0.9208(2) 0.34785(19) 0.0741(3) 0.0344(8) Uani 1 1 d . B 1 H25D H 0.9396 0.3848 0.0367 0.052 Uiso 1 1 calc R B 1 H25E H 0.9306 0.3059 0.0429 0.052 Uiso 1 1 calc R B 1 H25F H 0.9612 0.3484 0.1339 0.052 Uiso 1 1 calc R B 1 C26B C 0.7238(3) 0.29041(18) 0.1631(2) 0.0352(9) Uani 1 1 d . B 1 H26D H 0.6550 0.3019 0.1651 0.053 Uiso 1 1 calc R B 1 H26E H 0.7581 0.2893 0.2256 0.053 Uiso 1 1 calc R B 1 H26F H 0.7279 0.2468 0.1345 0.053 Uiso 1 1 calc R B 1 C27B C 0.7325(2) 0.45310(15) 0.27890(19) 0.0191(6) Uani 1 1 d . B 1 C28B C 0.8366(2) 0.4407(2) 0.3197(2) 0.0325(8) Uani 1 1 d . B 1 H28C H 0.8823 0.4717 0.2948 0.039 Uiso 1 1 calc R B 1 H28D H 0.8569 0.3946 0.3092 0.039 Uiso 1 1 calc R B 1 C29B C 0.8302(2) 0.45412(18) 0.4227(2) 0.0315(8) Uani 1 1 d . B 1 H29B H 0.8853 0.4350 0.4654 0.038 Uiso 1 1 calc R B 1 C30B C 0.8185(3) 0.5286(2) 0.4305(2) 0.0447(10) Uani 1 1 d . B 1 H30C H 0.8652 0.5524 0.3963 0.054 Uiso 1 1 calc R B 1 H30D H 0.8283 0.5430 0.4954 0.054 Uiso 1 1 calc R B 1 C31B C 0.7119(3) 0.54018(18) 0.3870(3) 0.0428(10) Uani 1 1 d . B 1 H31C H 0.7095 0.5698 0.3330 0.051 Uiso 1 1 calc R B 1 H31D H 0.6726 0.5600 0.4319 0.051 Uiso 1 1 calc R B 1 C32B C 0.6737(2) 0.46925(17) 0.3579(2) 0.0255(7) Uani 1 1 d . B 1 C33B C 0.7291(2) 0.42665(16) 0.4355(2) 0.0245(7) Uani 1 1 d . B 1 C34B C 0.7173(3) 0.35233(17) 0.4173(2) 0.0350(8) Uani 1 1 d . B 1 H34D H 0.7531 0.3276 0.4682 0.052 Uiso 1 1 calc R B 1 H34E H 0.7433 0.3412 0.3601 0.052 Uiso 1 1 calc R B 1 H34F H 0.6478 0.3406 0.4118 0.052 Uiso 1 1 calc R B 1 C35B C 0.7000(3) 0.4397(2) 0.5307(2) 0.0363(8) Uani 1 1 d . B 1 H35D H 0.7381 0.4108 0.5755 0.054 Uiso 1 1 calc R B 1 H35E H 0.6302 0.4304 0.5304 0.054 Uiso 1 1 calc R B 1 H35F H 0.7132 0.4861 0.5475 0.054 Uiso 1 1 calc R B 1 C36B C 0.5649(2) 0.4631(2) 0.3381(3) 0.0435(10) Uani 1 1 d . B 1 H36D H 0.5477 0.4173 0.3205 0.065 Uiso 1 1 calc R B 1 H36E H 0.5407 0.4931 0.2879 0.065 Uiso 1 1 calc R B 1 H36F H 0.5350 0.4749 0.3931 0.065 Uiso 1 1 calc R B 1 N1C N 0.6225(4) 0.33129(19) -0.0537(3) 0.0248(14) Uani 0.458(4) 1 d PD B 2 C2C C 0.6377(4) 0.27288(18) -0.0786(5) 0.024(3) Uani 0.458(4) 1 d PD B 2 C3C C 0.7307(3) 0.2347(3) -0.0834(4) 0.0309(18) Uani 0.458(4) 1 d PD B 2 H3CA H 0.7707 0.2320 -0.0227 0.037 Uiso 0.458(4) 1 calc PR B 2 H3CB H 0.7702 0.2545 -0.1282 0.037 Uiso 0.458(4) 1 calc PR B 2 C4C C 0.6906(4) 0.1666(2) -0.1153(4) 0.0289(17) Uani 0.458(4) 1 d PD B 2 H4CA H 0.7381 0.1380 -0.1435 0.035 Uiso 0.458(4) 1 calc PR B 2 C5C C 0.6484(5) 0.1348(2) -0.0340(4) 0.046(2) Uani 0.458(4) 1 d PD B 2 H5CA H 0.6948 0.1383 0.0229 0.055 Uiso 0.458(4) 1 calc PR B 2 H5CB H 0.6321 0.0876 -0.0462 0.055 Uiso 0.458(4) 1 calc PR B 2 C6C C 0.5551(5) 0.1765(3) -0.0272(4) 0.037(4) Uani 0.458(4) 1 d PD B 2 H6CA H 0.4960 0.1481 -0.0342 0.045 Uiso 0.458(4) 1 calc PR B 2 H6CB H 0.5594 0.2000 0.0323 0.045 Uiso 0.458(4) 1 calc PR B 2 C1C C 0.5528(3) 0.2260(2) -0.1073(4) 0.0323(19) Uani 0.458(4) 1 d PD B 2 C7C C 0.5982(4) 0.1842(2) -0.1799(3) 0.0294(17) Uani 0.458(4) 1 d PD B 2 C9C C 0.6177(7) 0.2245(4) -0.2639(3) 0.056(4) Uani 0.458(4) 1 d PD B 2 H9CA H 0.6469 0.1957 -0.3068 0.084 Uiso 0.458(4) 1 calc PR B 2 H9CB H 0.6628 0.2608 -0.2445 0.084 Uiso 0.458(4) 1 calc PR B 2 H9CC H 0.5561 0.2427 -0.2940 0.084 Uiso 0.458(4) 1 calc PR B 2 C10C C 0.5362(6) 0.1242(3) -0.2155(5) 0.050(3) Uani 0.458(4) 1 d PD B 2 H10G H 0.5691 0.1004 -0.2610 0.075 Uiso 0.458(4) 1 calc PR B 2 H10H H 0.4720 0.1395 -0.2439 0.075 Uiso 0.458(4) 1 calc PR B 2 H10I H 0.5279 0.0946 -0.1642 0.075 Uiso 0.458(4) 1 calc PR B 2 C8C C 0.4564(3) 0.2597(3) -0.1369(6) 0.058(3) Uani 0.458(4) 1 d PD B 2 H8CA H 0.4535 0.3016 -0.1036 0.087 Uiso 0.458(4) 1 calc PRD B 2 H8CB H 0.4028 0.2308 -0.1234 0.087 Uiso 0.458(4) 1 calc PRD B 2 H8CC H 0.4501 0.2685 -0.2030 0.087 Uiso 0.458(4) 1 calc PR B 2 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 Al1A 0.0344(6) 0.0227(5) 0.0245(5) 0.0045(4) -0.0067(4) -0.0059(4) Al2A 0.0232(5) 0.0189(5) 0.0217(5) -0.0016(4) 0.0003(4) -0.0007(4) Al3A 0.0265(5) 0.0167(5) 0.0257(5) 0.0022(4) -0.0015(4) 0.0013(4) N1A 0.0289(15) 0.0246(15) 0.0242(14) -0.0024(11) 0.0059(11) -0.0011(12) N2A 0.0233(13) 0.0277(15) 0.0209(13) -0.0002(11) 0.0042(11) 0.0042(12) N3A 0.0267(15) 0.0264(16) 0.0384(17) -0.0039(13) 0.0000(13) -0.0015(12) O1A 0.0287(12) 0.0252(12) 0.0196(11) -0.0017(9) 0.0010(9) -0.0062(9) O2A 0.0233(11) 0.0233(12) 0.0201(11) -0.0002(9) 0.0053(9) 0.0016(9) O3A 0.0247(11) 0.0202(11) 0.0239(11) -0.0005(9) -0.0020(9) -0.0039(9) C1A 0.032(2) 0.036(2) 0.077(3) -0.001(2) -0.014(2) 0.0040(17) C2A 0.078(3) 0.047(2) 0.026(2) 0.0046(18) -0.012(2) -0.024(2) C3A 0.0276(16) 0.0153(15) 0.0205(15) -0.0021(12) -0.0003(13) -0.0008(12) C4A 0.0338(19) 0.0206(17) 0.0369(19) 0.0009(14) 0.0001(15) 0.0022(14) C5A 0.042(2) 0.0161(15) 0.041(2) 0.0057(14) 0.0064(16) 0.0003(14) C6A 0.048(2) 0.033(2) 0.035(2) 0.0089(16) 0.0080(17) 0.0036(17) C7A 0.044(2) 0.034(2) 0.0299(18) 0.0068(15) 0.0068(16) 0.0109(16) C8A 0.0304(18) 0.0253(18) 0.0351(19) 0.0066(14) 0.0055(15) 0.0078(14) C9A 0.0325(19) 0.0319(19) 0.046(2) 0.0112(16) 0.0050(16) -0.0055(15) C10A 0.054(3) 0.035(2) 0.059(3) 0.0008(19) -0.010(2) -0.0205(19) C11A 0.047(3) 0.062(3) 0.082(3) 0.028(3) 0.014(2) -0.008(2) C12A 0.039(2) 0.046(2) 0.042(2) 0.0073(17) 0.0081(17) 0.0098(17) C13A 0.0315(18) 0.0315(18) 0.0295(17) -0.0031(15) -0.0020(14) -0.0035(15) C14A 0.036(2) 0.0251(19) 0.047(2) -0.0047(16) 0.0034(17) -0.0003(15) C15A 0.0243(16) 0.0202(15) 0.0216(15) 0.0008(12) 0.0002(13) -0.0050(12) C16A 0.0272(18) 0.042(2) 0.0274(17) 0.0082(15) -0.0055(14) -0.0001(15) C17A 0.038(2) 0.054(2) 0.0292(19) 0.0142(17) -0.0124(16) -0.0124(18) C18A 0.070(3) 0.051(3) 0.034(2) 0.0180(19) -0.013(2) -0.014(2) C19A 0.049(2) 0.058(3) 0.0304(18) 0.0150(18) -0.0026(17) -0.025(2) C20A 0.037(2) 0.041(2) 0.0235(17) 0.0020(15) 0.0049(15) -0.0079(16) C21A 0.052(2) 0.050(2) 0.0178(16) -0.0003(16) 0.0007(15) -0.0143(19) C22A 0.109(4) 0.090(4) 0.020(2) -0.008(2) 0.006(2) -0.025(3) C23A 0.088(4) 0.046(3) 0.041(2) -0.010(2) -0.005(2) -0.025(2) C24A 0.050(3) 0.085(4) 0.032(2) -0.005(2) 0.0154(19) 0.017(2) C25A 0.0305(18) 0.0216(18) 0.052(2) -0.0022(15) -0.0022(17) 0.0052(14) C26A 0.0374(19) 0.0233(18) 0.0315(18) 0.0055(14) -0.0021(15) -0.0062(15) C27A 0.0265(17) 0.0244(17) 0.0252(16) -0.0020(13) 0.0057(13) -0.0017(13) C28A 0.039(2) 0.046(3) 0.091(4) -0.035(2) 0.019(2) -0.0081(19) C29A 0.060(3) 0.050(3) 0.080(3) -0.037(3) 0.037(3) -0.019(2) C30A 0.177(7) 0.070(4) 0.057(3) -0.036(3) 0.068(4) -0.063(4) C31A 0.116(5) 0.042(3) 0.049(3) -0.006(2) -0.029(3) -0.011(3) C32A 0.0296(19) 0.033(2) 0.047(2) -0.0085(17) -0.0016(17) -0.0035(15) C33A 0.034(2) 0.033(2) 0.049(2) -0.0142(17) 0.0100(17) 0.0045(16) C34A 0.100(4) 0.032(2) 0.052(3) -0.0014(19) -0.008(3) -0.008(2) C35A 0.051(3) 0.038(2) 0.060(3) -0.021(2) 0.020(2) -0.0157(19) C36A 0.040(2) 0.048(3) 0.130(5) -0.050(3) 0.024(3) -0.018(2) Al1B 0.0345(6) 0.0216(5) 0.0166(5) -0.0035(4) 0.0035(4) -0.0039(4) Al2B 0.0325(6) 0.0275(5) 0.0169(4) 0.0003(4) -0.0023(4) -0.0036(4) Al3B 0.0275(5) 0.0208(5) 0.0198(5) 0.0003(4) 0.0017(4) -0.0028(4) N3B 0.0255(14) 0.0343(17) 0.0205(13) 0.0031(11) 0.0046(11) -0.0046(12) O1B 0.0300(12) 0.0284(13) 0.0189(11) -0.0015(9) 0.0046(9) -0.0051(10) O2B 0.0327(12) 0.0208(12) 0.0239(11) -0.0041(9) -0.0007(9) -0.0030(10) O3B 0.0355(13) 0.0258(12) 0.0159(10) -0.0041(9) 0.0071(9) -0.0026(10) C1B 0.0369(19) 0.0317(19) 0.0220(16) -0.0001(14) 0.0013(14) -0.0074(15) C2B 0.042(2) 0.0286(19) 0.042(2) -0.0120(16) 0.0093(17) -0.0012(16) N1B 0.0345(16) 0.0237(15) 0.0186(13) 0.0002(11) 0.0014(11) 0.0017(12) C3B 0.0332(18) 0.0218(17) 0.0185(15) -0.0023(12) 0.0024(13) 0.0026(14) C4B 0.0371(19) 0.0280(18) 0.0278(17) 0.0044(14) 0.0100(15) 0.0038(15) C5B 0.054(2) 0.0203(17) 0.048(2) 0.0149(16) 0.0225(19) 0.0065(16) C6B 0.053(3) 0.034(2) 0.061(3) -0.0026(19) 0.021(2) -0.0142(19) C7B 0.034(2) 0.043(2) 0.042(2) -0.0043(17) 0.0057(17) -0.0065(16) C8B 0.0341(18) 0.0256(17) 0.0271(17) 0.0025(14) 0.0085(14) 0.0042(14) C9B 0.047(2) 0.0311(18) 0.0312(18) 0.0094(15) 0.0166(16) 0.0112(16) C10B 0.056(3) 0.056(3) 0.0256(18) 0.0124(18) 0.0040(18) 0.019(2) C11B 0.062(3) 0.052(3) 0.059(3) 0.024(2) 0.036(2) 0.013(2) C12B 0.048(2) 0.035(2) 0.0331(19) 0.0019(15) 0.0098(17) 0.0177(17) C13B 0.059(3) 0.052(3) 0.0205(17) -0.0027(16) -0.0008(17) -0.020(2) C14B 0.034(2) 0.034(2) 0.039(2) 0.0014(16) -0.0074(16) 0.0006(16) N2B 0.025(2) 0.017(2) 0.015(2) 0.0004(17) 0.0036(18) 0.0023(19) C15B 0.017(4) 0.032(5) 0.018(3) -0.004(3) 0.004(3) -0.005(3) C16B 0.028(3) 0.030(3) 0.041(4) -0.010(3) -0.005(3) 0.008(3) C17B 0.026(4) 0.037(4) 0.039(4) -0.013(3) -0.002(3) 0.000(3) C18B 0.043(4) 0.041(4) 0.027(3) -0.007(3) -0.003(3) -0.001(3) C19B 0.038(5) 0.033(5) 0.034(4) -0.016(3) 0.015(4) 0.000(4) C20B 0.030(3) 0.020(3) 0.018(3) -0.005(2) 0.007(2) 0.003(3) C21B 0.017(3) 0.030(4) 0.034(3) -0.012(3) 0.009(3) -0.003(2) C22B 0.034(4) 0.028(4) 0.051(5) -0.026(4) 0.015(4) -0.007(3) C23B 0.065(9) 0.052(6) 0.022(5) 0.002(5) 0.007(5) -0.022(6) C24B 0.025(4) 0.039(4) 0.052(4) -0.009(3) 0.008(3) 0.006(3) C25B 0.0312(19) 0.0298(19) 0.041(2) 0.0048(16) 0.0010(15) -0.0016(15) C26B 0.050(2) 0.0270(19) 0.0303(18) 0.0052(15) 0.0132(17) -0.0069(16) C27B 0.0195(14) 0.0194(16) 0.0186(14) 0.0001(11) 0.0038(11) 0.0007(11) C28B 0.0193(16) 0.059(2) 0.0190(15) 0.0034(16) 0.0013(12) -0.0008(16) C29B 0.0267(17) 0.053(2) 0.0141(14) 0.0044(14) 0.0000(12) -0.0078(15) C30B 0.065(3) 0.049(3) 0.0201(17) -0.0019(16) 0.0047(17) -0.023(2) C31B 0.072(3) 0.0285(19) 0.0304(19) -0.0009(15) 0.0173(19) 0.0073(18) C32B 0.0264(16) 0.0324(17) 0.0184(15) 0.0025(13) 0.0060(12) 0.0064(14) C33B 0.0275(16) 0.0281(17) 0.0185(14) 0.0024(12) 0.0048(12) -0.0006(13) C34B 0.055(2) 0.0273(18) 0.0224(17) 0.0021(14) 0.0040(16) -0.0022(16) C35B 0.044(2) 0.045(2) 0.0219(16) 0.0017(16) 0.0113(15) 0.0017(18) C36B 0.0299(19) 0.068(3) 0.033(2) 0.0094(19) 0.0025(16) 0.0097(19) N1C 0.021(3) 0.032(3) 0.021(3) -0.009(2) -0.002(2) -0.004(3) C2C 0.024(5) 0.012(4) 0.036(6) -0.007(3) 0.002(4) 0.004(3) C3C 0.019(4) 0.035(4) 0.037(4) -0.005(3) -0.002(3) 0.005(3) C4C 0.022(4) 0.029(4) 0.039(4) -0.016(3) 0.015(4) 0.005(3) C5C 0.041(5) 0.032(5) 0.064(6) -0.013(4) 0.004(4) -0.005(4) C6C 0.037(8) 0.023(5) 0.057(8) -0.014(5) 0.026(6) -0.005(4) C1C 0.021(4) 0.029(4) 0.046(5) -0.017(4) -0.001(3) 0.007(3) C7C 0.024(4) 0.032(4) 0.032(4) -0.015(3) 0.001(3) -0.001(3) C9C 0.072(10) 0.064(9) 0.029(5) 0.012(5) -0.011(6) -0.019(7) C10C 0.052(6) 0.046(6) 0.055(7) -0.029(5) 0.015(5) -0.022(5) C8C 0.025(5) 0.064(7) 0.084(8) -0.028(6) -0.001(5) 0.006(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 Al1A O3A 1.846(2) . ? Al1A O1A 1.859(2) . ? Al1A C2A 1.940(4) . ? Al1A C1A 1.945(4) . ? Al2A O2A 1.848(2) . ? Al2A O1A 1.860(2) . ? Al2A C13A 1.944(3) . ? Al2A C14A 1.953(4) . ? Al3A O3A 1.844(2) . ? Al3A O2A 1.848(2) . ? Al3A C25A 1.944(4) . ? Al3A C26A 1.948(3) . ? N1A C3A 1.256(4) . ? N1A O1A 1.484(3) . ? N2A C15A 1.266(4) . ? N2A O2A 1.481(3) . ? N3A C27A 1.270(4) . ? N3A O3A 1.493(3) . ? C3A C8A 1.514(5) . ? C3A C4A 1.525(4) . ? C4A C5A 1.528(5) . ? C5A C6A 1.536(5) . ? C5A C9A 1.548(5) . ? C6A C7A 1.552(5) . ? C7A C8A 1.558(5) . ? C8A C12A 1.514(5) . ? C8A C9A 1.558(5) . ? C9A C10A 1.523(5) . ? C9A C11A 1.539(5) . ? C15A C16A 1.506(4) . ? C15A C20A 1.513(5) . ? C16A C17A 1.533(5) . ? C17A C18A 1.522(5) . ? C17A C21A 1.536(6) . ? C18A C19A 1.561(6) . ? C19A C20A 1.527(5) . ? C20A C24A 1.517(5) . ? C20A C21A 1.564(5) . ? C21A C23A 1.525(6) . ? C21A C22A 1.538(5) . ? C27A C28A 1.482(5) . ? C27A C32A 1.524(5) . ? C28A C29A 1.539(5) . ? C29A C30A 1.508(8) . ? C29A C33A 1.516(6) . ? C30A C31A 1.543(8) . ? C31A C32A 1.550(6) . ? C32A C36A 1.469(5) . ? C32A C33A 1.544(5) . ? C33A C34A 1.527(6) . ? C33A C35A 1.554(5) . ? Al1B O3B 1.853(2) . ? Al1B O1B 1.859(2) . ? Al1B C2B 1.944(4) . ? Al1B C1B 1.964(3) . ? Al2B O2B 1.847(2) . ? Al2B O1B 1.860(2) . ? Al2B C14B 1.952(4) . ? Al2B C13B 1.956(4) . ? Al3B O2B 1.845(2) . ? Al3B O3B 1.849(2) . ? Al3B C25B 1.942(4) . ? Al3B C26B 1.951(3) . ? N3B C27B 1.258(4) . ? N3B O3B 1.491(3) . ? O1B N1B 1.481(3) . ? O2B N2B 1.443(4) . ? N1B C3B 1.271(4) . ? C3B C4B 1.508(5) . ? C3B C8B 1.518(4) . ? C4B C5B 1.541(5) . ? C5B C6B 1.544(6) . ? C5B C9B 1.551(5) . ? C6B C7B 1.535(5) . ? C7B C8B 1.554(5) . ? C8B C12B 1.500(5) . ? C8B C9B 1.561(5) . ? C9B C10B 1.524(5) . ? C9B C11B 1.536(5) . ? N2B C15B 1.263(5) . ? C15B C16B 1.504(6) . ? C15B C20B 1.513(6) . ? C16B C17B 1.539(5) . ? C17B C21B 1.523(6) . ? C17B C18B 1.525(6) . ? C18B C19B 1.543(6) . ? C19B C20B 1.556(6) . ? C20B C24B 1.509(5) . ? C20B C21B 1.546(5) . ? C21B C23B 1.532(6) . ? C21B C22B 1.537(5) . ? C27B C28B 1.506(4) . ? C27B C32B 1.532(4) . ? C28B C29B 1.551(4) . ? C29B C30B 1.516(5) . ? C29B C33B 1.534(4) . ? C30B C31B 1.546(6) . ? C31B C32B 1.565(5) . ? C32B C36B 1.497(5) . ? C32B C33B 1.550(4) . ? C33B C35B 1.525(4) . ? C33B C34B 1.528(5) . ? N1C C2C 1.259(5) . ? C2C C3C 1.506(6) . ? C2C C1C 1.522(5) . ? C3C C4C 1.532(6) . ? C4C C5C 1.533(6) . ? C4C C7C 1.533(6) . ? C5C C6C 1.550(7) . ? C6C C1C 1.541(6) . ? C1C C8C 1.508(5) . ? C1C C7C 1.551(6) . ? C7C C9C 1.529(6) . ? C7C C10C 1.534(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 O3A Al1A O1A 97.82(10) . . ? O3A Al1A C2A 108.62(16) . . ? O1A Al1A C2A 109.97(16) . . ? O3A Al1A C1A 108.94(16) . . ? O1A Al1A C1A 106.16(15) . . ? C2A Al1A C1A 122.5(2) . . ? O2A Al2A O1A 96.03(10) . . ? O2A Al2A C13A 108.60(14) . . ? O1A Al2A C13A 111.60(13) . . ? O2A Al2A C14A 111.63(13) . . ? O1A Al2A C14A 107.75(14) . . ? C13A Al2A C14A 118.87(16) . . ? O3A Al3A O2A 99.70(10) . . ? O3A Al3A C25A 106.50(14) . . ? O2A Al3A C25A 106.05(13) . . ? O3A Al3A C26A 110.75(13) . . ? O2A Al3A C26A 112.18(14) . . ? C25A Al3A C26A 119.67(16) . . ? C3A N1A O1A 110.2(3) . . ? C15A N2A O2A 109.9(2) . . ? C27A N3A O3A 109.4(3) . . ? N1A O1A Al1A 115.73(16) . . ? N1A O1A Al2A 112.34(16) . . ? Al1A O1A Al2A 126.23(12) . . ? N2A O2A Al3A 117.97(17) . . ? N2A O2A Al2A 112.43(17) . . ? Al3A O2A Al2A 127.11(12) . . ? N3A O3A Al3A 118.72(17) . . ? N3A O3A Al1A 104.47(16) . . ? Al3A O3A Al1A 127.51(12) . . ? N1A C3A C8A 121.0(3) . . ? N1A C3A C4A 131.8(3) . . ? C8A C3A C4A 107.2(3) . . ? C3A C4A C5A 101.2(3) . . ? C4A C5A C6A 106.6(3) . . ? C4A C5A C9A 102.8(3) . . ? C6A C5A C9A 102.7(3) . . ? C5A C6A C7A 103.1(3) . . ? C6A C7A C8A 103.8(3) . . ? C3A C8A C12A 115.1(3) . . ? C3A C8A C9A 99.9(3) . . ? C12A C8A C9A 118.7(3) . . ? C3A C8A C7A 104.3(3) . . ? C12A C8A C7A 115.0(3) . . ? C9A C8A C7A 101.6(3) . . ? C10A C9A C11A 108.0(3) . . ? C10A C9A C5A 113.9(3) . . ? C11A C9A C5A 113.4(3) . . ? C10A C9A C8A 113.0(3) . . ? C11A C9A C8A 114.2(3) . . ? C5A C9A C8A 94.1(3) . . ? N2A C15A C16A 130.2(3) . . ? N2A C15A C20A 122.1(3) . . ? C16A C15A C20A 107.7(3) . . ? C15A C16A C17A 101.4(3) . . ? C18A C17A C16A 107.8(3) . . ? C18A C17A C21A 102.4(3) . . ? C16A C17A C21A 102.1(3) . . ? C17A C18A C19A 102.6(3) . . ? C20A C19A C18A 104.2(3) . . ? C15A C20A C24A 115.3(3) . . ? C15A C20A C19A 103.9(3) . . ? C24A C20A C19A 115.5(3) . . ? C15A C20A C21A 99.3(3) . . ? C24A C20A C21A 118.4(3) . . ? C19A C20A C21A 102.0(3) . . ? C23A C21A C17A 115.3(4) . . ? C23A C21A C22A 106.6(3) . . ? C17A C21A C22A 114.1(3) . . ? C23A C21A C20A 113.4(3) . . ? C17A C21A C20A 94.2(3) . . ? C22A C21A C20A 113.1(3) . . ? N3A C27A C28A 130.9(3) . . ? N3A C27A C32A 120.8(3) . . ? C28A C27A C32A 108.2(3) . . ? C27A C28A C29A 101.4(3) . . ? C30A C29A C33A 102.4(4) . . ? C30A C29A C28A 105.8(4) . . ? C33A C29A C28A 102.7(3) . . ? C29A C30A C31A 104.1(4) . . ? C30A C31A C32A 103.1(4) . . ? C36A C32A C27A 115.4(3) . . ? C36A C32A C33A 118.6(4) . . ? C27A C32A C33A 99.1(3) . . ? C36A C32A C31A 116.6(4) . . ? C27A C32A C31A 103.5(3) . . ? C33A C32A C31A 100.9(3) . . ? C29A C33A C34A 114.1(4) . . ? C29A C33A C32A 95.3(3) . . ? C34A C33A C32A 112.4(3) . . ? C29A C33A C35A 113.8(3) . . ? C34A C33A C35A 108.4(3) . . ? C32A C33A C35A 112.5(3) . . ? O3B Al1B O1B 96.52(10) . . ? O3B Al1B C2B 111.40(14) . . ? O1B Al1B C2B 108.75(14) . . ? O3B Al1B C1B 110.34(13) . . ? O1B Al1B C1B 110.19(13) . . ? C2B Al1B C1B 117.59(16) . . ? O2B Al2B O1B 99.28(10) . . ? O2B Al2B C14B 107.55(14) . . ? O1B Al2B C14B 105.85(14) . . ? O2B Al2B C13B 109.64(15) . . ? O1B Al2B C13B 110.71(14) . . ? C14B Al2B C13B 121.47(17) . . ? O2B Al3B O3B 98.36(10) . . ? O2B Al3B C25B 108.52(14) . . ? O3B Al3B C25B 105.86(14) . . ? O2B Al3B C26B 110.04(14) . . ? O3B Al3B C26B 112.31(14) . . ? C25B Al3B C26B 119.60(17) . . ? C27B N3B O3B 109.5(2) . . ? N1B O1B Al1B 114.81(17) . . ? N1B O1B Al2B 113.33(16) . . ? Al1B O1B Al2B 124.54(12) . . ? N2B O2B Al3B 98.79(19) . . ? N2B O2B Al2B 125.6(2) . . ? Al3B O2B Al2B 127.44(11) . . ? N3B O3B Al3B 117.62(17) . . ? N3B O3B Al1B 112.12(17) . . ? Al3B O3B Al1B 127.60(12) . . ? C3B N1B O1B 110.2(2) . . ? N1B C3B C4B 131.1(3) . . ? N1B C3B C8B 120.5(3) . . ? C4B C3B C8B 108.4(2) . . ? C3B C4B C5B 100.8(3) . . ? C4B C5B C6B 106.4(3) . . ? C4B C5B C9B 102.7(3) . . ? C6B C5B C9B 102.3(3) . . ? C7B C6B C5B 103.2(3) . . ? C6B C7B C8B 104.6(3) . . ? C12B C8B C3B 115.6(3) . . ? C12B C8B C7B 115.4(3) . . ? C3B C8B C7B 103.9(3) . . ? C12B C8B C9B 118.8(3) . . ? C3B C8B C9B 98.9(3) . . ? C7B C8B C9B 101.7(3) . . ? C10B C9B C11B 108.6(3) . . ? C10B C9B C5B 114.3(3) . . ? C11B C9B C5B 113.7(3) . . ? C10B C9B C8B 112.5(3) . . ? C11B C9B C8B 113.3(3) . . ? C5B C9B C8B 94.2(3) . . ? C15B N2B O2B 112.9(4) . . ? N2B C15B C16B 131.3(4) . . ? N2B C15B C20B 121.1(5) . . ? C16B C15B C20B 107.6(3) . . ? C15B C16B C17B 100.8(3) . . ? C21B C17B C18B 103.0(3) . . ? C21B C17B C16B 103.0(3) . . ? C18B C17B C16B 107.0(4) . . ? C17B C18B C19B 102.7(3) . . ? C18B C19B C20B 103.8(3) . . ? C24B C20B C15B 115.5(4) . . ? C24B C20B C21B 119.0(4) . . ? C15B C20B C21B 100.2(3) . . ? C24B C20B C19B 114.5(4) . . ? C15B C20B C19B 104.3(4) . . ? C21B C20B C19B 100.9(3) . . ? C17B C21B C23B 114.4(4) . . ? C17B C21B C22B 114.4(4) . . ? C23B C21B C22B 107.2(4) . . ? C17B C21B C20B 94.3(3) . . ? C23B C21B C20B 112.5(4) . . ? C22B C21B C20B 113.8(4) . . ? N3B C27B C28B 130.6(3) . . ? N3B C27B C32B 121.8(3) . . ? C28B C27B C32B 107.6(2) . . ? C27B C28B C29B 101.1(3) . . ? C30B C29B C33B 104.0(3) . . ? C30B C29B C28B 105.4(3) . . ? C33B C29B C28B 102.7(2) . . ? C29B C30B C31B 102.9(3) . . ? C30B C31B C32B 104.1(3) . . ? C36B C32B C27B 116.6(3) . . ? C36B C32B C33B 119.1(3) . . ? C27B C32B C33B 100.4(2) . . ? C36B C32B C31B 115.1(3) . . ? C27B C32B C31B 102.1(3) . . ? C33B C32B C31B 100.9(3) . . ? C35B C33B C34B 107.2(3) . . ? C35B C33B C29B 113.4(3) . . ? C34B C33B C29B 114.3(3) . . ? C35B C33B C32B 114.7(3) . . ? C34B C33B C32B 112.5(3) . . ? C29B C33B C32B 94.7(2) . . ? N1C C2C C3C 131.8(4) . . ? N1C C2C C1C 120.8(5) . . ? C3C C2C C1C 107.4(3) . . ? C2C C3C C4C 101.3(3) . . ? C3C C4C C5C 107.1(4) . . ? C3C C4C C7C 102.8(3) . . ? C5C C4C C7C 102.2(4) . . ? C4C C5C C6C 102.9(3) . . ? C1C C6C C5C 103.9(3) . . ? C8C C1C C2C 114.8(4) . . ? C8C C1C C6C 116.5(5) . . ? C2C C1C C6C 104.4(4) . . ? C8C C1C C7C 117.6(4) . . ? C2C C1C C7C 99.6(4) . . ? C6C C1C C7C 101.6(4) . . ? C9C C7C C4C 113.9(5) . . ? C9C C7C C10C 106.9(4) . . ? C4C C7C C10C 114.4(4) . . ? C9C C7C C1C 113.1(4) . . ? C4C C7C C1C 94.3(3) . . ? C10C C7C C1C 114.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.448 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.063 data_fro2779 _database_code_depnum_ccdc_archive 'CCDC 275305' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Al2 N2 O2' _chemical_formula_weight 446.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 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' _cell_length_a 10.920(1) _cell_length_b 16.960(1) _cell_length_c 29.994(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5555.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6113 _exptl_absorpt_correction_T_max 0.6692 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24698 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 65.01 _reflns_number_total 9145 _reflns_number_gt 8542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1091P)^2^+1.4992P] 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 riding _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 0.02(4) _refine_ls_number_reflns 9145 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.006 _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 0.83472(10) 0.56324(7) 0.12709(4) 0.0720(3) Uani 1 1 d . . . O1 O 0.7413(2) 0.56653(13) 0.07413(7) 0.0632(5) Uani 1 1 d . . . N1 N 0.6155(3) 0.54573(16) 0.08555(9) 0.0623(6) Uani 1 1 d . . . C1 C 0.5410(3) 0.60201(18) 0.07662(10) 0.0592(7) Uani 1 1 d . . . C11 C 0.5519(4) 0.6825(2) 0.05735(16) 0.0889(12) Uani 1 1 d . . . C12 C 0.4124(5) 0.7086(3) 0.0616(2) 0.1094(17) Uani 1 1 d . . . H12 H 0.3971 0.7661 0.0604 0.131 Uiso 1 1 calc R . . C13 C 0.3386(7) 0.6588(5) 0.0285(3) 0.163(3) Uani 1 1 d . . . H13A H 0.2536 0.6770 0.0271 0.196 Uiso 1 1 calc R . . H13B H 0.3745 0.6618 -0.0014 0.196 Uiso 1 1 calc R . . C14 C 0.3444(6) 0.5784(5) 0.0456(2) 0.137(2) Uani 1 1 d . . . H14A H 0.3898 0.5440 0.0252 0.165 Uiso 1 1 calc R . . H14B H 0.2623 0.5567 0.0502 0.165 Uiso 1 1 calc R . . C15 C 0.4091(4) 0.5877(2) 0.08780(14) 0.0769(9) Uani 1 1 d . . . C16 C 0.3731(4) 0.6667(4) 0.1052(2) 0.120(2) Uani 1 1 d . . . H16A H 0.4211 0.6832 0.1312 0.144 Uiso 1 1 calc R . . H16B H 0.2853 0.6712 0.1113 0.144 Uiso 1 1 calc R . . C17 C 0.6053(7) 0.6809(4) 0.0099(2) 0.143(3) Uani 1 1 d . . . H17A H 0.5866 0.7301 -0.0050 0.214 Uiso 1 1 calc R . . H17B H 0.5695 0.6374 -0.0066 0.214 Uiso 1 1 calc R . . H17C H 0.6934 0.6740 0.0115 0.214 Uiso 1 1 calc R . . C18 C 0.6319(7) 0.7372(3) 0.0857(3) 0.151(3) Uani 1 1 d . . . H18A H 0.7171 0.7218 0.0828 0.226 Uiso 1 1 calc R . . H18B H 0.6073 0.7335 0.1167 0.226 Uiso 1 1 calc R . . H18C H 0.6221 0.7912 0.0755 0.226 Uiso 1 1 calc R . . C19 C 0.3851(6) 0.5178(4) 0.1196(3) 0.149(3) Uani 1 1 d . . . H19A H 0.4146 0.4695 0.1060 0.224 Uiso 1 1 calc R . . H19B H 0.2978 0.5134 0.1251 0.224 Uiso 1 1 calc R . . H19C H 0.4276 0.5267 0.1475 0.224 Uiso 1 1 calc R . . C101 C 0.7436(5) 0.5825(4) 0.18217(16) 0.126(2) Uani 1 1 d . . . H10A H 0.6612 0.5618 0.1792 0.189 Uiso 1 1 calc R . . H10B H 0.7398 0.6388 0.1878 0.189 Uiso 1 1 calc R . . H10C H 0.7846 0.5566 0.2068 0.189 Uiso 1 1 calc R . . C102 C 0.9798(5) 0.6238(3) 0.1138(2) 0.1133(18) Uani 1 1 d . . . H10D H 1.0408 0.5898 0.1003 0.170 Uiso 1 1 calc R . . H10E H 1.0123 0.6461 0.1412 0.170 Uiso 1 1 calc R . . H10F H 0.9592 0.6660 0.0933 0.170 Uiso 1 1 calc R . . Al2 Al 0.80429(11) 0.49546(5) 0.03394(3) 0.0641(3) Uani 1 1 d . . . O2 O 0.8654(2) 0.46016(14) 0.12302(7) 0.0687(6) Uani 1 1 d . . . N2 N 0.8917(2) 0.43138(15) 0.08048(8) 0.0587(6) Uani 1 1 d . . . C2 C 0.9584(3) 0.36918(17) 0.08064(10) 0.0562(7) Uani 1 1 d . . . C21 C 1.0130(3) 0.3287(2) 0.12138(13) 0.0688(8) Uani 1 1 d . . . C22 C 1.0763(4) 0.2582(2) 0.09868(18) 0.0946(13) Uani 1 1 d . . . H22 H 1.1380 0.2312 0.1175 0.113 Uiso 1 1 calc R . . C23 C 0.9777(6) 0.2022(3) 0.0782(2) 0.1211(18) Uani 1 1 d . . . H23A H 1.0155 0.1537 0.0670 0.145 Uiso 1 1 calc R . . H23B H 0.9156 0.1883 0.1004 0.145 Uiso 1 1 calc R . . C24 C 0.9230(6) 0.2482(3) 0.0413(2) 0.1149(17) Uani 1 1 d . . . H24A H 0.8365 0.2594 0.0473 0.138 Uiso 1 1 calc R . . H24B H 0.9292 0.2193 0.0131 0.138 Uiso 1 1 calc R . . C25 C 0.9966(4) 0.3233(2) 0.03960(13) 0.0787(10) Uani 1 1 d . . . C26 C 1.1274(5) 0.2941(3) 0.0565(2) 0.1195(19) Uani 1 1 d . . . H26A H 1.1649 0.2551 0.0366 0.143 Uiso 1 1 calc R . . H26B H 1.1844 0.3375 0.0622 0.143 Uiso 1 1 calc R . . C27 C 1.1067(4) 0.3836(3) 0.14525(17) 0.1015(14) Uani 1 1 d . . . H27A H 1.0680 0.4336 0.1520 0.152 Uiso 1 1 calc R . . H27B H 1.1765 0.3924 0.1259 0.152 Uiso 1 1 calc R . . H27C H 1.1340 0.3589 0.1727 0.152 Uiso 1 1 calc R . . C28 C 0.9205(4) 0.3030(3) 0.15640(14) 0.0919(13) Uani 1 1 d . . . H28A H 0.8892 0.3491 0.1718 0.138 Uiso 1 1 calc R . . H28B H 0.9598 0.2681 0.1776 0.138 Uiso 1 1 calc R . . H28C H 0.8533 0.2755 0.1420 0.138 Uiso 1 1 calc R . . C29 C 1.0010(7) 0.3660(4) -0.00443(17) 0.136(3) Uani 1 1 d . . . H29A H 0.9206 0.3649 -0.0182 0.204 Uiso 1 1 calc R . . H29B H 1.0597 0.3404 -0.0239 0.204 Uiso 1 1 calc R . . H29C H 1.0255 0.4203 0.0004 0.204 Uiso 1 1 calc R . . C201 C 0.9178(5) 0.5580(3) -0.00169(16) 0.1091(16) Uani 1 1 d . . . H20A H 0.8856 0.6109 -0.0053 0.164 Uiso 1 1 calc R . . H20B H 0.9277 0.5337 -0.0308 0.164 Uiso 1 1 calc R . . H20C H 0.9965 0.5603 0.0132 0.164 Uiso 1 1 calc R . . C202 C 0.6762(5) 0.4339(2) 0.00666(13) 0.0942(13) Uani 1 1 d . . . H20D H 0.6596 0.3878 0.0248 0.141 Uiso 1 1 calc R . . H20E H 0.7019 0.4174 -0.0228 0.141 Uiso 1 1 calc R . . H20F H 0.6025 0.4656 0.0043 0.141 Uiso 1 1 calc R . . Al3 Al 0.69689(9) 0.03188(6) 0.12481(3) 0.0661(3) Uani 1 1 d . . . O3 O 0.80307(18) 0.01597(11) 0.17282(6) 0.0530(4) Uani 1 1 d . . . N3 N 0.9305(2) 0.02991(15) 0.15750(9) 0.0570(6) Uani 1 1 d . . . C3 C 0.9936(3) -0.03222(18) 0.16016(11) 0.0565(7) Uani 1 1 d . . . C31 C 0.9669(3) -0.11629(18) 0.17501(12) 0.0633(8) Uani 1 1 d . . . C32 C 1.0905(4) -0.1553(2) 0.16304(17) 0.0886(13) Uani 1 1 d . . . H32 H 1.1044 -0.2059 0.1787 0.106 Uiso 1 1 calc R . . C33 C 1.1061(6) -0.1615(3) 0.1122(2) 0.120(2) Uani 1 1 d . . . H33A H 1.0325 -0.1829 0.0980 0.144 Uiso 1 1 calc R . . H33B H 1.1767 -0.1944 0.1043 0.144 Uiso 1 1 calc R . . C34 C 1.1273(6) -0.0743(3) 0.0989(2) 0.136(3) Uani 1 1 d . . . H34A H 1.0615 -0.0553 0.0795 0.164 Uiso 1 1 calc R . . H34B H 1.2058 -0.0680 0.0835 0.164 Uiso 1 1 calc R . . C35 C 1.1275(3) -0.0292(3) 0.1443(2) 0.1005(17) Uani 1 1 d . . . C36 C 1.1824(4) -0.0920(3) 0.1756(2) 0.123(2) Uani 1 1 d . . . H36A H 1.2666 -0.1062 0.1677 0.148 Uiso 1 1 calc R . . H36B H 1.1776 -0.0770 0.2071 0.148 Uiso 1 1 calc R . . C37 C 0.8580(4) -0.1541(2) 0.1525(2) 0.0988(15) Uani 1 1 d . . . H37A H 0.7831 -0.1328 0.1650 0.148 Uiso 1 1 calc R . . H37B H 0.8604 -0.2106 0.1572 0.148 Uiso 1 1 calc R . . H37C H 0.8607 -0.1430 0.1207 0.148 Uiso 1 1 calc R . . C38 C 0.9464(6) -0.1191(3) 0.22489(15) 0.1045(16) Uani 1 1 d . . . H38A H 1.0099 -0.0891 0.2398 0.157 Uiso 1 1 calc R . . H38B H 0.9491 -0.1734 0.2350 0.157 Uiso 1 1 calc R . . H38C H 0.8670 -0.0966 0.2319 0.157 Uiso 1 1 calc R . . C39 C 1.1830(4) 0.0518(3) 0.1445(3) 0.166(4) Uani 1 1 d . . . H39A H 1.1348 0.0864 0.1257 0.249 Uiso 1 1 calc R . . H39B H 1.2661 0.0491 0.1332 0.249 Uiso 1 1 calc R . . H39C H 1.1840 0.0721 0.1747 0.249 Uiso 1 1 calc R . . C301 C 0.7717(5) 0.0158(3) 0.06636(13) 0.1059(17) Uani 1 1 d . . . H30A H 0.7098 0.0212 0.0434 0.159 Uiso 1 1 calc R . . H30B H 0.8069 -0.0367 0.0650 0.159 Uiso 1 1 calc R . . H30C H 0.8355 0.0547 0.0617 0.159 Uiso 1 1 calc R . . C302 C 0.5475(4) -0.0288(3) 0.1402(2) 0.1122(17) Uani 1 1 d . . . H30D H 0.5691 -0.0835 0.1454 0.168 Uiso 1 1 calc R . . H30E H 0.4895 -0.0257 0.1157 0.168 Uiso 1 1 calc R . . H30F H 0.5108 -0.0069 0.1669 0.168 Uiso 1 1 calc R . . Al4 Al 0.76705(9) 0.08416(5) 0.21879(3) 0.0574(2) Uani 1 1 d . . . O4 O 0.6804(2) 0.13591(13) 0.13527(6) 0.0626(5) Uani 1 1 d . . . N4 N 0.6710(2) 0.15901(13) 0.17999(7) 0.0472(5) Uani 1 1 d . . . C4 C 0.5991(2) 0.21691(15) 0.18715(9) 0.0485(6) Uani 1 1 d . . . C41 C 0.5164(3) 0.2577(2) 0.15316(11) 0.0663(8) Uani 1 1 d . . . C42 C 0.4504(4) 0.3172(2) 0.18530(15) 0.0812(10) Uani 1 1 d . . . H42 H 0.4137 0.3630 0.1698 0.097 Uiso 1 1 calc R . . C43 C 0.3614(4) 0.2742(3) 0.21593(18) 0.1012(14) Uani 1 1 d . . . H43A H 0.3110 0.3113 0.2330 0.121 Uiso 1 1 calc R . . H43B H 0.3079 0.2386 0.1991 0.121 Uiso 1 1 calc R . . C44 C 0.4485(4) 0.2287(3) 0.24608(15) 0.0913(13) Uani 1 1 d . . . H44A H 0.4381 0.1717 0.2420 0.110 Uiso 1 1 calc R . . H44B H 0.4336 0.2416 0.2775 0.110 Uiso 1 1 calc R . . C45 C 0.5768(4) 0.25431(19) 0.23208(11) 0.0670(8) Uani 1 1 d . . . C46 C 0.5515(5) 0.3393(2) 0.21730(16) 0.0885(12) Uani 1 1 d . . . H46A H 0.5228 0.3729 0.2418 0.106 Uiso 1 1 calc R . . H46B H 0.6218 0.3637 0.2024 0.106 Uiso 1 1 calc R . . C47 C 0.4296(4) 0.1987(3) 0.13038(16) 0.0982(14) Uani 1 1 d . . . H47A H 0.4741 0.1696 0.1078 0.147 Uiso 1 1 calc R . . H47B H 0.3624 0.2271 0.1166 0.147 Uiso 1 1 calc R . . H47C H 0.3976 0.1623 0.1524 0.147 Uiso 1 1 calc R . . C48 C 0.5878(4) 0.3024(3) 0.11754(15) 0.1012(16) Uani 1 1 d . . . H48A H 0.6398 0.2659 0.1014 0.152 Uiso 1 1 calc R . . H48B H 0.6380 0.3425 0.1316 0.152 Uiso 1 1 calc R . . H48C H 0.5309 0.3272 0.0970 0.152 Uiso 1 1 calc R . . C49 C 0.6782(5) 0.2455(3) 0.26714(13) 0.0944(13) Uani 1 1 d . . . H49A H 0.6821 0.1911 0.2770 0.142 Uiso 1 1 calc R . . H49B H 0.6604 0.2794 0.2924 0.142 Uiso 1 1 calc R . . H49C H 0.7561 0.2606 0.2542 0.142 Uiso 1 1 calc R . . C401 C 0.9185(5) 0.1251(3) 0.24474(16) 0.1041(17) Uani 1 1 d . . . H40A H 0.9759 0.0821 0.2491 0.156 Uiso 1 1 calc R . . H40B H 0.9007 0.1496 0.2732 0.156 Uiso 1 1 calc R . . H40C H 0.9541 0.1639 0.2248 0.156 Uiso 1 1 calc R . . C402 C 0.6476(6) 0.0270(3) 0.25481(16) 0.116(2) Uani 1 1 d . . . H40D H 0.5991 -0.0070 0.2357 0.175 Uiso 1 1 calc R . . H40E H 0.5943 0.0643 0.2698 0.175 Uiso 1 1 calc R . . H40F H 0.6901 -0.0047 0.2768 0.175 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 Al1 0.0620(6) 0.0770(6) 0.0770(6) -0.0291(5) -0.0119(5) 0.0216(5) O1 0.0539(11) 0.0615(12) 0.0743(13) -0.0070(10) -0.0050(10) 0.0141(10) N1 0.0654(15) 0.0560(14) 0.0655(14) 0.0058(12) 0.0021(12) 0.0042(13) C1 0.0619(17) 0.0565(16) 0.0593(16) -0.0050(13) -0.0112(14) 0.0158(14) C11 0.086(3) 0.062(2) 0.119(3) 0.006(2) -0.004(2) -0.001(2) C12 0.097(3) 0.074(3) 0.157(5) 0.027(3) -0.014(3) 0.033(3) C13 0.124(5) 0.177(7) 0.189(7) 0.027(6) -0.042(5) 0.035(5) C14 0.114(4) 0.181(7) 0.117(4) -0.024(4) -0.035(3) -0.006(5) C15 0.070(2) 0.071(2) 0.090(2) -0.0057(19) 0.0001(19) -0.0006(18) C16 0.066(2) 0.133(5) 0.162(5) -0.033(4) 0.017(3) 0.026(3) C17 0.166(6) 0.120(4) 0.142(5) 0.075(4) 0.030(5) 0.026(4) C18 0.156(5) 0.053(2) 0.243(8) -0.020(3) -0.039(6) -0.011(3) C19 0.116(4) 0.160(6) 0.172(6) 0.046(5) 0.044(4) -0.007(4) C101 0.109(4) 0.179(5) 0.089(3) -0.064(3) -0.017(3) 0.053(4) C102 0.081(3) 0.094(3) 0.165(5) -0.036(3) -0.021(3) 0.002(2) Al2 0.0856(7) 0.0566(5) 0.0501(4) 0.0036(4) 0.0009(4) 0.0203(5) O2 0.0823(15) 0.0748(14) 0.0489(10) -0.0058(10) -0.0016(10) 0.0259(12) N2 0.0697(15) 0.0579(14) 0.0485(12) 0.0014(11) 0.0077(11) 0.0205(13) C2 0.0534(16) 0.0486(15) 0.0665(17) 0.0069(13) 0.0079(14) 0.0085(13) C21 0.0554(17) 0.067(2) 0.084(2) 0.0199(17) -0.0104(16) 0.0032(15) C22 0.079(3) 0.062(2) 0.143(4) 0.021(2) -0.002(3) 0.024(2) C23 0.137(5) 0.071(3) 0.155(5) -0.006(3) 0.005(4) 0.010(3) C24 0.134(5) 0.077(3) 0.134(4) -0.016(3) 0.020(4) 0.010(3) C25 0.089(3) 0.065(2) 0.082(2) -0.0040(17) 0.017(2) 0.0211(19) C26 0.114(4) 0.079(3) 0.165(5) -0.005(3) 0.055(4) 0.031(3) C27 0.068(2) 0.119(4) 0.117(3) 0.006(3) -0.026(2) -0.003(2) C28 0.090(3) 0.098(3) 0.087(2) 0.039(2) 0.004(2) -0.002(2) C29 0.193(7) 0.124(4) 0.090(3) -0.006(3) 0.057(4) 0.056(5) C201 0.126(4) 0.114(4) 0.087(3) 0.028(3) 0.026(3) 0.027(3) C202 0.145(4) 0.071(2) 0.067(2) -0.0093(17) -0.014(2) 0.007(3) Al3 0.0537(5) 0.0787(6) 0.0659(5) -0.0265(5) -0.0133(4) 0.0148(4) O3 0.0491(10) 0.0488(10) 0.0611(10) -0.0016(8) -0.0013(8) 0.0008(8) N3 0.0439(12) 0.0522(13) 0.0749(15) 0.0140(11) -0.0061(11) 0.0003(11) C3 0.0488(15) 0.0495(15) 0.0711(17) 0.0151(13) -0.0074(13) 0.0027(13) C31 0.0627(18) 0.0452(15) 0.082(2) 0.0107(14) -0.0031(16) 0.0026(14) C32 0.075(2) 0.0551(19) 0.136(4) 0.034(2) 0.005(2) 0.0176(18) C33 0.134(4) 0.085(3) 0.141(4) 0.023(3) 0.054(4) 0.043(3) C34 0.134(5) 0.108(4) 0.167(5) 0.048(4) 0.087(4) 0.050(4) C35 0.0506(19) 0.069(2) 0.182(5) 0.055(3) 0.012(2) 0.0089(17) C36 0.056(2) 0.077(3) 0.237(7) 0.061(3) -0.019(3) 0.009(2) C37 0.088(3) 0.0502(19) 0.158(4) -0.009(2) -0.021(3) -0.0081(19) C38 0.142(4) 0.079(3) 0.092(3) 0.038(2) 0.021(3) 0.014(3) C39 0.052(2) 0.084(3) 0.362(11) 0.084(5) 0.013(4) 0.001(2) C301 0.109(3) 0.140(4) 0.068(2) -0.035(3) -0.023(2) 0.051(3) C302 0.062(2) 0.109(3) 0.165(5) -0.041(3) -0.017(3) -0.001(2) Al4 0.0780(6) 0.0462(4) 0.0480(4) 0.0048(3) -0.0056(4) 0.0025(4) O4 0.0689(13) 0.0733(13) 0.0455(10) -0.0034(9) -0.0032(9) 0.0209(11) N4 0.0506(12) 0.0462(11) 0.0446(11) -0.0020(9) 0.0007(9) -0.0037(10) C4 0.0443(14) 0.0417(13) 0.0595(15) 0.0006(12) 0.0052(12) -0.0042(11) C41 0.0493(17) 0.075(2) 0.0744(19) 0.0069(16) 0.0032(14) 0.0165(15) C42 0.065(2) 0.068(2) 0.110(3) 0.000(2) 0.013(2) 0.0257(18) C43 0.076(3) 0.100(3) 0.128(4) -0.004(3) 0.033(3) 0.019(2) C44 0.096(3) 0.085(3) 0.092(3) 0.000(2) 0.041(2) 0.013(2) C45 0.083(2) 0.0508(16) 0.0671(18) -0.0099(14) 0.0092(16) 0.0039(16) C46 0.101(3) 0.0502(18) 0.115(3) -0.0101(19) 0.008(3) 0.014(2) C47 0.062(2) 0.119(4) 0.113(3) -0.016(3) -0.031(2) 0.020(2) C48 0.095(3) 0.111(3) 0.097(3) 0.052(3) 0.019(2) 0.044(3) C49 0.125(4) 0.085(3) 0.073(2) -0.031(2) -0.011(2) 0.009(3) C401 0.122(4) 0.087(3) 0.103(3) -0.018(2) -0.063(3) 0.015(3) C402 0.182(6) 0.071(2) 0.097(3) 0.023(2) 0.057(4) 0.004(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 Al1 O2 1.784(3) . ? Al1 O1 1.889(2) . ? Al1 C102 1.929(6) . ? Al1 C101 1.956(5) . ? O1 N1 1.458(4) . ? O1 Al2 1.838(2) . ? N1 C1 1.282(4) . ? C1 C11 1.487(5) . ? C1 C15 1.499(5) . ? C11 C18 1.533(7) . ? C11 C17 1.537(7) . ? C11 C12 1.592(7) . ? C12 C13 1.531(9) . ? C12 C16 1.550(8) . ? C13 C14 1.457(10) . ? C14 C15 1.459(6) . ? C15 C16 1.491(7) . ? C15 C19 1.544(7) . ? Al2 C202 1.928(5) . ? Al2 C201 1.950(5) . ? Al2 N2 2.010(3) . ? O2 N2 1.396(3) . ? N2 C2 1.282(4) . ? C2 C25 1.515(5) . ? C2 C21 1.523(4) . ? C21 C28 1.521(5) . ? C21 C22 1.540(6) . ? C21 C27 1.558(6) . ? C22 C26 1.512(7) . ? C22 C23 1.561(8) . ? C23 C24 1.479(8) . ? C24 C25 1.507(7) . ? C25 C29 1.507(7) . ? C25 C26 1.595(7) . ? Al3 O4 1.801(2) . ? Al3 O3 1.868(2) . ? Al3 C301 1.953(4) . ? Al3 C302 1.983(5) . ? O3 N3 1.485(3) . ? O3 Al4 1.842(2) . ? N3 C3 1.261(4) . ? C3 C31 1.522(4) . ? C3 C35 1.539(5) . ? C31 C37 1.511(5) . ? C31 C38 1.514(6) . ? C31 C32 1.545(5) . ? C32 C36 1.517(7) . ? C32 C33 1.539(7) . ? C33 C34 1.548(7) . ? C34 C35 1.561(9) . ? C35 C39 1.500(7) . ? C35 C36 1.541(6) . ? Al4 C402 1.951(5) . ? Al4 C401 1.956(5) . ? Al4 N4 2.016(2) . ? O4 N4 1.401(3) . ? N4 C4 1.275(4) . ? C4 C45 1.509(4) . ? C4 C41 1.528(4) . ? C41 C48 1.524(5) . ? C41 C47 1.538(6) . ? C41 C42 1.571(5) . ? C42 C46 1.510(6) . ? C42 C43 1.524(6) . ? C43 C44 1.523(7) . ? C44 C45 1.526(6) . ? C45 C49 1.534(6) . ? C45 C46 1.534(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 O2 Al1 O1 94.17(11) . . ? O2 Al1 C102 110.71(18) . . ? O1 Al1 C102 104.7(2) . . ? O2 Al1 C101 108.5(2) . . ? O1 Al1 C101 115.49(17) . . ? C102 Al1 C101 120.2(3) . . ? N1 O1 Al2 110.35(18) . . ? N1 O1 Al1 107.71(17) . . ? Al2 O1 Al1 109.25(11) . . ? C1 N1 O1 111.6(3) . . ? N1 C1 C11 135.5(4) . . ? N1 C1 C15 116.3(3) . . ? C11 C1 C15 108.2(3) . . ? C1 C11 C18 112.7(4) . . ? C1 C11 C17 112.0(4) . . ? C18 C11 C17 107.9(5) . . ? C1 C11 C12 98.5(4) . . ? C18 C11 C12 109.5(5) . . ? C17 C11 C12 116.2(5) . . ? C13 C12 C16 98.5(5) . . ? C13 C12 C11 107.4(5) . . ? C16 C12 C11 101.8(4) . . ? C14 C13 C12 105.4(6) . . ? C13 C14 C15 103.0(6) . . ? C14 C15 C16 105.9(5) . . ? C14 C15 C1 106.8(4) . . ? C16 C15 C1 100.7(3) . . ? C14 C15 C19 111.8(5) . . ? C16 C15 C19 115.4(5) . . ? C1 C15 C19 115.2(4) . . ? C15 C16 C12 92.5(4) . . ? O1 Al2 C202 111.21(17) . . ? O1 Al2 C201 103.94(18) . . ? C202 Al2 C201 121.5(2) . . ? O1 Al2 N2 94.41(10) . . ? C202 Al2 N2 110.28(16) . . ? C201 Al2 N2 111.88(18) . . ? N2 O2 Al1 116.35(18) . . ? C2 N2 O2 113.7(2) . . ? C2 N2 Al2 135.8(2) . . ? O2 N2 Al2 110.35(17) . . ? N2 C2 C25 125.2(3) . . ? N2 C2 C21 126.6(3) . . ? C25 C2 C21 108.2(3) . . ? C28 C21 C2 115.0(3) . . ? C28 C21 C22 112.4(3) . . ? C2 C21 C22 99.9(3) . . ? C28 C21 C27 106.9(4) . . ? C2 C21 C27 110.9(3) . . ? C22 C21 C27 111.9(3) . . ? C26 C22 C21 102.9(3) . . ? C26 C22 C23 99.8(5) . . ? C21 C22 C23 109.7(4) . . ? C24 C23 C22 104.6(4) . . ? C23 C24 C25 104.8(5) . . ? C24 C25 C29 117.0(5) . . ? C24 C25 C2 105.0(3) . . ? C29 C25 C2 118.3(3) . . ? C24 C25 C26 101.8(4) . . ? C29 C25 C26 113.5(4) . . ? C2 C25 C26 98.5(3) . . ? C22 C26 C25 93.5(4) . . ? O4 Al3 O3 93.97(10) . . ? O4 Al3 C301 109.6(2) . . ? O3 Al3 C301 114.33(15) . . ? O4 Al3 C302 112.70(18) . . ? O3 Al3 C302 104.87(19) . . ? C301 Al3 C302 118.7(2) . . ? N3 O3 Al4 109.38(16) . . ? N3 O3 Al3 108.67(15) . . ? Al4 O3 Al3 110.71(11) . . ? C3 N3 O3 111.0(2) . . ? N3 C3 C31 134.2(3) . . ? N3 C3 C35 118.1(3) . . ? C31 C3 C35 107.7(3) . . ? C37 C31 C38 108.2(4) . . ? C37 C31 C3 114.6(3) . . ? C38 C31 C3 110.3(3) . . ? C37 C31 C32 113.7(3) . . ? C38 C31 C32 110.2(4) . . ? C3 C31 C32 99.6(3) . . ? C36 C32 C33 102.7(4) . . ? C36 C32 C31 102.5(3) . . ? C33 C32 C31 110.9(4) . . ? C32 C33 C34 101.9(4) . . ? C33 C34 C35 104.2(4) . . ? C39 C35 C3 114.4(4) . . ? C39 C35 C36 118.3(5) . . ? C3 C35 C36 99.1(3) . . ? C39 C35 C34 116.9(5) . . ? C3 C35 C34 104.6(4) . . ? C36 C35 C34 101.0(4) . . ? C32 C36 C35 94.7(4) . . ? O3 Al4 C402 104.20(17) . . ? O3 Al4 C401 109.88(18) . . ? C402 Al4 C401 121.4(3) . . ? O3 Al4 N4 94.27(9) . . ? C402 Al4 N4 106.5(2) . . ? C401 Al4 N4 116.51(16) . . ? N4 O4 Al3 116.61(16) . . ? C4 N4 O4 114.9(2) . . ? C4 N4 Al4 135.06(19) . . ? O4 N4 Al4 109.77(16) . . ? N4 C4 C45 125.0(3) . . ? N4 C4 C41 126.9(3) . . ? C45 C4 C41 108.1(3) . . ? C48 C41 C4 113.0(3) . . ? C48 C41 C47 109.1(4) . . ? C4 C41 C47 111.5(3) . . ? C48 C41 C42 110.2(3) . . ? C4 C41 C42 98.8(3) . . ? C47 C41 C42 114.1(3) . . ? C46 C42 C43 101.7(4) . . ? C46 C42 C41 102.4(3) . . ? C43 C42 C41 110.8(3) . . ? C44 C43 C42 101.7(3) . . ? C43 C44 C45 105.4(3) . . ? C4 C45 C44 105.9(3) . . ? C4 C45 C49 117.1(3) . . ? C44 C45 C49 116.5(4) . . ? C4 C45 C46 99.6(3) . . ? C44 C45 C46 100.5(3) . . ? C49 C45 C46 114.8(3) . . ? C42 C46 C45 94.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 O1 N1 85.99(18) . . . . ? C102 Al1 O1 N1 -161.3(2) . . . . ? C101 Al1 O1 N1 -26.8(3) . . . . ? O2 Al1 O1 Al2 -33.89(15) . . . . ? C102 Al1 O1 Al2 78.8(2) . . . . ? C101 Al1 O1 Al2 -146.7(2) . . . . ? Al2 O1 N1 C1 -121.9(2) . . . . ? Al1 O1 N1 C1 118.9(2) . . . . ? O1 N1 C1 C11 0.4(5) . . . . ? O1 N1 C1 C15 -178.9(3) . . . . ? N1 C1 C11 C18 -62.2(6) . . . . ? C15 C1 C11 C18 117.2(5) . . . . ? N1 C1 C11 C17 59.8(6) . . . . ? C15 C1 C11 C17 -120.8(5) . . . . ? N1 C1 C11 C12 -177.5(4) . . . . ? C15 C1 C11 C12 1.9(4) . . . . ? C1 C11 C12 C13 -68.8(5) . . . . ? C18 C11 C12 C13 173.4(5) . . . . ? C17 C11 C12 C13 50.8(6) . . . . ? C1 C11 C12 C16 34.1(5) . . . . ? C18 C11 C12 C16 -83.7(5) . . . . ? C17 C11 C12 C16 153.8(5) . . . . ? C16 C12 C13 C14 -37.9(7) . . . . ? C11 C12 C13 C14 67.4(7) . . . . ? C12 C13 C14 C15 4.8(8) . . . . ? C13 C14 C15 C16 32.4(7) . . . . ? C13 C14 C15 C1 -74.3(6) . . . . ? C13 C14 C15 C19 158.9(6) . . . . ? N1 C1 C15 C14 -109.1(5) . . . . ? C11 C1 C15 C14 71.4(5) . . . . ? N1 C1 C15 C16 140.6(4) . . . . ? C11 C1 C15 C16 -38.9(4) . . . . ? N1 C1 C15 C19 15.7(6) . . . . ? C11 C1 C15 C19 -163.8(5) . . . . ? C14 C15 C16 C12 -54.2(5) . . . . ? C1 C15 C16 C12 56.8(4) . . . . ? C19 C15 C16 C12 -178.4(5) . . . . ? C13 C12 C16 C15 53.3(5) . . . . ? C11 C12 C16 C15 -56.6(4) . . . . ? N1 O1 Al2 C202 16.0(2) . . . . ? Al1 O1 Al2 C202 134.22(17) . . . . ? N1 O1 Al2 C201 148.4(2) . . . . ? Al1 O1 Al2 C201 -93.4(2) . . . . ? N1 O1 Al2 N2 -97.78(18) . . . . ? Al1 O1 Al2 N2 20.46(15) . . . . ? O1 Al1 O2 N2 40.5(2) . . . . ? C102 Al1 O2 N2 -66.9(3) . . . . ? C101 Al1 O2 N2 159.2(3) . . . . ? Al1 O2 N2 C2 153.5(2) . . . . ? Al1 O2 N2 Al2 -30.3(3) . . . . ? O1 Al2 N2 C2 179.1(3) . . . . ? C202 Al2 N2 C2 64.6(4) . . . . ? C201 Al2 N2 C2 -73.9(4) . . . . ? O1 Al2 N2 O2 4.1(2) . . . . ? C202 Al2 N2 O2 -110.5(3) . . . . ? C201 Al2 N2 O2 111.0(3) . . . . ? O2 N2 C2 C25 177.2(3) . . . . ? Al2 N2 C2 C25 2.3(6) . . . . ? O2 N2 C2 C21 -2.9(5) . . . . ? Al2 N2 C2 C21 -177.8(3) . . . . ? N2 C2 C21 C28 57.4(5) . . . . ? C25 C2 C21 C28 -122.7(4) . . . . ? N2 C2 C21 C22 178.0(3) . . . . ? C25 C2 C21 C22 -2.1(4) . . . . ? N2 C2 C21 C27 -63.9(5) . . . . ? C25 C2 C21 C27 116.0(4) . . . . ? C28 C21 C22 C26 161.3(4) . . . . ? C2 C21 C22 C26 38.9(4) . . . . ? C27 C21 C22 C26 -78.4(5) . . . . ? C28 C21 C22 C23 55.8(5) . . . . ? C2 C21 C22 C23 -66.6(4) . . . . ? C27 C21 C22 C23 176.1(4) . . . . ? C26 C22 C23 C24 -39.8(5) . . . . ? C21 C22 C23 C24 67.7(5) . . . . ? C22 C23 C24 C25 4.4(5) . . . . ? C23 C24 C25 C29 154.8(4) . . . . ? C23 C24 C25 C2 -71.8(5) . . . . ? C23 C24 C25 C26 30.5(5) . . . . ? N2 C2 C25 C24 -107.9(4) . . . . ? C21 C2 C25 C24 72.1(4) . . . . ? N2 C2 C25 C29 24.8(6) . . . . ? C21 C2 C25 C29 -155.1(5) . . . . ? N2 C2 C25 C26 147.3(4) . . . . ? C21 C2 C25 C26 -32.6(4) . . . . ? C21 C22 C26 C25 -57.9(4) . . . . ? C23 C22 C26 C25 55.0(4) . . . . ? C24 C25 C26 C22 -53.7(4) . . . . ? C29 C25 C26 C22 179.7(4) . . . . ? C2 C25 C26 C22 53.7(4) . . . . ? O4 Al3 O3 N3 -88.13(17) . . . . ? C301 Al3 O3 N3 25.5(3) . . . . ? C302 Al3 O3 N3 157.1(2) . . . . ? O4 Al3 O3 Al4 32.02(13) . . . . ? C301 Al3 O3 Al4 145.6(2) . . . . ? C302 Al3 O3 Al4 -82.74(19) . . . . ? Al4 O3 N3 C3 122.6(2) . . . . ? Al3 O3 N3 C3 -116.4(2) . . . . ? O3 N3 C3 C31 0.6(5) . . . . ? O3 N3 C3 C35 178.3(3) . . . . ? N3 C3 C31 C37 52.8(6) . . . . ? C35 C3 C31 C37 -125.1(4) . . . . ? N3 C3 C31 C38 -69.6(5) . . . . ? C35 C3 C31 C38 112.5(4) . . . . ? N3 C3 C31 C32 174.5(4) . . . . ? C35 C3 C31 C32 -3.4(4) . . . . ? C37 C31 C32 C36 160.9(4) . . . . ? C38 C31 C32 C36 -77.4(4) . . . . ? C3 C31 C32 C36 38.5(4) . . . . ? C37 C31 C32 C33 51.8(5) . . . . ? C38 C31 C32 C33 173.5(4) . . . . ? C3 C31 C32 C33 -70.5(4) . . . . ? C36 C32 C33 C34 -37.5(5) . . . . ? C31 C32 C33 C34 71.4(5) . . . . ? C32 C33 C34 C35 2.6(6) . . . . ? N3 C3 C35 C39 23.1(7) . . . . ? C31 C3 C35 C39 -158.6(5) . . . . ? N3 C3 C35 C36 150.0(4) . . . . ? C31 C3 C35 C36 -31.8(5) . . . . ? N3 C3 C35 C34 -106.0(4) . . . . ? C31 C3 C35 C34 72.2(4) . . . . ? C33 C34 C35 C39 162.0(4) . . . . ? C33 C34 C35 C3 -70.4(5) . . . . ? C33 C34 C35 C36 32.2(5) . . . . ? C33 C32 C36 C35 56.8(5) . . . . ? C31 C32 C36 C35 -58.3(5) . . . . ? C39 C35 C36 C32 177.4(5) . . . . ? C3 C35 C36 C32 53.3(5) . . . . ? C34 C35 C36 C32 -53.6(5) . . . . ? N3 O3 Al4 C402 -150.5(2) . . . . ? Al3 O3 Al4 C402 89.8(2) . . . . ? N3 O3 Al4 C401 -18.9(2) . . . . ? Al3 O3 Al4 C401 -138.64(18) . . . . ? N3 O3 Al4 N4 101.28(16) . . . . ? Al3 O3 Al4 N4 -18.44(12) . . . . ? O3 Al3 O4 N4 -40.1(2) . . . . ? C301 Al3 O4 N4 -157.6(2) . . . . ? C302 Al3 O4 N4 67.9(3) . . . . ? Al3 O4 N4 C4 -144.0(2) . . . . ? Al3 O4 N4 Al4 31.2(2) . . . . ? O3 Al4 N4 C4 167.6(3) . . . . ? C402 Al4 N4 C4 61.5(3) . . . . ? C401 Al4 N4 C4 -77.6(3) . . . . ? O3 Al4 N4 O4 -6.25(18) . . . . ? C402 Al4 N4 O4 -112.4(2) . . . . ? C401 Al4 N4 O4 108.5(2) . . . . ? O4 N4 C4 C45 -177.8(3) . . . . ? Al4 N4 C4 C45 8.5(4) . . . . ? O4 N4 C4 C41 5.5(4) . . . . ? Al4 N4 C4 C41 -168.2(2) . . . . ? N4 C4 C41 C48 -67.3(5) . . . . ? C45 C4 C41 C48 115.6(4) . . . . ? N4 C4 C41 C47 56.0(4) . . . . ? C45 C4 C41 C47 -121.1(3) . . . . ? N4 C4 C41 C42 176.3(3) . . . . ? C45 C4 C41 C42 -0.8(3) . . . . ? C48 C41 C42 C46 -82.1(4) . . . . ? C4 C41 C42 C46 36.4(4) . . . . ? C47 C41 C42 C46 154.8(3) . . . . ? C48 C41 C42 C43 170.2(4) . . . . ? C4 C41 C42 C43 -71.3(4) . . . . ? C47 C41 C42 C43 47.0(5) . . . . ? C46 C42 C43 C44 -38.6(4) . . . . ? C41 C42 C43 C44 69.6(4) . . . . ? C42 C43 C44 C45 3.8(4) . . . . ? N4 C4 C45 C44 -107.3(4) . . . . ? C41 C4 C45 C44 69.8(3) . . . . ? N4 C4 C45 C49 24.5(5) . . . . ? C41 C4 C45 C49 -158.3(3) . . . . ? N4 C4 C45 C46 148.8(3) . . . . ? C41 C4 C45 C46 -34.0(4) . . . . ? C43 C44 C45 C4 -71.8(4) . . . . ? C43 C44 C45 C49 156.1(3) . . . . ? C43 C44 C45 C46 31.4(4) . . . . ? C43 C42 C46 C45 57.4(4) . . . . ? C41 C42 C46 C45 -57.2(4) . . . . ? C4 C45 C46 C42 54.7(3) . . . . ? C44 C45 C46 C42 -53.6(4) . . . . ? C49 C45 C46 C42 -179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 65.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.396 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.043