#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemsitry 2001 data_NL0010 _database_code_CSD 159092 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Gibson, Vernon C.' 'Long, Nicholas' 'Marshall, Edward L.' 'Oxford, Philip J.' 'White, Andrew J. P.' 'Williams, David J.' _publ_contact_author_name 'Dr Nicholas Long' _publ_contact_author_address ; Dr Nicholas Long Department of Chemistry Imperial College of Science, Technology and Medicine South Kensington London SW7 2AY UNITED KINGDOM ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H30 N2 O2 Al2 Fe' _chemical_formula_weight 536.35 _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' 0.0033 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' 'Fe' 'Fe' 0.3463 0.8444 '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 11.274(2) _cell_length_b 16.244(3) _cell_length_c 14.3527(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.465(9) _cell_angle_gamma 90.00 _cell_volume 2611.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.35 _cell_measurement_theta_max 12.46 _exptl_crystal_description prisms _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.673 _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 0.71073 _diffrn_radiation_type MoK\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_% 3.80 _diffrn_reflns_number 2432 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2308 _reflns_number_observed 1745 _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 163 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^)+(0.0545P)^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 2145 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_all 0.1095 _refine_ls_wR_factor_obs 0.0965 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.068 _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 Fe Fe 0.0000 0.35421(4) 0.7500 0.0274(2) Uani 1 d S . Al Al 0.25161(8) 0.55203(6) 0.66711(6) 0.0309(2) Uani 1 d . . O1 O 0.2125(2) 0.6577(2) 0.6684(2) 0.0484(6) Uani 1 d . . C1 C 0.1104(3) 0.6951(2) 0.6415(2) 0.0339(7) Uani 1 d . . C2 C 0.1065(3) 0.7799(2) 0.6296(3) 0.0441(8) Uani 1 d . . H2A H 0.1782(3) 0.8108(2) 0.6412(3) 0.053 Uiso 1 calc R . C3 C 0.0015(3) 0.8204(2) 0.6016(3) 0.0443(8) Uani 1 d . . H3A H 0.0021(3) 0.8783(2) 0.5928(3) 0.053 Uiso 1 calc R . C4 C -0.1049(3) 0.7776(2) 0.5860(2) 0.0415(8) Uani 1 d . . H4A H -0.1772(3) 0.8060(2) 0.5670(2) 0.050 Uiso 1 calc R . C5 C -0.1051(3) 0.6935(2) 0.5983(2) 0.0356(7) Uani 1 d . . H5A H -0.1784(3) 0.6642(2) 0.5887(2) 0.043 Uiso 1 calc R . C6 C 0.0020(3) 0.6501(2) 0.6250(2) 0.0310(6) Uani 1 d . . C7 C -0.0047(3) 0.5626(2) 0.6316(2) 0.0299(6) Uani 1 d . . H7A H -0.0821(3) 0.5390(2) 0.6213(2) 0.036 Uiso 1 calc R . N7 N 0.0838(2) 0.5118(2) 0.6502(2) 0.0290(6) Uani 1 d . . C8 C -0.0451(3) 0.3826(2) 0.6118(2) 0.0369(7) Uani 1 d . . H8A H -0.1182(3) 0.4068(2) 0.5858(2) 0.044 Uiso 1 calc R . C9 C -0.0210(4) 0.2963(2) 0.6221(2) 0.0425(8) Uani 1 d . . H9A H -0.0752(4) 0.2530(2) 0.6035(2) 0.051 Uiso 1 calc R . C10 C 0.0979(3) 0.2868(2) 0.6648(3) 0.0422(8) Uani 1 d . . H10A H 0.1368(3) 0.2360(2) 0.6803(3) 0.051 Uiso 1 calc R . C11 C 0.1481(3) 0.3653(2) 0.6804(2) 0.0365(7) Uani 1 d . . H11A H 0.2271(3) 0.3763(2) 0.7082(2) 0.044 Uiso 1 calc R . C12 C 0.0616(3) 0.4258(2) 0.6479(2) 0.0305(7) Uani 1 d . . C13 C 0.3229(3) 0.5218(3) 0.5540(2) 0.0454(9) Uani 1 d . . H13A H 0.2937(21) 0.4674(9) 0.5325(12) 0.068 Uiso 1 calc R . H13B H 0.4100(3) 0.5202(18) 0.5679(6) 0.068 Uiso 1 calc R . H13C H 0.3007(22) 0.5626(10) 0.5048(7) 0.068 Uiso 1 calc R . C14 C 0.3357(3) 0.5228(3) 0.7890(3) 0.0488(9) Uani 1 d . . H14A H 0.3879(21) 0.4754(12) 0.7818(4) 0.073 Uiso 1 calc R . H14B H 0.2776(4) 0.5085(19) 0.8323(7) 0.073 Uiso 1 calc R . H14C H 0.3840(22) 0.5696(7) 0.8141(10) 0.073 Uiso 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 Fe 0.0287(3) 0.0275(3) 0.0270(3) 0.000 0.0074(2) 0.000 Al 0.0237(5) 0.0377(5) 0.0311(5) 0.0037(4) 0.0024(4) 0.0028(4) O1 0.0291(12) 0.0380(14) 0.076(2) -0.0040(13) -0.0042(12) 0.0009(10) C1 0.030(2) 0.038(2) 0.033(2) -0.0013(14) 0.0020(13) 0.0036(13) C2 0.041(2) 0.033(2) 0.057(2) -0.003(2) -0.001(2) -0.0029(15) C3 0.050(2) 0.034(2) 0.048(2) 0.000(2) 0.003(2) 0.007(2) C4 0.040(2) 0.047(2) 0.039(2) 0.008(2) 0.0093(14) 0.014(2) C5 0.030(2) 0.041(2) 0.037(2) 0.0041(14) 0.0080(13) 0.0044(14) C6 0.032(2) 0.036(2) 0.0266(14) 0.0009(13) 0.0089(12) 0.0012(14) C7 0.0239(14) 0.038(2) 0.0284(15) 0.0018(13) 0.0069(11) -0.0014(13) N7 0.0282(13) 0.0353(14) 0.0243(11) 0.0032(10) 0.0059(10) -0.0001(11) C8 0.048(2) 0.038(2) 0.0256(15) -0.0030(13) 0.0058(13) -0.0027(15) C9 0.057(2) 0.037(2) 0.035(2) -0.0105(14) 0.011(2) -0.006(2) C10 0.051(2) 0.031(2) 0.049(2) -0.0023(14) 0.025(2) 0.008(2) C11 0.034(2) 0.037(2) 0.042(2) 0.0038(14) 0.0203(14) 0.0036(14) C12 0.032(2) 0.034(2) 0.0277(14) 0.0000(13) 0.0107(12) 0.0023(13) C13 0.035(2) 0.063(2) 0.039(2) 0.008(2) 0.0105(15) 0.006(2) C14 0.038(2) 0.070(3) 0.037(2) 0.009(2) 0.0001(15) 0.006(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 Fe C8 2.044(3) 2_556 ? Fe C8 2.044(3) . ? Fe C11 2.048(3) 2_556 ? Fe C11 2.048(3) . ? Fe C12 2.052(3) 2_556 ? Fe C12 2.052(3) . ? Fe C10 2.053(3) . ? Fe C10 2.053(3) 2_556 ? Fe C9 2.053(3) . ? Fe C9 2.053(3) 2_556 ? Al O1 1.773(3) . ? Al C14 1.952(4) . ? Al C13 1.953(4) . ? Al N7 1.990(3) . ? O1 C1 1.320(4) . ? C1 C2 1.389(5) . ? C1 C6 1.421(5) . ? C2 C3 1.373(5) . ? C3 C4 1.382(6) . ? C4 C5 1.379(5) . ? C5 C6 1.413(5) . ? C6 C7 1.427(5) . ? C7 N7 1.299(4) . ? N7 C12 1.419(4) . ? C8 C9 1.432(5) . ? C8 C12 1.439(5) . ? C9 C10 1.418(6) . ? C10 C11 1.402(5) . ? C11 C12 1.427(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 C8 Fe C8 154.0(2) 2_556 . ? C8 Fe C11 68.56(15) 2_556 2_556 ? C8 Fe C11 109.03(15) . 2_556 ? C8 Fe C11 109.03(15) 2_556 . ? C8 Fe C11 68.56(15) . . ? C11 Fe C11 169.9(2) 2_556 . ? C8 Fe C12 41.13(14) 2_556 2_556 ? C8 Fe C12 119.85(14) . 2_556 ? C11 Fe C12 40.72(13) 2_556 2_556 ? C11 Fe C12 131.19(14) . 2_556 ? C8 Fe C12 119.85(14) 2_556 . ? C8 Fe C12 41.13(14) . . ? C11 Fe C12 131.19(14) 2_556 . ? C11 Fe C12 40.72(13) . . ? C12 Fe C12 110.9(2) 2_556 . ? C8 Fe C10 127.3(2) 2_556 . ? C8 Fe C10 68.53(15) . . ? C11 Fe C10 149.27(15) 2_556 . ? C11 Fe C10 39.99(14) . . ? C12 Fe C10 167.23(15) 2_556 . ? C12 Fe C10 68.25(13) . . ? C8 Fe C10 68.53(15) 2_556 2_556 ? C8 Fe C10 127.3(2) . 2_556 ? C11 Fe C10 39.99(14) 2_556 2_556 ? C11 Fe C10 149.27(15) . 2_556 ? C12 Fe C10 68.25(13) 2_556 2_556 ? C12 Fe C10 167.23(15) . 2_556 ? C10 Fe C10 115.5(2) . 2_556 ? C8 Fe C9 164.21(15) 2_556 . ? C8 Fe C9 40.91(15) . . ? C11 Fe C9 117.3(2) 2_556 . ? C11 Fe C9 67.8(2) . . ? C12 Fe C9 152.14(14) 2_556 . ? C12 Fe C9 68.62(14) . . ? C10 Fe C9 40.4(2) . . ? C10 Fe C9 105.8(2) 2_556 . ? C8 Fe C9 40.91(15) 2_556 2_556 ? C8 Fe C9 164.21(15) . 2_556 ? C11 Fe C9 67.80(15) 2_556 2_556 ? C11 Fe C9 117.26(15) . 2_556 ? C12 Fe C9 68.62(14) 2_556 2_556 ? C12 Fe C9 152.14(15) . 2_556 ? C10 Fe C9 105.83(15) . 2_556 ? C10 Fe C9 40.4(2) 2_556 2_556 ? C9 Fe C9 125.5(2) . 2_556 ? O1 Al C14 108.8(2) . . ? O1 Al C13 112.2(2) . . ? C14 Al C13 118.7(2) . . ? O1 Al N7 94.88(12) . . ? C14 Al N7 112.88(15) . . ? C13 Al N7 106.86(15) . . ? C1 O1 Al 130.6(2) . . ? O1 C1 C2 120.4(3) . . ? O1 C1 C6 121.2(3) . . ? C2 C1 C6 118.4(3) . . ? C3 C2 C1 121.7(3) . . ? C2 C3 C4 120.7(3) . . ? C5 C4 C3 119.4(3) . . ? C4 C5 C6 121.0(3) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 C7 117.7(3) . . ? C1 C6 C7 123.5(3) . . ? N7 C7 C6 126.9(3) . . ? C7 N7 C12 119.4(3) . . ? C7 N7 Al 121.0(2) . . ? C12 N7 Al 119.3(2) . . ? C9 C8 C12 107.4(3) . . ? C9 C8 Fe 69.9(2) . . ? C12 C8 Fe 69.7(2) . . ? C10 C9 C8 108.1(3) . . ? C10 C9 Fe 69.8(2) . . ? C8 C9 Fe 69.2(2) . . ? C11 C10 C9 108.4(3) . . ? C11 C10 Fe 69.8(2) . . ? C9 C10 Fe 69.8(2) . . ? C10 C11 C12 109.0(3) . . ? C10 C11 Fe 70.2(2) . . ? C12 C11 Fe 69.8(2) . . ? N7 C12 C11 124.0(3) . . ? N7 C12 C8 128.9(3) . . ? C11 C12 C8 107.1(3) . . ? N7 C12 Fe 128.0(2) . . ? C11 C12 Fe 69.5(2) . . ? C8 C12 Fe 69.1(2) . . ? _refine_diff_density_max 0.837 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.062