# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Dominic S. Wright' 'Carmen Soria Alvarez' 'Felipe Garcia' 'Alexander Hopkins' 'Simon M. Humphrey' 'Richard A. Kowenicki' 'Richard A. Layfield' 'M. McPartlin' 'Robert Raja' 'Michael C. Rogers' 'Anthony Woods' _publ_contact_author_name 'Dominic S. Wright' _publ_contact_author_address ; Chemistry Cambridge University (U.K.) Lensfield Road Cambridge Cambridgeshire CB2 1EW UNITED KINGDOM ; _publ_contact_author_email DSW1000@CUS.CAM.AC.UK _publ_section_title ; A Simple Route to Heterometallic Transition Metal/Aluminium(III) Complexes via Transfer of the [MeAl(2-py)3]- anion (2-py== 2-pyridyl) ; data_dw0426squeeze _database_code_depnum_ccdc_archive 'CCDC 249604' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Al2 Fe N6' _chemical_formula_sum 'C32 H30 Al2 Fe N6' _chemical_formula_weight 608.43 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 10.2291(5) _cell_length_b 10.2291(5) _cell_length_c 33.6643(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3050.5(3) _cell_formula_units_Z 3 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16365 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 20.39 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 5072 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 20.39 _reflns_number_total 670 _reflns_number_gt 620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0655P)^2^+7.3593P] 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_number_reflns 670 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.0000 1.0000 0.0298(5) Uani 1 6 d S . . Al1 Al 1.0000 0.0000 1.09909(5) 0.0352(6) Uani 1 3 d S . . N16 N 1.1894(3) 0.0505(3) 1.03252(8) 0.0363(9) Uani 1 1 d . . . C11 C 1.1937(4) 0.0565(3) 1.07315(9) 0.0301(10) Uani 1 1 d . . . C12 C 1.3279(4) 0.0965(4) 1.09277(12) 0.0426(10) Uani 1 1 d . . . H12 H 1.323(4) 0.090(4) 1.1217(12) 0.051(11) Uiso 1 1 d . . . C13 C 1.4578(5) 0.1278(4) 1.07301(12) 0.0449(11) Uani 1 1 d . . . H13 H 1.554(5) 0.152(4) 1.0869(10) 0.050(10) Uiso 1 1 d . . . C14 C 1.4524(4) 0.1207(4) 1.03196(13) 0.0402(11) Uani 1 1 d . . . H14 H 1.533(5) 0.146(4) 1.0168(11) 0.043(11) Uiso 1 1 d . . . C15 C 1.3197(4) 0.0834(4) 1.01283(12) 0.0371(10) Uani 1 1 d . . . H15 H 1.317(4) 0.079(4) 0.9829(10) 0.036(9) Uiso 1 1 d . . . C1 C 1.0000 0.0000 1.1578(2) 0.061(2) Uani 1 3 d S . . H1 H 1.032(6) -0.069(5) 1.1687(13) 0.088(15) Uiso 1 1 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 Fe1 0.0288(6) 0.0288(6) 0.0317(8) 0.000 0.000 0.0144(3) Al1 0.0360(8) 0.0360(8) 0.0338(11) 0.000 0.000 0.0180(4) N16 0.034(2) 0.0305(18) 0.044(2) 0.0019(13) 0.0000(15) 0.0159(14) C11 0.028(2) 0.025(2) 0.036(2) -0.0024(15) -0.0052(16) 0.0120(16) C12 0.040(3) 0.040(2) 0.043(2) -0.0008(18) -0.004(2) 0.0168(19) C13 0.035(3) 0.040(2) 0.058(3) -0.0035(19) -0.010(2) 0.0171(19) C14 0.024(2) 0.033(2) 0.062(3) -0.0009(19) 0.004(2) 0.0130(18) C15 0.033(3) 0.030(2) 0.046(2) -0.0006(17) 0.004(2) 0.0135(17) C1 0.070(3) 0.070(3) 0.043(5) 0.000 0.000 0.0349(17) _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 Fe1 N16 2.054(3) 10_757 ? Fe1 N16 2.054(3) . ? Fe1 N16 2.054(3) 11_667 ? Fe1 N16 2.054(3) 2_645 ? Fe1 N16 2.054(3) 12_547 ? Fe1 N16 2.054(3) 3_765 ? Al1 C11 1.969(3) 3_765 ? Al1 C11 1.969(3) . ? Al1 C11 1.969(3) 2_645 ? Al1 C1 1.978(7) . ? N16 C11 1.369(4) . ? N16 C15 1.371(4) . ? C11 C12 1.388(5) . ? C12 C13 1.372(5) . ? C13 C14 1.383(6) . ? C14 C15 1.373(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 N16 Fe1 N16 180.000(1) 10_757 . ? N16 Fe1 N16 94.24(11) 10_757 11_667 ? N16 Fe1 N16 85.76(11) . 11_667 ? N16 Fe1 N16 85.76(11) 10_757 2_645 ? N16 Fe1 N16 94.24(11) . 2_645 ? N16 Fe1 N16 180.00(13) 11_667 2_645 ? N16 Fe1 N16 94.24(11) 10_757 12_547 ? N16 Fe1 N16 85.76(11) . 12_547 ? N16 Fe1 N16 94.24(11) 11_667 12_547 ? N16 Fe1 N16 85.76(11) 2_645 12_547 ? N16 Fe1 N16 85.76(11) 10_757 3_765 ? N16 Fe1 N16 94.24(11) . 3_765 ? N16 Fe1 N16 85.76(11) 11_667 3_765 ? N16 Fe1 N16 94.24(11) 2_645 3_765 ? N16 Fe1 N16 180.00(14) 12_547 3_765 ? C11 Al1 C11 101.83(12) 3_765 . ? C11 Al1 C11 101.83(12) 3_765 2_645 ? C11 Al1 C11 101.83(13) . 2_645 ? C11 Al1 C1 116.32(10) 3_765 . ? C11 Al1 C1 116.32(10) . . ? C11 Al1 C1 116.32(10) 2_645 . ? C11 N16 C15 117.8(3) . . ? C11 N16 Fe1 123.3(2) . . ? C15 N16 Fe1 118.9(2) . . ? N16 C11 C12 119.6(3) . . ? N16 C11 Al1 115.2(2) . . ? C12 C11 Al1 125.3(3) . . ? C13 C12 C11 122.5(4) . . ? C12 C13 C14 117.6(4) . . ? C15 C14 C13 119.4(4) . . ? N16 C15 C14 123.1(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.246 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.053 data_mw0429 _database_code_depnum_ccdc_archive 'CCDC 249605' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Al2 Mn N6 O' _chemical_formula_weight 679.62 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 9.2658(19) _cell_length_b 24.167(5) _cell_length_c 15.877(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.97(3) _cell_angle_gamma 90.00 _cell_volume 3553.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13966 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.488 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 9511 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4469 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.1132P)^2^+11.4513P] 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 0.48(3) _refine_ls_number_reflns 4469 _refine_ls_number_parameters 428 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1786 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.011 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 Mn1 Mn 0.71062(11) 0.58662(4) -0.12975(7) 0.0217(3) Uani 1 1 d D A 1 Al1 Al 0.46471(18) 0.48317(7) -0.19112(12) 0.0220(5) Uani 1 1 d D A 1 C1 C 0.3224(7) 0.4249(3) -0.2231(5) 0.0404(18) Uani 1 1 d D A 1 H1A H 0.3493 0.4079 -0.2749 0.061 Uiso 1 1 calc R A 1 H1B H 0.2283 0.4412 -0.2305 0.061 Uiso 1 1 calc R A 1 H1C H 0.3206 0.3974 -0.1794 0.061 Uiso 1 1 calc R A 1 C11 C 0.6523(5) 0.4531(2) -0.1425(4) 0.0276(16) Uani 1 1 d D A 1 C12 C 0.6893(7) 0.3976(3) -0.1317(5) 0.0287(15) Uani 1 1 d . A 1 H12 H 0.6239 0.3708 -0.1504 0.034 Uiso 1 1 calc R A 1 C13 C 0.8169(8) 0.3808(3) -0.0950(5) 0.0355(19) Uani 1 1 d U A 1 H13 H 0.8378 0.3435 -0.0880 0.043 Uiso 1 1 calc R A 1 C14 C 0.9160(7) 0.4216(3) -0.0681(5) 0.0373(18) Uani 1 1 d . A 1 H14 H 1.0040 0.4120 -0.0421 0.045 Uiso 1 1 calc R A 1 C15 C 0.8794(8) 0.4754(3) -0.0811(5) 0.0352(17) Uani 1 1 d . A 1 H15 H 0.9465 0.5023 -0.0644 0.042 Uiso 1 1 calc R A 1 N1 N 0.7523(5) 0.49293(14) -0.1165(4) 0.0234(12) Uani 1 1 d D A 1 C21 C 0.3970(6) 0.5347(2) -0.1010(3) 0.0226(14) Uani 1 1 d D A 1 C22 C 0.2661(7) 0.5280(3) -0.0625(5) 0.0289(16) Uani 1 1 d . A 1 H22 H 0.2062 0.4988 -0.0789 0.035 Uiso 1 1 calc R A 1 C23 C 0.2223(7) 0.5639(3) 0.0002(4) 0.0271(15) Uani 1 1 d . A 1 H23 H 0.1346 0.5588 0.0259 0.032 Uiso 1 1 calc R A 1 C24 C 0.3138(8) 0.6079(3) 0.0235(5) 0.0332(16) Uani 1 1 d . A 1 H24 H 0.2887 0.6332 0.0647 0.040 Uiso 1 1 calc R A 1 C25 C 0.4405(7) 0.6122(3) -0.0165(4) 0.0314(16) Uani 1 1 d . A 1 H25 H 0.5020 0.6412 -0.0012 0.038 Uiso 1 1 calc R A 1 N2 N 0.4835(4) 0.5769(2) -0.0775(3) 0.0260(13) Uani 1 1 d D A 1 C31 C 0.5237(6) 0.5335(2) -0.2848(3) 0.0214(13) Uani 1 1 d D A 1 C32 C 0.4713(7) 0.5296(3) -0.3704(5) 0.0326(17) Uani 1 1 d . A 1 H32 H 0.4083 0.5013 -0.3864 0.039 Uiso 1 1 calc R A 1 C33 C 0.5132(9) 0.5671(3) -0.4284(5) 0.0393(19) Uani 1 1 d . A 1 H33 H 0.4766 0.5647 -0.4836 0.047 Uiso 1 1 calc R A 1 C34 C 0.6067(9) 0.6075(3) -0.4071(4) 0.0383(18) Uani 1 1 d . A 1 H34 H 0.6358 0.6331 -0.4467 0.046 Uiso 1 1 calc R A 1 C35 C 0.6588(8) 0.6100(3) -0.3242(4) 0.0327(16) Uani 1 1 d . A 1 H35 H 0.7240 0.6378 -0.3092 0.039 Uiso 1 1 calc R A 1 N3 N 0.6196(6) 0.5740(2) -0.2647(2) 0.0286(12) Uani 1 1 d D A 1 Al2 Al 0.95861(19) 0.68905(7) -0.06941(12) 0.0234(5) Uani 1 1 d D A 1 C2 C 1.1013(8) 0.7469(3) -0.0368(5) 0.0421(19) Uani 1 1 d D A 1 H2A H 1.0563 0.7741 -0.0024 0.063 Uiso 1 1 calc R A 1 H2B H 1.1359 0.7643 -0.0866 0.063 Uiso 1 1 calc R A 1 H2C H 1.1808 0.7303 -0.0058 0.063 Uiso 1 1 calc R A 1 C41 C 1.0280(7) 0.6370(2) -0.1581(3) 0.0277(16) Uiso 1 1 d D A 1 C42 C 1.1550(6) 0.6430(3) -0.2005(4) 0.0273(15) Uani 1 1 d . A 1 H42 H 1.2153 0.6726 -0.1861 0.033 Uiso 1 1 calc R A 1 C43 C 1.1965(7) 0.6074(3) -0.2629(5) 0.0371(18) Uani 1 1 d . A 1 H43 H 1.2838 0.6120 -0.2893 0.045 Uiso 1 1 calc R A 1 C44 C 1.1053(8) 0.5655(3) -0.2845(5) 0.0378(17) Uani 1 1 d . A 1 H44 H 1.1297 0.5404 -0.3261 0.045 Uiso 1 1 calc R A 1 C45 C 0.9760(7) 0.5601(3) -0.2444(4) 0.0334(16) Uani 1 1 d . A 1 H45 H 0.9143 0.5313 -0.2602 0.040 Uiso 1 1 calc R A 1 N4 N 0.9363(4) 0.5950(2) -0.1836(4) 0.0252(13) Uani 1 1 d D A 1 C51 C 0.7716(4) 0.7186(2) -0.1199(3) 0.0180(13) Uani 1 1 d DU A 1 C52 C 0.7415(7) 0.7755(3) -0.1361(5) 0.0320(16) Uani 1 1 d . A 1 H52 H 0.8084 0.8023 -0.1189 0.038 Uiso 1 1 calc R A 1 C53 C 0.6151(9) 0.7913(3) -0.1765(5) 0.041(2) Uani 1 1 d U A 1 H53 H 0.5996 0.8282 -0.1909 0.049 Uiso 1 1 calc R A 1 C54 C 0.5094(8) 0.7515(3) -0.1960(5) 0.0402(19) Uani 1 1 d . A 1 H54 H 0.4196 0.7616 -0.2190 0.048 Uiso 1 1 calc R A 1 C55 C 0.5426(7) 0.6962(3) -0.1801(4) 0.0272(15) Uani 1 1 d . A 1 H55 H 0.4746 0.6693 -0.1951 0.033 Uiso 1 1 calc R A 1 N5 N 0.6694(5) 0.68005(14) -0.1438(4) 0.0237(12) Uani 1 1 d D A 1 C61 C 0.8979(6) 0.6396(2) 0.0249(3) 0.0245(14) Uani 1 1 d D A 1 C62 C 0.9456(7) 0.6441(3) 0.1103(4) 0.0290(15) Uani 1 1 d . A 1 H62 H 1.0111 0.6716 0.1262 0.035 Uiso 1 1 calc R A 1 C63 C 0.8961(8) 0.6081(4) 0.1698(5) 0.041(2) Uani 1 1 d . A 1 H63 H 0.9308 0.6104 0.2254 0.050 Uiso 1 1 calc R A 1 C64 C 0.7961(8) 0.5693(4) 0.1471(5) 0.0419(19) Uani 1 1 d . A 1 H64 H 0.7573 0.5460 0.1872 0.050 Uiso 1 1 calc R A 1 C65 C 0.7534(7) 0.5650(3) 0.0634(4) 0.0275(15) Uani 1 1 d . A 1 H65 H 0.6879 0.5375 0.0472 0.033 Uiso 1 1 calc R A 1 N6 N 0.8030(5) 0.5990(2) 0.0046(2) 0.0244(12) Uani 1 1 d D A 1 O1T O 1.1863(12) 0.2430(5) 0.1803(6) 0.110(3) Uani 1 1 d . B 1 C1T C 1.168(2) 0.2587(7) 0.1018(8) 0.139(8) Uani 1 1 d . B 1 H1T1 H 1.1799 0.2272 0.0647 0.167 Uiso 1 1 calc R B 1 H1T2 H 1.2403 0.2861 0.0886 0.167 Uiso 1 1 calc R B 1 C2T C 1.0089(18) 0.2845(6) 0.0871(9) 0.127(7) Uani 1 1 d . B 1 H2T1 H 1.0076 0.3242 0.0965 0.153 Uiso 1 1 calc R B 1 H2T2 H 0.9683 0.2763 0.0314 0.153 Uiso 1 1 calc R B 1 C3T C 0.9361(15) 0.2541(7) 0.1533(8) 0.098(4) Uani 1 1 d . B 1 H3T1 H 0.8981 0.2793 0.1946 0.117 Uiso 1 1 calc R B 1 H3T2 H 0.8573 0.2320 0.1295 0.117 Uiso 1 1 calc R B 1 C4T C 1.050(2) 0.2179(7) 0.1927(11) 0.120(5) Uani 1 1 d . B 1 H4T1 H 1.0347 0.2138 0.2525 0.144 Uiso 1 1 calc R B 1 H4T2 H 1.0471 0.1815 0.1669 0.144 Uiso 1 1 calc R B 1 Mn1X Mn 1.2122(11) 0.7442(3) -0.1314(6) 0.0069(15) Uiso 0.10 1 d P C 2 Mn2X Mn 0.9704(19) 0.6395(7) -0.1862(11) 0.059(4) Uiso 0.10 1 d P D 2 Al1X Al 0.209(3) 0.4284(8) -0.1325(17) 0.034(5) Uiso 0.10 1 d P E 2 Al2X Al 0.9564(18) 0.3466(7) -0.0663(11) 0.014(3) Uiso 0.10 1 d P F 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 Mn1 0.0220(4) 0.0162(4) 0.0268(5) 0.0001(3) 0.0002(3) -0.0042(3) Al1 0.0208(9) 0.0173(10) 0.0277(10) -0.0018(8) -0.0011(7) -0.0057(8) C1 0.038(4) 0.028(4) 0.056(5) -0.003(4) -0.001(3) -0.010(3) C11 0.029(3) 0.017(3) 0.038(4) 0.005(3) 0.016(3) 0.000(3) C12 0.033(4) 0.024(3) 0.029(3) -0.004(3) 0.003(3) -0.008(3) C13 0.045(4) 0.011(3) 0.052(5) 0.012(3) 0.023(4) 0.017(3) C14 0.027(4) 0.032(4) 0.053(5) 0.010(3) -0.004(3) 0.009(3) C15 0.031(4) 0.024(4) 0.051(5) -0.007(3) 0.002(3) 0.002(3) N1 0.018(3) 0.020(3) 0.033(3) 0.001(2) -0.003(2) 0.003(2) C21 0.028(3) 0.005(3) 0.034(4) 0.007(2) -0.003(3) -0.003(2) C22 0.027(3) 0.015(3) 0.044(4) 0.001(3) -0.011(3) 0.004(3) C23 0.024(3) 0.029(4) 0.029(4) 0.006(3) 0.008(3) -0.004(3) C24 0.034(4) 0.035(4) 0.032(4) -0.005(3) 0.010(3) 0.008(3) C25 0.038(4) 0.021(3) 0.036(4) -0.006(3) 0.002(3) -0.003(3) N2 0.035(3) 0.019(3) 0.024(3) 0.003(2) 0.001(3) -0.002(2) C31 0.017(3) 0.017(3) 0.030(3) -0.001(3) 0.000(2) 0.003(2) C32 0.028(3) 0.035(4) 0.035(4) -0.005(3) 0.003(3) 0.003(3) C33 0.057(5) 0.041(5) 0.020(4) -0.012(4) 0.000(3) 0.003(4) C34 0.058(5) 0.035(4) 0.023(4) 0.006(3) 0.007(3) -0.003(4) C35 0.040(4) 0.033(4) 0.026(4) 0.005(3) 0.006(3) -0.013(3) N3 0.042(3) 0.018(3) 0.025(3) 0.003(3) 0.003(2) 0.001(3) Al2 0.0225(9) 0.0155(10) 0.0322(11) -0.0017(8) 0.0007(8) -0.0044(8) C2 0.037(4) 0.027(4) 0.060(5) -0.005(4) -0.018(4) -0.015(3) C42 0.020(3) 0.033(4) 0.029(4) 0.004(3) 0.001(3) -0.002(3) C43 0.019(3) 0.052(5) 0.041(4) 0.006(4) 0.010(3) 0.011(3) C44 0.039(4) 0.036(4) 0.038(4) -0.005(4) 0.005(3) 0.009(3) C45 0.026(3) 0.040(4) 0.035(4) -0.011(3) 0.006(3) 0.000(3) N4 0.020(3) 0.015(3) 0.040(4) -0.006(3) 0.002(2) -0.004(2) C51 0.019(3) 0.010(3) 0.025(3) 0.000(2) 0.004(2) 0.002(2) C52 0.028(4) 0.022(3) 0.045(4) 0.007(3) -0.006(3) 0.002(3) C53 0.043(4) 0.028(4) 0.052(5) 0.000(4) -0.020(4) 0.009(4) C54 0.035(4) 0.033(4) 0.052(5) 0.006(4) -0.007(4) 0.009(3) C55 0.023(3) 0.027(4) 0.031(4) 0.007(3) -0.004(3) -0.002(3) N5 0.025(3) 0.014(2) 0.032(3) -0.002(2) 0.002(2) -0.002(2) C61 0.025(3) 0.020(3) 0.029(3) -0.004(3) 0.001(3) -0.001(3) C62 0.037(4) 0.027(4) 0.022(3) -0.009(3) 0.001(3) -0.009(3) C63 0.044(5) 0.058(5) 0.022(4) 0.012(4) -0.009(3) -0.015(4) C64 0.035(4) 0.050(5) 0.041(5) 0.008(4) 0.003(3) -0.002(4) C65 0.034(4) 0.019(3) 0.030(4) 0.007(3) 0.006(3) -0.007(3) N6 0.016(2) 0.021(3) 0.036(3) 0.002(3) 0.002(2) -0.005(2) O1T 0.109(7) 0.127(8) 0.093(7) -0.019(6) -0.008(5) 0.048(7) C1T 0.186(15) 0.169(15) 0.064(8) 0.035(9) 0.028(9) 0.141(14) C2T 0.180(15) 0.083(9) 0.113(11) 0.057(8) -0.090(11) -0.055(10) C3T 0.095(9) 0.121(11) 0.077(8) 0.015(8) -0.015(7) 0.001(8) C4T 0.159(16) 0.096(11) 0.104(11) -0.002(9) 0.000(11) 0.019(11) _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 Mn1 N6 2.291(3) . ? Mn1 N4 2.295(3) . ? Mn1 N5 2.300(3) . ? Mn1 N3 2.296(3) . ? Mn1 N1 2.305(3) . ? Mn1 N2 2.300(3) . ? Al1 C11 2.013(4) . ? Al1 C1 1.984(5) . ? Al1 C31 2.012(4) . ? Al1 C21 2.013(4) . ? C11 C12 1.393(9) . ? C11 N1 1.389(8) . ? C12 C13 1.361(10) . ? C13 C14 1.403(11) . ? C14 C15 1.359(10) . ? C15 N1 1.356(9) . ? C21 N2 1.343(8) . ? C21 C22 1.387(9) . ? C22 C23 1.391(10) . ? C23 C24 1.403(10) . ? C24 C25 1.358(10) . ? C25 N2 1.360(8) . ? C31 N3 1.353(8) . ? C31 C32 1.431(9) . ? C32 C33 1.358(11) . ? C33 C34 1.341(12) . ? C34 C35 1.387(10) . ? C35 N3 1.342(9) . ? Al2 C2 1.981(5) . ? Al2 C61 2.012(4) . ? Al2 C51 2.014(3) . ? Al2 C41 2.010(4) . ? C41 N4 1.376(8) . ? C41 C42 1.383(9) . ? C42 C43 1.377(10) . ? C43 C44 1.356(12) . ? C44 C45 1.381(10) . ? C45 N4 1.343(8) . ? C51 N5 1.372(7) . ? C51 C52 1.426(8) . ? C52 C53 1.370(10) . ? C53 C54 1.400(11) . ? C54 C55 1.392(10) . ? C55 N5 1.348(8) . ? C61 N6 1.348(7) . ? C61 C62 1.416(9) . ? C62 C63 1.374(10) . ? C63 C64 1.360(12) . ? C64 C65 1.377(11) . ? C65 N6 1.337(8) . ? O1T C1T 1.308(14) . ? O1T C4T 1.418(19) . ? C1T C2T 1.61(2) . ? C2T C3T 1.468(19) . ? C3T C4T 1.49(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 N6 Mn1 N4 91.1(2) . . ? N6 Mn1 N5 91.00(19) . . ? N4 Mn1 N5 91.57(19) . . ? N6 Mn1 N3 179.6(3) . . ? N4 Mn1 N3 88.5(2) . . ? N5 Mn1 N3 89.1(2) . . ? N6 Mn1 N1 89.30(19) . . ? N4 Mn1 N1 88.21(19) . . ? N5 Mn1 N1 179.6(2) . . ? N3 Mn1 N1 90.6(2) . . ? N6 Mn1 N2 89.68(19) . . ? N4 Mn1 N2 178.9(2) . . ? N5 Mn1 N2 89.1(2) . . ? N3 Mn1 N2 90.7(2) . . ? N1 Mn1 N2 91.1(2) . . ? C11 Al1 C1 113.5(3) . . ? C11 Al1 C31 104.4(2) . . ? C1 Al1 C31 115.8(3) . . ? C11 Al1 C21 103.7(2) . . ? C1 Al1 C21 113.6(3) . . ? C31 Al1 C21 104.5(2) . . ? C12 C11 N1 118.1(4) . . ? C12 C11 Al1 126.9(5) . . ? N1 C11 Al1 114.9(3) . . ? C13 C12 C11 123.1(6) . . ? C12 C13 C14 118.1(6) . . ? C15 C14 C13 117.9(6) . . ? N1 C15 C14 124.8(7) . . ? C15 N1 C11 117.9(4) . . ? C15 N1 Mn1 119.0(4) . . ? C11 N1 Mn1 123.1(3) . . ? N2 C21 C22 119.3(4) . . ? N2 C21 Al1 118.0(4) . . ? C22 C21 Al1 122.7(4) . . ? C23 C22 C21 121.6(6) . . ? C22 C23 C24 118.3(6) . . ? C25 C24 C23 117.3(6) . . ? N2 C25 C24 124.4(6) . . ? C21 N2 C25 119.2(4) . . ? C21 N2 Mn1 121.5(4) . . ? C25 N2 Mn1 119.1(4) . . ? N3 C31 C32 118.0(4) . . ? N3 C31 Al1 117.2(4) . . ? C32 C31 Al1 124.8(5) . . ? C33 C32 C31 120.3(6) . . ? C34 C33 C32 120.8(7) . . ? C33 C34 C35 118.2(7) . . ? N3 C35 C34 123.1(6) . . ? C35 N3 C31 119.6(4) . . ? C35 N3 Mn1 118.1(4) . . ? C31 N3 Mn1 122.2(3) . . ? C2 Al2 C61 115.3(3) . . ? C2 Al2 C51 114.3(3) . . ? C61 Al2 C51 104.4(2) . . ? C2 Al2 C41 113.4(3) . . ? C61 Al2 C41 104.7(2) . . ? C51 Al2 C41 103.5(2) . . ? N4 C41 C42 117.5(4) . . ? N4 C41 Al2 117.3(4) . . ? C42 C41 Al2 124.9(5) . . ? C43 C42 C41 123.2(6) . . ? C44 C43 C42 117.5(6) . . ? C43 C44 C45 119.8(7) . . ? N4 C45 C44 122.4(6) . . ? C41 N4 C45 119.5(4) . . ? C41 N4 Mn1 121.1(3) . . ? C45 N4 Mn1 119.3(4) . . ? N5 C51 C52 118.4(4) . . ? N5 C51 Al2 116.5(3) . . ? C52 C51 Al2 125.0(4) . . ? C53 C52 C51 120.8(6) . . ? C52 C53 C54 119.5(7) . . ? C55 C54 C53 118.1(7) . . ? N5 C55 C54 122.6(6) . . ? C55 N5 C51 120.3(4) . . ? C55 N5 Mn1 117.7(4) . . ? C51 N5 Mn1 121.9(3) . . ? N6 C61 C62 117.7(4) . . ? N6 C61 Al2 116.8(4) . . ? C62 C61 Al2 125.5(4) . . ? C63 C62 C61 120.6(6) . . ? C64 C63 C62 119.7(7) . . ? C63 C64 C65 118.6(7) . . ? N6 C65 C64 122.2(6) . . ? C61 N6 C65 121.2(4) . . ? C61 N6 Mn1 122.5(3) . . ? C65 N6 Mn1 116.3(4) . . ? C1T O1T C4T 99.8(14) . . ? O1T C1T C2T 109.8(12) . . ? C3T C2T C1T 98.2(10) . . ? C4T C3T C2T 104.9(13) . . ? O1T C4T C3T 108.3(13) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.868 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.097