# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1855 data_VG9855 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H42 N6 Al4' _chemical_formula_weight 522.56 _chemical_melting_point ? _chemical_compound_source ? 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' '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 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 8.7173(5) _cell_length_b 16.8678(7) _cell_length_c 20.416(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3002.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.76 _cell_measurement_theta_max 24.08 _exptl_crystal_description prisms _exptl_crystal_colour Clear _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.613 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2182 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 6.68 _diffrn_reflns_theta_max 59.98 _reflns_number_total 2182 _reflns_number_observed 1479 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 221 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1223P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1961 _refine_ls_number_parameters 162 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_obs 0.0693 _refine_ls_wR_factor_all 0.2410 _refine_ls_wR_factor_obs 0.1729 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.272 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.4301(2) -0.12867(8) 0.13008(7) 0.0264(4) Uani 1 d . . Al2 Al 0.7934(2) -0.06720(9) 0.09458(8) 0.0300(4) Uani 1 d . . N1 N 0.3637(4) -0.0368(2) 0.0814(2) 0.0255(9) Uani 1 d . . C1 C 0.4163(5) 0.0290(3) 0.1187(2) 0.0247(10) Uani 1 d . . C2 C 0.5443(6) 0.0127(3) 0.1577(2) 0.0264(10) Uani 1 d . . C3 C 0.6000(6) 0.0705(3) 0.2010(3) 0.0335(12) Uani 1 d . . H3A H 0.6885(6) 0.0602(3) 0.2268(3) 0.040 Uiso 1 calc R . C4 C 0.5258(7) 0.1421(3) 0.2058(3) 0.0426(14) Uani 1 d . . H4A H 0.5632(7) 0.1809(3) 0.2355(3) 0.051 Uiso 1 calc R . C5 C 0.3974(7) 0.1588(3) 0.1684(3) 0.0407(13) Uani 1 d . . H5A H 0.3481(7) 0.2089(3) 0.1720(3) 0.049 Uiso 1 calc R . C6 C 0.3413(6) 0.1019(3) 0.1255(3) 0.0316(11) Uani 1 d . . H6A H 0.2516(6) 0.1125(3) 0.1005(3) 0.038 Uiso 1 calc R . N7 N 0.6119(5) -0.0648(2) 0.1517(2) 0.0263(9) Uani 1 d D . H7A H 0.6341(63) -0.0835(30) 0.1919(11) 0.027(14) Uiso 1 d D . C8 C 0.3048(7) -0.1334(3) 0.2102(3) 0.0389(13) Uani 1 d . . H8A H 0.2946(7) -0.0800(3) 0.2288(3) 0.058 Uiso 1 calc R . H8B H 0.3544(7) -0.1682(3) 0.2423(3) 0.058 Uiso 1 calc R . H8C H 0.2028(7) -0.1542(3) 0.1996(3) 0.058 Uiso 1 calc R . C9 C 0.4679(8) -0.2276(3) 0.0834(3) 0.049(2) Uani 1 d . . H9A H 0.5007(8) -0.2685(3) 0.1146(3) 0.074 Uiso 1 calc R . H9B H 0.5486(8) -0.2194(3) 0.0507(3) 0.074 Uiso 1 calc R . H9C H 0.3735(8) -0.2448(3) 0.0615(3) 0.074 Uiso 1 calc R . C10 C 0.9477(7) 0.0056(4) 0.1291(3) 0.0468(15) Uani 1 d . . H10A H 0.9049(7) 0.0593(4) 0.1311(3) 0.070 Uiso 1 calc R . H10B H 1.0378(7) 0.0054(4) 0.1004(3) 0.070 Uiso 1 calc R . H10C H 0.9779(7) -0.0113(4) 0.1732(3) 0.070 Uiso 1 calc R . C11 C 0.8608(8) -0.1773(4) 0.0874(3) 0.049(2) Uani 1 d . . H11A H 0.7770(8) -0.2097(4) 0.0698(3) 0.074 Uiso 1 calc R . H11B H 0.8896(8) -0.1971(4) 0.1308(3) 0.074 Uiso 1 calc R . H11C H 0.9495(8) -0.1804(4) 0.0580(3) 0.074 Uiso 1 calc R . C12 C 0.3034(5) -0.0296(3) 0.0217(2) 0.0251(10) Uani 1 d . . C13 C 0.2449(7) -0.1041(3) -0.0098(3) 0.0405(13) Uani 1 d . . H13A H 0.3214(7) -0.1238(3) -0.0410(3) 0.061 Uiso 1 d R . H13B H 0.1489(7) -0.0928(3) -0.0330(3) 0.061 Uiso 1 d R . H13C H 0.2265(7) -0.1444(3) 0.0239(3) 0.061 Uiso 1 d R . N14 N 0.2916(5) 0.0375(2) -0.0124(2) 0.0288(10) Uani 1 d D . H14A H 0.3281(62) 0.0803(20) 0.0088(24) 0.030(14) Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0252(7) 0.0237(7) 0.0305(7) -0.0001(6) 0.0028(6) -0.0002(6) Al2 0.0170(7) 0.0388(8) 0.0344(8) 0.0028(6) -0.0013(6) 0.0054(6) N1 0.019(2) 0.026(2) 0.031(2) -0.001(2) 0.000(2) -0.004(2) C1 0.021(2) 0.021(2) 0.032(2) 0.001(2) 0.006(2) 0.002(2) C2 0.021(2) 0.030(2) 0.028(2) 0.000(2) 0.002(2) -0.005(2) C3 0.029(3) 0.037(3) 0.034(3) -0.007(2) -0.004(2) -0.002(2) C4 0.044(3) 0.036(3) 0.048(3) -0.008(2) 0.000(3) -0.007(3) C5 0.043(3) 0.025(2) 0.055(3) -0.004(2) 0.006(3) 0.000(2) C6 0.026(3) 0.029(2) 0.040(3) 0.000(2) 0.003(2) 0.003(2) N7 0.023(2) 0.029(2) 0.028(2) -0.001(2) 0.000(2) 0.008(2) C8 0.039(3) 0.040(3) 0.037(3) 0.005(2) 0.011(2) -0.008(2) C9 0.055(4) 0.032(3) 0.061(4) -0.009(3) -0.001(3) 0.003(3) C10 0.023(3) 0.062(4) 0.056(4) 0.002(3) -0.010(3) -0.002(3) C11 0.044(4) 0.045(3) 0.058(4) 0.005(3) 0.007(3) 0.021(3) C12 0.013(2) 0.028(2) 0.034(3) -0.003(2) 0.002(2) -0.003(2) C13 0.043(3) 0.033(3) 0.045(3) -0.003(2) -0.016(3) -0.005(2) N14 0.024(2) 0.030(2) 0.032(2) 0.005(2) -0.003(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.929(4) . ? Al1 C9 1.950(6) . ? Al1 N7 1.967(4) . ? Al1 C8 1.970(5) . ? Al2 N14 1.901(4) 5_655 ? Al2 C11 1.954(6) . ? Al2 C10 1.954(6) . ? Al2 N7 1.966(4) . ? N1 C12 1.334(7) . ? N1 C1 1.423(6) . ? C1 C2 1.398(7) . ? C1 C6 1.400(7) . ? C2 C3 1.402(7) . ? C2 N7 1.439(6) . ? C3 C4 1.374(8) . ? C4 C5 1.384(9) . ? C5 C6 1.389(8) . ? C12 N14 1.333(6) . ? C12 C13 1.500(7) . ? N14 Al2 1.901(4) 5_655 ? 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 N1 Al1 C9 119.1(2) . . ? N1 Al1 N7 85.3(2) . . ? C9 Al1 N7 116.3(2) . . ? N1 Al1 C8 107.1(2) . . ? C9 Al1 C8 117.7(3) . . ? N7 Al1 C8 106.4(2) . . ? N14 Al2 C11 107.6(3) 5_655 . ? N14 Al2 C10 114.9(2) 5_655 . ? C11 Al2 C10 114.7(3) . . ? N14 Al2 N7 101.8(2) 5_655 . ? C11 Al2 N7 107.8(2) . . ? C10 Al2 N7 109.1(2) . . ? C12 N1 C1 123.1(4) . . ? C12 N1 Al1 131.5(3) . . ? C1 N1 Al1 104.7(3) . . ? C2 C1 C6 119.3(5) . . ? C2 C1 N1 114.1(4) . . ? C6 C1 N1 126.0(4) . . ? C1 C2 C3 119.9(5) . . ? C1 C2 N7 117.2(4) . . ? C3 C2 N7 122.9(5) . . ? C4 C3 C2 119.6(5) . . ? C3 C4 C5 121.3(5) . . ? C4 C5 C6 119.5(5) . . ? C5 C6 C1 120.3(5) . . ? C2 N7 Al2 113.5(3) . . ? C2 N7 Al1 100.8(3) . . ? Al2 N7 Al1 120.3(2) . . ? N14 C12 N1 125.8(4) . . ? N14 C12 C13 117.4(4) . . ? N1 C12 C13 116.7(4) . . ? C12 N14 Al2 135.6(4) . 5_655 ? _refine_diff_density_max 0.420 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.081 data_VG9618 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 N6 O6 Al6' _chemical_formula_weight 822.68 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)2(1)2(1) 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 12.1515(12) _cell_length_b 16.0543(12) _cell_length_c 22.3100(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4352.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.96 _cell_measurement_theta_max 26.44 _exptl_crystal_description Rhombs _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method ? _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.788 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.4549 _exptl_absorpt_correction_T_max 0.5412 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.30 _diffrn_reflns_number 4017 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 63.99 _reflns_number_total 4017 _reflns_number_observed 3483 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+2.7858P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _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 -0.06(6) _refine_ls_number_reflns 4004 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_obs 0.0545 _refine_ls_wR_factor_all 0.1433 _refine_ls_wR_factor_obs 0.1333 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.42798(15) -0.18953(11) 0.85789(8) 0.0289(4) Uani 1 d . . Al2 Al 0.37623(13) -0.03546(10) 0.93208(8) 0.0252(4) Uani 1 d . . Al3 Al 0.32714(13) 0.14308(11) 0.88021(8) 0.0285(4) Uani 1 d . . Al4 Al 0.53829(14) 0.10649(11) 0.95481(8) 0.0291(4) Uani 1 d . . Al5 Al 0.75507(14) 0.01480(10) 0.98760(8) 0.0287(4) Uani 1 d . . Al6 Al 0.60697(13) -0.04499(11) 0.87886(8) 0.0274(4) Uani 1 d . . O1 O 0.4761(3) -0.0927(2) 0.8903(2) 0.0283(8) Uani 1 d . . O2 O 0.2562(3) -0.0494(3) 0.8876(2) 0.0316(9) Uani 1 d . . O3 O 0.4172(3) 0.0700(2) 0.9194(2) 0.0276(8) Uani 1 d . . O4 O 0.5773(3) 0.1898(3) 0.9064(2) 0.0367(10) Uani 1 d . . O5 O 0.6312(3) 0.0223(2) 0.9417(2) 0.0296(8) Uani 1 d . . O6 O 0.7073(4) -0.1241(3) 0.8920(2) 0.0383(11) Uani 1 d . . C1 C 0.2213(5) -0.0933(4) 0.8432(3) 0.0274(12) Uani 1 d . . N2 N 0.2786(4) -0.1599(3) 0.8242(2) 0.0312(11) Uani 1 d . . C3 C 0.2296(6) -0.2098(5) 0.7800(3) 0.0400(15) Uani 1 d . . N4 N 0.1392(5) -0.1908(4) 0.7509(3) 0.0419(13) Uani 1 d . . C5 C 0.0856(5) -0.1207(5) 0.7666(3) 0.0393(15) Uani 1 d . . C6 C 0.1204(5) -0.0694(4) 0.8144(3) 0.0333(13) Uani 1 d . . C7 C 0.0593(5) -0.0005(4) 0.8320(3) 0.0391(14) Uani 1 d . . H7A H 0.0822(5) 0.0323(4) 0.8652(3) 0.047 Uiso 1 calc R . C8 C -0.0354(6) 0.0200(5) 0.8008(4) 0.053(2) Uani 1 d . . H8A H -0.0782(6) 0.0665(5) 0.8131(4) 0.063 Uiso 1 calc R . C9 C -0.0683(6) -0.0268(6) 0.7517(4) 0.056(2) Uani 1 d . . H9A H -0.1314(6) -0.0106(6) 0.7295(4) 0.067 Uiso 1 calc R . C10 C -0.0102(6) -0.0967(6) 0.7350(4) 0.053(2) Uani 1 d . . H10A H -0.0347(6) -0.1291(6) 0.7019(4) 0.064 Uiso 1 calc R . C11 C 0.5261(6) -0.2158(5) 0.7906(4) 0.049(2) Uani 1 d . . H11A H 0.5293(6) -0.1682(5) 0.7632(4) 0.073 Uiso 1 calc R . H11B H 0.4978(6) -0.2646(5) 0.7691(4) 0.073 Uiso 1 calc R . H11C H 0.6000(6) -0.2279(5) 0.8058(4) 0.073 Uiso 1 calc R . C12 C 0.4015(8) -0.2698(5) 0.9214(4) 0.060(2) Uani 1 d . . H12A H 0.3507(8) -0.2458(5) 0.9508(4) 0.090 Uiso 1 calc R . H12B H 0.4712(8) -0.2836(5) 0.9410(4) 0.090 Uiso 1 calc R . H12C H 0.3691(8) -0.3204(5) 0.9043(4) 0.090 Uiso 1 calc R . C13 C 0.3549(6) -0.0651(5) 1.0154(3) 0.047(2) Uani 1 d . . H13A H 0.4236(6) -0.0562(5) 1.0376(3) 0.070 Uiso 1 calc R . H13B H 0.3337(6) -0.1239(5) 1.0182(3) 0.070 Uiso 1 calc R . H13C H 0.2967(6) -0.0304(5) 1.0327(3) 0.070 Uiso 1 calc R . C14 C 0.2839(6) -0.2909(5) 0.7652(4) 0.054(2) Uani 1 d . . H14A H 0.2330(6) -0.3260(5) 0.7442(4) 0.081 Uiso 1 d R . H14B H 0.3074(6) -0.3179(5) 0.8014(4) 0.081 Uiso 1 d R . H14C H 0.3476(6) -0.2811(5) 0.7408(4) 0.081 Uiso 1 d R . C21 C 0.5254(5) 0.2535(4) 0.8863(3) 0.0298(12) Uani 1 d . . N22 N 0.4160(4) 0.2503(3) 0.8762(2) 0.0295(10) Uani 1 d . . C23 C 0.3665(5) 0.3221(4) 0.8543(3) 0.0356(13) Uani 1 d . . N24 N 0.4142(5) 0.3928(4) 0.8443(3) 0.0398(12) Uani 1 d . . C25 C 0.5258(6) 0.3968(4) 0.8532(3) 0.0353(13) Uani 1 d . . C26 C 0.5852(5) 0.3279(4) 0.8742(3) 0.0329(13) Uani 1 d . . C27 C 0.7004(6) 0.3343(4) 0.8826(3) 0.0400(15) Uani 1 d . . H27A H 0.7410(6) 0.2885(4) 0.8980(3) 0.048 Uiso 1 calc R . C28 C 0.7526(6) 0.4068(5) 0.8685(3) 0.047(2) Uani 1 d . . H28A H 0.8300(6) 0.4108(5) 0.8734(3) 0.056 Uiso 1 calc R . C29 C 0.6935(7) 0.4756(5) 0.8467(3) 0.048(2) Uani 1 d . . H29A H 0.7315(7) 0.5255(5) 0.8371(3) 0.057 Uiso 1 calc R . C30 C 0.5811(7) 0.4718(5) 0.8393(3) 0.046(2) Uani 1 d . . H30A H 0.5414(7) 0.5187(5) 0.8249(3) 0.055 Uiso 1 calc R . C31 C 0.3144(6) 0.1105(5) 0.7957(3) 0.0425(15) Uani 1 d . . H31A H 0.3880(6) 0.1065(5) 0.7780(3) 0.064 Uiso 1 calc R . H31B H 0.2713(6) 0.1523(5) 0.7740(3) 0.064 Uiso 1 calc R . H31C H 0.2777(6) 0.0563(5) 0.7929(3) 0.064 Uiso 1 calc R . C32 C 0.2016(5) 0.1589(4) 0.9344(4) 0.043(2) Uani 1 d . . H32A H 0.2285(5) 0.1750(4) 0.9742(4) 0.064 Uiso 1 calc R . H32B H 0.1601(5) 0.1068(4) 0.9376(4) 0.064 Uiso 1 calc R . H32C H 0.1536(5) 0.2028(4) 0.9186(4) 0.064 Uiso 1 calc R . C33 C 0.5184(6) 0.1440(5) 1.0360(3) 0.044(2) Uani 1 d . . H33A H 0.5891(6) 0.1630(5) 1.0522(3) 0.067 Uiso 1 calc R . H33B H 0.4905(6) 0.0980(5) 1.0606(3) 0.067 Uiso 1 calc R . H33C H 0.4656(6) 0.1901(5) 1.0367(3) 0.067 Uiso 1 calc R . C34 C 0.2458(6) 0.3171(5) 0.8403(4) 0.049(2) Uani 1 d . . H34A H 0.2361(6) 0.2961(5) 0.8003(4) 0.074 Uiso 1 d R . H34B H 0.2132(6) 0.3713(5) 0.8436(4) 0.074 Uiso 1 d R . H34C H 0.2100(6) 0.2808(5) 0.8684(4) 0.074 Uiso 1 d R . C41 C 0.8080(5) -0.1296(4) 0.9091(3) 0.0306(12) Uani 1 d . . N42 N 0.8488(4) -0.0735(3) 0.9488(2) 0.0303(11) Uani 1 d . . C43 C 0.9580(5) -0.0839(4) 0.9672(3) 0.0304(13) Uani 1 d . . N44 N 1.0232(4) -0.1428(3) 0.9496(2) 0.0343(11) Uani 1 d . . C45 C 0.9828(5) -0.2018(4) 0.9103(3) 0.0312(12) Uani 1 d . . C46 C 0.8731(5) -0.1963(4) 0.8881(3) 0.0310(12) Uani 1 d . . C47 C 0.8375(5) -0.2566(4) 0.8467(3) 0.0402(14) Uani 1 d . . H47A H 0.7649(5) -0.2536(4) 0.8311(3) 0.048 Uiso 1 calc R . C48 C 0.9046(6) -0.3186(5) 0.8289(4) 0.046(2) Uani 1 d . . H48A H 0.8788(6) -0.3588(5) 0.8009(4) 0.056 Uiso 1 calc R . C49 C 1.0126(6) -0.3243(4) 0.8512(3) 0.044(2) Uani 1 d . . H49A H 1.0591(6) -0.3685(4) 0.8386(3) 0.053 Uiso 1 calc R . C50 C 1.0510(5) -0.2661(4) 0.8913(3) 0.0377(14) Uani 1 d . . H50A H 1.1242(5) -0.2699(4) 0.9060(3) 0.045 Uiso 1 calc R . C51 C 0.8253(6) 0.1244(4) 0.9779(3) 0.0396(15) Uani 1 d . . H51A H 0.8379(6) 0.1353(4) 0.9352(3) 0.059 Uiso 1 calc R . H51B H 0.8959(6) 0.1250(4) 0.9992(3) 0.059 Uiso 1 calc R . H51C H 0.7772(6) 0.1677(4) 0.9944(3) 0.059 Uiso 1 calc R . C52 C 0.7166(5) -0.0294(4) 1.0666(3) 0.0408(15) Uani 1 d . . H52A H 0.6827(5) -0.0844(4) 1.0621(3) 0.061 Uiso 1 calc R . H52B H 0.6647(5) 0.0084(4) 1.0863(3) 0.061 Uiso 1 calc R . H52C H 0.7833(5) -0.0343(4) 1.0911(3) 0.061 Uiso 1 calc R . C53 C 0.6273(6) 0.0106(4) 0.8031(3) 0.0412(15) Uani 1 d . . H53A H 0.7014(6) 0.0346(4) 0.8013(3) 0.062 Uiso 1 calc R . H53B H 0.5726(6) 0.0551(4) 0.7989(3) 0.062 Uiso 1 calc R . H53C H 0.6181(6) -0.0296(4) 0.7704(3) 0.062 Uiso 1 calc R . C54 C 1.0016(5) -0.0227(5) 1.0113(3) 0.0424(15) Uani 1 d . . H54A H 1.0330(5) 0.0240(5) 0.9905(3) 0.064 Uiso 1 d R . H54B H 1.0566(5) -0.0486(5) 1.0359(3) 0.064 Uiso 1 d R . H54C H 0.9430(5) -0.0040(5) 1.0368(3) 0.064 Uiso 1 d R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0241(8) 0.0249(7) 0.0378(9) -0.0006(7) -0.0025(7) 0.0006(7) Al2 0.0183(7) 0.0266(8) 0.0306(8) -0.0015(6) -0.0016(6) -0.0017(6) Al3 0.0184(7) 0.0301(8) 0.0371(9) -0.0014(7) -0.0028(7) 0.0016(7) Al4 0.0208(8) 0.0261(8) 0.0404(9) -0.0029(7) -0.0050(7) 0.0006(7) Al5 0.0201(7) 0.0288(8) 0.0373(9) -0.0007(7) -0.0051(7) -0.0007(7) Al6 0.0172(7) 0.0289(8) 0.0362(9) 0.0000(7) -0.0019(6) 0.0004(6) O1 0.021(2) 0.029(2) 0.035(2) 0.000(2) 0.001(2) 0.002(2) O2 0.017(2) 0.037(2) 0.040(2) -0.003(2) -0.005(2) -0.003(2) O3 0.019(2) 0.025(2) 0.039(2) -0.002(2) -0.003(2) -0.002(2) O4 0.020(2) 0.029(2) 0.062(3) 0.005(2) -0.006(2) 0.005(2) O5 0.019(2) 0.029(2) 0.041(2) -0.006(2) -0.004(2) 0.003(2) O6 0.024(2) 0.037(2) 0.054(3) -0.006(2) -0.010(2) 0.007(2) C1 0.019(2) 0.029(3) 0.035(3) 0.001(2) 0.002(2) -0.005(2) N2 0.025(2) 0.035(3) 0.034(2) -0.003(2) -0.002(2) -0.001(2) C3 0.033(3) 0.047(4) 0.040(3) -0.010(3) 0.004(3) -0.010(3) N4 0.028(3) 0.054(3) 0.043(3) -0.010(3) -0.006(2) -0.009(3) C5 0.023(3) 0.058(4) 0.037(3) -0.004(3) -0.002(3) -0.006(3) C6 0.020(3) 0.043(3) 0.037(3) -0.004(3) -0.008(2) -0.008(3) C7 0.022(3) 0.047(4) 0.048(4) -0.001(3) -0.005(3) 0.004(3) C8 0.027(3) 0.056(4) 0.076(5) -0.001(4) -0.009(4) 0.006(3) C9 0.027(3) 0.076(5) 0.064(5) 0.003(4) -0.019(3) 0.003(4) C10 0.033(4) 0.075(5) 0.052(4) -0.005(4) -0.019(3) 0.002(4) C11 0.029(3) 0.050(4) 0.067(5) -0.018(4) 0.001(3) -0.004(3) C12 0.074(6) 0.040(4) 0.065(5) 0.013(4) -0.018(5) -0.015(4) C13 0.046(4) 0.054(4) 0.040(3) 0.001(3) 0.002(3) -0.004(3) C14 0.037(4) 0.049(4) 0.076(5) -0.021(4) -0.004(4) -0.011(3) C21 0.023(3) 0.031(3) 0.035(3) -0.003(2) 0.000(2) -0.001(2) N22 0.023(2) 0.031(2) 0.034(2) 0.004(2) 0.002(2) 0.001(2) C23 0.027(3) 0.037(3) 0.043(3) 0.004(3) 0.003(3) 0.007(3) N24 0.036(3) 0.035(3) 0.049(3) 0.009(2) 0.001(2) 0.003(2) C25 0.041(3) 0.029(3) 0.036(3) 0.001(3) 0.004(3) 0.001(3) C26 0.033(3) 0.034(3) 0.031(3) 0.000(2) 0.001(2) -0.007(3) C27 0.030(3) 0.046(4) 0.044(3) 0.004(3) -0.003(3) -0.011(3) C28 0.041(4) 0.057(4) 0.042(4) -0.001(3) -0.004(3) -0.021(4) C29 0.052(4) 0.045(4) 0.047(4) 0.008(3) 0.003(3) -0.019(4) C30 0.050(4) 0.043(4) 0.044(4) 0.010(3) 0.000(3) -0.010(3) C31 0.040(3) 0.049(4) 0.038(3) 0.002(3) -0.006(3) -0.008(3) C32 0.025(3) 0.032(3) 0.071(5) 0.001(3) 0.011(3) 0.006(3) C33 0.038(3) 0.043(3) 0.052(4) -0.016(3) -0.005(3) 0.004(3) C34 0.026(3) 0.043(4) 0.079(5) 0.022(4) 0.004(3) 0.009(3) C41 0.018(3) 0.033(3) 0.040(3) 0.004(3) -0.005(2) -0.001(2) N42 0.020(2) 0.032(2) 0.039(3) 0.002(2) -0.002(2) 0.000(2) C43 0.016(2) 0.032(3) 0.043(3) 0.003(2) 0.000(2) -0.001(2) N44 0.020(2) 0.036(3) 0.047(3) 0.006(2) -0.003(2) 0.000(2) C45 0.019(3) 0.039(3) 0.036(3) 0.009(2) 0.001(2) 0.000(2) C46 0.024(3) 0.031(3) 0.038(3) 0.003(2) 0.000(2) 0.004(2) C47 0.028(3) 0.042(3) 0.051(4) -0.001(3) -0.005(3) 0.005(3) C48 0.041(4) 0.044(4) 0.054(4) -0.010(3) -0.007(3) 0.013(3) C49 0.035(3) 0.040(3) 0.057(4) 0.000(3) 0.009(3) 0.014(3) C50 0.023(3) 0.043(3) 0.047(4) 0.008(3) 0.001(3) 0.007(3) C51 0.036(3) 0.030(3) 0.053(4) 0.000(3) -0.009(3) -0.010(3) C52 0.030(3) 0.045(4) 0.047(4) 0.001(3) 0.000(3) 0.002(3) C53 0.033(3) 0.042(3) 0.048(4) 0.005(3) 0.004(3) -0.003(3) C54 0.023(3) 0.049(4) 0.054(4) -0.007(3) -0.008(3) 0.001(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 O1 1.811(4) . ? Al1 C12 1.942(8) . ? Al1 C11 1.963(8) . ? Al1 N2 2.021(5) . ? Al2 O2 1.779(4) . ? Al2 O1 1.785(4) . ? Al2 O3 1.788(4) . ? Al2 C13 1.937(7) . ? Al3 O3 1.827(4) . ? Al3 C31 1.963(7) . ? Al3 C32 1.964(7) . ? Al3 N22 2.034(5) . ? Al4 O3 1.770(4) . ? Al4 O4 1.783(5) . ? Al4 O5 1.785(4) . ? Al4 C33 1.925(7) . ? Al5 O5 1.825(4) . ? Al5 C52 1.957(7) . ? Al5 C51 1.968(6) . ? Al5 N42 2.015(5) . ? Al6 O1 1.784(4) . ? Al6 O6 1.785(5) . ? Al6 O5 1.794(4) . ? Al6 C53 1.928(7) . ? O2 C1 1.287(7) . ? O4 C21 1.283(8) . ? O6 C41 1.286(7) . ? C1 N2 1.345(8) . ? C1 C6 1.436(8) . ? N2 C3 1.402(8) . ? C3 N4 1.312(9) . ? C3 C14 1.496(11) . ? N4 C5 1.347(10) . ? C5 C6 1.412(9) . ? C5 C10 1.414(9) . ? C6 C7 1.390(10) . ? C7 C8 1.384(10) . ? C8 C9 1.387(12) . ? C9 C10 1.377(12) . ? C21 N22 1.349(8) . ? C21 C26 1.425(8) . ? N22 C23 1.389(8) . ? C23 N24 1.295(9) . ? C23 C34 1.502(9) . ? N24 C25 1.372(9) . ? C25 C26 1.400(9) . ? C25 C30 1.412(9) . ? C26 C27 1.417(9) . ? C27 C28 1.362(10) . ? C28 C29 1.404(11) . ? C29 C30 1.377(11) . ? C41 N42 1.356(8) . ? C41 C46 1.411(9) . ? N42 C43 1.399(7) . ? C43 N44 1.294(8) . ? C43 C54 1.488(9) . ? N44 C45 1.381(9) . ? C45 C50 1.392(9) . ? C45 C46 1.424(8) . ? C46 C47 1.405(9) . ? C47 C48 1.347(10) . ? C48 C49 1.406(10) . ? C49 C50 1.374(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C12 109.4(3) . . ? O1 Al1 C11 107.1(3) . . ? C12 Al1 C11 121.1(4) . . ? O1 Al1 N2 103.7(2) . . ? C12 Al1 N2 106.2(3) . . ? C11 Al1 N2 108.1(3) . . ? O2 Al2 O1 101.6(2) . . ? O2 Al2 O3 105.0(2) . . ? O1 Al2 O3 102.5(2) . . ? O2 Al2 C13 113.3(3) . . ? O1 Al2 C13 117.7(3) . . ? O3 Al2 C13 115.0(3) . . ? O3 Al3 C31 109.6(3) . . ? O3 Al3 C32 104.7(3) . . ? C31 Al3 C32 124.4(3) . . ? O3 Al3 N22 104.3(2) . . ? C31 Al3 N22 103.0(3) . . ? C32 Al3 N22 109.3(3) . . ? O3 Al4 O4 101.5(2) . . ? O3 Al4 O5 101.7(2) . . ? O4 Al4 O5 107.4(2) . . ? O3 Al4 C33 114.8(3) . . ? O4 Al4 C33 111.7(3) . . ? O5 Al4 C33 118.1(3) . . ? O5 Al5 C52 109.5(2) . . ? O5 Al5 C51 103.7(3) . . ? C52 Al5 C51 121.8(3) . . ? O5 Al5 N42 105.8(2) . . ? C52 Al5 N42 105.5(3) . . ? C51 Al5 N42 109.7(3) . . ? O1 Al6 O6 106.2(2) . . ? O1 Al6 O5 107.1(2) . . ? O6 Al6 O5 100.9(2) . . ? O1 Al6 C53 116.0(3) . . ? O6 Al6 C53 112.7(3) . . ? O5 Al6 C53 112.7(3) . . ? Al6 O1 Al2 117.3(2) . . ? Al6 O1 Al1 126.8(2) . . ? Al2 O1 Al1 115.5(2) . . ? C1 O2 Al2 140.2(4) . . ? Al4 O3 Al2 118.3(2) . . ? Al4 O3 Al3 119.9(2) . . ? Al2 O3 Al3 121.2(2) . . ? C21 O4 Al4 132.7(4) . . ? Al4 O5 Al6 118.7(2) . . ? Al4 O5 Al5 118.7(2) . . ? Al6 O5 Al5 122.3(2) . . ? C41 O6 Al6 138.4(5) . . ? O2 C1 N2 120.5(5) . . ? O2 C1 C6 118.7(5) . . ? N2 C1 C6 120.8(5) . . ? C1 N2 C3 117.1(5) . . ? C1 N2 Al1 122.3(4) . . ? C3 N2 Al1 120.6(4) . . ? N4 C3 N2 124.8(7) . . ? N4 C3 C14 117.5(6) . . ? N2 C3 C14 117.7(6) . . ? C3 N4 C5 118.1(6) . . ? N4 C5 C6 122.5(6) . . ? N4 C5 C10 119.8(7) . . ? C6 C5 C10 117.7(7) . . ? C7 C6 C5 121.2(6) . . ? C7 C6 C1 122.8(6) . . ? C5 C6 C1 116.0(6) . . ? C8 C7 C6 119.4(7) . . ? C7 C8 C9 120.5(8) . . ? C10 C9 C8 120.5(7) . . ? C9 C10 C5 120.6(7) . . ? O4 C21 N22 120.8(6) . . ? O4 C21 C26 119.0(5) . . ? N22 C21 C26 120.2(6) . . ? C21 N22 C23 117.0(5) . . ? C21 N22 Al3 123.3(4) . . ? C23 N22 Al3 119.2(4) . . ? N24 C23 N22 126.5(6) . . ? N24 C23 C34 116.6(6) . . ? N22 C23 C34 116.8(6) . . ? C23 N24 C25 117.3(6) . . ? N24 C25 C26 121.3(6) . . ? N24 C25 C30 118.6(6) . . ? C26 C25 C30 120.1(6) . . ? C25 C26 C27 119.7(6) . . ? C25 C26 C21 117.6(6) . . ? C27 C26 C21 122.6(6) . . ? C28 C27 C26 119.4(7) . . ? C27 C28 C29 121.0(7) . . ? C30 C29 C28 120.9(7) . . ? C29 C30 C25 118.9(7) . . ? O6 C41 N42 119.8(6) . . ? O6 C41 C46 119.1(6) . . ? N42 C41 C46 121.0(5) . . ? C41 N42 C43 117.4(5) . . ? C41 N42 Al5 122.7(4) . . ? C43 N42 Al5 119.6(4) . . ? N44 C43 N42 125.3(6) . . ? N44 C43 C54 117.8(5) . . ? N42 C43 C54 116.9(5) . . ? C43 N44 C45 118.4(5) . . ? N44 C45 C50 119.4(5) . . ? N44 C45 C46 120.8(6) . . ? C50 C45 C46 119.8(6) . . ? C47 C46 C41 124.6(6) . . ? C47 C46 C45 118.3(6) . . ? C41 C46 C45 117.1(6) . . ? C48 C47 C46 121.2(6) . . ? C47 C48 C49 120.5(7) . . ? C50 C49 C48 120.3(6) . . ? C49 C50 C45 120.0(6) . . ? _refine_diff_density_max 0.324 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.069