# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD John Arnold' _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Synthesis and Reactivity of Bis-Pentamethylcyclopentadienyl Diiodoalane (Cp*AlI)2: An Aluminum(II) Precursor to (Cp*Al)4 ; loop_ _publ_author_name 'John Arnold' 'Stefan Minasian' # Attachment '684336.cif' data_sgm1_15m _database_code_depnum_ccdc_archive 'CCDC 684336' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Al2 I2' _chemical_formula_sum 'C20 H30 Al2 I2' _chemical_formula_weight 578.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7521(12) _cell_length_b 14.660(2) _cell_length_c 18.022(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.253(2) _cell_angle_gamma 90.00 _cell_volume 2308.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7546 _cell_measurement_theta_min 6.898 _cell_measurement_theta_max 49.428 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 2.801 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10124 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 24.72 _reflns_number_total 3886 _reflns_number_gt 3509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0309P)^2^+1.3020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3886 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.005 _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 I1 I 0.06257(2) 0.763714(12) 0.722141(10) 0.04144(7) Uani 1 1 d . . . I2 I -0.44676(2) 0.630314(13) 0.778851(10) 0.03940(7) Uani 1 1 d . . . Al1 Al -0.04570(8) 0.59908(5) 0.69145(4) 0.02494(16) Uani 1 1 d . . . Al2 Al -0.16890(8) 0.56762(5) 0.81262(4) 0.02539(16) Uani 1 1 d . . . C14 C -0.0785(3) 0.44851(16) 0.88168(13) 0.0280(5) Uani 1 1 d . . . C11 C -0.1624(3) 0.58238(17) 0.93326(13) 0.0290(5) Uani 1 1 d . . . C3 C 0.0829(3) 0.56054(19) 0.59670(14) 0.0330(6) Uani 1 1 d . . . C12 C -0.0079(3) 0.59464(17) 0.91340(13) 0.0301(5) Uani 1 1 d . . . C5 C -0.1799(3) 0.55411(17) 0.58712(13) 0.0284(5) Uani 1 1 d . . . C1 C -0.1257(3) 0.47199(17) 0.62105(14) 0.0341(6) Uani 1 1 d . . . C4 C -0.0509(3) 0.60802(17) 0.57018(13) 0.0283(5) Uani 1 1 d . . . C13 C 0.0434(3) 0.51157(17) 0.88362(13) 0.0286(5) Uani 1 1 d . . . C2 C 0.0367(3) 0.47637(18) 0.62784(14) 0.0357(6) Uani 1 1 d . . . C15 C -0.2072(3) 0.49155(17) 0.91336(13) 0.0270(5) Uani 1 1 d . . . C20 C -0.3577(3) 0.44806(19) 0.92872(16) 0.0377(6) Uani 1 1 d . . . H20A H -0.3533 0.4245 0.9797 0.057 Uiso 1 1 calc R . . H20B H -0.3785 0.3978 0.8938 0.057 Uiso 1 1 calc R . . H20C H -0.4395 0.4936 0.9227 0.057 Uiso 1 1 calc R . . C19 C -0.0733(4) 0.35078(18) 0.85535(16) 0.0398(7) Uani 1 1 d . . . H19A H -0.0362 0.3115 0.8966 0.060 Uiso 1 1 calc R . . H19B H -0.0040 0.3460 0.8147 0.060 Uiso 1 1 calc R . . H19C H -0.1762 0.3314 0.8378 0.060 Uiso 1 1 calc R . . C18 C 0.1979(3) 0.4973(2) 0.85317(16) 0.0416(7) Uani 1 1 d . . . H18A H 0.2777 0.5183 0.8896 0.062 Uiso 1 1 calc R . . H18B H 0.2043 0.5320 0.8070 0.062 Uiso 1 1 calc R . . H18C H 0.2126 0.4323 0.8431 0.062 Uiso 1 1 calc R . . C17 C 0.0864(4) 0.6797(2) 0.92731(16) 0.0425(7) Uani 1 1 d . . . H17A H 0.1286 0.6799 0.9789 0.064 Uiso 1 1 calc R . . H17B H 0.0216 0.7335 0.9186 0.064 Uiso 1 1 calc R . . H17C H 0.1703 0.6808 0.8935 0.064 Uiso 1 1 calc R . . C10 C -0.3446(3) 0.5781(2) 0.56731(16) 0.0449(7) Uani 1 1 d . . . H10A H -0.3689 0.5643 0.5148 0.067 Uiso 1 1 calc R . . H10B H -0.3606 0.6433 0.5762 0.067 Uiso 1 1 calc R . . H10C H -0.4113 0.5424 0.5981 0.067 Uiso 1 1 calc R . . C16 C -0.2577(4) 0.65012(19) 0.97293(15) 0.0404(7) Uani 1 1 d . . . H16A H -0.2492 0.6378 1.0265 0.061 Uiso 1 1 calc R . . H16B H -0.3650 0.6447 0.9547 0.061 Uiso 1 1 calc R . . H16C H -0.2211 0.7120 0.9635 0.061 Uiso 1 1 calc R . . C9 C -0.0532(4) 0.69616(19) 0.52790(15) 0.0424(7) Uani 1 1 d . . . H9A H -0.0118 0.6863 0.4791 0.064 Uiso 1 1 calc R . . H9B H 0.0094 0.7415 0.5557 0.064 Uiso 1 1 calc R . . H9C H -0.1587 0.7183 0.5213 0.064 Uiso 1 1 calc R . . C8 C 0.2439(3) 0.5920(3) 0.58656(17) 0.0524(8) Uani 1 1 d . . . H8A H 0.2705 0.5800 0.5354 0.079 Uiso 1 1 calc R . . H8B H 0.3146 0.5588 0.6210 0.079 Uiso 1 1 calc R . . H8C H 0.2517 0.6575 0.5967 0.079 Uiso 1 1 calc R . . C7 C 0.1447(5) 0.4040(2) 0.65911(18) 0.0593(10) Uani 1 1 d . . . H7A H 0.1957 0.3745 0.6184 0.089 Uiso 1 1 calc R . . H7B H 0.0870 0.3583 0.6857 0.089 Uiso 1 1 calc R . . H7C H 0.2216 0.4321 0.6935 0.089 Uiso 1 1 calc R . . C6 C -0.2244(5) 0.3974(2) 0.64949(18) 0.0564(9) Uani 1 1 d . . . H6A H -0.3073 0.3837 0.6123 0.085 Uiso 1 1 calc R . . H6B H -0.2679 0.4172 0.6957 0.085 Uiso 1 1 calc R . . H6C H -0.1623 0.3425 0.6590 0.085 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 I1 0.05676(14) 0.03377(11) 0.03311(11) -0.00075(7) -0.00349(8) -0.01439(8) I2 0.02932(11) 0.04678(12) 0.04203(12) 0.00896(8) 0.00133(7) 0.00500(7) Al1 0.0249(4) 0.0274(4) 0.0224(4) 0.0001(3) 0.0006(3) 0.0009(3) Al2 0.0268(4) 0.0259(4) 0.0235(4) -0.0007(3) 0.0015(3) -0.0026(3) C14 0.0348(14) 0.0276(12) 0.0215(11) 0.0005(10) -0.0003(10) 0.0030(11) C11 0.0331(14) 0.0296(13) 0.0242(12) -0.0020(10) 0.0011(10) 0.0019(11) C3 0.0279(13) 0.0453(15) 0.0257(13) -0.0079(11) 0.0002(10) 0.0035(12) C12 0.0337(14) 0.0333(13) 0.0227(12) -0.0001(10) -0.0044(10) -0.0052(11) C5 0.0266(13) 0.0324(13) 0.0256(12) -0.0057(10) -0.0028(10) 0.0010(11) C1 0.0476(16) 0.0290(13) 0.0252(13) -0.0038(10) -0.0009(11) -0.0044(12) C4 0.0323(14) 0.0316(13) 0.0207(12) -0.0011(10) -0.0008(10) -0.0010(11) C13 0.0266(13) 0.0363(14) 0.0224(12) 0.0014(10) -0.0019(9) 0.0023(11) C2 0.0465(16) 0.0372(15) 0.0229(12) -0.0057(11) -0.0035(11) 0.0162(13) C15 0.0298(13) 0.0282(12) 0.0230(12) 0.0012(10) 0.0023(10) -0.0013(10) C20 0.0357(15) 0.0411(15) 0.0366(15) 0.0052(12) 0.0056(11) -0.0066(12) C19 0.0519(18) 0.0288(14) 0.0384(15) -0.0021(11) 0.0012(13) 0.0057(13) C18 0.0259(14) 0.0626(19) 0.0363(15) 0.0009(13) 0.0012(11) 0.0058(13) C17 0.0481(18) 0.0431(16) 0.0351(15) -0.0007(12) -0.0079(12) -0.0161(14) C10 0.0296(15) 0.0621(19) 0.0419(16) -0.0110(14) -0.0073(12) 0.0017(14) C16 0.0499(18) 0.0397(15) 0.0321(14) -0.0054(12) 0.0057(12) 0.0105(13) C9 0.0598(19) 0.0381(15) 0.0287(14) 0.0055(12) -0.0019(12) -0.0016(14) C8 0.0285(15) 0.088(2) 0.0413(17) -0.0131(17) 0.0068(12) 0.0006(16) C7 0.083(3) 0.0536(19) 0.0392(17) -0.0101(15) -0.0120(16) 0.0370(19) C6 0.085(3) 0.0397(17) 0.0444(18) -0.0034(14) 0.0032(17) -0.0231(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 I1 Al1 2.6400(8) . ? I2 Al2 2.6384(8) . ? Al1 C3 2.173(3) . ? Al1 C4 2.187(2) . ? Al1 C5 2.258(2) . ? Al1 C2 2.273(3) . ? Al1 C1 2.339(3) . ? Al1 Al2 2.5321(10) . ? Al2 C15 2.173(2) . ? Al2 C11 2.182(2) . ? Al2 C14 2.261(2) . ? Al2 C12 2.270(3) . ? Al2 C13 2.344(3) . ? C14 C13 1.411(4) . ? C14 C15 1.437(3) . ? C14 C19 1.511(3) . ? C11 C15 1.428(3) . ? C11 C12 1.430(4) . ? C11 C16 1.504(4) . ? C3 C4 1.421(4) . ? C3 C2 1.424(4) . ? C3 C8 1.504(4) . ? C12 C13 1.414(4) . ? C12 C17 1.508(4) . ? C5 C1 1.420(4) . ? C5 C4 1.426(3) . ? C5 C10 1.507(4) . ? C1 C2 1.421(4) . ? C1 C6 1.501(4) . ? C4 C9 1.500(4) . ? C13 C18 1.503(3) . ? C2 C7 1.509(4) . ? C15 C20 1.503(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 C3 Al1 C4 38.04(10) . . ? C3 Al1 C5 62.47(9) . . ? C4 Al1 C5 37.37(9) . . ? C3 Al1 C2 37.27(10) . . ? C4 Al1 C2 62.13(9) . . ? C5 Al1 C2 60.91(9) . . ? C3 Al1 C1 61.25(10) . . ? C4 Al1 C1 61.13(9) . . ? C5 Al1 C1 35.92(9) . . ? C2 Al1 C1 35.86(10) . . ? C3 Al1 Al2 153.56(8) . . ? C4 Al1 Al2 152.50(8) . . ? C5 Al1 Al2 115.98(7) . . ? C2 Al1 Al2 116.98(8) . . ? C1 Al1 Al2 101.17(7) . . ? C3 Al1 I1 101.93(8) . . ? C4 Al1 I1 98.13(7) . . ? C5 Al1 I1 127.23(7) . . ? C2 Al1 I1 135.15(8) . . ? C1 Al1 I1 159.19(7) . . ? Al2 Al1 I1 98.70(3) . . ? C15 Al2 C11 38.28(9) . . ? C15 Al2 C14 37.76(9) . . ? C11 Al2 C14 62.60(9) . . ? C15 Al2 C12 62.57(9) . . ? C11 Al2 C12 37.41(9) . . ? C14 Al2 C12 60.82(9) . . ? C15 Al2 C13 61.26(9) . . ? C11 Al2 C13 61.06(9) . . ? C14 Al2 C13 35.62(9) . . ? C12 Al2 C13 35.65(9) . . ? C15 Al2 Al1 155.17(8) . . ? C11 Al2 Al1 148.52(8) . . ? C14 Al2 Al1 117.56(7) . . ? C12 Al2 Al1 112.51(7) . . ? C13 Al2 Al1 99.87(7) . . ? C15 Al2 I2 100.81(7) . . ? C11 Al2 I2 99.60(7) . . ? C14 Al2 I2 133.24(7) . . ? C12 Al2 I2 130.26(7) . . ? C13 Al2 I2 160.00(7) . . ? Al1 Al2 I2 99.77(3) . . ? C13 C14 C15 108.1(2) . . ? C13 C14 C19 126.4(2) . . ? C15 C14 C19 125.4(2) . . ? C13 C14 Al2 75.41(14) . . ? C15 C14 Al2 67.79(13) . . ? C19 C14 Al2 125.14(17) . . ? C15 C11 C12 107.7(2) . . ? C15 C11 C16 125.7(2) . . ? C12 C11 C16 126.4(2) . . ? C15 C11 Al2 70.50(13) . . ? C12 C11 Al2 74.61(14) . . ? C16 C11 Al2 123.74(18) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 C8 124.7(3) . . ? C2 C3 C8 127.0(3) . . ? C4 C3 Al1 71.54(14) . . ? C2 C3 Al1 75.18(14) . . ? C8 C3 Al1 123.14(19) . . ? C13 C12 C11 108.2(2) . . ? C13 C12 C17 126.4(2) . . ? C11 C12 C17 125.4(2) . . ? C13 C12 Al2 75.04(14) . . ? C11 C12 Al2 67.98(14) . . ? C17 C12 Al2 125.90(18) . . ? C1 C5 C4 108.2(2) . . ? C1 C5 C10 126.3(2) . . ? C4 C5 C10 125.3(2) . . ? C1 C5 Al1 75.15(14) . . ? C4 C5 Al1 68.62(13) . . ? C10 C5 Al1 125.06(18) . . ? C5 C1 C2 107.9(2) . . ? C5 C1 C6 125.5(3) . . ? C2 C1 C6 126.5(3) . . ? C5 C1 Al1 68.93(14) . . ? C2 C1 Al1 69.52(14) . . ? C6 C1 Al1 123.73(18) . . ? C3 C4 C5 107.7(2) . . ? C3 C4 C9 125.5(2) . . ? C5 C4 C9 126.8(2) . . ? C3 C4 Al1 70.41(14) . . ? C5 C4 Al1 74.00(14) . . ? C9 C4 Al1 123.93(18) . . ? C14 C13 C12 108.5(2) . . ? C14 C13 C18 126.5(2) . . ? C12 C13 C18 124.7(2) . . ? C14 C13 Al2 68.97(14) . . ? C12 C13 Al2 69.30(14) . . ? C18 C13 Al2 123.47(17) . . ? C1 C2 C3 108.1(2) . . ? C1 C2 C7 127.1(3) . . ? C3 C2 C7 124.8(3) . . ? C1 C2 Al1 74.62(15) . . ? C3 C2 Al1 67.55(14) . . ? C7 C2 Al1 125.35(18) . . ? C11 C15 C14 107.4(2) . . ? C11 C15 C20 125.5(2) . . ? C14 C15 C20 127.0(2) . . ? C11 C15 Al2 71.22(13) . . ? C14 C15 Al2 74.44(14) . . ? C20 C15 Al2 123.36(18) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 C3 Al1 Al2 C15 17.8(3) . . . . ? C4 Al1 Al2 C15 109.6(2) . . . . ? C5 Al1 Al2 C15 97.70(19) . . . . ? C2 Al1 Al2 C15 28.7(2) . . . . ? C1 Al1 Al2 C15 63.0(2) . . . . ? I1 Al1 Al2 C15 -123.24(18) . . . . ? C3 Al1 Al2 C11 104.9(2) . . . . ? C4 Al1 Al2 C11 -163.2(2) . . . . ? C5 Al1 Al2 C11 -175.16(15) . . . . ? C2 Al1 Al2 C11 115.87(16) . . . . ? C1 Al1 Al2 C11 150.13(16) . . . . ? I1 Al1 Al2 C11 -36.10(15) . . . . ? C3 Al1 Al2 C14 23.07(19) . . . . ? C4 Al1 Al2 C14 114.94(18) . . . . ? C5 Al1 Al2 C14 103.00(10) . . . . ? C2 Al1 Al2 C14 34.03(12) . . . . ? C1 Al1 Al2 C14 68.29(11) . . . . ? I1 Al1 Al2 C14 -117.94(8) . . . . ? C3 Al1 Al2 C12 90.79(19) . . . . ? C4 Al1 Al2 C12 -177.34(17) . . . . ? C5 Al1 Al2 C12 170.72(10) . . . . ? C2 Al1 Al2 C12 101.75(11) . . . . ? C1 Al1 Al2 C12 136.02(10) . . . . ? I1 Al1 Al2 C12 -50.22(8) . . . . ? C3 Al1 Al2 C13 55.94(18) . . . . ? C4 Al1 Al2 C13 147.81(17) . . . . ? C5 Al1 Al2 C13 135.87(10) . . . . ? C2 Al1 Al2 C13 66.90(11) . . . . ? C1 Al1 Al2 C13 101.17(10) . . . . ? I1 Al1 Al2 C13 -85.07(7) . . . . ? C3 Al1 Al2 I2 -127.85(17) . . . . ? C4 Al1 Al2 I2 -35.98(17) . . . . ? C5 Al1 Al2 I2 -47.92(8) . . . . ? C2 Al1 Al2 I2 -116.89(8) . . . . ? C1 Al1 Al2 I2 -82.62(8) . . . . ? I1 Al1 Al2 I2 91.14(3) . . . . ? C15 Al2 C14 C13 -117.0(2) . . . . ? C11 Al2 C14 C13 -77.74(15) . . . . ? C12 Al2 C14 C13 -35.06(14) . . . . ? Al1 Al2 C14 C13 66.66(14) . . . . ? I2 Al2 C14 C13 -154.46(12) . . . . ? C11 Al2 C14 C15 39.23(14) . . . . ? C12 Al2 C14 C15 81.91(16) . . . . ? C13 Al2 C14 C15 117.0(2) . . . . ? Al1 Al2 C14 C15 -176.37(12) . . . . ? I2 Al2 C14 C15 -37.49(17) . . . . ? C15 Al2 C14 C19 118.6(3) . . . . ? C11 Al2 C14 C19 157.8(3) . . . . ? C12 Al2 C14 C19 -159.5(3) . . . . ? C13 Al2 C14 C19 -124.5(3) . . . . ? Al1 Al2 C14 C19 -57.8(2) . . . . ? I2 Al2 C14 C19 81.1(2) . . . . ? C14 Al2 C11 C15 -38.70(14) . . . . ? C12 Al2 C11 C15 -115.6(2) . . . . ? C13 Al2 C11 C15 -79.26(15) . . . . ? Al1 Al2 C11 C15 -137.39(15) . . . . ? I2 Al2 C11 C15 95.33(14) . . . . ? C15 Al2 C11 C12 115.6(2) . . . . ? C14 Al2 C11 C12 76.93(16) . . . . ? C13 Al2 C11 C12 36.36(14) . . . . ? Al1 Al2 C11 C12 -21.8(2) . . . . ? I2 Al2 C11 C12 -149.05(13) . . . . ? C15 Al2 C11 C16 -120.5(3) . . . . ? C14 Al2 C11 C16 -159.2(3) . . . . ? C12 Al2 C11 C16 123.9(3) . . . . ? C13 Al2 C11 C16 160.2(3) . . . . ? Al1 Al2 C11 C16 102.1(2) . . . . ? I2 Al2 C11 C16 -25.2(2) . . . . ? C5 Al1 C3 C4 37.99(14) . . . . ? C2 Al1 C3 C4 115.3(2) . . . . ? C1 Al1 C3 C4 78.90(16) . . . . ? Al2 Al1 C3 C4 131.51(17) . . . . ? I1 Al1 C3 C4 -87.97(14) . . . . ? C4 Al1 C3 C2 -115.3(2) . . . . ? C5 Al1 C3 C2 -77.27(16) . . . . ? C1 Al1 C3 C2 -36.35(15) . . . . ? Al2 Al1 C3 C2 16.2(3) . . . . ? I1 Al1 C3 C2 156.78(14) . . . . ? C4 Al1 C3 C8 119.9(3) . . . . ? C5 Al1 C3 C8 157.9(3) . . . . ? C2 Al1 C3 C8 -124.9(3) . . . . ? C1 Al1 C3 C8 -161.2(3) . . . . ? Al2 Al1 C3 C8 -108.6(3) . . . . ? I1 Al1 C3 C8 31.9(3) . . . . ? C15 C11 C12 C13 -1.7(3) . . . . ? C16 C11 C12 C13 174.3(2) . . . . ? Al2 C11 C12 C13 -64.81(17) . . . . ? C15 C11 C12 C17 -177.6(2) . . . . ? C16 C11 C12 C17 -1.6(4) . . . . ? Al2 C11 C12 C17 119.2(2) . . . . ? C15 C11 C12 Al2 63.16(16) . . . . ? C16 C11 C12 Al2 -120.9(3) . . . . ? C15 Al2 C12 C13 78.12(16) . . . . ? C11 Al2 C12 C13 117.1(2) . . . . ? C14 Al2 C12 C13 35.03(14) . . . . ? Al1 Al2 C12 C13 -74.98(15) . . . . ? I2 Al2 C12 C13 158.77(12) . . . . ? C15 Al2 C12 C11 -39.01(14) . . . . ? C14 Al2 C12 C11 -82.09(16) . . . . ? C13 Al2 C12 C11 -117.1(2) . . . . ? Al1 Al2 C12 C11 167.90(13) . . . . ? I2 Al2 C12 C11 41.64(17) . . . . ? C15 Al2 C12 C17 -157.5(3) . . . . ? C11 Al2 C12 C17 -118.5(3) . . . . ? C14 Al2 C12 C17 159.4(3) . . . . ? C13 Al2 C12 C17 124.3(3) . . . . ? Al1 Al2 C12 C17 49.4(3) . . . . ? I2 Al2 C12 C17 -76.9(3) . . . . ? C3 Al1 C5 C1 78.16(17) . . . . ? C4 Al1 C5 C1 116.8(2) . . . . ? C2 Al1 C5 C1 35.63(15) . . . . ? Al2 Al1 C5 C1 -72.21(15) . . . . ? I1 Al1 C5 C1 162.23(13) . . . . ? C3 Al1 C5 C4 -38.68(15) . . . . ? C2 Al1 C5 C4 -81.21(16) . . . . ? C1 Al1 C5 C4 -116.8(2) . . . . ? Al2 Al1 C5 C4 170.95(13) . . . . ? I1 Al1 C5 C4 45.39(16) . . . . ? C3 Al1 C5 C10 -157.6(3) . . . . ? C4 Al1 C5 C10 -119.0(3) . . . . ? C2 Al1 C5 C10 159.8(3) . . . . ? C1 Al1 C5 C10 124.2(3) . . . . ? Al2 Al1 C5 C10 52.0(2) . . . . ? I1 Al1 C5 C10 -73.6(2) . . . . ? C4 C5 C1 C2 2.2(3) . . . . ? C10 C5 C1 C2 178.3(2) . . . . ? Al1 C5 C1 C2 -58.79(17) . . . . ? C4 C5 C1 C6 178.2(2) . . . . ? C10 C5 C1 C6 -5.7(4) . . . . ? Al1 C5 C1 C6 117.1(3) . . . . ? C4 C5 C1 Al1 61.03(16) . . . . ? C10 C5 C1 Al1 -122.9(3) . . . . ? C3 Al1 C1 C5 -81.88(16) . . . . ? C4 Al1 C1 C5 -38.20(15) . . . . ? C2 Al1 C1 C5 -119.7(2) . . . . ? Al2 Al1 C1 C5 119.25(14) . . . . ? I1 Al1 C1 C5 -43.2(3) . . . . ? C3 Al1 C1 C2 37.79(15) . . . . ? C4 Al1 C1 C2 81.46(16) . . . . ? C5 Al1 C1 C2 119.7(2) . . . . ? Al2 Al1 C1 C2 -121.08(14) . . . . ? I1 Al1 C1 C2 76.5(3) . . . . ? C3 Al1 C1 C6 158.8(3) . . . . ? C4 Al1 C1 C6 -157.6(3) . . . . ? C5 Al1 C1 C6 -119.4(3) . . . . ? C2 Al1 C1 C6 121.0(3) . . . . ? Al2 Al1 C1 C6 -0.1(3) . . . . ? I1 Al1 C1 C6 -162.5(2) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C8 C3 C4 C5 176.8(2) . . . . ? Al1 C3 C4 C5 -65.14(17) . . . . ? C2 C3 C4 C9 -174.8(2) . . . . ? C8 C3 C4 C9 0.3(4) . . . . ? Al1 C3 C4 C9 118.3(2) . . . . ? C2 C3 C4 Al1 66.88(17) . . . . ? C8 C3 C4 Al1 -118.0(3) . . . . ? C1 C5 C4 C3 -2.5(3) . . . . ? C10 C5 C4 C3 -178.6(2) . . . . ? Al1 C5 C4 C3 62.78(16) . . . . ? C1 C5 C4 C9 174.0(2) . . . . ? C10 C5 C4 C9 -2.1(4) . . . . ? Al1 C5 C4 C9 -120.7(3) . . . . ? C1 C5 C4 Al1 -65.24(17) . . . . ? C10 C5 C4 Al1 118.6(2) . . . . ? C5 Al1 C4 C3 -115.9(2) . . . . ? C2 Al1 C4 C3 -38.28(16) . . . . ? C1 Al1 C4 C3 -79.23(16) . . . . ? Al2 Al1 C4 C3 -133.78(17) . . . . ? I1 Al1 C4 C3 98.99(14) . . . . ? C3 Al1 C4 C5 115.9(2) . . . . ? C2 Al1 C4 C5 77.66(16) . . . . ? C1 Al1 C4 C5 36.71(14) . . . . ? Al2 Al1 C4 C5 -17.8(2) . . . . ? I1 Al1 C4 C5 -145.07(13) . . . . ? C3 Al1 C4 C9 -120.2(3) . . . . ? C5 Al1 C4 C9 123.9(3) . . . . ? C2 Al1 C4 C9 -158.5(3) . . . . ? C1 Al1 C4 C9 160.6(3) . . . . ? Al2 Al1 C4 C9 106.0(2) . . . . ? I1 Al1 C4 C9 -21.2(2) . . . . ? C15 C14 C13 C12 -2.1(3) . . . . ? C19 C14 C13 C12 -178.7(2) . . . . ? Al2 C14 C13 C12 58.11(17) . . . . ? C15 C14 C13 C18 -177.0(2) . . . . ? C19 C14 C13 C18 6.4(4) . . . . ? Al2 C14 C13 C18 -116.8(2) . . . . ? C15 C14 C13 Al2 -60.25(16) . . . . ? C19 C14 C13 Al2 123.2(3) . . . . ? C11 C12 C13 C14 2.4(3) . . . . ? C17 C12 C13 C14 178.2(2) . . . . ? Al2 C12 C13 C14 -57.91(17) . . . . ? C11 C12 C13 C18 177.4(2) . . . . ? C17 C12 C13 C18 -6.8(4) . . . . ? Al2 C12 C13 C18 117.1(2) . . . . ? C11 C12 C13 Al2 60.26(17) . . . . ? C17 C12 C13 Al2 -123.8(3) . . . . ? C15 Al2 C13 C14 38.50(14) . . . . ? C11 Al2 C13 C14 82.46(15) . . . . ? C12 Al2 C13 C14 120.6(2) . . . . ? Al1 Al2 C13 C14 -124.29(13) . . . . ? I2 Al2 C13 C14 66.7(3) . . . . ? C15 Al2 C13 C12 -82.13(16) . . . . ? C11 Al2 C13 C12 -38.16(15) . . . . ? C14 Al2 C13 C12 -120.6(2) . . . . ? Al1 Al2 C13 C12 115.09(14) . . . . ? I2 Al2 C13 C12 -53.9(3) . . . . ? C15 Al2 C13 C18 159.1(3) . . . . ? C11 Al2 C13 C18 -156.9(3) . . . . ? C14 Al2 C13 C18 120.6(3) . . . . ? C12 Al2 C13 C18 -118.7(3) . . . . ? Al1 Al2 C13 C18 -3.6(2) . . . . ? I2 Al2 C13 C18 -172.65(17) . . . . ? C5 C1 C2 C3 -1.2(3) . . . . ? C6 C1 C2 C3 -177.0(2) . . . . ? Al1 C1 C2 C3 -59.57(17) . . . . ? C5 C1 C2 C7 -178.6(2) . . . . ? C6 C1 C2 C7 5.5(4) . . . . ? Al1 C1 C2 C7 123.0(3) . . . . ? C5 C1 C2 Al1 58.42(17) . . . . ? C6 C1 C2 Al1 -117.5(3) . . . . ? C4 C3 C2 C1 -0.4(3) . . . . ? C8 C3 C2 C1 -175.3(2) . . . . ? Al1 C3 C2 C1 64.10(17) . . . . ? C4 C3 C2 C7 177.2(2) . . . . ? C8 C3 C2 C7 2.2(4) . . . . ? Al1 C3 C2 C7 -118.4(2) . . . . ? C4 C3 C2 Al1 -64.48(17) . . . . ? C8 C3 C2 Al1 120.6(3) . . . . ? C3 Al1 C2 C1 -117.5(2) . . . . ? C4 Al1 C2 C1 -78.42(16) . . . . ? C5 Al1 C2 C1 -35.69(14) . . . . ? Al2 Al1 C2 C1 70.53(15) . . . . ? I1 Al1 C2 C1 -150.67(13) . . . . ? C4 Al1 C2 C3 39.09(15) . . . . ? C5 Al1 C2 C3 81.82(16) . . . . ? C1 Al1 C2 C3 117.5(2) . . . . ? Al2 Al1 C2 C3 -171.96(13) . . . . ? I1 Al1 C2 C3 -33.17(19) . . . . ? C3 Al1 C2 C7 117.7(3) . . . . ? C4 Al1 C2 C7 156.8(3) . . . . ? C5 Al1 C2 C7 -160.5(3) . . . . ? C1 Al1 C2 C7 -124.8(3) . . . . ? Al2 Al1 C2 C7 -54.3(3) . . . . ? I1 Al1 C2 C7 84.5(3) . . . . ? C12 C11 C15 C14 0.3(3) . . . . ? C16 C11 C15 C14 -175.7(2) . . . . ? Al2 C11 C15 C14 66.21(16) . . . . ? C12 C11 C15 C20 176.0(2) . . . . ? C16 C11 C15 C20 0.0(4) . . . . ? Al2 C11 C15 C20 -118.1(2) . . . . ? C12 C11 C15 Al2 -65.87(17) . . . . ? C16 C11 C15 Al2 118.1(3) . . . . ? C13 C14 C15 C11 1.1(3) . . . . ? C19 C14 C15 C11 177.7(2) . . . . ? Al2 C14 C15 C11 -64.06(16) . . . . ? C13 C14 C15 C20 -174.5(2) . . . . ? C19 C14 C15 C20 2.1(4) . . . . ? Al2 C14 C15 C20 120.3(3) . . . . ? C13 C14 C15 Al2 65.16(17) . . . . ? C19 C14 C15 Al2 -118.2(2) . . . . ? C14 Al2 C15 C11 115.0(2) . . . . ? C12 Al2 C15 C11 38.11(14) . . . . ? C13 Al2 C15 C11 78.70(15) . . . . ? Al1 Al2 C15 C11 122.68(19) . . . . ? I2 Al2 C15 C11 -91.83(14) . . . . ? C11 Al2 C15 C14 -115.0(2) . . . . ? C12 Al2 C15 C14 -76.88(15) . . . . ? C13 Al2 C15 C14 -36.30(14) . . . . ? Al1 Al2 C15 C14 7.7(3) . . . . ? I2 Al2 C15 C14 153.17(13) . . . . ? C11 Al2 C15 C20 120.6(3) . . . . ? C14 Al2 C15 C20 -124.4(3) . . . . ? C12 Al2 C15 C20 158.8(2) . . . . ? C13 Al2 C15 C20 -160.7(2) . . . . ? Al1 Al2 C15 C20 -116.7(2) . . . . ? I2 Al2 C15 C20 28.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.746 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.064 # Attachment '684337.cif' data_sgm464 _database_code_depnum_ccdc_archive 'CCDC 684337' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H80 Al2 I2 N4, 0.5( C5 H12 )' _chemical_formula_sum 'C70.5 H86 Al2 I2 N4' _chemical_formula_weight 1297.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0663 0.0621 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.7195 2.1212 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6194(10) _cell_length_b 15.9477(15) _cell_length_c 21.317(2) _cell_angle_alpha 105.315(2) _cell_angle_beta 94.491(2) _cell_angle_gamma 102.4080(10) _cell_volume 3365.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4962 _cell_measurement_theta_min 5.000 _cell_measurement_theta_max 46.381 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type 'Beamline 11.3.1 ALS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41370 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.21 _reflns_number_total 15352 _reflns_number_gt 10196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0483P)^2^+0.6125P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15352 _refine_ls_number_parameters 752 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 I2 I -0.08861(3) 0.09102(2) 0.174147(15) 0.04863(10) Uani 1 1 d . . . I1 I 0.09529(3) 0.41567(2) 0.15413(2) 0.07105(14) Uani 1 1 d . . . Al2 Al 0.05533(11) 0.02595(7) 0.23508(6) 0.0325(3) Uani 1 1 d . . . Al1 Al 0.31527(12) 0.45461(8) 0.22735(7) 0.0418(3) Uani 1 1 d . . . N2 N -0.0350(3) -0.0772(2) 0.25877(15) 0.0312(7) Uani 1 1 d . . . N3 N 0.0222(3) -0.1323(2) 0.21945(15) 0.0318(7) Uani 1 1 d . . . N4 N 0.0966(3) -0.0852(2) 0.18933(15) 0.0320(7) Uani 1 1 d . . . N1 N 0.3083(3) 0.3607(2) 0.25465(16) 0.0370(7) Uani 1 1 d . . . C3 C 0.3036(3) 0.1289(3) 0.24293(19) 0.0334(8) Uani 1 1 d . . . H3A H 0.3380 0.0818 0.2189 0.040 Uiso 1 1 calc R . . C4 C 0.2173(4) 0.1099(2) 0.29092(19) 0.0344(8) Uani 1 1 d . . . H4A H 0.2577 0.0777 0.3182 0.041 Uiso 1 1 calc R . . C61 C 0.0368(4) 0.0262(3) 0.42139(19) 0.0367(9) Uani 1 1 d . . . C2 C 0.3368(3) 0.2096(3) 0.23106(19) 0.0344(8) Uani 1 1 d . . . C1 C 0.2904(3) 0.2871(2) 0.26912(19) 0.0332(8) Uani 1 1 d . . . C46 C -0.2236(4) -0.2010(3) 0.25563(19) 0.0345(8) Uani 1 1 d . . . C60 C -0.0791(4) 0.0260(3) 0.38548(18) 0.0333(8) Uani 1 1 d . . . C45 C -0.1427(3) -0.1151(2) 0.28625(18) 0.0308(8) Uani 1 1 d . . . C51 C -0.2016(4) -0.2661(3) 0.19497(19) 0.0353(9) Uani 1 1 d . . . C50 C -0.1684(4) -0.0613(3) 0.34523(19) 0.0334(8) Uani 1 1 d . . . C42 C 0.5216(4) -0.0100(3) 0.1324(2) 0.0494(11) Uani 1 1 d . . . H42A H 0.5674 -0.0054 0.1754 0.074 Uiso 1 1 calc R . . H42B H 0.5304 0.0502 0.1273 0.074 Uiso 1 1 calc R . . H42C H 0.5595 -0.0458 0.0976 0.074 Uiso 1 1 calc R . . C48 C -0.3633(4) -0.1760(3) 0.3402(2) 0.0465(10) Uani 1 1 d . . . H48A H -0.4398 -0.1957 0.3579 0.056 Uiso 1 1 calc R . . C17 C 0.2143(4) 0.3535(3) 0.3782(2) 0.0421(10) Uani 1 1 d . . . C6 C 0.2270(4) 0.2732(3) 0.3263(2) 0.0378(9) Uani 1 1 d . . . C5 C 0.1931(4) 0.1904(3) 0.3344(2) 0.0379(9) Uani 1 1 d . . . H5A H 0.1505 0.1843 0.3710 0.046 Uiso 1 1 calc R . . C39 C 0.1640(4) -0.1001(3) 0.0812(2) 0.0382(9) Uani 1 1 d . . . C35 C 0.1770(4) -0.1290(3) 0.14327(19) 0.0355(9) Uani 1 1 d . . . C18 C 0.3082(4) 0.3871(3) 0.4347(2) 0.0473(11) Uani 1 1 d . . . C52 C -0.1391(4) -0.3332(3) 0.2019(2) 0.0405(9) Uani 1 1 d . . . C38 C 0.2828(4) -0.0588(3) 0.0724(2) 0.0388(9) Uani 1 1 d . . . C47 C -0.3340(4) -0.2307(3) 0.2836(2) 0.0406(9) Uani 1 1 d . . . H47A H -0.3892 -0.2888 0.2637 0.049 Uiso 1 1 calc R . . C31 C 0.3818(4) 0.2179(3) 0.1180(2) 0.0421(10) Uani 1 1 d . . . C65 C -0.1218(4) 0.1059(3) 0.3962(2) 0.0424(10) Uani 1 1 d . . . C54 C -0.1749(4) -0.3972(3) 0.0837(2) 0.0511(11) Uani 1 1 d . . . C37 C 0.3803(4) -0.0541(3) 0.1279(2) 0.0393(9) Uani 1 1 d . . . C26 C 0.4279(4) 0.2237(3) 0.18270(19) 0.0356(9) Uani 1 1 d . . . C27 C 0.5623(4) 0.2418(3) 0.2021(2) 0.0420(10) Uani 1 1 d . . . C56 C -0.2500(4) -0.2637(3) 0.1326(2) 0.0422(10) Uani 1 1 d . . . C40 C 0.1361(5) -0.2307(3) 0.1286(2) 0.0491(11) Uani 1 1 d . . . H40A H 0.0433 -0.2521 0.1107 0.074 Uiso 1 1 calc R . . H40B H 0.1514 -0.2471 0.1692 0.074 Uiso 1 1 calc R . . H40C H 0.1873 -0.2582 0.0964 0.074 Uiso 1 1 calc R . . C49 C -0.2801(4) -0.0926(3) 0.3707(2) 0.0404(9) Uani 1 1 d . . . H49A H -0.2996 -0.0560 0.4098 0.048 Uiso 1 1 calc R . . C62 C 0.1040(4) 0.1047(3) 0.4696(2) 0.0443(10) Uani 1 1 d . . . H62A H 0.1823 0.1042 0.4942 0.053 Uiso 1 1 calc R . . C43 C 0.3188(5) -0.0248(3) 0.0151(2) 0.0510(11) Uani 1 1 d . . . H43A H 0.2394 -0.0262 -0.0123 0.077 Uiso 1 1 calc R . . H43B H 0.3682 -0.0630 -0.0110 0.077 Uiso 1 1 calc R . . H43C H 0.3723 0.0369 0.0314 0.077 Uiso 1 1 calc R . . C11 C 0.4902(5) 0.5268(3) 0.1981(3) 0.0622(14) Uani 1 1 d . . . C59 C -0.3164(5) -0.1923(3) 0.1248(2) 0.0574(12) Uani 1 1 d . . . H59A H -0.3866 -0.1908 0.1520 0.086 Uiso 1 1 calc R . . H59B H -0.3530 -0.2054 0.0786 0.086 Uiso 1 1 calc R . . H59C H -0.2531 -0.1339 0.1387 0.086 Uiso 1 1 calc R . . C66 C 0.0891(4) -0.0567(3) 0.4112(2) 0.0462(10) Uani 1 1 d . . . H66A H 0.0163 -0.1101 0.3987 0.069 Uiso 1 1 calc R . . H66B H 0.1409 -0.0542 0.4520 0.069 Uiso 1 1 calc R . . H66C H 0.1440 -0.0594 0.3762 0.069 Uiso 1 1 calc R . . C41 C 0.3774(5) -0.1010(3) 0.2337(2) 0.0546(12) Uani 1 1 d . . . H41A H 0.4627 -0.0583 0.2491 0.082 Uiso 1 1 calc R . . H41B H 0.3876 -0.1621 0.2276 0.082 Uiso 1 1 calc R . . H41C H 0.3189 -0.0880 0.2664 0.082 Uiso 1 1 calc R . . C9 C 0.4464(5) 0.5706(3) 0.3030(2) 0.0536(12) Uani 1 1 d . . . C53 C -0.1270(4) -0.3967(3) 0.1459(2) 0.0475(11) Uani 1 1 d . . . H53A H -0.0841 -0.4418 0.1504 0.057 Uiso 1 1 calc R . . C36 C 0.3214(4) -0.0925(3) 0.1702(2) 0.0369(9) Uani 1 1 d . . . C29 C 0.6048(5) 0.2520(3) 0.0940(3) 0.0523(12) Uani 1 1 d . . . C8 C 0.3672(4) 0.6040(3) 0.2629(3) 0.0508(11) Uani 1 1 d . . . C30 C 0.4713(5) 0.2322(3) 0.0751(2) 0.0500(11) Uani 1 1 d . . . H30A H 0.4396 0.2284 0.0313 0.060 Uiso 1 1 calc R . . C55 C -0.2350(5) -0.3299(3) 0.0778(2) 0.0537(12) Uani 1 1 d . . . H55A H -0.2668 -0.3287 0.0352 0.064 Uiso 1 1 calc R . . C63 C 0.0617(5) 0.1830(3) 0.4832(2) 0.0507(11) Uani 1 1 d . . . C7 C 0.3980(5) 0.5776(3) 0.1985(3) 0.0575(13) Uani 1 1 d . . . C57 C -0.0846(5) -0.3353(3) 0.2687(2) 0.0511(11) Uani 1 1 d . . . H57A H -0.1532 -0.3359 0.2969 0.077 Uiso 1 1 calc R . . H57B H -0.0130 -0.2820 0.2885 0.077 Uiso 1 1 calc R . . H57C H -0.0520 -0.3893 0.2643 0.077 Uiso 1 1 calc R . . C28 C 0.6478(4) 0.2561(3) 0.1572(3) 0.0520(12) Uani 1 1 d . . . H28A H 0.7389 0.2691 0.1711 0.062 Uiso 1 1 calc R . . C10 C 0.5230(4) 0.5252(3) 0.2634(3) 0.0592(14) Uani 1 1 d . . . C64 C -0.0518(5) 0.1816(3) 0.4443(2) 0.0504(11) Uani 1 1 d . . . H64A H -0.0819 0.2348 0.4514 0.061 Uiso 1 1 calc R . . C25 C 0.0034(5) 0.3546(4) 0.3159(3) 0.0670(15) Uani 1 1 d . . . H25A H -0.0507 0.3971 0.3151 0.100 Uiso 1 1 calc R . . H25B H -0.0501 0.2993 0.3212 0.100 Uiso 1 1 calc R . . H25C H 0.0398 0.3409 0.2747 0.100 Uiso 1 1 calc R . . C23 C 0.4179(5) 0.3417(3) 0.4424(2) 0.0572(12) Uani 1 1 d . . . H23A H 0.4633 0.3366 0.4038 0.086 Uiso 1 1 calc R . . H23B H 0.3818 0.2818 0.4465 0.086 Uiso 1 1 calc R . . H23C H 0.4793 0.3774 0.4819 0.086 Uiso 1 1 calc R . . C22 C 0.1132(4) 0.3958(3) 0.3730(3) 0.0510(11) Uani 1 1 d . . . C68 C -0.2445(5) 0.1095(3) 0.3562(2) 0.0569(12) Uani 1 1 d . . . H68A H -0.2504 0.1720 0.3649 0.085 Uiso 1 1 calc R . . H68B H -0.3211 0.0744 0.3685 0.085 Uiso 1 1 calc R . . H68C H -0.2411 0.0847 0.3093 0.085 Uiso 1 1 calc R . . C34 C 0.2363(4) 0.1939(3) 0.0943(2) 0.0538(12) Uani 1 1 d . . . H34A H 0.2214 0.2066 0.0522 0.081 Uiso 1 1 calc R . . H34B H 0.1937 0.2297 0.1268 0.081 Uiso 1 1 calc R . . H34C H 0.2001 0.1300 0.0887 0.081 Uiso 1 1 calc R . . C44 C 0.0355(4) -0.1235(4) 0.0383(2) 0.0542(12) Uani 1 1 d . . . H44A H 0.0453 -0.0968 0.0020 0.081 Uiso 1 1 calc R . . H44B H -0.0283 -0.1003 0.0643 0.081 Uiso 1 1 calc R . . H44C H 0.0052 -0.1889 0.0206 0.081 Uiso 1 1 calc R . . C20 C 0.2071(5) 0.5081(3) 0.4782(3) 0.0623(14) Uani 1 1 d . . . C21 C 0.1125(5) 0.4730(4) 0.4225(3) 0.0648(15) Uani 1 1 d . . . H21A H 0.0452 0.5028 0.4182 0.078 Uiso 1 1 calc R . . C15 C 0.6200(6) 0.4805(4) 0.2886(5) 0.122(3) Uani 1 1 d . . . H15A H 0.6824 0.5247 0.3247 0.183 Uiso 1 1 calc R . . H15B H 0.6666 0.4561 0.2530 0.183 Uiso 1 1 calc R . . H15C H 0.5737 0.4318 0.3045 0.183 Uiso 1 1 calc R . . C19 C 0.3017(5) 0.4630(3) 0.4835(2) 0.0559(13) Uani 1 1 d . . . H19A H 0.3651 0.4844 0.5217 0.067 Uiso 1 1 calc R . . C12 C 0.3469(7) 0.6034(4) 0.1406(3) 0.104(3) Uani 1 1 d . . . H12A H 0.3975 0.6631 0.1419 0.155 Uiso 1 1 calc R . . H12B H 0.2551 0.6042 0.1421 0.155 Uiso 1 1 calc R . . H12C H 0.3545 0.5597 0.0999 0.155 Uiso 1 1 calc R . . C14 C 0.4483(7) 0.5860(4) 0.3752(3) 0.089(2) Uani 1 1 d . . . H14A H 0.5243 0.6343 0.3987 0.134 Uiso 1 1 calc R . . H14B H 0.4533 0.5309 0.3864 0.134 Uiso 1 1 calc R . . H14C H 0.3686 0.6030 0.3880 0.134 Uiso 1 1 calc R . . C13 C 0.2720(6) 0.6594(4) 0.2839(4) 0.087(2) Uani 1 1 d . . . H13A H 0.3171 0.7231 0.2972 0.130 Uiso 1 1 calc R . . H13B H 0.2338 0.6439 0.3209 0.130 Uiso 1 1 calc R . . H13C H 0.2028 0.6473 0.2471 0.130 Uiso 1 1 calc R . . C32 C 0.6158(4) 0.2461(3) 0.2713(2) 0.0546(12) Uani 1 1 d . . . H32A H 0.5737 0.2833 0.3030 0.082 Uiso 1 1 calc R . . H32B H 0.7100 0.2722 0.2793 0.082 Uiso 1 1 calc R . . H32C H 0.5984 0.1854 0.2762 0.082 Uiso 1 1 calc R . . C67 C 0.1328(6) 0.2650(3) 0.5378(2) 0.0701(16) Uani 1 1 d . . . H67A H 0.2111 0.2535 0.5579 0.105 Uiso 1 1 calc R . . H67B H 0.0757 0.2789 0.5711 0.105 Uiso 1 1 calc R . . H67C H 0.1578 0.3159 0.5200 0.105 Uiso 1 1 calc R . . C33 C 0.6993(6) 0.2718(4) 0.0468(3) 0.0779(18) Uani 1 1 d . . . H33A H 0.7695 0.2414 0.0501 0.117 Uiso 1 1 calc R . . H33B H 0.7363 0.3366 0.0580 0.117 Uiso 1 1 calc R . . H33C H 0.6530 0.2501 0.0018 0.117 Uiso 1 1 calc R . . C24 C 0.2040(6) 0.5937(4) 0.5291(3) 0.090(2) Uani 1 1 d . . . H24A H 0.2311 0.5896 0.5731 0.135 Uiso 1 1 calc R . . H24B H 0.1153 0.6023 0.5264 0.135 Uiso 1 1 calc R . . H24C H 0.2636 0.6446 0.5210 0.135 Uiso 1 1 calc R . . C58 C -0.1624(6) -0.4690(4) 0.0232(3) 0.085(2) Uani 1 1 d . . . H58A H -0.0941 -0.4976 0.0341 0.128 Uiso 1 1 calc R . . H58B H -0.1395 -0.4416 -0.0118 0.128 Uiso 1 1 calc R . . H58C H -0.2455 -0.5142 0.0082 0.128 Uiso 1 1 calc R . . C16 C 0.5501(8) 0.4838(4) 0.1395(4) 0.120(3) Uani 1 1 d . . . H16A H 0.6182 0.5294 0.1304 0.181 Uiso 1 1 calc R . . H16B H 0.4826 0.4571 0.1010 0.181 Uiso 1 1 calc R . . H16C H 0.5883 0.4370 0.1491 0.181 Uiso 1 1 calc R . . C69 C -0.5276(17) -0.1616(12) 0.5132(14) 0.151(13) Uani 0.50 1 d PD A -1 H69A H -0.5906 -0.2191 0.4920 0.227 Uiso 0.50 1 calc PR A -1 H69B H -0.5259 -0.1470 0.5609 0.227 Uiso 0.50 1 calc PR A -1 H69C H -0.4408 -0.1660 0.5024 0.227 Uiso 0.50 1 calc PR A -1 C70 C -0.5673(11) -0.0884(8) 0.4887(8) 0.084(5) Uani 0.50 1 d PD A -1 H70A H -0.6546 -0.0840 0.5003 0.101 Uiso 0.50 1 calc PR A -1 H70B H -0.5743 -0.1057 0.4401 0.101 Uiso 0.50 1 calc PR A -1 C71 C -0.4730(10) 0.0034(7) 0.5167(6) 0.070(4) Uani 0.50 1 d PD A -1 H71A H -0.4765 0.0247 0.5644 0.083 Uiso 0.50 1 calc PR A -1 H71B H -0.3835 -0.0032 0.5113 0.083 Uiso 0.50 1 calc PR A -1 C72 C -0.4994(12) 0.0742(8) 0.4851(9) 0.090(5) Uani 0.50 1 d PD A -1 H72A H -0.4996 0.0519 0.4371 0.107 Uiso 0.50 1 calc PR A -1 H72B H -0.5873 0.0829 0.4923 0.107 Uiso 0.50 1 calc PR A -1 C73 C -0.4007(18) 0.1643(9) 0.5116(10) 0.124(9) Uani 0.50 1 d PD A -1 H73A H -0.4224 0.2061 0.4886 0.186 Uiso 0.50 1 calc PR A -1 H73B H -0.3133 0.1564 0.5047 0.186 Uiso 0.50 1 calc PR A -1 H73C H -0.4028 0.1883 0.5588 0.186 Uiso 0.50 1 calc PR A -1 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 I2 0.04018(16) 0.05332(19) 0.0564(2) 0.02798(15) -0.00264(13) 0.00822(13) I1 0.04746(19) 0.0658(2) 0.1020(3) 0.0506(2) -0.01977(18) -0.00372(16) Al2 0.0301(6) 0.0305(6) 0.0360(6) 0.0138(5) 0.0032(5) 0.0006(5) Al1 0.0373(6) 0.0348(7) 0.0545(8) 0.0233(6) 0.0014(6) 0.0002(5) N2 0.0303(16) 0.0315(16) 0.0299(16) 0.0094(13) 0.0065(13) 0.0020(13) N3 0.0269(15) 0.0339(17) 0.0310(17) 0.0091(14) 0.0039(13) 0.0001(13) N4 0.0304(16) 0.0298(16) 0.0346(17) 0.0126(14) 0.0081(13) -0.0004(13) N1 0.0320(17) 0.0329(17) 0.046(2) 0.0160(15) 0.0027(14) 0.0023(13) C3 0.0285(18) 0.031(2) 0.039(2) 0.0118(17) 0.0003(16) 0.0025(15) C4 0.0324(19) 0.033(2) 0.039(2) 0.0191(17) 0.0025(16) 0.0011(16) C61 0.037(2) 0.042(2) 0.032(2) 0.0178(18) 0.0033(16) 0.0027(17) C2 0.0270(18) 0.033(2) 0.038(2) 0.0124(17) -0.0042(16) -0.0020(15) C1 0.0252(18) 0.031(2) 0.041(2) 0.0146(17) -0.0013(16) -0.0018(15) C46 0.0297(19) 0.035(2) 0.038(2) 0.0142(17) 0.0058(16) 0.0022(16) C60 0.036(2) 0.035(2) 0.0280(19) 0.0120(16) 0.0061(16) 0.0021(16) C45 0.0251(17) 0.0323(19) 0.036(2) 0.0142(16) 0.0056(15) 0.0032(15) C51 0.0307(19) 0.031(2) 0.040(2) 0.0122(17) 0.0047(16) -0.0029(15) C50 0.0301(19) 0.040(2) 0.035(2) 0.0175(17) 0.0051(16) 0.0104(16) C42 0.033(2) 0.049(3) 0.062(3) 0.011(2) 0.013(2) 0.0054(19) C48 0.035(2) 0.056(3) 0.047(3) 0.018(2) 0.0168(19) 0.0021(19) C17 0.043(2) 0.037(2) 0.045(2) 0.0140(19) 0.0159(19) 0.0003(18) C6 0.033(2) 0.038(2) 0.040(2) 0.0175(18) 0.0017(17) -0.0039(16) C5 0.037(2) 0.038(2) 0.035(2) 0.0149(18) 0.0013(17) -0.0032(17) C39 0.034(2) 0.041(2) 0.039(2) 0.0121(18) 0.0082(17) 0.0071(17) C35 0.0301(19) 0.038(2) 0.037(2) 0.0118(18) 0.0105(16) 0.0022(16) C18 0.054(3) 0.039(2) 0.042(2) 0.009(2) 0.013(2) -0.004(2) C52 0.036(2) 0.034(2) 0.047(2) 0.0138(19) 0.0053(18) -0.0022(17) C38 0.042(2) 0.036(2) 0.041(2) 0.0125(18) 0.0150(18) 0.0089(18) C47 0.031(2) 0.039(2) 0.045(2) 0.0124(19) 0.0047(17) -0.0050(17) C31 0.042(2) 0.034(2) 0.045(2) 0.0130(19) 0.0049(19) -0.0021(17) C65 0.051(3) 0.040(2) 0.040(2) 0.0163(19) 0.0086(19) 0.0125(19) C54 0.046(3) 0.047(3) 0.050(3) 0.005(2) 0.016(2) -0.002(2) C37 0.032(2) 0.036(2) 0.050(2) 0.0132(19) 0.0106(18) 0.0053(17) C26 0.0305(19) 0.034(2) 0.040(2) 0.0123(17) 0.0019(16) 0.0013(16) C27 0.030(2) 0.038(2) 0.060(3) 0.019(2) 0.0041(19) 0.0066(17) C56 0.040(2) 0.047(2) 0.035(2) 0.0140(19) 0.0039(18) -0.0018(19) C40 0.053(3) 0.041(2) 0.052(3) 0.011(2) 0.023(2) 0.006(2) C49 0.038(2) 0.045(2) 0.039(2) 0.0131(19) 0.0122(18) 0.0091(18) C62 0.045(2) 0.049(3) 0.035(2) 0.019(2) 0.0030(18) -0.003(2) C43 0.051(3) 0.060(3) 0.047(3) 0.023(2) 0.022(2) 0.008(2) C11 0.061(3) 0.037(3) 0.074(4) 0.007(2) 0.027(3) -0.014(2) C59 0.058(3) 0.064(3) 0.049(3) 0.024(2) -0.003(2) 0.008(2) C66 0.043(2) 0.055(3) 0.048(3) 0.024(2) 0.006(2) 0.017(2) C41 0.049(3) 0.062(3) 0.058(3) 0.027(2) 0.001(2) 0.012(2) C9 0.053(3) 0.038(2) 0.063(3) 0.025(2) -0.001(2) -0.012(2) C53 0.046(2) 0.033(2) 0.058(3) 0.008(2) 0.015(2) 0.0026(19) C36 0.031(2) 0.037(2) 0.043(2) 0.0138(18) 0.0046(17) 0.0080(16) C29 0.052(3) 0.039(2) 0.064(3) 0.014(2) 0.027(2) 0.001(2) C8 0.042(2) 0.038(2) 0.069(3) 0.020(2) 0.003(2) -0.0011(19) C30 0.061(3) 0.045(3) 0.038(2) 0.013(2) 0.009(2) -0.002(2) C55 0.051(3) 0.058(3) 0.041(3) 0.012(2) 0.003(2) -0.008(2) C63 0.068(3) 0.044(3) 0.035(2) 0.014(2) 0.013(2) -0.003(2) C7 0.065(3) 0.039(2) 0.062(3) 0.025(2) -0.003(2) -0.012(2) C57 0.054(3) 0.045(3) 0.056(3) 0.020(2) 0.002(2) 0.009(2) C28 0.036(2) 0.043(3) 0.079(4) 0.020(2) 0.017(2) 0.0068(19) C10 0.036(2) 0.032(2) 0.106(4) 0.029(3) -0.005(3) -0.0063(18) C64 0.069(3) 0.041(2) 0.047(3) 0.017(2) 0.020(2) 0.017(2) C25 0.040(3) 0.073(4) 0.090(4) 0.032(3) 0.008(3) 0.010(2) C23 0.063(3) 0.054(3) 0.042(3) 0.007(2) -0.009(2) 0.004(2) C22 0.038(2) 0.046(3) 0.069(3) 0.021(2) 0.018(2) 0.002(2) C68 0.063(3) 0.063(3) 0.056(3) 0.024(3) 0.007(2) 0.032(3) C34 0.049(3) 0.060(3) 0.046(3) 0.017(2) -0.006(2) 0.001(2) C44 0.037(2) 0.075(3) 0.047(3) 0.021(2) 0.003(2) 0.004(2) C20 0.064(3) 0.045(3) 0.068(3) 0.009(3) 0.025(3) -0.005(2) C21 0.053(3) 0.058(3) 0.093(4) 0.026(3) 0.041(3) 0.020(3) C15 0.053(3) 0.056(4) 0.251(10) 0.067(5) -0.036(5) -0.006(3) C19 0.060(3) 0.046(3) 0.052(3) 0.008(2) 0.017(2) -0.004(2) C12 0.132(6) 0.068(4) 0.087(4) 0.051(4) -0.040(4) -0.038(4) C14 0.102(5) 0.083(4) 0.064(4) 0.038(3) -0.007(3) -0.034(4) C13 0.067(4) 0.052(3) 0.137(6) 0.017(4) 0.024(4) 0.017(3) C32 0.034(2) 0.059(3) 0.070(3) 0.028(3) -0.006(2) 0.003(2) C67 0.085(4) 0.055(3) 0.049(3) 0.004(2) 0.005(3) -0.013(3) C33 0.078(4) 0.057(3) 0.095(4) 0.017(3) 0.052(3) -0.002(3) C24 0.079(4) 0.060(4) 0.107(5) -0.008(3) 0.047(4) -0.003(3) C58 0.090(4) 0.073(4) 0.066(4) -0.017(3) 0.019(3) 0.007(3) C16 0.117(6) 0.068(4) 0.131(6) -0.016(4) 0.072(5) -0.037(4) C69 0.128(18) 0.133(18) 0.27(3) 0.11(2) 0.13(2) 0.090(16) C70 0.062(9) 0.096(12) 0.094(12) 0.016(10) 0.035(9) 0.026(9) C71 0.047(9) 0.101(9) 0.082(12) 0.043(9) 0.031(7) 0.034(8) C72 0.068(10) 0.098(12) 0.119(15) 0.050(11) 0.045(10) 0.019(9) C73 0.18(2) 0.069(11) 0.146(17) 0.038(11) 0.111(18) 0.041(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I2 Al2 2.4867(12) . ? I1 Al1 2.5637(13) . ? Al2 N2 1.928(3) . ? Al2 N4 1.942(3) . ? Al2 C4 2.004(4) . ? Al2 N3 2.400(3) . ? Al1 N1 1.734(3) . ? Al1 C11 2.192(5) . ? Al1 C9 2.220(5) . ? Al1 C10 2.221(4) . ? Al1 C8 2.230(5) . ? Al1 C7 2.231(4) . ? N2 N3 1.327(4) . ? N2 C45 1.419(4) . ? N3 N4 1.297(4) . ? N4 C35 1.486(5) . ? N1 C1 1.271(5) . ? C3 C2 1.354(5) . ? C3 C4 1.473(5) . ? C3 H3A 0.9500 . ? C4 C5 1.457(6) . ? C4 H4A 1.0000 . ? C61 C60 1.396(5) . ? C61 C62 1.399(6) . ? C61 C66 1.511(6) . ? C2 C1 1.491(6) . ? C2 C26 1.495(5) . ? C1 C6 1.481(5) . ? C46 C47 1.405(5) . ? C46 C45 1.406(5) . ? C46 C51 1.499(6) . ? C60 C65 1.412(6) . ? C60 C50 1.499(5) . ? C45 C50 1.406(5) . ? C51 C56 1.401(6) . ? C51 C52 1.407(6) . ? C50 C49 1.392(5) . ? C42 C37 1.498(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C48 C49 1.385(6) . ? C48 C47 1.390(6) . ? C48 H48A 0.9500 . ? C17 C22 1.397(6) . ? C17 C18 1.405(6) . ? C17 C6 1.493(6) . ? C6 C5 1.353(5) . ? C5 H5A 0.9500 . ? C39 C38 1.342(5) . ? C39 C44 1.498(6) . ? C39 C35 1.519(5) . ? C35 C36 1.523(5) . ? C35 C40 1.524(6) . ? C18 C19 1.390(6) . ? C18 C23 1.518(7) . ? C52 C53 1.381(6) . ? C52 C57 1.507(6) . ? C38 C37 1.484(6) . ? C38 C43 1.505(6) . ? C47 H47A 0.9500 . ? C31 C30 1.393(6) . ? C31 C26 1.400(6) . ? C31 C34 1.520(6) . ? C65 C64 1.379(6) . ? C65 C68 1.521(6) . ? C54 C53 1.380(7) . ? C54 C55 1.389(7) . ? C54 C58 1.518(7) . ? C37 C36 1.340(5) . ? C26 C27 1.400(5) . ? C27 C28 1.399(6) . ? C27 C32 1.515(6) . ? C56 C55 1.398(6) . ? C56 C59 1.500(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C49 H49A 0.9500 . ? C62 C63 1.385(7) . ? C62 H62A 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C11 C7 1.398(8) . ? C11 C10 1.416(8) . ? C11 C16 1.516(8) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C41 C36 1.487(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C9 C10 1.390(7) . ? C9 C8 1.428(6) . ? C9 C14 1.491(7) . ? C53 H53A 0.9500 . ? C29 C28 1.368(7) . ? C29 C30 1.387(7) . ? C29 C33 1.520(6) . ? C8 C7 1.412(7) . ? C8 C13 1.499(7) . ? C30 H30A 0.9500 . ? C55 H55A 0.9500 . ? C63 C64 1.401(7) . ? C63 C67 1.506(6) . ? C7 C12 1.499(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C28 H28A 0.9500 . ? C10 C15 1.513(7) . ? C64 H64A 0.9500 . ? C25 C22 1.515(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 C21 1.397(7) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C20 C19 1.370(8) . ? C20 C21 1.398(8) . ? C20 C24 1.511(7) . ? C21 H21A 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 H19A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C69 C70 1.522(9) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.522(8) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.521(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.521(9) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? 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 N2 Al2 N4 66.16(13) . . ? N2 Al2 C4 121.31(15) . . ? N4 Al2 C4 108.87(15) . . ? N2 Al2 N3 33.53(11) . . ? N4 Al2 N3 32.65(11) . . ? C4 Al2 N3 119.38(14) . . ? N2 Al2 I2 114.17(10) . . ? N4 Al2 I2 118.92(11) . . ? C4 Al2 I2 117.20(12) . . ? N3 Al2 I2 122.98(8) . . ? N1 Al1 C11 123.9(2) . . ? N1 Al1 C9 107.51(17) . . ? C11 Al1 C9 62.09(19) . . ? N1 Al1 C10 99.54(17) . . ? C11 Al1 C10 37.4(2) . . ? C9 Al1 C10 36.50(19) . . ? N1 Al1 C8 141.82(18) . . ? C11 Al1 C8 62.12(18) . . ? C9 Al1 C8 37.44(17) . . ? C10 Al1 C8 61.71(17) . . ? N1 Al1 C7 159.95(19) . . ? C11 Al1 C7 36.8(2) . . ? C9 Al1 C7 61.71(17) . . ? C10 Al1 C7 61.43(18) . . ? C8 Al1 C7 36.90(18) . . ? N1 Al1 I1 102.90(12) . . ? C11 Al1 I1 119.56(18) . . ? C9 Al1 I1 139.27(15) . . ? C10 Al1 I1 155.75(15) . . ? C8 Al1 I1 103.87(13) . . ? C7 Al1 I1 95.09(14) . . ? N3 N2 C45 118.2(3) . . ? N3 N2 Al2 93.1(2) . . ? C45 N2 Al2 146.6(3) . . ? N4 N3 N2 107.2(3) . . ? N4 N3 Al2 53.89(18) . . ? N2 N3 Al2 53.34(17) . . ? N3 N4 C35 119.2(3) . . ? N3 N4 Al2 93.5(2) . . ? C35 N4 Al2 147.1(2) . . ? C1 N1 Al1 172.6(3) . . ? C2 C3 C4 123.8(4) . . ? C2 C3 H3A 118.1 . . ? C4 C3 H3A 118.1 . . ? C5 C4 C3 113.2(3) . . ? C5 C4 Al2 113.2(3) . . ? C3 C4 Al2 103.9(3) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? Al2 C4 H4A 108.8 . . ? C60 C61 C62 118.9(4) . . ? C60 C61 C66 121.9(4) . . ? C62 C61 C66 119.2(4) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 C26 120.3(4) . . ? C1 C2 C26 119.0(3) . . ? N1 C1 C6 122.6(4) . . ? N1 C1 C2 122.1(4) . . ? C6 C1 C2 115.3(3) . . ? C47 C46 C45 118.7(4) . . ? C47 C46 C51 115.9(3) . . ? C45 C46 C51 125.4(3) . . ? C61 C60 C65 119.4(4) . . ? C61 C60 C50 119.8(3) . . ? C65 C60 C50 119.9(3) . . ? C46 C45 C50 120.7(3) . . ? C46 C45 N2 122.4(3) . . ? C50 C45 N2 116.8(3) . . ? C56 C51 C52 120.6(4) . . ? C56 C51 C46 120.4(4) . . ? C52 C51 C46 118.8(4) . . ? C49 C50 C45 118.6(4) . . ? C49 C50 C60 116.9(4) . . ? C45 C50 C60 124.3(3) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C49 C48 C47 119.6(4) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C22 C17 C18 119.0(4) . . ? C22 C17 C6 122.8(4) . . ? C18 C17 C6 118.2(4) . . ? C5 C6 C1 120.4(4) . . ? C5 C6 C17 120.6(4) . . ? C1 C6 C17 118.6(3) . . ? C6 C5 C4 124.7(4) . . ? C6 C5 H5A 117.6 . . ? C4 C5 H5A 117.6 . . ? C38 C39 C44 130.0(4) . . ? C38 C39 C35 108.6(4) . . ? C44 C39 C35 121.2(3) . . ? N4 C35 C39 108.3(3) . . ? N4 C35 C36 110.6(3) . . ? C39 C35 C36 103.5(3) . . ? N4 C35 C40 111.0(3) . . ? C39 C35 C40 111.7(3) . . ? C36 C35 C40 111.5(3) . . ? C19 C18 C17 119.9(5) . . ? C19 C18 C23 119.8(4) . . ? C17 C18 C23 120.3(4) . . ? C53 C52 C51 118.6(4) . . ? C53 C52 C57 120.4(4) . . ? C51 C52 C57 121.0(4) . . ? C39 C38 C37 109.5(4) . . ? C39 C38 C43 127.5(4) . . ? C37 C38 C43 122.9(4) . . ? C48 C47 C46 120.7(4) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? C30 C31 C26 119.0(4) . . ? C30 C31 C34 120.5(4) . . ? C26 C31 C34 120.4(4) . . ? C64 C65 C60 119.3(4) . . ? C64 C65 C68 119.5(4) . . ? C60 C65 C68 121.1(4) . . ? C53 C54 C55 118.2(4) . . ? C53 C54 C58 121.2(5) . . ? C55 C54 C58 120.7(5) . . ? C36 C37 C38 109.9(3) . . ? C36 C37 C42 128.3(4) . . ? C38 C37 C42 121.8(4) . . ? C31 C26 C27 119.1(4) . . ? C31 C26 C2 121.5(3) . . ? C27 C26 C2 119.4(3) . . ? C28 C27 C26 119.5(4) . . ? C28 C27 C32 119.8(4) . . ? C26 C27 C32 120.7(4) . . ? C55 C56 C51 118.1(4) . . ? C55 C56 C59 120.9(4) . . ? C51 C56 C59 121.0(4) . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C48 C49 C50 121.5(4) . . ? C48 C49 H49A 119.2 . . ? C50 C49 H49A 119.2 . . ? C63 C62 C61 123.0(4) . . ? C63 C62 H62A 118.5 . . ? C61 C62 H62A 118.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C7 C11 C10 107.8(5) . . ? C7 C11 C16 126.9(6) . . ? C10 C11 C16 125.3(6) . . ? C7 C11 Al1 73.1(3) . . ? C10 C11 Al1 72.4(3) . . ? C16 C11 Al1 122.1(3) . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C10 C9 C8 108.2(4) . . ? C10 C9 C14 127.0(5) . . ? C8 C9 C14 124.8(5) . . ? C10 C9 Al1 71.8(3) . . ? C8 C9 Al1 71.7(3) . . ? C14 C9 Al1 124.1(3) . . ? C54 C53 C52 122.4(4) . . ? C54 C53 H53A 118.8 . . ? C52 C53 H53A 118.8 . . ? C37 C36 C41 129.5(4) . . ? C37 C36 C35 108.4(3) . . ? C41 C36 C35 122.1(4) . . ? C28 C29 C30 117.5(4) . . ? C28 C29 C33 121.6(5) . . ? C30 C29 C33 120.9(5) . . ? C7 C8 C9 107.0(4) . . ? C7 C8 C13 125.1(5) . . ? C9 C8 C13 127.9(5) . . ? C7 C8 Al1 71.6(3) . . ? C9 C8 Al1 70.9(3) . . ? C13 C8 Al1 124.2(3) . . ? C29 C30 C31 122.6(4) . . ? C29 C30 H30A 118.7 . . ? C31 C30 H30A 118.7 . . ? C54 C55 C56 122.0(4) . . ? C54 C55 H55A 119.0 . . ? C56 C55 H55A 119.0 . . ? C62 C63 C64 116.6(4) . . ? C62 C63 C67 121.6(5) . . ? C64 C63 C67 121.8(5) . . ? C11 C7 C8 108.6(5) . . ? C11 C7 C12 125.1(6) . . ? C8 C7 C12 126.3(6) . . ? C11 C7 Al1 70.0(3) . . ? C8 C7 Al1 71.5(3) . . ? C12 C7 Al1 126.8(3) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C29 C28 C27 122.3(4) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C9 C10 C11 108.3(4) . . ? C9 C10 C15 123.5(6) . . ? C11 C10 C15 128.1(6) . . ? C9 C10 Al1 71.7(3) . . ? C11 C10 Al1 70.2(3) . . ? C15 C10 Al1 122.4(3) . . ? C65 C64 C63 122.7(4) . . ? C65 C64 H64A 118.7 . . ? C63 C64 H64A 118.7 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 C17 118.9(5) . . ? C21 C22 C25 121.3(5) . . ? C17 C22 C25 119.7(4) . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C19 C20 C21 117.4(5) . . ? C19 C20 C24 122.5(6) . . ? C21 C20 C24 120.1(6) . . ? C22 C21 C20 122.4(5) . . ? C22 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C20 C19 C18 122.3(5) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C63 C67 H67A 109.5 . . ? C63 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C63 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C69 C70 C71 113.8(10) . . ? C69 C70 H70A 108.8 . . ? C71 C70 H70A 108.8 . . ? C69 C70 H70B 108.8 . . ? C71 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C72 C71 C70 114.6(9) . . ? C72 C71 H71A 108.6 . . ? C70 C71 H71A 108.6 . . ? C72 C71 H71B 108.6 . . ? C70 C71 H71B 108.6 . . ? H71A C71 H71B 107.6 . . ? C73 C72 C71 113.8(10) . . ? C73 C72 H72A 108.8 . . ? C71 C72 H72A 108.8 . . ? C73 C72 H72B 108.8 . . ? C71 C72 H72B 108.8 . . ? H72A C72 H72B 107.7 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? 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 N4 Al2 N2 N3 1.35(19) . . . . ? C4 Al2 N2 N3 -97.0(2) . . . . ? I2 Al2 N2 N3 113.75(18) . . . . ? N4 Al2 N2 C45 -159.4(5) . . . . ? C4 Al2 N2 C45 102.2(5) . . . . ? N3 Al2 N2 C45 -160.8(6) . . . . ? I2 Al2 N2 C45 -47.0(5) . . . . ? C45 N2 N3 N4 166.2(3) . . . . ? Al2 N2 N3 N4 -1.9(3) . . . . ? C45 N2 N3 Al2 168.1(4) . . . . ? N2 Al2 N3 N4 177.7(3) . . . . ? C4 Al2 N3 N4 -79.0(3) . . . . ? I2 Al2 N3 N4 93.2(2) . . . . ? N4 Al2 N3 N2 -177.7(3) . . . . ? C4 Al2 N3 N2 103.3(2) . . . . ? I2 Al2 N3 N2 -84.5(2) . . . . ? N2 N3 N4 C35 178.0(3) . . . . ? Al2 N3 N4 C35 176.1(4) . . . . ? N2 N3 N4 Al2 1.9(3) . . . . ? N2 Al2 N4 N3 -1.38(19) . . . . ? C4 Al2 N4 N3 115.3(2) . . . . ? I2 Al2 N4 N3 -106.9(2) . . . . ? N2 Al2 N4 C35 -175.1(5) . . . . ? C4 Al2 N4 C35 -58.4(5) . . . . ? N3 Al2 N4 C35 -173.7(6) . . . . ? I2 Al2 N4 C35 79.4(5) . . . . ? C2 C3 C4 C5 -12.4(5) . . . . ? C2 C3 C4 Al2 110.7(4) . . . . ? N2 Al2 C4 C5 -98.8(3) . . . . ? N4 Al2 C4 C5 -171.8(2) . . . . ? N3 Al2 C4 C5 -137.8(2) . . . . ? I2 Al2 C4 C5 49.5(3) . . . . ? N2 Al2 C4 C3 138.0(2) . . . . ? N4 Al2 C4 C3 65.0(3) . . . . ? N3 Al2 C4 C3 99.0(2) . . . . ? I2 Al2 C4 C3 -73.6(3) . . . . ? C4 C3 C2 C1 2.6(6) . . . . ? C4 C3 C2 C26 178.4(3) . . . . ? C3 C2 C1 N1 -172.5(4) . . . . ? C26 C2 C1 N1 11.6(5) . . . . ? C3 C2 C1 C6 9.8(5) . . . . ? C26 C2 C1 C6 -166.1(3) . . . . ? C62 C61 C60 C65 3.3(6) . . . . ? C66 C61 C60 C65 -178.7(4) . . . . ? C62 C61 C60 C50 -165.8(3) . . . . ? C66 C61 C60 C50 12.2(6) . . . . ? C47 C46 C45 C50 2.6(6) . . . . ? C51 C46 C45 C50 -176.4(4) . . . . ? C47 C46 C45 N2 -175.2(3) . . . . ? C51 C46 C45 N2 5.8(6) . . . . ? N3 N2 C45 C46 -26.7(5) . . . . ? Al2 N2 C45 C46 131.4(4) . . . . ? N3 N2 C45 C50 155.5(3) . . . . ? Al2 N2 C45 C50 -46.5(6) . . . . ? C47 C46 C51 C56 93.3(4) . . . . ? C45 C46 C51 C56 -87.7(5) . . . . ? C47 C46 C51 C52 -82.6(5) . . . . ? C45 C46 C51 C52 96.4(5) . . . . ? C46 C45 C50 C49 -3.7(5) . . . . ? N2 C45 C50 C49 174.2(3) . . . . ? C46 C45 C50 C60 172.2(3) . . . . ? N2 C45 C50 C60 -9.9(5) . . . . ? C61 C60 C50 C49 103.7(4) . . . . ? C65 C60 C50 C49 -65.4(5) . . . . ? C61 C60 C50 C45 -72.3(5) . . . . ? C65 C60 C50 C45 118.6(4) . . . . ? N1 C1 C6 C5 170.4(4) . . . . ? C2 C1 C6 C5 -11.9(5) . . . . ? N1 C1 C6 C17 -16.0(6) . . . . ? C2 C1 C6 C17 161.7(3) . . . . ? C22 C17 C6 C5 -103.2(5) . . . . ? C18 C17 C6 C5 76.5(5) . . . . ? C22 C17 C6 C1 83.2(5) . . . . ? C18 C17 C6 C1 -97.1(4) . . . . ? C1 C6 C5 C4 1.7(6) . . . . ? C17 C6 C5 C4 -171.7(4) . . . . ? C3 C4 C5 C6 10.3(5) . . . . ? Al2 C4 C5 C6 -107.6(4) . . . . ? N3 N4 C35 C39 134.6(3) . . . . ? Al2 N4 C35 C39 -52.6(6) . . . . ? N3 N4 C35 C36 -112.6(4) . . . . ? Al2 N4 C35 C36 60.1(6) . . . . ? N3 N4 C35 C40 11.7(5) . . . . ? Al2 N4 C35 C40 -175.5(4) . . . . ? C38 C39 C35 N4 120.6(4) . . . . ? C44 C39 C35 N4 -63.2(5) . . . . ? C38 C39 C35 C36 3.1(4) . . . . ? C44 C39 C35 C36 179.4(4) . . . . ? C38 C39 C35 C40 -116.9(4) . . . . ? C44 C39 C35 C40 59.3(5) . . . . ? C22 C17 C18 C19 -1.9(6) . . . . ? C6 C17 C18 C19 178.4(4) . . . . ? C22 C17 C18 C23 178.9(4) . . . . ? C6 C17 C18 C23 -0.8(6) . . . . ? C56 C51 C52 C53 -0.2(6) . . . . ? C46 C51 C52 C53 175.7(3) . . . . ? C56 C51 C52 C57 178.8(4) . . . . ? C46 C51 C52 C57 -5.3(5) . . . . ? C44 C39 C38 C37 -177.9(4) . . . . ? C35 C39 C38 C37 -2.1(5) . . . . ? C44 C39 C38 C43 -0.5(8) . . . . ? C35 C39 C38 C43 175.3(4) . . . . ? C49 C48 C47 C46 -2.4(6) . . . . ? C45 C46 C47 C48 0.5(6) . . . . ? C51 C46 C47 C48 179.6(4) . . . . ? C61 C60 C65 C64 -3.3(6) . . . . ? C50 C60 C65 C64 165.8(4) . . . . ? C61 C60 C65 C68 177.5(4) . . . . ? C50 C60 C65 C68 -13.4(6) . . . . ? C39 C38 C37 C36 0.1(5) . . . . ? C43 C38 C37 C36 -177.5(4) . . . . ? C39 C38 C37 C42 -178.8(4) . . . . ? C43 C38 C37 C42 3.7(6) . . . . ? C30 C31 C26 C27 -1.5(6) . . . . ? C34 C31 C26 C27 177.0(4) . . . . ? C30 C31 C26 C2 179.6(4) . . . . ? C34 C31 C26 C2 -1.8(6) . . . . ? C3 C2 C26 C31 97.8(5) . . . . ? C1 C2 C26 C31 -86.2(5) . . . . ? C3 C2 C26 C27 -81.0(5) . . . . ? C1 C2 C26 C27 94.9(4) . . . . ? C31 C26 C27 C28 1.9(6) . . . . ? C2 C26 C27 C28 -179.3(4) . . . . ? C31 C26 C27 C32 -178.3(4) . . . . ? C2 C26 C27 C32 0.6(6) . . . . ? C52 C51 C56 C55 0.3(6) . . . . ? C46 C51 C56 C55 -175.5(4) . . . . ? C52 C51 C56 C59 -179.8(4) . . . . ? C46 C51 C56 C59 4.3(6) . . . . ? C47 C48 C49 C50 1.2(7) . . . . ? C45 C50 C49 C48 1.8(6) . . . . ? C60 C50 C49 C48 -174.4(4) . . . . ? C60 C61 C62 C63 -0.7(6) . . . . ? C66 C61 C62 C63 -178.7(4) . . . . ? N1 Al1 C11 C7 -172.3(3) . . . . ? C9 Al1 C11 C7 -79.2(3) . . . . ? C10 Al1 C11 C7 -115.6(4) . . . . ? C8 Al1 C11 C7 -36.6(3) . . . . ? I1 Al1 C11 C7 54.1(3) . . . . ? N1 Al1 C11 C10 -56.7(4) . . . . ? C9 Al1 C11 C10 36.4(3) . . . . ? C8 Al1 C11 C10 79.0(3) . . . . ? C7 Al1 C11 C10 115.6(4) . . . . ? I1 Al1 C11 C10 169.7(3) . . . . ? N1 Al1 C11 C16 64.3(7) . . . . ? C9 Al1 C11 C16 157.5(7) . . . . ? C10 Al1 C11 C16 121.1(7) . . . . ? C8 Al1 C11 C16 -159.9(7) . . . . ? C7 Al1 C11 C16 -123.3(8) . . . . ? I1 Al1 C11 C16 -69.3(6) . . . . ? N1 Al1 C9 C10 82.3(3) . . . . ? C11 Al1 C9 C10 -37.3(3) . . . . ? C8 Al1 C9 C10 -117.0(4) . . . . ? C7 Al1 C9 C10 -79.3(3) . . . . ? I1 Al1 C9 C10 -141.2(3) . . . . ? N1 Al1 C9 C8 -160.7(3) . . . . ? C11 Al1 C9 C8 79.7(3) . . . . ? C10 Al1 C9 C8 117.0(4) . . . . ? C7 Al1 C9 C8 37.7(3) . . . . ? I1 Al1 C9 C8 -24.2(4) . . . . ? N1 Al1 C9 C14 -40.5(6) . . . . ? C11 Al1 C9 C14 -160.1(6) . . . . ? C10 Al1 C9 C14 -122.8(6) . . . . ? C8 Al1 C9 C14 120.1(6) . . . . ? C7 Al1 C9 C14 157.9(6) . . . . ? I1 Al1 C9 C14 95.9(5) . . . . ? C55 C54 C53 C52 1.3(6) . . . . ? C58 C54 C53 C52 -178.8(4) . . . . ? C51 C52 C53 C54 -0.6(6) . . . . ? C57 C52 C53 C54 -179.7(4) . . . . ? C38 C37 C36 C41 -177.5(4) . . . . ? C42 C37 C36 C41 1.3(8) . . . . ? C38 C37 C36 C35 2.0(5) . . . . ? C42 C37 C36 C35 -179.2(4) . . . . ? N4 C35 C36 C37 -118.8(4) . . . . ? C39 C35 C36 C37 -3.1(4) . . . . ? C40 C35 C36 C37 117.1(4) . . . . ? N4 C35 C36 C41 60.7(5) . . . . ? C39 C35 C36 C41 176.4(4) . . . . ? C40 C35 C36 C41 -63.4(5) . . . . ? C10 C9 C8 C7 0.0(5) . . . . ? C14 C9 C8 C7 177.8(4) . . . . ? Al1 C9 C8 C7 -62.9(3) . . . . ? C10 C9 C8 C13 -178.1(5) . . . . ? C14 C9 C8 C13 -0.3(7) . . . . ? Al1 C9 C8 C13 119.0(5) . . . . ? C10 C9 C8 Al1 63.0(3) . . . . ? C14 C9 C8 Al1 -119.3(4) . . . . ? N1 Al1 C8 C7 146.9(3) . . . . ? C11 Al1 C8 C7 36.6(3) . . . . ? C9 Al1 C8 C7 116.2(4) . . . . ? C10 Al1 C8 C7 79.2(3) . . . . ? I1 Al1 C8 C7 -79.8(3) . . . . ? N1 Al1 C8 C9 30.7(4) . . . . ? C11 Al1 C8 C9 -79.6(3) . . . . ? C10 Al1 C8 C9 -37.0(3) . . . . ? C7 Al1 C8 C9 -116.2(4) . . . . ? I1 Al1 C8 C9 164.0(3) . . . . ? N1 Al1 C8 C13 -92.6(5) . . . . ? C11 Al1 C8 C13 157.0(6) . . . . ? C9 Al1 C8 C13 -123.3(6) . . . . ? C10 Al1 C8 C13 -160.3(6) . . . . ? C7 Al1 C8 C13 120.5(6) . . . . ? I1 Al1 C8 C13 40.7(5) . . . . ? C28 C29 C30 C31 0.8(7) . . . . ? C33 C29 C30 C31 -176.9(4) . . . . ? C26 C31 C30 C29 0.2(7) . . . . ? C34 C31 C30 C29 -178.3(4) . . . . ? C53 C54 C55 C56 -1.2(7) . . . . ? C58 C54 C55 C56 178.9(4) . . . . ? C51 C56 C55 C54 0.4(6) . . . . ? C59 C56 C55 C54 -179.4(4) . . . . ? C61 C62 C63 C64 -2.0(6) . . . . ? C61 C62 C63 C67 176.8(4) . . . . ? C10 C11 C7 C8 -3.1(5) . . . . ? C16 C11 C7 C8 179.3(4) . . . . ? Al1 C11 C7 C8 61.4(3) . . . . ? C10 C11 C7 C12 173.9(4) . . . . ? C16 C11 C7 C12 -3.7(8) . . . . ? Al1 C11 C7 C12 -121.6(5) . . . . ? C10 C11 C7 Al1 -64.6(3) . . . . ? C16 C11 C7 Al1 117.9(5) . . . . ? C9 C8 C7 C11 1.9(5) . . . . ? C13 C8 C7 C11 -179.9(4) . . . . ? Al1 C8 C7 C11 -60.5(3) . . . . ? C9 C8 C7 C12 -175.0(4) . . . . ? C13 C8 C7 C12 3.2(8) . . . . ? Al1 C8 C7 C12 122.5(5) . . . . ? C9 C8 C7 Al1 62.4(3) . . . . ? C13 C8 C7 Al1 -119.4(5) . . . . ? N1 Al1 C7 C11 18.9(7) . . . . ? C9 Al1 C7 C11 80.3(3) . . . . ? C10 Al1 C7 C11 38.6(3) . . . . ? C8 Al1 C7 C11 118.6(4) . . . . ? I1 Al1 C7 C11 -135.0(3) . . . . ? N1 Al1 C7 C8 -99.7(6) . . . . ? C11 Al1 C7 C8 -118.6(4) . . . . ? C9 Al1 C7 C8 -38.3(3) . . . . ? C10 Al1 C7 C8 -80.0(3) . . . . ? I1 Al1 C7 C8 106.4(3) . . . . ? N1 Al1 C7 C12 138.4(6) . . . . ? C11 Al1 C7 C12 119.5(7) . . . . ? C9 Al1 C7 C12 -160.2(7) . . . . ? C10 Al1 C7 C12 158.1(7) . . . . ? C8 Al1 C7 C12 -121.9(7) . . . . ? I1 Al1 C7 C12 -15.5(6) . . . . ? C30 C29 C28 C27 -0.4(7) . . . . ? C33 C29 C28 C27 177.3(4) . . . . ? C26 C27 C28 C29 -0.9(7) . . . . ? C32 C27 C28 C29 179.2(4) . . . . ? C8 C9 C10 C11 -1.9(5) . . . . ? C14 C9 C10 C11 -179.6(4) . . . . ? Al1 C9 C10 C11 60.9(3) . . . . ? C8 C9 C10 C15 179.9(4) . . . . ? C14 C9 C10 C15 2.2(7) . . . . ? Al1 C9 C10 C15 -117.3(4) . . . . ? C8 C9 C10 Al1 -62.9(3) . . . . ? C14 C9 C10 Al1 119.4(5) . . . . ? C7 C11 C10 C9 3.1(5) . . . . ? C16 C11 C10 C9 -179.2(4) . . . . ? Al1 C11 C10 C9 -61.9(3) . . . . ? C7 C11 C10 C15 -178.8(4) . . . . ? C16 C11 C10 C15 -1.2(8) . . . . ? Al1 C11 C10 C15 116.2(5) . . . . ? C7 C11 C10 Al1 65.0(3) . . . . ? C16 C11 C10 Al1 -117.3(5) . . . . ? N1 Al1 C10 C9 -106.6(3) . . . . ? C11 Al1 C10 C9 118.1(4) . . . . ? C8 Al1 C10 C9 38.0(3) . . . . ? C7 Al1 C10 C9 80.1(3) . . . . ? I1 Al1 C10 C9 95.8(5) . . . . ? N1 Al1 C10 C11 135.3(3) . . . . ? C9 Al1 C10 C11 -118.1(4) . . . . ? C8 Al1 C10 C11 -80.2(3) . . . . ? C7 Al1 C10 C11 -38.0(3) . . . . ? I1 Al1 C10 C11 -22.3(6) . . . . ? N1 Al1 C10 C15 12.0(6) . . . . ? C11 Al1 C10 C15 -123.2(8) . . . . ? C9 Al1 C10 C15 118.6(7) . . . . ? C8 Al1 C10 C15 156.6(7) . . . . ? C7 Al1 C10 C15 -161.2(7) . . . . ? I1 Al1 C10 C15 -145.5(5) . . . . ? C60 C65 C64 C63 0.5(7) . . . . ? C68 C65 C64 C63 179.8(4) . . . . ? C62 C63 C64 C65 2.1(7) . . . . ? C67 C63 C64 C65 -176.8(4) . . . . ? C18 C17 C22 C21 3.3(6) . . . . ? C6 C17 C22 C21 -177.0(4) . . . . ? C18 C17 C22 C25 -173.5(4) . . . . ? C6 C17 C22 C25 6.2(6) . . . . ? C17 C22 C21 C20 -2.0(7) . . . . ? C25 C22 C21 C20 174.8(5) . . . . ? C19 C20 C21 C22 -0.9(7) . . . . ? C24 C20 C21 C22 177.9(5) . . . . ? C21 C20 C19 C18 2.4(7) . . . . ? C24 C20 C19 C18 -176.4(5) . . . . ? C17 C18 C19 C20 -1.0(7) . . . . ? C23 C18 C19 C20 178.1(4) . . . . ? C69 C70 C71 C72 171.1(14) . . . . ? C70 C71 C72 C73 -177.5(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.21 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.000 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.083 # Attachment '684338.cif' data_sgm1195m _database_code_depnum_ccdc_archive 'CCDC 684338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H36 Al2 I2' _chemical_formula_sum 'C22 H36 Al2 I2' _chemical_formula_weight 608.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.516(3) _cell_length_b 9.716(4) _cell_length_c 15.352(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.465(5) _cell_angle_gamma 90.00 _cell_volume 1269.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 157(2) _cell_measurement_reflns_used 4290 _cell_measurement_theta_min 6.766 _cell_measurement_theta_max 49.419 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 2.552 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 157(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5355 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 24.70 _reflns_number_total 2127 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0290P)^2^+0.5776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2127 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.043 _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 I1 I 0.117539(17) 0.917879(16) 0.097506(9) 0.03535(8) Uani 1 1 d . . . Al1 Al 0.16729(8) 0.92714(7) -0.08303(5) 0.03151(16) Uani 1 1 d . . . C2 C 0.3510(2) 0.7632(2) -0.14895(14) 0.0327(5) Uani 1 1 d . . . C3 C 0.2514(3) 0.7064(2) -0.08795(14) 0.0301(5) Uani 1 1 d . . . C5 C 0.0979(3) 0.7996(2) -0.20150(15) 0.0340(5) Uani 1 1 d . . . C6 C 0.2588(3) 0.8220(2) -0.21777(15) 0.0345(5) Uani 1 1 d . . . C7 C 0.5277(3) 0.7649(3) -0.1410(2) 0.0505(7) Uani 1 1 d . . . H7A H 0.5701 0.7054 -0.1859 0.076 Uiso 1 1 calc R . . H7B H 0.5627 0.7313 -0.0832 0.076 Uiso 1 1 calc R . . H7C H 0.5655 0.8592 -0.1488 0.076 Uiso 1 1 calc R . . C4 C 0.0916(2) 0.7287(2) -0.11989(15) 0.0305(5) Uani 1 1 d . . . C8 C 0.3011(3) 0.6236(3) -0.00861(17) 0.0462(6) Uani 1 1 d . . . H8A H 0.3123 0.5267 -0.0250 0.069 Uiso 1 1 calc R . . H8B H 0.2213 0.6319 0.0353 0.069 Uiso 1 1 calc R . . H8C H 0.4019 0.6582 0.0155 0.069 Uiso 1 1 calc R . . C10 C -0.0404(3) 0.8300(3) -0.26256(18) 0.0534(7) Uani 1 1 d . . . H10A H -0.0505 0.7573 -0.3067 0.080 Uiso 1 1 calc R . . H10B H -0.0245 0.9188 -0.2912 0.080 Uiso 1 1 calc R . . H10C H -0.1363 0.8337 -0.2296 0.080 Uiso 1 1 calc R . . C1 C 0.3148(3) 1.0793(2) -0.08591(18) 0.0385(6) Uani 1 1 d . . . H1A H 0.3162 1.1161 -0.1453 0.058 Uiso 1 1 calc R . . H1B H 0.4202 1.0467 -0.0679 0.058 Uiso 1 1 calc R . . H1C H 0.2826 1.1517 -0.0460 0.058 Uiso 1 1 calc R . . C9 C -0.0523(3) 0.6639(3) -0.08321(19) 0.0458(6) Uani 1 1 d . . . H9A H -0.0725 0.5748 -0.1114 0.069 Uiso 1 1 calc R . . H9B H -0.1431 0.7245 -0.0941 0.069 Uiso 1 1 calc R . . H9C H -0.0349 0.6504 -0.0203 0.069 Uiso 1 1 calc R . . C11 C 0.3190(4) 0.9013(3) -0.29325(19) 0.0554(8) Uani 1 1 d . . . H11A H 0.3023 0.8476 -0.3469 0.083 Uiso 1 1 calc R . . H11B H 0.4316 0.9191 -0.2832 0.083 Uiso 1 1 calc R . . H11C H 0.2626 0.9889 -0.2990 0.083 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 I1 0.03885(12) 0.03739(12) 0.02966(11) 0.00082(6) -0.00040(7) 0.00823(6) Al1 0.0335(4) 0.0275(4) 0.0335(4) -0.0020(3) 0.0011(3) -0.0036(3) C2 0.0270(11) 0.0313(12) 0.0400(13) -0.0091(10) 0.0026(9) -0.0021(9) C3 0.0314(11) 0.0265(11) 0.0322(11) -0.0030(9) -0.0014(9) 0.0026(9) C5 0.0388(12) 0.0303(11) 0.0322(12) -0.0072(9) -0.0062(9) 0.0047(9) C6 0.0430(13) 0.0293(12) 0.0317(11) -0.0046(9) 0.0076(9) -0.0024(10) C7 0.0273(12) 0.0628(18) 0.0617(17) -0.0171(14) 0.0045(11) -0.0052(12) C4 0.0261(10) 0.0282(11) 0.0372(12) -0.0042(9) 0.0028(9) -0.0012(9) C8 0.0572(16) 0.0404(14) 0.0404(14) 0.0016(12) -0.0040(12) 0.0149(13) C10 0.0575(17) 0.0566(17) 0.0444(15) -0.0153(13) -0.0191(12) 0.0193(14) C1 0.0382(13) 0.0349(13) 0.0427(14) -0.0013(10) 0.0034(11) -0.0053(10) C9 0.0351(13) 0.0397(14) 0.0636(17) -0.0077(13) 0.0124(12) -0.0098(11) C11 0.083(2) 0.0433(15) 0.0416(16) 0.0012(12) 0.0212(15) -0.0065(14) _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 I1 Al1 2.8231(13) . ? I1 Al1 2.8556(11) 3_575 ? Al1 C1 1.942(2) . ? Al1 C4 2.103(2) . ? Al1 C5 2.258(2) . ? Al1 C3 2.263(2) . ? Al1 C6 2.464(2) . ? Al1 C2 2.479(2) . ? Al1 I1 2.8556(11) 3_575 ? C2 C3 1.403(3) . ? C2 C6 1.410(3) . ? C2 C7 1.505(3) . ? C3 C4 1.444(3) . ? C3 C8 1.505(3) . ? C5 C6 1.420(3) . ? C5 C4 1.433(3) . ? C5 C10 1.503(3) . ? C6 C11 1.500(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C4 C9 1.508(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 Al1 I1 Al1 93.99(2) . 3_575 ? C1 Al1 C4 152.01(10) . . ? C1 Al1 C5 123.12(11) . . ? C4 Al1 C5 38.16(9) . . ? C1 Al1 C3 120.96(10) . . ? C4 Al1 C3 38.39(8) . . ? C5 Al1 C3 61.67(9) . . ? C1 Al1 C6 93.91(10) . . ? C4 Al1 C6 59.88(8) . . ? C5 Al1 C6 34.65(8) . . ? C3 Al1 C6 57.78(8) . . ? C1 Al1 C2 93.41(10) . . ? C4 Al1 C2 59.51(8) . . ? C5 Al1 C2 57.75(8) . . ? C3 Al1 C2 34.03(8) . . ? C6 Al1 C2 33.14(8) . . ? C1 Al1 I1 99.86(9) . . ? C4 Al1 I1 100.24(7) . . ? C5 Al1 I1 136.73(7) . . ? C3 Al1 I1 93.65(6) . . ? C6 Al1 I1 151.32(6) . . ? C2 Al1 I1 120.28(6) . . ? C1 Al1 I1 98.35(9) . 3_575 ? C4 Al1 I1 102.29(7) . 3_575 ? C5 Al1 I1 91.99(6) . 3_575 ? C3 Al1 I1 140.01(6) . 3_575 ? C6 Al1 I1 116.86(7) . 3_575 ? C2 Al1 I1 148.87(6) . 3_575 ? I1 Al1 I1 86.01(2) . 3_575 ? C3 C2 C6 109.06(19) . . ? C3 C2 C7 125.5(2) . . ? C6 C2 C7 125.4(2) . . ? C3 C2 Al1 64.54(12) . . ? C6 C2 Al1 72.83(13) . . ? C7 C2 Al1 127.31(16) . . ? C2 C3 C4 107.61(19) . . ? C2 C3 C8 126.4(2) . . ? C4 C3 C8 125.7(2) . . ? C2 C3 Al1 81.44(13) . . ? C4 C3 Al1 64.77(12) . . ? C8 C3 Al1 123.91(16) . . ? C6 C5 C4 107.5(2) . . ? C6 C5 C10 126.6(2) . . ? C4 C5 C10 125.6(2) . . ? C6 C5 Al1 80.62(14) . . ? C4 C5 Al1 65.04(12) . . ? C10 C5 Al1 124.44(17) . . ? C2 C6 C5 108.5(2) . . ? C2 C6 C11 126.1(2) . . ? C5 C6 C11 125.4(2) . . ? C2 C6 Al1 74.03(13) . . ? C5 C6 Al1 64.73(12) . . ? C11 C6 Al1 124.51(17) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C4 C3 107.37(19) . . ? C5 C4 C9 126.1(2) . . ? C3 C4 C9 125.5(2) . . ? C5 C4 Al1 76.81(13) . . ? C3 C4 Al1 76.84(13) . . ? C9 C4 Al1 121.80(16) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 Al1 I1 Al1 C1 97.79(9) 3_575 . . . ? Al1 I1 Al1 C4 -101.78(7) 3_575 . . . ? Al1 I1 Al1 C5 -88.66(10) 3_575 . . . ? Al1 I1 Al1 C3 -139.92(6) 3_575 . . . ? Al1 I1 Al1 C6 -144.69(13) 3_575 . . . ? Al1 I1 Al1 C2 -162.33(7) 3_575 . . . ? Al1 I1 Al1 I1 0.0 3_575 . . 3_575 ? C1 Al1 C2 C3 146.36(15) . . . . ? C4 Al1 C2 C3 -41.12(14) . . . . ? C5 Al1 C2 C3 -86.09(15) . . . . ? C6 Al1 C2 C3 -121.71(19) . . . . ? I1 Al1 C2 C3 42.85(14) . . . . ? I1 Al1 C2 C3 -101.31(15) 3_575 . . . ? C1 Al1 C2 C6 -91.93(15) . . . . ? C4 Al1 C2 C6 80.59(14) . . . . ? C5 Al1 C2 C6 35.62(13) . . . . ? C3 Al1 C2 C6 121.71(19) . . . . ? I1 Al1 C2 C6 164.57(11) . . . . ? I1 Al1 C2 C6 20.40(19) 3_575 . . . ? C1 Al1 C2 C7 29.8(2) . . . . ? C4 Al1 C2 C7 -157.6(3) . . . . ? C5 Al1 C2 C7 157.4(3) . . . . ? C3 Al1 C2 C7 -116.5(3) . . . . ? C6 Al1 C2 C7 121.8(3) . . . . ? I1 Al1 C2 C7 -73.7(2) . . . . ? I1 Al1 C2 C7 142.16(19) 3_575 . . . ? C6 C2 C3 C4 0.7(2) . . . . ? C7 C2 C3 C4 179.0(2) . . . . ? Al1 C2 C3 C4 60.00(14) . . . . ? C6 C2 C3 C8 174.5(2) . . . . ? C7 C2 C3 C8 -7.2(4) . . . . ? Al1 C2 C3 C8 -126.2(2) . . . . ? C6 C2 C3 Al1 -59.30(16) . . . . ? C7 C2 C3 Al1 119.0(2) . . . . ? C1 Al1 C3 C2 -40.16(18) . . . . ? C4 Al1 C3 C2 114.15(19) . . . . ? C5 Al1 C3 C2 73.45(14) . . . . ? C6 Al1 C3 C2 33.35(12) . . . . ? I1 Al1 C3 C2 -143.95(12) . . . . ? I1 Al1 C3 C2 127.92(12) 3_575 . . . ? C1 Al1 C3 C4 -154.31(15) . . . . ? C5 Al1 C3 C4 -40.70(13) . . . . ? C6 Al1 C3 C4 -80.80(14) . . . . ? C2 Al1 C3 C4 -114.15(19) . . . . ? I1 Al1 C3 C4 101.90(12) . . . . ? I1 Al1 C3 C4 13.77(17) 3_575 . . . ? C1 Al1 C3 C8 88.3(2) . . . . ? C4 Al1 C3 C8 -117.4(3) . . . . ? C5 Al1 C3 C8 -158.1(2) . . . . ? C6 Al1 C3 C8 161.8(2) . . . . ? C2 Al1 C3 C8 128.5(3) . . . . ? I1 Al1 C3 C8 -15.5(2) . . . . ? I1 Al1 C3 C8 -103.6(2) 3_575 . . . ? C1 Al1 C5 C6 36.82(18) . . . . ? C4 Al1 C5 C6 -114.38(19) . . . . ? C3 Al1 C5 C6 -73.42(14) . . . . ? C2 Al1 C5 C6 -34.06(13) . . . . ? I1 Al1 C5 C6 -135.58(13) . . . . ? I1 Al1 C5 C6 138.13(13) 3_575 . . . ? C1 Al1 C5 C4 151.20(14) . . . . ? C3 Al1 C5 C4 40.96(13) . . . . ? C6 Al1 C5 C4 114.38(19) . . . . ? C2 Al1 C5 C4 80.32(14) . . . . ? I1 Al1 C5 C4 -21.20(17) . . . . ? I1 Al1 C5 C4 -107.49(12) 3_575 . . . ? C1 Al1 C5 C10 -91.5(3) . . . . ? C4 Al1 C5 C10 117.3(3) . . . . ? C3 Al1 C5 C10 158.3(3) . . . . ? C6 Al1 C5 C10 -128.3(3) . . . . ? C2 Al1 C5 C10 -162.4(3) . . . . ? I1 Al1 C5 C10 96.1(2) . . . . ? I1 Al1 C5 C10 9.8(2) 3_575 . . . ? C3 C2 C6 C5 -1.3(3) . . . . ? C7 C2 C6 C5 -179.7(2) . . . . ? Al1 C2 C6 C5 -55.69(16) . . . . ? C3 C2 C6 C11 175.7(2) . . . . ? C7 C2 C6 C11 -2.6(4) . . . . ? Al1 C2 C6 C11 121.4(2) . . . . ? C3 C2 C6 Al1 54.35(15) . . . . ? C7 C2 C6 Al1 -124.0(2) . . . . ? C4 C5 C6 C2 1.5(3) . . . . ? C10 C5 C6 C2 -172.3(2) . . . . ? Al1 C5 C6 C2 61.42(17) . . . . ? C4 C5 C6 C11 -175.6(2) . . . . ? C10 C5 C6 C11 10.6(4) . . . . ? Al1 C5 C6 C11 -115.7(2) . . . . ? C4 C5 C6 Al1 -59.97(15) . . . . ? C10 C5 C6 Al1 126.3(3) . . . . ? C1 Al1 C6 C2 90.25(15) . . . . ? C4 Al1 C6 C2 -79.37(14) . . . . ? C5 Al1 C6 C2 -120.0(2) . . . . ? C3 Al1 C6 C2 -34.24(12) . . . . ? I1 Al1 C6 C2 -28.6(2) . . . . ? I1 Al1 C6 C2 -168.34(11) 3_575 . . . ? C1 Al1 C6 C5 -149.79(15) . . . . ? C4 Al1 C6 C5 40.59(14) . . . . ? C3 Al1 C6 C5 85.72(15) . . . . ? C2 Al1 C6 C5 120.0(2) . . . . ? I1 Al1 C6 C5 91.35(18) . . . . ? I1 Al1 C6 C5 -48.39(15) 3_575 . . . ? C1 Al1 C6 C11 -32.9(3) . . . . ? C4 Al1 C6 C11 157.5(3) . . . . ? C5 Al1 C6 C11 116.9(3) . . . . ? C3 Al1 C6 C11 -157.4(3) . . . . ? C2 Al1 C6 C11 -123.1(3) . . . . ? I1 Al1 C6 C11 -151.8(2) . . . . ? I1 Al1 C6 C11 68.5(2) 3_575 . . . ? C6 C5 C4 C3 -1.0(2) . . . . ? C10 C5 C4 C3 172.8(2) . . . . ? Al1 C5 C4 C3 -71.44(15) . . . . ? C6 C5 C4 C9 -169.7(2) . . . . ? C10 C5 C4 C9 4.2(4) . . . . ? Al1 C5 C4 C9 119.9(2) . . . . ? C6 C5 C4 Al1 70.42(16) . . . . ? C10 C5 C4 Al1 -115.7(2) . . . . ? C2 C3 C4 C5 0.2(2) . . . . ? C8 C3 C4 C5 -173.7(2) . . . . ? Al1 C3 C4 C5 71.41(15) . . . . ? C2 C3 C4 C9 168.9(2) . . . . ? C8 C3 C4 C9 -5.0(4) . . . . ? Al1 C3 C4 C9 -119.9(2) . . . . ? C2 C3 C4 Al1 -71.20(16) . . . . ? C8 C3 C4 Al1 114.9(2) . . . . ? C1 Al1 C4 C5 -59.3(3) . . . . ? C3 Al1 C4 C5 -111.70(18) . . . . ? C6 Al1 C4 C5 -36.78(13) . . . . ? C2 Al1 C4 C5 -75.36(14) . . . . ? I1 Al1 C4 C5 165.41(12) . . . . ? I1 Al1 C4 C5 77.31(12) 3_575 . . . ? C1 Al1 C4 C3 52.4(3) . . . . ? C5 Al1 C4 C3 111.70(18) . . . . ? C6 Al1 C4 C3 74.92(14) . . . . ? C2 Al1 C4 C3 36.34(12) . . . . ? I1 Al1 C4 C3 -82.89(12) . . . . ? I1 Al1 C4 C3 -170.99(11) 3_575 . . . ? C1 Al1 C4 C9 176.2(2) . . . . ? C5 Al1 C4 C9 -124.5(3) . . . . ? C3 Al1 C4 C9 123.8(3) . . . . ? C6 Al1 C4 C9 -161.3(2) . . . . ? C2 Al1 C4 C9 160.1(2) . . . . ? I1 Al1 C4 C9 40.9(2) . . . . ? I1 Al1 C4 C9 -47.2(2) 3_575 . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.368 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.062